# 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_ANiF_c2_p0
_database_code_depnum_ccdc_archive 'CCDC 1861349'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.28362(13)
_cell_length_b                   7.28362(13)
_cell_length_c                   8.04848(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     369.776(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    289
_cell_measurement_theta_min      2.3720
_cell_measurement_theta_max      16.8550

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.582
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75010
_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     0.41128
_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            1096
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.475
_diffrn_reflns_theta_max         19.838
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.737
_diffrn_measured_fraction_theta_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.737
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.722
_diffrn_reflns_point_group_measured_fraction_full 0.947
_reflns_number_total             425
_reflns_number_gt                374
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.471
_reflns_Friedel_fraction_max     0.690
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0146P)²+0.1955P] 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 115 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         425
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0722
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.209
_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 0.333333 0.666667 0.250000 0.0208(2) Uani 1 6 d S T P . .
O1 O 0.3090(4) 0.8882(3) 0.1055(3) 0.0307(5) Uani 1 1 d . . . . .
C1 C 0.4418(6) 1.000000 0.000000 0.0354(10) Uani 1 2 d S T P . .
H1 H 0.569500 1.000001 0.000000 0.042 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.060(2) Uani 1 6 d DS T P . .
H2 H 0.090(13) 1.122(8) 0.305(7) 0.073 Uiso 0.6667 1 d D 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 2.067(2) 10_665 ?
Ni1 O1 2.067(2) 11 ?
Ni1 O1 2.067(2) 2_665 ?
Ni1 O1 2.067(2) . ?
Ni1 O1 2.067(2) 12_565 ?
Ni1 O1 2.067(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 Ni1 O1 91.45(9) 10_665 11 ?
O1 Ni1 O1 94.93(13) 10_665 2_665 ?
O1 Ni1 O1 171.50(12) 11 2_665 ?
O1 Ni1 O1 82.79(12) 10_665 . ?
O1 Ni1 O1 94.93(13) 11 . ?
O1 Ni1 O1 91.45(9) 2_665 . ?
O1 Ni1 O1 91.45(9) 10_665 12_565 ?
O1 Ni1 O1 91.45(9) 11 12_565 ?
O1 Ni1 O1 82.79(12) 2_665 12_565 ?
O1 Ni1 O1 171.50(12) . 12_565 ?
O1 Ni1 O1 171.50(12) 10_665 3_565 ?
O1 Ni1 O1 82.79(12) 11 3_565 ?
O1 Ni1 O1 91.45(9) 2_665 3_565 ?
O1 Ni1 O1 91.45(9) . 3_565 ?
O1 Ni1 O1 94.93(13) 12_565 3_565 ?
C1 O1 Ni1 123.8(2) . . ?
O1 C1 O1 126.2(4) . 8_675 ?

_refine_diff_density_max         0.309
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.071


# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p0          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.927 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_ANiF_c2_p0          
;
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_c2_p0          
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         69 %     
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_ANiF_c2_p01
_database_code_depnum_ccdc_archive 'CCDC 1861350'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.27890(18)
_cell_length_b                   7.27890(18)
_cell_length_c                   8.0555(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     369.62(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    363
_cell_measurement_theta_min      1.8690
_cell_measurement_theta_max      18.3520

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.582
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85616
_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         '0.12 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41128
_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            1076
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.869
_diffrn_reflns_theta_max         20.017
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.728
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.674
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             406
_reflns_number_gt                373
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.390
_reflns_Friedel_fraction_max     0.567
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+0.1083P] 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 100 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         406
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0625
_refine_ls_wR_factor_gt          0.0569
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_restrained_S_all      1.243
_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 0.333333 0.666667 0.250000 0.0193(2) Uani 1 6 d S T P . .
O1 O 0.3092(3) 0.8887(3) 0.1060(2) 0.0300(4) Uani 1 1 d . . . . .
C1 C 0.4413(5) 1.000000 0.000000 0.0338(8) Uani 1 2 d S T P . .
H1 H 0.569037 1.000001 0.000001 0.041 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.061(2) Uani 1 6 d DS T P . .
H2 H 0.094(10) 1.123(7) 0.314(6) 0.074 Uiso 0.6667 1 d D 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 2.0671(17) 10_665 ?
Ni1 O1 2.0671(17) 11 ?
Ni1 O1 2.0671(17) 2_665 ?
Ni1 O1 2.0671(17) 3_565 ?
Ni1 O1 2.0671(17) 12_565 ?
Ni1 O1 2.0671(17) . ?
O1 C1 1.237(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 91.57(7) 10_665 11 ?
O1 Ni1 O1 94.76(11) 10_665 2_665 ?
O1 Ni1 O1 171.57(10) 11 2_665 ?
O1 Ni1 O1 171.57(10) 10_665 3_565 ?
O1 Ni1 O1 82.70(10) 11 3_565 ?
O1 Ni1 O1 91.57(7) 2_665 3_565 ?
O1 Ni1 O1 91.57(7) 10_665 12_565 ?
O1 Ni1 O1 91.57(7) 11 12_565 ?
O1 Ni1 O1 82.70(10) 2_665 12_565 ?
O1 Ni1 O1 94.76(11) 3_565 12_565 ?
O1 Ni1 O1 82.70(10) 10_665 . ?
O1 Ni1 O1 94.76(11) 11 . ?
O1 Ni1 O1 91.57(7) 2_665 . ?
O1 Ni1 O1 91.57(7) 3_565 . ?
O1 Ni1 O1 171.57(10) 12_565 . ?
C1 O1 Ni1 123.87(19) . . ?
O1 C1 O1 126.6(3) . 8_675 ?

