# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xi Chen' _publ_contact_author_email xyxyxyz2005@yahoo.com.cn loop_ _publ_author_name 'Xi Chen' 'Zhi-Yuan Zhang' 'Jian-Ping Lang' B.F.Abrahams 'Zhenrong Sun' data_1 _database_code_depnum_ccdc_archive 'CCDC 799106' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C21 H28 B Cu4 N10 O S3 W), 2(C3 N O), C4 N' _chemical_formula_sum 'C52 H56 B2 Cu8 N23 O4 S6 W2 ' _chemical_formula_weight 2157.32 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' 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' Cl Cl 0.1484 0.1585 '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' Ag Ag -0.8971 1.1015 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.200(5) _cell_length_b 16.905(3) _cell_length_c 19.395(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.36(3) _cell_angle_gamma 90.00 _cell_volume 7629(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4188.0 _exptl_absorpt_coefficient_mu 5.404 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.110 _exptl_absorpt_correction_T_max 0.141 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 w\ _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21730 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8747 _reflns_number_gt 7169 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+0.0000P] 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 8679 _refine_ls_number_parameters 400 _refine_ls_number_restraints 224 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2058 _refine_ls_wR_factor_gt 0.1928 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.192 _refine_ls_shift/su_mean 0.006 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 -0.477422(15) 0.76539(2) -0.46217(2) 0.03415(15) Uani 1 1 d . . . Cu1 Cu -0.39971(6) 0.87077(8) -0.37380(8) 0.0533(4) Uani 1 1 d . . . Cu2 Cu -0.42050(5) 0.82602(7) -0.53330(7) 0.0446(3) Uani 1 1 d . . . Cu3 Cu -0.37064(5) 0.71188(8) -0.40394(8) 0.0475(3) Uani 1 1 d . . . N1 N -0.6104(4) 0.7336(6) -0.5724(6) 0.0565(17) Uani 1 1 d U . . N2 N -0.5671(4) 0.6300(5) -0.4715(5) 0.0480(15) Uani 1 1 d U . . N3 N -0.5616(4) 0.7606(6) -0.5744(5) 0.0509(16) Uani 1 1 d U . . N4 N -0.5419(4) 0.8068(5) -0.4215(5) 0.0478(14) Uani 1 1 d U . . N5 N -0.5902(4) 0.7608(5) -0.4378(5) 0.0503(15) Uani 1 1 d U . . N6 N -0.5087(4) 0.6437(5) -0.4457(5) 0.0445(14) Uani 1 1 d U . . N8 N -0.2982(4) 0.6593(6) -0.3703(6) 0.060(2) Uani 1 1 d U . . N9 N -0.3585(4) 0.8903(6) -0.6193(5) 0.0532(19) Uani 1 1 d U . . N10 N -0.2274(7) 0.8729(12) -0.3662(12) 0.137(5) Uani 1 1 d U . . N15 N -0.3602(4) 0.9484(6) -0.2947(6) 0.064(2) Uani 1 1 d U . . B1 B -0.6103(6) 0.6969(8) -0.5007(8) 0.052(3) Uani 1 1 d . . . C1 C -0.7145(5) 0.7135(10) -0.6647(9) 0.083(3) Uani 1 1 d U . . H1A H -0.7157 0.6934 -0.6186 0.125 Uiso 1 1 calc R . . H1B H -0.7265 0.6722 -0.7038 0.125 Uiso 1 1 calc R . . H1C H -0.7402 0.7584 -0.6847 0.125 Uiso 1 1 calc R . . C2 C -0.6349(5) 0.5222(8) -0.4834(8) 0.072(3) Uani 1 1 d U . . H2A H -0.6629 0.5643 -0.5065 0.108 Uiso 1 1 calc R . . H2B H -0.6373 0.5016 -0.4383 0.108 Uiso 1 1 calc R . . H2C H -0.6429 0.4801 -0.5209 0.108 Uiso 1 1 calc R . . C3 C -0.5014(5) 0.9364(7) -0.3458(7) 0.065(3) Uani 1 1 d U . . H3A H -0.4713 0.9306 -0.3613 0.097 Uiso 1 1 calc R . . H3B H -0.4844 0.9393 -0.2896 0.097 Uiso 1 1 calc R . . H3C H -0.5229 0.9845 -0.3681 0.097 Uiso 1 1 calc R . . C4 C -0.5388(5) 0.8186(8) -0.6777(7) 0.064(3) Uani 1 1 d U . . H4A H -0.4998 0.8222 -0.6363 0.096 Uiso 1 1 calc R . . H4B H -0.5527 0.8710 -0.6979 0.096 Uiso 1 1 calc R . . H4C H -0.5396 0.7854 -0.7190 0.096 Uiso 1 1 calc R . . C5 C -0.6711(6) 0.7554(8) -0.4032(8) 0.070(3) Uani 1 1 d U . . H5A H -0.6812 0.7076 -0.4343 0.105 Uiso 1 1 calc R . . H5B H -0.7022 0.7934 -0.4263 0.105 Uiso 1 1 calc R . . H5C H -0.6646 0.7427 -0.3510 0.105 Uiso 1 1 calc R . . C6 C -0.4828(4) 0.5742(6) -0.4162(6) 0.0461(16) Uani 1 1 d U . . C7 C -0.6355(5) 0.7700(8) -0.6928(7) 0.0628(19) Uani 1 1 d U . . H7A H -0.6575 0.7805 -0.7461 0.075 Uiso 1 1 calc R . . C8 C -0.6182(5) 0.7896(8) -0.4001(7) 0.0567(16) Uani 1 1 d U . . C9 C -0.4198(5) 0.5576(6) -0.3827(7) 0.057(2) Uani 1 1 d U . . H9A H -0.3997 0.6058 -0.3829 0.085 Uiso 1 1 calc R . . H9B H -0.4133 0.5176 -0.4137 0.085 Uiso 1 1 calc R . . H9C H -0.4055 0.5388 -0.3298 0.085 Uiso 1 1 calc R . . C10 C -0.5755(5) 0.5543(6) -0.4591(7) 0.0528(17) Uani 1 1 d U . . C11 C -0.5904(5) 0.8559(8) -0.3614(7) 0.0598(17) Uani 1 1 d U . . H11A H -0.6011 0.8893 -0.3316 0.072 Uiso 1 1 calc R . . C12 C -0.5756(5) 0.7842(8) -0.6475(6) 0.0573(17) Uani 1 1 d U . . C13 C -0.6555(5) 0.7383(8) -0.6448(8) 