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_4118472
_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            'C16 H32.2 Fe2 N O4.1 P2 S2'
_chemical_formula_weight         541.99
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 94.324(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.053(6)
_cell_length_b                   7.261(2)
_cell_length_c                   21.693(7)
_cell_measurement_reflns_used    6852
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.26
_cell_volume                     2835.5(15)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25508
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  0.9378
_exptl_absorpt_correction_T_min  0.7629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4973
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0748P)^2^+7.8386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1650
_reflns_number_gt                3811
_reflns_number_total             4973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja304866r_si_002_3.cif
_cod_data_source_block           depdtNO
_cod_original_cell_volume        2835.6(16)
_cod_original_formula_sum        'C16 H32.20 Fe2 N O4.10 P2 S2'
_cod_database_code               4118472