# 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_AFeF_c4_p0
_database_code_depnum_ccdc_archive 'CCDC 1861340'
_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 Fe O6, N H4'
_chemical_formula_sum            'C3 H7 Fe N O6'
_chemical_formula_weight         208.95

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'
Fe Fe 0.1967 0.3056 '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                   7.3249(3)
_cell_length_b                   7.3249(3)
_cell_length_c                   8.3197(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     386.58(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    196
_cell_measurement_theta_min      2.3340
_cell_measurement_theta_max      15.3200

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_F_000             212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.429
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91035
_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            797
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.857
_diffrn_reflns_theta_max         20.263
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.571
_diffrn_measured_fraction_theta_full 0.868
_diffrn_reflns_Laue_measured_fraction_max 0.571
_diffrn_reflns_Laue_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.554
_diffrn_reflns_point_group_measured_fraction_full 0.901
_reflns_number_total             367
_reflns_number_gt                328
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.468
_reflns_Friedel_fraction_max     0.520
_reflns_Friedel_fraction_full    0.985

_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)+(0.0135P)²+0.0816P] 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   0.04(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         367
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_restrained_S_all      1.259
_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
Fe1 Fe 0.333333 0.666667 0.250000 0.0208(2) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.069(2) Uani 1 6 d DS T P . .
H2 H 1.087(11) 1.120(7) 0.182(5) 0.083 Uiso 0.6667 1 d D U P . .
O1 O 0.5864(3) 0.8918(3) 0.1042(3) 0.0328(5) Uani 1 1 d . U . . .
C1 C 0.5647(5) 1.000000 0.000000 0.0377(11) Uani 1 2 d S TU P . .
H1 H 0.437701 1.000002 -0.000001 0.045 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
Fe1 O1 2.1377(19) 12_565 ?
Fe1 O1 2.1377(19) 3_565 ?
Fe1 O1 2.1377(19) . ?
Fe1 O1 2.1377(19) 10_665 ?
Fe1 O1 2.1377(19) 2_665 ?
Fe1 O1 2.1377(19) 11 ?
O1 C1 1.237(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 Fe1 O1 96.18(12) 12_565 3_565 ?
O1 Fe1 O1 82.67(10) 12_565 . ?
O1 Fe1 O1 90.97(8) 3_565 . ?
O1 Fe1 O1 90.97(8) 12_565 10_665 ?
O1 Fe1 O1 82.67(10) 3_565 10_665 ?
O1 Fe1 O1 170.49(10) . 10_665 ?
O1 Fe1 O1 170.49(10) 12_565 2_665 ?
O1 Fe1 O1 90.97(8) 3_565 2_665 ?
O1 Fe1 O1 90.97(8) . 2_665 ?
O1 Fe1 O1 96.18(12) 10_665 2_665 ?
O1 Fe1 O1 90.97(8) 12_565 11 ?
O1 Fe1 O1 170.49(10) 3_565 11 ?
O1 Fe1 O1 96.18(12) . 11 ?
O1 Fe1 O1 90.97(8) 10_665 11 ?
O1 Fe1 O1 82.66(10) 2_665 11 ?
C1 O1 Fe1 123.5(2) . . ?
O1 C1 O1 126.7(4) 8_675 . ?

_refine_diff_density_max         0.209
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.058


# start Validation Reply Form
_vrf_PLAT029_AFeF_c4_p0          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.868 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_AFeF_c4_p0          
;
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_AFeF_c4_p0          
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         52 %     
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_AFeF_c4_p01
_database_code_depnum_ccdc_archive 'CCDC 1861341'
_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 Fe O6, N H4'
_chemical_formula_sum            'C3 H7 Fe N O6'
_chemical_formula_weight         208.95

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'
Fe Fe 0.1967 0.3056 '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                   7.31630(11)
_cell_length_b                   7.31630(11)
_cell_length_c                   8.31849(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     385.618(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    237
_cell_measurement_theta_min      1.8620
_cell_measurement_theta_max      17.4140

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_F_000             212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.430
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69710
_exptl_absorpt_correction_T_max  1.00000
_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_special_details   ?
_diffrn_ambient_pressure         '0.12 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            785
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.859
_diffrn_reflns_theta_max         20.287
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.565
_diffrn_measured_fraction_theta_full 0.861
_diffrn_reflns_Laue_measured_fraction_max 0.565
_diffrn_reflns_Laue_measured_fraction_full 0.861
_diffrn_reflns_point_group_measured_fraction_max 0.548
_diffrn_reflns_point_group_measured_fraction_full 0.896
_reflns_number_total             364
_reflns_number_gt                320
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.468
_reflns_Friedel_fraction_max     0.516
_reflns_Friedel_fraction_full    0.985

_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)+(0.0218P)²+0.1299P] 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 96 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.21(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         364
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0770
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_restrained_S_all      1.240
_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
Fe1 Fe 0.333333 0.666667 0.250000 0.0203(3) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.067(3) Uani 1 6 d DS T P . .
H2 H 1.099(12) 1.127(8) 0.180(6) 0.080 Uiso 0.6667 1 d D U P . .
O1 O 0.5868(4) 0.8919(4) 0.1046(3) 0.0332(6) Uani 1 1 d . U . . .
C1 C 0.5649(6) 1.000000 0.000000 0.0385(13) Uani 1 2 d S TU P . .
H1 H 0.437749 0.999997 0.000000 0.046 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
Fe1 O1 2.136(2) 11 ?
Fe1 O1 2.136(2) 2_665 ?
Fe1 O1 2.136(2) 10_665 ?
Fe1 O1 2.136(2) . ?
Fe1 O1 2.136(2) 3_565 ?
Fe1 O1 2.136(2) 12_565 ?
O1 C1 1.239(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 Fe1 O1 82.49(12) 11 2_665 ?
O1 Fe1 O1 91.07(10) 11 10_665 ?
O1 Fe1 O1 96.16(14) 2_665 10_665 ?
O1 Fe1 O1 96.16(14) 11 . ?
O1 Fe1 O1 91.07(10) 2_665 . ?
O1 Fe1 O1 170.38(12) 10_665 . ?
O1 Fe1 O1 170.38(12) 11 3_565 ?
O1 Fe1 O1 91.07(10) 2_665 3_565 ?
O1 Fe1 O1 82.49(12) 10_665 3_565 ?
O1 Fe1 O1 91.07(10) . 3_565 ?
O1 Fe1 O1 91.07(10) 11 12_565 ?
O1 Fe1 O1 170.38(12) 2_665 12_565 ?
O1 Fe1 O1 91.07(10) 10_665 12_565 ?
O1 Fe1 O1 82.49(12) . 12_565 ?
O1 Fe1 O1 96.16(14) 3_565 12_565 ?
C1 O1 Fe1 123.4(2) . . ?
O1 C1 O1 126.7(4) 8_675 . ?

