data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Leonard Lindoy' _publ_contact_author_address ; School of Chemistry F11 University of Sydney Centre for Heavy Metals Research Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_email LINDOY@CHEM.USYD.EDU.AU _publ_section_title ; New discrete and polymeric supramolecular architectures derived from dinuclear (bis-?-diketonato)copper(II) metallocycles ; loop_ _publ_author_name 'Leonard Lindoy' 'Jack K. Clegg' 'Karsten Gloe' 'Michael J. Hayter' 'Olga Kataeva' 'John C. McMurtrie' ; B.Moubaraki ; 'Keith S. Murray' 'David Schilter' data_lj61sad _database_code_depnum_ccdc_archive 'CCDC 606851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H106 Cu4 N6 O16, 3.5(C4 H8 O)' _chemical_formula_sum 'C102 H134 Cu4 N6 O19.50' _chemical_formula_weight 2010.31 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' 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 37.5224(17) _cell_length_b 15.0477(7) _cell_length_c 20.4243(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.6230(10) _cell_angle_gamma 90.00 _cell_volume 10217.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12412 _cell_measurement_theta_min 2.251 _cell_measurement_theta_max 27.6985 _exptl_crystal_description multi-faced _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4240 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 295 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.25 _diffrn_reflns_number 49929 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.04 _reflns_number_total 12121 _reflns_number_gt 8469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0826P)^2^+44.0226P] 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 12121 _refine_ls_number_parameters 609 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 C1 C 0.98035(14) 0.1846(4) 0.3128(3) 0.0627(15) Uani 1 1 d . . . H1A H 0.9681 0.2406 0.2881 0.094 Uiso 1 1 calc R . . H1B H 0.9761 0.1390 0.2757 0.094 Uiso 1 1 calc R . . H1C H 1.0093 0.1934 0.3442 0.094 Uiso 1 1 calc R . . C2 C 0.98054(14) 0.0693(3) 0.4006(3) 0.0572(13) Uani 1 1 d . . . H2A H 1.0092 0.0798 0.4332 0.086 Uiso 1 1 calc R . . H2B H 0.9775 0.0232 0.3645 0.086 Uiso 1 1 calc R . . H2C H 0.9675 0.0497 0.4300 0.086 Uiso 1 1 calc R . . C3 C 0.96747(12) 0.2266(3) 0.4175(2) 0.0458(11) Uani 1 1 d . . . H3A H 0.9545 0.2818 0.3923 0.069 Uiso 1 1 calc R . . H3B H 0.9964 0.2369 0.4478 0.069 Uiso 1 1 calc R . . H3C H 0.9558 0.2072 0.4492 0.069 Uiso 1 1 calc R . . C4 C 0.96095(11) 0.1549(3) 0.3603(2) 0.0343(8) Uani 1 1 d . . . C5 C 0.91640(10) 0.1346(2) 0.30856(18) 0.0288(7) Uani 1 1 d . . . C6 C 0.88580(11) 0.1731(3) 0.31957(19) 0.0328(8) Uani 1 1 d . . . H6 H 0.8934 0.2130 0.3599 0.039 Uiso 1 1 calc R . . C7 C 0.84477(10) 0.1571(2) 0.27563(18) 0.0261(7) Uani 1 1 d . . . C8 C 0.81409(10) 0.2073(2) 0.28834(18) 0.0258(7) Uani 1 1 d . . . C9 C 0.82381(11) 0.2792(3) 0.33701(19) 0.0324(8) Uani 1 1 d . . . H9 H 0.8511 0.2963 0.3654 0.039 Uiso 1 1 calc R . . C10 C 0.79411(12) 0.3254(3) 0.3442(2) 0.0371(9) Uani 1 1 d . . . H10 H 0.8012 0.3740 0.3776 0.044 Uiso 1 1 calc R . . C11 C 0.75390(11) 0.3018(2) 0.3032(2) 0.0319(8) Uani 1 1 d . . . H11 H 0.7337 0.3336 0.3091 0.038 Uiso 1 1 calc R . . C12 C 0.74333(10) 0.2310(2) 0.25319(17) 0.0243(7) Uani 1 1 d . . . C13 C 0.77381(10) 0.1844(2) 0.24697(17) 0.0240(6) Uani 1 1 d . . . H13 H 0.7668 0.1357 0.2136 0.029 Uiso 1 1 calc R . . C14 C 0.70052(10) 0.2059(2) 0.20311(17) 0.0239(6) Uani 1 1 d . B . C15 C 0.66916(10) 0.2533(2) 0.20547(19) 0.0275(7) Uani 1 1 d . . . H15 H 0.6762 0.2993 0.2412 0.033 Uiso 1 1 calc R . . C16 C 0.62850(11) 0.2385(2) 0.15976(19) 0.0308(8) Uani 1 1 d . A . C17 C 0.59639(12) 0.2953(3) 0.1659(2) 0.0488(11) Uani 1 1 d D . . C18 C 0.5617(3) 0.3108(8) 0.0942(5) 0.0520(11) Uiso 0.40 1 d PD A 1 H18A H 0.5502 0.2536 0.0710 0.078 Uiso 0.40 1 calc PR A 1 H18B H 0.5702 0.3440 0.0625 0.078 Uiso 0.40 1 calc PR A 1 H18C H 0.5415 0.3451 0.1008 0.078 Uiso 0.40 1 calc PR A 1 C19 C 0.6105(4) 0.3719(8) 0.2178(6) 0.0520(11) Uiso 0.40 1 d PD A 1 H19A H 0.6250 0.4139 0.2020 0.078 Uiso 0.40 1 calc PR A 1 H19B H 0.6286 0.3506 0.2677 0.078 Uiso 0.40 1 calc PR A 1 H19C H 0.5873 0.4017 0.2180 0.078 Uiso 0.40 1 calc PR A 1 C20 C 0.5762(4) 0.2247(7) 0.2035(7) 0.0520(11) Uiso 0.40 1 d PD A 1 H20A H 0.5529 0.2529 0.2046 0.078 Uiso 0.40 1 calc PR A 1 H20B H 0.5963 0.2099 0.2539 0.078 Uiso 0.40 1 calc PR A 1 H20C H 0.5675 0.1704 0.1737 0.078 Uiso 0.40 1 calc PR A 1 C18A C 0.5551(5) 0.2716(16) 0.1141(11) 0.0520(11) Uiso 0.20 1 d PD A 2 H18D H 0.5365 0.3088 0.1233 0.078 Uiso 0.20 1 calc PR A 2 H18E H 0.5505 0.2089 0.1206 0.078 Uiso 0.20 1 calc PR A 2 H18F H 0.5507 0.2812 0.0634 0.078 Uiso 0.20 1 calc PR A 2 C19A C 0.6052(7) 0.3926(11) 0.1453(12) 0.0520(11) Uiso 0.20 1 d PD A 2 H19D H 0.6072 0.3900 0.0992 0.078 Uiso 0.20 1 calc PR A 2 H19E H 0.6305 0.4148 0.1851 0.078 Uiso 0.20 1 calc PR A 2 H19F H 0.5832 0.4326 0.1390 0.078 Uiso 0.20 1 calc PR A 2 C20A C 0.6047(7) 0.3019(16) 0.2460(8) 0.0520(11) Uiso 0.20 1 d PD A 2 H20D H 0.5846 0.3404 0.2493 0.078 Uiso 0.20 1 calc PR A 2 H20E H 0.6316 0.3269 0.2758 0.078 Uiso 0.20 1 calc PR A 2 H20F H 0.6034 0.2425 0.2644 0.078 Uiso 0.20 1 calc PR A 2 C18B C 0.5788(4) 0.3561(8) 0.0931(6) 0.0520(11) Uiso 0.40 1 d PD A 3 H18G H 0.5707 0.3183 0.0494 0.078 Uiso 0.40 1 calc PR A 3 H18H H 0.5996 0.3979 0.0962 0.078 Uiso 0.40 1 calc PR A 3 H18I H 0.5554 0.3893 0.0892 0.078 Uiso 0.40 1 calc PR A 3 C19B C 0.6105(4) 0.3510(8) 0.2332(6) 0.0520(11) Uiso 0.40 1 d PD A 3 H19G H 0.5879 0.3858 0.2312 0.078 Uiso 0.40 1 calc PR A 3 H19H H 0.6316 0.3913 0.2359 0.078 Uiso 0.40 1 calc PR A 3 H19I H 0.6212 0.3128 0.2770 0.078 Uiso 0.40 1 calc PR A 3 C20B C 0.5610(3) 0.2398(8) 0.1548(7) 0.0520(11) Uiso 0.40 1 d PD A 3 H20G H 0.5401 0.2779 0.1560 0.078 Uiso 0.40 1 calc PR A 3 H20H H 0.5694 0.1953 0.1942 0.078 Uiso 0.40 1 calc PR A 3 H20I H 0.5503 0.2098 0.1068 0.078 Uiso 0.40 1 calc PR A 3 C21 C 0.52905(14) -0.0733(4) -0.0375(3) 0.0564(12) Uani 1 1 d . . . H21A H 0.5003 -0.0860 -0.0668 0.085 Uiso 1 1 calc R . . H21B H 0.5333 -0.0351 0.0044 0.085 Uiso 1 1 calc R . . H21C H 0.5438 -0.1292 -0.0190 0.085 Uiso 1 1 calc R . . C22 C 0.52251(15) 0.0632(4) -0.1131(3) 0.0712(17) Uani 1 1 d . . . H22A H 0.5326 0.0934 -0.1436 0.107 Uiso 1 1 calc R . . H22B H 0.5273 0.1005 -0.0704 0.107 Uiso 1 1 calc R . . H22C H 0.4936 0.0525 -0.1424 0.107 Uiso 1 1 calc R . . C23 C 0.53662(13) -0.0869(4) -0.1514(3) 0.0536(12) Uani 1 1 d . . . H23A H 0.5464 -0.0583 -0.1831 0.080 Uiso 1 1 calc R . . H23B H 0.5077 -0.0982 -0.1799 0.080 Uiso 1 1 calc R . . H23C H 0.5508 -0.1434 -0.1329 0.080 Uiso 1 1 calc R . . C24 C 0.54444(11) -0.0260(3) -0.0860(2) 0.0371(9) Uani 1 1 d . . . C25 C 0.58912(10) -0.0053(2) -0.03690(19) 0.0282(7) Uani 1 1 d . A . C26 C 0.61935(10) -0.0408(2) -0.05076(19) 0.0296(7) Uani 1 1 d . . . H26 H 0.6115 -0.0741 -0.0948 0.036 Uiso 1 1 calc R . . C27 C 0.66057(10) -0.0304(2) -0.00361(17) 0.0224(6) Uani 1 1 d . A . C28 C 0.69108(10) -0.0753(2) -0.02002(18) 0.0242(6) Uani 1 1 d . . . C29 C 0.68084(11) -0.1360(2) -0.07813(19) 0.0304(7) Uani 1 1 d . . . H29 H 0.6534 -0.1502 -0.1091 0.036 Uiso 1 1 calc R . . C30 C 0.71061(11) -0.1752(3) -0.0905(2) 0.0373(9) Uani 1 1 d . . . H30 H 0.7033 -0.2162 -0.1300 0.045 Uiso 1 1 calc R . . C31 C 0.75062(11) -0.1555(3) -0.0462(2) 0.0326(8) Uani 1 1 d . . . H31 H 0.7707 -0.1828 -0.0554 0.039 Uiso 1 1 calc R . . C32 C 0.76182(10) -0.0950(2) 0.01259(18) 0.0247(7) Uani 1 1 d . . . C33 C 0.73167(10) -0.0561(2) 0.02433(17) 0.0231(6) Uani 1 1 d . . . H33 H 0.7390 -0.0152 0.0639 0.028 Uiso 1 1 calc R . . C34 C 0.80466(10) -0.0683(2) 0.06158(18) 0.0254(7) Uani 1 1 d . . . C35 C 0.83584(11) -0.1062(2) 0.0518(2) 0.0303(7) Uani 1 1 d . . . H35 H 0.8293 -0.1536 0.0174 0.036 Uiso 1 1 calc R . . C36 C 0.87593(10) -0.0791(2) 0.08919(18) 0.0253(7) Uani 1 1 d . . . C37 C 0.90791(11) -0.1184(3) 0.0704(2) 0.0335(8) Uani 1 1 d . . . C38 C 0.89436(13) -0.2042(3) 0.0265(3) 0.0505(11) Uani 1 1 d . . . H38A H 0.8864 -0.2470 0.0534 0.076 Uiso 1 1 calc R . . H38B H 0.9165 -0.2288 0.0195 0.076 Uiso 1 1 calc R . . H38C H 0.8714 -0.1920 -0.0218 0.076 Uiso 1 1 calc R . . C39 C 0.9152(2) -0.0485(4) 0.0235(4) 0.0755(19) Uani 1 1 d . . . H39A H 0.9367 -0.0689 0.0124 0.113 Uiso 1 1 calc R . . H39B H 0.9233 0.0077 0.0508 0.113 Uiso 1 1 calc R . . H39C H 0.8905 -0.0394 -0.0228 0.113 Uiso 1 1 calc R . . C40 C 0.94635(15) -0.1340(5) 0.1411(3) 0.080(2) Uani 1 1 d . . . H40A H 0.9412 -0.1760 0.1724 0.120 Uiso 1 1 calc R . . H40B H 0.9559 -0.0776 0.1674 0.120 Uiso 1 1 calc R . . H40C H 0.9668 -0.1586 0.1291 0.120 Uiso 1 1 calc R . . C41A C 0.67605(12) 0.2062(3) -0.0235(2) 0.0395(9) Uani 0.80 1 d P B 1 H41A H 0.6989 0.1691 0.0016 0.047 Uiso 0.80 1 calc PR B 1 C41B C 0.67605(12) 0.2062(3) -0.0235(2) 0.0395(9) Uani 0.20 1 d P B 2 N4 N 0.7115(6) 0.1660(13) 0.0027(11) 0.048(4) Uiso 0.20 1 d P B 2 C42 C 0.61332(12) 0.2496(3) -0.0474(2) 0.0369(8) Uani 1 1 d . B . H42 H 0.5903 0.2432 -0.0398 0.044 Uiso 1 1 calc R . . C43 C 0.61333(11) 0.3132(3) -0.0945(2) 0.0364(8) Uani 1 1 d . B . H43 H 0.5903 0.3499 -0.1190 0.044 Uiso 1 1 calc R . . C44A C 0.67645(12) 0.2713(3) -0.0730(2) 0.0385(9) Uani 0.80 1 d P B 1 N3 N 0.70967(12) 0.2799(3) -0.0829(2) 0.0388(9) Uani 0.80 1 d P B 1 C44B C 0.67645(12) 0.2713(3) -0.0730(2) 0.0385(9) Uani 0.20 1 d P B 2 H44B H 0.6991 0.2762 -0.0818 0.046 Uiso 0.20 1 calc PR B 2 O1TA O 0.7457(2) 0.4870(4) 0.1763(3) 0.141(3) Uani 0.40 1 d PD C 1 C1TA C 0.7625(2) 0.4173(4) 0.1453(4) 0.098(2) Uani 0.40 1 d PD C 1 H1T1 H 0.7860 0.4428 0.1419 0.118 Uiso 0.40 1 calc PR C 1 H1T2 H 0.7724 0.3669 0.1803 0.118 Uiso 0.40 1 calc PR C 1 C2TA C 0.7379(3) 0.3878(8) 0.0823(6) 0.0488(15) Uiso 0.40 1 d PD C 1 H2T1 H 0.7434 0.3246 0.0768 0.059 Uiso 0.40 1 calc PR C 1 H2T2 H 0.7392 0.4228 0.0423 0.059 Uiso 0.40 1 calc PR C 1 C3TA C 0.7016(3) 0.3978(10) 0.0816(8) 0.0629(19) Uiso 0.40 1 d PD C 1 H3T1 H 0.6939 0.3405 0.0953 0.076 Uiso 0.40 1 calc PR C 1 H3T2 H 0.6810 0.4125 0.0308 0.076 Uiso 0.40 1 calc PR C 1 C4TA C 0.7013(2) 0.4743(5) 0.1374(4) 0.097(2) Uani 0.40 1 d PD C 1 H4T1 H 0.6867 0.5285 0.1111 0.116 Uiso 0.40 1 calc PR C 1 H4T2 H 0.6906 0.4527 0.1707 0.116 Uiso 0.40 1 calc PR C 1 O1TB O 0.7457(2) 0.4870(4) 0.1763(3) 0.141(3) Uani 0.60 1 d PD D 2 C1TB C 0.7625(2) 0.4173(4) 0.1453(4) 0.098(2) Uani 0.60 1 d PD D 2 H1T3 H 0.7852 0.3851 0.1852 0.118 Uiso 0.60 1 calc PR D 2 H1T4 H 0.7718 0.4440 0.1114 0.118 Uiso 0.60 1 calc PR D 2 C2TB C 0.7268(2) 0.3565(5) 0.1040(4) 0.0488(15) Uiso 0.60 1 d PD D 2 H2T3 H 0.7282 0.3302 0.0608 0.059 Uiso 0.60 1 calc PR D 2 H2T4 H 0.7273 0.3076 0.1368 0.059 Uiso 0.60 1 calc PR D 2 C3TB C 0.6897(3) 0.4083(7) 0.0795(6) 0.0629(19) Uiso 0.60 1 d PD D 2 H3T3 H 0.6818 0.4363 0.0309 0.076 Uiso 0.60 1 calc PR D 2 H3T4 H 0.6673 0.3709 0.0765 0.076 Uiso 0.60 1 calc PR D 2 C4TB C 0.7013(2) 0.4743(5) 0.1374(4) 0.097(2) Uani 0.60 1 d PD D 2 H4T3 H 0.6920 0.4552 0.1734 0.116 Uiso 0.60 1 calc PR D 2 H4T4 H 0.6880 0.5315 0.1157 0.116 Uiso 0.60 1 calc PR D 2 O2T O 0.5991(2) 0.0281(6) -0.3201(4) 0.0713(11) Uiso 0.50 1 d PD E 1 C5T C 0.5767(3) 0.0455(8) -0.2781(6) 0.0713(11) Uiso 0.50 1 d PD E 1 C6T C 0.6006(4) 0.1043(8) -0.2214(7) 0.0713(11) Uiso 0.50 1 d PD E 1 H6T1 H 0.5962 0.0958 -0.1777 0.086 Uiso 0.50 1 calc PR E 1 H6T2 H 0.5942 0.1666 -0.2383 0.086 Uiso 0.50 1 calc PR E 1 C7T C 0.6410(3) 0.0838(8) -0.2039(6) 0.0713(11) Uiso 0.50 1 d PD E 1 H7T1 H 0.6554 0.0594 -0.1532 0.086 Uiso 0.50 1 calc PR E 1 H7T2 H 0.6552 0.1381 -0.2066 0.086 Uiso 0.50 1 calc PR E 1 C8T C 0.6397(3) 0.0142(9) -0.2608(6) 0.0713(11) Uiso 0.50 1 d PD E 1 H8T1 H 0.6602 0.0266 -0.2772 0.086 Uiso 0.50 1 calc PR E 1 H8T2 H 0.6433 -0.0469 -0.2407 0.086 Uiso 0.50 1 calc PR E 1 O3T O 0.5854(5) -0.0105(10) -0.2462(9) 0.0713(11) Uiso 0.25 1 d PD F 2 C9T C 0.5961(8) 0.0739(12) -0.2153(14) 0.0713(11) Uiso 0.25 1 d PD F 2 H9T1 H 0.6148 0.0690 -0.1618 0.086 Uiso 0.25 1 calc PR F 2 H9T2 H 0.5718 0.1063 -0.2213 0.086 Uiso 0.25 1 calc PR F 2 C10T C 0.6147(8) 0.1207(14) -0.2508(13) 0.0713(11) Uiso 0.25 1 d PD F 2 H10A H 0.6391 0.1516 -0.2141 0.086 Uiso 0.25 1 calc PR F 2 H10B H 0.5961 0.1653 -0.2853 0.086 Uiso 0.25 1 calc PR F 2 C11T C 0.6259(8) 0.0501(13) -0.2934(14) 0.0713(11) Uiso 0.25 1 d PD F 2 H11A H 0.6156 0.0669 -0.3459 0.086 Uiso 0.25 1 calc PR F 2 H11B H 0.6554 0.0417 -0.2708 0.086 Uiso 0.25 1 calc PR F 2 C12T C 0.6058(7) -0.0310(13) -0.2858(13) 0.0713(11) Uiso 0.25 1 d PD F 2 H12A H 0.5867 -0.0537 -0.3353 0.086 Uiso 0.25 1 calc PR F 2 H12B H 0.6260 -0.0778 -0.2599 0.086 Uiso 0.25 1 calc PR F 2 N1 N 0.64489(10) 0.1955(2) -0.01131(18) 0.0380(7) Uani 1 1 d . . . N2 N 0.64500(10) 0.3261(2) -0.10762(18) 0.0353(7) Uani 1 1 d . . . O1 O 0.91076(7) 0.08107(18) 0.25686(14) 0.0323(6) Uani 1 1 d . . . O2 O 0.83003(7) 0.10260(17) 0.22192(14) 0.0318(6) Uani 1 1 d . . . O3 O 0.69596(7) 0.14102(16) 0.16003(13) 0.0300(5) Uani 1 1 d . . . O4 O 0.61465(8) 0.17881(19) 0.10964(15) 0.0398(7) Uani 1 1 d . . . O5 O 0.59530(7) 0.04523(18) 0.01690(15) 0.0366(6) Uani 1 1 d . . . O6 O 0.67545(7) 0.01554(15) 0.05545(12) 0.0256(5) Uani 1 1 d . . . O7 O 0.80927(7) -0.00991(18) 0.10965(14) 0.0343(6) Uani 1 1 d . . . O8 O 0.88932(7) -0.01880(17) 0.13840(14) 0.0302(5) Uani 1 1 d . . . Cu1 Cu 0.859342(12) 0.04575(3) 0.17741(2) 0.02828(13) Uani 1 1 d . . . Cu2 Cu 0.645698(12) 0.10088(3) 0.08124(2) 0.02805(13) Uani 1 1 d . A . 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 C1 0.042(3) 0.107(4) 0.047(3) -0.018(3) 0.028(2) -0.032(3) C2 0.034(2) 0.064(3) 0.055(3) -0.010(2) 0.005(2) 0.008(2) C3 0.0245(19) 0.069(3) 0.040(2) -0.021(2) 0.0120(17) -0.0108(19) C4 0.0227(17) 0.049(2) 0.0305(18) -0.0077(16) 0.0121(15) -0.0069(15) C5 0.0236(16) 0.0393(19) 0.0232(16) -0.0024(14) 0.0108(14) -0.0065(14) C6 0.0266(17) 0.045(2) 0.0254(17) -0.0114(15) 0.0111(14) -0.0084(15) C7 0.0270(16) 0.0310(17) 0.0221(15) -0.0029(13) 0.0130(13) -0.0033(13) C8 0.0270(17) 0.0313(17) 0.0202(15) -0.0046(13) 0.0121(13) -0.0054(13) C9 0.0297(18) 0.040(2) 0.0268(17) -0.0110(15) 0.0128(15) -0.0082(15) C10 0.036(2) 0.043(2) 0.0337(19) -0.0201(17) 0.0169(17) -0.0106(17) C11 0.0323(19) 0.0345(19) 0.0328(18) -0.0090(15) 0.0183(16) -0.0024(15) C12 0.0262(16) 0.0267(16) 0.0211(15) -0.0031(12) 0.0120(13) -0.0026(13) C13 0.0265(16) 0.0247(16) 0.0215(15) -0.0026(12) 0.0117(13) -0.0016(13) C14 0.0271(16) 0.0232(15) 0.0218(15) -0.0007(12) 0.0116(13) -0.0012(13) C15 0.0292(17) 0.0272(16) 0.0251(16) -0.0055(13) 0.0118(14) 0.0025(14) C16 0.0285(18) 0.0362(19) 0.0255(17) -0.0043(14) 0.0106(14) 0.0063(15) C17 0.034(2) 0.059(3) 0.044(2) -0.018(2) 0.0099(18) 0.0168(19) C21 0.039(2) 0.072(3) 0.062(3) -0.018(3) 0.026(2) -0.016(2) C22 0.039(3) 0.056(3) 0.085(4) 0.001(3) 0.000(3) 0.017(2) C23 0.028(2) 0.075(3) 0.043(2) -0.021(2) 0.0038(18) -0.006(2) C24 0.0238(18) 0.040(2) 0.038(2) -0.0082(16) 0.0061(15) 0.0025(15) C25 0.0247(17) 0.0270(17) 0.0275(17) -0.0016(14) 0.0076(14) 0.0005(13) C26 0.0269(17) 0.0329(18) 0.0243(16) -0.0069(14) 0.0079(14) -0.0005(14) C27 0.0252(16) 0.0219(15) 0.0201(15) 0.0021(12) 0.0104(13) 0.0022(12) C28 0.0259(16) 0.0241(15) 0.0217(15) 0.0009(12) 0.0103(13) 0.0007(13) C29 0.0258(17) 0.0349(18) 0.0284(17) -0.0104(15) 0.0108(14) -0.0036(14) C30 0.035(2) 0.043(2) 0.0330(19) -0.0195(17) 0.0150(16) -0.0027(16) C31 0.0298(18) 0.0371(19) 0.0335(19) -0.0123(15) 0.0170(15) -0.0013(15) C32 0.0258(16) 0.0265(16) 0.0223(15) -0.0024(12) 0.0115(13) 0.0001(13) C33 0.0259(16) 0.0239(16) 0.0199(15) -0.0008(12) 0.0109(13) 0.0000(12) C34 0.0276(17) 0.0262(16) 0.0243(16) -0.0014(13) 0.0135(14) -0.0020(13) C35 0.0307(18) 0.0317(18) 0.0331(18) -0.0080(14) 0.0188(15) -0.0027(14) C36 0.0273(17) 0.0252(16) 0.0274(17) 0.0002(13) 0.0159(14) 0.0004(13) C37 0.0285(18) 0.038(2) 0.041(2) -0.0082(16) 0.0219(16) -0.0022(15) C38 0.042(2) 0.046(2) 0.075(3) -0.022(2) 0.037(2) -0.0009(19) C39 0.109(5) 0.055(3) 0.118(5) -0.003(3) 0.099(5) -0.002(3) C40 0.038(3) 0.121(5) 0.066(3) -0.036(3) 0.011(2) 0.028(3) C41A 0.035(2) 0.036(2) 0.040(2) -0.0050(17) 0.0109(17) 0.0076(16) C41B 0.035(2) 0.036(2) 0.040(2) -0.0050(17) 0.0109(17) 0.0076(16) C42 0.034(2) 0.036(2) 0.040(2) 0.0049(16) 0.0169(17) 0.0066(16) C43 0.0304(19) 0.038(2) 0.039(2) 0.0006(16) 0.0145(16) 0.0045(16) C44A 0.034(2) 0.041(2) 0.039(2) -0.0129(17) 0.0156(17) 0.0009(16) N3 0.031(2) 0.046(2) 0.042(2) 0.0028(19) 0.0187(18) 0.0069(18) C44B 0.034(2) 0.041(2) 0.039(2) -0.0129(17) 0.0156(17) 0.0009(16) O1TA 0.244(8) 0.075(3) 0.125(5) -0.014(3) 0.103(6) -0.005(5) C1TA 0.153(7) 0.069(4) 0.079(5) 0.005(4) 0.060(5) 0.019(5) C4TA 0.113(6) 0.079(5) 0.069(4) -0.019(4) 0.017(4) -0.010(4) O1TB 0.244(8) 0.075(3) 0.125(5) -0.014(3) 0.103(6) -0.005(5) C1TB 0.153(7) 0.069(4) 0.079(5) 0.005(4) 0.060(5) 0.019(5) C4TB 0.113(6) 0.079(5) 0.069(4) -0.019(4) 0.017(4) -0.010(4) N1 0.0395(18) 0.0329(16) 0.0369(17) -0.0007(14) 0.0137(15) 0.0058(14) N2 0.0341(17) 0.0363(17) 0.0349(17) -0.0030(13) 0.0154(14) 0.0000(13) O1 0.0230(12) 0.0421(14) 0.0309(13) -0.0109(11) 0.0117(10) -0.0028(10) O2 0.0239(12) 0.0398(14) 0.0322(13) -0.0140(11) 0.0133(10) -0.0059(10) O3 0.0239(12) 0.0317(13) 0.0323(13) -0.0113(10) 0.0113(10) 0.0007(10) O4 0.0256(13) 0.0472(16) 0.0388(15) -0.0200(12) 0.0083(11) 0.0055(11) O5 0.0225(12) 0.0407(15) 0.0416(15) -0.0156(12) 0.0107(11) -0.0010(11) O6 0.0222(11) 0.0264(11) 0.0241(11) -0.0061(9) 0.0072(9) 0.0025(9) O7 0.0242(12) 0.0421(15) 0.0354(14) -0.0181(12) 0.0128(11) -0.0022(11) O8 0.0258(12) 0.0335(13) 0.0332(13) -0.0080(10) 0.0152(11) -0.0015(10) Cu1 0.0223(2) 0.0339(2) 0.0284(2) -0.00975(17) 0.01151(17) -0.00201(17) Cu2 0.0224(2) 0.0294(2) 0.0286(2) -0.00929(17) 0.00862(17) 0.00210(16) _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 C1 C4 1.524(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.522(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.524(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.539(5) . ? C5 O1 1.265(4) . ? C5 C6 1.394(5) . ? C6 C7 1.397(5) . ? C6 H6 0.9500 . ? C7 O2 1.273(4) . ? C7 C8 1.497(5) . ? C8 C13 1.391(5) . ? C8 C9 1.397(5) . ? C9 C10 1.378(5) . ? C9 H9 0.9500 . ? C10 C11 1.390(5) . ? C10 H10 0.9500 . ? C11 C12 1.401(5) . ? C11 H11 0.9500 . ? C12 C13 1.396(5) . ? C12 C14 1.498(4) . ? C13 H13 0.9500 . ? C14 O3 1.272(4) . ? C14 C15 1.396(5) . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 O4 1.277(4) . ? C16 C17 1.529(5) . ? C17 C18A 1.457(14) . ? C17 C18 1.457(10) . ? C17 C19B 1.483(11) . ? C17 C19 1.488(11) . ? C17 C20B 1.493(10) . ? C17 C20A 1.519(14) . ? C17 C19A 1.600(14) . ? C17 C18B 1.605(10) . ? C17 C20 1.683(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C18B H18G 0.9800 . ? C18B H18H 0.9800 . ? C18B H18I 0.9800 . ? C19B H19G 0.9800 . ? C19B H19H 0.9800 . ? C19B H19I 0.9800 . ? C20B H20G 0.9800 . ? C20B H20H 0.9800 . ? C20B H20I 0.9800 . ? C21 C24 1.535(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.536(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.532(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.535(5) . ? C25 O5 1.266(4) . ? C25 C26 1.397(5) . ? C26 C27 1.401(5) . ? C26 H26 0.9500 . ? C27 O6 1.273(4) . ? C27 C28 1.495(4) . ? C28 C33 1.394(5) . ? C28 C29 1.403(5) . ? C29 C30 1.386(5) . ? C29 H29 0.9500 . ? C30 C31 1.379(5) . ? C30 H30 0.9500 . ? C31 C32 1.407(5) . ? C31 H31 0.9500 . ? C32 C33 1.390(4) . ? C32 C34 1.501(5) . ? C33 H33 0.9500 . ? C34 O7 1.269(4) . ? C34 C35 1.397(5) . ? C35 C36 1.396(5) . ? C35 H35 0.9500 . ? C36 O8 1.271(4) . ? C36 C37 1.537(5) . ? C37 C40 1.512(6) . ? C37 C38 1.520(5) . ? C37 C39 1.532(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41A N1 1.313(5) . ? C41A C44A 1.412(6) . ? C41A H41A 0.9500 . ? C42 N1 1.342(5) . ? C42 C43 1.358(6) . ? C42 H42 0.9500 . ? C43 N2 1.348(5) . ? C43 H43 0.9500 . ? C44A N2 1.342(5) . ? C44A N3 1.358(6) . ? O1TA C4TA 1.489(8) . ? O1TA C1TA 1.507(7) . ? C1TA C2TA 1.266(11) . ? C1TA H1T1 0.9900 . ? C1TA H1T2 0.9900 . ? C2TA C3TA 1.368(13) . ? C2TA H2T1 0.9900 . ? C2TA H2T2 0.9900 . ? C3TA C4TA 1.624(12) . ? C3TA H3T1 0.9900 . ? C3TA H3T2 0.9900 . ? C4TA H4T1 0.9900 . ? C4TA H4T2 0.9900 . ? C2TB C3TB 1.466(11) . ? C2TB H2T3 0.9900 . ? C2TB H2T4 0.9900 . ? C3TB H3T3 0.9900 . ? C3TB H3T4 0.9900 . ? O2T C8T 1.456(11) . ? O2T C5T 1.475(11) . ? C5T C6T 1.402(13) . ? C6T C7T 1.418(13) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.548(13) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? O3T C12T 1.381(15) . ? O3T C9T 1.393(16) . ? C9T C10T 1.407(18) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? C10T C11T 1.549(18) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? C11T C12T 1.480(17) . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12A 0.9900 . ? C12T H12B 0.9900 . ? N1 Cu2 2.355(3) . ? N2 Cu1 2.358(3) 7_655 ? O1 Cu1 1.933(2) . ? O2 Cu1 1.922(2) . ? O3 Cu2 1.923(2) . ? O4 Cu2 1.922(2) . ? O5 Cu2 1.923(2) . ? O6 Cu2 1.928(2) . ? O7 Cu1 1.933(2) . ? O8 Cu1 1.917(2) . ? Cu1 N2 2.358(3) 7_655 ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C1 109.8(4) . . ? C2 C4 C3 108.6(3) . . ? C1 C4 C3 109.0(4) . . ? C2 C4 C5 107.5(3) . . ? C1 C4 C5 108.0(3) . . ? C3 C4 C5 113.8(3) . . ? O1 C5 C6 124.6(3) . . ? O1 C5 C4 114.1(3) . . ? C6 C5 C4 121.4(3) . . ? C5 C6 C7 124.7(3) . . ? C5 C6 H6 117.6 . . ? C7 C6 H6 117.6 . . ? O2 C7 C6 125.0(3) . . ? O2 C7 C8 114.4(3) . . ? C6 C7 C8 120.6(3) . . ? C13 C8 C9 118.4(3) . . ? C13 C8 C7 118.4(3) . . ? C9 C8 C7 123.1(3) . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.9(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 118.8(3) . . ? C13 C12 C14 118.4(3) . . ? C11 C12 C14 122.7(3) . . ? C8 C13 C12 121.7(3) . . ? C8 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? O3 C14 C15 124.8(3) . . ? O3 C14 C12 115.0(3) . . ? C15 C14 C12 120.1(3) . . ? C16 C15 C14 125.2(3) . . ? C16 C15 H15 117.4 . . ? C14 C15 H15 117.4 . . ? O4 C16 C15 124.3(3) . . ? O4 C16 C17 114.5(3) . . ? C15 C16 C17 121.1(3) . . ? C18A C17 C19B 127.8(11) . . ? C18 C17 C19B 127.5(8) . . ? C18A C17 C19 127.9(11) . . ? C18 C17 C19 116.7(7) . . ? C18 C17 C20B 67.7(6) . . ? C19B C17 C20B 111.5(7) . . ? C19 C17 C20B 122.7(8) . . ? C18A C17 C20A 114.7(11) . . ? C18 C17 C20A 135.6(11) . . ? C19 C17 C20A 49.8(9) . . ? C20B C17 C20A 85.7(10) . . ? C18A C17 C16 114.6(10) . . ? C18 C17 C16 112.1(6) . . ? C19B C17 C16 115.9(7) . . ? C19 C17 C16 117.2(6) . . ? C20B C17 C16 110.7(6) . . ? C20A C17 C16 110.4(10) . . ? C18A C17 C19A 108.1(11) . . ? C18 C17 C19A 77.6(9) . . ? C19B C17 C19A 72.4(9) . . ? C19 C17 C19A 55.2(9) . . ? C20B C17 C19A 138.5(10) . . ? C20A C17 C19A 105.0(10) . . ? C16 C17 C19A 102.9(9) . . ? C18A C17 C18B 67.9(10) . . ? C19B C17 C18B 110.7(7) . . ? C19 C17 C18B 94.4(7) . . ? C20B C17 C18B 102.9(6) . . ? C20A C17 C18B 138.7(10) . . ? C16 C17 C18B 104.1(5) . . ? C18A C17 C20 68.0(10) . . ? C18 C17 C20 100.3(6) . . ? C19B C17 C20 88.6(7) . . ? C19 C17 C20 104.5(7) . . ? C20A C17 C20 57.4(9) . . ? C16 C17 C20 103.0(5) . . ? C19A C17 C20 152.7(10) . . ? C18B C17 C20 134.7(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C18A H18D 109.5 . . ? C17 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C17 C19A H19D 109.5 . . ? C17 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C17 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C17 C20A H20D 109.5 . . ? C17 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C17 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C17 C18B H18G 109.5 . . ? C17 C18B H18H 109.5 . . ? C17 C18B H18I 109.5 . . ? C17 C19B H19G 109.5 . . ? C17 C19B H19H 109.5 . . ? C17 C19B H19I 109.5 . . ? C17 C20B H20G 109.5 . . ? C17 C20B H20H 109.5 . . ? C17 C20B H20I 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C24 C25 113.6(3) . . ? C23 C24 C21 107.9(4) . . ? C25 C24 C21 107.2(3) . . ? C23 C24 C22 110.8(4) . . ? C25 C24 C22 107.4(3) . . ? C21 C24 C22 109.8(4) . . ? O5 C25 C26 124.5(3) . . ? O5 C25 C24 113.2(3) . . ? C26 C25 C24 122.3(3) . . ? C25 C26 C27 124.0(3) . . ? C25 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? O6 C27 C26 124.9(3) . . ? O6 C27 C28 114.4(3) . . ? C26 C27 C28 120.8(3) . . ? C33 C28 C29 118.2(3) . . ? C33 C28 C27 118.7(3) . . ? C29 C28 C27 123.1(3) . