data_020_CoGF_0GPa _audit_creation_method ; XIA2 0.5.438-g5f426072-dials-1.7 SHELXL-2017/1 ; _audit_creation_date 2018-08-01 _publ_contact_author_address ; School of Physics and Astronomy Queen Mary University of London Mile End Rd, London E1 4NS U.K. ; _publ_contact_author_email a.e.phillips@qmul.ac.uk _publ_contact_author_name 'Anthony E. Phillips' _publ_contact_author_phone '+44 2078 823 429' _chemical_name_systematic 'guanidinium cobalt(II) formate' _chemical_name_common 'guanidinium cobalt(II) formate' _chemical_formula_moiety 'C3 H3 Co O6, C H6 N3' _chemical_formula_sum 'C4 H9 Co N3 O6' _chemical_formula_weight 254.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.2660 0.4750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_H-M_alt 'P n n a' _space_group_name_Hall '-P 2a 2bc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 8.319(8) _cell_length_b 11.735(5) _cell_length_c 8.920(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 870.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 526 _cell_measurement_theta_max 19.6723280156 _cell_measurement_theta_min 1.96351651763 _exptl_crystal_description block _exptl_crystal_colour 'intense pink' _exptl_crystal_density_diffrn 1.938 _exptl_crystal_F_000 516 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_T_min 0.999665587943 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CCP4 7.0.044: AIMLESS, version 0.5.32 : 29/03/17 Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 0 _diffrn_radiation_wavelength 0.4859 _diffrn_radiation_type 'Synchrotron' _diffrn_radiation_source 'Diamond Light Source Beamline I19' _diffrn_radiation_monochromator 'double crystal Silicon 111' _diffrn_measurement_specimen_support 'diamond anvil cell' _diffrn_measurement_device 'Newport IS4CCD (4 circle)' _diffrn_measurement_device_type 'Pilatus 300K' _diffrn_measurement_method ; \w scans with 0.2 degree frames ; _diffrn_reflns_number 1511 _diffrn_reflns_av_unetI/netI 0.0954 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.289 _diffrn_reflns_theta_max 17.695 _diffrn_reflns_theta_full 16.950 _diffrn_measured_fraction_theta_max 0.442 _diffrn_measured_fraction_theta_full 0.466 _diffrn_reflns_Laue_measured_fraction_max 0.442 _diffrn_reflns_Laue_measured_fraction_full 0.466 _diffrn_reflns_point_group_measured_fraction_max 0.442 _diffrn_reflns_point_group_measured_fraction_full 0.466 _reflns_number_total 399 _reflns_number_gt 201 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_reduction ; aimless (Evans, P. R. and Murshudov, G. N., 2013) ccp4 (Winn, M. D. et al., 2011) DIALS 1.7.3-gc8f60bf0-release pointless (Evans, P., 2006) XIA2 0.5.438-g5f426072-dials-1.7 (Winter, G., 2010) ; _publ_section_references ; Evans, P. (2006) Acta Cryst. D62, 72-82. Evans, P. R. and Murshudov, G. N. (2013) Acta Cryst. D69, 1204-1214. Winn, M. D. et al. (2011) Acta Cryst. D67, 235-242. Winter, G. (2010) J. Appl. Cryst. 43, 186-190. ; _computing_cell_refinement 'DIALS 2theta refinement, DIALS 1.7.3-gc8f60bf0-release' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 399 _refine_ls_number_parameters 66 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.835 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2536(3) 0.250000 0.250000 0.0161(5) Uani 1 2 d S T P . . O21 O 0.4057(9) 0.1827(5) 0.4131(5) 0.026(2) Uani 1 1 d . . . . . C21 C 0.5236(12) 0.2218(6) 0.4833(8) 0.021(3) Uani 1 1 d . . . . . H21 H 0.584506 0.277636 0.435928 0.025 Uiso 1 1 calc R U . . . O22 O 0.5664(8) 0.1920(5) 0.6116(5) 0.0268(19) Uani 1 1 d . . . . . O31 O 0.2552(9) 0.4052(4) 0.3655(5) 0.0253(17) Uani 1 1 d . . . . . C31 C 0.250000 0.500000 0.3024(11) 0.022(4) Uani 1 2 d S T P . . H31 H 0.249997 0.500000 0.198165 0.026 Uiso 1 2 calc R U P . . N41 N 0.250000 0.500000 0.9049(9) 0.022(3) Uani 1 2 d S TU P . . H41A H 0.190633 0.547507 0.953062 0.027 Uiso 0.5 1 calc R U P . . H41B H 0.309367 0.452493 0.953062 0.027 Uiso 0.5 1 calc R U P . . C41 C 0.250000 0.500000 0.7560(13) 0.023(3) Uani 1 2 d S T P . . N42 N 0.3417(11) 0.4266(6) 0.6834(7) 0.035(2) Uani 1 1 d . . . . . H42A H 0.342430 0.426045 0.586965 0.042 Uiso 1 1 calc R U . . . H42B H 0.400690 0.379421 0.732470 0.042 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0199(14) 0.0158(7) 0.0127(9) 0.0003(6) 0.000 0.000 O21 0.031(6) 0.028(4) 0.018(3) 0.003(3) -0.011(3) 0.000(4) C21 0.016(8) 0.028(5) 0.019(4) 0.011(4) 0.004(4) -0.006(5) O22 0.024(6) 0.037(4) 0.020(3) 0.000(3) -0.005(2) 0.003(4) O31 0.041(6) 0.012(2) 0.023(3) -0.002(2) -0.004(3) 0.001(4) C31 0.027(13) 0.021(5) 0.017(7) 0.000 0.000 -0.001(8) N41 0.010(10) 0.035(5) 0.023(4) 0.000 0.000 0.018(7) C41 0.030(10) 0.014(5) 0.026(5) 0.000 0.000 -0.002(8) N42 0.053(8) 0.039(5) 0.013(5) -0.011(3) -0.003(3) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O21 2.083(6) 4 ? Co1 O21 2.083(6) . ? Co1 O31 2.092(4) 4 ? Co1 O31 2.092(4) . ? Co1 O22 2.101(6) 7_565 ? Co1 O22 2.101(6) 6_556 ? O21 C21 1.250(10) . ? C21 O22 1.249(7) . ? C21 H21 0.9300 . ? O31 C31 1.248(6) . ? C31 H31 0.9300 . ? N41 C41 1.328(12) . ? N41 H41A 0.8600 . ? N41 H41B 0.8600 . ? C41 N42 1.320(8) 2_565 ? C41 N42 1.320(8) . ? N42 H42A 0.8600 . ? N42 H42B 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Co1 O21 105.2(4) 4 . ? O21 Co1 O31 89.0(2) 4 4 ? O21 Co1 O31 90.6(2) . 4 ? O21 Co1 O31 90.6(2) 4 . ? O21 Co1 O31 89.0(2) . . ? O31 Co1 O31 179.3(4) 4 . ? O21 Co1 O22 85.3(3) 4 7_565 ? O21 Co1 O22 169.5(3) . 7_565 ? O31 Co1 O22 89.8(3) 4 7_565 ? O31 Co1 O22 90.7(2) . 7_565 ? O21 Co1 O22 169.5(3) 4 6_556 ? O21 Co1 O22 85.3(3) . 6_556 ? O31 Co1 O22 90.7(2) 4 6_556 ? O31 Co1 O22 89.8(3) . 6_556 ? O22 Co1 O22 84.3(4) 7_565 6_556 ? C21 O21 Co1 133.4(5) . . ? O22 C21 O21 125.5(8) . . ? O22 C21 H21 117.3 . . ? O21 C21 H21 117.3 . . ? C21 O22 Co1 131.3(6) . 6_656 ? C31 O31 Co1 123.7(5) . . ? O31 C31 O31 126.4(9) . 2_565 ? O31 C31 H31 116.8 . . ? O31 C31 H31 116.8 2_565 . ? C41 N41 H41A 120.0 . . ? C41 N41 H41B 120.0 . . ? H41A N41 H41B 120.0 . . ? N42 C41 N42 121.2(12) 2_565 . ? N42 C41 N41 119.4(6) 2_565 . ? N42 C41 N41 119.4(6) . . ? C41 N42 H42A 120.0 . . ? C41 N42 H42B 120.0 . . ? H42A N42 H42B 120.0 . . ? _refine_diff_density_max 0.523 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.091 _shelx_res_file ; TITL CoGF 0 GPa in Pnna 020_CoGF_0GPa.res created by SHELXL-2017/1 at 14:12:35 on 01-Aug-2018 CELL 0.4859 8.3186 11.7352 8.92 90 90 90 ZERR 4 0.0077 0.0052 0.004 0 0 0 LATT 1 SYMM 0.5-X,-Y,+Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +X,0.5-Y,0.5-Z SFAC C H Co N O DISP C 0.001 0.001 6.068 DISP Co 0.266 0.475 1359.652 DISP H -0 0 0.607 DISP N 0.002 0.001 8.983 DISP O 0.004 0.003 13.336 UNIT 16 36 4 12 24 RIGU L.S. 10 PLAN 15 BOND $H LIST 3 FMAP 2 ACTA OMIT 7 2 7 RIGU ISOR 0.05 N41 WGHT 0.041100 FVAR 0.58097 CO1 3 0.253646 0.250000 0.250000 10.50000 0.01991 0.01579 = 0.01272 0.00033 0.00000 0.00000 O21 5 0.405736 0.182737 0.413060 11.00000 0.03075 0.02847 = 0.01798 0.00255 -0.01086 0.00016 C21 1 0.523599 0.221766 0.483271 11.00000 0.01605 0.02800 = 0.01853 0.01117 0.00374 -0.00577 AFIX 43 H21 2 0.584506 0.277636 0.435928 11.00000 -1.20000 AFIX 0 O22 5 0.566396 0.192032 0.611609 11.00000 0.02400 0.03678 = 0.01974 0.00045 -0.00470 0.00297 O31 5 0.255215 0.405178 0.365476 11.00000 0.04112 0.01166 = 0.02301 -0.00205 -0.00430 0.00079 C31 1 0.250000 0.500000 0.302425 10.50000 0.02727 0.02088 = 0.01670 0.00000 0.00000 -0.00108 AFIX 43 H31 2 0.249997 0.500000 0.198165 10.50000 -1.20000 AFIX 0 N41 4 0.250000 0.500000 0.904856 10.50000 0.00951 0.03464 = 0.02251 0.00000 0.00000 0.01813 AFIX 93 H41A 2 0.190633 0.547507 0.953062 10.50000 -1.20000 H41B 2 0.309367 0.452493 0.953062 10.50000 -1.20000 AFIX 0 C41 1 0.250000 0.500000 0.755993 10.50000 0.02973 0.01392 = 0.02626 0.00000 0.00000 -0.00168 N42 4 0.341693 0.426631 0.683372 11.00000 0.05257 0.03887 = 0.01289 -0.01066 -0.00286 0.01453 AFIX 93 H42A 2 0.342430 0.426045 0.586965 11.00000 -1.20000 H42B 2 0.400690 0.379421 0.732470 11.00000 -1.20000 AFIX 0 HKLF 4 REM CoGF 0 GPa in Pnna REM R1 = 0.0387 for 201 Fo > 4sig(Fo) and 0.0866 for all 399 data REM 66 parameters refined using 42 restraints END WGHT 0.0377 0.0000 REM Highest difference peak 0.523, deepest hole -0.396, 1-sigma level 0.091 Q1 1 0.2496 0.3418 0.2495 11.00000 0.05 0.52 Q2 1 0.3405 0.2452 0.3880 11.00000 0.05 0.41 Q3 1 0.6582 0.2467 0.6155 11.00000 0.05 0.41 Q4 1 0.6031 0.1228 0.7550 11.00000 0.05 0.38 Q5 1 0.2537 0.2008 0.3840 11.00000 0.05 0.32 Q6 1 0.6723 0.1591 0.6779 11.00000 0.05 0.31 Q7 1 0.4055 0.1317 0.2509 11.00000 0.05 0.30 Q8 1 0.2493 0.4307 0.7437 11.00000 0.05 0.29 Q9 1 0.5069 0.5017 0.7520 11.00000 0.05 0.28 Q10 1 0.5881 0.2614 0.6810 11.00000 0.05 0.28 Q11 1 0.3303 0.1626 0.3227 11.00000 0.05 0.28 Q12 1 0.4194 0.2504 0.4353 11.00000 0.05 0.27 Q13 1 0.4003 0.3683 0.8679 11.00000 0.05 0.25 Q14 1 0.0717 0.4500 0.9110 11.00000 0.05 0.25 Q15 1 0.0026 0.5607 1.0021 11.00000 0.05 0.24 ; _shelx_res_checksum 34091 _shelx_hkl_file ; 0 1 -2 2.25 10.85 0 -1 2 4.73 6.28 0 1 -3 1422.28 129.28 0 2 0 3292.08 215.40 0 2 0 3440.40 239.13 0 2 0 3197.18 244.52 0 -2 0 3475.28 334.67 0 -2 0 2910.07 285.74 0 -2 0 3450.22 239.29 0 2 1 3.02 6.45 0 2 1 5.68 16.97 0 -2 -1 -11.89 12.33 0 2 -1 -3.00 2.38 0 2 -1 -5.54 6.91 0 -2 1 1.88 7.50 0 -2 1 0.92 5.47 0 -2 1 -6.74 5.52 0 2 -2 14.79 12.34 0 -2 2 11.31 12.65 0 -2 2 11.82 7.56 0 2 -3 0.81 20.32 0 -2 3 -4.30 11.68 0 2 -4 1324.32 124.30 0 -2 4 1339.26 135.71 0 3 0 -0.75 6.32 0 3 0 -12.54 12.90 0 3 0 -5.56 6.98 0 -3 0 1.71 7.24 0 -3 0 6.85 14.44 0 3 1 1605.05 122.39 0 3 1 1590.66 203.34 0 -3 -1 1736.54 125.53 0 3 -1 1707.52 115.42 0 3 -1 1743.70 122.67 0 -3 1 1767.14 118.59 0 -3 1 1679.70 114.80 0 -3 1 1705.60 112.91 0 3 2 2.95 34.10 0 3 -2 -6.06 14.03 0 -3 2 7.39 16.01 0 -3 2 2.77 9.67 0 3 -4 -9.44 28.24 0 -3 4 -25.90 30.75 0 -3 4 -3.25 17.72 0 3 -5 103.38 41.48 0 -3 6 0.00 42.39 0 4 0 4331.86 287.32 0 4 0 4724.91 307.12 0 4 0 4505.48 316.13 0 -4 0 4040.43 332.72 0 -4 0 4160.25 306.45 0 4 1 -10.21 12.24 0 4 1 0.62 22.50 0 -4 -1 7.74 25.59 0 4 -1 -13.92 8.61 0 4 -1 -15.85 16.61 0 4 -1 -12.22 11.83 0 -4 1 7.65 14.41 0 -4 1 -1.11 5.74 0 -4 1 0.70 11.84 0 -4 1 1.64 17.98 0 4 2 1417.11 131.60 0 -4 -2 1363.68 118.39 0 4 -2 1484.40 117.18 0 4 -2 1448.64 106.87 0 -4 2 1512.01 106.61 0 -4 2 1447.26 98.75 0 4 -3 3.42 22.38 0 -4 3 -12.21 17.53 0 4 -4 3229.50 250.83 0 -4 4 3607.48 279.29 0 -4 4 3595.88 252.92 0 4 -5 -8.28 39.43 0 -4 5 -15.17 43.30 0 -4 5 0.00 23.14 0 4 -6 1264.27 131.55 0 -4 6 1067.29 117.73 0 5 0 -2.89 13.64 0 5 0 -44.73 24.87 0 5 0 0.43 15.40 0 -5 0 -16.36 16.47 0 -5 0 6.70 29.23 0 5 2 2.88 37.22 0 5 -2 1.52 10.63 0 -5 2 -32.33 22.88 0 5 -3 662.06 60.65 0 -5 3 658.60 60.27 0 -5 3 623.53 51.93 0 5 -5 607.17 67.63 0 -5 5 509.29 62.79 0 -5 5 569.66 57.74 0 5 -6 -41.76 55.07 0 -5 6 5.46 47.48 0 -5 6 -47.88 30.92 0 6 0 1346.83 94.43 0 6 0 1291.36 103.60 0 6 0 1246.73 101.09 0 -6 0 1209.42 95.65 0 -6 0 1247.85 105.66 0 -6 -1 -13.91 22.67 0 6 -1 0.64 14.37 0 6 -1 6.47 30.68 0 6 -1 1.75 20.73 0 -6 1 -32.99 20.80 0 -6 1 0.35 19.30 0 -6 1 -33.37 33.07 0 6 2 1743.41 159.98 0 6 2 1711.72 161.54 0 -6 -2 1830.25 152.26 0 6 -2 1778.07 117.58 0 6 -2 1891.52 137.19 0 6 -2 1824.50 148.78 0 -6 2 1720.45 120.53 0 -6 2 1553.06 129.88 0 6 3 -34.29 48.57 0 6 -3 1.25 12.08 0 6 -3 14.56 32.31 0 -6 3 -2.62 21.50 0 6 -4 1281.58 108.83 0 -6 4 1252.51 103.85 0 -6 4 1256.66 96.58 0 6 -6 13.23 52.02 0 -6 6 32.35 47.10 0 -6 6 -15.75 30.81 0 6 -7 -87.39 67.40 0 -6 7 3.47 53.16 0 7 0 1.45 22.77 0 7 0 16.48 22.74 0 -7 0 18.26 23.41 0 -7 0 -34.30 47.93 0 7 1 4.47 25.54 0 7 1 5.14 43.30 0 -7 -1 -25.19 22.78 0 -7 -1 25.30 51.06 0 7 -1 -15.11 35.95 0 -7 1 0.00 41.53 0 7 3 272.20 66.30 0 7 -3 351.00 48.62 0 7 -3 306.30 47.63 0 -7 3 300.58 45.29 0 -7 3 370.27 37.71 0 7 -4 4.18 41.89 0 -7 4 -21.05 39.39 0 -7 4 2.66 28.28 0 7 -5 15.70 50.55 0 -7 5 -44.25 44.06 0 -7 5 11.63 31.34 0 8 0 278.90 54.72 0 8 0 424.73 48.48 0 -8 0 257.42 61.75 0 8 1 2.79 32.15 0 8 1 16.24 48.75 0 -8 -1 8.18 25.84 0 -8 -1 0.00 61.23 0 8 -1 1.02 25.07 0 8 -1 2.43 26.36 0 -8 1 10.62 26.62 0 -8 1 2.99 25.36 0 -8 1 30.87 51.29 0 8 2 1678.36 146.22 0 8 -2 1619.59 131.44 0 8 -2 1621.89 135.62 0 -8 2 1585.99 139.13 0 -8 2 1708.58 119.45 0 8 -4 2157.46 172.52 0 8 -4 1815.64 222.35 0 -8 4 2280.64 167.87 0 -8 4 2175.93 156.22 0 8 -6 426.76 76.87 0 -8 6 415.86 64.48 0 -8 6 444.99 55.12 0 9 2 -19.28 61.26 0 9 -2 18.36 39.06 0 9 -2 6.41 36.07 0 -9 2 5.96 33.70 0 -9 2 -31.10 29.51 0 9 -3 120.26 47.37 0 9 -3 101.83 41.00 0 -9 3 125.15 41.05 0 -9 3 73.41 31.58 0 9 -5 48.19 58.93 0 9 -5 69.79 43.48 0 -9 5 58.91 49.94 0 -9 5 50.25 36.24 0 9 -6 10.20 64.52 0 -9 6 -26.28 57.08 0 10 0 27.31 38.90 0 10 -2 559.73 67.37 0 10 -3 -0.13 48.01 0 10 -3 -98.35 48.96 0 -10 3 0.62 40.34 0 -10 3 0.14 31.51 0 10 -4 1116.29 112.90 0 10 -4 1136.43 114.11 0 -10 4 1198.84 109.98 0 -10 4 1283.92 99.34 0 -10 5 -23.78 51.44 0 11 -4 46.70 57.95 0 -11 4 -69.74 37.46 1 0 -1 5051.56 327.41 1 0 -1 4597.05 356.27 -1 0 1 5087.80 422.56 -1 0 1 5123.33 390.86 -1 0 1 4883.11 339.21 -1 0 1 3911.16 376.10 1 0 -2 -1.72 9.13 1 0 -2 -12.61 15.44 -1 0 2 0.10 9.35 -1 0 2 -2.14 6.12 -1 0 2 -8.01 12.41 -1 0 2 -9.04 7.71 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3 -7 30.64 47.53 4 -4 -1 97.19 23.08 -4 4 1 106.77 25.52 4 -4 -3 88.36 27.06 -4 4 3 121.91 31.12 -4 4 3 109.33 63.51 -4 -4 3 83.33 37.62 4 4 -3 152.82 42.46 4 -4 -4 2119.52 149.40 -4 4 4 1901.91 144.24 -4 4 4 1954.46 175.09 -4 -4 4 1803.46 154.18 4 4 -4 2221.12 167.82 4 -4 -5 15.71 26.74 -4 4 5 10.98 30.46 -4 4 5 -33.16 69.09 -4 -4 5 0.00 36.27 -4 -4 5 -0.01 41.56 4 4 -5 9.78 42.49 -4 -4 7 46.22 42.61 4 4 -7 20.02 54.60 4 4 -8 436.06 73.00 -4 5 1 63.56 27.96 4 -5 -2 7.32 24.12 -4 5 2 10.33 29.26 -4 5 2 11.58 61.74 4 -5 -3 -15.25 25.01 -4 5 3 -13.87 30.03 -4 5 3 -6.29 63.43 -4 -5 3 -19.45 38.39 4 5 -3 12.90 39.43 4 -5 -5 18.82 28.24 -4 5 5 2.83 33.81 -4 -5 5 9.41 37.12 -4 -5 5 6.63 45.58 4 5 -5 4.08 43.81 -4 -5 6 24.52 42.92 -4 -5 6 -39.61 43.39 4 5 -6 8.87 51.16 -4 6 0 1202.90 128.25 4 -6 -1 34.81 25.94 -4 6 1 40.95 30.66 -4 6 1 89.35 62.80 4 -6 -2 294.03 36.07 -4 6 2 229.85 38.45 -4 6 2 224.17 