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.065


# start Validation Reply Form
_vrf_PLAT029_AFeF_c4_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_AFeF_c4_p01         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         24 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_AFeF_c4_p01         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         52 %     
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_AFeF_c4_p02
_database_code_depnum_ccdc_archive 'CCDC 1861342'
_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 Fe O6, N H4'
_chemical_formula_sum            'C3 H7 Fe N O6'
_chemical_formula_weight         208.95

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'
Fe Fe 0.1967 0.3056 '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                   7.30440(13)
_cell_length_b                   7.30440(13)
_cell_length_c                   8.31833(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     384.358(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    221
_cell_measurement_theta_min      1.8620
_cell_measurement_theta_max      17.4310

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_F_000             212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.431
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  1.141
_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         '0.19 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            782
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.862
_diffrn_reflns_theta_max         20.320
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.565
_diffrn_measured_fraction_theta_full 0.867
_diffrn_reflns_Laue_measured_fraction_max 0.565
_diffrn_reflns_Laue_measured_fraction_full 0.867
_diffrn_reflns_point_group_measured_fraction_max 0.547
_diffrn_reflns_point_group_measured_fraction_full 0.900
_reflns_number_total             363
_reflns_number_gt                319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.464
_reflns_Friedel_fraction_max     0.511
_reflns_Friedel_fraction_full    0.985

_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)+(0.0234P)²+0.0033P] 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 96 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         363
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0723
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_restrained_S_all      1.255
_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
Fe1 Fe 0.333333 0.666667 0.250000 0.0207(3) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.067(2) Uani 1 6 d DS T P . .
H2 H 1.087(11) 1.116(7) 0.177(4) 0.081 Uiso 0.6667 1 d D U P . .
O1 O 0.5871(3) 0.8919(3) 0.1049(3) 0.0333(5) Uani 1 1 d . U . . .
C1 C 0.5649(6) 1.000000 0.000000 0.0391(11) Uani 1 2 d S TU P . .
H1 H 0.437598 0.999998 -0.000001 0.047 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
Fe1 O1 2.1330(19) 11 ?
Fe1 O1 2.1330(19) 2_665 ?
Fe1 O1 2.1330(19) 10_665 ?
Fe1 O1 2.1330(19) 3_565 ?
Fe1 O1 2.1330(19) 12_565 ?
Fe1 O1 2.1330(19) . ?
O1 C1 1.240(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 Fe1 O1 82.38(10) 11 2_665 ?
O1 Fe1 O1 91.13(8) 11 10_665 ?
O1 Fe1 O1 96.17(12) 2_665 10_665 ?
O1 Fe1 O1 170.31(11) 11 3_565 ?
O1 Fe1 O1 91.13(8) 2_665 3_565 ?
O1 Fe1 O1 82.38(10) 10_665 3_565 ?
O1 Fe1 O1 91.13(8) 11 12_565 ?
O1 Fe1 O1 170.31(11) 2_665 12_565 ?
O1 Fe1 O1 91.13(8) 10_665 12_565 ?
O1 Fe1 O1 96.17(12) 3_565 12_565 ?
O1 Fe1 O1 96.17(12) 11 . ?
O1 Fe1 O1 91.13(8) 2_665 . ?
O1 Fe1 O1 170.31(11) 10_665 . ?
O1 Fe1 O1 91.13(8) 3_565 . ?
O1 Fe1 O1 82.38(10) 12_565 . ?
C1 O1 Fe1 123.3(2) . . ?
O1 C1 O1 126.7(4) . 8_675 ?

_refine_diff_density_max         0.226
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.069


# start Validation Reply Form
_vrf_PLAT029_AFeF_c4_p02         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.867 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_AFeF_c4_p02         
;
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_AFeF_c4_p02         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         51 %     
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_AFeF_c4_p03
_database_code_depnum_ccdc_archive 'CCDC 1861343'
_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 Fe O6, N H4'
_chemical_formula_sum            'C3 H7 Fe N O6'
_chemical_formula_weight         208.95

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'
Fe Fe 0.1967 0.3056 '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                   7.29055(13)
_cell_length_b                   7.29055(13)
_cell_length_c                   8.32778(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     383.336(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    218
_cell_measurement_theta_min      1.8610
_cell_measurement_theta_max      16.6150

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_F_000             212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.432
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88129
_exptl_absorpt_correction_T_max  1.00000
_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_special_details   ?
_diffrn_ambient_pressure         '0.33 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            782
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.233
_diffrn_reflns_theta_max         20.357
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.556
_diffrn_measured_fraction_theta_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.556
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_point_group_measured_fraction_max 0.537
_diffrn_reflns_point_group_measured_fraction_full 0.882
_reflns_number_total             358
_reflns_number_gt                318
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.461
_reflns_Friedel_fraction_max     0.500
_reflns_Friedel_fraction_full    0.970

_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)+0.1311P] 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 94 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.17(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         358
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0541
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_restrained_S_all      1.200
_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
Fe1 Fe 0.333333 0.666667 0.250000 0.0221(3) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.068(3) Uani 1 6 d DS T P . .
H2 H 1.088(12) 1.120(7) 0.184(6) 0.082 Uiso 0.6667 1 d D U P . .
O1 O 0.5876(3) 0.8928(3) 0.1049(3) 0.0350(5) Uani 1 1 d . U . . .
C1 C 0.5654(6) 1.000000 0.000000 0.0437(12) Uani 1 2 d S TU P . .
H1 H 0.437871 0.999995 -0.000001 0.052 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
Fe1 O1 2.135(2) 11 ?
Fe1 O1 2.135(2) 2_665 ?
Fe1 O1 2.135(2) . ?
Fe1 O1 2.135(2) 10_665 ?
Fe1 O1 2.135(2) 12_565 ?
Fe1 O1 2.135(2) 3_565 ?
O1 C1 1.236(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 Fe1 O1 82.47(11) 11 2_665 ?
O1 Fe1 O1 96.08(12) 11 . ?
O1 Fe1 O1 91.12(9) 2_665 . ?
O1 Fe1 O1 91.12(9) 11 10_665 ?
O1 Fe1 O1 96.08(12) 2_665 10_665 ?
O1 Fe1 O1 170.43(11) . 10_665 ?
O1 Fe1 O1 91.12(9) 11 12_565 ?
O1 Fe1 O1 170.44(11) 2_665 12_565 ?
O1 Fe1 O1 82.47(11) . 12_565 ?
O1 Fe1 O1 91.12(9) 10_665 12_565 ?
O1 Fe1 O1 170.44(11) 11 3_565 ?
O1 Fe1 O1 91.12(9) 2_665 3_565 ?
O1 Fe1 O1 91.12(9) . 3_565 ?
O1 Fe1 O1 82.47(11) 10_665 3_565 ?
O1 Fe1 O1 96.08(12) 12_565 3_565 ?
C1 O1 Fe1 123.4(2) . . ?
O1 C1 O1 126.9(4) 8_675 . ?