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.9(3) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 118.3(3) . . ? C33 C32 C34 118.6(3) . . ? C31 C32 C34 123.1(3) . . ? C32 C33 C28 122.2(3) . . ? C32 C33 H33 118.9 . . ? C28 C33 H33 118.9 . . ? O7 C34 C35 124.8(3) . . ? O7 C34 C32 114.9(3) . . ? C35 C34 C32 120.3(3) . . ? C36 C35 C34 124.3(3) . . ? C36 C35 H35 117.8 . . ? C34 C35 H35 117.8 . . ? O8 C36 C35 124.9(3) . . ? O8 C36 C37 113.8(3) . . ? C35 C36 C37 121.3(3) . . ? C40 C37 C38 109.9(4) . . ? C40 C37 C39 109.6(5) . . ? C38 C37 C39 108.7(4) . . ? C40 C37 C36 109.4(3) . . ? C38 C37 C36 112.9(3) . . ? C39 C37 C36 106.2(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N1 C41A C44A 121.8(4) . . ? N1 C41A H41A 119.1 . . ? C44A C41A H41A 119.1 . . ? N1 C42 C43 121.8(4) . . ? N1 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? N2 C43 C42 122.1(4) . . ? N2 C43 H43 118.9 . . ? C42 C43 H43 118.9 . . ? N2 C44A N3 120.4(4) . . ? N2 C44A C41A 120.3(4) . . ? N3 C44A C41A 119.2(4) . . ? C4TA O1TA C1TA 105.7(5) . . ? C2TA C1TA O1TA 114.9(8) . . ? C2TA C1TA H1T1 108.5 . . ? O1TA C1TA H1T1 108.5 . . ? C2TA C1TA H1T2 108.5 . . ? O1TA C1TA H1T2 108.5 . . ? H1T1 C1TA H1T2 107.5 . . ? C1TA C2TA C3TA 103.0(9) . . ? C1TA C2TA H2T1 111.2 . . ? C3TA C2TA H2T1 111.2 . . ? C1TA C2TA H2T2 111.2 . . ? C3TA C2TA H2T2 111.2 . . ? H2T1 C2TA H2T2 109.1 . . ? C2TA C3TA C4TA 113.7(9) . . ? C2TA C3TA H3T1 108.8 . . ? C4TA C3TA H3T1 108.8 . . ? C2TA C3TA H3T2 108.8 . . ? C4TA C3TA H3T2 108.8 . . ? H3T1 C3TA H3T2 107.7 . . ? O1TA C4TA C3TA 95.4(6) . . ? O1TA C4TA H4T1 112.7 . . ? C3TA C4TA H4T1 112.7 . . ? O1TA C4TA H4T2 112.7 . . ? C3TA C4TA H4T2 112.7 . . ? H4T1 C4TA H4T2 110.1 . . ? C3TB C2TB H2T3 109.9 . . ? C3TB C2TB H2T4 109.9 . . ? H2T3 C2TB H2T4 108.3 . . ? C2TB C3TB H3T3 111.4 . . ? C2TB C3TB H3T4 111.4 . . ? H3T3 C3TB H3T4 109.2 . . ? C8T O2T C5T 101.5(7) . . ? C6T C5T O2T 105.8(9) . . ? C5T C6T C7T 105.8(10) . . ? C5T C6T H6T1 110.6 . . ? C7T C6T H6T1 110.6 . . ? C5T C6T H6T2 110.6 . . ? C7T C6T H6T2 110.6 . . ? H6T1 C6T H6T2 108.7 . . ? C6T C7T C8T 107.3(9) . . ? C6T C7T H7T1 110.2 . . ? C8T C7T H7T1 110.2 . . ? C6T C7T H7T2 110.2 . . ? C8T C7T H7T2 110.2 . . ? H7T1 C7T H7T2 108.5 . . ? O2T C8T C7T 100.6(8) . . ? O2T C8T H8T1 111.6 . . ? C7T C8T H8T1 111.6 . . ? O2T C8T H8T2 111.6 . . ? C7T C8T H8T2 111.6 . . ? H8T1 C8T H8T2 109.4 . . ? C12T O3T C9T 110.4(13) . . ? O3T C9T C10T 109.3(16) . . ? O3T C9T H9T1 109.8 . . ? C10T C9T H9T1 109.8 . . ? O3T C9T H9T2 109.8 . . ? C10T C9T H9T2 109.8 . . ? H9T1 C9T H9T2 108.3 . . ? C9T C10T C11T 106.0(16) . . ? C9T C10T H10A 110.5 . . ? C11T C10T H10A 110.5 . . ? C9T C10T H10B 110.5 . . ? C11T C10T H10B 110.5 . . ? H10A C10T H10B 108.7 . . ? C12T C11T C10T 102.9(14) . . ? C12T C11T H11A 111.2 . . ? C10T C11T H11A 111.2 . . ? C12T C11T H11B 111.2 . . ? C10T C11T H11B 111.2 . . ? H11A C11T H11B 109.1 . . ? O3T C12T C11T 109.0(13) . . ? O3T C12T H12A 109.9 . . ? C11T C12T H12A 109.9 . . ? O3T C12T H12B 109.9 . . ? C11T C12T H12B 109.9 . . ? H12A C12T H12B 108.3 . . ? C41A N1 C42 117.3(4) . . ? C41A N1 Cu2 123.0(3) . . ? C42 N1 Cu2 119.2(3) . . ? C44A N2 C43 116.6(3) . . ? C44A N2 Cu1 128.2(3) . 7_655 ? C43 N2 Cu1 114.7(3) . 7_655 ? C5 O1 Cu1 126.3(2) . . ? C7 O2 Cu1 125.4(2) . . ? C14 O3 Cu2 125.8(2) . . ? C16 O4 Cu2 126.3(2) . . ? C25 O5 Cu2 125.5(2) . . ? C27 O6 Cu2 124.4(2) . . ? C34 O7 Cu1 126.4(2) . . ? C36 O8 Cu1 126.7(2) . . ? O8 Cu1 O2 175.37(11) . . ? O8 Cu1 O1 86.48(10) . . ? O2 Cu1 O1 92.74(10) . . ? O8 Cu1 O7 92.63(10) . . ? O2 Cu1 O7 87.25(10) . . ? O1 Cu1 O7 168.80(12) . . ? O8 Cu1 N2 93.02(11) . 7_655 ? O2 Cu1 N2 91.58(11) . 7_655 ? O1 Cu1 N2 92.58(11) . 7_655 ? O7 Cu1 N2 98.62(12) . 7_655 ? O4 Cu2 O3 92.99(10) . . ? O4 Cu2 O5 86.01(11) . . ? O3 Cu2 O5 168.72(12) . . ? O4 Cu2 O6 175.78(12) . . ? O3 Cu2 O6 88.31(10) . . ? O5 Cu2 O6 91.93(10) . . ? O4 Cu2 N1 95.14(12) . . ? O3 Cu2 N1 97.15(11) . . ? O5 Cu2 N1 94.13(12) . . ? O6 Cu2 N1 88.67(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C4 C5 O1 -65.7(4) . . . . ? C1 C4 C5 O1 52.8(5) . . . . ? C3 C4 C5 O1 174.0(3) . . . . ? C2 C4 C5 C6 114.3(4) . . . . ? C1 C4 C5 C6 -127.2(4) . . . . ? C3 C4 C5 C6 -6.1(5) . . . . ? O1 C5 C6 C7 0.8(6) . . . . ? C4 C5 C6 C7 -179.2(4) . . . . ? C5 C6 C7 O2 3.2(6) . . . . ? C5 C6 C7 C8 -175.0(3) . . . . ? O2 C7 C8 C13 6.4(5) . . . . ? C6 C7 C8 C13 -175.2(3) . . . . ? O2 C7 C8 C9 -170.2(3) . . . . ? C6 C7 C8 C9 8.3(5) . . . . ? C13 C8 C9 C10 0.7(5) . . . . ? C7 C8 C9 C10 177.2(3) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? C9 C10 C11 C12 -0.9(6) . . . . ? C10 C11 C12 C13 1.4(5) . . . . ? C10 C11 C12 C14 -175.4(3) . . . . ? C9 C8 C13 C12 -0.1(5) . . . . ? C7 C8 C13 C12 -176.9(3) . . . . ? C11 C12 C13 C8 -0.9(5) . . . . ? C14 C12 C13 C8 176.0(3) . . . . ? C13 C12 C14 O3 2.1(4) . . . . ? C11 C12 C14 O3 178.8(3) . . . . ? C13 C12 C14 C15 -177.3(3) . . . . ? C11 C12 C14 C15 -0.6(5) . . . . ? O3 C14 C15 C16 -2.1(6) . . . . ? C12 C14 C15 C16 177.2(3) . . . . ? C14 C15 C16 O4 0.4(6) . . . . ? C14 C15 C16 C17 -179.0(4) . . . . ? O4 C16 C17 C18A 0.5(11) . . . . ? C15 C16 C17 C18A 179.9(11) . . . . ? O4 C16 C17 C18 -34.9(7) . . . . ? C15 C16 C17 C18 144.5(6) . . . . ? O4 C16 C17 C19B 166.9(6) . . . . ? C15 C16 C17 C19B -13.7(8) . . . . ? O4 C16 C17 C19 -173.9(6) . . . . ? C15 C16 C17 C19 5.5(8) . . . . ? O4 C16 C17 C20B 38.6(7) . . . . ? C15 C16 C17 C20B -142.0(6) . . . . ? O4 C16 C17 C20A 131.8(10) . . . . ? C15 C16 C17 C20A -48.8(10) . . . . ? O4 C16 C17 C19A -116.6(9) . . . . ? C15 C16 C17 C19A 62.8(9) . . . . ? O4 C16 C17 C18B -71.3(6) . . . . ? C15 C16 C17 C18B 108.0(6) . . . . ? O4 C16 C17 C20 72.0(6) . . . . ? C15 C16 C17 C20 -108.6(6) . . . . ? C23 C24 C25 O5 179.9(4) . . . . ? C21 C24 C25 O5 -61.0(4) . . . . ? C22 C24 C25 O5 57.0(5) . . . . ? C23 C24 C25 C26 -1.1(6) . . . . ? C21 C24 C25 C26 118.0(4) . . . . ? C22 C24 C25 C26 -124.1(4) . . . . ? O5 C25 C26 C27 5.1(6) . . . . ? C24 C25 C26 C27 -173.8(3) . . . . ? C25 C26 C27 O6 -3.2(6) . . . . ? C25 C26 C27 C28 176.2(3) . . . . ? O6 C27 C28 C33 -6.7(4) . . . . ? C26 C27 C28 C33 173.8(3) . . . . ? O6 C27 C28 C29 173.3(3) . . . . ? C26 C27 C28 C29 -6.2(5) . . . . ? C33 C28 C29 C30 -0.1(5) . . . . ? C27 C28 C29 C30 179.9(3) . . . . ? C28 C29 C30 C31 0.0(6) . . . . ? C29 C30 C31 C32 0.1(6) . . . . ? C30 C31 C32 C33 -0.2(6) . . . . ? C30 C31 C32 C34 -178.1(4) . . . . ? C31 C32 C33 C28 0.0(5) . . . . ? C34 C32 C33 C28 178.1(3) . . . . ? C29 C28 C33 C32 0.1(5) . . . . ? C27 C28 C33 C32 -179.9(3) . . . . ? C33 C32 C34 O7 -1.2(5) . . . . ? C31 C32 C34 O7 176.8(3) . . . . ? C33 C32 C34 C35 179.7(3) . . . . ? C31 C32 C34 C35 -2.4(5) . . . . ? O7 C34 C35 C36 -6.1(6) . . . . ? C32 C34 C35 C36 172.9(3) . . . . ? C34 C35 C36 O8 2.5(6) . . . . ? C34 C35 C36 C37 -174.5(3) . . . . ? O8 C36 C37 C40 43.2(5) . . . . ? C35 C36 C37 C40 -139.5(4) . . . . ? O8 C36 C37 C38 165.9(3) . . . . ? C35 C36 C37 C38 -16.8(5) . . . . ? O8 C36 C37 C39 -75.0(4) . . . . ? C35 C36 C37 C39 102.3(4) . . . . ? N1 C42 C43 N2 -0.2(6) . . . . ? N1 C41A C44A N2 1.8(6) . . . . ? N1 C41A C44A N3 179.3(4) . . . . ? C4TA O1TA C1TA C2TA 22.2(10) . . . . ? O1TA C1TA C2TA C3TA -28.3(14) . . . . ? C1TA C2TA C3TA C4TA 24.2(16) . . . . ? C1TA O1TA C4TA C3TA -5.0(9) . . . . ? C2TA C3TA C4TA O1TA -10.9(14) . . . . ? C8T O2T C5T C6T 44.4(12) . . . . ? O2T C5T C6T C7T -30.9(14) . . . . ? C5T C6T C7T C8T 6.2(15) . . . . ? C5T O2T C8T C7T -37.5(11) . . . . ? C6T C7T C8T O2T 20.5(13) . . . . ? C12T O3T C9T C10T 17(3) . . . . ? O3T C9T C10T C11T -15(3) . . . . ? C9T C10T C11T C12T 9(3) . . . . ? C9T O3T C12T C11T -11(3) . . . . ? C10T C11T C12T O3T 1(3) . . . . ? C44A C41A N1 C42 -0.5(6) . . . . ? C44A C41A N1 Cu2 -172.0(3) . . . . ? C43 C42 N1 C41A -0.3(6) . . . . ? C43 C42 N1 Cu2 171.6(3) . . . . ? N3 C44A N2 C43 -179.7(4) . . . . ? C41A C44A N2 C43 -2.3(5) . . . . ? N3 C44A N2 Cu1 -8.1(5) . . . 7_655 ? C41A C44A N2 Cu1 169.4(3) . . . 7_655 ? C42 C43 N2 C44A 1.5(6) . . . . ? C42 C43 N2 Cu1 -171.2(3) . . . 7_655 ? C6 C5 O1 Cu1 4.5(5) . . . . ? C4 C5 O1 Cu1 -175.5(2) . . . . ? C6 C7 O2 Cu1 -11.8(5) . . . . ? C8 C7 O2 Cu1 166.6(2) . . . . ? C15 C14 O3 Cu2 7.2(5) . . . . ? C12 C14 O3 Cu2 -172.2(2) . . . . ? C15 C16 O4 Cu2 -4.0(6) . . . . ? C17 C16 O4 Cu2 175.4(3) . . . . ? C26 C25 O5 Cu2 11.3(5) . . . . ? C24 C25 O5 Cu2 -169.7(2) . . . . ? C26 C27 O6 Cu2 -14.5(5) . . . . ? C28 C27 O6 Cu2 166.1(2) . . . . ? C35 C34 O7 Cu1 3.4(5) . . . . ? C32 C34 O7 Cu1 -175.6(2) . . . . ? C35 C36 O8 Cu1 3.3(5) . . . . ? C37 C36 O8 Cu1 -179.6(2) . . . . ? C36 O8 Cu1 O1 164.4(3) . . . . ? C36 O8 Cu1 O7 -4.4(3) . . . . ? C36 O8 Cu1 N2 -103.2(3) . . . 7_655 ? C7 O2 Cu1 O1 12.6(3) . . . . ? C7 O2 Cu1 O7 -178.6(3) . . . . ? C7 O2 Cu1 N2 -80.0(3) . . . 7_655 ? C5 O1 Cu1 O8 175.4(3) . . . . ? C5 O1 Cu1 O2 -9.2(3) . . . . ? C5 O1 Cu1 O7 -98.8(6) . . . . ? C5 O1 Cu1 N2 82.5(3) . . . 7_655 ? C34 O7 Cu1 O8 1.1(3) . . . . ? C34 O7 Cu1 O2 -174.2(3) . . . . ? C34 O7 Cu1 O1 -84.0(6) . . . . ? C34 O7 Cu1 N2 94.6(3) . . . 7_655 ? C16 O4 Cu2 O3 6.5(3) . . . . ? C16 O4 Cu2 O5 175.2(3) . . . . ? C16 O4 Cu2 N1 -91.0(3) . . . . ? C14 O3 Cu2 O4 -8.0(3) . . . . ? C14 O3 Cu2 O5 -92.6(6) . . . . ? C14 O3 Cu2 O6 176.0(3) . . . . ? C14 O3 Cu2 N1 87.6(3) . . . . ? C25 O5 Cu2 O4 162.8(3) . . . . ? C25 O5 Cu2 O3 -111.9(5) . . . . ? C25 O5 Cu2 O6 -20.8(3) . . . . ? C25 O5 Cu2 N1 68.0(3) . . . . ? C27 O6 Cu2 O3 -169.1(3) . . . . ? C27 O6 Cu2 O5 22.2(3) . . . . ? C27 O6 Cu2 N1 -71.9(3) . . . . ? C41A N1 Cu2 O4 141.2(3) . . . . ? C42 N1 Cu2 O4 -30.1(3) . . . . ? C41A N1 Cu2 O3 47.6(3) . . . . ? C42 N1 Cu2 O3 -123.8(3) . . . . ? C41A N1 Cu2 O5 -132.4(3) . . . . ? C42 N1 Cu2 O5 56.2(3) . . . . ? C41A N1 Cu2 O6 -40.6(3) . . . . ? C42 N1 Cu2 O6 148.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.525 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.097 # Attachment 'Cu dabco.CIF' data_lj42sad _database_code_depnum_ccdc_archive 'CCDC 606852' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H120 Cu4 N4 O16, 3.2(C4 H8 O), 0.8(H2 O)' _chemical_formula_sum 'C104.80 H147.20 Cu4 N4 O20' _chemical_formula_weight 2037.23 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' 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 C2/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 37.3901(19) _cell_length_b 15.7180(8) _cell_length_c 20.6842(11) _cell_angle_alpha 90.00 _cell_angle_beta 118.9230(10) _cell_angle_gamma 90.00 _cell_volume 10639.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18801 _cell_measurement_theta_min 2.403 _cell_measurement_theta_max 28.256 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.669 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 378 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.21 _diffrn_reflns_number 51049 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.33 _reflns_number_total 12554 _reflns_number_gt 9650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1995)' _computing_cell_refinement 'SAINT (Bruker, 1995)' _computing_data_reduction 'SAINT and XPREP (Bruker, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEPIII (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0976P)^2^+50.2320P] 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 12554 _refine_ls_number_parameters 579 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1900 _refine_ls_wR_factor_gt 0.1685 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.046 _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 0.364464(12) 0.04932(3) 0.68622(2) 0.02582(12) Uani 1 1 d . B . Cu2 Cu 0.147557(12) 0.12570(3) 0.57346(2) 0.02687(12) Uani 1 1 d . . . O1 O 0.41680(7) 0.08539(16) 0.76628(13) 0.0287(5) Uani 1 1 d . . . O2 O 0.33511(7) 0.11208(17) 0.72596(14) 0.0327(5) Uani 1 1 d . . . O3 O 0.19909(7) 0.16080(16) 0.65533(13) 0.0287(5) Uani 1 1 d . . . O4 O 0.11720(8) 0.19648(18) 0.60690(14) 0.0374(6) Uani 1 1 d . A . O5 O 0.39501(7) -0.02518(15) 0.65632(13) 0.0280(5) Uani 1 1 d . . . O6 O 0.31382(7) -0.00772(17) 0.62176(14) 0.0340(6) Uani 1 1 d . B . O7 O 0.17753(7) 0.04378(15) 0.54878(13) 0.0284(5) Uani 1 1 d . . . O8 O 0.09604(7) 0.07206(17) 0.50794(15) 0.0353(6) Uani 1 1 d . . . C1 C 0.47491(12) 0.2302(3) 0.9236(2) 0.0459(10) Uani 1 1 d . . . H1A H 0.4634 0.2161 0.9558 0.069 Uiso 1 1 calc R . . H1B H 0.4615 0.2813 0.8948 0.069 Uiso 1 1 calc R . . H1C H 0.5043 0.2409 0.9537 0.069 Uiso 1 1 calc R . . C2 C 0.48559(14) 0.0743(3) 0.9154(3) 0.0554(12) Uani 1 1 d . . . H2A H 0.4714 0.0615 0.9436 0.083 Uiso 1 1 calc R . . H2B H 0.5148 0.0821 0.9495 0.083 Uiso 1 1 calc R . . H2C H 0.4818 0.0271 0.8817 0.083 Uiso 1 1 calc R . . C3 C 0.48984(14) 0.1755(4) 0.8262(3) 0.0646(16) Uani 1 1 d . . . H3A H 0.5191 0.1829 0.8598 0.097 Uiso 1 1 calc R . . H3B H 0.4786 0.2279 0.7978 0.097 Uiso 1 1 calc R . . H3C H 0.4857 0.1284 0.7922 0.097 Uiso 1 1 calc R . . C4 C 0.46806(11) 0.1557(3) 0.87088(19) 0.0338(8) Uani 1 1 d . . . C5 C 0.42290(10) 0.1382(2) 0.81683(17) 0.0263(7) Uani 1 1 d . . . C6 C 0.39206(10) 0.1781(2) 0.82534(18) 0.0301(7) Uani 1 1 d . . . H6 H 0.4000 0.2185 0.8640 0.036 Uiso 1 1 calc R . . C7 C 0.35027(10) 0.1626(2) 0.78084(17) 0.0250(6) Uani 1 1 d . . . C8 C 0.31980(10) 0.2064(2) 0.79691(17) 0.0261(6) Uani 1 1 d . . . C9 C 0.33120(11) 0.2561(2) 0.85977(19) 0.0332(8) Uani 1 1 d . . . H9 H 0.3593 0.2658 0.8934 0.040 Uiso 1 1 calc R . . C10 C 0.30122(12) 0.2914(3) 0.8729(2) 0.0372(8) Uani 1 1 d . . . H10 H 0.3091 0.3249 0.9160 0.045 Uiso 1 1 calc R . . C11 C 0.26032(11) 0.2788(2) 0.82490(18) 0.0308(7) Uani 1 1 d . . . H11 H 0.2403 0.3032 0.8351 0.037 Uiso 1 1 calc R . . C12 C 0.24822(10) 0.2303(2) 0.76115(17) 0.0254(6) Uani 1 1 d . . . C13 C 0.27827(10) 0.1946(2) 0.74766(17) 0.0250(6) Uani 1 1 d . . . H13 H 0.2703 0.1617 0.7043 0.030 Uiso 1 1 calc R . . C14 C 0.20445(10) 0.2132(2) 0.70605(17) 0.0246(6) Uani 1 1 d . . . C15 C 0.17305(11) 0.2548(2) 0.71191(19) 0.0313(7) Uani 1 1 d . A . H15 H 0.1805 0.2921 0.7525 0.038 Uiso 1 1 calc R . . C16 C 0.13159(10) 0.2451(2) 0.66215(19) 0.0336(8) Uani 1 1 d D . . C17A C 0.10045(17) 0.2920(4) 0.6790(3) 0.0392(12) Uiso 0.65 1 d PD A 1 C18A C 0.1053(2) 0.2706(5) 0.7529(3) 0.0641(18) Uiso 0.65 1 d PD A 1 H18A H 0.0840 0.2995 0.7594 0.096 Uiso 0.65 1 calc PR A 1 H18B H 0.1322 0.2892 0.7914 0.096 Uiso 0.65 1 calc PR A 1 H18C H 0.1027 0.2089 0.7565 0.096 Uiso 0.65 1 calc PR A 1 C19A C 0.05749(17) 0.2777(5) 0.6166(4) 0.0544(16) Uiso 0.65 1 d PD A 1 H19A H 0.0500 0.2178 0.6159 0.082 Uiso 0.65 1 calc PR A 1 H19B H 0.0563 0.2922 0.5695 0.082 Uiso 0.65 1 calc PR A 1 H19C H 0.0384 0.3138 0.6240 0.082 Uiso 0.65 1 calc PR A 1 C20A C 0.1090(3) 0.3897(4) 0.6778(5) 0.074(2) Uiso 0.65 1 d PD A 1 H20A H 0.0872 0.4224 0.6798 0.112 Uiso 0.65 1 calc PR A 1 H20B H 0.1097 0.4037 0.6323 0.112 Uiso 0.65 1 calc PR A 1 H20C H 0.1353 0.4040 0.7206 0.112 Uiso 0.65 1 calc PR A 1 C17B C 0.0994(3) 0.3070(5) 0.6599(5) 0.0392(12) Uiso 0.35 1 d PD A 2 C18B C 0.1143(4) 0.3543(8) 0.7311(6) 0.0641(18) Uiso 0.35 1 d PD A 2 H18D H 0.1185 0.3142 0.7705 0.096 Uiso 0.35 1 calc PR A 2 H18E H 0.0939 0.3967 0.7259 0.096 Uiso 0.35 1 calc PR A 2 H18F H 0.1401 0.3828 0.7434 0.096 Uiso 0.35 1 calc PR A 2 C19B C 0.0610(3) 0.2519(7) 0.6440(7) 0.0544(16) Uiso 0.35 1 d PD A 2 H19D H 0.0688 0.2080 0.6821 0.082 Uiso 0.35 1 calc PR A 2 H19E H 0.0503 0.2248 0.5955 0.082 Uiso 0.35 1 calc PR A 2 H19F H 0.0399 0.2885 0.6444 0.082 Uiso 0.35 1 calc PR A 2 C20B C 0.0860(4) 0.3691(7) 0.5956(7) 0.074(2) Uiso 0.35 1 d PD A 2 H20D H 0.0624 0.4017 0.5900 0.112 Uiso 0.35 1 calc PR A 2 H20E H 0.0786 0.3373 0.5500 0.112 Uiso 0.35 1 calc PR A 2 H20F H 0.1085 0.4081 0.6053 0.112 Uiso 0.35 1 calc PR A 2 C21 C 0.45488(14) -0.1083(4) 0.6500(3) 0.0712(17) Uani 1 1 d . . . H21A H 0.4581 -0.1359 0.6950 0.107 Uiso 1 1 calc R . . H21B H 0.4599 -0.0471 0.6588 0.107 Uiso 1 1 calc R . . H21C H 0.4745 -0.1325 0.6366 0.107 Uiso 1 1 calc R . . C22 C 0.4071(2) -0.0798(5) 0.5160(4) 0.0824(19) Uani 1 1 d . . . H22A H 0.4261 -0.1058 0.5020 0.124 Uiso 1 1 calc R . . H22B H 0.4128 -0.0188 0.5246 0.124 Uiso 1 1 calc R . . H22C H 0.3790 -0.0879 0.4762 0.124 Uiso 1 1 calc R . . C23 C 0.40344(16) -0.2149(3) 0.5694(4) 0.0694(17) Uani 1 1 d . . . H23A H 0.4248 -0.2394 0.5607 0.104 Uiso 1 1 calc R . . H23B H 0.3769 -0.2210 0.5248 0.104 Uiso 1 1 calc R . . H23C H 0.4029 -0.2448 0.6105 0.104 Uiso 1 1 calc R . . C24 C 0.41215(12) -0.1226(3) 0.5881(2) 0.0369(8) Uani 1 1 d . . . C25 C 0.38081(10) -0.0801(2) 0.60559(18) 0.0252(6) Uani 1 1 d . . . C26 C 0.33943(10) -0.1008(2) 0.56398(19) 0.0300(7) Uani 1 1 d . B . H26 H 0.3320 -0.1435 0.5271 0.036 Uiso 1 1 calc R . . C27 C 0.30838(10) -0.0633(2) 0.57279(19) 0.0279(7) Uani 1 1 d . . . C28A C 0.2640(3) -0.0801(5) 0.5165(5) 0.0239(9) Uiso 0.50 1 d PD B 1 C29A C 0.25188(19) -0.1314(4) 0.4546(4) 0.0273(10) Uiso 0.50 1 d PD B 1 H29A H 0.2718 -0.1571 0.4450 0.033 Uiso 0.50 1 calc PR B 1 C30A C 0.21077(19) -0.1451(5) 0.4069(4) 0.0325(11) Uiso 0.50 1 d PD B 1 H30A H 0.2028 -0.1810 0.3652 0.039 Uiso 0.50 1 calc PR B 1 C31A C 0.1812(2) -0.1072(4) 0.4191(4) 0.0260(10) Uiso 0.50 1 d PD B 1 H31A H 0.1530 -0.1149 0.3850 0.031 Uiso 0.50 1 calc PR B 1 C32A C 0.1931(5) -0.0579(10) 0.4819(8) 0.0238(9) Uiso 0.50 1 d PD B 1 C33A C 0.23433(10) -0.0441(2) 0.53142(18) 0.0238(6) Uani 0.50 1 d PD B 1 H33A H 0.2423 -0.0110 0.5746 0.029 Uiso 0.50 1 calc PR B 1 C28B C 0.2650(3) -0.0912(5) 0.5284(5) 0.0239(9) Uiso 0.50 1 d PD B 2 C29B C 0.25254(19) -0.1568(4) 0.4746(4) 0.0273(10) Uiso 0.50 1 d PD B 2 H29B H 0.2725 -0.1895 0.4699 0.033 Uiso 0.50 1 calc PR B 2 C30B C 0.21147(19) -0.1735(5) 0.4290(4) 0.0325(11) Uiso 0.50 1 d PD B 2 H30B H 0.2035 -0.2169 0.3926 0.039 Uiso 0.50 1 calc PR B 2 C31B C 0.1818(2) -0.1279(4) 0.4357(4) 0.0260(10) Uiso 0.50 1 d PD B 2 H31B H 0.1538 -0.1411 0.4047 0.031 Uiso 0.50 1 calc PR B 2 C32B C 0.1929(5) -0.0619(10) 0.4883(8) 0.0238(9) Uiso 0.50 1 d PD B 2 C33B C 0.23433(10) -0.0441(2) 0.53142(18) 0.0238(6) Uani 0.50 1 d PD B 2 H33B H 0.2421 0.0025 0.5647 0.029 Uiso 0.50 1 calc PR B 2 C34 C 0.16228(10) -0.0117(2) 0.49791(17) 0.0235(6) Uani 1 1 d . . . C35 C 0.12050(11) -0.0301(2) 0.4556(2) 0.0317(7) Uani 1 1 d . B . H35 H 0.1127 -0.0742 0.4199 0.038 Uiso 1 1 calc R . . C36 C 0.08980(9) 0.0120(2) 0.46219(18) 0.0313(7) Uani 1 1 d D . . C37A C 0.04501(19) -0.0179(4) 0.4205(4) 0.0360(11) Uiso 0.55 1 d PD B 1 C38A C 0.0353(2) -0.0768(5) 0.4674(4) 0.0528(16) Uiso 0.55 1 d PD B 1 H38A H 0.0066 -0.0943 0.4397 0.079 Uiso 0.55 1 calc PR B 1 H38B H 0.0401 -0.0472 0.5126 0.079 Uiso 0.55 1 calc PR B 1 H38C H 0.0529 -0.1271 0.4803 0.079 Uiso 0.55 1 calc PR B 1 C39A C 0.0174(2) 0.0615(5) 0.4012(5) 0.0585(18) Uiso 0.55 1 d PD B 1 H39A H -0.0111 0.0452 0.3681 0.088 Uiso 0.55 1 calc PR B 1 H39B H 0.0260 0.1037 0.3767 0.088 Uiso 0.55 1 calc PR B 1 H39C H 0.0196 0.0860 0.4466 0.088 Uiso 0.55 1 calc PR B 1 C40A C 0.0356(3) -0.0603(5) 0.3469(4) 0.0444(13) Uiso 0.55 1 d PD B 1 H40A H 0.0483 -0.1167 0.3566 0.067 Uiso 0.55 1 calc PR B 1 H40B H 0.0465 -0.0252 0.3214 0.067 Uiso 0.55 1 calc PR B 1 H40C H 0.0059 -0.0661 0.3159 0.067 Uiso 0.55 1 calc PR B 1 C37B C 0.0447(2) -0.0065(5) 0.4081(4) 0.0360(11) Uiso 0.45 1 d PD B 2 C38B C 0.0260(3) -0.0349(6) 0.4577(5) 0.0528(16) Uiso 0.45 1 d PD B 2 H38D H 0.0272 0.0126 0.4895 0.079 Uiso 0.45 1 calc PR B 2 H38E H 0.0415 -0.0831 0.4885 0.079 Uiso 0.45 1 calc PR B 2 H38F H -0.0026 -0.0518 0.4263 0.079 Uiso 0.45 1 calc PR B 2 C39B C 0.0227(3) 0.0726(5) 0.3664(5) 0.0585(18) Uiso 0.45 1 d PD B 2 H39D H 0.0357 0.0940 0.3382 0.088 Uiso 0.45 1 calc PR B 2 H39E H 0.0242 0.1162 0.4015 0.088 Uiso 0.45 1 calc PR B 2 H39F H -0.0059 0.0589 0.3325 0.088 Uiso 0.45 1 calc PR B 2 C40B C 0.0379(3) -0.0808(5) 0.3562(5) 0.0444(13) Uiso 0.45 1 d PD B 2 H40D H 0.0087 -0.0947 0.3293 0.067 Uiso 0.45 1 calc PR B 2 H40E H 0.0533 -0.1304 0.3848 0.067 Uiso 0.45 1 calc PR B 2 H40F H 0.0472 -0.0651 0.3209 0.067 Uiso 0.45 1 calc PR B 2 N1 N 0.35705(10) 0.1574(2) 0.60227(16) 0.0328(6) Uani 1 1 d . . . N2 N 0.35281(10) 0.2729(2) 0.50953(16) 0.0338(7) Uani 1 1 d . . . C41A C 0.3169(2) 0.1852(5) 0.5554(4) 0.0489(17) Uiso 0.60 1 d P C 1 H41A H 0.3053 0.2083 0.5858 0.059 Uiso 0.60 1 calc PR C 1 H41B H 0.3000 0.1360 0.5274 0.059 Uiso 0.60 1 calc PR C 1 C42A C 0.3148(3) 0.2545(6) 0.5003(5) 0.0557(19) Uiso 0.60 1 d P C 1 H42A H 0.2970 0.2345 0.4491 0.067 Uiso 0.60 1 calc PR C 1 H42B H 0.3025 0.3069 0.5078 0.067 Uiso 0.60 1 calc PR C 1 C43A C 0.3738(2) 0.1227(4) 0.5514(4) 0.0378(14) Uiso 0.60 1 d P C 1 H43A H 0.4026 0.1048 0.5821 0.045 Uiso 0.60 1 calc PR C 1 H43B H 0.3577 0.0724 0.5240 0.045 Uiso 0.60 1 calc PR C 1 C44A C 0.3712(2) 0.1914(5) 0.4965(4) 0.0459(16) Uiso 0.60 1 d P C 1 H44A H 0.3538 0.1711 0.4453 0.055 Uiso 0.60 1 calc PR C 1 H44B H 0.3988 0.2035 0.5034 0.055 Uiso 0.60 1 calc PR C 1 C45A C 0.3856(2) 0.2291(5) 0.6398(4) 0.0445(15) Uiso 0.60 1 d P C 1 H45A H 0.4139 0.2071 0.6671 0.053 Uiso 0.60 1 calc PR C 1 H45B H 0.3788 0.2555 0.6760 0.053 Uiso 0.60 1 calc PR C 1 C46A C 0.3830(3) 0.2974(6) 0.5838(4) 0.0534(18) Uiso 0.60 1 d P C 1 H46A H 0.3755 0.3529 0.5963 0.064 Uiso 0.60 1 calc PR C 1 H46B H 0.4100 0.3036 0.5864 0.064 Uiso 0.60 1 calc PR C 1 C41B C 0.3321(3) 0.1269(7) 0.5279(6) 0.042(2) Uiso 0.40 1 d P C 2 H41C H 0.3043 0.1137 0.5194 0.050 Uiso 0.40 1 calc PR C 2 H41D H 0.3440 0.0742 0.5202 0.050 Uiso 0.40 1 calc PR C 2 C42B C 0.3299(3) 0.1967(7) 0.4727(6) 0.043(2) Uiso 0.40 1 d P C 2 H42C H 0.3408 0.1732 0.4413 0.051 Uiso 0.40 1 calc PR C 2 H42D H 0.3010 0.2123 0.4401 0.051 Uiso 0.40 1 calc PR C 2 C43B C 0.3952(4) 0.1869(8) 0.6205(7) 0.050(3) Uiso 0.40 1 d P C 2 H43C H 0.4123 0.1393 0.6198 0.060 Uiso 0.40 1 calc PR C 2 H43D H 0.4082 0.2108 0.6711 0.060 Uiso 0.40 1 calc PR C 2 C44B C 0.3926(3) 0.2552(8) 0.5663(6) 0.047(2) Uiso 0.40 1 d P C 2 H44C H 0.4046 0.3083 0.5941 0.056 Uiso 0.40 1 calc PR C 2 H44D H 0.4094 0.2372 0.5437 0.056 Uiso 0.40 1 calc PR C 2 C45B C 0.3316(4) 0.2342(7) 0.6084(6) 0.048(2) Uiso 0.40 1 d P C 2 H45C H 0.3036 0.2153 0.5956 0.058 Uiso 0.40 1 calc PR C 2 H45D H 0.3450 0.2570 0.6593 0.058 Uiso 0.40 1 calc PR C 2 C46B C 0.3297(4) 0.3031(7) 0.5536(6) 0.047(2) Uiso 0.40 1 d P C 2 H46C H 0.3425 0.3560 0.5810 0.056 Uiso 0.40 1 calc PR C 2 H46D H 0.3008 0.3157 0.5180 0.056 Uiso 0.40 1 calc PR C 2 O1T O 0.41580(19) 0.5180(4) 0.7739(3) 0.1122(18) Uani 1 1 d U . . C1T C 0.3984(2) 0.4415(5) 0.7344(4) 0.096(2) Uani 1 1 d U . . H1T1 H 0.3858 0.4521 0.6807 0.115 Uiso 1 1 calc R . . H1T2 H 0.4200 0.3980 0.7479 0.115 Uiso 1 1 calc R . . C2T C 0.3695(3) 0.4125(7) 0.7515(5) 0.125(3) Uani 1 1 d U . . H2T1 H 0.3702 0.3497 0.7558 0.150 Uiso 1 1 calc R . . H2T2 H 0.3417 0.4303 0.7139 0.150 Uiso 1 1 calc R . . C3T C 0.3819(4) 0.4550(8) 0.8263(6) 0.144(4) Uani 1 1 d U . . H3T1 H 0.3578 0.4661 0.8330 0.172 Uiso 1 1 calc R . . H3T2 H 0.4017 0.4195 0.8678 0.172 Uiso 1 1 calc R . . C4T C 0.3994(3) 0.5292(6) 0.8209(5) 0.108(3) Uani 1 1 d U . . H4T1 H 0.4212 0.5465 0.8704 0.129 Uiso 1 1 calc R . . H4T2 H 0.3785 0.5748 0.8016 0.129 Uiso 1 1 calc R . . O2T O 0.2868(2) -0.0430(4) 0.9038(4) 0.0677(16) Uiso 0.60 1 d P D 1 C5T C 0.3054(3) -0.0052(6) 0.8629(4) 0.0534(18) Uiso 0.60 1 d P D 1 H5T1 H 0.3069 0.0574 0.8688 0.064 Uiso 0.60 1 calc PR D 1 H5T2 H 0.3335 -0.0274 0.8815 0.064 Uiso 0.60 1 calc PR D 1 C6T C 0.2802(2) -0.0275(5) 0.7856(4) 0.0490(17) Uiso 0.60 1 d P D 1 H6T1 H 0.2880 -0.0835 0.7742 0.059 Uiso 0.60 1 calc PR D 1 H6T2 H 0.2817 