# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_ANiF_p01
_database_code_depnum_ccdc_archive 'CCDC 1501449'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        'ammonium nickel formate'

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H7 N Ni O6'
_chemical_formula_weight         211.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.2312 0.4101 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0018 0.0018 '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'

_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                   7.1610(2)
_cell_length_b                   7.1610(2)
_cell_length_c                   8.0474(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     357.38(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    487
_cell_measurement_theta_min      1.9010
_cell_measurement_theta_max      16.9280

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.055
_exptl_absorpt_coefficient_mu    0.604
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58169
_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_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         'at 0.93 GPa'
_diffrn_radiation_wavelength     0.41168
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID09A beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1185
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.902
_diffrn_reflns_theta_max         20.792
_diffrn_reflns_theta_full        14.301
_diffrn_measured_fraction_theta_max 0.743
_diffrn_measured_fraction_theta_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.743
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.695
_diffrn_reflns_point_group_measured_fraction_full 0.924
_reflns_number_total             459
_reflns_number_gt                382
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.417
_reflns_Friedel_fraction_max     0.603
_reflns_Friedel_fraction_full    0.984

_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELX (Sheldrick, 2007)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0536P)²+0.2952P] 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 103 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         459
_refine_ls_number_parameters     22
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1216
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_restrained_S_all      1.234
_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
Ni1 Ni 0.6667 0.3333 0.2500 0.0275(4) Uani 1 6 d S T P . .
O1 O 0.6913(5) 0.1092(5) 0.1070(5) 0.0409(8) Uani 1 1 d . U . . .
N1 N 1.0000 0.0000 0.2500 0.061(3) Uani 1 6 d DS T P . .
H1 H 0.94(2) 0.04(2) 0.192(5) 0.073 Uiso 0.6667 1 d D U P . .
C1 C 0.5599(9) 0.0000 0.0000 0.0467(18) Uani 1 2 d S TU P . .
H2 H 0.4300 0.0000 0.0000 0.056 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
Ni1 O1 2.053(3) . ?
Ni1 O1 2.053(3) 10_665 ?
Ni1 O1 2.053(3) 11_655 ?
Ni1 O1 2.053(3) 2_655 ?
Ni1 O1 2.053(3) 12 ?
Ni1 O1 2.053(3) 3_665 ?
O1 C1 1.226(4) . ?
C1 O1 1.225(4) 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
O1 Ni1 O1 82.58(18) . 10_665 ?
O1 Ni1 O1 94.8(2) . 11_655 ?
O1 Ni1 O1 91.64(14) 10_665 11_655 ?
O1 Ni1 O1 91.64(14) . 2_655 ?
O1 Ni1 O1 94.8(2) 10_665 2_655 ?
O1 Ni1 O1 171.48(18) 11_655 2_655 ?
O1 Ni1 O1 171.48(18) . 12 ?
O1 Ni1 O1 91.64(14) 10_665 12 ?
O1 Ni1 O1 91.64(15) 11_655 12 ?
O1 Ni1 O1 82.58(18) 2_655 12 ?
O1 Ni1 O1 91.64(15) . 3_665 ?
O1 Ni1 O1 171.48(18) 10_665 3_665 ?
O1 Ni1 O1 82.58(18) 11_655 3_665 ?
O1 Ni1 O1 91.64(14) 2_655 3_665 ?
O1 Ni1 O1 94.8(2) 12 3_665 ?
C1 O1 Ni1 123.6(4) . . ?
O1 C1 O1 126.6(7) 8 . ?

