#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:37:40 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716690.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_7716690
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         '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             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                 101.706(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0472(4)
_cell_length_b                   12.4245(5)
_cell_length_c                   12.7142(5)
_cell_measurement_reflns_used    4327
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3160
_cell_measurement_theta_min      2.3720
_cell_volume                     1863.49(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 0.997
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00 -51.00   0.50   33.93    --   10.00 -51.00  19.00   52
  2  ω    -19.00  28.00   0.50   33.93    --   10.00 -51.00  19.00   94
  3  ω     38.00  63.00   0.50   33.93    --   10.00  51.00 165.00   50
  4  ω    -40.00  51.00   0.50   33.93    --  -10.20  51.00 165.00  182
  5  ω    -64.00  47.00   0.50   33.93    --   10.00 -38.00 -60.00  222
  6  ω    -76.00 -41.00   0.50   33.93    --   10.00 -57.00-120.00   70
  7  ω    -35.00  21.00   0.50   33.93    --   10.00 -57.00-120.00  112
  8  ω    -79.00 -31.00   0.50   33.93    --   10.00 -77.00 -60.00   96
  9  ω    -16.00  21.00   0.50   33.93    --   10.00 -77.00 -60.00   74
 10  ω    -39.00 -14.00   0.50   33.93    --  -10.20 -51.00  19.00   50
;
_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      0.0493317000
_diffrn_orient_matrix_UB_12      0.0009463000
_diffrn_orient_matrix_UB_13      0.0413493000
_diffrn_orient_matrix_UB_21      0.0273783000
_diffrn_orient_matrix_UB_22      -0.0356782000
_diffrn_orient_matrix_UB_23      -0.0301544000
_diffrn_orient_matrix_UB_31      0.0207968000
_diffrn_orient_matrix_UB_32      0.0445458000
_diffrn_orient_matrix_UB_33      -0.0250376000
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8376
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.974
_diffrn_reflns_theta_min         2.683
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36756
_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    2.836
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2013
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0340
_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/[σ²(Fo²)+(0.0284P)²+2.2877P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1601
_reflns_number_total             2013
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01692k2.cif
_cod_data_source_block           ab407_170223
_cod_depositor_comments
'Adding full bibliography for 7716690--7716700.cif.'
_cod_database_code               7716690
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Bi 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 99.15
_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,H,H,H) groups
2. Restrained distances
 C3-C1 \\sim C5-C1
 with sigma of 0.04
 N1-C3 \\sim N2-C5
 with sigma of 0.02
 C3-C2 \\sim C5-C4
 with sigma of 0.02
 C1-C2 \\sim C1-C4
 with sigma of 0.02
 N1-C2 \\sim N2-C4
 with sigma of 0.04
3. 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 C3 \\sim C1 \\sim C2 \\sim N2 \\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
 C1, N1, C3, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C3, C1, C2, N2, 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(0.7) H1A(0.7) H1B(0.7) H1C(0.7) C3(0.7) H3A(0.7) H3B(0.7)
 H1AA(0.7) H1AB(0.7) H1AC(0.7) H1BD(0.3) H1BE(0.3) H1BF(0.3) C2(0.7) H3C(0.7)
 H3D(0.7) N2(0.3) H2A(0.3) H2B(0.3) H2C(0.3) C5(0.3) H5A(0.3) H5B(0.3) C4(0.3)
 H5C(0.3) H5D(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H3C,H3D), C5(H5A,H5B), C4(H5C,H5D)
6.b Me refined with riding coordinates:
 N1(H1A,H1B,H1C), C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF), N2(H2A,H2B,H2C)
;
_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 2.804
_oxdiff_exptl_absorpt_empirical_full_min 0.355
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 0.05283(17) Uani 1 4 d S T P . .
I1 I 0.500000 0.25158(4) 0.500000 0.0659(2) Uani 1 2 d S T P . .
I2 I 0.25603(4) 0.500000 0.53907(5) 0.0643(2) Uani 1 2 d S T P . .
I3 I 0.40002(6) 0.500000 0.25703(5) 0.0739(2) Uani 1 2 d S T P . .
I5 I 0.000000 0.500000 0.000000 0.0987(4) Uani 1 4 d S T P . .
I4 I -0.01103(9) 0.500000 0.22877(9) 0.1278(4) Uani 1 2 d S T P . .
N1 N 0.2997(16) 0.2201(16) 0.6722(12) 0.084(4) Uani 0.7 1 d D U P A 1
H1A H 0.307609 0.148959 0.677140 0.100 Uiso 0.7 1 calc R U P A 1
H1B H 0.227814 0.236183 0.643906 0.100 Uiso 0.7 1 calc R U P A 1
H1C H 0.344288 0.246072 0.630315 0.100 Uiso 0.7 1 calc R U P A 1
C3 C 0.331(2) 0.2675(18) 0.7783(14) 0.176(8) Uani 0.7 1 d D U P A 1
H3A H 0.281913 0.220555 0.809180 0.211 Uiso 0.7 1 calc R U P A 1
H3B H 0.403660 0.230892 0.794975 0.211 Uiso 0.7 1 calc R U P A 1
C1 C 0.3420(14) 0.3534(11) 0.9476(11) 0.195(6) Uani 1 1 d D U . . .
