Three-Coordinate Co(I) Provides Access to Unsaturated Dihydrido-Co(III) and Seven-Coordinate Co(V)
Michael Ingleson; Hongjun Fan; Maren Pink; John Tomaszewski; Kenneth G. Caulton; Journal of the American Chemical Society 128 (2006) 1804–1805; doi:10.1021/ja0572452

data_4110414
_publ_section_title
;
 Three-Coordinate Co(I) Provides Access to Unsaturated Dihydrido-Co(III)
 and Seven-Coordinate Co(V)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1804
_journal_page_last               1805
_journal_paper_doi               10.1021/ja0572452
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C22 H52 Co N P2 Si2'
_chemical_formula_sum            'C22 H52 Co N P2 Si2'
_chemical_formula_weight         507.70
_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                77.808(3)
_cell_angle_beta                 77.742(3)
_cell_angle_gamma                66.448(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1630(11)
_cell_length_b                   11.1230(12)
_cell_length_c                   14.6824(16)
_cell_measurement_reflns_used    4863
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.2
_cell_volume                     1471.9(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2003), XTEL (loc. libr.)'
_computing_publication_material  'SHELXTL (Bruker, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
'0.30 degree frames measured for 3 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16897
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  256
_diffrn_standards_number         113
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.8721
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.9025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                5538
_reflns_number_total             6777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0572452si20051101_014508.cif
_cod_data_source_block           05126
_cod_database_code               4110414