# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p0
_database_code_depnum_ccdc_archive 'CCDC 1861329'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_sum            'C3 H7 Mn N O6'
_chemical_formula_weight         208.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1789 0.2612 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'

_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'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.3678(7)
_cell_length_b                   7.3678(7)
_cell_length_c                   8.4912(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     399.19(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    137
_cell_measurement_theta_min      2.3050
_cell_measurement_theta_max      17.4670

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_F_000             210
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.362
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_pressure         '0 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            779
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.308
_diffrn_reflns_theta_max         19.892
_diffrn_reflns_theta_full        14.273
_diffrn_measured_fraction_theta_max 0.493
_diffrn_measured_fraction_theta_full 0.756
_diffrn_reflns_Laue_measured_fraction_max 0.493
_diffrn_reflns_Laue_measured_fraction_full 0.756
_diffrn_reflns_point_group_measured_fraction_max 0.469
_diffrn_reflns_point_group_measured_fraction_full 0.768
_reflns_number_total             304
_reflns_number_gt                262
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.434
_reflns_Friedel_fraction_max     0.422
_reflns_Friedel_fraction_full    0.800

_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       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0391P)²+0.2577P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 73 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         304
_refine_ls_number_parameters     22
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1120
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.187
_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 0.333333 0.666667 0.250000 0.0203(4) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.076(5) Uani 1 6 d DS T P . .
H2 H 1.07(3) 1.110(16) 0.175(9) 0.091 Uiso 0.6667 1 d D U P . .
O1 O 0.5912(5) 0.8947(6) 0.1032(4) 0.0344(9) Uani 1 1 d . . . . .
C1 C 0.5710(11) 1.000000 0.000000 0.046(2) Uani 1 2 d S T P . .
H1 H 0.444770 0.999996 0.000000 0.055 Uiso 1 2 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 2.189(3) 11 ?
Mn1 O1 2.189(3) 2_665 ?
Mn1 O1 2.189(3) 10_665 ?
Mn1 O1 2.189(3) . ?
Mn1 O1 2.189(3) 3_565 ?
Mn1 O1 2.189(3) 12_565 ?
O1 C1 1.228(5) . ?

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 82.55(16) 11 2_665 ?
O1 Mn1 O1 90.80(12) 11 10_665 ?
O1 Mn1 O1 96.7(2) 2_665 10_665 ?
O1 Mn1 O1 96.7(2) 11 . ?
O1 Mn1 O1 90.80(12) 2_665 . ?
O1 Mn1 O1 170.00(18) 10_665 . ?
O1 Mn1 O1 170.01(19) 11 3_565 ?
O1 Mn1 O1 90.80(12) 2_665 3_565 ?
O1 Mn1 O1 82.55(16) 10_665 3_565 ?
O1 Mn1 O1 90.80(12) . 3_565 ?
O1 Mn1 O1 90.80(12) 11 12_565 ?
O1 Mn1 O1 170.01(18) 2_665 12_565 ?
O1 Mn1 O1 90.80(12) 10_665 12_565 ?
O1 Mn1 O1 82.55(16) . 12_565 ?
O1 Mn1 O1 96.7(2) 3_565 12_565 ?
C1 O1 Mn1 123.9(4) . . ?
O1 C1 O1 128.1(8) 8_675 . ?

_refine_diff_density_max         0.261
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.085


# start Validation Reply Form
_vrf_PLAT029_AMnF_c1_p0          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.756 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT911_AMnF_c1_p0          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         41 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT915_AMnF_c1_p0          
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         43 %     
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p01
_database_code_depnum_ccdc_archive 'CCDC 1861330'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_sum            'C3 H7 Mn N O6'
_chemical_formula_weight         208.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1789 0.2612 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'

_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'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.33778(19)
_cell_length_b                   7.33778(19)
_cell_length_c                   8.4822(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     395.52(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    204
_cell_measurement_theta_min      1.8490
_cell_measurement_theta_max      17.5430

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             210
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.366
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_pressure         '0.10 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            797
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.854
_diffrn_reflns_theta_max         19.928
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.610
_diffrn_measured_fraction_theta_full 0.861
_diffrn_reflns_Laue_measured_fraction_max 0.610
_diffrn_reflns_Laue_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.585
_diffrn_reflns_point_group_measured_fraction_full 0.892
_reflns_number_total             374
_reflns_number_gt                332
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.438
_reflns_Friedel_fraction_max     0.535
_reflns_Friedel_fraction_full    0.971

_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       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0238P)²+0.0023P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 101 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.19(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         374
_refine_ls_number_parameters     22
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0680
_refine_ls_wR_factor_gt          0.0600
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.147
_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 0.333333 0.666667 0.250000 0.0216(2) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.083(3) Uani 1 6 d DS T P . .
H2 H 1.083(11) 1.113(7) 0.175(5) 0.100 Uiso 0.6667 1 d D U P . .
O1 O 0.5919(2) 0.8944(3) 0.1035(2) 0.0360(4) Uani 1 1 d . . . . .
C1 C 0.5705(5) 1.000000 0.000000 0.0455(11) Uani 1 2 d S T P . .
H1 H 0.443740 1.000000 0.000000 0.055 Uiso 1 2 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 2.1832(16) 11 ?
Mn1 O1 2.1832(16) 2_665 ?
Mn1 O1 2.1832(16) 10_665 ?
Mn1 O1 2.1832(16) 12_565 ?
Mn1 O1 2.1832(16) 3_565 ?
Mn1 O1 2.1832(16) . ?
O1 C1 1.232(2) . ?

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 82.35(9) 11 2_665 ?
O1 Mn1 O1 90.80(7) 11 10_665 ?
O1 Mn1 O1 96.96(10) 2_665 10_665 ?
O1 Mn1 O1 90.80(7) 11 12_565 ?
O1 Mn1 O1 169.70(8) 2_665 12_565 ?
O1 Mn1 O1 90.80(7) 10_665 12_565 ?
O1 Mn1 O1 169.70(8) 11 3_565 ?
O1 Mn1 O1 90.80(7) 2_665 3_565 ?
O1 Mn1 O1 82.35(9) 10_665 3_565 ?
O1 Mn1 O1 96.96(10) 12_565 3_565 ?
O1 Mn1 O1 96.96(10) 11 . ?
O1 Mn1 O1 90.80(7) 2_665 . ?
O1 Mn1 O1 169.70(8) 10_665 . ?
O1 Mn1 O1 82.35(9) 12_565 . ?
O1 Mn1 O1 90.80(7) 3_565 . ?
C1 O1 Mn1 123.48(18) . . ?
O1 C1 O1 127.5(3) . 8_675 ?

_refine_diff_density_max         0.259
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.066


# start Validation Reply Form
_vrf_PLAT029_AMnF_c1_p01         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.861 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT911_AMnF_c1_p01         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         25 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT915_AMnF_c1_p01         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         54 %     
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p02
_database_code_depnum_ccdc_archive 'CCDC 1861331'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_sum            'C3 H7 Mn N O6'
_chemical_formula_weight         208.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1789 0.2612 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'

_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'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.32804(14)
_cell_length_b                   7.32804(14)
_cell_length_c                   8.49640(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     395.131(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    220
_cell_measurement_theta_min      1.8550
_cell_measurement_theta_max      17.1390

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_F_000             210
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.366
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_pressure         '0.25 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            804
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.856
_diffrn_reflns_theta_max         19.337
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.657
_diffrn_measured_fraction_theta_full 0.850
_diffrn_reflns_Laue_measured_fraction_max 0.657
_diffrn_reflns_Laue_measured_fraction_full 0.850
_diffrn_reflns_point_group_measured_fraction_max 0.633
_diffrn_reflns_point_group_measured_fraction_full 0.884
_reflns_number_total             371
_reflns_number_gt                333
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.444
_reflns_Friedel_fraction_max     0.585
_reflns_Friedel_fraction_full    0.971

_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       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)²+0.0626P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 98 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         371
_refine_ls_number_parameters     22
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_restrained_S_all      1.246
_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 0.333333 0.666667 0.250000 0.0233(3) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.083(3) Uani 1 6 d DS T P . .
H2 H 1.085(13) 1.111(8) 0.175(6) 0.100 Uiso 0.6667 1 d D U P . .
O1 O 0.5922(3) 0.8945(3) 0.1039(3) 0.0385(6) Uani 1 1 d . . . . .
C1 C 0.5703(6) 1.000000 0.000000 0.0489(13) Uani 1 2 d S T P . .
H1 H 0.443435 0.999999 0.000001 0.059 Uiso 1 2 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 2.182(2) 11 ?
Mn1 O1 2.182(2) 2_665 ?
Mn1 O1 2.182(2) 10_665 ?
Mn1 O1 2.182(2) . ?
Mn1 O1 2.182(2) 12_565 ?
Mn1 O1 2.182(2) 3_565 ?
O1 C1 1.235(3) . ?

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 82.32(11) 11 2_665 ?
O1 Mn1 O1 90.82(9) 11 10_665 ?
O1 Mn1 O1 96.97(12) 2_665 10_665 ?
O1 Mn1 O1 96.97(12) 11 . ?
O1 Mn1 O1 90.82(9) 2_665 . ?
O1 Mn1 O1 169.66(10) 10_665 . ?
O1 Mn1 O1 90.82(9) 11 12_565 ?
O1 Mn1 O1 169.67(10) 2_665 12_565 ?
O1 Mn1 O1 90.82(9) 10_665 12_565 ?
O1 Mn1 O1 82.32(11) . 12_565 ?
O1 Mn1 O1 169.67(10) 11 3_565 ?
O1 Mn1 O1 90.82(9) 2_665 3_565 ?
O1 Mn1 O1 82.31(11) 10_665 3_565 ?
O1 Mn1 O1 90.82(9) . 3_565 ?
O1 Mn1 O1 96.97(12) 12_565 3_565 ?
C1 O1 Mn1 123.4(2) . . ?
O1 C1 O1 127.5(4) . 8_675 ?