0.0162 0.7526 0.059 Uiso 0.60 1 calc PR D 1 C7T C 0.2358(3) -0.0303(6) 0.7797(5) 0.0559(19) Uiso 0.60 1 d P D 1 H7T1 H 0.2228 0.0266 0.7693 0.067 Uiso 0.60 1 calc PR D 1 H7T2 H 0.2174 -0.0711 0.7416 0.067 Uiso 0.60 1 calc PR D 1 C8T C 0.2471(3) -0.0606(6) 0.8573(4) 0.068(2) Uiso 0.60 1 d P D 1 H8T1 H 0.2297 -0.0318 0.8744 0.081 Uiso 0.60 1 calc PR D 1 H8T2 H 0.2424 -0.1227 0.8567 0.081 Uiso 0.60 1 calc PR D 1 O1W O 0.2561(3) -0.0225(6) 0.7712(4) 0.067(5) Uiso 0.20 1 d PR D 2 O2W O 0.2886(3) 0.0173(6) 0.8725(4) 0.080(6) Uiso 0.20 1 d PR D 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 0.0220(2) 0.0305(2) 0.0241(2) -0.00773(15) 0.01045(16) -0.00180(15) Cu2 0.0240(2) 0.0296(2) 0.0257(2) -0.00459(16) 0.01102(17) 0.00246(15) O1 0.0232(11) 0.0365(13) 0.0261(11) -0.0077(10) 0.0118(9) -0.0034(10) O2 0.0239(12) 0.0418(14) 0.0302(12) -0.0163(11) 0.0113(10) -0.0029(10) O3 0.0248(11) 0.0349(13) 0.0258(11) -0.0076(10) 0.0118(10) 0.0027(10) O4 0.0267(12) 0.0442(15) 0.0364(14) -0.0122(12) 0.0114(11) 0.0075(11) O5 0.0246(11) 0.0332(12) 0.0276(11) -0.0058(10) 0.0136(10) -0.0016(10) O6 0.0235(12) 0.0406(14) 0.0356(13) -0.0174(11) 0.0124(10) -0.0017(10) O7 0.0237(11) 0.0320(12) 0.0291(12) -0.0087(10) 0.0124(10) -0.0005(9) O8 0.0247(12) 0.0390(14) 0.0406(14) -0.0106(11) 0.0145(11) 0.0000(10) C1 0.0274(19) 0.055(3) 0.042(2) -0.0182(19) 0.0067(16) -0.0089(17) C2 0.036(2) 0.060(3) 0.049(3) -0.001(2) 0.0035(19) 0.009(2) C3 0.035(2) 0.118(5) 0.044(2) -0.020(3) 0.022(2) -0.033(3) C4 0.0244(17) 0.048(2) 0.0263(16) -0.0066(15) 0.0099(14) -0.0051(15) C5 0.0241(15) 0.0338(17) 0.0204(14) -0.0015(12) 0.0103(12) -0.0043(13) C6 0.0278(17) 0.0383(19) 0.0244(15) -0.0097(14) 0.0127(13) -0.0061(14) C7 0.0256(15) 0.0296(16) 0.0203(14) -0.0021(12) 0.0114(12) -0.0029(13) C8 0.0296(16) 0.0280(16) 0.0228(15) -0.0039(12) 0.0143(13) -0.0026(13) C9 0.0300(17) 0.0407(19) 0.0267(16) -0.0103(14) 0.0120(14) -0.0038(15) C10 0.0379(19) 0.046(2) 0.0280(17) -0.0153(16) 0.0166(15) -0.0023(16) C11 0.0355(18) 0.0342(18) 0.0268(16) -0.0044(14) 0.0183(14) 0.0025(14) C12 0.0292(16) 0.0271(16) 0.0207(14) 0.0003(12) 0.0125(13) 0.0016(13) C13 0.0281(16) 0.0268(15) 0.0212(14) -0.0026(12) 0.0128(13) 0.0005(13) C14 0.0268(15) 0.0275(16) 0.0206(14) 0.0018(12) 0.0123(12) 0.0040(12) C15 0.0305(17) 0.0363(18) 0.0251(16) -0.0054(14) 0.0119(14) 0.0077(14) C16 0.0294(17) 0.0370(19) 0.0313(17) -0.0043(15) 0.0122(15) 0.0097(14) C21 0.034(2) 0.092(4) 0.086(4) -0.033(3) 0.028(3) 0.001(3) C22 0.095(5) 0.104(5) 0.088(4) 0.016(4) 0.075(4) 0.015(4) C23 0.045(3) 0.056(3) 0.113(5) -0.036(3) 0.043(3) 0.000(2) C24 0.0300(18) 0.043(2) 0.045(2) -0.0107(17) 0.0235(17) 0.0004(15) C25 0.0258(15) 0.0266(15) 0.0263(15) 0.0012(12) 0.0151(13) 0.0018(12) C26 0.0268(16) 0.0306(17) 0.0327(17) -0.0102(14) 0.0143(14) -0.0011(13) C27 0.0258(16) 0.0260(16) 0.0301(16) -0.0059(13) 0.0121(13) 0.0007(13) C33A 0.0254(15) 0.0209(14) 0.0252(15) -0.0027(12) 0.0123(13) -0.0002(12) C33B 0.0254(15) 0.0209(14) 0.0252(15) -0.0027(12) 0.0123(13) -0.0002(12) C34 0.0246(15) 0.0216(14) 0.0237(14) 0.0031(12) 0.0112(12) 0.0013(12) C35 0.0257(16) 0.0295(17) 0.0341(18) -0.0069(14) 0.0099(14) -0.0004(13) C36 0.0255(16) 0.0305(17) 0.0335(17) -0.0014(14) 0.0107(14) 0.0013(13) N1 0.0364(16) 0.0309(15) 0.0274(14) -0.0003(12) 0.0125(13) -0.0007(13) N2 0.0370(16) 0.0304(15) 0.0272(14) 0.0002(12) 0.0101(13) -0.0001(13) O1T 0.118(3) 0.121(4) 0.116(3) -0.023(3) 0.072(3) -0.031(3) C1T 0.097(4) 0.109(4) 0.090(4) -0.034(3) 0.053(3) -0.019(3) C2T 0.144(5) 0.122(5) 0.122(5) -0.039(4) 0.075(4) -0.032(4) C3T 0.162(6) 0.156(6) 0.128(5) -0.019(4) 0.083(4) -0.028(4) C4T 0.119(4) 0.112(4) 0.106(4) -0.030(3) 0.065(4) -0.009(4) _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 O6 1.930(2) . ? Cu1 O2 1.930(2) . ? Cu1 O5 1.934(2) . ? Cu1 O1 1.939(2) . ? Cu1 N1 2.347(3) . ? Cu2 O3 1.931(2) . ? Cu2 O7 1.931(2) . ? Cu2 O8 1.932(3) . ? Cu2 O4 1.940(2) . ? Cu2 N2 2.337(3) 7_556 ? O1 C5 1.266(4) . ? O2 C7 1.272(4) . ? O3 C14 1.271(4) . ? O4 C16 1.259(4) . ? O5 C25 1.261(4) . ? O6 C27 1.278(4) . ? O7 C34 1.270(4) . ? O8 C36 1.276(4) . ? C1 C4 1.535(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.527(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.531(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.533(5) . ? C5 C6 1.396(5) . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C7 C8 1.500(4) . ? C8 C9 1.395(5) . ? C8 C13 1.398(5) . ? C9 C10 1.390(5) . ? C9 H9 0.9500 . ? C10 C11 1.377(5) . ? C10 H10 0.9500 . ? C11 C12 1.396(4) . ? C11 H11 0.9500 . ? C12 C13 1.399(4) . ? C12 C14 1.498(5) . ? C13 H13 0.9500 . ? C14 C15 1.399(5) . ? C15 C16 1.394(5) . ? C15 H15 0.9500 . ? C16 C17B 1.530(8) . ? C16 C17A 1.553(6) . ? C17A C18A 1.489(6) . ? C17A C19A 1.513(6) . ? C17A C20A 1.571(7) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C17B C18B 1.495(8) . ? C17B C20B 1.527(8) . ? C17B C19B 1.571(8) . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21 C24 1.505(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.562(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.496(6) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.536(5) . ? C25 C26 1.397(5) . ? C26 C27 1.391(5) . ? C26 H26 0.9500 . ? C27 C28B 1.491(10) . ? C27 C28A 1.521(10) . ? C28A C29A 1.391(11) . ? C28A C33A 1.405(10) . ? C29A C30A 1.384(7) . ? C29A H29A 0.9500 . ? C30A C31A 1.383(7) . ? C30A H30A 0.9500 . ? C31A C32A 1.387(17) . ? C31A H31A 0.9500 . ? C32A C33A 1.395(16) . ? C32A C34 1.527(16) . ? C33A H33A 0.9500 . ? C28B C29B 1.420(11) . ? C29B C30B 1.384(7) . ? C29B H29B 0.9500 . ? C30B C31B 1.382(7) . ? C30B H30B 0.9500 . ? C31B C32B 1.413(17) . ? C31B H31B 0.9500 . ? C32B C34 1.480(16) . ? C34 C35 1.403(5) . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 C37B 1.534(7) . ? C36 C37A 1.540(7) . ? C37A C38A 1.505(7) . ? C37A C40A 1.539(7) . ? C37A C39A 1.545(7) . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? C40A H40A 0.9800 . ? C40A H40B 0.9800 . ? C40A H40C 0.9800 . ? C37B C39B 1.511(8) . ? C37B C40B 1.522(8) . ? C37B C38B 1.561(8) . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? N1 C43B 1.367(12) . ? N1 C41A 1.407(8) . ? N1 C41B 1.442(11) . ? N1 C45A 1.487(8) . ? N1 C43A 1.559(7) . ? N1 C45B 1.581(12) . ? N2 C42A 1.372(9) . ? N2 C44B 1.407(11) . ? N2 C46A 1.451(9) . ? N2 C42B 1.455(11) . ? N2 C44A 1.537(8) . ? N2 C46B 1.600(11) . ? N2 Cu2 2.337(3) 7_556 ? C41A C42A 1.551(11) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C42A H42A 0.9900 . ? C42A H42B 0.9900 . ? C43A C44A 1.536(10) . ? C43A H43A 0.9900 . ? C43A H43B 0.9900 . ? C44A H44A 0.9900 . ? C44A H44B 0.9900 . ? C45A C46A 1.548(11) . ? C45A H45A 0.9900 . ? C45A H45B 0.9900 . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C41B C42B 1.557(15) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? C43B C44B 1.521(16) . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? C45B C46B 1.544(16) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? O1T C4T 1.390(9) . ? O1T C1T 1.422(9) . ? C1T C2T 1.370(11) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.535(12) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.367(13) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C8T 1.350(10) . ? O2T C5T 1.460(10) . ? C5T C6T 1.452(11) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C7T 1.608(11) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T C8T 1.524(12) . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? 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 O6 Cu1 O2 87.80(10) . . ? O6 Cu1 O5 91.82(10) . . ? O2 Cu1 O5 172.22(11) . . ? O6 Cu1 O1 166.82(11) . . ? O2 Cu1 O1 91.93(10) . . ? O5 Cu1 O1 86.67(10) . . ? O6 Cu1 N1 95.72(11) . . ? O2 Cu1 N1 93.29(11) . . ? O5 Cu1 N1 94.48(11) . . ? O1 Cu1 N1 97.45(11) . . ? O3 Cu2 O7 87.81(10) . . ? O3 Cu2 O8 166.74(12) . . ? O7 Cu2 O8 91.88(10) . . ? O3 Cu2 O4 91.79(10) . . ? O7 Cu2 O4 172.39(12) . . ? O8 Cu2 O4 86.76(11) . . ? O3 Cu2 N2 95.63(11) . 7_556 ? O7 Cu2 N2 93.35(11) . 7_556 ? O8 Cu2 N2 97.62(11) . 7_556 ? O4 Cu2 N2 94.26(12) . 7_556 ? C5 O1 Cu1 127.0(2) . . ? C7 O2 Cu1 126.8(2) . . ? C14 O3 Cu2 127.0(2) . . ? C16 O4 Cu2 127.2(2) . . ? C25 O5 Cu1 127.2(2) . . ? C27 O6 Cu1 126.3(2) . . ? C34 O7 Cu2 126.3(2) . . ? C36 O8 Cu2 127.3(2) . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 C3 109.7(4) . . ? C2 C4 C5 106.8(3) . . ? C3 C4 C5 108.4(3) . . ? C2 C4 C1 109.6(3) . . ? C3 C4 C1 108.6(4) . . ? C5 C4 C1 113.7(3) . . ? O1 C5 C6 124.6(3) . . ? O1 C5 C4 114.5(3) . . ? C6 C5 C4 120.9(3) . . ? C5 C6 C7 124.5(3) . . ? C5 C6 H6 117.7 . . ? C7 C6 H6 117.7 . . ? O2 C7 C6 124.7(3) . . ? O2 C7 C8 115.2(3) . . ? C6 C7 C8 120.1(3) . . ? C9 C8 C13 119.0(3) . . ? C9 C8 C7 122.8(3) . . ? C13 C8 C7 118.2(3) . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 121.4(3) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 118.9(3) . . ? C11 C12 C14 123.5(3) . . ? C13 C12 C14 117.6(3) . . ? C8 C13 C12 121.2(3) . . ? C8 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? O3 C14 C15 124.7(3) . . ? O3 C14 C12 115.0(3) . . ? C15 C14 C12 120.3(3) . . ? C16 C15 C14 124.4(3) . . ? C16 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? O4 C16 C15 124.8(3) . . ? O4 C16 C17B 112.0(4) . . ? C15 C16 C17B 122.0(4) . . ? O4 C16 C17A 117.0(3) . . ? C15 C16 C17A 118.0(3) . . ? C18A C17A C19A 113.1(5) . . ? C18A C17A C16 113.0(5) . . ? C19A C17A C16 109.9(4) . . ? C18A C17A C20A 108.2(5) . . ? C19A C17A C20A 105.8(5) . . ? C16 C17A C20A 106.4(5) . . ? C18B C17B C20B 110.5(7) . . ? C18B C17B C16 112.0(7) . . ? C20B C17B C16 110.8(7) . . ? C18B C17B C19B 110.3(7) . . ? C20B C17B C19B 106.7(7) . . ? C16 C17B C19B 106.4(6) . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C17B C20B H20D 109.5 . . ? C17B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C17B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C23 C24 C21 112.0(4) . . ? C23 C24 C25 112.8(3) . . ? C21 C24 C25 110.6(3) . . ? C23 C24 C22 105.1(5) . . ? C21 C24 C22 109.7(5) . . ? C25 C24 C22 106.4(4) . . ? O5 C25 C26 124.6(3) . . ? O5 C25 C24 115.5(3) . . ? C26 C25 C24 119.8(3) . . ? C27 C26 C25 124.5(3) . . ? C27 C26 H26 117.7 . . ? C25 C26 H26 117.7 . . ? O6 C27 C26 124.8(3) . . ? O6 C27 C28B 113.5(4) . . ? C26 C27 C28B 121.5(4) . . ? O6 C27 C28A 115.0(4) . . ? C26 C27 C28A 119.8(4) . . ? C29A C28A C33A 119.7(7) . . ? C29A C28A C27 123.7(7) . . ? C33A C28A C27 116.5(6) . . ? C30A C29A C28A 120.0(7) . . ? C30A C29A H29A 120.0 . . ? C28A C29A H29A 120.0 . . ? C31A C30A C29A 120.9(7) . . ? C31A C30A H30A 119.5 . . ? C29A C30A H30A 119.5 . . ? C30A C31A C32A 119.2(9) . . ? C30A C31A H31A 120.4 . . ? C32A C31A H31A 120.4 . . ? C31A C32A C33A 120.9(11) . . ? C31A C32A C34 122.3(11) . . ? C33A C32A C34 116.7(10) . . ? C32A C33A C28A 119.0(8) . . ? C32A C33A H33A 120.5 . . ? C28A C33A H33A 120.5 . . ? C29B C28B C27 122.9(7) . . ? C30B C29B C28B 120.5(7) . . ? C30B C29B H29B 119.7 . . ? C28B C29B H29B 119.7 . . ? C31B C30B C29B 120.8(7) . . ? C31B C30B H30B 119.6 . . ? C29B C30B H30B 119.6 . . ? C30B C31B C32B 120.6(9) . . ? C30B C31B H31B 119.7 . . ? C32B C31B H31B 119.7 . . ? C31B C32B C34 122.6(11) . . ? O7 C34 C35 125.2(3) . . ? O7 C34 C32B 114.2(7) . . ? C35 C34 C32B 120.4(7) . . ? O7 C34 C32A 115.0(6) . . ? C35 C34 C32A 119.7(7) . . ? C36 C35 C34 124.4(3) . . ? C36 C35 H35 117.8 . . ? C34 C35 H35 117.8 . . ? O8 C36 C35 124.2(3) . . ? O8 C36 C37B 115.0(4) . . ? C35 C36 C37B 120.5(4) . . ? O8 C36 C37A 113.6(4) . . ? C35 C36 C37A 121.8(4) . . ? C38A C37A C40A 111.0(6) . . ? C38A C37A C36 111.2(5) . . ? C40A C37A C36 110.6(5) . . ? C38A C37A C39A 108.9(6) . . ? C40A C37A C39A 106.9(5) . . ? C36 C37A C39A 108.0(5) . . ? C39B C37B C40B 111.6(6) . . ? C39B C37B C36 111.3(6) . . ? C40B C37B C36 114.3(6) . . ? C39B C37B C38B 108.5(6) . . ? C40B C37B C38B 105.6(6) . . ? C36 C37B C38B 105.0(5) . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C37B C39B H39D 109.5 . . ? C37B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C37B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C37B C40B H40D 109.5 . . ? C37B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C37B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? C43B N1 C41B 117.2(7) . . ? C41A N1 C45A 112.4(5) . . ? C41A N1 C43A 106.7(4) . . ? C45A N1 C43A 101.4(4) . . ? C43B N1 C45B 107.9(7) . . ? C41B N1 C45B 103.6(6) . . ? C43B N1 Cu1 107.9(5) . . ? C41A N1 Cu1 116.1(4) . . ? C41B N1 Cu1 109.4(4) . . ? C45A N1 Cu1 111.3(3) . . ? C43A N1 Cu1 107.7(3) . . ? C45B N1 Cu1 110.7(4) . . ? C42A N2 C44B 132.9(6) . . ? C42A N2 C46A 115.3(5) . . ? C42A N2 C42B 56.3(6) . . ? C44B N2 C42B 113.0(7) . . ? C46A N2 C42B 137.1(6) . . ? C42A N2 C44A 108.8(5) . . ? C44B N2 C44A 66.4(6) . . ? C46A N2 C44A 102.7(5) . . ? C42B N2 C44A 54.7(5) . . ? C42A N2 C46B 48.2(6) . . ? C44B N2 C46B 103.1(7) . . ? C46A N2 C46B 71.2(6) . . ? C42B N2 C46B 101.5(6) . . ? C44A N2 C46B 139.1(5) . . ? C42A N2 Cu2 113.8(4) . 7_556 ? C44B N2 Cu2 112.1(5) . 7_556 ? C46A N2 Cu2 108.8(4) . 7_556 ? C42B N2 Cu2 112.6(4) . 7_556 ? C44A N2 Cu2 106.5(3) . 7_556 ? C46B N2 Cu2 113.8(4) . 7_556 ? N1 C41A C42A 112.6(6) . . ? N1 C41A H41A 109.1 . . ? C42A C41A H41A 109.1 . . ? N1 C41A H41B 109.1 . . ? C42A C41A H41B 109.1 . . ? H41A C41A H41B 107.8 . . ? N2 C42A C41A 111.4(6) . . ? N2 C42A H42A 109.4 . . ? C41A C42A H42A 109.4 . . ? N2 C42A H42B 109.4 . . ? C41A C42A H42B 109.4 . . ? H42A C42A H42B 108.0 . . ? C44A C43A N1 110.5(5) . . ? C44A C43A H43A 109.5 . . ? N1 C43A H43A 109.5 . . ? C44A C43A H43B 109.5 . . ? N1 C43A H43B 109.5 . . ? H43A C43A H43B 108.1 . . ? C43A C44A N2 109.3(5) . . ? C43A C44A H44A 109.8 . . ? N2 C44A H44A 109.8 . . ? C43A C44A H44B 109.8 . . ? N2 C44A H44B 109.8 . . ? H44A C44A H44B 108.3 . . ? N1 C45A C46A 111.4(6) . . ? N1 C45A H45A 109.3 . . ? C46A C45A H45A 109.3 . . ? N1 C45A H45B 109.3 . . ? C46A C45A H45B 109.3 . . ? H45A C45A H45B 108.0 . . ? N2 C46A C45A 110.1(6) . . ? N2 C46A H46A 109.6 . . ? C45A C46A H46A 109.6 . . ? N2 C46A H46B 109.6 . . ? C45A C46A H46B 109.6 . . ? H46A C46A H46B 108.2 . . ? N1 C41B C42B 109.0(8) . . ? N1 C41B H41C 109.9 . . ? C42B C41B H41C 109.9 . . ? N1 C41B H41D 109.9 . . ? C42B C41B H41D 109.9 . . ? H41C C41B H41D 108.3 . . ? N2 C42B C41B 112.8(8) . . ? N2 C42B H42C 109.0 . . ? C41B C42B H42C 109.0 . . ? N2 C42B H42D 109.0 . . ? C41B C42B H42D 109.0 . . ? H42C C42B H42D 107.8 . . ? N1 C43B C44B 110.5(9) . . ? N1 C43B H43C 109.5 . . ? C44B C43B H43C 109.5 . . ? N1 C43B H43D 109.5 . . ? C44B C43B H43D 109.5 . . ? H43C C43B H43D 108.1 . . ? N2 C44B C43B 114.8(9) . . ? N2 C44B H44C 108.6 . . ? C43B C44B H44C 108.6 . . ? N2 C44B H44D 108.6 . . ? C43B C44B H44D 108.6 . . ? H44C C44B H44D 107.5 . . ? C46B C45B N1 106.9(8) . . ? C46B C45B H45C 110.3 . . ? N1 C45B H45C 110.3 . . ? C46B C45B H45D 110.3 . . ? N1 C45B H45D 110.3 . . ? H45C C45B H45D 108.6 . . ? C45B C46B N2 111.5(8) . . ? C45B C46B H46C 109.3 . . ? N2 C46B H46C 109.3 . . ? C45B C46B H46D 109.3 . . ? N2 C46B H46D 109.3 . . ? H46C C46B H46D 108.0 . . ? C4T O1T C1T 105.9(6) . . ? C2T C1T O1T 109.4(7) . . ? C2T C1T H1T1 109.8 . . ? O1T C1T H1T1 109.8 . . ? C2T C1T H1T2 109.8 . . ? O1T C1T H1T2 109.8 . . ? H1T1 C1T H1T2 108.2 . . ? C1T C2T C3T 102.9(8) . . ? C1T C2T H2T1 111.2 . . ? C3T C2T H2T1 111.2 . . ? C1T C2T H2T2 111.2 . . ? C3T C2T H2T2 111.2 . . ? H2T1 C2T H2T2 109.1 . . ? C4T C3T C2T 102.3(9) . . ? C4T C3T H3T1 111.3 . . ? C2T C3T H3T1 111.3 . . ? C4T C3T H3T2 111.3 . . ? C2T C3T H3T2 111.3 . . ? H3T1 C3T H3T2 109.2 . . ? C3T C4T O1T 109.9(8) . . ? C3T C4T H4T1 109.7 . . ? O1T C4T H4T1 109.7 . . ? C3T C4T H4T2 109.7 . . ? O1T C4T H4T2 109.7 . . ? H4T1 C4T H4T2 108.2 . . ? C8T O2T C5T 109.8(6) . . ? C6T C5T O2T 107.6(7) . . ? C6T C5T H5T1 110.2 . . ? O2T C5T H5T1 110.2 . . ? C6T C5T H5T2 110.2 . . ? O2T C5T H5T2 110.2 . . ? H5T1 C5T H5T2 108.5 . . ? C5T C6T C7T 100.8(6) . . ? C5T C6T H6T1 111.6 . . ? C7T C6T H6T1 111.6 . . ? C5T C6T H6T2 111.6 . . ? C7T C6T H6T2 111.6 . . ? H6T1 C6T H6T2 109.4 . . ? C8T C7T C6T 100.2(6) . . ? C8T C7T H7T1 111.7 . . ? C6T C7T H7T1 111.7 . . ? C8T C7T H7T2 111.7 . . ? C6T C7T H7T2 111.7 . . ? H7T1 C7T H7T2 109.5 . . ? O2T C8T C7T 109.7(7) . . ? O2T C8T H8T1 109.7 . . ? C7T C8T H8T1 109.7 . . ? O2T C8T H8T2 109.7 . . ? C7T C8T H8T2 109.7 . . ? H8T1 C8T H8T2 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Cu1 O1 C5 -94.5(5) . . . . ? O2 Cu1 O1 C5 -5.9(3) . . . . ? O5 Cu1 O1 C5 -178.2(3) . . . . ? N1 Cu1 O1 C5 87.7(3) . . . . ? O6 Cu1 O2 C7 173.2(3) . . . . ? O1 Cu1 O2 C7 6.4(3) . . . . ? N1 Cu1 O2 C7 -91.2(3) . . . . ? O7 Cu2 O3 C14 -173.4(3) . . . . ? O8 Cu2 O3 C14 -84.5(5) . . . . ? O4 Cu2 O3 C14 -1.0(3) . . . . ? N2 Cu2 O3 C14 93.4(3) 7_556 . . . ? O3 Cu2 O4 C16 1.7(3) . . . . ? O8 Cu2 O4 C16 168.5(3) . . . . ? N2 Cu2 O4 C16 -94.1(3) 7_556 . . . ? O6 Cu1 O5 C25 7.3(3) . . . . ? O1 Cu1 O5 C25 174.1(3) . . . . ? N1 Cu1 O5 C25 -88.6(3) . . . . ? O2 Cu1 O6 C27 178.3(3) . . . . ? O5 Cu1 O6 C27 -9.5(3) . . . . ? O1 Cu1 O6 C27 -92.6(5) . . . . ? N1 Cu1 O6 C27 85.2(3) . . . . ? O3 Cu2 O7 C34 175.6(3) . . . . ? O8 Cu2 O7 C34 8.9(3) . . . . ? N2 Cu2 O7 C34 -88.9(3) 7_556 . . . ? O3 Cu2 O8 C36 -96.1(5) . . . . ? O7 Cu2 O8 C36 -7.6(3) . . . . ? O4 Cu2 O8 C36 179.9(3) . . . . ? N2 Cu2 O8 C36 86.0(3) 7_556 . . . ? Cu1 O1 C5 C6 2.7(5) . . . . ? Cu1 O1 C5 C4 -178.0(2) . . . . ? C2 C4 C5 O1 -68.6(4) . . . . ? C3 C4 C5 O1 49.5(5) . . . . ? C1 C4 C5 O1 170.4(3) . . . . ? C2 C4 C5 C6 110.8(4) . . . . ? C3 C4 C5 C6 -131.1(4) . . . . ? C1 C4 C5 C6 -10.3(5) . . . . ? O1 C5 C6 C7 2.6(6) . . . . ? C4 C5 C6 C7 -176.7(3) . . . . ? Cu1 O2 C7 C6 -3.8(5) . . . . ? Cu1 O2 C7 C8 176.8(2) . . . . ? C5 C6 C7 O2 -2.0(6) . . . . ? C5 C6 C7 C8 177.4(3) . . . . ? O2 C7 C8 C9 172.4(3) . . . . ? C6 C7 C8 C9 -7.0(5) . . . . ? O2 C7 C8 C13 -5.7(5) . . . . ? C6 C7 C8 C13 174.9(3) . . . . ? C13 C8 C9 C10 1.3(5) . . . . ? C7 C8 C9 C10 -176.8(3) . . . . ? C8 C9 C10 C11 -0.4(6) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C10 C11 C12 C13 0.5(5) . . . . ? C10 C11 C12 C14 179.9(3) . . . . ? C9 C8 C13 C12 -1.2(5) . . . . ? C7 C8 C13 C12 176.9(3) . . . . ? C11 C12 C13 C8 0.4(5) . . . . ? C14 C12 C13 C8 -179.1(3) . . . . ? Cu2 O3 C14 C15 0.9(5) . . . . ? Cu2 O3 C14 C12 -178.1(2) . . . . ? C11 C12 C14 O3 -173.2(3) . . . . ? C13 C12 C14 O3 6.2(4) . . . . ? C11 C12 C14 C15 7.9(5) . . . . ? C13 C12 C14 C15 -172.7(3) . . . . ? O3 C14 C15 C16 -0.9(6) . . . . ? C12 C14 C15 C16 177.9(3) . . . . ? Cu2 O4 C16 C15 -2.3(6) . . . . ? Cu2 O4 C16 C17B 165.3(4) . . . . ? Cu2 O4 C16 C17A -177.3(3) . . . . ? C14 C15 C16 O4 1.7(6) . . . . ? C14 C15 C16 C17B -164.7(5) . . . . ? C14 C15 C16 C17A 176.7(4) . . . . ? O4 C16 C17A C18A 119.5(5) . . . . ? C15 C16 C17A C18A -55.9(6) . . . . ? C17B C16 C17A C18A -164.4(18) . . . . ? O4 C16 C17A C19A -7.9(6) . . . . ? C15 C16 C17A C19A 176.7(4) . . . . ? C17B C16 C17A C19A 68.2(16) . . . . ? O4 C16 C17A C20A -121.9(5) . . . . ? C15 C16 C17A C20A 62.6(6) . . . . ? C17B C16 C17A C20A -45.8(15) . . . . ? O4 C16 C17B C18B 170.2(7) . . . . ? C15 C16 C17B C18B -21.8(9) . . . . ? C17A C16 C17B C18B 59.0(15) . . . . ? O4 C16 C17B C20B -66.0(8) . . . . ? C15 C16 C17B C20B 102.0(8) . . . . ? C17A C16 C17B C20B -177(2) . . . . ? O4 C16 C17B C19B 49.6(7) . . . . ? C15 C16 C17B C19B -142.4(6) . . . . ? C17A C16 C17B C19B -61.5(15) . . . . ? Cu1 O5 C25 C26 -4.2(5) . . . . ? Cu1 O5 C25 C24 173.0(2) . . . . ? C23 C24 C25 O5 142.9(4) . . . . ? C21 C24 C25 O5 16.7(5) . . . . ? C22 C24 C25 O5 -102.4(4) . . . . ? C23 C24 C25 C26 -39.7(5) . . . . ? C21 C24 C25 C26 -165.9(4) . . . . ? C22 C24 C25 C26 75.0(5) . . . . ? O5 C25 C26 C27 0.3(6) . . . . ? C24 C25 C26 C27 -176.8(4) . . . . ? Cu1 O6 C27 C26 9.0(5) . . . . ? Cu1 O6 C27 C28B -176.1(4) . . . . ? Cu1 O6 C27 C28A -164.2(4) . . . . ? C25 C26 C27 O6 -2.9(6) . . . . ? C25 C26 C27 C28B -177.5(4) . . . . ? C25 C26 C27 C28A 170.0(4) . . . . ? O6 C27 C28A C29A 172.9(6) . . . . ? C26 C27 C28A C29A -0.6(9) . . . . ? C28B C27 C28A C29A -102(4) . . . . ? O6 C27 C28A C33A -10.2(7) . . . . ? C26 C27 C28A C33A 176.3(4) . . . . ? C28B C27 C28A C33A 74(3) . . . . ? C33A C28A C29A C30A 1.7(9) . . . . ? C27 C28A C29A C30A 178.4(6) . . . . ? C28A C29A C30A C31A 1.1(10) . . . . ? C29A C30A C31A C32A -2.8(12) . . . . ? C30A C31A C32A C33A 1.8(16) . . . . ? C30A C31A C32A C34 178.0(8) . . . . ? C31A C32A C33A C28A 0.9(15) . . . . ? C34 C32A C33A C28A -175.5(7) . . . . ? C29A C28A C33A C32A -2.6(11) . . . . ? C27 C28A C33A C32A -179.6(7) . . . . ? O6 C27 C28B C29B -175.4(5) . . . . ? C26 C27 C28B C29B -0.2(9) . . . . ? C28A C27 C28B C29B 84(3) . . . . ? C27 C28B C29B C30B -172.5(6) . . . . ? C28B C29B C30B C31B -1.2(10) . . . . ? C29B C30B C31B C32B 1.4(12) . . . . ? C30B C31B C32B C34 -179.5(8) . . . . ? Cu2 O7 C34 C35 -7.7(5) . . . . ? Cu2 O7 C34 C32B 175.8(6) . . . . ? Cu2 O7 C34 C32A 169.9(6) . . . . ? C31B C32B C34 O7 178.4(8) . . . . ? C31B C32B C34 C35 1.8(14) . . . . ? C31B C32B C34 C32A -82(13) . . . . ? C31A C32A C34 O7 -166.7(9) . . . . ? C33A C32A C34 O7 9.7(12) . . . . ? C31A C32A C34 C35 11.0(14) . . . . ? C33A C32A C34 C35 -172.6(7) . . . . ? C31A C32A C34 C32B 110(13) . . . . ? C33A C32A C34 C32B -74(12) . . . . ? O7 C34 C35 C36 1.9(6) . . . . ? C32B C34 C35 C36 178.2(7) . . . . ? C32A C34 C35 C36 -175.6(7) . . . . ? Cu2 O8 C36 C35 4.9(5) . . . . ? Cu2 O8 C36 C37B -169.6(4) . . . . ? Cu2 O8 C36 C37A 177.9(3) . . . . ? C34 C35 C36 O8 -0.4(6) . . . . ? C34 C35 C36 C37B 173.8(4) . . . . ? C34 C35 C36 C37A -172.8(4) . . . . ? O8 C36 C37A C38A -79.7(6) . . . . ? C35 C36 C37A C38A 93.5(6) . . . . ? C37B C36 C37A C38A -180(100) . . . . ? O8 C36 C37A C40A 156.4(5) . . . . ? C35 C36 C37A C40A -30.5(7) . . . . ? C37B C36 C37A C40A 56(2) . . . . ? O8 C36 C37A C39A 39.7(6) . . . . ? C35 C36 C37A C39A -147.1(5) . . . . ? C37B C36 C37A C39A -60(2) . . . . ? O8 C36 C37B C39B 54.9(7) . . . . ? C35 C36 C37B C39B -119.8(6) . . . . ? C37A C36 C37B C39B 140(3) . . . . ? O8 C36 C37B C40B -177.6(5) . . . . ? C35 C36 C37B C40B 7.7(8) . . . . ? C37A C36 C37B C40B -92(3) . . . . ? O8 C36 C37B C38B -62.3(6) . . . . ? C35 C36 C37B C38B 123.0(6) . . . . ? C37A C36 C37B C38B 23(2) . . . . ? O6 Cu1 N1 C43B -155.5(6) . . . . ? O2 Cu1 N1 C43B 116.4(6) . . . . ? O5 Cu1 N1 C43B -63.2(6) . . . . ? O1 Cu1 N1 C43B 24.1(6) . . . . ? O6 Cu1 N1 C41A 34.2(4) . . . . ? O2 Cu1 N1 C41A -53.9(4) . . . . ? O5 Cu1 N1 C41A 126.5(4) . . . . ? O1 Cu1 N1 C41A -146.3(4) . . . . ? O6 Cu1 N1 C41B -26.9(5) . . . . ? O2 Cu1 N1 C41B -115.0(5) . . . . ? O5 Cu1 N1 C41B 65.4(5) . . . . ? O1 Cu1 N1 C41B 152.7(5) . . . . ? O6 Cu1 N1 C45A 164.5(4) . . . . ? O2 Cu1 N1 C45A 76.4(4) . . . . ? O5 Cu1 N1 C45A -103.2(4) . . . . ? O1 Cu1 N1 C45A -16.0(4) . . . . ? O6 Cu1 N1 C43A -85.2(3) . . . . ? O2 Cu1 N1 C43A -173.4(3) . . . . ? O5 Cu1 N1 C43A 7.0(3) . . . . ? O1 Cu1 N1 C43A 94.3(3) . . . . ? O6 Cu1 N1 C45B 86.7(5) . . . . ? O2 Cu1 N1 C45B -1.4(5) . . . . ? O5 Cu1 N1 C45B 179.0(5) . . . . ? O1 Cu1 N1 C45B -93.8(5) . . . . ? C43B N1 C41A C42A 14.8(12) . . . . ? C41B N1 C41A C42A -81.4(8) . . . . ? C45A N1 C41A C42A 52.0(8) . . . . ? C43A N1 C41A C42A -58.2(7) . . . . ? C45B N1 C41A C42A 86.6(9) . . . . ? Cu1 N1 C41A C42A -178.2(5) . . . . ? C44B N2 C42A C41A -15.0(12) . . . . ? C46A N2 C42A C41A -54.8(8) . . . . ? C42B N2 C42A C41A 76.3(8) . . . . ? C44A N2 C42A C41A 59.9(7) . . . . ? C46B N2 C42A C41A -80.3(8) . . . . ? Cu2 N2 C42A C41A 178.4(5) 7_556 . . . ? N1 C41A C42A N2 0.3(9) . . . . ? C43B N1 C43A C44A -75.8(7) . . . . ? C41A N1 C43A C44A 56.6(6) . . . . ? C41B N1 C43A C44A 80.1(7) . . . . ? C45A N1 C43A C44A -61.2(6) . . . . ? C45B N1 C43A C44A 13.8(11) . . . . ? Cu1 N1 C43A C44A -178.1(4) . . . . ? N1 C43A C44A N2 0.1(7) . . . . ? C42A N2 C44A C43A -59.0(7) . . . . ? C44B N2 C44A C43A 70.6(7) . . . . ? C46A N2 C44A C43A 63.7(6) . . . . ? C42B N2 C44A C43A -75.7(7) . . . . ? C46B N2 C44A C43A -12.1(11) . . . . ? Cu2 N2 C44A C43A 178.0(4) 7_556 . . . ? C43B N1 C45A C46A 83.8(11) . . . . ? C41A N1 C45A C46A -52.0(7) . . . . ? C41B N1 C45A C46A 11.8(11) . . . . ? C43A N1 C45A C46A 61.5(7) . . . . ? C45B N1 C45A C46A -78.5(7) . . . . ? Cu1 N1 C45A C46A 175.8(5) . . . . ? C42A N2 C46A C45A 53.5(8) . . . . ? C44B N2 C46A C45A -75.1(10) . . . . ? C42B N2 C46A C45A -13.4(12) . . . . ? C44A N2 C46A C45A -64.6(7) . . . . ? C46B N2 C46A C45A 73.3(7) . . . . ? Cu2 N2 C46A C45A -177.2(5) 7_556 . . . ? N1 C45A C46A N2 0.9(9) . . . . ? C43B N1 C41B C42B -52.8(11) . . . . ? C41A N1 C41B C42B 75.0(8) . . . . ? C45A N1 C41B C42B -11.9(13) . . . . ? C43A N1 C41B C42B -77.6(8) . . . . ? C45B N1 C41B C42B 65.8(9) . . . . ? Cu1 N1 C41B C42B -176.1(6) . . . . ? C42A N2 C42B C41B -78.9(9) . . . . ? C44B N2 C42B C41B 48.5(10) . . . . ? C46A N2 C42B C41B 13.3(13) . . . . ? C44A N2 C42B C41B 82.0(9) . . . . ? C46B N2 C42B C41B -61.3(9) . . . . ? Cu2 N2 C42B C41B 176.7(6) 7_556 . . . ? N1 C41B C42B N2 -0.4(11) . . . . ? C41A N1 C43B C44B -14.3(15) . . . . ? C41B N1 C43B C44B 54.0(12) . . . . ? C45A N1 C43B C44B -80.0(11) . . . . ? C43A N1 C43B C44B 76.1(9) . . . . ? C45B N1 C43B C44B -62.3(11) . . . . ? Cu1 N1 C43B C44B 178.0(7) . . . . ? C42A N2 C44B C43B 15.7(14) . . . . ? C46A N2 C44B C43B 90.3(12) . . . . ? C42B N2 C44B C43B -49.0(11) . . . . ? C44A N2 C44B C43B -78.5(9) . . . . ? C46B N2 C44B C43B 59.7(11) . . . . ? Cu2 N2 C44B C43B -177.5(8) 7_556 . . . ? N1 C43B C44B N2 -0.8(14) . . . . ? C43B N1 C45B C46B 60.0(10) . . . . ? C41A N1 C45B C46B -75.1(9) . . . . ? C41B N1 C45B C46B -64.9(9) . . . . ? C45A N1 C45B C46B 71.3(8) . . . . ? C43A N1 C45B C46B -14.3(13) . . . . ? Cu1 N1 C45B C46B 177.9(6) . . . . ? N1 C45B C46B N2 1.2(11) . . . . ? C42A N2 C46B C45B 79.5(10) . . . . ? C44B N2 C46B C45B -57.5(10) . . . . ? C46A N2 C46B C45B -76.3(9) . . . . ? C42B N2 C46B C45B 59.7(10) . . . . ? C44A N2 C46B C45B 11.5(13) . . . . ? Cu2 N2 C46B C45B -179.1(7) 7_556 . . . ? C4T O1T C1T C2T 6.1(11) . . . . ? O1T C1T C2T C3T -22.2(12) . . . . ? C1T C2T C3T C4T 30.5(12) . . . . ? C2T C3T C4T O1T -28.1(12) . . . . ? C1T O1T C4T C3T 15.4(11) . . . . ? C8T O2T C5T C6T -20.3(9) . . . . ? O2T C5T C6T C7T 32.4(8) . . . . ? C5T C6T C7T C8T -32.2(8) . . . . ? C5T O2T C8T C7T -2.9(10) . . . . ? C6T C7T C8T O2T 22.