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_4104814
_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 K2 N4, C5 H12, 0.5(C6 H6)'
_chemical_formula_sum            'C78 H123 Co2 K2 N4'
_chemical_formula_weight         1312.86
_chemical_name_common            holkd18
_chemical_name_systematic
;
 potassium (diketiminate)cobalt(I) hydride
;
_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                75.232(2)
_cell_angle_beta                 69.676(2)
_cell_angle_gamma                77.776(2)
_cell_formula_units_Z            2
_cell_length_a                   14.078(2)
_cell_length_b                   15.470(2)
_cell_length_c                   19.469(3)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      32.77
_cell_measurement_theta_min      2.21
_cell_volume                     3809.1(9)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67910
_diffrn_reflns_theta_full        32.03
_diffrn_reflns_theta_max         32.03
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.9120
_exptl_absorpt_correction_T_min  0.8720
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            'deep orange'
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         26214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.7457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                16754
_reflns_number_total             26214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902812y_si_002_2.cif
_cod_data_source_block           2
_cod_original_cell_volume        3809.2(9)
_cod_database_code               4104814