Synthesis of Mono- and Dihalogenated Derivatives of (Me2S)2B12H10 and Palladium-Catalyzed Boron-Carbon Cross-Coupling Reactions of the Iodides with Grignard Reagents
Roman G. Kultyshev; Shengming Liu; Hoitung T. Leung; Jianping Liu; Sheldon G. Shore; Inorganic Chemistry 42 (2003) 3199–3207; doi:10.1021/ic020600u

data_4313586
_publ_section_title
;
 Synthesis of Mono- and Dihalogenated Derivatives of (Me2S)2B12H10 and
 Palladium-Catalyzed Boron-Carbon Cross-Coupling Reactions of the Iodides
 with Grignard Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3199
_journal_page_last               3207
_journal_paper_doi               10.1021/ic020600u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C11 H28 B12 S2'
_chemical_formula_weight         354.17
_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                95.078(10)
_cell_angle_beta                 98.175(10)
_cell_angle_gamma                101.251(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9365(10)
_cell_length_b                   10.3822(10)
_cell_length_c                   12.5820(10)
_cell_measurement_reflns_used    '10 frames'
_cell_measurement_temperature    150(2)
_cell_volume                     999.24(19)
_computing_cell_refinement       'DENZO (Otwinowsky & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowsky & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega at 55/-55'
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6905
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.9244
_exptl_absorpt_correction_T_min  0.8907
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.2904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                3034
_reflns_number_total             3533
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020600u_6.cif
_cod_data_source_block           compound19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        999.24(18)
_cod_database_code               4313586