72.24 4 -6 -4 261.45 39.32 -4 6 4 361.78 45.74 -4 6 4 325.07 89.40 -4 -6 4 413.81 55.67 4 6 -4 285.32 57.80 -4 -6 6 309.91 61.19 4 6 -6 341.18 63.55 -4 -6 7 0.00 46.42 4 6 -7 -31.88 58.28 4 -7 -2 -31.39 29.65 -4 7 2 8.40 34.02 -4 7 2 30.59 71.22 4 -7 -3 6.48 28.62 -4 7 3 -0.02 34.76 -4 -7 3 24.41 45.31 4 7 -3 33.22 49.87 4 -7 -5 225.39 37.96 -4 -7 5 258.28 54.93 4 7 -5 157.01 58.27 4 -8 0 2070.23 163.64 -4 8 0 2083.45 159.96 -4 8 0 2118.88 231.91 4 -8 -1 12.57 30.43 -4 8 1 37.73 35.35 -4 8 -1 0.02 32.95 4 -8 -2 824.91 71.81 -4 8 2 755.72 73.23 4 -8 -4 441.26 51.73 -4 -8 4 450.00 63.30 4 8 -4 407.47 67.13 4 -9 -1 9.81 32.59 4 -9 -2 -17.49 33.84 4 -9 -3 70.68 35.80 -4 -9 3 120.85 53.57 4 9 -3 102.89 57.61 4 -9 -5 6.58 36.54 -4 -9 5 0.00 49.96 4 -10 0 53.71 34.06 4 -10 -1 3.23 35.99 4 -10 -4 601.80 64.52 4 -10 -5 0.00 38.28 4 -11 0 -40.27 36.65 4 -11 -1 92.63 39.76 4 -11 -3 22.06 40.39 4 -11 -4 8.35 38.49 4 -11 -6 10.23 40.93 4 -12 -2 563.42 63.67 4 -12 -4 190.14 46.39 4 -13 -2 20.36 46.74 5 0 -4 13.96 43.42 -5 0 4 12.03 27.56 -5 0 4 9.00 36.43 5 0 -5 25.99 27.43 5 0 -5 20.39 40.82 -5 0 5 25.48 30.58 -5 0 5 -71.82 65.42 -5 0 5 46.82 38.52 -5 1 3 50.92 25.32 5 -1 -4 107.07 28.22 -5 1 4 102.50 60.99 -5 1 4 70.31 34.74 -5 -1 4 115.75 28.66 -5 -1 4 68.91 40.53 5 -1 -5 7.51 26.55 5 -1 -5 -56.26 40.10 -5 1 5 4.57 30.93 -5 1 5 29.91 70.63 -5 1 5 -16.40 36.45 -5 -1 5 12.91 28.59 -5 -1 5 -91.75 54.87 -5 -1 5 -31.10 41.02 5 1 -5 3.93 25.08 5 1 -5 -29.87 45.69 5 -1 -6 36.15 50.54 5 -2 -3 599.36 54.18 -5 2 3 594.58 58.43 -5 2 3 376.69 70.42 -5 2 3 317.54 65.00 5 -2 -5 1104.14 85.51 5 -2 -5 1021.25 98.15 -5 2 5 936.91 83.77 -5 2 5 979.26 83.47 -5 -2 5 906.92 90.61 5 2 -5 1014.51 97.31 5 -2 -6 9.14 32.44 -5 -2 6 10.27 42.15 5 2 -6 8.66 51.12 5 -2 -8 41.09 36.36 -5 3 2 360.93 51.02 5 -3 -3 -20.63 27.43 -5 3 3 11.51 30.84 -5 3 3 35.82 63.20 -5 3 4 4.36 32.63 -5 3 4 12.55 68.45 -5 -3 4 17.66 42.82 5 3 -4 -85.43 52.99 5 -3 -5 18.61 31.46 -5 3 5 -5.18 35.44 -5 -3 5 22.41 44.71 5 3 -5 23.06 47.59 5 -3 -6 33.77 33.12 -5 -3 6 -6.85 44.82 5 3 -6 23.14 49.79 5 -3 -7 14.62 34.10 -5 -3 7 16.95 46.30 -5 -3 7 -36.73 46.83 5 -3 -9 17.29 37.38 5 -4 -2 28.70 26.92 -5 4 2 7.55 30.35 -5 4 2 39.41 57.44 5 -4 -4 2.85 30.27 -5 4 4 6.10 32.74 -5 4 4 13.00 75.43 -5 -4 4 -46.96 44.59 5 4 -4 3.73 48.23 5 -4 -6 6.16 32.90 -5 -4 6 -30.86 48.17 5 4 -6 0.01 50.01 5 -4 -8 1.17 35.15 5 -4 -9 95.19 38.61 5 -5 -3 0.99 29.55 -5 5 3 0.69 33.22 -5 5 3 13.46 75.55 5 -5 -4 7.18 31.40 -5 5 4 40.24 35.51 -5 -5 4 28.02 47.25 5 5 -4 13.91 51.28 5 -5 -5 21.33 33.57 -5 -5 5 49.75 49.53 5 5 -5 10.50 57.15 5 -5 -7 27.23 37.08 5 -5 -8 -5.25 36.36 5 -5 -9 -29.26 40.50 -5 6 1 1319.09 123.54 5 -6 -2 7.30 31.26 -5 6 2 0.00 68.38 5 -6 -3 627.26 61.47 -5 6 3 654.50 65.51 5 6 -4 0.43 54.91 5 -6 -5 384.95 48.25 -5 -6 5 263.76 59.33 5 6 -5 274.74 64.79 -5 -6 6 -71.42 49.53 5 -6 -7 213.11 44.64 5 -7 -1 22.41 30.90 -5 7 1 43.96 38.01 5 -7 -2 0.00 33.43 -5 7 2 0.00 35.28 5 -7 -3 -41.45 34.82 5 -7 -4 0.00 33.87 -5 -7 4 1.93 52.68 5 7 -4 42.08 61.03 5 -7 -6 0.00 38.81 5 -7 -7 20.36 38.13 5 -7 -8 58.87 40.81 5 -8 -1 230.22 45.27 5 -8 -2 -7.97 36.30 5 -8 -3 816.43 75.85 5 -8 -5 498.50 58.57 5 -8 -6 12.59 40.65 5 -8 -7 101.93 44.66 5 -9 -1 13.02 36.91 5 -9 -4 5.91 39.39 5 -9 -5 4.32 41.26 5 -9 -7 -48.31 43.32 5 -10 -3 610.01 66.62 5 -10 -4 31.01 43.29 5 -10 -6 -11.77 43.80 5 -11 -2 0.00 39.25 5 -11 -3 9.70 43.31 5 -11 -5 -63.66 47.39 5 -12 -2 0.62 42.72 5 -12 -3 201.42 50.91 -6 0 4 24.70 31.10 -6 0 4 20.32 40.59 6 0 -5 39.37 53.94 -6 0 5 12.19 43.59 6 0 -6 1673.39 135.12 -6 1 4 -54.33 32.81 -6 1 4 2.69 38.34 6 -1 -5 28.29 34.74 -6 1 5 107.92 50.32 -6 -1 5 13.19 45.22 6 1 -5 16.21 53.75 6 -1 -7 22.28 36.18 6 -2 -4 320.01 40.25 -6 2 4 206.07 43.24 6 -2 -5 12.36 32.66 -6 -2 5 22.99 46.76 6 2 -5 48.08 57.76 6 -2 -7 0.00 34.89 -6 3 3 24.56 34.59 6 -3 -5 52.97 35.54 -6 -3 5 25.13 48.72 6 3 -5 18.35 60.05 6 -4 -3 15.29 30.89 -6 4 3 0.37 35.86 6 -4 -4 633.62 63.75 6 -4 -5 17.50 34.99 -6 -4 5 5.41 50.84 6 4 -5 9.24 64.30 6 -4 -7 16.34 40.98 6 -4 -8 12.18 43.24 6 -5 -4 -50.93 37.98 6 -5 -6 37.13 38.61 6 -5 -7 0.00 41.62 6 -5 -8 6.20 42.86 6 -6 -3 9.80 36.83 6 -6 -5 -8.95 38.58 -6 -6 5 26.06 54.63 6 -6 -6 133.19 45.33 6 -7 -2 17.30 35.80 6 -7 -4 6.16 38.38 6 -7 -5 13.37 40.34 6 -7 -6 38.44 44.21 6 -7 -7 14.60 44.83 6 -8 -3 -0.10 36.96 6 -8 -4 578.34 64.62 6 -8 -5 37.84 41.92 6 -8 -6 73.32 45.87 6 -9 -2 -24.88 39.66 6 -9 -3 -30.93 41.22 6 -9 -4 -12.32 42.59 6 -9 -6 20.24 47.72 6 -10 -2 184.57 46.19 6 -10 -3 -74.94 43.91 6 -10 -4 531.96 65.40 6 -10 -5 17.76 47.71 6 -11 -2 26.59 44.38 6 -11 -3 -55.84 47.13 7 -2 -7 105.10 42.13 7 -3 -6 15.18 38.57 7 -4 -5 276.56 48.37 7 -4 -6 24.64 40.21 7 -4 -7 19.00 41.55 7 -5 -4 5.54 36.99 7 -5 -5 22.62 41.56 7 -5 -6 2.28 40.55 7 -5 -7 8.04 42.42 7 -6 -4 30.70 39.78 7 -6 -5 127.45 44.40 7 -7 -4 -0.84 42.02 7 -7 -6 18.39 46.36 7 -8 -3 547.34 64.68 7 -8 -5 132.58 48.62 7 -9 -4 -39.89 45.94 7 -10 -3 287.01 54.07 8 -5 -6 5.13 45.23 8 -6 -5 15.57 41.18 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95220 data_022_CoGF_0-88GPa _audit_creation_method ; CrysAlisPro 1.171.38.46 (Rigaku OD, 2015) SHELXL-2017/1 ; _audit_creation_date 2018-08-01 _publ_contact_author_address ; School of Physics and Astronomy Queen Mary University of London Mile End Rd, London E1 4NS U.K. ; _publ_contact_author_email a.e.phillips@qmul.ac.uk _publ_contact_author_name 'Anthony E. Phillips' _publ_contact_author_phone '+44 2078 823 429' _chemical_name_systematic 'guanidinium cobalt(II) formate' _chemical_name_common 'guanidinium cobalt(II) formate' _chemical_formula_moiety 'C3 H3 Co O6, C H6 N3' _chemical_formula_sum 'C4 H9 Co N3 O6' _chemical_formula_weight 254.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.2660 0.4750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_H-M_alt 'P n n a' _space_group_name_Hall '-P 2a 2bc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 8.220(4) _cell_length_b 11.644(2) _cell_length_c 8.922(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 854.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 596 _cell_measurement_theta_min 1.9710 _cell_measurement_theta_max 20.8530 _exptl_crystal_description block _exptl_crystal_colour 'intense pink' _exptl_crystal_density_diffrn 1.976 _exptl_crystal_F_000 516 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_T_min 0.62695 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 880000 _diffrn_radiation_wavelength 0.4859 _diffrn_radiation_type 'Synchrotron' _diffrn_radiation_source 'Diamond Light Source Beamline I19' _diffrn_radiation_monochromator 'double crystal Silicon 111' _diffrn_measurement_specimen_support 'diamond anvil cell' _diffrn_measurement_device 'Newport IS4CCD (4 circle)' _diffrn_measurement_device_type 'Pilatus 300K' _diffrn_measurement_method ; \w scans with 0.2 degree frames ; _diffrn_reflns_number 2952 _diffrn_reflns_av_unetI/netI 0.1281 _diffrn_reflns_av_R_equivalents 0.1570 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.966 _diffrn_reflns_theta_max 17.668 _diffrn_reflns_theta_full 16.950 _diffrn_measured_fraction_theta_max 0.697 _diffrn_measured_fraction_theta_full 0.709 _diffrn_reflns_Laue_measured_fraction_max 0.697 _diffrn_reflns_Laue_measured_fraction_full 0.709 _diffrn_reflns_point_group_measured_fraction_max 0.697 _diffrn_reflns_point_group_measured_fraction_full 0.709 _reflns_number_total 613 _reflns_number_gt 315 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+20.9934P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 613 _refine_ls_number_parameters 66 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1691 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.2476 _refine_ls_wR_factor_gt 0.1980 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co01 Co 0.2597(4) 0.750000 0.250000 0.0208(8) Uani 1 2 d S T P . . O002 O 0.2613(15) 0.5950(6) 0.1313(11) 0.033(3) Uani 1 1 d . . . . . O003 O 0.4162(14) 0.6799(7) 0.4115(12) 0.033(3) Uani 1 1 d . . . . . O004 O 0.5701(14) 0.6904(8) 0.6104(11) 0.035(3) Uani 1 1 d . . . . . N005 N 0.250000 0.500000 0.5930(19) 0.030(4) Uani 1 2 d S T P . . H00A H 0.311064 0.547254 0.544761 0.036 Uiso 0.5 1 calc R U P . . H00B H 0.188936 0.452746 0.544760 0.036 Uiso 0.5 1 calc R U P . . N006 N 0.344(2) 0.5730(10) 0.8160(15) 0.043(4) Uani 1 1 d . . . . . H00C H 0.405724 0.620506 0.768487 0.051 Uiso 1 1 calc R U . . . H00D H 0.343766 0.572560 0.912355 0.051 Uiso 1 1 calc R U . . . C007 C 0.250000 0.500000 0.740(2) 0.025(4) Uani 1 2 d S T P . . C008 C 0.250000 0.500000 0.195(2) 0.037(6) Uani 1 2 d S T P . . H008 H 0.249997 0.500001 0.299204 0.044 Uiso 1 2 calc R U P . . C009 C 0.532(2) 0.7200(10) 0.4810(16) 0.028(4) Uani 1 1 d . . . . . H009 H 0.595011 0.775810 0.434191 0.034 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co01 0.038(2) 0.0173(10) 0.0072(16) 0.0002(9) 0.000 0.000 O002 0.067(10) 0.020(3) 0.011(6) -0.002(3) 0.003(5) -0.002(5) O003 0.046(9) 0.025(5) 0.027(6) 0.006(4) -0.012(4) -0.003(5) O004 0.050(10) 0.040(6) 0.014(6) 0.002(4) -0.008(4) -0.007(5) N005 0.049(15) 0.025(6) 0.017(7) 0.000 0.000 -0.001(9) N006 0.069(13) 0.045(6) 0.014(8) -0.003(5) 0.001(6) -0.018(7) C007 0.025(13) 0.032(7) 0.019(8) 0.000 0.000 -0.003(8) C008 0.07(2) 0.020(5) 0.016(12) 0.000 0.000 -0.005(9) C009 0.040(11) 0.029(6) 0.015(7) 0.006(5) -0.002(5) -0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co01 O002 2.093(8) 4_565 ? Co01 O002 2.093(8) . ? Co01 O003 2.097(10) . ? Co01 O003 2.097(10) 4_565 ? Co01 O004 2.112(11) 7_575 ? Co01 O004 2.112(11) 6_556 ? O002 C008 1.247(13) . ? O003 C009 1.229(18) . ? O004 C009 1.244(16) . ? N005 C007 1.31(3) . ? N005 H00A 0.8600 . ? N005 H00B 0.8600 . ? N006 C007 1.336(17) . ? N006 H00C 0.8600 . ? N006 H00D 0.8600 . ? C008 H008 0.9300 . ? C009 H009 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O002 Co01 O002 179.3(7) 4_565 . ? O002 Co01 O003 89.1(4) 4_565 . ? O002 Co01 O003 90.5(4) . . ? O002 Co01 O003 90.5(4) 4_565 4_565 ? O002 Co01 O003 89.1(4) . 4_565 ? O003 Co01 O003 104.3(7) . 4_565 ? O002 Co01 O004 91.1(4) 4_565 7_575 ? O002 Co01 O004 89.4(4) . 7_575 ? O003 Co01 O004 170.3(4) . 7_575 ? O003 Co01 O004 85.4(5) 4_565 7_575 ? O002 Co01 O004 89.4(4) 4_565 6_556 ? O002 Co01 O004 91.1(4) . 6_556 ? O003 Co01 O004 85.4(5) . 6_556 ? O003 Co01 O004 170.3(4) 4_565 6_556 ? O004 Co01 O004 84.9(6) 7_575 6_556 ? C008 O002 Co01 122.3(11) . . ? C009 O003 Co01 132.4(9) . . ? C009 O004 Co01 129.9(10) . 6_656 ? C007 N005 H00A 120.0 . . ? C007 N005 H00B 120.0 . . ? H00A N005 H00B 120.0 . . ? C007 N006 H00C 120.0 . . ? C007 N006 H00D 120.0 . . ? H00C N006 H00D 120.0 . . ? N005 C007 N006 120.5(11) . . ? N005 C007 N006 120.5(11) . 2_565 ? N006 C007 N006 119(2) . 2_565 ? O002 C008 O002 125.8(19) . 2_565 ? O002 C008 H008 117.1 . . ? O002 C008 H008 117.1 2_565 . ? O003 C009 O004 123.9(14) . . ? O003 C009 H009 118.0 . . ? O004 C009 H009 118.0 . . ? _refine_diff_density_max 0.789 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.185 _shelx_res_file ; TITL CoGF 0.88GPa in Pnna 022_CoGF_0-88GPa.res created by SHELXL-2017/1 at 14:19:33 on 01-Aug-2018 CELL 0.48590 8.220404 11.643740 8.922303 90.0000 90.0000 90.0000 ZERR 4.00 0.004261 0.002021 0.003024 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z SYMM -x+1/2, y+1/2,-z+1/2 SYMM x,-y+1/2,-z+1/2 SFAC C H Co N O DISP C 0.001 0.001 6.068 DISP Co 0.266 0.475 1359.652 DISP H -0 0 0.607 DISP N 0.002 0.001 8.983 DISP O 0.004 0.003 13.336 UNIT 16 36 4 12 24 RIGU L.S. 10 PLAN 15 BOND $H LIST 4 FMAP 2 ACTA SHEL 999 0.8 OMIT 5 1 7 OMIT 3 1 6 WGHT 0.062600 20.993402 FVAR 2.64384 CO01 3 0.259699 0.750000 0.250000 10.50000 0.03803 0.01726 = 0.00721 0.00021 0.00000 0.00000 O002 5 0.261279 0.595001 0.131307 11.00000 0.06744 0.02028 = 0.01150 -0.00229 0.00270 -0.00190 O003 5 0.416190 0.679860 0.411535 11.00000 0.04565 0.02535 = 0.02670 0.00610 -0.01250 -0.00273 O004 5 0.570108 0.690445 0.610382 11.00000 0.05042 0.04038 = 0.01392 0.00202 -0.00809 -0.00714 N005 4 0.250000 0.500000 0.592954 10.50000 0.04860 0.02504 = 0.01668 0.00000 0.00000 -0.00086 AFIX 93 H00A 2 0.311064 0.547254 0.544761 10.50000 -1.20000 H00B 2 0.188936 0.452746 0.544760 10.50000 -1.20000 AFIX 0 N006 4 0.344364 0.573023 0.815971 11.00000 0.06879 0.04478 = 0.01406 -0.00313 0.00112 -0.01841 AFIX 93 H00C 2 0.405724 0.620506 0.768487 11.00000 -1.20000 H00D 2 0.343766 0.572560 0.912355 11.00000 -1.20000 AFIX 0 C007 1 0.250000 0.500000 0.740029 10.50000 0.02474 0.03212 = 0.01865 0.00000 0.00000 -0.00259 C008 1 0.250000 0.500000 0.194971 10.50000 0.07440 0.01971 = 0.01615 0.00000 0.00000 -0.00489 AFIX 43 H008 2 0.249997 0.500001 0.299204 10.50000 -1.20000 AFIX 0 C009 1 0.532041 0.720008 0.481047 11.00000 0.03994 0.02921 = 0.01526 0.00561 -0.00232 -0.00473 AFIX 43 H009 2 0.595011 0.775810 0.434191 11.00000 -1.20000 AFIX 0 HKLF 4 REM CoGF 0.88GPa in Pnna REM R1 = 0.0868 for 315 Fo > 4sig(Fo) and 0.1691 for all 613 data REM 66 parameters refined using 36 restraints END WGHT 0.0577 21.1497 REM Highest difference peak 0.789, deepest hole -0.806, 1-sigma level 0.185 Q1 1 0.5054 0.8015 0.5012 11.00000 0.05 0.79 Q2 1 0.2427 0.4123 0.3826 11.00000 0.05 0.68 Q3 1 0.7514 0.7166 0.3259 11.00000 0.05 0.61 Q4 1 0.2500 0.5000 0.9118 10.50000 0.05 0.59 Q5 1 0.3112 0.7561 0.4881 11.00000 0.05 0.57 Q6 1 0.4942 0.5044 0.7991 11.00000 0.05 0.57 Q7 1 0.5804 0.7168 0.2991 11.00000 0.05 0.56 Q8 1 0.6987 0.6423 0.6915 11.00000 0.05 0.53 Q9 1 0.6628 0.6906 0.6268 11.00000 0.05 0.53 Q10 1 0.5826 0.9036 0.5082 11.00000 0.05 0.52 Q11 1 0.0634 0.4963 0.2553 11.00000 0.05 0.52 Q12 1 0.0797 0.4958 0.4984 11.00000 0.05 0.52 Q13 1 0.4949 0.7046 0.2363 11.00000 0.05 0.48 Q14 1 0.0764 0.5874 0.8016 11.00000 0.05 0.47 Q15 1 0.4733 0.7484 0.6398 11.00000 0.05 0.47 ; _shelx_res_checksum 23968 _shelx_hkl_file ; 0 2 0 55878.7 6245.58 5 0 2 0 64556.7 6242.62 1 0 2 0 65379.4 6230.55 2 0 -2 0 63851.5 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1021.69 1638.47 8 0 -14 0 2669.30 1463.55 6 0 14 0 2685.21 969.758 1 0 -15 0 87.9241 1309.47 6 0 15 0-1029.24 979.224 1 0 -15 0-408.156 628.903 4 0 15 0 82.8275 1549.45 8 0 -16 0 4538.51 1631.00 6 0 16 0 6423.43 1308.30 1 0 -16 0 5020.46 929.460 4 0 -17 0 308.169 682.117 4 0 -17 0-96.4196 1469.45 6 0 -1 -1 759.951 98.1799 4 0 1 1 681.526 142.621 8 0 -2 1 14.5687 109.071 3 0 2 -1-10.6266 154.306 5 0 -2 -1 26.1744 62.2664 4 0 2 1-12.5010 81.6955 1 0 2 1-271.123 176.481 8 0 3 1 40339.8 3878.55 2 0 3 1 32152.7 3976.73 8 0 3 1 38341.6 3918.77 1 0 3 -1 43781.1 3967.31 5 0 -3 1 40522.6 3926.23 3 0 -3 1 35059.3 3970.93 6 0 -3 -1 38366.2 3914.43 4 0 -4 -1-151.407 281.158 6 0 -4 1 168.157 216.892 3 0 4 -1 124.563 210.168 1 0 4 1 102.801 192.714 5 0 4 -1-15.9877 316.169 5 0 -4 -1 8.44081 172.570 7 0 4 -1 36.3902 189.518 2 0 4 1 100.302 98.7317 2 0 -4 1 110.772 264.771 6 0 4 1-72.1383 161.551 1 0 4 1-256.307 376.881 8 0 5 -1 105319. 