 
data_004_MnGF_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 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

_shelx_SHELXL_version_number      '2017/1'

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'
 'Mn'  'Mn'   0.2320   0.3560
 '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                    8.5145(11)
_cell_length_b                    11.9867(11)
_cell_length_c                    9.0577(9)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      924.44(17)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     825
_cell_measurement_theta_max       19.8944993222
_cell_measurement_theta_min       1.91139800718
 
_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     1.797          
_exptl_crystal_F_000              508
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     0.498
_exptl_absorpt_correction_T_min   0.999425942533
_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	
;
ω scans with 0.2 degree frames
;
_diffrn_reflns_number             3081
_diffrn_reflns_av_unetI/netI      0.1043
_diffrn_reflns_av_R_equivalents   0.0748
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          2.244
_diffrn_reflns_theta_max          20.009
_diffrn_reflns_theta_full         16.950
_diffrn_measured_fraction_theta_max   0.606
_diffrn_measured_fraction_theta_full  0.681
_diffrn_reflns_Laue_measured_fraction_max    0.606
_diffrn_reflns_Laue_measured_fraction_full   0.681
_diffrn_reflns_point_group_measured_fraction_max   0.606
_diffrn_reflns_point_group_measured_fraction_full  0.681
_reflns_number_total              821
_reflns_number_gt                 470
_reflns_threshold_expression      'I > 2σ(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/[σ²(Fo²)+(0.0775P)²+0.6293P] where P=(Fo²+2Fc²)/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          821
_refine_ls_number_parameters      66
_refine_ls_number_restraints      36
_refine_ls_R_factor_all           0.0664
_refine_ls_R_factor_gt            0.0322
_refine_ls_wR_factor_ref          0.1002
_refine_ls_wR_factor_gt           0.0812
_refine_ls_goodness_of_fit_ref    0.609
_refine_ls_restrained_S_all       0.595
_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 0.25173(8) 0.250000 0.250000 0.0150(2) Uani 1 2 d S T P . .
O21 O 0.4041(3) 0.17936(18) 0.4164(2) 0.0307(6) Uani 1 1 d . . . . .
C21 C 0.5198(4) 0.2169(3) 0.4845(3) 0.0258(7) Uani 1 1 d . . . . .
H21 H 0.582942 0.268408 0.435715 0.031 Uiso 1 1 calc R U . . .
O22 O 0.5573(3) 0.19079(18) 0.6123(2) 0.0275(5) Uani 1 1 d . . . . .
O31 O 0.2566(3) 0.40771(18) 0.3711(2) 0.0266(5) Uani 1 1 d . . . . .
C31 C 0.250000 0.500000 0.3098(5) 0.0279(10) Uani 1 2 d S T P . .
H31 H 0.249999 0.500000 0.207168 0.033 Uiso 1 2 calc R U P . .
N41 N 0.250000 0.500000 0.9056(4) 0.0327(10) Uani 1 2 d S T P . .
H41A H 0.306476 0.452552 0.953041 0.039 Uiso 0.5 1 calc R U P . .
H41B H 0.193524 0.547448 0.953041 0.039 Uiso 0.5 1 calc R U P . .
C41 C 0.250000 0.500000 0.7605(5) 0.0258(10) Uani 1 2 d S T P . .
N42 N 0.3364(4) 0.4274(2) 0.6869(3) 0.0374(8) Uani 1 1 d . . . . .
H42A H 0.393044 0.379822 0.733933 0.045 Uiso 1 1 calc R U . . .
H42B H 0.336004 0.427744 0.591990 0.045 Uiso 1 1 calc R U . . .
 
