# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_du2 _database_code_depnum_ccdc_archive 'CCDC 926653' #TrackingRef 'Complex_1D.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H72 Cd3 K3 N3 O30' _chemical_formula_weight 1805.74 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(5) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 20.5909(4) _cell_length_b 20.5909(4) _cell_length_c 28.3082(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10394.3(4) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30958 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .13 _exptl_crystal_size_mid .12 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5472 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9289 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 81503 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.49 _reflns_number_total 15839 _reflns_number_gt 15341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+7.2441P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(14) _refine_ls_number_reflns 15839 _refine_ls_number_parameters 922 _refine_ls_number_restraints 14 _refine_ls_R_factor_ref 0.0325 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.077 _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 Cd1 Cd 0.887997(13) 0.331248(13) -0.155598(9) 0.03167(6) Uani 1 1 d . . . Cd2 Cd 0.996989(13) 0.767497(13) 0.018009(7) 0.03201(7) Uani 1 1 d . . . Cd3 Cd 0.576462(12) 0.663827(12) -0.156460(8) 0.02912(5) Uani 1 1 d . . . K1 K 0.84955(5) 0.24554(5) -0.02815(3) 0.0471(2) Uani 1 1 d . . . K2 K 1.07441(6) 0.80244(6) -0.11036(4) 0.0629(3) Uani 1 1 d . . . K3 K 0.42519(5) 0.48268(5) -0.11394(3) 0.0496(2) Uani 1 1 d . . . N1 N 1.08886(18) 0.36947(19) 0.02611(13) 0.0495(8) Uani 1 1 d . . . H1B H 1.0972 0.3904 0.0546 0.074 Uiso 1 1 calc R . . H1C H 1.0534 0.3746 0.0116 0.074 Uiso 1 1 calc R . . H1D H 1.1309 0.3920 0.0092 0.074 Uiso 1 1 calc R . . N2 N 0.9567(2) 0.5746(2) -0.17014(13) 0.0569(9) Uani 1 1 d . . . H2A H 0.9379 0.5653 -0.1993 0.085 Uiso 1 1 calc R . . H2B H 0.9498 0.6101 -0.1570 0.085 Uiso 1 1 calc R . . H2C H 0.9334 0.5330 -0.1529 0.085 Uiso 1 1 calc R . . N3 N 0.3018(2) 0.2342(3) -0.16820(15) 0.0707(12) Uani 1 1 d . . . H3B H 0.2817 0.2254 -0.1970 0.106 Uiso 1 1 calc R . . H3C H 0.2924 0.2667 -0.1533 0.106 Uiso 1 1 calc R . . H3D H 0.2818 0.1914 -0.1520 0.106 Uiso 1 1 calc R . . O1 O 0.57940(16) 0.01657(16) -0.36255(10) 