#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:37:40 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716695.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_7716695
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         'Bi0.376 I6 Sb0.624, 2(I1.5), 4(C3 H10 N)'
_chemical_formula_sum            'C12 H40 Bi0.38 I9.01 N4 Sb0.62'
_chemical_formula_weight         1539.18
_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                 101.680(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0266(3)
_cell_length_b                   12.3856(4)
_cell_length_c                   12.7094(4)
_cell_measurement_reflns_used    5569
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6950
_cell_measurement_theta_min      2.3710
_cell_volume                     1853.95(10)
_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 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  35.00   0.50   12.23    --   10.00  46.00  58.00   52
  2  ω     41.00  67.00   0.50   12.23    --   10.00  46.00  58.00   52
  3  ω    -61.00 -14.00   0.50   12.23    --  -10.20 -46.00 -90.00   94
  4  ω    -40.00  28.00   0.50   12.23    --  -10.20  46.00  58.00  136
  5  ω    -42.00 -17.00   0.50   12.23    --   10.00 -46.00 -90.00   50
  6  ω    -18.00  99.00   0.50   12.23    --   10.00  57.00-180.00  234
  7  ω    -16.00  11.00   0.50   12.23    --   10.00  82.00 120.00   54
  8  ω    -36.00  16.00   0.50   12.23    --   10.00 -77.00 150.00  104
  9  ω   -100.00  17.00   0.50   12.23    --  -10.20 -82.00 -90.00  234
;
_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      0.0500790000
_diffrn_orient_matrix_UB_12      -0.0315148000
_diffrn_orient_matrix_UB_13      0.0052796000
_diffrn_orient_matrix_UB_21      0.0007850000
_diffrn_orient_matrix_UB_22      0.0090190000
_diffrn_orient_matrix_UB_23      -0.0549549000
_diffrn_orient_matrix_UB_31      0.0334539000
_diffrn_orient_matrix_UB_32      0.0469552000
_diffrn_orient_matrix_UB_33      0.0141011000
_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  0.0284
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8429
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.966
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46049
_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    2.757
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.519
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.268
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2013
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0328
_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)+(0.0474P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1649
_reflns_number_total             2013
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01692k2.cif
_cod_data_source_block           ab414_280223
_cod_depositor_comments
'Adding full bibliography for 7716690--7716700.cif.'
_cod_database_code               7716695
_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 99.34
_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
 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
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 C2 \\sim C3 \\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, C2, C3, 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) C2(0.54) H2A(0.54) H2B(0.54) C3(0.54) H3A(0.54) H3B(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:
 C2(H2A,H2B), C3(H3A,H3B), 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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.613
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 0.0505(2) Uani 0.376(4) 4 d S T P A 6
I1 I 0.500000 0.25336(4) 0.500000 0.06317(18) Uani 1 2 d S T P . .
I2 I 0.25796(4) 0.500000 0.53854(4) 0.06209(17) Uani 1 2 d S T P . .
I3 I 0.40180(5) 0.500000 0.25963(4) 0.07185(19) Uani 1 2 d S T P . .
I5 I 0.000000 0.500000 1.000000 0.0965(3) Uani 1 4 d S T P B 5
I4 I 0.01114(7) 0.500000 0.77123(7) 0.1261(3) Uani 1 2 d S T P . .
N1 N 0.280(2) 0.226(2) 0.6785(15) 0.073(5) Uani 0.54 1 d D U P C 1
