# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Jian-Ping Lang' 'Hong-Xi Li' 'Zhi-Gang Ren' 'Zhen-Rong Sun' ; Zhen-Hong Wei ; 'Yong Zhang' _publ_contact_author_name 'Jian-Ping Lang' _publ_contact_author_email JPLANG@SUDA.EDU.CN # Attachment 'JPLangCIF.cif' data_[Et4N][Tp*WS3(CuNCS)].0.5CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 714218' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C16 H22 B Cu N7 S4 W), 2(C8 H20 N), C H2 Cl2' _chemical_formula_sum 'C49 H86 B2 Cl2 Cu2 N16 S8 W2' _chemical_formula_weight 1743.20 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.336(2) _cell_length_b 23.747(5) _cell_length_c 14.945(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.92(3) _cell_angle_gamma 90.00 _cell_volume 3667.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12026 _cell_measurement_theta_min 3.2232 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 4.041 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1953 _exptl_absorpt_correction_T_max 0.4987 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35014 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6673 _reflns_number_gt 5640 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Shelxl-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _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^)+(0.0649P)^2^+20.2976P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6673 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1624 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _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 1.08641(3) 0.804905(15) 0.51919(2) 0.04037(16) Uani 1 1 d . . . Cu1 Cu 1.17882(13) 0.70570(5) 0.55445(10) 0.0567(3) Uani 1 1 d . . . S1 S 1.2110(3) 0.83575(12) 0.41600(19) 0.0574(7) Uani 1 1 d . . . S2 S 1.0167(3) 0.72121(11) 0.46232(19) 0.0561(7) Uani 1 1 d . . . S3 S 1.2333(3) 0.78241(11) 0.62749(18) 0.0535(6) Uani 1 1 d . . . S4 S 1.3501(4) 0.53359(14) 0.6390(3) 0.0922(11) Uani 1 1 d . . . C1 C 0.8866(12) 1.0141(5) 0.6509(9) 0.080(4) Uani 1 1 d . . . H1A H 0.8278 1.0191 0.6011 0.120 Uiso 1 1 calc R . . H1B H 0.9259 1.0496 0.6659 0.120 Uiso 1 1 calc R . . H1C H 0.8402 1.0001 0.7014 0.120 Uiso 1 1 calc R . . C2 C 0.9916(10) 0.9720(4) 0.6256(7) 0.049(2) Uani 1 1 d . . . C3 C 1.1227(11) 0.9788(4) 0.6266(7) 0.059(3) Uani 1 1 d . . . H3 H 1.1683 1.0109 0.6439 0.071 Uiso 1 1 calc R . . C4 C 1.1739(10) 0.9288(4) 0.5971(6) 0.050(2) Uani 1 1 d . . . C5 C 1.3133(9) 0.9189(5) 0.5840(8) 0.063(3) Uani 1 1 d . . . H5A H 1.3353 0.8815 0.6034 0.095 Uiso 1 1 calc R . . H5B H 1.3624 0.9458 0.6184 0.095 Uiso 1 1 calc R . . H5C H 1.3328 0.9230 0.5218 0.095 Uiso 1 1 calc R . . C6 C 0.6329(10) 0.8557(6) 0.7314(9) 0.075(4) Uani 1 1 d . . . H6A H 0.5931 0.8395 0.7830 0.113 Uiso 1 1 calc R . . H6B H 0.5716 0.8564 0.6824 0.113 Uiso 1 1 calc R . . H6C H 0.6604 0.8934 0.7450 0.113 Uiso 1 1 calc R . . C7 C 0.7483(10) 0.8208(5) 0.7060(7) 0.056(3) Uani 1 1 d . . . C8 C 0.7869(10) 0.7702(5) 0.7386(7) 0.060(3) Uani 1 1 d . . . H8 H 0.7475 0.7496 0.7836 0.071 Uiso 1 1 calc R . . C9 C 0.8952(10) 0.7551(4) 0.6927(7) 0.055(3) Uani 1 1 d . . . C10 C 0.9731(12) 0.7021(5) 0.7077(9) 0.071(3) Uani 1 1 d . . . H10A H 0.9737 0.6804 0.6536 0.106 Uiso 1 1 calc R . . H10B H 0.9349 0.6803 0.7545 0.106 Uiso 1 1 calc R . . H10C H 1.0602 0.7119 0.7247 0.106 Uiso 1 1 calc R . . C11 C 0.6063(10) 0.9194(6) 0.4523(9) 0.074(4) Uani 1 1 d . . . H11A H 0.5627 0.8999 0.4994 0.111 Uiso 1 1 calc R . . H11B H 0.5493 0.9227 0.4012 0.111 Uiso 1 1 calc R . . H11C H 0.6310 0.9562 0.4726 0.111 Uiso 1 1 calc R . . C12 C 0.7233(9) 0.8874(5) 0.4271(7) 0.054(3) Uani 1 1 d . . . C13 C 0.7549(9) 0.8651(5) 0.3454(7) 0.055(3) Uani 1 1 d . . . H13 H 0.7078 0.8683 0.2921 0.066 Uiso 1 1 calc R . . C14 C 0.8724(9) 0.8367(4) 0.3588(6) 0.051(2) Uani 1 1 d . . . C16 C 1.2878(11) 0.5927(5) 0.6052(7) 0.058(3) Uani 1 1 d . . . C17 C 0.6491(17) 0.6425(9) 0.6114(9) 0.123(7) Uani 1 1 d . . . H17A H 0.5995 0.6746 0.6294 0.184 Uiso 1 1 calc R . . H17B H 0.7177 0.6359 0.6541 0.184 Uiso 1 1 calc R . . H17C H 0.5940 0.6099 0.6083 0.184 Uiso 1 1 calc R . . C18 C 0.5645(19) 0.7612(7) 0.4880(15) 0.137(7) Uani 1 1 d . . . H18A H 0.6179 0.7577 0.5408 0.205 Uiso 1 1 calc R . . H18B H 0.4938 0.7862 0.4996 0.205 Uiso 1 1 calc R . . H18C H 0.6149 0.7760 0.4400 0.205 Uiso 1 1 calc R . . C19 C 0.4512(17) 0.5993(7) 0.3559(11) 0.121(6) Uani 1 1 d . . . H19A H 0.3727 0.6188 0.3697 0.181 Uiso 1 1 calc R . . H19B H 0.4321 0.5605 0.3432 0.181 Uiso 1 1 calc R . . H19C H 0.4899 0.6163 0.3045 0.181 Uiso 1 1 calc R . . C20 C 0.7769(15) 0.6291(7) 0.3320(10) 0.101(5) Uani 1 1 d . . . H20A H 0.8367 0.6193 0.3793 0.152 Uiso 1 1 calc R . . H20B H 0.8238 0.6421 0.2811 0.152 Uiso 1 1 calc R . . H20C H 0.7268 0.5965 0.3154 0.152 Uiso 1 1 calc R . . C21 C 0.7038(13) 0.6530(7) 0.5236(9) 0.093(5) Uani 1 1 d . . . H21A H 0.7632 0.6225 0.5106 0.112 Uiso 1 1 calc R . . H21B H 0.7544 0.6873 0.5273 0.112 Uiso 1 1 calc R . . C22 C 0.5426(14) 0.6028(6) 0.4336(9) 0.086(4) Uani 1 1 d . . . H22A H 0.6079 0.5738 0.4273 0.104 Uiso 1 1 calc R . . H22B H 0.4954 0.5947 0.4877 0.104 Uiso 1 1 calc R . . C23 C 0.6871(15) 0.6753(7) 0.3638(10) 0.094(4) Uani 1 1 d . . . H23A H 0.7382 0.7084 0.3787 0.113 Uiso 1 1 calc R . . H23B H 0.6281 0.6854 0.3153 0.113 Uiso 1 1 calc R . . C24 C 0.5118(15) 0.7036(6) 0.4617(12) 0.095(5) Uani 1 1 d . . . H24A H 0.4557 0.6908 0.5090 0.113 Uiso 1 1 calc R . . H24B H 0.4585 0.7081 0.4082 0.113 Uiso 1 1 calc R . . C25 C 1.034(4) 0.470(2) 0.332(4) 0.22(4) Uani 0.50 1 d P . . H25A H 1.0349 0.4363 0.3694 0.262 Uiso 0.50 1 calc PR A 1 H25B H 0.9434 0.4777 0.3195 0.262 Uiso 0.50 1 calc PR A 1 N1 N 0.9648(7) 0.9186(3) 0.5974(5) 0.0437(18) Uani 1 1 d . . . N2 N 1.0780(7) 0.8920(3) 0.5781(5) 0.0429(18) Uani 1 1 d . . . N3 N 0.8313(7) 0.8362(3) 0.6410(5) 0.0431(18) Uani 1 1 d . . . N4 N 0.9249(7) 0.7955(3) 0.6317(5) 0.0431(18) Uani 1 1 d . . . N5 N 0.8168(7) 0.8736(3) 0.4859(5) 0.0432(18) Uani 1 1 d . . . N6 N 0.9121(7) 0.8419(3) 0.4452(5) 0.0438(18) Uani 1 1 d . . . N7 N 1.2495(9) 0.6351(4) 0.5823(7) 0.064(2) Uani 1 1 d . . . N8 N 0.6091(9) 0.6585(4) 0.4446(6) 0.059(2) Uani 1 1 d . . . B1 B 0.8336(10) 0.8898(5) 0.5839(7) 0.044(2) Uani 1 1 d . . . H1 H 0.7639 0.9153 0.6016 0.053 Uiso 1 1 calc R . . Cl2 Cl 1.0765(19) 0.4544(9) 0.2616(12) 0.063(5) Uiso 0.197(11) 1 d P B 1 Cl2A Cl 1.0405(16) 0.4768(8) 0.2554(11) 0.094(4) Uiso 0.303(11) 1 d P B 2 Cl1 Cl 1.0987(17) 0.5352(8) 0.4150(11) 0.074(6) Uiso 0.197(11) 1 d P B 1 Cl1A Cl 1.1500(10) 0.5019(5) 0.4241(7) 0.068(4) Uiso 0.303(11) 1 d P B 2 C15 C 0.9468(13) 0.8063(6) 0.2872(8) 0.078(4) Uani 1 1 d . . . H15A H 1.0269 0.8255 0.2772 0.117 Uiso 1 1 calc R . . H15B H 0.8964 0.8056 0.2327 0.117 Uiso 1 1 calc R . . H15C H 0.9642 0.7684 0.3063 0.117 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 0.0362(2) 0.0398(2) 0.0450(2) -0.00314(16) -0.00084(16) 0.00484(15) Cu1 0.0521(8) 0.0455(7) 0.0724(9) 0.0004(6) -0.0013(6) 0.0092(6) S1 0.0545(16) 0.0583(16) 0.0598(16) -0.0037(13) 0.0085(13) 0.0020(13) S2 0.0501(15) 0.0499(15) 0.0681(17) -0.0123(13) -0.0062(13) -0.0001(12) S3 0.0489(14) 0.0506(14) 0.0604(16) 0.0013(12) -0.0137(12) 0.0067(11) S4 0.111(3) 0.0479(18) 0.118(3) 0.0223(19) -0.007(2) 0.0143(18) C1 0.084(9) 0.054(7) 0.101(10) -0.013(7) 0.015(8) 0.018(6) C2 0.057(6) 0.036(5) 0.054(6) 0.003(4) -0.003(5) -0.001(4) C3 0.077(8) 0.044(6) 0.057(6) -0.010(5) 0.005(6) -0.007(5) C4 0.058(6) 0.045(6) 0.047(5) 0.002(4) 0.004(5) -0.009(5) C5 0.045(6) 0.059(7) 0.085(8) -0.003(6) 0.001(6) -0.004(5) C6 0.046(6) 0.091(9) 0.090(9) 0.013(7) 0.031(6) 0.014(6) C7 0.043(6) 0.068(7) 0.056(6) 0.004(5) 0.007(5) -0.007(5) C8 0.059(7) 0.065(7) 0.055(6) 0.018(6) 0.012(5) -0.007(6) C9 0.061(6) 0.048(6) 0.054(6) 0.010(5) 0.001(5) 0.005(5) C10 0.067(8) 0.059(7) 0.088(9) 0.033(6) 0.007(6) 0.016(6) C11 0.040(6) 0.092(9) 0.091(9) 0.029(7) -0.008(6) 0.016(6) C12 0.034(5) 0.070(7) 0.058(6) 0.010(5) -0.006(5) 0.000(5) C13 0.044(6) 0.068(7) 0.052(6) 0.022(5) -0.011(5) -0.013(5) C14 0.045(6) 0.063(7) 0.044(5) -0.004(5) -0.004(4) 0.001(5) C16 0.065(7) 0.050(7) 0.059(6) -0.009(5) 0.003(5) -0.011(5) C17 0.124(14) 0.185(19) 0.060(8) -0.011(10) 0.005(9) -0.039(13) C18 0.151(17) 0.073(11) 0.187(19) -0.034(12) 0.035(15) -0.019(11) C19 0.144(15) 0.098(12) 0.118(13) -0.022(10) -0.065(12) -0.020(11) C20 0.105(12) 0.116(13) 0.083(10) -0.015(9) 0.032(9) -0.001(10) C21 0.074(9) 0.132(13) 0.075(9) -0.001(9) 0.005(7) -0.024(9) C22 0.095(10) 0.081(9) 0.084(9) -0.008(7) 0.007(8) -0.010(8) C23 0.095(11) 0.103(11) 0.085(10) 0.026(9) 0.023(8) -0.014(9) C24 0.092(11) 0.079(10) 0.114(12) -0.013(8) 0.028(9) 0.005(8) C25 0.08(3) 0.18(5) 0.39(9) 0.18(6) -0.12(4) -0.08(3) N1 0.049(5) 0.038(4) 0.044(4) 0.000(3) 0.008(4) 0.010(3) N2 0.043(4) 0.034(4) 0.053(5) 0.005(3) 0.009(4) 0.004(3) N3 0.036(4) 0.040(4) 0.054(5) 0.005(4) 0.006(4) 0.003(3) N4 0.038(4) 0.043(4) 0.048(4) 0.001(4) -0.002(3) 0.010(3) N5 0.038(4) 0.045(4) 0.046(4) 0.009(4) -0.001(3) 0.001(3) N6 0.039(4) 0.055(5) 0.037(4) -0.002(4) -0.004(3) 0.007(4) N7 0.066(6) 0.042(5) 0.084(7) 0.007(5) -0.003(5) 0.011(4) N8 0.057(5) 0.059(6) 0.061(5) 0.004(4) 0.004(4) -0.016(4) B1 0.038(6) 0.044(6) 