# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1NH4NiBiSCN6_20K_neutron
_database_code_depnum_ccdc_archive 'CCDC 2045258'
loop_
_audit_author_name
_audit_author_address
'Laura Canadillas Delgado'
;ILL
France
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_audit_creation_date             2020-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Ammonium nickel hexathiocyanatobismuthate'
_chemical_formula_moiety         'Bi0.667 C4 N4 Ni0.667 S4, 0.667(H4 N)'
_chemical_formula_sum            'C4 H2.67 Bi0.67 N4.67 Ni0.67 S4'
_chemical_formula_weight         422.81
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
S S 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Ni Ni 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Bi Bi 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.44100(10)
_cell_length_b                   8.68990(10)
_cell_length_c                   11.8177(2)
_cell_angle_alpha                97.5740(10)
_cell_angle_beta                 92.1370(10)
_cell_angle_gamma                91.8170(10)
_cell_volume                     858.10(2)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9374
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      60.791
_cell_measurement_theta_min      4.585
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.04734
_exptl_absorpt_correction_T_max  0.9203
_exptl_absorpt_correction_T_min  0.8824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          2.9
_exptl_crystal_size_mid          2.5
_exptl_crystal_size_min          2.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18745
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        34.566
_diffrn_reflns_theta_max         60.791
_diffrn_reflns_theta_min         4.585
_diffrn_ambient_temperature      20(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  'D19, Institut Laue Langevin'
_diffrn_measurement_method       ?
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     0.94558
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9374
_reflns_number_total             9590
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.227
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         9590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0448
_refine_ls_restrained_S_all      1.151
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0394P)²+6.1942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1117
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Bi1 Bi 0.500000 0.500000 1.000000 0.00459(7) Uani 1 2 d S . P . .
Bi2 Bi 0.000000 0.000000 0.500000 0.00465(7) Uani 1 2 d S . P . .
Ni2 Ni -0.500000 0.500000 0.500000 0.00535(6) Uani 1 2 d S . P . .
Ni1 Ni 0.000000 0.000000 1.000000 0.00541(6) Uani 1 2 d S . P . .
S1 S 0.52248(16) 0.21782(15) 1.09151(12) 0.00909(17) Uani 1 1 d . . . . .
S6 S -0.75994(16) 0.40238(15) 0.84661(10) 0.00814(17) Uani 1 1 d . . . . .
S5 S -0.76350(17) 0.00749(15) 0.33798(10) 0.00854(17) Uani 1 1 d . . . . .
S3 S -0.28623(16) 0.39014(15) 0.83227(10) 0.00790(17) Uani 1 1 d . . . . .
S4 S 0.02457(16) 0.32292(14) 0.55173(11) 0.00801(17) Uani 1 1 d . . . . .
S2 S 0.27108(16) -0.01003(16) 0.64569(10) 0.00886(17) Uani 1 1 d . . . . .
N1 N 0.19790(5) 0.13121(5) 1.06827(3) 0.00935(6) Uani 1 1 d . . . . .
N2 N 0.10638(5) -0.02508(5) 0.84646(3) 0.00908(6) Uani 1 1 d . . . . .
N6 N -0.59448(5) 0.45925(5) 0.65232(3) 0.00915(6) Uani 1 1 d . . . . .
N4 N -0.29915(5) 0.38809(5) 0.53468(3) 0.00904(6) Uani 1 1 d . . . . .
N3 N -0.10451(5) 0.19888(5) 0.95741(3) 0.00958(6) Uani 1 1 d . . . . .
N5 N -0.61122(5) 0.29499(5) 0.42333(3) 0.00945(6) Uani 1 1 d . . . . .
C5 C -0.67360(7) 0.17571(6) 0.39008(4) 0.00806(8) Uani 1 1 d . . . . .
C4 C -0.16729(7) 0.35555(6) 0.54105(4) 0.00782(8) Uani 1 1 d . . . . .
C6 C -0.66096(7) 0.43503(6) 0.73269(4) 0.00814(8) Uani 1 1 d . . . . .
C3 C -0.17848(7) 0.28076(6) 0.90800(4) 0.00815(8) Uani 1 1 d . . . . .
C2 C 0.17523(7) -0.01570(6) 0.76404(4) 0.00799(8) Uani 1 1 d . . . . .
C1 C 0.33210(7) 0.16816(6) 1.07687(5) 0.00803(8) Uani 1 1 d . . . . .
N7 N -0.03129(6) 0.65300(5) 0.74999(4) 0.01202(7) Uani 1 1 d . . . . .
H7A H 0.0717(3) 0.6119(4) 0.7784(3) 0.0418(5) Uani 1 1 d . . . . .
H7B H -0.1189(3) 0.5775(3) 0.7678(2) 0.0381(5) Uani 1 1 d . . . . .
H7C H -0.0490(4) 0.7602(3) 0.7926(2) 0.0431(6) Uani 1 1 d . . . . .
H7D H -0.0308(3) 0.6570(3) 0.66451(16) 0.0355(4) Uani 1 1 d . . . . .


_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
Bi1 S1 2.8163(13) 2_667 ?
Bi1 S1 2.8163(13) . ?
Bi1 S6 2.8284(13) 1_655 ?
Bi1 S6 2.8284(13) 2_567 ?
Bi1 S3 2.8237(12) 2_567 ?
Bi1 S3 2.8237(12) 1_655 ?
Bi2 S5 2.8222(13) 1_655 ?
Bi2 S5 2.8222(13) 2_456 ?
Bi2 S4 2.7915(12) . ?
Bi2 S4 2.7915(12) 2_556 ?
Bi2 S2 2.8225(14) 2_556 ?
Bi2 S2 2.8224(14) . ?
Ni2 N6 2.0637(4) 2_466 ?
Ni2 N6 2.0637(4) . ?
Ni2 N4 2.0361(4) 2_466 ?
Ni2 N4 2.0361(4) . ?
Ni2 N5 2.0691(4) . ?
Ni2 N5 2.0691(4) 2_466 ?
Ni1 N1 2.0683(4) . ?
Ni1 N1 2.0683(4) 2_557 ?
Ni1 N2 2.0435(4) . ?
Ni1 N2 2.0435(4) 2_557 ?
Ni1 N3 2.0763(4) . ?
Ni1 N3 2.0763(4) 2_557 ?
S1 C1 1.6475(15) . ?
S6 C6 1.6615(13) . ?
S5 C5 1.6581(14) . ?
S3 C3 1.6582(13) . ?
S4 C4 1.6560(14) . ?
S2 C2 1.6472(13) . ?
N1 C1 1.1646(7) . ?
N2 C2 1.1633(6) . ?
N6 C6 1.1604(6) . ?
N4 C4 1.1592(7) . ?
N3 C3 1.1609(6) . ?
N5 C5 1.1613(7) . ?
N7 H7A 1.013(2) . ?
N7 H7B 1.020(2) . ?
N7 H7C 1.017(2) . ?
N7 H7D 1.016(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
S1 Bi1 S1 180.0 2_667 . ?
S1 Bi1 S6 95.95(4) 2_667 2_567 ?
S1 Bi1 S6 84.05(4) . 2_567 ?
S1 Bi1 S6 84.05(4) 2_667 1_655 ?
S1 Bi1 S6 95.95(4) . 1_655 ?
S1 Bi1 S3 89.12(4) 2_667 2_567 ?
S1 Bi1 S3 90.88(4) 2_667 1_655 ?
S1 Bi1 S3 90.88(4) . 2_567 ?
S1 Bi1 S3 89.12(4) . 1_655 ?
S6 Bi1 S6 180.0 1_655 2_567 ?
S3 Bi1 S6 90.46(4) 2_567 2_567 ?
S3 Bi1 S6 89.54(4) 2_567 1_655 ?
S3 Bi1 S6 90.46(4) 1_655 1_655 ?
S3 Bi1 S6 89.54(4) 1_655 2_567 ?
S3 Bi1 S3 180.0 2_567 1_655 ?
S5 Bi2 S5 180.0 2_456 1_655 ?
S5 Bi2 S2 99.14(4) 1_655 2_556 ?
S5 Bi2 S2 80.86(4) 2_456 2_556 ?
S5 Bi2 S2 99.14(4) 2_456 . ?
S5 Bi2 S2 80.86(4) 1_655 . ?
S4 Bi2 S5 89.42(4) . 2_456 ?
S4 Bi2 S5 89.42(4) 2_556 1_655 ?
S4 Bi2 S5 90.58(4) 2_556 2_456 ?
S4 Bi2 S5 90.58(4) . 1_655 ?
S4 Bi2 S4 180.0 . 2_556 ?
S4 Bi2 S2 92.80(4) . 2_556 ?
S4 Bi2 S2 87.21(4) 2_556 2_556 ?
S4 Bi2 S2 92.80(4) 2_556 . ?
S4 Bi2 S2 87.20(4) . . ?
S2 Bi2 S2 180.0 . 2_556 ?
N6 Ni2 N6 180.0 . 2_466 ?
N6 Ni2 N5 91.468(16) 2_466 . ?
N6 Ni2 N5 88.532(16) 2_466 2_466 ?
N6 Ni2 N5 88.532(17) . . ?
N6 Ni2 N5 91.469(16) . 2_466 ?
N4 Ni2 N6 91.734(16) . . ?
N4 Ni2 N6 88.266(16) . 2_466 ?
N4 Ni2 N6 91.734(16) 2_466 2_466 ?
N4 Ni2 N6 88.267(16) 2_466 . ?
N4 Ni2 N4 180.0 . 2_466 ?
N4 Ni2 N5 91.523(17) 2_466 2_466 ?
N4 Ni2 N5 91.522(17) . . ?
N4 Ni2 N5 88.478(17) . 2_466 ?
N4 Ni2 N5 88.477(17) 2_466 . ?
N5 Ni2 N5 180.0 2_466 . ?
N1 Ni1 N1 180.0 2_557 . ?
N1 Ni1 N3 89.746(17) . 2_557 ?
N1 Ni1 N3 90.254(17) 2_557 2_557 ?
N1 Ni1 N3 90.255(17) . . ?
N1 Ni1 N3 89.745(17) 2_557 . ?
N2 Ni1 N1 87.987(17) . . ?
N2 Ni1 N1 87.987(17) 2_557 2_557 ?
N2 Ni1 N1 92.013(17) 2_557 . ?
N2 Ni1 N1 92.014(17) . 2_557 ?
N2 Ni1 N2 180.0 . 2_557 ?
N2 Ni1 N3 90.610(16) 2_557 . ?
N2 Ni1 N3 90.608(16) . 2_557 ?
N2 Ni1 N3 89.391(16) . . ?
N2 Ni1 N3 89.391(16) 2_557 2_557 ?
N3 Ni1 N3 180.00(2) . 2_557 ?
C1 S1 Bi1 96.38(6) . . ?
C6 S6 Bi1 93.32(6) . 1_455 ?
C5 S5 Bi2 98.72(5) . 1_455 ?
C3 S3 Bi1 98.94(5) . 1_455 ?
C4 S4 Bi2 97.29(6) . . ?
C2 S2 Bi2 96.45(6) . . ?
C1 N1 Ni1 155.54(4) . . ?
C2 N2 Ni1 169.39(4) . . ?
C6 N6 Ni2 173.76(4) . . ?
C4 N4 Ni2 162.05(4) . . ?
C3 N3 Ni1 160.91(4) . . ?
C5 N5 Ni2 173.79(4) . . ?
N5 C5 S5 177.93(7) . . ?
N4 C4 S4 175.79(7) . . ?
N6 C6 S6 178.62(7) . . ?
N3 C3 S3 177.08(7) . . ?
N2 C2 S2 177.66(7) . . ?
N1 C1 S1 178.62(7) . . ?
H7A N7 H7B 106.1(3) . . ?
H7A N7 H7C 110.0(3) . . ?
H7A N7 H7D 110.8(2) . . ?
H7C N7 H7B 109.3(3) . . ?
H7D N7 H7B 110.0(2) . . ?
H7D N7 H7C 110.4(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: butanone'
####################################################################### 
# 
# 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_1NH4NiBiSCN6_260K_neutron
_database_code_depnum_ccdc_archive 'CCDC 2045259'
loop_
_audit_author_name
_audit_author_address
'Laura Canadillas Delgado'
;ILL
France
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_audit_creation_date             2020-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'ammonium nickel hexathiocyanatobismuthate'
_chemical_formula_moiety         'Bi0.667 C4 N4 Ni0.667 S4, 0.667(H4 N)'
_chemical_formula_sum            'C4 H2.67 Bi0.67 N4.67 Ni0.67 S4'
_chemical_formula_weight         422.81
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
H H 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
N N 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
S S 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Ni Ni 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'
Bi Bi 0.0000 0.0000
'Neutron Data Booklet, ILL Grenoble, France (2003) ISBN 0-9704143-7-4'

# start Validation Reply Form
_vrf_PLAT029_1NH4NiBiSCN6_260K_neutron 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.745 Why?  
RESPONSE: Limited experiment time and long collection times meant full
collections at multiple temperatures was not feasible.
;
_vrf_PLAT939_1NH4NiBiSCN6_260K_neutron 
;
PROBLEM: Large Value of Not (SHELXL) Weight Optimized S .     616.56 Check 
RESPONSE: Limited experiment time and long collection times limited the
data quality.
;
_vrf_PLAT973_1NH4NiBiSCN6_260K_neutron 
;
PROBLEM: Check Calcd Positive Resid. Density on       Ni2       2.86 eA-3  
RESPONSE: Limited experiment time and long collection times limited the
data quality and led to significant ripples. Note, the units are 
incorrect in the alert as this is neutron data.
;
# end Validation Reply Form



_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4472(12)
_cell_length_b                   8.7119(10)
_cell_length_c                   11.9671(9)
_cell_angle_alpha                97.041(6)
_cell_angle_beta                 90.364(7)
_cell_angle_gamma                91.558(9)
_cell_volume                     873.67(17)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    4798
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      60.723
_cell_measurement_theta_min      4.552
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  0.9203
_exptl_absorpt_correction_T_min  0.8824
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          2.9
_exptl_crystal_size_mid          2.5
_exptl_crystal_size_min          2.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.745
_diffrn_reflns_Laue_measured_fraction_max 0.548
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9536
_diffrn_reflns_point_group_measured_fraction_full 0.745
_diffrn_reflns_point_group_measured_fraction_max 0.548
_diffrn_reflns_theta_full        34.562
_diffrn_reflns_theta_max         60.723
_diffrn_reflns_theta_min         4.552
_diffrn_ambient_temperature      260(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.745
_diffrn_measured_fraction_theta_max 0.548
_diffrn_measurement_device_type  'D19, Institut Laue Langevin'
_diffrn_measurement_method       ?
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     0.9455
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4798
_reflns_number_total             6293
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.564
_refine_diff_density_min         -2.165
_refine_diff_density_rms         0.276
_refine_ls_extinction_coef       0.076(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         6293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0963
_refine_ls_restrained_S_all      1.266
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2845
_refine_ls_wR_factor_ref         0.3111
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Bi1 Bi 0.500000 0.500000 0.000000 0.0338(3) Uani 1 2 d S . P . .
Bi2 Bi 0.000000 0.000000 0.500000 0.0331(3) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 0.500000 0.500000 0.0329(3) Uani 1 2 d S . P . .
Ni1 Ni 0.000000 0.000000 0.000000 0.0321(3) Uani 1 2 d S . P . .
S1 S 0.5143(6) 0.2203(6) 1.0953(5) 0.0556(14) Uani 1 1 d . . . . .
S6 S -0.7497(6) 0.3979(6) 0.8499(3) 0.0501(11) Uani 1 1 d . . . . .
S5 S -0.7637(6) 0.0201(5) 0.3377(3) 0.0534(11) Uani 1 1 d . . . . .
S3 S -0.2727(7) 0.3939(5) 0.8381(3) 0.0502(11) Uani 1 1 d . . . . .
S4 S 0.0196(6) 0.3196(5) 0.5649(5) 0.0577(13) Uani 1 1 d . . . . .
S2 S 0.2652(6) -0.0169(8) 0.6419(3) 0.0585(13) Uani 1 1 d . . . . .
N1 N 0.19652(15) 0.12824(15) 1.06361(10) 0.0446(3) Uani 1 1 d . . . . .
N2 N 0.10434(17) -0.01829(15) 0.84539(8) 0.0447(3) Uani 1 1 d . . . . .
N6 N -0.59536(16) 0.46310(14) 0.65368(9) 0.0433(3) Uani 1 1 d . . . . .
N4 N -0.29754(16) 0.39202(13) 0.53577(11) 0.0429(3) Uani 1 1 d . . . . .
N3 N -0.10463(18) 0.20106(15) 0.96315(12) 0.0491(4) Uani 1 1 d . . . . .
N5 N -0.60569(16) 0.29338(12) 0.43007(10) 0.0443(3) Uani 1 1 d . . . . .
C5 C -0.66985(19) 0.17982(15) 0.39410(11) 0.0363(3) Uani 1 1 d . . . . .
C4 C -0.1687(2) 0.35755(16) 0.54723(13) 0.0375(3) Uani 1 1 d . . . . .
C6 C -0.6563(2) 0.43614(17) 0.73481(11) 0.0384(4) Uani 1 1 d . . . . .
C3 C -0.1736(2) 0.28336(16) 0.91336(12) 0.0404(4) Uani 1 1 d . . . . .
C2 C 0.1711(2) -0.01448(17) 0.76166(10) 0.0377(3) Uani 1 1 d . . . . .
C1 C 0.3281(2) 0.16734(16) 1.07521(11) 0.0379(4) Uani 1 1 d . . . . .
N7 N -0.0169(4) 0.65718(19) 0.7545(2) 0.0741(7) Uani 1 1 d . . . . .
H H 0.0753(18) 0.620(5) 0.784(3) 0.327(18) Uani 1 1 d . . . . .
H7B H -0.0809(18) 0.5724(11) 0.7721(11) 0.147(5) Uani 1 1 d . . . . .
H7C H -0.042(2) 0.7491(11) 0.7852(15) 0.201(8) Uani 1 1 d . . . . .
H7D H -0.015(3) 0.650(2) 0.6774(11) 0.189(7) Uani 1 1 d . . . . .