_refine_diff_density_max         0.805
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.234

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT029_ANiF_p01            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.902 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_ANiF_p01            
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600         16 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_ANiF_p01            
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         61 %     
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT934_ANiF_p01            
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check 
RESPONSE: This reflection is very intense and broad,
and so its intensity may not be so accurately determined. Due to the high
number of reflections, the presence or absence of this outlier does not 
significantly change the structural model and its parameters.
;
_vrf_PLAT975_ANiF_p01            
;
PROBLEM: Check Calcd Residual Density  0.97A From      N1       0.59 eA-3  
RESPONSE: The ammonium cation is dynamically disordered and so the model used
may not adequately describe the actual vibrational motion, but since we are 
using X-ray diffraction within a high-pressure cell it is a good enough 
approximation. 
;
_vrf_PLAT978_ANiF_p01            
;
PROBLEM: Number C-C Bonds with Positive Residual Density           0 Note  
RESPONSE: There are no C-C bonds in the structure.
;
_chemical_properties_physical    ', Moisture-sensitive'
####################################################################### 
# 
# 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_ANiF_p02
_database_code_depnum_ccdc_archive 'CCDC 1501450'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        'ammonium nickel formate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H7 N Ni O6'
_chemical_formula_weight         211.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.2312 0.4101 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
O O 0.0018 0.0018 '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'

_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                   7.1208(6)
_cell_length_b                   7.1208(6)
_cell_length_c                   8.0513(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     353.56(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    468
_cell_measurement_theta_min      3.6260
_cell_measurement_theta_max      17.1110

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.055
_exptl_absorpt_coefficient_mu    0.610
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.48868
_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_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_ambient_pressure         'at 1.28 GPa'
_diffrn_radiation_wavelength     0.41168
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID09A beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1156
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.931
_diffrn_reflns_theta_max         21.096
_diffrn_reflns_theta_full        14.301
_diffrn_measured_fraction_theta_max 0.706
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.706
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.638
_diffrn_reflns_point_group_measured_fraction_full 0.942
_reflns_number_total             430
_reflns_number_gt                334
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.369
_reflns_Friedel_fraction_max     0.507
_reflns_Friedel_fraction_full    0.952

_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELX (Sheldrick, 2007)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0430P)²+0.4766P] 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 74 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.22(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         430
_refine_ls_number_parameters     22
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1086
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.102
_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
Ni1 Ni 0.6667 0.3333 0.2500 0.0353(4) Uani 1 6 d S T P . .
O1 O 0.6916(6) 0.1084(6) 0.1079(3) 0.0484(10) Uani 1 1 d . U . . .
N1 N 1.0000 0.0000 0.2500 0.066(3) Uani 1 6 d DS T P . .
H1 H 0.93(2) 0.04(3) 0.173(6) 0.079 Uiso 0.6667 1 d D U P . .
C1 C 0.5601(11) 0.0000 0.0000 0.054(2) Uani 1 2 d S TU P . .
H2 H 0.4295 0.0000 0.0000 0.065 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
Ni1 O1 2.047(4) . ?
Ni1 O1 2.047(4) 10_665 ?
Ni1 O1 2.047(4) 11_655 ?
Ni1 O1 2.047(4) 2_655 ?
Ni1 O1 2.047(4) 12 ?
Ni1 O1 2.047(4) 3_665 ?
O1 C1 1.227(5) . ?
C1 O1 1.227(5) 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
O1 Ni1 O1 82.32(19) . 10_665 ?
O1 Ni1 O1 94.7(2) . 11_655 ?
O1 Ni1 O1 91.82(13) 10_665 11_655 ?
O1 Ni1 O1 91.82(13) . 2_655 ?
O1 Ni1 O1 94.7(2) 10_665 2_655 ?
O1 Ni1 O1 171.4(2) 11_655 2_655 ?
O1 Ni1 O1 171.4(2) . 12 ?
O1 Ni1 O1 91.82(13) 10_665 12 ?
O1 Ni1 O1 91.82(13) 11_655 12 ?
O1 Ni1 O1 82.32(19) 2_655 12 ?
O1 Ni1 O1 91.82(13) . 3_665 ?
O1 Ni1 O1 171.4(2) 10_665 3_665 ?
O1 Ni1 O1 82.32(19) 11_655 3_665 ?
O1 Ni1 O1 91.82(13) 2_655 3_665 ?
O1 Ni1 O1 94.7(2) 12 3_665 ?
C1 O1 Ni1 123.4(4) . . ?
O1 C1 O1 126.7(8) . 8 ?

