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_7134536
_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_absolute_configuration ad
_chemical_formula_moiety         'Cl5 Sb, C7 H16 N2'
_chemical_formula_sum            'C7 H15 Cl5 N2 Sb'
_chemical_formula_weight         426.21
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-03-27
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5619(2)
_cell_length_b                   11.9096(2)
_cell_length_c                   13.6606(4)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.200
_cell_measurement_theta_min      2.930
_cell_volume                     1392.96(6)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 1.000
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38687
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.912
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0926 before and 0.0694 after correction. The Ratio of minimum to maximum transmission is 0.8966. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    2.032
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             828
_refine_diff_density_max         1.849
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3462
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+2.7754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                3291
_reflns_number_total             3462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5cc01861g2.cif
_cod_data_source_block           1746
_cod_depositor_comments
'Adding full bibliography for 7134531--7134536.cif.'
_cod_database_code               7134536
_olex2_refinement_description
;
1. 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
2. Rigid bond restraints
 C00F, N007, C009, C00A, C00C, C008, C00B, C00E, N00G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C00F \\sim N007 \\sim C009 \\sim C00A \\sim C00C \\sim C008 \\sim C00B \\sim
C00E \\sim N00G: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(N00G) \\sim Ueq, Uanis(N007) \\sim Ueq, Uanis(C009) \\sim Ueq,
Uanis(C00A) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(C008) \\sim Ueq,
Uanis(C00B) \\sim Ueq, Uanis(C00E) \\sim Ueq, Uanis(C00F) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 N007(H007), C00F(H00M)
4.b Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B), C009(H00C,H00D), C00A(H00E,H00F), C00B(H00G,H00H), C00C(H00I,
 H00J), C00E(H00K,H00L), N00G(H00N,H00O)
;
_olex2_submission_special_instructions 'No special instructions were received'