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_7134534
_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         'Cl10 Sb2, 2(C7 N2)'
_chemical_formula_sum            'C14 Cl10 N4 Sb2'
_chemical_formula_weight         822.20
_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                   13.9507(9)
_cell_length_b                   8.5795(5)
_cell_length_c                   11.9950(7)
_cell_measurement_reflns_used    4901
_cell_measurement_temperature    468.00(10)
_cell_measurement_theta_max      30.4140
_cell_measurement_theta_min      3.2480
_cell_volume                     1435.68(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.111a 64-bit (release 27-02-2024))'
_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      468.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.811
_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    -12.00  38.00   0.50    0.47    --    5.26 -99.00 -60.00  100
  2  \w    -10.00  15.00   0.50    0.47    --   -4.99 -99.00 -60.00   50
  3  \w     -5.00  21.00   0.50    0.47    --   -4.99 -99.00-120.00   52
  4  \w    -17.00   8.00   0.50    0.47    --   -4.99 -99.00-180.00   50
  5  \w    -57.00  11.00   0.50    0.47    --    5.26 -38.00-141.00  136
;
_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      0.0369565000
_diffrn_orient_matrix_UB_12      -0.0386780000
_diffrn_orient_matrix_UB_13      -0.0174453000
_diffrn_orient_matrix_UB_21      0.0340767000
_diffrn_orient_matrix_UB_22      0.0359834000
_diffrn_orient_matrix_UB_23      0.0351324000
_diffrn_orient_matrix_UB_31      -0.0075917000
_diffrn_orient_matrix_UB_32      -0.0266148000
_diffrn_orient_matrix_UB_33      0.0727485000
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9261
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.900
_diffrn_reflns_theta_min         2.919
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.822
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33431
_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    1.967
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0034(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1954
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0967P)^2^+0.6612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1634
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1411
_reflns_number_total             1954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01861g2.cif
_cod_data_source_block           wy-2-468k_auto
_cod_depositor_comments
'Adding full bibliography for 7134531--7134536.cif.'
_cod_database_code               7134534
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Sb Cl'
_olex2_refinement_description
;
1. Shared sites
{N1, C5}
{C3, N3}
2. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim C2 \\sim C3 \\sim N3 \\sim C5 \\sim C4: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) = Uanis(C5)
Uanis(C3) = Uanis(N3)
3. Others
 Fixed Sof: N1(0.5) C3(0.5) C5(0.5) N3(0.5)
;
_shelx_res_checksum              52955
_shelx_hkl_checksum              57069
_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 2.094
_oxdiff_exptl_absorpt_empirical_full_min 0.675