data_{[Bu4N][WS4Cu3(CN)2]}n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 Cu3 N3 S4 W' _chemical_formula_sum 'C18 H36 Cu3 N3 S4 W' _chemical_formula_weight 797.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P43212 _symmetry_space_group_name_Hall 'P 4nw 2abw ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+3/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+1/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' _cell_length_a 10.9115(15) _cell_length_b 10.9115(15) _cell_length_c 23.638(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2814.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.78 _exptl_crystal_description 'Block' _exptl_crystal_colour 'orange-red' _exptl_crystal_size_max 0.4200 _exptl_crystal_size_mid 0.2200 _exptl_crystal_size_min 0.1200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.882 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 6.617 _exptl_absorpt_correction_type 'Psi-scan' _exptl_absorpt_correction_T_min 0.106 _exptl_absorpt_correction_T_max 0.266 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 'no decay, variation 0.5' _diffrn_reflns_number 3112 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.97 _reflns_number_total 2758 _reflns_number_gt 1682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_cell_refinement 'SET4 and CELDIM in CAD-4-PC Software (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX96 (Gabe et al., 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+21.5594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00043(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.02(5) _refine_ls_number_reflns 2758 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1274 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1516 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.01149(6) -0.98851(6) -0.2500 0.0441(3) Uani 1 2 d S . . Cu1 Cu -0.18907(18) -0.81093(18) -0.2500 0.0624(9) Uani 1 2 d S . . Cu2 Cu 0.1041(2) -0.8660(2) -0.33074(9) 0.0645(7) Uani 1 1 d . . . S1 S 0.0719(6) -1.0675(5) -0.3258(2) 0.0802(16) Uani 1 1 d . . . S2 S 0.0234(4) -0.7868(4) -0.2519(3) 0.0635(12) Uani 1 1 d . . . N1 N -0.2664(16) -0.7482(17) -0.3189(6) 0.070(4) Uani 1 1 d . . . C1 C -0.3106(19) -0.7055(19) -0.3590(8) 0.064(5) Uani 1 1 d . . . N2 N -0.0882(12) -1.0882(12) -0.5000 0.069(7) Uani 1 2 d S . . C2 C -0.1684(19) -1.120(2) -0.4501(8) 0.080(7) Uani 1 1 d . . . H1A H -0.1568 -1.2063 -0.4422 0.096 Uiso 1 1 calc R . . H1B H -0.1371 -1.0752 -0.4177 0.096 Uiso 1 1 calc R . . C6 C 0.0443(17) -1.1090(18) -0.4815(8) 0.070(6) Uani 1 1 d . . . H3A H 0.0606 -1.0566 -0.4493 0.084 Uiso 1 1 calc R . . H3B H 0.0519 -1.1931 -0.4688 0.084 Uiso 1 1 calc R . . C7 C 0.1423(19) -1.0858(19) -0.5254(9) 0.079(7) Uani 1 1 d . . . H4A H 0.1351 -1.0034 -0.5404 0.095 Uiso 1 1 calc R . . H4B H 