0.050(6) -0.001(5) 0.010(5) 0.010(5) C15 0.077(9) 0.105(11) 0.052(7) -0.016(7) -0.010(6) 0.004(7) _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 2.154(3) . ? W1 N2 2.250(7) . ? W1 S3 2.265(3) . ? W1 S2 2.274(3) . ? W1 N6 2.275(7) . ? W1 N4 2.398(8) . ? W1 Cu1 2.5930(13) . ? Cu1 N7 1.872(9) . ? Cu1 S2 2.183(3) . ? Cu1 S3 2.192(3) . ? S4 C16 1.622(12) . ? C1 C2 1.528(14) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.363(12) . ? C2 C3 1.365(14) . ? C3 C4 1.378(14) . ? C3 H3 0.9300 . ? C4 N2 1.348(12) . ? C4 C5 1.475(14) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.506(15) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N3 1.356(12) . ? C7 C8 1.355(15) . ? C8 C9 1.369(15) . ? C8 H8 0.9300 . ? C9 N4 1.361(12) . ? C9 C10 1.510(14) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.482(14) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N5 1.336(12) . ? C12 C13 1.375(15) . ? C13 C14 1.400(14) . ? C13 H13 0.9300 . ? C14 N6 1.355(12) . ? C14 C15 1.511(15) . ? C16 N7 1.134(13) . ? C17 C21 1.458(18) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C24 1.52(2) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C22 1.487(18) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C23 1.52(2) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N8 1.527(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N8 1.500(15) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N8 1.515(15) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 N8 1.494(16) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 Cl2A 1.16(6) . ? C25 Cl2 1.20(7) . ? C25 Cl1A 1.97(5) . ? C25 Cl1 2.10(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? N1 N2 1.365(10) . ? N1 B1 1.528(13) . ? N3 N4 1.378(10) . ? N3 B1 1.534(13) . ? N5 N6 1.388(10) . ? N5 B1 1.521(13) . ? B1 H1 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 N2 89.7(2) . . ? S1 W1 S3 100.96(11) . . ? N2 W1 S3 88.1(2) . . ? S1 W1 S2 102.66(11) . . ? N2 W1 S2 159.3(2) . . ? S3 W1 S2 105.40(10) . . ? S1 W1 N6 89.9(2) . . ? N2 W1 N6 78.5(3) . . ? S3 W1 N6 162.7(2) . . ? S2 W1 N6 84.9(2) . . ? S1 W1 N4 164.73(19) . . ? N2 W1 N4 77.3(3) . . ? S3 W1 N4 86.73(19) . . ? S2 W1 N4 87.7(2) . . ? N6 W1 N4 79.7(3) . . ? S1 W1 Cu1 103.41(8) . . ? N2 W1 Cu1 140.5(2) . . ? S3 W1 Cu1 53.13(8) . . ? S2 W1 Cu1 52.79(8) . . ? N6 W1 Cu1 137.4(2) . . ? N4 W1 Cu1 91.77(17) . . ? N7 Cu1 S2 125.7(3) . . ? N7 Cu1 S3 122.5(3) . . ? S2 Cu1 S3 111.24(11) . . ? N7 Cu1 W1 178.2(3) . . ? S2 Cu1 W1 56.08(8) . . ? S3 Cu1 W1 55.75(7) . . ? Cu1 S2 W1 71.12(8) . . ? Cu1 S3 W1 71.12(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.2(9) . . ? N1 C2 C1 123.0(9) . . ? C3 C2 C1 128.9(10) . . ? C2 C3 C4 106.3(9) . . ? C2 C3 H3 126.9 . . ? C4 C3 H3 126.9 . . ? N2 C4 C3 109.9(9) . . ? N2 C4 C5 125.9(9) . . ? C3 C4 C5 124.1(10) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 108.1(9) . . ? N3 C7 C6 123.0(10) . . ? C8 C7 C6 128.8(10) . . ? C7 C8 C9 106.8(9) . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? N4 C9 C8 110.4(9) . . ? N4 C9 C10 124.1(9) . . ? C8 C9 C10 125.5(10) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 108.1(9) . . ? N5 C12 C11 122.9(10) . . ? C13 C12 C11 128.9(10) . . ? C12 C13 C14 106.0(9) . . ? C12 C13 H13 127.0 . . ? C14 C13 H13 127.0 . . ? N6 C14 C13 110.0(9) . . ? N6 C14 C15 124.6(9) . . ? C13 C14 C15 125.4(9) . . ? N7 C16 S4 176.9(11) . . ? C21 C17 H17A 109.5 . . ? C21 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C21 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C24 C18 H18A 109.5 . . ? C24 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C24 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 C19 H19A 109.5 . . ? C22 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C22 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 H20A 109.5 . . ? C23 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C23 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 N8 117.2(12) . . ? C17 C21 H21A 108.0 . . ? N8 C21 H21A 108.0 . . ? C17 C21 H21B 108.0 . . ? N8 C21 H21B 108.0 . . ? H21A C21 H21B 107.2 . . ? C19 C22 N8 114.8(12) . . ? C19 C22 H22A 108.6 . . ? N8 C22 H22A 108.6 . . ? C19 C22 H22B 108.6 . . ? N8 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? N8 C23 C20 113.3(12) . . ? N8 C23 H23A 108.9 . . ? C20 C23 H23A 108.9 . . ? N8 C23 H23B 108.9 . . ? C20 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N8 C24 C18 116.7(13) . . ? N8 C24 H24A 108.1 . . ? C18 C24 H24A 108.1 . . ? N8 C24 H24B 108.1 . . ? C18 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? Cl2A C25 Cl2 32(2) . . ? Cl2A C25 Cl1A 126(2) . . ? Cl2 C25 Cl1A 120(3) . . ? Cl2A C25 Cl1 117(3) . . ? Cl2 C25 Cl1 129(3) . . ? Cl1A C25 Cl1 27.1(9) . . ? Cl2A C25 H25A 133.9 . . ? Cl2 C25 H25A 105.1 . . ? Cl1A C25 H25A 84.9 . . ? Cl1 C25 H25A 105.1 . . ? Cl2A C25 H25B 81.7 . . ? Cl2 C25 H25B 105.1 . . ? Cl1A C25 H25B 129.0 . . ? Cl1 C25 H25B 105.1 . . ? H25A C25 H25B 105.9 . . ? C2 N1 N2 109.0(8) . . ? C2 N1 B1 129.2(8) . . ? N2 N1 B1 121.8(7) . . ? C4 N2 N1 106.6(8) . . ? C4 N2 W1 130.1(6) . . ? N1 N2 W1 123.1(6) . . ? C7 N3 N4 109.7(8) . . ? C7 N3 B1 129.7(8) . . ? N4 N3 B1 120.6(7) . . ? C9 N4 N3 105.0(8) . . ? C9 N4 W1 134.7(6) . . ? N3 N4 W1 120.2(5) . . ? C12 N5 N6 110.8(8) . . ? C12 N5 B1 129.9(8) . . ? N6 N5 B1 119.2(7) . . ? C14 N6 N5 105.1(7) . . ? C14 N6 W1 130.9(6) . . ? N5 N6 W1 123.9(5) . . ? C16 N7 Cu1 174.8(10) . . ? C24 N8 C22 110.0(10) . . ? C24 N8 C23 108.5(10) . . ? C22 N8 C23 113.2(10) . . ? C24 N8 C21 110.8(11) . . ? C22 N8 C21 107.2(10) . . ? C23 N8 C21 107.2(10) . . ? N5 B1 N1 109.2(7) . . ? N5 B1 N3 108.9(8) . . ? N1 B1 N3 108.6(8) . . ? N5 B1 H1 110.1 . . ? N1 B1 H1 110.1 . . ? N3 B1 H1 110.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.435 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.150 #===END data_[Et4N][Tp*W3S3(CuNCS)2].ClCH2CH2Cl _database_code_depnum_ccdc_archive 'CCDC 714219' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H44 B2 Cu4 N16 S10 W2, 2(C8 H20 N), 2(C2 H4 Cl2)' _chemical_formula_sum 'C54 H92 B2 Cl4 Cu4 N18 S10 W2' _chemical_formula_weight 2099.46 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.076(2) _cell_length_b 16.195(3) _cell_length_c 23.192(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.20(3) _cell_angle_gamma 90.00 _cell_volume 4106.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14194 _cell_measurement_theta_min 2.9999 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 4.237 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2820 _exptl_absorpt_correction_T_max 0.3630 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39329 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7492 _reflns_number_gt 6321 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Shelxl-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _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^)+(0.0298P)^2^+14.3626P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7492 _refine_ls_number_parameters 435 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.003 _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 -0.20179(3) 0.404136(17) 0.688986(12) 0.03358(10) Uani 1 1 d . . . Cu2 Cu -0.31048(10) 0.45625(6) 0.58555(4) 0.0563(3) Uani 1 1 d . . . Cu1 Cu -0.36673(9) 0.30263(6) 0.63336(4) 0.0507(3) Uani 1 1 d . . . S1 S -0.27239(19) 0.53019(12) 0.66615(9) 0.0481(5) Uani 1 1 d . . . S2 S -0.19786(18) 0.34038(12) 0.59966(8) 0.0432(5) Uani 1 1 d . . . S3 S -0.35775(18) 0.34435(13) 0.72360(8) 0.0444(5) Uani 1 1 d . . . S5 S -0.4445(2) 0.56642(15) 0.40119(9) 0.0563(6) Uani 1 1 d . . . C1 C 0.3122(8) 0.4688(6) 0.7541(4) 0.069(3) Uani 1 1 d . . . H1A H 0.3124 0.5076 0.7854 0.104 Uiso 1 1 calc R . . H1B H 0.3758 0.4828 0.7322 0.104 Uiso 1 1 calc R . . H1C H 0.3261 0.4142 0.7699 0.104 Uiso 1 1 calc R . . C2 C 0.1903(7) 0.4716(5) 0.7146(4) 0.048(2) Uani 1 1 d . . . C3 C 0.1628(8) 0.5005(5) 0.6593(4) 0.053(2) Uani 1 1 d . . . H3 H 0.2176 0.5235 0.6374 0.064 Uiso 1 1 calc R . . C4 C 0.0388(7) 0.4896(5) 0.6412(3) 0.0460(19) Uani 1 1 d . . . C5 C -0.0282(9) 0.5143(6) 0.5829(4) 0.071(3) Uani 1 1 d . . . H5A H -0.0536 0.4658 0.5604 0.107 Uiso 1 1 calc R . . H5B H 0.0245 0.5469 0.5628 0.107 Uiso 1 1 calc R . . H5C H -0.0988 0.5463 0.5878 0.107 Uiso 1 1 calc R . . C6 C 0.0746(9) 0.4831(6) 0.9123(4) 0.072(3) Uani 1 1 d . . . H6A H 0.0626 0.5197 0.9434 0.108 Uiso 1 1 calc R . . H6B H 0.1440 0.5011 0.8955 0.108 Uiso 1 1 calc R . . H6C H 0.0889 0.4281 0.9273 0.108 Uiso 1 1 calc R . . C7 C -0.0366(7) 0.4836(5) 0.8664(3) 0.048(2) Uani 1 1 d . . . C8 C -0.1499(8) 0.5127(5) 0.8682(3) 0.051(2) Uani 1 1 d . . . H8 H -0.1756 0.5395 0.8996 0.061 Uiso 1 1 calc R . . C9 C -0.2215(7) 0.4955(5) 0.8148(4) 0.049(2) Uani 1 1 d . . . C10 C -0.3530(8) 0.5194(6) 0.7979(4) 0.063(3) Uani 1 1 d . . . H10A H -0.3954 0.4770 0.7737 0.095 Uiso 1 1 calc R . . H10B H -0.3582 0.5705 0.7767 0.095 Uiso 1 1 calc R . . H10C H -0.3896 0.5260 0.8324 0.095 Uiso 1 1 calc R . . C11 C 0.1823(9) 0.2427(6) 0.8437(4) 0.075(3) Uani 1 1 d . . . H11A H 0.2535 0.2619 0.8290 0.112 Uiso 1 1 calc R . . H11B H 0.1956 0.1870 0.8576 0.112 Uiso 1 1 calc R . . H11C H 0.1672 0.2775 0.8753 0.112 Uiso 