_refine_diff_density_max         0.196
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.054


# start Validation Reply Form
_vrf_PLAT029_AFeF_c4_p03         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.849 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_AFeF_c4_p03         
;
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_AFeF_c4_p03         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         50 %     
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_AFeF_c4_p04
_database_code_depnum_ccdc_archive 'CCDC 1861344'
_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 Fe O6, N H4'
_chemical_formula_sum            'C3 H7 Fe N O6'
_chemical_formula_weight         208.95

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'
Fe Fe 0.1967 0.3056 '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                   7.28439(16)
_cell_length_b                   7.28439(16)
_cell_length_c                   8.3359(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     383.062(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    217
_cell_measurement_theta_min      1.8640
_cell_measurement_theta_max      16.6220

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_F_000             212
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.433
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93672
_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         '0.42 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            780
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.235
_diffrn_reflns_theta_max         20.373
_diffrn_reflns_theta_full        14.280
_diffrn_measured_fraction_theta_max 0.556
_diffrn_measured_fraction_theta_full 0.843
_diffrn_reflns_Laue_measured_fraction_max 0.556
_diffrn_reflns_Laue_measured_fraction_full 0.843
_diffrn_reflns_point_group_measured_fraction_max 0.537
_diffrn_reflns_point_group_measured_fraction_full 0.878
_reflns_number_total             358
_reflns_number_gt                310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.461
_reflns_Friedel_fraction_max     0.500
_reflns_Friedel_fraction_full    0.969

_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)+(0.0130P)²+0.0545P] 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 92 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.12(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         358
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0570
_refine_ls_goodness_of_fit_ref   1.254
_refine_ls_restrained_S_all      1.251
_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
Fe1 Fe 0.333333 0.666667 0.250000 0.0232(3) Uani 1 6 d S T P . .
N1 N 1.000000 1.000000 0.250000 0.068(2) Uani 1 6 d DS T P . .
H2 H 1.079(13) 1.119(8) 0.176(5) 0.082 Uiso 0.6667 1 d D U P . .
O1 O 0.5875(3) 0.8931(4) 0.1051(3) 0.0366(5) Uani 1 1 d . U . . .
C1 C 0.5646(6) 1.000000 0.000000 0.0439(13) Uani 1 2 d S TU P . .
H1 H 0.436885 1.000000 -0.000001 0.053 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
Fe1 O1 2.134(2) . ?
Fe1 O1 2.134(2) 11 ?
Fe1 O1 2.134(2) 2_665 ?
Fe1 O1 2.134(2) 10_665 ?
Fe1 O1 2.134(2) 12_565 ?
Fe1 O1 2.134(2) 3_565 ?
O1 C1 1.238(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 Fe1 O1 95.98(14) . 11 ?
O1 Fe1 O1 91.10(9) . 2_665 ?
O1 Fe1 O1 82.57(12) 11 2_665 ?
O1 Fe1 O1 170.57(12) . 10_665 ?
O1 Fe1 O1 91.10(9) 11 10_665 ?
O1 Fe1 O1 95.98(14) 2_665 10_665 ?
O1 Fe1 O1 82.57(12) . 12_565 ?
O1 Fe1 O1 91.10(9) 11 12_565 ?
O1 Fe1 O1 170.57(12) 2_665 12_565 ?
O1 Fe1 O1 91.10(9) 10_665 12_565 ?
O1 Fe1 O1 91.11(9) . 3_565 ?
O1 Fe1 O1 170.57(12) 11 3_565 ?
O1 Fe1 O1 91.10(9) 2_665 3_565 ?
O1 Fe1 O1 82.57(12) 10_665 3_565 ?
O1 Fe1 O1 95.98(14) 12_565 3_565 ?
C1 O1 Fe1 123.3(2) . . ?
O1 C1 O1 126.5(4) 8_675 . ?

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.053



# start Validation Reply Form
_vrf_PLAT029_AFeF_c4_p04         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.843 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_AFeF_c4_p04         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         24 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_AFeF_c4_p04         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         50 %     
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_AFeF_c4_p05
_database_code_depnum_ccdc_archive 'CCDC 1861345'
_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 Fe O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 Fe1 N1 O6'
_chemical_formula_weight         208.9
_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                   6.8121(17)
_cell_length_b                   8.3238(9)
_cell_length_c                   7.3916(17)
_cell_angle_alpha                90
_cell_angle_beta                 117.39(3)
_cell_angle_gamma                90
_cell_volume                     372.14(17)

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 0.138(3) 1 0 0 0 1 0 0 0 1
2 0.1962(13) 1 0 0 0 -1 0 0.848 0 -1
3 0.1690(12) -0.0513 0 -1.0583 0 1 0 0.8989 0 -0.9487
4 0.1883(12) -0.9487 0 1.0583 0 -1 0 0.0944 0 0.9487
5 0.1057(9) -0.9487 0 1.0583 0 1 0 -0.8989 0 -0.0513
6 0.2025(14) -0.0513 0 -1.0583 0 -1 0 -0.9424 0 0.0513

_cell_formula_units_Z            2

_cell_measurement_reflns_used    239
_cell_measurement_theta_min      1.95
_cell_measurement_theta_max      14.48
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.8646
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             204

_exptl_absorpt_coefficient_mu    0.425
_exptl_crystal_description       block
_exptl_crystal_size_max          0.170
_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  0.921
_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         '0.59 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            4649
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         20.35
_diffrn_reflns_theta_full        11.77
_diffrn_measured_fraction_theta_max 0.6
_diffrn_measured_fraction_theta_full 0.94
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_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             4649
_reflns_number_gt                3566
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0781
_refine_ls_wR_factor_gt          0.0960
_refine_ls_R_factor_all          0.0925
_refine_ls_wR_factor_ref         0.0989
_refine_ls_goodness_of_fit_ref   2.92
_refine_ls_goodness_of_fit_gt    3.24
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         4649
_refine_ls_number_parameters     69
_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          0.0288
_refine_ls_shift/su_mean         0.0026
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  1176 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'
Fe 0.1967 0.3056 '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
Fe1 Fe 0.66119(14) 0.24965(11) 0.32236(11) Uani 0.0336(3) 2 1 d . . .
O1 O 0.8876(8) 0.1065(5) 0.5664(6) Uani 0.0456(13) 2 1 d . . .
O2 O 0.6099(8) 0.6075(5) 0.7033(7) Uani 0.0468(14) 2 1 d . . .
O3 O 0.6994(8) 0.1030(5) 0.1058(6) Uani 0.0440(14) 2 1 d . . .
O4 O 0.9053(8) 0.3922(5) 0.2959(7) Uani 0.0456(13) 2 1 d . . .
O5 O 0.6838(8) 0.3937(5) 0.5677(6) Uani 0.0468(14) 2 1 d . . .
O6 O 0.4059(7) 0.3981(6) 0.1048(6) Uani 0.0440(14) 2 1 d . . .
C1 C 1.0363(12) 0.4751(7) 0.4417(10) Uani 0.0456(13) 2 1 d . . .
C2 C 0.5988(12) 0.5273(7) 0.5582(10) Uani 0.0468(14) 2 1 d . . .
C3 C 0.4334(12) 0.4993(8) 0.0004(12) Uani 0.0440(14) 2 1 d . . .
N1 N -0.0247(9) 0.2488(11) -0.0480(8) Uani 0.052(2) 2 1 d . . .
H1c1 H 1.082648 0.431102 0.575302 Uiso 0.0547 2 1 d . . .
H1c2 H 0.516194 0.572888 0.424841 Uiso 0.0561 2 1 d . . .
H1c3 H 0.573738 0.498173 0.00145 Uiso 0.0528 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
? ? ? ? ? ?

