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_4105770
_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 H29 Co N5 O S, F6 P'
_chemical_formula_sum            'C13 H29 Co F6 N5 O P S'
_chemical_formula_weight         507.38
_chemical_name_common            CDS002
_chemical_name_systematic        CDS002
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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                   7.5760(6)
_cell_length_b                   14.5673(13)
_cell_length_c                   18.3780(18)
_cell_measurement_reflns_used    2899
_cell_measurement_temperature    130(2)
_cell_volume                     2028.2(3)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.861
_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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0964
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4723
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4654
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.05
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+4.5357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1281
_reflns_number_gt                3256
_reflns_number_total             4654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja108749f_si_004.cif
_cod_data_source_block           shelxl
_cod_database_code               4105770