1 1 calc R . . C12 C 0.0740(7) 0.2450(5) 0.7958(4) 0.052(2) Uani 1 1 d . . . C13 C 0.0096(8) 0.1817(5) 0.7680(4) 0.054(2) Uani 1 1 d . . . H13 H 0.0255 0.1258 0.7744 0.064 Uiso 1 1 calc R . . C14 C -0.0841(7) 0.2153(5) 0.7285(3) 0.0467(19) Uani 1 1 d . . . C15 C -0.1762(9) 0.1668(5) 0.6879(4) 0.066(3) Uani 1 1 d . . . H15A H -0.2565 0.1773 0.6969 0.100 Uiso 1 1 calc R . . H15B H -0.1581 0.1089 0.6925 0.100 Uiso 1 1 calc R . . H15C H -0.1732 0.1829 0.6483 0.100 Uiso 1 1 calc R . . C16 C -0.5098(9) 0.1567(6) 0.5801(4) 0.068(3) Uani 1 1 d . . . C17 C -0.3865(7) 0.5303(5) 0.4650(3) 0.0447(19) Uani 1 1 d . . . C24 C -0.8393(10) 0.7343(9) 0.1203(5) 0.106(4) Uani 1 1 d . . . H24A H -0.8458 0.6774 0.1086 0.159 Uiso 1 1 calc R . . H24B H -0.9195 0.7582 0.1163 0.159 Uiso 1 1 calc R . . H24C H -0.8006 0.7379 0.1604 0.159 Uiso 1 1 calc R . . C25 C -0.7638(9) 0.7806(6) 0.0822(4) 0.074(3) Uani 1 1 d . . . H25A H -0.8064 0.7799 0.0422 0.088 Uiso 1 1 calc R . . H25B H -0.7564 0.8377 0.0948 0.088 Uiso 1 1 calc R . . C18 C -0.5530(11) 0.8281(7) 0.1748(4) 0.096(4) Uani 1 1 d . . . H18A H -0.5155 0.8663 0.1514 0.144 Uiso 1 1 calc R . . H18B H -0.5027 0.8223 0.2123 0.144 Uiso 1 1 calc R . . H18C H -0.6322 0.8484 0.1797 0.144 Uiso 1 1 calc R . . C20 C -0.4394(9) 0.7836(8) 0.0448(4) 0.089(4) Uani 1 1 d . . . H20A H -0.3951 0.7989 0.0823 0.133 Uiso 1 1 calc R . . H20B H -0.4110 0.8160 0.0150 0.133 Uiso 1 1 calc R . . H20C H -0.4263 0.7261 0.0378 0.133 Uiso 1 1 calc R . . C22 C -0.7278(9) 0.6402(6) 0.0054(4) 0.074(3) Uani 1 1 d . . . H22A H -0.8101 0.6556 0.0088 0.111 Uiso 1 1 calc R . . H22B H -0.7252 0.5824 -0.0035 0.111 Uiso 1 1 calc R . . H22C H -0.7011 0.6716 -0.0253 0.111 Uiso 1 1 calc R . . C23 C -0.6442(8) 0.6575(5) 0.0627(4) 0.058(2) Uani 1 1 d . . . H23A H -0.6707 0.6235 0.0928 0.070 Uiso 1 1 calc R . . H23B H -0.5622 0.6398 0.0587 0.070 Uiso 1 1 calc R . . C21 C -0.5753(9) 0.7992(6) 0.0437(4) 0.064(3) Uani 1 1 d . . . H21A H -0.5860 0.8564 0.0541 0.077 Uiso 1 1 calc R . . H21B H -0.6168 0.7916 0.0039 0.077 Uiso 1 1 calc R . . C19 C -0.5668(9) 0.7453(6) 0.1448(4) 0.064(2) Uani 1 1 d . . . H19A H -0.6071 0.7081 0.1684 0.076 Uiso 1 1 calc R . . H19B H -0.4858 0.7233 0.1436 0.076 Uiso 1 1 calc R . . N1 N 0.0852(5) 0.4449(4) 0.7306(3) 0.0403(15) Uani 1 1 d . . . N2 N -0.0105(5) 0.4535(4) 0.6846(3) 0.0391(14) Uani 1 1 d . . . N3 N -0.0384(5) 0.4496(4) 0.8126(3) 0.0405(15) Uani 1 1 d . . . N4 N -0.1527(6) 0.4572(4) 0.7804(2) 0.0406(15) Uani 1 1 d . . . N5 N 0.0214(5) 0.3155(4) 0.7741(3) 0.0406(15) Uani 1 1 d . . . N6 N -0.0762(5) 0.2986(3) 0.7322(2) 0.0360(14) Uani 1 1 d . . . N8 N -0.4629(6) 0.2137(5) 0.6010(3) 0.0574(19) Uani 1 1 d . . . N7 N -0.3442(6) 0.5041(5) 0.5098(3) 0.0567(19) Uani 1 1 d . . . N9 N -0.6374(6) 0.7451(4) 0.0835(3) 0.0470(16) Uani 1 1 d . . . B1 B 0.0623(8) 0.4043(5) 0.7872(4) 0.042(2) Uani 1 1 d . . . H1 H 0.1379 0.4047 0.8157 0.050 Uiso 1 1 calc R . . S4 S -0.5824(4) 0.0777(2) 0.54674(17) 0.1411(19) Uani 1 1 d . . . Cl2 Cl -1.2793(5) 0.7565(3) -0.19156(19) 0.1432(15) Uani 1 1 d . . . Cl1 Cl -1.0741(5) 0.7559(5) -0.0208(3) 0.236(3) Uani 1 1 d . . . C26 C -1.1469(17) 0.7561(13) -0.1311(11) 0.224(13) Uani 1 1 d D . . H26A H -1.1005 0.7052 -0.1307 0.268 Uiso 1 1 calc R . . H26B H -1.0931 0.8026 -0.1341 0.268 Uiso 1 1 calc R . . C27 C -1.1995(18) 0.7620(15) -0.0856(10) 0.232(13) Uani 1 1 d D . . H27A H -1.2575 0.7173 -0.0846 0.278 Uiso 1 1 calc R . . H27B H -1.2428 0.8141 -0.0857 0.278 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 0.03509(17) 0.03157(16) 0.03154(16) -0.00003(13) -0.00241(11) -0.00004(13) Cu2 0.0730(8) 0.0510(6) 0.0394(5) 0.0089(5) -0.0082(5) 0.0025(5) Cu1 0.0528(6) 0.0547(6) 0.0438(6) -0.0098(5) 0.0053(5) -0.0172(5) S1 0.0506(13) 0.0355(10) 0.0540(12) 0.0020(9) -0.0047(10) 0.0046(9) S2 0.0473(12) 0.0448(11) 0.0366(10) -0.0026(9) 0.0042(9) -0.0038(9) S3 0.0451(12) 0.0503(12) 0.0370(10) 0.0006(9) 0.0043(9) -0.0049(9) S5 0.0469(13) 0.0775(16) 0.0423(11) 0.0165(11) 0.0002(9) 0.0047(11) C1 0.038(5) 0.079(7) 0.091(7) 0.003(6) 0.009(5) -0.013(5) C2 0.030(4) 0.041(4) 0.073(6) -0.002(4) 0.003(4) 0.000(3) C3 0.045(5) 0.048(5) 0.067(6) 0.006(4) 0.015(4) -0.005(4) C4 0.040(5) 0.045(5) 0.053(5) 0.002(4) 0.009(4) -0.005(4) C5 0.068(7) 0.089(7) 0.056(6) 0.021(5) 0.008(5) -0.016(6) C6 0.069(7) 0.090(7) 0.047(5) -0.015(5) -0.017(5) -0.001(6) C7 0.046(5) 0.051(5) 0.042(5) -0.011(4) -0.006(4) -0.001(4) C8 0.059(6) 0.053(5) 0.036(4) -0.014(4) -0.007(4) 0.002(4) C9 0.044(5) 0.048(5) 0.053(5) -0.011(4) 0.004(4) 0.011(4) C10 0.059(6) 0.074(6) 0.056(5) -0.019(5) 0.007(4) 0.019(5) C11 0.070(7) 0.062(6) 0.082(7) 0.006(5) -0.015(5) 0.011(5) C12 0.045(5) 0.047(5) 0.059(5) 0.009(4) -0.006(4) 0.013(4) C13 0.057(6) 0.040(5) 0.064(6) 0.013(4) 0.010(4) 0.011(4) C14 0.051(5) 0.032(4) 0.056(5) 0.004(4) 0.005(4) 0.004(4) C15 0.086(7) 0.035(5) 0.072(6) -0.001(4) -0.007(5) -0.001(5) C16 0.085(7) 0.070(6) 0.058(6) -0.025(5) 0.036(5) -0.024(6) C17 0.040(5) 0.048(5) 0.045(5) 0.007(4) 0.003(4) -0.009(4) C24 0.075(8) 0.150(12) 0.101(9) -0.012(9) 0.041(7) -0.008(8) C25 0.068(7) 0.078(7) 0.072(7) -0.008(6) 0.001(5) 0.010(6) C18 0.125(10) 0.087(8) 0.068(7) -0.022(6) -0.010(7) -0.031(7) C20 0.070(7) 0.127(10) 0.070(7) 0.023(7) 0.017(5) -0.037(7) C22 0.070(7) 0.084(7) 0.064(6) -0.025(6) -0.002(5) -0.010(6) C23 0.071(6) 0.047(5) 0.058(5) 0.001(4) 0.011(5) -0.002(5) C21 0.075(7) 0.067(6) 0.048(5) 0.016(5) 0.002(5) -0.013(5) C19 0.068(6) 0.074(6) 0.045(5) 0.010(5) -0.002(4) -0.011(5) N1 0.031(4) 0.038(3) 0.051(4) -0.004(3) 0.004(3) 0.003(3) N2 0.028(3) 0.041(4) 0.047(4) 0.006(3) 0.001(3) -0.008(3) N3 0.034(4) 0.045(4) 0.040(4) -0.006(3) -0.003(3) 0.000(3) N4 0.045(4) 0.041(4) 0.035(3) -0.009(3) 0.003(3) 0.002(3) N5 0.037(4) 0.042(4) 0.038(3) -0.001(3) -0.010(3) 0.005(3) N6 0.042(4) 0.028(3) 0.037(3) 0.003(3) 0.006(3) 0.002(3) N8 0.059(5) 0.064(5) 0.049(4) -0.018(4) 0.007(3) -0.022(4) N7 0.048(4) 0.072(5) 0.047(4) 0.018(4) -0.002(3) -0.005(4) N9 0.053(4) 0.046(4) 0.041(4) 0.003(3) 0.005(3) -0.003(3) B1 0.036(5) 0.042(5) 0.043(5) 0.001(4) -0.009(4) 0.002(4) S4 0.199(4) 0.118(3) 0.128(3) -0.071(2) 0.090(3) -0.110(3) Cl2 0.162(4) 0.142(4) 0.134(3) -0.001(3) 0.049(3) -0.032(3) Cl1 0.122(4) 0.359(9) 0.207(6) 0.094(6) -0.029(4) -0.028(5) C26 0.129(17) 0.172(19) 0.40(4) 0.07(2) 0.15(2) -0.001(14) C27 0.149(19) 0.23(2) 0.35(4) 0.05(2) 0.16(2) 0.053(17) _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 2.220(2) . ? W1 S3 2.238(2) . ? W1 N4 2.271(6) . ? W1 N2 2.282(6) . ? W1 S2 2.3214(19) . ? W1 N6 2.326(6) . ? W1 Cu1 2.6364(11) . ? W1 Cu2 2.6444(12) . ? Cu2 N7 1.902(7) . ? Cu2 S1 2.203(2) . ? Cu2 S2 2.248(2) . ? Cu2 S5 2.804(3) 3_466 ? Cu2 Cu1 2.8336(15) . ? Cu1 N8 1.876(7) . ? Cu1 S3 2.186(2) . ? Cu1 S2 2.225(2) . ? S5 C17 1.625(8) . ? S5 Cu2 2.804(3) 3_466 ? C1 C2 1.506(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N1 1.349(9) . ? C2 C3 1.353(11) . ? C3 C4 1.382(11) . ? C3 H3 0.9300 . ? C4 N2 1.353(9) . ? C4 C5 1.489(11) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.493(11) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.347(11) . ? C7 N3 1.362(9) . ? C8 C9 1.388(10) . ? C8 H8 0.9300 . ? C9 N4 1.341(9) . ? C9 C10 1.497(11) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.500(11) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N5 1.342(9) . ? C12 C13 1.352(11) . ? C13 C14 1.382(11) . ? C13 H13 0.9300 . ? C14 N6 1.355(9) . ? C14 C15 1.495(11) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N8 1.129(10) . ? C16 S4 1.637(10) . ? C17 N7 1.150(9) . ? C24 C25 1.510(14) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N9 1.508(11) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C18 C19 1.507(13) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 C21 1.522(13) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C22 C23 1.520(11) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N9 1.497(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C21 N9 1.516(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C19 N9 1.508(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? N1 N2 1.386(8) . ? N1 B1 1.525(11) . ? N3 N4 1.368(8) . ? N3 B1 1.529(11) . ? N5 N6 1.361(8) . ? N5 B1 1.524(10) . ? B1 H1 0.9800 . ? Cl2 C26 1.86(2) . ? Cl1 C27 1.88(2) . ? C26 C27 1.290(16) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 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 S3 102.75(8) . . ? S1 W1 N4 84.11(16) . . ? S3 W1 N4 84.95(17) . . ? S1 W1 N2 87.79(16) . . ? S3 W1 N2 160.55(16) . . ? N4 W1 N2 79.9(2) . . ? S1 W1 S2 104.62(8) . . ? S3 W1 S2 104.68(7) . . ? N4 W1 S2 164.87(16) . . ? N2 W1 S2 88.04(16) . . ? S1 W1 N6 160.35(15) . . ? S3 W1 N6 88.32(15) . . ? N4 W1 N6 80.7(2) . . ? N2 W1 N6 77.3(2) . . ? S2 W1 N6 87.83(15) . . ? S1 W1 Cu1 105.46(6) . . ? S3 W1 Cu1 52.52(5) . . ? N4 W1 Cu1 137.41(16) . . ? N2 W1 Cu1 140.55(16) . . ? S2 W1 Cu1 52.87(6) . . ? N6 W1 Cu1 94.16(15) . . ? S1 W1 Cu2 53.00(6) . . ? S3 W1 Cu2 101.42(6) . . ? N4 W1 Cu2 137.08(16) . . ? N2 W1 Cu2 97.98(15) . . ? S2 W1 Cu2 53.35(6) . . ? N6 W1 Cu2 141.17(14) . . ? Cu1 W1 Cu2 64.90(4) . . ? N7 Cu2 S1 123.0(2) . . ? N7 Cu2 S2 119.8(2) . . ? S1 Cu2 S2 107.68(8) . . ? N7 Cu2 W1 164.1(2) . . ? S1 Cu2 W1 53.57(6) . . ? S2 Cu2 W1 55.95(5) . . ? N7 Cu2 S5 96.0(2) . 