0.0636(19) Uani 1 1 d U . . C14 C -0.5229(5) 0.5172(6) -0.4236(6) 0.0534(17) Uani 1 1 d U . . H14A H -0.5157 0.4641 -0.4078 0.064 Uiso 1 1 calc R . . C15 C -0.5422(5) 0.8647(7) -0.3748(7) 0.0540(16) Uani 1 1 d U . . C18 C -0.3833(4) 0.8668(6) -0.5892(6) 0.0459(19) Uani 1 1 d U . . C19 C -0.2752(8) 0.8775(14) -0.3641(14) 0.137(5) Uani 1 1 d U . . H19A H -0.2738 0.9102 -0.3241 0.165 Uiso 1 1 calc R . . C20 C -0.1763(9) 0.9109(16) -0.3168(14) 0.162(6) Uani 1 1 d U . . H20A H -0.1814 0.9390 -0.2769 0.244 Uiso 1 1 calc R . . H20B H -0.1660 0.9481 -0.3464 0.244 Uiso 1 1 calc R . . H20C H -0.1460 0.8719 -0.2929 0.244 Uiso 1 1 calc R . . C21 C -0.2289(9) 0.8286(15) -0.4295(15) 0.149(6) Uani 1 1 d U . . H21A H -0.2665 0.8043 -0.4579 0.223 Uiso 1 1 calc R . . H21B H -0.1997 0.7878 -0.4099 0.223 Uiso 1 1 calc R . . H21C H -0.2218 0.8635 -0.4637 0.223 Uiso 1 1 calc R . . C28 C -0.3413(5) 0.9942(7) -0.2469(7) 0.056(2) Uani 1 1 d U . . C22 C -0.2570(4) 0.6286(7) -0.3561(6) 0.050(2) Uani 1 1 d U . . O1 O -0.3216(3) 0.8486(5) -0.4028(5) 0.065(2) Uani 1 1 d . . . Cu4 Cu -0.31406(6) 0.92604(8) -0.67055(8) 0.0521(3) Uani 1 1 d . . . S7 S -0.43603(11) 0.69829(14) -0.52699(14) 0.0403(5) Uani 1 1 d . . . S9 S -0.41194(12) 0.75396(15) -0.33298(15) 0.0436(6) Uani 1 1 d . . . S10 S -0.47148(12) 0.89658(14) -0.49122(15) 0.0453(6) Uani 1 1 d . . . N14 N -0.5000 0.679(2) -0.2500 0.172(8) Uiso 1 2 d SU . . C25 C -0.3533(11) 1.0602(15) -0.4406(14) 0.142(7) Uiso 1 1 d U . . N13 N -0.2994(12) 1.0700(15) -0.4336(16) 0.187(6) Uiso 1 1 d U . . C29 C -0.5324(12) 0.6222(19) -0.2673(18) 0.180(8) Uiso 1 1 d U . . C26 C -0.5785(15) 0.567(2) -0.2894(18) 0.195(9) Uiso 1 1 d U . . C24 C -0.2714(14) 1.0598(19) -0.4751(19) 0.196(9) Uiso 1 1 d U . . O2 O -0.184(4) 1.050(6) -0.316(5) 0.81(7) Uiso 1 1 d . . . C23 C -0.2453(16) 1.086(2) -0.347(2) 0.202(7) Uiso 1 1 d U . . 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) 0.0356(2) 0.0354(2) -0.00133(13) 0.01789(18) -0.00271(15) Cu1 0.0634(9) 0.0459(7) 0.0482(8) -0.0113(5) 0.0235(7) -0.0159(6) Cu2 0.0487(7) 0.0437(7) 0.0505(7) 0.0014(5) 0.0306(6) -0.0039(6) Cu3 0.0374(7) 0.0531(7) 0.0498(8) 0.0015(6) 0.0181(6) 0.0048(6) N1 0.037(3) 0.085(4) 0.046(3) 0.000(3) 0.018(3) -0.003(3) N2 0.050(3) 0.049(3) 0.055(3) -0.008(3) 0.033(3) -0.013(3) N3 0.037(3) 0.077(4) 0.040(3) 0.002(3) 0.019(3) 0.000(3) N4 0.044(3) 0.059(3) 0.049(3) -0.008(3) 0.029(3) -0.002(3) N5 0.043(3) 0.066(4) 0.051(3) -0.003(3) 0.030(3) -0.002(3) N6 0.048(3) 0.043(3) 0.049(3) -0.005(3) 0.028(3) -0.010(2) N8 0.041(4) 0.069(5) 0.056(5) 0.009(4) 0.012(4) 0.007(4) N9 0.045(4) 0.065(5) 0.053(4) 0.010(4) 0.026(3) 0.001(4) N10 0.081(6) 0.161(11) 0.173(12) 0.058(9) 0.062(8) -0.009(7) N15 0.065(5) 0.066(5) 0.061(5) -0.017(4) 0.030(4) -0.025(4) B1 0.049(7) 0.058(7) 0.053(7) -0.003(6) 0.026(6) -0.005(6) C1 0.042(4) 0.120(8) 0.075(7) -0.006(6) 0.016(4) -0.019(6) C2 0.062(4) 0.073(6) 0.092(7) -0.015(6) 0.044(5) -0.030(5) C3 0.072(6) 0.064(5) 0.062(6) -0.018(4) 0.033(5) -0.009(4) C4 0.053(5) 0.089(7) 0.045(5) 0.024(5) 0.018(4) 0.001(5) C5 0.057(5) 0.102(7) 0.071(6) -0.018(5) 0.046(5) -0.010(5) C6 0.054(3) 0.040(3) 0.052(3) -0.007(3) 0.032(3) -0.010(3) C7 0.044(3) 0.089(5) 0.045(3) 0.004(3) 0.012(3) -0.002(4) C8 0.049(3) 0.077(4) 0.058(4) -0.007(3) 0.035(3) 0.000(3) C9 0.056(4) 0.047(5) 0.063(6) 0.004(4) 0.023(5) -0.001(4) C10 0.058(3) 0.052(3) 0.060(4) -0.010(3) 0.037(3) -0.017(3) C11 0.052(4) 0.077(4) 0.060(4) -0.011(3) 0.034(3) 0.004(3) C12 0.043(3) 0.083(4) 0.041(3) 0.005(3) 0.015(3) 0.001(3) C13 0.041(3) 0.091(4) 0.050(4) 0.000(3) 0.013(3) -0.009(3) C14 0.062(3) 0.045(3) 0.059(4) -0.008(3) 0.033(3) -0.015(3) C15 0.051(3) 0.065(4) 0.055(4) -0.010(3) 0.032(3) 0.001(3) C18 0.039(4) 0.057(5) 0.048(5) 0.005(4) 0.026(3) -0.002(4) C19 0.084(7) 0.159(12) 0.173(12) 0.062(9) 0.062(9) -0.007(8) C20 0.088(8) 0.179(13) 0.196(14) 0.053(11) 0.045(10) -0.019(9) C21 0.102(9) 0.168(14) 0.177(14) 0.056(10) 0.065(9) 0.006(9) C28 0.056(5) 0.063(5) 0.060(5) -0.019(4) 0.036(4) -0.023(4) C22 0.031(4) 0.063(5) 0.050(5) 0.015(4) 0.013(4) 0.006(4) O1 0.048(5) 0.079(6) 0.070(6) -0.007(4) 0.030(4) -0.007(4) Cu4 0.0450(7) 0.0607(8) 0.0538(8) 0.0187(6) 0.0256(6) 0.0080(6) S7 0.0435(13) 0.0400(12) 0.0433(13) -0.0043(9) 0.0249(11) -0.0017(11) S9 0.0450(14) 0.0491(13) 0.0354(13) -0.0007(10) 0.0174(11) -0.0045(11) S10 0.0532(15) 0.0371(12) 0.0524(15) 0.0021(10) 0.0301(13) 0.0018(11) _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 N3 2.280(9) . ? W1 N4 2.280(8) . ? W1 N6 2.290(8) . ? W1 S7 2.301(2) . ? W1 S9 2.304(3) . ? W1 S10 2.311(2) . ? W1 Cu3 2.6489(15) . ? W1 