Structural and Spectroscopic Features of Mixed Valent FeIIFeI Complexes and Factors Related to the Rotated Configuration of Diiron Hydrogenase
Chung-Hung Hsieh; Özlen F. Erdem; Scott D. Harman; Michael L. Singleton; Edward Reijerse; Wolfgang Lubitz; Codrina V. Popescu; Joseph H. Reibenspies; Scott M. Brothers; Michael B. Hall; Marcetta Y. Darensbourg; Journal of the American Chemical Society 134 (2012) 13089–13102; doi:10.1021/ja304866r

data_4118470
_publ_contact_author_address     'TX A&M University, Department of Chemistry'
_publ_contact_author_email       Marcetta@mail.chem.tamu.edu
_publ_contact_author_name
'Marcetta Y. Darensbourg; Joseph H. Reibenspies'
_publ_section_title
;
 Structural and Spectroscopic Features of Mixed Valent FeIIFeI Complexes
 and Factors Related to the Rotated Configuration of Diiron Hydrogenase
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13089
_journal_page_last               13102
_journal_paper_doi               10.1021/ja304866r
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C17 H32 Fe2 O4 P2 S2'
_chemical_formula_weight         538.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   11.574(9)
_cell_length_b                   12.767(10)
_cell_length_c                   16.533(14)
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.473
_cell_measurement_theta_min      2.374
_cell_volume                     2443(3)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26483
_diffrn_reflns_theta_full        28.44
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.508
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         6016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1181
_reflns_number_gt                4504
_reflns_number_total             6016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304866r_si_002_1.cif
_cod_data_source_block           depdtpme3
_cod_database_code               4118470