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.202 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.104 data_jack2 _database_code_depnum_ccdc_archive 'CCDC 606853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H38 Cu2 O8, 2(N3 C10 H14)' _chemical_formula_sum 'C60 H66 Cu2 N6 O8' _chemical_formula_weight 1126.29 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' O O 0.0106 0.0060 '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' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.856(1) _cell_length_b 10.7020(9) _cell_length_c 14.693(1) _cell_angle_alpha 96.408(9) _cell_angle_beta 90.624(8) _cell_angle_gamma 115.561(6) _cell_volume 1386.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 185 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 21.72 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 590 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7226 _exptl_absorpt_correction_T_max 0.8262 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'Nonius KappaCCD' _diffrn_measurement_method '/w and /p' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18019 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4502 _reflns_number_gt 3878 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DIRAX(Duisenberg, 1992)' _computing_data_reduction 'EVALCCD(Duisenberg, 2003)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WINGX-32 (Farrugia, 1999)' _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0395P)^2^+1.2027P] 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 4502 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 C1A C -0.2233(7) 0.7120(7) 0.6718(4) 0.0481(11) Uiso 0.50 1 d P A 1 H1A1 H -0.2983 0.6793 0.6216 0.072 Uiso 0.50 1 calc PR A 1 H1A2 H -0.2110 0.8019 0.7001 0.072 Uiso 0.50 1 calc PR A 1 H1A3 H -0.2545 0.6472 0.7162 0.072 Uiso 0.50 1 calc PR A 1 C2A C -0.0943(7) 0.5880(6) 0.5827(4) 0.0448(10) Uiso 0.50 1 d P A 1 H2A1 H -0.1264 0.5172 0.6230 0.067 Uiso 0.50 1 calc PR A 1 H2A2 H -0.0021 0.5958 0.5573 0.067 Uiso 0.50 1 calc PR A 1 H2A3 H -0.1706 0.5631 0.5339 0.067 Uiso 0.50 1 calc PR A 1 C3A C 0.0206(7) 0.7974(7) 0.5589(4) 0.0506(11) Uiso 0.50 1 d P A 1 H3A1 H 0.0976 0.7667 0.5462 0.076 Uiso 0.50 1 calc PR A 1 H3A2 H 0.0665 0.8965 0.5771 0.076 Uiso 0.50 1 calc PR A 1 H3A3 H -0.0450 0.7752 0.5047 0.076 Uiso 0.50 1 calc PR A 1 C1 C -0.1965(7) 0.7648(7) 0.6540(4) 0.0481(11) Uiso 0.50 1 d P A 2 H1A H -0.2724 0.7232 0.6042 0.072 Uiso 0.50 1 calc PR A 2 H1B H -0.1583 0.8646 0.6599 0.072 Uiso 0.50 1 calc PR A 2 H1C H -0.2397 0.7321 0.7099 0.072 Uiso 0.50 1 calc PR A 2 C2 C -0.1429(7) 0.5612(6) 0.6099(4) 0.0448(10) Uiso 0.50 1 d P A 2 H2A H -0.2149 0.5344 0.5584 0.067 Uiso 0.50 1 calc PR A 2 H2B H -0.1927 0.5176 0.6614 0.067 Uiso 0.50 1 calc PR A 2 H2C H -0.0658 0.5318 0.5942 0.067 Uiso 0.50 1 calc PR A 2 C3 C -0.0165(7) 0.8438(7) 0.5743(4) 0.0506(11) Uiso 0.50 1 d P A 2 H3A H 0.0805 0.8590 0.5530 0.076 Uiso 0.50 1 calc PR A 2 H3B H -0.0094 0.9278 0.6094 0.076 Uiso 0.50 1 calc PR A 2 H3C H -0.0877 0.8185 0.5226 0.076 Uiso 0.50 1 calc PR A 2 C4 C -0.0694(3) 0.7245(3) 0.63527(16) 0.0354(6) Uani 1 1 d . . . C5 C 0.0456(3) 0.7654(2) 0.71797(15) 0.0282(5) Uani 1 1 d . A . C6 C 0.0730(3) 0.8842(3) 0.77943(16) 0.0357(6) Uani 1 1 d . . . H6 H 0.0180 0.9339 0.7691 0.043 Uiso 1 1 calc R A . C7 C 0.1767(3) 0.9337(2) 0.85500(15) 0.0272(5) Uani 1 1 d . A . C8 C 0.1883(3) 1.0566(2) 0.92031(15) 0.0280(5) Uani 1 1 d . . . C9 C 0.0805(3) 1.1078(3) 0.92174(17) 0.0394(6) Uani 1 1 d . A . H9 H -0.0046 1.0648 0.8812 0.047 Uiso 1 1 calc R . . C10 C 0.0993(3) 1.2224(3) 0.9831(2) 0.0486(7) Uani 1 1 d . . . H10 H 0.0264 1.2557 0.9839 0.058 Uiso 1 1 calc R A . C11 C 0.2254(3) 1.2880(3) 1.04346(18) 0.0410(7) Uani 1 1 d . A . H11 H 0.2373 1.3658 1.0840 0.049 Uiso 1 1 calc R . . C12 C 0.3345(3) 1.2386(2) 1.04404(15) 0.0273(5) Uani 1 1 d . . . C13 C 0.3128(3) 1.1217(2) 0.98277(14) 0.0255(5) Uani 1 1 d . A . H13 H 0.3837 1.0860 0.9837 0.031 Uiso 1 1 calc R . . C14 C 0.4720(2) 1.3033(2) 1.10934(14) 0.0248(5) Uani 1 1 d . A . C15 C 0.5107(3) 1.4320(2) 1.16126(16) 0.0316(5) Uani 1 1 d . . . H15 H 0.4513 1.4779 1.1516 0.038 Uiso 1 1 calc R A . C16 C 0.6323(3) 1.4978(2) 1.22698(15) 0.0269(5) Uani 1 1 d . A . C17 C 0.6586(3) 1.6345(2) 1.28671(17) 0.0341(6) Uani 1 1 d . . . C18 C 0.5689(4) 1.7071(3) 1.2517(2) 0.0521(8) Uani 1 1 d . A . H18A H 0.5887 1.7208 1.1889 0.078 Uiso 1 1 calc R . . H18B H 0.5982 1.7960 1.2883 0.078 Uiso 1 1 calc R . . H18C H 0.4632 1.6503 1.2560 0.078 Uiso 1 1 calc R . . C19 C 0.6122(4) 1.5954(3) 1.38245(18) 0.0509(7) Uani 1 1 d . A . H19A H 0.6336 1.6786 1.4239 0.076 Uiso 1 1 calc R . . H19B H 0.6676 1.5482 1.4038 0.076 Uiso 1 1 calc R . . H19C H 0.5062 1.5349 1.3796 0.076 Uiso 1 1 calc R . . C20 C 0.8270(3) 1.7326(3) 1.2933(2) 0.0541(8) Uani 1 1 d . A . H20A H 0.8604 1.7494 1.2328 0.081 Uiso 1 1 calc R . . H20B H 0.8818 1.6905 1.3221 0.081 Uiso 1 1 calc R . . H20C H 0.8447 1.8195 1.3291 0.081 Uiso 1 1 calc R . . C21 C 0.3955(3) 0.7676(3) 0.60562(17) 0.0392(6) Uani 1 1 d . . . H21 H 0.3065 0.6856 0.6004 0.047 Uiso 1 1 calc R . . C22 C 0.4687(3) 0.8056(3) 0.52822(18) 0.0453(7) Uani 1 1 d . . . H22 H 0.4305 0.7524 0.4714 0.054 Uiso 1 1 calc R . . C23 C 0.6013(3) 0.9256(3) 0.53728(19) 0.0492(7) Uani 1 1 d . . . H23 H 0.6551 0.9539 0.4859 0.059 Uiso 1 1 calc R . . C24 C 0.6555(3) 1.0043(3) 0.62127(18) 0.0436(7) Uani 1 1 d . B . H24 H 0.7455 1.0854 0.6275 0.052 Uiso 1 1 calc R . . C25 C 0.5721(3) 0.9595(3) 0.69702(17) 0.0348(6) Uani 1 1 d . . . C26 C 0.7101(3) 1.1652(3) 0.81742(17) 0.0349(6) Uani 1 1 d . . . C27 C 0.7050(3) 1.2152(3) 0.90848(17) 0.0375(6) Uani 1 1 d . B . H27 H 0.6417 1.1561 0.9475 0.045 Uiso 1 1 calc R . . C28 C 0.7945(3) 1.3523(3) 0.93949(19) 0.0432(7) Uani 1 1 d . . . H28 H 0.7909 1.3890 0.9993 0.052 Uiso 1 1 calc R B . C29 C 0.8910(3) 1.4359(3) 0.8802(2) 0.0436(7) Uani 1 1 d . B . H29 H 0.9530 1.5298 0.8990 0.052 Uiso 1 1 calc R . . C30 C 0.8923(3) 1.3768(3) 0.7939(2) 0.0449(7) Uani 1 1 d . . . H30 H 0.9600 1.4325 0.7551 0.054 Uiso 1 1 calc R B . O1 O 0.11112(17) 0.68755(16) 0.72343(10) 0.0294(4) Uani 1 1 d . . . O2 O 0.26740(18) 0.88315(16) 0.87419(10) 0.0300(4) Uani 1 1 d . . . O3 O 0.54609(17) 1.23055(16) 1.11189(10) 0.0273(4) Uani 1 1 d . . . O4 O 0.72473(18) 1.44946(16) 1.24541(10) 0.0298(4) Uani 1 1 d . . . N1 N 0.4441(2) 0.8417(2) 0.68935(13) 0.0337(5) Uani 1 1 d . A . N2 N 0.6117(3) 1.0270(2) 0.78533(15) 0.0441(6) Uani 1 1 d . B 1 H1N H 0.553(3) 0.980(3) 0.826(2) 0.053 Uiso 1 1 d . C 1 N3 N 0.8030(3) 1.2436(2) 0.76034(16) 0.0446(6) Uani 1 1 d . B . Cu1 Cu 0.28646(3) 0.73003(3) 0.803028(17) 0.02423(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C4 0.0348(14) 0.0342(14) 0.0326(12) -0.0066(10) -0.0158(10) 0.0139(12) C5 0.0249(12) 0.0283(13) 0.0280(11) -0.0005(10) -0.0038(9) 0.0095(11) C6 0.0376(14) 0.0367(15) 0.0363(13) -0.0114(11) -0.0150(11) 0.0235(12) C7 0.0257(12) 0.0287(13) 0.0268(11) -0.0021(10) -0.0034(9) 0.0129(11) C8 0.0292(13) 0.0275(13) 0.0266(11) -0.0045(9) -0.0050(9) 0.0137(11) C9 0.0323(14) 0.0440(16) 0.0426(14) -0.0154(12) -0.0150(11) 0.0226(13) C10 0.0421(16) 0.0549(18) 0.0582(17) -0.0202(14) -0.0167(13) 0.0367(15) C11 0.0423(16) 0.0410(15) 0.0439(14) -0.0193(12) -0.0120(12) 0.0284(13) C12 0.0285(13) 0.0282(13) 0.0256(11) -0.0035(9) -0.0039(9) 0.0145(11) C13 0.0265(12) 0.0278(13) 0.0258(11) -0.0012(9) -0.0018(9) 0.0164(10) C14 0.0271(12) 0.0276(13) 0.0213(10) -0.0003(9) 0.0001(9) 0.0145(11) C15 0.0346(14) 0.0295(13) 0.0333(12) -0.0073(10) -0.0080(10) 0.0194(11) C16 0.0305(13) 0.0228(12) 0.0262(11) -0.0004(9) 0.0007(9) 0.0112(11) C17 0.0363(14) 0.0241(13) 0.0381(13) -0.0091(10) -0.0078(11) 0.0130(11) C18 0.064(2) 0.0325(15) 0.0619(18) -0.0145(13) -0.0202(15) 0.0288(15) C19 0.068(2) 0.0520(18) 0.0338(14) -0.0155(12) -0.0032(13) 0.0328(16) C20 0.0480(17) 0.0266(15) 0.073(2) -0.0152(14) -0.0087(15) 0.0082(13) C21 0.0457(16) 0.0329(14) 0.0359(13) -0.0020(11) -0.0014(11) 0.0157(13) C22 0.0580(18) 0.0403(16) 0.0357(14) -0.0029(12) 0.0043(12) 0.0214(15) C23 0.0592(19) 0.0438(17) 0.0420(15) 0.0044(13) 0.0186(13) 0.0198(15) C24 0.0424(16) 0.0351(15) 0.0476(16) 0.0068(12) 0.0124(12) 0.0110(13) C25 0.0364(14) 0.0290(14) 0.0378(13) 0.0037(11) 0.0010(11) 0.0133(12) C26 0.0275(13) 0.0297(14) 0.0439(14) 0.0028(11) -0.0011(11) 0.0096(12) C27 0.0297(14) 0.0381(15) 0.0391(14) 0.0020(11) 0.0007(11) 0.0102(12) C28 0.0368(15) 0.0426(17) 0.0453(15) -0.0072(13) -0.0031(12) 0.0158(13) C29 0.0348(15) 0.0267(14) 0.0629(18) -0.0044(13) -0.0030(13) 0.0098(12) C30 0.0380(15) 0.0287(15) 0.0589(17) 0.0029(13) 0.0076(13) 0.0065(13) O1 0.0283(9) 0.0254(9) 0.0306(8) -0.0068(7) -0.0100(7) 0.0107(8) O2 0.0318(9) 0.0314(9) 0.0284(8) -0.0106(7) -0.0110(7) 0.0188(8) O3 0.0290(9) 0.0263(9) 0.0261(8) -0.0086(6) -0.0077(6) 0.0146(7) O4 0.0315(9) 0.0226(8) 0.0317(8) -0.0068(7) -0.0081(7) 0.0112(7) N1 0.0346(12) 0.0280(11) 0.0315(10) -0.0002(9) 0.0002(9) 0.0081(10) N2 0.0438(14) 0.0316(13) 0.0360(12) 0.0009(10) 0.0022(10) -0.0022(11) N3 0.0397(13) 0.0319(13) 0.0521(14) 0.0034(10) 0.0091(10) 0.0065(11) Cu1 0.02453(17) 0.02124(17) 0.02410(15) -0.00618(10) -0.00699(10) 0.00965(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A C4 1.570(7) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C2A C4 1.492(6) . ? C2A H2A1 0.9600 . ? C2A H2A2 0.9600 . ? C2A H2A3 0.9600 . ? C3A C4 1.509(6) . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? C1 C4 1.510(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.573(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.548(6) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.541(3) . ? C5 O1 1.264(3) . ? C5 C6 1.395(3) . ? C6 C7 1.391(3) . ? C6 H6 0.9300 . ? C7 O2 1.271(3) . ? C7 C8 1.500(3) . ? C8 C13 1.388(3) . ? C8 C9 1.389(3) . ? C9 C10 1.380(4) . ? C9 H9 0.9300 . ? C10 C11 1.381(4) . ? C10 H10 0.9300 . ? C11 C12 1.388(3) . ? C11 H11 0.9300 . ? C12 C13 1.392(3) . ? C12 C14 1.500(3) . ? C13 H13 0.9300 . ? C14 O3 1.279(3) . ? C14 C15 1.389(3) . ? C15 C16 1.400(3) . ? C15 H15 0.9300 . ? C16 O4 1.266(3) . ? C16 C17 1.536(3) . ? C17 C18 1.524(4) . ? C17 C20 1.529(4) . ? C17 C19 1.531(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N1 1.346(3) . ? C21 C22 1.359(4) . ? C21 H21 0.9300 . ? C22 C23 1.373(4) . ? C22 H22 0.9300 . ? C23 C24 1.372(4) . ? C23 H23 0.9300 . ? C24 C25 1.394(4) . ? C24 H24 0.9300 . ? C25 N1 1.337(3) . ? C25 N2 1.376(3) . ? C26 N3 1.325(3) . ? C26 C27 1.394(4) . ? C26 N2 1.395(3) . ? C27 C28 1.366(4) . ? C27 H27 0.9300 . ? C28 C29 1.387(4) . ? C28 H28 0.9300 . ? C29 C30 1.355(4) . ? C29 H29 0.9300 . ? C30 N3 1.342(3) . ? C30 H30 0.9300 . ? O1 Cu1 1.9288(15) . ? O2 Cu1 1.9239(15) . ? O3 Cu1 1.9239(15) 2_677 ? O4 Cu1 1.9284(15) 2_677 ? N1 Cu1 2.352(2) . ? N2 H1N 0.87(3) . ? Cu1 O3 1.9239(15) 2_677 ? Cu1 O4 1.9283(15) 2_677 ? 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 C4 C1A H1A1 109.5 . . ? C4 C1A H1A2 109.5 . . ? C4 C1A H1A3 109.5 . . ? C4 C2A H2A1 109.5 . . ? C4 C2A H2A2 109.5 . . ? C4 C2A H2A3 109.5 . . ? C4 C3A H3A1 109.5 . . ? C4 C3A H3A2 109.5 . . ? C4 C3A H3A3 109.5 . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2A C4 C3A 89.0(4) . . ? C2A C4 C1 122.4(4) . . ? C3A C4 C1 111.0(4) . . ? C2A C4 C5 111.6(3) . . ? C3A C4 C5 105.3(3) . . ? C1 C4 C5 113.5(3) . . ? C2A C4 C3 112.2(4) . . ? C1 C4 C3 84.3(4) . . ? C5 C4 C3 109.2(3) . . ? C2A C4 C1A 108.7(4) . . ? C3A C4 C1A 131.8(4) . . ? C5 C4 C1A 108.5(3) . . ? C3 C4 C1A 106.4(4) . . ? C3A C4 C2 111.4(4) . . ? C1 C4 C2 106.9(4) . . ? C5 C4 C2 108.8(3) . . ? C3 C4 C2 131.3(4) . . ? C1A C4 C2 89.0(4) . . ? O1 C5 C6 124.7(2) . . ? O1 C5 C4 115.8(2) . . ? C6 C5 C4 119.4(2) . . ? C7 C6 C5 124.7(2) . . ? C7 C6 H6 117.7 . . ? C5 C6 H6 117.7 . . ? O2 C7 C6 124.9(2) . . ? O2 C7 C8 115.20(19) . . ? C6 C7 C8 119.9(2) . . ? C13 C8 C9 118.5(2) . . ? C13 C8 C7 118.2(2) . . ? C9 C8 C7 123.3(2) . . ? C10 C9 C8 120.2(2) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.6(2) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 118.2(2) . . ? C11 C12 C14 122.9(2) . . ? C13 C12 C14 118.8(2) . . ? C8 C13 C12 121.9(2) . . ? C8 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? O3 C14 C15 124.9(2) . . ? O3 C14 C12 114.49(19) . . ? C15 C14 C12 120.6(2) . . ? C14 C15 C16 124.9(2) . . ? C14 C15 H15 117.6 . . ? C16 C15 H15 117.6 . . ? O4 C16 C15 124.4(2) . . ? O4 C16 C17 114.42(19) . . ? C15 C16 C17 121.1(2) . . ? C18 C17 C20 110.0(2) . . ? C18 C17 C19 109.7(2) . . ? C20 C17 C19 108.4(2) . . ? C18 C17 C16 113.8(2) . . ? C20 C17 C16 108.6(2) . . ? C19 C17 C16 106.1(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 123.9(2) . . ? N1 C21 H21 118.0 . . ? C22 C21 H21 118.0 . . ? C21 C22 C23 117.3(3) . . ? C21 C22 H22 121.3 . . ? C23 C22 H22 121.3 . . ? C24 C23 C22 120.8(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 118.3(3) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? N1 C25 N2 113.5(2) . . ? N1 C25 C24 121.5(2) . . ? N2 C25 C24 125.0(2) . . ? N3 C26 C27 122.8(2) . . ? N3 C26 N2 119.0(2) . . ? C27 C26 N2 118.2(2) . . ? C28 C27 C26 118.9(2) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C29 118.8(3) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C30 C29 C28 118.1(2) . . ? C30 C29 H29 121.0 . . ? C28 C29 H29 121.0 . . ? N3 C30 C29 124.6(3) . . ? N3 C30 H30 117.7 . . ? C29 C30 H30 117.7 . . ? C5 O1 Cu1 125.65(14) . . ? C7 O2 Cu1 125.87(14) . . ? C14 O3 Cu1 125.83(14) . 2_677 ? C16 O4 Cu1 126.58(14) . 2_677 ? C25 N1 C21 118.2(2) . . ? C25 N1 Cu1 130.08(16) . . ? C21 N1 Cu1 111.70(16) . . ? C25 N2 C26 130.2(2) . . ? C25 N2 H1N 114(2) . . ? C26 N2 H1N 115(2) . . ? C26 N3 C30 116.7(2) . . ? O3 Cu1 O2 85.95(6) 2_677 . ? O3 Cu1 O4 92.76(6) 2_677 2_677 ? O2 Cu1 O4 165.68(7) . 2_677 ? O3 Cu1 O1 176.73(7) 2_677 . ? O2 Cu1 O1 92.69(7) . . ? O4 Cu1 O1 87.83(7) 2_677 . ? O3 Cu1 N1 92.95(7) 2_677 . ? O2 Cu1 N1 101.95(7) . . ? O4 Cu1 N1 92.36(7) 2_677 . ? O1 Cu1 N1 90.24(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A C4 C5 O1 6.8(4) . . . . ? C3A C4 C5 O1 -88.3(4) . . . . ? C1 C4 C5 O1 150.1(3) . . . . ? C3 C4 C5 O1 -117.8(3) . . . . ? C1A C4 C5 O1 126.6(3) . . . . ? C2 C4 C5 O1 31.2(4) . . . . ? C2A C4 C5 C6 -174.5(3) . . . . ? C3A C4 C5 C6 90.4(4) . . . . ? C1 C4 C5 C6 -31.2(4) . . . . ? C3 C4 C5 C6 60.9(4) . . . . ? C1A C4 C5 C6 -54.7(4) . . . . ? C2 C4 C5 C6 -150.1(3) . . . . ? O1 C5 C6 C7 0.3(4) . . . . ? C4 C5 C6 C7 -178.2(2) . . . . ? C5 C6 C7 O2 5.3(4) . . . . ? C5 C6 C7 C8 -175.5(2) . . . . ? O2 C7 C8 C13 13.0(3) . . . . ? C6 C7 C8 C13 -166.3(2) . . . . ? O2 C7 C8 C9 -166.6(2) . . . . ? C6 C7 C8 C9 14.1(4) . . . . ? C13 C8 C9 C10 1.1(4) . . . . ? C7 C8 C9 C10 -179.3(3) . . . . ? C8 C9 C10 C11 0.3(5) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? C10 C11 C12 C14 -178.5(3) . . . . ? C9 C8 C13 C12 -2.2(4) . . . . ? C7 C8 C13 C12 178.2(2) . . . . ? C11 C12 C13 C8 1.8(4) . . . . ? C14 C12 C13 C8 -179.9(2) . . . . ? C11 C12 C14 O3 167.9(2) . . . . ? C13 C12 C14 O3 -10.3(3) . . . . ? C11 C12 C14 C15 -12.0(4) . . . . ? C13 C12 C14 C15 169.7(2) . . . . ? O3 C14 C15 C16 -3.1(4) . . . . ? C12 C14 C15 C16 176.9(2) . . . . ? C14 C15 C16 O4 2.0(4) . . . . ? C14 C15 C16 C17 -174.9(2) . . . . ? O4 C16 C17 C18 168.1(2) . . . . ? C15 C16 C17 C18 -14.7(3) . . . . ? O4 C16 C17 C20 45.2(3) . . . . ? C15 C16 C17 C20 -137.6(2) . . . . ? O4 C16 C17 C19 -71.2(3) . . . . ? C15 C16 C17 C19 106.0(3) . . . . ? N1 C21 C22 C23 1.2(4) . . . . ? C21 C22 C23 C24 -1.0(4) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C23 C24 C25 N1 1.3(4) . . . . ? C23 C24 C25 N2 180.0(3) . . . . ? N3 C26 C27 C28 3.0(4) . . . . ? N2 C26 C27 C28 -176.3(2) . . . . ? C26 C27 C28 C29 -2.1(4) . . . . ? C27 C28 C29 C30 -0.4(4) . . . . ? C28 C29 C30 N3 2.4(5) . . . . ? C6 C5 O1 Cu1 -11.6(3) . . . . ? C4 C5 O1 Cu1 167.01(15) . . . . ? C6 C7 O2 Cu1 1.3(3) . . . . ? C8 C7 O2 Cu1 -177.93(14) . . . . ? C15 C14 O3 Cu1 7.5(3) . . . 2_677 ? C12 C14 O3 Cu1 -172.43(14) . . . 2_677 ? C15 C16 O4 Cu1 -5.5(3) . . . 2_677 ? C17 C16 O4 Cu1 171.55(15) . . . 2_677 ? N2 C25 N1 C21 -179.9(2) . . . . ? C24 C25 N1 C21 -1.1(4) . . . . ? N2 C25 N1 Cu1 -3.2(3) . . . . ? C24 C25 N1 Cu1 175.60(19) . . . . ? C22 C21 N1 C25 -0.2(4) . . . . ? C22 C21 N1 Cu1 -177.5(2) . . . . ? N1 C25 N2 C26 -161.1(3) . . . . ? C24 C25 N2 C26 20.1(5) . . . . ? N3 C26 N2 C25 -13.4(4) . . . . ? C27 C26 N2 C25 166.0(3) . . . . ? C27 C26 N3 C30 -1.1(4) . . . . ? N2 C26 N3 C30 178.2(2) . . . . ? C29 C30 N3 C26 -1.6(4) . . . . ? C7 O2 Cu1 O3 174.49(19) . . . 2_677 ? C7 O2 Cu1 O4 -100.2(3) . . . 2_677 ? C7 O2 Cu1 O1 -8.49(19) . . . . ? C7 O2 Cu1 N1 82.33(19) . . . . ? C5 O1 Cu1 O2 13.50(19) . . . . ? C5 O1 Cu1 O4 179.18(18) . . . 2_677 ? C5 O1 Cu1 N1 -88.47(18) . . . . ? C25 N1 Cu1 O3 -39.7(2) . . . 2_677 ? C21 N1 Cu1 O3 137.23(18) . . . 2_677 ? C25 N1 Cu1 O2 46.8(2) . . . . ? C21 N1 Cu1 O2 -136.29(17) . . . . ? C25 N1 Cu1 O4 -132.6(2) . . . 2_677 ? C21 N1 Cu1 O4 44.34(18) . . . 2_677 ? C25 N1 Cu1 O1 139.6(2) . . . . ? C21 N1 Cu1 O1 -43.50(18) . . . . ? _diffrn_measured_fraction_theta_max 0.791 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.651 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.050 # Attachment 'Cu dpsNew.cif' data_lj68sad _database_code_depnum_ccdc_archive 'CCDC 606854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H56 Cu2 N2 O8 S, 2(C4 H8 O)' _chemical_formula_sum 'C58 H72 Cu2 N2 O10 S' _chemical_formula_weight 1116.32 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4190(9) _cell_length_b 15.5925(14) _cell_length_c 18.4105(16) _cell_angle_alpha 99.2710(10) _cell_angle_beta 102.7000(10) _cell_angle_gamma 90.1040(10) _cell_volume 2877.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7245 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.45 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 143 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.21 _diffrn_reflns_number 27969 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.36 _reflns_number_total 13270 _reflns_number_gt 8541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.0867P)^2^+5.0591P] 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 13270 _refine_ls_number_parameters 618 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1988 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.025 _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 C1A C 0.0012(9) -0.2181(6) 0.1036(5) 0.0446(7) Uiso 0.50 1 d PD A 1 H1A1 H -0.0439 -0.1635 0.1118 0.067 Uiso 0.50 1 calc PR A 1 H1A2 H -0.0287 -0.2462 0.0509 0.067 Uiso 0.50 1 calc PR A 1 H1A3 H 0.0965 -0.2060 0.1147 0.067 Uiso 0.50 1 calc PR A 1 C2A C 0.0685(10) -0.3527(6) 0.1571(6) 0.0446(7) Uiso 0.50 1 d PD A 1 H2A1 H 0.0463 -0.3934 0.1093 0.067 Uiso 0.50 1 calc PR A 1 H2A2 H 0.0627 -0.3833 0.1988 0.067 Uiso 0.50 1 calc PR A 1 H2A3 H 0.1582 -0.3286 0.1646 0.067 Uiso 0.50 1 calc PR A 1 C3A C -0.1627(9) -0.3315(6) 0.1265(6) 0.0446(7) Uiso 0.50 1 d PD A 1 H3A1 H -0.2356 -0.2921 0.1179 0.067 Uiso 0.50 1 calc PR A 1 H3A2 H -0.1746 -0.3662 0.1646 0.067 Uiso 0.50 1 calc PR A 1 H3A3 H -0.1613 -0.3703 0.0792 0.067 Uiso 0.50 1 calc PR A 1 C4A C -0.0300(12) -0.2775(8) 0.1547(7) 0.0446(7) Uiso 0.50 1 d PD A 1 C1B C -0.0491(9) -0.2010(6) 0.1013(5) 0.0446(7) Uiso 0.50 1 d PD A 2 H1B1 H 0.0386 -0.1742 0.1075 0.067 Uiso 0.50 1 calc PR A 2 H1B2 H -0.1096 -0.1562 0.1150 0.067 Uiso 0.50 1 calc PR A 2 H1B3 H -0.0814 -0.2285 0.0486 0.067 Uiso 0.50 1 calc PR A 2 C2B C 0.0629(10) -0.3328(6) 0.1421(6) 0.0446(7) Uiso 0.50 1 d PD A 2 H2B1 H 0.1481 -0.3013 0.1517 0.067 Uiso 0.50 1 calc PR A 2 H2B2 H 0.0419 -0.3646 0.0903 0.067 Uiso 0.50 1 calc PR A 2 H2B3 H 0.0674 -0.3739 0.1776 0.067 Uiso 0.50 1 calc PR A 2 C3B C -0.1816(9) -0.3112(6) 0.1266(6) 0.0446(7) Uiso 0.50 1 d PD A 2 H3B1 H -0.1956 -0.3399 0.0739 0.067 Uiso 0.50 1 calc PR A 2 H3B2 H -0.2459 -0.2659 0.1309 0.067 Uiso 0.50 1 calc PR A 2 H3B3 H -0.1925 -0.3541 0.1585 0.067 Uiso 0.50 1 calc PR A 2 C4B C -0.0413(12) -0.2697(8) 0.1526(7) 0.0446(7) Uiso 0.50 1 d PD A 2 C5 C -0.0177(4) -0.2294(2) 0.23593(19) 0.0315(8) Uani 1 1 d D . . C6 C 0.0764(4) -0.1625(2) 0.2674(2) 0.0321(8) Uani 1 1 d . A . H6 H 0.1289 -0.1452 0.2358 0.039 Uiso 1 1 calc R . . C7 C 0.0997(4) -0.1190(2) 0.3417(2) 0.0284(8) Uani 1 1 d . . . C8 C 0.2108(4) -0.0529(2) 0.37128(19) 0.0257(7) Uani 1 1 d . A . C9 C 0.3203(4) -0.0508(3) 0.3394(2) 0.0352(9) Uani 1 1 d . . . H9 H 0.3257 -0.0922 0.2963 0.042 Uiso 1 1 calc R A . C10 C 0.4207(4) 0.0111(3) 0.3701(2) 0.0429(10) Uani 1 1 d . A . H10 H 0.4947 0.0121 0.3479 0.051 Uiso 1 1 calc R . . C11 C 0.4145(4) 0.0716(3) 0.4326(2) 0.0384(9) Uani 1 1 d . . . H11 H 0.4841 0.1141 0.4530 0.046 Uiso 1 1 calc R A . C12 C 0.3069(4) 0.0711(2) 0.4663(2) 0.0276(7) Uani 1 1 d . A . C13 C 0.2070(3) 0.0078(2) 0.43502(19) 0.0261(7) Uani 1 1 d . . . H13 H 0.1339 0.0061 0.4579 0.031 Uiso 1 1 calc R A . C14 C 0.2924(4) 0.1360(2) 0.5333(2) 0.0296(8) Uani 1 1 d . . . C15 C 0.3964(4) 0.1929(3) 0.5724(2) 0.0362(9) Uani 1 1 d . A . H15 H 0.4765 0.1887 0.5556 0.043 Uiso 1 1 calc R . . C16 C 0.3914(4) 0.2564(2) 0.6351(2) 0.0337(8) Uani 1 1 d . . . C17 C 0.5103(4) 0.3128(3) 0.6790(3) 0.0520(12) Uani 1 1 d . A . C18 C 0.6297(5) 0.3013(4) 0.6472(4) 0.0671(16) Uani 1 1 d . . . H18A H 0.6510 0.2397 0.6408 0.101 Uiso 1 1 calc R A . H18B H 0.7038 0.3357 0.6817 0.101 Uiso 1 1 calc R . . H18C H 0.6131 0.3208 0.5981 0.101 Uiso 1 1 calc R . . C19 