Bis[1,2-bis(ethoxycarbonyl)ethene-1,2-dithiolato-κ^2^<i>S</i>,<i>S</i>']bis(η^5^-pentamethylcyclopentadienyl)tetra-μ~3~-sulfido-diiron(IV)diiron(III)(3 <i>Fe</i>—<i>Fe</i>)
Ito, Shohei; Hisamichi, Nozomu; Takase, Tsugiko; Inomata, Shinji; Acta Crystallographica Section E 69 (2013) m181–; doi:10.1107/S1600536813005564

data_2237728
_publ_section_title
;
 Bis[1,2-bis(ethoxycarbonyl)ethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>']bis(\h^5^-pentamethylcyclopentadienyl)tetra-\m~3~-sulfido-diiron(IV)diiron(III)(3
 <i>Fe</i>---<i>Fe</i>)
;
_journal_coeditor_code           WM2725
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m181
_journal_paper_doi               10.1107/S1600536813005564
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe4 (C10 H15)2 (C8 H10 O4 S2)2 S4]'
_chemical_formula_moiety         'C36 H50 Fe4 O8 S8'
_chemical_formula_sum            'C36 H50 Fe4 O8 S8'
_chemical_formula_weight         1090.65
_chemical_name_systematic
'Bis[1,2-bis(ethoxycarbonyl)ethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>']bis(\h^5^-pentamethylcyclopentadienyl)tetra-\m~3~-sulfido-diiron(IV)diiron(III)(3 <i>Fe</i>---<i>Fe</i>)'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.6186(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   23.4532(5)
_cell_length_b                   10.4466(2)
_cell_length_c                   18.3113(3)
_cell_measurement_reflns_used    18942
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     4486.12(15)
_computing_cell_refinement
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_collection
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_reduction
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 2012)
;
_computing_publication_material
;
<i>CrystalStructure</i> (Rigaku, 2006)
;
_computing_structure_refinement
;
<i>SHELXL97</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SIR97</i> (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      296.0(10)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21429
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Jacobson, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5111
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0370P)^2^+5.9377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                4694
_reflns_number_total             5111
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2725.cif
_cod_data_source_block           I
_cod_original_cell_volume        4486.14(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2237728
_cod_database_fobs_code          2237728