0.0478(7) Uani 1 1 d . . . O2 O 0.60321(15) 0.00333(13) -0.28823(9) 0.0403(6) Uani 1 1 d . . . O3 O 0.82951(15) 0.33428(13) -0.22448(10) 0.0427(6) Uani 1 1 d . . . O4 O 0.77279(14) 0.22267(14) -0.19114(9) 0.0392(6) Uani 1 1 d . . . O5 O 1.18704(15) 0.18093(15) -0.24020(9) 0.0419(6) Uani 1 1 d . . . O6 O 1.11979(15) 0.22010(16) -0.27876(9) 0.0442(6) Uani 1 1 d . . . O7 O 0.91573(15) 0.22853(15) -0.11149(10) 0.0470(7) Uani 1 1 d . . . O8 O 0.94196(16) 0.26641(16) -0.18562(9) 0.0427(6) Uani 1 1 d . . . O9 O 0.81978(15) 0.32777(14) -0.09014(10) 0.0417(6) Uani 1 1 d . . . O10 O 0.87752(16) 0.43965(15) -0.12265(10) 0.0452(6) Uani 1 1 d . . . O11 O 0.8647(2) 0.64142(18) 0.04376(12) 0.0649(9) Uani 1 1 d . . . O12 O 0.92353(17) 0.65796(16) -0.02330(11) 0.0504(7) Uani 1 1 d . . . O13 O 0.25431(17) 0.35127(16) -0.34956(12) 0.0544(8) Uani 1 1 d . . . O14 O 0.30079(17) 0.34749(15) -0.28005(10) 0.0482(7) Uani 1 1 d . . . O15 O 0.52921(14) 0.67693(14) -0.23126(9) 0.0369(5) Uani 1 1 d . . . O16 O 0.45538(15) 0.57824(16) -0.18819(9) 0.0460(6) Uani 1 1 d . . . O17 O 0.50792(15) 0.64558(13) -0.08295(9) 0.0380(5) Uani 1 1 d . . . O18 O 0.53246(16) 0.74320(15) -0.12773(9) 0.0443(6) Uani 1 1 d . . . O19 O 0.54306(17) 0.96964(15) 0.02848(10) 0.0494(7) Uani 1 1 d . . . O20 O 0.61086(15) 0.97349(14) -0.03242(10) 0.0444(6) Uani 1 1 d . . . O21 O 0.68991(15) 0.78810(17) -0.17194(10) 0.0477(7) Uani 1 1 d . . . O22 O 0.68420(15) 0.72377(15) -0.10836(10) 0.0488(7) Uani 1 1 d . . . O23 O 0.90630(17) 0.80296(17) -0.00771(9) 0.0495(7) Uani 1 1 d . . . O24 O 1.01050(15) 0.84434(16) -0.04713(10) 0.0466(6) Uani 1 1 d . . . O25 O 0.94313(18) 0.2698(2) 0.05095(12) 0.0676(10) Uani 1 1 d . . . H25B H 0.9362 0.2972 0.0746 0.081 Uiso 1 1 calc R . . O26 O 0.98528(17) 0.39598(17) -0.02773(11) 0.0544(7) Uani 1 1 d . . . H26A H 1.0277 0.3965 -0.0395 0.065 Uiso 1 1 calc R . . O27 O 1.0595(3) 0.7215(2) -0.19250(14) 0.0832(12) Uani 1 1 d . . . H27B H 1.0377 0.7332 -0.2174 0.100 Uiso 1 1 calc R . . O28 O 0.92365(17) 0.67307(17) -0.11624(11) 0.0557(7) Uani 1 1 d . . . H28B H 0.9229 0.6292 -0.1074 0.067 Uiso 1 1 calc R . . O29 O 0.3981(3) 0.3851(3) -0.19021(17) 0.1137(16) Uani 1 1 d U . . H29B H 0.3661 0.3869 -0.2126 0.136 Uiso 1 1 calc R . . O30 O 0.2777(2) 0.3363(2) -0.11234(12) 0.0709(10) Uani 1 1 d . . . H30A H 0.2789 0.2941 -0.1018 0.085 Uiso 1 1 calc R . . C1 C 0.68873(18) 0.15751(19) -0.27437(13) 