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_1560105
_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         'C N S, C H6 N3'
_chemical_formula_sum            'C2 H6 N4 S'
_chemical_formula_weight         118.17
_chemical_name_systematic        'guanidinium thiocyanate'
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-15
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2021-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.894(5)
_cell_angle_beta                 104.311(7)
_cell_angle_gamma                101.787(7)
_cell_formula_units_Z            4
_cell_length_a                   6.9352(6)
_cell_length_b                   7.0096(5)
_cell_length_c                   12.3675(7)
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.4830
_cell_measurement_theta_min      3.6280
_cell_volume                     568.89(8)
_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)'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  32.00   1.00    1.00    --  -41.93  38.00 150.00   82
  2  \w    -92.00  -2.00   1.00    1.00    --  -41.93 125.00-150.00   90
  3  \w   -115.00 -14.00   1.00    1.00    --  -41.93 -57.00   0.00  101
  4  \w    -38.00  83.00   1.00    1.00    --   41.93 -19.00 -60.00  121
  5  \w      1.00  83.00   1.00    1.00    --   41.93 -99.00-120.00   82
  6  \w     80.00 178.00   1.00    1.86    --  105.94  45.00 -90.00   98
  7  \w     33.00  98.00   1.00    1.86    --  105.94 -45.00  60.00   65
  8  \w     27.00 111.00   1.00    1.86    --  105.94-103.00  68.00   84
  9  \w     30.00  91.00   1.00    1.86    --  105.94 -30.00   0.00   61
 10  \w     30.00  91.00   1.00    1.86    --  105.94 -30.00 150.00   61
 11  \w     24.00 110.00   1.00    1.86    --  105.94 -95.00 -60.00   86
 12  \w     33.00  98.00   1.00    1.86    --  105.94 -45.00 -60.00   65
 13  \w     33.00 118.00   1.00    1.86    --  105.94-125.00-150.00   85
 14  \w     30.00 139.00   1.00    1.86    --  105.94 -77.00-150.00  109
 15  \w     18.00 178.00   1.00    1.86    --  105.94   0.00-120.00  160
 16  \w     30.00  91.00   1.00    1.86    --  105.94 -30.00-120.00   61
 17  \w     94.00 178.00   1.00    1.86    --  105.94 125.00-120.00   84
 18  \w   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00  30.00  109
 19  \w   -115.00 -14.00   1.00    1.00    --  -41.93 -57.00 150.00  101
 20  \w   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00 120.00  109
 21  \w   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00 -30.00  109
 22  \w   -118.00  -9.00   1.00    1.00    --  -41.93 -77.00-120.00  109
 23  \w     77.00 178.00   1.00    1.86    --  105.94  61.00 -60.00  101
 24  \w     77.00 178.00   1.00    1.86    --  105.94  61.00 -30.00  101
 25  \w     53.00 178.00   1.00    1.86    --  105.94  15.00  60.00  125
 26  \w     73.00 178.00   1.00    1.86    --  105.94  77.00  30.00  105
 27  \w     77.00 178.00   1.00    1.86    --  105.94  61.00 150.00  101
 28  \w     73.00 178.00   1.00    1.86    --  105.94  77.00-180.00  105
 29  \w     73.00 178.00   1.00    1.86    --  105.94  77.00-150.00  105
 30  \w     77.00 178.00   1.00    1.86    --  105.94  61.00 120.00  101
 31  \w     73.00 178.00   1.00    1.86    --  105.94  77.00   0.00  105
 32  \w     77.00 178.00   1.00    1.86    --  105.94  61.00  90.00  101
 33  \w   -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       '\w 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_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_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_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       irregular
_exptl_crystal_F_000             248
_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
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.152
_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_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0898
_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^)+(0.1190P)^2^+3.4535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1975
_reflns_number_total             2256
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06619b3.cif
_cod_data_source_block           GuaSCN
_cod_depositor_comments
'Adding full bibliography for 1560103--1560109.cif.'
_cod_original_cell_volume        568.89(7)
_cod_database_code               1560105
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C2 N4 H6 S'
_chemical_oxdiff_usercomment
'omjclb #18016 in fomblin on micromount for MJC'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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)
;
_shelx_res_checksum              56663
_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