Cu1 2.6550(15) . ? W1 Cu2 2.6587(13) . ? Cu1 N15 1.920(9) . ? Cu1 S9 2.205(3) . ? Cu1 S10 2.231(3) . ? Cu1 O1 2.388(8) . ? Cu1 Cu3 2.923(2) . ? Cu1 Cu2 2.9817(19) . ? Cu2 C18 1.891(9) . ? Cu2 S10 2.208(3) . ? Cu2 S7 2.211(3) . ? Cu2 Cu3 2.9516(19) . ? Cu3 N8 1.918(9) . ? Cu3 S7 2.219(3) . ? Cu3 S9 2.223(3) . ? N1 C13 1.359(15) . ? N1 N3 1.376(13) . ? N1 B1 1.521(16) . ? N2 C10 1.338(13) . ? N2 N6 1.394(11) . ? N2 B1 1.514(16) . ? N3 C12 1.352(14) . ? N4 C15 1.336(13) . ? N4 N5 1.392(12) . ? N5 C8 1.342(13) . ? N5 B1 1.530(16) . ? N6 C6 1.346(13) . ? N8 C22 1.113(13) . ? N9 C18 1.127(12) . ? N9 Cu4 1.941(9) . ? N10 C19 1.27(2) . ? N10 C20 1.39(3) . ? N10 C21 1.42(3) . ? N15 C28 1.132(13) . ? C1 C13 1.474(17) . ? C2 C10 1.506(14) . ? C3 C15 1.541(16) . ? C4 C12 1.459(15) . ? C5 C8 1.476(16) . ? C6 C14 1.382(14) . ? C6 C9 1.498(14) . ? C7 C13 1.369(18) . ? C7 C12 1.423(16) . ? C8 C11 1.361(17) . ? C10 C14 1.376(16) . ? C11 C15 1.408(15) . ? C19 O1 1.20(2) . ? C28 Cu4 1.884(11) 6_576 ? C22 Cu4 1.924(10) 7_464 ? Cu4 C28 1.884(11) 6_575 ? Cu4 C22 1.924(10) 7_464 ? N14 C29 1.23(3) . ? N14 C29 1.23(3) 2_454 ? C25 N13 1.37(3) . ? N13 C24 1.33(4) . ? N13 C23 1.65(4) . ? C29 C26 1.43(4) . ? C29 C29 1.51(6) 2_454 ? O2 C23 1.56(9) . ? 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 N3 W1 N4 78.2(3) . . ? N3 W1 N6 81.4(3) . . ? N4 W1 N6 81.8(3) . . ? N3 W1 S7 87.3(2) . . ? N4 W1 S7 162.0(2) . . ? N6 W1 S7 85.6(2) . . ? N3 W1 S9 161.0(2) . . ? N4 W1 S9 87.1(2) . . ? N6 W1 S9 84.7(2) . . ? S7 W1 S9 104.51(9) . . ? N3 W1 S10 86.9(2) . . ? N4 W1 S10 86.2(2) . . ? N6 W1 S10 164.6(2) . . ? S7 W1 S10 103.79(9) . . ? S9 W1 S10 104.22(9) . . ? N3 W1 Cu3 139.8(2) . . ? N4 W1 Cu3 139.7(2) . . ? N6 W1 Cu3 90.6(2) . . ? S7 W1 Cu3 52.71(7) . . ? S9 W1 Cu3 52.77(8) . . ? S10 W1 Cu3 104.80(7) . . ? N3 W1 Cu1 139.3(2) . . ? N4 W1 Cu1 92.3(2) . . ? N6 W1 Cu1 136.9(2) . . ? S7 W1 Cu1 105.62(7) . . ? S9 W1 Cu1 52.21(7) . . ? S10 W1 Cu1 52.84(8) . . ? Cu3 W1 Cu1 66.89(5) . . ? N3 W1 Cu2 92.6(2) . . ? N4 W1 Cu2 138.0(2) . . ? N6 W1 Cu2 137.8(2) . . ? S7 W1 Cu2 52.34(7) . . ? S9 W1 Cu2 106.37(8) . . ? S10 W1 Cu2 52.18(7) . . ? Cu3 W1 Cu2 67.57(4) . . ? Cu1 W1 Cu2 68.27(4) . . ? N15 Cu1 S9 116.0(3) . . ? N15 Cu1 S10 125.0(3) . . ? S9 Cu1 S10 110.38(11) . . ? N15 Cu1 O1 95.2(4) . . ? S9 Cu1 O1 103.0(2) . . ? S10 Cu1 O1 101.7(2) . . ? N15 Cu1 W1 161.1(3) . . ? S9 Cu1 W1 55.67(8) . . ? S10 Cu1 W1 55.64(7) . . ? O1 Cu1 W1 103.2(2) . . ? N15 Cu1 Cu3 133.9(3) . . ? S9 Cu1 Cu3 48.94(8) . . ? S10 Cu1 Cu3 98.65(8) . . ? O1 Cu1 Cu3 58.6(2) . . ? W1 Cu1 Cu3 56.45(4) . . ? N15 Cu1 Cu2 141.0(3) . . ? S9 Cu1 Cu2 99.09(8) . . ? S10 Cu1 Cu2 47.47(7) . . ? O1 Cu1 Cu2 58.9(2) . . ? W1 Cu1 Cu2 55.92(4) . . ? Cu3 Cu1 Cu2 59.97(4) . . ? C18 Cu2 S10 125.1(3) . . ? C18 Cu2 S7 123.0(3) . . ? S10 Cu2 S7 110.43(10) . . ? C18 Cu2 W1 176.8(3) . . ? S10 Cu2 W1 55.78(7) . . ? S7 Cu2 W1 55.49(6) . . ? C18 Cu2 Cu3 125.6(3) . . ? S10 Cu2 Cu3 98.37(8) . . ? S7 Cu2 Cu3 48.35(7) . . ? W1 Cu2 Cu3 56.05(4) . . ? C18 Cu2 Cu1 127.3(3) . . ? S10 Cu2 Cu1 48.13(8) . . ? S7 Cu2 Cu1 98.10(8) . . ? W1 Cu2 Cu1 55.81(4) . . ? Cu3 Cu2 Cu1 59.03(5) . . ? N8 Cu3 S7 118.2(3) . . ? N8 Cu3 S9 128.7(3) . . ? S7 Cu3 S9 110.12(10) . . ? N8 Cu3 W1 171.6(3) . . ? S7 Cu3 W1 55.58(7) . . ? S9 Cu3 W1 55.62(8) . . ? N8 Cu3 Cu1 131.7(3) . . ? S7 Cu3 Cu1 99.60(8) . . ? S9 Cu3 Cu1 48.42(8) . . ? W1 Cu3 Cu1 56.65(4) . . ? N8 Cu3 Cu2 125.0(3) . . ? S7 Cu3 Cu2 48.10(7) . . ? S9 Cu3 Cu2 99.55(8) . . ? W1 Cu3 Cu2 56.37(4) . . ? Cu1 Cu3 Cu2 61.00(5) . . ? C13 N1 N3 109.1(10) . . ? C13 N1 B1 127.2(10) . . ? N3 N1 B1 123.4(9) . . ? C10 N2 N6 109.7(9) . . ? C10 N2 B1 128.7(9) . . ? N6 N2 B1 121.2(8) . . ? C12 N3 N1 108.7(9) . . ? C12 N3 W1 132.0(7) . . ? N1 N3 W1 119.3(7) . . ? C15 N4 N5 106.0(8) . . ? C15 N4 W1 134.1(7) . . ? N5 N4 W1 119.4(6) . . ? C8 N5 N4 109.9(9) . . ? C8 N5 B1 128.0(10) . . ? N4 N5 B1 121.3(8) . . ? C6 N6 N2 105.3(8) . . ? C6 N6 W1 134.4(7) . . ? N2 N6 W1 120.3(6) . . ? C22 N8 Cu3 175.1(10) . . ? C18 N9 Cu4 177.3(9) . . ? C19 N10 C20 127(3) . . ? C19 N10 C21 115(2) . . ? C20 N10 C21 118(2) . . ? C28 N15 Cu1 173.6(10) . . ? N2 B1 N1 109.4(9) . . ? N2 B1 N5 107.8(10) . . ? N1 B1 N5 107.2(10) . . ? N6 C6 C14 110.7(9) . . ? N6 C6 C9 126.0(9) . . ? C14 C6 C9 123.2(10) . . ? C13 C7 C12 107.7(11) . . ? N5 C8 C11 108.1(10) . . ? N5 C8 C5 125.0(11) . . ? C11 C8 C5 126.9(10) . . ? N2 C10 C14 108.5(9) . . ? N2 C10 C2 121.3(11) . . ? C14 C10 C2 130.3(11) . . ? C8 C11 C15 106.5(10) . . ? N3 C12 C7 106.8(10) . . ? N3 C12 C4 128.9(10) . . ? C7 C12 C4 124.4(10) . . ? N1 C13 C7 107.7(11) . . ? N1 C13 C1 124.2(12) . . ? C7 C13 C1 128.1(12) . . ? C10 C14 C6 105.8(10) . . ? N4 C15 C11 109.4(10) . . ? N4 C15 C3 127.2(10) . . ? C11 C15 C3 123.1(10) . . ? N9 C18 Cu2 176.5(10) . . ? O1 C19 N10 133(3) . . ? N15 C28 Cu4 176.5(12) . 