 
_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 O21 2.161(2) . ?
Mn1 O21 2.161(2) 4 ?
Mn1 O31 2.186(2) . ?
Mn1 O31 2.186(2) 4 ?
Mn1 O22 2.191(2) 7_565 ?
Mn1 O22 2.191(2) 6_556 ?
O21 C21 1.246(3) . ?
C21 O22 1.241(3) . ?
C21 H21 0.9300 . ?
O31 C31 1.239(3) . ?
C31 H31 0.9300 . ?
N41 C41 1.314(6) . ?
N41 H41A 0.8600 . ?
N41 H41B 0.8600 . ?
C41 N42 1.320(3) . ?
C41 N42 1.320(3) 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 Mn1 O21 106.25(13) . 4 ?
O21 Mn1 O31 88.71(8) . . ?
O21 Mn1 O31 90.00(9) 4 . ?
O21 Mn1 O31 89.99(8) . 4 ?
O21 Mn1 O31 88.71(8) 4 4 ?
O31 Mn1 O31 177.84(12) . 4 ?
O21 Mn1 O22 167.80(8) . 7_565 ?
O21 Mn1 O22 85.95(9) 4 7_565 ?
O31 Mn1 O22 91.14(8) . 7_565 ?
O31 Mn1 O22 90.49(8) 4 7_565 ?
O21 Mn1 O22 85.95(9) . 6_556 ?
O21 Mn1 O22 167.80(8) 4 6_556 ?
O31 Mn1 O22 90.49(8) . 6_556 ?
O31 Mn1 O22 91.14(8) 4 6_556 ?
O22 Mn1 O22 81.85(12) 7_565 6_556 ?
C21 O21 Mn1 132.7(2) . . ?
O22 C21 O21 125.0(3) . . ?
O22 C21 H21 117.5 . . ?
O21 C21 H21 117.5 . . ?
C21 O22 Mn1 130.1(2) . 6_656 ?
C31 O31 Mn1 123.1(2) . . ?
O31 C31 O31 126.8(4) 2_565 . ?
O31 C31 H31 116.6 2_565 . ?
O31 C31 H31 116.6 . . ?
C41 N41 H41A 120.0 . . ?
C41 N41 H41B 120.0 . . ?
H41A N41 H41B 120.0 . . ?
N41 C41 N42 120.3(2) . . ?
N41 C41 N42 120.3(2) . 2_565 ?
N42 C41 N42 119.3(4) . 2_565 ?
C41 N42 H42A 120.0 . . ?
C41 N42 H42B 120.0 . . ?
H42A N42 H42B 120.0 . . ?
 
_refine_diff_density_max    0.254
_refine_diff_density_min   -0.272
_refine_diff_density_rms    0.063



 
data_006_MnGF_0-63GPa
 
_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 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

_shelx_SHELXL_version_number      '2017/1'

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'
 'Mn'  'Mn'   0.2320   0.3560
 '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                    8.3814(13)
_cell_length_b                    11.8640(13)
_cell_length_c                    9.0589(11)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      900.8(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     763
_cell_measurement_theta_max       19.8218229235
_cell_measurement_theta_min       1.9214755534
 
_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     1.844          
_exptl_crystal_F_000              508
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     0.511
_exptl_absorpt_correction_T_min   0.999451088108
_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          630000
_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        		
;
ω scans with 0.2 degree frames
;
_diffrn_reflns_number             3257
_diffrn_reflns_av_unetI/netI      0.1020
_diffrn_reflns_av_R_equivalents   0.0867
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          1.934
_diffrn_reflns_theta_max          19.969
_diffrn_reflns_theta_full         16.950
_diffrn_measured_fraction_theta_max   0.616
_diffrn_measured_fraction_theta_full  0.689
_diffrn_reflns_Laue_measured_fraction_max    0.616
_diffrn_reflns_Laue_measured_fraction_full   0.689
_diffrn_reflns_point_group_measured_fraction_max   0.616
_diffrn_reflns_point_group_measured_fraction_full  0.689
_reflns_number_total              809
_reflns_number_gt                 507
_reflns_threshold_expression      'I > 2σ(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/[σ²(Fo²)] where P=(Fo²+2Fc²)/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          809
_refine_ls_number_parameters      66
_refine_ls_number_restraints      36
_refine_ls_R_factor_all           0.0761
_refine_ls_R_factor_gt            0.0388
_refine_ls_wR_factor_ref          0.1033
_refine_ls_wR_factor_gt           0.0851
_refine_ls_goodness_of_fit_ref    0.875
_refine_ls_restrained_S_all       0.856
_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 0.25804(6) 0.250000 0.250000 0.0162(2) Uani 1 2 d S T P . .
O21 O 0.4125(3) 0.17609(19) 0.4133(2) 0.0311(6) Uani 1 1 d . . . . .
C21 C 0.5265(4) 0.2153(3) 0.4843(3) 0.0269(8) Uani 1 1 d . . . . .
H21 H 0.591256 0.267687 0.436899 0.032 Uiso 1 1 calc R U . . .
O22 O 0.5606(3) 0.19037(18) 0.6129(2) 0.0288(6) Uani 1 1 d . . . . .
O31 O 0.2609(2) 0.4070(2) 0.3743(2) 0.0278(6) Uani 1 1 d . . . . .
C31 C 0.250000 0.500000 0.3133(5) 0.0277(12) Uani 1 2 d S T P . .
H31 H 0.250000 0.500000 0.210659 0.033 Uiso 1 2 calc R U P . .
N41 N 0.250000 0.500000 0.9067(4) 0.0324(11) Uani 1 2 d S T P . .
H41A H 0.191541 0.547279 0.954119 0.039 Uiso 0.5 1 calc R U P . .
H41B H 0.308459 0.452721 0.954119 0.039 Uiso 0.5 1 calc R U P . .
C41 C 0.250000 0.500000 0.7607(5) 0.0241(10) Uani 1 2 d S T P . .
N42 N 0.3397(3) 0.4275(2) 0.6885(3) 0.0383(8) Uani 1 1 d . . . . .
H42A H 0.339934 0.427266 0.593605 0.046 Uiso 1 1 calc R U . . .
H42B H 0.397980 0.380321 0.736340 0.046 Uiso 1 1 calc R U . . .
 
