Methylcyclopentadienyl-Substituted Tungsten(IV) Sulfido Cluster [(η5-Cp')3W3S4]+ and Its Heterobimetallic Derivative [(η5-Cp')3W3S4Ni(PPh3)]+
Konrad Herbst; Lutz Dahlenburg; Michael Brorson; Inorganic Chemistry 40 (2001) 1989–1992; doi:10.1021/ic001194m

data_4319559
_publ_section_title
;
 Methylcyclopentadienyl-Substituted Tungsten(IV) Sulfido Cluster
 [(\h5-Cp')3W3S4]+ and Its Heterobimetallic Derivative
 [(\h5-Cp')3W3S4Ni(PPh3)]+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1989
_journal_page_last               1992
_journal_paper_doi               10.1021/ic001194m
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C43 H43 Ni1 O3 P1 S5 W3'
_chemical_formula_structural     'C43 H43 NI O3 P S5 W3'
_chemical_formula_sum            'C43 H43 Ni O3 P S5 W3'
_chemical_formula_weight         1409.3
_chemical_name_systematic
;
 Tetra-\m3-thio-tris[(methylcyclopentadienyl)tungsten]-
 (triphenylphosphine)nickel toluenesulfonate
;
_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/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-05-03T15:20:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.04(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.469(2)
_cell_length_b                   10.834(1)
_cell_length_c                   41.839(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      9.2
_cell_measurement_wavelength     0.71073
_cell_volume                     4289.4(12)
_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., 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius MACH 3'
_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      -0.16635E-1
_diffrn_orient_matrix_UB_12      -0.79897E-1
_diffrn_orient_matrix_UB_13      0.11223E-1
_diffrn_orient_matrix_UB_21      0.32659E-1
_diffrn_orient_matrix_UB_22      -0.46179E-1
_diffrn_orient_matrix_UB_23      -0.01907
_diffrn_orient_matrix_UB_31      0.99113E-1
_diffrn_orient_matrix_UB_32      0.1864E-2
_diffrn_orient_matrix_UB_33      0.9075E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8359
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.771
_exptl_absorpt_correction_T_max  0.2178
_exptl_absorpt_correction_T_min  0.1353
_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.
        Weighted transmission curves were used.
        No Fourier smoothing was applied.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.169
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+28.2429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                5713
_reflns_number_total             7597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001194m.cif
_cod_data_source_block           '[2][pts]'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4319559
_exptl_absorpt_factor_mur        2.193
_exptl_absorpt_correction_t_ave  0.076
_diffrn_standards_decay_corr_max 1.017
_diffrn_standards_decay_corr_min 0.975