Controlling multiple orderings in metal thiocyanate molecular perovskites Ax{Ni[Bi(SCN)6]}
Lee, Jie Yie; Ling, Sanliang; Argent, Stephen P.; Senn, Mark S.; Cañadillas-Delgado, Laura; Cliffe, Matthew J.; Chemical Science 12 (2021) 3516–3525; doi:10.1039/D0SC06619B

data_1560107
_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         'Bi C6 N6 Ni S6, H4 N'
_chemical_formula_sum            'C6 H4 Bi N7 Ni S6'
_chemical_formula_weight         634.21
_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                97.187(2)
_cell_angle_beta                 91.149(2)
_cell_angle_gamma                91.610(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4699(2)
_cell_length_b                   8.6913(2)
_cell_length_c                   11.9058(3)
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.7520
_cell_measurement_theta_min      3.7000
_cell_volume                     868.96(4)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -73.00  29.00   1.00    1.00    --  -42.81  77.00 150.00  102
  2  \w     19.00 112.00   1.00    1.00    --   42.81  57.00  30.00   93
  3  \w    -27.00  67.00   1.00    1.00    --   42.81 -57.00-120.00   94
  4  \w     30.00  90.00   1.00    4.00    --  103.00 -30.00   0.00   60
  5  \w     31.00 118.00   1.00    4.00    --  103.00-125.00-150.00   87
  6  \w     30.00  90.00   1.00    4.00    --  103.00 -30.00 150.00   60
  7  \w    101.00 178.00   1.00    4.00    --  103.00  91.00  -7.00   77
  8  \w     22.00 110.00   1.00    4.00    --  103.00 -94.00 -30.00   88
  9  \w     31.00 133.00   1.00    4.00    --  103.00 -77.00  60.00  102
 10  \w     30.00  90.00   1.00    4.00    --  103.00 -30.00  60.00   60
 11  \w     34.00  98.00   1.00    4.00    --  103.00 -45.00 -60.00   64
 12  \w     80.00 172.00   1.00    4.00    --  103.00  45.00 -30.00   92
 13  \w     34.00 128.00   1.00    4.00    --  103.00 -61.00-180.00   94
 14  \w     80.00 176.00   1.00    4.00    --  103.00  30.00 -90.00   96
 15  \w     31.00 118.00   1.00    4.00    --  103.00-125.00  90.00   87
 16  \w     31.00 118.00   1.00    4.00    --  103.00-125.00 -60.00   87
 17  \w     19.00 112.00   1.00    1.00    --   42.81  57.00 120.00   93
 18  \w     19.00 112.00   1.00    1.00    --   42.81  57.00-150.00   93
 19  \w     19.00 112.00   1.00    1.00    --   42.81  57.00 -60.00   93
 20  \w     80.00 172.00   1.00    4.00    --  103.00  45.00  30.00   92
 21  \w     73.00 175.00   1.00    4.00    --  103.00  77.00  90.00  102
 22  \w     78.00 172.00   1.00    4.00    --  103.00  61.00  60.00   94
 23  \w     80.00 172.00   1.00    4.00    --  103.00  45.00-180.00   92
 24  \w     73.00 175.00   1.00    4.00    --  103.00  77.00 120.00  102
 25  \w     73.00 175.00   1.00    4.00    --  103.00  77.00 -90.00  102
 26  \w     73.00 175.00   1.00    4.00    --  103.00  77.00 -30.00  102
 27  \w     80.00 172.00   1.00    4.00    --  103.00  45.00-150.00   92
 28  \w     80.00 176.00   1.00    4.00    --  103.00  30.00 120.00   96
 29  \w     12.00 115.00   1.00    1.00    --   42.81  77.00 -60.00  103
 30  \w     12.00  76.00   1.00    1.00    --   42.81  77.00  90.00   64
 31  \w      1.00  82.00   1.00    1.00    --   42.81 -99.00  60.00   81
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_diffrn_measurement_method       '\w 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_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_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_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_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_preparation       'evaporated from methylethylketone solution'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: butanone'
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.187
_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_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0228
_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/[\s^2^(Fo^2^)+(0.0443P)^2^+0.5041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3367
_reflns_number_total             3468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06619b3.cif
_cod_data_source_block           1NH4NiBiSCN6_120K_Xray
_cod_depositor_comments
'Adding full bibliography for 1560103--1560109.cif.'
_cod_database_code               1560107
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'N H4 Ni Bi S6 C6 N6'
_chemical_oxdiff_usercomment
'#17938-NIMCLA GVA-1511 IN FOMBLIN FILM ON MICROMOUNT FOR MC'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
;
_shelx_res_checksum              22681
_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