(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_7716698
_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         'Bi I6, 2(I1.5), 4(C3 H10 N)'
_chemical_formula_sum            'C12 H40 Bi I9 N4'
_chemical_formula_weight         1591.56
_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             2024-05-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2024-05-23 deposited with the CCDC.	2024-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.505(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0165(5)
_cell_length_b                   12.2618(6)
_cell_length_c                   12.5979(5)
_cell_measurement_reflns_used    5635
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9430
_cell_measurement_theta_min      2.3910
_cell_volume                     1812.19(14)
_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 0.995
_diffrn_measured_fraction_theta_max 0.947
_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  31.00   0.50    7.69    --   10.00  54.00  73.00   52
  2  \w    -43.00 -18.00   0.50    7.69    --   10.00 -54.00 -70.00   50
  3  \w    -39.00  -9.00   0.50    7.69    --  -10.20 -54.00 -70.00   60
  4  \w    -43.00  70.00   0.50    7.69    --  -10.20  54.00  73.00  226
  5  \w     33.00  73.00   0.50    7.69    --   10.00  77.00 150.00   80
  6  \w    -54.00 -28.00   0.50    7.69    --   10.00 -82.00-150.00   52
  7  \w    -10.00  15.00   0.50    7.69    --   10.00 -82.00-150.00   50
  8  \w    -11.00  97.00   0.50    7.69    --   10.00  77.00 120.00  216
  9  \w    -56.00 -31.00   0.50    7.69    --   10.00 -57.00 120.00   50
 10  \w     15.00  40.00   0.50    7.69    --   10.00 -57.00 120.00   50
 11  \w    -40.00  75.00   0.50    7.69    --  -10.20  38.00   0.00  230
;
_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      -0.0436056000
_diffrn_orient_matrix_UB_12      -0.0377563000
_diffrn_orient_matrix_UB_13      0.0039904000
_diffrn_orient_matrix_UB_21      0.0190396000
_diffrn_orient_matrix_UB_22      -0.0007860000
_diffrn_orient_matrix_UB_23      0.0573931000
_diffrn_orient_matrix_UB_31      -0.0372244000
_diffrn_orient_matrix_UB_32      0.0438407000
_diffrn_orient_matrix_UB_33      0.0044135000
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8563
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.066
_diffrn_reflns_theta_min         2.403
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.296
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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_density_diffrn    2.917
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.667
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       0.00054(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1972
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0046P)^2^+2.9983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1609
_reflns_number_total             1972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01692k2.cif
_cod_data_source_block           ab411_180k_abs
_cod_depositor_comments
'Adding full bibliography for 7716690--7716700.cif.'
_cod_database_code               7716698
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Bi I'
_shelx_estimated_absorpt_t_max   0.367
_shelx_estimated_absorpt_t_min   0.188
_reflns_odcompleteness_completeness 99.08
_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,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3 \\sim N1-C6
 with sigma of 0.02
 C1-C2 \\sim C4-C5
 with sigma of 0.02
 C2-C3 \\sim C5-C6
 with sigma of 0.02
 N1-C2 \\sim N1-C5
 with sigma of 0.04
 C1-C3 \\sim C4-C6
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C4 \\sim N1 \\sim C3 \\sim C6 \\sim C2 \\sim C5 \\sim C1: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C4, N1, C3, C6, C2, C5, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(C5)=Sof(H5A)=Sof(H5B)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=
 Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C5(H5A,H5B)
6.b Me refined with riding coordinates:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF), C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_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 23.714
_oxdiff_exptl_absorpt_empirical_full_min 0.244