C 0.4725(5) 0.4055(3) 0.6940(4) 0.0715(18) Uani 1 1 d . . . H19A H 0.5458 0.4401 0.7291 0.107 Uiso 1 1 calc R A . H19B H 0.3950 0.4086 0.7162 0.107 Uiso 1 1 calc R . . H19C H 0.4520 0.4286 0.6465 0.107 Uiso 1 1 calc R . . C20 C 0.5439(6) 0.2833(4) 0.7586(3) 0.0764(18) Uani 1 1 d . . . H20A H 0.5669 0.2221 0.7527 0.115 Uiso 1 1 calc R A . H20B H 0.4672 0.2905 0.7814 0.115 Uiso 1 1 calc R . . H20C H 0.6185 0.3190 0.7912 0.115 Uiso 1 1 calc R . . C21A C 0.0875(12) 0.1147(8) 0.2282(6) 0.0750(12) Uiso 0.50 1 d PD B 1 H21A H -0.0088 0.1104 0.2123 0.113 Uiso 0.50 1 calc PR B 1 H21B H 0.1144 0.1685 0.2643 0.113 Uiso 0.50 1 calc PR B 1 H21C H 0.1189 0.0647 0.2523 0.113 Uiso 0.50 1 calc PR B 1 C22A C 0.0896(12) 0.0423(7) 0.0947(6) 0.0750(12) Uiso 0.50 1 d PD B 1 H22A H 0.1123 -0.0139 0.1103 0.113 Uiso 0.50 1 calc PR B 1 H22B H 0.1269 0.0484 0.0513 0.113 Uiso 0.50 1 calc PR B 1 H22C H -0.0063 0.0457 0.0807 0.113 Uiso 0.50 1 calc PR B 1 C23A C 0.2921(10) 0.0996(9) 0.1770(8) 0.0750(12) Uiso 0.50 1 d PD B 1 H23A H 0.3059 0.0395 0.1855 0.113 Uiso 0.50 1 calc PR B 1 H23B H 0.3362 0.1397 0.2223 0.113 Uiso 0.50 1 calc PR B 1 H23C H 0.3286 0.1092 0.1342 0.113 Uiso 0.50 1 calc PR B 1 C24A C 0.1459(12) 0.1156(7) 0.1601(6) 0.0750(12) Uiso 0.50 1 d PD B 1 C21B C 0.1251(13) 0.1569(8) 0.2630(6) 0.0750(12) Uiso 0.50 1 d PD B 2 H21D H 0.1475 0.1092 0.2916 0.113 Uiso 0.50 1 calc PR B 2 H21E H 0.0307 0.1670 0.2564 0.113 Uiso 0.50 1 calc PR B 2 H21F H 0.1754 0.2099 0.2906 0.113 Uiso 0.50 1 calc PR B 2 C22B C 0.0760(11) 0.0523(7) 0.1428(7) 0.0750(12) Uiso 0.50 1 d PD B 2 H22D H 0.0597 0.0529 0.0884 0.113 Uiso 0.50 1 calc PR B 2 H22E H -0.0081 0.0518 0.1582 0.113 Uiso 0.50 1 calc PR B 2 H22F H 0.1234 0.0002 0.1543 0.113 Uiso 0.50 1 calc PR B 2 C23B C 0.3057(10) 0.1179(9) 0.1984(8) 0.0750(12) Uiso 0.50 1 d PD B 2 H23D H 0.3309 0.1052 0.1496 0.113 Uiso 0.50 1 calc PR B 2 H23E H 0.3258 0.0685 0.2253 0.113 Uiso 0.50 1 calc PR B 2 H23F H 0.3549 0.1700 0.2285 0.113 Uiso 0.50 1 calc PR B 2 C24B C 0.1588(12) 0.1332(8) 0.1854(6) 0.0750(12) Uiso 0.50 1 d PD B 2 C25 C 0.1138(6) 0.2055(3) 0.1359(3) 0.0598(14) Uani 1 1 d D . . C26 C 0.2065(6) 0.2658(3) 0.1307(3) 0.0564(13) Uani 1 1 d . B . H26 H 0.2965 0.2538 0.1477 0.068 Uiso 1 1 calc R . . C27 C 0.1788(5) 0.3431(3) 0.1025(2) 0.0404(10) Uani 1 1 d . . . C28 C 0.2887(4) 0.4045(3) 0.1002(2) 0.0388(9) Uani 1 1 d . B . C29 C 0.4214(5) 0.3918(3) 0.1260(3) 0.0520(12) Uani 1 1 d . . . H29 H 0.4472 0.3420 0.1485 0.062 Uiso 1 1 calc R B . C30 C 0.5161(5) 0.4495(4) 0.1199(3) 0.0593(13) Uani 1 1 d . B . H30 H 0.6065 0.4386 0.1372 0.071 Uiso 1 1 calc R . . C31 C 0.4815(5) 0.5233(3) 0.0888(3) 0.0469(11) Uani 1 1 d . . . H31 H 0.5477 0.5635 0.0853 0.056 Uiso 1 1 calc R B . C32 C 0.3484(4) 0.5384(3) 0.0623(2) 0.0375(9) Uani 1 1 d . B . C33 C 0.2538(4) 0.4791(2) 0.0679(2) 0.0342(9) Uani 1 1 d . . . H33 H 0.1634 0.4890 0.0496 0.041 Uiso 1 1 calc R B . C34 C 0.3037(4) 0.6161(3) 0.0265(2) 0.0373(9) Uani 1 1 d . . . C35 C 0.3864(5) 0.6899(3) 0.0390(3) 0.0601(14) Uani 1 1 d . B . H35 H 0.4719 0.6892 0.0702 0.072 Uiso 1 1 calc R . . C36 C 0.3497(6) 0.7659(3) 0.0075(4) 0.0623(15) Uani 1 1 d D . . C37A C 0.4517(13) 0.8471(9) 0.0356(7) 0.0897(14) Uiso 0.50 1 d PD B 1 C38A C 0.3744(13) 0.9272(7) 0.0104(8) 0.0897(14) Uiso 0.50 1 d PD B 1 H38A H 0.3066 0.9405 0.0394 0.135 Uiso 0.50 1 calc PR B 1 H38B H 0.3327 0.9136 -0.0435 0.135 Uiso 0.50 1 calc PR B 1 H38C H 0.4355 0.9776 0.0193 0.135 Uiso 0.50 1 calc PR B 1 C39A C 0.5576(12) 0.8307(9) -0.0101(8) 0.0897(14) Uiso 0.50 1 d PD B 1 H39A H 0.6112 0.8842 -0.0038 0.135 Uiso 0.50 1 calc PR B 1 H39B H 0.5157 0.8128 -0.0636 0.135 Uiso 0.50 1 calc PR B 1 H39C H 0.6139 0.7847 0.0078 0.135 Uiso 0.50 1 calc PR B 1 C40A C 0.5072(13) 0.8621(9) 0.1172(6) 0.0897(14) Uiso 0.50 1 d PD B 1 H40A H 0.5516 0.8101 0.1318 0.135 Uiso 0.50 1 calc PR B 1 H40B H 0.4364 0.8748 0.1442 0.135 Uiso 0.50 1 calc PR B 1 H40C H 0.5709 0.9116 0.1303 0.135 Uiso 0.50 1 calc PR B 1 C37B C 0.4426(13) 0.8444(9) 0.0145(7) 0.0897(14) Uiso 0.50 1 d PD B 2 C38B C 0.4300(13) 0.8741(9) -0.0629(6) 0.0897(14) Uiso 0.50 1 d PD B 2 H38D H 0.4850 0.9270 -0.0566 0.135 Uiso 0.50 1 calc PR B 2 H38E H 0.3379 0.8860 -0.0832 0.135 Uiso 0.50 1 calc PR B 2 H38F H 0.4592 0.8281 -0.0979 0.135 Uiso 0.50 1 calc PR B 2 C39B C 0.5827(10) 0.8273(9) 0.0384(8) 0.0897(14) Uiso 0.50 1 d PD B 2 H39D H 0.6012 0.8158 0.0904 0.135 Uiso 0.50 1 calc PR B 2 H39E H 0.6359 0.8781 0.0357 0.135 Uiso 0.50 1 calc PR B 2 H39F H 0.6045 0.7766 0.0050 0.135 Uiso 0.50 1 calc PR B 2 C40B C 0.3946(13) 0.9154(8) 0.0704(7) 0.0897(14) Uiso 0.50 1 d PD B 2 H40D H 0.4063 0.8966 0.1196 0.135 Uiso 0.50 1 calc PR B 2 H40E H 0.3012 0.9248 0.0511 0.135 Uiso 0.50 1 calc PR B 2 H40F H 0.4458 0.9697 0.0758 0.135 Uiso 0.50 1 calc PR B 2 C100 C -0.0772(4) 0.3493(3) 0.5780(2) 0.0434(10) Uani 1 1 d . . . H100 H -0.1009 0.3450 0.6243 0.052 Uiso 1 1 calc R . . C101 C -0.1465(4) 0.4036(3) 0.5342(3) 0.0455(11) Uani 1 1 d . . . H101 H -0.2155 0.4360 0.5500 0.055 Uiso 1 1 calc R . . C102 C -0.1144(4) 0.4107(3) 0.4657(2) 0.0400(9) Uani 1 1 d . . . C103 C -0.0100(4) 0.3634(3) 0.4468(2) 0.0437(10) Uani 1 1 d . . . H103 H 0.0170 0.3675 0.4014 0.052 Uiso 1 1 calc R . . C104 C 0.0533(4) 0.3104(3) 0.4952(2) 0.0422(10) Uani 1 1 d . . . H104 H 0.1239 0.2780 0.4815 0.051 Uiso 1 1 calc R . . C105 C -0.1217(5) 0.4492(3) 0.2048(3) 0.0492(11) Uani 1 1 d . . . H105 H -0.0899 0.4848 0.1747 0.059 Uiso 1 1 calc R . . C106 C -0.1385(4) 0.4874(3) 0.2746(3) 0.0479(11) Uani 1 1 d . . . H106 H -0.1192 0.5477 0.2921 0.058 Uiso 1 1 calc R . . C107 C -0.1841(4) 0.4358(3) 0.3187(2) 0.0416(10) Uani 1 1 d . . . C108 C -0.2167(4) 0.3489(3) 0.2894(2) 0.0440(10) Uani 1 1 d . . . H108 H -0.2529 0.3125 0.3172 0.053 Uiso 1 1 calc R . . C109 C -0.1954(5) 0.3169(3) 0.2193(2) 0.0433(10) Uani 1 1 d . . . H109 H -0.2159 0.2570 0.1998 0.052 Uiso 1 1 calc R . . O1T O -0.3184(12) 0.1486(8) 0.3290(6) 0.0747(10) Uiso 0.45 1 d P C 1 C1T C -0.290(2) 0.0802(11) 0.2759(11) 0.0747(10) Uiso 0.45 1 d P C 1 H1T1 H -0.3734 0.0533 0.2438 0.090 Uiso 0.45 1 calc PR C 1 H1T2 H -0.2412 0.1047 0.2428 0.090 Uiso 0.45 1 calc PR C 1 C2T C -0.2197(15) 0.0193(10) 0.3052(8) 0.0747(10) Uiso 0.45 1 d P C 1 H2T1 H -0.1621 -0.0069 0.2721 0.090 Uiso 0.45 1 calc PR C 1 H2T2 H -0.2772 -0.0271 0.3135 0.090 Uiso 0.45 1 calc PR C 1 C3T C -0.1375(16) 0.0678(10) 0.3807(10) 0.0747(10) Uiso 0.45 1 d P C 1 H3T1 H -0.1118 0.0278 0.4176 0.090 Uiso 0.45 1 calc PR C 1 H3T2 H -0.0572 0.0961 0.3734 0.090 Uiso 0.45 1 calc PR C 1 C4T C -0.2290(19) 0.1341(11) 0.4064(10) 0.0747(10) Uiso 0.45 1 d P C 1 H4T1 H -0.1806 0.1884 0.4342 0.090 Uiso 0.45 1 calc PR C 1 H4T2 H -0.2812 0.1115 0.4386 0.090 Uiso 0.45 1 calc PR C 1 O2T O -0.3219(10) 0.1594(6) 0.3541(5) 0.0747(10) Uiso 0.55 1 d P D 2 C5T C -0.2983(17) 0.1009(9) 0.2893(9) 0.0747(10) Uiso 0.55 1 d P D 2 H5T1 H -0.2650 0.1325 0.2543 0.090 Uiso 0.55 1 calc PR D 2 H5T2 H -0.3784 0.0656 0.2617 0.090 Uiso 0.55 1 calc PR D 2 C6T C -0.1230(13) 0.1067(8) 0.3989(7) 0.0747(10) Uiso 0.55 1 d P D 2 H6T1 H -0.0597 0.1457 0.3856 0.090 Uiso 0.55 1 calc PR D 2 H6T2 H -0.0763 0.0786 0.4412 0.090 Uiso 0.55 1 calc PR D 2 C7T C -0.2387(15) 0.1577(9) 0.4202(8) 0.0747(10) Uiso 0.55 1 d P D 2 H7T1 H -0.2803 0.1279 0.4532 0.090 Uiso 0.55 1 calc PR D 2 H7T2 H -0.2094 0.2173 0.4464 0.090 Uiso 0.55 1 calc PR D 2 C8T C -0.1830(13) 0.0403(9) 0.3326(8) 0.0747(10) Uiso 0.55 1 d P D 2 H8T1 H -0.2217 -0.0103 0.3476 0.090 Uiso 0.55 1 calc PR D 2 H8T2 H -0.1193 0.0203 0.3013 0.090 Uiso 0.55 1 calc PR D 2 C9T C 0.489(2) 0.3524(13) 0.4159(11) 0.0850(11) Uiso 0.40 1 d P E 1 H9T1 H 0.4933 0.2914 0.4249 0.102 Uiso 0.40 1 calc PR E 1 H9T2 H 0.5790 0.3788 0.4319 0.102 Uiso 0.40 1 calc PR E 1 C10T C 0.4120(19) 0.3959(12) 0.4583(11) 0.0850(11) Uiso 0.40 1 d P E 1 H10A H 0.4655 0.4415 0.4968 0.102 Uiso 0.40 1 calc PR E 1 H10B H 0.3732 0.3555 0.4847 0.102 Uiso 0.40 1 calc PR E 1 O3T O 0.3138(12) 0.4332(8) 0.4123(7) 0.0850(11) Uiso 0.40 1 d P E 1 C11T C 0.293(2) 0.3854(14) 0.3219(12) 0.0850(11) Uiso 0.40 1 d P E 1 H11A H 0.2252 0.3372 0.3072 0.102 Uiso 0.40 1 calc PR E 1 H11B H 0.2758 0.4269 0.2858 0.102 Uiso 0.40 1 calc PR E 1 C12T C 0.441(3) 0.353(2) 0.3374(19) 0.0850(11) Uiso 0.40 1 d P E 1 H12A H 0.4434 0.2938 0.3088 0.102 Uiso 0.40 1 calc PR E 1 H12B H 0.4981 0.3924 0.3199 0.102 Uiso 0.40 1 calc PR E 1 O4T O 0.2669(8) 0.3966(5) 0.3963(5) 0.0850(11) Uiso 0.60 1 d P F 2 C13T C 0.3654(12) 0.3558(8) 0.4437(7) 0.0850(11) Uiso 0.60 1 d P F 2 H13A H 0.4098 0.3988 0.4877 0.102 Uiso 0.60 1 calc PR F 2 H13B H 0.3244 0.3090 0.4625 0.102 Uiso 0.60 1 calc PR F 2 C14T C 0.3073(16) 0.4087(9) 0.3371(9) 0.0850(11) Uiso 0.60 1 d P F 2 H14A H 0.3265 0.4716 0.3404 0.102 Uiso 0.60 1 calc PR F 2 H14B H 0.2357 0.3903 0.2919 0.102 Uiso 0.60 1 calc PR F 2 C15T C 0.4588(13) 0.3203(8) 0.4034(8) 0.0850(11) Uiso 0.60 1 d P F 2 H15A H 0.4492 0.2561 0.3923 0.102 Uiso 0.60 1 calc PR F 2 H15B H 0.5496 0.3374 0.4322 0.102 Uiso 0.60 1 calc PR F 2 C16T C 0.426(2) 0.3609(16) 0.3275(13) 0.0850(11) Uiso 0.60 1 d P F 2 H16A H 0.4980 0.4004 0.3243 0.102 Uiso 0.60 1 calc PR F 2 H16B H 0.4068 0.3151 0.2822 0.102 Uiso 0.60 1 calc PR F 2 N1 N 0.0219(3) 0.3017(2) 0.56051(19) 0.0369(8) Uani 1 1 d . A . N2 N -0.1473(4) 0.3655(2) 0.1769(2) 0.0435(9) Uani 1 1 d . B . O1 O -0.0902(3) -0.2603(2) 0.27257(16) 0.0508(8) Uani 1 1 d . . . O2 O 0.0319(3) -0.13024(18) 0.38893(15) 0.0407(7) Uani 1 1 d . . . O3 O 0.1798(3) 0.13368(18) 0.54929(15) 0.0390(7) Uani 1 1 d . A . O4 O 0.2901(3) 0.27054(19) 0.66218(16) 0.0425(7) Uani 1 1 d . A . O5 O -0.0091(4) 0.2107(2) 0.1134(2) 0.0635(10) Uani 1 1 d . B . O6 O 0.0637(3) 0.36740(19) 0.07773(18) 0.0460(8) Uani 1 1 d . B . O7 O 0.1882(3) 0.60912(18) -0.01321(16) 0.0405(7) Uani 1 1 d . . . O8 O 0.2458(4) 0.7766(2) -0.0343(2) 0.0664(10) Uani 1 1 d . . . S1 S -0.20323(12) 0.48236(8) 0.40995(7) 0.0524(3) Uani 1 1 d . . . Cu1 Cu 0.12322(5) 0.20649(3) 0.63114(3) 0.03723(15) Uani 1 1 d . . . Cu2 Cu -0.09934(6) 0.30356(3) 0.06715(3) 0.04813(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C5 0.040(2) 0.0304(19) 0.0245(18) 0.0017(14) 0.0111(16) 0.0043(16) C6 0.041(2) 0.035(2) 0.0237(18) 0.0034(15) 0.0155(16) 0.0003(16) C7 0.037(2) 0.0251(17) 0.0273(18) 0.0067(14) 0.0153(16) 0.0048(15) C8 0.0317(19) 0.0248(17) 0.0233(17) 0.0061(13) 0.0100(14) 0.0043(14) C9 0.040(2) 0.036(2) 0.032(2) -0.0013(16) 0.0177(17) 0.0033(17) C10 0.038(2) 0.049(3) 0.045(2) -0.0040(19) 0.025(2) -0.0032(19) C11 0.033(2) 0.040(2) 0.042(2) -0.0035(18) 0.0148(18) -0.0041(17) C12 0.0322(19) 0.0278(18) 0.0245(17) 0.0055(14) 0.0090(15) 0.0036(15) C13 0.0303(18) 0.0266(17) 0.0251(17) 0.0067(14) 0.0123(15) 0.0039(14) C14 0.037(2) 0.0277(18) 0.0258(18) 0.0055(14) 0.0094(16) 0.0029(15) C15 0.031(2) 0.034(2) 0.040(2) -0.0023(17) 0.0077(17) 0.0014(16) C16 0.033(2) 0.0304(19) 0.032(2) 0.0002(15) -0.0013(16) 0.0028(16) C17 0.032(2) 0.051(3) 0.059(3) -0.020(2) 0.001(2) 0.0036(19) C18 0.035(3) 0.061(3) 0.093(4) -0.021(3) 0.013(3) -0.012(2) C19 0.045(3) 0.038(3) 0.122(5) -0.016(3) 0.021(3) -0.005(2) C20 0.069(4) 0.098(5) 0.049(3) -0.006(3) -0.002(3) 0.019(3) C25 0.079(4) 0.050(3) 0.066(3) 0.034(3) 0.031(3) 0.030(3) C26 0.070(3) 0.048(3) 0.058(3) 0.030(2) 0.011(3) 0.019(2) C27 0.063(3) 0.037(2) 0.026(2) 0.0109(16) 0.0156(19) 0.020(2) C28 0.056(3) 0.038(2) 0.0245(19) 0.0079(16) 0.0110(18) 0.0160(19) C29 0.061(3) 0.048(3) 0.043(3) 0.015(2) -0.001(2) 0.017(2) C30 0.051(3) 0.067(3) 0.052(3) 0.005(2) -0.001(2) 0.016(3) C31 0.048(3) 0.047(3) 0.041(2) -0.001(2) 0.005(2) 0.004(2) C32 0.046(2) 0.038(2) 0.028(2) -0.0010(16) 0.0110(18) 0.0074(18) C33 0.044(2) 0.036(2) 0.0232(18) 0.0056(15) 0.0074(16) 0.0118(17) C34 0.046(2) 0.032(2) 0.040(2) 0.0023(17) 0.023(2) 0.0062(17) C35 0.046(3) 0.044(3) 0.089(4) 0.006(3) 0.015(3) 0.006(2) C36 0.072(4) 0.032(2) 0.095(4) 0.010(3) 0.044(3) 0.003(2) C100 0.040(2) 0.054(3) 0.038(2) 0.000(2) 0.0206(19) -0.006(2) C101 0.037(2) 0.056(3) 0.044(2) -0.004(2) 0.020(2) 0.002(2) C102 0.035(2) 0.045(2) 0.039(2) 0.0013(18) 0.0102(18) 0.0017(18) C103 0.041(2) 0.057(3) 0.039(2) 0.014(2) 0.0190(19) 0.006(2) C104 0.039(2) 0.053(3) 0.039(2) 0.0048(19) 0.0220(19) 0.0017(19) C105 0.050(3) 0.045(3) 0.059(3) 0.022(2) 0.017(2) -0.002(2) C106 0.045(3) 0.041(2) 0.057(3) 0.011(2) 0.008(2) -0.002(2) C107 0.036(2) 0.048(2) 0.041(2) 0.0084(19) 0.0073(19) 0.0084(19) C108 0.051(3) 0.046(2) 0.042(2) 0.0142(19) 0.019(2) 0.003(2) C109 0.056(3) 0.037(2) 0.042(2) 0.0147(18) 0.016(2) 0.0051(19) N1 0.0346(18) 0.0416(19) 0.0348(18) -0.0007(14) 0.0138(15) -0.0065(14) N2 0.053(2) 0.041(2) 0.045(2) 0.0208(16) 0.0182(18) 0.0102(17) O1 0.074(2) 0.0452(17) 0.0359(16) -0.0125(13) 0.0315(16) -0.0230(15) O2 0.0558(18) 0.0411(16) 0.0275(14) -0.0080(12) 0.0239(13) -0.0162(13) O3 0.0426(16) 0.0395(15) 0.0350(15) -0.0114(12) 0.0216(13) -0.0133(12) O4 0.0430(16) 0.0439(17) 0.0369(16) -0.0114(13) 0.0138(13) -0.0079(13) O5 0.082(3) 0.0466(19) 0.087(3) 0.0436(19) 0.048(2) 0.0240(18) O6 0.0553(19) 0.0399(16) 0.0566(19) 0.0303(14) 0.0252(16) 0.0181(14) O7 0.0514(18) 0.0363(15) 0.0400(16) 0.0197(12) 0.0136(14) 0.0028(13) O8 0.073(3) 0.046(2) 0.098(3) 0.034(2) 0.040(2) 0.0091(18) S1 0.0525(7) 0.0565(7) 0.0459(7) 0.0028(5) 0.0105(6) 0.0166(6) Cu1 0.0488(3) 0.0353(3) 0.0291(3) -0.00743(19) 0.0213(2) -0.0131(2) Cu2 0.0666(4) 0.0387(3) 0.0555(4) 0.0285(3) 0.0333(3) 0.0158(3) _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 C1A C4A 1.504(13) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C4A 1.559(12) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A C4A 1.559(13) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4A C5 1.539(12) . ? C1B C4B 1.529(12) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? C2B C4B 1.490(12) . ? C2B H2B1 0.9800 . ? C2B H2B2 0.9800 . ? C2B H2B3 0.9800 . ? C3B C4B 1.540(13) . ? C3B H3B1 0.9800 . ? C3B H3B2 0.9800 . ? C3B H3B3 0.9800 . ? C4B C5 1.528(12) . ? C5 O1 1.259(4) . ? C5 C6 1.392(5) . ? C6 C7 1.394(5) . ? C6 H6 0.9500 . ? C7 O2 1.267(4) . ? C7 C8 1.495(5) . ? C8 C13 1.392(5) . ? C8 C9 1.395(5) . ? C9 C10 1.381(6) . ? C9 H9 0.9500 . ? C10 C11 1.380(6) . ? C10 H10 0.9500 . ? C11 C12 1.397(5) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 C14 1.499(5) . ? C13 H13 0.9500 . ? C14 O3 1.273(4) . ? C14 C15 1.389(5) . ? C15 C16 1.404(5) . ? C15 H15 0.9500 . ? C16 O4 1.269(5) . ? C16 C17 1.513(6) . ? C17 C18 1.487(7) . ? C17 C19 1.498(6) . ? C17 C20 1.572(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C24A 1.513(13) . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A C24A 1.529(12) . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A C24A 1.515(13) . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C24A C25 1.553(12) . ? C21B C24B 1.533(13) . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B C24B 1.527(13) . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B C24B 1.522(13) . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24B C25 1.570(12) . ? C25 O5 1.264(6) . ? C25 C26 1.375(7) . ? C26 C27 1.395(6) . ? C26 H26 0.9500 . ? C27 O6 1.267(5) . ? C27 C28 1.502(6) . ? C28 C29 1.385(6) . ? C28 C33 1.403(5) . ? C29 C30 1.369(7) . ? C29 H29 0.9500 . ? C30 C31 1.381(7) . ? C30 H30 0.9500 . ? C31 C32 1.399(6) . ? C31 H31 0.9500 . ? C32 C33 1.382(6) . ? C32 C34 1.498(6) . ? C33 H33 0.9500 . ? C34 O7 1.258(5) . ? C34 C35 1.394(6) . ? C35 C36 1.419(7) . ? C35 H35 0.9500 . ? C36 O8 1.211(7) . ? C36 C37B 1.530(13) . ? C36 C37A 1.594(13) . ? C37A C40A 1.467(13) . ? C37A C39A 1.527(14) . ? C37A C38A 1.566(14) . ? C38A H38A 0.9800 . ? C38A H38B 0.9800 . ? C38A H38C 0.9800 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? C40A H40A 0.9800 . ? C40A H40B 0.9800 . ? C40A H40C 0.9800 . ? C37B C39B 1.466(14) . ? C37B C38B 1.546(14) . ? C37B C40B 1.549(14) . ? C38B H38D 0.9800 . ? C38B H38E 0.9800 . ? C38B H38F 0.9800 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? C40B H40D 0.9800 . ? C40B H40E 0.9800 . ? C40B H40F 0.9800 . ? C100 N1 1.340(5) . ? C100 C101 1.361(7) . ? C100 H100 0.9500 . ? C101 C102 1.396(6) . ? C101 H101 0.9500 . ? C102 C103 1.390(6) . ? C102 S1 1.764(5) . ? C103 C104 1.376(6) . ? C103 H103 0.9500 . ? C104 N1 1.340(5) . ? C104 H104 0.9500 . ? C105 N2 1.327(6) . ? C105 C106 1.375(7) . ? C105 H105 0.9500 . ? C106 C107 1.382(6) . ? C106 H106 0.9500 . ? C107 C108 1.388(6) . ? C107 S1 1.773(4) . ? C108 C109 1.372(6) . ? C108 H108 0.9500 . ? C109 N2 1.341(5) . ? C109 H109 0.9500 . ? O1T C1T 1.406(18) . ? O1T C4T 1.57(2) . ? C1T C2T 1.31(2) . ? C1T H1T1 0.9900 . ? C1T H1T2 0.9900 . ? C2T C3T 1.54(2) . ? C2T H2T1 0.9900 . ? C2T H2T2 0.9900 . ? C3T C4T 1.50(2) . ? C3T H3T1 0.9900 . ? C3T H3T2 0.9900 . ? C4T H4T1 0.9900 . ? C4T H4T2 0.9900 . ? O2T C7T 1.333(18) . ? O2T C5T 1.447(15) . ? C5T C8T 1.67(2) . ? C5T H5T1 0.9900 . ? C5T H5T2 0.9900 . ? C6T C8T 1.485(16) . ? C6T C7T 1.534(18) . ? C6T H6T1 0.9900 . ? C6T H6T2 0.9900 . ? C7T H7T1 0.9900 . ? C7T H7T2 0.9900 . ? C8T H8T1 0.9900 . ? C8T H8T2 0.9900 . ? C9T C10T 1.35(3) . ? C9T C12T 1.42(3) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? C10T O3T 1.37(2) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? O3T C11T 1.68(2) . ? C11T C12T 1.61(4) . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12A 0.9900 . ? C12T H12B 0.9900 . ? O4T C14T 1.293(17) . ? O4T C13T 1.416(14) . ? C13T C15T 1.410(17) . ? C13T H13A 0.9900 . ? C13T H13B 0.9900 . ? C14T C16T 1.47(3) . ? C14T H14A 0.9900 . ? C14T H14B 0.9900 . ? C15T C16T 1.59(2) . ? C15T H15A 0.9900 . ? C15T H15B 0.9900 . ? C16T H16A 0.9900 . ? C16T H16B 0.9900 . ? N1 Cu1 2.244(4) . ? N2 Cu2 2.254(4) . ? O1 Cu1 1.938(3) 2_556 ? O2 Cu1 1.937(3) 2_556 ? O3 Cu1 1.936(3) . ? O4 Cu1 1.929(3) . ? O5 Cu2 1.938(3) . ? O6 Cu2 1.924(3) . ? O7 Cu2 1.932(3) 2_565 ? O8 Cu2 1.898(4) 2_565 ? Cu1 O2 1.937(3) 2_556 ? Cu1 O1 1.938(3) 2_556 ? Cu2 O8 1.898(4) 2_565 ? Cu2 O7 1.932(3) 2_565 ? 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 C1A C4A C5 111.9(9) . . ? C1A C4A C2A 109.2(9) . . ? C5 C4A C2A 108.1(8) . . ? C1A C4A C3A 116.2(9) . . ? C5 C4A C3A 110.7(9) . . ? C2A C4A C3A 99.8(8) . . ? C4B C1B H1B1 109.5 . . ? C4B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C4B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C4B C2B H2B1 109.5 . . ? C4B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 109.5 . . ? C4B C2B H2B3 109.5 . . ? H2B1 C2B H2B3 109.5 . . ? H2B2 C2B H2B3 109.5 . . ? C4B C3B H3B1 109.5 . . ? C4B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C4B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C2B C4B C5 109.0(8) . . ? C2B C4B C1B 112.1(9) . . ? C5 C4B C1B 112.3(8) . . ? C2B C4B C3B 113.2(9) . . ? C5 C4B C3B 109.1(9) . . ? C1B C4B C3B 101.0(8) . . ? O1 C5 C6 123.5(3) . . ? O1 C5 C4B 115.2(6) . . ? C6 C5 C4B 121.4(6) . . ? O1 C5 C4A 114.9(6) . . ? C6 C5 C4A 121.3(6) . . ? C5 C6 C7 125.3(3) . . ? C5 C6 H6 117.4 . . ? C7 C6 H6 117.4 . . ? O2 C7 C6 124.8(3) . . ? O2 C7 C8 114.6(3) . . ? C6 C7 C8 120.6(3) . . ? C13 C8 C9 118.3(3) . . ? C13 C8 C7 118.6(3) . . ? C9 C8 C7 123.1(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.6(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 118.0(3) . . ? C13 C12 C14 118.5(3) . . ? C11 C12 C14 123.4(3) . . ? C12 C13 C8 122.1(3) . . ? C12 C13 H13 119.0 . . ? C8 C13 H13 119.0 . . ? O3 C14 C15 124.9(3) . . ? O3 C14 C12 114.6(3) . . ? C15 C14 C12 120.5(3) . . ? C14 C15 C16 124.5(4) . . ? C14 C15 H15 117.7 . . ? C16 C15 H15 117.7 . . ? O4 C16 C15 124.3(4) . . ? O4 C16 C17 113.2(3) . . ? C15 C16 C17 122.5(4) . . ? C18 C17 C19 113.8(5) . . ? C18 C17 C16 115.0(4) . . ? C19 C17 C16 109.9(4) . . ? C18 C17 C20 107.3(4) . . ? C19 C17 C20 105.1(5) . . ? C16 C17 C20 104.8(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21A C24A C23A 112.0(10) . . ? C21A C24A C22A 113.2(10) . . ? C23A C24A C22A 103.2(9) . . ? C21A C24A C25 105.4(8) . . ? C23A C24A C25 112.9(10) . . ? C22A C24A C25 110.3(9) . . ? C24B C21B H21D 109.5 . . ? C24B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C24B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C24B C22B H22D 109.5 . . ? C24B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C24B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C24B C23B H23D 109.5 . . ? C24B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C24B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C23B C24B C22B 112.1(10) . . ? C23B C24B C21B 107.7(9) . . ? C22B C24B C21B 108.4(9) . . ? C23B C24B C25 113.5(10) . . ? C22B C24B C25 104.4(8) . . ? C21B C24B C25 110.6(9) . . ? O5 C25 C26 124.9(4) . . ? O5 C25 C24A 110.1(6) . . ? C26 C25 C24A 124.6(6) . . ? O5 C25 C24B 115.7(6) . . ? C26 C25 C24B 118.6(6) . . ? C25 C26 C27 125.2(5) . . ? C25 C26 H26 117.4 . . ? C27 C26 H26 117.4 . . ? O6 C27 C26 124.3(5) . . ? O6 C27 C28 115.4(3) . . ? C26 C27 C28 120.4(4) . . ? C29 C28 C33 117.8(4) . . ? C29 C28 C27 124.9(4) . . ? C33 C28 C27 117.2(4) . . ? C30 C29 C28 121.5(4) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 120.6(5) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C32 119.5(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 119.3(4) . . ? C33 C32 C34 118.2(4) . . ? C31 C32 C34 122.5(4) . . ? C32 C33 C28 121.2(4) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? O7 C34 C35 124.3(4) . . ? O7 C34 C32 114.9(4) . . ? C35 C34 C32 120.7(4) . . ? C34 C35 C36 123.6(5) . . ? C34 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? O8 C36 C35 126.4(5) . . ? O8 C36 C37B 108.9(7) . . ? C35 C36 C37B 124.4(7) . . ? O8 C36 C37A 117.5(6) . . ? C35 C36 C37A 115.9(7) . . ? C40A C37A C39A 112.3(11) . . ? C40A C37A C38A 111.3(11) . . ? C39A C37A C38A 107.1(10) . . ? C40A C37A C36 113.9(10) . . ? C39A C37A C36 106.1(9) . . ? C38A C37A C36 105.7(9) . . ? C39B C37B C36 114.4(11) . . ? C39B C37B C38B 104.5(10) . . ? C36 C37B C38B 110.6(10) . . ? C39B C37B C40B 113.1(11) . . ? C36 C37B C40B 103.9(9) . . ? C38B C37B C40B 110.4(11) . . ? C37B C38B H38D 109.5 . . ? C37B C38B H38E 109.5 . . ? H38D C38B H38E 109.5 . . ? C37B C38B H38F 109.5 . . ? H38D C38B H38F 109.5 . . ? H38E C38B H38F 109.5 . . ? C37B C39B H39D 109.5 . . ? C37B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C37B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C37B C40B H40D 109.5 . . ? C37B C40B H40E 109.5 . . ? H40D C40B H40E 109.5 . . ? C37B C40B H40F 109.5 . . ? H40D C40B H40F 109.5 . . ? H40E C40B H40F 109.5 . . ? N1 C100 C101 124.7(4) . . ? N1 C100 H100 117.7 . . ? C101 C100 H100 117.7 . . ? C100 C101 C102 118.8(4) . . ? C100 C101 H101 120.6 . . ? C102 C101 H101 120.6 . . ? C103 C102 C101 117.8(4) . . ? C103 C102 S1 123.7(3) . . ? C101 C102 S1 118.4(3) . . ? C104 C103 C102 118.6(4) . . ? C104 C103 H103 120.7 . . ? C102 C103 H103 120.7 . . ? N1 C104 C103 124.2(4) . . ? N1 C104 H104 117.9 . . ? C103 C104 H104 117.9 . . ? N2 C105 C106 123.8(4) . . ? N2 C105 H105 118.1 . . ? C106 C105 H105 118.1 . . ? C105 C106 C107 118.4(4) . . ? C105 C106 H106 120.8 . . ? C107 C106 H106 120.8 . . ? C106 C107 C108 118.8(4) . . ? C106 C107 S1 119.6(4) . . ? C108 C107 S1 121.6(3) . . ? C109 C108 C107 118.3(4) . . ? C109 C108 H108 120.9 . . ? C107 C108 H108 120.9 . . ? N2 C109 C108 123.5(4) . . ? N2 C109 H109 118.2 . . ? C108 C109 H109 118.2 . . ? C1T O1T C4T 104.5(12) . . ? C2T C1T O1T 114.8(16) . . ? C2T C1T H1T1 108.6 . . ? O1T C1T H1T1 108.6 . . ? C2T C1T H1T2 108.6 . . ? O1T C1T H1T2 108.6 . . ? H1T1 C1T H1T2 107.6 . . ? C1T C2T C3T 103.6(14) . . ? C1T C2T H2T1 111.0 . . ? C3T C2T H2T1 111.0 . . ? C1T C2T H2T2 111.0 . . ? C3T C2T H2T2 111.0 . . ? H2T1 C2T H2T2 109.0 . . ? C4T C3T C2T 103.4(14) . . ? C4T C3T H3T1 111.1 . . ? C2T C3T H3T1 111.1 . . ? C4T C3T H3T2 111.1 . . ? C2T C3T H3T2 111.1 . . ? H3T1 C3T H3T2 109.0 . . ? C3T C4T O1T 101.5(12) . . ? C3T C4T H4T1 111.5 . . ? O1T C4T H4T1 111.5 . . ? C3T C4T H4T2 111.5 . . ? O1T C4T H4T2 111.5 . . ? H4T1 C4T H4T2 109.3 . . ? C7T O2T C5T 117.0(11) . . ? O2T C5T C8T 99.9(11) . . ? O2T C5T H5T1 111.8 . . ? C8T C5T H5T1 111.8 . . ? O2T C5T H5T2 111.8 . . ? C8T C5T H5T2 111.8 . . ? H5T1 C5T H5T2 109.5 . . ? C8T C6T C7T 105.2(11) . . ? C8T C6T H6T1 110.7 . . ? C7T C6T H6T1 110.7 . . ? C8T C6T H6T2 110.7 . . ? C7T C6T H6T2 110.7 . . ? H6T1 C6T H6T2 108.8 . . ? O2T C7T C6T 104.1(10) . . ? O2T C7T H7T1 110.9 . . ? C6T C7T H7T1 110.9 . . ? O2T C7T H7T2 110.9 . . ? C6T C7T H7T2 110.9 . . ? H7T1 C7T H7T2 109.0 . . ? C6T C8T C5T 98.4(10) . . ? C6T C8T H8T1 112.1 . . ? C5T C8T H8T1 112.1 . . ? C6T C8T H8T2 112.1 . . ? C5T C8T H8T2 112.1 . . ? H8T1 C8T H8T2 109.7 . . ? C10T C9T C12T 113(2) . . ? C10T C9T H9T1 109.1 . . ? C12T C9T H9T1 109.1 . . ? C10T C9T H9T2 109.1 . . ? C12T C9T H9T2 109.1 . . ? H9T1 C9T H9T2 107.8 . . ? C9T C10T O3T 109.0(17) . . ? C9T C10T H10A 109.9 . . ? O3T C10T H10A 109.9 . . ? C9T C10T H10B 109.9 . . ? O3T C10T H10B 109.9 . . ? H10A C10T H10B 108.3 . . ? C10T O3T C11T 111.4(14) . . ? C12T C11T O3T 90.9(17) . . ? C12T C11T H11A 113.5 . . ? O3T C11T H11A 113.5 . . ? C12T C11T H11B 113.5 . . ? O3T C11T H11B 113.5 . . ? H11A C11T H11B 110.8 . . ? C9T C12T C11T 110(3) . . ? C9T C12T H12A 109.7 . . ? C11T C12T H12A 109.7 . . ? C9T C12T H12B 109.7 . . ? C11T C12T H12B 109.7 . . ? H12A C12T H12B 108.2 . . ? C14T O4T C13T 109.5(10) . . ? C15T C13T O4T 110.2(11) . . ? C15T C13T H13A 109.6 . . ? O4T C13T H13A 109.6 . . ? C15T C13T H13B 109.6 . . ? O4T C13T H13B 109.6 . . ? H13A C13T H13B 108.1 . . ? O4T C14T C16T 113.5(14) . . ? O4T C14T H14A 108.9 . . ? C16T C14T H14A 108.9 . . ? O4T C14T H14B 108.9 . . ? C16T C14T H14B 108.9 . . ? H14A C14T H14B 107.7 . . ? C13T C15T C16T 103.9(13) . . ? C13T C15T H15A 111.0 . . ? C16T C15T H15A 111.0 . . ? C13T C15T H15B 111.0 . . ? C16T C15T H15B 111.0 . . ? H15A C15T H15B 109.0 . . ? C14T C16T C15T 100.8(16) . . ? C14T C16T H16A 111.6 . . ? C15T C16T H16A 111.6 . . ? C14T C16T H16B 111.6 . . ? C15T C16T H16B 111.6 . . ? H16A C16T H16B 109.4 . . ? C100 N1 C104 115.9(4) . . ? C100 N1 Cu1 123.0(3) . . ? C104 N1 Cu1 121.0(3) . . ? C105 N2 C109 117.1(4) . . ? C105 N2 Cu2 122.3(3) . . ? C109 N2 Cu2 120.4(3) . . ? C5 O1 Cu1 126.3(2) . 