_refine_diff_density_max         0.307
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.060




# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p01         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 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_ANiF_c2_p01         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 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_c2_p01         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         57 %     
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_ANiF_c2_p02
_database_code_depnum_ccdc_archive 'CCDC 1861351'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.24917(9)
_cell_length_b                   7.24917(9)
_cell_length_c                   8.04612(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     366.179(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    334
_cell_measurement_theta_min      1.8750
_cell_measurement_theta_max      18.8010

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.588
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61786
_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         '0.29 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41128
_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            1068
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.877
_diffrn_reflns_theta_max         20.061
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.728
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.672
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             404
_reflns_number_gt                374
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.388
_reflns_Friedel_fraction_max     0.562
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+0.1633P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 101 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         403
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0249
_refine_ls_wR_factor_ref         0.0628
_refine_ls_wR_factor_gt          0.0556
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_restrained_S_all      1.220
_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 0.333333 0.666667 0.250000 0.01905(19) Uani 1 6 d S T P . .
O1 O 0.3093(3) 0.8888(3) 0.1063(2) 0.0305(4) Uani 1 1 d . . . . .
C1 C 0.4420(5) 1.000000 0.000000 0.0341(9) Uani 1 2 d S T P . .
H1 H 0.570278 1.000000 0.000000 0.041 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.060(2) Uani 1 6 d DS T P . .
H2 H 0.092(11) 1.122(7) 0.308(7) 0.072 Uiso 0.6667 1 d D 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 2.0589(18) 10_665 ?
Ni1 O1 2.0589(18) 2_665 ?
Ni1 O1 2.0589(18) 11 ?
Ni1 O1 2.0589(18) 12_565 ?
Ni1 O1 2.0589(18) 3_565 ?
Ni1 O1 2.0589(18) . ?
O1 C1 1.238(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 94.75(11) 10_665 2_665 ?
O1 Ni1 O1 91.56(8) 10_665 11 ?
O1 Ni1 O1 171.60(11) 2_665 11 ?
O1 Ni1 O1 91.56(8) 10_665 12_565 ?
O1 Ni1 O1 82.74(11) 2_665 12_565 ?
O1 Ni1 O1 91.56(8) 11 12_565 ?
O1 Ni1 O1 171.60(11) 10_665 3_565 ?
O1 Ni1 O1 91.56(8) 2_665 3_565 ?
O1 Ni1 O1 82.74(11) 11 3_565 ?
O1 Ni1 O1 94.75(11) 12_565 3_565 ?
O1 Ni1 O1 82.74(11) 10_665 . ?
O1 Ni1 O1 91.56(8) 2_665 . ?
O1 Ni1 O1 94.75(11) 11 . ?
O1 Ni1 O1 171.60(11) 12_565 . ?
O1 Ni1 O1 91.56(8) 3_565 . ?
C1 O1 Ni1 123.75(19) . . ?
O1 C1 O1 126.3(3) . 8_675 ?

_refine_diff_density_max         0.321
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.064


# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p02         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 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_ANiF_c2_p02         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 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_c2_p02         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         56 %     
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_ANiF_c2_p03
_database_code_depnum_ccdc_archive 'CCDC 1861352'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.2211(2)
_cell_length_b                   7.2211(2)
_cell_length_c                   8.0490(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     363.48(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    393
_cell_measurement_theta_min      1.8840
_cell_measurement_theta_max      17.8030

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.592
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38672
_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         '0.51 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41128
_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            1063
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.884
_diffrn_reflns_theta_max         20.083
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.728
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.667
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             401
_reflns_number_gt                370
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.378
_reflns_Friedel_fraction_max     0.547
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0071P)²+0.2148P] 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   0.06(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         400
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0622
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_restrained_S_all      1.269
_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 0.333333 0.666667 0.250000 0.0184(2) Uani 1 6 d S T P . .
O1 O 0.3089(3) 0.8894(3) 0.1067(3) 0.0299(5) Uani 1 1 d . . . . .
C1 C 0.4415(5) 1.000000 0.000000 0.0349(10) Uani 1 2 d S T P . .
H1 H 0.570273 1.000000 -0.000001 0.042 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.057(2) Uani 1 6 d DS T P . .
H2 H 0.090(11) 1.119(7) 0.314(7) 0.069 Uiso 0.6667 1 d D 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 2.0571(19) . ?
Ni1 O1 2.0571(19) 10_665 ?
Ni1 O1 2.0571(19) 2_665 ?
Ni1 O1 2.0571(19) 11 ?
Ni1 O1 2.0571(19) 3_565 ?
Ni1 O1 2.0571(19) 12_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 Ni1 O1 82.59(11) . 10_665 ?
O1 Ni1 O1 91.63(8) . 2_665 ?
O1 Ni1 O1 94.78(12) 10_665 2_665 ?
O1 Ni1 O1 94.78(12) . 11 ?
O1 Ni1 O1 91.63(8) 10_665 11 ?
O1 Ni1 O1 171.47(12) 2_665 11 ?
O1 Ni1 O1 91.63(8) . 3_565 ?
O1 Ni1 O1 171.47(12) 10_665 3_565 ?
O1 Ni1 O1 91.63(8) 2_665 3_565 ?
O1 Ni1 O1 82.59(11) 11 3_565 ?
O1 Ni1 O1 171.48(12) . 12_565 ?
O1 Ni1 O1 91.63(8) 10_665 12_565 ?
O1 Ni1 O1 82.59(11) 2_665 12_565 ?
O1 Ni1 O1 91.63(8) 11 12_565 ?
O1 Ni1 O1 94.78(12) 3_565 12_565 ?
C1 O1 Ni1 123.6(2) . . ?
O1 C1 O1 126.3(4) 8_675 . ?

_refine_diff_density_max         0.590
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.085

# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p03         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 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_ANiF_c2_p03         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 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_c2_p03         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         55 %     
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired. 
;
_vrf_PLAT973_ANiF_c2_p03         
;
PROBLEM: Check Calcd Positive Resid. Density on       Ni1       1.02 eA-3  
RESPONSE: This was checked but does not correspond to any reasonable structural/
atomic changes. The residual density may arise due to a slightly worse crystal
centering for this particular pressure point.
;
_vrf_PLAT975_ANiF_c2_p03         
;
PROBLEM: Check Calcd Resid. Dens.  0.52A   From N1              0.50 eA-3  
RESPONSE: This was checked but does not correspond to any reasonable structural/
atomic changes. The residual density may arise due to a slightly worse crystal
centering for this particular pressure point.
;
_vrf_PLAT976_ANiF_c2_p03         
;
PROBLEM: Check Calcd Resid. Dens.  1.00A   From N1             -0.57 eA-3  
RESPONSE: This was checked but does not correspond to any reasonable structural/
atomic changes. The residual density may arise due to a slightly worse crystal
centering for this particular pressure point.
;
####################################################################### 
# 
# 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_c2_p04
_database_code_depnum_ccdc_archive 'CCDC 1861353'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.1831(2)
_cell_length_b                   7.1831(2)
_cell_length_c                   8.0511(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     359.76(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    412
_cell_measurement_theta_min      1.8950
_cell_measurement_theta_max      17.0000

