Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email paul.kruger@tcd.ie _publ_contact_author_name 'Paul E. Kruger' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; _publ_contact_author_phone ' 353 1 608 1422 ' _publ_contact_author_fax ' 353 1 671 2826 ' _publ_section_title ; Synthesis and structural and magnetic characterisation of tetranuclear Cu(II) complexes possessing novel [Cu4(m4-PO4)2(m2-CO3)] butterfly cores that exhibit supramolecular isomerism ; loop_ _publ_author_name _publ_author_address P.E.Kruger ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; R.P.Doyle ; Department of Chemistry Trinity College Dublin Dublin 2 Ireland ; M.Nieuwenhuyzen ; Chemistry Department Queen's University Belfast, BT9 5AG UK ; K.S.Murray ; School of Chemistry Monash University PO Box 23, Clayton Victoria 3800 Australia. ; B.Moubaraki ; School of Chemistry Monash University PO Box 23, Clayton Victoria 3800 Australia. ; data_compound_1 _database_code_CSD 216728 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H77 Cu4 N8 O35.50 P2' _chemical_formula_weight 1565.53 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 14.871(3) _cell_length_b 22.146(4) _cell_length_c 19.937(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6566(2) _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 Blue _exptl_crystal_colour Plate _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3030 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.806 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _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 ? _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 58321 _diffrn_reflns_av_R_equivalents 0.1000 _diffrn_reflns_av_sigmaI/netI 0.1332 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7205 _reflns_number_gt 3705 _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^)+(0.0815P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7205 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1522 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.213 _refine_ls_shift/su_mean 0.003 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 Cu1 Cu 0.18344(4) 0.23020(3) 0.14218(3) 0.02303(17) Uani 1 1 d . . . N1A N 0.1706(3) 0.26938(19) 0.05077(19) 0.0258(10) Uani 1 1 d . . . C2A C 0.1371(4) 0.3237(3) 0.0403(3) 0.0331(14) Uani 1 1 d . . . H2A H 0.1199 0.3469 0.0770 0.040 Uiso 1 1 calc R . . C3A C 0.1266(4) 0.3476(3) -0.0232(3) 0.0442(16) Uani 1 1 d . . . H3A H 0.1024 0.3859 -0.0297 0.053 Uiso 1 1 calc R . . C4A C 0.1542(5) 0.3112(3) -0.0780(3) 0.0550(18) Uani 1 1 d . . . H4A H 0.1489 0.3256 -0.1217 0.066 Uiso 1 1 calc R . . C5A C 0.1880(4) 0.2556(3) -0.0667(3) 0.0419(15) Uani 1 1 d . . . H5A H 0.2049 0.2311 -0.1024 0.050 Uiso 1 1 calc R . . C6A C 0.1975(3) 0.2351(3) -0.0006(3) 0.0306(13) Uani 1 1 d . . . C7A C 0.2357(4) 0.1758(3) 0.0177(3) 0.0320(13) Uani 1 1 d . . . C8A C 0.2637(4) 0.1323(3) -0.0282(3) 0.0436(16) Uani 1 1 d . . . H8A H 0.2596 0.1398 -0.0740 0.052 Uiso 1 1 calc R . . C9A C 0.2973(4) 0.0783(3) -0.0057(3) 0.0494(17) Uani 1 1 d . . . H9A H 0.3161 0.0487 -0.0356 0.059 Uiso 1 1 calc R . . C10A C 0.3024(4) 0.0693(3) 0.0637(3) 0.0436(16) Uani 1 1 d . . . H10A H 0.3261 0.0337 0.0809 0.052 Uiso 1 1 calc R . . C11A C 0.2718(4) 0.1139(2) 0.1060(3) 0.0355(14) Uani 1 1 d . . . H11A H 0.2740 0.1071 0.1520 0.043 Uiso 1 1 calc R . . N12A N 0.2396(3) 0.16583(18) 0.0843(2) 0.0273(10) Uani 1 1 d . . . Cu2 Cu -0.03047(4) 0.28501(3) 0.32660(3) 0.02383(18) Uani 1 1 d . . . N1B N -0.0747(3) 0.22715(19) 0.3946(2) 0.0309(11) Uani 1 1 d . . . C2B C -0.1049(4) 0.1721(3) 0.3815(3) 0.0477(17) Uani 1 1 d . . . H2B H -0.1092 0.1598 0.3370 0.057 Uiso 1 1 calc R . . C3B C -0.1306(5) 0.1319(3) 0.4321(4) 0.062(2) Uani 1 1 d . . . H3B H -0.1513 0.0934 0.4214 0.074 Uiso 1 1 calc R . . C4B C -0.1246(5) 0.1502(3) 0.4981(4) 0.066(2) Uani 1 1 d . . . H4B H -0.1420 0.1248 0.5329 0.079 Uiso 1 1 calc R . . C5B C -0.0918(4) 0.2077(3) 0.5112(3) 0.0492(18) Uani 1 1 d . . . H5B H -0.0868 0.2212 0.5552 0.059 Uiso 1 1 calc R . . C6B C -0.0669(4) 0.2446(2) 0.4591(3) 0.0313(13) Uani 1 1 d . . . C7B C -0.0276(4) 0.3055(2) 0.4681(2) 0.0298(13) Uani 1 1 d . . . C8B C -0.0129(4) 0.3339(3) 0.5288(3) 0.0408(16) Uani 1 1 d . . . H8B H -0.0276 0.3140 0.5685 0.049 Uiso 1 1 calc R . . C9B C 0.0223(4) 0.3900(3) 0.5316(3) 0.0483(18) Uani 1 1 d . . . H9B H 0.0318 0.4091 0.5725 0.058 Uiso 1 1 calc R . . C10B C 0.0436(4) 0.4183(3) 0.4728(3) 0.0454(16) Uani 1 1 d . . . H10B H 0.0680 0.4570 0.4732 0.054 Uiso 1 1 calc R . . C11B C 0.0285(4) 0.3888(2) 0.4124(3) 0.0353(14) Uani 1 1 d . . . H11B H 0.0424 0.4085 0.3726 0.042 Uiso 1 1 calc R . . N12B N -0.0050(3) 0.33338(18) 0.40972(19) 0.0246(10) Uani 1 1 d . . . P1 P 0.11156(9) 0.33579(6) 0.23103(6) 0.0228(3) Uani 1 1 d . . . O11 O 0.0243(2) 0.34567(14) 0.27169(16) 0.0277(8) Uani 1 1 d . . . O12 O 0.1907(2) 0.31954(14) 0.27804(16) 0.0257(8) Uani 1 1 d . . . O13 O 0.0949(2) 0.28383(14) 0.18113(15) 0.0227(8) Uani 1 1 d . . . O14 O 0.1351(3) 0.39429(15) 0.19467(17) 0.0329(9) Uani 1 1 d . . . O2 O 0.3086(2) 0.28464(16) 0.17697(19) 0.0392(10) Uani 1 1 d . . . O1S O -0.0933(3) 0.2500 0.2500 0.0381(14) Uani 1 2 d S . . C1S C -0.1816(8) 0.2500 0.2500 0.079(4) Uani 1 2 d S . . O2S O -0.1995(9) 0.2027(6) 0.1956(5) 0.050(4) Uani 0.53(2) 1 d P A 2 O2S' O -0.2359(8) 0.2353(7) 0.2189(6) 0.044(4) Uani 0.47(2) 1 d P . 1 O1W O 0.4504(3) 0.20533(19) 0.1811(2) 0.0525(12) Uani 1 1 d . . . O2W O 0.1580(3) 0.48286(17) 0.2959(2) 0.0522(12) Uani 1 1 d . . . O3W O -0.0878(3) 0.05776(18) 0.2441(2) 0.0548(12) Uani 1 1 d . . . O4W O 0.3090(3) 0.0914(2) 0.3458(2) 0.0720(15) Uani 1 1 d . . . O5W O 0.1311(4) 0.0195(2) -0.1321(2) 0.0751(15) Uani 1 1 d . . . O6W O 0.0983(4) 0.3933(3) -0.2185(4) 0.119(2) Uani 1 1 d . . . O7W O 0.4326(4) 0.0896(2) 0.2307(3) 0.099(2) Uani 1 1 d . . . O8W O 0.0974(5) 0.4857(2) 0.1116(3) 0.112(2) Uani 1 1 d . . . O9W O 0.0821(6) 0.4846(3) -0.1369(4) 0.170(4) Uani 1 1 d . . . O10W O -0.2518(4) 0.1039(3) 0.2046(3) 0.118(2) Uani 1 1 d . . . O11W O 0.5930(5) 0.2500 0.2500 0.124(4) Uani 1 2 d S . . O12W O 0.3492(10) 0.5081(6) -0.0140(7) 0.128(5) Uiso 0.50 1 d P B 2 O12' O 0.2500 0.5000 -0.0282(17) 0.247(15) Uiso 0.50 2 d SP C 1 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 Cu1 0.0214(3) 0.0259(3) 0.0218(3) -0.0009(3) 0.0043(3) 0.0000(3) N1A 0.024(2) 0.031(2) 0.022(2) -0.0019(19) 0.0003(19) -0.001(2) C2A 0.033(4) 0.043(4) 0.023(3) 0.002(3) 0.004(3) -0.001(3) C3A 0.048(4) 0.054(4) 0.031(3) 0.010(3) 0.008(3) 0.007(3) C4A 0.055(5) 0.082(5) 0.028(3) 0.008(4) 0.001(3) 0.000(4) C5A 0.037(4) 0.062(4) 0.027(3) -0.009(3) 0.006(3) -0.001(3) C6A 0.016(3) 0.047(3) 0.029(3) -0.011(3) 