Influence of Thiolate Ligands on Reductive N-O Bond Activation. Probing the O2-Binding Site of a Biomimetic Superoxide Reductase Analogue and Examining the Proton-Dependent Reduction of Nitrite
Gloria Villar-Acevedo; Elaine Nam; Sarah Fitch; Jason Benedict; John Freudenthal; Werner Kaminsky; Julie A. Kovacs; Journal of the American Chemical Society 133 (2011) 1419–1427; doi:10.1021/ja107551u

data_4105569
_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        'Jason B. Benedict'
_publ_section_title
;
 Influence of Thiolate Ligands on Reductive N-O Bond Activation. Probing
 the O2-Binding Site of a Biomimetic Superoxide Reductase Analogue and
 Examining the Proton-Dependent Reduction of Nitrite
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1419
_journal_page_last               1427
_journal_paper_doi               10.1021/ja107551u
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C11 H25 Fe N5 O2 S, F6 P'
_chemical_formula_sum            'C11 H25 F6 Fe N5 O2 P S'
_chemical_formula_weight         492.24
_chemical_name_common            575nm
_chemical_name_systematic        575nm
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   13.6260(5)
_cell_length_b                   8.5790(9)
_cell_length_c                   15.8870(10)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    130(2)
_cell_volume                     1857.1(2)
_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    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.927
_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  0.1474
_diffrn_reflns_av_sigmaI/netI    0.1947
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3444
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.9278
_exptl_absorpt_correction_T_min  0.7804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       0.0016(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.2284
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                733
_reflns_number_total             2023
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja107551u_si_003.cif
_cod_data_source_block           shelxl
_cod_database_code               4105569