Formation and Subsequent Reactivity of a N2-Stabilized Cobalt–Hydride Complex
Krogman, Jeremy P.; Foxman, Bruce M.; Thomas, Christine M.; Organometallics 34 (2015) 3159–; doi:10.1021/acs.organomet.5b00182

data_4085968
_publ_section_title
;
 Formation and Subsequent Reactivity of a N2-Stabilized Cobalt--Hydride
 Complex
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3159
_journal_paper_doi               10.1021/acs.organomet.5b00182
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C77 H104 Co1 N4 O1 P3 Si1 Zr1'
_chemical_formula_sum            'C77 H104 Co N4 O P3 Si Zr'
_chemical_formula_weight         1372.86
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-18
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 104.902(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8701(7)
_cell_length_b                   23.4332(12)
_cell_length_c                   24.7100(13)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     7201.6(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            95392
_diffrn_reflns_theta_full        30.020
_diffrn_reflns_theta_max         30.020
_diffrn_reflns_theta_min         1.217
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.65
_refine_diff_density_min         -1.06
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0239
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         20953
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.0026540
_refine_ls_shift/su_mean         0.0000866
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 7.90P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0910
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0910
_reflns_limit_h_max              17
_reflns_limit_h_min              -18
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              34
_reflns_limit_l_min              0
_reflns_number_gt                15756
_reflns_number_total             20953
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.22
_oxford_diffrn_Wilson_scale      203.45
_oxford_refine_ls_r_factor_ref   0.0591
_oxford_refine_ls_scale          0.073812(7)
_oxford_reflns_number_all        20953
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'JK_418_0m in P2(1)/c'
_cod_data_source_file            om5b00182_si_002.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 4085963--4085969.cif.'
_cod_original_cell_volume        7201.6(4)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C77 H104 Co1 N4 O1 P3 Si1 Zr1'
_cod_database_code               4085968