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.085

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT029_ANiF_p02            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_ANiF_p02            
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600          8 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_ANiF_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.
;
_vrf_PLAT978_ANiF_p02            
;
PROBLEM: Number C-C Bonds with Positive Residual Density           0 Note  
RESPONSE: There are no C-C bonds in the structure.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1501451'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        'ammonium nickel formate'
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 N1 Ni1 O6'
_chemical_formula_weight         211.78
_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                   6.306(13)
_cell_length_b                   8.0599(14)
_cell_length_c                   7.250(13)
_cell_angle_alpha                90
_cell_angle_beta                 115.6(2)
_cell_angle_gamma                90
_cell_volume                     332.3(11)

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 0.176(6) 1 0 0 0 1 0 0 0 1
2 0.202(3) 1 0 0 0 -1 0 0.7516 0 -1
3 0.144(2) -0.0851 0 -1.1041 0 1 0 0.8353 0 -0.9149
4 0.141(2) -0.9149 0 1.1041 0 -1 0 0.1477 0 0.9149
5 0.174(3) -0.9149 0 1.1041 0 1 0 -0.8353 0 -0.0851
6 0.163(3) -0.0851 0 -1.1041 0 -1 0 -0.8993 0 0.0851

_cell_formula_units_Z            2

_cell_measurement_reflns_used    541
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      13.24
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.0812
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             208

_exptl_absorpt_coefficient_mu    0.642
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.055
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.055
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            green
_exptl_absorpt_correction_type   multi-scan
_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_correction_T_min  0.236
_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_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     0.41168
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'ID09A beamline, ESRF'
_diffrn_measurement_device_type  ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            3401
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         13.24
_diffrn_reflns_theta_full        11.46
_diffrn_measured_fraction_theta_max 0.94
_diffrn_measured_fraction_theta_full 0.95
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_av_unetI/netI     0.1098
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_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             2542
_reflns_number_gt                1110
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1111
_refine_ls_wR_factor_gt          0.1271
_refine_ls_R_factor_all          0.1801
_refine_ls_wR_factor_ref         0.1417
_refine_ls_goodness_of_fit_ref   2.19
_refine_ls_goodness_of_fit_gt    2.97
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         2542
_refine_ls_number_parameters     46
_refine_ls_number_restraints     0
_refine_ls_number_constraints    21
_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          0.0476
_refine_ls_shift/su_mean         0.0088
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.93
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  453 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'
N 0.0006 0.0010 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Ni 0.2312 0.4101 '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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    JANA2006
_computing_structure_refinement  JANA2006
_computing_molecular_graphics    ?
_computing_publication_material  ?



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

# 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
Ni1 Ni 0.6598(5) 0.75 0.3190(4) Uani 0.0789(13) 2 1 d . . .
O1 O 0.921(2) 0.6169(16) 0.294(2) Uiso 0.0717(12) 2 1 d . . .
O2 O 0.679(2) 0.6117(16) 0.555(2) Uiso 0.0717(12) 2 1 d . . .
O3 O 0.409(2) 0.6080(16) 0.109(2) Uiso 0.0717(12) 2 1 d . . .
O4 O 0.884(2) 0.8873(16) 0.558(2) Uiso 0.0717(12) 2 1 d . . .
O5 O 0.381(2) 0.8843(16) 0.292(2) Uiso 0.0717(12) 2 1 d . . .
O6 O 0.696(2) 0.8967(15) 0.108(2) Uiso 0.0717(12) 2 1 d . . .
N1 N 0.030(2) 0.249(3) 0.055(2) Uiso 0.070(3) 2 1 d . . .
C1 C 1.064(3) 0.5375(19) 0.439(3) Uiso 0.0717(12) 2 1 d . . .
C2 C 0.613(3) 0.4648(19) 0.544(3) Uiso 0.0717(12) 2 1 d . . .
C3 C 0.449(4) 0.510(3) 0.002(4) Uiso 0.0717(12) 2 1 d . . .
H1 H 1.146151 0.597697 0.564371 Uiso 0.086 2 1 d . . .
H2 H 0.556015 0.408129 0.414871 Uiso 0.086 2 1 d . . .
H3 H 0.599517 0.516363 -0.001869 Uiso 0.086 2 1 d . . .





