# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1577 data_p21c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Cu3 Mo N4 O S3' _chemical_formula_weight 701.11 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/c 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 11.952(2) _cell_length_b 11.247(2) _cell_length_c 18.779(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.89(3) _cell_angle_gamma 90.00 _cell_volume 2470.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 3.316 _exptl_absorpt_correction_type abscor _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 Raxis-IV' _diffrn_measurement_method 'oscillation frames' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4512 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2029 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4512 _reflns_number_gt 4032 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _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^)+(0.0679P)^2^+1.0700P] 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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4512 _refine_ls_number_parameters 281 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.011 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.22005(3) 0.47227(3) 0.113193(16) 0.04105(8) Uani 1 1 d . . . Cu1 Cu 0.08127(4) 0.28369(4) 0.11772(3) 0.05085(12) Uani 1 1 d . . . Cu2 Cu 0.37015(4) 0.37941(4) 0.22551(3) 0.05180(13) Uani 1 1 d . . . Cu3 Cu 0.11016(4) 0.57389(4) 0.20678(3) 0.05326(13) Uani 1 1 d . . . S1 S 0.02807(8) 0.48084(9) 0.10424(5) 0.0507(2) Uani 1 1 d . . . S2 S 0.27513(8) 0.27951(8) 0.12599(5) 0.0481(2) Uani 1 1 d . . . S3 S 0.30030(9) 0.56901(9) 0.21783(6) 0.0528(3) Uani 1 1 d . . . N1 N 0.0133(3) 0.1981(3) 0.18931(19) 0.0607(10) Uani 1 1 d . . . N2 N 0.0181(3) 0.2032(3) 0.01612(18) 0.0575(9) Uani 1 1 d . . . N3 N 0.5418(3) 0.3981(3) 0.21177(19) 0.0532(9) Uani 1 1 d . . . N4 N 0.3794(3) 0.2910(3) 0.32001(18) 0.0525(9) Uani 1 1 d . . . C6 C 0.0837(4) 0.1310(4) -0.0143(3) 0.0779(15) Uani 1 1 d . . . H6A H 0.1575 0.1155 0.0113 0.093 Uiso 1 1 calc R . . O1 O 0.2583(2) 0.5356(3) 0.03926(15) 0.0617(8) Uani 1 1 d . . . C1 C -0.0314(3) 0.1525(4) 0.2288(2) 0.0532(10) Uani 1 1 d . . . C2 C -0.0861(5) 0.2237(4) -0.0208(3) 0.0851(18) Uani 1 1 d . . . H2A H -0.1343 0.2715 -0.0001 0.102 Uiso 1 1 calc R . . C3 C -0.1269(6) 0.1764(5) -0.0900(4) 0.120(2) Uani 1 1 d . . . H3A H -0.2000 0.1941 -0.1159 0.144 Uiso 1 1 calc R . . C4 C -0.0560(7) 0.1031(5) -0.1185(3) 0.115(3) Uani 1 1 d . . . H4A H -0.0812 0.0700 -0.1644 0.138 Uiso 1 1 calc R . . C5 C 0.0488(6) 0.0788(6) -0.0810(3) 0.102(2) Uani 1 1 d . . . H5A H 0.0969 0.0277 -0.0996 0.122 Uiso 1 1 calc R . . C7 C 0.5827(4) 0.3327(5) 0.1647(3) 0.0745(14) Uani 1 1 d . . . H7A H 0.5360 0.2745 0.1389 0.089 Uiso 1 1 calc R . . C8 C 0.6925(5) 0.3468(6) 0.1521(4) 0.0975(18) Uani 1 1 d . . . H8A H 0.7194 0.2982 0.1193 0.117 Uiso 1 1 calc R . . C9 C 0.7597(4) 0.4340(5) 0.1892(3) 0.0898(18) Uani 1 1 d . . . H9A H 0.8332 0.4467 0.1815 0.108 Uiso 1 1 calc R . . C10 C 0.7183(4) 0.5018(4) 0.2374(3) 0.0734(15) Uani 1 1 d . . . H10A H 0.7630 0.5611 0.2636 0.088 Uiso 1 1 calc R . . C11 C 0.6103(4) 0.4818(4) 0.2468(3) 0.0626(12) Uani 1 1 d . . . H11A H 0.5826 0.5296 0.2797 0.075 Uiso 1 1 calc R . . C12 C 0.4768(4) 0.2447(4) 0.3570(2) 0.0586(11) Uani 1 1 d . . . H12A H 0.5433 0.2576 0.3397 0.070 Uiso 1 1 calc R . . C13 C 0.4838(5) 0.1787(5) 0.4194(3) 0.0792(15) Uani 1 1 d . . . H13A H 0.5536 0.1486 0.4440 0.095 Uiso 1 1 calc R . . C14 C 0.3857(5) 0.1582(5) 0.4444(3) 0.0850(16) Uani 1 1 d . . . H14A H 0.3881 0.1138 0.4865 0.102 Uiso 1 1 calc R . . C15 C 0.2844(5) 0.2033(5) 0.4074(3) 0.0842(16) Uani 1 1 d . . . H15A H 0.2170 0.1893 0.4234 0.101 Uiso 1 1 calc R . . C16 C 0.2839(4) 0.2704(4) 0.3454(2) 0.0649(12) Uani 1 1 d . . . H16A H 0.2150 0.3023 0.3205 0.078 Uiso 1 1 calc R . . C17 C 0.3881(9) 0.5203(8) 0.4746(6) 0.204(6) Uani 1 1 d D . . C18 C 0.4618(9) 0.5352(7) 0.4317(5) 0.182(6) Uani 1 1 d D . . C19 C 0.5705(9) 0.5172(9) 0.4538(6) 0.177(4) Uani 1 1 d D . . 