#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:40:19 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289452 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/78/7247807.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_7247807
loop_
_publ_author_name
'Pradhan, Abinash'
'Sahoo, Sanand'
'Samal, Saroj L.'
_publ_section_title
;
 (C2H5NH3)2BiCl5−xBrx perovskites containing 1D chains: effect of
 Br substitution on their structural and optical properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              312
_journal_page_last               323
_journal_paper_doi               10.1039/D3CE01019H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'Bi Br1.188 Cl3.812, C4 H16 N2'
_chemical_formula_sum            'C4 H16 Bi Br1.18 Cl3.82 N2'
_chemical_formula_weight         531.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2023-10-09 deposited with the CCDC.	2023-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.6366(2)
_cell_length_b                   22.1176(8)
_cell_length_c                   17.8909(5)
_cell_measurement_reflns_used    4550
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0120
_cell_measurement_theta_min      1.8340
_cell_volume                     3021.83(16)
_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 1.000
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     14.00  39.00   0.50  163.05    --   10.00  47.00  25.00   50
  2  ω    -42.00 -17.00   0.50  163.05    --   10.00 -47.00-124.00   50
  3  ω      5.00  30.00   0.50  163.05    --  -10.20  47.00  25.00   50
  4  ω    -63.00 -38.00   0.50  163.05    --  -10.20 -47.00-124.00   50
  5  ω     41.00  67.00   0.50  163.05    --   10.00  77.00  90.00   52
  6  ω    -11.00  15.00   0.50  163.05    --   10.00  77.00-180.00   52
  7  ω     48.00  99.00   0.50  163.05    --   10.00  77.00-180.00  102
  8  ω    -63.00  47.00   0.50  163.05    --   10.00 -38.00  60.00  220
  9  ω     39.00  70.00   0.50  163.05    --   10.00  77.00-120.00   62
 10  ω    -11.00  23.50   0.50  163.05    --   10.00  77.00  90.00   69
;
_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      -0.0349614000
_diffrn_orient_matrix_UB_12      -0.0295378000
_diffrn_orient_matrix_UB_13      -0.0040745000
_diffrn_orient_matrix_UB_21      0.0417812000
_diffrn_orient_matrix_UB_22      -0.0027058000
_diffrn_orient_matrix_UB_23      -0.0352577000
_diffrn_orient_matrix_UB_31      0.0752308000
_diffrn_orient_matrix_UB_32      -0.0121907000
_diffrn_orient_matrix_UB_33      0.0176646000
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9731
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.031
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18276
_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    2.335
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             1946
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1719
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0351
_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)+(0.0379P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1241
_reflns_number_total             1719
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce01019h2.cif
_cod_data_source_block           ab259d_070222
_cod_depositor_comments
'Adding full bibliography for 7247803--7247812.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7247807
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         (C2H5NH3)2BiCl4Br
_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 99.72
_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
{Cl4, Br4}
{Cl2, Br2}
{Cl1, Br1}
{Cl3, Br3}
3. Uiso/Uaniso restraints and constraints
N1 \\sim C2 \\sim C1: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
Uanis(Cl4) = Uanis(Br4)
Uanis(Cl2) = Uanis(Br2)
Uanis(Cl1) = Uanis(Br1)
Uanis(Cl3) = Uanis(Br3)
4. Rigid body (RIGU) restrains
 N1, C2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(Br4)=0.5*(1-FVAR(2))
 Sof(Cl4)=0.5*FVAR(2)
 Sof(Br2)=0.5*(1-FVAR(3))
 Sof(Cl2)=0.5*FVAR(3)
 Sof(Br1)=1-FVAR(3)
 Sof(Cl1)=FVAR(3)
 Sof(Br3)=0.5*(1-FVAR(5))
 Sof(Cl3)=0.5*FVAR(5)
 Fixed Sof: H2B(0.5) H2C(0.5) H3B(0.5) H3C(0.5) H4A(0.5) H4B(0.5) N1(0.5)
 H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2D(0.5) H2E(0.5) C1(0.5) H1D(0.5) H1E(0.5)
 H1F(0.5)
6.a Free rotating group:
 N1(C2,C1)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2D,H2E)
6.c Me refined with riding coordinates:
 N2(H2A,H2B,H2C), C3(H3A,H3B,H3C), N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_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 3.998
_oxdiff_exptl_absorpt_empirical_full_min 0.533
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-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 0.36490(2) 0.36705(2) 0.04816(15) Uani 1 2 d S T P . .
Cl1 Cl 0.75219(17) 0.37930(7) 0.46605(8) 0.0935(7) Uani 0.737(5) 1 d . . P A 7
Cl3 Cl 0.500000 0.48735(9) 0.33546(12) 0.1048(11) Uani 0.693(7) 2 d S T P A 9
Cl2 Cl 0.500000 0.24474(9) 0.40033(14) 0.0962(11) Uani 0.756(8) 2 d S T P A 5
Cl4 Cl 0.250000 0.34758(15) 0.250000 0.1279(17) Uani 0.890(8) 2 d S T P A 3
N2 N 0.500000 0.4680(4) 0.1500(4) 0.087(3) Uani 1 2 d S T P . .