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

# 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
Ni1 O1 . . 2.038(17) ?
Ni1 O2 . . 2.002(15) ?
Ni1 O3 . . 2.011(15) ?
Ni1 O4 . . 2.026(15) ?
Ni1 O5 . . 2.000(16) ?
Ni1 O6 . . 2.023(16) ?
O1 C1 . . 1.23(2) ?
O2 C2 . . 1.25(2) ?
O3 C3 . . 1.21(3) ?
O4 C1 . 2_756 1.25(2) ?
O5 C2 . 2_656 1.34(3) ?
O6 C3 . 2_655 1.30(3) ?
C1 H1 . . 0.96 ?
C2 H2 . . 0.96 ?
C3 H3 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ni1 O2 . . . 91.7(6) ?
O1 Ni1 O3 . . . 91.9(6) ?
O1 Ni1 O4 . . . 94.0(6) ?
O1 Ni1 O5 . . . 170.3(7) ?
O1 Ni1 O6 . . . 83.1(7) ?
O2 Ni1 O3 . . . 93.9(6) ?
O2 Ni1 O4 . . . 79.2(6) ?
O2 Ni1 O5 . . . 96.3(7) ?
O2 Ni1 O6 . . . 170.7(5) ?
O3 Ni1 O4 . . . 171.0(8) ?
O3 Ni1 O5 . . . 82.3(6) ?
O3 Ni1 O6 . . . 94.0(6) ?
O4 Ni1 O5 . . . 92.7(6) ?
O4 Ni1 O6 . . . 93.4(6) ?
O5 Ni1 O6 . . . 89.6(7) ?
Ni1 O1 C1 . . . 121.4(18) ?
Ni1 O2 C2 . . . 125.3(14) ?
Ni1 O3 C3 . . . 123.0(15) ?
Ni1 O4 C1 . . 2_756 128.7(13) ?
Ni1 O5 C2 . . 2_656 119.3(11) ?
Ni1 O6 C3 . . 2_655 126.5(18) ?
O1 C1 O4 . . 2_746 127.5(19) ?
O1 C1 H1 . . . 116.24 ?
O4 C1 H1 2_746 . . 116.24 ?
O2 C2 O5 . . 2_646 121.4(19) ?
O2 C2 H2 . . . 119.3 ?
O5 C2 H2 2_646 . . 119.3 ?
O3 C3 O6 . . 2_645 124(3) ?
O3 C3 H3 . . . 117.76 ?
O6 C3 H3 2_645 . . 117.76 ?


# start Validation Reply Form
_vrf_PLAT902_I                   
;
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 and whether they
overlap with other domains. It seems this format cannot be read by checkcif.
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction 
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT021_I                   
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      4.994       
RESPONSE: The use of a high-pressure cell limits the access to reciprocal 
space. The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.950 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction 
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_I                   
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.03 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_I                   
;
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_I                   
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT149_I                   
;
PROBLEM: s.u. on the   beta   Angle is Too Large ........       0.20 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
Additionally the reflections were broad.
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT201_I                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         10 Report
RESPONSE: Due to the low resolution of the data, the low-scattering atoms
(C, N, O) were kept to refine isotropically.
;
_vrf_CHEMW03_I                   
;
PROBLEM: The ratio of given/expected molecular weight as
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_DENSD01_I                   
;
PROBLEM: The ratio of the submitted crystal density and that
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_GOODF01_I                   
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_RFACG01_I                   
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT027_I                   
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      11.46 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         44 %     
RESPONSE: The use of a high-pressure cell limits the access to reciprocal 
space. The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
;
_vrf_PLAT034_I                   
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: The formation of six domains complicates a refinement of an 
additional six inversion twins to determine the absolute configuration
of each twin. In the P6322 structure before the phase transition, 
the flack parameter was refined to 0.22(18), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_I                   
;
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_PLAT046_I                   
;
PROBLEM: Reported Z, MW and D(calc) are Inconsistent ....      2.117       
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_I                   
;
PROBLEM: High R1 Value ..................................       0.11 Report
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT148_I                   
;
PROBLEM: s.u. on the      a  - Axis is (Too) Large ......      0.013 Ang.  
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, so the number of reflections are low and of low resolution.
Additionally the reflections were broad.
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT162_I                   
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for .        NI1 Check 
RESPONSE: This position was used to fix the origin of the unit cell.
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact  O4     ..  N2      ..       2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ANiF_ambient
_database_code_depnum_ccdc_archive 'CCDC 1501452'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        'ammonium nickel formate'