3_466 ? S1 Cu2 S5 92.03(9) . 3_466 ? S2 Cu2 S5 113.51(8) . 3_466 ? W1 Cu2 S5 99.61(6) . 3_466 ? N7 Cu2 Cu1 134.1(2) . . ? S1 Cu2 Cu1 99.75(7) . . ? S2 Cu2 Cu1 50.34(6) . . ? W1 Cu2 Cu1 57.41(3) . . ? S5 Cu2 Cu1 64.20(6) 3_466 . ? N8 Cu1 S3 123.8(2) . . ? N8 Cu1 S2 121.7(2) . . ? S3 Cu1 S2 109.83(8) . . ? N8 Cu1 W1 168.4(2) . . ? S3 Cu1 W1 54.34(6) . . ? S2 Cu1 W1 56.28(5) . . ? N8 Cu1 Cu2 131.6(2) . . ? S3 Cu1 Cu2 97.13(7) . . ? S2 Cu1 Cu2 51.05(6) . . ? W1 Cu1 Cu2 57.68(3) . . ? Cu2 S1 W1 73.44(7) . . ? Cu1 S2 Cu2 78.61(8) . . ? Cu1 S2 W1 70.85(6) . . ? Cu2 S2 W1 70.70(6) . . ? Cu1 S3 W1 73.14(7) . . ? C17 S5 Cu2 95.8(3) . 3_466 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 107.4(7) . . ? N1 C2 C1 123.5(8) . . ? C3 C2 C1 129.1(8) . . ? C2 C3 C4 107.9(7) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? N2 C4 C3 109.2(7) . . ? N2 C4 C5 126.1(7) . . ? C3 C4 C5 124.7(8) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N3 107.0(7) . . ? C8 C7 C6 130.3(8) . . ? N3 C7 C6 122.7(8) . . ? C7 C8 C9 107.7(7) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? N4 C9 C8 109.0(7) . . ? N4 C9 C10 125.9(7) . . ? C8 C9 C10 125.1(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 107.6(7) . . ? N5 C12 C11 123.2(8) . . ? C13 C12 C11 129.2(8) . . ? C12 C13 C14 107.5(7) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? N6 C14 C13 108.4(7) . . ? N6 C14 C15 126.5(7) . . ? C13 C14 C15 125.1(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 S4 176.5(11) . . ? N7 C17 S5 178.9(9) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N9 C25 C24 113.5(9) . . ? N9 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? N9 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 C22 116.7(7) . . ? N9 C23 H23A 108.1 . . ? C22 C23 H23A 108.1 . . ? N9 C23 H23B 108.1 . . ? C22 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? N9 C21 C20 116.0(7) . . ? N9 C21 H21A 108.3 . . ? C20 C21 H21A 108.3 . . ? N9 C21 H21B 108.3 . . ? C20 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C18 C19 N9 115.8(8) . . ? C18 C19 H19A 108.3 . . ? N9 C19 H19A 108.3 . . ? C18 C19 H19B 108.3 . . ? N9 C19 H19B 108.3 . . ? H19A C19 H19B 107.4 . . ? C2 N1 N2 110.0(6) . . ? C2 N1 B1 130.2(7) . . ? N2 N1 B1 119.7(6) . . ? C4 N2 N1 105.5(6) . . ? C4 N2 W1 132.3(5) . . ? N1 N2 W1 122.1(4) . . ? C7 N3 N4 109.9(6) . . ? C7 N3 B1 129.9(6) . . ? N4 N3 B1 120.1(6) . . ? C9 N4 N3 106.4(6) . . ? C9 N4 W1 131.0(5) . . ? N3 N4 W1 122.5(4) . . ? C12 N5 N6 110.2(6) . . ? C12 N5 B1 129.1(6) . . ? N6 N5 B1 120.6(6) . . ? C14 N6 N5 106.3(6) . . ? C14 N6 W1 132.6(5) . . ? N5 N6 W1 120.8(4) . . ? C16 N8 Cu1 172.8(8) . . ? C17 N7 Cu2 167.4(7) . . ? C23 N9 C19 107.3(6) . . ? C23 N9 C25 110.8(7) . . ? C19 N9 C25 111.0(7) . . ? C23 N9 C21 110.8(6) . . ? C19 N9 C21 110.8(6) . . ? C25 N9 C21 106.2(7) . . ? N5 B1 N1 108.7(6) . . ? N5 B1 N3 108.6(6) . . ? N1 B1 N3 110.8(6) . . ? N5 B1 H1 109.6 . . ? N1 B1 H1 109.6 . . ? N3 B1 H1 109.6 . . ? C27 C26 Cl2 102.3(16) . . ? C27 C26 H26A 111.3 . . ? Cl2 C26 H26A 111.3 . . ? C27 C26 H26B 111.3 . . ? Cl2 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? C26 C27 Cl1 106.2(17) . . ? C26 C27 H27A 110.5 . . ? Cl1 C27 H27A 110.5 . . ? C26 C27 H27B 110.5 . . ? Cl1 C27 H27B 110.5 . . ? H27A C27 H27B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.428 _refine_diff_density_min -0.976 _refine_diff_density_rms 0.122 #===END data_[Et4N]2[Tp*WS3(CuNCS)3Br].2aniline _database_code_depnum_ccdc_archive 'CCDC 714220' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H22 B Br Cu3 N9 S6 W), 4(C8 H20 N), 2(C6 H7 N), C6 H7 N' _chemical_formula_sum 'C86 H145 B2 Br2 Cu6 N25 S12 W2' _chemical_formula_weight 2844.51 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.168(3) _cell_length_b 37.745(8) _cell_length_c 13.478(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.62(3) _cell_angle_gamma 90.00 _cell_volume 6228(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17378 _cell_measurement_theta_min 3.0585 _cell_measurement_theta_max 25.3491 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2860 _exptl_absorpt_coefficient_mu 3.733 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.122 _exptl_absorpt_correction_T_max 0.224 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45897 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11193 _reflns_number_gt 10090 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Shelxl-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _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^)+(0.1200P)^2^+24.9538P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11193 _refine_ls_number_parameters 617 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.2075 _refine_ls_wR_factor_gt 0.2005 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 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 0.47025(3) 0.104727(9) 0.18179(3) 0.03464(15) Uani 1 1 d . . . Cu1 Cu 0.60992(10) 0.11822(4) 0.37978(9) 0.0527(3) Uani 1 1 d . . . Cu2 Cu 0.46204(10) 0.17100(3) 0.24980(10) 0.0502(3) Uani 1 1 d . . . Cu3 Cu 0.64137(9) 0.14530(3) 0.19137(10) 0.0459(3) Uani 1 1 d . . . S1 S 0.4274(2) 0.12175(7) 0.32559(19) 0.0470(6) Uani 1 1 d . . . S2 S 0.46577(18) 0.15605(6) 0.08965(18) 0.0403(5) Uani 1 1 d . . . S3 S 0.65212(18) 0.08986(7) 0.25331(18) 0.0419(5) Uani 1 1 d . . . S4 S 0.3106(4) 0.27801(12) 0.3002(4) 0.0996(14) Uani 1 1 d . . . S5 S 0.857(4) 0.1082(11) 0.727(3) 0.136(9) Uani 0.57(12) 1 d P A 1 S5A S 0.830(5) 0.1127(5) 0.740(2) 0.116(12) Uani 0.43(12) 1 d P A 2 S6 S 0.9139(3) 0.19424(15) 0.0899(4) 0.1058(15) Uani 1 1 d . . . C1 C 0.0499(11) 0.0505(4) -0.0809(14) 0.102(6) Uani 1 1 d . . . H1A H 0.0829 0.0382 -0.1236 0.153 Uiso 1 1 calc R . . H1B H -0.0170 0.0613 -0.1265 0.153 Uiso 1 1 calc R . . H1C H 0.0348 0.0341 -0.0337 0.153 Uiso 1 1 calc R . . C2 C 0.1259(9) 0.0783(4) -0.0173(11) 0.067(3) Uani 1 1 d . . . C3 C 0.1032(10) 0.1122(4) -0.0018(11) 0.073(4) Uani 1 1 d . . . H3 H 0.0356 0.1234 -0.0293 0.087 Uiso 1 1 calc R . . C4 C 0.2030(8) 0.1273(3) 0.0647(8) 0.050(2) Uani 1 1 d . . . C5 C 0.2137(9) 0.1647(3) 0.1022(12) 0.073(4) Uani 1 1 d . . . H5A H 0.2502 0.1653 0.1783 0.109 Uiso 1 1 calc R . . H5B H 0.1424 0.1751 0.0829 0.109 Uiso 1 1 calc R . . H5C H 0.2554 0.1779 0.0694 0.109 Uiso 1 1 calc R . . C6 C 0.2545(11) -0.0292(3) 0.1456(12) 0.077(4) Uani 1 1 d . . . H6A H 0.1846 -0.0178 0.1160 0.115 Uiso 1 1 calc R . . H6B H 0.2525 -0.0468 0.1963 0.115 Uiso 1 1 calc R . . H6C H 0.2714 -0.0403 0.0895 0.115 Uiso 1 1 calc R . . C7 C 0.3399(9) -0.0024(3) 0.2003(9) 0.056(3) Uani 1 1 d . . . C8 C 0.4159(9) -0.0030(3) 0.3017(9) 0.055(3) Uani 1 1 d . . . H8 H 0.4256 -0.0210 0.3516 0.066 Uiso 1 1 calc R . . C9 C 0.4766(9) 0.0284(3) 0.3170(8) 0.051(2) Uani 1 1 d . . . C10 C 0.5698(12) 0.0381(4) 0.4163(9) 0.077(4) Uani 1 1 d . . . H10A H 0.6329 0.0432 0.3992 0.116 Uiso 1 1 calc R . . H10B H 0.5857 0.0188 0.4659 0.116 Uiso 1 1 calc R . . H10C H 0.5508 0.0587 0.4477 0.116 Uiso 1 1 calc R . . C11 C 0.3412(10) 0.0015(3) -0.1503(9) 0.067(3) Uani 1 1 d . . . H11A H 0.3556 -0.0193 -0.1063 0.101 Uiso 1 1 calc R . . H11B H 0.3621 -0.0027 -0.2104 0.101 Uiso 1 1 calc R . . H11C H 0.2647 0.0070 -0.1750 0.101 Uiso 1 1 calc R . . C12 C 0.4046(9) 0.0315(3) -0.0876(8) 0.051(2) Uani 1 1 d . . . C13 C 0.4884(10) 0.0495(3) -0.1033(7) 0.053(3) Uani 1 1 d . . . H13 H 0.5160 0.0449 -0.1564 0.064 Uiso 1 1 calc R . . C14 C 0.5245(8) 0.0756(3) -0.0259(7) 0.045(2) Uani 1 1 d . . . C15 C 0.6127(10) 0.1014(3) -0.0173(9) 0.057(3) Uani 1 1 d . . . H15A H 0.5879 0.1249 -0.0116 0.086 Uiso 1 1 calc R . . H15B H 0.6313 0.0997 -0.0796 0.086 Uiso 1 1 calc R . . H15C H 0.6758 0.0961 0.0450 0.086 Uiso 1 1 calc R . . C16 C 0.3642(8) 0.2406(3) 0.2819(8) 0.053(3) Uani 1 1 d . . . C17 C 0.7580(12) 0.1104(3) 0.6100(10) 0.072(4) Uani 1 1 d . . . C18 C 0.8204(8) 0.1755(3) 0.1250(8) 0.050(2) Uani 1 1 d . . . C19 C 0.4353(10) 0.3092(4) 0.0490(10) 0.079(4) Uani 1 1 d . . . H19A H 0.4110 0.2880 0.0076 0.118 Uiso 1 1 calc R . . H19B H 0.4016 0.3294 0.0065 0.118 Uiso 1 1 calc R . . H19C H 0.4154 0.3082 0.1107 0.118 Uiso 1 1 calc R . . C20 C 0.5576(9) 0.3121(3) 0.0841(8) 0.055(3) Uani 1 1 d . . . H20A H 0.5796 0.3355 0.1144 0.066 Uiso 1 1 calc R . . H20B H 0.5772 0.3102 0.0216 0.066 Uiso 1 1 calc R . . C21 C 0.6435(14) 0.3237(4) 0.3266(12) 0.089(4) Uani 1 1 d . . . H21A H 0.7219 0.3238 0.3566 0.133 Uiso 1 1 calc R . . H21B H 0.6156 0.3265 0.3826 0.133 Uiso 1 1 calc R . . H21C H 0.6182 0.3428 0.2766 0.133 Uiso 1 1 calc R . . C22 C 0.6042(11) 0.2893(3) 0.2705(9) 0.066(3) Uani 1 1 d . . . H22A H 0.5267 0.2871 0.2562 0.079 Uiso 1 1 calc R . . H22B H 0.6410 0.2701 0.3182 0.079 Uiso 1 1 calc R . . C23 C 0.8205(10) 0.2676(4) 0.2651(11) 0.077(4) Uani 1 1 d . . . H23A H 0.8153 0.2721 0.3332 0.116 Uiso 1 1 calc R . . H23B H 0.8935 0.2726 0.2693 0.116 Uiso 1 1 calc R . . H23C H 0.8034 0.2433 0.2460 0.116 Uiso 1 1 calc R . . C24 C 0.7409(8) 0.2912(3) 0.1815(9) 0.056(3) Uani 1 1 d . . . H24A H 0.7583 0.3158 0.2021 0.067 Uiso 1 1 calc R . . H24B H 0.7502 0.2876 0.1141 0.067 Uiso 1 1 calc R . . C25 C 0.5994(12) 