Co(III) Complexes with Coordinated Carboxamido Nitrogens and Thiolato Sulfurs as Models for Co-Containing Nitrile Hydratase and Their Conversion to the Corresponding Sulfinato Species
Laurie A. Tyler; Juan C. Noveron; Marilyn M. Olmstead; Pradip K. Mascharak; Inorganic Chemistry 39 (2000) 357–362; doi:10.1021/ic990794m

data_4300097
_publ_contact_author
; Pradip K. Mascharak
  Department of Chemistry and Biochemistry
  University of California
  Santa Cruz, CA 95064
  USA
;
_publ_contact_author_email       mascharak@chemistry.ucsc.edu
_publ_contact_author_fax         831-459-2935
_publ_contact_author_phone       831-459-4251
_publ_section_title
;
Co(III) Complexes with Coordinated Carboxamido Nitrogens and Thiolato
Sulfurs as Models for Co-Containing Nitrile Hydratase and Their Conversion
to the Corresponding Sulfinato Species
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              357
_journal_page_last               362
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C21 H30 Co N4 Na O8 S2'
_chemical_formula_weight         612.53
_chemical_name_common            Na[Co(PyPePRSO2)2].H2O.CH3OH
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.481(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7489(11)
_cell_length_b                   13.1151(13)
_cell_length_c                   20.998(3)
_cell_measurement_reflns_used    138
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     2640.0(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL v. 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13256
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.8441
_exptl_absorpt_correction_T_min  0.7913
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, Sheldrick, G.M., an empirical absorption correction program based 
 on the method of Blessing, R. H., Acta Cryst. (1995). A51, 33-38.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+2.0189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                2333
_reflns_number_total             3806
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        2640.0(5)
_cod_database_code               4300097
_journal_paper_doi 10.1021/ic990794m