(C2H5NH3)2BiCl5−xBrx perovskites containing 1D chains: effect of Br substitution on their structural and optical properties
Pradhan, Abinash; Sahoo, Sanand; Samal, Saroj L.; CrystEngComm 26 (2024) 312–323; doi:10.1039/D3CE01019H

data_7247804
_publ_section_title
;
 (C2H5NH3)2BiCl5&#x2212;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 Br2.259 Cl2.741, C4 H16 N2'
_chemical_formula_sum            'C4 H16 Bi Br2.27 Cl2.73 N2'
_chemical_formula_weight         579.23
_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                   7.6954(2)
_cell_length_b                   22.2151(8)
_cell_length_c                   17.9473(5)
_cell_measurement_reflns_used    3515
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.8430
_cell_measurement_theta_min      1.8230
_cell_volume                     3068.16(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 0.954
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -77.00 -51.00   0.50  171.53    --   10.00 -80.00 126.00   52
  2  \w     11.00  37.00   0.50  171.53    --   10.00  46.00  52.00   52
  3  \w    -21.00  16.00   0.50  171.53    --   10.00 -80.00 126.00   74
  4  \w    -17.00  28.00   0.50  171.53    --   10.00 -77.00-180.00   90
  5  \w    -13.00  99.00   0.50  171.53    --   10.00  77.00  60.00  224
  6  \w    -70.00 -33.00   0.50  171.53    --   10.00 -77.00-180.00   74
  7  \w    -38.00   6.00   0.50  171.53    --  -10.20 -77.00  90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0780942000
_diffrn_orient_matrix_UB_12      -0.0003674000
_diffrn_orient_matrix_UB_13      0.0209859000
_diffrn_orient_matrix_UB_21      0.0117863000
_diffrn_orient_matrix_UB_22      -0.0308669000
_diffrn_orient_matrix_UB_23      -0.0088542000
_diffrn_orient_matrix_UB_31      0.0475395000
_diffrn_orient_matrix_UB_32      0.0082163000
_diffrn_orient_matrix_UB_33      -0.0322703000
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8465
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.075
_diffrn_reflns_theta_min         1.833
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    17.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38775
_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    2.508
_exptl_crystal_description       crystalline
_exptl_crystal_F_000             2103
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1737
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0796
_refine_ls_R_factor_gt           0.0438
_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/[\s^2^(Fo^2^)+(0.0462P)^2^+1.2022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1193
_reflns_number_total             1737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01019h2.cif
_cod_data_source_block           ab256f
_cod_depositor_comments
'Adding full bibliography for 7247803--7247812.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7247804
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         (C2H5NH3)2BiCl3Br2
_reflns_odcompleteness_completeness 99.67
_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, {H2A,H2B,H2C} of N2, {H1A,H1B,H1C} of C1
 At 1.5 times of:
  {H1D,H1E,H1F} of N1, {H3A,H3B,H3C} of C3
2. Shared sites
{Cl1, Br1}
{Cl3, Br3}
{Cl4, Br4}
{Cl2, Br2}
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
Uanis(Cl1) = Uanis(Br1)
Uanis(Cl3) = Uanis(Br3)
Uanis(Cl4) = Uanis(Br4)
Uanis(Cl2) = Uanis(Br2)
4. Rigid body (RIGU) restrains
 N1, C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(Br3)=0.5*(1-FVAR(3))
 Sof(Cl3)=0.5*FVAR(3)
 Sof(Br4)=0.5*(1-FVAR(4))
 Sof(Cl4)=0.5*FVAR(4)
 Sof(Br2)=0.5*(1-FVAR(5))
 Sof(Cl2)=0.5*FVAR(5)
 Fixed Sof: H2B(0.5) H2C(0.5) H4A(0.5) H4B(0.5) H3B(0.5) H3C(0.5) C1(0.5)
 H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2D(0.5) H2E(0.5) N1(0.5) H1D(0.5) H1E(0.5)
 H1F(0.5)
6.a Free rotating group:
 C1(C2,N1)
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), C1(H1A,H1B,H1C), N1(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 2.793
_oxdiff_exptl_absorpt_empirical_full_min 0.476