Cobalt-Mediated Selective B-H Activation and Formation of a Co-B Bond in the Reaction of the 16-Electron CpCo Half-Sandwich Complex Containing an o-Carborane-1,2-dithiolate Ligand with Ethyl Diazoacetate
Guifeng Liu; Jiurong Hu; Jialin Wen; Huimin Dai; Yizhi Li; Hong Yan; Inorganic Chemistry 50 (2011) 4187–4194; doi:10.1021/ic200333q

data_4325018
_publ_contact_author_address
;
    State Key Laboratory of Coordination Chemistry, 
    Nanjing University, 
    Nanjing 210093, 
    P. R. China
;
_publ_contact_author_email       hyan1965@nju.edu.cn
_publ_contact_author_fax         '(+86)-25- 83314502'
_publ_contact_author_name        'H. Yan'
_publ_contact_author_phone       '(+86)-25- 83314502'
_publ_section_title
;
 Cobalt-Mediated Selective B-H Activation and Formation of a Co-B Bond in
 the Reaction of the 16-Electron CpCo Half-Sandwich Complex Containing an
 o-Carborane-1,2-dithiolate Ligand with Ethyl Diazoacetate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4187
_journal_page_last               4194
_journal_paper_doi               10.1021/ic200333q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         '2(C23 H39 B10 Co O8 S2), C H2 Cl2, H2 O '
_chemical_formula_sum            'C47 H82 B20 Cl2 Co2 O17 S4'
_chemical_formula_weight         1452.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0580(17)
_cell_length_b                   13.4281(15)
_cell_length_c                   33.516(4)
_cell_measurement_reflns_used    5302
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.32
_cell_volume                     7227.0(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            37732
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.9326
_exptl_absorpt_correction_T_min  0.9137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         7104
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                4506
_reflns_number_total             7104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200333q_si_001_3.cif
_cod_data_source_block           Compound-3
_cod_original_cell_volume        7227.1(13)
_cod_database_code               4325018