12024.9 2 0 -5 -1 133835. 11996.5 3 0 -5 1 118289. 12042.0 3 0 5 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88.4965 392.716 2 0 -10 -1-1241.05 847.203 6 0 10 1-112.113 441.944 1 0 10 1-179.585 1041.91 8 0 10 -1-272.245 631.951 1 0 -10 1-164.019 619.072 3 0 -10 1 1426.65 900.627 6 0 11 -1 265.847 691.948 1 0 -11 -1 918.280 922.789 6 0 11 1 912.294 1166.75 8 0 -11 1 391.694 966.454 6 0 -11 -1 369.950 462.608 4 0 11 1 272.420 481.809 1 0 11 -1-62.0441 1180.45 8 0 -12 -1 67.3714 956.383 6 0 12 1 82.6483 522.024 1 0 12 -1-144.442 743.917 1 0 -12 1 356.533 1035.44 6 0 12 -1 472.792 1248.40 8 0 13 1 461.826 619.800 1 0 -13 -1 663.453 1091.52 6 0 -13 -1 565.675 570.608 4 0 13 1-374.273 1351.51 8 0 -14 -1 179.988 547.029 4 0 14 -1-838.116 1016.14 1 0 14 1-684.134 633.104 1 0 -14 1-1555.63 1438.01 6 0 14 -1-77.7300 1494.93 8 0 14 1-467.282 1535.18 8 0 -14 -1-321.291 1159.54 6 0 15 1-1805.16 1522.51 8 0 15 -1-546.116 989.162 1 0 -15 1 1968.11 1424.50 6 0 -15 -1-168.781 1201.92 6 0 -15 -1 403.095 599.406 4 0 15 1-37.3542 855.464 1 0 16 1-84.4694 1564.39 8 0 -16 -1-324.396 676.831 4 0 16 1-305.301 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5679.68 7 2 2 -2 52273.3 5599.76 2 2 -2 -2 55588.4 5556.79 2 2 -2 -2 63045.4 5693.43 6 -2 2 2 58247.0 5592.37 7 2 2 -2 43157.2 5655.18 5 -2 2 2 60207.6 5593.62 1 2 -3 -2 238.480 344.958 6 -2 3 2-42.6592 197.889 1 -2 -4 2 52858.3 5428.37 6 -2 -4 2 54228.9 5524.22 7 2 4 -2 54006.4 5505.35 5 2 4 -2 57834.4 5435.28 2 2 4 -2 55531.9 5432.86 8 2 4 -2 56107.0 5380.65 1 -2 -4 2 51733.8 5372.83 4 2 -5 -2 5586.63 818.187 6 -2 -5 2 3308.53 528.817 3 -2 -5 2 5263.55 525.729 4 2 5 -2 4879.29 607.585 2 -2 5 2 5712.12 619.086 1 2 5 -2 3617.53 703.714 5 2 5 -2 4485.20 532.888 1 2 5 -2 5303.08 708.874 8 -2 -5 2 3360.75 753.672 7 2 -6 -2 21877.0 2247.33 6 -2 -6 2 17172.2 2107.05 7 -2 -6 -2 19617.8 1961.64 4 2 6 2 21613.7 2001.19 1 2 6 -2 15246.9 2084.14 5 2 6 -2 18961.7 1970.47 2 -2 6 2 23155.2 2012.66 1 2 6 -2 17802.2 1921.22 1 2 6 -2 16183.7 2101.90 8 -2 -6 2 17732.2 2039.11 6 -2 -6 2 17032.5 1928.10 3 -2 7 2 2124.35 461.142 1 2 -7 -2 1818.79 766.642 6 -2 -7 2 1475.32 691.728 7 -2 -7 2 1623.36 377.349 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-2 4831.48 768.625 4 -2 10 2 5305.30 1395.81 8 -2 -10 2 5767.30 1144.10 7 -2 -11 -2 2016.23 642.229 4 -2 -11 -2 7077.11 1395.90 6 2 11 2 2073.26 1498.84 8 2 11 -2 6616.45 1555.25 5 2 11 -2 5524.32 809.321 2 2 11 2 749.629 619.783 1 -2 -11 2 3442.51 872.722 3 2 -12 -2 7754.45 1755.28 6 2 12 -2 10473.0 1176.85 2 -2 -12 2 5866.74 1452.38 7 2 12 -2 6912.91 1472.23 5 -2 12 2 8412.23 1282.98 1 -2 12 2 9639.29 1951.19 8 -2 -12 2 9240.79 1210.07 3 2 -13 -2-2247.82 1414.11 6 2 13 2 169.818 546.883 1 -2 -13 -2-170.399 567.068 4 -2 13 2-1039.01 832.091 1 -2 13 2-2442.43 1767.73 8 2 14 2 2848.28 704.952 1 -2 14 2 413.510 1577.40 8 2 14 2 605.672 1485.01 8 -2 14 2 1840.20 861.705 1 -2 -14 -2 1207.10 668.848 4 -2 -14 -2 1385.98 1172.61 6 2 -14 -2 2962.36 1358.78 6 -2 15 2-4649.76 2048.80 8 2 15 2-4482.91 1962.68 8 2 -15 -2-3549.05 1852.79 6 -2 15 2-332.039 982.358 1 2 15 2-831.401 718.125 1 -2 -15 -2-1241.51 712.537 4 -2 -15 -2-2972.26 1480.70 6 2 16 2 2268.63 841.554 1 2 -16 -2 6567.47 1911.02 6 2 16 2 5642.71 2230.96 8 -2 -16 -2 5533.68 1688.55 6 2 -16 -2 3107.07 873.221 4 -2 16 2 4093.10 2102.14 8 -2 16 2 4121.57 1174.35 1 -2 -16 -2 4272.02 896.766 4 -2 17 2-203.930 1084.68 1 2 -17 -2-99.8400 1568.94 6 -2 17 2-550.437 1817.31 8 2 -17 -2-277.214 673.912 4 2 0 -3 53.3377 93.3367 4 2 0 -3-146.324 333.401 5 -2 0 3-269.241 249.975 8 -2 0 3-94.2506 311.690 7 2 0 -3-67.0560 242.520 6 -2 0 3-97.9335 140.017 1 2 1 -3 13477.7 1237.91 2 2 -1 -3 12831.8 1270.52 5 2 1 -3 11954.0 1312.53 5 2 -1 -3 12136.6 1208.33 2 -2 1 3 12924.9 1229.36 1 -2 1 3 7892.50 1344.93 8 2 -1 -3 14041.6 1210.82 4 -2 1 3 12627.4 1277.86 7 -2 -1 3 10040.5 1171.75 1 -2 1 3 11009.6 1192.07 3 -2 -1 3 11034.8 1210.13 3 2 -1 -3 15913.7 1349.60 6 -2 2 3 12283.8 1642.01 8 2 -2 -3 8676.02 1177.19 2 -2 2 3 8810.68 1242.50 1 -2 3 3 384.797 122.742 3 -2 3 3 404.966 203.911 7 2 -3 -3 152.912 214.761 5 2 3 -3 332.246 466.223 5 2 3 -3 208.547 251.136 2 -2 -3 3 210.734 188.231 3 2 -3 -3 306.874 120.834 2 -2 4 3 3456.96 782.677 8 -2 -4 3 1735.65 362.819 3 2 4 -3 2487.40 421.079 2 2 -4 -3 3808.46 668.860 6 2 4 -3 1620.44 593.426 5 -2 4 3 2469.90 414.500 1 2 5 -3 4400.96 606.564 2 -2 5 3 4126.16 597.713 1 2 5 -3 3539.70 820.114 5 2 -5 -3 4711.61 846.307 6 -2 5 3 4215.05 934.404 8 -2 -5 3 3928.54 553.965 3 -2 6 3 281.360 835.453 8 -2 -6 3 568.956 349.871 3 -2 6 3 576.814 331.728 1 2 6 -3 160.732 625.618 5 2 6 -3 529.841 384.735 2 2 -6 -3 451.491 644.971 6 2 7 3 82.8602 354.265 1 -2 -7 3-141.840 395.686 3 2 7 -3 138.533 777.903 5 -2 -7 -3 294.557 327.546 4 -2 7 3 60.4768 366.861 1 2 7 -3 101.267 393.462 2 -2 7 3 52.3137 934.312 8 2 7 -3-88.0117 688.798 8 2 -7 -3 448.171 683.139 6 -2 8 3 375.821 450.377 1 2 -8 -3 163.779 748.868 6 -2 -8 3-20.3541 422.590 3 2 8 3-211.306 1004.60 8 2 8 -3 450.733 817.539 5 2 8 -3 18.0940 437.459 2 -2 -8 -3-365.939 405.425 4 2 8 3 201.331 424.635 1 -2 8 3 460.529 1090.68 8 -2 -8 3-115.958 745.831 7 2 -9 -3-3083.03 1461.68 6 -2 -9 3-1465.20 946.698 7 -2 -9 3-709.817 546.431 3 2 9 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765.196 760.161 2 -2 -14 -3-150.723 1118.28 6 2 14 3-320.092 1593.12 8 2 14 3-122.154 592.447 1 2 -14 -3-172.872 1328.43 6 -2 -14 -3-216.803 642.051 4 2 -14 -3 253.093 623.465 4 -2 14 3-38.1908 773.029 1 -2 14 3-250.781 1661.41 8 -2 -15 -3-1176.14 1416.60 6 2 15 3-189.957 685.854 1 -2 15 3 712.802 874.392 1 -2 15 3-1912.01 1882.25 8 2 15 3-2943.34 1849.66 8 2 -15 -3-1742.62 735.929 4 -2 -15 -3-260.185 755.612 4 2 -16 -3-366.769 662.708 4 2 -16 -3 570.129 1435.42 6 -2 16 3 136.894 911.514 1 2 16 3 325.243 636.543 1 -2 -16 -3-486.279 1307.41 6 -2 -16 -3 203.674 701.511 4 -2 16 3 264.237 1643.80 8 2 16 3 526.893 1794.73 8 -2 -17 -3 956.706 765.565 4 -2 17 3 1274.97 1056.10 1 2 -17 -3 401.666 1557.81 6 -2 -17 -3 1250.16 1279.11 6 2 17 3 305.067 696.138 1 2 17 3-547.083 1788.84 8 2 0 -4 19786.9 2032.78 2 -2 -1 4 220.841 285.170 3 -2 1 4 339.889 270.534 3 2 -1 -4 151.520 411.937 5 2 1 -4 469.886 498.578 5 2 -1 -4 420.674 173.090 4 2 -1 -4 390.250 261.224 2 -2 -1 4 445.037 165.018 1 -2 1 4 339.376 399.161 8 -2 1 4 338.090 230.150 1 2 -2 -4 56030.5 5295.69 5 2 2 -4 52455.2 5376.92 5 2 -2 -4 52322.7 5230.65 2 -2 2 4 58753.0 5278.71 1 2 2 -4 47870.4 5271.51 2 -2 2 4 51905.4 5250.99 3 -2 -2 4 50400.6 5282.80 3 -2 3 4 2133.35 654.194 8 2 3 -4 1465.39 616.133 5 2 3 -4 1106.84 370.113 2 -2 3 4 1118.85 347.380 7 2 -3 -4 1653.43 264.528 2 -2 -3 4 1752.93 391.894 3 2 -3 -4 1766.47 314.230 4 2 -3 -4 1607.31 588.765 6 2 -4 -4 42171.2 3857.54 6 2 4 -4 32717.6 3730.71 5 2 4 -4 33793.6 3625.96 2 -2 -4 4 36949.3 3649.35 3 2 -4 -4 34116.1 3528.80 2 -2 4 4 37439.3 3634.95 1 -2 4 4 41513.7 3853.39 8 2 -4 -4 38544.3 3620.12 4 -2 5 4 215.224 348.393 1 2 5 -4 132.338 696.617 5 2 5 -4 540.773 395.695 2 2 -5 -4 211.843 309.270 4 -2 5 4-342.877 818.254 8 -2 -5 4-95.9114 410.191 3 2 -5 -4 89.5075 609.790 6 2 -6 -4 1127.23 698.815 6 -2 6 4 2075.00 994.834 8 -2 -6 4 851.894 481.373 3 -2 6 4 1166.61 434.432 1 2 6 -4 459.647 750.209 5 2 6 -4 1867.74 480.783 2 2 -6 -4 1102.82 384.396 4 2 -7 -4-1392.47 1027.43 6 -2 -7 4-780.317 575.686 3 -2 7 4-559.783 462.007 1 2 7 -4-1295.72 1024.46 5 2 7 -4-851.268 524.950 2 2 -7 -4-931.887 511.937 4 2 -8 -4 7231.09 1224.80 6 2 8 4 5149.13 877.834 1 2 8 -4 6752.05 897.487 2 2 8 -4 6540.71 1259.25 5 -2 8 4 6489.72 878.209 1 2 -8 -4 6137.75 872.090 4 -2 8 4 9130.01 1468.29 8 -2 -8 4 6238.07 942.568 3 2 9 4 25.8408 478.684 1 -2 -9 4-27.0740 615.370 3 2 -9 -4-249.204 851.632 6 2 9 -4-86.1413 1247.90 5 -2 9 4 373.399 484.745 1 2 9 -4 366.573 560.993 2 2 -9 -4 269.519 476.285 4 -2 -9 -4-165.631 428.862 4 -2 9 4 516.621 1179.58 8 2 10 -4 22594.5 2207.07 2 -2 -10 4 21264.7 2286.39 3 -2 -11 -4 463.327 537.726 4 2 -11 -4 500.155 1034.55 6 -2 11 4 866.171 1326.55 8 2 11 4 69.8400 1244.93 8 2 11 4-169.791 563.040 1 2 -11 -4 586.219 514.614 4 -2 11 4-28.8329 576.544 1 -2 12 4 2210.02 1532.82 8 -2 -12 4 4785.37 1046.36 3 -2 -12 -4 5662.14 897.065 4 2 -12 -4 6161.88 1418.88 6 2 -12 -4 4192.05 871.761 4 2 12 -4 5494.36 1429.92 5 2 12 -4 6891.88 982.688 2 2 12 4 5657.68 902.840 1 -2 -12 4 5127.32 1353.99 7 -2 12 4 6036.14 926.387 1 2 12 4 2009.88 1644.81 8 -2 13 4-32.8055 630.745 1 2 13 4-120.215 623.010 1 2 13 4-315.245 1501.51 8 -2 -13 -4 746.949 1088.05 6 2 -13 -4 884.281 1094.87 6 2 -13 -4-393.896 556.763 4 2 13 -4-320.443 684.949 2 2 13 -4 521.211 1198.17 5 -2 -13 -4-153.670 573.599 4 -2 13 4-79.9205 1347.42 8 -2 -13 4 426.654 839.739 3 -2 -13 4 282.482 1174.76 7 -2 -14 4 2760.81 1072.42 3 2 14 4 3557.00 815.556 1 2 14 -4 4082.80 910.581 2 -2 14 4 6143.02 937.720 1 2 -14 -4 4713.07 1442.64 6 2 14 -4 4630.83 1560.82 5 -2 -14 -4 3452.94 825.275 4 -2 14 4 4501.74 1607.01 8 2 -14 -4 3977.61 828.680 4 2 14 4 2156.13 1722.84 8 -2 -14 4 3498.43 1369.22 7 -2 -14 -4 2658.34 1294.71 6 -2 -15 -4 1360.48 1254.30 6 2 -15 -4-354.088 1333.56 6 -2 15 4-147.614 733.904 1 2 15 4 260.224 1640.60 8 -2 -15 -4 496.640 649.603 4 -2 15 4 84.8136 1543.14 8 2 15 4 194.598 612.755 1 2 -15 -4 326.494 624.856 4 2 -16 -4 6186.97 1083.39 4 -2 16 4 961.488 2047.09 8 -2 -16 -4 7664.91 1760.12 6 2 16 4 7087.03 1068.91 1 -2 16 4 8565.06 1255.26 1 -2 -16 -4 6530.74 1115.70 4 2 -16 -4 1966.51 1734.62 6 2 16 4 2976.14 2064.58 8 -2 -17 -4 590.839 1433.67 6 2 17 4 2612.09 2147.67 8 2 17 4 135.410 751.432 1 -2 0 5-16.5733 383.864 3 2 0 -5-169.013 576.355 5 2 0 -5 92.2291 365.605 2 -2 0 5-20.5387 263.136 1 2 1 -5-103.874 381.586 2 -2 1 5-173.178 286.769 1 -2 -1 5-53.4820 416.160 3 -2 -2 5 1898.76 513.866 3 -2 2 5 3268.17 742.401 8 2 2 -5 3090.65 771.409 5 2 2 -5 1740.98 510.288 2 2 -2 -5 1979.53 426.021 2 2 -2 -5 2606.57 395.244 4 2 3 -5 10297.9 1309.63 5 2 -3 -5 8876.68 1015.24 2 2 3 -5 8373.96 1126.01 2 -2 3 5 10599.7 1105.76 1 2 -3 -5 9886.19 1058.88 4 -2 3 5 10330.2 1318.55 8 -2 -3 5 9449.87 1144.51 3 -2 -4 5 67.1671 453.790 3 2 4 -5 731.308 747.590 5 2 4 -5-74.5407 457.785 2 2 -4 -5 168.980 297.366 4 -2 4 5 427.051 745.445 8 -2 4 5 555.418 385.168 1 -2 -5 5 841.064 536.733 3 -2 5 5 556.159 417.801 1 2 -5 -5 747.604 341.528 4 2 5 -5 292.609 801.149 5 -2 5 5 531.621 832.658 8 2 5 -5 797.449 492.052 2 2 -5 -5 585.490 746.496 6 -2 -6 5 128.448 550.460 3 -2 6 5 236.433 446.985 1 2 -6 -5 107.302 754.018 6 2 6 -5-156.471 836.930 5 2 6 -5-105.833 519.315 2 2 -6 -5 58.0198 351.188 4 -2 6 5 148.478 920.146 8 -2 -7 5 246.220 608.397 3 2 -7 -5-58.3464 809.185 6 -2 7 5 140.340 459.990 1 2 7 -5 250.069 888.108 5 2 7 -5 398.320 513.122 2 -2 7 5-382.790 1016.93 8 2 -7 -5 383.238 378.630 4 -2 8 5-149.629 476.988 1 -2 -8 5 381.771 657.910 3 2 8 -5 663.678 963.078 5 2 -8 -5 370.777 838.669 6 2 8 -5-371.404 531.025 2 -2 8 5 951.945 1123.11 8 2 -8 -5 254.132 452.259 4 -2 -9 5 1211.38 745.855 3 2 -9 -5-1181.39 1371.55 6 -2 9 5-52.7821 631.084 1 2 9 -5 1170.54 1120.91 5 2 9 -5-1499.60 785.719 2 2 -9 -5 1890.09 545.621 4 -2 -10 5-1211.87 744.329 3 2 10 -5 341.026 1063.35 5 -2 10 5 580.231 562.881 1 -2 10 5-136.779 1314.88 8 2 -10 -5-26.5395 491.489 4 2 -10 -5 1106.72 1038.76 6 -2 -11 5 1470.08 871.259 3 2 -11 -5 1020.41 1076.71 6 2 11 -5-512.288 1162.80 5 -2 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651.886 1 2 15 -5 30.3549 836.427 2 -2 -15 -5 240.765 727.812 4 -2 15 5-597.504 1826.84 8 2 -15 -5 927.974 792.658 4 -2 -16 -5-1339.86 1315.77 6 2 16 5-169.658 739.588 1 2 -16 -5-2119.90 1463.77 6 -2 16 5 922.021 818.328 1 -2 -16 -5 391.627 706.401 4 2 0 -6 20050.4 2145.39 2 2 -1 -6 1319.75 463.217 2 2 1 -6 1351.21 516.524 2 -2 -1 6-222.362 272.408 3 -2 2 6 15005.1 1617.77 1 2 2 -6 15817.8 1695.40 2 -2 -2 6 13981.9 1681.73 3 2 -3 -6 1396.26 408.355 4 -2 3 6 2155.52 560.195 1 2 4 -6 43947.4 4304.29 5 2 4 -6 34108.3 4073.55 2 -2 4 6 43287.9 4073.77 1 2 -4 -6 42742.5 4040.88 4 -2 4 6 37223.2 4259.16 8 -2 -4 6 35600.7 4118.64 3 -2 -5 6 85.0911 623.145 3 -2 5 6 47.9440 903.708 8 2 5 -6 744.997 931.200 5 2 5 -6-191.490 567.336 2 2 -5 -6 400.228 370.727 4 -2 5 6 499.934 465.840 1 -2 6 6 9276.51 1820.48 8 2 -6 -6 11545.7 1796.93 6 2 6 -6 12828.7 1501.29 2 -2 6 6 13253.3 1493.87 1 2 -6 -6 13557.1 1447.51 4 2 6 -6 17285.1 1850.13 5 -2 -6 6 9831.78 1527.06 3 2 -7 -6-62.1565 858.809 6 -2 7 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12 8 894.723 716.392 1 -3 12 8 83.8700 1950.91 8 3 -12 -8 528.269 731.664 4 3 -13 -8-87.1187 1284.92 6 -3 13 8 176.237 700.628 1 -3 13 8 259.578 1768.40 8 3 -13 -8-442.538 696.928 4 3 1 -9-25.1968 682.626 2 3 2 -9 14439.4 1746.32 2 -3 7 9 402.449 642.947 1 -3 8 9 2034.28 750.959 1 3 -8 -9 80.7344 1376.16 6 -3 8 9 302.115 1531.88 8 3 -8 -9 2222.83 691.108 4 3 -9 -9-1481.94 1649.60 6 -3 9 9-1624.41 794.270 1 -3 9 9-785.841 1969.98 8 3 -9 -9-185.180 630.721 4 3 -10 -9 591.391 1334.65 6 -3 10 9 915.549 744.781 1 -3 10 9 494.000 1636.68 8 3 -10 -9 2122.72 723.077 4 3 -11 -9 461.542 657.450 4 3 -11 -9 869.122 1372.96 6 -3 11 9-732.670 719.868 1 -3 11 9-336.146 1653.19 8 3 -12 -9 795.046 1522.08 6 -3 12 9 2854.02 847.764 1 -3 12 9-173.837 1786.53 8 3 -12 -9 1738.18 792.631 4 3 -13 -9 804.515 1600.91 6 -3 13 9 578.298 810.836 1 3 -10 -10-1063.45 1358.42 6 -3 10 10 892.411 782.887 1 3 -10 -10 133.149 640.580 4 3 -11 -10-540.239 1391.65 6 -3 11 10 180.645 704.673 1 3 -11 -10-276.088 687.144 4 3 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1 -2 506.580 270.627 2 4 2 -2 16524.3 1722.17 2 -4 -2 2 16128.4 1865.31 7 4 3 -2-150.901 285.892 2 -4 -3 2 253.402 527.787 7 4 4 -2 23626.4 2379.17 2 -4 -4 2 21071.2 2548.21 7 4 5 -2 559.967 375.472 2 4 -5 -2-51.9447 608.064 6 -4 -5 2 749.176 609.381 7 4 -6 -2 4790.65 1103.94 6 4 6 -2 5221.42 721.093 2 -4 -6 2 4737.96 984.498 7 4 -7 -2 62.8565 797.703 6 -4 7 2 825.427 627.446 1 4 7 -2 578.270 921.192 5 -4 -7 2 171.131 728.859 7 4 7 -2 761.916 443.704 2 4 -8 -2 16408.4 2145.40 6 4 8 -2 12719.4 2033.77 5 4 8 -2 14962.3 1721.02 2 -4 8 2 20332.5 1926.61 1 -4 -8 2 12743.0 1939.74 7 4 -9 -2 667.546 962.477 6 4 9 -2 1334.74 1057.69 5 -4 9 2-37.5057 684.651 1 -4 -9 2 482.227 870.927 7 4 9 -2 286.506 500.593 2 -4 -10 2 1865.06 484.657 3 4 10 2 2875.45 650.497 1 4 10 -2 2398.47 705.293 2 4 -11 -2 84.2004 1305.01 6 4 11 2 847.491 561.788 1 -4 11 2 1747.08 941.640 1 4 -12 -2 5676.26 1627.42 6 4 12 -2 3080.81 1278.58 5 -4 -12 2 5675.24 1476.61 7 -4 -12 2 5821.18 881.039 3 4 12 -2 5549.15 962.596 2 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2 4 -8 -3 484.640 1036.65 6 -4 -8 3-816.970 408.438 3 -4 8 3 490.272 668.308 1 4 8 -3-1827.35 1016.89 5 -4 -8 3-2253.47 1169.82 7 4 -9 -3 967.591 1036.27 6 -4 -9 3 1239.81 449.891 3 4 9 -3 1528.98 637.424 2 -4 9 3 2486.10 774.529 1 4 9 -3 584.962 816.170 5 -4 -9 3 354.658 921.476 7 -4 -11 3-456.168 516.584 3 4 -11 -3 83.8040 1129.11 6 4 11 -3-149.819 641.327 2 4 11 -3-48.6666 1048.89 5 -4 11 3 381.972 813.206 1 -4 11 3 75.8222 1396.04 8 -4 -11 3-336.824 1100.66 7 -4 -12 3-1484.84 649.059 3 4 12 -3 457.303 1356.08 5 4 12 3 2528.06 800.888 1 -4 12 3-1514.66 2617.91 8 4 12 -3 1617.12 846.580 2 4 -13 -3 1567.04 1553.50 6 -4 13 3 751.127 1093.57 1 -4 13 3 499.047 1864.94 8 4 13 3-29.9366 805.852 1 -4 -14 -3 3904.02 1419.01 6 -4 -14 3 1988.26 847.584 3 4 -14 -3-2101.06 2521.21 6 4 14 -3 2308.05 1502.44 5 -4 14 3 1021.73 1277.55 1 -4 14 3 691.131 2890.29 8 4 14 3 470.545 754.813 1 4 14 -3 1266.28 831.220 2 -4 15 3 1028.46 1099.55 1 4 -15 -3 406.078 1741.10 6 -4 15 3 356.046 1823.63 8 -4 16 3-948.816 1107.72 1 4 -16 -3-1352.48 1570.45 6 4 0 -4 19330.6 2455.68 6 4 0 -4 23121.3 2604.48 5 4 0 -4 25827.4 2427.01 2 -4 0 4 25093.2 2564.65 7 4 -1 -4 939.292 319.849 2 4 -1 -4 599.413 496.333 6 4 1 -4 987.287 718.516 5 4 -1 -4 739.055 655.251 5 -4 1 4 1360.72 646.498 8 4 1 -4 888.062 373.429 2 -4 -1 4 1543.88 628.216 7 -4 1 4 1238.51 529.729 7 -4 1 4 1337.90 404.935 1 4 2 -4 33778.3 4050.67 5 4 2 -4 38737.8 3928.83 2 -4 -2 4 44003.0 4095.76 7 -4 3 4 3066.72 886.935 8 4 -3 -4 3348.10 840.544 6 4 3 -4 2885.96 899.213 5 -4 3 4 2913.38 622.059 1 4 3 -4 3498.37 613.676 2 -4 3 4 4405.59 594.197 7 -4 -3 4 3898.35 844.644 7 4 -4 -4 36421.5 3468.10 6 4 4 -4 31910.9 3368.39 5 4 4 -4 25582.9 3181.74 2 -4 4 4 39141.0 3249.21 1 -4 -4 4 25181.4 3348.40 7 -4 -5 4 170.161 331.667 3 -4 5 4 965.996 518.043 1 4 5 -4 768.312 909.067 5 4 5 -4 1035.22 519.837 2 4 -5 -4 366.424 859.022 6 -4 5 4 893.231 1022.08 8 4 -6 -4 3306.94 1085.05 6 4 6 -4 5359.69 760.725 2 4 6 -4 2974.51 935.484 5 -4 6 4 5917.44 809.799 1 -4 6 4 5386.45 1235.40 8 -4 -6 4 3254.97 1080.99 7 -4 -6 4 3530.21 614.647 3 4 -7 -4 4627.21 1401.58 6 4 7 -4 1597.84 1161.59 5 -4 7 4 2454.06 817.718 1 -4 7 4 2163.14 1425.43 8 -4 -7 4 3907.34 703.676 3 -4 -8 4 3813.83 1279.53 7 4 -8 -4 6434.96 1373.32 6 4 8 -4 6195.40 939.364 2 4 8 -4 6727.18 1271.32 5 -4 8 4 9522.19 1061.94 1 -4 8 4 1299.11 1608.10 8 -4 -8 4 5810.89 855.320 3 4 -9 -4 512.422 1196.80 6 -4 9 4 3063.28 770.404 1 4 -10 -4 3834.09 1660.49 6 4 10 -4 7911.46 1106.41 2 4 10 -4 6126.60 1451.36 5 -4 10 4 11354.9 1295.87 1 -4 10 4 664.479 1894.45 8 -4 -10 4 8408.91 1574.15 7 -4 -10 4 7020.24 1015.38 3 -4 -11 4 706.768 612.444 3 4 -11 -4 504.398 1261.70 6 4 11 -4 1945.97 1187.78 5 -4 11 4 155.394 1471.90 8 -4 11 4 925.668 830.991 1 -4 -11 4 1303.92 1177.16 7 4 11 -4 839.270 684.959 2 -4 12 4 3029.66 937.485 1 -4 -12 4 3044.75 768.672 3 4 -12 -4 175.737 1345.56 6 4 12 -4 1714.71 1326.74 5 -4 12 4 244.194 1503.51 8 4 12 -4 2372.42 781.264 2 -4 -12 4 3887.11 1317.36 7 -4 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568.989 1 4 -3 -5-839.587 1067.95 6 -4 -3 5 2661.17 485.497 3 4 3 -5 1898.84 885.586 5 4 3 -5 3628.24 626.795 2 -4 3 5-2039.02 1236.81 8 -4 -3 5-1534.20 1113.03 7 4 -3 -5 2876.93 502.166 4 -4 4 5 310.041 453.472 1 4 -4 -5 525.590 730.309 6 -4 -4 5 221.967 370.846 3 4 4 -5 345.920 824.820 5 4 4 -5-302.724 535.887 2 -4 4 5 414.569 858.127 8 -4 -4 5 42.4316 802.557 7 4 -4 -5 52.6454 350.224 4 -4 5 5 584.044 486.457 1 4 -5 -5 799.308 882.416 6 -4 -5 5 231.444 382.511 3 4 5 -5 1394.14 904.746 5 4 5 -5 562.251 526.965 2 -4 5 5-310.336 1047.79 8 -4 -5 5-681.620 893.430 7 4 -5 -5 551.492 421.139 4 -4 6 5-570.367 602.253 1 4 -6 -5-2691.67 1382.83 6 4 6 -5-2700.22 1316.11 5 4 6 -5-1242.90 693.676 2 -4 6 5-1199.05 1424.88 8 -4 7 5 3068.79 685.345 1 4 -7 -5 2601.04 1065.15 6 -4 -7 5 2548.82 645.346 3 4 7 -5 3480.76 1141.19 5 4 7 -5 3458.42 729.574 2 -4 7 5 4229.65 1293.09 8 -4 -7 5 1073.78 1045.79 7 -4 8 5-1189.64 774.466 1 -4 8 5-1876.25 2101.15 8 -4 -9 5-54.3509 627.081 3 4 9 -5-300.775 1112.40 5 -4 -9 5-168.948 1049.00 7 4 9 -5 268.421 623.259 2 -4 9 5 214.546 1308.85 8 -4 -10 5 597.926 650.628 3 4 -10 -5 78.3568 1097.61 6 -4 10 5-325.733 662.754 1 4 10 -5 1282.99 1210.75 5 4 10 -5 362.891 680.479 2 -4 10 5 151.428 1366.35 8 -4 -10 5-727.606 1163.79 7 4 -10 -5 86.3868 525.205 4 -4 -11 5 62.0478 674.383 3 4 -11 -5-84.5433 1310.34 6 4 11 -5 107.257 1173.86 5 -4 11 5 260.711 723.861 1 4 11 -5-144.932 704.854 2 -4 11 5-237.916 1404.44 8 -4 -11 5-188.801 1229.52 7 4 -11 -5-453.785 586.962 4 -4 -12 5-549.477 850.082 3 4 -12 -5 2287.38 1685.47 6 4 12 -5-385.993 1441.52 5 -4 12 5-504.056 827.400 1 4 12 -5 89.9560 753.657 2 -4 12 5-82.7964 1792.05 8 -4 -12 5-2992.92 1520.19 7 4 -12 -5 189.456 658.955 4 -4 -13 5 3618.88 1084.73 3 4 -13 -5 5339.78 2045.82 6 4 13 -5 3553.54 1690.26 5 -4 13 5 1390.62 1077.31 1 -4 13 5 1546.93 2103.13 8 4 13 -5 2652.42 986.147 2 4 -13 -5 750.206 820.248 4 -4 -14 5 1875.92 1019.51 3 4 -14 -5 5588.68 2279.18 6 4 14 -5 4279.50 1662.15 5 -4 14 5 1304.33 2101.18 8 4 14 -5 570.492 863.838 2 4 -14 -5 235.598 726.709 4 -4 14 5-46.1577 1031.88 1 -4 -14 5 6097.02 1689.22 7 -4 -15 5 1163.36 970.009 3 -4 15 5 2111.29 1152.71 1 4 -15 -5 101.622 1544.63 6 4 15 -5 415.178 1495.42 5 -4 15 5 357.107 1786.78 8 4 15 -5 162.803 893.465 2 4 -15 -5-345.311 713.686 4 -4 -15 5 284.202 1422.23 7 -4 -16 5-1455.56 1043.82 3 4 16 -5-1931.01 1568.91 5 4 16 -5 432.162 907.219 2 -4 -16 5-2029.91 1495.95 7 4 0 -6 12243.6 1458.57 5 4 0 -6 11488.6 1229.88 2 -4 0 6 8579.81 1400.33 7 -4 0 6 9394.54 1197.74 3 -4 1 6-237.701 408.940 3 -4 -1 6 17.6372 409.534 3 4 -1 -6-341.092 721.643 5 4 1 -6 411.799 806.607 5 -4 1 6-156.941 652.679 7 4 1 -6 53.2450 458.467 2 4 -1 -6 28.7339 413.598 2 -4 -1 6 186.934 776.207 7 -4 -2 6 2236.31 551.376 3 -4 -2 6 2033.29 915.173 7 4 2 -6 1992.39 912.678 5 4 2 -6 3070.77 603.048 2 -4 -3 6 1336.62 489.273 3 4 3 -6 1695.93 961.907 5 -4 3 6 1037.85 481.819 1 4 3 -6 587.407 586.554 2 -4 -3 6 86.2052 882.724 7 4 -4 -6 18590.0 2161.47 6 4 4 -6 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7-63.5581 1241.71 8 4 -7 -7-249.841 525.164 4 -4 -7 7-410.525 1258.39 7 -4 -8 7-34.3140 753.326 3 4 8 -7 534.047 1229.33 5 4 8 -7 488.694 680.760 2 -4 8 7 68.0399 1301.15 8 4 -8 -7-79.9145 540.301 4 -4 -8 7 671.194 1151.88 7 -4 -9 7-35.6766 851.834 3 4 -9 -7 387.243 1163.23 6 4 9 -7-1388.98 1347.94 5 -4 9 7 249.293 647.226 1 4 9 -7-29.7891 743.089 2 -4 9 7-72.1890 1400.52 8 4 -9 -7-508.551 599.433 4 -4 -9 7-516.391 1308.76 7 -4 -10 7 666.120 939.522 3 4 10 -7-56.3932 1361.83 5 -4 10 7 2127.30 2328.69 8 4 10 -7 62.7391 775.524 2 4 -10 -7-1604.92 815.366 4 -4 -10 7-266.287 1334.22 7 -4 10 7 1984.05 878.758 1 -4 -11 7 1355.35 977.162 3 4 -11 -7-1802.14 1355.75 6 4 11 -7 58.3654 1371.97 5 4 11 -7 225.673 799.817 2 -4 11 7-477.841 1788.76 8 4 -11 -7 651.819 620.259 4 -4 -11 7-1367.72 1402.20 7 -4 11 7-104.776 736.448 1 -4 -12 7-79.9339 914.115 3 -4 12 7-324.318 752.766 1 4 -12 -7-88.5011 1305.26 6 4 12 -7 59.4584 1349.47 5 4 12 -7 68.3192 845.427 2 -4 12 7 247.217 1486.98 8 4 -12 -7 32.2165 624.976 4 -4 -12 7 286.436 1386.68 7 -4 -13 7-2928.39 1086.52 3 4 -13 -7 279.631 1388.55 6 -4 13 7-813.660 767.093 1 4 13 -7-1225.22 1541.86 5 4 13 -7 383.439 872.178 2 -4 13 7-255.090 1647.62 8 4 -13 -7-33.2290 643.860 4 -4 -13 7 73.0418 1420.66 7 -4 -14 7 343.885 1073.35 3 4 -14 -7 190.293 1403.46 6 4 14 -7-1253.83 1598.36 5 -4 14 7 356.096 820.515 1 4 14 -7-777.937 896.187 2 4 -14 -7-443.096 685.784 4 -4 -14 7-153.447 1506.90 7 -4 -1 8 2502.84 790.102 3 4 1 -8 3886.97 1099.29 5 4 1 -8 3371.18 702.306 2 -4 -1 8 2309.03 1032.35 7 4 2 -8 11165.7 1484.46 5 4 2 -8 7915.16 1090.05 2 -4 -2 8 8070.15 1178.69 3 -4 -3 8 1773.80 772.424 3 4 3 -8 2988.64 1106.73 5 4 3 -8 2686.49 737.440 2 -4 -3 8 2129.84 1195.54 7 -4 -5 8-234.061 854.537 3 4 5 -8 100.476 1145.56 5 4 5 -8-512.605 724.370 2 -4 -5 8-1677.80 1310.49 7 4 6 -8 14448.4 1949.83 5 4 6 -8 12334.3 1462.45 2 -4 -6 8 10029.1 1538.07 3 4 7 -8 10844.1 2137.04 5 4 7 -8-234.938 1054.24 2 -4 7 8-201.219 1907.02 8 -4 -7 8 7057.42 1399.25 3 -4 -8 8 2175.49 933.359 3 4 -8 -8 919.393 1341.40 6 4 8 -8 3396.29 1356.87 5 -4 8 8 3660.68 825.056 1 4 8 -8 4555.70 929.260 2 -4 8 8 351.059 1475.92 8 4 -8 -8 3615.27 755.731 4 -4 -8 8 3047.07 1455.90 7 -4 -9 8 670.701 904.996 3 4 -9 -8-317.752 1248.40 6 4 9 -8-1958.54 1354.19 5 4 9 -8-1093.63 811.065 2 -4 9 8-481.004 705.242 1 -4 9 8 74.2485 1455.80 8 4 -9 -8 380.772 587.558 4 -4 -9 8-409.530 1305.40 7 -4 -10 8-692.048 1196.39 3 4 -10 -8 1236.59 1595.73 6 4 10 -8 951.637 1693.32 5 4 10 -8 1221.67 909.039 2 -4 10 8 545.392 2264.43 8 4 -10 -8 1290.34 754.289 4 -4 10 8 4028.76 881.979 1 -4 -10 8-3362.81 1729.05 7 -4 -11 8 125.764 984.247 3 4 -11 -8-173.855 1313.20 6 4 11 -8 549.244 1495.55 5 4 11 -8 585.996 858.773 2 -4 11 8-80.7778 1618.99 8 4 -11 -8-255.961 644.565 4 -4 11 8-594.580 734.081 1 -4 -11 8-731.511 1365.26 7 -4 -12 8 2375.62 1145.83 3 4 -12 -8 1826.24 1611.00 6 4 12 -8 3162.20 981.284 2 -4 12 8 668.989 1741.60 8 4 -12 -8 3443.13 854.668 4 -4 -12 8 2906.49 1551.77 7 -4 12 8 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260.719 934.796 2 -5 -9 10-950.893 1539.94 7 5 5 -11 242.996 923.291 2 -5 -5 11-226.795 1593.69 7 5 6 -11 3339.66 1053.18 2 -5 -6 11-1640.83 1669.67 7 -6 -7 1 357.207 602.189 7 -6 -10 1 1425.91 982.898 7 -6 -11 1-1544.57 1229.69 7 6 11 -1-1142.11 768.346 2 -6 -12 1-1290.39 1155.62 7 6 12 -1 925.346 686.972 2 6 12 -1-1242.22 1363.33 5 6 13 -1 9146.41 2494.34 5 -6 -13 1 31019.3 2866.39 7 -6 -5 2 46.9586 835.751 7 6 5 -2 2464.95 567.899 2 -6 -6 2 6222.43 1189.35 7 6 6 -2 6616.45 912.771 2 -6 -7 2 1654.97 920.337 7 6 7 -2 741.388 521.811 2 -6 -9 2-392.892 1029.67 7 6 9 -2 460.175 573.262 2 -6 -10 2 3266.23 1123.54 7 6 10 -2 2375.69 712.912 2 6 10 -2 3132.14 1356.50 5 -6 -11 2 2238.60 1118.41 7 6 11 -2 863.054 672.521 2 -6 -12 2 1252.54 1160.42 7 6 12 -2 2751.03 737.093 2 6 12 -2 2619.59 1384.79 5 -6 -13 2-166.873 557.087 3 6 13 -2-3622.51 1504.15 5 -6 -14 2-133.279 1320.34 7 6 14 -2 109.598 734.855 2 -6 -14 2 696.397 588.375 3 6 14 -2-353.870 1181.46 5 -6 -2 3 40.9473 700.016 7 -6 -3 3 388.166 665.611 7 6 3 -3 338.754 434.374 2 -6 -4 3-503.720 777.507 7 6 4 -3 18.7189 447.443 2 -6 -5 3-145.210 812.180 7 6 5 -3 722.006 454.795 2 -6 -6 3-1572.52 879.143 7 6 6 -3 225.088 507.815 2 6 8 -3 66.6379 548.630 2 6 8 -3 297.299 1139.09 5 -6 -8 3 55.8700 933.101 7 6 9 -3-69.4659 563.012 2 6 9 -3 121.154 1232.10 5 -6 -9 3-58.2208 1031.03 7 6 10 -3 1926.80 781.902 2 -6 -10 3 3389.81 1617.55 7 6 11 -3-299.842 609.164 2 6 11 -3 1796.14 1225.22 5 -6 -11 3 627.620 1141.91 7 6 12 -3 77.5596 653.130 2 -6 -12 3-210.800 485.437 3 6 12 -3 1188.13 1109.02 5 -6 -12 3 2142.12 1261.56 7 6 13 -3-26.6783 695.048 2 -6 -13 3-516.696 557.222 3 6 13 -3 216.781 1214.22 5 -6 -13 3 133.888 1247.20 7 6 14 -3-274.687 766.702 2 -6 -14 3 78.2386 606.963 3 6 14 -3 2125.96 1383.31 5 -6 -14 3 1652.65 1304.98 7 -6 -15 3 420.659 1283.15 7 6 15 -3-397.809 762.821 2 -6 -15 3 227.271 671.008 3 6 15 -3-724.561 1400.26 5 -6 0 4 299.041 609.855 7 -6 -1 4 280.611 681.852 7 6 1 -4 457.967 422.405 2 -6 -2 4 1450.19 857.801 7 6 2 -4 2883.03 583.106 2 6 3 -4 251.832 573.968 2 -6 -3 4 13479.8 1408.16 7 6 4 -4 10820.8 1277.22 2 6 5 -4 454.712 515.726 2 6 5 -4 384.635 1078.41 5 -6 -5 4 859.978 856.385 7 6 7 -4-227.634 543.347 2 6 7 -4-117.392 1150.98 5 -6 -7 4-556.520 1010.70 7 6 8 -4 10257.7 1229.19 2 -6 -8 4 10406.5 1687.62 7 6 9 -4 179.005 643.324 2 6 -9 -4 264.512 912.091 6 6 9 -4 1752.85 1129.28 5 -6 -9 4 61.5483 1072.15 7 6 -10 -4 3253.47 1396.51 6 6 10 -4 8155.59 1021.72 2 6 10 -4 3778.96 1232.34 5 -6 -10 4 5112.56 1389.11 7 -6 -10 4 4814.64 798.985 3 6 11 -4-1650.84 856.086 2 -6 -11 4-623.104 601.896 3 6 -11 -4 97.2382 1059.70 6 -6 11 4-82.5640 1550.83 8 6 12 -4 2534.70 928.698 2 -6 -12 4 3006.46 805.780 3 6 -12 -4 1111.85 1379.71 6 6 12 -4 6478.75 1684.53 5 -6 12 4 1199.09 2206.16 8 6 13 -4 312.006 758.314 2 -6 -13 4 392.460 670.460 3 6 13 -4 1615.65 1479.93 5 -6 13 4 442.134 1996.93 8 -6 -13 4-345.835 1467.38 7 6 14 -4 203.901 775.696 2 -6 -14 4 1079.45 791.011 3 6 14 -4-244.735 1458.79 5 -6 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34050.6 3089.14 2 -6 0 6 28229.7 3342.85 7 -6 0 6 24851.9 3023.88 3 6 1 -6 7552.88 1379.55 5 6 1 -6 6715.75 890.215 2 -6 -1 6 3882.90 712.902 3 6 2 -6 9324.99 1035.50 2 6 2 -6 6329.34 1270.47 5 -6 -2 6 4316.64 1473.23 7 -6 -2 6 6738.18 913.969 3 -6 -3 6 1454.67 447.025 3 6 3 -6 970.324 916.131 5 6 3 -6 1018.88 611.888 2 -6 -3 6 2002.90 1064.27 7 -6 -5 6 1993.17 528.048 3 6 5 -6 518.732 1084.96 5 6 5 -6 2095.48 720.141 2 -6 -5 6 228.114 1142.20 7 -6 -6 6 1017.37 553.865 3 6 6 -6 1525.63 1079.27 5 6 6 -6 2198.79 719.699 2 -6 -6 6 1495.74 1113.00 7 -6 -7 6 817.793 558.333 3 6 7 -6-704.025 1340.53 5 6 7 -6 166.184 724.399 2 -6 -7 6-1562.98 1228.01 7 -6 