Iron Acyl Thiolato Carbonyls: Structural Models for the Active Site of the [Fe]-Hydrogenase (Hmd)
Aaron M. Royer; Marco Salomone-Stagni; Thomas B. Rauchfuss; Wolfram Meyer-Klaucke; Journal of the American Chemical Society 132 (2010) 16997–17003; doi:10.1021/ja1072228

data_4103585
_publ_contact_author
; 
Thomas B. Rauchfuss 
University of Illinois 
School of Chemical Sciences, Box 12-6 
600 South Mathews Avenue
M/C 712 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       rauchfuz@illinois.edu
_publ_contact_author_fax         '1  217 244 3186'
_publ_contact_author_phone       '1  217 333 7355'
_publ_section_title
;
 Iron Acyl Thiolato Carbonyls: Structural Models for the Active Site of
 the [Fe]-Hydrogenase (Hmd)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16997
_journal_page_last               17003
_journal_paper_doi               10.1021/ja1072228
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C28 H19 Fe O4 P S'
_chemical_formula_sum            'C28 H19 Fe O4 P S'
_chemical_formula_weight         538.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 110.767(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.4050(6)
_cell_length_b                   11.3697(5)
_cell_length_c                   15.8982(6)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.68
_cell_measurement_theta_min      2.26
_cell_volume                     2434.65(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
'SAINT V7.23A, XPREP V2005/2 (Bruker, 2005 & 2007)'
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1087
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46385
_diffrn_reflns_theta_full        27.16
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.82108
_exptl_absorpt_correction_T_min  0.77308
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP (Bruker, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.362
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5387
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.1923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                4297
_reflns_number_total             5387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1072228_si_002.cif
_cod_data_source_block           fa47jaface
_cod_original_cell_volume        2434.65(17)
_cod_database_code               4103585