0.005(2) -0.009(2) C7A 0.017(3) 0.045(4) 0.034(3) -0.009(3) 0.005(2) -0.011(3) C8A 0.029(4) 0.058(4) 0.045(4) -0.027(3) 0.008(3) -0.012(3) C9A 0.033(4) 0.048(4) 0.067(5) -0.026(4) 0.014(3) -0.009(3) C10A 0.029(4) 0.029(3) 0.073(5) -0.017(3) 0.012(3) -0.004(3) C11A 0.024(3) 0.032(3) 0.051(4) -0.002(3) 0.006(3) -0.003(3) N12A 0.021(2) 0.028(2) 0.034(3) -0.007(2) 0.005(2) -0.003(2) Cu2 0.0231(4) 0.0320(4) 0.0164(3) -0.0022(3) 0.0021(3) -0.0027(3) N1B 0.033(3) 0.028(3) 0.032(3) 0.002(2) 0.011(2) -0.001(2) C2B 0.045(4) 0.044(4) 0.054(4) -0.006(3) 0.025(3) -0.006(3) C3B 0.068(5) 0.032(4) 0.086(6) 0.009(4) 0.035(5) -0.001(3) C4B 0.071(5) 0.047(4) 0.080(5) 0.032(4) 0.043(4) 0.020(4) C5B 0.057(5) 0.052(4) 0.039(4) 0.017(3) 0.022(3) 0.022(3) C6B 0.032(3) 0.036(3) 0.026(3) 0.007(3) 0.010(2) 0.014(3) C7B 0.024(3) 0.041(3) 0.024(3) -0.001(2) 0.001(2) 0.014(3) C8B 0.032(4) 0.068(5) 0.023(3) -0.007(3) 0.000(3) 0.016(3) C9B 0.028(4) 0.078(5) 0.039(4) -0.031(4) -0.008(3) 0.010(3) C10B 0.024(3) 0.057(4) 0.055(4) -0.033(3) -0.003(3) 0.003(3) C11B 0.027(3) 0.043(4) 0.036(3) -0.009(3) 0.004(3) 0.002(3) N12B 0.019(2) 0.029(3) 0.025(2) -0.0054(19) 0.0015(18) -0.0001(19) P1 0.0253(8) 0.0230(7) 0.0201(6) 0.0032(6) 0.0051(6) 0.0023(6) O11 0.031(2) 0.0260(19) 0.0263(18) 0.0054(15) 0.0103(17) 0.0050(16) O12 0.022(2) 0.0271(19) 0.0281(19) 0.0016(15) 0.0001(16) -0.0017(15) O13 0.0218(19) 0.0254(19) 0.0210(17) 0.0033(15) 0.0039(14) 0.0040(15) O14 0.043(2) 0.026(2) 0.030(2) 0.0067(16) 0.0065(18) 0.0018(17) O2 0.029(2) 0.046(2) 0.042(2) 0.0052(19) -0.0054(19) -0.0141(19) O1S 0.014(3) 0.070(4) 0.030(3) -0.021(3) 0.000 0.000 C1S 0.030(7) 0.114(11) 0.092(10) 0.076(9) 0.000 0.000 O2S 0.044(7) 0.068(8) 0.037(5) -0.015(5) -0.013(5) -0.013(6) O2S' 0.023(6) 0.067(9) 0.043(6) -0.012(6) -0.013(5) 0.006(5) O1W 0.047(3) 0.068(3) 0.042(2) -0.022(2) 0.005(2) -0.002(2) O2W 0.045(3) 0.042(3) 0.070(3) -0.008(2) -0.002(2) 0.002(2) O3W 0.054(3) 0.045(3) 0.065(3) -0.006(2) 0.004(2) -0.016(2) O4W 0.079(4) 0.052(3) 0.085(4) -0.010(3) -0.038(3) 0.019(3) O5W 0.098(4) 0.065(3) 0.062(3) -0.014(3) 0.011(3) -0.004(3) O6W 0.092(5) 0.121(5) 0.145(6) 0.028(5) -0.020(4) 0.000(4) O7W 0.079(4) 0.056(3) 0.162(6) -0.010(4) -0.033(4) -0.006(3) O8W 0.178(7) 0.066(4) 0.092(4) 0.032(3) -0.031(4) 0.003(4) O9W 0.182(9) 0.121(6) 0.208(9) 0.065(6) -0.077(7) -0.026(5) O10W 0.061(4) 0.164(6) 0.129(5) -0.082(5) -0.031(4) 0.028(4) O11W 0.031(4) 0.261(11) 0.079(6) -0.095(7) 0.000 0.000 _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 Cu1 O13 1.936(3) . ? Cu1 O12 1.938(3) 4 ? Cu1 N12A 2.016(4) . ? Cu1 N1A 2.028(4) . ? Cu1 O2 2.324(3) . ? N1A C2A 1.319(6) . ? N1A C6A 1.335(6) . ? C2A C3A 1.379(7) . ? C3A C4A 1.419(8) . ? C4A C5A 1.350(9) . ? C5A C6A 1.401(8) . ? C6A C7A 1.478(8) . ? C7A N12A 1.348(6) . ? C7A C8A 1.391(7) . ? C8A C9A 1.370(8) . ? C9A C10A 1.400(9) . ? C10A C11A 1.376(7) . ? C11A N12A 1.320(6) . ? Cu2 O11 1.915(3) . ? Cu2 O1S 1.951(2) . ? Cu2 N1B 1.979(4) . ? Cu2 N12B 2.009(4) . ? Cu2 O13 2.413(3) 4 ? N1B C2B 1.325(7) . ? N1B C6B 1.348(7) . ? C2B C3B 1.399(8) . ? C3B C4B 1.381(10) . ? C4B C5B 1.388(9) . ? C5B C6B 1.373(7) . ? C6B C7B 1.480(8) . ? C7B N12B 1.359(6) . ? C7B C8B 1.382(7) . ? C8B C9B 1.350(8) . ? C9B C10B 1.366(9) . ? C10B C11B 1.387(7) . ? C11B N12B 1.326(6) . ? P1 O14 1.525(3) . ? P1 O13 1.541(3) . ? P1 O11 1.546(3) . ? P1 O12 1.547(3) . ? O12 Cu1 1.938(3) 4 ? O13 Cu2 2.413(3) 4 ? O1S C1S 1.313(12) . ? O1S Cu2 1.951(2) 4 ? C1S O2S' 1.068(11) . ? C1S O2S' 1.068(11) 4 ? C1S O2S 1.532(13) . ? C1S O2S 1.532(13) 4 ? O2S' O2S' 1.40(3) 4 ? 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 O13 Cu1 O12 93.31(13) . 4 ? O13 Cu1 N12A 161.01(16) . . ? O12 Cu1 N12A 92.57(16) 4 . ? O13 Cu1 N1A 91.92(15) . . ? O12 Cu1 N1A 170.53(16) 4 . ? N12A Cu1 N1A 80.04(17) . . ? O13 Cu1 O2 96.14(14) . . ? O12 Cu1 O2 90.29(13) 4 . ? N12A Cu1 O2 101.87(15) . . ? N1A Cu1 O2 97.00(15) . . ? C2A N1A C6A 120.6(5) . . ? C2A N1A Cu1 124.7(3) . . ? C6A N1A Cu1 114.7(4) . . ? N1A C2A C3A 122.5(5) . . ? C2A C3A C4A 117.2(6) . . ? C5A C4A C3A 119.8(6) . . ? C4A C5A C6A 119.3(6) . . ? N1A C6A C5A 120.5(5) . . ? N1A C6A C7A 115.6(5) . . ? C5A C6A C7A 123.9(5) . . ? N12A C7A C8A 121.4(6) . . ? N12A C7A C6A 113.8(5) . . ? C8A C7A C6A 124.7(5) . . ? C9A C8A C7A 119.8(6) . . ? C8A C9A C10A 117.9(6) . . ? C11A C10A C9A 119.0(6) . . ? N12A C11A C10A 123.0(6) . . ? C11A N12A C7A 118.8(5) . . ? C11A N12A Cu1 125.4(4) . . ? C7A N12A Cu1 115.5(4) . . ? O11 Cu2 O1S 92.00(12) . . ? O11 Cu2 N1B 171.04(17) . . ? O1S Cu2 N1B 96.89(15) . . ? O11 Cu2 N12B 90.99(16) . . ? O1S Cu2 N12B 161.41(17) . . ? N1B Cu2 N12B 80.95(18) . . ? O11 Cu2 O13 94.50(12) . 4 ? O1S Cu2 O13 93.95(13) . 4 ? N1B Cu2 O13 83.77(14) . 4 ? N12B Cu2 O13 104.10(14) . 4 ? C2B N1B C6B 118.9(5) . . ? C2B N1B Cu2 124.9(4) . . ? C6B N1B Cu2 116.0(4) . . ? N1B C2B C3B 122.4(6) . . ? C4B C3B C2B 118.8(6) . . ? C3B C4B C5B 118.2(6) . . ? C6B C5B C4B 119.9(6) . . ? N1B C6B C5B 121.8(5) . . ? N1B C6B C7B 114.3(4) . . ? C5B C6B C7B 123.9(5) . . ? N12B C7B C8B 120.3(5) . . ? N12B C7B C6B 114.1(4) . . ? C8B C7B C6B 125.6(5) . . ? C9B C8B C7B 121.0(6) . . ? C8B C9B C10B 118.5(5) . . ? C9B C10B C11B 119.4(6) . . ? N12B C11B C10B 122.2(6) . . ? C11B N12B C7B 118.6(4) . . ? C11B N12B Cu2 126.7(4) . . ? C7B N12B Cu2 114.7(3) . . ? O14 P1 O13 111.36(19) . . ? O14 P1 O11 108.76(19) . . ? O13 P1 O11 107.98(19) . . ? O14 P1 O12 108.1(2) . . ? O13 P1 O12 109.88(18) . . ? O11 P1 O12 110.75(18) . . ? P1 O11 Cu2 123.89(19) . . ? P1 O12 Cu1 125.9(2) . 4 ? P1 O13 Cu1 127.4(2) . . ? P1 O13 Cu2 129.60(18) . 4 ? Cu1 O13 Cu2 96.45(13) . 4 ? C1S O1S Cu2 118.61(12) . 4 ? C1S O1S Cu2 118.61(12) . . ? Cu2 O1S Cu2 122.8(2) 4 . ? O2S' C1S O2S' 82(2) . 4 ? O2S' C1S O1S 139.1(10) . . ? O2S' C1S O1S 139.1(10) 4 . ? O2S' C1S O2S 41.4(6) . . ? O2S' C1S O2S 119.2(16) 4 . ? O1S C1S O2S 100.0(7) . . ? O2S' C1S O2S 119.2(16) . 4 ? O2S' C1S O2S 41.4(6) 4 4 ? O1S C1S O2S 100.0(7) . 4 ? O2S C1S O2S 160.0(14) . 4 ? C1S O2S' O2S' 49.1(10) . 