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
? ? ? ? ? ? ? ?

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_AFeF_c4_p05         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      11.77 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_AFeF_c4_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_PLAT029_AFeF_c4_p05         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.940 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_AFeF_c4_p05         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       3.99 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_PLAT112_AFeF_c4_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_AFeF_c4_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_PLAT230_AFeF_c4_p05         
;
PROBLEM: Hirshfeld Test Diff for   O1       --C1_e      .       11.0 s.u.
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_PLAT250_AFeF_c4_p05         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.7 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_GOODF01_AFeF_c4_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_AFeF_c4_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 0.00(9), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_AFeF_c4_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_PLAT213_AFeF_c4_p05         
;
PROBLEM: Atom Fe1             has ADP max/min Ratio .....        3.8 oblate  
RESPONSE: The reason for the oblate thermal ellipsoid of Fe1 is not known.
Many different integrations and refinements were tested, but all gave the same
oblate thermal ellipsoid for Fe1. The reason could lie with the data collection 
(previous data on AFeF-II did not show this problem: CCDC 1501454). It is 
possible that the crytal was not as well centered and so as the DAC rotates 
different parts of the crystal are radiated. Due to the many domains, this 
could influence the intensities of peaks from each domain with the scanning 
angle. 
;
_vrf_PLAT430_AFeF_c4_p05         
;
PROBLEM: Short Inter D...A Contact  O3       ..N1               2.88 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_AFeF_c4_p12
_database_code_depnum_ccdc_archive 'CCDC 1861346'
_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 Fe2 O12, N2 H8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C6 H14 Fe2 N2 O12'
_chemical_formula_weight         417.9
_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                   6.5890(12)
_cell_length_b                   7.004(2)
_cell_length_c                   13.771(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.00(2)
_cell_angle_gamma                90
_cell_volume                     635.5(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 0.257 1 0 0 0 1 0 0 0 1
2 0.302 0.9911 0 -0.2787 0 -1 0 -0.0638 0 -0.9911
3 0.225 -0.5 0 -1.81 0 1 0 0.4144 0 -0.5
4 0.216 -0.611 0 -1.6545 0 -1 0 -0.3788 0 0.611

_cell_formula_units_Z            2

_cell_measurement_reflns_used    237
_cell_measurement_theta_min      1.88
_cell_measurement_theta_max      12.93
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.1837
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             408

_exptl_absorpt_coefficient_mu    0.497
_exptl_crystal_description       block
_exptl_crystal_size_max          0.170
_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  0.286
_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         '2.37 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            3453
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         13.26
_diffrn_reflns_theta_full        10.32
_diffrn_measured_fraction_theta_max 0.87
_diffrn_measured_fraction_theta_full 0.88
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_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             3453
_reflns_number_gt                1840
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1447
_refine_ls_wR_factor_gt          0.1689
_refine_ls_R_factor_all          0.2025
_refine_ls_wR_factor_ref         0.1751
_refine_ls_goodness_of_fit_ref   3.59
_refine_ls_goodness_of_fit_gt    4.78
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3453
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_number_constraints    38
_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          0.0448
_refine_ls_shift/su_mean         0.0092
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  967 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'
Fe 0.1967 0.3056 '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
Fe1 Fe 0.6351(5) 0.7132(7) 0.8502(2) Uani 0.0621(15) 2 1 d . . .
Fe2 Fe 1.1368(5) 1.2183(7) 0.6486(3) Uani 0.0593(14) 2 1 d . . .
O1 O 1.054(3) 1.092(3) 0.7754(13) Uiso 0.085(4) 2 1 d . . .
O2 O 0.509(3) 0.929(3) 0.9325(13) Uiso 0.091(4) 2 1 d . . .
O3 O 0.368(3) 0.586(3) 0.8560(13) Uiso 0.078(4) 2 1 d . . .
O4 O 0.729(4) 0.588(3) 0.9851(14) Uiso 0.091(4) 2 1 d . . .
O5 O 0.775(3) 0.486(3) 0.7796(13) Uiso 0.077(4) 2 1 d . . .
O6 O 0.418(4) 1.072(3) 0.6377(14) Uiso 0.096(5) 2 1 d . . .
O7 O 0.911(3) 0.864(3) 0.8563(14) Uiso 0.085(4) 2 1 d . . .
O8 O 0.280(3) 0.455(3) 0.7238(13) Uiso 0.078(4) 2 1 d . . .
O9 O 0.847(3) 0.337(3) 0.6355(13) Uiso 0.077(4) 2 1 d . . .
O10 O 1.005(4) 0.994(3) 0.5662(14) Uiso 0.100(5) 2 1 d . . .
O11 O 0.576(4) 0.868(4) 0.7224(15) Uiso 0.096(5) 2 1 d . . .
O12 O 1.220(4) 1.340(3) 0.5134(16) Uiso 0.100(5) 2 1 d . . .
N1 N 0.638(3) 0.217(5) 0.4667(16) Uiso 0.093(4) 2 1 d . . .
N2 N 1.144(3) 0.713(5) 1.0257(16) Uiso 0.093(4) 2 1 d . . .
C1 C 1.129(6) 1.371(5) 0.443(2) Uiso 0.100(5) 2 1 d . . .
C2 C 0.538(5) 1.025(5) 0.705(2) Uiso 0.096(5) 2 1 d . . .
C3 C 1.018(5) 0.928(5) 0.798(2) Uiso 0.085(4) 2 1 d . . .
C5 C 0.759(5) 0.460(4) 0.6915(19) Uiso 0.077(4) 2 1 d . . .
C6 C 0.618(5) 0.573(5) 1.045(2) Uiso 0.091(4) 2 1 d . . .
C4 C 0.238(5) 0.481(4) 0.8082(19) Uiso 0.078(4) 2 1 d . . .
H1c1 H 1.160238 1.294071 0.387405 Uiso 0.1199 2 1 d . . .
H1c2 H 0.599607 1.124176 0.74299 Uiso 0.1152 2 1 d . . .
H1c3 H 1.090276 0.835002 0.759911 Uiso 0.1023 2 1 d . . .
H1c5 H 0.666541 0.544332 0.659125 Uiso 0.0919 2 1 d . . .
H1c6 H 0.612678 0.68054 1.0887 Uiso 0.1087 2 1 d . . .
H1c4 H 0.118562 0.428592 0.837758 Uiso 0.094 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
Fe1 O2 . . 2.07(2) ?
Fe1 O3 . . 1.97(2) ?
Fe1 O5 . . 2.080(19) ?
Fe1 O7 . . 2.11(2) ?
Fe1 O11 . . 2.10(2) ?
Fe2 O1 . . 2.03(2) ?
Fe2 O6 . 1_655 2.12(2) ?
Fe2 O9 . 1_565 2.09(2) ?
Fe2 O10 . . 2.12(2) ?
Fe2 O12 . . 2.12(2) ?
O1 C3 . . 1.21(4) ?
O2 C6 . 2_657 1.35(4) ?
O3 C4 . . 1.31(4) ?
O4 C6 . . 1.11(4) ?
O5 C5 . . 1.23(3) ?
O6 C2 . . 1.26(4) ?
O7 C3 . . 1.16(4) ?
O8 C4 . . 1.21(3) ?
O9 C5 . . 1.29(3) ?
O10 C1 . 2_746 1.24(4) ?
O11 C2 . . 1.16(5) ?
O12 C1 . . 1.16(4) ?
C1 H1c1 . . 0.96 ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?
C5 H1c5 . . 0.96 ?
C6 H1c6 . . 0.96 ?
C4 H1c4 . . 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 Fe1 O3 . . . 87.2(8) ?
O2 Fe1 O5 . . . 174.4(8) ?
O2 Fe1 O7 . . . 87.6(9) ?
O2 Fe1 O11 . . . 90.4(9) ?
O3 Fe1 O5 . . . 93.9(8) ?
O3 Fe1 O7 . . . 174.4(8) ?
O3 Fe1 O11 . . . 95.9(9) ?
O5 Fe1 O7 . . . 91.1(8) ?
O5 Fe1 O11 . . . 94.9(8) ?
O7 Fe1 O11 . . . 86.3(9) ?
O1 Fe2 O6 . . 1_655 94.8(9) ?
O1 Fe2 O9 . . 1_565 90.2(8) ?
O1 Fe2 O10 . . . 91.6(8) ?
O1 Fe2 O12 . . . 177.8(9) ?
O6 Fe2 O9 1_655 . 1_565 169.4(8) ?
O6 Fe2 O10 1_655 . . 87.7(9) ?
O6 Fe2 O12 1_655 . . 84.7(9) ?
O9 Fe2 O10 1_565 . . 82.8(9) ?
O9 Fe2 O12 1_565 . . 90.0(9) ?
O10 Fe2 O12 . . . 86.2(8) ?
Fe2 O1 C3 . . . 133.0(19) ?
Fe1 O2 C6 . . 2_657 157.4(19) ?
Fe1 O3 C4 . . . 144.9(18) ?
Fe1 O5 C5 . . . 122.4(18) ?
Fe2 O6 C2 1_455 . . 128(2) ?
Fe1 O7 C3 . . . 134(2) ?
Fe2 O9 C5 1_545 . . 128.5(18) ?
Fe2 O10 C1 . . 2_746 149(2) ?
Fe1 O11 C2 . . . 135(2) ?
Fe2 O12 C1 . . . 132(3) ?
O10 C1 O12 2_756 . . 126(3) ?
O10 C1 H1c1 2_756 . . 117.17 ?
O12 C1 H1c1 . . . 117.17 ?
O6 C2 O11 . . . 122(3) ?
O6 C2 H1c2 . . . 118.75 ?
O11 C2 H1c2 . . . 118.76 ?
O1 C3 O7 . . . 131(3) ?
O1 C3 H1c3 . . . 114.27 ?
O7 C3 H1c3 . . . 114.27 ?
O5 C5 O9 . . . 130(3) ?
O5 C5 H1c5 . . . 114.82 ?
O9 C5 H1c5 . . . 114.82 ?
O2 C6 O4 2_647 . . 130(3) ?
O2 C6 H1c6 2_647 . . 114.75 ?
O4 C6 H1c6 . . . 114.75 ?
O3 C4 O8 . . . 115(3) ?
O3 C4 H1c4 . . . 122.64 ?
O8 C4 H1c4 . . . 122.64 ?