H1A H 0.217643 0.189862 0.648092 0.088 Uiso 0.54 1 calc R U P C 1
H1B H 0.288734 0.282682 0.638161 0.088 Uiso 0.54 1 calc R U P C 1
H1C H 0.340064 0.182599 0.684067 0.088 Uiso 0.54 1 calc R U P C 1
C1 C 0.366(3) 0.349(5) 0.958(2) 0.168(12) Uani 0.54 1 d D U P C 1
H1D H 0.434597 0.389259 0.984546 0.251 Uiso 0.54 1 calc R U P C 1
H1E H 0.301626 0.392891 0.963388 0.251 Uiso 0.54 1 calc R U P C 1
H1F H 0.365873 0.284726 0.999337 0.251 Uiso 0.54 1 calc R U P C 1
C2 C 0.3612(14) 0.3213(15) 0.8465(12) 0.124(5) Uani 0.54 1 d D U P C 1
H2A H 0.366270 0.388531 0.808584 0.149 Uiso 0.54 1 calc R U P C 1
H2B H 0.429996 0.281244 0.844242 0.149 Uiso 0.54 1 calc R U P C 1
C3 C 0.2696(13) 0.2617(16) 0.7840(13) 0.119(5) Uani 0.54 1 d D U P C 1
H3A H 0.201816 0.306002 0.775796 0.143 Uiso 0.54 1 calc R U P C 1
H3B H 0.256931 0.198539 0.825088 0.143 Uiso 0.54 1 calc R U P C 1
C4 C 0.315(3) 0.349(5) 0.947(3) 0.160(13) Uani 0.46 1 d D U P D 2
H4A H 0.252265 0.370088 0.978235 0.240 Uiso 0.46 1 calc R U P D 2
H4B H 0.359831 0.295939 0.991276 0.240 Uiso 0.46 1 calc R U P D 2
H4C H 0.361438 0.411483 0.941250 0.240 Uiso 0.46 1 calc R U P D 2
N2 N 0.305(3) 0.205(3) 0.6794(19) 0.086(8) Uani 0.46 1 d D U P D 2
H2C H 0.360993 0.187111 0.646979 0.103 Uiso 0.46 1 calc R U P D 2
H2D H 0.271978 0.144954 0.697636 0.103 Uiso 0.46 1 calc R U P D 2
H2E H 0.253319 0.243767 0.634859 0.103 Uiso 0.46 1 calc R U P D 2
C6 C 0.3487(15) 0.2670(16) 0.7745(13) 0.110(5) Uani 0.46 1 d D U P D 2
H6A H 0.406600 0.223604 0.819675 0.133 Uiso 0.46 1 calc R U P D 2
H6B H 0.386587 0.329589 0.752341 0.133 Uiso 0.46 1 calc R U P D 2
C5 C 0.2732(18) 0.305(2) 0.8404(17) 0.143(6) Uani 0.46 1 d D U P D 2
H5A H 0.223886 0.244865 0.849076 0.172 Uiso 0.46 1 calc R U P D 2
H5B H 0.225481 0.359579 0.799409 0.172 Uiso 0.46 1 calc R U P D 2
Sb1 Sb 0.500000 0.500000 0.500000 0.0505(2) Uani 0.624(4) 4 d S T P A 7
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 5_666 5_666 ?
I2 Bi1 I1 90.0 . . ?
I2 Bi1 I2 180.0 5_666 . ?
I3 Bi1 I1 90.0 5_666 5_666 ?
I3 Bi1 I1 90.0 . . ?
I3 Bi1 I1 90.0 5_666 . ?
I3 Bi1 I1 90.0 . 5_666 ?
I3 Bi1 I2 91.595(15) . 5_666 ?
I3 Bi1 I2 88.404(15) . . ?
I3 Bi1 I2 91.596(14) 5_666 . ?
I3 Bi1 I2 88.404(14) 5_666 5_666 ?
I3 Bi1 I3 180.0 . 5_666 ?
I4 I5 I4 180.0 . 5_567 ?
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 106.6 . . ?
C1 C2 H2B 106.6 . . ?
H2A C2 H2B 106.6 . . ?
C3 C2 C1 123(2) . . ?
C3 C2 H2A 106.6 . . ?
C3 C2 H2B 106.6 . . ?
N1 C3 H3A 107.7 . . ?
N1 C3 H3B 107.7 . . ?
C2 C3 N1 118.3(17) . . ?
C2 C3 H3A 107.7 . . ?
C2 C3 H3B 107.7 . . ?
H3A C3 H3B 107.1 . . ?
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 107.4 . . ?
N2 C6 H6B 107.4 . . ?
H6A C6 H6B 106.9 . . ?
C5 C6 N2 120(2) . . ?
C5 C6 H6A 107.4 . . ?
C5 C6 H6B 107.4 . . ?
C4 C5 H5A 106.9 . . ?
C4 C5 H5B 106.9 . . ?
C6 C5 C4 122(2) . . ?
C6 C5 H5A 106.9 . . ?
C6 C5 H5B 106.9 . . ?
H5A C5 H5B 106.7 . . ?
I1 Sb1 I1 180.0 . 5_666 ?
I2 Sb1 I1 90.0 . . ?
I2 Sb1 I1 90.0 5_666 5_666 ?
I2 Sb1 I1 90.0 . 5_666 ?
I2 Sb1 I1 90.0 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 91.595(15) . 5_666 ?
I3 Sb1 I2 88.404(15) . . ?
I3 Sb1 I2 91.596(14) 5_666 . ?
I3 Sb1 I2 88.404(14) 5_666 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 3.0548(5) 5_666 ?
Bi1 I1 3.0548(5) . ?
Bi1 I2 3.0481(4) 5_666 ?
Bi1 I2 3.0481(4) . ?
Bi1 I3 3.0442(5) 5_666 ?
Bi1 I3 3.0442(5) . ?
I1 Sb1 3.0548(5) . ?
I2 Sb1 3.0481(4) . ?
I3 Sb1 3.0442(5) . ?
I5 I4 2.9376(9) . ?
I5 I4 2.9376(9) 5_567 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C3 1.442(17) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C1 C2 1.446(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.428(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C5 1.453(19) . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C6 1.441(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.433(17) . ?
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
C1 C2 C3 N1 -172(3) . . . . ?
N2 C6 C5 C4 168(4) . . . . ?