_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
Bi1 S1 2.819(4) 2_666 ?
Bi1 S1 2.819(4) 1_554 ?
Bi1 S6 2.815(4) 1_654 ?
Bi1 S6 2.815(4) 2_566 ?
Bi1 S3 2.828(5) 2_566 ?
Bi1 S3 2.828(5) 1_654 ?
Bi2 S5 2.811(5) 1_655 ?
Bi2 S5 2.811(5) 2_456 ?
Bi2 S4 2.797(4) 2_556 ?
Bi2 S4 2.797(4) . ?
Bi2 S2 2.820(5) . ?
Bi2 S2 2.820(5) 2_556 ?
Ni2 N6 2.0698(11) 1_655 ?
Ni2 N6 2.0698(11) 2_566 ?
Ni2 N4 2.0420(13) 1_655 ?
Ni2 N4 2.0420(13) 2_566 ?
Ni2 N5 2.0667(10) 1_655 ?
Ni2 N5 2.0667(10) 2_566 ?
Ni1 N1 2.0635(10) 2_556 ?
Ni1 N1 2.0635(10) 1_554 ?
Ni1 N2 2.0449(12) 2_556 ?
Ni1 N2 2.0449(12) 1_554 ?
Ni1 N3 2.0766(13) 2_556 ?
Ni1 N3 2.0766(13) 1_554 ?
S1 C1 1.635(4) . ?
S6 C6 1.657(4) . ?
S5 C5 1.650(4) . ?
S3 C3 1.639(4) . ?
S4 C4 1.651(5) . ?
S2 C2 1.641(5) . ?
N1 C1 1.1561(19) . ?
N2 C2 1.1566(19) . ?
N6 C6 1.1481(18) . ?
N4 C4 1.149(2) . ?
N3 C3 1.1540(18) . ?
N5 C5 1.1494(15) . ?
N7 H 0.94(2) . ?
N7 H7B 0.949(12) . ?
N7 H7C 0.873(10) . ?
N7 H7D 0.917(15) . ?

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
S1 Bi1 S1 180.0(2) 1_554 2_666 ?
S1 Bi1 S3 90.41(16) 2_666 2_566 ?
S1 Bi1 S3 89.59(16) 1_554 2_566 ?
S1 Bi1 S3 90.41(16) 1_554 1_654 ?
S1 Bi1 S3 89.59(16) 2_666 1_654 ?
S6 Bi1 S1 85.17(12) 1_654 2_666 ?
S6 Bi1 S1 85.17(12) 2_566 1_554 ?
S6 Bi1 S1 94.83(12) 1_654 1_554 ?
S6 Bi1 S1 94.83(12) 2_566 2_666 ?
S6 Bi1 S6 180.0 2_566 1_654 ?
S6 Bi1 S3 88.75(14) 2_566 1_654 ?
S6 Bi1 S3 88.75(14) 1_654 2_566 ?
S6 Bi1 S3 91.25(14) 2_566 2_566 ?
S6 Bi1 S3 91.25(14) 1_654 1_654 ?
S3 Bi1 S3 180.0 2_566 1_654 ?
S5 Bi2 S5 180.0 2_456 1_655 ?
S5 Bi2 S2 82.17(14) 1_655 . ?
S5 Bi2 S2 97.83(14) 2_456 . ?
S5 Bi2 S2 97.83(14) 1_655 2_556 ?
S5 Bi2 S2 82.17(14) 2_456 2_556 ?
S4 Bi2 S5 88.53(16) 2_556 1_655 ?
S4 Bi2 S5 91.47(16) 2_556 2_456 ?
S4 Bi2 S5 91.47(16) . 1_655 ?
S4 Bi2 S5 88.53(16) . 2_456 ?
S4 Bi2 S4 180.0 . 2_556 ?
S4 Bi2 S2 93.88(17) . 2_556 ?
S4 Bi2 S2 86.12(17) . . ?
S4 Bi2 S2 93.88(17) 2_556 . ?
S4 Bi2 S2 86.12(17) 2_556 2_556 ?
S2 Bi2 S2 180.00(12) 2_556 . ?
N6 Ni2 N6 180.0 2_566 1_655 ?
N4 Ni2 N6 88.88(6) 2_566 1_655 ?
N4 Ni2 N6 91.12(6) 2_566 2_566 ?
N4 Ni2 N6 88.88(6) 1_655 2_566 ?
N4 Ni2 N6 91.12(6) 1_655 1_655 ?
N4 Ni2 N4 180.00(7) 2_566 1_655 ?
N4 Ni2 N5 88.35(5) 1_655 2_566 ?
N4 Ni2 N5 91.65(5) 1_655 1_655 ?
N4 Ni2 N5 91.65(5) 2_566 2_566 ?
N4 Ni2 N5 88.35(5) 2_566 1_655 ?
N5 Ni2 N6 91.21(5) 2_566 1_655 ?
N5 Ni2 N6 91.21(5) 1_655 2_566 ?
N5 Ni2 N6 88.79(5) 1_655 1_655 ?
N5 Ni2 N6 88.79(5) 2_566 2_566 ?
N5 Ni2 N5 180.0 2_566 1_655 ?
N1 Ni1 N1 180.00(10) 1_554 2_556 ?
N1 Ni1 N3 90.10(5) 1_554 2_556 ?
N1 Ni1 N3 89.90(5) 2_556 2_556 ?
N1 Ni1 N3 89.90(5) 1_554 1_554 ?
N1 Ni1 N3 90.10(5) 2_556 1_554 ?
N2 Ni1 N1 91.91(5) 2_556 1_554 ?
N2 Ni1 N1 91.91(5) 1_554 2_556 ?
N2 Ni1 N1 88.09(5) 2_556 2_556 ?
N2 Ni1 N1 88.09(5) 1_554 1_554 ?
N2 Ni1 N2 180.00(7) 2_556 1_554 ?
N2 Ni1 N3 88.75(6) 2_556 2_556 ?
N2 Ni1 N3 91.25(6) 2_556 1_554 ?
N2 Ni1 N3 88.75(6) 1_554 1_554 ?
N2 Ni1 N3 91.25(6) 1_554 2_556 ?
N3 Ni1 N3 180.00(9) 2_556 1_554 ?
C1 S1 Bi1 97.0(2) . 1_556 ?
C6 S6 Bi1 95.71(17) . 1_456 ?
C5 S5 Bi2 99.36(19) . 1_455 ?
C3 S3 Bi1 98.65(19) . 1_456 ?
C4 S4 Bi2 98.23(15) . . ?
C2 S2 Bi2 98.2(2) . . ?
C1 N1 Ni1 158.83(15) . 1_556 ?
C2 N2 Ni1 173.05(11) . 1_556 ?
C6 N6 Ni2 175.20(10) . 1_455 ?
C4 N4 Ni2 165.55(11) . 1_455 ?
C3 N3 Ni1 159.21(13) . 1_556 ?
C5 N5 Ni2 177.10(14) . 1_455 ?
N5 C5 S5 177.6(2) . . ?
N4 C4 S4 176.43(18) . . ?
N6 C6 S6 178.1(2) . . ?
N3 C3 S3 177.4(2) . . ?
N2 C2 S2 177.6(3) . . ?
N1 C1 S1 178.2(2) . . ?
H N7 H7B 93(2) . . ?
H7C N7 H 115(2) . . ?
H7C N7 H7B 117.0(14) . . ?
H7C N7 H7D 112.0(17) . . ?
H7D N7 H 112(2) . . ?
H7D N7 H7B 106.4(13) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_GuaSCN
_database_code_depnum_ccdc_archive 'CCDC 2045275'
loop_
_audit_author_name
_audit_author_address
'Matthew Cliffe'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_audit_creation_date             2019-08-15
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'guanidinium thiocyanate'
_chemical_formula_moiety         'C N S, C H6 N3'
_chemical_formula_sum            'C2 H6 N4 S'
_chemical_formula_weight         118.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C2 N4 H6 S'
_chemical_oxdiff_usercomment     
'omjclb #18016 in fomblin on micromount for MJC'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9352(6)
_cell_length_b                   7.0096(5)
_cell_length_c                   12.3675(7)
_cell_angle_alpha                90.894(5)
_cell_angle_beta                 104.311(7)
_cell_angle_gamma                101.787(7)
_cell_volume                     568.89(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.4830
_cell_measurement_theta_min      3.6280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.110
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             248
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 0 5 0.0503
3 -2 5 0.0590
0 4 2 0.0901
-4 0 1 0.0286
-2 -2 7 0.0604
-2 0 8 0.0525
0 4 0 0.0887
2 0 -8 0.0534
1 -4 -3 0.0907
-4 0 -1 0.0248
4 0 0 0.0199

_exptl_crystal_preparation       'as received'
_exptl_crystal_recrystallization_method 'from bottle'
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.047
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.0147 -0.0099 4.9754 0.7444 -0.3921 0.2852
3.0067 -2.0122 4.9779 0.9915 -0.4182 -0.1028
0.0235 3.9971 1.9754 0.0649 -0.0192 0.9509
-4.0032 0.0109 1.0304 -0.8093 -0.3914 -0.1666
-1.9955 -1.9992 7.0146 0.0262 -0.9875 -0.2834
-1.9838 -0.0006 8.0023 0.0587 -0.9971 0.1921
0.0187 3.9988 -0.0212 -0.0586 0.1945 0.8775
1.9838 0.0006 -8.0023 -0.0587 0.9971 -0.1921
0.9756 -3.9993 -2.9817 0.0911 0.1972 -0.9368
-4.0080 0.0125 -0.9662 -0.9329 -0.1776 -0.2400
4.0056 -0.0117 -0.0321 0.8711 0.2845 0.2033

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2392
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.681
_diffrn_reflns_theta_min         3.697
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1806
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00  32.00   1.00    1.00    --  -41.93  38.00 150.00   82
  2  ω    -92.00  -2.00   1.00    1.00    --  -41.93 125.00-150.00   90
  3  ω   -115.00 -14.00   1.00    1.00    --  -41.93 -57.00   0.00  101
  4  ω    -38.00  83.00   1.00    1.00    --   41.93 -19.00 -60.00  121
  5  ω      1.00  83.00   1.00    1.00    --   41.93 -99.00-120.00   82
  6  ω     80.00 178.00   1.00    1.86    --  105.94  45.00 -90.00   98
  7  ω     33.00  98.00   1.00    1.86    --  105.94 -45.00  60.00   65
  8  ω     27.00 111.00   1.00    1.86    --  105.94-103.00  68.00   84
  9  ω     30.00  91.00   1.00    1.86    --  105.94 -30.00   0.00   61
 10  ω     30.00  91.00   1.00    1.86    --  105.94 -30.00 150.00   61
 11  ω     24.00 110.00   1.00    1.86    --  105.94 -95.00 -60.00   86
 12  ω     33.00  98.00   1.00    1.86    --  105.94 -45.00 -60.00   65
 13  ω     33.00 118.00   1.00    1.86    --  105.94-125.00-150.00   85
 14  ω     30.00 139.00   1.00    1.86    --  105.94 -77.00-150.00  109
 15  ω     18.00 178.00   1.00    1.86    --  105.94   0.00-120.00  160
 16  ω     30.00  91.00   1.00    1.86    --  105.94 -30.00-120.00   61
 17  ω     94.00 178.00   1.00    1.86    --  105.94 125.00-120.00   84
 18  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00  30.00  109
 19  ω   -115.00 -14.00   1.00    1.00    --  -41.93 -57.00 150.00  101
 20  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00 120.00  109
 21  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00 -30.00  109
 22  ω   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00-120.00  109
 23  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 -60.00  101
 24  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 -30.00  101
 25  ω     53.00 178.00   1.00    1.86    --  105.94  15.00  60.00  125
 26  ω     73.00 178.00   1.00    1.86    --  105.94  77.00  30.00  105
 27  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 150.00  101
 28  ω     73.00 178.00   1.00    1.86    --  105.94  77.00-180.00  105
 29  ω     73.00 178.00   1.00    1.86    --  105.94  77.00-150.00  105
 30  ω     77.00 178.00   1.00    1.86    --  105.94  61.00 120.00  101
 31  ω     73.00 178.00   1.00    1.86    --  105.94  77.00   0.00  105
 32  ω     77.00 178.00   1.00    1.86    --  105.94  61.00  90.00  101
 33  ω   -116.00 -42.00   1.00    1.00    --  -41.93 -38.00-150.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2179114000
_diffrn_orient_matrix_UB_12      -0.0153606000
_diffrn_orient_matrix_UB_13      0.0613508000
_diffrn_orient_matrix_UB_21      0.0703046000
_diffrn_orient_matrix_UB_22      0.0477463000
_diffrn_orient_matrix_UB_23      -0.1071752000
_diffrn_orient_matrix_UB_31      0.0516811000
_diffrn_orient_matrix_UB_32      0.2193997000
_diffrn_orient_matrix_UB_33      0.0368301000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1975
_reflns_number_total             2256
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0898
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1190P)²+3.4535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2627
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2.a X=CH2 refined with riding coordinates:
 N003(H00A,H00B), N004(H00G,H00H), N005(H00I,H00J), N006(H00C,H00D), N009(H00E,
 H00F), N00A(H00K,H00L)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
S001 S 0.8059(2) 0.5908(2) 0.68433(11) 0.0325(4) Uani 1 1 d . . . . .
S002 S 0.7722(2) 1.0625(2) 0.91180(11) 0.0290(4) Uani 1 1 d . . . . .
N003 N 0.2574(8) 1.0879(7) 0.5218(4) 0.0307(11) Uani 1 1 d . . . . .
H00A H 0.290753 1.097377 0.593776 0.037 Uiso 1 1 calc R . . . .
H00B H 0.252204 1.191132 0.485500 0.037 Uiso 1 1 calc R . . . .
N004 N 0.2162(7) 0.4249(7) 1.0413(4) 0.0288(10) Uani 1 1 d . . . . .
H00G H 0.201126 0.314716 1.071164 0.035 Uiso 1 1 calc R . . . .
H00H H 0.207173 0.528371 1.076345 0.035 Uiso 1 1 calc R . . . .
N005 N 0.2675(7) 0.2794(7) 0.8862(4) 0.0294(10) Uani 1 1 d . . . . .
H00I H 0.290573 0.287315 0.821031 0.035 Uiso 1 1 calc R . . . .
H00J H 0.253630 0.168714 0.915686 0.035 Uiso 1 1 calc R . . . .
N006 N 0.2222(8) 0.7557(7) 0.5227(4) 0.0329(11) Uani 1 1 d . . . . .
H00C H 0.255469 0.764568 0.594681 0.039 Uiso 1 1 calc R . . . .
H00D H 0.194058 0.643221 0.486863 0.039 Uiso 1 1 calc R . . . .
N007 N 0.3875(8) 0.9529(7) 0.7579(4) 0.0319(11) Uani 1 1 d . . . . .
N008 N 0.3954(8) 0.4573(8) 0.6863(4) 0.0352(12) Uani 1 1 d . . . . .
N009 N 0.1582(8) 0.8994(7) 0.3560(4) 0.0315(11) Uani 1 1 d . . . . .
H00E H 0.149882 1.002086 0.319476 0.038 Uiso 1 1 calc R . . . .
H00F H 0.130219 0.786545 0.320550 0.038 Uiso 1 1 calc R . . . .
N00A N 0.2747(8) 0.6071(7) 0.8954(4) 0.0317(11) Uani 1 1 d . . . . .
H00K H 0.297786 0.615818 0.830271 0.038 Uiso 1 1 calc R . . . .
H00L H 0.265317 0.709307 0.931414 0.038 Uiso 1 1 calc R . . . .
C00B C 0.2535(7) 0.4355(8) 0.9404(4) 0.0237(11) Uani 1 1 d . . . . .
C00C C 0.5448(9) 0.9988(8) 0.8215(4) 0.0274(12) Uani 1 1 d . . . . .
C00D C 0.5628(9) 0.5121(8) 0.6842(4) 0.0286(12) Uani 1 1 d . . . . .
C00E C 0.2144(8) 0.9151(8) 0.4672(4) 0.0255(11) Uani 1 1 d . . . . .