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H7 N Ni O6'
_chemical_formula_weight         211.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.28640(16)
_cell_length_b                   7.28640(16)
_cell_length_c                   8.05248(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     370.242(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3020
_cell_measurement_theta_min      3.2070
_cell_measurement_theta_max      28.7780

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.606
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode'
_diffrn_measurement_device_type  MAR345dbt
_diffrn_measurement_method       'Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7581
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.228
_diffrn_reflns_theta_max         29.771
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             361
_reflns_number_gt                330
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.438
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELX (Sheldrick, 2007)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0206P)²+0.0925P] 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 97 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         361
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0455
_refine_ls_wR_factor_gt          0.0448
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.173
_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
Ni1 Ni 0.6667 0.3333 0.2500 0.01459(17) Uani 1 6 d S T P . .
O1 O 0.6911(2) 0.1116(2) 0.10613(16) 0.0243(4) Uani 1 1 d . . . . .
N1 N 0.0000 0.0000 0.2500 0.0586(18) Uani 1 6 d DS T P . .
H1 H -0.027(13) 0.077(10) 0.316(4) 0.088 Uiso 0.6667 1 d D U P . .
C1 C 0.5580(5) 0.0000 0.0000 0.0281(8) Uani 1 2 d S T P . .
H2 H 0.4303 0.0000 0.0000 0.042 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
Ni1 O1 2.0667(14) 10_665 ?
Ni1 O1 2.0667(14) . ?
Ni1 O1 2.0667(14) 11_655 ?
Ni1 O1 2.0667(14) 2_655 ?
Ni1 O1 2.0667(14) 12 ?
Ni1 O1 2.0667(14) 3_665 ?
O1 C1 1.243(2) . ?
C1 O1 1.243(2) 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
O1 Ni1 O1 82.55(8) 10_665 . ?
O1 Ni1 O1 91.64(5) 10_665 11_655 ?
O1 Ni1 O1 94.79(8) . 11_655 ?
O1 Ni1 O1 94.79(8) 10_665 2_655 ?
O1 Ni1 O1 91.64(5) . 2_655 ?
O1 Ni1 O1 171.45(9) 11_655 2_655 ?
O1 Ni1 O1 91.64(5) 10_665 12 ?
O1 Ni1 O1 171.45(9) . 12 ?
O1 Ni1 O1 91.64(5) 11_655 12 ?
O1 Ni1 O1 82.55(8) 2_655 12 ?
O1 Ni1 O1 171.45(9) 10_665 3_665 ?
O1 Ni1 O1 91.64(5) . 3_665 ?
O1 Ni1 O1 82.55(8) 11_655 3_665 ?
O1 Ni1 O1 91.64(5) 2_655 3_665 ?
O1 Ni1 O1 94.79(8) 12 3_665 ?
C1 O1 Ni1 123.57(18) . . ?
O1 C1 O1 126.1(3) . 8 ?