6_576 ? N8 C22 Cu4 178.4(10) . 7_464 ? C19 O1 Cu1 121.4(14) . . ? C28 Cu4 C22 121.7(4) 6_575 7_464 ? C28 Cu4 N9 121.7(4) 6_575 . ? C22 Cu4 N9 116.5(4) 7_464 . ? Cu2 S7 Cu3 83.55(9) . . ? Cu2 S7 W1 72.17(8) . . ? Cu3 S7 W1 71.71(8) . . ? Cu1 S9 Cu3 82.64(10) . . ? Cu1 S9 W1 72.12(8) . . ? Cu3 S9 W1 71.61(8) . . ? Cu2 S10 Cu1 84.40(10) . . ? Cu2 S10 W1 72.04(8) . . ? Cu1 S10 W1 71.52(8) . . ? C29 N14 C29 76(4) . 2_454 ? C24 N13 C25 139(3) . . ? C24 N13 C23 101(3) . . ? C25 N13 C23 119(3) . . ? N14 C29 C26 169(3) . . ? N14 C29 C29 51.8(18) . 2_454 ? C26 C29 C29 138.9(18) . 2_454 ? O2 C23 N13 125(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.710 _refine_diff_density_min -1.517 _refine_diff_density_rms 0.179 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 799107' #TrackingRef '2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H84 B2 Cu10 K N26 O6 S6 W2, C4 N, C N, 2(C)' _chemical_formula_sum 'C65 H84 B2 Cu10 K N28 O6 S6 W2 ' _chemical_formula_weight 2609.93 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' 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' K K 0.2009 0.2494 '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 ? _symmetry_space_group_name_H-M 'C 2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.165(3) _cell_length_b 26.907(5) _cell_length_c 23.715(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.91(3) _cell_angle_gamma 90.00 _cell_volume 9258(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5124.0 _exptl_absorpt_coefficient_mu 4.960 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5036 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 MoK\a _diffrn_measurement_method 'fine-focus sealed tube' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25302 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10606 _reflns_number_gt 8645 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1000P)^2^+0.0000P] 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 10517 _refine_ls_number_parameters 555 _refine_ls_number_restraints 304 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0705 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1848 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.007 _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 0.36878(2) 0.620420(12) 0.543426(14) 0.02744(13) Uani 1 1 d . . . Cu2 Cu 0.27167(8) 0.55000(4) 0.57722(5) 0.0373(3) Uani 1 1 d . . . Cu3 Cu 0.26015(8) 0.65649(4) 0.60510(5) 0.0397(3) Uani 1 1 d . . . Cu1 Cu 0.19231(8) 0.62327(4) 0.48064(5) 0.0376(3) Uani 1 1 d . . . S1 S 0.28350(15) 0.55822(8) 0.48705(10) 0.0330(5) Uani 1 1 d . . . Cu4 Cu 0.16079(8) 0.76883(4) 0.74164(5) 0.0406(3) Uani 1 1 d . . . S2 S 0.37164(16) 0.60023(8) 0.63817(10) 0.0343(5) Uani 1 1 d . . . S3 S 0.27451(16) 0.68886(8) 0.52167(11) 0.0368(5) Uani 1 1 d . . . Cu5 Cu 0.36411(8) 0.89661(4) 0.86505(5) 0.0404(3) Uani 1 1 d . . . O1 O 0.1282(5) 0.6049(3) 0.5760(3) 0.0439(16) Uani 1 1 d . . . N4 N 0.5756(5) 0.5855(3) 0.5540(3) 0.0343(15) Uani 1 1 d U . . N1 N 0.4852(5) 0.6767(3) 0.5856(3) 0.0363(15) Uani 1 1 d U . . N6 N 0.5116(5) 0.6429(3) 0.4695(3) 0.0350(15) Uani 1 1 d U . . N3 N 0.4927(5) 0.5685(3) 0.5578(3) 0.0299(14) Uani 1 1 d U . . C16 C 0.0693(7) 0.6199(3) 0.4310(4) 0.040(2) Uani 1 1 d U . . N8 N 0.2166(6) 0.4918(3) 0.5981(4) 0.054(2) Uani 1 1 d U . . C17 C 0.1845(7) 0.4560(3) 0.6114(5) 0.042(2) Uani 1 1 d U . . N5 N 0.4185(5) 0.6395(3) 0.4640(3) 0.0333(15) Uani 1 1 d U . . N2 N 0.5675(5) 0.6761(3) 0.5712(3) 0.0382(16) Uani 1 1 d U . . N10 N 0.2416(6) 0.8208(3) 0.7842(4) 0.0428(18) Uani 1 1 d U . . N7 N -0.0050(6) 0.6136(3) 0.4033(4) 0.0461(19) Uani 1 1 d U . . N9 N 0.1979(6) 0.7218(3) 0.6921(4) 0.050(2) Uani 1 1 d U . . C18 C 0.2190(6) 0.6952(3) 0.6591(4) 0.0358(19) Uani 1 1 d U . . C8 C 0.6424(6) 0.5513(3) 0.5730(4) 0.0372(17) Uani 1 1 d U . . C19 C 0.2893(6) 0.8507(3) 0.8125(4) 0.0369(19) Uani 1 1 d U . . C7 C 0.6013(6) 0.5093(3) 0.5879(4) 0.0364(17) Uani 1 1 d U . . H7 H 0.6299 0.4791 0.6011 0.044 Uiso 1 1 calc R . . C6 C 0.5093(6) 0.5208(3) 0.5790(4) 0.0319(16) Uani 1 1 d U . . C3 C 0.6239(7) 0.7121(4) 0.6015(5) 0.0436(19) Uani 1 1 d U . . C13 C 0.5234(7) 0.6516(4) 0.4162(4) 0.0399(18) Uani 1 1 d U . . C9 C 0.4404(7) 0.4860(3) 0.5900(4) 0.040(2) Uani 1 1 d U . . H9A H 0.4146 0.4999 0.6189 0.059 Uiso 1 1 calc R . . H9B H 0.4697 0.4549 0.6041 0.059 Uiso 1 1 