Bis[1,2-bis(methoxycarbonyl)ethene-1,2-dithiolato-κ^2^<i>S</i>,<i>S</i>']bis(η^5^-pentamethylcyclopentadienyl)tetra-μ~3~-sulfido-tetrairon(4 <i>Fe</i>‒<i>Fe</i>) hexafluoridophosphate
Inomata, Shinji; Ito, Shohei; Takase, Tsugiko; Acta Crystallographica Section E 69 (2013) m227–m228; doi:10.1107/S1600536813007514

data_2237732
_publ_section_title
;
 Bis[1,2-bis(methoxycarbonyl)ethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>']bis(\h^5^-pentamethylcyclopentadienyl)tetra-\m~3~-sulfido-tetrairon(4
 <i>Fe</i>--<i>Fe</i>) hexafluoridophosphate
;
_journal_coeditor_code           WM2732
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m227
_journal_page_last               m228
_journal_paper_doi               10.1107/S1600536813007514
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe4 (C6 H6 O4 S2)2 (C10 H15)2 S4] P F6'
_chemical_formula_moiety         'C32 H42 Fe4 O8 S8 +, F6 P1 -'
_chemical_formula_sum            'C32 H42 F6 Fe4 O8 P S8'
_chemical_formula_weight         1179.51
_chemical_name_systematic
'Bis[1,2-bis(methoxycarbonyl)ethene-1,2-dithiolato-\k^2^<i>S</i>,<i>S</i>']bis(\h^5^-pentamethylcyclopentadienyl)tetra-\m~3~-sulfido-tetrairon(4 <i>Fe</i>--<i>Fe</i>) hexafluoridophosphate'
_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'
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.209(6)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   15.546(9)
_cell_length_b                   23.767(13)
_cell_length_c                   24.872(14)
_cell_measurement_reflns_used    16701
_cell_measurement_temperature    93.0(10)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     8982(9)
_computing_cell_refinement
;
<i>CrystalClear</i> (Rigaku, 2009)
;
_computing_data_collection
;
<i>CrystalClear</i> (Rigaku, 2009)
;
_computing_data_reduction
;
<i>CrystalClear</i> (Rigaku, 2009)
;
_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      93.0(10)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.062
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            81617
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.743
_exptl_absorpt_correction_T_max  0.770
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>REQAB</i>; Jacobson, 1998)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4792.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.94
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         20169
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0697P)^2^+28.5393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1862
_reflns_number_gt                16442
_reflns_number_total             20169
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm2732.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237732
_cod_database_fobs_code          2237732