_refine_diff_density_max         0.289
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.073


# start Validation Reply Form
_vrf_PLAT029_AMnF_c1_p02         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.850 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT911_AMnF_c1_p02         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         27 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT915_AMnF_c1_p02         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         58 %     
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p04
_database_code_depnum_ccdc_archive 'CCDC 1861332'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_sum            'C3 H7 Mn N O6'
_chemical_formula_weight         208.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0006 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1789 0.2612 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           182
_space_group_name_H-M_alt        'P 63 2 2'
_space_group_name_Hall           'P 6c 2c'

_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'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   7.2974(3)
_cell_length_b                   7.2974(3)
_cell_length_c                   8.4850(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     391.31(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    268
_cell_measurement_theta_min      1.8650
_cell_measurement_theta_max      14.3310

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             210
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.370
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_pressure         '0.36 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            832
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.864
_diffrn_reflns_theta_max         19.384
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.652
_diffrn_measured_fraction_theta_full 0.870
_diffrn_reflns_Laue_measured_fraction_max 0.652
_diffrn_reflns_Laue_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.628
_diffrn_reflns_point_group_measured_fraction_full 0.906
_reflns_number_total             368
_reflns_number_gt                302
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.443
_reflns_Friedel_fraction_max     0.579
_reflns_Friedel_fraction_full    1.000

_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       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0489P)²+0.3746P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 79 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         368
_refine_ls_number_parameters     22
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.142
_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 0.333333 0.666667 0.250000 0.0323(5) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.087(5) Uani 1 6 d DS T P . .
H2 H 1.08(2) 1.121(10) 0.181(9) 0.104 Uiso 0.6667 1 d D U P . .
O1 O 0.5934(5) 0.8958(5) 0.1043(5) 0.0481(9) Uani 1 1 d . . . . .
C1 C 0.5716(11) 1.000000 0.000000 0.061(3) Uani 1 2 d S T P . .
H1 H 0.444180 0.999999 0.000001 0.073 Uiso 1 2 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 2.180(3) 11 ?
Mn1 O1 2.180(3) 2_665 ?
Mn1 O1 2.180(3) 10_665 ?
Mn1 O1 2.180(3) 12_565 ?
Mn1 O1 2.180(3) 3_565 ?
Mn1 O1 2.180(3) . ?
O1 C1 1.228(5) . ?

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 82.14(18) 11 2_665 ?
O1 Mn1 O1 91.00(15) 11 10_665 ?
O1 Mn1 O1 96.8(2) 2_665 10_665 ?
O1 Mn1 O1 91.00(15) 11 12_565 ?
O1 Mn1 O1 169.70(18) 2_665 12_565 ?
O1 Mn1 O1 91.00(15) 10_665 12_565 ?
O1 Mn1 O1 169.70(18) 11 3_565 ?
O1 Mn1 O1 91.00(15) 2_665 3_565 ?
O1 Mn1 O1 82.14(18) 10_665 3_565 ?
O1 Mn1 O1 96.8(2) 12_565 3_565 ?
O1 Mn1 O1 96.8(2) 11 . ?
O1 Mn1 O1 91.01(15) 2_665 . ?
O1 Mn1 O1 169.70(17) 10_665 . ?
O1 Mn1 O1 82.14(18) 12_565 . ?
O1 Mn1 O1 91.00(15) 3_565 . ?
C1 O1 Mn1 123.4(4) . . ?
O1 C1 O1 127.9(8) 8_675 . ?

_refine_diff_density_max         0.363
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.077


# start Validation Reply Form
_vrf_PLAT029_AMnF_c1_p04         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.870 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT911_AMnF_c1_p04         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         23 Report
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT915_AMnF_c1_p04         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         58 %     
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p05
_database_code_depnum_ccdc_archive 'CCDC 1861333'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'

#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 Mn1 N1 O6'
_chemical_formula_weight         208
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.741(3)
_cell_length_b                   8.486(3)
_cell_length_c                   7.440(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.87(5)
_cell_angle_gamma                90
_cell_volume                     379.6(3)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.153(3) 1 0 0 0 1 0 0 0 1
2 0.1550(14) 1 0 0 0 -1 0 0.819 0 -1
3 0.1419(14) -0.0612 0 -1.0715 0 1 0 0.8796 0 -0.9388
4 0.1282(14) -0.9388 0 1.0715 0 -1 0 0.1107 0 0.9388
5 0.2192(14) -0.9388 0 1.0715 0 1 0 -0.8796 0 -0.0612
6 0.2028(13) -0.0612 0 -1.0715 0 -1 0 -0.9297 0 0.0612

_cell_formula_units_Z            2

_cell_measurement_reflns_used    174
_cell_measurement_theta_min      1.78
_cell_measurement_theta_max      13.03
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.8198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             202

_exptl_absorpt_coefficient_mu    0.369
_exptl_crystal_description       block
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_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.
;
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '0.45 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            3084
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         13.21
_diffrn_reflns_theta_full        12.75
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measured_fraction_theta_full 0.94
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             2531
_reflns_number_gt                1961
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_gt          0.0759
_refine_ls_R_factor_all          0.0816
_refine_ls_wR_factor_ref         0.0792
_refine_ls_goodness_of_fit_ref   2.36
_refine_ls_goodness_of_fit_gt    2.58
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         2531
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_number_constraints    31
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0364
_refine_ls_shift/su_mean         0.0033
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  547 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_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    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.6622(2) 0.25 0.32421(13) Uani 0.0410(5) 2 1 d . . .
O1 O 0.8806(10) 0.1018(8) 0.5720(7) Uani 0.055(3) 2 1 d . . .
O2 O 0.3756(10) 0.1108(8) 0.2922(8) Uani 0.053(3) 2 1 d . . .
O3 O 0.7023(10) 0.1013(8) 0.1037(7) Uani 0.053(3) 2 1 d . . .
O4 O 0.9172(10) 0.3867(8) 0.2944(8) Uani 0.053(3) 2 1 d . . .
O5 O 0.6903(10) 0.3975(8) 0.5720(7) Uani 0.055(3) 2 1 d . . .
O6 O 0.4013(9) 0.3966(8) 0.1028(7) Uani 0.052(2) 2 1 d . . .
C1 C 0.9435(16) -0.0330(11) 0.5666(13) Uani 0.055(3) 2 1 d . . .
C2 C 0.6176(15) 0.5326(11) 0.5625(12) Uani 0.055(3) 2 1 d . . .
C3 C 0.4317(16) 0.4984(12) -0.0016(14) Uani 0.052(2) 2 1 d . . .
N1 N -0.0222(10) 0.2517(13) -0.0476(8) Uani 0.052(3) 2 1 d . . .
H1c1 H 0.875497 -0.083206 0.436996 Uiso 0.0665 2 1 d . . .
H1c2 H 0.549833 0.581711 0.43222 Uiso 0.0655 2 1 d . . .
H1c3 H 0.573138 0.497524 -0.003528 Uiso 0.0619 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 . . 2.166(6) ?
Mn1 O2 . . 2.184(7) ?
Mn1 O3 . . 2.181(7) ?
Mn1 O4 . . 2.167(7) ?
Mn1 O5 . . 2.165(6) ?
Mn1 O6 . . 2.176(6) ?
O1 C1 . . 1.227(12) ?
O2 C2 . 2_646 1.251(12) ?
O3 C3 . 2_645 1.239(11) ?
O4 C1 . 2_756 1.240(10) ?
O5 C2 . . 1.236(11) ?
O6 C3 . . 1.240(13) ?
C1 H1c1 . . 0.96 ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Mn1 O2 . . . 90.4(2) ?
O1 Mn1 O3 . . . 92.1(2) ?
O1 Mn1 O4 . . . 97.6(2) ?
O1 Mn1 O5 . . . 81.2(2) ?
O1 Mn1 O6 . . . 169.1(3) ?
O2 Mn1 O3 . . . 90.5(3) ?
O2 Mn1 O4 . . . 169.2(2) ?
O2 Mn1 O5 . . . 97.9(3) ?
O2 Mn1 O6 . . . 81.6(2) ?
O3 Mn1 O4 . . . 81.9(3) ?
O3 Mn1 O5 . . . 169.2(2) ?
O3 Mn1 O6 . . . 95.4(2) ?
O4 Mn1 O5 . . . 90.5(3) ?
O4 Mn1 O6 . . . 91.3(2) ?
O5 Mn1 O6 . . . 92.5(2) ?
Mn1 O1 C1 . . . 128.7(5) ?
Mn1 O2 C2 . . 2_646 120.5(5) ?
Mn1 O3 C3 . . 2_645 124.4(8) ?
Mn1 O4 C1 . . 2_756 123.1(7) ?
Mn1 O5 C2 . . . 127.4(5) ?
Mn1 O6 C3 . . . 124.5(6) ?
O1 C1 O4 . . 2_746 128.9(8) ?
O1 C1 H1c1 . . . 115.56 ?
O4 C1 H1c1 2_746 . . 115.56 ?
O2 C2 O5 2_656 . . 125.7(8) ?
O2 C2 H1c2 2_656 . . 117.15 ?
O5 C2 H1c2 . . . 117.15 ?
O3 C3 O6 2_655 . . 126.5(11) ?
O3 C3 H1c3 2_655 . . 116.77 ?
O6 C3 H1c3 . . . 116.77 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?



# start Validation Reply Form
_vrf_PLAT027_AMnF_c1_p05         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      12.75 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_AMnF_c1_p05         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_THETM01_AMnF_c1_p05         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT029_AMnF_c1_p05         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.950 Note  
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT043_AMnF_c1_p05         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.00 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT112_AMnF_c1_p05         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        2        100 %Fit  
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT113_AMnF_c1_p05         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT430_AMnF_c1_p05         
;
PROBLEM: Short Inter D...A Contact  O1       ..N1               2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_AMnF_c1_p05         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, giving broader and lower resolution reflections. 
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro was performed on each domain individually. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT034_AMnF_c1_p05         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: In the P6322 structure before the phase transition, 
the flack parameter was refined to -0.05(10), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_AMnF_c1_p05         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT162_AMnF_c1_p05         
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for .        MN1 Check 
RESPONSE: The origin of the unit cell was fixed using the
y-coordinate of the Mn atom.
;
_vrf_PLAT250_AMnF_c1_p05         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p06
_database_code_depnum_ccdc_archive 'CCDC 1861334'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'

#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 Mn1 N1 O6'
_chemical_formula_weight         208
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.6400(19)
_cell_length_b                   8.4889(18)
_cell_length_c                   7.422(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.45(4)
_cell_angle_gamma                90
_cell_volume                     374.6(2)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.161(3) 1 0 0 0 1 0 0 0 1
2 0.1583(15) 1 0 0 0 -1 0 0.797 0 -1
3 0.1404(14) -0.0692 0 -1.0812 0 1 0 0.8654 0 -0.9308
4 0.1243(14) -0.9308 0 1.0812 0 -1 0 0.1235 0 0.9309
5 0.2159(14) -0.9308 0 1.0812 0 1 0 -0.8654 0 -0.0692
6 0.2004(14) -0.0692 0 -1.0812 0 -1 0 -0.9205 0 0.0691

_cell_formula_units_Z            2

_cell_measurement_reflns_used    168
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      13.19
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.8445
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             202

