Band gap modulation of organic–inorganic Sb(iii) halide by molecular design
Wang, Yan-Ning; Tong, Liang; Min-Wan,; Liu, Jing-Yuan; Ye, Si-Yu; Mensah, Abraham; Li, Jun-Yi; Chen, Li-Zhuang; CrystEngComm  (2022) –; doi:10.1039/D1CE01615F

data_7244276
_publ_section_title
;
 Band gap modulation of organic--inorganic Sb(iii) halide by molecular
 design
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01615F
_journal_year                    2022
_chemical_formula_moiety         'Cl4 Sb, Cl3 Sb, 3(C10 H15 F N), 2(Cl)'
_chemical_formula_sum            'C30 H45 Cl9 F3 N3 Sb2'
_chemical_formula_weight         1067.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-25 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                83.423(5)
_cell_angle_beta                 89.796(6)
_cell_angle_gamma                76.621(5)
_cell_formula_units_Z            2
_cell_length_a                   9.275(2)
_cell_length_b                   13.826(3)
_cell_length_c                   18.274(4)
_cell_measurement_reflns_used    4558
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.43
_cell_measurement_theta_min      2.50
_cell_volume                     2264.1(9)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16879
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.8299
_exptl_absorpt_correction_T_min  0.8035
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: HCl'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.544
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         9192
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1772P)^2^+17.5220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2772
_refine_ls_wR_factor_ref         0.3029
_reflns_number_gt                6739
_reflns_number_total             9192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1ce01615f2.cif
_cod_data_source_block           1
_cod_database_code               7244276
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.12
3. Uiso/Uaniso restraints and constraints
Uanis(N17) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.006 and sigma for terminal
atoms of 0.012
4.a Secondary CH2 refined with riding coordinates:
 C77(H77A,H77B), C15(H15A,H15B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C48(H48), C54(H54), C64(H64), C12(H12), C31(H31), C44(H44), C79(H79),
 C20(H20), C28(H28), C30(H30), C36(H36), C2(H2)
4.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C11(H11A,H11B,H11C), C27(H27A,H27B,
 H27C), C33(H33A,H33B,H33C), C26(H26A,H26B,H26C), C49(H49A,H49B,H49C), C1(H1A,
 H1B,H1C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'