A Complete Family of Isostructural Cluster Compounds with Cubane-like M3S4M' Cores (M = Mo, W; M' = Ni, Pd, Pt): Comparative Crystallography and Electrochemistry
Konrad Herbst; Piero Zanello; Maddalena Corsini; Nicola D'Amelio; Lutz Dahlenburg; Michael Brorson; Inorganic Chemistry 42 (2003) 974–981; doi:10.1021/ic0205379

data_4313109
_publ_section_title
;
 A Complete Family of Isostructural Cluster Compounds with Cubane-like
 M3S4M' Cores (M = Mo, W; M' = Ni, Pd, Pt): Comparative Crystallography
 and Electrochemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              974
_journal_page_last               981
_journal_paper_doi               10.1021/ic0205379
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C43 H43 As1 Mo3 Ni1 O3 S5'
_chemical_formula_structural     'C43 H43 AS1 MO3 NI1 O3 S5'
_chemical_formula_sum            'C43 H43 As Mo3 Ni O3 S5'
_chemical_formula_weight         1189.52
_chemical_name_systematic
;
  Tetra-\m3-thio-tris[(methylcyclopentadienyl)molybdenum]-
  (triphenylarsine)nickel p-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             2000-04-25T11:47:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.10(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.484(1)
_cell_length_b                   10.8772(6)
_cell_length_c                   42.327(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.0
_cell_measurement_theta_min      8.5
_cell_measurement_wavelength     0.71073
_cell_volume                     4363.5(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf 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      -0.13364E-1
_diffrn_orient_matrix_UB_12      -0.78077E-1
_diffrn_orient_matrix_UB_13      0.12003E-1
_diffrn_orient_matrix_UB_21      0.01184
_diffrn_orient_matrix_UB_22      -0.48327E-1
_diffrn_orient_matrix_UB_23      -0.19824E-1
_diffrn_orient_matrix_UB_31      0.103991
_diffrn_orient_matrix_UB_32      -0.4538E-2
_diffrn_orient_matrix_UB_33      0.4677E-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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0717
_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       50
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7833
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.55
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.298
_exptl_absorpt_correction_T_max  0.8938
_exptl_absorpt_correction_T_min  0.46
_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   3
         Theta correction was applied.
         Averaged transmission function was used.
         No Fourier smoothing was applied.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         7725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.097
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                5133
_reflns_number_total             7725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0205379_3.cif
_cod_data_source_block           tops01
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4313109
_exptl_absorpt_factor_mur        0.115
_exptl_absorpt_correction_t_ave  0.7982
_diffrn_standards_decay_corr_max 1.034
_diffrn_standards_decay_corr_min 0.974