Synthesis and Molecular and Electronic Structures of Reduced Bis(imino)pyridine Cobalt Dinitrogen Complexes: Ligand versus Metal Reduction
Amanda C. Bowman; Carsten Milsmann; Crisita Carmen Hojilla Atienza; Emil Lobkovsky; Karl Wieghardt; Paul J. Chirik; Journal of the American Chemical Society 132 (2010) 1676–1684; doi:10.1021/ja908955t

data_4101857
_publ_section_title
;
 Synthesis and Molecular and Electronic Structures of Reduced
 Bis(imino)pyridine Cobalt Dinitrogen Complexes: Ligand versus Metal
 Reduction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1676
_journal_page_last               1684
_journal_paper_doi               10.1021/ja908955t
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C33 H43 Co N5'
_chemical_formula_sum            'C33 H43 Co N5'
_chemical_formula_weight         568.65
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   8.4360(12)
_cell_length_b                   17.851(3)
_cell_length_c                   20.117(3)
_cell_measurement_reflns_used    6485
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.29
_cell_volume                     3029.4(8)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21677
_diffrn_reflns_theta_full        28.53
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.8901
_exptl_absorpt_correction_T_min  0.7753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.688(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0806
_reflns_number_gt                5922
_reflns_number_total             7486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja908955t_si_002.cif
_cod_data_source_block           acb13
_cod_original_cell_volume        3029.5(8)
_cod_database_code               4101857