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.598
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50830
_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         '0.82 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41128
_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            1045
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.894
_diffrn_reflns_theta_max         19.558
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measured_fraction_theta_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.709
_diffrn_reflns_point_group_measured_fraction_full 0.951
_reflns_number_total             395
_reflns_number_gt                351
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.381
_reflns_Friedel_fraction_max     0.592
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+0.2027P] 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 90 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         395
_refine_ls_number_parameters     22
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0668
_refine_ls_wR_factor_gt          0.0610
_refine_ls_goodness_of_fit_ref   1.253
_refine_ls_restrained_S_all      1.252
_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 0.333333 0.666667 0.250000 0.0240(2) Uani 1 6 d S T P . .
O1 O 0.3091(4) 0.8908(3) 0.1069(3) 0.0357(5) Uani 1 1 d . . . . .
C1 C 0.4414(6) 1.000000 0.000000 0.0397(11) Uani 1 2 d S T P . .
H1 H 0.570850 1.000001 0.000003 0.048 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.056(2) Uani 1 6 d DS T P . .
H2 H 0.085(12) 1.118(7) 0.310(7) 0.068 Uiso 0.6667 1 d D 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 2.056(2) 12_565 ?
Ni1 O1 2.056(2) 3_565 ?
Ni1 O1 2.056(2) 11 ?
Ni1 O1 2.056(2) 2_665 ?
Ni1 O1 2.056(2) . ?
Ni1 O1 2.056(2) 10_665 ?
O1 C1 1.230(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 Ni1 O1 94.63(13) 12_565 3_565 ?
O1 Ni1 O1 91.68(9) 12_565 11 ?
O1 Ni1 O1 82.62(12) 3_565 11 ?
O1 Ni1 O1 82.62(12) 12_565 2_665 ?
O1 Ni1 O1 91.68(9) 3_565 2_665 ?
O1 Ni1 O1 171.61(13) 11 2_665 ?
O1 Ni1 O1 171.60(13) 12_565 . ?
O1 Ni1 O1 91.68(9) 3_565 . ?
O1 Ni1 O1 94.63(13) 11 . ?
O1 Ni1 O1 91.68(9) 2_665 . ?
O1 Ni1 O1 91.68(9) 12_565 10_665 ?
O1 Ni1 O1 171.60(13) 3_565 10_665 ?
O1 Ni1 O1 91.68(9) 11 10_665 ?
O1 Ni1 O1 94.63(13) 2_665 10_665 ?
O1 Ni1 O1 82.61(12) . 10_665 ?
C1 O1 Ni1 123.4(2) . . ?
O1 C1 O1 126.1(4) 8_675 . ?

_refine_diff_density_max         0.280
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.068


# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p04         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.933 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_ANiF_c2_p04         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         11 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_c2_p04         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         60 %     
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_ANiF_c2_p05
_database_code_depnum_ccdc_archive 'CCDC 1861354'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.15551(17)
_cell_length_b                   7.15551(17)
_cell_length_c                   8.05112(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     357.000(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    339
_cell_measurement_theta_min      1.9020
_cell_measurement_theta_max      16.2570

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.603
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79313
_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         '1.03 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41128
_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            1034
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.902
_diffrn_reflns_theta_max         19.629
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.710
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             397
_reflns_number_gt                326
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.383
_reflns_Friedel_fraction_max     0.595
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       ?
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2013)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2013)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXLE-2011 (Huebschle, 2011)'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+0.5918P] 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 85 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         396
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0858
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_restrained_S_all      1.214
_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 0.333333 0.666667 0.250000 0.0309(3) Uani 1 6 d S T P . .
O1 O 0.3089(5) 0.8906(5) 0.1073(4) 0.0412(8) Uani 1 1 d . . . . .
C1 C 0.4409(9) 1.000000 0.000000 0.0473(17) Uani 1 2 d S T P . .
H1 H 0.570887 1.000001 0.000001 0.057 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.058(3) Uani 1 6 d DS T P . .
H2 H 0.091(14) 1.132(7) 0.306(9) 0.069 Uiso 0.6667 1 d D 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 2.050(3) . ?
Ni1 O1 2.050(3) 10_665 ?
Ni1 O1 2.050(3) 2_665 ?
Ni1 O1 2.050(3) 11 ?
Ni1 O1 2.050(3) 3_565 ?
Ni1 O1 2.050(3) 12_565 ?
O1 C1 1.229(4) . ?

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 82.61(17) . 10_665 ?
O1 Ni1 O1 91.63(12) . 2_665 ?
O1 Ni1 O1 94.75(19) 10_665 2_665 ?
O1 Ni1 O1 94.75(19) . 11 ?
O1 Ni1 O1 91.63(12) 10_665 11 ?
O1 Ni1 O1 171.51(18) 2_665 11 ?
O1 Ni1 O1 91.63(12) . 3_565 ?
O1 Ni1 O1 171.51(19) 10_665 3_565 ?
O1 Ni1 O1 91.63(12) 2_665 3_565 ?
O1 Ni1 O1 82.61(17) 11 3_565 ?
O1 Ni1 O1 171.51(19) . 12_565 ?
O1 Ni1 O1 91.63(12) 10_665 12_565 ?
O1 Ni1 O1 82.61(17) 2_665 12_565 ?
O1 Ni1 O1 91.63(12) 11 12_565 ?
O1 Ni1 O1 94.75(19) 3_565 12_565 ?
C1 O1 Ni1 123.5(3) . . ?
O1 C1 O1 126.5(6) 8_675 . ?