 
_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 O21 2.152(2) 4 ?
Mn1 O21 2.152(2) . ?
Mn1 O31 2.177(2) 4 ?
Mn1 O31 2.177(2) . ?
Mn1 O22 2.186(2) 7_565 ?
Mn1 O22 2.186(2) 6_556 ?
O21 C21 1.243(3) . ?
C21 O22 1.236(3) . ?
C21 H21 0.9300 . ?
O31 C31 1.237(3) . ?
C31 H31 0.9300 . ?
N41 C41 1.323(6) . ?
N41 H41A 0.8600 . ?
N41 H41B 0.8600 . ?
C41 N42 1.316(3) 2_565 ?
C41 N42 1.316(3) . ?
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 Mn1 O21 106.06(13) 4 . ?
O21 Mn1 O31 89.23(8) 4 4 ?
O21 Mn1 O31 90.02(9) . 4 ?
O21 Mn1 O31 90.02(9) 4 . ?
O21 Mn1 O31 89.23(8) . . ?
O31 Mn1 O31 178.74(12) 4 . ?
O21 Mn1 O22 86.15(10) 4 7_565 ?
O21 Mn1 O22 167.77(8) . 7_565 ?
O31 Mn1 O22 89.50(8) 4 7_565 ?
O31 Mn1 O22 91.45(8) . 7_565 ?
O21 Mn1 O22 167.77(8) 4 6_556 ?
O21 Mn1 O22 86.15(10) . 6_556 ?
O31 Mn1 O22 91.45(8) 4 6_556 ?
O31 Mn1 O22 89.50(8) . 6_556 ?
O22 Mn1 O22 81.65(12) 7_565 6_556 ?
C21 O21 Mn1 131.7(2) . . ?
O22 C21 O21 125.2(3) . . ?
O22 C21 H21 117.4 . . ?
O21 C21 H21 117.4 . . ?
C21 O22 Mn1 129.3(2) . 6_656 ?
C31 O31 Mn1 122.1(2) . . ?
O31 C31 O31 127.0(4) . 2_565 ?
O31 C31 H31 116.5 . . ?
O31 C31 H31 116.5 2_565 . ?
C41 N41 H41A 120.0 . . ?
C41 N41 H41B 120.0 . . ?
H41A N41 H41B 120.0 . . ?
N42 C41 N42 120.5(4) 2_565 . ?
N42 C41 N41 119.8(2) 2_565 . ?
N42 C41 N41 119.8(2) . . ?
C41 N42 H42A 120.0 . . ?
C41 N42 H42B 120.0 . . ?
H42A N42 H42B 120.0 . . ?
 