_exptl_absorpt_coefficient_mu    0.374
_exptl_crystal_description       block
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_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.
;
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '0.62 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            3023
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         13.22
_diffrn_reflns_theta_full        7.23
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measured_fraction_theta_full 0.95
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             3023
_reflns_number_gt                2179
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0687
_refine_ls_wR_factor_gt          0.0798
_refine_ls_R_factor_all          0.0880
_refine_ls_wR_factor_ref         0.0851
_refine_ls_goodness_of_fit_ref   2.14
_refine_ls_goodness_of_fit_gt    2.38
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3023
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_number_constraints    13
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0292
_refine_ls_shift/su_mean         0.0063
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  802 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_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    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.6620(2) 0.25 0.32432(15) Uani 0.0456(5) 2 1 d . . .
O1 O 0.8774(10) 0.1013(8) 0.5715(7) Uani 0.058(3) 2 1 d . . .
O2 O 0.3677(11) 0.1133(8) 0.2903(9) Uani 0.060(3) 2 1 d . . .
O3 O 0.7033(11) 0.0996(9) 0.1028(8) Uani 0.059(3) 2 1 d . . .
O4 O 0.9234(10) 0.3828(8) 0.2939(8) Uani 0.056(3) 2 1 d . . .
O5 O 0.6904(11) 0.3968(9) 0.5710(8) Uani 0.062(4) 2 1 d . . .
O6 O 0.4017(10) 0.3976(8) 0.1036(8) Uani 0.055(3) 2 1 d . . .
C1 C 0.9406(16) -0.0336(13) 0.5700(14) Uani 0.063(5) 2 1 d . . .
C2 C 0.6241(16) 0.5336(14) 0.5640(14) Uani 0.066(6) 2 1 d . . .
C3 C 0.4350(17) 0.4995(15) 0.0001(17) Uani 0.063(5) 2 1 d . . .
N1 N -0.0220(10) 0.2514(14) -0.0482(8) Uani 0.054(3) 2 1 d . . .
H1c1 H 0.872714 -0.083431 0.440345 Uiso 0.0752 2 1 d . . .
H1c2 H 0.560153 0.583954 0.43467 Uiso 0.0795 2 1 d . . .
H1c3 H 0.57958 0.500635 0.000039 Uiso 0.0761 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 . . 2.160(6) ?
Mn1 O2 . . 2.188(7) ?
Mn1 O3 . . 2.193(7) ?
Mn1 O4 . . 2.164(7) ?
Mn1 O5 . . 2.152(7) ?
Mn1 O6 . . 2.172(6) ?
O1 C1 . . 1.222(13) ?
O2 C2 . 2_646 1.256(14) ?
O3 C3 . 2_645 1.234(13) ?
O4 C1 . 2_756 1.236(11) ?
O5 C2 . . 1.235(14) ?
O6 C3 . . 1.240(15) ?
C1 H1c1 . . 0.96 ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Mn1 O2 . . . 90.4(2) ?
O1 Mn1 O3 . . . 92.3(2) ?
O1 Mn1 O4 . . . 97.7(2) ?
O1 Mn1 O5 . . . 80.9(2) ?
O1 Mn1 O6 . . . 168.8(3) ?
O2 Mn1 O3 . . . 90.5(3) ?
O2 Mn1 O4 . . . 168.7(2) ?
O2 Mn1 O5 . . . 98.1(3) ?
O2 Mn1 O6 . . . 81.3(2) ?
O3 Mn1 O4 . . . 81.5(3) ?
O3 Mn1 O5 . . . 169.1(3) ?
O3 Mn1 O6 . . . 95.4(2) ?
O4 Mn1 O5 . . . 90.9(3) ?
O4 Mn1 O6 . . . 91.5(2) ?
O5 Mn1 O6 . . . 92.7(2) ?
Mn1 O1 C1 . . . 129.8(6) ?
Mn1 O2 C2 . . 2_646 119.5(5) ?
Mn1 O3 C3 . . 2_645 123.9(8) ?
Mn1 O4 C1 . . 2_756 122.8(7) ?
Mn1 O5 C2 . . . 127.9(6) ?
Mn1 O6 C3 . . . 124.6(6) ?
O1 C1 O4 . . 2_746 131.3(9) ?
O1 C1 H1c1 . . . 114.35 ?
O4 C1 H1c1 2_746 . . 114.35 ?
O2 C2 O5 2_656 . . 126.4(9) ?
O2 C2 H1c2 2_656 . . 116.82 ?
O5 C2 H1c2 . . . 116.82 ?
O3 C3 O6 2_655 . . 125.1(11) ?
O3 C3 H1c3 2_655 . . 117.47 ?
O6 C3 H1c3 . . . 117.47 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_PLAT027_AMnF_c1_p06         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      7.23 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_AMnF_c1_p06         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_THETM01_AMnF_c1_p06         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT021_AMnF_c1_p06         
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      5.159 
RESPONSE: Reflections from six twin domains were used in the refinement.
;
_vrf_PLAT029_AMnF_c1_p06         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.950 Note  
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT043_AMnF_c1_p06         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.00 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT112_AMnF_c1_p06         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        2        100 %Fit  
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT113_AMnF_c1_p06         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT430_AMnF_c1_p06         
;
PROBLEM: Short Inter D...A Contact  O1       ..N1               2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_AMnF_c1_p06         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, giving broader and lower resolution reflections. 
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro was performed on each domain individually. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT034_AMnF_c1_p06         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: In the P6322 structure before the phase transition, 
the flack parameter was refined to -0.05(10), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_AMnF_c1_p06         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT162_AMnF_c1_p06         
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for .        MN1 Check 
RESPONSE: The origin of the unit cell was fixed using the
y-coordinate of the Mn atom.
;
_vrf_PLAT234_AMnF_c1_p06         
;
PROBLEM: Large Hirshfeld Difference O2       --C2_b             0.21 Ang.  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_PLAT250_AMnF_c1_p06         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p07
_database_code_depnum_ccdc_archive 'CCDC 1861335'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'


# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 Mn1 N1 O6'
_chemical_formula_weight         208
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.537(2)
_cell_length_b                   8.4865(16)
_cell_length_c                   7.405(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.09(4)
_cell_angle_gamma                90
_cell_volume                     368.9(2)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.242(3) 1 0 0 0 1 0 0 0 1
2 0.1450(13) 1 0 0 0 -1 0 0.7765 0 -1
3 0.1133(11) -0.0759 0 -1.0923 0 1 0 0.8512 0 -0.9241
4 0.1000(11) -0.9241 0 1.0923 0 -1 0 0.1336 0 0.9241
5 0.1595(11) -0.9241 0 1.0923 0 1 0 -0.8512 0 -0.0759
6 0.2405(16) -0.0759 0 -1.0923 0 -1 0 -0.9101 0 0.0759

_cell_formula_units_Z            2

_cell_measurement_reflns_used    239
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      14.68
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.8726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             202

_exptl_absorpt_coefficient_mu    0.379
_exptl_crystal_description       block
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_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.
;
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '0.85 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            3805
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         14.87
_diffrn_reflns_theta_full        7.18
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measured_fraction_theta_full 0.96
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             3805
_reflns_number_gt                3016
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_gt          0.0923
_refine_ls_R_factor_all          0.0876
_refine_ls_wR_factor_ref         0.0950
_refine_ls_goodness_of_fit_ref   2.87
_refine_ls_goodness_of_fit_gt    3.14
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3805
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_number_constraints    13
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0356
_refine_ls_shift/su_mean         0.0071
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  995 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_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    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.66261(17) 0.25 0.32416(12) Uani 0.0424(4) 2 1 d . . .
O1 O 0.8754(9) 0.0990(7) 0.5688(7) Uani 0.059(3) 2 1 d . . .
O2 O 0.3658(9) 0.1170(7) 0.2940(7) Uani 0.054(2) 2 1 d . . .
O3 O 0.7008(10) 0.1003(8) 0.1035(7) Uani 0.060(3) 2 1 d . . .
O4 O 0.9290(9) 0.3819(7) 0.2930(7) Uani 0.057(3) 2 1 d . . .
O5 O 0.6891(9) 0.3982(7) 0.5706(7) Uani 0.058(3) 2 1 d . . .
O6 O 0.4061(8) 0.3994(7) 0.1049(7) Uani 0.054(2) 2 1 d . . .
C1 C 0.9291(13) -0.0402(10) 0.5648(11) Uani 0.058(4) 2 1 d . . .
C2 C 0.3658(14) 0.0378(11) 0.4360(12) Uani 0.065(5) 2 1 d . . .
C3 C 0.4405(14) 0.5003(11) 0.0021(13) Uani 0.056(4) 2 1 d . . .
N1 N -0.0250(9) 0.2519(12) -0.0553(7) Uani 0.054(3) 2 1 d . . .
H1c1 H 0.853233 -0.093935 0.438356 Uiso 0.0698 2 1 d . . .
H1c2 H 0.413245 0.090701 0.562685 Uiso 0.0776 2 1 d . . .
H1c3 H 0.587967 0.502041 0.003476 Uiso 0.067 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 . . 2.154(5) ?
Mn1 O2 . . 2.170(6) ?
Mn1 O3 . . 2.169(7) ?
Mn1 O4 . . 2.166(7) ?
Mn1 O5 . . 2.160(6) ?
Mn1 O6 . . 2.159(5) ?
O1 C1 . . 1.237(11) ?
O2 C2 . . 1.248(11) ?
O3 C3 . 2_645 1.245(10) ?
O4 C1 . 2_756 1.244(9) ?
O5 C2 . 2_656 1.233(11) ?
O6 C3 . . 1.230(12) ?
C1 H1c1 . . 0.96 ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Mn1 O2 . . . 89.7(2) ?
O1 Mn1 O3 . . . 92.2(2) ?
O1 Mn1 O4 . . . 98.3(2) ?
O1 Mn1 O5 . . . 81.6(2) ?
O1 Mn1 O6 . . . 169.2(3) ?
O2 Mn1 O3 . . . 90.7(2) ?
O2 Mn1 O4 . . . 169.20(18) ?
O2 Mn1 O5 . . . 97.2(2) ?
O2 Mn1 O6 . . . 82.2(2) ?
O3 Mn1 O4 . . . 81.9(2) ?
O3 Mn1 O5 . . . 169.9(2) ?
O3 Mn1 O6 . . . 94.9(2) ?
O4 Mn1 O5 . . . 91.1(2) ?
O4 Mn1 O6 . . . 90.6(2) ?
O5 Mn1 O6 . . . 92.3(2) ?
Mn1 O1 C1 . . . 129.3(5) ?
Mn1 O2 C2 . . . 121.6(4) ?
Mn1 O3 C3 . . 2_645 125.0(7) ?
Mn1 O4 C1 . . 2_756 121.3(6) ?
Mn1 O5 C2 . . 2_656 127.8(5) ?
Mn1 O6 C3 . . . 125.6(5) ?
O1 C1 O4 . . 2_746 127.0(7) ?
O1 C1 H1c1 . . . 116.52 ?
O4 C1 H1c1 2_746 . . 116.52 ?
O2 C2 O5 . . 2_646 126.3(8) ?
O2 C2 H1c2 . . . 116.86 ?
O5 C2 H1c2 2_646 . . 116.86 ?
O3 C3 O6 2_655 . . 125.2(9) ?
O3 C3 H1c3 2_655 . . 117.39 ?
O6 C3 H1c3 . . . 117.39 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_PLAT027_AMnF_c1_p07         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      7.18 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_AMnF_c1_p07         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_PLAT021_AMnF_c1_p07         
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      4.669
RESPONSE: Reflections from six twin domains were used in the refinement.
;
_vrf_PLAT043_AMnF_c1_p07         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.00 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT112_AMnF_c1_p07         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        2        100 %Fit  
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT113_AMnF_c1_p07         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT430_AMnF_c1_p07         
;
PROBLEM: Short Inter D...A Contact  O1       ..N1               2.87 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_AMnF_c1_p07         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, giving broader and lower resolution reflections. 
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro was performed on each domain individually. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT029_AMnF_c1_p07         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.960 Note  
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.8 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT034_AMnF_c1_p07         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: In the P6322 structure before the phase transition, 
the flack parameter was refined to -0.05(10), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_AMnF_c1_p07         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT162_AMnF_c1_p07         
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for .        MN1 Check 
RESPONSE: The origin of the unit cell was fixed using the
y-coordinate of the Mn atom.
;
_vrf_PLAT250_AMnF_c1_p07         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c1_p08
_database_code_depnum_ccdc_archive 'CCDC 1861336'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'

