Synthesis of the New, Cubane-like W3S4Co Cluster Core. Completion of the Homologous Series [(η5-Cp')3M3S4Co(CO)] (M = Cr, Mo, W)
Konrad Herbst; Lutz Dahlenburg; Michael Brorson; Inorganic Chemistry 43 (2004) 3327–3328; doi:10.1021/ic049742+

data_4327435
_publ_section_title
;
 Synthesis of the New, Cubane-like W3S4Co Cluster Core. Completion of the
 Homologous Series [(\h5-Cp')3M3S4Co(CO)] (M = Cr, Mo, W)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3327
_journal_page_last               3328
_journal_paper_doi               10.1021/ic049742+
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C19 H21 Co1 O1 S4 W3'
_chemical_formula_sum            'C19 H21 Co O S4 W3'
_chemical_formula_weight         1004.08
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2004-02-20T14:41:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.85(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.150(2)
_cell_length_b                   18.309(3)
_cell_length_c                   15.111(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      7.3
_cell_measurement_wavelength     0.71073
_cell_volume                     2253.7(9)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
  x-axis points to radiation source
  the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.032095
_diffrn_orient_matrix_UB_12      -0.032206
_diffrn_orient_matrix_UB_13      -0.051122
_diffrn_orient_matrix_UB_21      0.057308
_diffrn_orient_matrix_UB_22      -0.042074
_diffrn_orient_matrix_UB_23      0.02977
_diffrn_orient_matrix_UB_31      -0.103718
_diffrn_orient_matrix_UB_32      -0.013248
_diffrn_orient_matrix_UB_33      0.029732
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4824
_diffrn_reflns_theta_full        26.17
_diffrn_reflns_theta_max         26.17
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    16.365
_exptl_absorpt_correction_T_max  0.4342
_exptl_absorpt_correction_T_min  0.0839
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
        Number of psi-scan sets used was   2
        Theta correction was applied.
        Averaged transmission function was used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            'greenish black'
_exptl_crystal_density_diffrn    2.959
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.377
_refine_diff_density_min         -2.173
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+10.7780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                3573
_reflns_number_total             4502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497422Bsi20040228_085728.cif
_cod_data_source_block           tops10
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4327435
_exptl_absorpt_factor_mur        0.818
_exptl_absorpt_correction_t_ave  0.2595
_diffrn_standards_decay_corr_max 1.053
_diffrn_standards_decay_corr_min 0.997