0.2376(3) 0.0212(9) 0.069(3) Uani 1 1 d . . . H25A H 0.5641 0.2552 -0.0314 0.103 Uiso 1 1 calc R . . H25B H 0.5656 0.2150 -0.0023 0.103 Uiso 1 1 calc R . . H25C H 0.6754 0.2363 0.0312 0.103 Uiso 1 1 calc R . . C26 C 0.5884(10) 0.2475(3) 0.1272(8) 0.058(3) Uani 1 1 d . . . H26A H 0.5128 0.2442 0.1195 0.070 Uiso 1 1 calc R . . H26B H 0.6321 0.2311 0.1816 0.070 Uiso 1 1 calc R . . C27 C 0.9788(17) 0.1906(7) 0.6184(18) 0.141(8) Uani 1 1 d . . . H27A H 0.9695 0.2148 0.5951 0.212 Uiso 1 1 calc R . . H27B H 0.9953 0.1897 0.6939 0.212 Uiso 1 1 calc R . . H27C H 0.9127 0.1777 0.5819 0.212 Uiso 1 1 calc R . . C28 C 1.0724(12) 0.1741(5) 0.5934(12) 0.088(4) Uani 1 1 d . . . H28A H 1.1384 0.1876 0.6293 0.105 Uiso 1 1 calc R . . H28B H 1.0847 0.1502 0.6220 0.105 Uiso 1 1 calc R . . C29 C 1.113(2) 0.2357(7) 0.476(2) 0.180(11) Uani 1 1 d . . . H29A H 1.1196 0.2404 0.5478 0.270 Uiso 1 1 calc R . . H29B H 1.0928 0.2571 0.4345 0.270 Uiso 1 1 calc R . . H29C H 1.1821 0.2275 0.4754 0.270 Uiso 1 1 calc R . . C30 C 1.0242(17) 0.2068(7) 0.4260(16) 0.135(8) Uani 1 1 d . . . H30A H 0.9561 0.2147 0.4309 0.162 Uiso 1 1 calc R . . H30B H 1.0124 0.2043 0.3510 0.162 Uiso 1 1 calc R . . C31 C 0.9591(16) 0.1153(7) 0.462(2) 0.157(11) Uani 1 1 d . . . H31A H 1.0290 0.1054 0.4708 0.235 Uiso 1 1 calc R . . H31B H 0.9023 0.1007 0.4142 0.235 Uiso 1 1 calc R . . H31C H 0.9514 0.1163 0.5301 0.235 Uiso 1 1 calc R . . C32 C 0.9514(13) 0.1492(7) 0.4203(15) 0.116(7) Uani 1 1 d . . . H32A H 0.8874 0.1607 0.4250 0.139 Uiso 1 1 calc R . . H32B H 0.9409 0.1475 0.3454 0.139 Uiso 1 1 calc R . . C33 C 1.1539(17) 0.1541(8) 0.3586(16) 0.170(12) Uani 1 1 d . . . H33A H 1.0852 0.1446 0.3121 0.255 Uiso 1 1 calc R . . H33B H 1.2118 0.1384 0.3597 0.255 Uiso 1 1 calc R . . H33C H 1.1650 0.1769 0.3332 0.255 Uiso 1 1 calc R . . C34 C 1.1534(10) 0.1576(5) 0.4703(12) 0.092(5) Uani 1 1 d . . . H34A H 1.1653 0.1343 0.5032 0.110 Uiso 1 1 calc R . . H34B H 1.2144 0.1724 0.5117 0.110 Uiso 1 1 calc R . . C35 C 0.279(2) 0.1081(6) -0.2542(17) 0.112(7) Uani 1 1 d . . . C36 C 0.213(2) 0.0810(7) -0.306(2) 0.133(8) Uani 1 1 d . . . H36 H 0.1537 0.0740 -0.2888 0.160 Uiso 1 1 calc R . . C37 C 0.239(2) 0.0642(7) -0.384(3) 0.152(11) Uani 1 1 d . . . H37 H 0.1950 0.0452 -0.4186 0.183 Uiso 1 1 calc R . . C38 C 0.328(3) 0.0739(8) -0.417(3) 0.169(11) Uani 1 1 d . . . H38 H 0.3427 0.0621 -0.4703 0.203 Uiso 1 1 calc R . . C39 C 0.387(2) 0.1013(8) -0.363(3) 0.148(10) Uani 1 1 d . . . H39 H 0.4454 0.1090 -0.3807 0.177 Uiso 1 1 calc R . . C40 C 0.367(2) 0.1192(7) -0.282(2) 0.135(9) Uani 1 1 d . . . H40 H 0.4104 0.1381 -0.2464 0.162 Uiso 1 1 calc R . . C41 C 0.017(2) 0.0605(6) 0.2260(19) 0.124(12) Uiso 0.50 1 d PGU . . C42 C 0.1201(17) 0.0452(7) 0.259(2) 0.115(11) Uiso 0.50 1 d PGU . . H42 H 0.1733 0.0548 0.2367 0.138 Uiso 0.50 1 calc PR . . C43 C 0.1437(14) 0.0156(6) 0.3248(19) 0.096(9) Uiso 0.50 1 d PGU . . H43 H 0.2127 0.0054 0.3468 0.115 Uiso 0.50 1 calc PR . . C44 C 0.0642(18) 0.0013(5) 0.3580(17) 0.113(10) Uiso 0.50 1 d PGU . . H44 H 0.0800 -0.0185 0.4021 0.135 Uiso 0.50 1 calc PR . . C45 C -0.0390(16) 0.0166(6) 0.3251(17) 0.103(10) Uiso 0.50 1 d PGU . . H45 H -0.0922 0.0071 0.3473 0.123 Uiso 0.50 1 calc PR . . C46 C -0.0626(14) 0.0462(6) 0.2591(18) 0.087(8) Uiso 0.50 1 d PGU . . H46 H -0.1316 0.0565 0.2372 0.105 Uiso 0.50 1 calc PR . . N13 N -0.050(4) 0.0766(16) 0.189(4) 0.22(2) Uiso 0.50 1 d PU . . H13A H -0.0460 0.0932 0.1466 0.266 Uiso 0.50 1 calc PR . . H13B H -0.1093 0.0735 0.2004 0.266 Uiso 0.50 1 calc PR . . N1 N 0.2348(6) 0.0727(2) 0.0333(7) 0.050(2) Uani 1 1 d . . . N2 N 0.2831(7) 0.1029(2) 0.0870(7) 0.048(2) Uani 1 1 d . . . N3 N 0.3547(6) 0.0281(2) 0.1562(7) 0.0464(19) Uani 1 1 d . . . N4 N 0.4376(6) 0.0479(2) 0.2255(6) 0.0454(19) Uani 1 1 d . . . N5 N 0.3890(6) 0.0471(2) -0.0052(6) 0.0439(18) Uani 1 1 d . . . N6 N 0.4618(6) 0.07416(19) 0.0348(5) 0.0366(16) Uani 1 1 d . . . N7 N 0.4039(7) 0.2148(3) 0.2698(7) 0.056(2) Uani 1 1 d . . . N8 N 0.6985(8) 0.1125(3) 0.5259(7) 0.062(2) Uani 1 1 d . A . N9 N 0.7562(7) 0.1639(2) 0.1525(7) 0.051(2) Uani 1 1 d . . . N10 N 0.6220(7) 0.2844(2) 0.1657(6) 0.0468(19) Uani 1 1 d . . . N11 N 1.0520(8) 0.1727(4) 0.4769(8) 0.079(3) Uani 1 1 d . . . N12 N 0.2523(19) 0.1241(7) -0.1836(16) 0.174(9) Uani 1 1 d . . . H12A H 0.1955 0.1175 -0.1715 0.209 Uiso 1 1 calc R . . H12B H 0.2911 0.1416 -0.1484 0.209 Uiso 1 1 calc R . . Br1 Br 0.67922(8) 0.18748(3) 0.36777(7) 0.0461(3) Uani 1 1 d . . . B1 B 0.2994(10) 0.0394(3) 0.0400(10) 0.051(3) Uani 1 1 d . . . H1 H 0.2512 0.0204 -0.0012 0.061 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 0.0338(2) 0.0364(2) 0.0325(2) -0.00153(14) 0.01069(16) -0.00051(14) Cu1 0.0497(7) 0.0681(9) 0.0347(6) -0.0048(6) 0.0090(5) 0.0081(6) Cu2 0.0569(7) 0.0434(7) 0.0526(7) -0.0054(5) 0.0227(6) 0.0060(6) Cu3 0.0379(6) 0.0475(7) 0.0527(7) 0.0033(5) 0.0173(5) -0.0019(5) S1 0.0490(13) 0.0546(16) 0.0420(12) -0.0019(11) 0.0219(11) 0.0029(11) S2 0.0396(12) 0.0382(13) 0.0384(11) 0.0031(9) 0.0089(9) 0.0025(9) S3 0.0371(12) 0.0459(14) 0.0402(12) -0.0020(10) 0.0113(10) 0.0034(10) S4 0.097(3) 0.078(3) 0.116(3) -0.015(2) 0.032(2) 0.042(2) S5 0.133(16) 0.15(2) 0.064(10) 0.024(9) -0.032(9) 0.007(11) S5A 0.21(3) 0.041(13) 0.040(7) 0.008(5) -0.023(10) 0.012(9) S6 0.062(2) 0.161(5) 0.109(3) 0.023(3) 0.049(2) -0.019(2) C1 0.054(8) 0.075(10) 0.139(14) -0.022(9) -0.009(8) -0.008(7) C2 0.045(6) 0.061(8) 0.080(8) -0.001(6) 0.005(6) 0.000(5) C3 0.042(6) 0.071(9) 0.090(9) 0.010(7) 0.006(6) -0.003(6) C4 0.037(5) 0.050(6) 0.056(6) 0.000(5) 0.008(4) 0.005(4) C5 0.045(6) 0.057(8) 0.116(11) -0.014(7) 0.030(7) 0.009(5) C6 0.085(9) 0.056(8) 0.099(10) -0.003(7) 0.046(8) -0.029(7) C7 0.058(6) 0.048(7) 0.071(7) 0.000(5) 0.033(6) 0.000(5) C8 0.074(7) 0.049(7) 0.057(6) 0.015(5) 0.041(6) 0.002(5) C9 0.063(6) 0.054(7) 0.040(5) 0.008(5) 0.023(5) 0.004(5) C10 0.100(10) 0.081(10) 0.039(6) 0.022(6) 0.013(6) -0.009(8) C11 0.076(8) 0.047(7) 0.060(7) -0.015(5) 0.002(6) -0.013(6) C12 0.066(7) 0.037(6) 0.041(5) 0.000(4) 0.010(5) -0.001(5) C13 0.082(7) 0.048(6) 0.030(4) -0.003(4) 0.021(5) 0.013(5) C14 0.058(6) 0.039(5) 0.036(5) 0.001(4) 0.014(4) 0.007(4) C15 0.079(8) 0.049(7) 0.060(7) -0.002(5) 0.045(6) -0.004(5) C16 0.047(6) 0.056(7) 0.050(6) -0.009(5) 0.012(5) 0.001(5) C17 0.089(9) 0.045(7) 0.059(8) 0.010(5) 0.001(7) 0.010(6) C18 0.042(5) 0.061(7) 0.045(5) 0.004(5) 0.013(5) 0.004(5) C19 0.058(7) 0.117(13) 0.064(7) 0.016(7) 0.026(6) 0.025(7) C20 0.066(7) 0.054(7) 0.044(5) 0.016(5) 0.020(5) 0.015(5) C21 0.125(13) 0.081(11) 0.079(9) -0.011(8) 0.058(9) 0.014(9) C22 0.086(8) 0.077(9) 0.049(6) 0.018(6) 0.041(6) 0.022(7) C23 0.066(8) 0.086(10) 0.076(8) 0.018(7) 0.021(7) 0.007(7) C24 0.046(6) 0.065(8) 0.055(6) 0.000(5) 0.016(5) -0.001(5) C25 0.107(10) 0.051(7) 0.050(6) -0.005(5) 0.030(6) 0.002(7) C26 0.079(8) 0.053(7) 0.046(6) 0.006(5) 0.026(5) -0.017(6) C27 0.122(16) 0.19(2) 0.133(17) -0.021(16) 0.065(14) 0.017(15) C28 0.070(9) 0.089(11) 0.092(10) 0.004(8) 0.014(8) 0.002(8) C29 0.20(3) 0.15(3) 0.17(3) 0.06(2) 0.04(2) 0.01(2) C30 0.110(15) 0.16(2) 0.105(14) 0.023(14) 0.004(11) 0.062(15) C31 0.065(12) 0.21(3) 0.16(2) -0.07(2) 0.000(13) -0.019(15) C32 0.052(9) 0.18(2) 0.088(11) 0.000(13) -0.002(8) 0.031(11) C33 0.117(16) 0.30(4) 0.110(15) 0.013(19) 0.060(13) 0.079(19) C34 0.041(7) 0.128(14) 0.089(10) 0.016(9) 0.003(6) 0.019(7) C35 0.134(18) 0.090(14) 0.078(12) 0.032(10) -0.001(12) 0.007(13) C36 0.118(17) 0.12(2) 0.125(18) 0.018(15) 0.002(15) -0.013(15) C37 0.14(2) 0.089(17) 0.17(3) 0.043(17) -0.016(18) -0.022(15) C38 0.16(3) 0.10(2) 0.20(3) 0.07(2) 0.02(2) 0.043(18) C39 0.120(19) 0.12(2) 0.17(3) 0.038(18) 0.007(18) 0.018(16) C40 0.118(18) 0.103(18) 0.132(19) 0.040(15) -0.015(15) -0.010(14) N1 0.032(4) 0.047(5) 0.055(5) 0.001(4) -0.003(4) -0.001(3) N2 0.044(5) 0.046(5) 0.050(5) 0.006(4) 0.014(4) 0.003(4) N3 0.042(4) 0.040(5) 0.057(5) 0.004(4) 0.018(4) -0.001(4) N4 0.044(4) 0.040(5) 0.049(4) 0.010(4) 0.014(4) 0.004(4) N5 0.044(4) 0.046(5) 0.038(4) -0.007(3) 0.011(3) -0.006(4) N6 0.047(4) 0.030(4) 0.032(3) -0.001(3) 0.014(3) 0.005(3) N7 0.052(5) 0.050(6) 0.059(5) -0.009(4) 0.012(4) 0.009(4) N8 0.066(6) 0.064(6) 0.040(5) 0.004(4) 0.003(5) 0.002(5) N9 0.042(5) 0.054(6) 0.061(5) -0.006(4) 0.023(4) -0.008(4) N10 0.050(5) 0.052(5) 0.041(4) 0.008(4) 0.020(4) 0.003(4) N11 0.050(6) 0.115(10) 0.059(6) 0.009(6) 0.005(5) 0.017(6) N12 0.19(2) 0.20(2) 0.096(13) 0.032(15) 0.019(14) -0.021(19) Br1 0.0438(5) 0.0505(6) 0.0409(5) -0.0062(4) 0.0120(4) 0.0008(4) B1 0.048(6) 0.043(7) 0.055(7) 0.001(5) 0.010(5) -0.005(5) _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 N6 2.260(7) . ? W1 S2 2.290(2) . ? W1 S3 2.297(2) . ? W1 N4 2.306(8) . ? W1 S1 2.300(2) . ? W1 N2 2.322(8) . ? W1 Cu1 2.6732(15) . ? W1 Cu2 2.6800(14) . ? W1 Cu3 2.6881(13) . ? Cu1 N8 1.896(9) . ? Cu1 S1 2.243(3) . ? Cu1 S3 2.249(3) . ? Cu1 Br1 2.7932(19) . ? Cu1 Cu2 2.884(2) . ? Cu1 Cu3 2.9051(18) . ? Cu2 N7 1.883(9) . ? Cu2 S1 2.247(3) . ? Cu2 S2 2.249(3) . ? Cu2 Br1 2.7825(18) . ? Cu2 Cu3 2.9168(18) . ? Cu3 N9 1.908(8) . ? Cu3 S3 2.238(3) . ? Cu3 S2 2.248(3) . ? Cu3 Br1 2.7498(16) . ? S4 C16 1.637(12) . ? S5 C17 1.64(3) . ? S5A C17 1.66(3) . ? S6 C18 