Synthesis and Characterization of the Octahydrotriborate Complexes Cp*V(B3H8)2 and Cp*Cr(B3H8)2 and the Unusual Cobaltaborane Cluster Cp*2Co2(B6H14)
Do Young Kim; Gregory S. Girolami; Journal of the American Chemical Society 128 (2006) 10969–10977; doi:10.1021/ja063285+

data_4110819
_publ_contact_author_address
;School of Chemical Sciences
University of Illinois at Urbana-Champaign
600 S. Mathews Ave, Urbana, Illinois, 61801
;
_publ_contact_author_email       girolami@scs.uiuc.edu
_publ_contact_author_name        'Gregory S. Girolami'
_publ_section_title
;
 Synthesis and Characterization of the Octahydrotriborate Complexes
 Cp*V(B3H8)2 and Cp*Cr(B3H8)2 and the Unusual Cobaltaborane Cluster
 Cp*2Co2(B6H14)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10969
_journal_page_last               10977
_journal_paper_doi               10.1021/ja063285+
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C20 H39 B5 Mo2'
_chemical_formula_sum            'C20 H39 B5 Mo2'
_chemical_formula_weight         525.44
_chemical_name_common            Cp*2Mo2B5H9
_chemical_name_systematic
(Nonahydropentaborato)bis(pentamethylcyclorpentadienyl)dimolybdenum
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                109.562(4)
_cell_angle_beta                 91.892(4)
_cell_angle_gamma                92.495(4)
_cell_formula_units_Z            2
_cell_length_a                   8.998(2)
_cell_length_b                   11.701(3)
_cell_length_c                   11.971(3)
_cell_measurement_temperature    193(2)
_cell_volume                     1185.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15350
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.81
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.89608
_exptl_absorpt_correction_T_min  0.83311
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5746
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                4000
_reflns_number_total             5746
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063285si20060622_054111.cif
_cod_data_source_block           f21bface
_cod_database_code               4110819