_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
S001 C00D 1.663(6) . ?
S002 C00C 1.661(6) . ?
N003 C00E 1.319(7) . ?
N004 C00B 1.335(7) . ?
N005 C00B 1.308(7) . ?
N006 C00E 1.324(7) . ?
N007 C00C 1.156(8) . ?
N008 C00D 1.153(8) . ?
N009 C00E 1.330(7) . ?
N00A C00B 1.329(7) . ?

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
N005 C00B N004 120.6(5) . . ?
N005 C00B N00A 120.4(5) . . ?
N00A C00B N004 119.0(5) . . ?
N007 C00C S002 179.2(5) . . ?
N008 C00D S001 178.6(5) . . ?
N003 C00E N006 120.3(5) . . ?
N003 C00E N009 120.2(5) . . ?
N006 C00E N009 119.6(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.211
_oxdiff_exptl_absorpt_empirical_full_min 0.693
####################################################################### 
# 
# 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_3MeNH3NiBiSCN6
_database_code_depnum_ccdc_archive 'CCDC 2045278'
loop_
_audit_author_name
_audit_author_address
'Matthew Cliffe'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT214_3MeNH3NiBiSCN6      
;
PROBLEM: Atom C8MA      (Anion/Solvent) ADP max/min Ratio        5.1 prolat
RESPONSE: Cation is disordered.
;
# Added during the CSD deposition process: Wednesday 18 November 2020 06:33 PM
# end Validation Reply Form

_audit_creation_date             2020-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'Methylammonium nickel hexathiocyanatobismuthate'
_chemical_formula_moiety         'Bi C6 N6 Ni S6, C N'
_chemical_formula_sum            'C7 Bi N7 Ni S6'
_chemical_formula_weight         642.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         C7N7H6S6Ni1Bi1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/n 1'
_space_group_name_Hall           '-P 2yac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'

_cell_length_a                   12.21600(10)
_cell_length_b                   36.8375(4)
_cell_length_c                   24.5263(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.2240(10)
_cell_angle_gamma                90
_cell_volume                     11036.9(2)
_cell_formula_units_Z            24
_cell_measurement_reflns_used    18570
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      72.7830
_cell_measurement_theta_min      6.2390
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    26.251
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7152
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0312
0 24 -2 0.0066
0 -24 -1 0.0116
0 -2 -16 0.0328
0 2 16 0.0279
-8 1 0 0.0246

_exptl_crystal_preparation       'Evaporation from butanone'
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.022
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0003 -0.0034 -0.0034 0.0596 0.1110 -0.0057
0.4557 23.7361 -1.7368 -0.8530 0.5218 -0.0089
-0.3975 -23.8694 -0.5152 0.8456 -0.5171 -0.1326
0.2989 -2.4330 -15.8216 -0.0038 -0.0085 -1.0000
0.1663 2.3533 15.8315 0.0345 0.0586 0.9977
-7.9144 1.4455 0.4217 -0.5204 -0.8505 0.0758

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            123648
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.978
_diffrn_reflns_theta_min         3.600
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -5.00  38.00   1.00    5.00    --  -41.82  19.00-180.00   43
  2  ω   -130.00  46.00   1.00    5.00    --  -41.82   0.00   0.00  176
  3  ω     27.00  98.00   1.00    5.00    --   41.82-125.00  90.00   71
  4  ω     25.00  96.00   1.00    5.00    --   41.82-122.00 -68.00   71
  5  ω     28.00  57.00   1.00   20.00    --  104.36 -30.00 120.00   29
  6  ω     76.00 178.00   1.00   20.00    --  104.36  30.00  90.00  102
  7  ω     22.00 106.00   1.00   20.00    --  104.36 -94.00  90.00   84
  8  ω     28.00  57.00   1.00   20.00    --  104.36 -30.00 -90.00   29
  9  ω     28.00  57.00   1.00   20.00    --  104.36 -30.00 150.00   29
 10  ω     97.00 178.00   1.00   20.00    --  104.36 125.00 -90.00   81
 11  ω     97.00 178.00   1.00   20.00    --  104.36 125.00 150.00   81
 12  ω     31.00 112.00   1.00   20.00    --  104.36-125.00 -60.00   81
 13  ω     28.00  57.00   1.00   20.00    --  104.36 -30.00-180.00   29
 14  ω     31.00  72.00   1.00   20.00    --  104.36 -45.00-120.00   41
 15  ω     97.00 178.00   1.00   20.00    --  104.36 125.00 -30.00   81
 16  ω    103.00 178.00   1.00   20.00    --  104.36  77.00 -60.00   75
 17  ω     39.00 130.00   1.00   20.00    --  104.36-150.00 129.00   91
 18  ω     31.00  72.00   1.00   20.00    --  104.36 -45.00  60.00   41
 19  ω     28.00  57.00   1.00   20.00    --  104.36 -30.00 -60.00   29
 20  ω    103.00 178.00   1.00   20.00    --  104.36  77.00-180.00   75
 21  ω     28.00 127.00   1.00   20.00    --  104.36 -77.00-120.00   99
 22  ω   -116.00 -17.00   1.00    5.00    --  -41.82 -38.00-150.00   99
 23  ω   -114.00 -14.00   1.00    5.00    --  -41.82 -57.00 -30.00  100
 24  ω    -21.00  32.00   1.00    5.00    --  -41.82  38.00 120.00   53
 25  ω     14.00 114.00   1.00    5.00    --   41.82  57.00-180.00  100
 26  ω     76.00 118.00   1.00   20.00    --  104.36  30.00 -90.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0594501000
_diffrn_orient_matrix_UB_12      -0.0365669000
_diffrn_orient_matrix_UB_13      0.0069873000
_diffrn_orient_matrix_UB_21      0.1110664000
_diffrn_orient_matrix_UB_22      0.0198224000
_diffrn_orient_matrix_UB_23      -0.0004108000
_diffrn_orient_matrix_UB_31      -0.0054616000
_diffrn_orient_matrix_UB_32      0.0042984000
_diffrn_orient_matrix_UB_33      0.0624376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                18472
_reflns_number_total             21661
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1272
_refine_ls_number_reflns         21661
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0236P)²+68.6271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0962
_refine_special_details          'Refined as a 2-component twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.811(1)
 0.189(1)
2. Uiso/Uaniso restraints and constraints
Uanis(C51A) = Uanis(C51B)
Uanis(S50A) = Uanis(S50B)
Uanis(C54B) = Uanis(C54A)
Uanis(C21B) = Uanis(C21A)
Uanis(C7MB) = Uanis(C7MA)
Uanis(S54A) = Uanis(S54B) = Uanis(C54A) = Uanis(C54B)
Uanis(S42B) = Uanis(S42A)
Uanis(C50) = Uanis(S50A)
Uanis(C21B) = Uanis(S21B)
Uanis(C21A) = Uanis(S21A)
3. Others
 Sof(C7MB)=1-FVAR(1)
 Sof(C7MA)=FVAR(1)
 Sof(S52B)=1-FVAR(2)
 Sof(S52A)=FVAR(2)
 Sof(C54B)=Sof(S54B)=1-FVAR(3)
 Sof(C54A)=Sof(S54A)=FVAR(3)
 Sof(S50B)=1-FVAR(4)
 Sof(S50A)=FVAR(4)
 Sof(C51A)=Sof(S51A)=1-FVAR(5)
 Sof(C51B)=Sof(S51B)=FVAR(5)
 Sof(C21A)=Sof(S21A)=1-FVAR(6)
 Sof(C21B)=Sof(S21B)=FVAR(6)
 Sof(S22A)=1-FVAR(7)
 Sof(S22B)=FVAR(7)
 Sof(S20B)=1-FVAR(8)
 Sof(S20A)=FVAR(8)
 Sof(S42A)=1-FVAR(9)
 Sof(S42B)=FVAR(9)
 Fixed Sof: C1MA(0.5) C2MA(0.5) C4MA(0.5) C6MA(0.5) N1MA(0.5) N2MA(0.5)
 N4MA(0.5) N6MA(0.5)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Bi1 Bi 0.00540(2) 0.25553(2) 0.62944(2) 0.02050(7) Uani 1 1 d . . . . .
Bi2 Bi 0.49992(2) 0.41409(2) 0.62899(2) 0.01775(7) Uani 1 1 d . . . . .
Bi3 Bi 0.48574(2) 0.58738(2) 0.87218(2) 0.02028(7) Uani 1 1 d . . . . .
Bi4 Bi 0.49682(3) 0.91566(2) 0.86785(2) 0.02649(8) Uani 1 1 d . . . . .
Bi5 Bi 1.01092(2) 0.75295(2) 0.87220(2) 0.02055(7) Uani 1 1 d . . . . .
Bi6 Bi 0.01616(3) 0.08767(2) 0.87148(2) 0.02176(7) Uani 1 1 d . . . . .
C7MA C 0.2559(18) 0.8465(7) 0.9604(8) 0.056(5) Uani 0.58(2) 1 d . . P A 1
C1MA C -0.2015(17) -0.0244(6) 0.7432(10) 0.038(4) Uani 0.5 1 d . . P B -1
C2MA C 0.767(8) 0.1687(11) 0.746(5) 0.14(2) Uiso 0.5 1 d . . P C -1
C3MA C 0.2988(14) 0.5212(6) 0.9613(10) 0.145(12) Uani 1 1 d . . . . .
C4MA C 0.771(2) 0.4721(5) 0.7672(10) 0.045(6) Uani 0.5 1 d . . P D -1
C5MA C 0.7207(16) 0.6693(4) 1.0421(5) 0.085(6) Uani 1 1 d . . . . .
C6MA C 0.742(8) 0.6660(11) 0.745(3) 0.15(3) Uani 0.5 1 d . . P E -1
C7MB C 0.221(2) 0.8205(10) 0.9593(11) 0.056(5) Uani 0.42(2) 1 d . . P A 2
C8MA C 1.216(3) 1.0185(6) 0.9646(9) 0.23(2) Uani 1 1 d . . . . .
C10 C -0.0888(7) 0.0069(2) 0.5988(3) 0.0242(17) Uani 1 1 d . . . . .
C11 C 0.0625(7) 0.1142(2) 0.5020(4) 0.0303(19) Uani 1 1 d . . . . .
C12 C 0.0609(8) 0.1656(2) 0.6681(4) 0.031(2) Uani 1 1 d . . . . .
C13 C 0.2330(7) 0.0571(2) 0.6607(4) 0.0301(19) Uani 1 1 d . . . . .
C14 C -0.0869(6) 0.0694(2) 0.7410(4) 0.0267(18) Uani 1 1 d . . . . .
C15 C -0.2431(7) 0.1162(2) 0.6002(3) 0.0248(17) Uani 1 1 d . . . . .
C20 C -0.0609(8) 0.3403(2) 0.5787(4) 0.034(2) Uani 1 1 d . . . . .
C21A C -0.2400(16) 0.4518(6) 0.5991(8) 0.0319(7) Uani 0.552(5) 1 d . . P F 2
C21B C -0.2357(19) 0.4521(7) 0.6168(9) 0.0319(7) Uani 0.448(5) 1 d . . P F 1
C22 C 0.0564(9) 0.4455(2) 0.5035(4) 0.035(2) Uani 1 1 d . . . . .
C23 C 0.0904(6) 0.4969(2) 0.6641(3) 0.0196(16) Uani 1 1 d . . . . .
C24 C 0.2397(7) 0.3880(2) 0.6563(3) 0.0244(17) Uani 1 1 d . . . . .
C25 C -0.0825(6) 0.3930(2) 0.7426(3) 0.0227(17) Uani 1 1 d . . . . .
C30 C 0.4310(6) 0.5029(2) 0.6693(3) 0.0210(16) Uani 1 1 d . . . . .
C31 C 0.5894(7) 0.5659(2) 0.5077(3) 0.0231(17) Uani 1 1 d . . . . .
C32 C 0.7402(7) 0.5682(2) 0.6703(3) 0.0236(17) Uani 1 1 d . . . . .
C33 C 0.5874(6) 0.6625(2) 0.6030(3) 0.0223(16) Uani 1 1 d . . . . .
C34 C 0.4323(8) 0.6148(2) 0.7422(4) 0.0296(19) Uani 1 1 d . . . . .
C35 C 0.2640(7) 0.6080(2) 0.5808(3) 0.0252(17) Uani 1 1 d . . . . .
C40 C 0.5859(7) 0.6719(2) 0.9008(4) 0.0262(18) Uani 1 1 d . . . . .
C41 C 0.4274(7) 0.7238(2) 0.7571(4) 0.0267(18) Uani 1 1 d . . . . .
C42 C 0.7411(7) 0.7721(2) 0.8297(4) 0.0277(18) Uani 1 1 d . . . . .
C43 C 0.4157(6) 0.8305(2) 0.8374(4) 0.0272(19) Uani 1 1 d . . . . .
C44 C 0.5919(7) 0.7715(2) 0.9949(4) 0.0255(18) Uani 1 1 d . . . . .
C45 C 0.2659(7) 0.7324(3) 0.9232(3) 0.0280(18) Uani 1 1 d . . . . .
C55 C 1.0677(6) 0.9488(2) 0.7594(4) 0.0245(17) Uani 1 1 d . . . . .
C50 C 1.0840(7) 0.8405(2) 0.8406(4) 0.0304(15) Uani 1 1 d . . . . .
C51A C 1.2395(16) 0.9358(5) 0.9244(9) 0.026(4) Uani 0.631(9) 1 d . . P G 1
C51B C 1.232(3) 0.9202(8) 0.9255(17) 0.026(4) Uani 0.369(9) 1 d . . P G 2
C52 C 0.9388(10) 0.9991(2) 0.9168(4) 0.038(2) Uani 1 1 d . . . . .
C53 C 0.9082(7) 0.8915(2) 0.9934(4) 0.0251(18) Uani 1 1 d . . . . .
C54A C 0.756(2) 0.8939(7) 0.8317(12) 0.0274(10) Uani 0.521(8) 1 d . . P H 2
C54B C 0.766(2) 0.9000(7) 0.8284(13) 0.0274(10) Uani 0.479(8) 1 d . . P H 1
C60 C -0.0863(6) 0.2749(2) 0.7588(4) 0.0266(18) Uani 1 1 d . . . . .
C61 C 0.2386(6) 0.2810(2) 0.8372(4) 0.0239(17) Uani 1 1 d . . . . .
C62 C -0.0639(7) 0.3308(2) 0.9226(3) 0.0261(18) Uani 1 1 d . . . . .
C63 C 0.0648(6) 0.2209(2) 0.9950(4) 0.0244(17) Uani 1 1 d . . . . .
C64 C -0.2374(7) 0.2235(2) 0.8995(4) 0.0246(17) Uani 1 1 d . . . . .
C65 C 0.0709(7) 0.1743(2) 0.8311(4) 0.0278(18) Uani 1 1 d . . . . .
N1MA N -0.1892(15) -0.0256(5) 0.7847(10) 0.049(5) Uani 0.5 1 d . . P I -1
N2MA N 0.680(2) 0.1928(6) 0.7244(10) 0.074(7) Uani 0.5 1 d . . P . .
N3MA N 0.2026(12) 0.5216(3) 0.9498(8) 0.111(6) Uani 1 1 d . . . . .
N4MA N 0.6569(14) 0.4808(5) 0.7648(8) 0.042(4) Uani 0.5 1 d . . P D -1
N5MA N 0.7965(9) 0.6989(3) 1.0336(4) 0.059(3) Uani 1 1 d . . . . .
N6MA N 0.678(2) 0.6911(6) 0.7750(9) 0.062(6) Uani 0.5 1 d . . P E -1
N7MA N 0.3408(9) 0.8176(3) 0.9639(5) 0.068(3) Uani 1 1 d . . . . .
N8MA N 1.2870(16) 1.0393(3) 0.9708(6) 0.108(6) Uani 1 1 d . . . . .
N10 N -0.0414(6) 0.03373(18) 0.5970(3) 0.0301(17) Uani 1 1 d . . . . .
N11 N 0.0438(6) 0.1007(2) 0.5436(3) 0.0312(17) Uani 1 1 d . . . . .
N12 N 0.0389(6) 0.13841(18) 0.6478(3) 0.0257(15) Uani 1 1 d . . . . .
N13 N 0.1539(6) 0.06886(19) 0.6417(3) 0.0267(15) Uani 1 1 d . . . . .
N14 N -0.0496(6) 0.0743(2) 0.6989(3) 0.0276(15) Uani 1 1 d . . . . .
N15 N -0.1595(5) 0.10317(18) 0.6050(3) 0.0236(14) Uani 1 1 d . . . . .
N20 N -0.0404(6) 0.36801(18) 0.5964(3) 0.0242(14) Uani 1 1 d . . . . .
N21 N -0.1547(5) 0.43804(19) 0.6113(3) 0.0275(16) Uani 1 1 d . . . . .
N22 N 0.0419(5) 0.43383(18) 0.5462(3) 0.0233(14) Uani 1 1 d . . . . .
N23 N 0.0488(6) 0.46997(18) 0.6516(3) 0.0233(14) Uani 1 1 d . . . . .
N24 N 0.1583(6) 0.40055(19) 0.6420(3) 0.0250(15) Uani 1 1 d . . . . .
N25 N -0.0463(5) 0.40317(19) 0.7027(3) 0.0252(15) Uani 1 1 d . . . . .
N30 N 0.4508(5) 0.53013(18) 0.6486(3) 0.0221(14) Uani 1 1 d . . . . .
N31 N 0.5385(6) 0.56503(19) 0.5469(3) 0.0259(15) Uani 1 1 d . . . . .
N32 N 0.6552(5) 0.57173(18) 0.6509(3) 0.0223(14) Uani 1 1 d . . . . .
N33 N 0.5462(5) 0.63454(18) 0.6061(3) 0.0228(14) Uani 1 1 d . . . . .
N34 N 0.4570(6) 0.60081(19) 0.7022(3) 0.0259(15) Uani 1 1 d . . . . .
N35 N 0.3424(6) 0.59470(19) 0.5980(3) 0.0260(15) Uani 1 1 d . . . . .
N40 N 0.5498(6) 0.6997(2) 0.8924(3) 0.0273(15) Uani 1 1 d . . . . .
N41 N 0.4566(6) 0.7358(2) 0.7975(3) 0.0298(16) Uani 1 1 d . . . . .
N42 N 0.6589(6) 0.76414(19) 0.8487(3) 0.0261(15) Uani 1 1 d . . . . .
N43 N 0.4523(6) 0.80411(19) 0.8537(3) 0.0280(16) Uani 1 1 d . . . . .
N44 N 0.5476(6) 0.76752(19) 0.9533(3) 0.0273(15) Uani 1 1 d . . . . .
N45 N 0.3471(5) 0.7408(2) 0.9036(3) 0.0303(17) Uani 1 1 d . . . . .
N55 N 1.0409(6) 0.93731(19) 0.8003(3) 0.0262(15) Uani 1 1 d . . . . .
N50 N 1.0454(6) 0.86706(18) 0.8544(3) 0.0278(16) Uani 1 1 d . . . . .
N51 N 1.1534(6) 0.9278(2) 0.9056(3) 0.0339(17) Uani 1 1 d . . . . .
N52 N 0.9543(5) 0.97095(18) 0.8983(3) 0.0233(14) Uani 1 1 d . . . . .
N53 N 0.9490(6) 0.90121(18) 0.9532(3) 0.0271(15) Uani 1 1 d . . . . .
N54 N 0.8408(5) 0.90657(18) 0.8497(3) 0.0261(15) Uani 1 1 d . . . . .
N60 N -0.0489(6) 0.2678(2) 0.7999(3) 0.0289(16) Uani 1 1 d . . . . .
N61 N 0.1597(6) 0.26919(18) 0.8556(3) 0.0254(15) Uani 1 1 d . . . . .
N62 N -0.0316(6) 0.30387(18) 0.9065(3) 0.0273(15) Uani 1 1 d . . . . .
N63 N 0.0504(6) 0.23622(19) 0.9542(3) 0.0268(15) Uani 1 1 d . . . . .
N64 N -0.1540(6) 0.23689(18) 0.8932(3) 0.0265(15) Uani 1 1 d . . . . .
N65 N 0.0414(6) 0.20122(18) 0.8487(3) 0.0238(14) Uani 1 1 d . . . . .
Ni1 Ni -0.00149(11) 0.08673(3) 0.62165(6) 0.0222(3) Uani 1 1 d . . . . .
Ni2 Ni 0.00174(10) 0.41844(3) 0.62455(5) 0.0162(3) Uani 1 1 d . . . . .
Ni3 Ni 0.49702(10) 0.58235(3) 0.62542(5) 0.0152(2) Uani 1 1 d . . . . .
Ni4 Ni 0.50243(11) 0.75177(3) 0.87490(6) 0.0225(3) Uani 1 1 d . . . . .
Ni5 Ni 0.99710(10) 0.91859(3) 0.87721(6) 0.0198(3) Uani 1 1 d . . . . .
Ni6 Ni 0.00377(11) 0.25274(3) 0.87699(6) 0.0196(3) Uani 1 1 d . . . . .
S10 S -0.16327(19) -0.03044(7) 0.60132(13) 0.0447(6) Uani 1 1 d . . . . .
S11 S 0.0915(2) 0.13513(7) 0.44357(11) 0.0413(6) Uani 1 1 d . . . . .
S12 S 0.0927(3) 0.20389(6) 0.70081(11) 0.0471(7) Uani 1 1 d . . . . .
S13 S 0.34713(19) 0.03938(7) 0.68690(13) 0.0450(7) Uani 1 1 d . . . . .
S14 S -0.1467(2) 0.06180(8) 0.80145(10) 0.0423(6) Uani 1 1 d . . . . .
S15 S -0.36269(18) 0.13862(6) 0.59338(13) 0.0413(6) Uani 1 1 d . . . . .
S20A S -0.0991(6) 0.30051(8) 0.55171(18) 0.0414(18) Uani 0.817(18) 1 d . . P J
2
S20B S -0.030(2) 0.3026(3) 0.5374(6) 0.028(6) Uani 0.183(18) 1 d . . P J 1
S21A S -0.3604(3) 0.47052(11) 0.5841(2) 0.0319(7) Uani 0.552(5) 1 d . . P F 2
S21B S -0.3490(4) 0.47599(13) 0.6224(3) 0.0319(7) Uani 0.448(5) 1 d . . P F 1
S22A S 0.0388(13) 0.46805(15) 0.4458(2) 0.029(3) Uani 0.39(2) 1 d . . P K 2
S22B S 0.1054(8) 0.4620(2) 0.44354(18) 0.042(2) Uani 0.61(2) 1 d . . P K 1
S23 S 0.15307(17) 0.53507(5) 0.68301(9) 0.0260(4) Uani 1 1 d . . . . .
S24 S 0.35542(17) 0.36731(6) 0.67621(11) 0.0327(5) Uani 1 1 d . . . . .
S25 S -0.13956(17) 0.37885(6) 0.80045(8) 0.0267(4) Uani 1 1 d . . . . .
S30 S 0.4010(2) 0.46428(6) 0.70148(9) 0.0317(5) Uani 1 1 d . . . . .
S31 S 0.66615(17) 0.56859(7) 0.45278(9) 0.0338(5) Uani 1 1 d . . . . .
S32 S 0.85917(18) 0.56260(9) 0.70229(10) 0.0481(8) Uani 1 1 d . . . . .
S33 S 0.65438(18) 0.70146(6) 0.60001(11) 0.0351(5) Uani 1 1 d . . . . .
S34 S 0.3976(3) 0.63599(7) 0.79924(10) 0.0469(7) Uani 1 1 d . . . . .
S35 S 0.15061(18) 0.62601(8) 0.55506(10) 0.0426(7) Uani 1 1 d . . . . .
S40 S 0.64619(18) 0.63200(6) 0.91356(11) 0.0350(5) Uani 1 1 d . . . . .
S41 S 0.3839(2) 0.70527(6) 0.69824(9) 0.0346(5) Uani 1 1 d . . . . .
S42A S 0.8621(13) 0.7783(5) 0.7950(7) 0.033(2) Uani 0.56(3) 1 d . . P L 2
S42B S 0.8543(17) 0.7880(6) 0.8052(8) 0.033(2) Uani 0.44(3) 1 d . . P L 1
S43 S 0.35896(18) 0.86923(6) 0.81492(10) 0.0317(5) Uani 1 1 d . . . . .
S44 S 0.65525(18) 0.77866(7) 1.05344(9) 0.0319(5) Uani 1 1 d . . . . .
S45 S 0.1494(2) 0.72006(11) 0.95230(12) 0.0599(9) Uani 1 1 d . . . . .
S55 S 1.1065(2) 0.96636(7) 0.69956(11) 0.0432(6) Uani 1 1 d . . . . .
S50A S 1.1531(13) 0.8025(4) 0.8303(8) 0.0304(15) Uani 0.44(3) 1 d . . P L 1
S50B S 1.1431(10) 0.8020(3) 0.8138(7) 0.0304(15) Uani 0.56(3) 1 d . . P L 2
S51A S 1.3612(3) 0.94561(14) 0.95206(16) 0.0391(15) Uani 0.631(9) 1 d . . P G 1
S51B S 1.3491(5) 0.9155(2) 0.9609(2) 0.032(2) Uani 0.369(9) 1 d . . P G 2
S52A S 0.8952(6) 1.03874(9) 0.94462(19) 0.0431(19) Uani 0.698(15) 1 d . . P M 2
S52B S 0.9677(10) 1.03641(18) 0.9532(3) 0.023(3) Uani 0.302(15) 1 d . . P M 1
S53 S 0.84434(17) 0.87802(6) 1.04988(9) 0.0278(4) Uani 1 1 d . . . . .
S54A S 0.6467(5) 0.87654(19) 0.8048(3) 0.0274(10) Uani 0.521(8) 1 d . . P H 2
S54B S 0.6433(6) 0.8908(2) 0.7929(3) 0.0274(10) Uani 0.479(8) 1 d . . P H 1
S60 S -0.1464(2) 0.28554(10) 0.69969(10) 0.0496(8) Uani 1 1 d . . . . .
S61 S 0.35166(17) 0.29925(6) 0.81093(10) 0.0301(5) Uani 1 1 d . . . . .
S62 S -0.1106(2) 0.36977(6) 0.94692(10) 0.0392(6) Uani 1 1 d . . . . .
S63 S 0.0880(2) 0.19830(7) 1.05220(10) 0.0406(6) Uani 1 1 d . . . . .
S64 S -0.35588(18) 0.20198(6) 0.90615(13) 0.0436(7) Uani 1 1 d . . . . .
S65 S 0.1120(2) 0.13575(6) 0.80168(11) 0.0405(6) Uani 1 1 d . . . . .