calc R . . H9C H 0.3923 0.4805 0.5539 0.059 Uiso 1 1 calc R . . C11 C 0.3738(7) 0.6470(4) 0.4067(4) 0.0403(18) Uani 1 1 d U . . C12 C 0.4378(7) 0.6554(4) 0.3761(4) 0.0433(19) Uani 1 1 d U . . H12 H 0.4251 0.6623 0.3361 0.052 Uiso 1 1 calc R . . C1 C 0.4938(7) 0.7145(4) 0.6248(5) 0.0434(19) Uani 1 1 d U . . C10 C 0.7408(7) 0.5589(4) 0.5750(5) 0.046(2) Uani 1 1 d U . . H10A H 0.7452 0.5617 0.5355 0.069 Uiso 1 1 calc R . . H10B H 0.7768 0.5310 0.5942 0.069 Uiso 1 1 calc R . . H10C H 0.7636 0.5887 0.5964 0.069 Uiso 1 1 calc R . . C4 C 0.4229(8) 0.7304(5) 0.6544(6) 0.065(3) Uani 1 1 d U . . H4A H 0.3716 0.7455 0.6258 0.097 Uiso 1 1 calc R . . H4B H 0.4499 0.7540 0.6849 0.097 Uiso 1 1 calc R . . H4C H 0.4020 0.7019 0.6712 0.097 Uiso 1 1 calc R . . C20 C 0.0373(6) 0.7684(3) 0.7479(4) 0.0375(19) Uani 0.50 1 d PU . . N17 C 0.0373(6) 0.7684(3) 0.7479(4) 0.0375(19) Uani 0.50 1 d PU . . N11 N 0.0298(7) 0.5583(4) 0.6075(5) 0.065(2) Uani 1 1 d U . . B1 B 0.5844(8) 0.6376(4) 0.5286(5) 0.040(2) Uani 1 1 d . . . C14 C 0.2718(7) 0.6491(5) 0.3796(4) 0.054(3) Uani 1 1 d U . . H14A H 0.2465 0.6163 0.3783 0.082 Uiso 1 1 calc R . . H14B H 0.2583 0.6620 0.3402 0.082 Uiso 1 1 calc R . . H14C H 0.2450 0.6703 0.4027 0.082 Uiso 1 1 calc R . . C2 C 0.5791(7) 0.7356(4) 0.6352(5) 0.047(2) Uani 1 1 d U . . H2 H 0.6021 0.7617 0.6610 0.057 Uiso 1 1 calc R . . C15 C 0.6158(8) 0.6596(5) 0.4072(5) 0.061(3) Uani 1 1 d U . . H15A H 0.6422 0.6898 0.4264 0.091 Uiso 1 1 calc R . . H15B H 0.6092 0.6621 0.3658 0.091 Uiso 1 1 calc R . . H15C H 0.6554 0.6322 0.4235 0.091 Uiso 1 1 calc R . . C5 C 0.7179(7) 0.7210(4) 0.5938(5) 0.055(3) Uani 1 1 d U . . H5A H 0.7387 0.7537 0.6075 0.083 Uiso 1 1 calc R . . H5B H 0.7145 0.7180 0.5529 0.083 Uiso 1 1 calc R . . H5C H 0.7605 0.6968 0.6162 0.083 Uiso 1 1 calc R . . C21 C 0.0968(8) 0.5895(5) 0.6136(6) 0.061(3) Uani 1 1 d U . . H21 H 0.1238 0.6014 0.6515 0.073 Uiso 1 1 calc R . . C22 C -0.0017(10) 0.5418(6) 0.6572(7) 0.096(4) Uani 1 1 d U . . H22A H 0.0473 0.5457 0.6932 0.144 Uiso 1 1 calc R . . H22B H -0.0194 0.5075 0.6521 0.144 Uiso 1 1 calc R . . H22C H -0.0536 0.5615 0.6591 0.144 Uiso 1 1 calc R . . C23 C -0.0112(11) 0.5369(6) 0.5533(7) 0.101(5) Uani 1 1 d U . . H23A H 0.0144 0.5511 0.5244 0.151 Uiso 1 1 calc R . . H23B H -0.0764 0.5430 0.5421 0.151 Uiso 1 1 calc R . . H23C H -0.0002 0.5018 0.5556 0.151 Uiso 1 1 calc R . . K1 K 0.0000 0.65722(19) 0.7500 0.127(3) Uani 1 2 d S . . N12 N -0.0392(7) 0.6971(4) 0.5530(5) 0.068(2) Uani 1 1 d U . . O2 O -0.0711(7) 0.6684(4) 0.6334(4) 0.084(3) Uani 1 1 d . . . C26 C 0.0212(10) 0.7256(5) 0.5297(6) 0.074(3) Uani 1 1 d U . . H26A H 0.0612 0.7452 0.5605 0.111 Uiso 1 1 calc R . . H26B H -0.0143 0.7472 0.4992 0.111 Uiso 1 1 calc R . . H26C H 0.0575 0.7037 0.5135 0.111 Uiso 1 1 calc R . . C24 C -0.0306(8) 0.6950(5) 0.6097(6) 0.066(3) Uani 1 1 d U . . H24 H 0.0118 0.7166 0.6338 0.079 Uiso 1 1 calc R . . C28 C -0.3794(12) 0.6082(7) 0.7081(5) 0.097(4) Uani 1 1 d U . . H28A H -0.3818 0.6437 0.7030 0.146 Uiso 1 1 calc R . . H28B H -0.4051 0.5994 0.7392 0.146 Uiso 1 1 calc R . . H28C H -0.4143 0.5926 0.6721 0.146 Uiso 1 1 calc R . . C25 C -0.1044(11) 0.6644(6) 0.5120(6) 0.089(4) Uani 1 1 d U . . H25A H -0.0730 0.6349 0.5055 0.133 Uiso 1 1 calc R . . H25B H -0.1299 0.6813 0.4753 0.133 Uiso 1 1 calc R . . H25C H -0.1531 0.6554 0.5284 0.133 Uiso 1 1 calc R . . N13 N -0.2898(13) 0.5927(8) 0.7221(7) 0.121(5) Uani 1 1 d U . . O3 O -0.1435(14) 0.6063(7) 0.7358(8) 0.162(6) Uani 1 1 d . . . C27 C -0.2199(19) 0.6178(10) 0.7205(9) 0.123(5) Uani 1 1 d U . . H27 H -0.2319 0.6496 0.7049 0.147 Uiso 1 1 calc R . . C29 C -0.2712(16) 0.5373(9) 0.7414(9) 0.143(6) Uani 1 1 d U . . H29A H -0.2906 0.5161 0.7075 0.215 Uiso 1 1 calc R . . H29B H -0.3049 0.5290 0.7687 0.215 Uiso 1 1 calc R . . H29C H -0.2065 0.5326 0.7601 0.215 Uiso 1 1 calc R . . C32 C 0.0000 0.5894(18) 0.2500 0.205(13) Uani 1 2 d SU . . N16 N 0.0000 0.6352(14) 0.2500 0.219(13) Uani 1 2 d SU . . C33 C 0.118(2) 0.5517(9) 0.2857(12) 0.175(9) Uani 1 1 d U . . N15 N -0.5000 0.5014(15) 0.7500 0.46(4) Uani 1 2 d SU . . C30 C -0.440(6) 0.4655(12) 0.747(3) 0.47(4) Uani 1 1 d U . . C31 C -0.399(5) 0.4132(14) 0.7652(18) 0.49(4) Uani 1 1 d U . . 