_refine_diff_density_max    0.315
_refine_diff_density_min   -0.338
_refine_diff_density_rms    0.082



 
data_008_MnGF_0-96GPa
 
_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 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

_shelx_SHELXL_version_number      '2017/1'

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'
 'Mn'  'Mn'   0.2320   0.3560
 '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                    8.2781(9)
_cell_length_b                    11.7712(8)
_cell_length_c                    9.0479(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      881.66(13)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     814
_cell_measurement_theta_max       19.9038316369
_cell_measurement_theta_min       1.92349310062
 
_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     1.884          
_exptl_crystal_F_000              508
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     0.522
_exptl_absorpt_correction_T_min   0.883168971791
_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          960000
_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        		
;
ω scans with 0.2 degree frames
;
_diffrn_reflns_number             1805
_diffrn_reflns_av_unetI/netI      5.4780
_diffrn_reflns_av_R_equivalents   0.0981
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          1.941
_diffrn_reflns_theta_max          19.967
_diffrn_reflns_theta_full         16.950
_diffrn_measured_fraction_theta_max   0.529
_diffrn_measured_fraction_theta_full  0.619
_diffrn_reflns_Laue_measured_fraction_max    0.529
_diffrn_reflns_Laue_measured_fraction_full   0.619
_diffrn_reflns_point_group_measured_fraction_max   0.529
_diffrn_reflns_point_group_measured_fraction_full  0.619
_reflns_number_total              684
_reflns_number_gt                 391
_reflns_threshold_expression      'I > 2σ(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/[σ²(Fo²)+(0.0775P)²+0.6293P] where P=(Fo²+2Fc²)/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          684
_refine_ls_number_parameters      66
_refine_ls_number_restraints      36
_refine_ls_R_factor_all           0.2001
_refine_ls_R_factor_gt            0.0612
_refine_ls_wR_factor_ref          0.1760
_refine_ls_wR_factor_gt           0.1508
_refine_ls_goodness_of_fit_ref    1.017
_refine_ls_restrained_S_all       0.999
_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 0.26230(13) 0.250000 0.250000 0.0203(5) Uani 1 2 d S T P . .
O21 O 0.4181(5) 0.1735(3) 0.4104(4) 0.0345(12) Uani 1 1 d . . . . .
C21 C 0.5311(8) 0.2139(5) 0.4839(6) 0.0333(15) Uani 1 1 d . . . . .
H21 H 0.596591 0.267282 0.437488 0.040 Uiso 1 1 calc R U . . .
O22 O 0.5643(5) 0.1893(3) 0.6134(4) 0.0311(11) Uani 1 1 d . . . . .
O31 O 0.2649(5) 0.4070(4) 0.3764(4) 0.0320(11) Uani 1 1 d . . . . .
C31 C 0.250000 0.500000 0.3162(10) 0.033(2) Uani 1 2 d S T P . .
H31 H 0.250003 0.500001 0.213370 0.040 Uiso 1 2 calc R U P . .
N41 N 0.250000 0.500000 0.9076(8) 0.036(2) Uani 1 2 d S T P . .
H41A H 0.309196 0.452353 0.955169 0.043 Uiso 0.5 1 calc R U P . .
H41B H 0.190804 0.547647 0.955169 0.043 Uiso 0.5 1 calc R U P . .
C41 C 0.250000 0.500000 0.7613(9) 0.029(2) Uani 1 2 d S T P . .
N42 N 0.3406(6) 0.4271(4) 0.6899(4) 0.0383(15) Uani 1 1 d . . . . .
H42A H 0.341089 0.426682 0.594804 0.046 Uiso 1 1 calc R U . . .
H42B H 0.399508 0.379659 0.737996 0.046 Uiso 1 1 calc R U . . .
 