#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C3 H3 Mn O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 Mn1 N1 O6'
_chemical_formula_weight         208
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.443(3)
_cell_length_b                   8.496(2)
_cell_length_c                   7.372(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.64(8)
_cell_angle_gamma                90
_cell_volume                     363.8(4)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.164(4) 1 0 0 0 1 0 0 0 1
2 0.1495(18) 1 0 0 0 -1 0 0.7564 0 -1
3 0.1361(18) -0.0843 0 -1.0991 0 1 0 0.8396 0 -0.9157
4 0.1408(19) -0.9157 0 1.0991 0 -1 0 0.147 0 0.9157
5 0.2158(19) -0.9157 0 1.0991 0 1 0 -0.8396 0 -0.0843
6 0.1935(18) -0.0843 0 -1.0991 0 -1 0 -0.9034 0 0.0843

_cell_formula_units_Z            2

_cell_measurement_reflns_used    162
_cell_measurement_theta_min      1.77
_cell_measurement_theta_max      13.79
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             202

_exptl_absorpt_coefficient_mu    0.385
_exptl_crystal_description       block
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_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.
;
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '1.09 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            3707
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         14.91
_diffrn_reflns_theta_full        7.17
_diffrn_measured_fraction_theta_max 0.92
_diffrn_measured_fraction_theta_full 0.96
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             3707
_reflns_number_gt                2557
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0964
_refine_ls_wR_factor_gt          0.1167
_refine_ls_R_factor_all          0.1206
_refine_ls_wR_factor_ref         0.1235
_refine_ls_goodness_of_fit_ref   3.20
_refine_ls_goodness_of_fit_gt    3.65
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3707
_refine_ls_number_parameters     104
_refine_ls_number_restraints     0
_refine_ls_number_constraints    13
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0145
_refine_ls_shift/su_mean         0.0028
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  937 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_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    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.6626(3) 0.25 0.32476(18) Uani 0.0569(6) 2 1 d . . .
O1 O 0.8754(14) 0.0991(11) 0.5689(10) Uani 0.074(4) 2 1 d . . .
O2 O 0.3593(14) 0.1199(10) 0.2923(11) Uani 0.068(4) 2 1 d . . .
O3 O 0.7010(14) 0.0988(12) 0.1026(10) Uani 0.071(4) 2 1 d . . .
O4 O 0.9315(13) 0.3788(10) 0.2912(12) Uani 0.069(4) 2 1 d . . .
O5 O 0.6867(15) 0.4002(11) 0.5693(11) Uani 0.073(4) 2 1 d . . .
O6 O 0.4038(13) 0.4019(11) 0.1049(10) Uani 0.070(4) 2 1 d . . .
C1 C 0.928(2) -0.0383(17) 0.568(2) Uani 0.083(7) 2 1 d . . .
C2 C 0.3583(19) 0.0443(15) 0.4287(16) Uani 0.072(6) 2 1 d . . .
C3 C 0.560(2) 0.0045(18) -0.001(2) Uani 0.079(7) 2 1 d . . .
N1 N -0.0257(14) 0.2495(17) -0.0546(10) Uani 0.063(4) 2 1 d . . .
H1c1 H 0.851156 -0.091101 0.440856 Uiso 0.0994 2 1 d . . .
H1c2 H 0.396488 0.100417 0.552066 Uiso 0.0867 2 1 d . . .
H1c3 H 0.410023 0.008525 -0.003516 Uiso 0.0946 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 . . 2.151(8) ?
Mn1 O2 . . 2.166(9) ?
Mn1 O3 . . 2.178(10) ?
Mn1 O4 . . 2.152(10) ?
Mn1 O5 . . 2.159(9) ?
Mn1 O6 . . 2.175(8) ?
O1 C1 . . 1.216(17) ?
O2 C2 . . 1.195(15) ?
O3 C3 . . 1.203(16) ?
O4 C1 . 2_756 1.257(14) ?
O5 C2 . 2_656 1.259(16) ?
O6 C3 . 2_655 1.25(2) ?
C1 H1c1 . . 0.96 ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Mn1 O2 . . . 90.4(3) ?
O1 Mn1 O3 . . . 92.2(3) ?
O1 Mn1 O4 . . . 98.4(3) ?
O1 Mn1 O5 . . . 82.2(3) ?
O1 Mn1 O6 . . . 169.2(4) ?
O2 Mn1 O3 . . . 90.4(3) ?
O2 Mn1 O4 . . . 168.3(3) ?
O2 Mn1 O5 . . . 97.4(4) ?
O2 Mn1 O6 . . . 81.8(3) ?
O3 Mn1 O4 . . . 81.6(4) ?
O3 Mn1 O5 . . . 170.4(3) ?
O3 Mn1 O6 . . . 95.1(3) ?
O4 Mn1 O5 . . . 91.4(4) ?
O4 Mn1 O6 . . . 90.5(3) ?
O5 Mn1 O6 . . . 91.5(3) ?
Mn1 O1 C1 . . . 130.2(8) ?
Mn1 O2 C2 . . . 121.0(7) ?
Mn1 O3 C3 . . . 124.7(11) ?
Mn1 O4 C1 . . 2_756 121.2(10) ?
Mn1 O5 C2 . . 2_656 130.6(7) ?
Mn1 O6 C3 . . 2_655 125.9(9) ?
O1 C1 O4 . . 2_746 129.5(12) ?
O1 C1 H1c1 . . . 115.27 ?
O4 C1 H1c1 2_746 . . 115.27 ?
O2 C2 O5 . . 2_646 128.1(11) ?
O2 C2 H1c2 . . . 115.93 ?
O5 C2 H1c2 2_646 . . 115.93 ?
O3 C3 O6 . . 2_645 124.5(16) ?
O3 C3 H1c3 . . . 117.77 ?
O6 C3 H1c3 2_645 . . 117.77 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_PLAT027_AMnF_c1_p08         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      7.17 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_AMnF_c1_p08         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_PLAT021_AMnF_c1_p08         
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      4.622
RESPONSE: Reflections from six twin domains were used in the refinement.
;
_vrf_PLAT043_AMnF_c1_p08         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.00 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT112_AMnF_c1_p08         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        2        100 %Fit  
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT113_AMnF_c1_p08         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT149_AMnF_c1_p08         
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.08 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, as well as upon increase in pressure. The broad reflections
give a large uncertainty on certain parameters. 
;
_vrf_PLAT430_AMnF_c1_p08         
;
PROBLEM: Short Inter D...A Contact  O1       ..N1               2.87 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_AMnF_c1_p08         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, giving broader and lower resolution reflections. 
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro was performed on each domain individually. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT029_AMnF_c1_p08         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.960 Note  
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.8 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT034_AMnF_c1_p08         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: In the P6322 structure before the phase transition, 
the flack parameter was refined to -0.05(10), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_AMnF_c1_p08         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT162_AMnF_c1_p08         
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for .        MN1 Check 
RESPONSE: The origin of the unit cell was fixed using the
y-coordinate of the Mn atom.
;
_vrf_PLAT250_AMnF_c1_p08         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.3 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c2_p01
_database_code_depnum_ccdc_archive 'CCDC 1861337'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'

#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C6 H6 Mn2 O12, N2 H8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C6 H14 Mn2 N2 O12'
_chemical_formula_weight         416
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.714(5)
_cell_length_b                   7.119(4)
_cell_length_c                   14.031(5)
_cell_angle_alpha                90
_cell_angle_beta                 89.99(4)
_cell_angle_gamma                90
_cell_volume                     670.6(7)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.264(6) 1 0 0 0 1 0 0 0 1
2 0.301(4) 0.991 0 -0.2787 0 -1 0 -0.064 0 -0.991
3 0.435(4) -0.611 0 -1.6542 0 -1 0 -0.3787 0 0.6113

_cell_formula_units_Z            2

_cell_measurement_reflns_used    132
_cell_measurement_theta_min      1.95
_cell_measurement_theta_max      10.97
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.0604
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             404

