#------------------------------------------------------------------------------
#$Date: 2024-09-06 03:37:40 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294537 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716698.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_7716698
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             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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      5.00  31.00   0.50    7.69    --   10.00  54.00  73.00   52
  2  ω    -43.00 -18.00   0.50    7.69    --   10.00 -54.00 -70.00   50
  3  ω    -39.00  -9.00   0.50    7.69    --  -10.20 -54.00 -70.00   60
  4  ω    -43.00  70.00   0.50    7.69    --  -10.20  54.00  73.00  226
  5  ω     33.00  73.00   0.50    7.69    --   10.00  77.00 150.00   80
  6  ω    -54.00 -28.00   0.50    7.69    --   10.00 -82.00-150.00   52
  7  ω    -10.00  15.00   0.50    7.69    --   10.00 -82.00-150.00   50
  8  ω    -11.00  97.00   0.50    7.69    --   10.00  77.00 120.00  216
  9  ω    -56.00 -31.00   0.50    7.69    --   10.00 -57.00 120.00   50
 10  ω     15.00  40.00   0.50    7.69    --   10.00 -57.00 120.00   50
 11  ω    -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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0046P)²+2.9983P] where P=(Fo²+2Fc²)/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 > 2σ(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_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.
;
_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
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 0.03067(16) Uani 1 4 d S T P . .
I1 I 0.500000 0.24864(5) 0.500000 0.03707(18) Uani 1 2 d S T P . .
I2 I 0.25813(5) 0.500000 0.54434(5) 0.03564(18) Uani 1 2 d S T P . .
I3 I 0.39354(5) 0.500000 0.25524(5) 0.0432(2) Uani 1 2 d S T P . .
I4 I -0.01364(8) 0.500000 0.22988(7) 0.0942(3) Uani 1 2 d S T P . .
I5 I 0.000000 0.500000 0.000000 0.0689(3) Uani 1 4 d S T P . .
N1 N 0.2945(5) 0.2166(5) 0.6771(4) 0.0522(15) Uani 1 1 d D U . . .
H1AA H 0.343175 0.187496 0.640905 0.063 Uiso 0.530(13) 1 calc R U P A 1
H1AB H 0.247601 0.165123 0.691264 0.063 Uiso 0.530(13) 1 calc R U P A 1
H1AC H 0.254270 0.268709 0.636915 0.063 Uiso 0.530(13) 1 calc R U P A 1
H1BD H 0.239465 0.171263 0.645347 0.063 Uiso 0.470(13) 1 calc R U P A 2
H1BE H 0.293184 0.276035 0.636252 0.063 Uiso 0.470(13) 1 calc R U P A 2
H1BF H 0.361777 0.183704 0.684375 0.063 Uiso 0.470(13) 1 calc R U P A 2
C1 C 0.318(3) 0.361(3) 0.9446(18) 0.115(12) Uani 0.530(13) 1 d D U P A 1
H1A H 0.255999 0.388835 0.973264 0.173 Uiso 0.530(13) 1 calc R U P A 1
H1B H 0.359053 0.307455 0.993258 0.173 Uiso 0.530(13) 1 calc R U P A 1
H1C H 0.368735 0.420080 0.937056 0.173 Uiso 0.530(13) 1 calc R U P A 1
C2 C 0.2739(15) 0.3115(15) 0.8378(14) 0.078(5) Uani 0.530(13) 1 d D U P A 1
H2A H 0.230684 0.366527 0.790938 0.094 Uiso 0.530(13) 1 calc R U P A 1
H2B H 0.221037 0.254309 0.846937 0.094 Uiso 0.530(13) 1 calc R U P A 1
C3 C 0.3587(11) 0.2640(12) 0.7805(10) 0.056(4) Uani 0.530(13) 1 d D U P A 1
H3A H 0.410285 0.320207 0.766061 0.067 Uiso 0.530(13) 1 calc R U P A 1
H3B H 0.403060 0.207988 0.824940 0.067 Uiso 0.530(13) 1 calc R U P A 1
C4 C 0.367(3) 0.343(3) 0.9659(15) 0.072(8) Uani 0.470(13) 1 d D U P A 2
H4A H 0.427160 0.393187 0.995150 0.108 Uiso 0.470(13) 1 calc R U P A 2
H4B H 0.295477 0.372437 0.974287 0.108 Uiso 0.470(13) 1 calc R U P A 2
H4C H 0.380761 0.274808 1.004073 0.108 Uiso 0.470(13) 1 calc R U P A 2
C6 C 0.2757(15) 0.2492(15) 0.7902(12) 0.062(5) Uani 0.470(13) 1 d D U P A 2
H6A H 0.201495 0.283394 0.781582 0.074 Uiso 0.470(13) 1 calc R U P A 2
H6B H 0.275444 0.183854 0.833463 0.074 Uiso 0.470(13) 1 calc R U P A 2
C5 C 0.3637(16) 0.3250(15) 0.8494(12) 0.063(5) Uani 0.470(13) 1 d D U P A 2
H5A H 0.437740 0.297884 0.842692 0.076 Uiso 0.470(13) 1 calc R U P A 2
H5B H 0.352764 0.395160 0.813013 0.076 Uiso 0.470(13) 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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
11 -13 -1 0.0654
12 -12 -4 0.0687
-1 -2 18 0.0595
-11 12 9 0.1156
-12 -12 1 0.0721
12 12 -1 0.0469
-12 13 4 0.1298
1 2 -17 0.0423
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 . . ?
