#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:37:40 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716696.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_7716696
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         '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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     18.00  43.00   0.50   45.76    --   10.00  65.00 -45.00   50
  2  ω    -47.00 -22.00   0.50   45.76    --   10.00 -65.00 178.00   50
  3  ω    -47.00  13.00   0.50   45.76    --  -10.20 -65.00 178.00  120
  4  ω      7.00  33.00   0.50   45.76    --  -10.20  65.00 -45.00   52
  5  ω    -27.00  99.00   0.50   45.76    --   10.00  38.00-120.00  252
  6  ω     18.00  99.00   0.50   45.76    --   10.00  82.00  60.00  162
  7  ω    -13.00  77.00   0.50   45.76    --   10.00  77.00 -30.00  180
  8  ω      7.00  32.00   0.50   45.76    --   10.00  77.00-180.00   50
  9  ω     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       'ω 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/[σ²(Fo²)+(0.0356P)²+2.6328P] where P=(Fo²+2Fc²)/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 > 2σ(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'
_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 99.40
_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
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
Bi1 Bi 0.500000 0.500000 0.500000 0.05208(19) Uani 0.771(5) 4 d S T P A 7
I1 I 0.500000 0.25225(4) 0.500000 0.06539(18) Uani 1 2 d S T P . .
I2 I 0.25664(4) 0.500000 0.53889(4) 0.06394(18) Uani 1 2 d S T P . .
I3 I 0.40075(5) 0.500000 0.25795(4) 0.0737(2) Uani 1 2 d S T P . .
I5 I 0.000000 0.500000 0.000000 0.0982(3) Uani 1 4 d S T P B 3
I4 I -0.01097(8) 0.500000 0.22879(7) 0.1279(3) Uani 1 2 d S T P . .
N1 N 0.289(3) 0.218(3) 0.6830(16) 0.106(8) Uani 0.54 1 d D U P C 1
H1A H 0.230535 0.178210 0.651237 0.128 Uiso 0.54 1 calc R U P C 1
H1B H 0.298293 0.273032 0.640821 0.128 Uiso 0.54 1 calc R U P C 1
H1C H 0.351803 0.177537 0.694767 0.128 Uiso 0.54 1 calc R U P C 1
C1 C 0.367(4) 0.355(5) 0.954(2) 0.175(14) Uani 0.54 1 d D U P C 1
H1D H 0.432945 0.398744 0.975931 0.263 Uiso 0.54 1 calc R U P C 1
H1E H 0.300545 0.395603 0.961153 0.263 Uiso 0.54 1 calc R U P C 1
H1F H 0.372165 0.291941 0.998244 0.263 Uiso 0.54 1 calc R U P C 1
C3 C 0.2688(16) 0.2589(16) 0.7862(14) 0.127(5) Uani 0.54 1 d D U P C 1
H3A H 0.199275 0.300672 0.772300 0.153 Uiso 0.54 1 calc R U P C 1
H3B H 0.256871 0.197886 0.830366 0.153 Uiso 0.54 1 calc R U P C 1
C2 C 0.3575(19) 0.3244(18) 0.8461(14) 0.144(6) Uani 0.54 1 d D U P C 1
H2A H 0.427956 0.288077 0.842501 0.173 Uiso 0.54 1 calc R U P C 1
H2B H 0.357032 0.390732 0.805770 0.173 Uiso 0.54 1 calc R U P C 1
C4 C 0.317(4) 0.348(6) 0.947(3) 0.177(15) Uani 0.46 1 d D U P D 2
H4A H 0.252686 0.356375 0.980894 0.265 Uiso 0.46 1 calc R U P D 2
H4B H 0.373189 0.304332 0.992645 0.265 Uiso 0.46 1 calc R U P D 2
H4C H 0.348238 0.416973 0.937147 0.265 Uiso 0.46 1 calc R U P D 2
N2 N 0.294(3) 0.218(3) 0.6716(19) 0.075(7) Uani 0.46 1 d D U P D 2
H2C H 0.344219 0.204032 0.631276 0.090 Uiso 0.46 1 calc R U P D 2
H2D H 0.261207 0.156574 0.686043 0.090 Uiso 0.46 1 calc R U P D 2
H2E H 0.240687 0.262139 0.636491 0.090 Uiso 0.46 1 calc R U P D 2
C6 C 0.3506(18) 0.2688(17) 0.7729(14) 0.117(5) Uani 0.46 1 d D U P D 2
H6A H 0.409619 0.220366 0.808352 0.140 Uiso 0.46 1 calc R U P D 2
H6B H 0.387567 0.333807 0.755103 0.140 Uiso 0.46 1 calc R U P D 2
C5 C 0.282(2) 0.297(2) 0.8477(18) 0.149(7) Uani 0.46 1 d D U P D 2
H5A H 0.221992 0.341370 0.808147 0.179 Uiso 0.46 1 calc R U P D 2
H5B H 0.246655 0.230028 0.863006 0.179 Uiso 0.46 1 calc R U P D 2
Sb1 Sb 0.500000 0.500000 0.500000 0.05208(19) Uani 0.229(5) 4 d S T P A 8
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'
Bi Bi -4.1077 10.2566 '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 Bi1 I1 180.0 5_666 . ?