_exptl_absorpt_coefficient_mu    0.418
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_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.
;
_exptl_absorpt_correction_T_min  0.381
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '1.38 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            1974
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         11.9
_diffrn_reflns_theta_full        10.18
_diffrn_measured_fraction_theta_max 0.82
_diffrn_measured_fraction_theta_full 0.84
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0982
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             1974
_reflns_number_gt                1076
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1402
_refine_ls_wR_factor_gt          0.1499
_refine_ls_R_factor_all          0.1952
_refine_ls_wR_factor_ref         0.1631
_refine_ls_goodness_of_fit_ref   2.97
_refine_ls_goodness_of_fit_gt    3.74
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         1974
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_number_constraints    49
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0167
_refine_ls_shift/su_mean         0.0020
_refine_diff_density_max         1.30
_refine_diff_density_min         -1.20
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  714 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_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    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.6340(7) 0.7078(8) 0.8501(3) Uani 0.0488(13) 2 1 d . . .
Mn2 Mn 0.1336(7) 0.2202(8) 0.6501(3) Uani 0.0488(13) 2 1 d . . .
C1 C 0.906(5) -0.138(6) 0.551(2) Uiso 0.078(5) 2 1 d . . .
C2 C 0.523(6) 1.014(6) 0.705(3) Uiso 0.078(5) 2 1 d . . .
C3 C 1.019(5) 0.913(5) 0.801(2) Uiso 0.057(4) 2 1 d . . .
C4 C 0.253(5) 0.473(5) 0.816(2) Uiso 0.063(4) 2 1 d . . .
C5 C 0.762(5) 0.423(4) 0.6920(18) Uiso 0.052(4) 2 1 d . . .
C6 C 0.616(5) 0.583(5) 1.040(2) Uiso 0.056(4) 2 1 d . . .
O1 O 1.069(3) 1.075(3) 0.7819(13) Uiso 0.057(4) 2 1 d . . .
O2 O 0.488(3) 0.948(3) 0.9280(13) Uiso 0.056(4) 2 1 d . . .
O3 O 0.362(3) 0.576(4) 0.8644(14) Uiso 0.063(4) 2 1 d . . .
O4 O 0.729(3) 0.596(3) 0.9835(13) Uiso 0.056(4) 2 1 d . . .
O5 O 0.776(3) 0.474(3) 0.7700(13) Uiso 0.052(4) 2 1 d . . .
O6 O 0.419(4) 1.087(4) 0.6337(16) Uiso 0.078(5) 2 1 d . . .
O7 O 0.912(3) 0.854(3) 0.8574(13) Uiso 0.057(4) 2 1 d . . .
O8 O 0.276(3) 0.452(3) 0.7297(13) Uiso 0.063(4) 2 1 d . . .
O9 O 0.842(3) 0.333(3) 0.6328(13) Uiso 0.052(4) 2 1 d . . .
O10 O 0.986(4) 0.018(4) 0.5663(16) Uiso 0.078(5) 2 1 d . . .
O11 O 0.570(4) 0.861(4) 0.7182(16) Uiso 0.078(5) 2 1 d . . .
O12 O 0.235(4) 0.352(4) 0.5122(15) Uiso 0.078(5) 2 1 d . . .
N1 N 0.637(3) 0.213(5) 0.4741(15) Uani 0.061(8) 2 1 d . . .
N2 N 0.117(3) 0.708(5) 1.0230(15) Uani 0.061(8) 2 1 d . . .
H1c1 H 0.948229 -0.248111 0.585849 Uiso 0.0932 2 1 d . . .
H1c2 H 0.565061 1.101996 0.753067 Uiso 0.0937 2 1 d . . .
H1c6 H 0.590086 0.699329 1.072711 Uiso 0.0672 2 1 d . . .
H1c5 H 0.638901 0.469569 0.666221 Uiso 0.062 2 1 d . . .
H1c3 H 1.080374 0.818581 0.761125 Uiso 0.069 2 1 d . . .
H1c4 H 0.146152 0.406806 0.847244 Uiso 0.0756 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O2 . . 2.25(2) ?
Mn1 O3 . . 2.06(2) ?
Mn1 O4 . . 2.13(2) ?
Mn1 O5 . . 2.22(2) ?
Mn1 O7 . . 2.14(2) ?
Mn1 O11 . . 2.19(2) ?
Mn2 O1 . 1_445 2.16(2) ?
Mn2 O6 . 1_545 2.15(3) ?
Mn2 O8 . . 2.21(2) ?
Mn2 O9 . 1_455 2.13(2) ?
Mn2 O10 . 1_455 2.11(3) ?
Mn2 O12 . . 2.25(2) ?
C1 O10 . . 1.25(5) ?
C1 O12 . 2_646 1.31(4) ?
C1 H1c1 . . 0.96 ?
C2 O6 . . 1.33(4) ?
C2 O11 . . 1.15(5) ?
C2 H1c2 . . 0.96 ?
C3 O1 . . 1.23(4) ?
C3 O7 . . 1.15(4) ?
C3 H1c3 . . 0.96 ?
C4 O3 . . 1.24(4) ?
C4 O8 . . 1.23(3) ?
C4 H1c4 . . 0.96 ?
C5 O5 . . 1.16(3) ?
C5 O9 . . 1.18(3) ?
C5 H1c5 . . 0.96 ?
C6 O2 . 2_647 1.26(4) ?
C6 O4 . . 1.11(4) ?
C6 H1c6 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Mn1 O3 . . . 85.0(9) ?
O2 Mn1 O4 . . . 89.4(8) ?
O2 Mn1 O5 . . . 178.6(7) ?
O2 Mn1 O7 . . . 89.3(8) ?
O2 Mn1 O11 . . . 86.9(9) ?
O3 Mn1 O4 . . . 90.6(8) ?
O3 Mn1 O5 . . . 95.1(9) ?
O3 Mn1 O7 . . . 171.5(8) ?
O3 Mn1 O11 . . . 97.8(9) ?
O4 Mn1 O5 . . . 92.0(8) ?
O4 Mn1 O7 . . . 83.0(8) ?
O4 Mn1 O11 . . . 170.5(9) ?
O5 Mn1 O7 . . . 90.8(8) ?
O5 Mn1 O11 . . . 91.7(8) ?
O7 Mn1 O11 . . . 88.1(9) ?
O1 Mn2 O6 1_445 . 1_545 93.4(9) ?
O1 Mn2 O8 1_445 . . 90.7(8) ?
O1 Mn2 O9 1_445 . 1_455 95.4(8) ?
O1 Mn2 O10 1_445 . 1_455 93.2(9) ?
O1 Mn2 O12 1_445 . . 173.1(9) ?
O6 Mn2 O8 1_545 . . 89.8(9) ?
O6 Mn2 O9 1_545 . 1_455 166.8(8) ?
O6 Mn2 O10 1_545 . 1_455 93.4(10) ?
O6 Mn2 O12 1_545 . . 79.8(9) ?
O8 Mn2 O9 . . 1_455 99.9(8) ?
O8 Mn2 O10 . . 1_455 174.8(9) ?
O8 Mn2 O12 . . . 89.5(8) ?
O9 Mn2 O10 1_455 . 1_455 76.3(9) ?
O9 Mn2 O12 1_455 . . 91.3(8) ?
O10 Mn2 O12 1_455 . . 87.0(9) ?
O10 C1 O12 . . 2_646 118(3) ?
O10 C1 H1c1 . . . 120.99 ?
O12 C1 H1c1 2_646 . . 120.99 ?
O6 C2 O11 . . . 130(4) ?
O6 C2 H1c2 . . . 115.23 ?
O11 C2 H1c2 . . . 115.23 ?
O1 C3 O7 . . . 131(3) ?
O1 C3 H1c3 . . . 114.53 ?
O7 C3 H1c3 . . . 114.53 ?
O3 C4 O8 . . . 122(3) ?
O3 C4 H1c4 . . . 118.95 ?
O8 C4 H1c4 . . . 118.95 ?
O5 C5 O9 . . . 143(3) ?
O5 C5 H1c5 . . . 108.5 ?
O9 C5 H1c5 . . . 108.5 ?
O2 C6 O4 2_647 . . 134(3) ?
O2 C6 H1c6 2_647 . . 113.1 ?
O4 C6 H1c6 . . . 113.1 ?
Mn2 O1 C3 1_665 . . 133.3(19) ?
Mn1 O2 C6 . . 2_657 169.9(19) ?
Mn1 O3 C4 . . . 138(2) ?
Mn1 O4 C6 . . . 117(2) ?
Mn1 O5 C5 . . . 133(2) ?
Mn2 O6 C2 1_565 . . 124(2) ?
Mn1 O7 C3 . . . 133(2) ?
Mn2 O8 C4 . . . 122(2) ?
Mn2 O9 C5 1_655 . . 123.2(19) ?
Mn2 O10 C1 1_655 . . 154(2) ?
Mn1 O11 C2 . . . 131(3) ?
Mn2 O12 C1 . . 2_656 113(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_THETM01_AMnF_c2_p01         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A significant loss in resolution is observed in the second
high-pressure phase, therefore the integration was performed to a 
resolution limit of 1.0 A in order to reduce the risk of integrating
diamond peaks.
;
_vrf_PLAT027_AMnF_c2_p01         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      10.18 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT029_AMnF_c2_p01         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.840 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT201_AMnF_c2_p01         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         18 Report
RESPONSE: Due to the reduced quality of the data, isotropic thermal parameters
were preferred for the formate anions.
;
_vrf_PLAT902_AMnF_c2_p01         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_GOODF01_AMnF_c2_p01         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated even further after the 
second high-pressure phase transition, giving broader and 
lower resolution reflections. Six overlapping twin domains still 
coexist upon the transition, however the intensities of the six domains
were not equal and so three of the most intense domains were integrated
individually in CrysAlisPro and refined together in JANA.
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain, as well
as small residual intensity from another domain that was not taken into 
account in the refinement.
;
_vrf_PLAT043_AMnF_c2_p01         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     7.99 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT034_AMnF_c2_p01         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: The refinement of a Flack parameter would probably not be very
reliable given the quality of the data. A similar configuration to the 
ambient c2 structure is chosen.
;
_vrf_PLAT041_AMnF_c2_p01         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT082_AMnF_c2_p01         
;
PROBLEM: High R1 Value ..................................       0.14 Report
RESPONSE: The crystal quality deteriorated even further after the 
second high-pressure phase transition, giving broader and 
lower resolution reflections.
;
_vrf_PLAT157_AMnF_c2_p01         
;
PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg        89.99 Degree
RESPONSE: A setting was chosen that bears closest structural similarity
to the previous HP-II phase.
;
_vrf_PLAT242_AMnF_c2_p01         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Mn2 Check 
RESPONSE: Due to the low-quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT112_AMnF_c2_p01         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        21        100 %Fit  
RESPONSE: The P212121 space group was tested and could be used for
data integration and structure refinement. The data quality was not good enough
to distinguish between P21 and P212121 structural models. We chose the P21 
structure due to the Mossbauer data we obtained on AFeF-III that suggest 
two unique Fe environments in the HP-III phase, which is only compatible 
with the P21 structure.  
;
_vrf_PLAT113_AMnF_c2_p01         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      P212121 Check 
RESPONSE: The P212121 space group was tested and could be used for
data integration and structure refinement. The data quality was not good enough
to distinguish between P21 and P212121 structural models. We chose the P21 
structure due to the Mossbauer data we obtained on AFeF-III that suggest 
two unique Fe environments in the HP-III phase, which is only compatible 
with the P21 structure.   
;
_vrf_PLAT430_AMnF_c2_p01         
;
PROBLEM: Short Inter D...A Contact  O7       ..N2               2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c2_p03
_database_code_depnum_ccdc_archive 'CCDC 1861338'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'