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 Mo1 0.03617(14) 0.04828(15) 0.04258(15) -0.00124(13) 0.01711(12) -0.00056(12) Cu1 0.0471(2) 0.0593(2) 0.0496(2) 0.0010(2) 0.0178(2) -0.0076(2) Cu2 0.0435(2) 0.0596(2) 0.0522(3) -0.0020(2) 0.0095(2) 0.0018(2) Cu3 0.0509(2) 0.0593(2) 0.0556(3) -0.0064(2) 0.0248(2) 0.0052(2) S1 0.0368(4) 0.0621(5) 0.0548(5) -0.0021(4) 0.0129(4) 0.0022(4) S2 0.0429(5) 0.0492(4) 0.0539(5) -0.0079(4) 0.0142(4) 0.0020(4) S3 0.0446(5) 0.0547(5) 0.0596(6) -0.0121(4) 0.0118(4) -0.0018(4) N1 0.0557(19) 0.071(2) 0.060(2) 0.0059(17) 0.0219(16) -0.0054(17) N2 0.060(2) 0.0600(18) 0.0510(19) 0.0007(15) 0.0083(16) -0.0188(16) N3 0.0386(16) 0.0652(18) 0.0577(19) 0.0043(16) 0.0143(14) 0.0028(15) N4 0.0511(18) 0.0574(17) 0.0519(18) -0.0007(15) 0.0174(15) 0.0029(15) C6 0.078(3) 0.094(3) 0.067(3) -0.026(2) 0.027(2) -0.022(3) O1 0.0603(16) 0.0691(16) 0.0623(16) 0.0063(14) 0.0277(14) 0.0034(14) C1 0.0481(19) 0.063(2) 0.054(2) 0.0076(18) 0.0245(17) -0.0049(18) C2 0.090(4) 0.061(2) 0.088(4) 0.001(3) -0.018(3) -0.006(3) C3 0.122(5) 0.079(3) 0.119(5) 0.005(3) -0.066(4) -0.004(3) C4 0.159(7) 0.090(4) 0.078(4) -0.015(3) -0.018(4) -0.030(4) C5 0.115(5) 0.114(4) 0.080(4) -0.031(3) 0.029(3) -0.035(4) C7 0.053(2) 0.088(3) 0.089(3) -0.018(3) 0.030(2) 0.004(2) C8 0.077(3) 0.114(4) 0.116(4) -0.012(3) 0.053(3) 0.010(3) C9 0.045(2) 0.112(4) 0.116(4) 0.023(3) 0.025(3) -0.004(3) C10 0.048(2) 0.075(3) 0.093(4) 0.012(3) 0.006(2) -0.008(2) C11 0.043(2) 0.074(3) 0.069(3) 0.000(2) 0.006(2) -0.001(2) C12 0.050(2) 0.070(2) 0.059(2) 0.004(2) 0.0187(19) 0.010(2) C13 0.087(3) 0.085(3) 0.068(3) 0.019(3) 0.021(3) 0.023(3) C14 0.126(4) 0.075(3) 0.065(3) 0.012(2) 0.045(3) 0.011(3) C15 0.089(3) 0.093(3) 0.086(3) 0.003(3) 0.053(3) -0.005(3) C16 0.050(2) 0.081(3) 0.069(3) -0.001(2) 0.024(2) -0.001(2) C17 0.240(12) 0.125(6) 0.217(11) -0.050(7) -0.024(10) -0.037(8) C18 0.315(16) 0.095(5) 0.121(7) -0.009(5) 0.007(8) -0.045(7) C19 0.251(11) 0.134(6) 0.167(8) -0.034(6) 0.093(8) -0.075(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 Mo1 O1 1.705(3) . ? Mo1 S2 2.2640(10) . ? Mo1 S1 2.2679(11) . ? Mo1 S3 2.2779(12) . ? Mo1 Cu3 2.6591(8) . ? Mo1 Cu2 2.6829(10) . ? Mo1 Cu1 2.7046(7) . ? Cu1 N1 1.961(4) . ? Cu1 N2 2.106(3) . ? Cu1 S2 2.2904(12) . ? Cu1 S1 2.3062(12) . ? Cu2 N4 2.017(3) . ? Cu2 N3 2.130(3) . ? Cu2 S2 2.2738(12) . ? Cu2 S3 2.2837(12) . ? Cu3 C1 1.898(4) 2 ? Cu3 S1 2.2332(12) . ? Cu3 S3 2.2397(12) . ? N1 C1 1.123(5) . ? N2 C2 1.315(6) . ? N2 C6 1.336(6) . ? N3 C7 1.318(6) . ? N3 C11 1.330(5) . ? N4 C12 1.332(5) . ? N4 C16 1.345(6) . ? C6 C5 1.368(7) . ? C1 Cu3 1.898(4) 2_545 ? C2 C3 1.395(8) . ? C3 C4 1.368(10) . ? C4 C5 1.333(9) . ? C7 C8 1.390(7) . ? C8 C9 1.364(8) . ? C9 C10 1.352(8) . ? C10 C11 1.356(7) . ? C12 C13 1.375(6) . ? C13 C14 1.369(8) . ? C14 C15 1.363(8) . ? C15 C16 1.386(7) . ? C17 C18 1.321(12) . ? C17 C19 1.400(14) 3_666 ? C18 C19 1.296(12) . ? C19 C17 1.400(14) 3_666 ? 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 O1 Mo1 S2 111.45(10) . . ? O1 Mo1 S1 111.05(10) . . ? S2 Mo1 S1 108.43(4) . . ? O1 Mo1 S3 111.53(10) . . ? S2 Mo1 S3 107.71(4) . . ? S1 Mo1 S3 106.47(5) . . ? O1 Mo1 Cu3 127.63(10) . . ? S2 Mo1 Cu3 120.92(3) . . ? S1 Mo1 Cu3 53.19(3) . . ? S3 Mo1 Cu3 53.28(3) . . ? O1 Mo1 Cu2 123.68(10) . . ? S2 Mo1 Cu2 53.92(3) . . ? S1 Mo1 Cu2 125.26(4) . . ? S3 Mo1 Cu2 54.07(3) . . ? Cu3 Mo1 Cu2 89.37(2) . . ? O1 Mo1 Cu1 128.50(10) . . ? S2 Mo1 Cu1 54.02(3) . . ? S1 Mo1 Cu1 54.41(3) . . ? S3 Mo1 Cu1 119.97(3) . . ? Cu3 Mo1 Cu1 85.80(2) . . ? Cu2 Mo1 Cu1 89.15(2) . . ? N1 Cu1 N2 106.74(14) . . ? N1 Cu1 S2 119.99(11) . . ? N2 Cu1 S2 102.80(11) . . ? N1 Cu1 S1 113.78(11) . . ? N2 Cu1 S1 105.94(10) . . ? S2 Cu1 S1 106.22(4) . . ? N1 Cu1 Mo1 138.59(11) . . ? N2 Cu1 Mo1 114.61(10) . . ? S2 Cu1 Mo1 53.12(3) . . ? S1 Cu1 Mo1 53.10(3) . . ? N4 Cu2 N3 106.00(14) . . ? N4 Cu2 S2 114.02(10) . . ? N3 Cu2 S2 106.24(10) . . ? N4 Cu2 S3 117.96(10) . . ? N3 Cu2 S3 104.40(9) . . ? S2 Cu2 S3 107.18(4) . . ? N4 Cu2 Mo1 142.19(10) . . ? N3 Cu2 Mo1 111.78(9) . . ? S2 Cu2 Mo1 53.59(3) . . ? S3 Cu2 Mo1 53.87(3) . . ? C1 Cu3 S1 125.50(12) 2 . ? C1 Cu3 S3 125.40(12) 2 . ? S1 Cu3 S3 109.00(5) . . ? C1 Cu3 Mo1 177.55(13) 2 . ? S1 Cu3 Mo1 54.39(3) . . ? S3 Cu3 Mo1 54.61(3) . . ? Cu3 S1 Mo1 72.42(4) . . ? Cu3 S1 Cu1 107.08(4) . . ? Mo1 S1 Cu1 72.49(3) . . ? Mo1 S2 Cu2 72.49(3) . . ? Mo1 S2 Cu1 72.86(3) . . ? Cu2 S2 Cu1 111.88(5) . . ? Cu3 S3 Mo1 72.11(4) . . ? Cu3 S3 Cu2 112.30(5) . . ? Mo1 S3 Cu2 72.05(4) . . ? C1 N1 Cu1 176.0(4) . . ? C2 N2 C6 117.2(4) . . ? C2 N2 Cu1 121.8(3) . . ? C6 N2 Cu1 121.0(3) . . ? C7 N3 C11 116.8(4) . . ? C7 N3 Cu2 121.7(3) . . ? C11 N3 Cu2 121.4(3) . . ? C12 N4 C16 117.5(4) . . ? C12 N4 Cu2 122.4(3) . . ? C16 N4 Cu2 120.0(3) . . ? N2 C6 C5 123.8(5) . . ? N1 C1 Cu3 178.4(4) . 