4 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.304 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.107 data_1a _database_code_CSD 216729 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H67 Cu4 N8 O26.50 P2' _chemical_formula_weight 1411.09 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.250(9) _cell_length_b 18.493(12) _cell_length_c 21.397(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.30(2) _cell_angle_gamma 90.00 _cell_volume 5564(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2892 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6188 _exptl_absorpt_correction_T_max 0.7326 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39187 _diffrn_reflns_av_R_equivalents 0.1341 _diffrn_reflns_av_sigmaI/netI 0.1138 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9811 _reflns_number_gt 5812 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1065P)^2^+32.1738P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9811 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1356 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2352 _refine_ls_wR_factor_gt 0.2002 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Cu1 Cu 1.68050(8) -0.14439(6) 0.84417(5) 0.0222(3) Uani 1 1 d . . . Cu2 Cu 1.66720(8) -0.37588(6) 0.84460(6) 0.0236(3) Uani 1 1 d . . . Cu3 Cu 1.88405(8) -0.17382(6) 0.93311(6) 0.0271(3) Uani 1 1 d . . . Cu4 Cu 1.85313(8) -0.34992(6) 0.95860(6) 0.0270(3) Uani 1 1 d . . . P1 P 1.81621(16) -0.26437(12) 0.81379(11) 0.0198(5) Uani 1 1 d . . . O11 O 1.7254(4) -0.2167(3) 0.7931(3) 0.0261(15) Uani 1 1 d . . . O12 O 1.7903(4) -0.3285(3) 0.8550(3) 0.0240(14) Uani 1 1 d . . . O13 O 1.8940(4) -0.2194(3) 0.8543(3) 0.0274(15) Uani 1 1 d . . . O14 O 1.8509(4) -0.2915(3) 0.7545(3) 0.0290(15) Uani 1 1 d . . . P2 P 1.66892(17) -0.25940(13) 0.94875(12) 0.0243(5) Uani 1 1 d . . . O21 O 1.7232(4) -0.1954(3) 0.9224(3) 0.0260(14) Uani 1 1 d . . . O22 O 1.6120(4) -0.3014(3) 0.8922(3) 0.0285(15) Uani 1 1 d . . . O23 O 1.7420(5) -0.3099(4) 0.9869(3) 0.0321(16) Uani 1 1 d . . . O24 O 1.6014(5) -0.2310(4) 0.9897(3) 0.0346(16) Uani 1 1 d . . . C3 C 1.9907(8) -0.2633(6) 1.0330(6) 0.044(3) Uani 1 1 d . . . O31 O 1.9274(5) -0.2619(3) 0.9795(3) 0.0369(18) Uani 1 1 d . . . O32 O 1.9798(6) -0.3111(4) 1.0731(5) 0.062(3) Uani 1 1 d . . . O33 O 2.0567(5) -0.2174(4) 1.0395(4) 0.048(2) Uani 1 1 d . . . O1W O 1.5252(4) -0.1891(3) 0.8184(3) 0.0300(15) Uani 1 1 d . . . O2W O 1.5967(4) -0.3235(3) 0.7507(3) 0.0273(15) Uani 1 1 d . . . N1A N 1.6465(5) -0.0555(4) 0.8891(4) 0.0290(19) Uani 1 1 d . . . C2A C 1.6379(7) -0.0510(6) 0.9501(5) 0.033(2) Uani 1 1 d . . . H2A H 1.6463 -0.0935 0.9753 0.040 Uiso 1 1 calc R . . C3A C 1.6174(8) 0.0127(7) 0.9779(6) 0.049(3) Uani 1 1 d . . . H3A H 1.6114 0.0138 1.0215 0.058 Uiso 1 1 calc R . . C4A C 1.6056(10) 0.0741(7) 0.9428(7) 0.060(4) Uani 1 1 d . . . H4A H 1.5918 0.1185 0.9618 0.072 Uiso 1 1 calc R . . C5A C 1.6139(9) 0.0718(6) 0.8780(7) 0.059(4) Uani 1 1 d . . . H5A H 1.6059 0.1140 0.8524 0.070 Uiso 1 1 calc R . . C6A C 1.6344(7) 0.0047(5) 0.8530(5) 0.032(2) Uani 1 1 d . . . C7A C 1.6432(7) -0.0062(5) 0.7865(5) 0.028(2) Uani 1 1 d . . . C8A C 1.6309(9) 0.0470(6) 0.7386(6) 0.050(3) Uani 1 1 d . . . H8A H 1.6141 0.0949 0.7483 0.060 Uiso 1 1 calc R . . C9A C 1.6430(9) 0.0300(7) 0.6793(6) 0.055(3) Uani 1 1 d . . . H9A H 1.6366 0.0663 0.6475 0.065 Uiso 1 1 calc R . . C10A C 1.6646(9) -0.0397(7) 0.6646(6) 0.049(3) Uani 1 1 d . . . H10A H 1.6698 -0.0529 0.6224 0.059 Uiso 1 1 calc R . . C11A C 1.6785(7) -0.0901(6) 0.7127(5) 0.033(2) Uani 1 1 d . . . H11A H 1.6966 -0.1378 0.7032 0.040 Uiso 1 1 calc R . . N12A N 1.6675(6) -0.0746(4) 0.7718(4) 0.0278(18) Uani 1 1 d . . . N1B N 1.8742(6) -0.1139(5) 1.0090(4) 0.034(2) Uani 1 1 d . . . C2B C 1.8630(8) -0.1404(7) 1.0659(6) 0.049(3) Uani 1 1 d . . . H2B H 1.8597 -0.1912 1.0719 0.059 Uiso 1 1 calc R . . C3B C 1.8562(10) -0.0931(9) 1.1167(6) 0.065(4) Uani 1 1 d . . . H3B H 1.8478 -0.1119 1.1567 0.078 Uiso 1 1 calc R . . C4B C 1.8619(10) -0.0187(9) 1.1078(8) 0.067(4) Uani 1 1 d . . . H4B H 1.8592 0.0138 1.1419 0.081 Uiso 1 1 calc R . . C5B C 1.8713(8) 0.0064(7) 1.0496(6) 0.050(3) Uani 1 1 d . . . H5B H 1.8738 0.0570 1.0424 0.060 Uiso 1 1 calc R . . C6B C 1.8771(7) -0.0417(6) 1.0005(6) 0.039(3) Uani 1 1 d . . . C7B C 1.8853(7) -0.0188(5) 0.9348(6) 0.039(3) Uani 1 1 d . . . C8B C 1.8868(8) 0.0531(6) 0.9176(7) 0.049(3) Uani 1 1 d . . . H8B H 1.8825 0.0909 0.9470 0.059 Uiso 1 1 calc R . . C9B C 1.8947(9) 0.0670(6) 0.8558(8) 0.064(4) Uani 1 1 d . . . H9B H 1.8965 0.1156 0.8417 0.076 Uiso 1 1 calc R . . C10B C 1.9003(8) 0.0095(6) 0.8126(7) 0.053(3) Uani 1 1 d . . . H10B H 1.9050 0.0189 0.7696 0.064 Uiso 1 1 calc R . . C11B C 1.8989(7) -0.0595(6) 0.8347(5) 0.037(3) Uani 1 1 d . . . H11B H 1.9039 -0.0985 0.8065 0.044 Uiso 1 1 calc R . . N12B N 1.8906(6) -0.0742(4) 0.8949(4) 0.033(2) Uani 1 1 d . . . N1C N 1.5603(6) -0.4455(4) 0.8511(4) 0.0269(18) Uani 1 1 d . . . C2C C 1.4811(7) -0.4300(5) 0.8741(5) 0.030(2) Uani 1 1 d . . . H2C H 1.4721 -0.3824 0.8885 0.036 Uiso 1 1 calc R . . C3C C 1.4126(7) -0.4807(6) 0.8774(5) 0.036(2) Uani 1 1 d . . . H3C H 1.3557 -0.4677 0.8925 0.043 Uiso 1 1 calc R . . C4C C 1.4262(8) -0.5509(6) 0.8587(5) 0.036(3) Uani 1 1 d . . . H4C H 1.3798 -0.5871 0.8619 0.043 Uiso 1 1 calc R . . C5C C 1.5082(8) -0.5677(6) 0.8352(5) 0.039(3) Uani 1 1 d . . . H5C H 1.5187 -0.6155 0.8215 0.046 Uiso 1 1 calc R . . C6C C 1.5757(7) -0.5136(5) 0.8317(5) 0.028(2) Uani 1 1 d . . . C7C C 1.6649(7) -0.5239(5) 0.8071(5) 0.030(2) Uani 1 1 d . . . C8C C 1.6958(8) -0.5909(5) 0.7886(5) 0.038(3) Uani 1 1 d . . . H8C H 1.6581 -0.6331 0.7902 0.045 Uiso 1 1 calc R . . C9C C 1.7837(8) -0.5946(6) 0.7678(5) 0.041(3) Uani 1 1 d . . . H9C H 1.8071 -0.6393 0.7548 0.050 Uiso 1 1 calc R . . C10C C 1.8358(8) -0.5319(5) 0.7667(5) 0.034(2) Uani 1 1 d . . . H10C H 1.8956 -0.5332 0.7525 0.041 Uiso 1 1 calc R . . C11C C 1.8019(7) -0.4676(5) 0.7860(4) 0.030(2) Uani 1 1 d . . . H11C H 1.8387 -0.4249 0.7850 0.036 Uiso 1 1 calc R . . N12C N 1.7176(5) -0.4639(4) 0.8063(4) 0.0242(17) Uani 1 1 d . . . N1D N 1.8033(6) -0.4525(4) 0.9621(4) 0.0266(18) Uani 1 1 d . . . C2D C 1.7198(7) -0.4718(5) 0.9777(5) 0.031(2) Uani 1 1 d . . . H2D H 1.6789 -0.4357 0.9900 0.037 Uiso 1 1 calc R . . C3D C 1.6923(7) -0.5431(6) 0.9762(5) 0.033(2) Uani 1 1 d . . . H3D H 1.6333 -0.5563 0.9882 0.039 Uiso 1 1 calc R . . C4D C 1.7506(7) -0.5957(6) 0.9572(5) 0.035(2) Uani 1 1 d . . . H4D H 1.7308 -0.6448 0.9544 0.041 Uiso 1 1 calc R . . C5D C 1.8376(7) -0.5764(5) 0.9423(5) 0.030(2) Uani 1 1 d . . . H5D H 1.8799 -0.6121 0.9312 0.036 Uiso 1 1 calc R . . C6D C 1.8624(6) -0.5033(5) 0.9437(4) 0.023(2) Uani 1 1 d . . . C7D C 1.9517(7) -0.4757(5) 0.9266(4) 0.028(2) Uani 1 1 d . . . C8D C 2.0207(7) -0.5184(6) 0.9074(5) 0.033(2) Uani 1 1 d . . . H8D H 2.0131 -0.5695 0.9057 0.039 Uiso 1 1 calc R . . C9D C 2.1010(7) -0.4870(6) 0.8908(5) 0.038(3) Uani 1 1 d . . . H9D H 2.1494 -0.5158 0.8776 0.046 Uiso 1 1 calc R . . C10D C 2.1095(8) -0.4117(6) 0.8937(5) 0.036(3) Uani 1 1 d . . . H10D H 2.1634 -0.3884 0.8817 0.043 Uiso 1 1 calc R . . C11D C 2.0387(7) -0.3715(6) 0.9141(5) 0.038(3) Uani 1 1 d . . . H11D H 2.0450 -0.3204 0.9163 0.045 Uiso 1 1 calc R . . N12D N 1.9611(5) -0.4022(4) 0.9311(4) 0.0282(18) Uani 1 1 d . . . O3W O 1.0743(5) -0.1923(4) 0.8214(4) 