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_4111472
_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            'C15.5 H33 Cl F6 Fe N4 P S'
_chemical_formula_weight         543.79
_chemical_name_common            'Complex 3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.037(2)
_cell_length_b                   15.037(2)
_cell_length_c                   17.395(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.85
_cell_measurement_theta_min      7.70
_cell_volume                     3406.3(9)
_computing_data_reduction        XCAD4
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0736
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4003
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '5400 seconds'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.217
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0710
_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^)+(0.1155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                1298
_reflns_number_total             2009
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046939ssi20040524_063507.cif
_cod_data_source_block           030061
_cod_original_formula_sum        'C15.50 H33 Cl F6 Fe N4 P S'
_cod_database_code               4111472