Diiron Thiadithiolates as Active Site Models for the Iron-Only Hydrogenases: Synthesis, Structures, and Catalytic H2Production
Song, Li-Cheng; Yang, Zhi-Yong; Hua, Yu-Juan; Wang, Hu-Ting; Liu, Yang; Hu, Qing-Mei; Organometallics 26 (2007) 2106–; doi:10.1021/om061186z

data_4072987
_publ_section_title
;
 Diiron Thiadithiolates as Active Site Models for the Iron-Only
 Hydrogenases:&#x00A0; Synthesis, Structures, and Catalytic H2Production
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2106
_journal_paper_doi               10.1021/om061186z
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C15 H9 B F4 Fe3 O8 S3'
_chemical_formula_sum            'C15 H9 B F4 Fe3 O8 S3'
_chemical_formula_weight         667.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.078(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.929(6)
_cell_length_b                   7.5006(18)
_cell_length_c                   14.284(4)
_cell_measurement_reflns_used    6237
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.6
_cell_volume                     2336.2(11)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS97
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21013
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  0.6699
_exptl_absorpt_correction_T_min  0.6699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         5526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0433
_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^)+(0.0641P)^2^+0.3677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                4301
_reflns_number_total             5526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061186zsi20061229_025849.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2336.2(10)
_cod_database_code               4072987