Addition of Dioxygen to an N4S(thiolate) Iron(II) Cysteine Dioxygenase Model Gives a Structurally Characterized Sulfinato-Iron(II) Complex
Alison C. McQuilken; Yunbo Jiang; Maxime A. Siegler; David P. Goldberg; Journal of the American Chemical Society 134 (2012) 8758–8761; doi:10.1021/ja302112y

data_4117985
_publ_contact_author_address
;Department of Chemistry
Johns Hopkins University
Baltimore, Maryland, 21218
United States
;
_publ_contact_author_email       dpg@jhu.edu
_publ_contact_author_name        'David P. Goldberg'
_publ_contact_author_phone       410.516.6658
_publ_section_title
;
 Addition of Dioxygen to an N4S(thiolate) Iron(II) Cysteine Dioxygenase
 Model Gives a Structurally Characterized Sulfinato-Iron(II) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8758
_journal_page_last               8761
_journal_paper_doi               10.1021/ja302112y
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C26 H24 Fe N5 S, B F4'
_chemical_formula_sum            'C26 H24 B F4 Fe N5 S'
_chemical_formula_weight         581.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_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                   12.40931(14)
_cell_length_b                   14.52864(16)
_cell_length_c                   27.6028(3)
_cell_measurement_reflns_used    30334
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      1.58
_cell_volume                     4976.52(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 15.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            55244
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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            'dark brown'
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5709
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0343P)^2^+3.6802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                5028
_reflns_number_total             5709
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja302112y_si_001.cif
_cod_data_source_block           1
_cod_database_code               4117985