 
data_MnGF_1p70GPa_twin
 
_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'


_audit_creation_date              2018-07-12 
  
 
_audit_creation_method            
;
'SHELXL-2018/3'
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic        'guanidinium manganese(II) formate'
_chemical_name_common            'guanidinium manganese(II) formate'
_chemical_formula_moiety         'C3 H3 Mn O6, C H6 N3'
_chemical_formula_sum            'C4 H9 Mn N3 O6'
_chemical_formula_weight          250.08


loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 '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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mn'  'Mn'   0.3368   0.7283
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            167
_space_group_name_H-M_alt         'R -3 c :H'
_space_group_name_Hall            '-R 3 2"c'
 
_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'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z+1/2'
 'x-y, -y, -z+1/2'
 '-x, -x+y, -z+1/2'
 'x+2/3, y+1/3, z+1/3'
 '-y+2/3, x-y+1/3, z+1/3'
 '-x+y+2/3, -x+1/3, z+1/3'
 'y+2/3, x+1/3, -z+5/6'
 'x-y+2/3, -y+1/3, -z+5/6'
 '-x+2/3, -x+y+1/3, -z+5/6'
 'x+1/3, y+2/3, z+2/3'
 '-y+1/3, x-y+2/3, z+2/3'
 '-x+y+1/3, -x+2/3, z+2/3'
 'y+1/3, x+2/3, -z+7/6'
 'x-y+1/3, -y+2/3, -z+7/6'
 '-x+1/3, -x+y+2/3, -z+7/6'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z-1/2'
 '-x+y, y, z-1/2'
 'x, x-y, z-1/2'
 '-x+2/3, -y+1/3, -z+1/3'
 'y+2/3, -x+y+1/3, -z+1/3'
 'x-y+2/3, x+1/3, -z+1/3'
 '-y+2/3, -x+1/3, z-1/6'
 '-x+y+2/3, y+1/3, z-1/6'
 'x+2/3, x-y+1/3, z-1/6'
 '-x+1/3, -y+2/3, -z+2/3'
 'y+1/3, -x+y+2/3, -z+2/3'
 'x-y+1/3, x+2/3, -z+2/3'
 '-y+1/3, -x+2/3, z+1/6'
 '-x+y+1/3, y+2/3, z+1/6'
 'x+1/3, x-y+2/3, z+1/6'
 
_cell_length_a                    8.9825(5)
_cell_length_b                    8.9825(5)
_cell_length_c                    18.175(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1270.0(3)
_cell_formula_units_Z             6
_cell_measurement_temperature     298(2)
_cell_measurement_reflns_used   2144
_cell_measurement_theta_min     4.5130
_cell_measurement_theta_max     26.6240
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1  1.0000  0.0000  0.0000  0.0000  1.0000  0.0000  0.0000  0.0000  1.0000
2 -0.1467  0.4250  0.4258 -0.0008 -1.0001 -0.0001  2.2961  1.1515  0.1485 