_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
Bi1 S12 2.794(2) . ?
Bi1 S20A 2.827(3) . ?
Bi1 S20B 2.877(13) . ?
Bi1 S44 2.905(2) 4_565 ?
Bi1 S60 2.767(3) . ?
Bi1 S61 2.786(2) 2_556 ?
Bi1 S64 2.824(2) 2_456 ?
Bi2 S21A 2.908(4) 1_655 ?
Bi2 S21B 2.938(5) 1_655 ?
Bi2 S24 2.728(2) . ?
Bi2 S25 2.751(2) 2_556 ?
Bi2 S30 2.839(2) . ?
Bi2 S31 2.918(2) 3_666 ?
Bi2 S62 2.825(2) 2_556 ?
Bi3 S22A 2.801(6) 4_666 ?
Bi3 S22B 2.913(4) 4_666 ?
Bi3 S23 2.899(2) 2_556 ?
Bi3 S32 2.790(2) 2_656 ?
Bi3 S34 2.748(3) . ?
Bi3 S35 2.830(2) 2_556 ?
Bi3 S40 2.749(2) . ?
Bi4 S10 2.939(2) 2_566 ?
Bi4 S11 2.876(3) 4_666 ?
Bi4 S43 2.726(2) . ?
Bi4 S55 2.793(3) 2_656 ?
Bi4 S51A 2.873(4) 1_455 ?
Bi4 S51B 2.915(6) 1_455 ?
Bi4 S54A 2.801(7) . ?
Bi4 S54B 2.728(7) . ?
Bi5 S33 2.855(2) 2_656 ?
Bi5 S41 2.781(2) 2_656 ?
Bi5 S42A 2.781(17) . ?
Bi5 S42B 2.83(2) . ?
Bi5 S45 2.857(3) 1_655 ?
Bi5 S50A 2.724(15) . ?
Bi5 S50B 2.819(12) . ?
Bi5 S63 2.853(2) 3_667 ?
Bi6 S13 2.832(2) 2_556 ?
Bi6 S14 2.791(2) . ?
Bi6 S15 2.791(2) 2_456 ?
Bi6 S52A 2.944(4) 1_445 ?
Bi6 S52B 2.818(7) 1_445 ?
Bi6 S53 2.863(2) 3_667 ?
Bi6 S65 2.730(2) . ?
C7MA N7MA 1.49(3) . ?
C1MA N1MA 1.50(3) 2_456 ?
C2MA N2MA 1.48(9) . ?
C3MA N3MA 1.21(2) . ?
C4MA N4MA 1.43(3) . ?
C5MA N5MA 1.447(17) . ?
C6MA N6MA 1.42(6) . ?
C7MB N7MA 1.47(3) . ?
C8MA N8MA 1.17(3) . ?
C10 N10 1.147(11) . ?
C10 S10 1.650(9) . ?
C11 N11 1.159(12) . ?
C11 S11 1.666(10) . ?
C12 N12 1.149(11) . ?
C12 S12 1.668(9) . ?
C13 N13 1.155(11) . ?
C13 S13 1.666(9) . ?
C14 N14 1.147(11) . ?
C14 S14 1.678(9) . ?
C15 N15 1.135(11) . ?
C15 S15 1.685(9) . ?
C20 N20 1.138(11) . ?
C20 S20A 1.673(9) . ?
C20 S20B 1.760(17) . ?
C21A N21 1.20(2) . ?
C21A S21A 1.67(2) . ?
C21B N21 1.12(3) . ?
C21B S21B 1.65(2) . ?
C22 N22 1.147(11) . ?
C22 S22A 1.653(10) . ?
C22 S22B 1.702(10) . ?
C23 N23 1.156(10) . ?
C23 S23 1.666(8) . ?
C24 N24 1.151(11) . ?
C24 S24 1.676(9) . ?
C25 N25 1.140(11) . ?
C25 S25 1.666(8) . ?
C30 N30 1.151(10) . ?
C30 S30 1.668(8) . ?
C31 N31 1.148(11) . ?
C31 S31 1.647(9) . ?
C32 N32 1.148(11) . ?
C32 S32 1.662(8) . ?
C33 N33 1.150(10) . ?
C33 S33 1.654(8) . ?
C34 N34 1.151(11) . ?
C34 S34 1.657(9) . ?
C35 N35 1.154(11) . ?
C35 S35 1.659(9) . ?
C40 N40 1.133(11) . ?
C40 S40 1.672(9) . ?
C41 N41 1.143(11) . ?
C41 S41 1.680(9) . ?
C42 N42 1.146(11) . ?
C42 S42A 1.725(18) . ?
C42 S42B 1.62(2) . ?
C43 N43 1.142(11) . ?
C43 S43 1.678(9) . ?
C44 N44 1.164(11) . ?
C44 S44 1.649(9) . ?
C45 N45 1.148(11) . ?
C45 S45 1.658(9) . ?
C55 N55 1.138(11) . ?
C55 S55 1.674(9) . ?
C50 N50 1.137(11) . ?
C50 S50A 1.655(17) . ?
C50 S50B 1.722(14) . ?
C51A N51 1.18(2) . ?
C51A S51A 1.67(2) . ?
C51B N51 1.11(4) . ?
C51B S51B 1.68(4) . ?
C52 N52 1.148(11) . ?
C52 S52A 1.698(10) . ?
C52 S52B 1.675(11) . ?
C53 N53 1.162(11) . ?
C53 S53 1.669(9) . ?
C54A N54 1.22(3) . ?
C54A S54A 1.62(2) . ?
C54B N54 1.07(3) . ?
C54B S54B 1.77(3) . ?
C60 N60 1.135(12) . ?
C60 S60 1.670(9) . ?
C61 N61 1.151(11) . ?
C61 S61 1.668(8) . ?
C62 N62 1.138(11) . ?
C62 S62 1.657(9) . ?
C63 N63 1.163(11) . ?
C63 S63 1.653(9) . ?
C64 N64 1.142(11) . ?
C64 S64 1.660(8) . ?
C65 N65 1.142(11) . ?
C65 S65 1.670(9) . ?
N10 Ni1 2.101(7) . ?
N11 Ni1 2.060(7) . ?
N12 Ni1 2.068(7) . ?
N13 Ni1 2.067(7) . ?
N14 Ni1 2.037(7) . ?
N15 Ni1 2.062(7) . ?
N20 Ni2 2.047(7) . ?
N21 Ni2 2.068(7) . ?
N22 Ni2 2.064(7) . ?
N23 Ni2 2.091(7) . ?
N24 Ni2 2.066(7) . ?
N25 Ni2 2.084(7) . ?
N30 Ni3 2.084(7) . ?
N31 Ni3 2.093(7) . ?
N32 Ni3 2.066(7) . ?
N33 Ni3 2.069(7) . ?
N34 Ni3 2.063(7) . ?
N35 Ni3 2.054(7) . ?
N40 Ni4 2.049(8) . ?
N41 Ni4 2.062(8) . ?
N42 Ni4 2.070(7) . ?
N43 Ni4 2.088(7) . ?
N44 Ni4 2.080(7) . ?
N45 Ni4 2.066(7) . ?
N55 Ni5 2.081(7) . ?
N50 Ni5 2.066(7) . ?
N51 Ni5 2.058(7) . ?
N52 Ni5 2.064(7) . ?
N53 Ni5 2.059(7) . ?
N54 Ni5 2.071(7) . ?
N60 Ni6 2.070(8) . ?
N61 Ni6 2.068(7) . ?
N62 Ni6 2.064(7) . ?
N63 Ni6 2.067(7) . ?
N64 Ni6 2.054(7) . ?
N65 Ni6 2.073(7) . ?