0.0343(7) Uani 1 1 d . . . H1A H 0.6859 0.1255 -0.2502 0.041 Uiso 1 1 calc R . . C2 C 0.64965(18) 0.12720(17) -0.31651(13) 0.0347(7) Uani 1 1 d . . . C3 C 0.6518(2) 0.1756(2) -0.35104(14) 0.0434(9) Uani 1 1 d . . . H3A H 0.6255 0.1562 -0.3790 0.052 Uiso 1 1 calc R . . C4 C 0.6922(3) 0.2525(2) -0.34477(15) 0.0496(10) Uani 1 1 d . . . H4A H 0.6920 0.2841 -0.3682 0.060 Uiso 1 1 calc R . . C5 C 0.7329(2) 0.2824(2) -0.30393(14) 0.0457(9) Uani 1 1 d . . . H5A H 0.7611 0.3341 -0.3001 0.055 Uiso 1 1 calc R . . C6 C 0.73161(19) 0.23434(18) -0.26798(13) 0.0341(7) Uani 1 1 d . . . C7 C 0.60728(17) 0.04354(18) -0.32312(14) 0.0344(7) Uani 1 1 d . . . C8 C 0.77969(18) 0.26520(18) -0.22486(13) 0.0330(7) Uani 1 1 d . . . C9 C 1.03513(19) 0.20466(19) -0.19627(13) 0.0354(7) Uani 1 1 d . . . H9A H 1.0333 0.2339 -0.2207 0.043 Uiso 1 1 calc R . . C10 C 1.08048(18) 0.17313(18) -0.20062(12) 0.0321(7) Uani 1 1 d . . . C11 C 1.0818(2) 0.1270(2) -0.16511(13) 0.0395(8) Uani 1 1 d . . . H11A H 1.1122 0.1057 -0.1679 0.047 Uiso 1 1 calc R . . C12 C 1.0369(2) 0.1133(2) -0.12534(14) 0.0439(9) Uani 1 1 d . . . H12A H 1.0364 0.0817 -0.1017 0.053 Uiso 1 1 calc R . . C13 C 0.9931(2) 0.1463(2) -0.12063(14) 0.0407(8) Uani 1 1 d . . . H13A H 0.9639 0.1371 -0.0937 0.049 Uiso 1 1 calc R . . C14 C 0.99228(17) 0.19333(18) -0.15587(13) 0.0336(7) Uani 1 1 d . . . C15 C 1.13206(19) 0.19252(18) -0.24294(12) 0.0342(7) Uani 1 1 d . . . C16 C 0.94673(18) 0.23162(19) -0.15007(14) 0.0365(7) Uani 1 1 d . . . C17 C 0.84788(19) 0.5035(2) -0.04277(14) 0.0374(8) Uani 1 1 d . . . H17A H 0.8803 0.5358 -0.0657 0.045 Uiso 1 1 calc R . . C18 C 0.81528(19) 0.4262(2) -0.04890(13) 0.0360(7) Uani 1 1 d . . . C19 C 0.7643(2) 0.3780(2) -0.01607(16) 0.0498(10) Uani 1 1 d . . . H19A H 0.7413 0.3264 -0.0204 0.060 Uiso 1 1 calc R . . C20 C 0.7479(2) 0.4068(3) 0.02334(17) 0.0570(12) Uani 1 1 d . . . H20A H 0.7144 0.3744 0.0458 0.068 Uiso 1 1 calc R . . C21 C 0.7811(2) 0.4843(2) 0.02964(16) 0.0526(10) Uani 1 1 d . . . H21A H 0.7686 0.5033 0.0557 0.063 Uiso 1 1 calc R . . C22 C 0.8327(2) 0.5327(2) -0.00307(14) 0.0430(9) Uani 1 1 d . . . C23 C 0.83862(18) 0.3965(2) -0.09016(13) 0.0345(7) Uani 1 1 d . . . C24 C 0.8753(2) 0.6167(2) 0.00641(16) 0.0477(9) Uani 1 1 d . . . C25 C 0.3750(2) 0.50222(19) -0.27018(13) 0.0352(7) Uani 1 1 d . . . H25A H 0.3751 0.4734 -0.2449 0.042 Uiso 1 1 calc R . . C26 C 0.33228(18) 