1.635(11) . ? C1 C2 1.485(18) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.348(18) . ? C2 N1 1.359(13) . ? C3 C4 1.409(16) . ? C3 H3 0.9300 . ? C4 N2 1.349(13) . ? C4 C5 1.487(16) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.493(16) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N3 1.339(14) . ? C7 C8 1.365(16) . ? C8 C9 1.401(15) . ? C8 H8 0.9300 . ? C9 N4 1.365(12) . ? C9 C10 1.490(16) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.475(14) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 N5 1.336(13) . ? C12 C13 1.376(16) . ? C13 C14 1.387(14) . ? C13 H13 0.9300 . ? C14 N6 1.360(12) . ? C14 C15 1.486(15) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N7 1.146(13) . ? C17 N8 1.117(14) . ? C18 N9 1.128(13) . ? C19 C20 1.506(16) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N10 1.528(12) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.497(19) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N10 1.525(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.513(16) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 N10 1.522(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.534(15) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N10 1.497(14) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.53(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N11 1.494(18) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.56(3) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N11 1.44(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.39(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 N11 1.54(2) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.51(2) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 N11 1.483(16) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N12 1.28(3) . ? C35 C36 1.36(3) . ? C35 C40 1.40(3) . ? C36 C37 1.37(4) . ? C36 H36 0.9300 . ? C37 C38 1.45(4) . ? C37 H37 0.9300 . ? C38 C39 1.34(3) . ? C38 H38 0.9300 . ? C39 C40 1.39(4) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 N13 1.03(6) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? N13 H13A 0.8600 . ? N13 H13B 0.8600 . ? N1 N2 1.374(12) . ? N1 B1 1.503(15) . ? N3 N4 1.369(11) . ? N3 B1 1.524(14) . ? N5 N6 1.368(11) . ? N5 B1 1.543(15) . ? N12 H12A 0.8600 . ? N12 H12B 0.8600 . ? B1 H1 0.9800 . ? 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 N6 W1 S2 88.47(19) . . ? N6 W1 S3 87.14(19) . . ? S2 W1 S3 104.40(9) . . ? N6 W1 N4 78.2(3) . . ? S2 W1 N4 162.8(2) . . ? S3 W1 N4 86.0(2) . . ? N6 W1 S1 158.9(2) . . ? S2 W1 S1 104.79(9) . . ? S3 W1 S1 104.83(9) . . ? N4 W1 S1 85.3(2) . . ? N6 W1 N2 78.6(3) . . ? S2 W1 N2 85.2(2) . . ? S3 W1 N2 162.7(2) . . ? N4 W1 N2 81.5(3) . . ? S1 W1 N2 86.1(2) . . ? N6 W1 Cu1 140.00(18) . . ? S2 W1 Cu1 104.53(7) . . ? S3 W1 Cu1 53.16(7) . . ? N4 W1 Cu1 92.7(2) . . ? S1 W1 Cu1 52.98(7) . . ? N2 W1 Cu1 139.1(2) . . ? N6 W1 Cu2 141.37(19) . . ? S2 W1 Cu2 53.11(7) . . ? S3 W1 Cu2 104.58(7) . . ? N4 W1 Cu2 138.2(2) . . ? S1 W1 Cu2 52.98(7) . . ? N2 W1 Cu2 92.7(2) . . ? Cu1 W1 Cu2 65.19(4) . . ? N6 W1 Cu3 95.89(19) . . ? S2 W1 Cu3 52.96(6) . . ? S3 W1 Cu3 52.64(7) . . ? N4 W1 Cu3 138.56(19) . . ? S1 W1 Cu3 105.17(8) . . ? N2 W1 Cu3 138.1(2) . . ? Cu1 W1 Cu3 65.62(5) . . ? Cu2 W1 Cu3 65.83(4) . . ? N8 Cu1 S1 121.3(3) . . ? N8 Cu1 S3 120.2(3) . . ? S1 Cu1 S3 108.40(10) . . ? N8 Cu1 W1 161.6(3) . . ? S1 Cu1 W1 54.96(7) . . ? S3 Cu1 W1 54.83(6) . . ? N8 Cu1 Br1 94.5(3) . . ? S1 Cu1 Br1 105.03(9) . . ? S3 Cu1 Br1 102.96(9) . . ? W1 Cu1 Br1 103.87(5) . . ? N8 Cu1 Cu2 136.8(3) . . ? S1 Cu1 Cu2 50.11(8) . . ? S3 Cu1 Cu2 99.70(8) . . ? W1 Cu1 Cu2 57.52(4) . . ? Br1 Cu1 Cu2 58.68(5) . . ? N8 Cu1 Cu3 135.8(3) . . ? S1 Cu1 Cu3 100.09(8) . . ? S3 Cu1 Cu3 49.49(8) . . ? W1 Cu1 Cu3 57.44(4) . . ? Br1 Cu1 Cu3 57.67(4) . . ? Cu2 Cu1 Cu3 60.51(5) . . ? N7 Cu2 S1 120.0(3) . . ? N7 Cu2 S2 120.8(3) . . ? S1 Cu2 S2 107.97(10) . . ? N7 Cu2 W1 159.8(3) . . ? S1 Cu2 W1 54.82(7) . . ? S2 Cu2 W1 54.52(7) . . ? N7 Cu2 Br1 96.2(3) . . ? S1 Cu2 Br1 105.25(8) . . ? S2 Cu2 Br1 102.89(8) . . ? W1 Cu2 Br1 103.98(5) . . ? N7 Cu2 Cu1 137.6(3) . . ? S1 Cu2 Cu1 49.99(7) . . ? S2 Cu2 Cu1 99.26(8) . . ? W1 Cu2 Cu1 57.29(4) . . ? Br1 Cu2 Cu1 59.04(5) . . ? N7 Cu2 Cu3 138.0(3) . . ? S1 Cu2 Cu3 99.65(8) . . ? S2 Cu2 Cu3 49.55(7) . . ? W1 Cu2 Cu3 57.22(4) . . ? Br1 Cu2 Cu3 57.64(4) . . ? Cu1 Cu2 Cu3 60.11(4) . . ? N9 Cu3 S3 120.0(3) . . ? N9 Cu3 S2 120.5(3) . . ? S3 Cu3 S2 107.79(10) . . ? N9 Cu3 W1 158.7(3) . . ? S3 Cu3 W1 54.68(7) . . ? S2 Cu3 W1 54.40(7) . . ? N9 Cu3 Br1 96.6(3) . . ? S3 Cu3 Br1 104.63(8) . . ? S2 Cu3 Br1 103.93(8) . . ? W1 Cu3 Br1 104.66(5) . . ? N9 Cu3 Cu1 138.8(3) . . ? S3 Cu3 Cu1 49.82(7) . . ? S2 Cu3 Cu1 98.66(8) . . ? W1 Cu3 Cu1 56.94(4) . . ? Br1 Cu3 Cu1 59.12(4) . . ? N9 Cu3 Cu2 139.0(3) . . ? S3 Cu3 Cu2 99.00(8) . . ? S2 Cu3 Cu2 49.58(7) . . ? W1 Cu3 Cu2 56.95(4) . . ? Br1 Cu3 Cu2 58.73(5) . . ? Cu1 Cu3 Cu2 59.38(5) . . ? Cu1 S1 Cu2 79.91(10) . . ? Cu1 S1 W1 72.06(8) . . ? Cu2 S1 W1 72.21(8) . . ? Cu3 S2 Cu2 80.87(9) . . ? Cu3 S2 W1 72.64(7) . . ? Cu2 S2 W1 72.37(8) . . ? Cu3 S3 Cu1 80.69(10) . . ? Cu3 S3 W1 72.68(8) . . ? Cu1 S3 W1 72.02(8) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 N1 108.9(11) . . ? C3 C2 C1 128.3(11) . . ? N1 C2 C1 122.7(12) . . ? C2 C3 C4 105.9(10) . . ? C2 C3 H3 127.0 . . ? C4 C3 H3 127.0 . . ? N2 C4 C3 109.6(10) . . ? N2 C4 C5 127.1(9) . . ? C3 C4 C5 123.3(10) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 C8 106.7(10) . . ? N3 C7 C6 124.8(11) . . ? C8 C7 C6 128.5(11) . . ? C7 C8 C9 107.5(9) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? N4 C9 C8 108.6(9) . . ? N4 C9 C10 126.1(10) . . ? C8 C9 C10 125.3(10) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 106.9(9) . . ? N5 C12 C11 125.9(10) . . ? C13 C12 C11 127.3(10) . . ? C12 C13 C14 107.8(9) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N6 C14 C13 108.0(9) . . ? N6 C14 C15 127.5(9) . . ? C13 C14 C15 124.4(10) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 S4 178.4(11) . . ? N8 C17 S5 173(3) . . ? N8 C17 S5A 169(2) . . ? S5 C17 S5A 17(2) . . ? N9 C18 S6 176.6(11) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C19 C20 N10 114.9(10) . . ? C19 C20 H20A 108.6 . . ? N10 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? N10 C20 H20B 108.6 . . ? H20A C20 H20B 107.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 C22 N10 115.4(10) . . ? C21 C22 H22A 108.4 . . ? N10 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? N10 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N10 C24 C23 113.6(9) . . ? N10 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? N10 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N10 C26 C25 115.6(9) . . ? N10 C26 H26A 108.4 . . ? C25 C26 H26A 108.4 . . ? N10 C26 H26B 108.4 . . ? C25 C26 H26B 108.4 . . ? H26A C26 H26B 107.4 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N11 C28 C27 113.6(13) . . ? N11 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? N11 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N11 C30 C29 113.7(15) . . ? N11 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? N11 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C31 C32 N11 114.1(14) . . ? C31 C32 H32A 108.7 . . ? N11 C32 H32A 108.7 . . ? C31 C32 H32B 108.7 . . ? N11 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N11 C34 C33 115.3(12) . . ? N11 C34 H34A 108.5 . . ? C33 C34 H34A 108.5 . . ? N11 C34 H34B 108.5 . . ? C33 C34 H34B 108.5 . . ? H34A C34 H34B 107.5 . . ? N12 C35 C36 116(3) . . ? N12 C35 C40 122(3) . . ? C36 C35 C40 122(3) . . ? C35 C36 C37 117(3) . . ? C35 C36 H36 121.6 . . ? C37 C36 H36 121.6 . . ? C36 C37 C38 125(3) . . ? C36 C37 H37 117.5 . . ? C38 C37 H37 117.5 . . ? C39 C38 C37 114(3) . . ? C39 C38 H38 123.0 . . ? C37 C38 H38 123.0 . . ? C38 C39 C40 124(3) . . ? C38 C39 H39 118.1 . . ? C40 C39 H39 118.1 . . ? C35 C40 C39 119(3) . . ? C35 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? N13 C41 C42 163(4) . . ? N13 C41 C46 77(4) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C41 N13 H13A 120.0 . . ? C41 N13 H13B 120.0 . . ? H13A N13 H13B 120.0 . . ? C2 N1 N2 109.4(9) . . ? C2 N1 B1 129.1(10) . . ? N2 N1 B1 121.4(8) . . ? C4 N2 N1 106.1(8) . . ? C4 N2 W1 133.4(7) . . ? N1 N2 W1 120.4(6) . . ? C7 N3 N4 112.1(8) . . ? C7 N3 B1 127.1(9) . . ? N4 N3 B1 120.5(8) . . ? C9 N4 N3 105.1(8) . . ? C9 N4 W1 133.6(7) . . ? N3 N4 W1 120.8(6) . . ? C12 N5 N6 110.8(8) . . ? C12 N5 B1 128.2(9) . . ? N6 N5 B1 120.8(8) . . ? C14 N6 N5 106.6(7) . . ? C14 N6 W1 131.4(6) . . ? N5 N6 W1 121.8(5) . . ? C16 N7 Cu2 176.7(10) . . ? C17 N8 Cu1 173.8(12) . . ? C18 N9 Cu3 176.7(9) . . ? C26 N10 C24 111.3(9) . . ? C26 N10 C22 107.8(8) . . ? C24 N10 C22 110.6(8) . . ? C26 N10 C20 111.9(8) . . ? C24 N10 C20 104.8(8) . . ? C22 N10 C20 110.5(8) . . ? C30 N11 C34 113.0(14) . . ? C30 N11 C28 112.6(14) . . ? C34 N11 C28 105.1(10) . . ? C30 N11 C32 104.8(14) . . ? C34 N11 C32 112.3(13) . . ? C28 N11 C32 109.2(12) . . ? C35 N12 H12A 120.0 . . ? C35 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? Cu3 Br1 Cu2 63.63(5) . . ? Cu3 Br1 Cu1 63.21(4) . . ? Cu2 Br1 Cu1 62.29(4) . . ? N1 B1 N3 110.0(9) . . ? N1 B1 N5 108.4(9) . . ? N3 B1 N5 