Unusual Cationic Tris(Dimethylsulfide)-Substitutedcloso-Boranes: Preparation and Characterization of [1,7,9-(Me2S)3-B12H9] BF4 and [1,2,10-(Me2S)3-B10H7] BF4
Ewan J. M. Hamilton; Hoitung T. Leung; Roman G. Kultyshev; Xuenian Chen; Edward A. Meyers; Sheldon G. Shore; Inorganic Chemistry 51 (2012) 2374–2380; doi:10.1021/ic2023709

data_4328379
_publ_section_title
;
 Unusual Cationic Tris(Dimethylsulfide)-Substitutedcloso-Boranes:
 Preparation and Characterization of [1,7,9-(Me2S)3-B12H9] BF4 and
 [1,2,10-(Me2S)3-B10H7] BF4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2374
_journal_page_last               2380
_journal_paper_doi               10.1021/ic2023709
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C5 H24 B12 S3'
_chemical_formula_weight         310.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.8446(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.86920(10)
_cell_length_b                   14.59720(10)
_cell_length_c                   18.26530(10)
_cell_measurement_temperature    299(2)
_cell_volume                     3455.81(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15490
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_correction_T_min  0.9163
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7907
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0734P)^2^+0.8652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                5338
_reflns_number_total             7907
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2023709_si_003_1.cif
_cod_data_source_block           1,7-(SMe2)2-9-(SMe)-B12H9
_cod_database_code               4328379