#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:37:40 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716691.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716691
loop_
_publ_author_name
'Pradhan, Abinash'
'Rana, Rajanikanta'
'Rajaraman, Gopalan'
'Pradhan, Monalisa'
'Samal, Saroj L.'
_publ_section_title
;
 (C₃H₇NH₃)₄Bi₁₋ₓSbₓI₉:
 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         'I6 Sb, 2(I1.5), 4(C3 H10 N)'
_chemical_formula_sum            'C12 H40 I9 N4 Sb'
_chemical_formula_weight         1504.33
_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                 101.585(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0079(7)
_cell_length_b                   12.3595(8)
_cell_length_c                   12.7066(8)
_cell_measurement_reflns_used    4191
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6380
_cell_measurement_theta_min      2.3900
_cell_volume                     1847.4(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -31.00  34.00   0.50   59.91    --   10.00 -57.00   0.00  130
  2  ω    -88.00 -46.00   0.50   59.91    --  -10.20 -57.00-150.00   84
  3  ω    -57.00  14.00   0.50   59.91    --  -10.20 -82.00-150.00  142
  4  ω    -35.00  12.00   0.50   59.91    --  -10.20  82.00  90.00   94
  5  ω    -93.00 -22.00   0.50   59.91    --  -10.20 -77.00 -90.00  142
  6  ω    -13.00  14.00   0.50   59.91    --  -10.20 -77.00 -90.00   54
  7  ω     -5.00  20.00   0.50   59.91    --  -10.20 -57.00-150.00   50
  8  ω    -51.00   3.00   0.50   59.91    --  -10.20 -82.00 120.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051944000
_diffrn_orient_matrix_UB_12      0.0241076000
_diffrn_orient_matrix_UB_13      0.0494366000
_diffrn_orient_matrix_UB_21      0.0260936000
_diffrn_orient_matrix_UB_22      -0.0459654000
_diffrn_orient_matrix_UB_23      0.0280872000
_diffrn_orient_matrix_UB_31      0.0541075000
_diffrn_orient_matrix_UB_32      0.0244745000
_diffrn_orient_matrix_UB_33      0.0040108000
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6649
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.021
_diffrn_reflns_theta_min         2.390
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54140
_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    2.704
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.768
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2014
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0528
_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/[σ²(Fo²)+(0.0966P)²+9.1644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1702
_reflns_number_total             2014
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01692k2.cif
_cod_data_source_block           ab408_170223
_cod_depositor_comments
'Adding full bibliography for 7716690--7716700.cif.'
_cod_database_code               7716691
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Sb I'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.80
_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. Restrained distances
 N1-C3 \\sim N2-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 N2-C5
 with sigma of 0.04
 C1-C3 \\sim C4-C6
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N1 \\sim C3 \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N1 \\sim C1 \\sim C2 \\sim C3 \\sim N2 \\sim C6 \\sim C5 \\sim C4: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 N1, C3, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C1, C2, C3, N2, C6, C5, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.52) H1A(0.52) H1B(0.52) H1C(0.52) C1(0.52) H1D(0.52)
 H1E(0.52) H1F(0.52) C2(0.52) H2A(0.52) H2B(0.52) C3(0.52) H3A(0.52) H3B(0.52)
 N2(0.48) H2C(0.48) H2D(0.48) H2E(0.48) C6(0.48) H6A(0.48) H6B(0.48) C5(0.48)
 H5A(0.48) H5B(0.48) C4(0.48) H4A(0.48) H4B(0.48) H4C(0.48)
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(H1A,H1B,H1C), C1(H1D,H1E,H1F), N2(H2C,H2D,H2E), 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 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.733
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.500000 0.500000 0.500000 0.0518(3) Uani 1 4 d S T P . .
I1 I 0.500000 0.25442(7) 0.500000 0.0634(3) Uani 1 2 d S T P . .
I2 I 0.25910(7) 0.500000 0.53806(8) 0.0621(3) Uani 1 2 d S T P . .
I3 I 0.40295(10) 0.500000 0.26118(8) 0.0722(4) Uani 1 2 d S T P . .
I5 I 0.000000 0.500000 0.000000 0.0978(6) Uani 1 4 d S T P . .
I4 I -0.01103(16) 0.500000 0.22898(15) 0.1272(6) Uani 1 2 d S T P . .