_refine_diff_density_max         0.475
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.078


# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p05         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 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_ANiF_c2_p05         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 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_c2_p05         
;
PROBLEM: No Flack x Check Done: Low Friedel Pair Coverage         60 %     
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_ANiF_c2_p06
_database_code_depnum_ccdc_archive 'CCDC 1861355'
_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 Ni O6, N H4'
_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
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'
Ni Ni 0.2309 0.4094 '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                   7.1272(3)
_cell_length_b                   7.1272(3)
_cell_length_c                   8.0615(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     354.64(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    287
_cell_measurement_theta_min      1.9110
_cell_measurement_theta_max      14.7660

_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_F_000             216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.607
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.17410
_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         '1.26 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41128
_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            1040
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.909
_diffrn_reflns_theta_max         19.503
_diffrn_reflns_theta_full        14.286
_diffrn_measured_fraction_theta_max 0.770
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.770
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.716
_diffrn_reflns_point_group_measured_fraction_full 0.951
_reflns_number_total             390
_reflns_number_gt                288
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.388
_reflns_Friedel_fraction_max     0.606
_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 (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)+(0.0272P)²+0.1969P] 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 67 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         390
_refine_ls_number_parameters     22
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.124
_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 0.333333 0.666667 0.250000 0.0336(4) Uani 1 6 d S T P . .
O1 O 0.3094(5) 0.8921(5) 0.1078(4) 0.0472(8) Uani 1 1 d . . . . .
C1 C 0.4392(9) 1.000000 0.000000 0.0528(18) Uani 1 2 d S T P . .
H1 H 0.569693 0.999999 -0.000001 0.063 Uiso 1 2 calc R U P . .
N1 N 0.000000 1.000000 0.250000 0.062(3) Uani 1 6 d DS T P . .
H2 H 0.098(12) 1.131(7) 0.305(9) 0.074 Uiso 0.6667 1 d D 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 2.049(3) 10_665 ?
Ni1 O1 2.049(3) 11 ?
Ni1 O1 2.049(3) 2_665 ?
Ni1 O1 2.049(3) . ?
Ni1 O1 2.049(3) 12_565 ?
Ni1 O1 2.049(3) 3_565 ?
O1 C1 1.221(4) . ?

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 91.75(12) 10_665 11 ?
O1 Ni1 O1 94.46(19) 10_665 2_665 ?
O1 Ni1 O1 171.74(18) 11 2_665 ?
O1 Ni1 O1 82.63(17) 10_665 . ?
O1 Ni1 O1 94.46(19) 11 . ?
O1 Ni1 O1 91.75(12) 2_665 . ?
O1 Ni1 O1 91.75(12) 10_665 12_565 ?
O1 Ni1 O1 91.75(12) 11 12_565 ?
O1 Ni1 O1 82.63(17) 2_665 12_565 ?
O1 Ni1 O1 171.74(18) . 12_565 ?
O1 Ni1 O1 171.74(18) 10_665 3_565 ?
O1 Ni1 O1 82.63(17) 11 3_565 ?
O1 Ni1 O1 91.75(12) 2_665 3_565 ?
O1 Ni1 O1 91.75(12) . 3_565 ?
O1 Ni1 O1 94.46(19) 12_565 3_565 ?
C1 O1 Ni1 123.9(3) . . ?
O1 C1 O1 127.4(6) . 8_675 ?

_refine_diff_density_max         0.430
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.081


# start Validation Reply Form
_vrf_PLAT029_ANiF_c2_p06         
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.939 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_ANiF_c2_p06         
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         10 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_c2_p06         
;
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. 
;
####################################################################### 
# 
# 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_c2_p08
_database_code_depnum_ccdc_archive 'CCDC 1861356'
_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 Ni O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 N1 Ni1 O6'
_chemical_formula_weight         211.8
_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                   6.607(3)
_cell_length_b                   8.0559(10)
_cell_length_c                   7.270(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.96(5)
_cell_angle_gamma                90
_cell_volume                     344.9(2)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.172(4) 1 0 0 0 1 0 0 0 1
2 0.1762(19) 1 0 0 0 -1 0 0.8244 0 -1
3 0.151(2) -0.0597 0 -1.0682 0 1 0 0.8836 0 -0.9403
4 0.1619(18) -0.9403 0 1.0682 0 -1 0 0.1084 0 0.9403
5 0.1765(17) -0.9403 0 1.0682 0 1 0 -0.8836 0 -0.0597
6 0.1618(18) -0.0597 0 -1.0682 0 -1 0 -0.9328 0 0.0597

_cell_formula_units_Z            2

_cell_measurement_reflns_used    147
_cell_measurement_theta_min      2
_cell_measurement_theta_max      12.71
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.0393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             208

_exptl_absorpt_coefficient_mu    0.619
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            green
_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  0.876
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '1.60 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     0.41128
_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            3466
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         13.21
_diffrn_reflns_theta_full        13.2
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

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

_diffrn_radiation_probe          X-ray

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

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             2918
_reflns_number_gt                2237
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0916
_refine_ls_wR_factor_gt          0.1136
_refine_ls_R_factor_all          0.1079
_refine_ls_wR_factor_ref         0.1165
_refine_ls_goodness_of_fit_ref   3.20
_refine_ls_goodness_of_fit_gt    3.57
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         2918
_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          0.0062
_refine_ls_shift/su_mean         0.0008
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  519 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 0.2309 0.4094 '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
Ni1 Ni 0.6606(2) 0.2537(2) 0.32059(18) Uani 0.0464(6) 2 1 d . . .
N1 N 0.9764(15) 0.257(2) 0.9538(13) Uani 0.055(4) 2 1 d . . .
O1 O 0.4065(15) 0.3967(11) 0.1060(11) Uani 0.058(3) 2 1 d . . .
O2 O 0.6785(16) 0.3914(10) 0.5601(12) Uani 0.057(3) 2 1 d . . .
C3 C 0.958(2) -0.0233(14) 0.5508(19) Uani 0.057(3) 2 1 d . . .
O4 O 0.6978(15) 0.1094(11) 0.1063(11) Uani 0.058(3) 2 1 d . . .
O5 O 0.3921(16) 0.1110(11) 0.2966(12) Uani 0.057(3) 2 1 d . . .
C2 C 0.590(2) 0.5305(15) 0.549(2) Uani 0.057(3) 2 1 d . . .
O3 O 0.8833(15) 0.1151(10) 0.5589(11) Uani 0.057(3) 2 1 d . . .
O6 O 0.9026(15) 0.3931(11) 0.2935(12) Uani 0.057(3) 2 1 d . . .
C1 C 0.452(3) 0.4984(19) -0.002(2) Uani 0.058(3) 2 1 d . . .
H1c1 H 0.594568 0.493605 -0.005988 Uiso 0.0694 2 1 d . . .
H1c2 H 0.503856 0.578565 0.41487 Uiso 0.0689 2 1 d . . .
H1c3 H 0.908637 -0.072299 0.416802 Uiso 0.0689 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
Ni1 O1 . . 2.055(8) ?
Ni1 O2 . . 2.019(9) ?
Ni1 O4 . . 2.052(10) ?
Ni1 O5 . . 2.050(10) ?
Ni1 O3 . . 2.022(8) ?
Ni1 O6 . . 2.032(11) ?
O1 C1 . . 1.26(2) ?
O2 C2 . . 1.252(15) ?
C3 O3 . . 1.237(16) ?
C3 O6 . 2_746 1.284(13) ?
C3 H1c1 . . 0.96 ?
O4 C1 . 2_645 1.310(17) ?
O5 C2 . 2_646 1.261(17) ?
C2 H1c2 . . 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
? ? ? ? ? ? ? ?

