Nitrile Hydration by Thiolate- and Alkoxide-Ligated Co-NHase Analogues. Isolation of Co(III)-Amidate and Co(III)-Iminol Intermediates
Rodney D. Swartz; Michael K. Coggins; Werner Kaminsky; Julie A. Kovacs; Journal of the American Chemical Society 133 (2011) 3954–3963; doi:10.1021/ja108749f

data_4105768
_publ_contact_author_address
;
Department of Chemistry, BOX 351700
University of Washington
Seattle, WA 98195
USA
;
_publ_contact_author_email       wernerka@u.washington.edu
_publ_contact_author_name        'Werner Kaminsky'
_publ_section_title
;
 Nitrile Hydration by Thiolate- and Alkoxide-Ligated Co-NHase Analogues.
 Isolation of Co(III)-Amidate and Co(III)-Iminol Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3954
_journal_page_last               3963
_journal_paper_doi               10.1021/ja108749f
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C13 H28 Co N5 S, 2(F6 P)'
_chemical_formula_sum            'C13 H28 Co F12 N5 P2 S'
_chemical_formula_weight         635.33
_chemical_name_common            CoIIITren
_chemical_name_systematic        CoIIITren
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 100.5910(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0740(3)
_cell_length_b                   16.1330(7)
_cell_length_c                   18.6270(8)
_cell_measurement_reflns_used    551
_cell_measurement_temperature    130(2)
_cell_volume                     2384.98(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens  et al. 1996)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \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  0.0965
_diffrn_reflns_av_sigmaI/netI    0.1684
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9946
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.047
_exptl_absorpt_correction_T_max  0.8258
_exptl_absorpt_correction_T_min  0.7871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1544
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                2552
_reflns_number_total             5436
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108749f_si_001.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4105768