 
_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 O21 2.140(4) . ?
Mn1 O21 2.140(4) 4 ?
Mn1 O22 2.174(4) 7_565 ?
Mn1 O22 2.174(4) 6_556 ?
Mn1 O31 2.174(4) . ?
Mn1 O31 2.174(4) 4 ?
O21 C21 1.243(6) . ?
C21 O22 1.238(6) . ?
C21 H21 0.9300 . ?
O31 C31 1.229(6) . ?
C31 H31 0.9300 . ?
N41 C41 1.324(11) . ?
N41 H41A 0.8600 . ?
N41 H41B 0.8600 . ?
C41 N42 1.310(6) . ?
C41 N42 1.310(6) 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 Mn1 O21 105.9(2) . 4 ?
O21 Mn1 O22 168.03(14) . 7_565 ?
O21 Mn1 O22 86.02(16) 4 7_565 ?
O21 Mn1 O22 86.02(16) . 6_556 ?
O21 Mn1 O22 168.03(14) 4 6_556 ?
O22 Mn1 O22 82.1(2) 7_565 6_556 ?
O21 Mn1 O31 89.72(15) . . ?
O21 Mn1 O31 89.59(16) 4 . ?
O22 Mn1 O31 91.56(14) 7_565 . ?
O22 Mn1 O31 89.30(14) 6_556 . ?
O21 Mn1 O31 89.59(16) . 4 ?
O21 Mn1 O31 89.72(15) 4 4 ?
O22 Mn1 O31 89.30(14) 7_565 4 ?
O22 Mn1 O31 91.56(14) 6_556 4 ?
O31 Mn1 O31 178.9(2) . 4 ?
C21 O21 Mn1 130.9(4) . . ?
O22 C21 O21 125.7(6) . . ?
O22 C21 H21 117.1 . . ?
O21 C21 H21 117.1 . . ?
C21 O22 Mn1 128.9(4) . 6_656 ?
C31 O31 Mn1 121.5(4) . . ?
O31 C31 O31 127.3(8) 2_565 . ?
O31 C31 H31 116.4 2_565 . ?
O31 C31 H31 116.4 . . ?
C41 N41 H41A 120.0 . . ?
C41 N41 H41B 120.0 . . ?
H41A N41 H41B 120.0 . . ?
N42 C41 N42 120.9(8) . 2_565 ?
N42 C41 N41 119.6(4) . . ?
N42 C41 N41 119.6(4) 2_565 . ?
C41 N42 H42A 120.0 . . ?
C41 N42 H42B 120.0 . . ?
H42A N42 H42B 120.0 . . ?
 
_refine_diff_density_max    0.636
_refine_diff_density_min   -1.009
_refine_diff_density_rms    0.124



 
data_010_MnGF_1-70GPa
 
_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 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

_shelx_SHELXL_version_number      '2017/1'

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0007   0.0007
 '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'   0.0018   0.0014
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0040   0.0026
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mn'  'Mn'   0.2318   0.3560
 '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                    9.041(2)
_cell_length_b                    9.041(2)
_cell_length_c                    18.091(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1280.5(7)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used   309
_cell_measurement_theta_min     2.3470
_cell_measurement_theta_max     20.2900
 
_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     1.946          
_exptl_crystal_F_000              762
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     0.539
_exptl_absorpt_correction_T_min                   0.55086
_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_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        		
;
ω scans with 0.2 degree frames
;
_diffrn_reflns_number             4342
_diffrn_reflns_av_unetI/netI      0.0655