0.046(2) Uani 1 1 d . . . O4W O 0.8458(6) -0.1792(4) 0.5539(4) 0.057(2) Uani 1 1 d . . . O5W O 1.2861(5) -0.3376(4) 0.8379(4) 0.047(2) Uani 1 1 d . . . O6W O 1.4078(8) 0.2518(5) 0.6346(6) 0.088(4) Uani 1 1 d . . . O7W O 1.3151(6) -0.7483(5) 0.4425(4) 0.060(2) Uani 1 1 d . . . O8W O 1.2278(7) -0.3465(5) 0.3886(4) 0.067(3) Uani 1 1 d . . . O9W O 1.2142(7) -0.7598(6) 0.6316(6) 0.089(3) Uani 1 1 d . . . O10W O 1.5418(6) -0.3167(5) 0.4719(4) 0.063(3) Uani 1 1 d . . . O11W O 1.4526(5) -0.1524(4) 0.9277(4) 0.0452(19) Uani 1 1 d . . . O12W O 1.0000 -0.3908(5) 0.7500 0.036(2) Uani 1 2 d S . . O13W O 1.1703(12) -0.8025(7) 0.7497(8) 0.127(5) Uani 1 1 d . . . O14W O 1.0530(16) -0.3243(12) 0.3139(10) 0.116(9) Uiso 0.67(3) 1 d P A 2 O15W O 0.9912(19) -0.2606(15) 0.2926(13) 0.060(10) Uiso 0.33(3) 1 d P A 1 O16W O 1.465(3) 0.2395(19) 0.762(2) 0.178(16) Uiso 0.50 1 d P . . O17W O 1.4159(10) -0.8274(8) 0.9019(6) 0.035(3) Uiso 0.50 1 d P B 2 O18W O 1.3465(19) -0.7902(15) 0.8718(13) 0.105(8) Uiso 0.50 1 d P B 2 O19W O 1.3107(11) -0.7393(9) 0.8161(8) 0.050(4) Uiso 0.50 1 d P C 1 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 Cu1 0.0260(6) 0.0127(6) 0.0268(6) 0.0001(5) 0.0013(5) 0.0017(4) Cu2 0.0237(6) 0.0123(6) 0.0333(7) 0.0006(5) 0.0000(5) -0.0005(4) Cu3 0.0296(6) 0.0147(6) 0.0342(7) -0.0017(5) -0.0033(5) 0.0001(5) Cu4 0.0308(6) 0.0150(6) 0.0331(7) 0.0024(5) -0.0008(5) 0.0019(5) P1 0.0177(11) 0.0114(11) 0.0299(13) -0.0021(9) 0.0020(9) 0.0008(9) O11 0.020(3) 0.014(3) 0.042(4) 0.001(3) 0.000(3) -0.001(3) O12 0.023(3) 0.023(3) 0.025(4) -0.001(3) 0.000(3) -0.004(3) O13 0.024(3) 0.020(3) 0.037(4) -0.005(3) 0.001(3) -0.006(3) O14 0.024(3) 0.026(4) 0.037(4) -0.002(3) 0.008(3) 0.002(3) P2 0.0299(13) 0.0142(12) 0.0299(14) 0.0026(10) 0.0080(10) 0.0028(10) O21 0.029(3) 0.016(3) 0.031(4) -0.001(3) -0.001(3) 0.002(3) O22 0.025(3) 0.019(3) 0.041(4) 0.000(3) 0.003(3) -0.001(3) O23 0.038(4) 0.025(4) 0.032(4) 0.002(3) 0.003(3) 0.013(3) O24 0.038(4) 0.028(4) 0.040(4) 0.006(3) 0.014(3) 0.002(3) C3 0.050(7) 0.025(6) 0.052(7) 0.001(5) -0.009(6) 0.001(5) O31 0.039(4) 0.017(4) 0.047(5) 0.000(3) -0.013(3) -0.005(3) O32 0.061(6) 0.029(5) 0.089(7) 0.019(5) -0.010(5) -0.003(4) O33 0.040(4) 0.039(5) 0.059(5) 0.000(4) -0.008(4) -0.010(4) O1W 0.026(3) 0.024(4) 0.040(4) -0.001(3) 0.005(3) -0.001(3) O2W 0.026(3) 0.023(4) 0.030(4) 0.000(3) -0.005(3) -0.001(3) N1A 0.023(4) 0.022(4) 0.040(5) -0.007(4) 0.000(4) -0.003(3) C2A 0.035(6) 0.030(6) 0.033(6) -0.006(4) 0.001(5) 0.007(5) C3A 0.049(7) 0.043(8) 0.052(8) -0.023(6) 0.002(6) -0.003(6) C4A 0.076(9) 0.034(7) 0.076(10) -0.025(7) 0.031(8) 0.002(7) C5A 0.064(8) 0.012(6) 0.105(12) 0.003(6) 0.031(8) -0.002(5) C6A 0.020(5) 0.022(5) 0.054(7) -0.005(5) 0.002(5) -0.002(4) C7A 0.029(5) 0.003(4) 0.052(7) 0.004(4) 0.000(5) 0.000(4) C8A 0.058(8) 0.030(6) 0.063(9) 0.020(6) 0.009(7) 0.003(6) C9A 0.058(8) 0.045(8) 0.058(9) 0.027(6) 0.000(7) -0.007(6) C10A 0.064(8) 0.044(8) 0.036(7) 0.011(5) -0.002(6) -0.008(6) C11A 0.037(6) 0.027(6) 0.036(6) 0.005(5) 0.003(5) -0.008(4) N12A 0.031(4) 0.016(4) 0.034(5) 0.002(3) 0.000(4) -0.004(3) N1B 0.027(4) 0.041(5) 0.030(5) -0.003(4) -0.006(4) 0.000(4) C2B 0.047(7) 0.058(8) 0.041(7) -0.006(6) 0.001(6) -0.001(6) C3B 0.066(9) 0.096(12) 0.035(7) -0.010(7) 0.013(6) 0.022(8) C4B 0.055(8) 0.074(11) 0.071(11) -0.038(8) 0.004(7) 0.007(7) C5B 0.043(7) 0.038(7) 0.064(9) -0.026(6) -0.006(6) 0.005(5) C6B 0.031(6) 0.029(6) 0.053(7) -0.007(5) -0.009(5) 0.010(5) C7B 0.025(5) 0.022(6) 0.064(8) -0.011(5) -0.011(5) -0.002(4) C8B 0.038(6) 0.018(6) 0.087(10) -0.002(6) -0.005(6) 0.003(5) C9B 0.059(8) 0.015(6) 0.110(13) 0.012(7) -0.007(8) -0.004(6) C10B 0.046(7) 0.034(7) 0.077(9) 0.020(6) 0.002(6) -0.011(6) C11B 0.032(6) 0.033(6) 0.042(7) 0.004(5) -0.004(5) 0.002(5) N12B 0.031(5) 0.016(4) 0.049(6) -0.008(4) -0.005(4) 0.001(3) N1C 0.035(5) 0.011(4) 0.031(5) 0.003(3) -0.002(4) -0.001(3) C2C 0.030(5) 0.020(5) 0.037(6) 0.002(4) 0.003(4) 0.000(4) C3C 0.034(6) 0.034(6) 0.036(6) 0.009(5) -0.002(5) -0.003(5) C4C 0.040(6) 0.028(6) 0.038(6) 0.003(5) 0.000(5) -0.016(5) C5C 0.058(7) 0.017(5) 0.039(6) -0.004(4) -0.001(5) -0.017(5) C6C 0.035(5) 0.014(5) 0.032(5) -0.002(4) -0.007(4) 0.000(4) C7C 0.040(6) 0.018(5) 0.028(6) -0.002(4) -0.010(4) -0.002(4) C8C 0.059(7) 0.017(5) 0.032(6) -0.007(4) -0.007(5) 0.010(5) C9C 0.058(7) 0.025(6) 0.040(7) -0.001(5) 0.005(6) 0.017(5) C10C 0.037(6) 0.028(6) 0.034(6) -0.008(4) -0.002(5) 0.010(5) C11C 0.039(6) 0.024(5) 0.026(5) -0.001(4) -0.001(4) 0.005(4) N12C 0.028(4) 0.012(4) 0.031(5) 0.000(3) 0.001(3) 0.001(3) N1D 0.033(5) 0.019(4) 0.023(4) 0.006(3) -0.007(3) 0.005(3) C2D 0.035(6) 0.032(6) 0.024(5) 0.004(4) -0.001(4) 0.002(5) C3D 0.032(5) 0.033(6) 0.029(6) 0.009(4) -0.004(4) -0.010(5) C4D 0.037(6) 0.023(5) 0.041(6) 0.004(4) -0.002(5) -0.012(5) C5D 0.022(5) 0.018(5) 0.047(6) -0.002(4) -0.004(4) 0.004(4) C6D 0.024(5) 0.020(5) 0.024(5) 0.005(4) -0.002(4) 0.003(4) C7D 0.030(5) 0.027(6) 0.022(5) 0.005(4) -0.008(4) 0.007(4) C8D 0.037(6) 0.029(6) 0.029(6) 0.000(4) -0.003(5) 0.008(5) C9D 0.032(6) 0.050(7) 0.031(6) 0.005(5) 0.000(5) 0.008(5) C10D 0.040(6) 0.044(7) 0.022(5) 0.011(5) 0.000(5) -0.003(5) C11D 0.035(6) 0.035(6) 0.040(6) 0.011(5) -0.004(5) -0.001(5) N12D 0.029(4) 0.022(4) 0.030(5) 0.004(3) -0.006(4) -0.003(3) O3W 0.040(4) 0.039(5) 0.058(5) -0.010(4) 0.008(4) -0.004(4) O4W 0.059(5) 0.043(5) 0.068(6) 0.015(4) 0.006(5) 0.007(4) O5W 0.041(4) 0.052(5) 0.048(5) 0.016(4) 0.007(4) 0.000(4) O6W 0.079(7) 0.043(6) 0.131(10) 0.013(6) -0.016(7) -0.014(5) O7W 0.046(5) 0.073(7) 0.059(6) -0.003(5) 0.002(4) 0.001(5) O8W 0.097(7) 0.053(6) 0.045(5) -0.001(4) -0.008(5) -0.005(5) O9W 0.065(7) 0.069(7) 0.121(10) 0.008(6) -0.016(6) -0.018(5) O10W 0.053(5) 0.057(6) 0.081(7) -0.028(5) 0.014(5) 0.009(4) O11W 0.045(5) 0.041(5) 0.052(5) 0.004(4) 0.014(4) 0.012(4) O12W 0.038(6) 0.026(5) 0.044(6) 0.000 0.003(5) 0.000 O13W 0.157(13) 0.070(9) 0.155(13) 0.010(8) 0.031(11) -0.013(9) _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 Cu1 O11 1.902(6) . ? Cu1 O21 1.931(6) . ? Cu1 N12A 2.002(8) . ? Cu1 N1A 2.003(8) . ? Cu1 O1W 2.343(7) . ? Cu2 O12 1.941(6) . ? Cu2 O22 1.953(6) . ? Cu2 N12C 2.007(7) . ? Cu2 N1C 2.016(8) . ? Cu2 O2W 2.309(6) . ? Cu3 O13 1.912(7) . ? Cu3 O31 1.955(7) . ? Cu3 N1B 1.990(9) . ? Cu3 N12B 2.023(8) . ? Cu3 O21 2.302(7) . ? Cu4 O23 1.932(7) . ? Cu4 O31 1.953(7) . ? Cu4 N12D 1.986(8) . ? Cu4 N1D 2.031(8) . ? Cu4 O12 2.287(6) . ? P1 O14 1.519(7) . ? P1 O13 1.536(6) . ? P1 O12 1.557(6) . ? P1 O11 1.569(6) . ? P2 O24 1.497(7) . ? P2 O23 1.532(7) . ? P2 O22 1.552(7) . ? P2 O21 1.568(7) . ? C3 O33 1.257(13) . ? C3 O32 1.259(14) . ? C3 O31 1.339(13) . ? N1A C2A 1.334(13) . ? N1A C6A 