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
S12 Bi1 S20A 172.73(10) . . ?
S12 Bi1 S20B 163.2(5) . . ?
S12 Bi1 S44 82.34(8) . 4_565 ?
S12 Bi1 S64 87.88(8) . 2_456 ?
S20B Bi1 S44 81.4(5) . 4_565 ?
S60 Bi1 S12 97.88(9) . . ?
S60 Bi1 S20A 83.33(16) . . ?
S60 Bi1 S20B 98.5(5) . . ?
S60 Bi1 S44 176.80(8) . 4_565 ?
S60 Bi1 S61 82.09(8) . 2_556 ?
S60 Bi1 S64 92.13(9) . 2_456 ?
S61 Bi1 S12 80.08(7) 2_556 . ?
S61 Bi1 S20A 107.20(10) 2_556 . ?
S61 Bi1 S20B 99.0(3) 2_556 . ?
S61 Bi1 S44 101.09(6) 2_556 4_565 ?
S61 Bi1 S64 165.75(8) 2_556 2_456 ?
S64 Bi1 S20A 84.90(11) 2_456 . ?
S64 Bi1 S20B 94.8(4) 2_456 . ?
S64 Bi1 S44 84.68(7) 2_456 4_565 ?
S24 Bi2 S21A 173.52(10) . 1_655 ?
S24 Bi2 S21B 157.08(13) . 1_655 ?
S24 Bi2 S25 80.53(7) . 2_556 ?
S24 Bi2 S30 82.39(7) . . ?
S24 Bi2 S31 88.89(7) . 3_666 ?
S24 Bi2 S62 103.12(7) . 2_556 ?
S25 Bi2 S21A 102.24(10) 2_556 1_655 ?
S25 Bi2 S21B 90.74(11) 2_556 1_655 ?
S25 Bi2 S30 100.24(7) 2_556 . ?
S25 Bi2 S31 164.47(7) 2_556 3_666 ?
S25 Bi2 S62 81.07(7) 2_556 2_556 ?
S30 Bi2 S21A 91.32(10) . 1_655 ?
S30 Bi2 S21B 78.35(12) . 1_655 ?
S30 Bi2 S31 89.50(7) . 3_666 ?
S31 Bi2 S21B 103.15(12) 3_666 1_655 ?
S62 Bi2 S21A 83.16(10) 2_556 1_655 ?
S62 Bi2 S21B 96.32(12) 2_556 1_655 ?
S62 Bi2 S30 174.49(7) 2_556 . ?
S62 Bi2 S31 90.38(8) 2_556 3_666 ?
S23 Bi3 S22B 99.0(2) 2_556 4_666 ?
S32 Bi3 S22A 91.6(2) 2_656 4_666 ?
S32 Bi3 S22B 81.29(14) 2_656 4_666 ?
S32 Bi3 S23 82.78(7) 2_656 2_556 ?
S32 Bi3 S35 168.57(9) 2_656 2_556 ?
S34 Bi3 S22A 169.8(3) . 4_666 ?
S34 Bi3 S22B 172.9(2) . 4_666 ?
S34 Bi3 S23 84.39(8) . 2_556 ?
S34 Bi3 S32 93.00(9) . 2_656 ?
S34 Bi3 S35 81.54(8) . 2_556 ?
S34 Bi3 S40 97.33(9) . . ?
S35 Bi3 S22B 103.32(12) 2_556 4_666 ?
S35 Bi3 S23 106.50(7) 2_556 2_556 ?
S40 Bi3 S22A 92.0(3) . 4_666 ?
S40 Bi3 S22B 78.2(2) . 4_666 ?
S40 Bi3 S23 169.98(7) . 2_556 ?
S40 Bi3 S32 87.27(8) . 2_656 ?
S40 Bi3 S35 83.52(7) . 2_556 ?
S11 Bi4 S10 89.85(8) 4_666 2_566 ?
S11 Bi4 S51B 75.02(14) 4_666 1_455 ?
S43 Bi4 S10 166.42(8) . 2_566 ?
S43 Bi4 S11 98.36(7) . 4_666 ?
S43 Bi4 S55 82.00(8) . 2_656 ?
S43 Bi4 S51A 103.09(9) . 1_455 ?
S43 Bi4 S51B 89.32(14) . 1_455 ?
S43 Bi4 S54A 79.52(14) . . ?
S43 Bi4 S54B 82.77(15) . . ?
S55 Bi4 S10 90.63(9) 2_656 2_566 ?
S55 Bi4 S11 175.66(8) 2_656 4_666 ?
S55 Bi4 S51A 84.73(11) 2_656 1_455 ?
S55 Bi4 S51B 100.68(14) 2_656 1_455 ?
S55 Bi4 S54A 108.18(16) 2_656 . ?
S51A Bi4 S10 87.47(10) 1_455 2_566 ?
S51A Bi4 S11 90.98(11) 1_455 4_666 ?
S51A Bi4 S51B 22.73(16) 1_455 1_455 ?
S54B Bi4 S10 86.85(15) . 2_566 ?
S54B Bi4 S11 87.33(17) . 4_666 ?
S54B Bi4 S55 97.00(17) . 2_656 ?
S54B Bi4 S51A 174.08(16) . 1_455 ?
S54B Bi4 S51B 159.4(2) . 1_455 ?
S33 Bi5 S45 88.36(8) 2_656 1_655 ?
S41 Bi5 S33 93.30(7) 2_656 2_656 ?
S41 Bi5 S42B 103.9(3) 2_656 . ?
S41 Bi5 S45 83.44(9) 2_656 1_655 ?
S41 Bi5 S50B 79.8(3) 2_656 . ?
S41 Bi5 S63 177.26(8) 2_656 3_667 ?
S42A Bi5 S50B 79.2(5) . . ?
S42B Bi5 S33 88.0(5) . 2_656 ?
S42B Bi5 S45 172.0(4) . 1_655 ?
S42B Bi5 S63 78.6(3) . 3_667 ?
S50A Bi5 S33 171.1(4) . 2_656 ?
S50A Bi5 S41 83.8(3) . 2_656 ?
S50A Bi5 S42B 84.6(6) . . ?
S50A Bi5 S45 99.6(4) . 1_655 ?
S50A Bi5 S63 95.5(3) . 3_667 ?
S63 Bi5 S33 87.78(8) 3_667 2_656 ?
S63 Bi5 S45 94.08(9) 3_667 1_655 ?
S13 Bi6 S52A 102.81(10) 2_556 1_445 ?
S13 Bi6 S53 105.50(7) 2_556 3_667 ?
S14 Bi6 S13 83.96(8) . 2_556 ?
S14 Bi6 S15 86.65(8) . 2_456 ?
S14 Bi6 S52A 78.92(15) . 1_445 ?
S14 Bi6 S52B 93.3(2) . 1_445 ?
S14 Bi6 S53 170.53(8) . 3_667 ?
S15 Bi6 S13 167.51(9) 2_456 2_556 ?
S15 Bi6 S52A 83.36(11) 2_456 1_445 ?
S15 Bi6 S52B 95.0(2) 2_456 1_445 ?
S15 Bi6 S53 83.92(7) 2_456 3_667 ?
S52B Bi6 S13 93.7(2) 1_445 2_556 ?
S52B Bi6 S52A 18.05(18) 1_445 1_445 ?
S52B Bi6 S53 86.74(19) 1_445 3_667 ?
S53 Bi6 S52A 99.13(14) 3_667 1_445 ?
S65 Bi6 S13 80.52(8) . 2_556 ?
S65 Bi6 S14 98.16(8) . . ?
S65 Bi6 S15 92.73(8) . 2_456 ?
S65 Bi6 S52A 175.21(16) . 1_445 ?
S65 Bi6 S52B 166.5(3) . 1_445 ?
S65 Bi6 S53 83.13(7) . 3_667 ?
N10 C10 S10 176.8(8) . . ?
N11 C11 S11 177.7(9) . . ?
N12 C12 S12 176.9(8) . . ?
N13 C13 S13 178.6(10) . . ?
N14 C14 S14 177.5(8) . . ?
N15 C15 S15 175.8(8) . . ?
N20 C20 S20A 176.3(9) . . ?
N20 C20 S20B 151.8(13) . . ?
N21 C21A S21A 178.1(17) . . ?
N21 C21B S21B 175(2) . . ?
N22 C22 S22A 161.7(11) . . ?
N22 C22 S22B 168.3(10) . . ?
N23 C23 S23 178.4(8) . . ?
N24 C24 S24 176.7(8) . . ?
N25 C25 S25 178.0(8) . . ?
N30 C30 S30 177.9(8) . . ?
N31 C31 S31 177.2(8) . . ?
N32 C32 S32 176.2(8) . . ?
N33 C33 S33 176.1(7) . . ?
N34 C34 S34 178.5(9) . . ?
N35 C35 S35 178.2(9) . . ?
N40 C40 S40 176.7(8) . . ?
N41 C41 S41 178.8(8) . . ?
N42 C42 S42A 171.3(10) . . ?
N42 C42 S42B 173.5(11) . . ?
N43 C43 S43 178.3(9) . . ?
N44 C44 S44 178.1(8) . . ?
N45 C45 S45 179.2(9) . . ?
N55 C55 S55 179.0(8) . . ?
N50 C50 S50A 169.9(12) . . ?
N50 C50 S50B 174.8(10) . . ?
N51 C51A S51A 177.8(17) . . ?
N51 C51B S51B 170(3) . . ?
N52 C52 S52A 171.2(10) . . ?
N52 C52 S52B 156.5(11) . . ?
N53 C53 S53 177.5(8) . . ?
N54 C54A S54A 177(2) . . ?
N54 C54B S54B 178(3) . . ?
N60 C60 S60 177.6(8) . . ?
N61 C61 S61 178.5(8) . . ?
N62 C62 S62 179.2(9) . . ?
N63 C63 S63 178.3(8) . . ?
N64 C64 S64 176.3(8) . . ?
N65 C65 S65 176.6(8) . . ?
C10 N10 Ni1 155.2(7) . . ?
C11 N11 Ni1 168.5(8) . . ?
C12 N12 Ni1 172.4(7) . . ?
C13 N13 Ni1 169.0(7) . . ?
C14 N14 Ni1 172.6(7) . . ?
C15 N15 Ni1 170.5(7) . . ?
C20 N20 Ni2 176.8(8) . . ?
C21A N21 Ni2 172.5(11) . . ?
C21B N21 Ni2 162.7(14) . . ?
C22 N22 Ni2 172.5(7) . . ?
C23 N23 Ni2 169.8(7) . . ?
C24 N24 Ni2 171.8(7) . . ?
C25 N25 Ni2 172.2(7) . . ?
C30 N30 Ni3 169.3(7) . . ?
C31 N31 Ni3 153.7(7) . . ?
C32 N32 Ni3 172.0(7) . . ?
C33 N33 Ni3 167.3(7) . . ?
C34 N34 Ni3 172.3(7) . . ?
C35 N35 Ni3 167.0(7) . . ?
C40 N40 Ni4 173.4(7) . . ?
C41 N41 Ni4 173.0(7) . . ?
C42 N42 Ni4 173.6(7) . . ?
C43 N43 Ni4 171.0(7) . . ?
C44 N44 Ni4 165.3(7) . . ?
C45 N45 Ni4 173.0(8) . . ?
C55 N55 Ni5 176.8(7) . . ?
C50 N50 Ni5 171.7(7) . . ?
C51A N51 Ni5 173.9(11) . . ?
C51B N51 Ni5 155.0(17) . . ?
C52 N52 Ni5 170.1(7) . . ?
C53 N53 Ni5 171.1(7) . . ?
C54A N54 Ni5 169.3(15) . . ?
C54B N54 Ni5 169.7(16) . . ?
C60 N60 Ni6 174.2(7) . . ?
C61 N61 Ni6 169.6(7) . . ?
C62 N62 Ni6 171.7(7) . . ?
C63 N63 Ni6 166.5(7) . . ?
C64 N64 Ni6 170.6(7) . . ?
C65 N65 Ni6 173.6(7) . . ?
N11 Ni1 N10 91.6(3) . . ?
N11 Ni1 N12 89.7(3) . . ?
N11 Ni1 N13 92.9(3) . . ?
N11 Ni1 N15 89.8(3) . . ?
N12 Ni1 N10 178.6(3) . . ?
N13 Ni1 N10 89.1(3) . . ?
N13 Ni1 N12 90.1(3) . . ?
N14 Ni1 N10 89.5(3) . . ?
N14 Ni1 N11 178.1(3) . . ?
N14 Ni1 N12 89.3(3) . . ?
N14 Ni1 N13 88.6(3) . . ?
N14 Ni1 N15 88.7(3) . . ?
N15 Ni1 N10 90.0(3) . . ?
N15 Ni1 N12 90.8(3) . . ?
N15 Ni1 N13 177.1(3) . . ?
N20 Ni2 N21 91.9(3) . . ?
N20 Ni2 N22 89.8(3) . . ?
N20 Ni2 N23 178.2(3) . . ?
N20 Ni2 N24 90.7(3) . . ?
N20 Ni2 N25 89.6(3) . . ?
N21 Ni2 N23 89.2(3) . . ?
N21 Ni2 N25 88.6(3) . . ?
N22 Ni2 N21 88.9(3) . . ?
N22 Ni2 N23 88.8(3) . . ?
N22 Ni2 N24 93.3(3) . . ?
N22 Ni2 N25 177.4(3) . . ?
N24 Ni2 N21 176.6(3) . . ?
N24 Ni2 N23 88.3(3) . . ?
N24 Ni2 N25 89.2(3) . . ?
N25 Ni2 N23 91.8(3) . . ?
N30 Ni3 N31 92.1(3) . . ?
N32 Ni3 N30 89.8(3) . . ?
N32 Ni3 N31 89.5(3) . . ?
N32 Ni3 N33 88.5(3) . . ?
N33 Ni3 N30 177.2(3) . . ?
N33 Ni3 N31 90.1(3) . . ?
N34 Ni3 N30 89.4(3) . . ?
N34 Ni3 N31 178.5(3) . . ?
N34 Ni3 N32 90.6(3) . . ?
N34 Ni3 N33 88.4(3) . . ?
N35 Ni3 N30 92.5(3) . . ?
N35 Ni3 N31 89.5(3) . . ?
N35 Ni3 N32 177.5(3) . . ?
N35 Ni3 N33 89.2(3) . . ?
N35 Ni3 N34 90.3(3) . . ?
N40 Ni4 N41 90.1(3) . . ?
N40 Ni4 N42 90.6(3) . . ?
N40 Ni4 N43 177.5(3) . . ?
N40 Ni4 N44 89.7(3) . . ?
N40 Ni4 N45 90.3(3) . . ?
N41 Ni4 N42 91.4(3) . . ?
N41 Ni4 N43 87.4(3) . . ?
N41 Ni4 N44 179.5(3) . . ?
N41 Ni4 N45 90.6(3) . . ?
N42 Ni4 N43 89.4(3) . . ?
N42 Ni4 N44 89.1(3) . . ?
N44 Ni4 N43 92.8(3) . . ?
N45 Ni4 N42 177.8(3) . . ?
N45 Ni4 N43 89.8(3) . . ?
N45 Ni4 N44 88.9(3) . . ?
N50 Ni5 N55 89.1(3) . . ?
N50 Ni5 N54 88.8(3) . . ?
N51 Ni5 N55 90.6(3) . . ?
N51 Ni5 N50 88.7(3) . . ?
N51 Ni5 N52 89.8(3) . . ?
N51 Ni5 N53 90.7(3) . . ?
N51 Ni5 N54 177.1(3) . . ?
N52 Ni5 N55 89.1(3) . . ?
N52 Ni5 N50 177.6(3) . . ?
N52 Ni5 N54 92.7(3) . . ?
N53 Ni5 N55 178.0(3) . . ?
N53 Ni5 N50 92.4(3) . . ?
N53 Ni5 N52 89.5(3) . . ?
N53 Ni5 N54 87.9(3) . . ?
N54 Ni5 N55 90.9(3) . . ?
N60 Ni6 N65 90.4(3) . . ?
N61 Ni6 N60 88.5(3) . . ?
N61 Ni6 N65 88.7(3) . . ?
N62 Ni6 N60 90.7(3) . . ?
N62 Ni6 N61 90.9(3) . . ?
N62 Ni6 N63 90.2(3) . . ?
N62 Ni6 N65 178.8(3) . . ?
N63 Ni6 N60 177.4(3) . . ?
N63 Ni6 N61 93.9(3) . . ?
N63 Ni6 N65 88.7(3) . . ?
N64 Ni6 N60 87.9(3) . . ?
N64 Ni6 N61 176.3(3) . . ?
N64 Ni6 N62 89.7(3) . . ?
N64 Ni6 N63 89.7(3) . . ?
N64 Ni6 N65 90.8(3) . . ?
C10 S10 Bi4 101.0(3) . 2_546 ?
C11 S11 Bi4 99.7(3) . 4_565 ?
C12 S12 Bi1 100.8(3) . . ?
C13 S13 Bi6 93.0(3) . 2_556 ?
C14 S14 Bi6 100.1(3) . . ?
C15 S15 Bi6 102.9(3) . 2_456 ?
C20 S20A Bi1 97.0(3) . . ?
C20 S20B Bi1 93.2(7) . . ?
C21B S21B Bi2 96.7(9) . 1_455 ?
C22 S22A Bi3 102.4(4) . 4_565 ?
C22 S22B Bi3 96.8(4) . 4_565 ?
C23 S23 Bi3 99.4(3) . 2_556 ?
C24 S24 Bi2 97.8(3) . . ?
C25 S25 Bi2 97.3(3) . 2_556 ?
C30 S30 Bi2 99.5(3) . . ?
C31 S31 Bi2 100.3(3) . 3_666 ?
C32 S32 Bi3 104.2(3) . 2_656 ?
C33 S33 Bi5 102.4(3) . 2_656 ?
C34 S34 Bi3 98.1(3) . . ?
C35 S35 Bi3 93.0(3) . 2_556 ?
C40 S40 Bi3 98.2(3) . . ?
C41 S41 Bi5 97.6(3) . 2_656 ?
C42 S42A Bi5 100.3(8) . . ?
C42 S42B Bi5 101.3(10) . . ?
C43 S43 Bi4 97.1(3) . . ?
C44 S44 Bi1 101.2(3) . 4_666 ?
C45 S45 Bi5 95.4(3) . 1_455 ?
C55 S55 Bi4 97.5(3) . 2_656 ?
C50 S50A Bi5 100.6(7) . . ?
C50 S50B Bi5 95.3(6) . . ?
C51A S51A Bi4 98.0(7) . 1_655 ?
C52 S52A Bi6 97.1(4) . 1_665 ?
C52 S52B Bi6 102.5(4) . 1_665 ?
C53 S53 Bi6 98.6(3) . 3_667 ?
C54A S54A Bi4 96.3(10) . . ?
C54B S54B Bi4 99.4(9) . . ?
C60 S60 Bi1 98.8(3) . . ?
C61 S61 Bi1 94.7(3) . 2_556 ?
C62 S62 Bi2 95.6(3) . 2_556 ?
C63 S63 Bi5 99.4(3) . 3_667 ?
C64 S64 Bi1 101.5(3) . 2_456 ?
C65 S65 Bi6 98.6(3) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N20 C20 S20B Bi1 109.6(18) . . . . ?
N22 C22 S22A Bi3 -104(3) . . . 4_565 ?
N22 C22 S22B Bi3 126(4) . . . 4_565 ?
N50 C50 S50A Bi5 96(5) . . . . ?
N52 C52 S52B Bi6 103(2) . . . 1_665 ?

