Synthesis and structure-dependent optical properties of two new organic-inorganic hybrid antimony(III) chlorides.
Wen, Xuemei; Cheng, Juan; Qian, Peiqi; Zhang, Zhizhuan; Zeng, Hongmei; Huang, Ling; Zou, Guohong; Lin, Zhien; Dalton transactions (Cambridge, England : 2003) 53 (2023) 260–266; doi:10.1039/d3dt02867d

data_7714540
_publ_section_title
;
 Synthesis and structure-dependent optical properties of two new
 organic-inorganic hybrid antimony(III) chlorides.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              260
_journal_page_last               266
_journal_paper_doi               10.1039/d3dt02867d
_journal_volume                  53
_journal_year                    2023
_chemical_formula_moiety         'Cl6 Sb, C9 H26 N3'
_chemical_formula_sum            'C9 H26 Cl6 N3 Sb'
_chemical_formula_weight         510.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-27 deposited with the CCDC.	2023-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.307(3)
_cell_length_b                   12.149(3)
_cell_length_c                   13.378(2)
_cell_measurement_reflns_used    6681
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.36
_cell_volume                     2000.2(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16901
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         2.356
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5671
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0875 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.7606. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.312
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4522
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+1.3002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                3192
_reflns_number_total             4522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02867d2.cif
_cod_data_source_block           mo_xm2_60_3_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7714540--7714541.cif.'
_cod_original_cell_volume        2000.2(7)
_cod_database_code               7714540
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.550
_shelx_estimated_absorpt_t_min   0.387
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.59(4)
 0.41(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C)
;
_shelx_res_checksum              48264
_olex2_submission_special_instructions 'No special instructions were received'