Decacarbonyl(μ~4~-2-thiodithiobenzoato- κ^4^C,<i>S,S</i>',<i>S</i>'')bis(trimethyl phosphite)tetrafer
Laifa, El Adoui; Benali-Cherif, Nourredine; Acta Crystallographica Section E 59 (2003) m283–m285; doi:10.1107/S1600536803008638

data_2201969
_publ_section_title
;
 Decacarbonyl(\m~4~-2-thiodithiobenzoato-
 \k^4^C,<i>S,S</i>',<i>S</i>'')bis(trimethyl phosphite)tetrafer
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m283
_journal_page_last               m285
_journal_paper_doi               10.1107/S1600536803008638
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Fe4 (C3 H9 O3 P)2 (C7 H4 S3) (CO )10]'
_chemical_formula_moiety         'C23 H22 Fe4 O16 P2 S3'
_chemical_formula_structural     'FE4 S3 P2 C23 O16 H22'
_chemical_formula_sum            'C23 H22 Fe4 O16 P2 S3'
_chemical_formula_weight         935.96
_chemical_melting_point          172
_chemical_name_common
;
Decacarbonyl(\m~4~-2-thiodithiobenzoato-
\k^4^C,S,S',S'')bis(trimethyl phosphite)tetrafer
;
_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
_cell_angle_alpha                90.0
_cell_angle_beta                 96.529(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.4390(2)
_cell_length_b                   8.9990(3)
_cell_length_c                   23.9750(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     3523.73(13)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2002 (Burla et al, 2003)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0057
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7804
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.950
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0302P)^2^+2.4041P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                5439
_reflns_number_total             6840
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6067.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201969
_cod_database_fobs_code          2201969