N1 N 0.285(5) 0.232(2) 0.675(2) 0.076(8) Uani 0.52 1 d D U P A 1
H1A H 0.227064 0.191673 0.641764 0.091 Uiso 0.52 1 calc R U P A 1
H1B H 0.286929 0.293558 0.639348 0.091 Uiso 0.52 1 calc R U P A 1
H1C H 0.349732 0.196093 0.677997 0.091 Uiso 0.52 1 calc R U P A 1
C1 C 0.359(5) 0.337(4) 0.961(2) 0.133(13) Uani 0.52 1 d D U P A 1
H1D H 0.422495 0.381875 0.992519 0.199 Uiso 0.52 1 calc R U P A 1
H1E H 0.289631 0.372033 0.968125 0.199 Uiso 0.52 1 calc R U P A 1
H1F H 0.365041 0.268450 0.996458 0.199 Uiso 0.52 1 calc R U P A 1
C2 C 0.360(3) 0.321(3) 0.847(2) 0.116(8) Uani 0.52 1 d D U P A 1
H2A H 0.356866 0.392138 0.813945 0.139 Uiso 0.52 1 calc R U P A 1
H2B H 0.431938 0.289018 0.842152 0.139 Uiso 0.52 1 calc R U P A 1
C3 C 0.270(3) 0.256(3) 0.784(2) 0.110(7) Uani 0.52 1 d D U P A 1
H3A H 0.198248 0.292881 0.779959 0.132 Uiso 0.52 1 calc R U P A 1
H3B H 0.265874 0.187931 0.821576 0.132 Uiso 0.52 1 calc R U P A 1
N2 N 0.297(5) 0.200(3) 0.682(2) 0.081(10) Uani 0.48 1 d D U P B 2
H2C H 0.347655 0.181702 0.643111 0.097 Uiso 0.48 1 calc R U P B 2
H2D H 0.269373 0.140323 0.707062 0.097 Uiso 0.48 1 calc R U P B 2
H2E H 0.240478 0.236796 0.641902 0.097 Uiso 0.48 1 calc R U P B 2
C6 C 0.352(3) 0.267(3) 0.773(3) 0.108(7) Uani 0.48 1 d D U P B 2
H6A H 0.414530 0.226673 0.814817 0.129 Uiso 0.48 1 calc R U P B 2
H6B H 0.383428 0.330515 0.744681 0.129 Uiso 0.48 1 calc R U P B 2
C5 C 0.278(3) 0.303(4) 0.844(3) 0.134(9) Uani 0.48 1 d D U P B 2
H5A H 0.252025 0.238377 0.874980 0.161 Uiso 0.48 1 calc R U P B 2
H5B H 0.212297 0.336083 0.799248 0.161 Uiso 0.48 1 calc R U P B 2
C4 C 0.321(5) 0.377(4) 0.932(3) 0.154(17) Uani 0.48 1 d D U P B 2
H4A H 0.261582 0.392115 0.970189 0.231 Uiso 0.48 1 calc R U P B 2
H4B H 0.384360 0.345009 0.979252 0.231 Uiso 0.48 1 calc R U P B 2
H4C H 0.344387 0.443319 0.903052 0.231 Uiso 0.48 1 calc R U P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Sb1 I1 180.0 . 5_666 ?
I2 Sb1 I1 90.0 . 5_666 ?
I2 Sb1 I1 90.0 5_666 . ?
I2 Sb1 I1 90.0 5_666 5_666 ?
I2 Sb1 I1 90.0 . . ?
I2 Sb1 I2 180.0 5_666 . ?
I3 Sb1 I1 90.0 5_666 . ?
I3 Sb1 I1 90.0 . 5_666 ?
I3 Sb1 I1 90.0 . . ?
I3 Sb1 I1 90.0 5_666 5_666 ?
I3 Sb1 I2 91.59(3) 5_666 . ?
I3 Sb1 I2 88.41(3) 5_666 5_666 ?
I3 Sb1 I2 91.59(3) . 5_666 ?
I3 Sb1 I2 88.41(3) . . ?
I3 Sb1 I3 180.0 . 5_666 ?
I4 I5 I4 180.0 . 5_565 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 N1 H1A 109.5 . . ?
C3 N1 H1B 109.5 . . ?
C3 N1 H1C 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
C2 C1 H1F 109.5 . . ?
C1 C2 H2A 107.8 . . ?
C1 C2 H2B 107.8 . . ?
H2A C2 H2B 107.1 . . ?
C3 C2 C1 118(3) . . ?
C3 C2 H2A 107.8 . . ?
C3 C2 H2B 107.8 . . ?
N1 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C2 C3 N1 115(3) . . ?
C2 C3 H3A 108.6 . . ?
C2 C3 H3B 108.6 . . ?
H3A C3 H3B 107.5 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C6 N2 H2C 109.5 . . ?
C6 N2 H2D 109.5 . . ?
C6 N2 H2E 109.5 . . ?
N2 C6 H6A 108.5 . . ?
N2 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C5 C6 N2 115(3) . . ?
C5 C6 H6A 108.5 . . ?
C5 C6 H6B 108.5 . . ?
C6 C5 H5A 107.2 . . ?
C6 C5 H5B 107.2 . . ?
C6 C5 C4 120(4) . . ?
H5A C5 H5B 106.9 . . ?
C4 C5 H5A 107.2 . . ?
C4 C5 H5B 107.2 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 I1 3.0352(8) . ?
Sb1 I1 3.0352(8) 5_666 ?
Sb1 I2 3.0271(8) 5_666 ?
Sb1 I2 3.0272(8) . ?
Sb1 I3 3.0243(10) 5_666 ?
Sb1 I3 3.0243(10) . ?
I5 I4 2.9390(19) 5_565 ?
I5 I4 2.9390(19) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C3 1.46(3) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C1 C2 1.46(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.45(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C6 1.46(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.45(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.46(4) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 N1 -172(4) . . . . ?
N2 C6 C5 C4 -175(4) . . . . ?
