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_4328380
_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_moiety         'C6 H27 B12 S3 B F4'
_chemical_formula_sum            'C6 H27 B13 F4 S3'
_chemical_formula_weight         411.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.9478(6)
_cell_angle_beta                 88.4436(6)
_cell_angle_gamma                88.3986(8)
_cell_formula_units_Z            4
_cell_length_a                   11.3549(2)
_cell_length_b                   13.4361(2)
_cell_length_c                   13.7877(2)
_cell_measurement_reflns_used    7309
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.04
_cell_volume                     2093.89(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0511
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14229
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (BLESSING, 1995)'
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0519P)^2^+2.7160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                5351
_reflns_number_total             7379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2023709_si_003_2.cif
_cod_data_source_block           '[1,7,9-(SMe2)3-B12H9]BF4'
_cod_database_code               4328380