_diffrn_reflns_av_R_equivalents   0.2312
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.352
_diffrn_reflns_theta_max          16.394
_diffrn_reflns_theta_full         16.394
_diffrn_measured_fraction_theta_max   0.979
_diffrn_measured_fraction_theta_full  0.979
_diffrn_reflns_Laue_measured_fraction_max    0.979
_diffrn_reflns_Laue_measured_fraction_full   0.979
_diffrn_reflns_point_group_measured_fraction_max   0.979
_diffrn_reflns_point_group_measured_fraction_full  0.979
_reflns_number_total              452
_reflns_number_gt                 305
_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 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_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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          452
_refine_ls_number_parameters      25
_refine_ls_number_restraints      12
_refine_ls_R_factor_all           0.1370
_refine_ls_R_factor_gt            0.1041
_refine_ls_wR_factor_ref          0.2951
_refine_ls_wR_factor_gt           0.2585
_refine_ls_goodness_of_fit_ref    1.127
_refine_ls_restrained_S_all       1.115
_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 0.666667 0.333333 0.333333 0.0261(16) Uani 1 6 d S T P . .
O21 O 0.4666(9) 0.3436(9) 0.3960(6) 0.043(2) Uani 1 1 d . . . . .
C22 C 0.333333 0.2150(18) 0.416667 0.035(4) Uani 1 2 d S T P . .
H22 H 0.333330 0.112106 0.416664 0.042 Uiso 1 2 calc R U P . .
C31 C 0.333333 0.666667 0.416667 0.026(5) Uani 1 6 d S T P . .
N32 N 0.4798(15) 0.666667 0.416667 0.046(4) Uani 1 2 d S T P . .
H32A H 0.574894 0.761794 0.416665 0.055 Uiso 0.5 1 calc R U P . .
H32B H 0.479767 0.571539 0.416669 0.055 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 O21 2.175(8) 32 ?
Mn1 O21 2.175(8) 2_655 ?
Mn1 O21 2.175(8) 3_665 ?
Mn1 O21 2.175(8) 33_545 ?
Mn1 O21 2.175(8) . ?
Mn1 O21 2.175(8) 31_655 ?
O21 C22 1.242(11) . ?
C22 H22 0.9300 . ?
C31 N32 1.324(13) . ?
C31 N32 1.324(13) 2_665 ?
C31 N32 1.324(13) 3_565 ?
N32 H32A 0.8600 . ?
N32 H32B 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 Mn1 O21 180.0 32 2_655 ?
O21 Mn1 O21 84.7(4) 32 3_665 ?
O21 Mn1 O21 95.3(4) 2_655 3_665 ?
O21 Mn1 O21 95.3(4) 32 33_545 ?
O21 Mn1 O21 84.7(4) 2_655 33_545 ?
O21 Mn1 O21 180.0 3_665 33_545 ?
O21 Mn1 O21 84.7(4) 32 . ?
O21 Mn1 O21 95.3(4) 2_655 . ?
O21 Mn1 O21 95.3(4) 3_665 . ?
O21 Mn1 O21 84.7(4) 33_545 . ?
O21 Mn1 O21 95.3(4) 32 31_655 ?
O21 Mn1 O21 84.7(4) 2_655 31_655 ?
O21 Mn1 O21 84.7(4) 3_665 31_655 ?
O21 Mn1 O21 95.3(4) 33_545 31_655 ?
O21 Mn1 O21 180.0 . 31_655 ?
C22 O21 Mn1 123.7(9) . . ?
O21 C22 O21 126.4(16) . 12 ?
O21 C22 H22 116.8 . . ?
O21 C22 H22 116.8 12 . ?
N32 C31 N32 119.999(5) . 2_665 ?
N32 C31 N32 120.001(3) . 3_565 ?
N32 C31 N32 120.000(4) 2_665 3_565 ?
C31 N32 H32A 120.0 . . ?
C31 N32 H32B 120.0 . . ?
H32A N32 H32B 120.0 . . ?
 