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
C1 H1c1 O11 . . 2_756 0.96 2.36 2.99(4) 123.25 ?
C5 H1c5 O11 . . . 0.96 2.50 3.13(4) 123.28 ?
C4 H1c4 O5 . . 1_455 0.96 2.43 3.08(4) 124.08 ?



# start Validation Reply Form
_vrf_THETM01_AFeF_c4_p12         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: A significant loss in resolution is observed in the second
high-pressure phase, therefore the integration was performed to a 
resolution limit of 0.9 A in order to reduce the risk of integrating
diamond peaks.
;
_vrf_PLAT027_AFeF_c4_p12         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      10.32 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT029_AFeF_c4_p12         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.880 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT902_AFeF_c4_p12         
;
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_AFeF_c4_p12         
;
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 four 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_AFeF_c4_p12         
;
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_AFeF_c4_p12         
;
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 
previous AFeF-II structure is chosen.
;
_vrf_PLAT041_AFeF_c4_p12         
;
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_AFeF_c4_p12         
;
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_PLAT201_AFeF_c4_p12         
;
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_PLAT202_AFeF_c4_p12         
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          2 Check 
RESPONSE: Due to the reduced quality of the data, isotropic thermal parameters
were preferred for the nitrogen atoms of the ammonium cations.
;
_vrf_PLAT241_AFeF_c4_p12         
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O1 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT242_AFeF_c4_p12         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Fe1 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT112_AFeF_c4_p12         
;
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_AFeF_c4_p12         
;
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_PLAT181_AFeF_c4_p12         
;
PROBLEM: All Angles Exactly 90 Degrees in Monoclinic Cell     Please Check
RESPONSE: The beta angle is very close to 90, but due to the broad 
diffraction spots, it is not possible to ascertain which cell (monoclinic
or orthorhombic) is best represented by the data. See the ADDSYM response 
for the choice of P21 over P212121.
;
_vrf_SYMMS02_AFeF_c4_p12         
;
PROBLEM:  All angles should not be 90 for a monoclinic cell
RESPONSE: The beta angle is very close to 90, but due to the broad 
diffraction spots, it is not possible to ascertain which cell (monoclinic
or orthorhombic) is best represented by the data. See the ADDSYM response 
for the choice of P21 over P212121.
;
_vrf_PLAT430_AFeF_c4_p12         
;
PROBLEM: Short Inter D...A Contact  O3       ..N2               2.83 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_AFeF_c4_p13
_database_code_depnum_ccdc_archive 'CCDC 1861347'
_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 Fe2 O12, N2 H8'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C6 H14 Fe2 N2 O12'
_chemical_formula_weight         417.9
_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                   6.599(5)
_cell_length_b                   6.957(5)
_cell_length_c                   13.695(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.19(7)
_cell_angle_gamma                90
_cell_volume                     628.7(8)

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 0.259(5) 1 0 0 0 1 0 0 0 1
2 0.287(3) 0.9914 0 -0.2788 0 -1 0 -0.0616 0 -0.9914
3 0.231(3) -0.4971 0 -1.7973 0 1 0 0.4173 0 -0.5029
4 0.223(3) -0.6092 0 -1.6416 0 -1 0 -0.3831 0 0.6093

