Rational Tuning of the Thiolate Donor in Model Complexes of Superoxide Reductase: Direct Evidence for a trans Influence in FeIII-OOR Complexes
Frances Namuswe; Gary D. Kasper; Amy A. Narducci Sarjeant; Takahiro Hayashi; Courtney M. Krest; Michael T. Green; Pierre Moënne-Loccoz; David P. Goldberg; Journal of the American Chemical Society 130 (2008) 14189–14200; doi:10.1021/ja8031828

data_4108539
_publ_section_title
;
 Rational Tuning of the Thiolate Donor in Model Complexes of Superoxide
 Reductase: Direct Evidence for a trans Influence in FeIII-OOR Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14189
_journal_page_last               14200
_journal_paper_doi               10.1021/ja8031828
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C18 H33 Fe N4 O S, B F4'
_chemical_formula_sum            'C18 H33 B F4 Fe N4 O S'
_chemical_formula_weight         496.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Wed Feb 07 17:01:29 2007'
;
_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                   15.7595(4)
_cell_length_b                   14.3395(3)
_cell_length_c                   10.0194(3)
_cell_measurement_reflns_used    15282
_cell_measurement_theta_max      27.9998
_cell_measurement_theta_min      3.8655
_cell_volume                     2264.22(10)
_computing_cell_refinement       'Oxford Diffraction CrysAlis RED'
_computing_data_collection       'Oxford Diffraction CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction CrysAlis RED'
_computing_molecular_graphics    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_publication_material  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_refinement  'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_computing_structure_solution    'Sheldrick, G.M. (2000). SHELXTL v6.10.'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 15.9890
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      'see scan set'
_diffrn_measurement_device       Kappa
_diffrn_measurement_device_type  Xcalibur3
_diffrn_measurement_method       ' omega phi scans'
_diffrn_orient_matrix_UB_11      0.0025100739
_diffrn_orient_matrix_UB_12      0.0070797796
_diffrn_orient_matrix_UB_13      -0.0488253831
_diffrn_orient_matrix_UB_21      -0.0294527054
_diffrn_orient_matrix_UB_22      -0.0402910426
_diffrn_orient_matrix_UB_23      -0.0078160608
_diffrn_orient_matrix_UB_31      -0.0643597764
_diffrn_orient_matrix_UB_32      0.0187884266
_diffrn_orient_matrix_UB_33      0.0016245081
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30422
_diffrn_reflns_resolution_max    0.75
_diffrn_reflns_theta_full        28.10
_diffrn_reflns_theta_max         28.10
_diffrn_reflns_theta_min         4.07
_diffrn_source_current           40
_diffrn_source_power             2
_diffrn_source_voltage           50
_diffrn_standards_interval_count 2
_diffrn_standards_interval_time  50
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       rod
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.8939
_exptl_crystal_size_mid          0.1808
_exptl_crystal_size_min          0.1569
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5490
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0947
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+21.0067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2428
_reflns_number_gt                4572
_reflns_number_total             5490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8031828_si_002.cif
_cod_data_source_block           x0339
_cod_database_code               4108539
_audit_creation_method_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection_reference
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinment_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction_reference
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_cell_measurement_resolution_max 0.76
_jhu_your_name_here              'Dr. Amy A Sarjeant'
_jhu_your_lab_here               'NCB 240'
_jhu_your_phone_number_here      x6-8569
_jhu_your_email_here             xray@jhu.edu
_jhu_institutional_source        'Goldberg Lab'
_jhu_submitting_scientist        'Gary Kasper'
_jhu_scientist_phone             x6-7464
_jhu_scientist_email             gkasper@jhu.edu
_jhu_identifying_number          x0339
_jhu_xray_labbook                II-54
_jhu_crystalization_labbook
;
;
_jhu_crystalization_solvent      'Methylene Chloride, Diethyl Ether'
_jhu_crystalization_method
;
;
_jhu_diffraction_detector_distance 50
_jhu_quality_factor              4