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_7134531
_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         'Br5 Sb, C7 H16 N2'
_chemical_formula_sum            'C7 H16 Br5 N2 Sb'
_chemical_formula_weight         649.52
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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            4
_cell_length_a                   8.7842(3)
_cell_length_b                   12.4619(3)
_cell_length_c                   13.8984(5)
_cell_measurement_reflns_used    7916
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.261
_cell_measurement_theta_min      2.837
_cell_volume                     1521.43(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.195
_exptl_absorpt_coefficient_mu    14.920
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1427 before and 0.0856 after correction. The Ratio of minimum to maximum transmission is 0.4879. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    2.836
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.020(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3771
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0257P)^2^+0.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                3354
_reflns_number_total             3771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01861g2.cif
_cod_data_source_block           940
_cod_depositor_comments
'Adding full bibliography for 7134531--7134536.cif.'
_cod_database_code               7134531
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.980(15)
 0.020(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
3. Restrained distances
 C00C-C008 \\sim C00B-C00A \\sim C00F-C00E \\sim C00E-C009 \\sim C00F-C00A
 with sigma of 0.000001
4. Uiso/Uaniso restraints and constraints
Uanis(C009) \\sim Ueq, Uanis(N007) \\sim Ueq, Uanis(C008) \\sim Ueq,
Uanis(C00B) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(C00E) \\sim Ueq,
Uanis(C00A) \\sim Ueq, Uanis(N00D) \\sim Ueq, Uanis(C00F) \\sim Ueq, : with
sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 N007(H007), C00F(H00o)
5.b Secondary CH2 refined with riding coordinates:
 C008(H00a,H00b), C009(H00c,H00d), C00A(H00e,H00f), C00B(H00g,H00h), C00C(H00i,
 H00j), N00D(H00k,H00l), C00E(H00m,H00n)
;
_shelx_res_checksum              60821
_shelx_hkl_checksum              37085
_olex2_submission_special_instructions 'No special instructions were received'