0.46664(19) -0.30992(13) 0.0357(7) Uani 1 1 d . . . C27 C 0.3305(2) 0.5109(2) -0.34649(14) 0.0416(8) Uani 1 1 d . . . H27A H 0.3027 0.4883 -0.3736 0.050 Uiso 1 1 calc R . . C28 C 0.3699(2) 0.5886(2) -0.34282(15) 0.0467(9) Uani 1 1 d . . . H28A H 0.3661 0.6177 -0.3666 0.056 Uiso 1 1 calc R . . C29 C 0.4147(2) 0.6229(2) -0.30377(13) 0.0384(8) Uani 1 1 d . . . H29A H 0.4430 0.6749 -0.3022 0.046 Uiso 1 1 calc R . . C30 C 0.41769(18) 0.58015(18) -0.26726(12) 0.0309(7) Uani 1 1 d . . . C31 C 0.2927(2) 0.3830(2) -0.31359(14) 0.0407(8) Uani 1 1 d . . . C32 C 0.46977(19) 0.61380(19) -0.22622(12) 0.0335(7) Uani 1 1 d . . . C33 C 0.52242(19) 0.81879(19) -0.04767(12) 0.0347(7) Uani 1 1 d . . . H33A H 0.5556 0.8477 -0.0714 0.042 Uiso 1 1 calc R . . C34 C 0.48680(18) 0.74091(18) -0.05075(12) 0.0319(7) Uani 1 1 d . . . C35 C 0.4350(2) 0.6974(2) -0.01660(13) 0.0398(8) Uani 1 1 d . . . H35A H 0.4114 0.6454 -0.0180 0.048 Uiso 1 1 calc R . . C36 C 0.4187(2) 0.7327(2) 0.01989(15) 0.0482(10) Uani 1 1 d . . . H36A H 0.3825 0.7040 0.0422 0.058 Uiso 1 1 calc R . . C37 C 0.4563(2) 0.8104(2) 0.02293(14) 0.0444(9) Uani 1 1 d . . . H37A H 0.4454 0.8334 0.0475 0.053 Uiso 1 1 calc R . . C38 C 0.5097(2) 0.85399(19) -0.01031(13) 0.0347(7) Uani 1 1 d . . . C39 C 0.50938(19) 0.70702(19) -0.08953(12) 0.0334(7) Uani 1 1 d . . . C40 C 0.5568(2) 0.93785(19) -0.00483(13) 0.0378(8) Uani 1 1 d . . . C41 C 0.8361(2) 0.8193(2) -0.08810(13) 0.0361(7) Uani 1 1 d D . . H41A H 0.812(2) 0.7894(19) -0.0659(11) 0.043 Uiso 1 1 d D . . C42 C 0.8024(2) 0.82949(19) -0.12795(13) 0.0364(7) Uani 1 1 d . . . C43 C 0.8477(2) 0.8813(2) -0.16151(14) 0.0435(9) Uani 1 1 d . . . H43A H 0.8261 0.8900 -0.1878 0.052 Uiso 1 1 calc R . . C44 C 0.9250(2) 0.9202(2) -0.15623(16) 0.0502(10) Uani 1 1 d . . . H44A H 0.9549 0.9552 -0.1789 0.060 Uiso 1 1 calc R . . C45 C 0.9581(2) 0.9074(2) -0.11733(14) 0.0429(9) Uani 1 1 d . . . H45A H 1.0100 0.9327 -0.1144 0.051 Uiso 1 1 calc R . . C46 C 0.91345(19) 0.85668(19) -0.08284(12) 0.0343(7) Uani 1 1 d . . . C47 C 0.7199(2) 0.7777(2) -0.13597(14) 0.0385(8) Uani 1 1 d . . . C48 C 0.9453(2) 0.83399(19) -0.04265(13) 0.0365(7) Uani 1 1 d . . . C49 C 1.0503(3) 0.2543(3) -0.01839(17) 0.0632(13) Uani 1 1 d . . . H49A H 1.0344 0.2020 -0.0161 0.095 Uiso 1 1 calc R . . H49B H 1.0959 0.2795 -0.0364 0.095 Uiso 1 1 calc R . . H49C H 1.0121 0.2603 -0.0338 0.095 Uiso 1 1 calc R . . C50 C 1.0639(2) 0.2881(2) 