2_545 ? N2 C2 C3 122.4(6) . . ? C4 C3 C2 117.9(6) . . ? C5 C4 C3 120.5(6) . . ? C4 C5 C6 118.1(6) . . ? N3 C7 C8 122.9(5) . . ? C9 C8 C7 118.2(6) . . ? C10 C9 C8 119.2(5) . . ? C9 C10 C11 118.9(5) . . ? N3 C11 C10 124.0(5) . . ? N4 C12 C13 123.3(4) . . ? C14 C13 C12 118.5(5) . . ? C15 C14 C13 119.7(5) . . ? C14 C15 C16 118.8(5) . . ? N4 C16 C15 122.3(4) . . ? C18 C17 C19 118.4(10) . 3_666 ? C19 C18 C17 122.4(10) . . ? C18 C19 C17 119.1(10) . 3_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo1 Cu1 N1 -174.6(2) . . . . ? S2 Mo1 Cu1 N1 95.40(17) . . . . ? S1 Mo1 Cu1 N1 -84.90(17) . . . . ? S3 Mo1 Cu1 N1 4.51(17) . . . . ? Cu3 Mo1 Cu1 N1 -38.23(16) . . . . ? Cu2 Mo1 Cu1 N1 51.20(16) . . . . ? O1 Mo1 Cu1 N2 2.22(17) . . . . ? S2 Mo1 Cu1 N2 -87.77(12) . . . . ? S1 Mo1 Cu1 N2 91.93(12) . . . . ? S3 Mo1 Cu1 N2 -178.65(11) . . . . ? Cu3 Mo1 Cu1 N2 138.60(11) . . . . ? Cu2 Mo1 Cu1 N2 -131.96(11) . . . . ? O1 Mo1 Cu1 S2 89.99(13) . . . . ? S1 Mo1 Cu1 S2 179.70(5) . . . . ? S3 Mo1 Cu1 S2 -90.89(5) . . . . ? Cu3 Mo1 Cu1 S2 -133.63(4) . . . . ? Cu2 Mo1 Cu1 S2 -44.19(4) . . . . ? O1 Mo1 Cu1 S1 -89.71(13) . . . . ? S2 Mo1 Cu1 S1 -179.70(5) . . . . ? S3 Mo1 Cu1 S1 89.41(5) . . . . ? Cu3 Mo1 Cu1 S1 46.67(4) . . . . ? Cu2 Mo1 Cu1 S1 136.10(4) . . . . ? O1 Mo1 Cu2 N4 -176.12(19) . . . . ? S2 Mo1 Cu2 N4 -82.79(16) . . . . ? S1 Mo1 Cu2 N4 5.14(16) . . . . ? S3 Mo1 Cu2 N4 90.35(16) . . . . ? Cu3 Mo1 Cu2 N4 47.28(15) . . . . ? Cu1 Mo1 Cu2 N4 -38.53(15) . . . . ? O1 Mo1 Cu2 N3 1.24(15) . . . . ? S2 Mo1 Cu2 N3 94.57(10) . . . . ? S1 Mo1 Cu2 N3 -177.50(10) . . . . ? S3 Mo1 Cu2 N3 -92.29(10) . . . . ? Cu3 Mo1 Cu2 N3 -135.36(10) . . . . ? Cu1 Mo1 Cu2 N3 138.83(10) . . . . ? O1 Mo1 Cu2 S2 -93.33(12) . . . . ? S1 Mo1 Cu2 S2 87.93(5) . . . . ? S3 Mo1 Cu2 S2 173.14(5) . . . . ? Cu3 Mo1 Cu2 S2 130.07(4) . . . . ? Cu1 Mo1 Cu2 S2 44.27(4) . . . . ? O1 Mo1 Cu2 S3 93.53(12) . . . . ? S2 Mo1 Cu2 S3 -173.14(5) . . . . ? S1 Mo1 Cu2 S3 -85.21(5) . . . . ? Cu3 Mo1 Cu2 S3 -43.07(4) . . . . ? Cu1 Mo1 Cu2 S3 -128.88(4) . . . . ? O1 Mo1 Cu3 C1 1(3) . . . 2 ? S2 Mo1 Cu3 C1 -179(100) . . . 2 ? S1 Mo1 Cu3 C1 -89(3) . . . 2 ? S3 Mo1 Cu3 C1 91(3) . . . 2 ? Cu2 Mo1 Cu3 C1 135(3) . . . 2 ? Cu1 Mo1 Cu3 C1 -136(3) . . . 2 ? O1 Mo1 Cu3 S1 89.39(13) . . . . ? S2 Mo1 Cu3 S1 -90.69(5) . . . . ? S3 Mo1 Cu3 S1 179.55(5) . . . . ? Cu2 Mo1 Cu3 S1 -136.82(4) . . . . ? Cu1 Mo1 Cu3 S1 -47.63(3) . . . . ? O1 Mo1 Cu3 S3 -90.16(13) . . . . ? S2 Mo1 Cu3 S3 89.75(5) . . . . ? S1 Mo1 Cu3 S3 -179.55(5) . . . . ? Cu2 Mo1 Cu3 S3 43.62(4) . . . . ? Cu1 Mo1 Cu3 S3 132.81(4) . . . . ? C1 Cu3 S1 Mo1 176.99(15) 2 . . . ? S3 Cu3 S1 Mo1 0.38(4) . . . . ? C1 Cu3 S1 Cu1 -118.33(16) 2 . . . ? S3 Cu3 S1 Cu1 65.07(5) . . . . ? Mo1 Cu3 S1 Cu1 64.69(4) . . . . ? O1 Mo1 S1 Cu3 -121.95(11) . . . . ? S2 Mo1 S1 Cu3 115.28(4) . . . . ? S3 Mo1 S1 Cu3 -0.37(4) . . . . ? Cu2 Mo1 S1 Cu3 56.92(4) . . . . ? Cu1 Mo1 S1 Cu3 115.03(4) . . . . ? O1 Mo1 S1 Cu1 123.02(11) . . . . ? S2 Mo1 S1 Cu1 0.25(4) . . . . ? S3 Mo1 S1 Cu1 -115.40(4) . . . . ? Cu3 Mo1 S1 Cu1 -115.03(4) . . . . ? Cu2 Mo1 S1 Cu1 -58.11(4) . . . . ? N1 Cu1 S1 Cu3 69.31(12) . . . . ? N2 Cu1 S1 Cu3 -173.74(11) . . . . ? S2 Cu1 S1 Cu3 -64.89(6) . . . . ? Mo1 Cu1 S1 Cu3 -64.64(4) . . . . ? N1 Cu1 S1 Mo1 133.95(12) . . . . ? N2 Cu1 S1 Mo1 -109.10(11) . . . . ? S2 Cu1 S1 Mo1 -0.25(4) . . . . ? O1 Mo1 S2 Cu2 116.81(11) . . . . ? S1 Mo1 S2 Cu2 -120.67(4) . . . . ? S3 Mo1 S2 Cu2 -5.83(4) . . . . ? Cu3 Mo1 S2 Cu2 -63.12(4) . . . . ? Cu1 Mo1 S2 Cu2 -120.41(4) . . . . ? O1 Mo1 S2 Cu1 -122.78(11) . . . . ? S1 Mo1 