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_4110816
_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         'C10 H31 B6 V'
_chemical_formula_sum            'C10 H31 B6 V'
_chemical_formula_weight         267.15
_chemical_name_common            Cp*V(B3H8)2
_chemical_name_systematic
; 
 Bis(octahydrotriborato)(pentamethycyclopentadienyl)vanadium(III)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 116.825(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.745(3)
_cell_length_b                   16.065(6)
_cell_length_c                   7.513(3)
_cell_measurement_temperature    193(2)
_cell_volume                     834.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_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  0.0882
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3841
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         794
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+2.0610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.1910
_reflns_number_gt                584
_reflns_number_total             794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063285si20060622_054036.cif
_cod_data_source_block           f53yc2m
_cod_original_cell_volume        834.1(6)
_cod_database_code               4110816