Mo(W)/Cu/S Cluster-Based Supramolecular Arrays Assembled from Preformed Clusters [Et4N]4[WS4Cu4I6] and [(n-Bu)4N]2[MoOS3Cu3X3] (X = I, SCN) with Flexible Ditopic Ligands
Lang, Jian-Ping; Xu, Qing-Feng; Zhang, Wen-Hua; Li, Hong-Xi; Ren, Zhi-Gang; Chen, Jin-Xiang; Zhang, Yong; Inorganic Chemistry 45 (2006) 10487–10496; doi:10.1021/ic060974d

data_4332867
_publ_section_title
;
 Mo(W)/Cu/S Cluster-Based Supramolecular Arrays Assembled from Preformed
 Clusters [Et4N]4[WS4Cu4I6] and [(n-Bu)4N]2[MoOS3Cu3X3] (X = I, SCN) with
 Flexible Ditopic Ligands
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10487
_journal_page_last               10496
_journal_paper_doi               10.1021/ic060974d
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C24 H14 Cu4 N10 S8 W, C4 H10 O, 2(C2 H3 N)'
_chemical_formula_sum            'C32 H30 Cu4 N12 O S8 W'
_chemical_formula_weight         1293.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.396(2)
_cell_length_b                   17.135(2)
_cell_length_c                   18.341(3)
_cell_measurement_reflns_used    5654
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     5152.8(12)
_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     0.71070
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_sigmaI/netI    0.0584
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25841
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.33
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.210
_exptl_absorpt_correction_T_max  0.6560
_exptl_absorpt_correction_T_min  0.3649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.166
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         5898
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0811
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+72.3457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.1935
_reflns_number_gt                5608
_reflns_number_total             5898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060974dsup2.cif
_cod_data_source_block           tmp
_cod_original_sg_symbol_H-M      C2221
_cod_database_code               4332867