2_556 ? C7 O2 Cu1 125.8(2) . 2_556 ? C14 O3 Cu1 126.9(2) . . ? C16 O4 Cu1 127.5(2) . . ? C25 O5 Cu2 126.6(3) . . ? C27 O6 Cu2 127.0(3) . . ? C34 O7 Cu2 125.9(3) . 2_565 ? C36 O8 Cu2 126.4(3) . 2_565 ? C102 S1 C107 101.3(2) . . ? O4 Cu1 O3 91.82(11) . . ? O4 Cu1 O2 170.93(13) . 2_556 ? O3 Cu1 O2 88.35(11) . 2_556 ? O4 Cu1 O1 86.11(12) . 2_556 ? O3 Cu1 O1 166.23(15) . 2_556 ? O2 Cu1 O1 91.57(11) 2_556 2_556 ? O4 Cu1 N1 95.26(13) . . ? O3 Cu1 N1 95.42(12) . . ? O2 Cu1 N1 93.75(13) 2_556 . ? O1 Cu1 N1 98.32(14) 2_556 . ? O8 Cu2 O6 164.65(15) 2_565 . ? O8 Cu2 O7 93.31(15) 2_565 2_565 ? O6 Cu2 O7 88.25(12) . 2_565 ? O8 Cu2 O5 85.31(17) 2_565 . ? O6 Cu2 O5 91.92(14) . . ? O7 Cu2 O5 175.34(15) 2_565 . ? O8 Cu2 N2 97.44(15) 2_565 . ? O6 Cu2 N2 97.73(14) . . ? O7 Cu2 N2 92.81(12) 2_565 . ? O5 Cu2 N2 91.77(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2B C4B C5 O1 -101.5(8) . . . . ? C1B C4B C5 O1 133.7(7) . . . . ? C3B C4B C5 O1 22.6(9) . . . . ? C2B C4B C5 C6 79.5(9) . . . . ? C1B C4B C5 C6 -45.4(10) . . . . ? C3B C4B C5 C6 -156.5(6) . . . . ? C2B C4B C5 C4A -12(8) . . . . ? C1B C4B C5 C4A -137(9) . . . . ? C3B C4B C5 C4A 112(8) . . . . ? C1A C4A C5 O1 151.9(7) . . . . ? C2A C4A C5 O1 -87.9(8) . . . . ? C3A C4A C5 O1 20.5(9) . . . . ? C1A C4A C5 C6 -34.1(10) . . . . ? C2A C4A C5 C6 86.1(9) . . . . ? C3A C4A C5 C6 -165.5(6) . . . . ? C1A C4A C5 C4B 58(8) . . . . ? C2A C4A C5 C4B 179(9) . . . . ? C3A C4A C5 C4B -73(8) . . . . ? O1 C5 C6 C7 -2.5(6) . . . . ? C4B C5 C6 C7 176.4(6) . . . . ? C4A C5 C6 C7 -176.0(6) . . . . ? C5 C6 C7 O2 -5.3(6) . . . . ? C5 C6 C7 C8 175.0(3) . . . . ? O2 C7 C8 C13 -19.8(5) . . . . ? C6 C7 C8 C13 159.8(3) . . . . ? O2 C7 C8 C9 158.2(4) . . . . ? C6 C7 C8 C9 -22.1(5) . . . . ? C13 C8 C9 C10 -1.0(6) . . . . ? C7 C8 C9 C10 -179.0(4) . . . . ? C8 C9 C10 C11 0.1(7) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C10 C11 C12 C13 0.1(6) . . . . ? C10 C11 C12 C14 -178.6(4) . . . . ? C11 C12 C13 C8 -1.0(5) . . . . ? C14 C12 C13 C8 177.8(3) . . . . ? C9 C8 C13 C12 1.5(5) . . . . ? C7 C8 C13 C12 179.6(3) . . . . ? C13 C12 C14 O3 -8.9(5) . . . . ? C11 C12 C14 O3 169.9(4) . . . . ? C13 C12 C14 C15 171.6(3) . . . . ? C11 C12 C14 C15 -9.6(6) . . . . ? O3 C14 C15 C16 -0.3(7) . . . . ? C12 C14 C15 C16 179.2(4) . . . . ? C14 C15 C16 O4 -1.8(7) . . . . ? C14 C15 C16 C17 175.7(4) . . . . ? O4 C16 C17 C18 -177.4(4) . . . . ? C15 C16 C17 C18 4.9(7) . . . . ? O4 C16 C17 C19 -47.4(6) . . . . ? C15 C16 C17 C19 134.9(5) . . . . ? O4 C16 C17 C20 65.1(5) . . . . ? C15 C16 C17 C20 -112.6(5) . . . . ? C21A C24A C25 O5 -65.7(9) . . . . ? C23A C24A C25 O5 171.7(8) . . . . ? C22A C24A C25 O5 56.8(10) . . . . ? C21A C24A C25 C26 122.0(8) . . . . ? C23A C24A C25 C26 -0.6(12) . . . . ? C22A C24A C25 C26 -115.5(9) . . . . ? C21A C24A C25 C24B 46(2) . . . . ? C23A C24A C25 C24B -77(2) . . . . ? C22A C24A C25 C24B 168(3) . . . . ? C23B C24B C25 O5 168.9(7) . . . . ? C22B C24B C25 O5 46.5(10) . . . . ? C21B C24B C25 O5 -69.9(10) . . . . ? C23B C24B C25 C26 -21.4(11) . . . . ? C22B C24B C25 C26 -143.8(8) . . . . ? C21B C24B C25 C26 99.8(9) . . . . ? C23B C24B C25 C24A 93(3) . . . . ? C22B C24B C25 C24A -29(2) . . . . ? C21B C24B C25 C24A -146(3) . . . . ? O5 C25 C26 C27 2.5(9) . . . . ? C24A C25 C26 C27 173.7(6) . . . . ? C24B C25 C26 C27 -166.1(6) . . . . ? C25 C26 C27 O6 -0.2(8) . . . . ? C25 C26 C27 C28 179.5(5) . . . . ? O6 C27 C28 C29 178.4(4) . . . . ? C26 C27 C28 C29 -1.3(6) . . . . ? O6 C27 C28 C33 -3.2(5) . . . . ? C26 C27 C28 C33 177.2(4) . . . . ? C33 C28 C29 C30 -0.6(7) . . . . ? C27 C28 C29 C30 177.9(4) . . . . ? C28 C29 C30 C31 1.2(8) . . . . ? C29 C30 C31 C32 -0.9(7) . . . . ? C30 C31 C32 C33 0.1(6) . . . . ? C30 C31 C32 C34 -178.8(4) . . . . ? C31 C32 C33 C28 0.6(6) . . . . ? C34 C32 C33 C28 179.5(3) . . . . ? C29 C28 C33 C32 -0.3(6) . . . . ? C27 C28 C33 C32 -178.9(3) . . . . ? C33 C32 C34 O7 -18.4(5) . . . . ? C31 C32 C34 O7 160.5(4) . . . . ? C33 C32 C34 C35 160.5(4) . . . . ? C31 C32 C34 C35 -20.6(6) . . . . ? O7 C34 C35 C36 -0.5(8) . . . . ? C32 C34 C35 C36 -179.3(4) . . . . ? C34 C35 C36 O8 -1.3(9) . . . . ? C34 C35 C36 C37B -174.2(7) . . . . ? C34 C35 C36 C37A 173.4(7) . . . . ? O8 C36 C37A C40A 132.1(10) . . . . ? C35 C36 C37A C40A -43.1(12) . . . . ? C37B C36 C37A C40A -175(4) . . . . ? O8 C36 C37A C39A -103.8(10) . . . . ? C35 C36 C37A C39A 80.9(10) . . . . ? C37B C36 C37A C39A -51(3) . . . . ? O8 C36 C37A C38A 9.7(11) . . . . ? C35 C36 C37A C38A -165.5(8) . . . . ? C37B C36 C37A C38A 63(4) . . . . ? O8 C36 C37B C39B -158.0(9) . . . . ? C35 C36 C37B C39B 15.9(14) . . . . ? C37A C36 C37B C39B 71(4) . . . . ? O8 C36 C37B C38B -40.4(11) . . . . ? C35 C36 C37B C38B 133.6(9) . . . . ? C37A C36 C37B C38B -172(4) . . . . ? O8 C36 C37B C40B 78.2(10) . . . . ? C35 C36 C37B C40B -107.9(10) . . . . ? C37A C36 C37B C40B -53(3) . . . . ? N1 C100 C101 C102 0.5(7) . . . . ? C100 C101 C102 C103 -1.8(6) . . . . ? C100 C101 C102 S1 -179.1(3) . . . . ? C101 C102 C103 C104 1.8(7) . . . . ? S1 C102 C103 C104 179.0(3) . . . . ? C102 C103 C104 N1 -0.6(7) . . . . ? N2 C105 C106 C107 0.3(7) . . . . ? C105 C106 C107 C108 -3.0(7) . . . . ? C105 C106 C107 S1 178.5(3) . . . . ? C106 C107 C108 C109 3.5(7) . . . . ? S1 C107 C108 C109 -178.1(3) . . . . ? C107 C108 C109 N2 -1.4(7) . . . . ? C4T O1T C1T C2T 11(2) . . . . ? O1T C1T C2T C3T -29(2) . . . . ? C1T C2T C3T C4T 35.4(18) . . . . ? C2T C3T C4T O1T -27.7(16) . . . . ? C1T O1T C4T C3T 12.6(17) . . . . ? C7T O2T C5T C8T 10.0(15) . . . . ? C5T O2T C7T C6T 13.7(16) . . . . ? C8T C6T C7T O2T -34.7(14) . . . . ? C7T C6T C8T C5T 38.2(13) . . . . ? O2T C5T C8T C6T -29.5(12) . . . . ? C12T C9T C10T O3T -4(3) . . . . ? C9T C10T O3T C11T 19(2) . . . . ? C10T O3T C11T C12T -24(2) . . . . ? C10T C9T C12T C11T -14(3) . . . . ? O3T C11T C12T C9T 21(3) . . . . ? C14T O4T C13T C15T -15.8(14) . . . . ? C13T O4T C14T C16T 12.7(18) . . . . ? O4T C13T C15T C16T 11.8(16) . . . . ? O4T C14T C16T C15T -5(2) . . . . ? C13T C15T C16T C14T -4.4(18) . . . . ? C101 C100 N1 C104 0.8(6) . . . . ? C101 C100 N1 Cu1 -175.6(3) . . . . ? C103 C104 N1 C100 -0.7(6) . . . . ? C103 C104 N1 Cu1 175.8(3) . . . . ? C106 C105 N2 C109 1.8(7) . . . . ? C106 C105 N2 Cu2 -173.9(4) . . . . ? C108 C109 N2 C105 -1.2(7) . . . . ? C108 C109 N2 Cu2 174.5(3) . . . . ? C6 C5 O1 Cu1 17.2(6) . . . 2_556 ? C4B C5 O1 Cu1 -161.8(5) . . . 2_556 ? C4A C5 O1 Cu1 -168.9(5) . . . 2_556 ? C6 C7 O2 Cu1 -2.5(6) . . . 2_556 ? C8 C7 O2 Cu1 177.1(2) . . . 2_556 ? C15 C14 O3 Cu1 -0.6(6) . . . . ? C12 C14 O3 Cu1 179.9(2) . . . . ? C15 C16 O4 Cu1 4.4(6) . . . . ? C17 C16 O4 Cu1 -173.2(3) . . . . ? C26 C25 O5 Cu2 -0.6(8) . . . . ? C24A C25 O5 Cu2 -172.9(5) . . . . ? C24B C25 O5 Cu2 168.4(5) . . . . ? C26 C27 O6 Cu2 -3.7(6) . . . . ? C28 C27 O6 Cu2 176.6(3) . . . . ? C35 C34 O7 Cu2 1.1(6) . . . 2_565 ? C32 C34 O7 Cu2 179.9(2) . . . 2_565 ? C35 C36 O8 Cu2 2.3(8) . . . 2_565 ? C37B C36 O8 Cu2 176.1(6) . . . 2_565 ? C37A C36 O8 Cu2 -172.4(6) . . . 2_565 ? C103 C102 S1 C107 27.6(4) . . . . ? C101 C102 S1 C107 -155.2(4) . . . . ? C106 C107 S1 C102 -127.9(4) . . . . ? C108 C107 S1 C102 53.6(4) . . . . ? C16 O4 Cu1 O3 -4.0(4) . . . . ? C16 O4 Cu1 O1 162.3(4) . . . 2_556 ? C16 O4 Cu1 N1 -99.6(4) . . . . ? C14 O3 Cu1 O4 2.1(3) . . . . ? C14 O3 Cu1 O2 -168.8(3) . . . 2_556 ? C14 O3 Cu1 O1 -78.9(6) . . . 2_556 ? C14 O3 Cu1 N1 97.6(3) . . . . ? C100 N1 Cu1 O4 -113.3(3) . . . . ? C104 N1 Cu1 O4 70.4(3) . . . . ? C100 N1 Cu1 O3 154.3(3) . . . . ? C104 N1 Cu1 O3 -21.9(3) . . . . ? C100 N1 Cu1 O2 65.6(3) . . . 2_556 ? C104 N1 Cu1 O2 -110.6(3) . . . 2_556 ? C100 N1 Cu1 O1 -26.5(3) . . . 2_556 ? C104 N1 Cu1 O1 157.3(3) . . . 2_556 ? C27 O6 Cu2 O8 -75.0(7) . . . 2_565 ? C27 O6 Cu2 O7 -171.2(3) . . . 2_565 ? C27 O6 Cu2 O5 4.2(4) . . . . ? C27 O6 Cu2 N2 96.2(3) . . . . ? C25 O5 Cu2 O8 162.8(5) . . . 2_565 ? C25 O5 Cu2 O6 -2.1(4) . . . . ? C25 O5 Cu2 N2 -99.9(4) . . . . ? C105 N2 Cu2 O8 -145.2(4) . . . 2_565 ? C109 N2 Cu2 O8 39.3(4) . . . 2_565 ? C105 N2 Cu2 O6 37.1(4) . . . . ? C109 N2 Cu2 O6 -138.4(3) . . . . ? C105 N2 Cu2 O7 -51.5(4) . . . 2_565 ? C109 N2 Cu2 O7 133.0(3) . . . 2_565 ? C105 N2 Cu2 O5 129.3(4) . . . . ? C109 N2 Cu2 O5 -46.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.062 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.089 # Attachment 'Cu hmt.CIF' data_lj52sad _database_code_depnum_ccdc_archive 'CCDC 606855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '1.5(C40 H48 O8 Cu2), (N4 C6 H12)' _chemical_formula_sum 'C66 H84 Cu3 N4 O12' _chemical_formula_weight 1316.0472 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 _symmetry_space_group_name_Hall '-P 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 18.6380(5) _cell_length_b 18.6380(5) _cell_length_c 11.5817(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3484.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12431 _cell_measurement_theta_min 2.5235 _cell_measurement_theta_max 28.2775 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1382 _exptl_absorpt_coefficient_mu 0.965 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 272 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.11 _diffrn_reflns_number 34505 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5639 _reflns_number_gt 4730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.1013P)^2^+0.9839P] 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 5639 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_restrained_S_all 1.236 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37995(19) 0.19341(18) -0.0279(3) 0.0315(6) Uani 1 1 d . . . H1A H 0.3863 0.2268 0.0407 0.047 Uiso 1 1 calc R . . H1B H 0.3462 0.2017 -0.0854 0.047 Uiso 1 1 calc R . . H1C H 0.4346 0.2103 -0.0607 0.047 Uiso 1 1 calc R . . C2 C 0.2503(2) 0.0743(2) 0.0551(3) 0.0411(8) Uani 1 1 d . . . H2A H 0.2245 0.0164 0.0801 0.062 Uiso 1 1 calc R . . H2B H 0.2160 0.0796 -0.0046 0.062 Uiso 1 1 calc R . . H2C H 0.2553 0.1093 0.1212 0.062 Uiso 1 1 calc R . . C3 C 0.3302(2) 0.0503(2) -0.1020(3) 0.0364(7) Uani 1 1 d . . . H3A H 0.3856 0.0639 -0.1277 0.055 Uiso 1 1 calc R . . H3B H 0.3023 0.0629 -0.1639 0.055 Uiso 1 1 calc R . . H3C H 0.2979 -0.0088 -0.0829 0.055 Uiso 1 1 calc R . . C4 C 0.33742(17) 0.10198(17) 0.0056(2) 0.0261(6) Uani 1 1 d . . . C5 C 0.38642(16) 0.09154(16) 0.1047(2) 0.0213(5) Uani 1 1 d . . . C6 C 0.40152(17) 0.02530(17) 0.1081(2) 0.0250(5) Uani 1 1 d . . . H6 H 0.3823 -0.0128 0.0455 0.030 Uiso 1 1 calc R . . C7 C 0.44330(16) 0.01169(16) 0.1983(2) 0.0210(5) Uani 1 1 d . . . C8 C 0.44619(16) -0.06717(16) 0.2044(2) 0.0206(5) Uani 1 1 d . . . C9 C 0.41782(17) -0.12618(16) 0.1149(2) 0.0238(5) Uani 1 1 d . . . H9 H 0.3974 -0.1161 0.0453 0.029 Uiso 1 1 calc R . . C10 C 0.41969(17) -0.19912(17) 0.1287(2) 0.0250(5) Uani 1 1 d . . . H10 H 0.3994 -0.2392 0.0687 0.030 Uiso 1 1 calc R . . C11 C 0.45047(17) -0.21446(16) 0.2280(2) 0.0235(5) Uani 1 1 d . . . H11 H 0.4519 -0.2645 0.2356 0.028 Uiso 1 1 calc R . . C12 C 0.47971(16) -0.15631(15) 0.3177(2) 0.0201(5) Uani 1 1 d . . . C13 C 0.47576(16) -0.08363(16) 0.3055(2) 0.0203(5) Uani 1 1 d . . . H13 H 0.4935 -0.0449 0.3672 0.024 Uiso 1 1 calc R . . C14 C 0.51627(16) -0.16926(15) 0.4252(2) 0.0201(5) Uani 1 1 d . . . C15 C 0.56834(18) -0.20308(17) 0.4142(2) 0.0256(5) Uani 1 1 d . . . H15 H 0.5763 -0.2188 0.3394 0.031 Uiso 1 1 calc R . . C16 C 0.60902(17) -0.21485(16) 0.5068(2) 0.0246(5) Uani 1 1 d . . . C17 C 0.6698(2) -0.2470(2) 0.4890(3) 0.0342(7) Uani 1 1 d . . . C18 C 0.6905(3) -0.2519(3) 0.3630(3) 0.0529(10) Uani 1 1 d . . . H18A H 0.7151 -0.1967 0.3280 0.079 Uiso 1 1 calc R . . H18B H 0.6398 -0.2901 0.3214 0.079 Uiso 1 1 calc R . . H18C H 0.7300 -0.2720 0.3586 0.079 Uiso 1 1 calc R . . C19 C 0.6285(3) -0.3337(3) 0.5437(4) 0.0636(12) Uani 1 1 d . . . H19A H 0.5787 -0.3713 0.4998 0.095 Uiso 1 1 calc R . . H19B H 0.6132 -0.3305 0.6237 0.095 Uiso 1 1 calc R . . H19C H 0.6674 -0.3547 0.5426 0.095 Uiso 1 1 calc R . . C20 C 0.7496(3) -0.1898(3) 0.5548(4) 0.0599(12) Uani 1 1 d . . . H20A H 0.7867 -0.2130 0.5525 0.090 Uiso 1 1 calc R . . H20B H 0.7362 -0.1851 0.6352 0.090 Uiso 1 1 calc R . . H20C H 0.7771 -0.1349 0.5188 0.090 Uiso 1 1 calc R . . C21 C 0.58896(16) 0.26551(16) 0.1572(2) 0.0227(5) Uani 1 1 d . . . H21A H 0.5816 0.2123 0.1280 0.027 Uiso 1 1 calc R . . H21B H 0.5424 0.2715 0.1278 0.027 Uiso 1 1 calc R . . C22 C 0.65676(15) 0.25462(15) 0.3262(2) 0.0207(5) Uani 1 1 d . . . H22A H 0.6567 0.2539 0.4117 0.025 Uiso 1 1 calc R . . H22B H 0.6499 0.2012 0.2988 0.025 Uiso 1 1 calc R . . O1 O 0.40723(13) 0.14548(12) 0.18457(16) 0.0254(4) Uani 1 1 d . . . O2 O 0.47913(12) 0.06133(12) 0.28191(16) 0.0247(4) Uani 1 1 d . . . O3 O 0.49893(11) -0.14485(11) 0.51785(15) 0.0216(4) Uani 1 1 d . . . O4 O 0.59959(13) -0.20165(13) 0.61053(16) 0.0276(4) Uani 1 1 d . . . Cu1 Cu 0.457837(19) 0.147752(19) 0.33145(3) 0.01999(14) Uani 1 1 d . . . N1 N 0.58624(13) 0.26330(13) 0.28481(18) 0.0199(4) Uani 1 1 d . . . N2 N 0.6667 0.3333 0.1129(3) 0.0223(8) Uani 1 3 d S . . 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 C1 0.0397(16) 0.0303(14) 0.0277(14) 0.0038(11) -0.0047(12) 0.0199(13) C2 0.0277(15) 0.0501(19) 0.0434(19) 0.0054(15) -0.0058(13) 0.0180(14) C3 0.0502(19) 0.0350(16) 0.0255(15) -0.0028(12) -0.0149(13) 0.0226(14) C4 0.0283(13) 0.0277(13) 0.0238(13) 0.0007(10) -0.0072(10) 0.0152(11) C5 0.0210(12) 0.0228(12) 0.0181(12) 0.0010(9) -0.0019(9) 0.0095(10) C6 0.0308(13) 0.0254(13) 0.0198(13) -0.0043(10) -0.0076(10) 0.0147(11) C7 0.0236(12) 0.0228(12) 0.0177(12) -0.0006(9) 0.0000(9) 0.0124(10) C8 0.0224(12) 0.0210(12) 0.0187(12) -0.0021(9) 0.0008(9) 0.0112(10) C9 0.0279(13) 0.0270(13) 0.0162(12) -0.0035(10) -0.0031(10) 0.0134(11) C10 0.0296(13) 0.0242(13) 0.0196(12) -0.0061(10) -0.0029(10) 0.0121(11) C11 0.0287(13) 0.0191(12) 0.0226(13) -0.0026(10) -0.0009(10) 0.0119(10) C12 0.0224(12) 0.0195(11) 0.0179(12) -0.0012(9) -0.0003(9) 0.0101(10) C13 0.0235(12) 0.0202(11) 0.0177(12) -0.0035(9) -0.0014(9) 0.0113(10) C14 0.0230(12) 0.0158(11) 0.0191(12) -0.0019(9) -0.0021(9) 0.0079(9) C15 0.0339(14) 0.0251(13) 0.0221(13) -0.0038(10) -0.0028(11) 0.0181(11) C16 0.0281(13) 0.0193(11) 0.0283(14) -0.0033(10) -0.0031(11) 0.0133(11) C17 0.0454(17) 0.0386(16) 0.0340(16) -0.0057(13) -0.0037(13) 0.0325(15) C18 0.069(3) 0.080(3) 0.041(2) -0.0074(19) 0.0029(18) 0.061(2) C19 0.097(3) 0.045(2) 0.072(3) 0.009(2) 0.012(3) 0.052(2) C20 0.046(2) 0.084(3) 0.068(3) -0.026(2) -0.018(2) 0.046(2) C21 0.0239(12) 0.0238(12) 0.0190(12) -0.0026(10) -0.0040(10) 0.0108(10) C22 0.0218(12) 0.0200(11) 0.0203(12) 0.0023(9) -0.0004(9) 0.0104(10) O1 0.0323(10) 0.0253(9) 0.0215(9) -0.0016(7) -0.0068(8) 0.0166(8) O2 0.0322(10) 0.0260(9) 0.0205(9) -0.0060(7) -0.0090(7) 0.0181(8) O3 0.0274(9) 0.0227(9) 0.0177(9) -0.0001(7) -0.0013(7) 0.0146(8) O4 0.0369(11) 0.0340(11) 0.0220(10) -0.0013(8) -0.0029(8) 0.0252(9) Cu1 0.0254(2) 0.02068(19) 0.0164(2) -0.00134(11) -0.00329(11) 0.01336(14) N1 0.0218(10) 0.0200(10) 0.0176(10) 0.0000(8) -0.0010(8) 0.0102(8) N2 0.0253(11) 0.0253(11) 0.0165(17) 0.000 0.000 0.0126(6) _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 C1 C4 1.527(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.547(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.540(4) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.539(3) . ? C5 O1 1.275(3) . ? C5 C6 1.397(4) . ? C6 C7 1.399(4) . ? C6 H6 0.9500 . ? C7 O2 1.274(3) . ? C7 C8 1.499(3) . ? C8 C13 1.392(4) . ? C8 C9 1.407(3) . ? C9 C10 1.386(4) . ? C9 H9 0.9500 . ? C10 C11 1.377(4) . ? C10 H10 0.9500 . ? C11 C12 1.400(3) . ? C11 H11 0.9500 . ? C12 C13 1.400(3) . ? C12 C14 1.496(3) . ? C13 H13 0.9500 . ? C14 O3 1.269(3) . ? C14 C15 1.403(4) . ? C15 C16 1.393(4) . ? C15 H15 0.9500 . ? C16 O4 1.256(3) . ? C16 C17 1.538(4) . ? C17 C18 1.523(5) . ? C17 C19 1.537(5) . ? C17 C20 1.532(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N2 1.459(3) . ? C21 N1 1.479(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N1 1.474(3) 2_655 ? C22 N1 1.482(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O1 Cu1 1.9353(18) . ? O2 Cu1 1.9288(19) . ? O3 Cu1 1.9345(18) 4_656 ? O4 Cu1 1.9186(19) 4_656 ? Cu1 O4 1.9186(19) 4_656 ? Cu1 O3 1.9345(18) 4_656 ? Cu1 N1 2.346(2) . ? N1 C22 1.474(3) 3_665 ? N2 C21 1.459(3) 2_655 ? N2 C21 1.459(3) 3_665 ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 C3 109.1(2) . . ? C1 C4 C5 108.7(2) . . ? C3 C4 C5 113.4(2) . . ? C1 C4 C2 109.9(2) . . ? C3 C4 C2 110.0(3) . . ? C5 C4 C2 105.7(2) . . ? O1 C5 C6 124.0(2) . . ? O1 C5 C4 114.0(2) . . ? C6 C5 C4 121.8(2) . . ? C5 C6 C7 123.9(2) . . ? C5 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? O2 C7 C6 125.0(2) . . ? O2 C7 C8 114.4(2) . . ? C6 C7 C8 120.6(2) . . ? C13 C8 C9 118.8(2) . . ? C13 C8 C7 117.9(2) . . ? C9 C8 C7 123.2(2) . . ? C10 C9 C8 119.8(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 121.1(2) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 120.0(2) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 119.1(2) . . ? C11 C12 C14 121.7(2) . . ? C13 C12 C14 119.3(2) . . ? C8 C13 C12 121.1(2) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? O3 C14 C15 126.6(2) . . ? O3 C14 C12 115.3(2) . . ? C15 C14 C12 118.0(2) . . ? C16 C15 C14 123.6(2) . . ? C16 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? O4 C16 C15 124.4(2) . . ? O4 C16 C17 114.1(2) . . ? C15 C16 C17 121.5(3) . . ? C18 C17 C19 109.9(3) . . ? C18 C17 C20 109.3(3) . . ? C19 C17 C20 109.1(3) . . ? C18 C17 C16 114.2(3) . . ? C19 C17 C16 106.0(3) . . ? C20 C17 C16 108.1(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N2 C21 N1 112.4(2) . . ? N2 C21 H21A 109.1 . . ? N1 C21 H21A 109.1 . . ? N2 C21 H21B 109.1 . . ? N1 C21 H21B 109.1 . . ? H21A C21 H21B 107.9 . . ? N1 C22 N1 111.6(2) 2_655 . ? N1 C22 H22A 109.3 2_655 . ? N1 C22 H22A 109.3 . . ? N1 C22 H22B 109.3 2_655 . ? N1 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C5 O1 Cu1 127.40(17) . . ? C7 O2 Cu1 125.50(17) . . ? C14 O3 Cu1 124.65(16) . 4_656 ? C16 O4 Cu1 127.36(18) . 4_656 ? O4 Cu1 O2 160.55(9) 4_656 . ? O4 Cu1 O1 85.75(8) 4_656 . ? O2 Cu1 O1 91.25(8) . . ? O4 Cu1 O3 92.74(8) 4_656 4_656 ? O2 Cu1 O3 89.00(8) . 4_656 ? O1 Cu1 O3 176.15(8) . 4_656 ? O4 Cu1 N1 100.38(8) 4_656 . ? O2 Cu1 N1 99.02(8) . . ? O1 Cu1 N1 94.59(8) . . ? O3 Cu1 N1 89.16(8) 4_656 . ? C22 N1 C21 108.1(2) 3_665 . ? C22 N1 C22 108.4(2) 3_665 . ? C21 N1 C22 107.9(2) . . ? C22 N1 Cu1 114.82(15) 3_665 . ? C21 N1 Cu1 105.12(15) . . ? C22 N1 Cu1 112.25(15) . . ? C21 N2 C21 108.31(18) 2_655 . ? C21 N2 C21 108.31(18) 2_655 3_665 ? C21 N2 C21 108.31(18) . 3_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C4 C5 O1 45.2(3) . . . . ? C3 C4 C5 O1 166.7(2) . . . . ? C2 C4 C5 O1 -72.7(3) . . . . ? C1 C4 C5 C6 -138.4(3) . . . . ? C3 C4 C5 C6 -17.0(4) . . . . ? C2 C4 C5 C6 103.6(3) . . . . ? O1 C5 C6 C7 -1.8(4) . . . . ? C4 C5 C6 C7 -177.8(3) . . . . ? C5 C6 C7 O2 -6.9(5) . . . . ? C5 C6 C7 C8 170.9(3) . . . . ? O2 C7 C8 C13 9.1(3) . . . . ? C6 C7 C8 C13 -169.0(2) . . . . ? O2 C7 C8 C9 -173.3(2) . . . . ? C6 C7 C8 C9 8.6(4) . . . . ? C13 C8 C9 C10 0.0(4) . . . . ? C7 C8 C9 C10 -177.6(2) . . . . ? C8 C9 C10 C11 -1.3(4) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C10 C11 C12 C13 1.1(4) . . . . ? C10 C11 C12 C14 -177.9(2) . . . . ? C9 C8 C13 C12 1.8(4) . . . . ? C7 C8 C13 C12 179.6(2) . . . . ? C11 C12 C13 C8 -2.4(4) . . . . ? C14 C12 C13 C8 176.6(2) . . . . ? C11 C12 C14 O3 -142.5(3) . . . . ? C13 C12 C14 O3 38.5(3) . . . . ? C11 C12 C14 C15 40.3(4) . . . . ? C13 C12 C14 C15 -138.7(3) . . . . ? O3 C14 C15 C16 0.2(4) . . . . ? C12 C14 C15 C16 177.1(3) . . . . ? C14 C15 C16 O4 4.8(5) . . . . ? C14 C15 C16 C17 -176.1(3) . . . . ? O4 C16 C17 C18 -172.0(3) . . . . ? C15 C16 C17 C18 8.7(4) . . . . ? O4 C16 C17 C19 66.7(4) . . . . ? C15 C16 C17 C19 -112.5(3) . . . . ? O4 C16 C17 C20 -50.1(4) . . . . ? C15 C16 C17 C20 130.6(3) . . . . ? C6 C5 O1 Cu1 -3.7(4) . . . . ? C4 C5 O1 Cu1 172.50(17) . . . . ? C6 C7 O2 Cu1 19.8(4) . . . . ? C8 C7 O2 Cu1 -158.12(17) . . . . ? C15 C14 O3 Cu1 0.6(4) . . . 4_656 ? C12 C14 O3 Cu1 -176.38(16) . . . 4_656 ? C15 C16 O4 Cu1 -10.0(4) . . . 4_656 ? C17 C16 O4 Cu1 170.80(19) . . . 4_656 ? C7 O2 Cu1 O4 61.8(4) . . . 4_656 ? C7 O2 Cu1 O1 -18.9(2) . . . . ? C7 O2 Cu1 O3 157.2(2) . . . 4_656 ? C7 O2 Cu1 N1 -113.8(2) . . . . ? C5 O1 Cu1 O4 -149.5(2) . . . 4_656 ? C5 O1 Cu1 O2 11.3(2) . . . . ? C5 O1 Cu1 N1 110.5(2) . . . . ? N2 C21 N1 C22 58.4(2) . . . 3_665 ? N2 C21 N1 C22 -58.6(2) . . . . ? N2 C21 N1 Cu1 -178.51(13) . . . . ? N1 C22 N1 C22 -58.8(3) 2_655 . . 3_665 ? N1 C22 N1 C21 58.1(3) 2_655 . . . ? N1 C22 N1 Cu1 173.39(13) 2_655 . . . ? O4 Cu1 N1 C22 9.72(18) 4_656 . . 3_665 ? O2 Cu1 N1 C22 -171.77(17) . . . 3_665 ? O1 Cu1 N1 C22 96.23(17) . . . 3_665 ? O3 Cu1 N1 C22 -82.92(17) 4_656 . . 3_665 ? O4 Cu1 N1 C21 -108.98(16) 4_656 . . . ? O2 Cu1 N1 C21 69.53(16) . . . . ? O1 Cu1 N1 C21 -22.47(16) . . . . ? O3 Cu1 N1 C21 158.39(16) 4_656 . . . ? O4 Cu1 N1 C22 134.05(16) 4_656 . . . ? O2 Cu1 N1 C22 -47.44(17) . . . . ? O1 Cu1 N1 C22 -139.44(16) . . . . ? O3 Cu1 N1 C22 41.41(17) 4_656 . . . ? N1 C21 N2 C21 58.8(2) . . . 2_655 ? N1 C21 N2 C21 -58.5(2) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.477 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.149 # Attachment 'Cu xbp.CIF' data_lj82sad _database_code_depnum_ccdc_archive 'CCDC 606856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cu2 C40 H48 O8, C18 H22 N4, 2.2(C4 H8 O)' _chemical_formula_sum 'C66.80 H87.60 Cu2 N4 O10.20' _chemical_formula_weight 1236.89 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' 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 P1 _symmetry_space_group_name_Hall 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.285(1) _cell_length_b 11.104(2) _cell_length_c 15.772(2) _cell_angle_alpha 90.096(2) _cell_angle_beta 100.647(2) _cell_angle_gamma 100.187(2) _cell_volume 1741.