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_ANiF_c2_p08         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      13.20 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_ANiF_c2_p08         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_THETM01_ANiF_c2_p08         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT043_ANiF_c2_p08         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.05 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_ANiF_c2_p08         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.        2        100 %Fit  
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT113_ANiF_c2_p08         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT430_ANiF_c2_p08         
;
PROBLEM: Short Inter D...A Contact  O3       ..N1               2.89 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_ANiF_c2_p08         
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, giving broader and lower resolution reflections. 
Six overlapping twin domains are formed upon the transition,
and while we refine all six domains in JANA, data integration
in CrysAlisPro was performed on each domain individually. 
Thus there may be a loss in  the accuracy of determined intensities
and peak positions during the data integration of each domain.
;
_vrf_PLAT034_ANiF_c2_p08         
;
PROBLEM: No Flack Parameter Given. Z > Si, NonCentro ....     Please Do ! 
RESPONSE: In the P6322 structure before the phase transition, 
the flack parameter was refined to 0.00(9), and so the same absolute 
configuration was kept for the high-pressure phase.
;
_vrf_PLAT041_ANiF_c2_p08         
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: The positions of the hydrogen atoms on the ammoniun
cation could not be located in the Fourier difference maps,
and were excluded from the refinement.
;
_vrf_PLAT232_ANiF_c2_p08         
;
PROBLEM: Hirshfeld Test Diff (M-X) Ni1      --O4        .        5.3 s.u.  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_PLAT250_ANiF_c2_p08         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.1 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ANiF_c2_p09
_database_code_depnum_ccdc_archive 'CCDC 1861357'
_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 Ni O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 N1 Ni1 O6'
_chemical_formula_weight         211.8
_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                   6.470(2)
_cell_length_b                   8.0553(8)
_cell_length_c                   7.263(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.33(4)
_cell_angle_gamma                90
_cell_volume                     339.26(19)

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 0.188(4) 1 0 0 0 1 0 0 0 1
2 0.1772(15) 1 0 0 0 -1 0 0.789 0 -1
3 0.1518(14) -0.0714 0 -1.0864 0 1 0 0.8594 0 -0.9286
4 0.1679(17) -0.9286 0 1.0864 0 -1 0 0.1267 0 0.9286
5 0.1641(16) -0.9286 0 1.0864 0 1 0 -0.8594 0 -0.0714
6 0.1507(16) -0.0714 0 -1.0864 0 -1 0 -0.9157 0 0.0714

_cell_formula_units_Z            2

_cell_measurement_reflns_used    118
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      12.57
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.0731
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             216

_exptl_absorpt_coefficient_mu    0.63
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            green
_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  0.779
_exptl_absorpt_correction_T_max  1
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
? ? ? ?

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_pressure         '1.90 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     0.41128
_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            3405
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         13.23
_diffrn_reflns_theta_full        11.93
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