S2 Cu1 -0.26(4) . . . . ? S3 Mo1 S2 Cu1 114.59(4) . . . . ? Cu3 Mo1 S2 Cu1 57.29(4) . . . . ? Cu2 Mo1 S2 Cu1 120.41(4) . . . . ? N4 Cu2 S2 Mo1 138.25(11) . . . . ? N3 Cu2 S2 Mo1 -105.38(9) . . . . ? S3 Cu2 S2 Mo1 5.79(4) . . . . ? N4 Cu2 S2 Cu1 75.62(12) . . . . ? N3 Cu2 S2 Cu1 -168.01(10) . . . . ? S3 Cu2 S2 Cu1 -56.83(6) . . . . ? Mo1 Cu2 S2 Cu1 -62.63(4) . . . . ? N1 Cu1 S2 Mo1 -130.50(12) . . . . ? N2 Cu1 S2 Mo1 111.31(9) . . . . ? S1 Cu1 S2 Mo1 0.25(4) . . . . ? N1 Cu1 S2 Cu2 -68.10(13) . . . . ? N2 Cu1 S2 Cu2 173.72(10) . . . . ? S1 Cu1 S2 Cu2 62.66(5) . . . . ? Mo1 Cu1 S2 Cu2 62.41(4) . . . . ? C1 Cu3 S3 Mo1 -176.99(15) 2 . . . ? S1 Cu3 S3 Mo1 -0.38(4) . . . . ? C1 Cu3 S3 Cu2 121.85(16) 2 . . . ? S1 Cu3 S3 Cu2 -61.54(6) . . . . ? Mo1 Cu3 S3 Cu2 -61.16(4) . . . . ? O1 Mo1 S3 Cu3 121.65(11) . . . . ? S2 Mo1 S3 Cu3 -115.76(4) . . . . ? S1 Mo1 S3 Cu3 0.37(4) . . . . ? Cu2 Mo1 S3 Cu3 -121.58(4) . . . . ? Cu1 Mo1 S3 Cu3 -57.61(4) . . . . ? O1 Mo1 S3 Cu2 -116.77(11) . . . . ? S2 Mo1 S3 Cu2 5.82(4) . . . . ? S1 Mo1 S3 Cu2 121.95(4) . . . . ? Cu3 Mo1 S3 Cu2 121.58(4) . . . . ? Cu1 Mo1 S3 Cu2 63.96(4) . . . . ? N4 Cu2 S3 Cu3 -74.86(12) . . . . ? N3 Cu2 S3 Cu3 167.86(10) . . . . ? S2 Cu2 S3 Cu3 55.42(6) . . . . ? Mo1 Cu2 S3 Cu3 61.19(4) . . . . ? N4 Cu2 S3 Mo1 -136.05(11) . . . . ? N3 Cu2 S3 Mo1 106.67(10) . . . . ? S2 Cu2 S3 Mo1 -5.77(4) . . . . ? N2 Cu1 N1 C1 -76(5) . . . . ? S2 Cu1 N1 C1 168(5) . . . . ? S1 Cu1 N1 C1 41(5) . . . . ? Mo1 Cu1 N1 C1 101(5) . . . . ? N1 Cu1 N2 C2 76.9(4) . . . . ? S2 Cu1 N2 C2 -156.0(3) . . . . ? S1 Cu1 N2 C2 -44.7(4) . . . . ? Mo1 Cu1 N2 C2 -100.9(4) . . . . ? N1 Cu1 N2 C6 -104.8(4) . . . . ? S2 Cu1 N2 C6 22.3(4) . . . . ? S1 Cu1 N2 C6 133.6(3) . . . . ? Mo1 Cu1 N2 C6 77.4(3) . . . . ? N4 Cu2 N3 C7 104.8(4) . . . . ? S2 Cu2 N3 C7 -16.9(4) . . . . ? S3 Cu2 N3 C7 -130.0(3) . . . . ? Mo1 Cu2 N3 C7 -73.5(4) . . . . ? N4 Cu2 N3 C11 -79.7(3) . . . . ? S2 Cu2 N3 C11 158.6(3) . . . . ? S3 Cu2 N3 C11 45.5(3) . . . . ? Mo1 Cu2 N3 C11 101.9(3) . . . . ? N3 Cu2 N4 C12 -7.5(3) . . . . ? S2 Cu2 N4 C12 109.1(3) . . . . ? S3 Cu2 N4 C12 -123.9(3) . . . . ? Mo1 Cu2 N4 C12 170.0(2) . . . . ? N3 Cu2 N4 C16 176.9(3) . . . . ? S2 Cu2 N4 C16 -66.6(3) . . . . ? S3 Cu2 N4 C16 60.5(3) . . . . ? Mo1 Cu2 N4 C16 -5.7(4) . . . . ? C2 N2 C6 C5 0.3(7) . . . . ? Cu1 N2 C6 C5 -178.1(4) . . . . ? Cu1 N1 C1 Cu3 56(17) . . . 2_545 ? C6 N2 C2 C3 -2.1(7) . . . . ? Cu1 N2 C2 C3 176.3(4) . . . . ? N2 C2 C3 C4 2.2(9) . . . . ? C2 C3 C4 C5 -0.3(10) . . . . ? C3 C4 C5 C6 -1.3(10) . . . . ? N2 C6 C5 C4 1.4(9) . . . . ? C11 N3 C7 C8 1.2(7) . . . . ? Cu2 N3 C7 C8 176.9(4) . . . . ? N3 C7 C8 C9 -1.3(9) . . . . ? C7 C8 C9 C10 1.0(9) . . . . ? C8 C9 C10 C11 -0.7(8) . . . . ? C7 N3 C11 C10 -0.8(7) . . . . ? Cu2 N3 C11 C10 -176.5(4) . . . . ? C9 C10 C11 N3 0.6(8) . . . . ? C16 N4 C12 C13 -0.6(6) . . . . ? Cu2 N4 C12 C13 -176.4(4) . . . . ? N4 C12 C13 C14 0.8(7) . . . . ? C12 C13 C14 C15 0.0(8) . . . . ? C13 C14 C15 C16 -0.8(8) . . . . ? C12 N4 C16 C15 -0.3(7) . . . . ? Cu2 N4 C16 C15 175.6(4) . . . . ? C14 C15 C16 N4 1.0(8) . . . . ? C19 C17 C18 C19 -0.4(18) 3_666 . . . ? C17 C18 C19 C17 0.4(18) . . . 3_666 ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 0.710 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.112 data_p21n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 Cu3 N5 O S3 W' _chemical_formula_weight 829.07 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 MONOCLINIC _symmetry_space_group_name_H-M P2(1)/n 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 13.023(3) _cell_length_b 12.199(2) _cell_length_c 17.579(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.09(3) _cell_angle_gamma 90.00 _cell_volume 2781.