H2A H 0.500000 0.438274 0.116414 0.105 Uiso 0.5 1 calc R U P B -1
H2B H 0.595158 0.465106 0.178454 0.105 Uiso 0.5 1 calc R U P B -1
H2C H 0.404842 0.465106 0.178454 0.105 Uiso 0.5 1 calc R U P B -1
C3 C 0.500000 0.5774(6) 0.1506(7) 0.186(9) Uani 1 2 d S T P . .
H3A H 0.500000 0.610988 0.116656 0.280 Uiso 0.5 1 calc R U P C -1
H3B H 0.397358 0.579144 0.181530 0.280 Uiso 0.5 1 calc R U P C -1
H3C H 0.602642 0.579144 0.181530 0.280 Uiso 0.5 1 calc R U P C -1
C4 C 0.500000 0.5257(7) 0.1118(8) 0.149(7) Uani 1 2 d S T P . .
H4A H 0.601992 0.526385 0.079526 0.179 Uiso 0.5 1 calc R U P . .
H4B H 0.398008 0.526385 0.079526 0.179 Uiso 0.5 1 calc R U P . .
Br4 Br 0.250000 0.34758(15) 0.250000 0.1279(17) Uani 0.110(8) 2 d S T P A 4
Br2 Br 0.500000 0.24474(9) 0.40033(14) 0.0962(11) Uani 0.244(8) 2 d S T P A 6
Br1 Br 0.75219(17) 0.37930(7) 0.46605(8) 0.0935(7) Uani 0.263(5) 1 d . . P A 8
Br3 Br 0.500000 0.48735(9) 0.33546(12) 0.1048(11) Uani 0.307(7) 2 d S T P A 10
N1 N 0.4587(16) 0.2443(7) 0.5900(7) 0.123(6) Uani 0.5 1 d G U P D -1
H1A H 0.522760 0.228036 0.553638 0.148 Uiso 0.5 1 calc R U P D -1
H1B H 0.439447 0.216709 0.625321 0.148 Uiso 0.5 1 calc R U P D -1
H1C H 0.356782 0.256773 0.571461 0.148 Uiso 0.5 1 calc R U P D -1
C2 C 0.5568(15) 0.2981(8) 0.6238(7) 0.149(8) Uani 0.5 1 d G U P D -1
H2D H 0.668633 0.284651 0.643401 0.178 Uiso 0.5 1 calc R U P D -1
H2E H 0.579316 0.327939 0.585208 0.178 Uiso 0.5 1 calc R U P D -1
C1 C 0.4504(18) 0.3268(7) 0.6862(7) 0.127(7) Uani 0.5 1 d G U P D -1
H1D H 0.513812 0.360413 0.706634 0.191 Uiso 0.5 1 calc R U P D -1
H1E H 0.340429 0.340657 0.666579 0.191 Uiso 0.5 1 calc R U P D -1
H1F H 0.429596 0.297442 0.724675 0.191 Uiso 0.5 1 calc R U P D -1
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
Cl1 Bi1 Cl1 93.89(7) 12_655 . ?
Bi1 Cl4 Bi1 164.60(13) 14_456 . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C4 N2 H2A 109.5 . . ?
C4 N2 H2B 109.5 . . ?
C4 N2 H2C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
N2 C4 H4A 107.2 . . ?
N2 C4 H4B 107.2 . . ?
C3 C4 N2 120.6(12) . . ?
C3 C4 H4A 107.2 . . ?
C3 C4 H4B 107.2 . . ?
H4A C4 H4B 106.8 . . ?
Bi1 Br4 Bi1 164.60(13) 14_456 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
N1 C2 H2D 109.5 . . ?
N1 C2 H2E 109.5 . . ?
H2D C2 H2E 108.1 . . ?
C1 C2 N1 110.6 . . ?
C1 C2 H2D 109.5 . . ?
C1 C2 H2E 109.5 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
C2 C1 H1F 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 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
Bi1 Cl1 2.6358(12) 12_655 ?
Bi1 Cl1 2.6358(12) . ?
Bi1 Cl3 2.767(2) . ?
Bi1 Cl2 2.723(2) . ?
Bi1 Cl4 2.8596(5) 14_556 ?
Bi1 Cl4 2.8596(5) . ?
Bi1 Br4 2.8596(5) . ?
Bi1 Br2 2.723(2) . ?
Bi1 Br1 2.6358(12) . ?
Bi1 Br3 2.767(2) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C4 1.447(15) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C4 1.338(18) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.5320 . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C2 C1 1.5189 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