I3 Bi1 I1 90.0 5_666 5_666 ?
I3 Bi1 I1 90.0 . 5_666 ?
I3 Bi1 I1 90.0 5_666 . ?
I3 Bi1 I2 91.273(16) 5_666 . ?
I3 Bi1 I2 88.727(16) 5_666 5_666 ?
I3 Bi1 I2 91.272(16) . 5_666 ?
I3 Bi1 I2 88.727(16) . . ?
I3 Bi1 I3 180.0 5_666 . ?
I4 I5 I4 180.0 . 5_565 ?
H1AA N1 H1AB 109.5 . . ?
H1AA N1 H1AC 109.5 . . ?
H1AB N1 H1AC 109.5 . . ?
H1BD N1 H1BE 109.5 . . ?
H1BD N1 H1BF 109.5 . . ?
H1BE N1 H1BF 109.5 . . ?
C3 N1 H1AA 109.5 . . ?
C3 N1 H1AB 109.5 . . ?
C3 N1 H1AC 109.5 . . ?
C6 N1 H1BD 109.5 . . ?
C6 N1 H1BE 109.5 . . ?
C6 N1 H1BF 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 108.0 . . ?
C1 C2 H2B 108.0 . . ?
C1 C2 C3 117.2(17) . . ?
H2A C2 H2B 107.3 . . ?
C3 C2 H2A 108.0 . . ?
C3 C2 H2B 108.0 . . ?
N1 C3 C2 107.4(11) . . ?
N1 C3 H3A 110.2 . . ?
N1 C3 H3B 110.2 . . ?
C2 C3 H3A 110.2 . . ?
C2 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
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 . . ?
N1 C6 H6A 108.9 . . ?
N1 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C5 C6 N1 113.3(11) . . ?
C5 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C4 C5 C6 117.2(18) . . ?
C4 C5 H5A 108.0 . . ?
C4 C5 H5B 108.0 . . ?
C6 C5 H5A 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
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 3.0821(6) . ?
Bi1 I1 3.0821(6) 5_666 ?
Bi1 I2 3.0761(5) 5_666 ?
Bi1 I2 3.0761(5) . ?
Bi1 I3 3.0718(6) 5_666 ?
Bi1 I3 3.0718(6) . ?
I4 I5 2.9358(8) . ?
N1 H1AA 0.8900 . ?
N1 H1AB 0.8900 . ?
N1 H1AC 0.8900 . ?
N1 H1BD 0.8900 . ?
N1 H1BE 0.8900 . ?
N1 H1BF 0.8900 . ?
N1 C3 1.482(12) . ?
N1 C6 1.543(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.468(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.489(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C5 1.477(17) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.482(16) . ?
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 C6 C5 C4 -167.7(19) . . . . ?
C1 C2 C3 N1 179(2) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
10.7591 -13.3146 -1.3855 0.0280 0.1358 -0.9903
12.1229 -12.0311 -3.8689 -0.0898 0.0182 -0.9958
-1.4141 -1.6002 17.5151 0.1920 0.9796 0.0598
-10.7325 11.8535 8.6615 0.0550 0.2835 0.9574
-12.3468 -11.6391 0.5888 0.9802 -0.1921 -0.0481
12.2575 11.7350 -0.5592 -0.9798 0.1921 0.0557
-11.5782 12.5655 3.8605 0.0459 -0.0088 0.9989
1.2366 1.8138 -17.4677 -0.1921 -0.9804 -0.0436
