Three-Coordinate and Four-Coordinate Cobalt Hydride Complexes That React with Dinitrogen
Keying Ding; William W. Brennessel; Patrick L. Holland; Journal of the American Chemical Society 131 (2009) 10804–10805; doi:10.1021/ja902812y

data_4104813
_publ_section_title
;
 Three-Coordinate and Four-Coordinate Cobalt Hydride Complexes That React
 with Dinitrogen
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10804
_journal_page_last               10805
_journal_paper_doi               10.1021/ja902812y
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C70 H108 Co2 N4, C7 H8'
_chemical_formula_sum            'C77 H116 Co2 N4'
_chemical_formula_weight         1215.60
_chemical_name_common            holkd15
_chemical_name_systematic
;
 (diketiminate)cobalt(II) hydride dimer
;
_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                80.537(5)
_cell_angle_beta                 83.396(4)
_cell_angle_gamma                80.793(5)
_cell_formula_units_Z            6
_cell_length_a                   13.283(4)
_cell_length_b                   24.629(8)
_cell_length_c                   32.790(10)
_cell_measurement_reflns_used    4096
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.26
_cell_volume                     10401(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.1405
_diffrn_reflns_av_sigmaI/netI    0.1516
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            186084
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             3960
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2356
_refine_ls_number_reflns         36503
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1656
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.4320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                18717
_reflns_number_total             36503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902812y_si_002_1.cif
_cod_data_source_block           1
_cod_database_code               4104813