1.350(13) . ? C2A C3A 1.372(15) . ? C3A C4A 1.358(18) . ? C4A C5A 1.411(19) . ? C5A C6A 1.401(15) . ? C6A C7A 1.462(15) . ? C7A N12A 1.361(12) . ? C7A C8A 1.411(14) . ? C8A C9A 1.345(18) . ? C9A C10A 1.374(18) . ? C10A C11A 1.377(15) . ? C11A N12A 1.331(13) . ? N1B C2B 1.346(15) . ? N1B C6B 1.348(13) . ? C2B C3B 1.410(17) . ? C3B C4B 1.39(2) . ? C4B C5B 1.36(2) . ? C5B C6B 1.390(15) . ? C6B C7B 1.492(16) . ? C7B N12B 1.344(13) . ? C7B C8B 1.380(15) . ? C8B C9B 1.368(19) . ? C9B C10B 1.420(19) . ? C10B C11B 1.361(15) . ? C11B N12B 1.342(14) . ? N1C C2C 1.333(12) . ? N1C C6C 1.355(12) . ? C2C C3C 1.363(14) . ? C3C C4C 1.383(15) . ? C4C C5C 1.381(15) . ? C5C C6C 1.398(14) . ? C6C C7C 1.466(14) . ? C7C N12C 1.342(12) . ? C7C C8C 1.393(13) . ? C8C C9C 1.398(16) . ? C9C C10C 1.379(15) . ? C10C C11C 1.372(13) . ? C11C N12C 1.343(12) . ? N1D C2D 1.335(13) . ? N1D C6D 1.361(12) . ? C2D C3D 1.376(14) . ? C3D C4D 1.382(15) . ? C4D C5D 1.375(14) . ? C5D C6D 1.396(13) . ? C6D C7D 1.472(13) . ? C7D N12D 1.368(12) . ? C7D C8D 1.373(14) . ? C8D C9D 1.381(15) . ? C9D C10D 1.398(15) . ? C10D C11D 1.379(15) . ? C11D N12D 1.344(13) . ? O16W O16W 1.19(7) 2_856 ? O17W O18W 1.29(3) . ? 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 O11 Cu1 O21 93.8(3) . . ? O11 Cu1 N12A 90.4(3) . . ? O21 Cu1 N12A 164.1(3) . . ? O11 Cu1 N1A 169.3(3) . . ? O21 Cu1 N1A 92.9(3) . . ? N12A Cu1 N1A 80.9(3) . . ? O11 Cu1 O1W 90.5(2) . . ? O21 Cu1 O1W 100.7(3) . . ? N12A Cu1 O1W 94.6(3) . . ? N1A Cu1 O1W 96.3(3) . . ? O12 Cu2 O22 93.1(3) . . ? O12 Cu2 N12C 92.1(3) . . ? O22 Cu2 N12C 170.5(3) . . ? O12 Cu2 N1C 163.5(3) . . ? O22 Cu2 N1C 92.4(3) . . ? N12C Cu2 N1C 80.5(3) . . ? O12 Cu2 O2W 99.7(2) . . ? O22 Cu2 O2W 90.1(3) . . ? N12C Cu2 O2W 96.9(3) . . ? N1C Cu2 O2W 95.8(3) . . ? O13 Cu3 O31 91.0(3) . . ? O13 Cu3 N1B 172.3(3) . . ? O31 Cu3 N1B 96.2(3) . . ? O13 Cu3 N12B 91.7(3) . . ? O31 Cu3 N12B 158.8(3) . . ? N1B Cu3 N12B 80.6(4) . . ? O13 Cu3 O21 92.9(2) . . ? O31 Cu3 O21 97.7(3) . . ? N1B Cu3 O21 88.7(3) . . ? N12B Cu3 O21 103.2(3) . . ? O23 Cu4 O31 92.9(3) . . ? O23 Cu4 N12D 173.4(3) . . ? O31 Cu4 N12D 93.2(3) . . ? O23 Cu4 N1D 92.1(3) . . ? O31 Cu4 N1D 161.7(3) . . ? N12D Cu4 N1D 81.3(3) . . ? O23 Cu4 O12 91.4(3) . . ? O31 Cu4 O12 101.0(3) . . ? N12D Cu4 O12 89.9(3) . . ? N1D Cu4 O12 96.5(3) . . ? O14 P1 O13 110.3(4) . . ? O14 P1 O12 111.2(4) . . ? O13 P1 O12 108.0(4) . . ? O14 P1 O11 108.3(4) . . ? O13 P1 O11 110.0(4) . . ? O12 P1 O11 109.1(3) . . ? P1 O11 Cu1 124.9(4) . . ? P1 O12 Cu2 124.9(4) . . ? P1 O12 Cu4 126.1(3) . . ? Cu2 O12 Cu4 103.8(3) . . ? P1 O13 Cu3 125.9(4) . . ? O24 P2 O23 110.3(4) . . ? O24 P2 O22 109.1(4) . . ? O23 P2 O22 109.6(4) . . ? O24 P2 O21 110.3(4) . . ? O23 P2 O21 108.6(4) . . ? O22 P2 O21 108.9(4) . . ? P2 O21 Cu1 125.2(4) . . ? P2 O21 Cu3 129.5(3) . . ? Cu1 O21 Cu3 99.8(3) . . ? P2 O22 Cu2 123.7(4) . . ? P2 O23 Cu4 126.0(4) . . ? O33 C3 O32 124.9(11) . . ? O33 C3 O31 118.1(10) . . ? O32 C3 O31 117.0(10) . . ? C3 O31 Cu4 116.5(7) . . ? C3 O31 Cu3 124.3(6) . . ? Cu4 O31 Cu3 117.6(3) . . ? C2A N1A C6A 119.1(9) . . ? C2A N1A Cu1 126.1(7) . . ? C6A N1A Cu1 114.8(7) . . ? N1A C2A C3A 122.5(11) . . ? C4A C3A C2A 119.7(12) . . ? C3A C4A C5A 119.7(11) . . ? C6A C5A C4A 117.3(11) . . ? N1A C6A C5A 121.7(11) . . ? N1A C6A C7A 114.9(8) . . ? C5A C6A C7A 123.4(10) . . ? N12A C7A C8A 119.1(10) . . ? N12A C7A C6A 114.7(8) . . ? C8A C7A C6A 126.2(9) . . ? C9A C8A C7A 120.2(11) . . ? C8A C9A C10A 120.1(11) . . ? C9A C10A C11A 118.4(12) . . ? N12A C11A C10A 122.6(11) . . ? C11A N12A C7A 119.6(9) . . ? C11A N12A Cu1 125.9(7) . . ? C7A N12A Cu1 114.6(7) . . ? C2B N1B C6B 119.5(10) . . ? C2B N1B Cu3 124.7(8) . . ? C6B N1B Cu3 115.7(7) . . ? N1B C2B C3B 120.3(13) . . ? C4B C3B C2B 119.7(13) . . ? C5B C4B C3B 118.7(12) . . ? C4B C5B C6B 120.1(12) . . ? N1B C6B C5B 121.7(12) . . ? N1B C6B C7B 114.6(9) . . ? C5B C6B C7B 123.7(11) . . ? N12B C7B C8B 124.1(12) . . ? N12B C7B C6B 113.7(9) . . ? C8B C7B C6B 122.1(11) . . ? C9B C8B C7B 116.4(12) . . ? C8B C9B C10B 120.7(11) . . ? C11B C10B C9B 118.0(13) . . ? N12B C11B C10B 122.2(11) . . ? C11B N12B C7B 118.5(9) . . ? C11B N12B Cu3 126.2(7) . . ? C7B N12B Cu3 115.3(8) . . ? C2C N1C C6C 120.0(8) . . ? C2C N1C Cu2 125.7(6) . . ? C6C N1C Cu2 114.3(7) . . ? N1C C2C C3C 121.9(9) . . ? C2C C3C C4C 119.7(10) . . ? C5C C4C C3C 118.9(9) . . ? C4C C5C C6C 119.3(10) . . ? N1C C6C C5C 120.2(9) . . ? N1C C6C C7C 115.1(8) . . ? C5C C6C C7C 124.7(9) . . ? N12C C7C C8C 122.0(10) . . ? N12C C7C C6C 114.6(8) . . ? C8C C7C C6C 123.4(9) . . ? C7C C8C C9C 118.2(10) . . ? C10C C9C C8C 118.6(10) . . ? C11C C10C C9C 120.4(10) . . ? N12C C11C C10C 121.2(10) . . ? C7C N12C C11C 119.5(8) . . ? C7C N12C Cu2 115.4(6) . . ? C11C N12C Cu2 124.8(6) . . ? C2D N1D C6D 120.4(8) . . ? C2D N1D Cu4 126.2(7) . . ? C6D N1D Cu4 113.4(6) . . ? N1D C2D C3D 120.9(10) . . ? C2D C3D C4D 119.9(10) . . ? C5D C4D C3D 119.5(9) . . ? C4D C5D C6D 118.7(9) . . ? N1D C6D C5D 120.6(9) . . ? N1D C6D C7D 115.7(8) . . ? C5D C6D C7D 123.7(9) . . ? N12D C7D C8D 121.7(9) . . ? N12D C7D C6D 113.9(8) . . ? C8D C7D C6D 124.4(9) . . ? C7D C8D C9D 119.8(10) . . ? C8D C9D C10D 118.5(10) . . ? C11D C10D C9D 119.2(10) . . ? N12D C11D C10D 122.3(10) . . ? C11D N12D C7D 118.4(9) . . ? C11D N12D Cu4 125.8(7) . . ? C7D N12D Cu4 115.7(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.256 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.161 data_2 _database_code_CSD 216730 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H79 Cu4 N8 O32.50 P2' _chemical_formula_weight 1616.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4810(17) _cell_length_b 14.7144(18) _cell_length_c 20.655(3) _cell_angle_alpha 97.999(10) _cell_angle_beta 100.838(10) _cell_angle_gamma 114.495(10) _cell_volume 3288.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 4.90 _cell_measurement_theta_max 12.47 _exptl_crystal_description 'Irregular block' _exptl_crystal_colour Blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1662 _exptl_absorpt_coefficient_mu 1.