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_7134533
_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         'I5 Sb, C7 H16 N2'
_chemical_formula_sum            'C7 H16 I5 N2 Sb'
_chemical_formula_weight         884.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 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                   14.8591(5)
_cell_length_b                   13.0389(4)
_cell_length_c                   9.1663(2)
_cell_measurement_reflns_used    9004
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.288
_cell_measurement_theta_min      2.741
_cell_volume                     1775.94(9)
_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      298.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            40103
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.300
_diffrn_reflns_theta_min         2.078
_exptl_absorpt_coefficient_mu    10.226
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1790
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1536 before and 0.0790 after correction. The Ratio of minimum to maximum transmission is 0.2400. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    3.308
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.869
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(12)
_refine_ls_extinction_coef       0.00064(15)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         4291
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0518P)^2^+8.7370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.841
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                4140
_reflns_number_total             4291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01861g2.cif
_cod_data_source_block           t
_cod_depositor_comments
'Adding full bibliography for 7134531--7134536.cif.'
_cod_database_code               7134533
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.56(12)
 0.44(12)
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
 C5-C4 \\sim C7-C6 \\sim C6-C3 \\sim C3-C2 \\sim C2-C1
 with sigma of 0.001
4.a Ternary CH refined with riding coordinates:
 N1(H1), C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), N2(H2c,H2d), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 C7(H7a,H7b)
;
_shelx_res_checksum              24557
_shelx_hkl_checksum              59804
_olex2_submission_special_instructions 'No special instructions were received'