_olex2_submission_original_sample_id NIMJCC
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.788
_oxdiff_exptl_absorpt_empirical_full_min 0.651
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.811(1)
2 0.189(1)

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: butanone'
####################################################################### 
# 
# 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_1NH4NiBiSCN6_120K_Xray
_database_code_depnum_ccdc_archive 'CCDC 2045274'
loop_
_audit_author_name
_audit_author_address
'Matthew Cliffe'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_audit_creation_date             2020-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'ammonium nickel hexathiocyanatobismuthate'
_chemical_formula_moiety         'Bi C6 N6 Ni S6, H4 N'
_chemical_formula_sum            'C6 H4 Bi N7 Ni S6'
_chemical_formula_weight         634.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'N H4 Ni Bi S6 C6 N6'
_chemical_oxdiff_usercomment     
'#17938-NIMCLA GVA-1511 IN FOMBLIN FILM ON MICROMOUNT FOR MC'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4699(2)
_cell_length_b                   8.6913(2)
_cell_length_c                   11.9058(3)
_cell_angle_alpha                97.187(2)
_cell_angle_beta                 91.149(2)
_cell_angle_gamma                91.610(2)
_cell_volume                     868.96(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.7520
_cell_measurement_theta_min      3.7000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    27.765
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.101
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             592
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 0 -6 0.0954
-1 0 8 0.0881
-5 -1 1 0.0706
4 1 -5 0.0690
1 4 -6 0.1459
-5 3 1 0.0697
-4 -1 5 0.0462
1 -6 2 0.1102
0 6 0 0.1026
4 0 6 0.1350
-1 5 1 0.1014
-5 0 3 0.0429
-5 0 4 0.0443
5 0 -4 0.0426

_exptl_crystal_preparation       'evaporated from methylethylketone solution'
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.087
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.9976 -0.0014 -5.9979 -0.8822 0.2653 0.5659
-1.0001 0.0023 7.9962 0.2762 -0.9533 -0.3569
-4.9981 -0.9988 0.9990 -0.7586 -0.5337 0.1213
3.9989 0.9977 -4.9973 0.4073 0.8683 0.1513
1.0018 3.9958 -5.9983 0.2297 0.5508 0.8125
-4.9963 2.9988 0.9978 -0.3573 -0.7214 0.6818
-3.9989 -0.9977 4.9973 -0.4073 -0.8683 -0.1513
0.9966 -5.9958 2.0011 -0.3553 0.1617 -1.0085
0.0027 5.9963 -0.0019 0.6020 -0.2817 0.8408
3.9976 0.0014 5.9979 0.8822 -0.2653 -0.5659
-1.0000 5.0000 1.0000 0.4118 -0.4373 0.7115
-5.0000 -0.0000 3.0000 -0.5540 -0.7957 0.1564
-5.0000 -0.0000 4.0000 -0.5017 -0.9030 0.1038
5.0000 0.0000 -4.0000 0.5017 0.9030 -0.1038

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15829
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.681
_diffrn_reflns_theta_min         3.743
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -73.00  29.00   1.00    1.00    --  -42.81  77.00 150.00  102
  2  ω     19.00 112.00   1.00    1.00    --   42.81  57.00  30.00   93
  3  ω    -27.00  67.00   1.00    1.00    --   42.81 -57.00-120.00   94
  4  ω     30.00  90.00   1.00    4.00    --  103.00 -30.00   0.00   60
  5  ω     31.00 118.00   1.00    4.00    --  103.00-125.00-150.00   87
  6  ω     30.00  90.00   1.00    4.00    --  103.00 -30.00 150.00   60
  7  ω    101.00 178.00   1.00    4.00    --  103.00  91.00  -7.00   77
  8  ω     22.00 110.00   1.00    4.00    --  103.00 -94.00 -30.00   88
  9  ω     31.00 133.00   1.00    4.00    --  103.00 -77.00  60.00  102
 10  ω     30.00  90.00   1.00    4.00    --  103.00 -30.00  60.00   60
 11  ω     34.00  98.00   1.00    4.00    --  103.00 -45.00 -60.00   64
 12  ω     80.00 172.00   1.00    4.00    --  103.00  45.00 -30.00   92
 13  ω     34.00 128.00   1.00    4.00    --  103.00 -61.00-180.00   94
 14  ω     80.00 176.00   1.00    4.00    --  103.00  30.00 -90.00   96
 15  ω     31.00 118.00   1.00    4.00    --  103.00-125.00  90.00   87
 16  ω     31.00 118.00   1.00    4.00    --  103.00-125.00 -60.00   87
 17  ω     19.00 112.00   1.00    1.00    --   42.81  57.00 120.00   93
 18  ω     19.00 112.00   1.00    1.00    --   42.81  57.00-150.00   93
 19  ω     19.00 112.00   1.00    1.00    --   42.81  57.00 -60.00   93
 20  ω     80.00 172.00   1.00    4.00    --  103.00  45.00  30.00   92
 21  ω     73.00 175.00   1.00    4.00    --  103.00  77.00  90.00  102
 22  ω     78.00 172.00   1.00    4.00    --  103.00  61.00  60.00   94
 23  ω     80.00 172.00   1.00    4.00    --  103.00  45.00-180.00   92
 24  ω     73.00 175.00   1.00    4.00    --  103.00  77.00 120.00  102
 25  ω     73.00 175.00   1.00    4.00    --  103.00  77.00 -90.00  102
 26  ω     73.00 175.00   1.00    4.00    --  103.00  77.00 -30.00  102
 27  ω     80.00 172.00   1.00    4.00    --  103.00  45.00-150.00   92
 28  ω     80.00 176.00   1.00    4.00    --  103.00  30.00 120.00   96
 29  ω     12.00 115.00   1.00    1.00    --   42.81  77.00 -60.00  103
 30  ω     12.00  76.00   1.00    1.00    --   42.81  77.00  90.00   64
 31  ω      1.00  82.00   1.00    1.00    --   42.81 -99.00  60.00   81
;
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1421740000
_diffrn_orient_matrix_UB_12      0.1003409000
_diffrn_orient_matrix_UB_13      0.0522953000
_diffrn_orient_matrix_UB_21      0.0947189000
_diffrn_orient_matrix_UB_22      -0.0470499000
_diffrn_orient_matrix_UB_23      -0.1073561000
_diffrn_orient_matrix_UB_31      -0.0627879000
_diffrn_orient_matrix_UB_32      0.1402388000
_diffrn_orient_matrix_UB_33      -0.0525274000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3367
_reflns_number_total             3468
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0228
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0443P)²+0.5041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0652
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H7C-N7
 0.88 with sigma of 0.02
 H7A-N7
 0.88 with sigma of 0.02
 H7B-N7
 0.88 with sigma of 0.02
 H7D-N7
 0.88 with sigma of 0.02
 H7C-H7D
 1.44 with sigma of 0.02
 H7C-H7B
 1.44 with sigma of 0.02
 H7C-H7A
 1.44 with sigma of 0.02
 H7B-H7A
 1.44 with sigma of 0.02
 H7D-H7A
 1.44 with sigma of 0.02
 H7D-H7B
 1.44 with sigma of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Bi1 Bi 0.500000 0.500000 1.000000 0.01262(8) Uani 1 2 d S . P . .
Bi2 Bi 0.000000 0.000000 0.500000 0.01230(8) Uani 1 2 d S . P . .
Ni2 Ni -0.500000 0.500000 0.500000 0.01281(18) Uani 1 2 d S . P . .
Ni1 Ni 0.000000 0.000000 1.000000 0.01205(18) Uani 1 2 d S . P . .
S1 S 0.51872(8) 0.21821(9) 1.09301(7) 0.02365(16) Uani 1 1 d . . . . .
S6 S -0.75566(8) 0.40131(10) 0.84909(6) 0.02048(16) Uani 1 1 d . . . . .
S5 S -0.76401(8) 0.01390(9) 0.33715(6) 0.02393(17) Uani 1 1 d . . . . .
S3 S -0.28077(8) 0.39234(9) 0.83431(6) 0.02085(16) Uani 1 1 d . . . . .
S4 S 0.02261(8) 0.32189(8) 0.55849(7) 0.02481(17) Uani 1 1 d . . . . .
S2 S 0.26816(8) -0.01466(10) 0.64295(6) 0.02318(17) Uani 1 1 d . . . . .
N1 N 0.1975(3) 0.1290(3) 1.0655(2) 0.0180(5) Uani 1 1 d . . . . .
N2 N 0.1056(3) -0.0224(3) 0.8453(2) 0.0177(6) Uani 1 1 d . . . . .
N6 N -0.5948(3) 0.4612(3) 0.6535(2) 0.0180(6) Uani 1 1 d . . . . .
N4 N -0.2987(3) 0.3898(3) 0.5359(2) 0.0170(5) Uani 1 1 d . . . . .
N3 N -0.1047(3) 0.2009(3) 0.9606(2) 0.0204(5) Uani 1 1 d . . . . .
N5 N -0.6073(3) 0.2932(3) 0.4273(2) 0.0178(5) Uani 1 1 d . . . . .
C5 C -0.6711(3) 0.1783(3) 0.3922(2) 0.0148(5) Uani 1 1 d . . . . .
C4 C -0.1686(3) 0.3575(3) 0.5447(2) 0.0149(5) Uani 1 1 d . . . . .
C6 C -0.6591(3) 0.4360(4) 0.7338(2) 0.0158(6) Uani 1 1 d . . . . .
C3 C -0.1762(3) 0.2820(3) 0.9107(2) 0.0157(5) Uani 1 1 d . . . . .
C2 C 0.1724(3) -0.0160(4) 0.7627(2) 0.0152(5) Uani 1 1 d . . . . .
C1 C 0.3300(3) 0.1664(3) 1.0752(2) 0.0146(5) Uani 1 1 d . . . . .
N7 N -0.0253(4) 0.6552(3) 0.7536(3) 0.0311(6) Uani 1 1 d D . . . .
H7A H 0.072(3) 0.639(5) 0.776(4) 0.072(19) Uiso 1 1 d D . . . .
H7B H -0.025(7) 0.649(6) 0.6783(14) 0.13(3) Uiso 1 1 d D . . . .
H7C H -0.091(5) 0.586(4) 0.774(4) 0.08(2) Uiso 1 1 d D . . . .
H7D H -0.047(5) 0.751(3) 0.782(4) 0.049(13) Uiso 1 1 d D . . . .


_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
Bi1 S1 2.8184(8) . ?
Bi1 S1 2.8184(8) 2_667 ?
Bi1 S6 2.8297(7) 1_655 ?
Bi1 S6 2.8297(7) 2_567 ?
Bi1 S3 2.8280(6) 2_567 ?
Bi1 S3 2.8280(6) 1_655 ?
Bi2 S5 2.8230(6) 1_655 ?
Bi2 S5 2.8230(6) 2_456 ?
Bi2 S4 2.7973(7) 2_556 ?
Bi2 S4 2.7974(7) . ?
Bi2 S2 2.8262(7) 2_556 ?
Bi2 S2 2.8261(7) . ?
Ni2 N6 2.073(3) 2_466 ?
Ni2 N6 2.073(3) . ?
Ni2 N4 2.043(2) 2_466 ?
Ni2 N4 2.043(2) . ?
Ni2 N5 2.072(2) . ?
Ni2 N5 2.072(2) 2_466 ?
Ni1 N1 2.071(2) . ?
Ni1 N1 2.071(2) 2_557 ?
Ni1 N2 2.053(3) 2_557 ?
Ni1 N2 2.053(3) . ?
Ni1 N3 2.081(3) . ?
Ni1 N3 2.081(3) 2_557 ?
S1 C1 1.651(3) . ?
S6 C6 1.667(3) . ?
S5 C5 1.665(3) . ?
S3 C3 1.663(3) . ?
S4 C4 1.666(3) . ?
S2 C2 1.655(3) . ?
N1 C1 1.158(4) . ?
N2 C2 1.151(4) . ?
N6 C6 1.151(4) . ?
N4 C4 1.150(4) . ?
N3 C3 1.153(4) . ?
N5 C5 1.149(4) . ?
N7 H7A 0.885(17) . ?
N7 H7B 0.891(17) . ?
N7 H7C 0.865(17) . ?
N7 H7D 0.882(17) . ?

