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

data_4345977
_publ_section_title
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 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_absolute_configuration ad
_chemical_formula_moiety         '1(C28 H33 F4 O3 S Sb)'
_chemical_formula_sum            'C28 H33 F4 O3 S Sb'
_chemical_formula_weight         647.35
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.10.22 svn.r3046 for OlexSys, GUI svn.r4928)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   27.1408(10)
_cell_length_b                   27.1408(10)
_cell_length_c                   12.7751(6)
_cell_measurement_reflns_used    9290
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      27.416
_cell_measurement_theta_min      2.334
_cell_volume                     8149.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 0.977
_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  0.1853
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            39533
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.501
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.8417.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         6372
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0601
_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^)+78.0352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1015
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5683
_reflns_number_total             6372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00293_si_003.cif
_cod_data_source_block           4_Mes3SbF(OTf)
_cod_original_cell_volume        8149.7(7)
_cod_database_code               4345977
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(4) 0.03(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
S2 \\sim O5 \\sim O6 \\sim C38 \\sim F6 \\sim F7 \\sim F8: within 1.7A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5) = Uanis(O6)
Uanis(O4) = Uanis(Sb2)
4. Rigid body (RIGU) restrains
 S2, O5, O6, C38, F6, F7, F8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Same fragment restrains
{O1, S1, O2, O3, C28, F2, F3, F4} sigma for 1-2: 0.005, 1-3: 0.04
as
{O4, S2, O5, O6, C38, F6, F7, F8}
6. Others
 Fixed Sof: O4(0.33333) S2(0.33333) O5(0.33333) O6(0.33333) C38(0.33333)
 F6(0.33333) F7(0.33333) F8(0.33333)
7.a Riding coordinates:
 C8(H8A,H8B,H8C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23), C31(H31), C33(H33)
7.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              77063
_shelx_hkl_checksum              71559
_olex2_submission_special_instructions 'No special instructions were received'