_refine_diff_density_max         0.188
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.051

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT978_ANiF_ambient        
;
PROBLEM: Number C-C Bonds with Positive Residual Density           0 Note  
RESPONSE: There are no C-C bonds in the structure.
;
####################################################################### 
# 
# 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_ANiF_100K
_database_code_depnum_ccdc_archive 'CCDC 1501453'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        'ammonium nickel formate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H7 N Ni O6'
_chemical_formula_weight         211.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.26097(16)
_cell_length_b                   7.26097(16)
_cell_length_c                   8.0811(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     368.969(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4923
_cell_measurement_theta_min      3.2000
_cell_measurement_theta_max      29.7310

_exptl_crystal_description       'hexagonal block'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   0.75759
_exptl_transmission_factor_max   1.0000
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.615
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating anode'
_diffrn_measurement_device_type  MAR345dbt
_diffrn_measurement_method       'Phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7561
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.240
_diffrn_reflns_theta_max         29.785
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             361
_reflns_number_gt                351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.438
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELX (Sheldrick, 2007)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_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)+(0.0271P)²+0.1336P] 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 104 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         361
_refine_ls_number_parameters     25
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0179
_refine_ls_wR_factor_ref         0.0477
_refine_ls_wR_factor_gt          0.0473
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001

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
Ni1 Ni 0.6667 0.3333 0.2500 0.00583(17) Uani 1 6 d S T P . .
O1 O 0.6915(2) 0.1114(2) 0.10668(14) 0.0106(3) Uani 1 1 d . . . . .
N1 N 0.0000 0.0000 0.2077(6) 0.0130(11) Uani 0.5 3 d DS T P . .
H1 H -0.110(10) 0.033(11) 0.163(7) 0.047(19) Uiso 0.5 1 d . . P . .
H2 H 0.0000 0.0000 0.159(16) 0.057 Uiso 0.5 3 d S U P . .
C1 C 0.5564(4) 0.0000 0.0000 0.0134(5) Uani 1 2 d S T P . .
H3 H 0.4283 0.0000 0.0000 0.020 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
Ni1 O1 2.0643(12) . ?
Ni1 O1 2.0643(12) 10_665 ?
Ni1 O1 2.0643(12) 11_655 ?
Ni1 O1 2.0643(12) 2_655 ?
Ni1 O1 2.0643(12) 12 ?
Ni1 O1 2.0643(12) 3_665 ?
O1 C1 1.2516(17) . ?
N1 N1 0.684(10) 10 ?
C1 O1 1.2516(17) 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
O1 Ni1 O1 82.52(7) . 10_665 ?
O1 Ni1 O1 94.93(7) . 11_655 ?
O1 Ni1 O1 91.59(5) 10_665 11_655 ?
O1 Ni1 O1 91.59(5) . 2_655 ?
O1 Ni1 O1 94.93(7) 10_665 2_655 ?
O1 Ni1 O1 171.32(7) 11_655 2_655 ?
O1 Ni1 O1 171.32(7) . 12 ?
O1 Ni1 O1 91.59(5) 10_665 12 ?
O1 Ni1 O1 91.59(5) 11_655 12 ?
O1 Ni1 O1 82.52(7) 2_655 12 ?
O1 Ni1 O1 91.59(5) . 3_665 ?
O1 Ni1 O1 171.32(7) 10_665 3_665 ?
O1 Ni1 O1 82.52(7) 11_655 3_665 ?
O1 Ni1 O1 91.59(5) 2_655 3_665 ?
O1 Ni1 O1 94.93(7) 12 3_665 ?
C1 O1 Ni1 123.00(14) . . ?
O1 C1 O1 125.1(3) 8 . ?

_refine_diff_density_max         0.251
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.058

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_PLAT420_ANiF_100K           
;
PROBLEM: D-H Without Acceptor      *N1     -- *H2     ...     Please Check 
RESPONSE: Three N-H bonds are with acceptors and one N-H bond is without
due to the tetrahedral geometry of NH4+ cation.