H1AA H 0.390997 0.414605 0.964985 0.293 Uiso 0.7 1 calc R U P B 1
H1AB H 0.265417 0.374072 0.948458 0.293 Uiso 0.7 1 calc R U P B 1
H1AC H 0.365363 0.297589 0.999575 0.293 Uiso 0.7 1 calc R U P B 1
H1BD H 0.298055 0.391489 0.990678 0.293 Uiso 0.3 1 calc R U P C 2
H1BE H 0.384136 0.297088 0.989508 0.293 Uiso 0.3 1 calc R U P C 2
H1BF H 0.393555 0.402393 0.923960 0.293 Uiso 0.3 1 calc R U P C 2
C2 C 0.348(2) 0.314(2) 0.8423(15) 0.191(8) Uani 0.7 1 d D U P A 1
H3C H 0.333187 0.382564 0.804816 0.229 Uiso 0.7 1 calc R U P A 1
H3D H 0.430340 0.308219 0.854505 0.229 Uiso 0.7 1 calc R U P A 1
N2 N 0.274(3) 0.211(3) 0.693(2) 0.067(7) Uani 0.3 1 d D U P A 2
H2A H 0.210192 0.181958 0.656334 0.081 Uiso 0.3 1 calc R U P A 2
H2B H 0.300808 0.257850 0.651440 0.081 Uiso 0.3 1 calc R U P A 2
H2C H 0.325166 0.158932 0.712797 0.081 Uiso 0.3 1 calc R U P A 2
C5 C 0.252(3) 0.265(4) 0.788(3) 0.130(9) Uani 0.3 1 d D U P A 2
H5A H 0.189145 0.308842 0.750765 0.156 Uiso 0.3 1 calc R U P A 2
H5B H 0.214669 0.205193 0.815057 0.156 Uiso 0.3 1 calc R U P A 2
C4 C 0.267(3) 0.307(5) 0.855(3) 0.167(10) Uani 0.3 1 d D U P A 2
H5C H 0.215757 0.268930 0.891881 0.201 Uiso 0.3 1 calc R U P A 2
H5D H 0.224930 0.371482 0.828046 0.201 Uiso 0.3 1 calc R U P A 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'
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'
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 5_666 ?
I2 Bi1 I1 90.0 . . ?
I2 Bi1 I1 90.0 . 5_666 ?
I2 Bi1 I1 90.0 5_666 . ?
I2 Bi1 I2 180.0 . 5_666 ?
I2 Bi1 I3 88.276(19) 5_666 5_666 ?
I2 Bi1 I3 91.724(19) . 5_666 ?
I2 Bi1 I3 88.277(19) . . ?
I2 Bi1 I3 91.724(19) 5_666 . ?
I3 Bi1 I1 90.0 . 5_666 ?
I3 Bi1 I1 90.0 . . ?
I3 Bi1 I1 90.0 5_666 5_666 ?
I3 Bi1 I1 90.0 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 . . ?
N1 C3 H3A 93.8 . . ?
N1 C3 H3B 93.8 . . ?
H3A C3 H3B 103.1 . . ?
C2 C3 N1 168(3) . . ?
C2 C3 H3A 93.8 . . ?
C2 C3 H3B 93.8 . . ?
H1AA C1 H1AB 109.5 . . ?
H1AA C1 H1AC 109.5 . . ?
H1AB C1 H1AC 109.5 . . ?
H1BD C1 H1BE 109.5 . . ?
H1BD C1 H1BF 109.5 . . ?
H1BE C1 H1BF 109.5 . . ?
C2 C1 H1AA 109.5 . . ?
C2 C1 H1AB 109.5 . . ?
C2 C1 H1AC 109.5 . . ?
C4 C1 H1BD 109.5 . . ?
C4 C1 H1BE 109.5 . . ?
C4 C1 H1BF 109.5 . . ?
C3 C2 C1 157(3) . . ?
C3 C2 H3C 97.1 . . ?
C3 C2 H3D 97.1 . . ?
C1 C2 H3C 97.1 . . ?
C1 C2 H3D 97.1 . . ?
H3C C2 H3D 103.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C5 N2 H2A 109.5 . . ?
C5 N2 H2B 109.5 . . ?
C5 N2 H2C 109.5 . . ?
N2 C5 H5A 96.5 . . ?
N2 C5 H5B 96.5 . . ?
H5A C5 H5B 103.4 . . ?
C4 C5 N2 159(4) . . ?
C4 C5 H5A 96.5 . . ?
C4 C5 H5B 96.5 . . ?
C1 C4 H5C 98.4 . . ?
C1 C4 H5D 98.4 . . ?
C5 C4 C1 153(5) . . ?
C5 C4 H5C 98.4 . . ?
C5 C4 H5D 98.4 . . ?
H5C C4 H5D 103.8 . . ?
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 3.0864(6) 5_666 ?
Bi1 I1 3.0864(6) . ?
Bi1 I2 3.0786(5) 5_666 ?
Bi1 I2 3.0786(5) . ?
Bi1 I3 3.0795(7) . ?
Bi1 I3 3.0796(7) 5_666 ?
I5 I4 2.9384(12) . ?
I5 I4 2.9384(12) 5_565 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C3 1.451(16) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 0.988(16) . ?
C1 H1AA 0.9600 . ?
C1 H1AB 0.9600 . ?
C1 H1AC 0.9600 . ?
C1 H1BD 0.9600 . ?
C1 H1BE 0.9600 . ?
C1 H1BF 0.9600 . ?
C1 C2 1.441(16) . ?
C1 C4 1.46(2) . ?
C2 H3C 0.9700 . ?
C2 H3D 0.9700 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C5 1.46(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 0.98(2) . ?
C4 H5C 0.9700 . ?
C4 H5D 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 125(13) . . . . ?
N2 C5 C4 C1 -16(31) . . . . ?