_cell_formula_units_Z            2

_cell_measurement_reflns_used    124
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      12.07
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.2073
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             408

_exptl_absorpt_coefficient_mu    0.503
_exptl_crystal_description       block
_exptl_crystal_size_max          0.170
_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  0.736
_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         '2.55 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            3407
_diffrn_reflns_theta_min         1.9
_diffrn_reflns_theta_max         13.21
_diffrn_reflns_theta_full        12.13
_diffrn_measured_fraction_theta_max 0.88
_diffrn_measured_fraction_theta_full 0.88
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_unetI/netI     0.116
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_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             3407
_reflns_number_gt                1174
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1408
_refine_ls_wR_factor_gt          0.1638
_refine_ls_R_factor_all          0.2354
_refine_ls_wR_factor_ref         0.1765
_refine_ls_goodness_of_fit_ref   2.37
_refine_ls_goodness_of_fit_gt    3.80
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3407
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_number_constraints    38
_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          0.0229
_refine_ls_shift/su_mean         0.0045
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  956 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'
Fe 0.1967 0.3056 '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
Fe1 Fe 0.6347(6) 0.7162(7) 0.8496(3) Uani 0.0893(18) 2 1 d . . .
Fe2 Fe 1.1361(6) 1.2149(7) 0.6481(3) Uani 0.0861(17) 2 1 d . . .
O1 O 1.051(4) 1.082(4) 0.7764(15) Uiso 0.109(5) 2 1 d . . .
O2 O 0.515(4) 0.927(3) 0.9376(16) Uiso 0.126(5) 2 1 d . . .
O3 O 0.355(3) 0.591(3) 0.8548(14) Uiso 0.094(4) 2 1 d . . .
O4 O 0.729(4) 0.588(3) 0.9890(16) Uiso 0.126(5) 2 1 d . . .
O5 O 0.755(3) 0.489(3) 0.7844(17) Uiso 0.114(5) 2 1 d . . .
O6 O 0.431(4) 1.080(4) 0.6380(19) Uiso 0.135(6) 2 1 d . . .
O7 O 0.896(3) 0.880(3) 0.8613(16) Uiso 0.109(5) 2 1 d . . .
O8 O 0.284(3) 0.444(3) 0.7213(15) Uiso 0.094(4) 2 1 d . . .
O9 O 0.855(4) 0.337(3) 0.6349(16) Uiso 0.114(5) 2 1 d . . .
O10 O 0.999(4) 0.992(3) 0.5634(16) Uiso 0.119(5) 2 1 d . . .
O11 O 0.569(4) 0.850(4) 0.7234(18) Uiso 0.135(6) 2 1 d . . .
O12 O 1.225(4) 1.342(3) 0.5197(17) Uiso 0.119(5) 2 1 d . . .
N1 N 0.624(3) 0.214(5) 0.4711(18) Uiso 0.120(5) 2 1 d . . .
N2 N 1.116(4) 0.738(5) 1.033(2) Uiso 0.120(5) 2 1 d . . .
C1 C 1.128(6) 1.373(6) 0.456(3) Uiso 0.119(5) 2 1 d . . .
C2 C 0.518(6) 1.013(7) 0.704(3) Uiso 0.135(6) 2 1 d . . .
C3 C 1.019(5) 0.929(5) 0.798(2) Uiso 0.109(5) 2 1 d . . .
C5 C 0.763(5) 0.462(5) 0.688(2) Uiso 0.114(5) 2 1 d . . .
C6 C 0.410(6) 1.068(6) 0.947(3) Uiso 0.126(5) 2 1 d . . .
C4 C 0.234(5) 0.485(4) 0.805(2) Uiso 0.094(4) 2 1 d . . .
H1c1 H 1.150899 1.285625 0.402819 Uiso 0.143 2 1 d . . .
H1c2 H 0.557782 1.105787 0.752469 Uiso 0.1623 2 1 d . . .
H1c3 H 1.092641 0.829078 0.764923 Uiso 0.1305 2 1 d . . .
H1c5 H 0.685749 0.55328 0.650862 Uiso 0.137 2 1 d . . .
H1c6 H 0.43231 1.173079 0.903062 Uiso 0.1507 2 1 d . . .
H1c4 H 0.108899 0.439631 0.832541 Uiso 0.1128 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
Fe1 O2 . . 2.06(2) ?
Fe1 O3 . . 2.04(2) ?
Fe1 O5 . . 1.98(2) ?
Fe1 O7 . . 2.07(2) ?
Fe1 O11 . . 2.01(3) ?
Fe2 O1 . . 2.06(2) ?
Fe2 O8 . 1_665 2.12(2) ?
Fe2 O9 . 1_565 2.05(2) ?
Fe2 O10 . . 2.14(2) ?
Fe2 O12 . . 2.05(2) ?
O1 C3 . . 1.13(4) ?
O2 C6 . . 1.21(5) ?
O3 C4 . . 1.28(4) ?
O4 C6 . 2_647 1.27(4) ?
O5 C5 . . 1.34(4) ?
O6 C2 . . 1.17(5) ?
O7 C3 . . 1.24(4) ?
O8 C4 . . 1.23(3) ?
O9 C5 . . 1.29(4) ?
O10 C1 . 2_746 1.21(4) ?
O11 C2 . . 1.21(5) ?
O12 C1 . . 1.10(4) ?
C1 H1c1 . . 0.96 ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?
C5 H1c5 . . 0.96 ?
C6 H1c6 . . 0.96 ?
C4 H1c4 . . 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 Fe1 O3 . . . 86.2(9) ?
O2 Fe1 O5 . . . 170.8(9) ?
O2 Fe1 O7 . . . 83.3(9) ?
O2 Fe1 O11 . . . 95.3(10) ?
O3 Fe1 O5 . . . 92.3(9) ?
O3 Fe1 O7 . . . 169.5(9) ?
O3 Fe1 O11 . . . 92.0(10) ?
O5 Fe1 O7 . . . 98.0(9) ?
O5 Fe1 O11 . . . 93.9(10) ?
O7 Fe1 O11 . . . 89.4(10) ?
O1 Fe2 O8 . . 1_665 93.5(9) ?
O1 Fe2 O9 . . 1_565 90.6(9) ?
O1 Fe2 O10 . . . 91.2(9) ?
O1 Fe2 O12 . . . 178.7(9) ?
O8 Fe2 O9 1_665 . 1_565 98.3(8) ?
O8 Fe2 O10 1_665 . . 175.2(8) ?
O8 Fe2 O12 1_665 . . 87.2(8) ?
O9 Fe2 O10 1_565 . . 82.4(9) ?
O9 Fe2 O12 1_565 . . 90.4(9) ?
O10 Fe2 O12 . . . 88.1(9) ?
Fe2 O1 C3 . . . 134(2) ?
Fe1 O2 C6 . . . 150(2) ?
Fe1 O3 C4 . . . 142.0(19) ?
Fe1 O5 C5 . . . 125(2) ?
Fe1 O7 C3 . . . 130(2) ?
Fe2 O8 C4 1_445 . . 119.5(19) ?
Fe2 O9 C5 1_545 . . 131(2) ?
Fe2 O10 C1 . . 2_746 156(2) ?
Fe1 O11 C2 . . . 133(3) ?
Fe2 O12 C1 . . . 127(3) ?
O10 C1 O12 2_756 . . 135(4) ?
O10 C1 H1c1 2_756 . . 112.36 ?
O12 C1 H1c1 . . . 112.36 ?
O6 C2 O11 . . . 132(4) ?
O6 C2 H1c2 . . . 113.81 ?
O11 C2 H1c2 . . . 113.81 ?
O1 C3 O7 . . . 125(3) ?
O1 C3 H1c3 . . . 117.71 ?
O7 C3 H1c3 . . . 117.71 ?
O5 C5 O9 . . . 133(3) ?
O5 C5 H1c5 . . . 113.7 ?
O9 C5 H1c5 . . . 113.7 ?
O2 C6 O4 . . 2_657 125(4) ?
O2 C6 H1c6 . . . 117.38 ?
O4 C6 H1c6 2_657 . . 117.38 ?
O3 C4 O8 . . . 118(3) ?
O3 C4 H1c4 . . . 121.24 ?
O8 C4 H1c4 . . . 121.24 ?