8 6 825.984 989.748 1 -6 -8 6 1903.18 688.162 3 6 -8 -6 858.138 1480.12 6 6 8 -6 2136.46 1314.82 5 -6 8 6 377.009 1535.58 8 6 8 -6 2019.10 729.980 2 -6 -8 6 2668.04 1319.49 7 -6 9 6 275.056 1060.41 1 -6 -9 6-1505.05 797.648 3 6 -9 -6-632.933 1688.26 6 6 9 -6 752.196 1295.41 5 -6 9 6 714.898 1879.01 8 6 9 -6-209.535 883.127 2 -6 -9 6 134.997 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596.477 2 -6 -2 7-879.932 1005.89 7 -6 -4 7-264.447 548.471 3 6 4 -7-152.122 1080.11 5 6 4 -7 813.833 698.855 2 -6 -4 7-405.884 1120.83 7 -6 -5 7-25.0842 565.731 3 6 5 -7 1111.36 1270.72 5 6 5 -7-634.970 709.644 2 -6 -5 7-60.6430 1178.55 7 -6 -6 7-614.178 679.145 3 6 6 -7-3195.17 1529.30 5 6 6 -7-1069.88 864.809 2 -6 -6 7-4569.73 1723.18 7 -6 -7 7-927.120 697.346 3 6 7 -7-282.347 1292.47 5 6 7 -7-391.940 757.433 2 -6 -7 7 926.254 1221.44 7 -6 -8 7-689.712 701.249 3 6 8 -7 701.565 1353.66 5 6 8 -7-532.292 840.180 2 -6 -8 7-1717.26 1352.53 7 -6 -9 7-65.5719 766.482 3 6 9 -7-120.791 1503.61 5 6 9 -7-518.334 847.293 2 -6 -9 7-2343.93 1443.10 7 -6 -10 7 337.781 756.628 3 6 -10 -7-97.8868 1491.60 6 -6 10 7-1136.26 1067.67 1 6 10 -7 304.007 1420.46 5 -6 10 7-166.296 1663.66 8 6 10 -7 33.4007 801.027 2 -6 -10 7 731.688 1411.83 7 -6 -11 7 36.2091 865.593 3 6 -11 -7-809.530 1733.96 6 6 11 -7 750.201 1528.72 5 -6 11 7 714.999 1088.04 1 -6 11 7-172.441 1681.58 8 6 -11 -7 230.113 700.519 4 -6 -12 7 148.541 928.196 3 6 -12 -7-311.837 1681.17 6 6 12 -7 1328.34 1624.17 5 -6 12 7-52.4934 1086.59 1 -6 12 7-444.319 1664.87 8 6 12 -7 137.184 863.638 2 6 -12 -7 304.680 712.777 4 -6 -12 7-77.2302 1503.59 7 6 -13 -7 426.847 1747.79 6 -6 13 7 447.497 1736.30 8 6 -13 -7-69.3597 730.207 4 -6 13 7 704.383 1189.40 1 6 2 -8-481.516 1343.91 5 -6 -3 8 2500.58 833.950 3 6 3 -8-957.503 1481.35 5 -6 -4 8 1201.21 751.729 3 6 4 -8 1051.80 1265.16 5 6 4 -8 2191.92 776.346 2 -6 -4 8 558.139 1253.37 7 -6 -5 8 243.715 740.530 3 6 5 -8-54.6986 1212.54 5 6 5 -8 559.994 793.265 2 -6 -5 8 324.476 1294.49 7 -6 -6 8 5932.33 1124.24 3 6 6 -8 5841.79 1587.59 5 6 6 -8 6649.76 1151.83 2 -6 -6 8 7312.78 1719.49 7 -6 -7 8 374.914 799.675 3 6 7 -8-352.189 1373.29 5 6 7 -8 576.133 811.411 2 -6 -7 8-211.074 1330.86 7 -6 -8 8 1476.57 918.751 3 6 8 -8-1374.34 1575.57 5 6 8 -8 231.952 961.928 2 -6 -9 8 305.794 894.383 3 6 9 -8-553.716 1430.47 5 6 9 -8 683.632 886.752 2 -6 -9 8-450.339 1419.59 7 -6 -10 8 1216.85 992.720 3 6 10 -8 2464.83 1509.13 5 6 10 -8 491.685 854.012 2 -6 -10 8-1081.28 1511.09 7 -6 -11 8 643.456 984.933 3 6 11 -8 757.290 895.977 2 -6 12 8-88.3953 1797.91 8 -6 -3 9-1406.99 875.713 3 6 3 -9 794.972 1285.73 5 6 3 -9 718.399 811.834 2 -6 -3 9 316.878 1338.02 7 -6 -4 9-34.7710 863.263 3 6 4 -9-2201.65 1402.81 5 6 4 -9-181.243 817.997 2 -6 -4 9-1198.12 1359.31 7 -6 -5 9-396.045 920.391 3 6 5 -9 1710.72 1379.70 5 6 5 -9 916.010 840.197 2 -6 -5 9 765.383 1423.08 7 -6 -6 9-111.555 986.166 3 6 6 -9-2945.45 1668.29 5 6 6 -9-1907.22 940.689 2 -6 -6 9-4415.99 1934.27 7 -6 -7 9 781.581 990.367 3 6 7 -9 910.691 1467.03 5 6 7 -9 136.359 882.050 2 -6 -7 9 524.758 1547.56 7 -6 -8 9-40.1695 942.286 3 6 8 -9 124.871 1520.02 5 6 8 -9-140.675 899.725 2 -6 -8 9-2242.81 1744.07 7 -6 -9 9-82.3982 976.612 3 6 9 -9-940.259 1571.58 5 6 9 -9 108.503 901.045 2 -6 -9 9-79.4580 1499.90 7 6 10 -9-185.149 966.635 2 -6 -10 9-1708.41 1527.94 7 -6 -4 10 1312.00 1056.30 3 6 4 -10 1369.09 1464.01 5 6 4 -10 3117.90 997.109 2 -6 -4 10 70.9888 1531.73 7 -6 -5 10-238.610 1030.32 3 6 5 -10 1588.21 1579.71 5 6 5 -10 1252.51 911.552 2 -6 -5 10-1701.31 1675.09 7 -6 -6 10 4375.26 1303.13 3 6 6 -10 6323.32 1252.39 2 -6 -6 10 3145.47 1784.66 7 -6 -7 10 125.891 1055.42 3 6 7 -10-1056.37 1566.14 5 6 7 -10 544.392 946.832 2 -6 -7 10-1346.64 1613.77 7 -6 -8 10 2020.00 1155.64 3 6 8 -10 2865.20 1595.70 5 6 8 -10 3247.96 1056.24 2 -6 -8 10 2280.29 1655.72 7 -6 -5 11-1037.96 1005.75 3 6 5 -11-252.552 949.321 2 -6 -5 11-78.8942 1737.32 7 -6 -6 11-531.591 1047.99 3 6 6 -11-37.3220 988.378 2 -6 -6 11-652.504 1750.36 7 -6 -7 11-543.464 980.821 3 6 7 -11-115.274 1046.33 2 -6 -7 11-503.759 1791.39 7 7 13 -1 7836.14 2046.63 5 7 14 -1 3776.72 1727.07 5 -7 -7 2 451.398 791.529 7 -7 -8 2 933.196 885.834 7 -7 -10 2-312.554 966.171 7 7 10 -2-26.1013 633.255 2 -7 -11 2 966.585 1051.98 7 7 11 -2 322.972 682.663 2 7 11 -2 1634.11 1419.36 5 -7 -12 2-1989.61 1413.18 7 7 12 -2-3218.47 1622.23 5 -7 -13 2-1770.96 1314.62 7 7 13 -2 56.9757 761.049 2 7 13 -2-63.3724 1421.74 5 -7 -14 2-2084.66 1302.08 7 -7 -14 2 67.4970 535.220 3 7 14 -2-875.056 1369.80 5 -7 -15 2 2274.88 1296.17 7 -7 -15 2 422.117 617.841 3 -7 -4 3 6647.11 1223.38 7 -7 -6 3 3242.68 1184.47 7 7 6 -3 3891.02 741.423 2 -7 -7 3 5597.46 1268.05 7 7 7 -3 684.861 608.771 2 -7 -8 3 2871.16 1192.02 7 7 8 -3 3991.30 780.647 2 -7 -9 3-2475.60 1216.58 7 7 9 -3-1673.63 772.308 2 7 9 -3-865.847 1449.24 5 -7 -10 3 1662.49 1191.31 7 7 10 -3 2830.99 751.069 2 7 10 -3 1343.90 1404.02 5 -7 -11 3-593.455 1230.64 7 7 11 -3 216.356 663.539 2 7 11 -3-872.623 1347.09 5 -7 -12 3 1831.79 1294.51 7 7 12 -3 1141.57 722.666 2 7 12 -3 230.100 1306.48 5 -7 -13 3-766.323 1244.43 7 7 13 -3 457.634 707.609 2 -7 -13 3-636.791 553.604 3 7 13 -3 160.254 1174.38 5 -7 -14 3 1712.75 1363.47 7 7 14 -3 1289.95 800.855 2 -7 -14 3-50.2413 601.293 3 7 14 -3 1275.73 1344.44 5 -7 -2 4-566.933 794.729 7 7 3 -4 4671.51 864.090 2 -7 -6 4 2342.42 1131.29 7 7 6 -4 1059.23 627.508 2 -7 -7 4-59.3988 1013.14 7 7 7 -4 71.8452 577.034 2 7 7 -4 194.482 1322.80 5 7 8 -4 223.769 826.793 2 7 8 -4-2035.60 1916.90 5 -7 -9 4 191.388 1050.15 7 7 9 -4-178.893 641.617 2 7 9 -4-550.325 1291.05 5 7 10 -4-765.954 686.611 2 7 10 -4 339.493 1216.37 5 -7 -10 4 465.037 1151.73 7 7 11 -4-544.591 822.921 2 -7 -11 4-876.367 590.979 3 7 12 -4 672.281 739.521 2 -7 -12 4 522.467 598.638 3 7 12 -4 2431.81 1244.74 5 -7 -13 4-71.5729 1338.43 7 7 13 -4 463.301 720.784 2 -7 -13 4-384.428 673.906 3 7 13 -4 2231.16 1438.94 5 -7 -14 4-1024.79 1400.86 7 7 14 -4-1036.88 800.300 2 -7 0 5 3646.01 886.251 7 -7 -1 5 370.084 780.746 7 7 1 -5 729.613 488.668 2 7 2 -5 12065.6 1392.64 2 -7 -2 5 10403.6 1661.95 7 -7 -3 5 2176.04 1036.35 7 7 3 -5 3104.66 682.572 2 7 4 -5 2377.26 1349.93 5 7 5 -5 633.608 574.887 2 7 5 -5-370.164 1324.69 5 -7 -5 5 627.892 1070.53 7 7 6 -5 3210.12 721.676 2 7 6 -5 1791.95 1304.13 5 -7 -6 5 1487.99 1126.74 7 7 7 -5-787.152 843.793 2 7 7 -5-4841.10 1996.13 5 7 8 -5 1107.01 692.636 2 7 8 -5 943.785 1154.05 5 -7 -8 5 1225.07 1117.47 7 7 9 -5 982.224 695.934 2 -7 -9 5 155.083 509.179 3 7 9 -5 51.8741 1093.76 5 -7 9 5-242.852 1472.83 8 -7 -9 5-1400.93 1218.71 7 7 10 -5 3944.46 892.524 2 -7 -10 5 1180.82 671.868 3 -7 10 5 252.881 2582.49 8 -7 -10 5-1720.71 1556.13 7 7 11 -5 1073.08 741.621 2 -7 -11 5-571.844 644.671 3 7 11 -5-1220.59 1367.82 5 -7 11 5-87.3783 1624.45 8 -7 -11 5 779.269 1314.49 7 7 12 -5-89.3424 767.568 2 -7 -12 5 530.044 618.134 3 7 12 -5 881.781 1351.79 5 -7 12 5-269.858 1630.09 8 -7 -12 5 363.565 1298.93 7 7 13 -5 396.487 793.500 2 -7 -13 5-666.991 1326.40 7 -7 -1 6 146.369 905.676 7 7 1 -6 215.440 552.963 2 7 1 -6 638.062 1148.36 5 7 2 -6-163.777 542.969 2 -7 -2 6 258.761 993.238 7 7 3 -6 339.068 1059.25 5 7 4 -6 303.331 607.334 2 7 4 -6-706.514 1124.62 5 -7 -4 6-1716.88 1116.30 7 7 5 -6-1976.94 813.667 2 -7 -5 6-936.432 525.703 3 7 5 -6-3251.22 1563.76 5 7 6 -6 26.2690 650.127 2 -7 -6 6-485.154 507.420 3 7 6 -6-986.009 1135.96 5 -7 -6 6-2599.69 1290.72 7 7 7 -6 1065.57 725.194 2 -7 -7 6-23.5562 536.171 3 7 7 -6-203.889 1066.84 5 -7 -7 6 527.345 1098.64 7 7 8 -6-481.594 698.098 2 -7 -8 6 121.458 523.532 3 7 8 -6 1674.52 1240.31 5 -7 -8 6 136.659 1238.05 7 7 9 -6 937.353 811.292 2 -7 -9 6-80.9017 645.974 3 7 9 -6 402.291 1403.96 5 7 10 -6-422.689 775.280 2 -7 -10 6-909.490 694.810 3 7 10 -6-187.321 1373.75 5 -7 10 6 345.180 1648.25 8 -7 -10 6-1091.19 1327.49 7 7 11 -6-279.225 789.941 2 -7 -11 6-511.258 718.608 3 7 -11 -6-851.584 1290.10 6 7 11 -6 127.307 1403.26 5 -7 11 6 178.510 1731.75 8 -7 -11 6 74.6858 1320.16 7 7 12 -6-158.921 841.287 2 -7 -12 6 32.9087 774.443 3 7 -12 -6-109.577 1284.67 6 7 12 -6 1042.28 1516.28 5 -7 12 6-274.796 1767.44 8 -7 -12 6-229.430 1382.82 7 -7 13 6-187.384 1634.37 8 -7 -2 7 2791.90 722.330 3 7 2 -7 7241.87 1590.48 5 7 3 -7-338.088 755.592 2 -7 -3 7 1801.28 637.391 3 7 3 -7-1571.88 1392.28 5 -7 -4 7 1058.72 590.095 3 7 4 -7-51.1389 1163.36 5 -7 -4 7 612.479 1213.08 7 7 4 -7 1367.76 688.352 2 -7 -5 7 599.438 534.174 3 7 5 -7-637.137 1205.30 5 -7 -5 7 64.0033 1199.30 7 7 5 -7 26.4908 661.086 2 -7 -6 7 3567.13 824.475 3 7 6 -7 2325.42 1453.18 5 -7 -6 7 5586.58 1572.57 7 7 6 -7 5647.18 950.076 2 -7 -7 7 819.558 688.506 3 7 7 -7-360.216 1326.91 5 -7 -7 7 1588.39 1317.67 7 7 7 -7 729.419 734.179 2 -7 -8 7 1426.35 723.396 3 7 8 -7-1844.81 1486.99 5 7 8 -7 90.6172 806.886 2 -7 -8 7-1929.32 1667.61 7 -7 -9 7 767.914 738.679 3 7 9 -7 821.815 1539.44 5 7 9 -7 1246.71 816.029 2 -7 -9 7 73.6906 1329.77 7 -7 -10 7 1903.62 871.437 3 7 10 -7 2882.15 1596.72 5 7 10 -7 2403.69 872.124 2 -7 -10 7 2044.91 1587.55 7 -7 -11 7-1629.40 1423.16 7 7 11 -7 98.5944 845.160 2 -7 -3 8 55.6670 705.168 3 7 3 -8 2575.41 1448.42 5 -7 -3 8 3149.65 1410.75 7 7 3 -8 1223.20 734.851 2 -7 -4 8-28.9079 698.195 3 7 4 -8-626.316 1367.14 5 7 4 -8 381.950 731.788 2 -7 -4 8 711.690 1275.02 7 -7 -5 8 329.284 724.547 3 7 5 -8-873.529 1264.42 5 7 5 -8 455.853 743.344 2 -7 -5 8 2025.72 1397.97 7 7 6 -8-120.349 1824.85 5 7 6 -8 92.8849 959.007 2 -7 -7 8-168.647 789.170 3 7 7 -8-558.160 1471.84 5 7 7 -8 96.2851 777.923 2 -7 -7 8-870.613 1407.53 7 -7 -8 8 2080.02 991.048 3 7 8 -8 1466.99 1721.22 5 7 8 -8 1293.02 988.211 2 -7 -9 8 497.565 830.149 3 7 9 -8 1086.61 1530.38 5 7 9 -8 614.410 866.592 2 -7 -9 8 77.0423 1413.91 7 7 10 -8-455.113 892.890 2 -7 -10 8 396.186 1520.92 7 -7 -4 9 1630.40 950.012 3 7 4 -9 2334.95 1405.09 5 7 4 -9 2267.47 868.749 2 -7 -4 9 136.979 1514.07 7 -7 -5 9 315.622 844.757 3 7 5 -9 361.684 1431.54 5 7 5 -9 819.362 870.860 2 -7 -5 9 784.843 1409.49 7 -7 -6 9 5597.93 1285.78 3 7 6 -9 3798.26 1760.24 5 7 6 -9 6544.01 1276.03 2 -7 -6 9 7623.08 2067.30 7 -7 -7 9 371.009 904.328 3 7 7 -9 1447.83 1468.51 5 7 7 -9 1692.02 914.515 2 -7 -7 9 229.587 1461.31 7 -7 -8 9 1647.01 1077.57 3 7 8 -9 1807.49 1579.66 5 7 8 -9 1882.69 954.961 2 -7 -8 9 551.606 1636.45 7 -7 -5 10-240.487 1014.69 3 7 5 -10-683.582 1539.86 5 7 5 -10-34.1602 900.173 2 -7 -5 10-376.088 1621.10 7 -7 -6 10-534.822 1034.75 3 7 6 -10-2105.41 1600.26 5 7 6 -10 141.530 909.777 2 -7 -6 10-545.031 1634.66 7 -7 -7 10-1601.10 1058.60 3 7 7 -10 767.385 1601.10 5 7 7 -10-1277.75 1018.60 2 -7 -7 10-160.579 1614.77 7 7 6 -11 708.811 1042.19 2 -7 -6 11-657.007 1782.90 7 8 12 -2 741.704 1654.17 5 8 13 -2 962.303 1651.99 5 -8 -7 3 61.8648 842.589 7 -8 -8 3 63.6726 924.581 7 -8 -9 3-982.343 1036.29 7 8 10 -3 5935.54 2747.24 5 -8 -10 3 29466.8 2780.71 7 -8 -11 3-207.017 1213.04 7 8 11 -3-1906.19 1592.11 5 -8 -12 3 141.342 1120.61 7 8 12 -3-1349.41 1526.25 5 -8 -13 3 1083.05 1251.59 7 8 13 -3-308.950 1426.20 5 -8 -4 4 3062.19 967.589 7 -8 -5 4 761.930 974.650 7 8 6 -4-1519.59 869.938 2 -8 -7 4 691.277 1070.96 7 8 7 -4 1622.10 701.643 2 -8 -8 4 259.196 1099.14 7 8 8 -4 1019.23 702.035 2 8 8 -4 1656.11 1486.33 5 -8 -9 4 2902.96 1259.94 7 8 9 -4-801.195 717.932 2 8 9 -4 506.257 1571.92 5 -8 -10 4 485.634 1200.74 7 8 10 -4 823.763 707.448 2 8 10 -4 2269.81 1484.61 5 -8 -11 4 355.790 1340.70 7 8 11 -4 145.743 707.198 2 8 11 -4-183.882 1336.01 5 -8 -12 4-1383.67 1354.79 7 8 12 -4 1253.62 777.192 2 -8 -12 4 482.703 558.418 3 8 12 -4-249.701 1508.30 5 -8 -3 5 1451.71 1081.04 7 8 4 -5 6282.78 1189.77 2 -8 -5 5-2976.73 1242.24 7 8 5 -5-768.947 665.885 2 8 5 -5-342.138 1493.22 5 -8 -6 5 628.952 1061.00 7 8 6 -5 436.698 635.409 2 8 6 -5-414.784 1490.19 5 -8 -7 5 455.114 1131.59 7 8 7 -5-105.540 671.940 2 8 7 -5 141.926 1540.18 5 -8 -8 5-202.733 1221.92 7 8 8 -5-54.4699 673.311 2 8 8 -5 263.133 1367.86 5 -8 -9 5 973.971 1270.93 7 8 9 -5-28.0645 688.164 2 8 9 -5 666.436 1277.38 5 8 10 -5 28.8418 760.915 2 -8 -10 5 239.771 541.482 3 8 10 -5-681.079 1474.14 5 -8 -11 5-1904.73 1390.70 7 8 11 -5-88.7148 728.901 2 -8 -11 5 79.2821 613.886 3 8 11 -5-401.113 1307.36 5 8 2 -6-867.805 767.409 2 8 2 -6-3067.59 1703.46 5 -8 -3 6 579.948 1063.52 7 8 3 -6 23.6391 598.909 2 8 3 -6-714.105 1438.62 5 -8 -4 6 850.343 1295.82 7 8 4 -6 4518.53 809.678 2 8 4 -6 1214.34 1379.96 5 -8 -5 6 1135.19 1131.24 7 8 5 -6 608.690 685.123 2 8 5 -6 1065.22 1342.76 5 -8 -6 6 1764.20 1208.59 7 8 6 -6 1840.80 707.360 2 8 6 -6 1567.86 1270.65 5 8 7 -6-1781.28 846.501 2 -8 -7 6-92.6286 544.372 3 8 7 -6 119.333 1388.26 5 8 8 -6 3036.63 822.041 2 -8 -8 6 1875.16 656.368 3 8 8 -6 2664.01 1311.93 5 -8 -8 6 3089.38 1363.45 7 8 9 -6 57.3512 763.835 2 -8 -9 6 1049.81 661.984 3 8 9 -6 422.103 1465.40 5 8 10 -6 1177.94 769.106 2 -8 -10 6 28.9180 679.855 3 8 10 -6 616.161 1351.00 5 -8 -10 6-1483.41 1434.17 7 8 2 -7 815.923 715.161 2 8 2 -7 335.462 1117.51 5 -8 -3 7-1939.24 1277.65 7 8 3 -7 145.993 684.775 2 -8 -3 7-42.6537 517.167 3 8 3 -7-696.170 1062.50 5 8 4 -7 25.1500 671.344 2 -8 -4 7 524.350 550.015 3 8 4 -7 566.231 1111.24 5 -8 -4 7-508.506 1215.78 7 8 5 -7-1332.63 795.254 2 -8 -5 7-73.7863 563.705 3 -8 -5 7-1122.36 1286.73 7 8 6 -7-189.614 755.696 2 -8 -6 7-1012.50 609.361 3 8 6 -7-1973.86 1394.83 5 8 7 -7-28.9508 725.883 2 -8 -7 7 252.377 647.953 3 8 7 -7 2027.84 1410.35 5 8 8 -7-806.167 798.613 2 -8 -8 7-1063.07 717.886 3 8 8 -7-1228.55 1438.61 5 -8 -8 7-1900.87 1478.63 7 8 9 -7 767.203 791.211 2 -8 -9 7-217.848 733.362 3 8 9 -7-463.001 1495.38 5 -8 -9 7-2855.31 1488.38 7 8 3 -8 151.267 756.125 2 8 3 -8-875.857 1554.34 5 8 4 -8 2035.64 762.310 2 -8 -4 8 484.212 718.220 3 8 4 -8-362.269 1378.20 5 -8 -4 8-799.973 1375.83 7 8 5 -8 563.831 794.757 2 -8 -5 8 411.123 711.058 3 8 5 -8 2054.70 1501.05 5 -8 -5 8-692.228 1399.79 7 8 6 -8 1548.02 937.997 2 -8 -6 8 2294.72 889.716 3 8 7 -8 1088.97 818.425 2 -8 -7 8 1027.19 831.731 3 8 7 -8 1698.74 1628.61 5 -8 -7 8 2292.82 1499.55 7 8 8 -8 2883.47 923.556 2 -8 -8 8 1661.89 908.064 3 8 8 -8 3277.10 1675.82 5 -8 -8 8 77.3880 1567.91 7 8 4 -9 2364.08 1555.53 