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_7244275
_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         '2(Cl4 Sb), 3(C10 H16 N), Cl'
_chemical_formula_sum            'C30 H48 Cl9 N3 Sb2'
_chemical_formula_weight         1013.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-05-27
_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                90.00
_cell_angle_beta                 92.2610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2809(9)
_cell_length_b                   25.774(3)
_cell_length_c                   17.6172(18)
_cell_measurement_reflns_used    4558
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.43
_cell_measurement_theta_min      2.50
_cell_volume                     4210.9(8)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27639
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.40
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.879
_exptl_absorpt_correction_T_max  0.8200
_exptl_absorpt_correction_T_min  0.7923
_exptl_absorpt_correction_type   multi-scan
_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    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_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         2.010
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8251
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0771P)^2^+19.0794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                7095
_reflns_number_total             8251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1ce01615f2.cif
_cod_data_source_block           rtp
_cod_original_cell_volume        4210.8(7)
_cod_database_code               7244275
_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. Uiso/Uaniso restraints and constraints
N2 \\sim C7AA \\sim C9AA \\sim C3AA \\sim C5: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C2AA(H2AA,H2AB), C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C8AA(H8AA), C6(H6), C7(H7),
 C8(H8), C10(H10), C0AA(H0AA), C1AA(H1AA), C5AA(H5AA), C6AA(H6AA), C4AA(H4AA)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,H22C), C3(H3A,H3B,
 H3C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C3AA(H3AA,H3AB,H3AC), C7AA(H7AA,
 H7AB,H7AC), C9AA(H9AA,H9AB,H9AC)
;
_olex2_submission_special_instructions 'No special instructions were received'