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
C5 H1c5 O11 . . . 0.96 2.42 3.03(4) 121.30 ?
C4 H1c4 O5 . . 1_455 0.96 2.45 3.17(4) 131.90 ?



# start Validation Reply Form
_vrf_THETM01_AFeF_c4_p13         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: A significant loss in resolution is observed in the second
high-pressure phase, therefore the integration was performed to a 
resolution limit of 0.9 A in order to reduce the risk of integrating
diamond peaks.
;
_vrf_PLAT027_AFeF_c4_p13         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      12.13 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT029_AFeF_c4_p13         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.880 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT902_AFeF_c4_p13         
;
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_AFeF_c4_p13         
;
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 four 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_AFeF_c4_p13         
;
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_AFeF_c4_p13         
;
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 
previous AFeF-II structure is chosen.
;
_vrf_PLAT041_AFeF_c4_p13         
;
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_AFeF_c4_p13         
;
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_PLAT201_AFeF_c4_p13         
;
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_PLAT202_AFeF_c4_p13         
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          2 Check 
RESPONSE: Due to the reduced quality of the data, isotropic thermal parameters
were preferred for the nitrogen atoms of the ammonium cations.
;
_vrf_PLAT241_AFeF_c4_p13         
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O1 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT242_AFeF_c4_p13         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Fe1 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT112_AFeF_c4_p13         
;
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_AFeF_c4_p13         
;
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_PLAT149_AFeF_c4_p13         
;
PROBLEM: s.u. on the   beta    Angle is Too Large .......       0.07 Degree
RESPONSE: The large error arises from the broad diffraction spots.
;
_vrf_PLAT430_AFeF_c4_p13         
;
PROBLEM: Short Inter D...A Contact  O4       ..N2               2.66 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_AFeF_c3_p01
_database_code_depnum_ccdc_archive 'CCDC 1861348'
_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         'C6 H6 Fe2 O12, N2 H8'
_chemical_formula_sum            'C6 H14 Fe2 N2 O12'
_chemical_formula_weight         417.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0010 0.0002 '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 -0.0010 0.0005 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0009 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1071 0.1589 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   6.558(6)
_cell_length_b                   6.9977(19)
_cell_length_c                   13.697(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.05(5)
_cell_angle_gamma                90
_cell_volume                     628.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    183
_cell_measurement_theta_min      1.7310
_cell_measurement_theta_max      8.4640

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.208
_exptl_crystal_F_000             408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.224
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_T_max  1.792
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_pressure         '2.8 GPa'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.29464
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'P02.2 beamline, DESY'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            984
_diffrn_reflns_av_unetI/netI     0.1312
_diffrn_reflns_av_R_equivalents  ?
_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_theta_min         1.725
_diffrn_reflns_theta_max         8.463
_diffrn_reflns_theta_full        8.463
_diffrn_measured_fraction_theta_max 0.686
_diffrn_measured_fraction_theta_full 0.686
_diffrn_reflns_Laue_measured_fraction_max 0.686
_diffrn_reflns_Laue_measured_fraction_full 0.686
_diffrn_reflns_point_group_measured_fraction_max 0.660
_diffrn_reflns_point_group_measured_fraction_full 0.660
_reflns_number_total             984
_reflns_number_gt                504
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.739
_reflns_Friedel_fraction_max     0.628
_reflns_Friedel_fraction_full    0.628

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_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          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   1.8(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         984
_refine_ls_number_parameters     71
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1675
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.2461
_refine_ls_wR_factor_gt          0.2026
_refine_ls_goodness_of_fit_ref   1.311
_refine_ls_restrained_S_all      1.310
_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
Fe1 Fe 0.6380(13) 0.7141(12) 0.8522(5) 0.047(2) Uiso 1 1 d . . . . .
Fe2 Fe 1.1355(12) 1.2193(11) 0.6481(5) 0.044(2) Uiso 1 1 d . . . . .
O1 O 1.072(8) 1.087(5) 0.782(3) 0.066(3) Uiso 1 1 d . U . . .
O2 O 0.507(8) 0.939(4) 0.935(3) 0.066(3) Uiso 1 1 d . U . . .
O3 O 0.349(8) 0.587(5) 0.863(3) 0.066(3) Uiso 1 1 d . U . . .
O4 O 0.722(8) 0.601(5) 0.980(3) 0.066(3) Uiso 1 1 d . U . . .
O5 O 0.766(8) 0.476(5) 0.788(3) 0.066(3) Uiso 1 1 d . U . . .
O6 O 0.417(7) 1.082(6) 0.640(3) 0.066(3) Uiso 1 1 d . U . . .
O7 O 0.921(8) 0.845(6) 0.860(3) 0.066(3) Uiso 1 1 d . U . . .
O8 O 0.275(8) 0.446(5) 0.725(4) 0.066(3) Uiso 1 1 d . U . . .
O9 O 0.852(8) 0.342(5) 0.635(3) 0.066(3) Uiso 1 1 d . U . . .
O10 O 0.995(7) 1.004(4) 0.572(3) 0.066(3) Uiso 1 1 d . U . . .
O11 O 0.561(7) 0.844(5) 0.715(3) 0.066(3) Uiso 1 1 d . U . . .
O12 O 1.220(8) 1.335(4) 0.510(3) 0.066(3) Uiso 1 1 d . U . . .
C1 C 1.100(10) 1.350(9) 0.448(5) 0.066(3) Uiso 1 1 d . U . . .
H1C1 H 1.071029 1.241955 0.411506 0.079 Uiso 1 1 calc R U . . .
C2 C 0.528(11) 1.017(8) 0.712(5) 0.066(3) Uiso 1 1 d . U . . .
H1C2 H 0.581223 1.099103 0.758873 0.079 Uiso 1 1 calc R U . . .
C3 C 1.042(12) 0.920(8) 0.800(5) 0.066(3) Uiso 1 1 d . U . . .
H1C3 H 1.119309 0.834379 0.763237 0.066(3) Uiso 1 1 calc R U . . .
C5 C 0.758(12) 0.451(7) 0.695(5) 0.066(3) Uiso 1 1 d . U . . .
H1C5 H 0.662292 0.529554 0.665328 0.079 Uiso 1 1 calc R U . . .
C6 C 0.379(11) 1.086(9) 0.947(5) 0.066(3) Uiso 1 1 d . U . . .
H1C6 H 0.368818 1.178374 0.898685 0.079 Uiso 1 1 calc R U . . .
C4 C 0.251(12) 0.481(7) 0.811(5) 0.066(3) Uiso 1 1 d . U . . .
H1C4 H 0.142426 0.419354 0.841528 0.079 Uiso 1 1 calc R U . . .
N1 N 0.629(7) 0.205(7) 0.460(3) 0.066(3) Uiso 1 1 d . U . . .
N2 N 0.133(7) 0.708(7) 1.027(3) 0.066(3) Uiso 1 1 d . U . . .

