Cobalt(II) "Scorpionate" Complexes as Models for Cobalt-Substituted Zinc Enzymes: Electronic Structure Investigation by High-Frequency and -Field Electron Paramagnetic Resonance Spectroscopy
J. Krzystek; Dale C. Swenson; S. A. Zvyagin; Dmitry Smirnov; Andrew Ozarowski; Joshua Telser; Journal of the American Chemical Society 132 (2010) 5241–5253; doi:10.1021/ja910766w

data_4102271
_publ_section_title
;
 Cobalt(II) "Scorpionate" Complexes as Models for Cobalt-Substituted Zinc
 Enzymes: Electronic Structure Investigation by High-Frequency and -Field
 Electron Paramagnetic Resonance Spectroscopy
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5241
_journal_page_last               5253
_journal_paper_doi               10.1021/ja910766w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C25 H40 B Co N7 S'
_chemical_formula_sum            'C25 H40 B Co N7 S'
_chemical_formula_weight         540.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.059(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6545(11)
_cell_length_b                   17.4408(18)
_cell_length_c                   17.9183(18)
_cell_measurement_reflns_used    13045
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     2987.3(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'Denzo, HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 2001)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 2001)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD 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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54226
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_correction_T_min  0.8094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.6680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1011
_reflns_number_gt                4399
_reflns_number_total             6838
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910766w_si_002_6.cif
_cod_data_source_block           Tp(t-Bu)(Me)CoNCS
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_database_code               4102271