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5382 _cell_measurement_theta_min 2.216 _cell_measurement_theta_max 26.7105 _exptl_crystal_description Plate _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7392 _exptl_absorpt_correction_T_max 0.9395 _exptl_absorpt_process_details 'SADABS, (Sheldrick 2003)' _exptl_special_details ; The crystal was coated in Exxon Paratone N hydrocarbon oil and mounted on a thin mohair fibre attached to a copper pin. Upon mounting on the diffractometer, the crystal was quenched to 150(K) under a cold nitrogen gas stream supplied by an Oxford Cryosystems Cryostream and data were collected at this temperature. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 138 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.05 _diffrn_reflns_number 17455 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.35 _reflns_number_total 14663 _reflns_number_gt 11213 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 2005) WINGX-32 (Farrugia, 2005) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _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^)+(0.1327P)^2^+0.1540P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 6355 Friedal Pairs' _refine_ls_abs_structure_Flack 0.535(17) _refine_ls_number_reflns 14663 _refine_ls_number_parameters 732 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1971 _refine_ls_wR_factor_gt 0.1770 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.031 _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 C1 C 0.7114(16) 0.2720(14) 0.6794(11) 0.0652(18) Uiso 0.50 1 d PD A 1 H1A H 0.7993 0.2846 0.6619 0.098 Uiso 0.50 1 calc PR A 1 H1B H 0.6456 0.2177 0.6368 0.098 Uiso 0.50 1 calc PR A 1 H1C H 0.7183 0.2348 0.7360 0.098 Uiso 0.50 1 calc PR A 1 C2 C 0.7674(15) 0.4773(14) 0.7504(10) 0.0652(18) Uiso 0.50 1 d PD A 1 H2A H 0.7286 0.5009 0.7988 0.098 Uiso 0.50 1 calc PR A 1 H2B H 0.8097 0.5510 0.7249 0.098 Uiso 0.50 1 calc PR A 1 H2C H 0.8352 0.4270 0.7712 0.098 Uiso 0.50 1 calc PR A 1 C3 C 0.5267(15) 0.3834(18) 0.7070(15) 0.0652(18) Uiso 0.50 1 d PD A 1 H3A H 0.4643 0.3322 0.6609 0.098 Uiso 0.50 1 calc PR A 1 H3B H 0.4960 0.4611 0.7130 0.098 Uiso 0.50 1 calc PR A 1 H3C H 0.5298 0.3408 0.7615 0.098 Uiso 0.50 1 calc PR A 1 C1A C 0.7708(15) 0.3369(16) 0.7214(13) 0.0652(18) Uiso 0.50 1 d PD A 2 H1A1 H 0.8589 0.3898 0.7254 0.098 Uiso 0.50 1 calc PR A 2 H1A2 H 0.7652 0.2657 0.6832 0.098 Uiso 0.50 1 calc PR A 2 H1A3 H 0.7592 0.3093 0.7790 0.098 Uiso 0.50 1 calc PR A 2 C2A C 0.6995(16) 0.5299(13) 0.7441(11) 0.0652(18) Uiso 0.50 1 d PD A 2 H2A1 H 0.7060 0.5092 0.8050 0.098 Uiso 0.50 1 calc PR A 2 H2A2 H 0.6298 0.5800 0.7284 0.098 Uiso 0.50 1 calc PR A 2 H2A3 H 0.7862 0.5760 0.7352 0.098 Uiso 0.50 1 calc PR A 2 C3A C 0.5236(14) 0.3440(15) 0.6936(13) 0.0652(18) Uiso 0.50 1 d PD A 2 H3A1 H 0.4874 0.2847 0.6452 0.098 Uiso 0.50 1 calc PR A 2 H3A2 H 0.4647 0.4045 0.6929 0.098 Uiso 0.50 1 calc PR A 2 H3A3 H 0.5283 0.3011 0.7481 0.098 Uiso 0.50 1 calc PR A 2 C4 C 0.6616(9) 0.4075(10) 0.6854(6) 0.064(3) Uani 1 1 d . . . C5 C 0.6711(8) 0.4563(6) 0.5940(5) 0.0349(16) Uani 1 1 d . A . C6 C 0.5558(7) 0.4673(7) 0.5364(5) 0.0370(17) Uani 1 1 d . . . H6 H 0.4718 0.4409 0.5536 0.044 Uiso 1 1 calc R A . C7 C 0.5548(7) 0.5152(6) 0.4535(5) 0.0267(15) Uani 1 1 d . A . C8 C 0.4236(7) 0.5246(6) 0.3961(4) 0.0253(14) Uani 1 1 d . . . C9 C 0.4288(7) 0.5918(6) 0.3217(4) 0.0238(14) Uani 1 1 d . A . H9 H 0.5131 0.6295 0.3090 0.029 Uiso 1 1 calc R . . C10 C 0.3091(6) 0.6037(6) 0.2657(4) 0.0223(14) Uani 1 1 d . . . C11 C 0.1834(7) 0.5503(6) 0.2849(4) 0.0249(14) Uani 1 1 d . A . H11 H 0.1025 0.5579 0.2466 0.030 Uiso 1 1 calc R . . C12 C 0.1787(8) 0.4865(7) 0.3604(5) 0.0360(18) Uani 1 1 d . . . H12 H 0.0945 0.4514 0.3744 0.043 Uiso 1 1 calc R A . C13 C 0.2998(7) 0.4741(6) 0.4164(5) 0.0318(16) Uani 1 1 d . A . H13 H 0.2965 0.4310 0.4682 0.038 Uiso 1 1 calc R . . C14 C 0.3176(7) 0.6727(6) 0.1844(5) 0.0267(16) Uani 1 1 d . A . C15 C 0.2131(6) 0.6483(6) 0.1114(4) 0.0254(14) Uani 1 1 d . . . H15 H 0.1434 0.5801 0.1133 0.030 Uiso 1 1 calc R A . C16 C 0.2039(7) 0.7148(6) 0.0383(5) 0.0280(14) Uani 1 1 d . A . C17 C 0.0864(7) 0.6814(7) -0.0361(5) 0.0353(16) Uani 1 1 d . . . C18 C 0.1233(7) 0.5901(6) -0.0962(4) 0.0464(15) Uani 1 1 d . A . H18A H 0.2100 0.6240 -0.1119 0.070 Uiso 1 1 calc R . . H18B H 0.0537 0.5746 -0.1485 0.070 Uiso 1 1 calc R . . H18C H 0.1299 0.5132 -0.0667 0.070 Uiso 1 1 calc R . . C19 C 0.0637(6) 0.7989(6) -0.0874(4) 0.0411(13) Uani 1 1 d . A . H19A H 0.0505 0.8621 -0.0480 0.062 Uiso 1 1 calc R . . H19B H -0.0161 0.7787 -0.1332 0.062 Uiso 1 1 calc R . . H19C H 0.1425 0.8293 -0.1131 0.062 Uiso 1 1 calc R . . C20 C -0.0463(5) 0.6265(6) -0.0069(4) 0.0438(14) Uani 1 1 d . A . H20A H -0.0370 0.5490 0.0211 0.066 Uiso 1 1 calc R . . H20B H -0.1195 0.6119 -0.0573 0.066 Uiso 1 1 calc R . . H20C H -0.0665 0.6839 0.0340 0.066 Uiso 1 1 calc R . . C21 C 0.5337(10) 1.0140(10) -0.1676(7) 0.0405(12) Uiso 0.60 1 d PD B 1 H21A H 0.5395 1.0298 -0.2280 0.061 Uiso 0.60 1 calc PR B 1 H21B H 0.5410 1.0918 -0.1360 0.061 Uiso 0.60 1 calc PR B 1 H21C H 0.4472 0.9618 -0.1648 0.061 Uiso 0.60 1 calc PR B 1 C22 C 0.6202(11) 0.8238(8) -0.1800(7) 0.0405(12) Uiso 0.60 1 d PD B 1 H22A H 0.5238 0.7897 -0.1933 0.061 Uiso 0.60 1 calc PR B 1 H22B H 0.6678 0.7670 -0.1445 0.061 Uiso 0.60 1 calc PR B 1 H22C H 0.6547 0.8361 -0.2339 0.061 Uiso 0.60 1 calc PR B 1 C23 C 0.7834(10) 1.0250(10) -0.1420(9) 0.0405(12) Uiso 0.60 1 d PD B 1 H23A H 0.8552 0.9831 -0.1138 0.061 Uiso 0.60 1 calc PR B 1 H23B H 0.7975 1.1081 -0.1168 0.061 Uiso 0.60 1 calc PR B 1 H23C H 0.7847 1.0293 -0.2039 0.061 Uiso 0.60 1 calc PR B 1 C22A C 0.5632(15) 0.8435(12) -0.1829(10) 0.0405(12) Uiso 0.40 1 d PD B 2 H22D H 0.4670 0.8433 -0.1865 0.061 Uiso 0.40 1 calc PR B 2 H22E H 0.5857 0.7680 -0.1567 0.061 Uiso 0.40 1 calc PR B 2 H22F H 0.5845 0.8481 -0.2410 0.061 Uiso 0.40 1 calc PR B 2 C21A C 0.5749(15) 1.0623(14) -0.1454(11) 0.0405(12) Uiso 0.40 1 d PD B 2 H21D H 0.5711 1.0843 -0.2059 0.061 Uiso 0.40 1 calc PR B 2 H21E H 0.6259 1.1315 -0.1077 0.061 Uiso 0.40 1 calc PR B 2 H21F H 0.4833 1.0423 -0.1337 0.061 Uiso 0.40 1 calc PR B 2 C23A C 0.7821(13) 0.9806(14) -0.1513(11) 0.0405(12) Uiso 0.40 1 d PD B 2 H23D H 0.8334 0.9172 -0.1292 0.061 Uiso 0.40 1 calc PR B 2 H23E H 0.8290 1.0604 -0.1253 0.061 Uiso 0.40 1 calc PR B 2 H23F H 0.7736 0.9827 -0.2142 0.061 Uiso 0.40 1 calc PR B 2 C24 C 0.6434(7) 0.9521(7) -0.1285(5) 0.0393(16) Uani 1 1 d . . . C25 C 0.6412(7) 0.9200(6) -0.0335(5) 0.0287(14) Uani 1 1 d . A . C26 C 0.7556(7) 0.9049(6) 0.0241(5) 0.0320(15) Uani 1 1 d . . . H26 H 0.8375 0.9162 0.0031 0.038 Uiso 1 1 calc R B . C27 C 0.7613(7) 0.8748(6) 0.1095(4) 0.0253(14) Uani 1 1 d . A . C28 C 0.8924(7) 0.8632(6) 0.1665(5) 0.0242(14) Uani 1 1 d . . . C29 C 0.8923(7) 0.8015(6) 0.2428(5) 0.0278(16) Uani 1 1 d . B . H29 H 0.8086 0.7613 0.2549 0.033 Uiso 1 1 calc R . . C30 C 1.0085(7) 0.7954(6) 0.3027(5) 0.0287(16) Uani 1 1 d . . . C31 C 1.1303(7) 0.8531(7) 0.2807(5) 0.0351(18) Uani 1 1 d . B . H31 H 1.2123 0.8512 0.3196 0.042 Uiso 1 1 calc R . . C32 C 1.1335(7) 0.9122(6) 0.2043(5) 0.0276(16) Uani 1 1 d . . . H32 H 1.2177 0.9473 0.1903 0.033 Uiso 1 1 calc R B . C33 C 1.0183(7) 0.9212(6) 0.1487(5) 0.0281(15) Uani 1 1 d . B . H33 H 1.0220 0.9664 0.0978 0.034 Uiso 1 1 calc R . . C34 C 0.9990(7) 0.7279(6) 0.3826(4) 0.0267(15) Uani 1 1 d . A . C35 C 1.0992(8) 0.7626(7) 0.4539(5) 0.0389(18) Uani 1 1 d . . . H35 H 1.1685 0.8301 0.4497 0.047 Uiso 1 1 calc R B . C36 C 1.1032(8) 0.7011(7) 0.5343(5) 0.0343(16) Uani 1 1 d . A . C37 C 1.2194(8) 0.7470(8) 0.6119(5) 0.047(2) Uani 1 1 d . . . C38 C 1.3274(18) 0.6613(14) 0.6091(11) 0.0620(17) Uiso 0.50 1 d PD B 1 H38A H 1.4013 0.6821 0.6587 0.093 Uiso 0.50 1 calc PR B 1 H38B H 1.3628 0.6736 0.5556 0.093 Uiso 0.50 1 calc PR B 1 H38C H 1.2848 0.5755 0.6114 0.093 Uiso 0.50 1 calc PR B 1 C39 C 1.1743(18) 0.7555(18) 0.6863(13) 0.0620(17) Uiso 0.50 1 d PD B 1 H39A H 1.1385 0.6734 0.7036 0.093 Uiso 0.50 1 calc PR B 1 H39B H 1.1030 0.8048 0.6779 0.093 Uiso 0.50 1 calc PR B 1 H39C H 1.2486 0.7946 0.7315 0.093 Uiso 0.50 1 calc PR B 1 C40 C 1.3156(18) 0.8757(14) 0.5911(12) 0.0620(17) Uiso 0.50 1 d PD B 1 H40A H 1.3974 0.8921 0.6356 0.093 Uiso 0.50 1 calc PR B 1 H40B H 1.2663 0.9435 0.5911 0.093 Uiso 0.50 1 calc PR B 1 H40C H 1.3399 0.8673 0.5344 0.093 Uiso 0.50 1 calc PR B 1 C38A C 1.3014(19) 0.6532(15) 0.6322(12) 0.0620(17) Uiso 0.50 1 d PD B 2 H38D H 1.3373 0.6342 0.5813 0.093 Uiso 0.50 1 calc PR B 2 H38E H 1.2462 0.5791 0.6490 0.093 Uiso 0.50 1 calc PR B 2 H38F H 1.3760 0.6829 0.6799 0.093 Uiso 0.50 1 calc PR B 2 C39A C 1.2820(18) 0.8764(14) 0.6067(12) 0.0620(17) Uiso 0.50 1 d PD B 2 H39D H 1.3519 0.9006 0.6580 0.093 Uiso 0.50 1 calc PR B 2 H39E H 1.2133 0.9281 0.6037 0.093 Uiso 0.50 1 calc PR B 2 H39F H 1.3223 0.8865 0.5549 0.093 Uiso 0.50 1 calc PR B 2 C40A C 1.1391(17) 0.7493(17) 0.6946(13) 0.0620(17) Uiso 0.50 1 d PD B 2 H40D H 1.0714 0.6746 0.6920 0.093 Uiso 0.50 1 calc PR B 2 H40E H 1.0950 0.8209 0.6913 0.093 Uiso 0.50 1 calc PR B 2 H40F H 1.2040 0.7538 0.7490 0.093 Uiso 0.50 1 calc PR B 2 C41 C 1.0503(14) 0.1111(12) 0.4373(9) 0.071(3) Uiso 0.80 1 d PD C 1 H41A H 1.0876 0.1243 0.4991 0.106 Uiso 0.40 1 calc PR C 1 H41B H 1.1237 0.1226 0.4047 0.106 Uiso 0.40 1 calc PR C 1 H41C H 0.9989 0.0277 0.4264 0.106 Uiso 0.40 1 calc PR C 1 H41D H 1.0526 0.0587 0.3877 0.106 Uiso 0.40 1 calc PR C 1 H41E H 1.0164 0.0604 0.4821 0.106 Uiso 0.40 1 calc PR C 1 H41F H 1.1412 0.1554 0.4604 0.106 Uiso 0.40 1 calc PR C 1 C41A C 1.067(5) 0.135(5) 0.461(3) 0.071(3) Uiso 0.20 1 d PD C 2 H41G H 1.0844 0.1608 0.5221 0.106 Uiso 0.10 1 calc PR C 2 H41H H 1.1501 0.1543 0.4382 0.106 Uiso 0.10 1 calc PR C 2 H41I H 1.0338 0.0460 0.4553 0.106 Uiso 0.10 1 calc PR C 2 H41J H 1.0945 0.0799 0.4217 0.106 Uiso 0.10 1 calc PR C 2 H41K H 1.0287 0.0864 0.5056 0.106 Uiso 0.10 1 calc PR C 2 H41L H 1.1451 0.1947 0.4884 0.106 Uiso 0.10 1 calc PR C 2 C42 C 0.9568(11) 0.2037(7) 0.4084(8) 0.065(3) Uani 1 1 d D . . C43 C 0.8871(10) 0.2191(7) 0.3326(8) 0.062(3) Uani 1 1 d . C . C44 C 0.8306(8) 0.3269(7) 0.3399(6) 0.0415(19) Uani 1 1 d . . . C45 C 0.7484(7) 0.3871(7) 0.2730(5) 0.0563(18) Uani 1 1 d . C . H45A H 0.7220 0.4571 0.2990 0.084 Uiso 1 1 calc R . . H45B H 0.6677 0.3288 0.2469 0.084 Uiso 1 1 calc R . . H45C H 0.8005 0.4157 0.2285 0.084 Uiso 1 1 calc R . . C46 C 0.8694(9) 0.1433(8) 0.2520(6) 0.074(3) Uani 1 1 d . . . H46A H 0.7722 0.1245 0.2267 0.089 Uiso 1 1 calc R C . H46B H 0.8985 0.0646 0.2677 0.089 Uiso 1 1 calc R . . C47 C 0.9441(7) 0.1988(6) 0.1831(6) 0.057(2) Uani 1 1 d . C . C48 C 1.0809(7) 0.2319(5) 0.2008(5) 0.0487(16) Uani 1 1 d . . . H48 H 1.1265 0.2213 0.2576 0.058 Uiso 1 1 calc R C . C49 C 1.1587(7) 0.2808(5) 0.1401(4) 0.0440(14) Uani 1 1 d . C . C50 C 1.0949(8) 0.3008(6) 0.0616(5) 0.0572(18) Uani 1 1 d . . . H50 H 1.1449 0.3357 0.0199 0.069 Uiso 1 1 calc R C . C51 C 0.9530(10) 0.2703(8) 0.0398(6) 0.078(3) Uani 1 1 d . C . H51 H 0.9073 0.2841 -0.0165 0.094 Uiso 1 1 calc R . . C52 C 0.8818(8) 0.2205(7) 0.1013(7) 0.069(2) Uani 1 1 d . . . H52 H 0.7866 0.2004 0.0865 0.083 Uiso 1 1 calc R C . C53 C 1.3141(7) 0.3119(5) 0.1654(6) 0.0496(16) Uani 1 1 d . . . H53A H 1.3505 0.3604 0.1197 0.060 Uiso 1 1 calc R C . H53B H 1.3396 0.3626 0.2196 0.060 Uiso 1 1 calc R . . C54 C 1.4560(10) 0.2044(8) 0.3464(5) 0.069(2) Uani 1 1 d . C . H54A H 1.4019 0.1468 0.3788 0.104 Uiso 1 1 calc R . . H54B H 1.4291 0.2846 0.3479 0.104 Uiso 1 1 calc R . . H54C H 1.5513 0.2120 0.3725 0.104 Uiso 1 1 calc R . . C55 C 1.4336(8) 0.1575(6) 0.2534(6) 0.0439(18) Uani 1 1 d . . . C56 C 1.3754(8) 0.1987(7) 0.1777(6) 0.047(2) Uani 1 1 d . C . C57 C 1.3842(7) 0.1181(6) 0.1096(5) 0.0384(17) Uani 1 1 d . . . C58 C 1.3372(7) 0.1161(6) 0.0180(4) 0.0499(15) Uani 1 1 d . C . H58A H 1.3624 0.0461 -0.0089 0.075 Uiso 1 1 calc R . . H58B H 1.3781 0.1921 -0.0055 0.075 Uiso 1 1 calc R . . H58C H 1.2391 0.1086 0.0058 0.075 Uiso 1 1 calc R . . O1TA O 0.5034(14) 0.3866(11) -0.0503(8) 0.0801(15) Uiso 0.50 1 d PD D 1 C1TA C 0.612(3) 0.414(2) 0.0248(14) 0.0801(15) Uiso 0.50 1 d PD D 1 H1T1 H 0.6989 0.4099 0.0079 0.096 Uiso 0.50 1 calc PR D 1 H1T2 H 0.5972 0.3524 0.0692 0.096 Uiso 0.50 1 calc PR D 1 C3TA C 0.512(2) 0.5850(18) -0.0078(12) 0.0801(15) Uiso 0.50 1 d PD D 1 H3T1 H 0.4244 0.5789 0.0108 0.096 Uiso 0.50 1 calc PR D 1 H3T2 H 0.5441 0.6711 -0.0209 0.096 Uiso 0.50 1 calc PR D 1 C2TA C 0.614(2) 0.540(2) 0.0609(11) 0.0801(15) Uiso 0.50 1 d PD D 1 H2T1 H 0.7039 0.5915 0.0666 0.096 Uiso 0.50 1 calc PR D 1 H2T2 H 0.5853 0.5362 0.1176 0.096 Uiso 0.50 1 calc PR D 1 C4TA C 0.501(2) 0.5062(15) -0.0801(11) 0.0801(15) Uiso 0.50 1 d PD D 1 H4T1 H 0.4165 0.5082 -0.1212 0.096 Uiso 0.50 1 calc PR D 1 H4T2 H 0.5775 0.5325 -0.1102 0.096 Uiso 0.50 1 calc PR D 1 O1TB O 0.5792(14) 0.4088(12) -0.0460(8) 0.0801(15) Uiso 0.50 1 d PD E 2 C1TB C 0.631(3) 0.421(2) 0.0446(11) 0.0801(15) Uiso 0.50 1 d PD E 2 H1T3 H 0.7301 0.4266 0.0550 0.096 Uiso 0.50 1 calc PR E 2 H1T4 H 0.5924 0.3475 0.0732 0.096 Uiso 0.50 1 calc PR E 2 C3TB C 0.498(2) 0.5694(18) 0.0105(12) 0.0801(15) Uiso 0.50 1 d PD E 2 H3T3 H 0.4162 0.5812 0.0321 0.096 Uiso 0.50 1 calc PR E 2 H3T4 H 0.5364 0.6474 -0.0131 0.096 Uiso 0.50 1 calc PR E 2 C2TB C 0.598(2) 0.532(2) 0.0818(11) 0.0801(15) Uiso 0.50 1 d PD E 2 H2T3 H 0.6784 0.5969 0.0969 0.096 Uiso 0.50 1 calc PR E 2 H2T4 H 0.5582 0.5128 0.1339 0.096 Uiso 0.50 1 calc PR E 2 C4TB C 0.4640(17) 0.4737(18) -0.0554(11) 0.0801(15) Uiso 0.50 1 d PD E 2 H4T3 H 0.4482 0.5087 -0.1133 0.096 Uiso 0.50 1 calc PR E 2 H4T4 H 0.3815 0.4166 -0.0482 0.096 Uiso 0.50 1 calc PR E 2 O2TA O 1.063(2) 0.242(2) 0.6587(13) 0.083(2) Uiso 0.30 1 d PD F 1 C6TA C 1.096(3) 0.239(3) 0.8178(16) 0.083(2) Uiso 0.30 1 d PD F 1 H6T1 H 1.0931 0.1792 0.8641 0.100 Uiso 0.30 1 calc PR F 1 H6T2 H 1.0667 0.3138 0.8362 0.100 Uiso 0.30 1 calc PR F 1 C7TA C 1.233(2) 0.269(3) 0.7965(16) 0.083(2) Uiso 0.30 1 d PD F 1 H7T1 H 1.2842 0.3462 0.8262 0.100 Uiso 0.30 1 calc PR F 1 H7T2 H 1.2843 0.2022 0.8125 0.100 Uiso 0.30 1 calc PR F 1 C8TA C 1.205(2) 0.281(3) 0.7037(15) 0.083(2) Uiso 0.30 1 d PD F 1 H8T1 H 1.2617 0.2334 0.6780 0.100 Uiso 0.30 1 calc PR F 1 H8T2 H 1.2341 0.3684 0.6914 0.100 Uiso 0.30 1 calc PR F 1 C5TA C 1.012(2) 0.186(3) 0.7350(15) 0.083(2) Uiso 0.30 1 d PD F 1 H5T1 H 0.9184 0.1994 0.7326 0.100 Uiso 0.30 1 calc PR F 1 H5T2 H 1.0100 0.0969 0.7326 0.100 Uiso 0.30 1 calc PR F 1 C6TB C 1.132(3) 0.2818(18) 0.8027(13) 0.083(2) Uiso 0.40 1 d PD G 2 H6T3 H 1.0445 0.2761 0.8219 0.100 Uiso 0.40 1 calc PR G 2 H6T4 H 1.2044 0.3218 0.8496 0.100 Uiso 0.40 1 calc PR G 2 C7TB C 1.155(3) 0.1530(17) 0.7785(13) 0.083(2) Uiso 0.40 1 d PD G 2 H7T3 H 1.2517 0.1466 0.7926 0.100 Uiso 0.40 1 calc PR G 2 H7T4 H 1.1023 0.0874 0.8069 0.100 Uiso 0.40 1 calc PR G 2 C5TB C 1.132(3) 0.3489(18) 0.7252(12) 0.083(2) Uiso 0.40 1 d PD G 2 H5T3 H 1.0573 0.3957 0.7183 0.100 Uiso 0.40 1 calc PR G 2 H5T4 H 1.2169 0.4088 0.7320 0.100 Uiso 0.40 1 calc PR G 2 C8TB C 1.106(3) 0.1508(17) 0.6844(12) 0.083(2) Uiso 0.40 1 d PD G 2 H8T3 H 1.0101 0.1102 0.6716 0.100 Uiso 0.40 1 calc PR G 2 H8T4 H 1.1573 0.1019 0.6552 0.100 Uiso 0.40 1 calc PR G 2 O2TB O 1.1182(18) 0.2775(14) 0.6487(10) 0.083(2) Uiso 0.40 1 d PD G 2 C9T C 1.7038(18) -0.1218(18) 0.4061(10) 0.084(2) Uiso 0.50 1 d PD I . H9T1 H 1.7828 -0.0785 0.3839 0.100 Uiso 0.50 1 calc PR . . H9T2 H 1.6706 -0.2010 0.3735 0.100 Uiso 0.50 1 calc PR . . O3T O 1.6016(13) -0.0501(12) 0.3963(8) 0.084(2) Uiso 0.50 1 d PD . . C10T C 1.7429(19) -0.1433(19) 0.5032(11) 0.084(2) Uiso 0.50 1 d PD . . H10A H 1.7598 -0.2275 0.5138 0.100 Uiso 0.50 1 calc PR H 1 H10B H 1.8228 -0.0837 0.5309 0.100 Uiso 0.50 1 calc PR H 1 C11T C 1.623(3) -0.124(4) 0.5321(14) 0.084(2) Uiso 0.25 1 d PD I 1 H11A H 1.6433 -0.0506 0.5715 0.100 Uiso 0.25 1 calc PR I 1 H11B H 1.5869 -0.1954 0.5634 0.100 Uiso 0.25 1 calc PR I 1 C12T C 1.525(2) -0.106(3) 0.4555(17) 0.084(2) Uiso 0.25 1 d PD I 1 H12A H 1.4713 -0.1856 0.4316 0.100 Uiso 0.25 1 calc PR I 1 H12B H 1.4640 -0.0529 0.4697 0.100 Uiso 0.25 1 calc PR I 1 C14T C 1.633(4) 0.025(3) 0.4800(16) 0.084(2) Uiso 0.25 1 d PD I 2 H14A H 1.6759 0.1096 0.4700 0.100 Uiso 0.25 1 calc PR I 2 H14B H 1.5486 0.0289 0.5006 0.100 Uiso 0.25 1 calc PR I 2 C13T C 1.721(4) -0.028(3) 0.5439(15) 0.084(2) Uiso 0.25 1 d PD I 2 H13A H 1.6797 -0.0463 0.5954 0.100 Uiso 0.25 1 calc PR I 2 H13B H 1.8074 0.0295 0.5616 0.100 Uiso 0.25 1 calc PR I 2 N1 N 0.8698(6) 0.3731(6) 0.4206(5) 0.0369(16) Uani 1 1 d . A . N2 N 0.9425(8) 0.2987(6) 0.4587(5) 0.054(2) Uani 1 1 d . A . H2 H 0.9804 0.3084 0.5137 0.065 Uiso 1 1 calc R . . N3 N 1.4538(6) 0.0293(6) 0.1476(4) 0.0371(16) Uani 1 1 d . . . N4 N 1.4790(6) 0.0544(6) 0.2346(4) 0.0403(15) Uani 1 1 d . . . H4 H 1.5194 0.0096 0.2734 0.048 Uiso 1 1 calc R . . O1 O 0.7921(6) 0.4811(5) 0.5782(4) 0.0391(13) Uani 1 1 d . . . O2 O 0.6571(5) 0.5513(5) 0.4203(4) 0.0357(13) Uani 1 1 d . . . O3 O 0.4239(5) 0.7534(4) 0.1874(3) 0.0287(12) Uani 1 1 d . . . O4 O 0.2936(5) 0.8043(5) 0.0233(3) 0.0350(12) Uani 1 1 d . . . O5 O 0.5257(5) 0.9066(5) -0.0149(3) 0.0332(12) Uani 1 1 d . . . O6 O 0.6589(5) 0.8527(5) 0.1465(3) 0.0264(11) Uani 1 1 d . . . O7 O 0.8949(5) 0.6446(4) 0.3787(3) 0.0312(12) Uani 1 1 d . . . O8 O 1.0213(5) 0.6080(5) 0.5458(4) 0.0406(14) Uani 1 1 d . . . Cu1 Cu 0.84454(5) 0.55171(5) 0.47559(4) 0.0306(2) Uani 1 1 d . A . Cu2 Cu 0.47433(5) 0.84933(5) 0.09239(4) 0.0289(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C4 0.039(4) 0.109(8) 0.044(5) 0.032(5) 0.007(3) 0.013(4) C5 0.037(4) 0.031(3) 0.038(4) 0.005(3) 0.012(3) 0.005(3) C6 0.026(3) 0.051(4) 0.032(4) 0.012(3) 0.008(3) -0.002(3) C7 0.026(3) 0.025(3) 0.029(4) -0.002(3) 0.013(3) -0.001(2) C8 0.025(3) 0.026(3) 0.025(3) 0.003(2) 0.006(3) 0.003(2) C9 0.021(3) 0.023(3) 0.028(4) 0.004(3) 0.008(3) 0.003(2) C10 0.021(3) 0.022(3) 0.023(4) -0.003(3) 0.004(3) 0.004(3) C11 0.022(3) 0.028(3) 0.026(4) 0.007(3) 0.004(3) 0.009(3) C12 0.025(4) 0.044(4) 0.037(5) -0.004(4) 0.007(3) 0.000(3) C13 0.024(4) 0.035(4) 0.036(4) 0.009(3) 0.010(3) -0.002(3) C14 0.020(3) 0.022(3) 0.040(4) -0.003(3) 0.011(3) 0.006(3) C15 0.021(3) 0.028(3) 0.021(3) -0.002(2) -0.004(3) -0.003(2) C16 0.018(3) 0.036(3) 0.032(3) -0.006(3) 0.008(2) 0.008(2) C17 0.029(3) 0.047(4) 0.028(3) -0.001(3) 0.000(2) 0.007(3) C18 0.053(4) 0.047(4) 0.037(3) -0.006(3) -0.001(3) 0.012(3) C19 0.034(3) 0.047(3) 0.037(3) 0.004(3) -0.010(2) 0.011(2) C20 0.021(2) 0.063(4) 0.040(3) 0.003(3) -0.006(2) 0.000(2) C24 0.027(3) 0.056(4) 0.033(3) 0.008(3) 0.004(2) 0.004(3) C25 0.032(3) 0.029(3) 0.025(3) 0.004(2) 0.006(2) 0.006(2) C26 0.029(3) 0.036(3) 0.034(3) 0.007(3) 0.011(3) 0.007(2) C27 0.026(3) 0.020(3) 0.030(4) 0.003(2) 0.001(3) 0.008(2) C28 0.023(3) 0.019(3) 0.029(4) -0.006(2) 0.006(3) 0.000(2) C29 0.025(4) 0.026(3) 0.033(4) -0.002(3) 0.008(3) 0.003(3) C30 0.023(4) 0.023(3) 0.040(4) 0.003(3) 0.008(3) 0.004(3) C31 0.017(3) 0.039(4) 0.045(5) -0.015(4) 0.002(3) 0.000(3) C32 0.018(3) 0.027(3) 0.038(4) 0.005(3) 0.013(3) -0.001(3) C33 0.033(4) 0.025(3) 0.028(4) -0.002(3) 0.012(3) 0.003(3) C34 0.021(3) 0.033(4) 0.024(4) 0.003(3) 0.000(3) 0.006(3) C35 0.033(4) 0.039(4) 0.045(5) 0.008(3) 0.008(3) 0.005(3) C36 0.032(4) 0.039(4) 0.030(4) 0.001(3) 0.000(3) 0.008(3) C37 0.044(4) 0.062(5) 0.027(3) -0.002(3) -0.005(3) -0.005(3) C42 0.078(6) 0.029(4) 0.105(8) 0.020(4) 0.057(6) 0.018(4) C43 0.058(5) 0.033(4) 0.102(8) -0.017(5) 0.056(6) -0.016(4) C44 0.029(3) 0.033(3) 0.062(5) -0.003(3) 0.024(3) -0.011(3) C45 0.043(3) 0.061(4) 0.060(4) -0.023(3) 0.012(3) -0.005(3) C46 0.074(6) 0.052(5) 0.103(7) -0.028(5) 0.059(5) -0.015(4) C47 0.050(4) 0.033(3) 0.092(6) -0.028(4) 0.022(4) 0.004(3) C48 0.052(3) 0.030(3) 0.071(4) -0.009(3) 0.031(3) 0.005(3) C49 0.056(4) 0.022(3) 0.061(4) 0.000(2) 0.026(3) 0.012(2) C50 0.074(5) 0.042(4) 0.067(5) 0.010(3) 0.027(4) 0.026(3) C51 0.090(6) 0.060(5) 0.081(6) -0.015(4) -0.015(5) 0.038(5) C52 0.048(4) 0.050(4) 0.116(8) -0.025(5) 0.024(5) 0.017(3) C53 0.047(4) 0.027(3) 0.077(5) 0.005(3) 0.021(4) 0.004(3) C54 0.094(7) 0.063(5) 0.056(5) -0.008(4) 0.022(4) 0.019(5) C55 0.037(4) 0.029(3) 0.068(5) -0.006(3) 0.022(3) -0.001(3) C56 0.046(4) 0.029(4) 0.072(5) 0.000(3) 0.033(4) 0.000(3) C57 0.035(3) 0.024(3) 0.061(5) 0.012(3) 0.020(3) 0.007(3) C58 0.064(4) 0.044(3) 0.054(4) 0.013(3) 0.021(3) 0.031(3) N1 0.024(3) 0.032(3) 0.060(5) 0.008(3) 0.017(3) 0.011(3) N2 0.066(5) 0.039(3) 0.075(5) 0.017(3) 0.047(4) 0.018(3) N3 0.032(4) 0.034(3) 0.045(4) -0.004(3) 0.013(3) -0.001(3) N4 0.029(3) 0.042(3) 0.048(4) -0.007(3) 0.006(3) 0.002(2) O1 0.034(3) 0.050(3) 0.037(3) 0.019(2) 0.010(2) 0.014(2) O2 0.028(3) 0.041(3) 0.038(3) 0.013(2) 0.006(2) 0.006(2) O3 0.014(2) 0.035(3) 0.034(3) 0.006(2) 0.002(2) -0.0030(19) O4 0.027(3) 0.045(3) 0.031(3) 0.012(2) 0.006(2) 0.001(2) O5 0.021(3) 0.047(3) 0.031(3) 0.007(2) 0.005(2) 0.006(2) O6 0.017(2) 0.044(3) 0.020(2) 0.005(2) 0.0061(19) 0.005(2) O7 0.031(3) 0.034(3) 0.026(3) 0.005(2) 0.001(2) 0.003(2) O8 0.032(3) 0.042(3) 0.041(3) 0.012(2) -0.008(2) 0.005(2) Cu1 0.0255(4) 0.0355(4) 0.0309(5) 0.0062(4) 0.0058(4) 0.0053(3) Cu2 0.0201(4) 0.0345(4) 0.0321(5) 0.0079(3) 0.0047(3) 0.0048(3) _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 C1 C4 1.680(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.457(15) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.468(18) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1A C4 1.509(17) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2A C4 1.591(17) . ? C2A H2A1 0.9800 . ? C2A H2A2 0.9800 . ? C2A H2A3 0.9800 . ? C3A C4 1.498(17) . ? C3A H3A1 0.9800 . ? C3A H3A2 0.9800 . ? C3A H3A3 0.9800 . ? C4 C5 1.555(11) . ? C5 O1 1.296(9) . ? C5 C6 1.378(11) . ? C6 C7 1.412(10) . ? C6 H6 0.9500 . ? C7 O2 1.262(8) . ? C7 C8 1.500(9) . ? C8 C13 1.392(9) . ? C8 C9 1.396(9) . ? C9 C10 1.403(9) . ? C9 H9 0.9500 . ? C10 C11 1.411(9) . ? C10 C14 1.503(9) . ? C11 C12 1.390(10) . ? C11 H11 0.9500 . ? C12 C13 1.416(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O3 1.279(8) . ? C14 C15 1.412(9) . ? C15 C16 1.369(10) . ? C15 H15 0.9500 . ? C16 O4 1.286(8) . ? C16 C17 1.513(9) . ? C17 C18 1.528(9) . ? C17 C20 1.545(9) . ? C17 C19 1.566(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.464(12) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.597(12) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.574(12) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22A C24 1.502(15) . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C21A C24 1.517(16) . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C23A C24 1.515(15) . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24 C25 1.543(10) . ? C25 O5 1.259(9) . ? C25 C26 1.383(10) . ? C26 C27 1.382(10) . ? C26 H26 0.9500 . ? C27 O6 1.282(8) . ? C27 C28 1.502(9) . ? C28 C29 1.387(10) . ? C28 C33 1.417(9) . ? C29 C30 1.391(10) . ? C29 H29 0.9500 . ? C30 C31 1.406(9) . ? C30 C34 1.477(10) . ? C31 C32 1.376(11) . ? C31 H31 0.9500 . ? C32 C33 1.357(9) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 O7 1.278(8) . ? C34 C35 1.380(10) . ? C35 C36 1.439(11) . ? C35 H35 0.9500 . ? C36 O8 1.249(9) . ? C36 C37 1.557(10) . ? C37 C39 1.349(18) . ? C37 C38A 1.453(17) . ? C37 C39A 1.477(17) . ? C37 C38 1.592(17) . ? C37 C40 1.658(17) . ? C37 C40A 1.670(17) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40A H40D 0.9800 . ? C40A H40E 0.9800 . ? C40A H40F 0.9800 . ? C41 C42 1.543(13) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 H41D 0.9800 . ? C41 H41E 0.9800 . ? C41 H41F 0.9800 . ? C41A C42 1.588(19) . ? C41A H41G 0.9800 . ? C41A H41H 0.9800 . ? C41A H41I 0.9800 . ? C41A H41J 0.9800 . ? C41A H41K 0.9800 . ? C41A H41L 0.9800 . ? C42 C43 1.304(15) . ? C42 N2 1.363(11) . ? C43 C44 1.434(12) . ? C43 C46 1.488(12) . ? C44 N1 1.335(10) . ? C44 C45 1.465(12) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.516(11) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.366(9) . ? C47 C52 1.371(12) . ? C48 C49 1.407(9) . ? C48 H48 0.9500 . ? C49 C50 1.328(10) . ? C49 C53 1.550(9) . ? C50 C51 1.415(12) . ? C50 H50 0.9500 . ? C51 C52 1.380(13) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C56 1.500(10) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.519(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.353(12) . ? C55 N4 1.362(10) . ? C56 C57 1.423(11) . ? C57 N3 1.391(10) . ? C57 C58 1.435(10) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O1TA C4TA 1.411(15) . ? O1TA C1TA 1.458(16) . ? C1TA C2TA 1.504(16) . ? C1TA H1T1 0.9900 . ? C1TA H1T2 0.9900 . ? C3TA C4TA 1.413(16) . ? C3TA C2TA 1.513(16) . ? C3TA H3T1 0.9900 . ? C3TA H3T2 0.9900 . ? C2TA H2T1 0.9900 . ? C2TA H2T2 0.9900 . ? C4TA H4T1 0.9900 . ? C4TA H4T2 0.9900 . ? O1TB C1TB 1.427(16) . ? O1TB C4TB 1.476(15) . ? C1TB C2TB 1.486(16) . ? C1TB H1T3 0.9900 . ? C1TB H1T4 0.9900 . ? C3TB C4TB 1.436(16) . ? C3TB C2TB 1.491(16) . ? C3TB H3T3 0.9900 . ? C3TB H3T4 0.9900 . ? C2TB H2T3 0.9900 . ? C2TB H2T4 0.9900 . ? C4TB H4T3 0.9900 . ? C4TB H4T4 0.9900 . ? O2TA C5TA 1.491(18) . ? O2TA C8TA 1.495(18) . ? C6TA C5TA 1.484(18) . ? C6TA C7TA 1.490(18) . ? C6TA H6T1 0.9900 . ? C6TA H6T2 0.9900 . ? C7TA C8TA 1.450(18) . ? C7TA H7T1 0.9900 . ? C7TA H7T2 0.9900 . ? C8TA H8T1 0.9900 . ? C8TA H8T2 0.9900 . ? C5TA H5T1 0.9900 . ? C5TA H5T2 0.9900 . ? C6TB C5TB 1.433(17) . ? C6TB C7TB 1.552(17) . ? C6TB H6T3 0.9900 . ? C6TB H6T4 0.9900 . ? C7TB C8TB 1.477(17) . ? C7TB H7T3 0.9900 . ? C7TB H7T4 0.9900 . ? C5TB O2TB 1.413(16) . ? C5TB H5T3 0.9900 . ? C5TB H5T4 0.9900 . ? C8TB O2TB 1.510(17) . ? C8TB H8T3 0.9900 . ? C8TB H8T4 0.9900 . ? C9T O3T 1.415(15) . ? C9T C10T 1.540(15) . ? C9T H9T1 0.9900 . ? C9T H9T2 0.9900 . ? O3T C12T 1.405(18) . ? O3T C14T 1.512(18) . ? C10T C11T 1.442(17) . ? C10T C13T 1.506(17) . ? C10T H10A 0.9900 . ? C10T H10B 0.9900 . ? C11T C12T 1.458(18) . ? C11T H11A 0.9900 . ? C11T H11B 0.9900 . ? C12T H12A 0.9900 . ? C12T H12B 0.9900 . ? C14T C13T 1.423(18) . ? C14T H14A 0.9900 . ? C14T H14B 0.9900 . ? C13T H13A 0.9900 . ? C13T H13B 0.9900 . ? N1 N2 1.288(10) . ? N1 Cu1 2.239(6) . ? N2 H2 0.8800 . ? N3 N4 1.367(9) . ? N3 Cu2 2.238(6) 1_645 ? N4 H4 0.8800 . ? O1 Cu1 1.925(5) . ? O2 Cu1 1.963(5) . ? O3 Cu2 1.936(5) . ? O4 Cu2 1.953(5) . ? O5 Cu2 1.939(5) . ? O6 Cu2 1.926(5) . ? O7 Cu1 1.943(5) . ? O8 Cu1 1.943(5) . ? Cu2 N3 2.238(6) 1_465 ? 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 C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? C4 C1A H1A1 109.5 . . ? C4 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C4 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C4 C2A H2A1 109.5 . . ? C4 C2A H2A2 109.5 . . ? H2A1 C2A H2A2 109.5 . . ? C4 C2A H2A3 109.5 . . ? H2A1 C2A H2A3 109.5 . . ? H2A2 C2A H2A3 109.5 . . ? C4 C3A H3A1 109.5 . . ? C4 C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C4 C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C2 C4 C3 115.8(11) . . ? C2 C4 C3A 129.4(12) . . ? C2 C4 C1A 66.8(9) . . ? C3 C4 C1A 123.4(13) . . ? C3A C4 C1A 113.5(11) . . ? C2 C4 C5 110.6(9) . . ? C3 C4 C5 116.3(11) . . ? C3A C4 C5 113.8(10) . . ? C1A C4 C5 113.7(10) . . ? C3 C4 C2A 90.6(11) . . ? C3A C4 C2A 108.8(11) . . ? C1A C4 C2A 103.3(10) . . ? C5 C4 C2A 102.4(9) . . ? C2 C4 C1 103.3(9) . . ? C3 C4 C1 107.5(10) . . ? C3A C4 C1 90.7(10) . . ? C5 C4 C1 101.4(9) . . ? C2A C4 C1 139.4(10) . . ? O1 C5 C6 125.2(7) . . ? O1 C5 C4 114.7(7) . . ? C6 C5 C4 120.0(7) . . ? C5 C6 C7 124.0(7) . . ? C5 C6 H6 118.0 . . ? C7 C6 H6 118.0 . . ? O2 C7 C6 125.8(7) . . ? O2 C7 C8 114.4(6) . . ? C6 C7 C8 119.8(6) . . ? C13 C8 C9 119.9(6) . . ? C13 C8 C7 122.6(6) . . ? C9 C8 C7 117.4(6) . . ? C8 C9 C10 119.8(6) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.5(6) . . ? C9 C10 C14 118.7(6) . . ? C11 C10 C14 120.8(6) . . ? C12 C11 C10 119.4(6) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 119.9(7) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 120.4(7) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? O3 C14 C15 123.9(7) . . ? O3 C14 C10 115.3(6) . . ? C15 C14 C10 120.9(6) . . ? C16 C15 C14 125.3(6) . . ? C16 C15 H15 117.3 . . ? C14 C15 H15 117.3 . . ? O4 C16 C15 125.1(6) . . ? O4 C16 C17 113.8(6) . . ? C15 C16 C17 121.1(6) . . ? C16 C17 C18 107.8(5) . . ? C16 C17 C20 113.2(6) . . ? C18 C17 C20 110.1(6) . . ? C16 C17 C19 109.3(6) . . ? C18 C17 C19 108.5(6) . . ? C20 C17 C19 107.9(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 H21A 109.5 . . ? C24 C21 H21B 109.5 . . ? C24 C21 H21C 109.5 . . ? C24 C22 H22A 109.5 . . ? C24 C22 H22B 109.5 . . ? C24 C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? C24 C22A H22D 109.5 . . ? C24 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C24 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C24 C21A H21D 109.5 . . ? C24 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C24 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C24 C23A H23D 109.5 . . ? C24 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C24 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C21 C24 C22A 84.3(8) . . ? C21 C24 C23A 122.5(9) . . ? C22A C24 C23A 108.7(9) . . ? C22A C24 C21A 110.2(9) . . ? C23A C24 C21A 109.5(9) . . ? C21 C24 C25 113.6(7) . . ? C22A C24 C25 106.7(8) . . ? C23A C24 C25 115.1(9) . . ? C21A C24 C25 106.6(9) . . ? C21 C24 C23 111.1(8) . . ? C22A C24 C23 125.1(9) . . ? C21A C24 C23 93.2(8) . . ? C25 C24 C23 113.0(7) . . ? C21 C24 C22 106.4(7) . . ? C23A C24 C22 88.3(8) . . ? C21A C24 C22 131.3(9) . . ? C25 C24 C22 105.5(6) . . ? C23 C24 C22 106.6(7) . . ? O5 C25 C26 124.0(6) . . ? O5 C25 C24 113.5(6) . . ? C26 C25 C24 122.5(6) . . ? C27 C26 C25 125.8(7) . . ? C27 C26 H26 117.1 . . ? C25 C26 H26 117.1 . . ? O6 C27 C26 124.4(6) . . ? O6 C27 C28 114.6(6) . . ? C26 C27 C28 121.0(6) . . ? C29 C28 C33 117.7(7) . . ? C29 C28 C27 119.8(6) . . ? C33 C28 C27 122.4(6) . . ? C28 C29 C30 123.4(7) . . ? C28 C29 H29 118.3 . . ? C30 C29 H29 118.3 . . ? C29 C30 C31 116.2(7) . . ? C29 C30 C34 119.8(6) . . ? C31 C30 C34 124.0(7) . . ? C32 C31 C30 121.5(7) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C33 C32 C31 121.1(6) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C28 120.0(7) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? O7 C34 C35 126.6(7) . . ? O7 C34 C30 115.5(6) . . ? C35 C34 C30 117.9(6) . . ? C34 C35 C36 122.9(7) . . ? C34 C35 H35 118.6 . . ? C36 C35 H35 118.6 . . ? O8 C36 C35 124.0(7) . . ? O8 C36 C37 116.4(7) . . ? C35 C36 C37 119.5(7) . . ? C39 C37 C38A 100.8(12) . . ? C39 C37 C39A 98.7(12) . . ? C38A C37 C39A 120.9(11) . . ? C39 C37 C36 112.3(11) . . ? C38A C37 C36 109.5(10) . . ? C39A C37 C36 113.3(10) . . ? C39 C37 C38 117.6(12) . . ? C39A C37 C38 109.9(11) . . ? C36 C37 C38 105.3(9) . . ? C39 C37 C40 112.4(11) . . ? C38A C37 C40 109.3(11) . . ? C36 C37 C40 111.9(9) . . ? C38 C37 C40 96.2(9) . . ? C38A C37 C40A 104.6(10) . . ? C39A C37 C40A 103.2(10) . . ? C36 C37 C40A 103.1(9) . . ? C38 C37 C40A 122.1(10) . . ? C40 C37 C40A 117.9(10) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? C37 C38A H38D 109.5 . . ? C37 C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37 C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C37 C39A H39D 109.5 . . ? C37 C39A H39E 109.5 . . ? H39D C39A H39E 109.5 . . ? C37 C39A H39F 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C37 C40A H40D 109.5 . . ? C37 C40A H40E 109.5 . . ? H40D C40A H40E 109.5 . . ? C37 C40A H40F 109.5 . . ? H40D C40A H40F 109.5 . . ? H40E C40A H40F 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C42 C41 H41D 109.5 . . ? H41A C41 H41D 141.1 . . ? H41B C41 H41D 56.3 . . ? H41C C41 H41D 56.3 . . ? C42 C41 H41E 109.5 . . ? H41A C41 H41E 56.3 . . ? H41B C41 H41E 141.1 . . ? H41C C41 H41E 56.3 . . ? H41D C41 H41E 109.5 . . ? C42 C41 H41F 109.5 . . ? H41A C41 H41F 56.3 . . ? H41B C41 H41F 56.3 . . ? H41C C41 H41F 141.1 . . ? H41D C41 H41F 109.5 . . ? H41E C41 H41F 109.5 . . ? C42 C41A H41G 109.5 . . ? C42 C41A H41H 109.5 . . ? H41G C41A H41H 109.5 . . ? C42 C41A H41I 109.5 . . ? H41G C41A H41I 109.5 . . ? H41H C41A H41I 109.5 . . ? C42 C41A H41J 109.5 . . ? H41G C41A H41J 141.1 . . ? H41H C41A H41J 56.3 . . ? H41I C41A H41J 56.3 . . ? C42 C41A H41K 109.5 . . ? H41G C41A H41K 56.3 . . ? H41H C41A H41K 141.1 . . ? H41I C41A H41K 56.3 . . ? H41J C41A H41K 109.5 . . ? C42 C41A H41L 109.5 . . ? H41G C41A H41L 56.3 . . ? H41H C41A H41L 56.3 . . ? H41I C41A H41L 141.1 . . ? H41J C41A H41L 109.5 . . ? H41K C41A H41L 109.5 . . ? C43 C42 N2 104.7(8) . . ? C43 C42 C41 130.2(10) . . ? N2 C42 C41 124.7(11) . . ? C43 C42 C41A 146(2) . . ? N2 C42 C41A 109(2) . . ? C42 C43 C44 106.8(8) . . ? C42 C43 C46 128.1(10) . . ? C44 C43 C46 125.1(11) . . ? N1 C44 C43 108.9(8) . . ? N1 C44 C45 121.9(7) . . ? C43 C44 C45 129.1(8) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 C47 116.3(6) . . ? C43 C46 H46A 108.2 . . ? C47 C46 H46A 108.2 . . ? C43 C46 H46B 108.2 . . ? C47 C46 H46B 108.2 . . ? H46A C46 H46B 107.4 . . ? C48 C47 C52 116.1(7) . . ? C48 C47 C46 120.3(8) . . ? C52 C47 C46 123.6(7) . . ? C47 C48 C49 124.1(8) . . ? C47 C48 H48 117.9 . . ? C49 C48 H48 117.9 . . ? C50 C49 C48 118.1(7) . . ? C50 C49 C53 121.5(6) . . ? C48 C49 C53 120.4(7) . . ? C49 C50 C51 120.4(7) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 119.1(8) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C47 C52 C51 122.2(8) . . ? C47 C52 H52 118.9 . . ? C51 C52 H52 118.9 . . ? C56 C53 C49 111.8(5) . . ? C56 C53 H53A 109.3 . . ? C49 C53 H53A 109.3 . . ? C56 C53 H53B 109.3 . . ? C49 C53 H53B 109.3 . . ? H53A C53 H53B 107.9 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 N4 107.0(7) . . ? C56 C55 C54 133.0(7) . . ? N4 C55 C54 119.9(8) . . ? C55 C56 C57 108.7(7) . . ? C55 C56 C53 126.6(8) . . ? C57 C56 C53 124.7(8) . . ? N3 C57 C56 106.6(7) . . ? N3 C57 C58 121.0(7) . . ? C56 C57 C58 132.4(7) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C4TA O1TA C1TA 99.6(14) . . ? O1TA C1TA C2TA 109.1(13) . . ? O1TA C1TA H1T1 109.9 . . ? C2TA C1TA H1T1 109.9 . . ? O1TA C1TA H1T2 109.9 . . ? C2TA C1TA H1T2 109.9 . . ? H1T1 C1TA H1T2 108.3 . . ? C4TA C3TA C2TA 104.0(12) . . ? C4TA C3TA H3T1 111.0 . . ? C2TA C3TA H3T1 111.0 . . ? C4TA C3TA H3T2 111.0 . . ? C2TA C3TA H3T2 111.0 . . ? H3T1 C3TA H3T2 109.0 . . ? C1TA C2TA C3TA 101.1(11) . . ? C1TA C2TA H2T1 111.6 . . ? C3TA C2TA H2T1 111.6 . . ? C1TA C2TA H2T2 111.6 . . ? C3TA C2TA H2T2 111.6 . . ? H2T1 C2TA H2T2 109.4 . . ? O1TA C4TA C3TA 107.9(14) . . ? O1TA C4TA H4T1 110.1 . . ? C3TA C4TA H4T1 110.1 . . ? O1TA C4TA H4T2 110.1 . . ? C3TA C4TA H4T2 110.1 . . ? H4T1 C4TA H4T2 108.4 . . ? C1TB O1TB C4TB 102.7(14) . . ? O1TB C1TB C2TB 110.4(13) . . ? O1TB C1TB H1T3 109.6 . . ? C2TB C1TB H1T3 109.6 . . ? O1TB C1TB H1T4 109.6 . . ? C2TB C1TB H1T4 109.6 . . ? H1T3 C1TB H1T4 108.1 . . ? C4TB C3TB C2TB 107.5(12) . . ? C4TB C3TB H3T3 110.2 . . ? C2TB C3TB H3T3 110.2 . . ? C4TB C3TB H3T4 110.2 . . ? C2TB C3TB H3T4 110.2 . . ? H3T3 C3TB H3T4 108.5 . . ? C1TB C2TB C3TB 103.0(11) . . ? C1TB C2TB H2T3 111.2 . . ? C3TB C2TB H2T3 111.2 . . ? C1TB C2TB H2T4 111.2 . . ? C3TB C2TB H2T4 111.2 . . ? H2T3 C2TB H2T4 109.1 . . ? C3TB C4TB O1TB 106.9(13) . . ? C3TB C4TB H4T3 110.3 . . ? O1TB C4TB H4T3 110.3 . . ? C3TB C4TB H4T4 110.3 . . ? O1TB C4TB H4T4 110.3 . . ? H4T3 C4TB H4T4 108.6 . . ? C5TA O2TA C8TA 96.2(17) . . ? C5TA C6TA C7TA 102.9(14) . . ? C5TA C6TA H6T1 111.2 . . ? C7TA C6TA H6T1 111.2 . . ? C5TA C6TA H6T2 111.2 . . ? C7TA C6TA H6T2 111.2 . . ? H6T1 C6TA H6T2 109.1 . . ? C8TA C7TA C6TA 102.9(14) . . ? C8TA C7TA H7T1 111.2 . . ? C6TA C7TA H7T1 111.2 . . ? C8TA C7TA H7T2 111.2 . . ? C6TA C7TA H7T2 111.2 . . ? H7T1 C7TA H7T2 109.1 . . ? C7TA C8TA O2TA 116.8(17) . . ? C7TA C8TA H8T1 108.1 . . ? O2TA C8TA H8T1 108.1 . . ? C7TA C8TA H8T2 108.1 . . ? O2TA C8TA H8T2 108.1 . . ? H8T1 C8TA H8T2 107.3 . . ? C6TA C5TA O2TA 112.3(19) . . ? C6TA C5TA H5T1 109.2 . . ? O2TA C5TA H5T1 109.2 . . ? C6TA C5TA H5T2 109.2 . . ? O2TA C5TA H5T2 109.2 . . ? H5T1 C5TA H5T2 107.9 . . ? C5TB C6TB C7TB 105.0(13) . . ? C5TB C6TB H6T3 110.7 . . ? C7TB C6TB H6T3 110.7 . . ? C5TB C6TB H6T4 110.7 . . ? C7TB C6TB H6T4 110.7 . . ? H6T3 C6TB H6T4 108.8 . . ? C8TB C7TB C6TB 99.4(11) . . ? C8TB C7TB H7T3 111.9 . . ? C6TB C7TB H7T3 111.9 . . ? C8TB C7TB H7T4 111.9 . . ? C6TB C7TB H7T4 111.9 . . ? H7T3 C7TB H7T4 109.6 . . ? O2TB C5TB C6TB 115.5(15) . . ? O2TB C5TB H5T3 108.4 . . ? C6TB C5TB H5T3 108.4 . . ? O2TB C5TB H5T4 108.4 . . ? C6TB C5TB H5T4 108.4 . . ? H5T3 C5TB H5T4 107.5 . . ? C7TB C8TB O2TB 112.4(15) . . ? C7TB C8TB H8T3 109.1 . . ? O2TB C8TB H8T3 109.1 . . ? C7TB C8TB H8T4 109.1 . . ? O2TB C8TB H8T4 109.1 . . ? H8T3 C8TB H8T4 107.9 . . ? C5TB O2TB C8TB 100.4(15) . . ? O3T C9T C10T 107.1(12) . . ? O3T C9T H9T1 110.3 . . ? C10T C9T H9T1 110.3 . . ? O3T C9T H9T2 110.3 . . ? C10T C9T H9T2 110.3 . . ? H9T1 C9T H9T2 108.5 . . ? C12T O3T C9T 99.8(16) . . ? C12T O3T C14T 69(2) . . ? C9T O3T C14T 103.4(14) . . ? C11T C10T C13T 53(2) . . ? C11T C10T C9T 100.3(11) . . ? C13T C10T C9T 102.4(12) . . ? C11T C10T H10A 111.7 . . ? C13T C10T H10A 145.1 . . ? C9T C10T H10A 111.7 . . ? C11T C10T H10B 111.7 . . ? C13T C10T H10B 61.8 . . ? C9T C10T H10B 111.7 . . ? H10A C10T H10B 109.5 . . ? C10T C11T C12T 107.2(14) . . ? C10T C11T H11A 110.3 . . ? C12T C11T H11A 110.3 . . ? C10T C11T H11B 110.3 . . ? C12T C11T H11B 110.3 . . ? H11A C11T H11B 108.5 . . ? O3T C12T C11T 105.6(18) . . ? O3T C12T H12A 110.6 . . ? C11T C12T H12A 110.6 . . ? O3T C12T H12B 110.6 . . ? C11T C12T H12B 110.6 . . ? H12A C12T H12B 108.8 . . ? C13T C14T O3T 110.6(15) . . ? C13T C14T H14A 109.5 . . ? O3T C14T H14A 109.5 . . ? C13T C14T H14B 109.5 . . ? O3T C14T H14B 109.5 . . ? H14A C14T H14B 108.1 . . ? C14T C13T C10T 106.3(14) . . ? C14T C13T H13A 110.5 . . ? C10T C13T H13A 110.5 . . ? C14T C13T H13B 110.5 . . ? C10T C13T H13B 110.5 . . ? H13A C13T H13B 108.7 . . ? N2 N1 C44 104.0(7) . . ? N2 N1 Cu1 126.2(6) . . ? C44 N1 Cu1 129.3(5) . . ? N1 N2 C42 115.6(9) . . ? N1 N2 H2 122.2 . . ? C42 N2 H2 122.2 . . ? N4 N3 C57 106.4(6) . . ? N4 N3 Cu2 122.0(5) . 1_645 ? C57 N3 Cu2 129.5(5) . 1_645 ? C55 N4 N3 111.3(7) . . ? C55 N4 H4 124.3 . . ? N3 N4 H4 124.3 . . ? C5 O1 Cu1 126.7(5) . . ? C7 O2 Cu1 125.9(5) . . ? C14 O3 Cu2 126.2(5) . . ? C16 O4 Cu2 125.0(5) . . ? C25 O5 Cu2 127.1(5) . . ? C27 O6 Cu2 126.3(4) . . ? C34 O7 Cu1 125.3(5) . . ? C36 O8 Cu1 126.3(5) . . ? O1 Cu1 O7 172.0(3) . . ? O1 Cu1 O8 86.9(3) . . ? O7 Cu1 O8 91.4(2) . . ? O1 Cu1 O2 92.2(2) . . ? O7 Cu1 O2 86.7(2) . . ? O8 Cu1 O2 159.4(2) . . ? O1 Cu1 N1 94.0(2) . . ? O7 Cu1 N1 93.9(2) . . ? O8 Cu1 N1 101.6(2) . . ? O2 Cu1 N1 98.9(2) . . ? O6 Cu2 O3 87.4(2) . . ? O6 Cu2 O5 91.9(2) . . ? O3 Cu2 O5 166.0(2) . . ? O6 Cu2 O4 164.3(2) . . ? O3 Cu2 O4 91.9(2) . . ? O5 Cu2 O4 85.1(2) . . ? O6 Cu2 N3 97.0(2) . 1_465 ? O3 Cu2 N3 95.7(2) . 1_465 ? O5 Cu2 N3 98.3(2) . 1_465 ? O4 Cu2 N3 98.7(2) . 1_465 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C4 C5 O1 42.6(12) . . . . ? C3 C4 C5 O1 177.4(10) . . . . ? C3A C4 C5 O1 -162.2(9) . . . . ? C1A C4 C5 O1 -30.2(13) . . . . ? C2A C4 C5 O1 80.5(10) . . . . ? C1 C4 C5 O1 -66.4(9) . . . . ? C2 C4 C5 C6 -138.9(10) . . . . ? C3 C4 C5 C6 -4.1(14) . . . . ? C3A C4 C5 C6 16.2(13) . . . . ? C1A C4 C5 C6 148.3(10) . . . . ? C2A C4 C5 C6 -101.1(10) . . . . ? C1 C4 C5 C6 112.1(9) . . . . ? O1 C5 C6 C7 -4.4(13) . . . . ? C4 C5 C6 C7 177.4(8) . . . . ? C5 C6 C7 O2 1.7(12) . . . . ? C5 C6 C7 C8 -179.2(7) . . . . ? O2 C7 C8 C13 171.0(6) . . . . ? C6 C7 C8 C13 -8.2(10) . . . . ? O2 C7 C8 C9 -11.9(9) . . . . ? C6 C7 C8 C9 169.0(6) . . . . ? C13 C8 C9 C10 -2.8(9) . . . . ? C7 C8 C9 C10 180.0(6) . . . . ? C8 C9 C10 C11 1.4(9) . . . . ? C8 C9 C10 C14 -177.8(6) . . . . ? C9 C10 C11 C12 0.5(10) . . . . ? C14 C10 C11 C12 179.7(6) . . . . ? C10 C11 C12 C13 -1.0(10) . . . . ? C9 C8 C13 C12 2.3(10) . . . . ? C7 C8 C13 C12 179.4(6) . . . . ? C11 C12 C13 C8 -0.4(11) . . . . ? C9 C10 C14 O3 -26.1(8) . . . . ? C11 C10 C14 O3 154.7(6) . . . . ? C9 C10 C14 C15 154.4(6) . . . . ? C11 C10 C14 C15 -24.8(9) . . . . ? O3 C14 C15 C16 -7.2(11) . . . . ? C10 C14 C15 C16 172.2(6) . . . . ? C14 C15 C16 O4 4.7(11) . . . . ? C14 C15 C16 C17 -179.4(6) . . . . ? O4 C16 C17 C18 87.1(7) . . . . ? C15 C16 C17 C18 -89.2(8) . . . . ? O4 C16 C17 C20 -150.9(6) . . . . ? C15 C16 C17 C20 32.8(9) . . . . ? O4 C16 C17 C19 -30.5(8) . . . . ? C15 C16 C17 C19 153.1(6) . . . . ? C21 C24 C25 O5 26.2(9) . . . . ? C22A C24 C25 O5 -64.9(10) . . . . ? C23A C24 C25 O5 174.5(8) . . . . ? C21A C24 C25 O5 52.9(9) . . . . ? C23 C24 C25 O5 153.9(7) . . . . ? C22 C24 C25 O5 -90.0(8) . . . . ? C21 C24 C25 C26 -155.2(7) . . . . ? C22A C24 C25 C26 113.7(9) . . . . ? C23A C24 C25 C26 -6.9(12) . . . . ? C21A C24 C25 C26 -128.5(9) . . . . ? C23 C24 C25 C26 -27.5(10) . . . . ? C22 C24 C25 C26 88.6(8) . . . . ? O5 C25 C26 C27 -0.8(12) . . . . ? C24 C25 C26 C27 -179.2(6) . . . . ? C25 C26 C27 O6 2.4(11) . . . . ? C25 C26 C27 C28 -178.9(6) . . . . ? O6 C27 C28 C29 16.6(8) . . . . ? C26 C27 C28 C29 -162.3(6) . . . . ? O6 C27 C28 C33 -158.5(6) . . . . ? C26 C27 C28 C33 22.7(9) . . . . ? C33 C28 C29 C30 0.9(9) . . . . ? C27 C28 C29 C30 -174.3(6) . . . . ? C28 C29 C30 C31 -1.9(10) . . . . ? C28 C29 C30 C34 179.8(6) . . . . ? C29 C30 C31 C32 0.1(10) . . . . ? C34 C30 C31 C32 178.3(6) . . . . ? C30 C31 C32 C33 2.7(10) . . . . ? C31 C32 C33 C28 -3.7(10) . . . . ? C29 C28 C33 C32 1.9(9) . . . . ? C27 C28 C33 C32 177.0(6) . . . . ? C29 C30 C34 O7 24.1(9) . . . . ? C31 C30 C34 O7 -154.1(7) . . . . ? C29 C30 C34 C35 -154.0(7) . . . . ? C31 C30 C34 C35 27.9(10) . . . . ? O7 C34 C35 C36 4.4(12) . . . . ? C30 C34 C35 C36 -177.9(6) . . . . ? C34 C35 C36 O8 3.6(12) . . . . ? C34 C35 C36 C37 -179.5(7) . . . . ? O8 C36 C37 C39 -48.8(13) . . . . ? C35 C36 C37 C39 134.1(11) . . . . ? O8 C36 C37 C38A 62.2(11) . . . . ? C35 C36 C37 C38A -114.9(10) . . . . ? O8 C36 C37 C39A -159.6(9) . . . . ? C35 C36 C37 C39A 23.3(12) . . . . ? O8 C36 C37 C38 80.3(10) . . . . ? C35 C36 C37 C38 -96.8(9) . . . . ? O8 C36 C37 C40 -176.4(8) . . . . ? C35 C36 C37 C40 6.5(11) . . . . ? O8 C36 C37 C40A -48.7(10) . . . . ? C35 C36 C37 C40A 134.2(9) . . . . ? N2 C42 C43 C44 0.0(10) . . . . ? C41 C42 C43 C44 -173.4(11) . . . . ? C41A C42 C43 C44 -165(4) . . . . ? N2 C42 C43 C46 178.7(7) . . . . ? C41 C42 C43 C46 5.4(18) . . . . ? C41A C42 C43 C46 13(4) . . . . ? C42 C43 C44 N1 0.4(10) . . . . ? C46 C43 C44 N1 -178.4(7) . . . . ? C42 C43 C44 C45 177.5(8) . . . . ? C46 C43 C44 C45 -1.3(13) . . . . ? C42 C43 C46 C47 -106.5(12) . . . . ? C44 C43 C46 C47 72.0(11) . . . . ? C43 C46 C47 C48 58.9(11) . . . . ? C43 C46 C47 C52 -120.3(9) . . . . ? C52 C47 C48 C49 -2.6(9) . . . . ? C46 C47 C48 C49 178.1(6) . . . . ? C47 C48 C49 C50 2.9(9) . . . . ? C47 C48 C49 C53 -178.1(5) . . . . ? C48 C49 C50 C51 -1.7(9) . . . . ? C53 C49 C50 C51 179.3(6) . . . . ? C49 C50 C51 C52 0.5(10) . . . . ? C48 C47 C52 C51 1.3(10) . . . . ? C46 C47 C52 C51 -179.5(6) . . . . ? C50 C51 C52 C47 -0.3(11) . . . . ? C50 C49 C53 C56 -110.5(8) . . . . ? C48 C49 C53 C56 70.5(8) . . . . ? N4 C55 C56 C57 0.4(9) . . . . ? C54 C55 C56 C57 179.4(8) . . . . ? N4 C55 C56 C53 -178.2(6) . . . . ? C54 C55 C56 C53 0.7(14) . . . . ? C49 C53 C56 C55 -108.9(9) . . . . ? C49 C53 C56 C57 72.7(9) . . . . ? C55 C56 C57 N3 -1.9(9) . . . . ? C53 C56 C57 N3 176.8(6) . . . . ? C55 C56 C57 C58 178.4(8) . . . . ? C53 C56 C57 C58 -2.9(13) . . . . ? C4TA O1TA C1TA C2TA 30(3) . . . . ? O1TA C1TA C2TA C3TA -8(3) . . . . ? C4TA C3TA C2TA C1TA -18(2) . . . . ? C1TA O1TA C4TA C3TA -43(2) . . . . ? C2TA C3TA C4TA O1TA 40(2) . . . . ? C4TB O1TB C1TB C2TB -26(3) . . . . ? O1TB C1TB C2TB C3TB 12(3) . . . . ? C4TB C3TB C2TB C1TB 8(3) . . . . ? C2TB C3TB C4TB O1TB -25(2) . . . . ? C1TB O1TB C4TB C3TB 31(2) . . . . ? C5TA C6TA C7TA C8TA 24(3) . . . . ? C6TA C7TA C8TA O2TA -10(4) . . . . ? C5TA O2TA C8TA C7TA -8(4) . . . . ? C7TA C6TA C5TA O2TA -32(3) . . . . ? C8TA O2TA C5TA C6TA 24(3) . . . . ? C5TB C6TB C7TB C8TB -24(3) . . . . ? C7TB C6TB C5TB O2TB 15(3) . . . . ? C6TB C7TB C8TB O2TB 27(3) . . . . ? C6TB C5TB O2TB C8TB 1(3) . . . . ? C7TB C8TB O2TB C5TB -19(3) . . . . ? C10T C9T O3T C12T -41(2) . . . . ? C10T C9T O3T C14T 30(2) . . . . ? O3T C9T C10T C11T 22(3) . . . . ? O3T C9T C10T C13T -32(3) . . . . ? C13T C10T C11T C12T 103(3) . . . . ? C9T C10T C11T C12T 5(3) . . . . ? C9T O3T C12T C11T 44(3) . . . . ? C14T O3T C12T C11T -57(3) . . . . ? C10T C11T C12T O3T -31(4) . . . . ? C12T O3T C14T C13T 78(3) . . . . ? C9T O3T C14T C13T -17(4) . . . . ? O3T C14T C13T C10T -3(5) . . . . ? C11T C10T C13T C14T -74(3) . . . . ? C9T C10T C13T C14T 20(4) . . . . ? C43 C44 N1 N2 -0.5(8) . . . . ? C45 C44 N1 N2 -177.9(6) . . . . ? C43 C44 N1 Cu1 171.1(5) . . . . ? C45 C44 N1 Cu1 -6.2(10) . . . . ? C44 N1 N2 C42 0.6(9) . . . . ? Cu1 N1 N2 C42 -171.5(6) . . . . ? C43 C42 N2 N1 -0.3(11) . . . . ? C41 C42 N2 N1 173.5(10) . . . . ? C41A C42 N2 N1 171(2) . . . . ? C56 C57 N3 N4 2.6(8) . . . . ? C58 C57 N3 N4 -177.7(6) . . . . ? C56 C57 N3 Cu2 165.9(5) . . . 1_645 ? C58 C57 N3 Cu2 -14.4(10) . . . 1_645 ? C56 C55 N4 N3 1.3(8) . . . . ? C54 C55 N4 N3 -177.8(7) . . . . ? C57 N3 N4 C55 -2.5(8) . . . . ? Cu2 N3 N4 C55 -167.3(5) 1_645 . . . ? C6 C5 O1 Cu1 5.5(11) . . . . ? C4 C5 O1 Cu1 -176.1(6) . . . . ? C6 C7 O2 Cu1 -0.5(10) . . . . ? C8 C7 O2 Cu1 -179.6(4) . . . . ? C15 C14 O3 Cu2 -5.8(9) . . . . ? C10 C14 O3 Cu2 174.8(4) . . . . ? C15 C16 O4 Cu2 10.1(9) . . . . ? C17 C16 O4 Cu2 -166.1(4) . . . . ? C26 C25 O5 Cu2 -5.7(10) . . . . ? C24 C25 O5 Cu2 172.9(5) . . . . ? C26 C27 O6 Cu2 2.6(9) . . . . ? C28 C27 O6 Cu2 -176.2(4) . . . . ? C35 C34 O7 Cu1 4.4(10) . . . . ? C30 C34 O7 Cu1 -173.4(4) . . . . ? C35 C36 O8 Cu1 -19.4(11) . . . . ? C37 C36 O8 Cu1 163.7(5) . . . . ? C5 O1 Cu1 O8 156.0(6) . . . . ? C5 O1 Cu1 O2 -3.4(6) . . . . ? C5 O1 Cu1 N1 -102.6(6) . . . . ? C34 O7 Cu1 O8 -13.5(6) . . . . ? C34 O7 Cu1 O2 146.0(6) . . . . ? C34 O7 Cu1 N1 -115.3(5) . . . . ? C36 O8 Cu1 O1 -151.1(7) . . . . ? C36 O8 Cu1 O7 21.1(7) . . . . ? C36 O8 Cu1 O2 -63.0(11) . . . . ? C36 O8 Cu1 N1 115.4(7) . . . . ? C7 O2 Cu1 O1 1.1(6) . . . . ? C7 O2 Cu1 O7 -171.1(6) . . . . ? C7 O2 Cu1 O8 -86.1(9) . . . . ? C7 O2 Cu1 N1 95.5(6) . . . . ? N2 N1 Cu1 O1 -53.5(6) . . . . ? C44 N1 Cu1 O1 136.5(6) . . . . ? N2 N1 Cu1 O7 126.4(6) . . . . ? C44 N1 Cu1 O7 -43.6(6) . . . . ? N2 N1 Cu1 O8 34.2(6) . . . . ? C44 N1 Cu1 O8 -135.8(6) . . . . ? N2 N1 Cu1 O2 -146.4(6) . . . . ? C44 N1 Cu1 O2 43.6(6) . . . . ? C27 O6 Cu2 O3 159.8(5) . . . . ? C27 O6 Cu2 O5 -6.2(5) . . . . ? C27 O6 Cu2 O4 72.3(10) . . . . ? C27 O6 Cu2 N3 -104.7(5) . . . 1_465 ? C14 O3 Cu2 O6 -150.0(5) . . . . ? C14 O3 Cu2 O5 -62.7(12) . . . . ? C14 O3 Cu2 O4 14.3(5) . . . . ? C14 O3 Cu2 N3 113.2(5) . . . 1_465 ? C25 O5 Cu2 O6 7.7(6) . . . . ? C25 O5 Cu2 O3 -78.9(11) . . . . ? C25 O5 Cu2 O4 -156.8(6) . . . . ? C25 O5 Cu2 N3 105.1(6) . . . 1_465 ? C16 O4 Cu2 O6 70.5(10) . . . . ? C16 O4 Cu2 O3 -16.4(5) . . . . ? C16 O4 Cu2 O5 149.9(6) . . . . ? C16 O4 Cu2 N3 -112.5(5) . . . 1_465 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 O2TA 0.88 2.45 3.27(2) 155.8 . N2 H2 O2TB 0.88 2.39 3.232(19) 160.0 . N4 H4 O3T 0.88 2.12 2.963(15) 159.4 . _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.343 _refine_diff_density_min -0.386 _refine_diff_density_rms 0.112