I2 Bi1 I1 90.0 5_666 . ?
I2 Bi1 I1 90.0 . 5_666 ?
I2 Bi1 I1 90.0 . . ?
I2 Bi1 I1 90.0 5_666 5_666 ?
I2 Bi1 I2 180.0 . 5_666 ?
I3 Bi1 I1 90.0 5_666 . ?
I3 Bi1 I1 90.0 . 5_666 ?
I3 Bi1 I1 90.0 5_666 5_666 ?
I3 Bi1 I1 90.0 . . ?
I3 Bi1 I2 88.306(15) . . ?
I3 Bi1 I2 91.695(15) . 5_666 ?
I3 Bi1 I2 88.305(15) 5_666 5_666 ?
I3 Bi1 I2 91.694(15) 5_666 . ?
I3 Bi1 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 . . ?
N1 C3 H3A 108.4 . . ?
N1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C2 C3 N1 115.3(18) . . ?
C2 C3 H3A 108.4 . . ?
C2 C3 H3B 108.4 . . ?
C1 C2 C3 125(2) . . ?
C1 C2 H2A 106.1 . . ?
C1 C2 H2B 106.1 . . ?
C3 C2 H2A 106.1 . . ?
C3 C2 H2B 106.1 . . ?
H2A C2 H2B 106.3 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
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 108.0 . . ?
N2 C6 H6B 108.0 . . ?
H6A C6 H6B 107.2 . . ?
C5 C6 N2 117.3(19) . . ?
C5 C6 H6A 108.0 . . ?
C5 C6 H6B 108.0 . . ?
C4 C5 C6 128(3) . . ?
C4 C5 H5A 105.4 . . ?
C4 C5 H5B 105.4 . . ?
C6 C5 H5A 105.4 . . ?
C6 C5 H5B 105.4 . . ?
H5A C5 H5B 106.0 . . ?
I1 Sb1 I1 180.0 5_666 . ?
I2 Sb1 I1 90.0 . 5_666 ?
I2 Sb1 I1 90.0 . . ?
I2 Sb1 I1 90.0 5_666 . ?
I2 Sb1 I1 90.0 5_666 5_666 ?
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 5_666 5_666 ?
I3 Sb1 I1 90.0 . . ?
I3 Sb1 I2 88.306(15) . . ?
I3 Sb1 I2 88.305(15) 5_666 5_666 ?
I3 Sb1 I2 91.694(15) 5_666 . ?
I3 Sb1 I2 91.695(15) . 5_666 ?
I3 Sb1 I3 180.0 . 5_666 ?
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
Bi1 I1 3.0753(5) . ?
Bi1 I1 3.0753(5) 5_666 ?
Bi1 I2 3.0687(5) . ?
Bi1 I2 3.0687(5) 5_666 ?
Bi1 I3 3.0683(5) 5_666 ?
Bi1 I3 3.0683(5) . ?
I1 Sb1 3.0753(5) . ?
I2 Sb1 3.0687(5) . ?
I3 Sb1 3.0683(5) . ?
I5 I4 2.9385(9) . ?
I5 I4 2.9385(9) 5_565 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C3 1.474(18) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C1 C2 1.405(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.433(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C5 1.40(2) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C6 1.474(19) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.420(18) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
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
N1 C3 C2 C1 -167(4) . . . . ?
N2 C6 C5 C4 -178(5) . . . . ?
