#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:16:29 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263673 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/01/1560103.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1560103
loop_
_publ_author_name
'Lee, Jie Yie'
'Ling, Sanliang'
'Argent, Stephen P.'
'Senn, Mark S.'
'Cañadillas-Delgado, Laura'
'Cliffe, Matthew J.'
_publ_section_title
;
 Controlling multiple orderings in metal thiocyanate molecular perovskites
 Ax{Ni[Bi(SCN)6]}
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3516
_journal_page_last               3525
_journal_paper_doi               10.1039/D0SC06619B
_journal_volume                  12
_journal_year                    2021
_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_name_systematic        'Ammonium nickel hexathiocyanatobismuthate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                97.5740(10)
_cell_angle_beta                 92.1370(10)
_cell_angle_gamma                91.8170(10)
_cell_formula_units_Z            3
_cell_length_a                   8.44100(10)
_cell_length_b                   8.68990(10)
_cell_length_c                   11.8177(2)
_cell_measurement_reflns_used    9374
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      60.791
_cell_measurement_theta_min      4.585
_cell_volume                     858.10(2)
_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)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  'D19, Institut Laue Langevin'
_diffrn_radiation_type           neutrons
_diffrn_radiation_wavelength     0.94558
_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
_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_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.455
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: butanone'
_exptl_crystal_size_max          2.9
_exptl_crystal_size_mid          2.5
_exptl_crystal_size_min          2.2
_refine_diff_density_max         1.227
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.251
_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_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0448
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9374
_reflns_number_total             9590
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc06619b3.cif
_cod_data_source_block           1NH4NiBiSCN6_20K_neutron
_cod_depositor_comments
'Adding full bibliography for 1560103--1560109.cif.'
_cod_database_code               1560103
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 . . . . .
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'
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) . . ?
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) . ?