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
S1 Bi1 S1 180.00(3) . 2_667 ?
S1 Bi1 S6 84.57(2) 2_667 1_655 ?
S1 Bi1 S6 84.57(2) . 2_567 ?
S1 Bi1 S6 95.43(2) . 1_655 ?
S1 Bi1 S6 95.43(2) 2_667 2_567 ?
S1 Bi1 S3 90.17(2) . 2_567 ?
S1 Bi1 S3 90.17(2) 2_667 1_655 ?
S1 Bi1 S3 89.83(2) . 1_655 ?
S1 Bi1 S3 89.83(2) 2_667 2_567 ?
S6 Bi1 S6 180.0 1_655 2_567 ?
S3 Bi1 S6 90.91(2) 2_567 2_567 ?
S3 Bi1 S6 89.09(2) 2_567 1_655 ?
S3 Bi1 S6 90.91(2) 1_655 1_655 ?
S3 Bi1 S6 89.09(2) 1_655 2_567 ?
S3 Bi1 S3 180.0 2_567 1_655 ?
S5 Bi2 S5 180.0 2_456 1_655 ?
S5 Bi2 S2 98.56(2) 1_655 2_556 ?
S5 Bi2 S2 81.44(2) 2_456 2_556 ?
S5 Bi2 S2 81.44(2) 1_655 . ?
S5 Bi2 S2 98.56(2) 2_456 . ?
S4 Bi2 S5 91.01(2) . 1_655 ?
S4 Bi2 S5 88.99(2) . 2_456 ?
S4 Bi2 S5 88.99(2) 2_556 1_655 ?
S4 Bi2 S5 91.01(2) 2_556 2_456 ?
S4 Bi2 S4 180.0 2_556 . ?
S4 Bi2 S2 93.36(2) 2_556 . ?
S4 Bi2 S2 86.64(2) 2_556 2_556 ?
S4 Bi2 S2 93.36(2) . 2_556 ?
S4 Bi2 S2 86.64(2) . . ?
S2 Bi2 S2 180.0 . 2_556 ?
N6 Ni2 N6 180.0 . 2_466 ?
N4 Ni2 N6 88.81(10) . 2_466 ?
N4 Ni2 N6 91.19(10) . . ?
N4 Ni2 N6 88.81(10) 2_466 . ?
N4 Ni2 N6 91.19(10) 2_466 2_466 ?
N4 Ni2 N4 180.00(12) . 2_466 ?
N4 Ni2 N5 91.44(10) 2_466 2_466 ?
N4 Ni2 N5 88.56(10) 2_466 . ?
N4 Ni2 N5 88.56(10) . 2_466 ?
N4 Ni2 N5 91.44(10) . . ?
N5 Ni2 N6 88.66(10) 2_466 2_466 ?
N5 Ni2 N6 88.66(10) . . ?
N5 Ni2 N6 91.34(10) . 2_466 ?
N5 Ni2 N6 91.34(10) 2_466 . ?
N5 Ni2 N5 180.0 2_466 . ?
N1 Ni1 N1 180.00(13) 2_557 . ?
N1 Ni1 N3 89.71(10) 2_557 . ?
N1 Ni1 N3 90.29(10) . . ?
N1 Ni1 N3 90.29(10) 2_557 2_557 ?
N1 Ni1 N3 89.71(10) . 2_557 ?
N2 Ni1 N1 88.00(10) 2_557 2_557 ?
N2 Ni1 N1 88.00(10) . . ?
N2 Ni1 N1 92.00(10) 2_557 . ?
N2 Ni1 N1 92.00(10) . 2_557 ?
N2 Ni1 N2 180.0 2_557 . ?
N2 Ni1 N3 90.65(11) 2_557 . ?
N2 Ni1 N3 89.35(11) 2_557 2_557 ?
N2 Ni1 N3 90.65(11) . 2_557 ?
N2 Ni1 N3 89.35(11) . . ?
N3 Ni1 N3 180.00(13) . 2_557 ?
C1 S1 Bi1 96.68(10) . . ?
C6 S6 Bi1 94.44(10) . 1_455 ?
C5 S5 Bi2 98.96(9) . 1_455 ?
C3 S3 Bi1 98.46(9) . 1_455 ?
C4 S4 Bi2 97.65(10) . . ?
C2 S2 Bi2 97.01(10) . . ?
C1 N1 Ni1 157.2(2) . . ?
C2 N2 Ni1 171.3(3) . . ?
C6 N6 Ni2 174.2(3) . . ?
C4 N4 Ni2 163.2(2) . . ?
C3 N3 Ni1 159.5(2) . . ?
C5 N5 Ni2 176.4(2) . . ?
N5 C5 S5 178.1(3) . . ?
N4 C4 S4 176.6(3) . . ?
N6 C6 S6 178.8(3) . . ?
N3 C3 S3 177.5(3) . . ?
N2 C2 S2 177.7(3) . . ?
N1 C1 S1 178.3(3) . . ?
H7A N7 H7B 107(3) . . ?
H7A N7 H7C 111(3) . . ?
H7A N7 H7D 107(2) . . ?
H7B N7 H7C 110(3) . . ?
H7B N7 H7D 109(3) . . ?
H7C N7 H7D 113(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.201
_oxdiff_exptl_absorpt_empirical_full_min 0.606
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: butanone'
####################################################################### 
# 
# 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_2KNiBiSCN6
_database_code_depnum_ccdc_archive 'CCDC 2045276'
loop_
_audit_author_name
_audit_author_address
'Matthew Cliffe'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_2KNiBiSCN6          
;
PROBLEM: Check Calcd Positive Resid. Density on       Bi1       3.46 eA-3
RESPONSE: Significant additional density around heavy atoms is often found, due to Fourier termination ripples.
;
_vrf_PLAT971_2KNiBiSCN6          
;
PROBLEM: Check Calcd Resid. Dens.  1.07A   From S5              3.49 eA-3
RESPONSE: Significant additional density around heavy atoms is often found, due to Fourier termination ripples.
;
_vrf_PLAT972_2KNiBiSCN6          
;
PROBLEM: Check Calcd Resid. Dens.  0.38A   From Bi2            -3.23 eA-3
RESPONSE: Significant additional density around heavy atoms is often found, due to Fourier termination ripples.
;
# Added during the CSD deposition process: Wednesday 18 November 2020 06:33 PM
# end Validation Reply Form


_audit_creation_date             2020-04-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'potassium nickel hexathiocyanatobismuthate'
_chemical_formula_moiety         'Bi C6 K N6 Ni S6'
_chemical_formula_sum            'C6 Bi K N6 Ni S6'
_chemical_formula_weight         655.27
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5073(2)
_cell_length_b                   8.5686(2)
_cell_length_c                   11.9651(3)
_cell_angle_alpha                97.5730(10)
_cell_angle_beta                 89.7810(10)
_cell_angle_gamma                90.9970(10)
_cell_volume                     864.46(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3750
_cell_measurement_temperature    180
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_shelx_estimated_absorpt_T_max   0.792
_shelx_estimated_absorpt_T_min   0.528
_exptl_absorpt_coefficient_mu    12.215
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.517
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_recrystallization_method 'evaporation from butanone'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7203
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         1.717
_diffrn_ambient_temperature      180.0
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2896
_reflns_number_total             3926
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.567
_refine_diff_density_min         -3.225
_refine_diff_density_rms         0.299
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3926
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0568
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0246P)²+33.8988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1452
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Bi1 Bi 0.500000 0.500000 0.000000 0.02259(17) Uani 1 2 d S . P . .
Bi2 Bi 0.000000 0.000000 0.500000 0.0369(2) Uani 1 2 d S . P . .
Ni1 Ni 0.000000 0.000000 0.000000 0.0198(4) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 0.500000 0.500000 0.0201(4) Uani 1 2 d S . P . .
S3 S 0.2646(5) 0.5932(5) 1.1606(3) 0.0403(9) Uani 1 1 d . . . . .
S6 S 0.2520(4) 0.3956(5) 0.8507(3) 0.0372(8) Uani 1 1 d . . . . .
S1 S 0.5152(4) 1.2142(4) 1.0922(4) 0.0385(9) Uani 1 1 d . . . . .
S5 S 0.2301(6) 0.0209(6) 0.3340(4) 0.0587(13) Uani 1 1 d . . . . .
S2 S -0.2637(5) 1.0204(6) 1.3599(4) 0.0526(11) Uani 1 1 d . . . . .
S4 S -0.0167(5) 0.6788(6) 0.4270(5) 0.0595(13) Uani 1 1 d . . . . .
K1 K 0.0140(8) 1.3439(6) 1.2356(6) 0.0986(19) Uani 1 1 d . . . . .
N1 N 0.1995(13) 1.1254(13) 1.0613(10) 0.032(2) Uani 1 1 d . . . . .
N5 N 0.4023(13) 0.2876(13) 0.4263(10) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.1001(12) 0.7958(13) 1.0410(10) 0.033(3) Uani 1 1 d . . . . .
N2 N -0.1011(12) 1.0288(14) 1.1563(10) 0.030(2) Uani 1 1 d . . . . .
N6 N 0.4031(13) 0.4604(14) 0.6545(10) 0.032(3) Uani 1 1 d . . . . .
N4 N 0.2972(13) 0.6071(14) 0.4641(10) 0.034(3) Uani 1 1 d . . . . .
C1 C 0.3294(14) 1.1633(14) 1.0725(10) 0.023(2) Uani 1 1 d . . . . .
C3 C 0.1666(15) 0.7095(14) 1.0881(11) 0.026(3) Uani 1 1 d . . . . .
C5 C 0.3305(16) 0.1797(18) 0.3912(13) 0.036(3) Uani 1 1 d . . . . .
C6 C 0.3443(13) 0.4337(15) 0.7340(10) 0.023(2) Uani 1 1 d . . . . .
C4 C 0.1676(15) 0.6403(17) 0.4503(12) 0.033(3) Uani 1 1 d . . . . .
C2 C -0.170(2) 1.0240(18) 1.2358(16) 0.048(4) Uani 1 1 d . . . . .


_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
Bi1 S3 2.821(4) 1_554 ?
Bi1 S3 2.821(4) 2_666 ?
Bi1 S6 2.826(3) 2_666 ?
Bi1 S6 2.826(3) 1_554 ?
Bi1 S1 2.820(4) 2_676 ?
Bi1 S1 2.820(4) 1_544 ?
Bi2 S5 2.804(4) . ?
Bi2 S5 2.804(4) 2_556 ?
Bi2 S2 2.827(4) 1_544 ?
Bi2 S2 2.827(4) 2_567 ?
Bi2 S4 2.777(5) 2_566 ?
Bi2 S4 2.777(5) 1_545 ?
Ni1 K1 3.800(6) 1_544 ?
Ni1 K1 3.800(6) 2_566 ?
Ni1 N1 2.076(11) 2_566 ?
Ni1 N1 2.076(11) 1_544 ?
Ni1 N3 2.075(11) 2_566 ?
Ni1 N3 2.075(11) 1_544 ?
Ni1 N2 2.043(12) 2_566 ?
Ni1 N2 2.043(12) 1_544 ?
Ni2 N5 2.076(11) . ?
Ni2 N5 2.076(11) 2_666 ?
Ni2 N6 2.087(11) 2_666 ?
Ni2 N6 2.087(11) . ?
Ni2 N4 2.042(12) 2_666 ?
Ni2 N4 2.042(12) . ?
S3 K1 3.201(7) 1_545 ?
S3 C3 1.645(13) . ?
S6 K1 3.460(8) 2_577 ?
S6 C6 1.666(12) . ?
S1 C1 1.642(12) . ?
S5 K1 3.671(9) 1_544 ?
S5 C5 1.664(16) . ?
S2 C2 1.69(2) . ?
S4 K1 3.441(7) 1_544 ?
S4 C4 1.640(14) . ?
K1 N1 3.065(13) . ?
K1 N2 2.896(13) . ?
K1 C2 3.133(18) . ?
N1 C1 1.150(16) . ?
N5 C5 1.133(18) . ?
N3 C3 1.145(16) . ?
N2 C2 1.12(2) . ?
N6 C6 1.121(16) . ?
N4 C4 1.161(17) . ?

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
S3 Bi1 S3 180.0 1_554 2_666 ?
S3 Bi1 S6 93.50(11) 1_554 2_666 ?
S3 Bi1 S6 86.50(11) 2_666 2_666 ?
S3 Bi1 S6 86.50(11) 1_554 1_554 ?
S3 Bi1 S6 93.50(11) 2_666 1_554 ?
S6 Bi1 S6 180.00(11) 1_554 2_666 ?
S1 Bi1 S3 87.73(11) 1_544 1_554 ?
S1 Bi1 S3 87.73(11) 2_676 2_666 ?
S1 Bi1 S3 92.27(11) 1_544 2_666 ?
S1 Bi1 S3 92.27(11) 2_676 1_554 ?
S1 Bi1 S6 94.29(11) 1_544 1_554 ?
S1 Bi1 S6 85.71(11) 2_676 1_554 ?
S1 Bi1 S6 94.29(11) 2_676 2_666 ?
S1 Bi1 S6 85.71(11) 1_544 2_666 ?
S1 Bi1 S1 180.00(15) 2_676 1_544 ?
S5 Bi2 S5 180.0 2_556 . ?
S5 Bi2 S2 83.18(14) 2_556 1_544 ?
S5 Bi2 S2 83.18(14) . 2_567 ?
S5 Bi2 S2 96.82(14) 2_556 2_567 ?
S5 Bi2 S2 96.82(14) . 1_544 ?
S2 Bi2 S2 180.0 2_567 1_544 ?
S4 Bi2 S5 87.41(15) 2_566 2_556 ?
S4 Bi2 S5 92.59(15) 2_566 . ?
S4 Bi2 S5 87.41(15) 1_545 . ?
S4 Bi2 S5 92.59(15) 1_545 2_556 ?
S4 Bi2 S2 94.49(14) 2_566 1_544 ?
S4 Bi2 S2 85.51(14) 2_566 2_567 ?
S4 Bi2 S2 94.49(14) 1_545 2_567 ?
S4 Bi2 S2 85.51(14) 1_545 1_544 ?
S4 Bi2 S4 180.00(6) 2_566 1_545 ?
K1 Ni1 K1 180.00(17) 1_544 2_566 ?
N1 Ni1 K1 126.4(3) 2_566 1_544 ?
N1 Ni1 K1 53.6(3) 2_566 2_566 ?
N1 Ni1 K1 126.4(3) 1_544 2_566 ?
N1 Ni1 K1 53.6(3) 1_544 1_544 ?
N1 Ni1 N1 180.0(9) 1_544 2_566 ?
N3 Ni1 K1 65.7(4) 1_544 2_566 ?
N3 Ni1 K1 65.7(4) 2_566 1_544 ?
N3 Ni1 K1 114.3(4) 2_566 2_566 ?
N3 Ni1 K1 114.3(4) 1_544 1_544 ?
N3 Ni1 N1 90.9(4) 2_566 1_544 ?
N3 Ni1 N1 90.9(4) 1_544 2_566 ?
N3 Ni1 N1 89.1(4) 2_566 2_566 ?
N3 Ni1 N1 89.1(4) 1_544 1_544 ?
N3 Ni1 N3 180.0(6) 2_566 1_544 ?
N2 Ni1 K1 131.2(3) 2_566 1_544 ?
N2 Ni1 K1 131.2(3) 1_544 2_566 ?
N2 Ni1 K1 48.8(3) 1_544 1_544 ?
N2 Ni1 K1 48.8(3) 2_566 2_566 ?
N2 Ni1 N1 88.7(5) 2_566 1_544 ?
N2 Ni1 N1 88.7(5) 1_544 2_566 ?
N2 Ni1 N1 91.3(5) 1_544 1_544 ?
N2 Ni1 N1 91.3(5) 2_566 2_566 ?
N2 Ni1 N3 91.9(5) 1_544 2_566 ?
N2 Ni1 N3 88.1(5) 1_544 1_544 ?
N2 Ni1 N3 88.1(5) 2_566 2_566 ?
N2 Ni1 N3 91.9(5) 2_566 1_544 ?
N2 Ni1 N2 180.0(8) 2_566 1_544 ?
N5 Ni2 N5 180.0 2_666 . ?
N5 Ni2 N6 90.6(4) 2_666 . ?
N5 Ni2 N6 89.4(4) . . ?
N5 Ni2 N6 90.6(4) . 2_666 ?
N5 Ni2 N6 89.4(4) 2_666 2_666 ?
N6 Ni2 N6 180.0 2_666 . ?
N4 Ni2 N5 88.5(5) . . ?
N4 Ni2 N5 91.5(5) . 2_666 ?
N4 Ni2 N5 88.5(5) 2_666 2_666 ?
N4 Ni2 N5 91.5(5) 2_666 . ?
N4 Ni2 N6 89.1(5) 2_666 2_666 ?
N4 Ni2 N6 90.9(4) . 2_666 ?
N4 Ni2 N6 89.1(5) . . ?
N4 Ni2 N6 90.9(5) 2_666 . ?
N4 Ni2 N4 180.0 . 2_666 ?
Bi1 S3 K1 121.11(17) 1_556 1_545 ?
C3 S3 Bi1 98.5(5) . 1_556 ?
C3 S3 K1 106.4(5) . 1_545 ?
Bi1 S6 K1 121.41(16) 1_556 2_577 ?
C6 S6 Bi1 96.0(4) . 1_556 ?
C6 S6 K1 81.6(4) . 2_577 ?
C1 S1 Bi1 96.5(4) . 1_566 ?
Bi2 S5 K1 89.46(18) . 1_544 ?
C5 S5 Bi2 100.4(5) . . ?
C5 S5 K1 77.3(5) . 1_544 ?
C2 S2 Bi2 99.1(5) . 1_566 ?
Bi2 S4 K1 155.7(2) 1_565 1_544 ?
C4 S4 Bi2 97.2(5) . 1_565 ?
C4 S4 K1 81.9(5) . 1_544 ?
S3 K1 Ni1 106.64(19) 1_565 1_566 ?
S3 K1 S6 82.60(16) 1_565 2_577 ?
S3 K1 S5 108.2(2) 1_565 1_566 ?
S3 K1 S4 73.46(16) 1_565 1_566 ?
S6 K1 Ni1 103.4(2) 2_577 1_566 ?
S6 K1 S5 169.1(2) 2_577 1_566 ?
S5 K1 Ni1 72.85(12) 1_566 1_566 ?
S4 K1 Ni1 171.4(2) 1_566 1_566 ?
S4 K1 S6 68.02(14) 1_566 2_577 ?
S4 K1 S5 115.4(2) 1_566 1_566 ?
N1 K1 Ni1 33.0(2) . 1_566 ?
N1 K1 S3 80.7(3) . 1_565 ?
N1 K1 S6 120.4(3) . 2_577 ?
N1 K1 S5 62.0(2) . 1_566 ?
N1 K1 S4 151.6(3) . 1_566 ?
N1 K1 C2 78.3(4) . . ?
N2 K1 Ni1 32.1(2) . 1_566 ?
N2 K1 S3 138.3(3) . 1_565 ?
N2 K1 S6 107.3(3) . 2_577 ?
N2 K1 S5 64.0(3) . 1_566 ?
N2 K1 S4 148.1(3) . 1_566 ?
N2 K1 N1 59.1(3) . . ?
N2 K1 C2 20.9(4) . . ?
C2 K1 Ni1 53.0(4) . 1_566 ?
C2 K1 S3 158.9(4) . 1_565 ?
C2 K1 S6 106.0(3) . 2_577 ?
C2 K1 S5 63.4(3) . 1_566 ?
C2 K1 S4 127.6(4) . 1_566 ?
Ni1 N1 K1 93.3(4) 1_566 . ?
C1 N1 Ni1 160.2(11) . 1_566 ?
C1 N1 K1 106.4(9) . . ?
C5 N5 Ni2 170.9(12) . . ?
C3 N3 Ni1 162.0(12) . 1_566 ?
Ni1 N2 K1 99.2(4) 1_566 . ?
C2 N2 Ni1 169.0(12) . 1_566 ?
C2 N2 K1 91.5(11) . . ?
C6 N6 Ni2 175.9(11) . . ?
C4 N4 Ni2 165.9(12) . . ?
N1 C1 S1 178.2(12) . . ?
N3 C3 S3 177.1(13) . . ?
N5 C5 S5 177.2(14) . . ?
N6 C6 S6 178.4(12) . . ?
N4 C4 S4 177.2(14) . . ?
S2 C2 K1 110.2(8) . . ?
N2 C2 S2 176.5(15) . . ?
N2 C2 K1 67.5(10) . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Bi2 S2 C2 K1 -69.9(5) 1_566 . . . ?
Ni1 N2 C2 K1 -167(6) 1_566 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4GuaNiBiSCN6
_database_code_depnum_ccdc_archive 'CCDC 2045277'
loop_
_audit_author_name
_audit_author_address
'Matthew Cliffe'
;University of Nottingham
United Kingdom
;
_audit_update_record             
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_audit_creation_date             2020-04-30
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
        triguanidinium hexanickel(II) pentahexathiocyanatobismuthate
;
_chemical_formula_moiety         'Bi0.15 C0.841 N Ni0.167 S0.86, C0.083 N0.25'
_chemical_formula_sum            'C0.92 Bi0.15 N1.25 Ni0.17 S0.86'
_chemical_formula_weight         97.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -3.3078 10.1165 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0032 0.0015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3581 1.0631 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1181 0.1169 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           201
_space_group_name_H-M_alt        'P n -3'
_space_group_name_Hall           '-P 2ab 2bc 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x, y'
'z, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y'
'-z+1/2, x, -y+1/2'
'y, z, x'
'-y+1/2, z, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-z, -x, -y'
'-z, x-1/2, y-1/2'
'z-1/2, x-1/2, -y'
'z-1/2, -x, y-1/2'
'-y, -z, -x'
'y-1/2, -z, x-1/2'
'-y, z-1/2, x-1/2'
'y-1/2, z-1/2, -x'

