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

data_4345975
_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_formula_moiety         'C29 H33 F6 O6 S2 Sb'
_chemical_formula_sum            'C29 H33 F6 O6 S2 Sb'
_chemical_formula_weight         777.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                74.358(2)
_cell_angle_beta                 78.509(2)
_cell_angle_gamma                62.115(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8717(4)
_cell_length_b                   11.1644(4)
_cell_length_c                   17.4203(7)
_cell_measurement_reflns_used    8185
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.57
_cell_measurement_theta_min      2.44
_cell_volume                     1793.03(12)
_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      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.618
_diffrn_reflns_theta_min         1.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0652 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.8967.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8243
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0298P)^2^+2.7299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6937
_reflns_number_total             8243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00293_si_003.cif
_cod_data_source_block           2_Mes3Sb(OTf)2
_cod_database_code               4345975
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F7-F8 = F7-F9 = F8-F9
 2.15 with sigma of 0.04
 O4-O7 = O4-O8 = O7-O8 = O4-O5 = O4-O6 = O5-O6
 2.42 with sigma of 0.04
 C28-F1 \\sim C28-F2 \\sim C28-F3
 with sigma of 0.02
 C29-F4 \\sim C29-F5 \\sim C29-F6
 with sigma of 0.02
 C30-F7 \\sim C30-F8 \\sim C30-F9
 with sigma of 0.02
 S1-O2 \\sim S1-O3
 with sigma of 0.02
 S2-O5 \\sim S2-O6
 with sigma of 0.02
 S3-O7 \\sim S3-O8
 with sigma of 0.02
 S3-C30 \\sim S2-C29
 with sigma of 0.02
3. Others
 Sof(S3)=Sof(F7)=Sof(F8)=Sof(F9)=Sof(O7)=Sof(O8)=Sof(C30)=1-FVAR(1)
 Sof(S2)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O5)=Sof(O6)=Sof(C29)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C23(H23)
4.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), 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)
;
_shelx_res_checksum              74458
_shelx_hkl_checksum              14614
_shelx_fab_checksum              68914
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'