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O4 1.99(4) . ?
Fe1 O5 2.06(4) . ?
Fe1 O7 2.07(5) . ?
Fe1 O3 2.10(5) . ?
Fe1 O2 2.13(4) . ?
Fe1 O11 2.14(4) . ?
Fe2 O10 2.05(4) . ?
Fe2 O9 2.05(5) 1_565 ?
Fe2 O6 2.09(5) 1_655 ?
Fe2 O1 2.10(4) . ?
Fe2 O8 2.11(4) 1_665 ?
Fe2 O12 2.13(4) . ?
O1 C3 1.21(5) . ?
O2 C6 1.33(6) . ?
O3 C4 1.21(7) . ?
O4 C6 1.21(7) 2_647 ?
O5 C5 1.28(7) . ?
O6 C2 1.30(6) . ?
O7 C3 1.27(8) . ?
O8 C4 1.23(7) . ?
O9 C5 1.29(7) . ?
O10 C1 1.28(6) 2_746 ?
O11 C2 1.23(5) . ?
O12 C1 1.15(8) . ?

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
O4 Fe1 O5 86.4(17) . . ?
O4 Fe1 O7 83.2(19) . . ?
O5 Fe1 O7 91(2) . . ?
O4 Fe1 O3 91.0(19) . . ?
O5 Fe1 O3 93.2(19) . . ?
O7 Fe1 O3 172.7(18) . . ?
O4 Fe1 O2 86.5(18) . . ?
O5 Fe1 O2 172.6(17) . . ?
O7 Fe1 O2 90.4(19) . . ?
O3 Fe1 O2 84.9(19) . . ?
O4 Fe1 O11 177(2) . . ?
O5 Fe1 O11 93.9(15) . . ?
O7 Fe1 O11 94.0(17) . . ?
O3 Fe1 O11 91.8(16) . . ?
O2 Fe1 O11 93.4(16) . . ?
O10 Fe2 O9 81.7(18) . 1_565 ?
O10 Fe2 O6 91.9(17) . 1_655 ?
O9 Fe2 O6 171.5(17) 1_565 1_655 ?
O10 Fe2 O1 91.7(16) . . ?
O9 Fe2 O1 94.7(18) 1_565 . ?
O6 Fe2 O1 91.0(18) 1_655 . ?
O10 Fe2 O8 178.6(17) . 1_665 ?
O9 Fe2 O8 97.1(19) 1_565 1_665 ?
O6 Fe2 O8 89(2) 1_655 1_665 ?
O1 Fe2 O8 89.1(18) . 1_665 ?
O10 Fe2 O12 86.9(18) . . ?
O9 Fe2 O12 90.0(18) 1_565 . ?
O6 Fe2 O12 84.1(17) 1_655 . ?
O1 Fe2 O12 174.9(17) . . ?
O8 Fe2 O12 92.4(17) 1_665 . ?
C3 O1 Fe2 129(4) . . ?
C6 O2 Fe1 153(4) . . ?
C4 O3 Fe1 134(5) . . ?
C6 O4 Fe1 127(4) 2_647 . ?
C5 O5 Fe1 121(4) . . ?
C2 O6 Fe2 128(4) . 1_455 ?
C3 O7 Fe1 135(4) . . ?
C4 O8 Fe2 125(4) . 1_445 ?
C5 O9 Fe2 129(4) . 1_545 ?
C1 O10 Fe2 162(4) 2_746 . ?
C2 O11 Fe1 120(4) . . ?
C1 O12 Fe2 120(5) . . ?
O12 C1 O10 125(6) . 2_756 ?
O11 C2 O6 118(6) . . ?
O1 C3 O7 129(7) . . ?
O5 C5 O9 134(6) . . ?
O4 C6 O2 121(6) 2_657 . ?
O3 C4 O8 128(7) . . ?

_refine_diff_density_max         0.995
_refine_diff_density_min         -1.006
_refine_diff_density_rms         0.193


# start Validation Reply Form
_vrf_THETM01_AFeF_c3_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_PLAT029_AFeF_c3_p01         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.686 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT902_AFeF_c3_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_PLAT043_AFeF_c3_p01         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..     8.09 Check 
RESPONSE: Due to the low data/parameter ratio, hydrogen atoms for the 
ammonium cations were omitted.
;
_vrf_STRVA01_AFeF_c3_p01         
;
PROBLEM:     Chirality of atom sites is inverted?
RESPONSE: The inverted structure was also tested and gave a Flack parameter
of -0.8(7). Due to the low quality of the data and problems with twinning, 
the same configuration as the previous AFeF-III structures was chosen.
;
_vrf_PLAT907_AFeF_c3_p01         
;
PROBLEM: Flack x > 0.5, Structure Needs to be Inverted? .       1.80 Check 
RESPONSE: The inverted structure was also tested and gave a Flack parameter
of -0.8(7). Due to the low quality of the data and problems with twinning, 
the same configuration as the previous AFeF-III structures was chosen.
;
_vrf_PLAT041_AFeF_c3_p01         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Due to the low data/parameter ratio, hydrogen atoms for the 
ammonium cations were omitted.
;
_vrf_PLAT201_AFeF_c3_p01         
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         20 Report
RESPONSE: Due to the reduced quality of the data and low data/parameter ratio,
isotropic thermal parameters were preferred.
;
_vrf_PLAT202_AFeF_c3_p01         
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          2 Check 
RESPONSE: Due to the reduced quality of the data and low data/parameter ratio,
isotropic thermal parameters were preferred.
;
_vrf_PLAT242_AFeF_c3_p01         
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Fe1 Check 
RESPONSE: Due to the low quality of the data, thermal parameters may not be so
reliable.
;
_vrf_PLAT112_AFeF_c3_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_AFeF_c3_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_AFeF_c3_p01         
;
PROBLEM: Short Inter D...A Contact  O3       ..N2               2.79 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
# end Validation Reply Form 