_refine_diff_density_max    1.189
_refine_diff_density_min   -1.198
_refine_diff_density_rms    0.239



 
data_012_MnGF_2-14GPa_CrysAlisPro
 
_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 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

_shelx_SHELXL_version_number      '2017/1'

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0007   0.0007
 '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'   0.0018   0.0014
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0040   0.0026
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mn'  'Mn'   0.2318   0.3560
 '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                    9.030(3)
_cell_length_b                    9.030(3)
_cell_length_c                    17.969(7)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1268.9(10)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used   320
_cell_measurement_theta_min     2.3640
_cell_measurement_theta_max     19.9550
 
_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     1.964          
_exptl_crystal_F_000              762
_exptl_absorpt_coefficient_mu     0.544
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.05
_exptl_absorpt_correction_T_min                   0.52228
_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          2140000
_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        		
;
ω scans with 0.2 degree frames
;
_diffrn_reflns_number             4276
_diffrn_reflns_av_unetI/netI      0.0684
_diffrn_reflns_av_R_equivalents   0.2143
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          2.360
_diffrn_reflns_theta_max          16.376
_diffrn_reflns_theta_full         16.376
_diffrn_measured_fraction_theta_max   0.962
_diffrn_measured_fraction_theta_full  0.962
_diffrn_reflns_Laue_measured_fraction_max    0.962
_diffrn_reflns_Laue_measured_fraction_full   0.962
_diffrn_reflns_point_group_measured_fraction_max   0.962
_diffrn_reflns_point_group_measured_fraction_full  0.962
_reflns_number_total              432
_reflns_number_gt                 283
_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 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)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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          432
_refine_ls_number_parameters      25
_refine_ls_number_restraints      12
_refine_ls_R_factor_all           0.1343
_refine_ls_R_factor_gt            0.1063
_refine_ls_wR_factor_ref          0.2762
_refine_ls_wR_factor_gt           0.2544
_refine_ls_goodness_of_fit_ref    1.041
_refine_ls_restrained_S_all       1.029
_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 0.666667 0.333333 0.333333 0.0296(16) Uani 1 6 d S T P . .
O21 O 0.4670(9) 0.3440(8) 0.3961(5) 0.044(2) Uani 1 1 d . . . . .
C22 C 0.333333 0.2144(18) 0.416667 0.041(4) Uani 1 2 d S T P . .
H22 H 0.333331 0.111439 0.416664 0.050 Uiso 1 2 calc R U P . .
C31 C 0.333333 0.666667 0.416667 0.028(5) Uani 1 6 d S T P . .
N32 N 0.4801(13) 0.666667 0.416667 0.047(4) Uani 1 2 d S T P . .
H32A H 0.575337 0.761905 0.416665 0.056 Uiso 0.5 1 calc R U P . .
H32B H 0.480099 0.571429 0.416669 0.056 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 O21 2.170(7) 32 ?
Mn1 O21 2.170(7) 2_655 ?
Mn1 O21 2.170(7) 3_665 ?
Mn1 O21 2.170(7) 33_545 ?
Mn1 O21 2.170(7) . ?
Mn1 O21 2.170(7) 31_655 ?
O21 C22 1.245(11) . ?
C22 H22 0.9300 . ?
C31 N32 1.325(12) 2_665 ?
C31 N32 1.325(12) 3_565 ?
C31 N32 1.325(12) . ?
N32 H32A 0.8600 . ?
N32 H32B 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 Mn1 O21 180.0 32 2_655 ?
O21 Mn1 O21 84.6(3) 32 3_665 ?
O21 Mn1 O21 95.4(3) 2_655 3_665 ?
O21 Mn1 O21 95.4(3) 32 33_545 ?
O21 Mn1 O21 84.6(3) 2_655 33_545 ?
O21 Mn1 O21 180.0 3_665 33_545 ?
O21 Mn1 O21 84.6(3) 32 . ?
O21 Mn1 O21 95.4(3) 2_655 . ?
O21 Mn1 O21 95.4(3) 3_665 . ?
O21 Mn1 O21 84.6(3) 33_545 . ?
O21 Mn1 O21 95.4(3) 32 31_655 ?
O21 Mn1 O21 84.6(3) 2_655 31_655 ?
O21 Mn1 O21 84.6(3) 3_665 31_655 ?
O21 Mn1 O21 95.4(3) 33_545 31_655 ?
O21 Mn1 O21 180.0 . 31_655 ?
C22 O21 Mn1 123.3(8) . . ?
O21 C22 O21 125.9(15) . 12 ?
O21 C22 H22 117.1 . . ?
O21 C22 H22 117.1 12 . ?
N32 C31 N32 120.000(3) 2_665 3_565 ?
N32 C31 N32 119.999(11) 2_665 . ?
N32 C31 N32 120.001(3) 3_565 . ?
C31 N32 H32A 120.0 . . ?
C31 N32 H32B 120.0 . . ?
H32A N32 H32B 120.0 . . ?
 
_refine_diff_density_max    1.086
_refine_diff_density_min   -1.278
_refine_diff_density_rms    0.225



 
data_012_MnGF_2-14GPa_xia2
 
_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 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

_shelx_SHELXL_version_number      '2017/1'

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0007   0.0007
 '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'   0.0018   0.0014
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0040   0.0026
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mn'  'Mn'   0.2318   0.3560
 '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                    8.938(10)
_cell_length_b                    8.938(10)
_cell_length_c                    17.63(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      1220(4)
_cell_formula_units_Z             6
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     111
_cell_measurement_theta_max       13.6662285838
_cell_measurement_theta_min       3.10694509279
 