_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_length_a                   12.12528(2)
_cell_length_b                   12.12528(2)
_cell_length_c                   12.12528(2)
_cell_measurement_reflns_used    19048
_cell_measurement_theta_max      35.603121777092255
_cell_measurement_theta_min      1.628674428570269
_cell_volume                     1782.689(10)
_cell_formula_units_Z            24
_cell_measurement_temperature    100(2)
_computing_cell_refinement       
;
DIALS 2theta refinement, DIALS 2.2.0-gfdf98e000
;
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19048
_diffrn_reflns_theta_max         35.603121777092255
_diffrn_reflns_theta_min         1.628674428570269
_exptl_absorpt_correction_T_min  0.9719420218039372
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
DIALS 2.2.0-gfdf98e000
Scaling & analysis of unmerged intensities, 
absorption correction using spherical harmonics
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_ambient_temperature      100(2)

_diffrn_radiation_wavelength     0.6889
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris PILATUS 2M'
_diffrn_source                   Synchrotron
_diffrn_measurement_device       'Fixed χ 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_source_details           'Allan et al. (2017)'
_diffrn_source_type              'Diamond Light Source Beamline I19-1'
_computing_data_collection       'GDA - generic data acquisition software'

_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                906
_reflns_number_total             1524
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         1524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0263
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0333P)²+2.0239P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0866
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: N2(0.25)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Bi1 Bi 0.500000 0.500000 0.500000 0.03510(9) Uani 0.900(4) 6 d S T . . 1
Ni1 Ni 0.500000 0.500000 1.000000 0.0264(2) Uani 1 6 d S T P . .
S1 S 0.39864(11) 0.64906(7) 0.64370(7) 0.0553(4) Uani 0.860(6) 1 d . . . A 1
C2 C 0.750000 0.750000 0.750000 0.069(4) Uani 1 12 d S T P . .
N1 N 0.4579(2) 0.5550(2) 0.8449(2) 0.0457(6) Uani 1 1 d . . . . .
C1 C 0.4352(3) 0.5914(3) 0.7620(3) 0.0412(11) Uani 0.841(12) 1 d . . . A 1
N2 N 0.671(6) 0.679(6) 0.7770(15) 0.104(13) Uani 0.25 1 d . . 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
Bi1 S1 2.7952(10) . ?
Bi1 S1 2.7952(10) 17_666 ?
Bi1 S1 2.7952(10) 5 ?
Bi1 S1 2.7952(10) 13_666 ?
Bi1 S1 2.7952(10) 21_666 ?
Bi1 S1 2.7952(10) 9 ?
Ni1 N1 2.060(2) . ?
Ni1 N1 2.060(2) 20_566 ?
Ni1 N1 2.060(2) 13_667 ?
Ni1 N1 2.060(2) 23_656 ?
Ni1 N1 2.060(2) 11_566 ?
Ni1 N1 2.060(2) 8_656 ?
S1 C1 1.656(3) . ?
C2 N2 1.336(17) 8_656 ?
C2 N2 1.336(17) 12_665 ?
C2 N2 1.336(17) . ?
C2 N2 1.336(17) 3_656 ?
C2 N2 1.336(17) 6_566 ?
C2 N2 1.336(17) 4_566 ?
C2 N2 1.336(17) 10_656 ?
C2 N2 1.336(17) 7_665 ?
C2 N2 1.336(17) 9 ?
C2 N2 1.336(17) 11_566 ?
C2 N2 1.336(17) 5 ?
C2 N2 1.336(17) 2_665 ?
N1 C1 1.132(4) . ?
N2 N2 1.76(3) 5 ?
N2 N2 1.76(3) 9 ?
N2 N2 0.84(5) 8_656 ?
N2 N2 1.85(13) 4_566 ?
N2 N2 0.84(5) 11_566 ?

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
S1 Bi1 S1 180.0 . 13_666 ?
S1 Bi1 S1 98.94(3) 21_666 17_666 ?
S1 Bi1 S1 180.00(3) 21_666 9 ?
S1 Bi1 S1 81.06(3) . 21_666 ?
S1 Bi1 S1 98.94(3) . 9 ?
S1 Bi1 S1 98.94(3) 13_666 21_666 ?
S1 Bi1 S1 98.94(3) 13_666 17_666 ?
S1 Bi1 S1 98.94(3) . 5 ?
S1 Bi1 S1 180.0 5 17_666 ?
S1 Bi1 S1 81.06(3) 13_666 5 ?
S1 Bi1 S1 81.06(3) 13_666 9 ?
S1 Bi1 S1 81.06(3) 21_666 5 ?
S1 Bi1 S1 98.94(3) 5 9 ?
S1 Bi1 S1 81.06(3) . 17_666 ?
S1 Bi1 S1 81.06(3) 17_666 9 ?
N1 Ni1 N1 89.36(11) . 23_656 ?
N1 Ni1 N1 89.36(11) 11_566 20_566 ?
N1 Ni1 N1 90.64(11) 11_566 8_656 ?
N1 Ni1 N1 90.64(11) . 11_566 ?
N1 Ni1 N1 90.64(11) . 8_656 ?
N1 Ni1 N1 180.0 23_656 11_566 ?
N1 Ni1 N1 180.0 20_566 8_656 ?
N1 Ni1 N1 180.0 . 13_667 ?
N1 Ni1 N1 90.64(11) 13_667 20_566 ?
N1 Ni1 N1 90.64(11) 23_656 13_667 ?
N1 Ni1 N1 89.36(11) 23_656 8_656 ?
N1 Ni1 N1 89.36(11) 11_566 13_667 ?
N1 Ni1 N1 89.36(11) 13_667 8_656 ?
N1 Ni1 N1 89.36(11) . 20_566 ?
N1 Ni1 N1 90.64(11) 23_656 20_566 ?
C1 S1 Bi1 98.56(12) . . ?
N2 C2 N2 119.0(13) 9 8_656 ?
N2 C2 N2 119.0(13) 7_665 11_566 ?
N2 C2 N2 119.0(13) 10_656 4_566 ?
N2 C2 N2 117(2) 12_665 8_656 ?
N2 C2 N2 37(2) 5 12_665 ?
N2 C2 N2 117(2) . 7_665 ?
N2 C2 N2 99(8) 6_566 8_656 ?
N2 C2 N2 82.4(12) 2_665 7_665 ?
N2 C2 N2 99(8) 10_656 12_665 ?
N2 C2 N2 36.6(19) 9 7_665 ?
N2 C2 N2 82.4(12) 6_566 4_566 ?
N2 C2 N2 82.4(12) 12_665 7_665 ?
N2 C2 N2 117(2) 12_665 4_566 ?
N2 C2 N2 151.7(17) 8_656 7_665 ?
N2 C2 N2 82.4(12) 10_656 8_656 ?
N2 C2 N2 117(2) 6_566 3_656 ?
N2 C2 N2 82.4(12) 2_665 12_665 ?
N2 C2 N2 82.4(12) 10_656 3_656 ?
N2 C2 N2 88(9) 9 12_665 ?
N2 C2 N2 36.6(19) 5 3_656 ?
N2 C2 N2 88(9) . 4_566 ?
N2 C2 N2 151.7(17) 4_566 3_656 ?
N2 C2 N2 99(8) 2_665 4_566 ?
N2 C2 N2 119.0(13) 7_665 3_656 ?
N2 C2 N2 119.0(13) 5 4_566 ?
N2 C2 N2 82.4(12) 6_566 11_566 ?
N2 C2 N2 36.6(19) . 8_656 ?
N2 C2 N2 88(9) 10_656 11_566 ?
N2 C2 N2 119.0(13) 2_665 8_656 ?
N2 C2 N2 117(2) 5 11_566 ?
N2 C2 N2 82.4(12) 4_566 11_566 ?
N2 C2 N2 88(9) 5 8_656 ?
N2 C2 N2 119.0(13) . 6_566 ?
N2 C2 N2 117(2) 4_566 8_656 ?
N2 C2 N2 151.7(17) . 2_665 ?
N2 C2 N2 88(9) 6_566 7_665 ?
N2 C2 N2 36.6(19) 6_566 2_665 ?
N2 C2 N2 117(2) 10_656 7_665 ?
N2 C2 N2 117(2) . 10_656 ?
N2 C2 N2 99(8) 5 7_665 ?
N2 C2 N2 37(2) 6_566 10_656 ?
N2 C2 N2 37(2) 4_566 7_665 ?
N2 C2 N2 37(2) 2_665 10_656 ?
N2 C2 N2 99(8) . 3_656 ?
N2 C2 N2 82.4(12) . 9 ?
N2 C2 N2 88(9) 2_665 3_656 ?
N2 C2 N2 117(2) 6_566 9 ?
N2 C2 N2 117(2) 9 3_656 ?
N2 C2 N2 119.0(13) 2_665 9 ?
N2 C2 N2 37(2) 12_665 3_656 ?
N2 C2 N2 151.7(17) 10_656 9 ?
N2 C2 N2 82.4(12) 8_656 3_656 ?
N2 C2 N2 82.4(12) . 5 ?
N2 C2 N2 37(2) . 11_566 ?
N2 C2 N2 151.7(17) 6_566 5 ?
N2 C2 N2 117(2) 2_665 11_566 ?
N2 C2 N2 117(2) 2_665 5 ?
N2 C2 N2 99(8) 9 11_566 ?
N2 C2 N2 119.0(13) 10_656 5 ?
N2 C2 N2 151.7(17) 12_665 11_566 ?
N2 C2 N2 82.4(12) 9 5 ?
N2 C2 N2 37(2) 8_656 11_566 ?
N2 C2 N2 119.0(13) . 12_665 ?
N2 C2 N2 119.0(13) 3_656 11_566 ?
N2 C2 N2 119.0(13) 6_566 12_665 ?
N2 C2 N2 36.6(19) 9 4_566 ?
C1 N1 Ni1 175.9(3) . . ?
N1 C1 S1 177.3(3) . . ?
C2 N2 N2 48.8(6) . 5 ?
C2 N2 N2 46(4) . 4_566 ?
C2 N2 N2 48.8(6) . 9 ?
N2 N2 C2 71.7(10) 11_566 . ?
N2 N2 C2 71.7(10) 8_656 . ?
N2 N2 N2 120.5(7) 8_656 9 ?
N2 N2 N2 60.001(4) 9 5 ?
N2 N2 N2 97(9) 11_566 9 ?
N2 N2 N2 71(8) 11_566 4_566 ?
N2 N2 N2 110(8) 8_656 4_566 ?
N2 N2 N2 79(5) 5 4_566 ?
N2 N2 N2 27(3) 9 4_566 ?
N2 N2 N2 118(5) 11_566 5 ?
N2 N2 N2 60.000(14) 8_656 11_566 ?
N2 N2 N2 83(10) 8_656 5 ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 N2 N2 -64(17) 6_566 . . 8_656 ?
N2 C2 N2 N2 -118.7(12) 10_656 . . 5 ?
N2 C2 N2 N2 -152.4(14) 3_656 . . 4_566 ?
N2 C2 N2 N2 -39(10) 2_665 . . 8_656 ?
N2 C2 N2 N2 80(5) 6_566 . . 4_566 ?
N2 C2 N2 N2 -22(16) 10_656 . . 8_656 ?
N2 C2 N2 N2 -116(3) 3_656 . . 9 ?
N2 C2 N2 N2 180(15) 9 . . 8_656 ?
N2 C2 N2 N2 -96(15) 8_656 . . 5 ?
N2 C2 N2 N2 96(15) 5 . . 8_656 ?
N2 C2 N2 N2 -120(3) 5 . . 4_566 ?
N2 C2 N2 N2 97(5) 12_665 . . 8_656 ?
N2 C2 N2 N2 -180(15) 8_656 . . 9 ?
N2 C2 N2 N2 -144(12) 4_566 . . 8_656 ?
N2 C2 N2 N2 -160(3) 6_566 . . 5 ?
N2 C2 N2 N2 -167(5) 7_665 . . 8_656 ?
N2 C2 N2 N2 0(10) 12_665 . . 5 ?
N2 C2 N2 N2 64(12) 3_656 . . 8_656 ?
N2 C2 N2 N2 -33(3) 3_656 . . 5 ?
N2 C2 N2 N2 -63.6(4) 11_566 . . 8_656 ?
N2 C2 N2 N2 122(4) 10_656 . . 4_566 ?
N2 C2 N2 N2 0(17) 6_566 . . 11_566 ?
N2 C2 N2 N2 144(12) 8_656 . . 4_566 ?
N2 C2 N2 N2 25(10) 2_665 . . 11_566 ?
N2 C2 N2 N2 36(3) 4_566 . . 9 ?
N2 C2 N2 N2 41(16) 10_656 . . 11_566 ?
N2 C2 N2 N2 13(10) 7_665 . . 9 ?
N2 C2 N2 N2 -117(15) 9 . . 11_566 ?
N2 C2 N2 N2 117(15) 11_566 . . 9 ?
N2 C2 N2 N2 160(14) 5 . . 11_566 ?
N2 C2 N2 N2 -135(5) 2_665 . . 5 ?
N2 C2 N2 N2 160(4) 12_665 . . 11_566 ?
N2 C2 N2 N2 83.3(9) 9 . . 5 ?
N2 C2 N2 N2 -80(12) 4_566 . . 11_566 ?
N2 C2 N2 N2 120(3) 4_566 . . 5 ?
N2 C2 N2 N2 63.6(4) 8_656 . . 11_566 ?
N2 C2 N2 N2 96(9) 7_665 . . 5 ?
N2 C2 N2 N2 -103(5) 7_665 . . 11_566 ?
N2 C2 N2 N2 -160(14) 11_566 . . 5 ?
N2 C2 N2 N2 127(12) 3_656 . . 11_566 ?
N2 C2 N2 N2 105(2) 2_665 . . 4_566 ?
N2 C2 N2 N2 116(2) 6_566 . . 9 ?
N2 C2 N2 N2 -36(3) 9 . . 4_566 ?
N2 C2 N2 N2 142(5) 2_665 . . 9 ?
N2 C2 N2 N2 -120(7) 12_665 . . 4_566 ?
N2 C2 N2 N2 158.0(16) 10_656 . . 9 ?
N2 C2 N2 N2 -23(7) 7_665 . . 4_566 ?
N2 C2 N2 N2 -83.3(9) 5 . . 9 ?
N2 C2 N2 N2 80(12) 11_566 . . 4_566 ?
N2 C2 N2 N2 -83(10) 12_665 . . 9 ?

_olex2_submission_special_instructions 'No special instructions were received'

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: butanone'
