Undecacarbonyl(μ~4~-2-thiodithiobenzoato-κ^4^C,<i>S,S</i>',<i>S</i>'')(trimethylphosphite)tetrafer
Laifa El Adoui; Nourredine Benali-Cherif; Hocine Merazig; Acta Crystallographica Section E 59 (2003) m108–m110; doi:10.1107/S1600536803003052

data_2201956
_publ_section_title
Undecacarbonyl(\m~4~-2-thiodithiobenzoato-\k^4^C,<i>S,S</i>',<i>S</i>'')(trimethylphosphite)tetrafer
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m108
_journal_page_last               m110
_journal_paper_doi               10.1107/S1600536803003052
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Fe4 (C3 H9 O3 P1) (C7 H4 S3) (C O)11]'
_chemical_formula_moiety         'C21 H13 Fe4 O14 P1 S3'
_chemical_formula_structural     'FE4 S3 P C21 O14 H13'
_chemical_formula_sum            'C21 H13 Fe4 O14 P S3'
_chemical_formula_weight         839.89
_chemical_melting_point          210
_chemical_name_common
;
Undecacarbonyl(\m~4~-2-thiodithiobenzoato-
\k^4^C,S,S',S'')(trimethylphosphite)tetrafer
;
_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
_cell_angle_alpha                93.971(2)
_cell_angle_beta                 100.923(5)
_cell_angle_gamma                111.959(5)
_cell_formula_units_Z            2
_cell_length_a                   9.263(5)
_cell_length_b                   11.588(5)
_cell_length_c                   15.784(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1524.5(11)
_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 publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6499
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.187
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.474
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6179
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.2274P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                4937
_reflns_number_total             6179
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn6051.cif
_cod_data_source_block           I
_cod_original_cell_volume        1524.5(12)
_cod_original_formula_sum        'C21 H13 Fe4 O14 P1 S3'
_cod_database_code               2201956
_cod_database_fobs_code          2201956