;
_vrf_PLAT978_ANiF_100K           
;
PROBLEM: Number C-C Bonds with Positive Residual Density           0 Note  
RESPONSE: There are no C-C bonds in the structure.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_I
_database_code_depnum_ccdc_archive 'CCDC 1501454'
_audit_update_record             
;
2016-08-29 deposited with the CCDC.
2016-10-19 downloaded from the CCDC.
;
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        'ammonium iron formate'
_chemical_name_common            ?
_chemical_formula_moiety         ?
_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                   6.668(6)
_cell_length_b                   8.298(4)
_cell_length_c                   7.393(6)
_cell_angle_alpha                90
_cell_angle_beta                 116.64(11)
_cell_angle_gamma                90
_cell_volume                     365.6(6)

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(6) 1 0 0 0 1 0 0 0 1
2 0.141(2) 1 0 0 0 -1 0 0.8088 0 -1
3 0.189(2) -0.0656 0 -1.0742 0 1 0 0.8739 0 -0.9344
4 0.220(3) -0.9344 0 1.0742 0 -1 0 0.1182 0 0.9344
5 0.176(3) -0.9344 0 1.0742 0 1 0 -0.8739 0 -0.0656
6 0.136(3) -0.0656 0 -1.0742 0 -1 0 -0.927 0 0.0656

_cell_formula_units_Z            2

_cell_measurement_reflns_used    859
_cell_measurement_theta_min      1.72
_cell_measurement_theta_max      9.28
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.8978
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             204

_exptl_absorpt_coefficient_mu    0.177
_exptl_crystal_description       'irregular block'
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.015
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless
_exptl_absorpt_correction_type   multi-scan
_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_correction_T_min  0.541
_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_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     0.2903
_diffrn_radiation_monochromator  synchrotron
_diffrn_measurement_device       'P02.2 Beamline, DESY'
_diffrn_measurement_device_type  ?
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            4154
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         9.29
_diffrn_reflns_theta_full        9.29
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measured_fraction_theta_full 0.95
_diffrn_reflns_av_R_equivalents  0.1405
_diffrn_reflns_av_unetI/netI     0.1338
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

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

_diffrn_radiation_probe          X-ray

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

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             3250
_reflns_number_gt                1549
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1431
_refine_ls_wR_factor_gt          0.1562
_refine_ls_R_factor_all          0.1914
_refine_ls_wR_factor_ref         0.1657
_refine_ls_goodness_of_fit_ref   2.44
_refine_ls_goodness_of_fit_gt    3.31
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3250
_refine_ls_number_parameters     46
_refine_ls_number_restraints     0
_refine_ls_number_constraints    21
_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          0.0335
_refine_ls_shift/su_mean         0.0071
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  567 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 -0.0010 0.0002 '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 0.1036 0.1542 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N -0.0011 0.0004 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O -0.0009 0.0008 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'superflip in JANA'
_computing_structure_refinement  JANA2006
_computing_molecular_graphics    ?
_computing_publication_material  ?



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

# 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 0.3394(4) 0.25 0.6782(3) Uani 0.0661(10) 2 1 d . . .
O1 O 0.103(2) 0.1058(16) 0.7032(17) Uiso 0.0784(13) 2 1 d . . .
O2 O 0.314(2) 0.1062(15) 0.4424(16) Uiso 0.0784(13) 2 1 d . . .
O3 O 0.5953(19) 0.1142(16) 0.8949(16) Uiso 0.0784(13) 2 1 d . . .
O4 O 0.117(2) 0.3942(15) 0.4410(15) Uiso 0.0784(13) 2 1 d . . .
O5 O 0.6263(19) 0.3874(16) 0.7078(17) Uiso 0.0784(13) 2 1 d . . .
O6 O 0.297(2) 0.4038(16) 0.8936(16) Uiso 0.0784(13) 2 1 d . . .
C1 C 0.070(3) 0.535(2) 0.449(3) Uiso 0.0784(13) 2 1 d . . .
C2 C 0.583(3) 0.473(2) 0.562(3) Uiso 0.0784(13) 2 1 d . . .
C3 C 0.541(3) 0.008(2) 0.977(3) Uiso 0.0784(13) 2 1 d . . .
N1 N 1.037(2) 0.247(3) 1.0518(17) Uiso 0.078(3) 2 1 d . . .
H1 H 0.158697 0.596454 0.568302 Uiso 0.0941 2 1 d . . .
H2 H 0.46036 0.439669 0.436363 Uiso 0.0941 2 1 d . . .
H3 H 0.387578 -0.003461 0.952385 Uiso 0.0941 2 1 d . . .