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 0.02634(19) 0.0246(2) 0.0315(2) -0.00082(12) 0.00858(15) -0.00074(13) Cu2 0.0399(6) 0.0307(6) 0.0438(7) 0.0021(5) 0.0160(5) -0.0049(5) Cu3 0.0397(6) 0.0377(6) 0.0444(7) -0.0047(5) 0.0168(5) 0.0054(5) Cu1 0.0298(6) 0.0373(6) 0.0428(7) -0.0005(5) 0.0061(5) 0.0009(5) S1 0.0345(11) 0.0296(11) 0.0350(11) -0.0062(9) 0.0100(10) -0.0036(9) Cu4 0.0441(7) 0.0392(6) 0.0393(6) -0.0046(5) 0.0134(5) -0.0022(5) S2 0.0347(12) 0.0347(11) 0.0339(11) -0.0001(9) 0.0109(10) 0.0024(9) S3 0.0351(12) 0.0264(10) 0.0484(13) 0.0010(9) 0.0112(11) 0.0040(9) Cu5 0.0344(6) 0.0372(6) 0.0463(7) -0.0057(5) 0.0067(5) 0.0041(5) O1 0.042(4) 0.044(4) 0.046(4) -0.011(3) 0.012(3) 0.008(3) N4 0.037(3) 0.030(3) 0.037(3) -0.005(3) 0.011(3) -0.002(3) N1 0.034(3) 0.035(3) 0.040(4) -0.009(3) 0.011(3) -0.004(3) N6 0.036(3) 0.032(3) 0.037(3) 0.005(3) 0.012(3) 0.000(3) N3 0.038(3) 0.025(3) 0.028(3) 0.000(3) 0.013(3) 0.004(3) C16 0.039(4) 0.041(5) 0.038(5) 0.006(4) 0.011(4) 0.002(4) N8 0.049(5) 0.044(4) 0.067(5) 0.009(4) 0.015(4) -0.001(4) C17 0.037(5) 0.026(4) 0.063(6) 0.011(4) 0.017(4) -0.005(4) N5 0.036(3) 0.035(3) 0.032(3) 0.003(3) 0.015(3) 0.000(3) N2 0.033(3) 0.036(4) 0.046(4) -0.005(3) 0.014(3) -0.008(3) N10 0.042(4) 0.039(4) 0.043(4) 0.000(3) 0.005(4) 0.008(3) N7 0.035(4) 0.047(4) 0.052(5) 0.013(4) 0.007(4) 0.003(4) N9 0.041(4) 0.048(5) 0.060(5) -0.010(4) 0.014(4) -0.005(4) C18 0.026(4) 0.040(4) 0.044(5) -0.009(4) 0.015(4) 0.000(4) C8 0.036(4) 0.029(4) 0.043(4) -0.009(3) 0.007(4) 0.001(3) C19 0.035(4) 0.033(4) 0.040(5) -0.001(4) 0.007(4) 0.004(3) C7 0.039(4) 0.034(4) 0.034(4) -0.001(3) 0.007(3) 0.009(3) C6 0.038(4) 0.030(3) 0.026(3) -0.002(3) 0.007(3) 0.004(3) C3 0.036(4) 0.040(4) 0.054(5) -0.009(4) 0.011(4) -0.007(3) C13 0.043(4) 0.043(4) 0.039(4) 0.008(4) 0.020(3) 0.004(4) C9 0.042(5) 0.023(4) 0.052(5) 0.003(4) 0.012(4) 0.003(4) C11 0.043(4) 0.047(4) 0.033(4) 0.006(4) 0.015(3) 0.007(4) C12 0.045(4) 0.050(5) 0.039(4) 0.009(4) 0.017(3) 0.004(4) C1 0.038(4) 0.038(4) 0.056(5) -0.013(4) 0.016(4) -0.008(4) C10 0.041(5) 0.041(5) 0.052(6) -0.008(4) 0.009(5) 0.002(4) C4 0.048(6) 0.066(7) 0.086(8) -0.049(6) 0.030(6) -0.017(5) C20 0.043(4) 0.035(4) 0.031(4) -0.002(4) 0.005(4) -0.002(4) N17 0.043(4) 0.035(4) 0.031(4) -0.002(4) 0.005(4) -0.002(4) N11 0.047(5) 0.071(6) 0.081(6) -0.012(5) 0.024(5) -0.010(4) B1 0.037(6) 0.037(6) 0.047(6) -0.006(5) 0.015(5) -0.001(5) C14 0.049(5) 0.078(7) 0.035(5) 0.015(5) 0.011(4) 0.005(6) C2 0.035(4) 0.043(4) 0.062(5) -0.018(4) 0.010(4) -0.012(4) C15 0.047(5) 0.078(8) 0.068(7) 0.018(6) 0.034(5) 0.006(6) C5 0.040(5) 0.052(6) 0.078(7) -0.019(6) 0.025(5) -0.012(5) C21 0.044(5) 0.063(6) 0.079(7) -0.014(5) 0.022(5) -0.007(5) C22 0.066(8) 0.118(11) 0.112(9) 0.017(9) 0.039(8) -0.025(8) C23 0.086(10) 0.096(10) 0.105(8) -0.015(8) 0.003(8) -0.031(8) K1 0.193(7) 0.062(3) 0.083(4) 0.000 -0.026(4) 0.000 N12 0.054(5) 0.070(6) 0.083(6) -0.012(5) 0.023(5) 0.006(4) O2 0.068(6) 0.106(8) 0.076(6) 0.002(6) 0.016(5) -0.001(6) C26 0.072(8) 0.075(8) 0.078(8) 0.000(6) 0.026(7) 0.007(6) C24 0.044(6) 0.071(7) 0.077(6) -0.008(6) 0.009(5) 0.004(5) C28 0.111(10) 0.150(12) 0.025(6) -0.002(7) 0.011(7) 0.030(9) C25 0.098(10) 0.098(10) 0.078(8) -0.027(7) 0.037(7) -0.018(7) N13 0.116(9) 0.162(12) 0.073(7) -0.013(8) 0.009(8) 0.039(9) O3 0.161(16) 0.189(16) 0.129(13) -0.034(12) 0.030(13) 0.015(14) C27 0.118(11) 0.170(13) 0.069(8) -0.003(9) 0.010(10) 0.032(10) C29 0.158(15) 0.167(13) 0.090(11) 0.008(11) 0.012(11) 0.049(11) C32 0.32(3) 0.17(3) 0.17(2) 0.000 0.15(2) 0.000 N16 0.33(3) 0.18(3) 0.20(2) 0.000 0.14(2) 0.000 C33 0.24(3) 0.16(2) 0.16(2) -0.043(15) 0.12(2) -0.058(15) N15 1.02(11) 0.12(2) 0.126(17) 0.000 0.00(4) 0.000 C30 1.02(11) 0.13(2) 0.136(16) 0.004(9) -0.01(4) 0.006(8) C31 1.03(11) 0.15(2) 0.16(2) -0.005(17) -0.02(4) 0.035(15) _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 N5 2.281(7) . ? W1 N3 2.286(7) . ? W1 S1 2.292(2) . ? W1 S3 2.296(2) . ? W1 S2 2.300(2) . ? W1 N1 2.321(7) . ? W1 Cu1 2.6582(15) . ? W1 Cu2 2.6623(12) . ? W1 Cu3 2.6826(13) . ? Cu2 N8 1.906(9) . ? Cu2 S1 2.208(2) . ? Cu2 S2 2.222(3) . ? Cu2 Cu3 2.9571(17) . ? Cu2 Cu1 2.9961(17) . ? Cu3 C18 1.891(9) . ? Cu3 S3 2.230(3) . ? Cu3 S2 2.235(3) . ? Cu3 O1 2.366(7) . ? Cu3 Cu1 2.9668(18) . ? Cu1 C16 1.896(11) . ? Cu1 S1 2.208(2) . ? Cu1 S3 2.216(3) . ? Cu4 N9 1.920(9) . ? Cu4 C20 1.922(9) . ? Cu4 N10 1.937(9) . ? Cu4 K1 3.910(4) . ? Cu5 C19 1.881(10) . ? Cu5 C17 1.911(9) 4_556 ? Cu5 N7 1.947(9) 8_566 ? O1 C21 1.200(13) . ? N4 C8 1.347(11) . ? N4 N3 1.366(10) . ? N4 B1 1.547(13) . ? N1 C1 1.357(11) . ? N1 N2 1.387(10) . ? N6 C13 1.348(11) . ? N6 N5 1.383(10) . ? N6 B1 1.516(14) . ? N3 C6 1.376(11) . ? C16 N7 1.140(13) . ? N8 C17 1.163(12) . ? C17 Cu5 1.911(9) 4_546 ? N5 C11 1.345(11) . ? N2 C3 1.352(12) . ? N2 B1 1.520(13) . ? N10 C19 1.159(12) . ? N7 Cu5 1.947(9) 8_465 ? N9 C18 1.171(12) . ? C8 C7 1.385(13) . ? C8 C10 1.492(13) . ? C7 C6 1.385(12) . ? C7 H7 0.9300 . ? C6 C9 1.481(12) . ? C3 