0.1349 -1.1436 -0.5563 0.095 Uiso 1 1 calc R . . C3 C -0.302(2) -1.098(3) -0.4527(11) 0.096(8) Uani 1 1 d . . . H6B H -0.3392 -1.1570 -0.4779 0.116 Uiso 1 1 calc R . . H6C H -0.3166 -1.0165 -0.4681 0.116 Uiso 1 1 calc R . . C4 C -0.362(2) -1.108(3) -0.3925(11) 0.102(8) Uani 1 1 d . . . H7A H -0.3396 -1.1864 -0.3764 0.122 Uiso 1 1 calc R . . H7B H -0.3262 -1.0448 -0.3685 0.122 Uiso 1 1 calc R . . C5 C -0.492(3) -1.096(2) -0.3904(10) 0.115(9) Uani 1 1 d . . . H8A H -0.5191 -1.1048 -0.3520 0.173 Uiso 1 1 calc R . . H8B H -0.5285 -1.1584 -0.4134 0.173 Uiso 1 1 calc R . . H8C H -0.5151 -1.0167 -0.4044 0.173 Uiso 1 1 calc R . . C9 C 0.369(2) -1.072(2) -0.5370(11) 0.124(11) Uani 1 1 d . . . H5A H 0.4467 -1.0814 -0.5184 0.185 Uiso 1 1 calc R . . H5B H 0.3603 -0.9896 -0.5502 0.185 Uiso 1 1 calc R . . H5C H 0.3649 -1.1275 -0.5686 0.185 Uiso 1 1 calc R . . C8 C 0.2652(18) -1.102(2) -0.4952(13) 0.090(7) Uani 1 1 d . . . H2A H 0.2733 -1.1856 -0.4818 0.107 Uiso 1 1 calc R . . H2B H 0.2697 -1.0474 -0.4628 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0509(4) 0.0509(4) 0.0305(4) 0.0014(3) 0.0014(3) 0.0037(5) Cu1 0.0703(13) 0.0703(13) 0.0466(18) 0.0003(15) 0.0003(15) 0.0169(16) Cu2 0.0700(18) 0.0810(19) 0.0426(12) 0.0082(13) 0.0082(12) -0.0119(12) S1 0.120(5) 0.065(4) 0.056(3) -0.006(3) 0.036(4) 0.007(3) S2 0.071(3) 0.060(3) 0.060(3) -0.014(3) 0.012(4) -0.013(2) N1 0.071(13) 0.087(14) 0.051(9) 0.005(10) -0.003(10) 0.042(8) C1 0.068(15) 0.073(15) 0.053(11) 0.009(11) 0.000(11) 0.017(10) N2 0.071(10) 0.071(10) 0.065(15) 0.027(12) -0.027(12) -0.019(12) C2 0.083(17) 0.091(17) 0.066(14) 0.025(12) 0.000(12) -0.035(13) C6 0.068(13) 0.076(13) 0.066(14) 0.012(10) -0.025(11) -0.016(11) C7 0.073(15) 0.071(15) 0.094(17) 0.011(12) 0.008(13) -0.008(11) C3 0.071(17) 0.14(2) 0.083(18) 0.015(17) -0.021(14) -0.034(15) C4 0.085(19) 0.11(2) 0.11(2) 0.005(17) 0.003(17) -0.026(16) C5 0.13(3) 0.13(2) 0.081(19) 0.006(16) 0.039(18) 0.00(2) C9 0.068(16) 0.13(2) 0.18(3) -0.03(2) 0.022(19) 0.011(16) C8 0.065(14) 0.120(19) 0.084(18) -0.012(19) -0.009(16) 0.013(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 S1 2.187(5) . ? W1 S1 2.187(5) 8_444 ? W1 S2 2.234(4) 8_444 ? W1 S2 2.234(4) . ? W1 Cu2 2.650(2) 8_444 ? W1 Cu2 2.650(2) . ? W1 Cu1 2.740(3) . ? Cu1 N1 1.959(14) . ? Cu1 N1 1.959(14) 8_444 ? Cu1 S2 2.333(5) 8_444 ? Cu1 S2 2.333(5) . ? Cu2 C1 1.872(18) 5_534 ? Cu2 S1 2.230(7) . ? Cu2 S2 2.235(6) . ? N1 C1 1.160(19) . ? C1 Cu2 1.872(18) 5_434 ? N2 C2 1.51(2) 6_644 ? N2 C2 1.51(2) . ? N2 C6 1.53(2) . ? N2 C6 1.53(2) 6_644 ? C2 C3 1.47(3) . ? C2 H1A 0.9700 . ? C2 H1B 0.9700 . ? C6 C7 1.51(3) . ? C6 H3A 0.9700 . ? C6 H3B 0.9700 . ? C7 C8 1.53(3) . ? C7 H4A 0.9700 . ? C7 H4B 0.9700 . ? C3 C4 1.57(3) . ? C3 H6B 0.9700 . ? C3 H6C 0.9700 . ? C4 C5 1.43(3) . ? C4 H7A 0.9700 . ? C4 H7B 0.9700 . ? C5 H8A 0.9600 . ? C5 H8B 0.9600 . ? C5 H8C 0.9600 . ? C9 C8 1.54(3) . ? C9 H5A 0.9600 . ? C9 H5B 0.9600 . ? C9 H5C 0.9600 . ? C8 H2A 0.9700 . ? C8 H2B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 W1 S1 110.1(3) . 