Construction of [(η5-C5Me5)WS3Cu3]-Based Supramolecular Compounds from Preformed Incomplete Cubane-Like Clusters [PPh4][(η5-C5Me5)WS3(CuX)3] (X = CN, Br)
Xu, Qing-Feng; Chen, Jin-Xiang; Zhang, Wen-Hua; Ren, Zhi-Gang; Li, Hong-Xi; Zhang, Yong; Lang, Jian-Ping; Inorganic Chemistry 45 (2006) 4055–4064; doi:10.1021/ic060115p

data_4332197
_publ_section_title
;
 Construction of [(\h5-C5Me5)WS3Cu3]-Based Supramolecular Compounds from
 Preformed Incomplete Cubane-Like Clusters [PPh4][(\h5-C5Me5)WS3(CuX)3] (X
 = CN, Br)
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4055
_journal_page_last               4064
_journal_paper_doi               10.1021/ic060115p
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C12 H15 Cl Cu3 N2 S3 W, C24 H20 P, C5 H5 N'
_chemical_formula_sum            'C41 H40 Cl Cu3 N3 P S3 W'
_chemical_formula_weight         1111.83
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.532(4)
_cell_length_b                   14.132(3)
_cell_length_c                   14.589(3)
_cell_measurement_reflns_used    1079
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.0
_cell_volume                     4301.7(16)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    'Shelxl-97 (Sheldrick, 1997)'
_computing_publication_material  'Shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \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  0.0973
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41319
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.405
_exptl_absorpt_correction_T_max  0.8098
_exptl_absorpt_correction_T_min  0.3078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7856
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.1028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+47.3285P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2141
_refine_ls_wR_factor_ref         0.2296
_reflns_number_gt                6081
_reflns_number_total             7856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060115psup3.cif
_cod_data_source_block           t
_cod_original_cell_volume        4302.7(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4332197