C2 1.349(14) . ? C3 C5 1.508(13) . ? C13 C12 1.372(14) . ? C13 C15 1.493(13) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C12 1.389(13) . ? C11 C14 1.494(14) . ? C12 H12 0.9300 . ? C1 C2 1.367(13) . ? C1 C4 1.507(13) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C20 N17 1.162(18) 2_556 ? C20 C20 1.162(18) 2_556 ? C20 K1 3.048(10) . ? N11 C21 1.294(14) . ? N11 C23 1.381(17) . ? N11 C22 1.463(17) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C2 H2 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? K1 O3 2.51(2) . ? K1 O3 2.51(2) 2_556 ? K1 O2 2.677(10) . ? K1 O2 2.677(10) 2_556 ? K1 N17 3.048(10) 2_556 ? K1 C20 3.048(10) 2_556 ? K1 C27 3.37(3) . ? K1 C27 3.37(3) 2_556 ? K1 C24 3.379(15) 2_556 ? K1 C24 3.379(15) . ? N12 C24 1.313(16) . ? N12 C26 1.425(16) . ? N12 C25 1.463(17) . ? O2 C24 1.187(15) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C24 H24 0.9300 . ? C28 N13 1.37(2) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? N13 C27 1.27(3) . ? N13 C29 1.56(3) . ? O3 C27 1.15(2) . ? C27 H27 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C32 N16 1.23(5) . ? C32 C33 2.01(4) 2 ? C32 C33 2.01(4) . ? N15 C30 1.34(6) 2_456 ? N15 C30 1.34(6) . ? C30 C31 1.55(6) . ? C30 C30 1.87(18) 2_456 ? 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 N5 W1 N3 78.8(2) . . ? N5 W1 S1 87.1(2) . . ? N3 W1 S1 86.59(19) . . ? N5 W1 S3 88.1(2) . . ? N3 W1 S3 162.66(19) . . ? S1 W1 S3 104.23(9) . . ? N5 W1 S2 160.5(2) . . ? N3 W1 S2 85.95(18) . . ? S1 W1 S2 104.15(8) . . ? S3 W1 S2 104.04(8) . . ? N5 W1 N1 79.4(3) . . ? N3 W1 N1 81.1(3) . . ? S1 W1 N1 163.21(19) . . ? S3 W1 N1 85.4(2) . . ? S2 W1 N1 86.4(2) . . ? N5 W1 Cu1 92.97(19) . . ? N3 W1 Cu1 138.67(18) . . ? S1 W1 Cu1 52.35(6) . . ? S3 W1 Cu1 52.52(6) . . ? S2 W1 Cu1 106.49(7) . . ? N1 W1 Cu1 137.59(19) . . ? N5 W1 Cu2 138.90(19) . . ? N3 W1 Cu2 91.33(18) . . ? S1 W1 Cu2 52.29(6) . . ? S3 W1 Cu2 106.01(7) . . ? S2 W1 Cu2 52.60(7) . . ? N1 W1 Cu2 138.85(19) . . ? Cu1 W1 Cu2 68.54(4) . . ? N5 W1 Cu3 140.46(19) . . ? N3 W1 Cu3 138.47(17) . . ? S1 W1 Cu3 104.50(6) . . ? S3 W1 Cu3 52.51(7) . . ? S2 W1 Cu3 52.62(6) . . ? N1 W1 Cu3 92.27(18) . . ? Cu1 W1 Cu3 67.49(4) . . ? Cu2 W1 Cu3 67.18(4) . . ? N8 Cu2 S1 119.9(3) . . ? N8 Cu2 S2 126.7(3) . . ? S1 Cu2 S2 109.67(9) . . ? N8 Cu2 W1 170.1(3) . . ? S1 Cu2 W1 55.20(6) . . ? S2 Cu2 W1 55.29(6) . . ? N8 Cu2 Cu3 132.7(3) . . ? S1 Cu2 Cu3 98.40(7) . . ? S2 Cu2 Cu3 48.61(7) . . ? W1 Cu2 Cu3 56.74(3) . . ? N8 Cu2 Cu1 129.1(3) . . ? S1 Cu2 Cu1 47.28(7) . . ? S2 Cu2 Cu1 98.24(8) . . ? W1 Cu2 Cu1 55.66(4) . . ? Cu3 Cu2 Cu1 59.78(4) . . ? C18 Cu3 S3 121.5(3) . . ? C18 Cu3 S2 120.0(3) . . ? S3 Cu3 S2 108.47(9) . . ? C18 Cu3 O1 95.9(3) . . ? S3 Cu3 O1 105.26(19) . . ? S2 Cu3 O1 101.19(18) . . ? C18 Cu3 W1 160.7(3) . . ? S3 Cu3 W1 54.80(6) . . ? S2 Cu3 W1 54.85(6) . . ? O1 Cu3 W1 103.30(16) . . ? C18 Cu3 Cu2 137.5(3) . . ? S3 Cu3 Cu2 98.79(7) . . ? S2 Cu3 Cu2 48.26(7) . . ? O1 Cu3 Cu2 57.76(16) . . ? W1 Cu3 Cu2 56.08(3) . . ? C18 Cu3 Cu1 138.8(3) . . ? S3 Cu3 Cu1 47.94(7) . . ? S2 Cu3 Cu1 98.80(7) . . ? O1 Cu3 Cu1 60.95(17) . . ? W1 Cu3 Cu1 55.86(4) . . ? Cu2 Cu3 Cu1 60.76(4) . . ? C16 Cu1 S1 119.2(3) . . ? C16 Cu1 S3 129.5(3) . . ? S1 Cu1 S3 109.87(10) . . ? C16 Cu1 W1 174.0(3) . . ? S1 Cu1 W1 55.27(6) . . ? S3 Cu1 W1 55.31(7) . . ? C16 Cu1 Cu3 128.7(3) . . ? S1 Cu1 Cu3 98.13(8) . . ? S3 Cu1 Cu3 48.33(7) . . ? W1 Cu1 Cu3 56.65(4) . . ? C16 Cu1 Cu2 123.2(3) . . ? S1 Cu1 Cu2 47.29(7) . . ? S3 Cu1 Cu2 97.98(8) . . ? W1 Cu1 Cu2 55.79(4) . . ? Cu3 Cu1 Cu2 59.46(4) . . ? Cu1 S1 Cu2 85.43(9) . . ? Cu1 S1 W1 72.38(7) . . ? Cu2 S1 W1 72.51(7) . . ? N9 Cu4 C20 120.6(4) . . ? N9 Cu4 N10 122.7(4) . . ? C20 Cu4 N10 116.6(4) . . ? N9 Cu4 K1 79.8(3) . . ? C20 Cu4 K1 49.9(3) . . ? N10 Cu4 K1 146.8(2) . . ? Cu2 S2 Cu3 83.13(9) . . ? Cu2 S2 W1 72.11(8) . . ? Cu3 S2 W1 72.53(8) . . ? Cu1 S3 Cu3 83.73(9) . . ? Cu1 S3 W1 72.17(8) . . ? Cu3 S3 W1 72.69(8) . . ? C19 Cu5 C17 122.2(4) . 4_556 ? C19 Cu5 N7 123.5(4) . 8_566 ? C17 Cu5 N7 114.2(4) 4_556 8_566 ? C21 O1 Cu3 118.1(7) . . ? C8 N4 N3 111.5(7) . . ? C8 N4 B1 127.6(8) . . ? N3 N4 B1 120.9(7) . . ? C1 N1 N2 105.3(7) . . ? C1 N1 W1 133.9(6) . . ? N2 N1 W1 120.8(5) . . ? C13 N6 N5 109.5(7) . . ? C13 N6 B1 128.5(8) . . ? N5 N6 B1 122.0(7) . . ? N4 N3 C6 105.2(7) . . ? N4 N3 W1 121.2(5) . . ? C6 N3 W1 132.8(6) . . ? N7 C16 Cu1 173.7(9) . . ? C17 N8 Cu2 178.8(10) . . ? N8 C17 Cu5 178.0(10) . 4_546 ? C11 N5 N6 106.6(7) . . ? C11 N5 W1 132.6(6) . . ? N6 N5 W1 120.7(5) . . ? C3 N2 N1 109.6(7) . . ? C3 N2 B1 129.7(8) . . ? N1 N2 B1 120.6(7) . . ? C19 N10 Cu4 176.1(8) . . ? C16 N7 Cu5 173.0(9) . 