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 6.632 _exptl_absorpt_correction_type abscor _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 0.967 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 raxis-IV' _diffrn_measurement_method 'oscillation frames' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3708 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.57 _reflns_number_total 3708 _reflns_number_gt 3127 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _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^)+(0.1660P)^2^+5.2200P] 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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0058(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3708 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.2513 _refine_ls_wR_factor_gt 0.2257 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W -0.45859(3) 0.18219(4) -0.29603(3) 0.05887(15) Uani 1 1 d . . . Cu1 Cu -0.54314(13) 0.25928(14) -0.43109(10) 0.0755(5) Uani 1 1 d . . . Cu2 Cu -0.61229(11) 0.03317(13) -0.28605(10) 0.0719(5) Uani 1 1 d . . . Cu3 Cu -0.54831(11) 0.34730(13) -0.21953(10) 0.0685(4) Uani 1 1 d . . . S1 S -0.5318(3) 0.0794(3) -0.39331(19) 0.0700(9) Uani 1 1 d . . . S2 S -0.5493(2) 0.1579(3) -0.19421(19) 0.0664(9) Uani 1 1 d . . . S3 S -0.4664(3) 0.3603(3) -0.3294(2) 0.0709(9) Uani 1 1 d . . . N1 N -0.6838(9) 0.3201(9) -0.4702(7) 0.077(3) Uani 1 1 d . . . N2 N -0.4470(9) 0.2830(10) -0.5160(7) 0.083(3) Uani 1 1 d . . . N3 N -0.5245(8) -0.1149(9) -0.2418(8) 0.087(4) Uani 1 1 d . . . N4 N -0.4314(8) 0.3951(8) -0.1328(6) 0.074(3) Uani 1 1 d . . . N5 N -0.6752(10) 0.4360(10) -0.2124(7) 0.088(4) Uani 1 1 d . . . O1 O -0.3352(6) 0.1420(8) -0.2738(5) 0.074(3) Uani 1 1 d . . . C1 C -0.7483(13) 0.3524(17) -0.4215(9) 0.113(6) Uani 1 1 d . . . H1A H -0.7300 0.3459 -0.3694 0.136 Uiso 1 1 calc R . . C2 C -0.8442(12) 0.3966(18) -0.4472(13) 0.127(8) Uani 1 1 d . . . H2A H -0.8926 0.4133 -0.4131 0.153 Uiso 1 1 calc R . . C3 C -0.8646(13) 0.4143(17) -0.5233(12) 0.128(7) Uani 1 1 d . . . H3A H -0.9236 0.4527 -0.5409 0.154 Uiso 1 1 calc R . . C4 C -0.8008(13) 0.3770(15) -0.5736(9) 0.104(6) Uani 1 1 d . . . H4A H -0.8169 0.3840 -0.6260 0.125 Uiso 1 1 calc R . . C5 C -0.7107(13) 0.3283(12) -0.5442(11) 0.096(5) Uani 1 1 d . . . H5A H -0.6666 0.2998 -0.5780 0.115 Uiso 1 1 calc R . . C6 C -0.4442(11) 0.3732(12) -0.5581(9) 0.089(5) Uani 1 1 d . . . H6A H -0.4971 0.4234 -0.5539 0.107 Uiso 1 1 calc R . . C7 C -0.3754(11) 0.3990(15) -0.6044(10) 0.106(6) Uani 1 1 d . . . H7A H -0.3818 0.4644 -0.6316 0.127 Uiso 1 1 calc R . . C8 C -0.2924(17) 0.3298(17) -0.6137(15) 0.155(9) Uani 1 1 d . . . H8A H -0.2444 0.3435 -0.6486 0.186 Uiso 1 1 calc R . . C9 C -0.2875(15) 0.2380(16) -0.5660(11) 0.120(6) Uani 1 1 d . . . H9A H -0.2302 0.1922 -0.5635 0.144 Uiso 1 1 calc R . . C10 C -0.3695(12) 0.2153(14) -0.5218(9) 0.094(5) Uani 1 1 d . . . H10A H -0.3691 0.1493 -0.4953 0.113 Uiso 1 1 calc R . . C11 C -0.4193(12) -0.1122(12) -0.2255(13) 0.145(7) Uani 1 1 d . . . H11A H -0.3858 -0.0463 -0.2332 0.174 Uiso 1 1 calc R . . C12 C -0.3631(17) -0.1947(17) -0.200(2) 0.213(15) Uani 1 1 d . . . H12A H -0.2932 -0.1858 -0.1855 0.255 Uiso 1 1 calc R . . C13 C -0.409(2) -0.294(2) -0.196(2) 0.208(14) Uani 1 1 d . . . H13A H -0.3684 -0.3551 -0.1828 0.249 Uiso 1 1 calc R . . C14 C -0.507(2) -0.3037(14) -0.2086(14) 0.162(11) Uani 1 1 d . . . H14A H -0.5376 -0.3720 -0.2052 0.195 Uiso 1 1 calc R . . C15 C -0.5669(15) -0.2107(14) -0.2279(12) 0.107(6) Uani 1 1 d . . . H15A H -0.6383 -0.2165 -0.2311 0.129 Uiso 1 1 calc R . . C16 C -0.3348(11) 0.4279(12) -0.1453(10) 0.087(4) Uani 1 1 d . . . H16A H -0.3195 0.4351 -0.1957 0.104 Uiso 1 1 calc R . . C17 C -0.2583(12) 0.4511(15) -0.0892(10) 0.108(6) Uani 1 1 d . . . H17A H -0.1932 0.4733 -0.1008 0.129 Uiso 1 1 calc R . . C18 C -0.2814(14) 0.4404(15) -0.0168(11) 0.127(7) Uani 1 1 d . . . H18A H -0.2304 0.4520 0.0229 0.153 Uiso 1 1 calc R . . C19 C -0.3741(14) 0.4141(17) -0.0009(10) 0.124(7) Uani 1 1 d . . . H19A H -0.3909 0.4162 0.0494 0.149 Uiso 1 1 calc R . . C20 C -0.4488(15) 0.3825(15) -0.0596(9) 0.105(6) Uani 1 1 d . . . H20A H -0.5108 0.3526 -0.0472 0.126 Uiso 1 1 calc R . . C21 C -0.7519(8) 0.4815(10) -0.2091(7) 0.064(3) Uani 1 1 d . . . 