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

_diffrn_radiation_probe          X-ray

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

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             3405
_reflns_number_gt                2083
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0896
_refine_ls_wR_factor_gt          0.1010
_refine_ls_R_factor_all          0.1163
_refine_ls_wR_factor_ref         0.1075
_refine_ls_goodness_of_fit_ref   2.12
_refine_ls_goodness_of_fit_gt    2.55
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3405
_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          0.0352
_refine_ls_shift/su_mean         0.0043
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  899 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 0.2309 0.4094 '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
Ni1 Ni 0.6608(2) 0.2535(2) 0.31932(17) Uani 0.0543(6) 2 1 d . . .
N1 N 0.9793(13) 0.2508(19) 0.9511(12) Uani 0.059(4) 2 1 d . . .
O1 O 0.4063(13) 0.3982(10) 0.1081(10) Uani 0.060(2) 2 1 d . . .
O2 O 0.6778(14) 0.3945(9) 0.5568(11) Uani 0.064(3) 2 1 d . . .
C3 C 0.953(2) -0.0274(13) 0.5524(18) Uani 0.064(3) 2 1 d . . .
O4 O 0.6976(13) 0.1104(10) 0.1064(10) Uani 0.060(2) 2 1 d . . .
O5 O 0.3859(14) 0.1137(10) 0.2944(11) Uani 0.064(3) 2 1 d . . .
C2 C 0.596(2) 0.5350(14) 0.5481(18) Uani 0.064(3) 2 1 d . . .
O3 O 0.8817(14) 0.1125(9) 0.5575(11) Uani 0.064(3) 2 1 d . . .
O6 O 0.9098(14) 0.3931(10) 0.2889(12) Uani 0.064(3) 2 1 d . . .
C1 C 0.451(2) 0.5016(18) -0.006(2) Uani 0.060(2) 2 1 d . . .
H1c1 H 0.594372 0.495678 -0.01502 Uiso 0.0717 2 1 d . . .
H1c2 H 0.515395 0.586635 0.416017 Uiso 0.0773 2 1 d . . .
H1c3 H 0.902648 -0.080165 0.420949 Uiso 0.0769 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
Ni1 O1 . . 2.045(7) ?
Ni1 O2 . . 2.027(8) ?
Ni1 O4 . . 2.026(8) ?
Ni1 O5 . . 2.044(9) ?
Ni1 O3 . . 2.033(7) ?
Ni1 O6 . . 2.055(10) ?
O1 C1 . . 1.296(18) ?
O2 C2 . . 1.239(14) ?
C3 O3 . . 1.225(14) ?
C3 O6 . 2_746 1.273(12) ?
C3 H1c3 . . 0.96 ?
O4 C1 . 2_645 1.265(15) ?
O5 C2 . 2_646 1.267(16) ?
C2 H1c2 . . 0.96 ?
C1 H1c1 . . 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 . . . 92.3(3) ?
O1 Ni1 O4 . . . 94.6(3) ?
O1 Ni1 O5 . . . 82.4(3) ?
O1 Ni1 O3 . . . 170.1(4) ?
O1 Ni1 O6 . . . 90.9(3) ?
O2 Ni1 O4 . . . 171.1(3) ?
O2 Ni1 O5 . . . 95.8(4) ?
O2 Ni1 O3 . . . 80.6(3) ?
O2 Ni1 O6 . . . 92.1(4) ?
O4 Ni1 O5 . . . 90.6(4) ?
O4 Ni1 O3 . . . 93.2(3) ?
O4 Ni1 O6 . . . 82.3(4) ?
O5 Ni1 O3 . . . 91.3(3) ?
O5 Ni1 O6 . . . 169.9(3) ?
O3 Ni1 O6 . . . 96.2(3) ?
Ni1 O1 C1 . . . 120.9(8) ?
Ni1 O2 C2 . . . 127.4(7) ?
O3 C3 O6 . . 2_746 123.8(11) ?
O3 C3 H1c3 . . . 118.11 ?
O6 C3 H1c3 2_746 . . 118.11 ?
Ni1 O4 C1 . . 2_645 121.1(10) ?
Ni1 O5 C2 . . 2_646 117.9(7) ?
O2 C2 O5 . . 2_656 123.0(10) ?
O2 C2 H1c2 . . . 118.5 ?
O5 C2 H1c2 2_656 . . 118.5 ?
Ni1 O3 C3 . . . 128.3(7) ?
Ni1 O6 C3 . . 2_756 116.3(9) ?
O1 C1 O4 . . 2_655 119.1(14) ?
O1 C1 H1c1 . . . 120.46 ?
O4 C1 H1c1 2_655 . . 120.46 ?

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 O5 . . 2_655 0.96 2.29 2.88(2) 118.20 ?
C1 H1c1 O6 . . . 0.96 2.39 2.921(14) 114.27 ?



# start Validation Reply Form
_vrf_PLAT027_ANiF_c2_p09         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      11.93 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_ANiF_c2_p09         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_THETM01_ANiF_c2_p09         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT043_ANiF_c2_p09         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.05 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_ANiF_c2_p09         
;
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_ANiF_c2_p09         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT430_ANiF_c2_p09         
;
PROBLEM: Short Inter D...A Contact  O3       ..N1               2.87 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_ANiF_c2_p09         
;
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_ANiF_c2_p09         
;
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_ANiF_c2_p09         
;
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_PLAT232_ANiF_c2_p09         
;
PROBLEM: Hirshfeld Test Diff (M-X) Ni1      --O5        .        5.3 s.u.  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_PLAT250_ANiF_c2_p09         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.9 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ANiF_c2_p10
_database_code_depnum_ccdc_archive 'CCDC 1861358'
_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 Ni O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 N1 Ni1 O6'
_chemical_formula_weight         211.8
_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                   6.426(3)
_cell_length_b                   8.0477(10)
_cell_length_c                   7.255(3)
_cell_angle_alpha                90
_cell_angle_beta                 116.12(5)
_cell_angle_gamma                90
_cell_volume                     336.9(3)

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.180(4) 1 0 0 0 1 0 0 0 1
2 0.1770(16) 1 0 0 0 -1 0 0.7799 0 -1
3 0.1523(16) -0.0754 0 -1.089 0 1 0 0.8543 0 -0.9246
4 0.1799(18) -0.9246 0 1.089 0 -1 0 0.1332 0 0.9247
5 0.1794(16) -0.9246 0 1.089 0 1 0 -0.8543 0 -0.0754
6 0.1316(14) -0.0754 0 -1.089 0 -1 0 -0.9131 0 0.0753

_cell_formula_units_Z            2

_cell_measurement_reflns_used    119
_cell_measurement_theta_min      2.05
_cell_measurement_theta_max      12.58
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.0878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             208

_exptl_absorpt_coefficient_mu    0.634
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            green
_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  0.795
_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         '2.02 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     0.41128
_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            2736
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         13.47
_diffrn_reflns_theta_full        11.94
_diffrn_measured_fraction_theta_max 0.9
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