_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     1.962          
_exptl_crystal_F_000              762
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.25
_exptl_crystal_size_mid           0.15
_exptl_crystal_size_min           0.06
_exptl_absorpt_coefficient_mu     1.571
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_T_min                   0.78948
_exptl_absorpt_correction_T_max                   1.00000
_exptl_absorpt_correction_type            'multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       298(2)
_diffrn_ambient_pressure         1700000
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe 'x-ray'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Xcalibur, Sapphire3'
_diffrn_detector 'CCD plate'
_diffrn_detector_type 'Sapphire3'
_diffrn_detector_area_resol_mean 15.9682
_diffrn_measurement_method 'ω scans'
_diffrn_oxdiff_twin_integration_method 'simultaneous'
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.5996 3697 1068
2 0.4004 3635 1068
_diffrn_reflns_number             8400
_diffrn_reflns_av_unetI/netI      0.0185
_diffrn_reflns_av_R_equivalents   0.0960
_diffrn_reflns_av_sigmaI/netI 0.0362
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          4.538
_diffrn_reflns_theta_max          27.761
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.962
_diffrn_measured_fraction_theta_full  0.992
_diffrn_reflns_Laue_measured_fraction_max    0.962
_diffrn_reflns_Laue_measured_fraction_full   0.992
_diffrn_reflns_point_group_measured_fraction_max   0.962
_diffrn_reflns_point_group_measured_fraction_full  0.992
_reflns_number_total              619
_reflns_number_gt                 505
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 _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, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     'ShelXLe (Huebschle et al, 2011)'
_computing_publication_material   'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details
;
 Refined as a 2-component twin. The twin component was refined to
37°.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1667P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      iterative
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          619
_refine_ls_number_parameters      25
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0811
_refine_ls_R_factor_gt            0.0685
_refine_ls_wR_factor_ref          0.2166
_refine_ls_wR_factor_gt           0.2068
_refine_ls_goodness_of_fit_ref    1.111
_refine_ls_restrained_S_all       1.111
_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
Mn1 Mn 0.0000 0.0000 0.0000 0.0221(8) Uani 1 6 d S T P . .
O1 O 0.2091(4) 0.2001(4) 0.0623(2) 0.0345(11) Uani 1 1 d . . . . .
C1 C 0.2143(9) 0.3333 0.0833 0.0342(19) Uani 1 2 d S T P . .
H1 H 0.1107 0.3333 0.0833 0.041 Uiso 1 2 calc R U P . .
C2 C 0.0000 0.0000 0.2500 0.027(3) Uani 1 6 d S T P . .
N1 N 0.1464(6) 0.1464(6) 0.2500 0.0396(18) Uani 1 2 d S T P . .
H1A H 0.2422 0.1464 0.2500 0.047 Uiso 0.5 1 calc R U P . .
H1B H 0.1464 0.2422 0.2500 0.047 Uiso 0.5 1 calc R U P . .
 
 
_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
Mn1 O1 2.160(3) 21 ?
Mn1 O1 2.160(3) 3 ?
Mn1 O1 2.160(3) 19 ?
Mn1 O1 2.160(3) . ?
Mn1 O1 2.160(3) 20 ?
Mn1 O1 2.160(3) 2 ?
O1 C1 1.235(5) . ?
C1 O1 1.235(5) 17_554 ?
C1 H1 0.9300 . ?
C2 N1 1.315(6) 3 ?
C2 N1 1.315(6) 2 ?
C2 N1 1.315(6) . ?
N1 H1A 0.8600 . ?
N1 H1B 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
O1 Mn1 O1 180.0(2) 21 3 ?
O1 Mn1 O1 95.01(16) 21 19 ?
O1 Mn1 O1 84.99(16) 3 19 ?
O1 Mn1 O1 84.99(16) 21 . ?
O1 Mn1 O1 95.01(16) 3 . ?
O1 Mn1 O1 180.0(2) 19 . ?
O1 Mn1 O1 95.01(16) 21 20 ?
O1 Mn1 O1 84.99(16) 3 20 ?
O1 Mn1 O1 95.01(16) 19 20 ?
O1 Mn1 O1 84.99(16) . 20 ?
O1 Mn1 O1 84.99(16) 21 2 ?
O1 Mn1 O1 95.01(16) 3 2 ?
O1 Mn1 O1 84.99(16) 19 2 ?
O1 Mn1 O1 95.01(16) . 2 ?
O1 Mn1 O1 180.0(2) 20 2 ?
C1 O1 Mn1 124.3(4) . . ?
O1 C1 O1 126.9(8) . 17_554 ?
O1 C1 H1 116.6 . . ?
O1 C1 H1 116.6 17_554 . ?
N1 C2 N1 120.000(2) 3 2 ?
N1 C2 N1 120.000(1) 3 . ?
N1 C2 N1 120.000(1) 2 . ?
C2 N1 H1A 120.0 . . ?
C2 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
Mn1 O1 C1 O1 -162.8(4) . . . 17_554 ?
 
_refine_diff_density_max    0.719
_refine_diff_density_min   -0.506
_refine_diff_density_rms    0.137



