Synthesis and Properties of Triarylhalostibonium Cations.
Yang, Mengxi; Gabbaï, François P; Inorganic chemistry 56 (2017) 8644–8650; doi:10.1021/acs.inorgchem.7b00293

data_4345978
_publ_section_title
;
 Synthesis and Properties of Triarylhalostibonium Cations.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8644
_journal_page_last               8650
_journal_paper_doi               10.1021/acs.inorgchem.7b00293
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C29 H33 Cl11 Sb2'
_chemical_formula_weight         1015.00
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1353(6)
_cell_length_b                   14.9499(6)
_cell_length_c                   21.8393(10)
_cell_measurement_reflns_used    4610
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      23.00
_cell_measurement_theta_min      3.10
_cell_volume                     4288.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.1231
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            73310
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.368
_diffrn_reflns_theta_min         1.651
_exptl_absorpt_coefficient_mu    1.964
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.831
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         10681
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+7.0161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7901
_reflns_number_total             10681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00293_si_003.cif
_cod_data_source_block           6_[Mes3SbCl][SbCl6]
_cod_database_code               4345978
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.683
_shelx_estimated_absorpt_t_max   0.843
_shelx_res_checksum              49097
_shelx_hkl_checksum              22077
_shelx_fab_checksum              68242