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

# 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 O1 . . 2.054(15) ?
Fe1 O2 . . 2.056(13) ?
Fe1 O3 . . 2.072(12) ?
Fe1 O4 . . 2.091(11) ?
O1 C1 . 2_546 1.331(19) ?
O2 C2 . 2_646 1.31(2) ?
O3 C3 . . 1.21(3) ?
O4 C1 . . 1.22(2) ?
O5 C2 . . 1.22(2) ?
O6 C3 . 2_657 1.38(2) ?
C1 H1 . . 0.96 ?
C2 H2 . . 0.96 ?
C3 H3 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Fe1 O2 . . . 87.9(6) ?
O1 Fe1 O3 . . . 90.8(5) ?
O1 Fe1 O4 . . . 97.2(5) ?
O2 Fe1 O3 . . . 93.8(5) ?
O2 Fe1 O4 . . . 82.1(5) ?
O3 Fe1 O4 . . . 170.9(6) ?
Fe1 O1 C1 . . 2_546 126.0(13) ?
Fe1 O2 C2 . . 2_646 131.6(10) ?
Fe1 O3 C3 . . . 117.1(12) ?
Fe1 O4 C1 . . . 127.6(10) ?
O1 C1 O4 2_556 . . 121.8(15) ?
O1 C1 H1 2_556 . . 119.09 ?
O4 C1 H1 . . . 119.09 ?
O2 C2 O5 2_656 . . 126.5(14) ?
O2 C2 H2 2_656 . . 116.75 ?
O5 C2 H2 . . . 116.75 ?
O3 C3 O6 . . 2_647 119.0(19) ?
O3 C3 H3 . . . 120.5 ?
O6 C3 H3 2_647 . . 120.5 ?


# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: The ratio of given/expected molecular weight as
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_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction 
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT021_I                   
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      5.722       
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction 
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.950 Note  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction 
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT043_I                   
;
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_I                   
;
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_I                   
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT149_I                   
;
PROBLEM: s.u. on the   beta   Angle is Too Large ........       0.11 Degree
RESPONSE: The reflections are broad due to the high-pressure phase transition.
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT201_I                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         10 Report
RESPONSE: Due to the low resolution of the data, the low-scattering atoms
(C, N, O) were kept to refine isotropically.
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact  O3     ..  N1      ..       2.85 Ang.  
RESPONSE:  This contact may contain a hydrogen bond from the ammonium cation. 
;
_vrf_GOODF01_I                   
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_RFACG01_I                   
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_RINTA01_I                   
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT902_I                   
;
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 and whether they
overlap with other domains. It seems this format cannot be read by checkcif.
;
_vrf_PLAT020_I                   
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.140 Report
RESPONSE: Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT026_I                   
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         48 %     
RESPONSE: The use of a high-pressure cell limits the access to reciprocal 
space. 
;
_vrf_PLAT034_I                   
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: The formation of six domains complicates a refinement of an 
additional six inversion twins to determine the absolute configuration
of each twin. The refinement was repeated in the inverted configuration,
but no significant differences in the refinement were observed.
;
_vrf_PLAT041_I                   
;
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_I                   
;
PROBLEM: High R1 Value ..................................       0.14 Report
RESPONSE: Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro could not integrate all six domains at once. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT162_I                   
;
PROBLEM: Missing or Zero s.u. (esd) on y-coordinate for .        FE1 Check 
RESPONSE: This position was used to fix the origin of the unit cell.
;
# end Validation Reply Form