5 8 5 -9-274.125 807.566 2 -8 -5 9 104.678 877.187 3 8 5 -9-64.0542 1505.89 5 -8 -5 9-2211.99 1556.96 7 8 6 -9 378.200 877.572 2 -8 -6 9 286.469 850.770 3 8 6 -9-2183.64 1633.90 5 -8 -6 9-76.2491 1535.77 7 -8 -7 9 146.646 845.930 3 8 7 -9 394.867 1636.38 5 -8 -7 9-550.021 1543.63 7 8 7 -9 974.904 861.976 2 -8 -6 10-1195.34 1657.20 7 8 6 -10 671.247 973.467 2 -9 -8 4 68.8987 886.315 7 -9 -9 4 1763.99 1145.38 7 9 9 -4-1336.95 1746.02 5 -9 -10 4-72.1610 1083.70 7 9 10 -4 313.516 1701.16 5 -9 -5 5-1545.92 984.857 7 -9 -6 5 2120.25 1257.70 7 9 6 -5 5853.01 2020.46 5 -9 -7 5-479.024 1058.16 7 9 7 -5-426.947 727.096 2 9 7 -5 380.862 1593.97 5 -9 -8 5 4353.68 1474.01 7 9 8 -5 1402.71 843.106 2 9 8 -5 2327.68 1761.12 5 -9 -9 5 1726.66 1333.48 7 9 9 -5 1138.37 754.283 2 9 9 -5 1712.55 1571.55 5 9 10 -5 2177.30 849.176 2 9 2 -6 279.928 1617.08 5 -9 -3 6 493.573 969.439 7 9 3 -6-920.301 1521.20 5 -9 -4 6-2292.72 1260.77 7 9 4 -6 2327.41 1810.83 5 -9 -5 6-2046.35 1299.44 7 9 5 -6-82.2257 731.123 2 9 5 -6-337.202 1474.81 5 -9 -6 6 67.9919 1132.84 7 9 6 -6 282.486 707.566 2 9 6 -6-1932.38 1470.09 5 -9 -7 6-424.480 1402.91 7 9 7 -6-635.445 760.904 2 9 7 -6-1078.71 1441.70 5 -9 -8 6 799.107 1261.60 7 9 8 -6 207.706 723.081 2 -9 -8 6-301.370 575.138 3 9 8 -6 64.7200 1404.69 5 -9 -9 6 967.363 1365.58 7 9 9 -6 395.350 773.057 2 9 9 -6 597.641 1202.89 5 -9 -3 7-63.5776 1177.77 7 9 3 -7 1107.03 713.278 2 9 3 -7 531.595 1351.54 5 -9 -4 7 532.090 1249.36 7 9 4 -7 1652.59 744.867 2 -9 -4 7 118.170 570.894 3 9 4 -7-1397.90 1488.55 5 9 5 -7 363.754 800.849 2 -9 -5 7 1018.19 639.712 3 9 5 -7-1131.40 1348.63 5 -9 -6 7 1980.73 1389.30 7 9 6 -7 3663.75 869.884 2 -9 -6 7 2360.62 770.155 3 9 6 -7 3360.67 1402.34 5 -9 -7 7 1393.04 1415.93 7 9 7 -7 88.4716 809.761 2 -9 -7 7 520.691 670.414 3 9 7 -7 1776.90 1359.41 5 -9 -8 7-225.663 1364.47 7 9 8 -7 968.770 794.831 2 9 8 -7 448.873 1337.05 5 -9 -4 8 481.092 1338.98 7 9 4 -8-361.192 766.047 2 -9 -4 8-882.994 713.744 3 9 4 -8-423.156 1408.05 5 9 5 -8 775.089 816.510 2 -9 -5 8 263.040 748.161 3 9 5 -8 131.245 1538.70 5 -9 -6 8-1031.50 1442.15 7 9 6 -8-88.7844 803.825 2 -9 -6 8-1645.01 801.165 3 9 6 -8-470.293 1473.23 5 -9 -7 8-1665.99 1572.57 7 9 7 -8 513.487 813.079 2 -9 -7 8 647.184 795.496 3 9 5 -9 531.739 842.668 2 9 5 -9 1421.42 1552.23 5 -9 -5 9 1495.21 1669.95 7 -9 -6 9-2078.69 1601.58 7 10 4 -6-1728.10 1708.51 5 10 5 -6 1681.91 1755.94 5 10 6 -6-1253.44 1749.91 5 -10 -7 6 513.186 1143.96 7 10 7 -6 674.120 1707.53 5 -10 -4 7 416.659 1055.41 7 10 4 -7 65.0427 1464.89 5 -10 -5 7 1638.96 1242.65 7 10 5 -7-66.4149 1441.51 5 -10 -6 7 657.639 1374.11 7 -10 -6 7-105.268 647.766 3 -10 -5 8-513.652 1460.87 7 -10 -5 8 514.968 724.135 3 10 5 -8-304.286 865.362 2 10 5 -8 65.4837 1053.67 5 0 0 0 0.00 0.00 0 TITL CoGF_newpar_ in Pnna REM Pnna (#52, found as Pnan in a-cb setting) CELL 0.48590 8.220404 11.643740 8.922303 90.0000 90.0000 90.0000 ZERR 4.00 0.004261 0.002021 0.003024 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z SYMM -x+1/2, y+1/2,-z+1/2 SYMM x,-y+1/2,-z+1/2 SFAC C H N O Co UNIT 16.00 36.00 12.00 24.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 47576 data_023_CoGF_1-21GPa _audit_creation_method ; XIA2 0.5.438-g5f426072-dials-1.7 SHELXL-2017/1 ; _audit_creation_date 2018-08-01 _publ_contact_author_address ; School of Physics and Astronomy Queen Mary University of London Mile End Rd, London E1 4NS U.K. ; _publ_contact_author_email a.e.phillips@qmul.ac.uk _publ_contact_author_name 'Anthony E. Phillips' _publ_contact_author_phone '+44 2078 823 429' _chemical_name_systematic 'guanidinium cobalt(II) formate' _chemical_name_common 'guanidinium cobalt(II) formate' _chemical_formula_moiety 'C3 H3 Co O6, C H6 N3' _chemical_formula_sum 'C4 H9 Co N3 O6' _chemical_formula_weight 254.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.2660 0.4750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_H-M_alt 'P n n a' _space_group_name_Hall '-P 2a 2bc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 8.141(12) _cell_length_b 11.583(5) _cell_length_c 8.896(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 838.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 498 _cell_measurement_theta_max 19.5719820457 _cell_measurement_theta_min 1.95231678705 _exptl_crystal_description block _exptl_crystal_colour 'intense pink' _exptl_crystal_density_diffrn 2.012 _exptl_crystal_F_000 516 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_T_min 0.99947259045 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CCP4 7.0.044: AIMLESS, version 0.5.32 : 29/03/17 Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics ; _diffrn_ambient_temperature 293(2) _diffrn_ambient_pressure 1210000 _diffrn_radiation_wavelength 0.4859 _diffrn_radiation_type 'Synchrotron' _diffrn_radiation_source 'Diamond Light Source Beamline I19' _diffrn_radiation_monochromator 'double crystal Silicon 111' _diffrn_measurement_specimen_support 'diamond anvil cell' _diffrn_measurement_device 'Newport IS4CCD (4 circle)' _diffrn_measurement_device_type 'Pilatus 300K' _diffrn_measurement_method ; \w scans with 0.2 degree frames ; _diffrn_reflns_number 1445 _diffrn_reflns_av_unetI/netI 0.1163 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.318 _diffrn_reflns_theta_max 18.637 _diffrn_reflns_theta_full 16.950 _diffrn_measured_fraction_theta_max 0.431 _diffrn_measured_fraction_theta_full 0.457 _diffrn_reflns_Laue_measured_fraction_max 0.431 _diffrn_reflns_Laue_measured_fraction_full 0.457 _diffrn_reflns_point_group_measured_fraction_max 0.431 _diffrn_reflns_point_group_measured_fraction_full 0.457 _reflns_number_total 433 _reflns_number_gt 208 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_reduction ; aimless (Evans, P. R. and Murshudov, G. N., 2013) ccp4 (Winn, M. D. et al., 2011) DIALS 1.7.3-gc8f60bf0-release pointless (Evans, P., 2006) XIA2 0.5.438-g5f426072-dials-1.7 (Winter, G., 2010) ; _publ_section_references ; Evans, P. (2006) Acta Cryst. D62, 72-82. Evans, P. R. and Murshudov, G. N. (2013) Acta Cryst. D69, 1204-1214. Winn, M. D. et al. (2011) Acta Cryst. D67, 235-242. Winter, G. (2010) J. Appl. Cryst. 43, 186-190. ; _computing_cell_refinement 'DIALS 2theta refinement, DIALS 1.7.3-gc8f60bf0-release' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 433 _refine_ls_number_parameters 66 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2626(2) 0.250000 0.250000 0.0201(6) Uani 1 2 d S T P . . O21 O 0.4171(8) 0.1781(4) 0.4096(6) 0.0262(19) Uani 1 1 d . . . . . C21 C 0.5331(12) 0.2209(6) 0.4823(8) 0.021(3) Uani 1 1 d . . . . . H21 H 0.594976 0.278729 0.437069 0.025 Uiso 1 1 calc R U . . . O22 O 0.5707(8) 0.1902(4) 0.6128(6) 0.0283(19) Uani 1 1 d . . . . . O31 O 0.2637(7) 0.4047(3) 0.3697(6) 0.0273(19) Uani 1 1 d . . . . . C31 C 0.250000 0.500000 0.3039(12) 0.028(4) Uani 1 2 d S TU P . . H31 H 0.250002 0.500001 0.199361 0.033 Uiso 1 2 calc R U P . . N41 N 0.250000 0.500000 0.9048(11) 0.033(3) Uani 1 2 d S T P . . H41A H 0.312931 0.453331 0.953183 0.039 Uiso 0.5 1 calc R U P . . H41B H 0.187069 0.546669 0.953183 0.039 Uiso 0.5 1 calc R U P . . C41 C 0.250000 0.500000 0.7588(14) 0.028(3) Uani 1 2 d S T P . . N42 N 0.3468(11) 0.4282(5) 0.6830(8) 0.037(3) Uani 1 1 d . . . . . H42A H 0.410042 0.381315 0.730642 0.044 Uiso 1 1 calc R U . . . H42B H 0.346194 0.428664 0.586337 0.044 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0278(19) 0.0161(6) 0.0163(12) 0.0014(6) 0.000 0.000 O21 0.027(6) 0.027(3) 0.025(4) 0.003(2) -0.014(3) -0.002(3) C21 0.020(8) 0.022(4) 0.021(6) 0.003(3) -0.006(4) -0.009(4) O22 0.035(7) 0.037(3) 0.013(4) 0.002(3) -0.009(3) -0.005(3) O31 0.047(7) 0.0102(19) 0.025(4) -0.003(2) 0.001(3) 0.004(3) C31 0.047(15) 0.025(4) 0.011(9) 0.000 0.000 -0.002(6) N41 0.059(12) 0.023(4) 0.016(6) 0.000 0.000 0.012(6) C41 0.042(12) 0.022(4) 0.019(6) 0.000 0.000 -0.004(6) N42 0.055(10) 0.045(3) 0.010(6) -0.005(3) -0.002(4) 0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O21 2.071(6) 4 ? Co1 O21 2.071(6) . ? Co1 O31 2.084(4) . ? Co1 O31 2.084(4) 4 ? Co1 O22 2.100(6) 7_565 ? Co1 O22 2.100(6) 6_556 ? O21 C21 1.247(8) . ? C21 O22 1.252(8) . ? C21 H21 0.9300 . ? O31 C31 1.255(7) . ? C31 H31 0.9300 . ? N41 C41 1.299(13) . ? N41 H41A 0.8600 . ? N41 H41B 0.8600 . ? C41 N42 1.329(8) . ? C41 N42 1.329(8) 2_565 ? N42 H42A 0.8600 . ? N42 H42B 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O21 Co1 O21 105.2(4) 4 . ? O21 Co1 O31 90.1(2) 4 . ? O21 Co1 O31 89.6(2) . . ? O21 Co1 O31 89.6(2) 4 4 ? O21 Co1 O31 90.1(2) . 4 ? O31 Co1 O31 179.5(3) . 4 ? O21 Co1 O22 85.5(2) 4 7_565 ? O21 Co1 O22 169.3(3) . 7_565 ? O31 Co1 O22 91.0(2) . 7_565 ? O31 Co1 O22 89.4(2) 4 7_565 ? O21 Co1 O22 169.3(3) 4 6_556 ? O21 Co1 O22 85.5(2) . 6_556 ? O31 Co1 O22 89.4(2) . 6_556 ? O31 Co1 O22 91.0(2) 4 6_556 ? O22 Co1 O22 83.9(3) 7_565 6_556 ? C21 O21 Co1 130.9(5) . . ? O21 C21 O22 123.6(8) . . ? O21 C21 H21 118.2 . . ? O22 C21 H21 118.2 . . ? C21 O22 Co1 128.9(5) . 6_656 ? C31 O31 Co1 121.2(6) . . ? O31 C31 O31 124.4(10) . 2_565 ? O31 C31 H31 117.8 . . ? O31 C31 H31 117.8 2_565 . ? C41 N41 H41A 120.0 . . ? C41 N41 H41B 120.0 . . ? H41A N41 H41B 120.0 . . ? N41 C41 N42 120.5(6) . . ? N41 C41 N42 120.5(6) . 2_565 ? N42 C41 N42 119.0(13) . 2_565 ? C41 N42 H42A 120.0 . . ? C41 N42 H42B 120.0 . . ? H42A N42 H42B 120.0 . . ? _refine_diff_density_max 0.417 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.088 _shelx_res_file ; TITL CoGF 1.21 GPa in Pnna 023_CoGF_1-21GPa.res created by SHELXL-2017/1 at 15:01:21 on 01-Aug-2018 CELL 0.4859 8.141 11.5833 8.8956 90 90 90 ZERR 4 0.0117 0.0054 0.0082 0 0 0 LATT 1 SYMM 0.5-X,-Y,+Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +X,0.5-Y,0.5-Z SFAC C H Co N O DISP C 0.001 0.001 6.068 DISP Co 0.266 0.475 1359.652 DISP H -0 0 0.607 DISP N 0.002 0.001 8.983 DISP O 0.004 0.003 13.336 UNIT 16 36 4 12 24 RIGU L.S. 10 PLAN 15 BOND $H LIST 3 FMAP 2 ACTA OMIT 2 5 7 OMIT 1 13 1 OMIT 6 10 5 OMIT 2 13 3 OMIT 2 8 8 RIGU ISOR 0.05 C31 WGHT 0.029800 FVAR 0.62442 CO1 3 0.262617 0.250000 0.250000 10.50000 0.02784 0.01608 = 0.01634 0.00135 0.00000 0.00000 O21 5 0.417102 0.178077 0.409578 11.00000 0.02696 0.02693 = 0.02473 0.00342 -0.01377 -0.00220 C21 1 0.533050 0.220874 0.482266 11.00000 0.01990 0.02208 = 0.02102 0.00281 -0.00649 -0.00852 AFIX 43 H21 2 0.594976 0.278729 0.437069 11.00000 -1.20000 AFIX 0 O22 5 0.570665 0.190217 0.612776 11.00000 0.03486 0.03713 = 0.01285 0.00174 -0.00859 -0.00503 O31 5 0.263730 0.404657 0.369671 11.00000 0.04698 0.01021 = 0.02481 -0.00326 0.00136 0.00352 C31 1 0.250000 0.500000 0.303907 10.50000 0.04738 0.02520 = 0.01059 0.00000 0.00000 -0.00210 AFIX 43 H31 2 0.250002 0.500001 0.199361 10.50000 -1.20000 AFIX 0 N41 4 0.250000 0.500000 0.904844 10.50000 0.05890 0.02271 = 0.01642 0.00000 0.00000 0.01190 AFIX 93 H41A 2 0.312931 0.453331 0.953183 10.50000 -1.20000 H41B 2 0.187069 0.546669 0.953183 10.50000 -1.20000 AFIX 0 C41 1 0.250000 0.500000 0.758826 10.50000 0.04227 0.02152 = 0.01889 0.00000 0.00000 -0.00389 N42 4 0.346807 0.428209 0.683011 11.00000 0.05471 0.04476 = 0.01023 -0.00483 -0.00246 0.01787 AFIX 93 H42A 2 0.410042 0.381315 0.730642 11.00000 -1.20000 H42B 2 0.346194 0.428664 0.586337 11.00000 -1.20000 AFIX 0 HKLF 4 REM CoGF 1.21 GPa in Pnna REM R1 = 0.0499 for 208 Fo > 4sig(Fo) and 0.1188 for all 433 data REM 66 parameters refined using 42 restraints END WGHT 0.0283 0.0000 REM Highest difference peak 0.417, deepest hole -0.461, 1-sigma level 0.088 Q1 1 0.2500 0.5000 0.8276 10.50000 0.05 0.42 Q2 1 0.6179 0.2525 0.6718 11.00000 0.05 0.40 Q3 1 0.1940 0.3317 0.3270 11.00000 0.05 0.36 Q4 1 0.7301 0.2939 0.4161 11.00000 0.05 0.35 Q5 1 0.2500 0.5000 0.6772 10.50000 0.05 0.34 Q6 1 0.4238 0.2533 0.3277 11.00000 0.05 0.33 Q7 1 0.5977 0.1378 0.7525 11.00000 0.05 0.33 Q8 1 0.6941 0.1678 0.6746 11.00000 0.05 0.31 Q9 1 0.2734 0.3498 0.2507 11.00000 0.05 0.30 Q10 1 0.0496 0.4396 0.9410 11.00000 0.05 0.27 Q11 1 0.2593 0.3399 0.6815 11.00000 0.05 0.27 Q12 1 0.2574 0.3379 0.8215 11.00000 0.05 0.26 Q13 1 0.1664 0.4225 0.6619 11.00000 0.05 0.26 Q14 1 0.3459 0.4233 0.8254 11.00000 0.05 0.26 Q15 1 0.5177 0.2106 0.7446 11.00000 0.05 0.25 ; _shelx_res_checksum 42604 _shelx_hkl_file ; 0 2 0 3657.90 253.86 0 2 0 3687.79 268.27 0 2 0 3533.07 252.38 0 2 0 3209.39 262.84 0 -2 0 3089.52 233.17 0 -2 0 3282.60 338.91 0 2 1 3.76 9.31 0 -2 -1 2.79 3.95 0 2 -1 5.58 6.01 0 2 -1 1.74 11.87 0 -2 1 0.63 5.23 0 2 -2 10.63 14.37 0 -2 2 0.67 7.37 0 3 0 1.83 7.61 0 3 0 0.58 5.20 0 3 0 -8.70 9.39 0 -3 0 1.66 4.75 0 -3 0 -1.90 11.86 0 3 1 2033.28 254.46 0 -3 -1 2095.57 171.24 0 -3 -1 2065.02 229.82 0 3 -1 1935.69 141.91 0 3 -1 1993.40 150.49 0 3 -1 1823.06 152.81 0 3 -1 1910.67 146.82 0 -3 1 2002.67 148.50 0 -3 1 2038.16 157.52 0 3 -2 2.49 12.60 0 3 -2 -8.58 21.98 0 -3 2 4.46 9.88 0 4 0 4690.99 338.94 0 4 0 4236.51 305.25 0 4 0 4116.26 328.86 0 4 0 3791.05 312.03 0 -4 0 4396.22 308.31 0 -4 0 4342.10 374.01 0 4 1 -6.88 10.13 0 4 1 0.69 18.60 0 4 1 3.25 26.17 0 -4 -1 -2.33 8.16 0 -4 -1 -9.80 18.89 0 4 -1 2.44 12.53 0 4 -1 2.73 8.35 0 4 -1 -7.57 14.32 0 4 -1 -2.98 24.71 0 -4 1 10.85 24.29 0 -4 1 -28.87 14.17 0 4 -3 -3.78 18.39 0 4 -3 3.15 31.82 0 -4 3 0.68 17.51 0 4 -4 3876.95 457.68 0 -4 4 3764.25 287.96 0 -5 0 0.00 10.15 0 5 -2 3.93 18.83 0 5 -2 4.09 20.56 0 5 -2 8.98 39.26 0 -5 2 1.18 17.86 0 5 -3 696.50 64.48 0 5 -3 698.23 75.08 0 -5 3 699.05 59.56 0 5 -5 700.43 85.21 0 -5 5 685.20 63.02 0 6 0 1105.47 96.49 0 6 0 1075.48 83.27 0 6 0 1156.66 106.10 0 6 0 1144.24 99.87 0 -6 0 1290.68 90.67 0 -6 0 1084.01 102.75 0 6 1 6.69 38.97 0 6 -1 -48.07 23.36 0 6 -1 8.20 12.94 0 6 -1 1.26 25.48 0 6 -1 -13.09 41.13 0 -6 1 -13.63 12.08 0 -6 1 -29.59 33.31 0 -6 1 -22.80 23.47 0 6 2 1950.26 193.87 0 6 -2 2043.47 152.15 0 6 -2 1987.44 152.10 0 6 -2 2114.49 170.17 0 -6 2 2127.92 154.90 0 6 -4 1499.42 130.70 0 6 -4 1654.01 154.15 0 -6 4 1545.63 120.85 0 6 -6 15.61 32.25 0 7 0 2.82 21.91 0 7 0 6.89 16.70 0 7 0 -52.68 45.76 0 -7 0 -43.83 36.67 0 -7 -1 -4.07 18.23 0 -7 1 1.31 15.95 0 7 3 369.37 48.03 0 7 -3 374.30 44.98 0 7 -3 453.67 69.36 0 -7 3 429.57 44.95 0 7 -4 14.82 30.71 0 7 -4 7.91 62.46 0 -7 4 10.72 31.67 0 7 -5 12.28 33.56 0 7 -5 74.86 64.60 0 -7 5 21.05 33.04 0 7 -6 12.16 37.34 0 8 0 352.68 42.79 0 8 0 338.68 51.81 0 8 0 488.43 67.64 0 -8 0 372.99 37.19 0 -8 0 386.37 60.48 0 8 1 -24.65 20.78 0 8 1 -87.08 43.99 0 8 1 -9.59 50.76 0 -8 -1 23.66 20.38 0 -8 -1 -3.87 44.23 0 8 -1 1.85 27.53 0 8 -1 6.30 18.28 0 8 -1 0.40 33.09 0 8 -1 -28.87 58.91 0 -8 1 -19.74 17.79 0 -8 1 -8.64 44.12 0 8 2 1668.33 147.16 0 8 2 1812.33 216.89 0 8 -2 1814.29 138.04 0 8 -2 1711.87 157.85 0 -8 2 1909.02 141.37 0 -8 2 1638.56 232.62 0 8 -4 2176.92 168.32 0 8 -4 2215.76 200.32 0 -8 4 2218.69 172.12 0 8 -6 530.45 61.94 0 8 -6 517.32 97.62 0 -8 6 496.36 58.88 0 9 2 -39.72 26.30 0 9 2 -37.41 61.58 0 -9 -2 32.42 42.23 0 9 -2 3.98 35.91 0 9 -2 33.69 71.17 0 -9 2 -11.59 32.52 0 -9 2 21.55 55.22 0 9 -3 122.98 38.65 0 9 -3 125.51 69.02 0 -9 3 174.18 37.95 0 9 -5 105.60 43.57 0 9 -5 108.54 79.38 0 -9 5 175.86 42.74 0 9 -7 -3.02 47.12 0 10 0 2.23 27.11 0 10 0 6.91 64.78 0 10 1 5.60 61.05 0 10 -1 9.82 34.36 0 10 -1 -62.34 79.36 0 10 3 -38.16 73.17 0 10 -3 0.00 43.27 0 10 -3 9.97 70.55 0 -10 3 10.12 35.97 0 10 -4 1168.74 100.88 0 -10 5 -56.47 43.01 0 10 -6 159.02 52.86 0 -10 6 229.80 49.94 0 11 0 65.95 77.35 0 11 1 55.99 67.94 0 11 -1 0.01 36.95 0 11 -1 -20.27 77.66 0 -11 1 8.86 38.37 0 11 2 26.99 68.31 0 11 -2 -22.24 40.53 0 11 -2 -25.25 86.65 0 -11 2 -19.60 41.44 0 -11 4 11.17 45.99 0 11 -5 101.55 48.72 0 -11 5 202.96 56.21 0 -11 6 -44.30 47.11 0 11 -7 18.46 53.05 0 -11 7 71.07 44.76 0 12 -1 -63.22 37.30 0 -12 2 843.91 80.89 0 12 -3 20.51 44.58 0 -12 3 -52.86 45.10 0 12 -4 93.58 47.39 0 -12 4 68.76 53.09 0 12 -6 294.93 59.15 0 13 -1 0.00 35.94 0 -13 1 23.96 43.62 0 13 -2 -38.44 43.73 0 -13 2 0.00 43.23 0 13 -4 13.47 49.36 0 -13 4 14.01 52.65 0 13 -5 -64.55 52.05 0 -14 1 24.02 46.78 0 14 -2 167.24 48.30 0 -14 2 222.71 52.66 0 14 -3 154.36 55.86 1 0 -1 3605.65 396.17 1 0 -1 5478.45 495.16 1 0 -1 4713.44 537.78 1 0 -1 5272.12 412.29 -1 0 1 5552.52 362.41 -1 0 1 4970.65 367.79 -1 0 1 4789.56 371.95 -1 0 1 6169.35 1215.42 -1 0 1 4814.52 372.47 1 0 -2 -3.77 4.92 1 0 -2 2.31 8.92 -1 0 2 0.52 5.71 -1 0 2 -3.35 3.87 -1 0 2 0.38 9.90 1 0 -3 289.22 29.69 -1 0 3 380.65 69.63 1 -1 0 2.66 6.10 -1 1 0 1.68 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-53.43 47.32 -4 3 3 29.02 27.48 -4 -3 3 47.15 33.98 -4 3 4 325.23 37.51 -4 3 4 236.58 57.97 -4 -3 4 174.62 44.89 -4 -3 4 215.00 49.42 4 3 -4 221.75 54.05 -4 3 5 260.84 35.84 -4 -3 5 99.16 53.16 4 3 -5 214.76 32.82 4 -3 -6 71.94 28.90 4 3 -6 75.56 32.35 4 3 -6 23.10 58.28 4 -3 -7 24.26 30.73 4 -3 -8 239.83 44.97 4 -4 -1 146.35 46.24 -4 4 1 106.01 51.17 -4 4 3 50.24 29.64 -4 4 3 124.08 53.20 -4 -4 3 88.78 42.67 -4 -4 3 49.76 38.12 4 4 -3 92.79 52.61 -4 4 4 1948.09 151.02 -4 4 4 1892.95 156.79 -4 -4 4 1616.68 158.98 4 4 -4 1679.65 150.77 4 -4 -5 12.17 24.36 -4 4 5 12.92 29.69 -4 4 5 10.49 58.92 -4 -4 5 14.31 27.26 4 4 -5 10.69 25.78 4 4 -5 -76.65 58.57 -4 5 1 90.25 31.12 -4 5 1 57.89 55.62 -4 5 2 40.42 29.82 -4 5 2 1.49 56.40 -4 -5 2 74.54 29.92 4 5 -2 29.08 63.43 -4 5 3 10.99 29.08 -4 5 3 -4.96 56.29 -4 -5 3 -64.50 43.24 4 5 -3 -76.45 55.17 4 -5 -4 85.22 26.56 -4 5 4 93.45 33.07 -4 5 4 125.30 63.05 -4 -5 4 71.40 54.12 4 5 -4 124.78 63.65 4 -5 -5 25.28 27.64 4 5 -5 25.09 26.84 4 5 -5 10.13 63.83 4 -5 -6 12.36 31.36 -4 -5 6 36.43 34.14 4 5 -6 45.98 36.27 4 5 -6 60.78 67.82 4 -5 -8 0.02 37.52 -4 6 0 1108.86 141.00 -4 6 1 75.79 23.68 -4 6 1 76.25 33.97 -4 6 1 97.91 63.81 -4 6 2 202.42 39.10 -4 6 2 270.83 61.71 -4 -6 2 221.41 52.15 4 6 -2 268.15 75.06 -4 6 3 -59.99 33.22 -4 -6 3 1.78 50.51 4 -6 -4 338.05 38.26 4 6 -4 179.93 72.46 4 6 -5 4.94 29.82 -4 -6 6 431.51 53.04 4 6 -6 394.93 91.26 4 -6 -7 6.74 34.19 -4 -6 7 23.88 35.39 4 6 -7 24.38 40.70 4 -6 -8 743.38 80.16 -4 7 1 21.57 35.09 -4 7 2 25.51 35.21 -4 7 2 34.24 60.79 -4 -7 2 27.25 50.83 4 7 -2 51.11 64.70 4 7 -3 10.33 64.28 4 -7 -5 159.71 35.41 4 7 -5 142.93 34.70 4 7 -5 164.49 78.79 4 -7 -6 0.00 33.48 -4 -7 6 198.86 44.17 4 7 -6 61.79 41.49 4 -7 -7 0.00 39.30 -4 -7 7 1.73 36.52 4 7 -7 9.31 43.22 -4 8 0 2248.59 187.63 -4 8 -1 11.34 30.00 4 8 -2 734.37 107.03 4 -8 -3 25.23 28.62 4 8 -3 36.74 69.13 4 -8 -4 324.88 41.08 4 8 -4 224.13 88.64 4 8 -5 -59.83 33.90 4 -8 -6 443.49 54.29 4 -8 -7 -0.51 41.48 -4 -8 7 -54.24 46.42 4 -8 -8 158.45 45.71 4 8 -8 151.22 50.07 -4 9 -1 34.91 34.03 4 9 -2 19.77 70.78 4 -9 -3 108.37 32.88 4 9 -3 -33.35 74.67 4 -9 -5 15.03 35.54 4 -9 -6 66.57 39.77 -4 -9 6 51.54 45.25 4 9 -6 43.15 44.13 4 -9 -7 0.00 45.12 -4 -9 7 -44.95 50.37 4 9 -7 34.88 49.64 4 -9 -8 2.76 45.63 -4 10 -2 211.30 47.68 4 -10 -4 529.09 58.43 4 -10 -5 -25.21 38.18 -4 -10 5 -41.63 47.24 4 -10 -6 276.65 48.48 4 10 -6 187.01 51.24 4 -10 -7 25.35 46.79 -4 11 -2 90.94 44.53 4 -11 -3 5.83 34.32 4 -11 -4 78.34 40.39 4 -11 -5 21.94 39.41 -4 -11 5 0.00 49.91 4 -11 -6 29.96 50.22 4 11 -6 1020.09 102.32 4 -12 -4 178.35 45.65 4 -12 -5 -207.67 50.98 4 -13 -2 29.49 37.22 4 -13 -3 46.38 45.10 4 -13 -4 1.19 42.45 -5 0 3 229.49 59.17 -5 0 5 7.93 54.53 5 0 -6 -17.31 24.66 -5 1 3 236.04 36.80 -5 1 3 185.18 58.02 -5 -1 3 196.18 58.35 5 -1 -6 -51.08 26.91 -5 2 2 4.82 52.69 -5 2 3 459.63 50.96 -5 2 3 596.44 74.89 -5 -2 3 405.17 76.59 5 2 -3 279.43 78.37 5 -2 -6 -0.25 27.18 5 -2 -8 6.26 33.95 -5 3 2 545.73 61.43 -5 3 2 395.95 77.82 -5 3 3 157.77 37.24 -5 3 3 205.73 66.67 5 3 -3 103.98 66.65 -5 3 4 15.18 33.42 -5 3 4 24.12 62.55 5 3 -4 -95.80 55.16 5 -3 -6 15.26 28.23 5 -3 -7 21.46 33.49 5 -3 -9 -88.57 43.27 -5 4 2 1.91 33.20 -5 4 2 36.06 63.93 5 4 -4 14.82 54.68 5 -4 -6 14.76 28.14 5 -4 -8 17.93 37.86 5 -4 -9 84.95 43.30 -5 5 3 28.87 36.28 -5 5 3 45.52 63.06 5 5 -3 26.80 63.53 5 5 -4 -16.86 62.15 5 -5 -5 74.77 29.12 5 5 -5 73.80 62.02 5 -5 -7 20.52 36.22 5 -5 -9 33.48 42.35 -5 6 1 1061.44 117.48 -5 6 1 1208.95 133.91 5 6 -3 832.87 116.50 5 6 -4 16.19 67.87 5 6 -5 148.41 69.42 5 -6 -6 -19.25 31.20 -5 -6 6 15.09 38.28 5 -6 -7 205.14 43.76 5 -6 -8 12.94 41.43 5 -6 -9 185.17 46.80 5 7 -3 23.22 70.89 5 7 -4 24.27 73.15 5 -7 -5 98.02 34.03 5 -7 -6 0.00 35.53 -5 -7 6 37.89 42.28 5 -7 -8 56.80 43.71 5 8 -3 635.08 100.69 5 -8 -4 21.84 29.63 5 -8 -5 402.85 49.76 5 -8 -6 -11.69 38.13 5 -8 -7 44.56 39.47 -5 -8 7 -18.29 48.16 5 8 -7 24.15 37.57 5 -8 -8 20.95 47.68 5 -9 -4 25.53 32.39 5 -9 -5 123.74 38.92 5 -9 -6 0.00 39.17 5 -9 -7 32.04 41.97 5 -10 -3 483.22 54.46 5 -10 -4 3.42 34.07 5 -11 -5 202.50 52.46 5 -12 -2 2.26 35.71 5 -12 -3 71.04 40.48 5 -12 -4 28.83 41.18 5 -13 -2 44.88 41.18 -6 1 3 4.97 66.12 6 -1 -7 30.65 30.88 -6 2 3 7.88 66.98 6 -2 -7 10.54 30.73 6 -3 -6 74.24 31.07 6 -3 -9 -21.47 40.00 6 4 -4 425.73 81.00 6 -4 -7 0.00 32.65 6 -4 -8 44.98 39.94 6 -4 -9 9.72 40.11 6 5 -4 82.28 65.70 6 -5 -6 70.70 34.68 6 -5 -7 0.00 36.55 6 -5 -8 12.13 41.69 6 -6 -6 87.57 35.26 6 -6 -8 219.41 48.02 6 -7 -5 -18.87 33.01 6 -7 -7 49.97 40.94 6 -7 -8 27.27 43.29 6 -8 -5 -5.61 33.48 6 -8 -6 42.30 37.43 6 -8 -7 -112.76 44.77 6 -9 -5 0.00 35.78 6 -9 -6 167.35 49.35 6 -10 -4 435.77 53.52 6 -10 -5 972.83 90.67 6 -11 -4 25.61 39.51 6 -12 -3 19.95 37.37 7 -3 -8 43.65 40.75 7 -4 -7 16.41 33.99 7 -4 -8 3.64 41.55 7 -5 -7 0.12 35.82 7 -6 -6 2.74 35.28 7 -6 -7 66.48 37.48 7 -7 -6 0.00 36.45 7 -7 -7 0.01 35.91 7 -8 -6 0.01 36.80 7 -9 -5 14.21 38.03 8 -3 -7 5.05 36.10 8 -4 -7 -41.80 39.07 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1701 data_027_CoGF_1-75GPa _audit_creation_method ; XIA2 0.5.438-g5f426072-dials-1.7 SHELXL-2017/1 ; _audit_creation_date 2018-08-01 _publ_contact_author_address ; School of Physics and Astronomy Queen Mary University of London Mile End Rd, London E1 4NS U.K. ; _publ_contact_author_email a.e.phillips@qmul.ac.uk _publ_contact_author_name 'Anthony E. Phillips' _publ_contact_author_phone '+44 2078 823 429' _chemical_name_systematic 'guanidinium cobalt(II) formate' _chemical_name_common 'guanidinium cobalt(II) formate' _chemical_formula_moiety 'C3 H3 Co O6, C H6 N3' _chemical_formula_sum 'C4 H9 Co N3 O6' _chemical_formula_weight 254.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.2660 0.4750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0020 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 52 _space_group_name_H-M_alt 'P n n a' _space_group_name_Hall '-P 2a 2bc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 8.020(2) _cell_length_b 11.4685(15) _cell_length_c 8.908(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 819.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 498 _cell_measurement_theta_max 19.5719820457 _cell_measurement_theta_min 1.95231678705 _exptl_crystal_description block _exptl_crystal_colour 'intense pink' _exptl_crystal_density_diffrn 2.060 _exptl_crystal_F_000 516 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_T_min 0.999665587943 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CCP4 7.0.044: AIMLESS, version 0.5.32 : 29/03/17 Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.4859 _diffrn_ambient_pressure 1750000 _diffrn_radiation_type 'Synchrotron' _diffrn_radiation_source 'Diamond Light Source Beamline I19' _diffrn_radiation_monochromator 'double crystal Silicon 111' _diffrn_measurement_specimen_support 'diamond anvil cell' _diffrn_measurement_device 'Newport IS4CCD (4 circle)' _diffrn_measurement_device_type 'Pilatus 300K' _diffrn_measurement_method ; \w scans with 0.2 degree frames ; _diffrn_reflns_number 1533 _diffrn_reflns_av_unetI/netI 0.1546 _diffrn_reflns_av_R_equivalents 0.1158 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.428 _diffrn_reflns_theta_max 17.643 _diffrn_reflns_theta_full 16.950 _diffrn_measured_fraction_theta_max 0.459 _diffrn_measured_fraction_theta_full 0.476 _diffrn_reflns_Laue_measured_fraction_max 0.459 _diffrn_reflns_Laue_measured_fraction_full 0.476 _diffrn_reflns_point_group_measured_fraction_max 0.459 _diffrn_reflns_point_group_measured_fraction_full 0.476 _reflns_number_total 384 _reflns_number_gt 236 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_reduction ; aimless (Evans, P. R. and Murshudov, G. N., 2013) ccp4 (Winn, M. D. et al., 2011) DIALS 1.7.3-gc8f60bf0-release pointless (Evans, P., 2006) XIA2 0.5.438-g5f426072-dials-1.7 (Winter, G., 2010) ; _publ_section_references ; Evans, P. (2006) Acta Cryst. D62, 72-82. Evans, P. R. and Murshudov, G. N. (2013) Acta Cryst. D69, 1204-1214. Winn, M. D. et al. (2011) Acta Cryst. D67, 235-242. Winter, G. (2010) J. Appl. Cryst. 43, 186-190. ; _computing_cell_refinement 'DIALS 2theta refinement, DIALS 1.7.3-gc8f60bf0-release' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.3957P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 384 _refine_ls_number_parameters 66 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co01 Co 0.26617(18) 0.750000 0.250000 0.0212(8) Uani 1 2 d S T P . . O002 O 0.2668(6) 0.5954(4) 0.1289(9) 0.0273(19) Uani 1 1 d . . . . . O003 O 0.4226(8) 0.6760(5) 0.4066(9) 0.036(2) Uani 1 1 d . . . . . O004 O 0.5743(7) 0.6900(5) 0.6105(9) 0.035(2) Uani 1 1 d . . . . . N005 N 0.250000 0.500000 0.5939(16) 0.029(3) Uani 1 2 d S T P . . H00A H 0.186070 0.452894 0.545606 0.035 Uiso 0.5 1 calc R U P . . H00B H 0.313930 0.547106 0.545606 0.035 Uiso 0.5 1 calc R U P . . N006 N 0.3472(11) 0.5717(5) 0.8160(9) 0.043(3) Uani 1 1 d . . . . . H00C H 0.411832 0.619247 0.769212 0.051 Uiso 1 1 calc R U . . . H00D H 0.345915 0.570675 0.912489 0.051 Uiso 1 1 calc R U . . . C007 C 0.250000 0.500000 0.739(2) 0.023(3) Uani 1 2 d S T P . . C008 C 0.250000 0.500000 0.193(2) 0.033(4) Uani 1 2 d S T P . . H008 H 0.250000 0.500000 0.296908 0.040 Uiso 1 2 calc R U P . . C009 C 0.5369(13) 0.7208(8) 0.4817(11) 0.030(3) Uani 1 1 d . . . . . H009 H 0.597870 0.781000 0.438352 0.036 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co01 0.0160(17) 0.0178(11) 0.030(2) 0.0003(9) 0.000 0.000 O002 0.033(6) 0.018(3) 0.031(7) 0.001(3) 0.003(2) 0.000(2) O003 0.019(5) 0.033(3) 0.057(7) 0.004(4) -0.016(3) -0.001(3) O004 0.032(6) 0.031(3) 0.042(7) 0.002(4) -0.009(3) -0.007(3) N005 0.014(10) 0.036(6) 0.038(9) 0.000 0.000 -0.007(4) N006 0.047(9) 0.040(4) 0.041(9) -0.009(4) 0.006(4) -0.020(4) C007 0.010(11) 0.019(7) 0.040(10) 0.000 0.000 0.000(4) C008 0.045(14) 0.025(6) 0.029(14) 0.000 0.000 0.006(5) C009 0.032(7) 0.021(5) 0.038(9) 0.006(5) -0.006(4) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co01 O003 2.059(6) . ? Co01 O003 2.059(6) 4_565 ? Co01 O002 2.075(6) . ? Co01 O002 2.075(6) 4_565 ? Co01 O004 2.094(6) 7_575 ? Co01 O004 2.094(6) 6_556 ? O002 C008 1.240(10) . ? O003 C009 1.246(10) . ? O004 C009 1.237(10) . ? N005 C007 1.297(17) . ? N005 H00A 0.8600 . ? N005 H00B 0.8600 . ? N006 C007 1.322(12) . ? N006 H00C 0.8600 . ? N006 H00D 0.8600 . ? C008 H008 0.9300 . ? C009 H009 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O003 Co01 O003 104.9(4) . 4_565 ? O003 Co01 O002 89.9(3) . . ? O003 Co01 O002 89.9(2) 4_565 . ? O003 Co01 O002 89.9(2) . 4_565 ? O003 Co01 O002 89.9(3) 4_565 4_565 ? O002 Co01 O002 179.7(3) . 4_565 ? O003 Co01 O004 170.1(3) . 7_575 ? O003 Co01 O004 84.8(3) 4_565 7_575 ? O002 Co01 O004 88.5(2) . 7_575 ? O002 Co01 O004 91.7(2) 4_565 7_575 ? O003 Co01 O004 84.8(3) . 6_556 ? O003 Co01 O004 170.1(3) 4_565 6_556 ? O002 Co01 O004 91.7(2) . 6_556 ? O002 Co01 O004 88.5(2) 4_565 6_556 ? O004 Co01 O004 85.4(4) 7_575 6_556 ? C008 O002 Co01 121.1(9) . . ? C009 O003 Co01 129.9(6) . . ? C009 O004 Co01 129.4(5) . 6_656 ? C007 N005 H00A 120.0 . . ? C007 N005 H00B 120.0 . . ? H00A N005 H00B 120.0 . . ? C007 N006 H00C 120.0 . . ? C007 N006 H00D 120.0 . . ? H00C N006 H00D 120.0 . . ? N005 C007 N006 121.0(8) . 2_565 ? N005 C007 N006 121.0(8) . . ? N006 C007 N006 117.9(16) 2_565 . ? O002 C008 O002 125.6(17) . 