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

_diffrn_radiation_probe          X-ray

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

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             2736
_reflns_number_gt                1880
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.0853
_refine_ls_wR_factor_gt          0.0945
_refine_ls_R_factor_all          0.1050
_refine_ls_wR_factor_ref         0.0997
_refine_ls_goodness_of_fit_ref   2.35
_refine_ls_goodness_of_fit_gt    2.69
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         2736
_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          0.0433
_refine_ls_shift/su_mean         0.0042
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  736 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 0.2309 0.4094 '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
Ni1 Ni 0.6607(3) 0.2536(2) 0.31888(19) Uani 0.0644(7) 2 1 d . . .
N1 N 0.9785(14) 0.253(2) 0.9477(12) Uani 0.064(4) 2 1 d . . .
O1 O 0.4058(14) 0.3986(11) 0.1074(11) Uani 0.073(3) 2 1 d . . .
O2 O 0.6768(16) 0.3940(10) 0.5573(12) Uani 0.076(3) 2 1 d . . .
C3 C 0.951(2) -0.0260(15) 0.553(2) Uani 0.076(3) 2 1 d . . .
O4 O 0.7004(16) 0.1081(11) 0.1082(11) Uani 0.073(3) 2 1 d . . .
O5 O 0.3836(16) 0.1156(11) 0.2934(13) Uani 0.076(3) 2 1 d . . .
C2 C 0.601(2) 0.5346(15) 0.551(2) Uani 0.076(3) 2 1 d . . .
O3 O 0.8778(16) 0.1120(10) 0.5556(12) Uani 0.076(3) 2 1 d . . .
O6 O 0.9136(15) 0.3925(11) 0.2912(13) Uani 0.076(3) 2 1 d . . .
C1 C 0.450(3) 0.503(2) -0.005(2) Uani 0.073(3) 2 1 d . . .
H1c1 H 0.596418 0.500296 -0.009829 Uiso 0.0878 2 1 d . . .
H1c2 H 0.52486 0.587338 0.419302 Uiso 0.0913 2 1 d . . .
H1c3 H 0.902187 -0.078078 0.421639 Uiso 0.0916 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
Ni1 O1 . . 2.046(8) ?
Ni1 O2 . . 2.030(9) ?
Ni1 O4 . . 2.029(10) ?
Ni1 O5 . . 2.037(10) ?
Ni1 O3 . . 2.021(8) ?
Ni1 O6 . . 2.054(10) ?
O1 C1 . . 1.28(2) ?
O2 C2 . . 1.225(15) ?
C3 O3 . . 1.209(15) ?
C3 O6 . 2_746 1.264(14) ?
C3 H1c3 . . 0.96 ?
O4 C1 . 2_645 1.253(17) ?
O5 C2 . 2_646 1.268(18) ?
C2 H1c2 . . 0.96 ?
C1 H1c1 . . 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 . . . 92.6(3) ?
O1 Ni1 O4 . . . 95.1(3) ?
O1 Ni1 O5 . . . 82.2(4) ?
O1 Ni1 O3 . . . 169.8(4) ?
O1 Ni1 O6 . . . 91.3(4) ?
O2 Ni1 O4 . . . 170.7(3) ?
O2 Ni1 O5 . . . 95.5(4) ?
O2 Ni1 O3 . . . 80.4(3) ?
O2 Ni1 O6 . . . 92.0(4) ?
O4 Ni1 O5 . . . 90.7(4) ?
O4 Ni1 O3 . . . 92.6(4) ?
O4 Ni1 O6 . . . 82.7(4) ?
O5 Ni1 O3 . . . 91.0(4) ?
O5 Ni1 O6 . . . 170.3(3) ?
O3 Ni1 O6 . . . 96.3(4) ?
Ni1 O1 C1 . . . 121.4(9) ?
Ni1 O2 C2 . . . 127.8(8) ?
O3 C3 O6 . . 2_746 125.6(12) ?
O3 C3 H1c3 . . . 117.17 ?
O6 C3 H1c3 2_746 . . 117.18 ?
Ni1 O4 C1 . . 2_645 121.4(12) ?
Ni1 O5 C2 . . 2_646 118.5(7) ?
O2 C2 O5 . . 2_656 124.6(11) ?
O2 C2 H1c2 . . . 117.7 ?
O5 C2 H1c2 2_656 . . 117.7 ?
Ni1 O3 C3 . . . 129.3(8) ?
Ni1 O6 C3 . . 2_756 117.3(10) ?
O1 C1 O4 . . 2_655 119.7(16) ?
O1 C1 H1c1 . . . 120.17 ?
O4 C1 H1c1 2_655 . . 120.17 ?

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 O5 . . 2_655 0.96 2.31 2.89(2) 117.70 ?
C1 H1c1 O6 . . . 0.96 2.40 2.942(16) 115.43 ?


# start Validation Reply Form
_vrf_PLAT027_ANiF_c2_p10         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      11.94 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_ANiF_c2_p10         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_THETM01_ANiF_c2_p10         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT043_ANiF_c2_p10         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.05 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_ANiF_c2_p10         
;
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_ANiF_c2_p10         
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group      C2221 Check 
RESPONSE: The C2221 space group was tested and could be used for
data integration and structure refinement. However, the reproducible
sixfold twinning upon recompression and from several tested crystals
suggest that the monoclinic cell is formed upon the transition,
as sixfold twinning from an orthorhombic cell could only occur from the crystal
breaking into two domains.
;
_vrf_PLAT430_ANiF_c2_p10         
;
PROBLEM: Short Inter D...A Contact  O3       ..N1               2.86 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_ANiF_c2_p10         
;
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_ANiF_c2_p10         
;
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_ANiF_c2_p10         
;
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_PLAT250_ANiF_c2_p10         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.3 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ANiF_c2_p11
_database_code_depnum_ccdc_archive 'CCDC 1861359'
_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 Ni O6, N H4'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C3 H7 N1 Ni1 O6'
_chemical_formula_weight         211.8
_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                   6.373(5)
_cell_length_b                   8.036(2)
_cell_length_c                   7.247(5)
_cell_angle_alpha                90
_cell_angle_beta                 115.83(9)
_cell_angle_gamma                90
_cell_volume                     334.1(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 0.184698 1 0 0 0 1 0 0 0 1
2 0.182594 1 0 0 0 -1 0 0.7663 0 -1
3 0.148724 -0.0808 0 -1.0941 0 1 0 0.8461 0 -0.9192
4 0.182207 -0.9192 0 1.0941 0 -1 0 0.1417 0 0.9192
5 0.182907 -0.9192 0 1.0941 0 1 0 -0.8461 0 -0.0808
6 0.11887 -0.0808 0 -1.0941 0 -1 0 -0.908 0 0.0808

_cell_formula_units_Z            2

_cell_measurement_reflns_used    114
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      12.2
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    2.1053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             208

_exptl_absorpt_coefficient_mu    0.639
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            green
_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  0.71
_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         '2.19 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     0.41128
_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            3348
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         13.21
_diffrn_reflns_theta_full        11.95
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_reduction_process ?