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 0.0588(3) 0.0447(2) 0.0726(3) 0.0039(2) 0.0028(2) -0.00130(19) Cu1 0.0824(10) 0.0670(10) 0.0772(10) 0.0085(8) 0.0072(8) 0.0055(8) Cu2 0.0658(8) 0.0592(8) 0.0903(10) 0.0019(7) 0.0050(8) -0.0080(7) Cu3 0.0647(8) 0.0551(8) 0.0847(10) -0.0009(7) 0.0018(8) 0.0056(7) S1 0.0803(19) 0.0562(17) 0.0722(19) -0.0010(14) 0.0000(16) 0.0003(15) S2 0.0698(18) 0.0527(16) 0.077(2) 0.0044(13) 0.0057(17) -0.0041(13) S3 0.0780(19) 0.0466(15) 0.088(2) 0.0097(15) 0.0074(16) -0.0027(15) N1 0.081(7) 0.075(7) 0.073(7) 0.000(5) -0.003(6) -0.002(5) N2 0.101(8) 0.068(6) 0.083(7) 0.019(6) 0.020(6) 0.021(6) N3 0.072(6) 0.053(6) 0.135(10) 0.024(6) 0.011(7) 0.009(5) N4 0.072(6) 0.051(5) 0.095(7) 0.003(5) -0.011(6) 0.000(5) N5 0.116(8) 0.063(7) 0.085(7) 0.006(6) 0.000(7) -0.013(7) O1 0.051(4) 0.077(5) 0.094(6) 0.018(5) 0.006(4) 0.001(4) C1 0.119(11) 0.156(15) 0.067(9) -0.012(9) 0.023(9) 0.057(11) C2 0.075(9) 0.141(17) 0.165(18) -0.002(15) 0.002(11) 0.018(11) C3 0.104(11) 0.111(13) 0.160(18) -0.007(12) -0.037(12) 0.040(10) C4 0.127(12) 0.105(12) 0.074(9) -0.015(8) -0.024(9) 0.018(11) C5 0.105(10) 0.074(9) 0.101(11) -0.003(7) -0.036(9) 0.020(8) C6 0.099(10) 0.062(8) 0.109(11) 0.023(8) 0.027(9) 0.013(8) C7 0.092(9) 0.091(11) 0.140(13) 0.036(10) 0.038(10) 0.007(9) C8 0.140(14) 0.113(15) 0.23(2) 0.058(13) 0.107(14) 0.020(12) C9 0.122(12) 0.111(13) 0.131(14) 0.019(11) 0.039(11) 0.053(11) C10 0.104(11) 0.094(10) 0.087(10) 0.017(8) 0.017(9) 0.024(9) C11 0.091(10) 0.063(7) 0.28(2) 0.097(10) 0.012(12) 0.030(7) C12 0.093(12) 0.111(15) 0.45(4) 0.11(2) 0.094(19) 0.027(11) C13 0.153(18) 0.128(19) 0.32(4) 0.05(2) -0.09(2) 0.022(16) C14 0.26(3) 0.039(9) 0.18(2) 0.018(10) -0.04(2) 0.000(13) C15 0.111(11) 0.061(9) 0.151(15) -0.010(10) 0.018(11) -0.001(9) C16 0.088(9) 0.063(8) 0.111(11) 0.017(8) 0.014(8) 0.011(7) C17 0.094(9) 0.105(12) 0.115(12) 0.009(10) -0.046(9) -0.023(9) C18 0.139(11) 0.080(11) 0.146(15) 0.015(9) -0.088(11) -0.005(10) C19 0.129(13) 0.131(14) 0.104(12) -0.050(10) -0.031(11) 0.006(12) C20 0.142(14) 0.094(12) 0.080(10) -0.006(9) 0.010(10) -0.010(11) C21 0.056(6) 0.054(6) 0.081(8) -0.002(6) 0.003(6) 0.016(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 O1 1.693(8) . ? W1 S2 2.250(3) . ? W1 S3 2.251(3) . ? W1 S1 2.262(3) . ? W1 Cu1 2.6963(18) . ? W1 Cu2 2.7211(16) . ? W1 Cu3 2.7403(18) . ? Cu1 N1 2.038(12) . ? Cu1 N2 2.053(12) . ? Cu1 S1 2.294(4) . ? Cu1 S3 2.324(4) . ? Cu2 C21 1.872(11) 2_344 ? Cu2 N3 2.240(11) . ? Cu2 S1 2.307(4) . ? Cu2 S2 2.315(4) . ? Cu3 N5 1.988(13) . ? Cu3 N4 2.137(10) . ? Cu3 S3 2.293(4) . ? Cu3 S2 2.353(4) . ? N1 C1 1.31(2) . ? N1 C5 1.32(2) . ? N2 C10 1.314(19) . ? N2 C6 1.327(18) . ? N3 C15 1.32(2) . ? N3 C11 1.375(18) . ? N4 C20 1.336(19) . ? N4 C16 1.357(17) . ? N5 C21 1.150(16) . ? C1 C2 1.40(2) . ? C2 C3 1.36(3) . ? C3 C4 1.34(3) . ? C4 C5 1.38(2) . ? C6 C7 1.30(2) . ? C7 C8 1.39(3) . ? C8 C9 1.40(3) . ? C9 C10 1.40(3) . ? C11 C12 1.30(2) . ? C12 C13 1.35(3) . ? C13 C14 1.28(4) . ? C14 C15 1.40(3) . ? C16 C17 1.37(2) . ? C17 C18 1.34(3) . ? C18 C19 1.30(3) . ? C19 C20 1.41(2) . ? C21 Cu2 1.872(11) 2_354 ? 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 O1 W1 S2 109.5(3) . . ? O1 W1 S3 111.1(3) . . ? S2 W1 S3 108.63(13) . . ? O1 W1 S1 110.0(3) . . ? S2 W1 S1 108.22(12) . . ? S3 W1 S1 109.41(12) . . ? O1 W1 Cu1 127.5(3) . . ? S2 W1 Cu1 122.97(9) . . ? S3 W1 Cu1 55.15(10) . . ? S1 W1 Cu1 54.26(9) . . ? O1 W1 Cu2 118.7(3) . . ? S2 W1 Cu2 54.53(9) . . ? S3 W1 Cu2 130.20(9) . . ? S1 W1 Cu2 54.21(10) . . ? Cu1 W1 Cu2 92.55(5) . . ? O1 W1 Cu3 122.5(3) . . ? S2 W1 Cu3 55.21(9) . . ? S3 W1 Cu3 53.61(10) . . ? S1 W1 Cu3 127.52(9) . . ? Cu1 W1 Cu3 90.98(5) . . ? Cu2 W1 Cu3 96.39(5) . . ? N1 Cu1 N2 106.9(5) . . ? N1 Cu1 S1 118.6(3) . . ? N2 Cu1 S1 108.5(3) . . ? N1 Cu1 S3 112.3(3) . . ? N2 Cu1 S3 103.7(4) . . ? S1 Cu1 S3 105.81(13) . . ? N1 Cu1 W1 135.1(4) . . ? N2 Cu1 W1 117.5(3) . . ? S1 Cu1 W1 53.17(9) . . ? S3 Cu1 W1 52.64(9) . . ? C21 Cu2 N3 101.2(5) 2_344 . ? C21 Cu2 S1 122.8(4) 2_344 . ? N3 Cu2 S1 103.1(3) . . ? C21 Cu2 S2 121.9(4) 2_344 . ? N3 Cu2 S2 98.6(3) . . ? S1 Cu2 S2 104.52(13) . . ? C21 Cu2 W1 156.8(4) 2_344 . ? N3 Cu2 W1 101.9(3) . . ? S1 Cu2 W1 52.69(9) . . ? S2 Cu2 W1 52.31(9) . . ? N5 Cu3 N4 110.5(4) . . ? N5 Cu3 S3 117.8(4) . . ? N4 Cu3 S3 103.1(3) . . ? N5 Cu3 S2 120.3(4) . . ? N4 Cu3 S2 98.5(3) . . ? S3 Cu3 S2 103.78(13) . . ? N5 Cu3 W1 145.5(3) . . ? N4 Cu3 W1 