2_565 ? O002 C008 H008 117.2 . . ? O002 C008 H008 117.2 2_565 . ? O004 C009 O003 123.9(9) . . ? O004 C009 H009 118.0 . . ? O003 C009 H009 118.0 . . ? _refine_diff_density_max 0.467 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.107 _shelx_res_file ; TITL CoGF 1.75 GPa in Pnna 027_CoGF_1-75GPa.res created by SHELXL-2017/1 at 17:33:58 on 01-Aug-2018 CELL 0.4859 8.0196 11.4685 8.9082 90 90 90 ZERR 4 0.0023 0.0015 0.0031 0 0 0 LATT 1 SYMM 0.5-X,-Y,+Z SYMM 0.5-X,0.5+Y,0.5-Z SYMM +X,0.5-Y,0.5-Z SFAC C H Co N O DISP C 0.001 0.001 6.068 DISP Co 0.266 0.475 1359.652 DISP H -0 0 0.607 DISP N 0.002 0.001 8.983 DISP O 0.004 0.003 13.336 UNIT 16 36 4 12 24 RIGU L.S. 10 PLAN 15 BOND $H LIST 4 FMAP 2 ACTA SHEL 999 0.8 OMIT 1 2 5 WGHT 0.023700 0.395700 FVAR 0.65147 CO01 3 0.266166 0.750000 0.250000 10.50000 0.01603 0.01780 = 0.02991 0.00025 0.00000 0.00000 O002 5 0.266772 0.595414 0.128866 11.00000 0.03254 0.01833 = 0.03112 0.00126 0.00345 -0.00020 O003 5 0.422583 0.675964 0.406559 11.00000 0.01924 0.03319 = 0.05678 0.00400 -0.01569 -0.00139 O004 5 0.574301 0.689965 0.610461 11.00000 0.03171 0.03072 = 0.04215 0.00189 -0.00857 -0.00680 N005 4 0.250000 0.500000 0.593876 10.50000 0.01438 0.03558 = 0.03843 0.00000 0.00000 -0.00705 AFIX 93 H00A 2 0.186070 0.452894 0.545606 10.50000 -1.20000 H00B 2 0.313930 0.547106 0.545606 10.50000 -1.20000 AFIX 0 N006 4 0.347248 0.571657 0.815965 11.00000 0.04696 0.04033 = 0.04109 -0.00922 0.00623 -0.01972 AFIX 93 H00C 2 0.411832 0.619247 0.769212 11.00000 -1.20000 H00D 2 0.345915 0.570675 0.912489 11.00000 -1.20000 AFIX 0 C007 1 0.250000 0.500000 0.739442 10.50000 0.00981 0.01910 = 0.04010 0.00000 0.00000 0.00021 C008 1 0.250000 0.500000 0.192509 10.50000 0.04495 0.02508 = 0.02876 0.00000 0.00000 0.00622 AFIX 43 H008 2 0.250000 0.500000 0.296908 10.50000 -1.20000 AFIX 0 C009 1 0.536945 0.720773 0.481697 11.00000 0.03174 0.02124 = 0.03781 0.00625 -0.00646 -0.00885 AFIX 43 H009 2 0.597870 0.781000 0.438352 11.00000 -1.20000 AFIX 0 HKLF 4 REM CoGF 1.75 GPa in Pnna REM R1 = 0.0705 for 236 Fo > 4sig(Fo) and 0.1142 for all 384 data REM 66 parameters refined using 36 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 0.467, deepest hole -0.409, 1-sigma level 0.107 Q1 1 0.5810 0.7500 0.7500 10.50000 0.05 0.47 Q2 1 0.6053 0.6221 0.7469 11.00000 0.05 0.40 Q3 1 0.5834 0.8167 0.6243 11.00000 0.05 0.39 Q4 1 0.3611 0.7268 0.3319 11.00000 0.05 0.36 Q5 1 0.6633 0.7449 0.6625 11.00000 0.05 0.35 Q6 1 0.2410 0.6697 0.3465 11.00000 0.05 0.35 Q7 1 0.4895 0.6951 0.7454 11.00000 0.05 0.35 Q8 1 0.5004 0.7500 0.2500 10.50000 0.05 0.34 Q9 1 0.4981 0.6776 0.5648 11.00000 0.05 0.31 Q10 1 0.3387 0.6061 0.0305 11.00000 0.05 0.30 Q11 1 0.4001 0.6279 0.2568 11.00000 0.05 0.30 Q12 1 0.0443 0.6018 0.7710 11.00000 0.05 0.29 Q13 1 0.6573 0.6778 0.5589 11.00000 0.05 0.29 Q14 1 0.3592 0.6886 0.1250 11.00000 0.05 0.28 Q15 1 0.0834 0.4846 0.6696 11.00000 0.05 0.27 ; _shelx_res_checksum 36116 _shelx_hkl_file ; 0 2 0 3277.88 771.39 0 2 0 3825.18 742.05 0 -2 0 3674.44 765.28 0 -2 0 4021.52 738.62 0 -2 0 3947.47 750.54 0 -2 0 3279.63 769.55 0 2 1 2.83 2.48 0 2 1 9.28 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-4 201.88 42.99 4 -1 -5 43.77 10.98 4 -1 -5 24.66 50.70 4 -1 -5 28.30 17.79 -4 1 5 57.11 11.96 -4 1 5 0.00 30.17 -4 1 5 48.88 21.05 -4 -1 5 58.65 12.54 -4 -1 5 49.77 23.01 4 1 -5 35.87 11.04 4 1 -5 0.00 20.88 -4 -1 6 7.04 10.18 -4 -1 6 -0.02 22.00 -4 -1 7 21.09 12.61 -4 -2 2 1029.90 209.80 -4 -2 2 955.13 208.62 4 2 -2 1045.33 198.84 4 -2 -4 1849.74 350.65 4 -2 -4 2018.31 349.94 4 -2 -4 1480.45 358.98 4 -2 -4 1564.60 344.59 -4 2 4 2005.07 345.14 -4 2 4 1714.26 346.87 -4 2 4 2355.86 412.08 -4 2 4 2016.46 447.93 -4 -2 4 1579.92 337.56 -4 -2 4 1702.55 346.12 4 2 -4 1720.66 343.79 4 2 -4 1833.12 348.06 4 -2 -6 0.41 65.87 -4 2 6 114.14 40.84 -4 2 6 222.81 83.69 -4 -2 6 132.61 28.56 -4 -2 7 0.00 11.53 -4 -3 1 236.56 54.86 -4 -3 1 364.81 86.81 4 3 -1 202.45 44.24 -4 -3 2 26.88 8.63 -4 -3 2 8.94 18.23 4 3 -2 24.16 8.40 4 -3 -3 49.11 27.16 4 -3 -3 -0.02 37.23 -4 3 3 55.14 12.90 -4 3 3 51.65 24.31 -4 -3 3 51.71 13.24 -4 -3 3 41.85 22.30 4 3 -3 54.39 12.57 4 -3 -4 590.02 96.50 4 -3 -4 337.51 97.51 -4 3 4 421.51 91.66 -4 3 4 498.25 128.89 -4 -3 4 373.76 83.44 -4 -3 4 519.25 91.82 4 3 -4 423.41 85.51 4 3 -4 499.44 90.13 4 -3 -5 137.48 51.68 4 -3 -5 0.00 72.91 -4 3 5 171.54 51.65 -4 3 5 164.55 78.65 -4 -3 5 196.36 38.19 -4 -3 5 208.54 46.38 4 3 -5 167.67 42.51 -4 3 6 129.37 44.04 -4 3 6 159.69 83.60 -4 -3 7 22.89 13.44 4 -4 -3 26.36 31.99 4 -4 -3 -0.09 46.71 -4 4 3 70.07 29.87 -4 -4 3 78.38 17.74 -4 -4 3 70.20 27.42 4 4 -3 86.40 17.54 4 4 -3 71.81 25.81 4 -4 -4 1730.18 344.88 4 -4 -4 1119.76 343.18 -4 4 4 2117.13 354.58 -4 4 4 1484.06 407.00 -4 -4 4 1841.40 338.25 -4 -4 4 2034.79 352.65 4 4 -4 1620.78 342.04 4 4 -4 1765.53 342.09 4 -4 -5 108.30 40.93 4 -4 -5 0.02 66.64 -4 4 5 43.26 35.06 -4 4 5 -0.02 72.61 -4 -4 5 19.87 11.28 -4 -4 5 37.03 27.39 4 4 -5 35.65 23.77 4 -4 -6 727.06 181.20 -4 4 6 631.69 160.43 -4 4 6 1715.72 252.43 -4 -4 6 746.59 152.19 -4 -5 0 1073.18 256.30 -4 -5 1 81.82 19.63 -4 -5 1 53.61 27.69 4 5 -1 99.52 19.58 4 -5 -2 47.47 35.18 -4 5 2 103.13 30.03 -4 -5 2 120.40 20.88 -4 -5 2 100.83 28.86 4 5 -2 69.65 19.96 4 -5 -3 36.48 32.59 4 -5 -3 13.23 49.37 -4 5 3 0.00 29.93 -4 -5 3 -0.06 10.15 -4 -5 3 -0.12 24.46 4 5 -3 12.86 9.40 4 5 -3 -0.06 23.21 4 -5 -4 -0.09 49.92 4 -5 -4 -0.08 63.13 -4 5 4 170.76 52.48 -4 5 4 143.12 80.51 -4 -5 4 205.48 34.60 -4 -5 4 122.42 41.67 4 5 -4 156.71 33.48 4 5 -4 157.43 40.87 4 -5 -5 2.46 43.61 4 -5 -5 1.75 69.84 -4 5 5 70.51 40.03 -4 5 5 53.33 83.09 -4 -5 5 42.66 14.70 4 -5 -6 37.05 49.48 -4 5 6 27.16 42.77 -4 -5 6 72.76 18.68 -4 5 7 -10.79 44.45 4 6 0 1015.74 188.38 -4 -6 0 832.09 190.83 -4 -6 1 121.82 24.65 -4 -6 1 79.33 31.69 4 6 -1 109.82 24.23 4 -6 -2 140.65 62.55 4 -6 -2 126.80 70.80 -4 6 2 225.30 60.93 -4 -6 2 306.61 54.83 4 6 -2 291.71 54.19 4 -6 -3 -1.93 36.51 4 -6 -3 0.00 57.76 -4 6 3 -17.34 40.31 -4 -6 3 -0.05 11.19 -4 -6 3 0.00 27.34 4 6 -3 -0.03 9.45 4 6 -3 -0.02 25.70 4 -6 -4 176.35 63.68 4 -6 -4 16.29 72.01 -4 6 4 251.57 61.26 -4 6 4 68.92 87.53 -4 -6 4 284.13 49.23 -4 -6 4 265.53 57.83 4 6 -4 217.34 47.82 4 -6 -5 -0.24 43.00 -4 6 5 -13.30 45.45 -4 6 5 -0.57 100.60 -4 -6 5 -0.55 12.77 -4 6 7 23.27 41.04 -4 -7 0 730.18 209.54 -4 -7 0 4203.06 737.28 -4 -7 1 -3.20 9.97 -4 -7 1 -0.84 26.50 4 7 -1 -1.27 10.38 4 -7 -2 80.70 40.03 4 -7 -2 101.20 53.73 -4 7 2 84.85 37.70 -4 -7 2 101.08 23.65 -4 -7 2 131.51 37.49 4 7 -2 119.20 23.42 4 7 -2 79.13 30.94 4 -7 -3 34.34 41.67 4 -7 -3 104.28 59.03 -4 7 3 -1.32 35.62 -4 -7 3 5.95 11.40 4 7 -3 -0.03 9.78 4 -7 -4 0.00 52.52 -4 7 4 47.61 51.70 -4 -7 4 185.56 34.08 4 -7 -5 148.06 59.84 -4 7 5 132.72 56.58 -4 -7 5 183.57 38.24 -4 7 6 73.91 52.22 4 8 0 2271.49 446.43 -4 -8 0 2277.54 446.97 -4 -8 -1 42.16 11.22 -4 -8 1 36.02 12.00 4 8 -1 0.00 11.71 4 -8 -3 -1.90 51.99 -4 8 3 30.86 38.73 -4 -8 3 32.28 14.40 4 8 -3 35.61 12.77 4 -8 -4 276.04 82.94 -4 8 4 258.84 78.29 -4 -8 4 331.21 66.16 4 8 -4 336.82 67.06 -4 8 6 380.82 94.73 -4 8 7 -4.35 51.22 4 9 0 0.00 12.20 -4 -9 0 0.66 10.46 -4 -9 -1 7.70 11.94 -4 -9 1 0.92 10.61 4 9 -1 21.09 12.74 4 -9 -2 35.97 46.92 -4 9 2 -0.08 39.46 -4 -9 2 51.07 16.67 4 9 -2 71.38 16.56 4 9 -4 224.03 47.62 -4 9 5 -0.08 50.70 -4 9 6 36.98 56.55 -4 10 2 212.49 59.87 -4 10 3 -0.05 45.48 4 10 -3 -0.11 12.86 -4 10 4 414.56 106.39 4 10 -4 469.18 93.39 -4 10 5 1.07 52.66 -4 11 2 212.97 57.36 4 11 -2 162.68 36.54 -4 11 3 0.00 43.69 4 11 -3 11.71 14.62 4 11 -5 13.13 14.28 4 12 0 556.40 110.62 4 12 -3 0.00 14.86 4 12 -4 163.52 35.99 4 12 -5 12.35 14.05 4 13 0 32.84 16.70 4 13 -1 -0.02 15.40 4 13 -3 -40.00 19.87 4 13 -4 -0.21 14.74 4 13 -5 8.92 14.63 4 14 -1 0.00 16.44 4 14 -3 14.79 15.69 4 14 -4 65.79 20.42 -5 0 3 182.63 38.90 5 0 -5 20.04 8.43 5 0 -5 -0.02 20.86 -5 0 5 13.81 9.81 -5 0 5 2.82 20.13 -5 0 6 -13.07 11.14 -5 -1 2 366.75 92.74 -5 1 3 230.91 54.11 -5 -1 3 257.67 53.13 -5 -1 3 264.54 66.68 5 1 -3 282.82 52.87 -5 1 5 70.03 16.92 -5 1 5 56.99 25.79 -5 -1 5 67.19 17.25 -5 -1 5 67.65 27.23 5 1 -5 83.37 17.57 -5 -1 6 -0.11 10.21 5 1 -6 -4.58 9.74 -5 -2 2 68.15 17.47 5 -2 -3 529.11 128.28 -5 -2 3 384.68 80.58 -5 -2 3 488.83 92.26 5 2 -3 397.00 79.79 5 -2 -4 0.00 34.55 5 -2 -5 769.32 160.90 5 -2 -5 639.79 172.26 -5 -2 5 839.16 153.75 5 2 -5 764.38 152.36 -5 -2 6 11.73 10.67 5 2 -6 15.08 9.45 5 2 -7 1162.97 233.69 -5 -3 2 486.63 109.59 -5 -3 2 700.74 151.75 5 3 -2 554.86 107.40 5 -3 -3 298.86 82.57 -5 -3 3 334.16 65.73 -5 -3 3 323.14 71.29 5 3 -3 330.17 65.32 5 -3 -4 0.02 36.40 5 -3 -4 27.52 38.13 -5 3 4 2.50 26.71 -5 -3 4 1.32 10.16 -5 -3 4 34.95 22.21 5 3 -4 3.29 9.92 5 3 -4 10.59 23.30 -5 3 5 259.53 63.53 -5 3 5 179.93 94.56 -5 -3 5 271.87 55.16 5 3 -5 281.21 55.14 -5 -3 6 36.77 12.06 5 3 -6 12.86 10.13 -5 -4 1 290.03 67.36 -5 -4 2 15.20 10.46 -5 -4 2 0.00 26.84 5 4 -2 23.31 10.16 5 -4 -3 1134.85 277.47 -5 -4 3 1316.68 246.19 -5 -4 3 1205.30 251.39 5 4 -3 1252.23 244.96 5 -4 -4 51.85 38.70 5 -4 -4 3.32 48.14 -5 4 4 -0.02 31.49 -5 -4 4 9.49 10.39 -5 -4 4 0.05 26.13 5 4 -4 10.06 10.04 5 -4 -5 223.22 105.32 -5 4 5 408.91 106.27 -5 4 5 458.95 145.84 -5 -4 5 550.34 101.63 5 4 -5 599.42 102.12 5 -4 -6 -2.88 48.73 -5 4 6 17.71 42.83 5 4 -6 23.57 11.21 -5 -5 2 299.58 50.64 -5 -5 2 -35.91 55.08 5 5 -2 261.63 48.88 5 -5 -3 131.59 47.73 -5 -5 3 170.93 32.39 -5 -5 3 124.52 41.78 5 5 -3 136.15 31.70 5 -5 -5 144.06 59.46 -5 5 5 98.51 52.81 -5 -5 5 180.48 39.48 5 5 -5 223.79 40.55 -5 5 6 300.77 78.18 -5 -6 1 1087.03 224.22 -5 -6 1 1686.92 349.07 5 6 -1 1078.14 219.18 -5 -6 2 11.47 10.29 -5 -6 2 -4.33 30.75 5 6 -2 10.96 10.59 -5 -6 3 679.11 133.70 5 -6 -4 0.00 50.03 -5 6 4 23.56 37.99 -5 -6 4 8.79 12.57 5 6 -4 7.98 10.23 -5 6 6 -0.21 47.93 -5 -7 1 208.71 46.40 5 7 -1 248.16 47.82 5 -7 -3 86.60 43.57 -5 7 3 15.63 36.13 -5 -7 3 62.73 19.92 5 7 -3 101.91 19.82 5 -7 -4 44.26 49.14 -5 7 4 -0.12 39.76 -5 7 5 253.43 61.05 5 7 -5 186.21 40.43 5 7 -6 0.00 12.05 -5 -8 0 10.50 11.91 -5 -8 1 81.13 20.65 5 8 -1 90.44 21.29 -5 -8 2 -0.03 11.66 5 8 -2 -3.61 12.75 5 8 -4 16.17 13.62 -5 8 5 221.37 70.20 5 8 -5 274.17 55.31 -5 8 6 0.00 48.56 5 8 -6 29.44 13.85 -5 9 3 96.07 50.12 5 9 -3 171.27 35.04 -5 9 4 84.59 46.49 5 9 -4 2.23 15.29 -5 9 5 85.94 60.74 5 9 -5 199.46 40.23 5 9 -6 -0.06 13.30 5 9 -7 57.30 19.21 5 10 -1 237.03 49.78 5 10 -2 5.33 15.02 -5 10 3 440.09 97.76 5 10 -3 407.44 83.08 -5 10 4 51.96 45.45 5 10 -4 -0.09 14.40 5 10 -5 513.89 102.56 5 10 -6 43.86 19.09 5 11 0 13.09 14.40 5 11 -1 47.38 17.33 5 11 -4 1.93 13.79 5 11 -5 1599.93 313.14 5 11 -6 0.00 14.85 5 11 -7 0.00 15.11 5 12 0 -6.60 16.99 5 12 -1 387.19 78.88 5 12 -2 0.00 15.09 5 12 -3 102.90 27.28 5 12 -4 -0.11 16.39 5 12 -6 0.00 15.54 5 13 0 14.68 16.61 5 13 -1 54.33 19.67 5 13 -2 54.07 20.33 5 13 -4 -0.93 17.05 5 14 0 0.00 16.32 5 14 -1 191.44 41.87 5 14 -2 29.84 19.52 -6 0 3 0.00 9.32 -6 0 4 -0.11 9.51 6 0 -5 7.58 10.49 -6 0 5 0.00 10.27 -6 -1 3 0.00 9.77 -6 1 4 79.60 19.95 -6 -1 4 96.49 20.27 6 1 -4 80.12 20.25 -6 -1 5 22.10 11.79 6 1 -5 1.07 10.61 -6 -2 3 0.02 10.24 -6 -2 5 -0.09 10.84 6 2 -5 -0.02 10.18 6 2 -6 363.51 72.87 -6 -3 3 12.26 11.16 6 3 -3 11.53 12.77 6 -3 -4 208.11 59.59 -6 -3 4 196.69 44.61 6 3 -4 236.65 44.88 -6 -3 5 63.99 18.19 6 3 -5 72.07 17.67 6 3 -6 170.56 36.48 -6 -4 2 860.10 177.36 6 -4 -4 777.65 141.42 -6 -4 4 619.04 119.66 6 4 -4 562.40 118.26 6 4 -7 33.62 14.37 6 4 -8 22.32 13.96 -6 -5 3 44.33 12.92 6 5 -3 0.00 12.52 6 -5 -4 158.58 52.52 -6 -5 4 120.14 31.31 6 5 -4 172.48 32.56 -6 5 5 315.33 75.64 6 5 -6 241.24 50.04 6 5 -8 24.74 13.64 -6 -6 2 329.54 68.46 6 6 -2 348.93 69.68 -6 -6 3 34.93 14.13 6 6 -3 28.86 13.65 -6 6 5 17.51 37.41 6 6 -5 -0.05 12.75 -6 6 6 82.16 53.84 6 6 -6 142.47 31.24 6 6 -7 0.00 13.16 6 6 -8 87.13 22.41 6 6 -9 -1.87 15.14 -6 -7 1 3.66 12.58 6 7 -4 46.64 16.49 6 7 -5 17.85 13.73 6 7 -7 1.42 13.82 6 7 -8 26.77 15.08 6 7 -9 0.00 14.16 6 8 -2 735.91 145.55 6 8 -3 0.00 13.59 6 8 -4 529.29 105.70 6 8 -6 118.56 28.27 6 8 -7 -0.05 14.07 6 8 -8 18.49 14.94 6 9 -1 45.79 16.85 6 9 -2 108.41 26.35 6 9 -3 15.32 15.77 6 9 -5 -0.03 14.39 6 9 -6 428.73 86.40 6 10 -1 35.13 17.79 6 10 -3 28.79 18.48 6 10 -4 357.54 73.57 6 10 -5 314.00 67.11 6 10 -7 -1.87 18.14 6 11 -1 48.30 19.18 6 11 -2 32.18 17.36 6 11 -3 -0.05 17.10 6 11 -4 102.35 26.91 6 11 -6 115.04 29.56 6 12 -1 0.21 16.58 6 12 -2 138.06 33.34 6 12 -4 44.72 19.67 6 13 -1 -4.35 18.94 6 13 -2 16.32 17.45 6 13 -3 17.74 18.71 7 1 -5 257.82 53.72 7 2 -5 562.47 112.45 7 2 -6 0.00 12.83 -7 -3 3 340.45 70.48 7 3 -5 420.21 84.09 7 4 -6 25.84 14.27 7 4 -7 13.90 14.27 7 5 -4 22.09 14.85 7 5 -5 80.60 21.28 7 5 -7 28.44 16.00 7 6 -3 256.50 54.13 7 6 -4 0.00 14.56 7 6 -5 170.35 37.47 7 6 -6 -2.13 14.30 7 6 -7 243.35 51.44 7 6 -8 4.41 15.80 7 7 -3 192.01 41.32 7 7 -4 12.98 15.43 7 7 -5 -4.33 16.56 7 7 -6 -0.02 15.78 7 7 -7 109.51 27.13 7 7 -8 0.00 15.71 7 8 -5 53.07 19.89 7 8 -6 0.00 15.22 7 8 -7 37.81 18.54 7 9 -2 140.31 34.57 7 9 -3 79.43 23.54 7 9 -4 -0.02 16.06 7 9 -5 84.75 24.23 7 10 -2 -0.05 16.56 7 10 -3 122.56 30.48 7 10 -4 3.34 16.90 7 11 -2 23.90 16.73 7 11 -4 1.39 17.39 7 12 -2 0.00 18.75 7 12 -3 93.69 26.30 8 3 -6 48.21 18.11 8 4 -5 844.59 170.29 8 4 -6 217.07 46.54 8 4 -7 20.68 15.35 8 5 -5 0.02 16.04 8 5 -6 60.70 19.24 8 6 -4 1.87 15.20 8 6 -5 14.65 16.13 8 6 -6 105.47 26.62 8 6 -7 -1.32 16.23 8 7 -4 94.57 25.29 8 7 -5 11.37 17.10 8 8 -4 30.10 18.55 8 8 -6 185.00 40.96 8 9 -5 24.83 19.12 8 10 -3 30.25 18.16 8 10 -4 57.37 21.09 9 5 -6 20.05 16.87 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 2252 # start Validation Reply Form _vrf_PLAT029_020_CoGF_0GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.466 Why? RESPONSE: A substantial portion of the reflections were blocked by the diamond anvil cell in which measurements were made. ; _vrf_PLAT214_020_CoGF_0GPa ; PROBLEM: Atom N41 (Anion/Solvent) ADP max/min Ratio 8.7 oblate RESPONSE: This atom was especially badly affected by the missing data and needed spherical restraints (ISOR) to maintain a positive definite displacement ellipsoid. This restraint was kept to a maximum possible sigma, leaving the shape significantly anisotropic. ; _vrf_PLAT029_022_CoGF_0-88GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.709 Why? RESPONSE: A substantial portion of the reflections were blocked by the diamond anvil cell in which measurements were made. ; _vrf_PLAT029_023_CoGF_1-21GPa ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.457 Why? RESPONSE: A substantial portion of the reflections were blocked by the diamond anvil cell in which measurements were made. ; # end Validation Reply Form