#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C6 H6 Mn2 O12, N2 H8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C6 H14 Mn2 N2 O12'
_chemical_formula_weight         416.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.680(3)
_cell_length_b                   7.097(3)
_cell_length_c                   13.944(5)
_cell_angle_alpha                90
_cell_angle_beta                 89.98(3)
_cell_angle_gamma                90
_cell_volume                     661.1(5)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.278(6) 1 0 0 0 1 0 0 0 1
2 0.357(4) 0.991 0 -0.2787 0 -1 0 -0.0643 0 -0.991
3 0.365(4) -0.6111 0 -1.6522 0 -1 0 -0.379 0 0.6117

_cell_formula_units_Z            2

_cell_measurement_reflns_used    180
_cell_measurement_theta_min      1.69
_cell_measurement_theta_max      11.55
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.0901
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             404

_exptl_absorpt_coefficient_mu    0.424
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '1.54 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            1964
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         11.88
_diffrn_reflns_theta_full        10.57
_diffrn_measured_fraction_theta_max 0.81
_diffrn_measured_fraction_theta_full 0.83
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     0.085
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             1964
_reflns_number_gt                1125
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1350
_refine_ls_wR_factor_gt          0.1583
_refine_ls_R_factor_all          0.1947
_refine_ls_wR_factor_ref         0.1706
_refine_ls_goodness_of_fit_ref   3.46
_refine_ls_goodness_of_fit_gt    4.30
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         1964
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_number_constraints    49
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0499
_refine_ls_shift/su_mean         0.0078
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.45
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  731 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.6330(7) 0.7082(7) 0.8503(3) Uani 0.0528(13) 2 1 d . . .
Mn2 Mn 1.1345(7) 0.2206(8) 0.6498(3) Uani 0.0528(13) 2 1 d . . .
C1 C 0.904(6) -0.132(6) 0.551(2) Uiso 0.084(5) 2 1 d . . .
C2 C 0.526(6) 1.010(6) 0.707(2) Uiso 0.074(4) 2 1 d . . .
C3 C 1.015(5) 0.922(5) 0.7967(19) Uiso 0.057(4) 2 1 d . . .
C4 C 0.248(5) 0.481(5) 0.811(2) Uiso 0.075(5) 2 1 d . . .
C5 C 0.739(5) 0.425(5) 0.6847(18) Uiso 0.060(4) 2 1 d . . .
C6 C 0.614(5) 0.598(5) 1.047(2) Uiso 0.066(4) 2 1 d . . .
O1 O 1.072(3) 1.084(3) 0.7839(12) Uiso 0.057(4) 2 1 d . . .
O2 O 0.492(3) 0.945(3) 0.9288(13) Uiso 0.066(4) 2 1 d . . .
O3 O 0.360(4) 0.574(4) 0.8685(14) Uiso 0.075(5) 2 1 d . . .
O4 O 0.730(3) 0.597(3) 0.9837(13) Uiso 0.066(4) 2 1 d . . .
O5 O 0.773(3) 0.471(3) 0.7733(12) Uiso 0.060(4) 2 1 d . . .
O6 O 0.428(4) 1.079(4) 0.6381(14) Uiso 0.074(4) 2 1 d . . .
O7 O 0.918(3) 0.848(3) 0.8615(12) Uiso 0.057(4) 2 1 d . . .
O8 O 0.265(3) 0.456(4) 0.7279(14) Uiso 0.075(5) 2 1 d . . .
O9 O 0.849(3) 0.347(3) 0.6357(13) Uiso 0.060(4) 2 1 d . . .
O10 O 0.993(4) 0.002(4) 0.5661(15) Uiso 0.084(5) 2 1 d . . .
O11 O 0.570(4) 0.849(4) 0.7187(14) Uiso 0.074(4) 2 1 d . . .
O12 O 1.235(4) 0.346(4) 0.5120(15) Uiso 0.084(5) 2 1 d . . .
N1 N 0.637(3) 0.216(4) 0.4755(14) Uani 0.054(7) 2 1 d . . .
N2 N 0.121(3) 0.710(5) 1.0295(14) Uani 0.054(7) 2 1 d . . .
H1c1 H 0.935935 -0.239897 0.590113 Uiso 0.1012 2 1 d . . .
H1c2 H 0.570024 1.097548 0.754788 Uiso 0.0887 2 1 d . . .
H1c6 H 0.594763 0.711771 1.082565 Uiso 0.0792 2 1 d . . .
H1c5 H 0.610967 0.458315 0.65818 Uiso 0.0722 2 1 d . . .
H1c3 H 1.05293 0.836911 0.746532 Uiso 0.0686 2 1 d . . .
H1c4 H 0.133468 0.423312 0.839423 Uiso 0.09 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O2 . . 2.22(2) ?
Mn1 O3 . . 2.07(3) ?
Mn1 O4 . . 2.12(2) ?
Mn1 O5 . . 2.21(2) ?
Mn1 O7 . . 2.16(2) ?
Mn1 O11 . . 2.13(2) ?
Mn2 O1 . 1_545 2.148(19) ?
Mn2 O6 . 1_645 2.21(3) ?
Mn2 O8 . 1_655 2.18(2) ?
Mn2 O9 . . 2.12(2) ?
Mn2 O10 . . 2.16(3) ?
Mn2 O12 . . 2.22(2) ?
C1 O10 . . 1.15(5) ?
C1 O12 . 2_746 1.29(4) ?
C1 H1c1 . . 0.96 ?
C2 O6 . . 1.26(4) ?
C2 O11 . . 1.19(5) ?
C2 H1c2 . . 0.96 ?
C3 O1 . . 1.22(4) ?
C3 O7 . . 1.23(3) ?
C3 H1c3 . . 0.96 ?
C4 O3 . . 1.28(4) ?
C4 O8 . . 1.17(3) ?
C4 H1c4 . . 0.96 ?
C5 O5 . . 1.30(3) ?
C5 O9 . . 1.15(4) ?
C5 H1c5 . . 0.96 ?
C6 O2 . 2_647 1.34(4) ?
C6 O4 . . 1.17(4) ?
C6 H1c6 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Mn1 O3 . . . 85.1(9) ?
O2 Mn1 O4 . . . 88.7(8) ?
O2 Mn1 O5 . . . 179.4(7) ?
O2 Mn1 O7 . . . 89.5(8) ?
O2 Mn1 O11 . . . 89.2(9) ?
O3 Mn1 O4 . . . 89.5(9) ?
O3 Mn1 O5 . . . 94.7(9) ?
O3 Mn1 O7 . . . 168.8(7) ?
O3 Mn1 O11 . . . 98.4(9) ?
O4 Mn1 O5 . . . 90.8(8) ?
O4 Mn1 O7 . . . 80.6(8) ?
O4 Mn1 O11 . . . 171.6(10) ?
O5 Mn1 O7 . . . 90.7(8) ?
O5 Mn1 O11 . . . 91.4(8) ?
O7 Mn1 O11 . . . 91.2(9) ?
O1 Mn2 O6 1_545 . 1_645 91.7(8) ?
O1 Mn2 O8 1_545 . 1_655 89.4(8) ?
O1 Mn2 O9 1_545 . . 95.7(8) ?
O1 Mn2 O10 1_545 . . 93.5(9) ?
O1 Mn2 O12 1_545 . . 173.0(9) ?
O6 Mn2 O8 1_645 . 1_655 91.8(9) ?
O6 Mn2 O9 1_645 . . 170.3(7) ?
O6 Mn2 O10 1_645 . . 91.2(10) ?
O6 Mn2 O12 1_645 . . 81.4(9) ?
O8 Mn2 O9 1_655 . . 94.7(9) ?
O8 Mn2 O10 1_655 . . 175.7(9) ?
O8 Mn2 O12 1_655 . . 90.3(9) ?
O9 Mn2 O10 . . . 82.0(9) ?
O9 Mn2 O12 . . . 91.3(9) ?
O10 Mn2 O12 . . . 87.2(9) ?
O10 C1 O12 . . 2_746 127(4) ?
O10 C1 H1c1 . . . 116.58 ?
O12 C1 H1c1 2_746 . . 116.58 ?
O6 C2 O11 . . . 127(3) ?
O6 C2 H1c2 . . . 116.31 ?
O11 C2 H1c2 . . . 116.31 ?
O1 C3 O7 . . . 132(3) ?
O1 C3 H1c3 . . . 113.78 ?
O7 C3 H1c3 . . . 113.78 ?
O3 C4 O8 . . . 130(3) ?
O3 C4 H1c4 . . . 114.98 ?
O8 C4 H1c4 . . . 114.98 ?
O5 C5 O9 . . . 125(3) ?
O5 C5 H1c5 . . . 117.53 ?
O9 C5 H1c5 . . . 117.53 ?
O2 C6 O4 2_647 . . 123(3) ?
O2 C6 H1c6 2_647 . . 118.7 ?
O4 C6 H1c6 . . . 118.7 ?
Mn2 O1 C3 1_565 . . 127.8(17) ?
Mn1 O2 C6 . . 2_657 164.6(18) ?
Mn1 O3 C4 . . . 132(2) ?
Mn1 O4 C6 . . . 117(2) ?
Mn1 O5 C5 . . . 125(2) ?
Mn2 O6 C2 1_465 . . 126(2) ?
Mn1 O7 C3 . . . 127.5(18) ?
Mn2 O8 C4 1_455 . . 125(2) ?
Mn2 O9 C5 . . . 137(2) ?
Mn2 O10 C1 . . . 158(2) ?
Mn1 O11 C2 . . . 128(2) ?
Mn2 O12 C1 . . 2_756 115(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_THETM01_AMnF_c2_p03         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A significant loss in resolution is observed in the second
high-pressure phase, therefore the integration was performed to a 
resolution limit of 1.0 A in order to reduce the risk of integrating
diamond peaks.
;
_vrf_PLAT027_AMnF_c2_p03         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      10.57 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT029_AMnF_c2_p03         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.830 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT201_AMnF_c2_p03         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         18 Report
RESPONSE: Due to the reduced quality of the data, isotropic thermal parameters
were preferred for the formate anions.
;
_vrf_PLAT902_AMnF_c2_p03         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_GOODF01_AMnF_c2_p03         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated even further after the 
second high-pressure phase transition, giving broader and 
lower resolution reflections. Six overlapping twin domains still 
coexist upon the transition, however the intensities of the six domains
were not equal and so three of the most intense domains were integrated
individually in CrysAlisPro and refined together in JANA.
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain, as well
as small residual intensity from another domain that was not taken into 
account in the refinement.
;
_vrf_PLAT043_AMnF_c2_p03         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     8.09 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT034_AMnF_c2_p03         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: The refinement of a Flack parameter would probably not be very
reliable given the quality of the data. A similar configuration to the 
ambient c2 structure is chosen.
;
_vrf_PLAT041_AMnF_c2_p03         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT082_AMnF_c2_p03         
;
PROBLEM: High R1 Value ..................................       0.14 Report
RESPONSE: The crystal quality deteriorated even further after the 
second high-pressure phase transition, giving broader and 
lower resolution reflections.
;
_vrf_PLAT157_AMnF_c2_p03         
;
PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg        89.98 Degree
RESPONSE: A setting was chosen that bears closest structural similarity
to the previous HP-II phase.
;
_vrf_PLAT242_AMnF_c2_p03         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Mn2 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT241_AMnF_c2_p03         
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O10 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT112_AMnF_c2_p03         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        21        100 %Fit  
RESPONSE: The P212121 space group was tested and could be used for
data integration and structure refinement. The data quality was not good enough
to distinguish between P21 and P212121 structural models. We chose the P21 
structure due to the Mossbauer data we obtained on AFeF-III that suggest 
two unique Fe environments in the HP-III phase, which is only compatible 
with the P21 structure. 
;
_vrf_PLAT113_AMnF_c2_p03         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      P212121 Check 
RESPONSE: The P212121 space group was tested and could be used for
data integration and structure refinement. The data quality was not good enough
to distinguish between P21 and P212121 structural models. We chose the P21 
structure due to the Mossbauer data we obtained on AFeF-III that suggest 
two unique Fe environments in the HP-III phase, which is only compatible 
with the P21 structure.   
;
_vrf_PLAT430_AMnF_c2_p03         
;
PROBLEM: Short Inter D...A Contact  O7       ..N2               2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AMnF_c2_p04
_database_code_depnum_ccdc_archive 'CCDC 1861339'
_audit_update_record             
;
2018-08-09 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
#=======================================================================