_exptl_crystal_description       block
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn     2.043          
_exptl_crystal_F_000              762
_exptl_crystal_size_max           0.1
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.05
_exptl_absorpt_coefficient_mu     0.566
_exptl_absorpt_correction_T_min   0.999587717149
_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          2140000
_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        		
;
ω scans with 0.2 degree frames
;
_diffrn_reflns_number             449
_diffrn_reflns_av_unetI/netI      0.1375
_diffrn_reflns_av_R_equivalents   0.0978
_diffrn_reflns_limit_h_min        -4
_diffrn_reflns_limit_h_max        5
_diffrn_reflns_limit_k_min        -3
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -16
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.394
_diffrn_reflns_theta_max          16.551
_diffrn_reflns_theta_full         16.551
_diffrn_measured_fraction_theta_max   0.631
_diffrn_measured_fraction_theta_full  0.631
_diffrn_reflns_Laue_measured_fraction_max    0.631
_diffrn_reflns_Laue_measured_fraction_full   0.631
_diffrn_reflns_point_group_measured_fraction_max   0.631
_diffrn_reflns_point_group_measured_fraction_full  0.631
_reflns_number_total              147
_reflns_number_gt                 88
_reflns_threshold_expression      'I > 2σ(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_special_details           
;
These data represent only one component of a two-component non-merohedral twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/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          147
_refine_ls_number_parameters      24
_refine_ls_number_restraints      12
_refine_ls_R_factor_all           0.1071
_refine_ls_R_factor_gt            0.0766
_refine_ls_wR_factor_ref          0.2236
_refine_ls_wR_factor_gt           0.2023
_refine_ls_goodness_of_fit_ref    0.779
_refine_ls_restrained_S_all       0.744
_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 0.666667 0.333333 0.333333 0.0277(18) Uani 1 6 d S T P . .
O21 O 0.4672(11) 0.3438(10) 0.3963(6) 0.044(3) Uani 1 1 d . . . . .
C22 C 0.333333 0.211(2) 0.416667 0.040(5) Uani 1 2 d S T P . .
H22 H 0.333333 0.106742 0.416665 0.048 Uiso 1 2 calc R U P . .
C31 C 0.333333 0.666667 0.416667 0.036(7) Uani 1 6 d S T P . .
N32 N 0.4785(16) 0.666667 0.416667 0.045(5) Uani 1 2 d S T P . .
H32A H 0.574704 0.762881 0.416665 0.054 Uiso 0.5 1 calc R U P . .
H32B H 0.478490 0.570453 0.416669 0.054 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 O21 2.141(9) 32 ?
Mn1 O21 2.141(9) 2_655 ?
Mn1 O21 2.141(9) 3_665 ?
Mn1 O21 2.141(9) 33_545 ?
Mn1 O21 2.141(9) . ?
Mn1 O21 2.141(9) 31_655 ?
O21 C22 1.246(12) . ?
C22 H22 0.9300 . ?
C31 N32 1.297(14) 2_665 ?
C31 N32 1.297(14) . ?
C31 N32 1.297(15) 3_565 ?
N32 H32A 0.8600 . ?
N32 H32B 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 Mn1 O21 180.0 32 2_655 ?
O21 Mn1 O21 84.4(4) 32 3_665 ?
O21 Mn1 O21 95.6(4) 2_655 3_665 ?
O21 Mn1 O21 95.6(4) 32 33_545 ?
O21 Mn1 O21 84.4(4) 2_655 33_545 ?
O21 Mn1 O21 180.0 3_665 33_545 ?
O21 Mn1 O21 84.4(4) 32 . ?
O21 Mn1 O21 95.6(4) 2_655 . ?
O21 Mn1 O21 95.6(4) 3_665 . ?
O21 Mn1 O21 84.4(4) 33_545 . ?
O21 Mn1 O21 95.6(4) 32 31_655 ?
O21 Mn1 O21 84.4(4) 2_655 31_655 ?
O21 Mn1 O21 84.4(4) 3_665 31_655 ?
O21 Mn1 O21 95.6(4) 33_545 31_655 ?
O21 Mn1 O21 180.0 . 31_655 ?
C22 O21 Mn1 122.1(10) . . ?
O21 C22 O21 123.4(19) . 12 ?
O21 C22 H22 118.3 . . ?
O21 C22 H22 118.3 12 . ?
N32 C31 N32 119.999(14) 2_665 . ?
N32 C31 N32 120.003(4) 2_665 3_565 ?
N32 C31 N32 119.998(3) . 3_565 ?
C31 N32 H32A 120.0 . . ?
C31 N32 H32B 120.0 . . ?
H32A N32 H32B 120.0 . . ?
 
_refine_diff_density_max    0.726
_refine_diff_density_min   -0.681
_refine_diff_density_rms    0.178



# start Validation Reply Form
_vrf_PLAT029_004_MnGF_0GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.681 Why?  
RESPONSE: A substantial portion of the reflections were blocked by the diamond 
anvil cell in which measurements were made.
;
_vrf_PLAT029_006_MnGF_0-63GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.689 Why?  
RESPONSE: A substantial portion of the reflections were blocked by the diamond 
anvil cell in which measurements were made.
;
_vrf_PLAT029_008_MnGF_0-96GPa
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.619 Why?  
RESPONSE: A substantial portion of the reflections were blocked by the diamond 
anvil cell in which measurements were made.
;
_vrf_PLAT029_012_MnGF_2-14GPa_xia2
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.631 Why?  
RESPONSE: A substantial portion of the reflections were blocked by the diamond 
anvil cell in which measurements were made.
;
# end Validation Reply Form