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

_diffrn_radiation_probe          X-ray

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

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             3348
_reflns_number_gt                2143
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           0.1037
_refine_ls_wR_factor_gt          0.1186
_refine_ls_R_factor_all          0.1304
_refine_ls_wR_factor_ref         0.1251
_refine_ls_goodness_of_fit_ref   2.59
_refine_ls_goodness_of_fit_gt    3.07
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         3348
_refine_ls_number_parameters     64
_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          0.0418
_refine_ls_shift/su_mean         0.0081
_refine_diff_density_max         ?
_refine_diff_density_min         ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;  883 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 0.2309 0.4094 '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
Ni1 Ni 0.6609(3) 0.2535(3) 0.3177(2) Uani 0.0589(7) 2 1 d . . .
N1 N 0.9812(18) 0.253(2) 0.9403(13) Uani 0.064(5) 2 1 d . . .
O1 O 0.4051(16) 0.4004(13) 0.1103(12) Uani 0.068(3) 2 1 d . . .
O2 O 0.6731(18) 0.3949(12) 0.5562(13) Uani 0.071(3) 2 1 d . . .
C3 C 0.944(3) -0.0289(17) 0.547(2) Uani 0.084(4) 2 1 d . . .
O4 O 0.6974(18) 0.1082(12) 0.1090(13) Uani 0.068(3) 2 1 d . . .
O5 O 0.3823(18) 0.1131(12) 0.2951(14) Uani 0.071(3) 2 1 d . . .
C2 C 0.608(2) 0.5378(18) 0.549(2) Uani 0.071(3) 2 1 d . . .
O3 O 0.8807(18) 0.1113(12) 0.5531(14) Uani 0.084(4) 2 1 d . . .
O6 O 0.9173(17) 0.3916(13) 0.2914(15) Uani 0.084(4) 2 1 d . . .
C1 C 0.444(3) 0.501(2) -0.001(3) Uani 0.068(3) 2 1 d . . .
H1c1 H 0.593215 0.496394 -0.004483 Uiso 0.0816 2 1 d . . .
H1c2 H 0.54616 0.595173 0.419849 Uiso 0.0852 2 1 d . . .
H1c3 H 0.887682 -0.083846 0.41682 Uiso 0.1003 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
Ni1 O1 . . 2.044(9) ?
Ni1 O2 . . 2.041(11) ?
Ni1 O4 . . 2.003(11) ?
Ni1 O5 . . 2.049(12) ?
Ni1 O3 . . 2.024(9) ?
Ni1 O6 . . 2.052(12) ?
O1 C1 . . 1.25(2) ?
O2 C2 . . 1.215(18) ?
C3 O3 . . 1.203(17) ?
C3 O6 . 2_746 1.288(17) ?
C3 H1c3 . . 0.96 ?
O4 C1 . 2_645 1.244(18) ?
O5 C2 . 2_646 1.26(2) ?
C2 H1c2 . . 0.96 ?
C1 H1c1 . . 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 . . . 91.4(4) ?
O1 Ni1 O4 . . . 95.7(4) ?
O1 Ni1 O5 . . . 82.7(4) ?
O1 Ni1 O3 . . . 169.6(5) ?
O1 Ni1 O6 . . . 91.8(4) ?
O2 Ni1 O4 . . . 171.8(4) ?
O2 Ni1 O5 . . . 95.0(5) ?
O2 Ni1 O3 . . . 81.0(4) ?
O2 Ni1 O6 . . . 92.3(5) ?
O4 Ni1 O5 . . . 90.0(5) ?
O4 Ni1 O3 . . . 92.4(4) ?
O4 Ni1 O6 . . . 83.5(5) ?
O5 Ni1 O3 . . . 90.8(4) ?
O5 Ni1 O6 . . . 171.0(4) ?
O3 Ni1 O6 . . . 95.6(4) ?
Ni1 O1 C1 . . . 122.2(10) ?
Ni1 O2 C2 . . . 127.1(10) ?
O3 C3 O6 . . 2_746 122.7(15) ?
O3 C3 H1c3 . . . 118.63 ?
O6 C3 H1c3 2_746 . . 118.63 ?
Ni1 O4 C1 . . 2_645 125.8(13) ?
Ni1 O5 C2 . . 2_646 119.3(8) ?
O2 C2 O5 . . 2_656 122.2(13) ?
O2 C2 H1c2 . . . 118.89 ?
O5 C2 H1c2 2_656 . . 118.88 ?
Ni1 O3 C3 . . . 128.2(10) ?
Ni1 O6 C3 . . 2_756 116.4(12) ?
O1 C1 O4 . . 2_655 124.1(18) ?
O1 C1 H1c1 . . . 117.95 ?
O4 C1 H1c1 2_655 . . 117.94 ?

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 O5 . . 2_655 0.96 2.37 2.93(2) 116.92 ?
C1 H1c1 O6 . . . 0.96 2.39 2.965(18) 118.03 ?


# start Validation Reply Form
_vrf_PLAT027_ANiF_c2_p11         
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      11.95 Degree
RESPONSE: The crystal quality deteriorated after the high-pressure
phase transition, and the reflections diffracted to lower resolution.
;
_vrf_PLAT902_ANiF_c2_p11         
;
PROBLEM: No (Interpretable) Reflections Found in FCF ....     Please Check
RESPONSE: The structure factor list contains information about which
reflections belong to the corresponding twin domain. This format cannot
be read by checkcif.
;
_vrf_THETM01_ANiF_c2_p11         
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to the loss in resolution in the high-pressure phase, the 
integration was performed to a resolution limit of 0.9 A in order to reduce
the risk of integrating diamond peaks.
;
_vrf_PLAT043_ANiF_c2_p11         
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.05 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_ANiF_c2_p11         
;
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_ANiF_c2_p11         
;
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_ANiF_c2_p11         
;
PROBLEM: s.u. on the   beta   Angle is Too Large ........       0.09 Degree
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_PLAT430_ANiF_c2_p11         
;
PROBLEM: Short Inter D...A Contact  O3       ..N1               2.83 Ang.  
RESPONSE: This contact may contain a hydrogen bond from the ammonium cation.
;
_vrf_GOODF01_ANiF_c2_p11         
;
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_ANiF_c2_p11         
;
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_ANiF_c2_p11         
;
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_PLAT232_ANiF_c2_p11         
;
PROBLEM: Hirshfeld Test Diff (M-X) Ni1      --O2        .        6.5 s.u.  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_PLAT234_ANiF_c2_p11         
;
PROBLEM: Large Hirshfeld Difference O5       --C2_b             0.16 Ang.  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
_vrf_PLAT250_ANiF_c2_p11         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.9 Note  
RESPONSE: Systematic errors may have arisen due to the difficulty in
refining six twin domains simulatenously that were integrated separately.
;
# end Validation Reply Form