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8070 _exptl_absorpt_correction_T_max 0.9452 _exptl_absorpt_process_details 'Psi Scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11941 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11366 _reflns_number_gt 7933 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+18.2607P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11366 _refine_ls_number_parameters 786 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2114 _refine_ls_wR_factor_gt 0.1866 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.022 _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 Cu1 Cu 0.92949(8) 0.61203(6) 0.32935(4) 0.0286(2) Uani 1 1 d . . . Cu2 Cu 1.18832(8) 0.80699(7) 0.34333(5) 0.0341(3) Uani 1 1 d . . . Cu3 Cu 0.79884(8) 0.59552(6) 0.16748(4) 0.0275(2) Uani 1 1 d . . . Cu4 Cu 0.99180(8) 0.82769(7) 0.15989(5) 0.0318(2) Uani 1 1 d . . . P1 P 0.9397(2) 0.81369(14) 0.30088(11) 0.0344(5) Uani 1 1 d . . . O11 O 0.8870(5) 0.7239(4) 0.3356(3) 0.0387(13) Uani 1 1 d . . . O12 O 1.0811(5) 0.8712(4) 0.3278(3) 0.0371(13) Uani 1 1 d . . . O13 O 0.9021(4) 0.7669(4) 0.2233(3) 0.0325(12) Uani 1 1 d . . . O14 O 0.8867(6) 0.8880(4) 0.3156(3) 0.0474(15) Uani 1 1 d . . . P2 P 1.07524(17) 0.66865(14) 0.19702(10) 0.0273(4) Uani 1 1 d . . . O21 O 0.9443(4) 0.5870(4) 0.1557(2) 0.0298(11) Uani 1 1 d . . . O22 O 1.1058(5) 0.7730(4) 0.1788(3) 0.0316(11) Uani 1 1 d . . . O23 O 1.0817(4) 0.6822(3) 0.2739(2) 0.0277(11) Uani 1 1 d . . . O24 O 1.1676(5) 0.6338(4) 0.1804(3) 0.0329(12) Uani 1 1 d . . . C3 C 0.7090(7) 0.4478(6) 0.2455(4) 0.0343(17) Uani 1 1 d . . . O31 O 0.8018(4) 0.5346(4) 0.2448(3) 0.0349(12) Uani 1 1 d . . . O32 O 0.7017(5) 0.4277(5) 0.3025(3) 0.0486(15) Uani 1 1 d . . . O33 O 0.6344(5) 0.3904(4) 0.1894(3) 0.0455(14) Uani 1 1 d . . . N1A N 1.0256(6) 0.6638(5) 0.4287(3) 0.0353(15) Uani 1 1 d . . . C2A C 1.0387(8) 0.7446(6) 0.4739(4) 0.049(2) Uani 1 1 d . . . H2AA H 1.0017 0.7859 0.4596 0.058 Uiso 1 1 calc R . . C3A C 1.1059(9) 0.7702(8) 0.5424(5) 0.063(3) Uani 1 1 d . . . H3AA H 1.1130 0.8271 0.5742 0.075 Uiso 1 1 calc R . . C4A C 1.1606(9) 0.7113(9) 0.5619(5) 0.066(3) Uani 1 1 d . . . H4AA H 1.2093 0.7292 0.6073 0.079 Uiso 1 1 calc R . . C5A C 1.1459(7) 0.6247(8) 0.5157(5) 0.055(3) Uani 1 1 d . . . C6A C 1.1952(8) 0.5564(10) 0.5315(5) 0.066(3) Uani 1 1 d . . . H6AA H 1.2420 0.5690 0.5766 0.079 Uiso 1 1 calc R . . C7A C 1.1776(8) 0.4740(10) 0.4843(5) 0.062(3) Uani 1 1 d . . . H7AA H 1.2136 0.4309 0.4964 0.074 Uiso 1 1 calc R . . C8A C 1.1043(8) 0.4515(8) 0.4156(5) 0.049(2) Uani 1 1 d . . . C9A C 1.0791(9) 0.3674(8) 0.3644(5) 0.059(3) Uani 1 1 d . . . H9AA H 1.1110 0.3206 0.3732 0.070 Uiso 1 1 calc R . . C10A C 1.0066(9) 0.3528(7) 0.3003(5) 0.055(3) Uani 1 1 d . . . H10A H 0.9873 0.2950 0.2651 0.066 Uiso 1 1 calc R . . C11A C 0.9623(8) 0.4229(6) 0.2878(4) 0.0375(18) Uani 1 1 d . . . H11A H 0.9151 0.4133 0.2433 0.045 Uiso 1 1 calc R . . N12A N 0.9836(5) 0.5020(5) 0.3355(3) 0.0309(14) Uani 1 1 d . . . C13A C 1.0554(7) 0.5170(6) 0.3988(4) 0.0366(18) Uani 1 1 d . . . C14A C 1.0765(7) 0.6046(7) 0.4485(4) 0.041(2) Uani 1 1 d . . . N1B N 1.2950(5) 0.7410(5) 0.3771(3) 0.0343(15) Uani 1 1 d . . . C2B C 1.3007(7) 0.6582(6) 0.3442(4) 0.0400(19) Uani 1 1 d . . . H2BA H 1.2555 0.6270 0.2979 0.048 Uiso 1 1 calc R . . C3B C 1.3716(7) 0.6180(7) 0.3770(4) 0.047(2) Uani 1 1 d . . . H3BA H 1.3745 0.5595 0.3530 0.056 Uiso 1 1 calc R . . C4B C 1.4381(8) 0.6618(7) 0.4441(4) 0.049(2) Uani 1 1 d . . . H4BA H 1.4866 0.6335 0.4660 0.059 Uiso 1 1 calc R . . C5B C 1.4342(7) 0.7467(7) 0.4792(4) 0.049(2) Uani 1 1 d . . . C6B C 1.4964(8) 0.7983(9) 0.5495(4) 0.060(3) Uani 1 1 d . . . H6BA H 1.5462 0.7739 0.5746 0.072 Uiso 1 1 calc R . . C7B C 1.4871(9) 0.8788(9) 0.5805(5) 0.069(3) Uani 1 1 d . . . H7BA H 1.5302 0.9107 0.6270 0.083 Uiso 1 1 calc R . . C8B C 0.9414(8) 0.8703(6) -0.0386(4) 0.044(2) Uani 1 1 d . . . C9B C 1.3973(9) 1.0033(8) 0.5732(5) 0.063(3) Uani 1 1 d . . . H9BA H 1.4397 1.0404 0.6190 0.076 Uiso 1 1 calc R . . C10B C 1.3234(10) 1.0314(8) 0.5357(5) 0.066(3) Uani 1 1 d . . . H10B H 1.3110 1.0873 0.5555 0.080 Uiso 1 1 calc R . . C11B C 1.2620(9) 0.9789(7) 0.4661(5) 0.056(3) Uani 1 1 d . . . H11B H 1.2109 1.0014 0.4400 0.067 Uiso 1 1 calc R . . N12B N 1.2752(6) 0.8999(5) 0.4376(3) 0.0432(18) Uani 1 1 d . . . C13B C 1.3508(7) 0.8701(7) 0.4762(4) 0.044(2) Uani 1 1 d . . . C14B C 1.3604(7) 0.7844(6) 0.4434(4) 0.041(2) Uani 1 1 d . . . N1C N 0.7567(5) 0.6123(4) 0.0718(3) 0.0272(13) Uani 1 1 d . . . C2C C 0.8149(7) 0.6124(5) 0.0243(4) 0.0332(17) Uani 1 1 d . . . H2CA H 0.8874 0.6043 0.0345 0.040 Uiso 1 1 calc R . . C3C C 0.7739(7) 0.6239(5) -0.0397(4) 0.0349(18) Uani 1 1 d . . . H3CA H 0.8181 0.6238 -0.0724 0.042 Uiso 1 1 calc R . . C4C C 0.6684(7) 0.6355(5) -0.0558(4) 0.0359(18) Uani 1 1 d . . . H4CA H 0.6401 0.6447 -0.0992 0.043 Uiso 1 1 calc R . . C5C C 0.6040(7) 0.6333(5) -0.0071(4) 0.0321(17) Uani 1 1 d . . . C6C C 0.4906(8) 0.6403(6) -0.0185(4) 0.041(2) Uani 1 1 d . . . H6CA H 0.4565 0.6484 -0.0611 0.050 Uiso 1 1 calc R . . C7C C 0.4316(7) 0.6356(6) 0.0309(4) 0.0400(19) Uani 1 1 d . . . H7CA H 0.3581 0.6425 0.0225 0.048 Uiso 1 1 calc R . . C8C C 0.4768(7) 0.6207(5) 0.0948(4) 0.0337(17) Uani 1 1 d . . . C9C C 0.4172(7) 0.6094(6) 0.1467(4) 0.043(2) Uani 1 1 d . . . H9CA H 0.3414 0.6122 0.1408 0.051 Uiso 1 1 calc R . . C10C C 0.4706(8) 0.5943(6) 0.2064(5) 0.045(2) Uani 1 1 d . . . H10C H 0.4308 0.5856 0.2417 0.054 Uiso 1 1 calc R . . C11C C 0.5817(7) 0.5919(6) 0.2149(4) 0.0375(18) Uani 1 1 d . . . H11C H 0.6182 0.5837 0.2570 0.045 Uiso 1 1 calc R . . N12C N 0.6397(6) 0.6006(5) 0.1666(3) 0.0316(14) Uani 1 1 d . . . C13C C 0.5893(6) 0.6151(5) 0.1081(4) 0.0276(15) Uani 1 1 d . . . C14C C 0.6522(6) 0.6211(5) 0.0565(4) 0.0263(15) Uani 1 1 d . . . N1D N 0.8626(6) 0.8688(5) 0.1227(3) 0.0359(15) Uani 1 1 d . . . C2D C 0.7806(8) 0.8786(6) 0.1511(5) 0.046(2) Uani 1 1 d . . . H2DA H 0.7851 0.8726 0.1966 0.056 Uiso 1 1 calc R . . C3D C 0.6870(9) 0.8977(7) 0.1167(6) 0.058(3) Uani 1 1 d . . . H3DA H 0.6291 0.9043 0.1384 0.069 Uiso 1 1 calc R . . C4D C 0.6807(9) 0.9067(7) 0.0514(6) 0.058(3) Uani 1 1 d . . . H4DA H 0.6174 0.9191 0.0273 0.070 Uiso 1 1 calc R . . C5D C 0.7664(8) 0.8977(6) 0.0199(5) 0.047(2) Uani 1 1 d . . . C6D C 0.7662(9) 0.9026(7) -0.0489(5) 0.055(2) Uani 1 1 d . . . H6DA H 0.7052 0.9147 -0.0759 0.066 Uiso 1 1 calc R . . C7D C 0.8505(9) 0.8905(6) -0.0759(5) 0.053(2) Uani 1 1 d . . . H7DA H 0.8489 0.8956 -0.1214 0.063 Uiso 1 1 calc R . . C8D C 1.4127(8) 0.9182(7) 0.5448(5) 0.058(3) Uani 1 1 d . . . C9D C 1.0307(9) 0.8541(6) -0.0635(5) 0.053(2) Uani 1 1 d . . . H9DA H 1.0335 0.8574 -0.1088 0.063 Uiso 1 1 calc R . . C10D C 1.1130(9) 0.8338(7) -0.0234(5) 0.051(2) Uani 1 1 d . . . H10D H 1.1732 0.8229 -0.0406 0.061 Uiso 1 1 calc R . . C11D C 1.1096(9) 0.8286(6) 0.0441(4) 0.045(2) Uani 1 1 d . . . H11D H 1.1671 0.8138 0.0719 0.054 Uiso 1 1 calc R . . N12D N 1.0266(6) 0.8445(5) 0.0688(3) 0.0368(15) Uani 1 1 d . . . C13D C 0.9467(7) 0.8662(5) 0.0290(4) 0.0358(18) Uani 1 1 d . . . C14D C 0.8579(7) 0.8787(5) 0.0576(4) 0.0376(19) Uani 1 1 d . . . O1W O 1.3139(5) 0.9034(4) 0.2863(3) 0.0465(15) Uani 1 1 d . . . O2W O 1.1321(5) 0.9849(4) 0.2326(3) 0.0411(13) Uani 1 1 d . . . O3W O 0.2110(8) 0.2193(7) 0.4547(5) 0.096(3) Uiso 