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_4102273
_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         '(C24 H40 B Co N9) 0.5(C7 H8)'
_chemical_formula_sum            'C27.5 H44 B Co N9'
_chemical_formula_weight         570.46
_chemical_name_systematic
; 
 ? 
;
_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                 90.437(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5385(12)
_cell_length_b                   19.126(2)
_cell_length_c                   15.7062(17)
_cell_measurement_reflns_used    11661
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.0
_cell_volume                     3165.6(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo, Scalepack (Otwinowski & Minor, 1997'
_computing_molecular_graphics    'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXTL v6.1 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL v6.1 (Sheldrick, 1997)'
_diffrn_ambient_temperature      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48065
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9943
_exptl_absorpt_correction_T_min  0.8334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5569
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+3.4331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                4229
_reflns_number_total             5569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910766w_si_002_8.cif
_cod_data_source_block           Tp(t-Bu)(Me)CoN3
_cod_original_formula_sum        'C27.50 H44 B Co N9'
_cod_database_code               4102273