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_4110817
_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 Cr'
_chemical_formula_sum            'C10 H31 B6 Cr'
_chemical_formula_weight         268.21
_chemical_name_common            Cp*Cr(B3H8)2
_chemical_name_systematic
Bis(octahydrotriborato)(pentamethylcyclopentadienyl)chromium(III)
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   15.517(3)
_cell_length_b                   15.489(3)
_cell_length_c                   14.462(3)
_cell_measurement_temperature    193(2)
_cell_volume                     3475.8(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26740
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.86
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.93640
_exptl_absorpt_correction_T_min  0.79870
_exptl_absorpt_correction_type   integration
_exptl_crystal_density_diffrn    1.025
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                1998
_reflns_number_total             3199
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063285si20060622_054047.cif
_cod_data_source_block           abs78zf_60
_cod_original_cell_volume        3475.7(13)
_cod_database_code               4110817