1 1 d . . . O4W O 0.6514(7) 0.8200(6) 0.3206(4) 0.076(2) Uiso 1 1 d . . . O5W O 0.4068(6) 0.2933(5) 0.2016(3) 0.0613(18) Uiso 1 1 d . . . O6W O 0.8830(6) 0.3884(5) 0.0939(3) 0.0543(16) Uiso 1 1 d . . . O7W O 0.2377(6) 0.3388(5) 0.2454(3) 0.0603(17) Uiso 1 1 d . . . O8W O 0.0581(6) 0.1343(5) 0.2288(3) 0.0607(17) Uiso 1 1 d . . . O9W O 0.1236(5) 0.4349(4) 0.1725(3) 0.0416(13) Uiso 1 1 d . . . O10W O 0.5720(7) 0.4951(6) 0.3740(4) 0.072(2) Uiso 1 1 d . . . O11W O 0.7133(7) 0.7028(5) 0.4040(4) 0.0678(19) Uiso 1 1 d . . . O12W O 0.6857(9) 0.2435(8) 0.1247(5) 0.106(3) Uiso 1 1 d . . . O13W O 0.6119(9) 0.2203(8) 0.2962(5) 0.105(3) Uiso 1 1 d . . . O14W O 0.3506(11) 0.3565(9) 0.3839(6) 0.131(4) Uiso 1 1 d . . . O15W O 0.3449(15) 0.7905(12) 0.1356(8) 0.184(6) Uiso 1 1 d . . . O16W O 0.702(2) 0.0952(17) 0.2552(10) 0.254(9) Uiso 1 1 d . . . O17W O 0.0000 0.0000 0.5000 0.083(6) Uiso 0.50 2 d SP A 1 O17' O 0.0188(15) 0.0411(12) 0.4428(8) 0.016(3) Uiso 0.25 1 d P B 2 O18W O 0.8991(11) 0.0793(9) 0.3015(6) 0.043(3) Uiso 0.50 1 d P C 1 O18' O 0.9744(19) 0.0892(15) 0.3454(10) 0.104(6) Uiso 0.50 1 d P D 2 O19W O 0.4151(12) 0.8047(10) 0.2267(6) 0.053(3) Uiso 0.50 1 d P E 1 O19' O 0.5204(13) 0.8872(11) 0.2564(7) 0.063(4) Uiso 0.50 1 d P F 2 O20W O 0.0790(15) 0.5584(12) 0.0302(8) 0.066(4) Uiso 0.50 1 d P G 1 O20' O 0.1392(14) 0.6045(11) 0.0404(7) 0.056(3) Uiso 0.50 1 d P H 2 O21W O 0.3671(12) 0.0913(10) 0.2072(7) 0.058(3) Uiso 0.50 1 d P I 1 O21' O 0.378(3) 0.170(3) 0.2719(19) 0.217(14) Uiso 0.50 1 d P J 2 O22W O 0.409(3) 0.896(2) 0.0083(14) 0.160(10) Uiso 0.50 1 d P K 1 O22' O 0.432(3) 0.961(2) 0.1269(15) 0.174(11) Uiso 0.50 1 d P L 2 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 Cu1 0.0300(5) 0.0251(5) 0.0293(5) 0.0084(4) 0.0126(4) 0.0090(4) Cu2 0.0311(5) 0.0262(5) 0.0368(5) 0.0016(4) 0.0161(4) 0.0042(4) Cu3 0.0290(5) 0.0276(5) 0.0299(5) 0.0104(4) 0.0121(4) 0.0136(4) Cu4 0.0369(5) 0.0249(5) 0.0418(5) 0.0135(4) 0.0210(4) 0.0156(4) P1 0.0442(12) 0.0240(10) 0.0451(12) 0.0119(8) 0.0294(10) 0.0165(9) O11 0.047(3) 0.034(3) 0.051(3) 0.018(3) 0.034(3) 0.022(3) O12 0.036(3) 0.023(3) 0.044(3) 0.003(2) 0.017(2) 0.005(2) O13 0.032(3) 0.027(3) 0.044(3) 0.011(2) 0.021(2) 0.014(2) O14 0.060(4) 0.037(3) 0.066(4) 0.021(3) 0.044(3) 0.027(3) P2 0.0294(10) 0.0231(9) 0.0331(10) 0.0073(7) 0.0150(8) 0.0123(8) O21 0.032(3) 0.027(3) 0.031(3) 0.005(2) 0.010(2) 0.014(2) O22 0.035(3) 0.031(3) 0.038(3) 0.014(2) 0.023(2) 0.016(2) O23 0.026(3) 0.020(2) 0.036(3) 0.007(2) 0.016(2) 0.005(2) O24 0.034(3) 0.031(3) 0.043(3) 0.010(2) 0.020(2) 0.019(2) C3 0.038(4) 0.035(4) 0.033(4) 0.017(3) 0.015(4) 0.014(4) O31 0.028(3) 0.029(3) 0.040(3) 0.017(2) 0.005(2) 0.005(2) O32 0.037(3) 0.064(4) 0.035(3) 0.023(3) 0.012(3) 0.010(3) O33 0.045(3) 0.038(3) 0.035(3) 0.007(3) -0.001(3) 0.007(3) N1A 0.032(3) 0.036(4) 0.030(3) 0.009(3) 0.016(3) 0.004(3) C2A 0.051(5) 0.039(5) 0.041(5) 0.003(4) 0.024(4) 0.003(4) C3A 0.049(6) 0.066(7) 0.035(5) 0.001(5) 0.020(4) -0.010(5) C4A 0.036(5) 0.088(8) 0.027(5) 0.005(5) 0.008(4) -0.013(5) C5A 0.025(4) 0.084(7) 0.040(5) 0.027(5) 0.014(4) 0.004(5) C6A 0.030(5) 0.117(10) 0.052(6) 0.037(7) 0.017(4) 0.027(6) C7A 0.040(5) 0.109(9) 0.068(7) 0.066(7) 0.029(5) 0.043(6) C8A 0.037(5) 0.069(6) 0.067(6) 0.048(5) 0.035(4) 0.031(5) C9A 0.063(6) 0.079(7) 0.080(7) 0.055(6) 0.051(6) 0.050(6) C10A 0.074(7) 0.057(6) 0.065(6) 0.030(5) 0.047(6) 0.042(5) C11A 0.051(5) 0.038(4) 0.038(4) 0.020(4) 0.026(4) 0.024(4) N12A 0.031(3) 0.039(4) 0.031(3) 0.017(3) 0.018(3) 0.017(3) C13A 0.031(4) 0.047(5) 0.043(5) 0.028(4) 0.025(4) 0.017(4) C14A 0.029(4) 0.050(5) 0.036(4) 0.016(4) 0.012(4) 0.006(4) N1B 0.022(3) 0.036(4) 0.031(3) 0.005(3) 0.009(3) 0.001(3) C2B 0.029(4) 0.048(5) 0.032(4) 0.002(4) 0.011(3) 0.008(4) C3B 0.033(5) 0.067(6) 0.046(5) 0.018(4) 0.018(4) 0.023(4) C4B 0.031(4) 0.068(6) 0.042(5) 0.015(4) 0.008(4) 0.018(4) C5B 0.023(4) 0.063(6) 0.044(5) 0.007(4) 0.010(4) 0.005(4) C6B 0.030(5) 0.094(8) 0.030(5) 0.002(5) 0.004(4) 0.009(5) C7B 0.039(5) 0.098(9) 0.030(5) 0.003(5) 0.008(4) -0.003(6) C8B 0.051(5) 0.024(4) 0.048(5) 0.009(4) 0.015(4) 0.009(4) C9B 0.049(6) 0.059(6) 0.043(6) -0.007(5) 0.019(5) -0.008(5) C10B 0.064(7) 0.051(6) 0.058(7) -0.016(5) 0.036(6) 0.003(5) C11B 0.057(6) 0.042(5) 0.056(6) -0.001(4) 0.033(5) 0.007(4) N12B 0.041(4) 0.027(3) 0.041(4) -0.005(3) 0.019(3) -0.004(3) C13B 0.025(4) 0.047(5) 0.038(5) 0.005(4) 0.017(4) -0.006(4) C14B 0.023(4) 0.047(5) 0.037(4) 0.005(4) 0.017(3) -0.001(4) N1C 0.027(3) 0.025(3) 0.029(3) 0.007(2) 0.008(3) 0.011(3) C2C 0.039(4) 0.027(4) 0.036(4) 0.006(3) 0.022(4) 0.012(3) C3C 0.042(5) 0.028(4) 0.028(4) 0.004(3) 0.016(3) 0.009(3) C4C 0.045(5) 0.022(4) 0.027(4) 0.003(3) 0.006(3) 0.005(3) C5C 0.037(4) 0.023(4) 0.030(4) 0.002(3) 0.006(3) 0.010(3) C6C 0.047(5) 0.026(4) 0.043(5) 0.005(3) -0.002(4) 0.015(4) C7C 0.030(4) 0.037(4) 0.054(5) 0.007(4) 0.003(4) 0.020(4) C8C 0.031(4) 0.025(4) 0.039(4) 0.001(3) 0.005(3) 0.012(3) C9C 0.032(4) 0.036(4) 0.058(6) -0.001(4) 0.016(4) 0.016(4) C10C 0.044(5) 0.046(5) 0.058(6) 0.014(4) 0.031(4) 0.023(4) C11C 0.041(5) 0.041(4) 0.041(5) 0.014(4) 0.023(4) 0.023(4) N12C 0.036(4) 0.032(3) 0.035(3) 0.013(3) 0.017(3) 0.018(3) C13C 0.025(4) 0.022(4) 0.031(4) 0.003(3) 0.010(3) 0.007(3) C14C 0.024(4) 0.020(3) 0.031(4) 0.005(3) 0.008(3) 0.006(3) N1D 0.039(4) 0.025(3) 0.045(4) 0.010(3) 0.013(3) 0.016(3) C2D 0.051(5) 0.032(4) 0.067(6) 0.018(4) 0.025(5) 0.023(4) C3D 0.040(5) 0.056(6) 0.080(7) 0.014(5) 0.015(5) 0.025(5) C4D 0.040(5) 0.051(6) 0.089(8) 0.026(5) 0.015(5) 0.024(5) C5D 0.041(5) 0.033(4) 0.056(6) 0.010(4) 0.006(4) 0.009(4) C6D 0.048(6) 0.038(5) 0.063(6) 0.013(4) -0.004(5) 0.013(4) C7D 0.062(6) 0.032(5) 0.043(5) 0.012(4) -0.001(5) 0.008(4) C8D 0.040(5) 0.057(6) 0.038(5) -0.008(4) 0.021(4) -0.013(4) C9D 0.078(7) 0.026(4) 0.044(5) 0.010(4) 0.022(5) 0.011(4) C10D 0.068(6) 0.040(5) 0.051(5) 0.014(4) 0.034(5) 0.022(5) C11D 0.062(6) 0.042(5) 0.054(5) 0.025(4) 0.038(5) 0.031(4) N12D 0.047(4) 0.029(3) 0.043(4) 0.019(3) 0.021(3) 0.019(3) C13D 0.036(4) 0.020(4) 0.045(5) 0.010(3) 0.015(4) 0.004(3) C14D 0.032(4) 0.018(4) 0.054(5) 0.007(3) 0.009(4) 0.006(3) O1W 0.033(3) 0.045(3) 0.056(4) 0.020(3) 0.021(3) 0.006(3) O2W 0.043(3) 0.028(3) 0.051(3) 0.008(2) 0.024(3) 0.010(2) _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 Cu1 O11 1.923(5) . ? Cu1 O31 1.944(5) . ? Cu1 N12A 2.006(6) . ? Cu1 N1A 2.027(6) . ? Cu1 O23 2.347(4) . ? Cu2 O23 1.930(5) . ? Cu2 O12 1.938(6) . ? Cu2 N12B 2.017(6) . ? Cu2 N1B 2.028(7) . ? Cu2 O1W 2.274(5) . ? Cu3 O21 1.928(5) . ? Cu3 O31 1.940(5) . ? Cu3 N12C 2.014(6) . ? Cu3 N1C 2.023(6) . ? Cu3 O13 2.300(5) . ? Cu4 O22 1.911(5) . ? Cu4 O13 1.953(5) . ? Cu4 N1D 2.007(7) . ? Cu4 