Synthesis, Structure Determination, and Spectroscopic/Computational Characterization of a Series of Fe(II)-Thiolate Model Complexes: Implications for Fe-S Bonding in Superoxide Reductases
Adam T. Fiedler; Heather L. Halfen; Jason A. Halfen; Thomas C. Brunold; Journal of the American Chemical Society 127 (2005) 1675–1689; doi:10.1021/ja046939s

data_4111473
_publ_section_title
;
 Synthesis, Structure Determination, and Spectroscopic/Computational
 Characterization of a Series of Fe(II)-Thiolate Model Complexes:
 Implications for Fe-S Bonding in Superoxide Reductases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1675
_journal_page_last               1689
_journal_paper_doi               10.1021/ja046939s
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C22 H39 F3 Fe N4 O4 S2'
_chemical_formula_weight         600.54
_chemical_name_common            040038
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.952(2)
_cell_length_b                   16.829(2)
_cell_length_c                   17.932(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      16.07
_cell_measurement_theta_min      10.32
_cell_volume                     5417.5(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker/Nonius MACH3S'
_diffrn_measurement_method       'Omega 2-theta 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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11929
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.01
_diffrn_standards_interval_time  '5400 seconds'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.515
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         6073
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                4734
_reflns_number_total             6073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046939ssi20041008_063450.cif
_cod_data_source_block           040038
_cod_database_code               4111473