_audit_creation_method           'Jana2006 Version : 25/10/2015'

#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C6 H6 Mn2 O12, N2 H8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C6 H14 Mn2 N2 O12'
_chemical_formula_weight         416.1
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration ?

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z

_cell_length_a                   6.651(3)
_cell_length_b                   7.067(3)
_cell_length_c                   13.839(4)
_cell_angle_alpha                90
_cell_angle_beta                 89.96(3)
_cell_angle_gamma                90
_cell_volume                     650.5(4)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.240(7) 1 0 0 0 1 0 0 0 1
2 0.379(5) -1 0 -0.0975 0 -1 0 -0.02 0 1
3 0.380(5) 0.4617 0 1.8584 0 -1 0 0.4244 0 -0.4617

_cell_formula_units_Z            2

_cell_measurement_reflns_used    114
_cell_measurement_theta_min      1.96
_cell_measurement_theta_max      11.28
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.1242
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             404

_exptl_absorpt_coefficient_mu    0.43
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '1.98 GPa'
_diffrn_ambient_temperature      293
_diffrn_source                   synchrotron
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_wavelength     0.41111
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID15B beamline, ESRF'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'diamond-anvil cell'

_diffrn_reflns_number            1960
_diffrn_reflns_theta_min         1.7
_diffrn_reflns_theta_max         11.89
_diffrn_reflns_theta_full        8.26
_diffrn_measured_fraction_theta_max 0.81
_diffrn_measured_fraction_theta_full 0.84
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_reduction_process ?

_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?

_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             1960
_reflns_number_gt                1168
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1587
_refine_ls_wR_factor_gt          0.1768
_refine_ls_R_factor_all          0.2059
_refine_ls_wR_factor_ref         0.1856
_refine_ls_goodness_of_fit_ref   3.76
_refine_ls_goodness_of_fit_gt    4.69
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         1960
_refine_ls_number_parameters     87
_refine_ls_number_restraints     0
_refine_ls_number_constraints    49
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(F)+0.0001F²)
_refine_ls_hydrogen_treatment    constr
_refine_ls_shift/su_max          0.0425
_refine_ls_shift/su_mean         0.0086
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.45
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  730 of Friedel pairs used in the refinement
;
_refine_ls_abs_structure_Flack   ?
_refine_ls_abs_structure_Rogers  ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C -0.0001 0.0005 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Mn 0.1790 0.2615 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0018 0.0018 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
? ? ? ? ? ?

loop_
_restr_angle_atom_site_label_1
_restr_angle_site_symmetry_1
_restr_angle_atom_site_label_2
_restr_angle_site_symmetry_2
_restr_angle_atom_site_label_3
_restr_angle_site_symmetry_3
_restr_angle_target
_restr_angle_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_torsion_atom_site_label_1
_restr_torsion_site_symmetry_1
_restr_torsion_atom_site_label_2
_restr_torsion_site_symmetry_2
_restr_torsion_atom_site_label_3
_restr_torsion_site_symmetry_3
_restr_torsion_atom_site_label_4
_restr_torsion_site_symmetry_4
_restr_torsion_angle_target
_restr_torsion_weight_param
? ? ? ? ? ? ? ? ? ?

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_site_symmetry_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
? ? ? ? ? ?

loop_
_restr_equal_angle_atom_site_label_1
_restr_equal_angle_site_symmetry_1
_restr_equal_angle_atom_site_label_2
_restr_equal_angle_site_symmetry_2
_restr_equal_angle_atom_site_label_3
_restr_equal_angle_site_symmetry_3
_restr_equal_angle_class_class_id
_restr_equal_angle_class_target_weight_param
? ? ? ? ? ? ? ?

loop_
_restr_equal_torsion_atom_site_label_1
_restr_equal_torsion_site_symmetry_1
_restr_equal_torsion_atom_site_label_2
_restr_equal_torsion_site_symmetry_2
_restr_equal_torsion_atom_site_label_3
_restr_equal_torsion_site_symmetry_3
_restr_equal_torsion_atom_site_label_4
_restr_equal_torsion_site_symmetry_4
_restr_equal_torsion_class_class_id
_restr_equal_torsion_class_target_weight_param
? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.6355(8) 0.7099(9) 0.8505(3) Uani 0.0518(15) 2 1 d . . .
Mn2 Mn 1.1352(8) 0.2200(9) 0.6489(3) Uani 0.0518(15) 2 1 d . . .
C1 C 0.892(6) -0.139(6) 0.552(2) Uiso 0.062(4) 2 1 d . . .
C2 C 0.528(7) 1.009(7) 0.709(3) Uiso 0.085(6) 2 1 d . . .
C3 C 1.041(5) 0.906(5) 0.8000(19) Uiso 0.049(4) 2 1 d . . .
C4 C 0.240(6) 0.483(5) 0.8162(18) Uiso 0.056(4) 2 1 d . . .
C5 C 0.759(5) 0.445(5) 0.6856(18) Uiso 0.055(4) 2 1 d . . .
C6 C 0.618(6) 0.584(6) 1.046(2) Uiso 0.054(4) 2 1 d . . .
O1 O 1.068(3) 1.080(3) 0.7806(13) Uiso 0.049(4) 2 1 d . . .
O2 O 0.497(4) 0.949(4) 0.9306(13) Uiso 0.054(4) 2 1 d . . .
O3 O 0.357(4) 0.574(4) 0.8666(13) Uiso 0.056(4) 2 1 d . . .
O4 O 0.735(4) 0.592(3) 0.9872(14) Uiso 0.054(4) 2 1 d . . .
O5 O 0.782(3) 0.470(4) 0.7739(13) Uiso 0.055(4) 2 1 d . . .
O6 O 0.427(5) 1.083(5) 0.6316(16) Uiso 0.085(6) 2 1 d . . .
O7 O 0.928(3) 0.854(4) 0.8619(12) Uiso 0.049(4) 2 1 d . . .
O8 O 0.264(4) 0.457(4) 0.7242(13) Uiso 0.056(4) 2 1 d . . .
O9 O 0.848(3) 0.352(4) 0.6287(13) Uiso 0.055(4) 2 1 d . . .
O10 O 1.006(4) 0.000(4) 0.5665(14) Uiso 0.062(4) 2 1 d . . .
O11 O 0.564(5) 0.857(5) 0.7129(18) Uiso 0.085(6) 2 1 d . . .
O12 O 1.243(4) 0.341(4) 0.5075(15) Uiso 0.062(4) 2 1 d . . .
N1 N 0.634(4) 0.208(5) 0.4667(15) Uani 0.051(8) 2 1 d . . .
N2 N 0.122(4) 0.704(5) 1.0306(15) Uani 0.051(8) 2 1 d . . .
H1c1 H 0.914807 -0.246315 0.593338 Uiso 0.0746 2 1 d . . .
H1c2 H 0.568794 1.09138 0.760932 Uiso 0.1017 2 1 d . . .
H1c6 H 0.60277 0.696516 1.083716 Uiso 0.0642 2 1 d . . .
H1c5 H 0.648938 0.514821 0.658528 Uiso 0.0654 2 1 d . . .
H1c3 H 1.114067 0.81304 0.763668 Uiso 0.0582 2 1 d . . .
H1c4 H 0.124696 0.427067 0.846709 Uiso 0.0675 2 1 d . . .