108.3(8) . . ? N1 B1 H1 110.1 . . ? N3 B1 H1 110.1 . . ? N5 B1 H1 110.1 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.234 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.126 data_[Et4N][Tp*WS3(CuSCN)4] _database_code_depnum_ccdc_archive 'CCDC 714221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H22 B Cu4 N10 S7 W, C8 H20 N' _chemical_formula_sum 'C27 H42 B Cu4 N11 S7 W' _chemical_formula_weight 1194.05 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.643(3) _cell_length_b 17.390(4) _cell_length_c 33.613(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8559(3) _cell_formula_units_Z 8 _cell_measurement_temperature 303(2) _cell_measurement_reflns_used 27677 _cell_measurement_theta_min 3.0177 _cell_measurement_theta_max 25.3491 _exptl_crystal_description BLOCK _exptl_crystal_colour black _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4696 _exptl_absorpt_coefficient_mu 5.01 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.213 _exptl_absorpt_correction_T_max 0.645 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 303(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 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 77941 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7826 _reflns_number_gt 6560 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Shelxl-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _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^)+(0.1180P)^2^+41.7844P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7826 _refine_ls_number_parameters 457 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1174 _refine_ls_R_factor_gt 0.0972 _refine_ls_wR_factor_ref 0.2649 _refine_ls_wR_factor_gt 0.2547 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_restrained_S_all 1.317 _refine_ls_shift/su_max 0.070 _refine_ls_shift/su_mean 0.008 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 0.59019(4) -1.06843(3) 0.592752(17) 0.0434(2) Uani 1 1 d . . . Cu3 Cu 0.42940(14) -1.13677(12) 0.59342(6) 0.0602(6) Uani 1 1 d . . . Cu2 Cu 0.54581(15) -1.13183(12) 0.66258(6) 0.0624(6) Uani 1 1 d . . . Cu1 Cu 0.46106(14) -0.99530(12) 0.63377(7) 0.0643(6) Uani 1 1 d . . . S3 S 0.6064(3) -1.0150(2) 0.65434(12) 0.0549(10) Uani 1 1 d . . . S1 S 0.4555(3) -1.0208(2) 0.56851(13) 0.0564(10) Uani 1 1 d . . . S2 S 0.5612(3) -1.1966(2) 0.60558(12) 0.0517(9) Uani 1 1 d . . . N1 N 0.8002(8) -1.0778(7) 0.5668(4) 0.051(3) Uani 1 1 d . . . N2 N 0.7422(8) -1.0994(7) 0.5968(3) 0.047(3) Uani 1 1 d . . . N4 N 0.6184(9) -1.1065(8) 0.5296(4) 0.056(3) Uani 1 1 d . . . C12 C 0.7539(11) -0.8853(9) 0.5349(5) 0.061(4) Uani 1 1 d . . . N3 N 0.6954(9) -1.0848(7) 0.5095(3) 0.049(3) Uani 1 1 d . . . N5 N 0.7267(9) -0.9585(7) 0.5439(3) 0.053(3) Uani 1 1 d . . . C5 C 0.7577(12) -1.1707(11) 0.6628(5) 0.076(5) Uani 1 1 d . . . H5A H 0.7373 -1.1302 0.6800 0.115 Uiso 1 1 calc R . . H5B H 0.8061 -1.1987 0.6755 0.115 Uiso 1 1 calc R . . H5C H 0.7078 -1.2049 0.6573 0.115 Uiso 1 1 calc R . . C9 C 0.5760(12) -1.1531(9) 0.5036(5) 0.058(4) Uani 1 1 d . . . N10 N 0.3873(11) -1.0985(10) 0.6669(5) 0.075(4) Uani 1 1 d . . . C3 C 0.8811(10) -1.1390(9) 0.6126(5) 0.056(4) Uani 1 1 d . . . H3 H 0.9293 -1.1609 0.6266 0.067 Uiso 1 1 calc R . . N8 N 0.3148(10) -1.1805(9) 0.5883(5) 0.074(4) Uani 1 1 d . . . C1 C 0.9668(13) -1.0887(12) 0.5488(7) 0.087(6) Uani 1 1 d . . . H1A H 0.9873 -1.0365 0.5517 0.131 Uiso 1 1 calc R . . H1B H 0.9482 -1.0973 0.5218 0.131 Uiso 1 1 calc R . . H1C H 1.0156 -1.1232 0.5555 0.131 Uiso 1 1 calc R . . N6 N 0.6549(8) -0.9567(7) 0.5705(4) 0.050(3) Uani 1 1 d . . . C18 C 0.5319(10) -1.1943(9) 0.7456(5) 0.055(4) Uani 1 1 d . . . C15 C 0.5715(13) -0.8511(10) 0.6063(6) 0.072(5) Uani 1 1 d . . . H15A H 0.5117 -0.8695 0.5995 0.108 Uiso 1 1 calc R . . H15B H 0.5722 -0.7959 0.6052 0.108 Uiso 1 1 calc R . . H15C H 0.5868 -0.8677 0.6327 0.108 Uiso 1 1 calc R . . C13 C 0.7024(11) -0.8375(9) 0.5569(5) 0.063(4) Uani 1 1 d . . . H13 H 0.7082 -0.7843 0.5578 0.075 Uiso 1 1 calc R . . C4 C 0.7923(11) -1.1366(9) 0.6242(4) 0.052(4) Uani 1 1 d . . . N9 N 0.5417(10) -1.1774(10) 0.7142(4) 0.071(4) Uani 1 1 d . . . C14 C 0.6377(12) -0.8816(8) 0.5784(5) 0.056(4) Uani 1 1 d . . . C2 C 0.8859(11) -1.1029(9) 0.5767(5) 0.054(4) Uani 1 1 d . . . C6 C 0.7770(18) -1.1055(17) 0.4449(6) 0.123(10) Uani 1 1 d . . . H6A H 0.7743 -1.0538 0.4350 0.184 Uiso 1 1 calc R . . H6B H 0.7723 -1.1410 0.4231 0.184 Uiso 1 1 calc R . . H6C H 0.8339 -1.1134 0.4585 0.184 Uiso 1 1 calc R . . C7 C 0.6985(16) -1.1188(12) 0.4736(5) 0.079(6) Uani 1 1 d . . . B1 B 0.7687(12) -1.0329(10) 0.5302(6) 0.055(4) Uani 1 1 d . . . S7 S 0.2410(4) -1.1171(4) 0.71808(17) 0.101(2) Uani 1 1 d . . . S6 S 0.5102(3) -1.2224(3) 0.79145(13) 0.0758(14) Uani 1 1 d . . . S5 S 0.1320(4) -1.1947(4) 0.61440(16) 0.0959(19) Uani 1 1 d . . . C8 C 0.6217(14) -1.1598(11) 0.4688(5) 0.069(5) Uani 1 1 d . . . H8 H 0.6037 -1.1870 0.4464 0.083 Uiso 1 1 calc R . . C19 C 0.3256(12) -1.1099(9) 0.6868(5) 0.055(4) Uani 1 1 d . . . C17 C 0.2383(14) -1.1860(11) 0.6004(5) 0.072(5) Uani 1 1 d . . . C11 C 0.8304(16) -0.8696(12) 0.5064(7) 0.101(7) Uani 1 1 d . . . H11A H 0.8873 -0.8694 0.5206 0.151 Uiso 1 1 calc R . . H11B H 0.8211 -0.8205 0.4941 0.151 Uiso 1 1 calc R . . H11C H 0.8317 -0.9089 0.4864 0.151 Uiso 1 1 calc R . . C10 C 0.4843(14) -1.1907(11) 0.5118(6) 0.088(6) Uani 1 1 d . . . H10A H 0.4904 -1.2263 0.5334 0.132 Uiso 1 1 calc R . . H10B H 0.4643 -1.2177 0.4884 0.132 Uiso 1 1 calc R . . H10C H 0.4404 -1.1519 0.5186 0.132 Uiso 1 1 calc R . . N7 N 0.3822(12) -0.9223(8) 0.6566(5) 0.078(5) Uani 1 1 d . . . C16 C 0.3304(14) -0.8815(10) 0.6677(8) 0.090(7) Uani 1 1 d . . . N11 N 0.9669(13) -0.9371(8) 0.6870(5) 0.083(5) Uani 1 1 d . . . C27 C 1.014(3) -0.895(2) 0.7212(11) 0.170(8) Uani 1 1 d U . . H27A H 1.0597 -0.8614 0.7100 0.204 Uiso 1 1 calc R . . H27B H 0.9685 -0.8627 0.7340 0.204 Uiso 1 1 calc R . . C23 C 1.021(2) -1.0025(14) 0.6689(10) 0.138(10) Uani 1 1 d U . . H23A H 0.9839 -1.0305 0.6498 0.166 Uiso 1 1 calc R . . H23B H 1.0410 -1.0379 0.6894 0.166 Uiso 1 1 calc R . . C25 C 0.941(3) -0.8798(16) 0.6578(10) 0.182(16) Uani 1 1 d U . . H25A H 0.9957 -0.8605 0.6448 0.218 Uiso 1 1 calc R . . H25B H 0.9121 -0.8369 0.6712 0.218 Uiso 1 1 calc R . . C26 C 1.057(3) -0.941(2) 0.7514(10) 0.169(14) Uani 1 1 d U . . H26A H 1.0106 -0.9651 0.7675 0.254 Uiso 1 1 calc R . . H26B H 1.0943 -0.9089 0.7678 0.254 Uiso 1 1 calc R . . H26C H 1.0936 -0.9799 0.7391 0.254 Uiso 1 1 calc R . . C22 C 1.105(3) -0.964(3) 0.6477(14) 0.201(17) Uani 1 1 d U . . H22A H 1.1426 -1.0025 0.6356 0.301 Uiso 1 1 calc R . . H22B H 1.1409 -0.9359 0.6670 0.301 Uiso 1 1 calc R . . H22C H 1.0841 -0.9285 0.6276 0.301 Uiso 1 1 calc R . . C21 C 0.892(2) -0.9891(19) 0.7060(13) 0.171(13) Uani 1 1 d U . . H21A H 0.8651 -1.0227 0.6863 0.206 Uiso 1 1 calc R . . H21B H 0.9176 -1.0202 0.7273 0.206 Uiso 1 1 calc R . . Cu4 Cu 0.15720(15) -1.20830(13) 0.68352(7) 0.0699(6) Uani 1 1 d . . . C20 C 0.820(3) -0.9306(19) 0.7226(11) 0.170(8) Uani 1 1 d U . . H20A H 0.8363 -0.9164 0.7493 0.255 Uiso 1 1 calc R . . H20B H 0.7608 -0.9541 0.7226 0.255 Uiso 1 1 calc R . . H20C H 0.8191 -0.8856 0.7061 0.255 Uiso 1 1 calc R . . S4 S 0.2563(5) -0.8214(4) 0.6888(4) 0.168(5) Uani 1 1 d . . . C24 C 0.877(3) -0.911(2) 0.6265(11) 0.170(8) Uani 1 1 d U . . H24A H 0.8616 -0.9632 0.6327 0.255 Uiso 1 1 calc R . . H24B H 0.9055 -0.9085 0.6009 0.255 Uiso 1 1 calc R . . H24C H 0.8219 -0.8804 0.6262 0.255 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 0.0463(4) 0.0420(4) 0.0418(4) 0.0007(2) 0.0005(3) 0.0008(2) Cu3 0.0507(10) 0.0570(12) 0.0729(14) 0.0021(10) -0.0038(9) -0.0083(9) Cu2 0.0780(14) 0.0644(12) 0.0449(11) 0.0063(9) 0.0004(10) -0.0050(11) Cu1 0.0630(12) 0.0587(12) 0.0712(14) -0.0100(10) 0.0092(11) 0.0063(10) S3 0.062(2) 0.059(2) 0.044(2) -0.0065(18) 0.0027(18) -0.0069(19) S1 0.054(2) 0.049(2) 0.066(3) 0.0051(19) -0.007(2) 0.0057(17) S2 0.062(2) 0.0428(19) 0.051(2) 0.0020(17) -0.0036(18) 0.0005(17) N1 0.045(7) 0.058(7) 0.049(7) 0.002(6) -0.001(6) 0.001(6) N2 0.044(6) 0.050(7) 0.047(7) 0.008(6) 0.008(6) -0.009(6) N4 0.056(7) 0.061(8) 0.052(8) 0.006(6) -0.006(6) 0.010(6) C12 0.055(9) 0.050(9) 0.079(12) 0.019(8) -0.007(9) -0.010(8) N3 0.063(8) 0.052(7) 0.032(6) 0.001(5) 0.001(6) 0.007(6) N5 0.065(8) 0.051(7) 0.041(7) 0.002(6) 0.004(6) 0.006(6) C5 0.066(11) 0.093(13) 0.070(11) 0.039(10) -0.025(9) 0.010(10) C9 0.079(11) 0.043(8) 0.053(9) -0.018(7) -0.016(8) -0.010(8) N10 0.063(9) 0.092(11) 0.071(10) -0.007(9) 0.011(8) -0.023(8) C3 0.034(7) 0.057(9) 0.075(11) 0.001(8) 0.001(7) 0.016(7) N8 0.047(8) 0.079(10) 0.096(12) -0.009(9) 0.008(8) -0.017(7) C1 0.062(11) 0.096(14) 0.103(16) 0.015(13) 0.020(11) 0.024(10) N6 0.049(7) 0.050(7) 0.051(7) 0.010(6) 0.014(6) 0.000(6) C18 0.049(8) 0.064(10) 0.051(10) 0.008(8) -0.010(7) 0.008(7) C15 0.085(12) 0.048(9) 0.082(12) -0.003(9) 0.021(10) 0.018(9) C13 0.058(10) 0.047(9) 0.083(12) 0.011(9) -0.007(9) -0.006(8) C4 0.059(9) 0.058(9) 0.040(8) -0.006(7) -0.015(7) -0.008(7) N9 0.067(9) 0.107(12) 0.040(8) 0.023(8) -0.013(7) -0.012(8) C14 0.073(11) 0.043(8) 0.052(9) -0.002(7) 0.000(8) -0.002(8) C2 0.062(9) 0.053(9) 0.046(9) -0.012(7) 0.009(7) 0.009(8) C6 