104.0(3) . . ? S3 Cu3 W1 52.21(9) . . ? S2 Cu3 W1 51.75(9) . . ? W1 S1 Cu1 72.57(11) . . ? W1 S1 Cu2 73.09(11) . . ? Cu1 S1 Cu2 116.62(15) . . ? W1 S2 Cu2 73.16(11) . . ? W1 S2 Cu3 73.04(11) . . ? Cu2 S2 Cu3 121.40(15) . . ? W1 S3 Cu3 74.18(11) . . ? W1 S3 Cu1 72.21(11) . . ? Cu3 S3 Cu1 114.24(15) . . ? C1 N1 C5 119.4(14) . . ? C1 N1 Cu1 119.8(11) . . ? C5 N1 Cu1 120.8(11) . . ? C10 N2 C6 114.8(13) . . ? C10 N2 Cu1 119.3(10) . . ? C6 N2 Cu1 124.8(10) . . ? C15 N3 C11 114.0(13) . . ? C15 N3 Cu2 124.6(11) . . ? C11 N3 Cu2 121.4(9) . . ? C20 N4 C16 115.3(13) . . ? C20 N4 Cu3 119.1(10) . . ? C16 N4 Cu3 125.3(10) . . ? C21 N5 Cu3 175.8(11) . . ? N1 C1 C2 120.8(16) . . ? C3 C2 C1 118.0(18) . . ? C4 C3 C2 121.0(16) . . ? C3 C4 C5 117.1(16) . . ? N1 C5 C4 123.1(17) . . ? C7 C6 N2 127.1(15) . . ? C6 C7 C8 120.7(17) . . ? C7 C8 C9 114.3(19) . . ? C8 C9 C10 119.5(17) . . ? N2 C10 C9 123.1(16) . . ? C12 C11 N3 124.9(16) . . ? C11 C12 C13 118(2) . . ? C14 C13 C12 121(2) . . ? C13 C14 C15 119(2) . . ? N3 C15 C14 121.7(19) . . ? N4 C16 C17 124.9(16) . . ? C18 C17 C16 117.0(16) . . ? C19 C18 C17 121.2(16) . . ? C18 C19 C20 120.3(19) . . ? N4 C20 C19 120.7(17) . . ? N5 C21 Cu2 169.3(11) . 2_354 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 W1 Cu1 N1 -175.8(6) . . . . ? S2 W1 Cu1 N1 5.9(5) . . . . ? S3 W1 Cu1 N1 -84.8(5) . . . . ? S1 W1 Cu1 N1 95.5(5) . . . . ? Cu2 W1 Cu1 N1 54.4(5) . . . . ? Cu3 W1 Cu1 N1 -42.1(5) . . . . ? O1 W1 Cu1 N2 -4.6(6) . . . . ? S2 W1 Cu1 N2 177.1(4) . . . . ? S3 W1 Cu1 N2 86.4(4) . . . . ? S1 W1 Cu1 N2 -93.3(4) . . . . ? Cu2 W1 Cu1 N2 -134.4(4) . . . . ? Cu3 W1 Cu1 N2 129.1(4) . . . . ? O1 W1 Cu1 S1 88.7(4) . . . . ? S2 W1 Cu1 S1 -89.57(15) . . . . ? S3 W1 Cu1 S1 179.73(16) . . . . ? Cu2 W1 Cu1 S1 -41.13(11) . . . . ? Cu3 W1 Cu1 S1 -137.57(12) . . . . ? O1 W1 Cu1 S3 -91.0(4) . . . . ? S2 W1 Cu1 S3 90.70(15) . . . . ? S1 W1 Cu1 S3 -179.73(16) . . . . ? Cu2 W1 Cu1 S3 139.14(12) . . . . ? Cu3 W1 Cu1 S3 42.70(12) . . . . ? O1 W1 Cu2 C21 178.1(11) . . . 2_344 ? S2 W1 Cu2 C21 83.7(10) . . . 2_344 ? S3 W1 Cu2 C21 -1.2(10) . . . 2_344 ? S1 W1 Cu2 C21 -87.1(10) . . . 2_344 ? Cu1 W1 Cu2 C21 -45.9(10) . . . 2_344 ? Cu3 W1 Cu2 C21 45.4(10) . . . 2_344 ? O1 W1 Cu2 N3 2.6(5) . . . . ? S2 W1 Cu2 N3 -91.8(4) . . . . ? S3 W1 Cu2 N3 -176.7(4) . . . . ? S1 W1 Cu2 N3 97.5(4) . . . . ? Cu1 W1 Cu2 N3 138.7(4) . . . . ? Cu3 W1 Cu2 N3 -130.1(4) . . . . ? O1 W1 Cu2 S1 -94.9(4) . . . . ? S2 W1 Cu2 S1 170.74(15) . . . . ? S3 W1 Cu2 S1 85.83(17) . . . . ? Cu1 W1 Cu2 S1 41.16(11) . . . . ? Cu3 W1 Cu2 S1 132.44(11) . . . . ? O1 W1 Cu2 S2 94.4(4) . . . . ? S3 W1 Cu2 S2 -84.91(17) . . . . ? S1 W1 Cu2 S2 -170.74(15) . . . . ? Cu1 W1 Cu2 S2 -129.58(11) . . . . ? Cu3 W1 Cu2 S2 -38.30(11) . . . . ? O1 W1 Cu3 N5 178.6(7) . . . . ? S2 W1 Cu3 N5 -89.2(6) . . . . ? S3 W1 Cu3 N5 85.1(6) . . . . ? S1 W1 Cu3 N5 -2.3(6) . . . . ? Cu1 W1 Cu3 N5 41.4(6) . . . . ? Cu2 W1 Cu3 N5 -51.3(6) . . . . ? O1 W1 Cu3 N4 -2.4(5) . . . . ? S2 W1 Cu3 N4 89.8(3) . . . . ? S3 W1 Cu3 N4 -95.8(3) . . . . ? S1 W1 Cu3 N4 176.8(3) . . . . ? Cu1 W1 Cu3 N4 -139.6(3) . . . . ? Cu2 W1 Cu3 N4 127.8(3) . . . . ? O1 W1 Cu3 S3 93.5(4) . . . . ? S2 W1 Cu3 S3 -174.34(14) . . . . ? S1 W1 Cu3 S3 -87.40(16) . . . . ? Cu1 W1 Cu3 S3 -43.74(11) . . . . ? Cu2 W1 Cu3 S3 -136.41(12) . . . . ? O1 W1 Cu3 S2 -92.2(4) . . . . ? S3 W1 Cu3 S2 174.34(14) . . . . ? S1 W1 Cu3 S2 86.94(15) . . . . ? Cu1 W1 Cu3 S2 130.60(10) . . . . ? Cu2 W1 Cu3 S2 37.93(10) . . . . ? O1 W1 S1 Cu1 -122.5(3) . . . . ? S2 W1 S1 Cu1 117.96(11) . . . . ? S3 W1 S1 Cu1 -0.24(14) . . . . ? Cu2 W1 S1 Cu1 125.90(12) . . . . ? Cu3 W1 S1 Cu1 58.27(13) . . . . ? O1 W1 S1 Cu2 111.6(3) . . . . ? S2 W1 S1 Cu2 -7.93(13) . . . . ? S3 W1 S1 Cu2 -126.13(12) . . . . ? Cu1 W1 S1 Cu2 -125.90(12) . . . . ? Cu3 W1 S1 Cu2 -67.63(12) . . . . ? N1 Cu1 S1 W1 -126.9(4) . . . . ? N2 Cu1 S1 W1 111.0(4) . . . . ? S3 Cu1 S1 W1 0.22(13) . . . . ? N1 Cu1 S1 Cu2 -66.8(4) . . . . ? N2 Cu1 S1 Cu2 171.1(4) . . . . ? S3 Cu1 S1 Cu2 60.33(18) . . . . ? W1 Cu1 S1 Cu2 60.11(12) . . . . ? C21 Cu2 S1 W1 152.1(5) 2_344 . . . ? N3 Cu2 S1 W1 -95.1(3) . . . . ? S2 Cu2 S1 W1 