Cyclic Voltammetric Studies of Chlorine-Substituted Diiron Benzenedithiolato Hexacarbonyl Electrocatalysts Inspired by the [FeFe]-Hydrogenase Active Site
Donovan, Elizabeth S.; McCormick, Joseph J.; Nichol, Gary S.; Felton, Greg A. N.; Organometallics 31 (2012) 8067–; doi:10.1021/om300938e

data_4079683
_publ_section_title
;
 Cyclic Voltammetric Studies of Chlorine-Substituted Diiron
 Benzenedithiolato Hexacarbonyl Electrocatalysts Inspired by the
 [FeFe]-Hydrogenase Active Site
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8067
_journal_paper_doi               10.1021/om300938e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C12 H Cl3 Fe2 O6 S2'
_chemical_formula_sum            'C12 H Cl3 Fe2 O6 S2'
_chemical_formula_weight         523.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.938(4)
_cell_angle_beta                 80.939(4)
_cell_angle_gamma                64.881(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5788(5)
_cell_length_b                   8.8191(6)
_cell_length_c                   14.7063(9)
_cell_measurement_reflns_used    5284
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.55
_cell_volume                     877.59(10)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11513
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    2.373
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_correction_T_min  0.7173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0415P)^2^+2.3169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                2602
_reflns_number_total             3186
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300938e_si_002.cif
_cod_data_source_block           ex1004
_cod_database_code               4079683