N12D 2.033(6) . ? Cu4 O2W 2.315(5) . ? P1 O14 1.519(6) . ? P1 O12 1.549(6) . ? P1 O13 1.551(5) . ? P1 O11 1.553(5) . ? P2 O24 1.517(5) . ? P2 O22 1.541(5) . ? P2 O21 1.551(5) . ? P2 O23 1.554(5) . ? C3 O33 1.262(9) . ? C3 O32 1.265(9) . ? C3 O31 1.325(9) . ? N1A C2A 1.337(10) . ? N1A C14A 1.337(11) . ? C2A C3A 1.411(13) . ? C3A C4A 1.364(16) . ? C4A C5A 1.403(15) . ? C5A C14A 1.409(12) . ? C5A C6A 1.422(15) . ? C6A C7A 1.357(15) . ? C7A C8A 1.446(13) . ? C8A C13A 1.388(11) . ? C8A C9A 1.391(14) . ? C9A C10A 1.389(14) . ? C10A C11A 1.389(12) . ? C11A N12A 1.311(10) . ? N12A C13A 1.369(10) . ? C13A C14A 1.426(12) . ? N1B C2B 1.346(10) . ? N1B C14B 1.362(10) . ? C2B C3B 1.383(12) . ? C3B C4B 1.378(12) . ? C4B C5B 1.379(13) . ? C5B C14B 1.409(13) . ? C5B C6B 1.438(12) . ? C6B C7B 1.326(16) . ? C7B C8D 1.431(16) . ? C8B C13D 1.396(11) . ? C8B C9D 1.401(13) . ? C8B C7D 1.408(13) . ? C9B C10B 1.326(15) . ? C9B C8D 1.410(15) . ? C10B C11B 1.427(13) . ? C11B N12B 1.316(11) . ? N12B C13B 1.370(12) . ? C13B C8D 1.402(12) . ? C13B C14B 1.407(12) . ? N1C C2C 1.327(9) . ? N1C C14C 1.347(9) . ? C2C C3C 1.385(11) . ? C3C C4C 1.382(11) . ? C4C C5C 1.395(11) . ? C5C C14C 1.406(10) . ? C5C C6C 1.440(11) . ? C6C C7C 1.360(12) . ? C7C C8C 1.417(11) . ? C8C C9C 1.406(11) . ? C8C C13C 1.418(10) . ? C9C C10C 1.379(12) . ? C10C C11C 1.381(11) . ? C11C N12C 1.329(9) . ? N12C C13C 1.341(9) . ? C13C C14C 1.429(10) . ? N1D C2D 1.318(10) . ? N1D C14D 1.365(10) . ? C2D C3D 1.401(12) . ? C3D C4D 1.363(14) . ? C4D C5D 1.393(13) . ? C5D C14D 1.408(12) . ? C5D C6D 1.432(13) . ? C6D C7D 1.341(14) . ? C9D C10D 1.354(13) . ? C10D C11D 1.415(12) . ? C11D N12D 1.324(10) . ? N12D C13D 1.343(10) . ? C13D C14D 1.413(11) . ? 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 O11 Cu1 O31 92.0(2) . . ? O11 Cu1 N12A 172.8(2) . . ? O31 Cu1 N12A 94.7(2) . . ? O11 Cu1 N1A 91.2(3) . . ? O31 Cu1 N1A 163.1(2) . . ? N12A Cu1 N1A 81.7(3) . . ? O11 Cu1 O23 95.60(19) . . ? O31 Cu1 O23 93.46(19) . . ? N12A Cu1 O23 86.6(2) . . ? N1A Cu1 O23 102.7(2) . . ? O23 Cu2 O12 95.0(2) . . ? O23 Cu2 N12B 158.3(2) . . ? O12 Cu2 N12B 91.3(3) . . ? O23 Cu2 N1B 89.9(2) . . ? O12 Cu2 N1B 169.2(2) . . ? N12B Cu2 N1B 80.8(3) . . ? O23 Cu2 O1W 102.0(2) . . ? O12 Cu2 O1W 92.5(2) . . ? N12B Cu2 O1W 98.4(2) . . ? N1B Cu2 O1W 95.9(2) . . ? O21 Cu3 O31 91.2(2) . . ? O21 Cu3 N12C 172.6(2) . . ? O31 Cu3 N12C 94.8(2) . . ? O21 Cu3 N1C 91.4(2) . . ? O31 Cu3 N1C 161.7(2) . . ? N12C Cu3 N1C 81.5(2) . . ? O21 Cu3 O13 94.12(19) . . ? O31 Cu3 O13 99.6(2) . . ? N12C Cu3 O13 89.1(2) . . ? N1C Cu3 O13 98.2(2) . . ? O22 Cu4 O13 94.3(2) . . ? O22 Cu4 N1D 169.4(2) . . ? O13 Cu4 N1D 90.4(2) . . ? O22 Cu4 N12D 91.0(2) . . ? O13 Cu4 N12D 157.8(2) . . ? N1D Cu4 N12D 81.2(3) . . ? O22 Cu4 O2W 90.7(2) . . ? O13 Cu4 O2W 98.8(2) . . ? N1D Cu4 O2W 98.0(2) . . ? N12D Cu4 O2W 102.7(2) . . ? O14 P1 O12 109.7(3) . . ? O14 P1 O13 110.0(3) . . ? O12 P1 O13 109.8(3) . . ? O14 P1 O11 109.3(3) . . ? O12 P1 O11 110.3(3) . . ? O13 P1 O11 107.8(3) . . ? P1 O11 Cu1 123.0(3) . . ? P1 O12 Cu2 125.7(3) . . ? P1 O13 Cu4 125.2(3) . . ? P1 O13 Cu3 127.4(3) . . ? Cu4 O13 Cu3 101.9(2) . . ? O24 P2 O22 107.9(3) . . ? O24 P2 O21 109.5(3) . . ? O22 P2 O21 110.8(3) . . ? O24 P2 O23 111.1(3) . . ? O22 P2 O23 109.0(3) . . ? O21 P2 O23 108.4(3) . . ? P2 O21 Cu3 123.0(3) . . ? P2 O22 Cu4 124.6(3) . . ? P2 O23 Cu2 124.9(3) . . ? P2 O23 Cu1 131.1(3) . . ? Cu2 O23 Cu1 97.93(19) . . ? O33 C3 O32 124.3(7) . . ? O33 C3 O31 118.2(6) . . ? O32 C3 O31 117.5(7) . . ? C3 O31 Cu3 121.6(5) . . ? C3 O31 Cu1 117.8(5) . . ? Cu3 O31 Cu1 119.8(2) . . ? C2A N1A C14A 119.6(7) . . ? C2A N1A Cu1 127.9(6) . . ? C14A N1A Cu1 112.5(5) . . ? N1A C2A C3A 121.8(10) . . ? C4A C3A C2A 118.3(10) . . ? C3A C4A C5A 120.9(9) . . ? C4A C5A C14A 116.8(10) . . ? C4A C5A C6A 125.3(10) . . ? C14A C5A C6A 118.0(10) . . ? C7A C6A C5A 122.3(9) . . ? C6A C7A C8A 120.1(9) . . ? C13A C8A C9A 117.2(9) . . ? C13A C8A C7A 118.8(10) . . ? C9A C8A C7A 124.0(9) . . ? C10A C9A C8A 119.1(9) . . ? C9A C10A C11A 119.8(9) . . ? N12A C11A C10A 122.1(8) . . ? C11A N12A C13A 118.3(7) . . ? C11A N12A Cu1 129.1(5) . . ? C13A N12A Cu1 112.6(5) . . ? N12A C13A C8A 123.4(8) . . ? N12A C13A C14A 116.0(7) . . ? C8A C13A C14A 120.5(8) . . ? N1A C14A C5A 122.5(9) . . ? N1A C14A C13A 117.2(7) . . ? C5A C14A C13A 120.3(9) . . ? C2B N1B C14B 118.7(7) . . ? C2B N1B Cu2 128.3(5) . . ? C14B N1B Cu2 112.8(6) . . ? N1B C2B C3B 120.7(8) . . ? C4B C3B C2B 120.9(9) . . ? C3B C4B C5B 119.8(9) . . ? C4B C5B C14B 117.0(8) . . ? C4B C5B C6B 125.7(10) . . ? C14B C5B C6B 117.3(9) . . ? C7B C6B C5B 122.6(10) . . ? C6B C7B C8D 120.8(9) . . ? C13D C8B C9D 115.4(8) . . ? C13D C8B C7D 119.2(8) . . ? C9D C8B C7D 125.3(9) . . ? C10B C9B C8D 119.7(9) . . ? C9B C10B C11B 121.0(10) . . ? N12B C11B C10B 121.0(11) . . ? C11B N12B C13B 118.3(8) . . ? C11B N12B Cu2 128.2(7) . . ? C13B N12B Cu2 113.4(5) . . ? N12B C13B C8D 123.3(9) . . ? N12B C13B C14B 115.9(7) . . ? C8D C13B C14B 120.8(10) . . ? N1B C14B C13B 116.9(8) . . ? N1B C14B C5B 122.9(8) . . ? C13B C14B C5B 120.2(8) . . ? C2C N1C C14C 118.6(6) . . ? C2C N1C Cu3 129.0(5) . . ? C14C N1C Cu3 112.4(5) . . ? N1C C2C C3C 122.4(7) . . ? C4C C3C C2C 119.8(7) . . ? C3C C4C C5C 118.9(7) . . ? C4C C5C C14C 117.6(7) . . ? C4C C5C C6C 124.2(7) . . ? C14C C5C C6C 118.2(7) . . ? C7C C6C C5C 121.0(7) . . ? C6C C7C C8C 121.7(7) . . ? C9C C8C C7C 124.7(8) . . ? C9C C8C C13C 116.5(7) . . ? C7C C8C C13C 118.8(7) . . ? C10C C9C C8C 119.0(8) . . ? C9C C10C C11C 120.0(8) . . ? N12C C11C C10C 122.7(8) . . ? C11C N12C C13C 118.2(7) . . ? C11C N12C Cu3 129.1(5) . . ? C13C N12C Cu3 112.7(5) . . ? N12C C13C C8C 123.5(7) . . ? N12C C13C C14C 116.8(6) . . ? C8C C13C C14C 119.6(7) . . ? N1C C14C C5C 122.8(6) . . ? N1C C14C C13C 116.5(6) . . ? C5C C14C C13C 120.7(7) . . ? C2D N1D C14D 119.2(7) . . ? C2D N1D Cu4 128.3(6) . . ? C14D N1D Cu4 112.3(5) . . ? N1D C2D C3D 122.5(9) . . ? C4D C3D C2D 118.8(9) . . ? C3D C4D C5D 120.4(9) . . ? C4D C5D C14D 117.6(9) . . ? C4D C5D C6D 125.1(9) . . ? C14D C5D C6D 117.2(9) . . ? C7D C6D C5D 121.2(9) . . ? C6D C7D C8B 121.8(9) . . ? C13B C8D C9B 116.7(11) . . ? C13B C8D C7B 118.3(10) . . ? C9B C8D C7B 125.0(9) . . ? C10D C9D C8B 120.4(8) . . ? C9D C10D C11D 120.3(9) . . ? N12D C11D C10D 120.3(9) . . ? C11D N12D C13D 118.9(7) . . ? C11D N12D Cu4 127.9(6) . . ? C13D N12D Cu4 113.0(5) . . ? N12D C13D C8B 124.6(8) . . ? N12D C13D C14D 116.0(7) . . ? C8B C13D C14D 119.2(8) . . ? N1D C14D C5D 121.5(8) . . ? N1D C14D C13D 117.3(7) . . ? C5D C14D C13D 121.3(8) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.371 _refine_diff_density_min -1.010 _refine_diff_density_rms 0.133