Three antimony-based organic–inorganic hybrid perovskites (1,4-3.2.2-H2dabcn)SbX5 (X = Cl, Br, I) show progressively decreasing phase transition temperatures and bandgaps
Wei, Ying; Zhou, Jie; Zhou, Lin; Wei, Zhenhong; Chemical Communications 61 (2025) 8600–8603; doi:10.1039/D5CC01861G

data_7134532
_publ_section_title
;
 Three antimony-based organic--inorganic hybrid perovskites
 (1,4-3.2.2-H2dabcn)SbX5 (X = Cl, Br, I) show progressively decreasing
 phase transition temperatures and bandgaps
;
_journal_issue                   47
_journal_name_full               'Chemical Communications'
_journal_page_first              8600
_journal_page_last               8603
_journal_paper_doi               10.1039/D5CC01861G
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'Br10 Sb2, 2(C7 N2)'
_chemical_formula_sum            'C14 Br10 N4 Sb2'
_chemical_formula_weight         1266.70
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-03-27 deposited with the CCDC.	2025-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1887(13)
_cell_length_b                   8.8334(7)
_cell_length_c                   12.4471(10)
_cell_measurement_reflns_used    3517
_cell_measurement_temperature    420.02(10)
_cell_measurement_theta_max      29.4770
_cell_measurement_theta_min      3.1870
_cell_volume                     1560.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      420.02(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.767
_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    -22.00  21.00   0.50    3.12    --   -4.99   9.00 104.00   86
  2  \w     14.00  69.00   0.50    3.12    --   -4.99   9.00 104.00  110
  3  \w    -60.00 -16.00   0.50    3.12    --    5.26  -9.00 -69.00   88
  4  \w    -16.00  27.00   0.50    3.12    --   -4.99 -99.00-120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0235773000
_diffrn_orient_matrix_UB_12      -0.0086310000
_diffrn_orient_matrix_UB_13      -0.0498475000
_diffrn_orient_matrix_UB_21      -0.0438879000
_diffrn_orient_matrix_UB_22      -0.0020054000
_diffrn_orient_matrix_UB_23      0.0272394000
_diffrn_orient_matrix_UB_31      -0.0036612000
_diffrn_orient_matrix_UB_32      0.0798402000
_diffrn_orient_matrix_UB_33      -0.0047745000
_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  0.1196
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9727
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.767
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.989
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.111a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.757
_exptl_crystal_description       Block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.341
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         2019
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0588
_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/[\s^2^(Fo^2^)+(0.0669P)^2^+7.5289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1456
_reflns_number_total             2019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01861g2.cif
_cod_data_source_block           wy-1-420k_auto
_cod_depositor_comments
'Adding full bibliography for 7134531--7134536.cif.'
_cod_database_code               7134532
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Sb Br'
_olex2_refinement_description
;
1. Shared sites
{N1, C5}
{C2, N2}
2. Uiso/Uaniso restraints and constraints
N1 \\sim C4 \\sim C2 \\sim C3 \\sim C1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2A
Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.01
Uanis(N1) = Uanis(C5)
Uanis(C2) = Uanis(N2)
3. Rigid body (RIGU) restrains
 N1, C4, C2, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: N1(0.5) C2(0.5) C5(0.5) N2(0.5)
;
_shelx_res_checksum              40984
_shelx_hkl_checksum              17487
_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 6.695
_oxdiff_exptl_absorpt_empirical_full_min 0.262