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_1560106
_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, C N'
_chemical_formula_sum            'C7 Bi N7 Ni S6'
_chemical_formula_weight         642.19
_chemical_name_systematic
'Methylammonium nickel hexathiocyanatobismuthate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 90.2240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   12.21600(10)
_cell_length_b                   36.8375(4)
_cell_length_c                   24.5263(3)
_cell_measurement_reflns_used    18570
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      72.7830
_cell_measurement_theta_min      6.2390
_cell_volume                     11036.9(2)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  38.00   1.00    5.00    --  -41.82  19.00-180.00   43
  2  \w   -130.00  46.00   1.00    5.00    --  -41.82   0.00   0.00  176
  3  \w     27.00  98.00   1.00    5.00    --   41.82-125.00  90.00   71
  4  \w     25.00  96.00   1.00    5.00    --   41.82-122.00 -68.00   71
  5  \w     28.00  57.00   1.00   20.00    --  104.36 -30.00 120.00   29
  6  \w     76.00 178.00   1.00   20.00    --  104.36  30.00  90.00  102
  7  \w     22.00 106.00   1.00   20.00    --  104.36 -94.00  90.00   84
  8  \w     28.00  57.00   1.00   20.00    --  104.36 -30.00 -90.00   29
  9  \w     28.00  57.00   1.00   20.00    --  104.36 -30.00 150.00   29
 10  \w     97.00 178.00   1.00   20.00    --  104.36 125.00 -90.00   81
 11  \w     97.00 178.00   1.00   20.00    --  104.36 125.00 150.00   81
 12  \w     31.00 112.00   1.00   20.00    --  104.36-125.00 -60.00   81
 13  \w     28.00  57.00   1.00   20.00    --  104.36 -30.00-180.00   29
 14  \w     31.00  72.00   1.00   20.00    --  104.36 -45.00-120.00   41
 15  \w     97.00 178.00   1.00   20.00    --  104.36 125.00 -30.00   81
 16  \w    103.00 178.00   1.00   20.00    --  104.36  77.00 -60.00   75
 17  \w     39.00 130.00   1.00   20.00    --  104.36-150.00 129.00   91
 18  \w     31.00  72.00   1.00   20.00    --  104.36 -45.00  60.00   41
 19  \w     28.00  57.00   1.00   20.00    --  104.36 -30.00 -60.00   29
 20  \w    103.00 178.00   1.00   20.00    --  104.36  77.00-180.00   75
 21  \w     28.00 127.00   1.00   20.00    --  104.36 -77.00-120.00   99
 22  \w   -116.00 -17.00   1.00    5.00    --  -41.82 -38.00-150.00   99
 23  \w   -114.00 -14.00   1.00    5.00    --  -41.82 -57.00 -30.00  100
 24  \w    -21.00  32.00   1.00    5.00    --  -41.82  38.00 120.00   53
 25  \w     14.00 114.00   1.00    5.00    --   41.82  57.00-180.00  100
 26  \w     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       '\w 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_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_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_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_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.319
_exptl_crystal_description       block
_exptl_crystal_F_000             7152
_exptl_crystal_preparation       'Evaporation from butanone'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: butanone'
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.167
_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_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0422
_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/[\s^2^(Fo^2^)+(0.0236P)^2^+68.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18472
_reflns_number_total             21661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06619b3.cif
_cod_data_source_block           3MeNH3NiBiSCN6
_cod_depositor_comments
'Adding full bibliography for 1560103--1560109.cif.'
_cod_database_code               1560106
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C7N7H6S6Ni1Bi1
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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)
;
_shelx_res_checksum              12502
_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