(C<sub>3</sub>H<sub>7</sub>NH<sub>3</sub>)<sub>4</sub>Bi<sub>1-<i>x</i></sub>Sb<sub><i>x</i></sub>I<sub>9</sub>: 0D hybrid halide perovskite-like compounds with isolated triiodide units.
Pradhan, Abinash; Rana, Rajanikanta; Rajaraman, Gopalan; Pradhan, Monalisa; Samal, Saroj L.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13628–13637; doi:10.1039/d4dt01692k

data_7716696
_publ_section_title
;
 (C<sub>3</sub>H<sub>7</sub>NH<sub>3</sub>)<sub>4</sub>Bi<sub>1-<i>x</i></sub>Sb<sub><i>x</i></sub>I<sub>9</sub>:
 0D hybrid halide perovskite-like compounds with isolated triiodide units.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13628
_journal_page_last               13637
_journal_paper_doi               10.1039/d4dt01692k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Bi0.771 I6 Sb0.229, 2(I1.5), 4(C3 H10 N)'
_chemical_formula_sum            'C12 H40 Bi0.77 I9 N4 Sb0.23'
_chemical_formula_weight         1571.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2024-02-22 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.651(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0415(4)
_cell_length_b                   12.4130(5)
_cell_length_c                   12.7149(4)
_cell_measurement_reflns_used    4981
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3630
_cell_measurement_theta_min      2.3760
_cell_volume                     1861.35(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.950
_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     18.00  43.00   0.50   45.76    --   10.00  65.00 -45.00   50
  2  \w    -47.00 -22.00   0.50   45.76    --   10.00 -65.00 178.00   50
  3  \w    -47.00  13.00   0.50   45.76    --  -10.20 -65.00 178.00  120
  4  \w      7.00  33.00   0.50   45.76    --  -10.20  65.00 -45.00   52
  5  \w    -27.00  99.00   0.50   45.76    --   10.00  38.00-120.00  252
  6  \w     18.00  99.00   0.50   45.76    --   10.00  82.00  60.00  162
  7  \w    -13.00  77.00   0.50   45.76    --   10.00  77.00 -30.00  180
  8  \w      7.00  32.00   0.50   45.76    --   10.00  77.00-180.00   50
  9  \w     24.00  72.00   0.50   45.76    --   10.00  77.00  30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0007418000
_diffrn_orient_matrix_UB_12      0.0171853000
_diffrn_orient_matrix_UB_13      0.0530596000
_diffrn_orient_matrix_UB_21      0.0417738000
_diffrn_orient_matrix_UB_22      0.0393280000
_diffrn_orient_matrix_UB_23      -0.0036146000
_diffrn_orient_matrix_UB_31      -0.0432537000
_diffrn_orient_matrix_UB_32      0.0377277000
_diffrn_orient_matrix_UB_33      -0.0204129000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8454
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.056
_diffrn_reflns_theta_min         2.382
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.289
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.804
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             1385
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.604
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2030
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0356P)^2^+2.6328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1702
_reflns_number_total             2030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01692k2.cif
_cod_data_source_block           ab412_270223
_cod_depositor_comments
'Adding full bibliography for 7716690--7716700.cif.'
_cod_database_code               7716696
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Bi Sb I'
_reflns_odcompleteness_completeness 99.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Bi1, Sb1}
3. Restrained distances
 N1-C3 \\sim N2-C6
 with sigma of 0.02
 C3-C2 \\sim C6-C5
 with sigma of 0.02
 C1-C3 \\sim C4-C6
 with sigma of 0.04
 C1-C2 \\sim C4-C5
 with sigma of 0.02
 N1-C2 \\sim N2-C5
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim C3 \\sim C2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C3 \\sim C2 \\sim C4 \\sim N2 \\sim C6 \\sim C5: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Bi1) = Uanis(Sb1)
5. Rigid body (RIGU) restrains
 C1, N1, C3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C3, C2, C4, N2, C6, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Sb1)=0.25*(1-FVAR(2))
 Sof(Bi1)=0.25*FVAR(2)
 Fixed Sof: N1(0.54) H1A(0.54) H1B(0.54) H1C(0.54) C1(0.54) H1D(0.54)
 H1E(0.54) H1F(0.54) C3(0.54) H3A(0.54) H3B(0.54) C2(0.54) H2A(0.54) H2B(0.54)
 C4(0.46) H4A(0.46) H4B(0.46) H4C(0.46) N2(0.46) H2C(0.46) H2D(0.46) H2E(0.46)
 C6(0.46) H6A(0.46) H6B(0.46) C5(0.46) H5A(0.46) H5B(0.46)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B)
7.b Me refined with riding coordinates:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F), C4(H4A,H4B,H4C), N2(H2C,H2D,H2E)
;
_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 2.162
_oxdiff_exptl_absorpt_empirical_full_min 0.530