loop_
_jana_atom_site_ADP_C_label
_jana_atom_site_ADP_C_type_symbol
_jana_atom_site_ADP_C_111
_jana_atom_site_ADP_C_112
_jana_atom_site_ADP_C_113
_jana_atom_site_ADP_C_122
_jana_atom_site_ADP_C_123
_jana_atom_site_ADP_C_133
_jana_atom_site_ADP_C_222
_jana_atom_site_ADP_C_223
_jana_atom_site_ADP_C_233
_jana_atom_site_ADP_C_333
? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_D_label
_jana_atom_site_ADP_D_type_symbol
_jana_atom_site_ADP_D_1111
_jana_atom_site_ADP_D_1112
_jana_atom_site_ADP_D_1113
_jana_atom_site_ADP_D_1122
_jana_atom_site_ADP_D_1123
_jana_atom_site_ADP_D_1133
_jana_atom_site_ADP_D_1222
_jana_atom_site_ADP_D_1223
_jana_atom_site_ADP_D_1233
_jana_atom_site_ADP_D_1333
_jana_atom_site_ADP_D_2222
_jana_atom_site_ADP_D_2223
_jana_atom_site_ADP_D_2233
_jana_atom_site_ADP_D_2333
_jana_atom_site_ADP_D_3333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_E_label
_jana_atom_site_ADP_E_type_symbol
_jana_atom_site_ADP_E_11111
_jana_atom_site_ADP_E_11112
_jana_atom_site_ADP_E_11113
_jana_atom_site_ADP_E_11122
_jana_atom_site_ADP_E_11123
_jana_atom_site_ADP_E_11133
_jana_atom_site_ADP_E_11222
_jana_atom_site_ADP_E_11223
_jana_atom_site_ADP_E_11233
_jana_atom_site_ADP_E_11333
_jana_atom_site_ADP_E_12222
_jana_atom_site_ADP_E_12223
_jana_atom_site_ADP_E_12233
_jana_atom_site_ADP_E_12333
_jana_atom_site_ADP_E_13333
_jana_atom_site_ADP_E_22222
_jana_atom_site_ADP_E_22223
_jana_atom_site_ADP_E_22233
_jana_atom_site_ADP_E_22333
_jana_atom_site_ADP_E_23333
_jana_atom_site_ADP_E_33333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?

loop_
_jana_atom_site_ADP_F_label
_jana_atom_site_ADP_F_type_symbol
_jana_atom_site_ADP_F_111111
_jana_atom_site_ADP_F_111112
_jana_atom_site_ADP_F_111113
_jana_atom_site_ADP_F_111122
_jana_atom_site_ADP_F_111123
_jana_atom_site_ADP_F_111133
_jana_atom_site_ADP_F_111222
_jana_atom_site_ADP_F_111223
_jana_atom_site_ADP_F_111233
_jana_atom_site_ADP_F_111333
_jana_atom_site_ADP_F_112222
_jana_atom_site_ADP_F_112223
_jana_atom_site_ADP_F_112233
_jana_atom_site_ADP_F_112333
_jana_atom_site_ADP_F_113333
_jana_atom_site_ADP_F_122222
_jana_atom_site_ADP_F_122223
_jana_atom_site_ADP_F_122233
_jana_atom_site_ADP_F_122333
_jana_atom_site_ADP_F_123333
_jana_atom_site_ADP_F_133333
_jana_atom_site_ADP_F_222222
_jana_atom_site_ADP_F_222223
_jana_atom_site_ADP_F_222233
_jana_atom_site_ADP_F_222333
_jana_atom_site_ADP_F_223333
_jana_atom_site_ADP_F_233333
_jana_atom_site_ADP_F_333333
? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ?


#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O2 . . 2.22(2) ?
Mn1 O3 . . 2.10(3) ?
Mn1 O4 . . 2.17(2) ?
Mn1 O5 . . 2.23(2) ?
Mn1 O7 . . 2.20(2) ?
Mn1 O11 . . 2.22(3) ?
Mn2 O1 . 1_545 2.12(2) ?
Mn2 O6 . 1_645 2.18(3) ?
Mn2 O8 . 1_655 2.15(2) ?
Mn2 O9 . . 2.15(2) ?
Mn2 O10 . . 2.11(3) ?
Mn2 O12 . . 2.25(2) ?
C1 O10 . . 1.26(5) ?
C1 O12 . 2_746 1.23(4) ?
C1 H1c1 . . 0.96 ?
C2 O6 . . 1.37(5) ?
C2 O11 . . 1.10(6) ?
C2 H1c2 . . 0.96 ?
C3 O1 . . 1.27(4) ?
C3 O7 . . 1.20(4) ?
C3 H1c3 . . 0.96 ?
C4 O3 . . 1.23(4) ?
C4 O8 . . 1.30(3) ?
C4 H1c4 . . 0.96 ?
C5 O5 . . 1.24(3) ?
C5 O9 . . 1.18(4) ?
C5 H1c5 . . 0.96 ?
C6 O2 . 2_647 1.26(5) ?
C6 O4 . . 1.13(4) ?
C6 H1c6 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Mn1 O3 . . . 86.0(9) ?
O2 Mn1 O4 . . . 89.0(8) ?
O2 Mn1 O5 . . . 178.1(8) ?
O2 Mn1 O7 . . . 88.7(9) ?
O2 Mn1 O11 . . . 89.0(10) ?
O3 Mn1 O4 . . . 90.1(9) ?
O3 Mn1 O5 . . . 95.0(9) ?
O3 Mn1 O7 . . . 169.8(7) ?
O3 Mn1 O11 . . . 96.7(10) ?
O4 Mn1 O5 . . . 89.4(8) ?
O4 Mn1 O7 . . . 81.1(8) ?
O4 Mn1 O11 . . . 172.8(11) ?
O5 Mn1 O7 . . . 90.0(9) ?
O5 Mn1 O11 . . . 92.4(10) ?
O7 Mn1 O11 . . . 91.9(10) ?
O1 Mn2 O6 1_545 . 1_645 94.2(9) ?
O1 Mn2 O8 1_545 . 1_655 91.7(8) ?
O1 Mn2 O9 1_545 . . 97.4(8) ?
O1 Mn2 O10 1_545 . . 92.0(9) ?
O1 Mn2 O12 1_545 . . 171.9(10) ?
O6 Mn2 O8 1_645 . 1_655 92.6(10) ?
O6 Mn2 O9 1_645 . . 166.2(8) ?
O6 Mn2 O10 1_645 . . 88.6(11) ?
O6 Mn2 O12 1_645 . . 77.9(10) ?
O8 Mn2 O9 1_655 . . 94.6(9) ?
O8 Mn2 O10 1_655 . . 176.0(9) ?
O8 Mn2 O12 1_655 . . 89.9(8) ?
O9 Mn2 O10 . . . 83.4(10) ?
O9 Mn2 O12 . . . 90.3(9) ?
O10 Mn2 O12 . . . 86.6(9) ?
O10 C1 O12 . . 2_746 130(4) ?
O10 C1 H1c1 . . . 115.2 ?
O12 C1 H1c1 2_746 . . 115.2 ?
O6 C2 O11 . . . 121(4) ?
O6 C2 H1c2 . . . 119.61 ?
O11 C2 H1c2 . . . 119.61 ?
O1 C3 O7 . . . 123(3) ?
O1 C3 H1c3 . . . 118.74 ?
O7 C3 H1c3 . . . 118.74 ?
O3 C4 O8 . . . 124(3) ?
O3 C4 H1c4 . . . 118.16 ?
O8 C4 H1c4 . . . 118.16 ?
O5 C5 O9 . . . 132(3) ?
O5 C5 H1c5 . . . 113.96 ?
O9 C5 H1c5 . . . 113.96 ?
O2 C6 O4 2_647 . . 130(4) ?
O2 C6 H1c6 2_647 . . 114.9 ?
O4 C6 H1c6 . . . 114.9 ?
Mn2 O1 C3 1_565 . . 131.5(18) ?
Mn1 O2 C6 . . 2_657 162(2) ?
Mn1 O3 C4 . . . 138(2) ?
Mn1 O4 C6 . . . 116(2) ?
Mn1 O5 C5 . . . 121(2) ?
Mn2 O6 C2 1_465 . . 121(2) ?
Mn1 O7 C3 . . . 130.3(19) ?
Mn2 O8 C4 1_455 . . 122(2) ?
Mn2 O9 C5 . . . 127(2) ?
Mn2 O10 C1 . . . 155(2) ?
Mn1 O11 C2 . . . 123(3) ?
Mn2 O12 C1 . . 2_756 113(2) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
? ? ? ? ? ? ? ? ? ? ?


# start Validation Reply Form
_vrf_THETM01_AMnF_c2_p04         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A significant loss in resolution is observed in the second
high-pressure phase, therefore the integration was performed to a 
resolution limit of 1.0 A in order to reduce the risk of integrating
diamond peaks.
;
_vrf_PLAT027_AMnF_c2_p04         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      8.26 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT029_AMnF_c2_p04         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.840 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT201_AMnF_c2_p04         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         18 Report
RESPONSE: Due to the reduced quality of the data, isotropic thermal parameters
were preferred for the formate anions.
;
_vrf_PLAT902_AMnF_c2_p04         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_GOODF01_AMnF_c2_p04         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated even further after the 
second high-pressure phase transition, giving broader and 
lower resolution reflections. Six overlapping twin domains still 
coexist upon the transition, however the intensities of the six domains
were not equal and so three of the most intense domains were integrated
individually in CrysAlisPro and refined together in JANA.
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain, as well
as small residual intensity from another domain that was not taken into 
account in the refinement.
;
_vrf_PLAT043_AMnF_c2_p04         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     8.09 Check 
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT034_AMnF_c2_p04         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: The refinement of a Flack parameter would probably not be very
reliable given the quality of the data. A similar configuration to the 
ambient c2 structure is chosen.
;
_vrf_PLAT041_AMnF_c2_p04         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT082_AMnF_c2_p04         
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: The crystal quality deteriorated even further after the 
second high-pressure phase transition, giving broader and 
lower resolution reflections.
;
_vrf_PLAT157_AMnF_c2_p04         
;
PROBLEM: Non-standard Monoclinic Beta Angle less 90 Deg        89.96 Degree
RESPONSE: A setting was chosen that bears closest structural similarity
to the previous HP-II phase.
;
_vrf_PLAT241_AMnF_c2_p04         
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O11 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT112_AMnF_c2_p04         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        21        100 %Fit  
RESPONSE: The P212121 space group was tested and could be used for
data integration and structure refinement. The data quality was not good enough
to distinguish between P21 and P212121 structural models. We chose the P21 
structure due to the Mossbauer data we obtained on AFeF-III that suggest 
two unique Fe environments in the HP-III phase, which is only compatible 
with the P21 structure.  
;
_vrf_PLAT113_AMnF_c2_p04         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      P212121 Check 
RESPONSE: The P212121 space group was tested and could be used for
data integration and structure refinement. The data quality was not good enough
to distinguish between P21 and P212121 structural models. We chose the P21 
structure due to the Mossbauer data we obtained on AFeF-III that suggest 
two unique Fe environments in the HP-III phase, which is only compatible 
with the P21 structure.  
;
_vrf_PLAT430_AMnF_c2_p04         
;
PROBLEM: Short Inter D...A Contact  O7       ..N2               2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
# end Validation Reply Form 