7.56(12) . . . . ? C21 Cu2 S1 Cu1 92.3(5) 2_344 . . . ? N3 Cu2 S1 Cu1 -154.9(3) . . . . ? S2 Cu2 S1 Cu1 -52.27(18) . . . . ? W1 Cu2 S1 Cu1 -59.83(13) . . . . ? O1 W1 S2 Cu2 -111.9(4) . . . . ? S3 W1 S2 Cu2 126.60(11) . . . . ? S1 W1 S2 Cu2 7.90(13) . . . . ? Cu1 W1 S2 Cu2 66.61(11) . . . . ? Cu3 W1 S2 Cu2 131.41(11) . . . . ? O1 W1 S2 Cu3 116.7(3) . . . . ? S3 W1 S2 Cu3 -4.81(12) . . . . ? S1 W1 S2 Cu3 -123.51(11) . . . . ? Cu1 W1 S2 Cu3 -64.80(11) . . . . ? Cu2 W1 S2 Cu3 -131.41(11) . . . . ? C21 Cu2 S2 W1 -152.6(5) 2_344 . . . ? N3 Cu2 S2 W1 98.4(3) . . . . ? S1 Cu2 S2 W1 -7.60(12) . . . . ? C21 Cu2 S2 Cu3 -95.4(5) 2_344 . . . ? N3 Cu2 S2 Cu3 155.6(3) . . . . ? S1 Cu2 S2 Cu3 49.59(19) . . . . ? W1 Cu2 S2 Cu3 57.19(13) . . . . ? N5 Cu3 S2 W1 139.0(4) . . . . ? N4 Cu3 S2 W1 -101.2(3) . . . . ? S3 Cu3 S2 W1 4.61(12) . . . . ? N5 Cu3 S2 Cu2 81.7(4) . . . . ? N4 Cu3 S2 Cu2 -158.5(3) . . . . ? S3 Cu3 S2 Cu2 -52.64(19) . . . . ? W1 Cu3 S2 Cu2 -57.25(14) . . . . ? O1 W1 S3 Cu3 -115.6(4) . . . . ? S2 W1 S3 Cu3 4.91(13) . . . . ? S1 W1 S3 Cu3 122.86(12) . . . . ? Cu1 W1 S3 Cu3 122.62(12) . . . . ? Cu2 W1 S3 Cu3 63.78(14) . . . . ? O1 W1 S3 Cu1 121.8(4) . . . . ? S2 W1 S3 Cu1 -117.71(11) . . . . ? S1 W1 S3 Cu1 0.23(14) . . . . ? Cu2 W1 S3 Cu1 -58.84(15) . . . . ? Cu3 W1 S3 Cu1 -122.62(12) . . . . ? N5 Cu3 S3 W1 -140.3(4) . . . . ? N4 Cu3 S3 W1 97.8(3) . . . . ? S2 Cu3 S3 W1 -4.58(12) . . . . ? N5 Cu3 S3 Cu1 -78.7(4) . . . . ? N4 Cu3 S3 Cu1 159.3(3) . . . . ? S2 Cu3 S3 Cu1 57.01(17) . . . . ? W1 Cu3 S3 Cu1 61.59(12) . . . . ? N1 Cu1 S3 W1 130.6(4) . . . . ? N2 Cu1 S3 W1 -114.4(3) . . . . ? S1 Cu1 S3 W1 -0.23(13) . . . . ? N1 Cu1 S3 Cu3 67.9(4) . . . . ? N2 Cu1 S3 Cu3 -177.1(3) . . . . ? S1 Cu1 S3 Cu3 -62.94(18) . . . . ? W1 Cu1 S3 Cu3 -62.71(12) . . . . ? N2 Cu1 N1 C1 -155.4(13) . . . . ? S1 Cu1 N1 C1 81.6(13) . . . . ? S3 Cu1 N1 C1 -42.4(14) . . . . ? W1 Cu1 N1 C1 16.4(15) . . . . ? N2 Cu1 N1 C5 24.0(12) . . . . ? S1 Cu1 N1 C5 -98.9(11) . . . . ? S3 Cu1 N1 C5 137.1(10) . . . . ? W1 Cu1 N1 C5 -164.1(9) . . . . ? N1 Cu1 N2 C10 -151.5(12) . . . . ? S1 Cu1 N2 C10 -22.4(13) . . . . ? S3 Cu1 N2 C10 89.8(12) . . . . ? W1 Cu1 N2 C10 35.0(13) . . . . ? N1 Cu1 N2 C6 41.6(13) . . . . ? S1 Cu1 N2 C6 170.7(11) . . . . ? S3 Cu1 N2 C6 -77.2(12) . . . . ? W1 Cu1 N2 C6 -131.9(11) . . . . ? C21 Cu2 N3 C15 2.4(15) 2_344 . . . ? S1 Cu2 N3 C15 -125.4(14) . . . . ? S2 Cu2 N3 C15 127.4(14) . . . . ? W1 Cu2 N3 C15 -179.5(14) . . . . ? C21 Cu2 N3 C11 -176.7(14) 2_344 . . . ? S1 Cu2 N3 C11 55.6(14) . . . . ? S2 Cu2 N3 C11 -51.6(14) . . . . ? W1 Cu2 N3 C11 1.5(15) . . . . ? N5 Cu3 N4 C20 62.3(12) . . . . ? S3 Cu3 N4 C20 -171.0(11) . . . . ? S2 Cu3 N4 C20 -64.6(11) . . . . ? W1 Cu3 N4 C20 -117.1(11) . . . . ? N5 Cu3 N4 C16 -124.7(10) . . . . ? S3 Cu3 N4 C16 2.1(11) . . . . ? S2 Cu3 N4 C16 108.4(10) . . . . ? W1 Cu3 N4 C16 55.9(11) . . . . ? N4 Cu3 N5 C21 -138(16) . . . . ? S3 Cu3 N5 C21 104(16) . . . . ? S2 Cu3 N5 C21 -24(16) . . . . ? W1 Cu3 N5 C21 41(16) . . . . ? C5 N1 C1 C2 -1(3) . . . . ? Cu1 N1 C1 C2 178.6(15) . . . . ? N1 C1 C2 C3 -6(3) . . . . ? C1 C2 C3 C4 9(3) . . . . ? C2 C3 C4 C5 -5(3) . . . . ? C1 N1 C5 C4 5(2) . . . . ? Cu1 N1 C5 C4 -174.4(13) . . . . ? C3 C4 C5 N1 -2(3) . . . . ? C10 N2 C6 C7 2(2) . . . . ? Cu1 N2 C6 C7 169.1(14) . . . . ? N2 C6 C7 C8 -1(3) . . . . ? C6 C7 C8 C9 -4(3) . . . . ? C7 C8 C9 C10 8(3) . . . . ? C6 N2 C10 C9 3(2) . . . . ? Cu1 N2 C10 C9 -165.4(14) . . . . ? C8 C9 C10 N2 -8(3) . . . . ? C15 N3 C11 C12 1(3) . . . . ? Cu2 N3 C11 C12 -180(2) . . . . ? N3 C11 C12 C13 6(5) . . . . ? C11 C12 C13 C14 -7(6) . . . . ? C12 C13 C14 C15 0(5) . . . . ? C11 N3 C15 C14 -8(3) . . . . ? Cu2 N3 C15 C14 172.6(16) . . . . ? C13 C14 C15 N3 8(4) . . . . ? C20 N4 C16 C17 -2(2) . . . . ? Cu3 N4 C16 C17 -175.3(12) . . . . ? N4 C16 C17 C18 0(3) . . . . ? C16 C17 C18 C19 -3(3) . . . . ? C17 C18 C19 C20 8(3) . . . . ? C16 N4 C20 C19 7(2) . . . . ? Cu3 N4 C20 C19 -179.3(14) . . . . ? C18 C19 C20 N4 -10(3) . . . . ? Cu3 N5 C21 Cu2 -21(21) . . . 2_354 ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 2.078 _refine_diff_density_min -1.954 _refine_diff_density_rms 0.278