8_465 ? C18 N9 Cu4 175.9(9) . . ? N9 C18 Cu3 175.2(9) . . ? N4 C8 C7 107.1(8) . . ? N4 C8 C10 124.4(8) . . ? C7 C8 C10 128.6(9) . . ? N10 C19 Cu5 174.4(9) . . ? C6 C7 C8 106.7(8) . . ? C6 C7 H7 126.7 . . ? C8 C7 H7 126.7 . . ? N3 C6 C7 109.5(8) . . ? N3 C6 C9 126.3(8) . . ? C7 C6 C9 124.2(8) . . ? C2 C3 N2 107.5(9) . . ? C2 C3 C5 130.9(9) . . ? N2 C3 C5 121.6(9) . . ? N6 C13 C12 107.8(8) . . ? N6 C13 C15 123.1(9) . . ? C12 C13 C15 128.9(9) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C11 C12 109.2(9) . . ? N5 C11 C14 126.5(8) . . ? C12 C11 C14 124.2(9) . . ? C13 C12 C11 106.9(8) . . ? C13 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? N1 C1 C2 109.4(8) . . ? N1 C1 C4 126.3(8) . . ? C2 C1 C4 124.3(9) . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N17 C20 C20 0.0(8) 2_556 2_556 ? N17 C20 Cu4 179.5(10) 2_556 . ? C20 C20 Cu4 179.5(10) 2_556 . ? N17 C20 K1 79.01(18) 2_556 . ? C20 C20 K1 79.01(18) 2_556 . ? Cu4 C20 K1 101.3(3) . . ? C21 N11 C23 120.0(12) . . ? C21 N11 C22 122.5(12) . . ? C23 N11 C22 117.4(12) . . ? N6 B1 N2 109.4(8) . . ? N6 B1 N4 108.8(8) . . ? N2 B1 N4 108.0(8) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 C2 C1 108.1(9) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O1 C21 N11 127.6(13) . . ? O1 C21 H21 116.2 . . ? N11 C21 H21 116.2 . . ? N11 C22 H22A 109.5 . . ? N11 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N11 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N11 C23 H23A 109.5 . . ? N11 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N11 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 K1 O3 113.8(9) . 2_556 ? O3 K1 O2 81.3(5) . . ? O3 K1 O2 105.9(5) 2_556 . ? O3 K1 O2 105.9(5) . 2_556 ? O3 K1 O2 81.3(5) 2_556 2_556 ? O2 K1 O2 167.1(5) . 2_556 ? O3 K1 C20 133.7(5) . . ? O3 K1 C20 112.4(5) 2_556 . ? O2 K1 C20 83.9(3) . . ? O2 K1 C20 83.4(3) 2_556 . ? O3 K1 N17 112.4(5) . 2_556 ? O3 K1 N17 133.7(5) 2_556 2_556 ? O2 K1 N17 83.4(3) . 2_556 ? O2 K1 N17 83.9(3) 2_556 2_556 ? C20 K1 N17 22.0(3) . 2_556 ? O3 K1 C20 112.4(5) . 2_556 ? O3 K1 C20 133.7(5) 2_556 2_556 ? O2 K1 C20 83.4(3) . 2_556 ? O2 K1 C20 83.9(3) 2_556 2_556 ? C20 K1 C20 22.0(3) . 2_556 ? N17 K1 C20 0.0(4) 2_556 2_556 ? O3 K1 C27 15.0(6) . . ? O3 K1 C27 128.5(6) 2_556 . ? O2 K1 C27 75.2(4) . . ? O2 K1 C27 109.1(4) 2_556 . ? C20 K1 C27 118.8(5) . . ? N17 K1 C27 97.8(5) 2_556 . ? C20 K1 C27 97.8(5) 2_556 . ? O3 K1 C27 128.5(6) . 2_556 ? O3 K1 C27 15.0(6) 2_556 2_556 ? O2 K1 C27 109.1(4) . 2_556 ? O2 K1 C27 75.2(4) 2_556 2_556 ? C20 K1 C27 97.8(5) . 2_556 ? N17 K1 C27 118.8(5) 2_556 2_556 ? C20 K1 C27 118.8(5) 2_556 2_556 ? C27 K1 C27 143.3(9) . 2_556 ? O3 K1 C24 99.3(4) . 2_556 ? O3 K1 C24 99.6(5) 2_556 2_556 ? O2 K1 C24 151.9(4) . 2_556 ? O2 K1 C24 18.3(3) 2_556 2_556 ? C20 K1 C24 75.4(3) . 2_556 ? N17 K1 C24 70.2(3) 2_556 2_556 ? C20 K1 C24 70.2(3) 2_556 2_556 ? C27 K1 C24 98.2(4) . 2_556 ? C27 K1 C24 92.6(4) 2_556 2_556 ? O3 K1 C24 99.6(5) . . ? O3 K1 C24 99.3(4) 2_556 . ? O2 K1 C24 18.3(3) . . ? O2 K1 C24 151.9(4) 2_556 . ? C20 K1 C24 70.2(3) . . ? N17 K1 C24 75.4(3) 2_556 . ? C20 K1 C24 75.4(3) 2_556 . ? C27 K1 C24 92.6(4) . . ? C27 K1 C24 98.2(4) 2_556 . ? C24 K1 C24 145.0(5) 2_556 . ? C24 N12 C26 122.5(12) . . ? C24 N12 C25 120.1(12) . . ? C26 N12 C25 116.9(12) . . ? C24 O2 K1 116.6(9) . . ? N12 C26 H26A 109.5 . . ? N12 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N12 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O2 C24 N12 126.9(14) . . ? O2 C24 K1 45.1(7) . . ? N12 C24 K1 164.8(10) . . ? O2 C24 H24 116.6 . . ? N12 C24 H24 116.6 . . ? K1 C24 H24 73.2 . . ? N13 C28 H28A 109.5 . . ? N13 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N13 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N12 C25 H25A 109.5 . . ? N12 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N12 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 N13 C28 128(2) . . ? C27 N13 C29 116(2) . . ? C28 N13 C29 117(2) . . ? C27 O3 K1 131(2) . . ? O3 C27 N13 128(3) . . ? O3 C27 K1 34.4(17) . . ? N13 C27 K1 161.2(18) . . ? O3 C27 H27 115.8 . . ? N13 C27 H27 115.8 . . ? K1 C27 H27 81.9 . . ? N13 C29 H29A 109.5 . . ? N13 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N13 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N16 C32 C33 120.3(15) . 2 ? N16 C32 C33 120.3(15) . . ? C33 C32 C33 119(3) 2 . ? C30 N15 C30 88(6) 2_456 . ? N15 C30 C31 149(6) . . ? N15 C30 C30 46(3) . 2_456 ? C31 C30 C30 107(4) . 2_456 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.731 _refine_diff_density_min -1.754 _refine_diff_density_rms 0.166