8_444 ? S1 W1 S2 111.1(2) . 8_444 ? S1 W1 S2 107.5(2) 8_444 8_444 ? S1 W1 S2 107.5(2) . . ? S1 W1 S2 111.1(2) 8_444 . ? S2 W1 S2 109.6(2) 8_444 . ? S1 W1 Cu2 127.80(18) . 8_444 ? S1 W1 Cu2 53.88(17) 8_444 8_444 ? S2 W1 Cu2 53.65(15) 8_444 8_444 ? S2 W1 Cu2 124.70(15) . 8_444 ? S1 W1 Cu2 53.88(17) . . ? S1 W1 Cu2 127.80(18) 8_444 . ? S2 W1 Cu2 124.70(15) 8_444 . ? S2 W1 Cu2 53.65(15) . . ? Cu2 W1 Cu2 177.67(13) 8_444 . ? S1 W1 Cu1 124.93(15) . . ? S1 W1 Cu1 124.93(15) 8_444 . ? S2 W1 Cu1 54.81(12) 8_444 . ? S2 W1 Cu1 54.81(12) . . ? Cu2 W1 Cu1 88.83(6) 8_444 . ? Cu2 W1 Cu1 88.83(6) . . ? N1 Cu1 N1 113.0(8) . 8_444 ? N1 Cu1 S2 108.3(6) . 8_444 ? N1 Cu1 S2 111.9(6) 8_444 8_444 ? N1 Cu1 S2 111.9(6) . . ? N1 Cu1 S2 108.3(6) 8_444 . ? S2 Cu1 S2 103.0(2) 8_444 . ? N1 Cu1 W1 123.5(4) . . ? N1 Cu1 W1 123.5(4) 8_444 . ? S2 Cu1 W1 51.49(12) 8_444 . ? S2 Cu1 W1 51.49(12) . . ? C1 Cu2 S1 121.9(7) 5_534 . ? C1 Cu2 S2 132.0(7) 5_534 . ? S1 Cu2 S2 106.01(19) . . ? C1 Cu2 W1 174.3(7) 5_534 . ? S1 Cu2 W1 52.41(13) . . ? S2 Cu2 W1 53.62(13) . . ? W1 S1 Cu2 73.72(17) . . ? W1 S2 Cu2 72.73(15) . . ? W1 S2 Cu1 73.70(15) . . ? Cu2 S2 Cu1 111.3(2) . . ? C1 N1 Cu1 177(2) . . ? N1 C1 Cu2 174.2(17) . 5_434 ? C2 N2 C2 110(2) 6_644 . ? C2 N2 C6 110.7(12) 6_644 . ? C2 N2 C6 107.0(11) . . ? C2 N2 C6 107.0(11) 6_644 6_644 ? C2 N2 C6 110.7(12) . 6_644 ? C6 N2 C6 111.3(19) . 6_644 ? C3 C2 N2 120.1(18) . . ? C3 C2 H1A 107.3 . . ? N2 C2 H1A 107.3 . . ? C3 C2 H1B 107.3 . . ? N2 C2 H1B 107.3 . . ? H1A C2 H1B 106.9 . . ? C7 C6 N2 116.7(15) . . ? C7 C6 H3A 108.1 . . ? N2 C6 H3A 108.1 . . ? C7 C6 H3B 108.1 . . ? N2 C6 H3B 108.1 . . ? H3A C6 H3B 107.3 . . ? C6 C7 C8 106.3(19) . . ? C6 C7 H4A 110.5 . . ? C8 C7 H4A 110.5 . . ? C6 C7 H4B 110.5 . . ? C8 C7 H4B 110.5 . . ? H4A C7 H4B 108.7 . . ? C2 C3 C4 111(2) . . ? C2 C3 H6B 109.4 . . ? C4 C3 H6B 109.4 . . ? C2 C3 H6C 109.4 . . ? C4 C3 H6C 109.4 . . ? H6B C3 H6C 108.0 . . ? C5 C4 C3 116(2) . . ? C5 C4 H7A 108.3 . . ? C3 C4 H7A 108.3 . . ? C5 C4 H7B 108.3 . . ? C3 C4 H7B 108.3 . . ? H7A C4 H7B 107.4 . . ? C4 C5 H8A 109.5 . . ? C4 C5 H8B 109.5 . . ? H8A C5 H8B 109.5 . . ? C4 C5 H8C 109.5 . . ? H8A C5 H8C 109.5 . . ? H8B C5 H8C 109.5 . . ? C8 C9 H5A 109.5 . . ? C8 C9 H5B 109.5 . . ? H5A C9 H5B 109.5 . . ? C8 C9 H5C 109.5 . . ? H5A C9 H5C 109.5 . . ? H5B C9 H5C 109.5 . . ? C7 C8 C9 109(2) . . ? C7 C8 H2A 109.9 . . ? C9 C8 H2A 109.9 . . ? C7 C8 H2B 109.9 . . ? C9 C8 H2B 109.9 . . ? H2A C8 H2B 108.3 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.154 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.156