Synthesis, Structure, and Electrocatalysis of Diiron C-Functionalized Propanedithiolate (PDT) Complexes Related to the Active Site of [FeFe]-Hydrogenases
Li-Cheng Song; Chang-Gong Li; Jie Gao; Bang-Shao Yin; Xiang Luo; Xiao-Guang Zhang; Hai-Lin Bao; Qing-Mei Hu; Inorganic Chemistry 47 (2008) 4545–4553; doi:10.1021/ic701982z

data_4304482
_publ_section_title
;
Synthesis, Structure, and Electrocatalysis of Diiron C-Functionalized
Propanedithiolate (PDT) Complexes Related to the Active Site of
[FeFe]-Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4545
_journal_page_last               4553
_journal_paper_doi               10.1021/ic701982z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C9 H4 Fe2 O7 S2'
_chemical_formula_sum            'C9 H4 Fe2 O7 S2'
_chemical_formula_weight         399.94
_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                 100.805(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.259(3)
_cell_length_b                   8.8183(12)
_cell_length_c                   18.165(3)
_cell_measurement_reflns_used    8050
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.5
_cell_volume                     2715.6(7)
_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      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25097
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    2.468
_exptl_absorpt_correction_T_max  0.6381
_exptl_absorpt_correction_T_min  0.6108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00003(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                5525
_reflns_number_total             6482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701982z-file008.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2715.7(7)
_cod_database_code               4304482