0.14(2) 0.18(3) 0.045(12) -0.050(14) 0.013(13) 0.00(2) C7 0.115(16) 0.088(13) 0.035(9) -0.003(9) 0.007(10) 0.043(13) B1 0.051(10) 0.045(9) 0.068(12) 0.010(9) 0.009(9) 0.000(8) S7 0.094(4) 0.120(5) 0.088(4) -0.054(3) 0.030(3) -0.052(3) S6 0.062(3) 0.118(4) 0.047(2) 0.010(2) 0.000(2) -0.017(3) S5 0.063(3) 0.157(6) 0.067(3) -0.033(3) 0.004(2) -0.018(3) C8 0.084(12) 0.081(12) 0.042(9) -0.009(9) -0.009(9) -0.003(11) C19 0.070(11) 0.052(9) 0.042(9) -0.002(7) -0.012(8) -0.008(8) C17 0.090(15) 0.083(13) 0.044(9) -0.011(8) -0.019(9) -0.012(11) C11 0.121(18) 0.064(12) 0.117(19) 0.033(12) 0.004(15) -0.026(12) C10 0.101(15) 0.074(13) 0.089(15) -0.034(11) -0.009(12) -0.019(11) N7 0.086(10) 0.048(8) 0.101(13) -0.027(8) 0.037(10) 0.009(8) C16 0.082(13) 0.044(10) 0.14(2) -0.023(11) 0.042(14) -0.021(9) N11 0.115(14) 0.057(9) 0.077(11) 0.018(8) -0.001(10) 0.008(9) C27 0.21(2) 0.149(16) 0.153(17) 0.005(12) -0.063(14) 0.011(13) C23 0.17(3) 0.077(16) 0.17(3) -0.019(17) -0.04(2) -0.002(16) C25 0.34(4) 0.083(17) 0.13(2) 0.010(16) -0.11(3) 0.04(2) C26 0.21(3) 0.20(3) 0.10(2) -0.017(19) -0.05(2) 0.05(3) C22 0.20(4) 0.19(4) 0.21(4) -0.06(3) 0.02(3) -0.04(3) C21 0.15(3) 0.11(2) 0.25(4) 0.01(2) -0.01(3) -0.045(16) Cu4 0.0669(13) 0.0743(14) 0.0686(14) -0.0219(11) 0.0116(11) -0.0139(11) C20 0.21(2) 0.149(16) 0.153(17) 0.005(12) -0.063(14) 0.011(13) S4 0.099(5) 0.098(5) 0.306(12) -0.081(6) 0.122(7) -0.027(4) C24 0.21(2) 0.149(16) 0.153(17) 0.005(12) -0.063(14) 0.011(13) _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 N4 2.263(13) . ? W1 S3 2.281(4) . ? W1 N6 2.288(12) . ? W1 S1 2.288(4) . ? W1 N2 2.294(12) . ? W1 S2 2.309(4) . ? W1 Cu3 2.637(2) . ? W1 Cu1 2.663(2) . ? W1 Cu2 2.673(2) . ? Cu3 N8 1.851(14) . ? Cu3 S1 2.217(5) . ? Cu3 S2 2.230(5) . ? Cu3 Cu1 2.847(3) . ? Cu3 Cu2 2.884(3) . ? Cu2 N9 1.908(14) . ? Cu2 S2 2.234(4) . ? Cu2 S3 2.234(5) . ? Cu2 N10 2.397(16) . ? Cu2 Cu1 2.849(3) . ? Cu1 N7 1.879(14) . ? Cu1 S1 2.240(5) . ? Cu1 S3 2.263(5) . ? Cu1 N10 2.373(16) . ? N1 C2 1.369(19) . ? N1 N2 1.370(16) . ? N1 B1 1.53(2) . ? N2 C4 1.343(18) . ? N4 C9 1.342(19) . ? N4 N3 1.367(18) . ? C12 C13 1.34(2) . ? C12 N5 1.367(19) . ? C12 C11 1.50(3) . ? N3 C7 1.35(2) . ? N3 B1 1.56(2) . ? N5 N6 1.378(16) . ? N5 B1 1.51(2) . ? C5 C4 1.51(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C9 C8 1.35(2) . ? C9 C10 1.52(2) . ? N10 C19 1.14(2) . ? C3 C2 1.36(2) . ? C3 C4 1.36(2) . ? C3 H3 0.9300 . ? N8 C17 1.19(2) . ? C1 C2 1.53(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? N6 C14 1.357(19) . ? C18 N9 1.105(19) . ? C18 S6 1.649(17) . ? C15 C14 1.45(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C13 C14 1.42(2) . ? C13 H13 0.9300 . ? C6 C7 1.52(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.34(3) . ? S7 C19 1.629(18) . ? S7 Cu4 2.318(5) . ? S6 Cu4 2.324(5) 6_657 ? S5 C17 1.63(2) . ? S5 Cu4 2.364(6) . ? C8 H8 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? N7 C16 1.10(2) . ? C16 S4 1.66(2) . ? N11 C25 1.45(3) . ? N11 C23 1.51(3) . ? N11 C27 1.52(4) . ? N11 C21 1.56(3) . ? C27 C26 1.44(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C23 C22 1.58(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 C24 1.51(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C21 C20 1.57(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? Cu4 S6 2.324(5) 6_557 ? Cu4 S4 2.346(7) 8_655 ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? S4 Cu4 2.346(7) 8_665 ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 N4 W1 S3 162.2(4) . . ? N4 W1 N6 82.3(5) . . ? S3 W1 N6 84.7(3) . . ? N4 W1 S1 85.9(3) . . ? S3 W1 S1 105.39(15) . . ? N6 W1 S1 86.2(3) . . ? N4 W1 N2 79.1(4) . . ? S3 W1 N2 86.6(3) . . ? N6 W1 N2 79.4(4) . . ? S1 W1 N2 160.4(3) . . ? N4 W1 S2 85.8(4) . . ? S3 W1 S2 104.04(15) . . ? N6 W1 S2 163.1(3) . . ? S1 W1 S2 104.91(14) . . ? N2 W1 S2 86.6(3) . . ? N4 W1 Cu3 92.2(3) . . ? S3 W1 Cu3 105.57(11) . . ? N6 W1 Cu3 139.1(3) . . ? S1 W1 Cu3 52.91(11) . . ? N2 W1 Cu3 139.5(3) . . ? S2 W1 Cu3 53.10(11) . . ? N4 W1 Cu1 139.0(3) . . ? S3 W1 Cu1 53.81(12) . . ? N6 W1 Cu1 93.3(3) . . ? S1 W1 Cu1 53.13(12) . . ? N2 W1 Cu1 140.4(3) . . ? S2 W1 Cu1 103.52(11) . . ? Cu3 W1 Cu1 64.98(7) . . ? N4 W1 Cu2 138.4(3) . . ? S3 W1 Cu2 52.88(11) . . ? N6 W1 Cu2 137.6(3) . . ? S1 W1 Cu2 104.62(12) . . ? N2 W1 Cu2 95.0(3) . . ? S2 W1 Cu2 52.66(11) . . ? Cu3 W1 Cu2 65.78(7) . . ? Cu1 W1 Cu2 64.53(7) . . ? N8 Cu3 S1 119.7(5) . . ? N8 Cu3 S2 127.6(5) . . ? S1 Cu3 S2 110.12(16) . . ? N8 Cu3 W1 173.7(5) . . ? S1 Cu3 W1 55.44(11) . . ? S2 Cu3 W1 55.88(11) . . ? N8 Cu3 Cu1 123.2(5) . . ? S1 Cu3 Cu1 50.65(13) . . ? S2 Cu3 Cu1 100.06(13) . . ? W1 Cu3 Cu1 57.95(6) . . ? N8 Cu3 Cu2 128.5(5) . . ? S1 Cu3 Cu2 100.10(13) . . ? S2 Cu3 Cu2 49.81(12) . . ? W1 Cu3 Cu2 57.71(6) . . ? Cu1 Cu3 Cu2 59.61(7) . . ? N9 Cu2 S2 125.0(5) . . ? N9 Cu2 S3 120.2(5) . . ? S2 Cu2 S3 108.18(16) . . ? N9 Cu2 N10 90.9(6) . . ? S2 Cu2 N10 105.7(4) . . ? S3 Cu2 N10 99.9(4) . . ? N9 Cu2 W1 167.7(4) . . ? S2 Cu2 W1 55.27(11) . . ? S3 Cu2 W1 54.52(11) . . ? N10 Cu2 W1 100.9(4) . . ? N9 Cu2 Cu1 129.9(5) . . ? S2 Cu2 Cu1 99.94(13) . . ? S3 Cu2 Cu1 51.15(13) . . ? N10 Cu2 Cu1 52.9(4) . . ? W1 Cu2 Cu1 57.57(6) . . ? N9 Cu2 Cu3 134.6(4) . . ? S2 Cu2 Cu3 49.71(12) . . ? S3 Cu2 Cu3 99.31(13) . . ? N10 Cu2 Cu3 58.9(4) . . ? W1 Cu2 Cu3 56.51(6) . . ? Cu1 Cu2 Cu3 59.56(7) . . ? N7 Cu1 S1 120.8(6) . . ? N7 Cu1 S3 123.7(6) . . ? S1 Cu1 S3 107.65(16) . . ? N7 Cu1 N10 92.3(6) . . ? S1 Cu1 N10 107.0(4) . . ? S3 Cu1 N10 99.8(4) . . ? N7 Cu1 W1 165.9(5) . . ? S1 Cu1 W1 54.82(11) . . ? S3 Cu1 W1 54.44(11) . . ? N10 Cu1 W1 101.8(4) . . ? N7 Cu1 Cu3 132.7(5) . . ? S1 Cu1 Cu3 49.93(12) . . ? S3 Cu1 Cu3 99.66(13) . . ? N10 Cu1 Cu3 59.7(4) . . ? W1 Cu1 Cu3 57.07(6) . . ? N7 Cu1 Cu2 133.7(6) . . ? S1 Cu1 Cu2 100.57(13) . . ? S3 Cu1 Cu2 50.24(12) . . ? N10 Cu1 Cu2 53.7(4) . . ? W1 Cu1 Cu2 57.91(6) . . ? Cu3 Cu1 Cu2 60.84(7) . . ? Cu2 S3 Cu1 78.61(15) . . ? Cu2 S3 W1 72.60(13) . . ? Cu1 S3 W1 71.75(13) . . ? Cu3 S1 Cu1 79.43(16) . . ? Cu3 S1 W1 71.65(12) . . ? Cu1 S1 W1 72.05(13) . . ? Cu3 S2 Cu2 80.48(15) . . ? Cu3 S2 W1 71.02(12) . . ? Cu2 S2 W1 72.08(12) . . ? C2 N1 N2 107.7(12) . . ? C2 N1 B1 129.3(13) . . ? N2 N1 B1 123.0(12) . . ? C4 N2 N1 107.3(12) . . ? C4 N2 W1 133.1(10) . . ? N1 N2 W1 119.6(9) . . ? C9 N4 N3 103.2(13) . . ? C9 N4 W1 134.6(12) . . ? N3 N4 W1 122.1(10) . . ? C13 C12 N5 106.9(14) . . ? C13 C12 C11 131.1(16) . . ? N5 C12 C11 121.9(16) . . ? C7 N3 N4 110.4(15) . . ? C7 N3 B1 128.9(16) . . ? N4 N3 B1 120.5(12) . . ? C12 N5 N6 110.2(12) . . ? C12 N5 B1 127.7(13) . . ? N6 N5 B1 122.0(12) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C9 C8 112.6(16) . . ? N4 C9 C10 123.5(16) . . ? C8 C9 C10 123.8(15) . . ? C19 N10 Cu1 140.0(15) . . ? C19 N10 Cu2 139.4(15) . . ? Cu1 N10 Cu2 73.3(4) . . ? C2 C3 C4 106.8(14) . . ? C2 C3 H3 126.6 . . ? C4 C3 H3 126.6 . . ? C17 N8 Cu3 148.4(15) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C14 N6 N5 106.9(12) . . ? C14 N6 W1 132.5(10) . . ? N5 N6 W1 120.6(9) . . ? N9 C18 S6 175.8(16) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C13 C14 108.7(14) . . ? C12 C13 H13 125.6 . . ? C14 C13 H13 125.6 . . ? N2 C4 C3 110.0(14) . . ? N2 C4 C5 126.4(14) . . ? C3 C4 C5 123.6(14) . . ? C18 N9 Cu2 169.4(17) . . ? N6 C14 C13 107.2(14) . . ? N6 C14 C15 127.1(14) . . ? C13 C14 C15 125.4(15) . . ? C3 C2 N1 108.3(13) . . ? C3 C2 C1 131.1(15) . . ? N1 C2 C1 120.7(15) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N3 108.2(17) . . ? C8 C7 C6 129.8(17) . . ? N3 C7 C6 122(2) . . ? N5 B1 N1 108.3(14) . . ? N5 B1 N3 110.6(13) . . ? N1 B1 N3 105.6(12) . . ? C19 S7 Cu4 97.6(6) . . ? C18 S6 Cu4 97.4(6) . 6_657 ? C17 S5 Cu4 98.3(6) . . ? C7 C8 C9 105.5(15) . . ? C7 C8 H8 127.3 . . ? C9 C8 H8 127.3 . . ? N10 C19 S7 173.3(16) . . ? N8 C17 S5 176.9(16) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 N7 Cu1 174(2) . . ? N7 C16 S4 175(3) . . ? C25 N11 C23 112(2) . . ? C25 N11 C27 107(2) . . ? C23 N11 C27 115(2) . . ? C25 N11 C21 120(3) . . ? C23 N11 C21 95(2) . . ? C27 N11 C21 106(3) . . ? C26 C27 N11 118(3) . . ? C26 C27 H27A 107.9 . . ? N11 C27 H27A 107.9 . . ? C26 C27 H27B 107.9 . . ? N11 C27 H27B 107.9 . . ? H27A C27 H27B 107.2 . . ? N11 C23 C22 105(2) . . ? N11 C23 H23A 110.7 . . ? C22 C23 H23A 110.7 . . ? N11 C23 H23B 110.6 . . ? C22 C23 H23B 110.6 . . ? H23A C23 H23B 108.8 . . ? N11 C25 C24 113(3) . . ? N11 C25 H25A 109.0 . . ? C24 C25 H25A 109.0 . . ? N11 C25 H25B 109.0 . . ? C24 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.4 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C21 N11 104(2) . . ? C20 C21 H21A 110.9 . . ? N11 C21 H21A 110.9 . . ? C20 C21 H21B 111.0 . . ? N11 C21 H21B 110.9 . . ? H21A C21 H21B 109.0 . . ? S7 Cu4 S6 112.38(19) . 6_557 ? S7 Cu4 S4 104.5(3) . 8_655 ? S6 Cu4 S4 112.6(3) 6_557 8_655 ? S7 Cu4 S5 120.4(2) . . ? S6 Cu4 S5 102.83(19) 6_557 . ? S4 Cu4 S5 104.0(3) 8_655 . ? C21 C20 H20A 109.4 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 S4 Cu4 98.2(6) . 8_665 ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.4 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.191 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.137 #===END