0.03100(14) 0.0463(9) Uani 1 1 d . . . H50A H 1.1049 0.2838 0.0454 0.056 Uiso 1 1 calc R . . C51 C 0.9972(2) 0.2506(3) 0.06317(16) 0.0520(10) Uani 1 1 d . . . H51A H 0.9755 0.1967 0.0612 0.062 Uiso 1 1 calc R . . H51B H 1.0132 0.2657 0.0955 0.062 Uiso 1 1 calc R . . C52 C 0.9628(3) 0.4609(3) 0.03432(17) 0.0621(12) Uani 1 1 d . . . H52A H 0.9710 0.5090 0.0443 0.093 Uiso 1 1 calc R . . H52B H 0.9847 0.4426 0.0569 0.093 Uiso 1 1 calc R . . H52C H 0.9100 0.4263 0.0320 0.093 Uiso 1 1 calc R . . C53 C 0.9986(2) 0.4684(2) -0.01293(15) 0.0495(10) Uani 1 1 d . . . H53A H 0.9775 0.4878 -0.0358 0.059 Uiso 1 1 calc R . . H53B H 1.0521 0.5031 -0.0108 0.059 Uiso 1 1 calc R . . C54 C 1.0682(3) 0.6152(3) -0.12174(19) 0.0729(15) Uani 1 1 d . . . H54A H 1.1209 0.6321 -0.1216 0.109 Uiso 1 1 calc R . . H54B H 1.0420 0.5696 -0.1039 0.109 Uiso 1 1 calc R . . H54C H 1.0598 0.6529 -0.1078 0.109 Uiso 1 1 calc R . . C55 C 1.0397(3) 0.6012(2) -0.17209(17) 0.0530(11) Uani 1 1 d . . . H55A H 1.0462 0.5608 -0.1853 0.064 Uiso 1 1 calc R . . C56 C 1.0780(3) 0.6674(3) -0.20353(17) 0.0588(12) Uani 1 1 d . . . H56A H 1.1319 0.6888 -0.2007 0.071 Uiso 1 1 calc R . . H56B H 1.0641 0.6517 -0.2360 0.071 Uiso 1 1 calc R . . C57 C 0.8547(3) 0.6962(3) -0.17500(18) 0.0680(13) Uani 1 1 d . . . H57A H 0.8059 0.6874 -0.1839 0.102 Uiso 1 1 calc R . . H57B H 0.8731 0.6764 -0.1988 0.102 Uiso 1 1 calc R . . H57C H 0.8884 0.7492 -0.1719 0.102 Uiso 1 1 calc R . . C58 C 0.8494(3) 0.6588(3) -0.12925(17) 0.0572(11) Uani 1 1 d . . . H58A H 0.8302 0.6782 -0.1051 0.069 Uiso 1 1 calc R . . H58B H 0.8153 0.6052 -0.1321 0.069 Uiso 1 1 calc R . . C59 C 0.4162(4) 0.2794(3) -0.1224(2) 0.0830(17) Uani 1 1 d . . . H59A H 0.4694 0.2992 -0.1238 0.124 Uiso 1 1 calc R . . H59B H 0.3932 0.2329 -0.1052 0.124 Uiso 1 1 calc R . . H59C H 0.4060 0.3146 -0.1066 0.124 Uiso 1 1 calc R . . C60 C 0.3844(3) 0.2659(3) -0.17210(18) 0.0619(12) Uani 1 1 d . . . H60A H 0.3930 0.2278 -0.1867 0.074 Uiso 1 1 calc R . . C61 C 0.4218(4) 0.3346(3) -0.2021(2) 0.0819(17) Uani 1 1 d U . . H61A H 0.4757 0.3585 -0.1981 0.098 Uiso 1 1 calc R . . H61B H 0.4104 0.3205 -0.2351 0.098 Uiso 1 1 calc R . . C62 C 0.2145(4) 0.3595(3) -0.17527(19) 0.0739(15) Uani 1 1 d . . . H62A H 0.1673 0.3537 -0.1850 0.111 Uiso 1 1 calc R . . H62B H 0.2298 0.3341 -0.1972 0.111 Uiso 1 1 calc R . . H62C H 0.2516 0.4118 -0.1744 0.111 Uiso 1 1 calc R . . C63 C 0.2065(3) 0.3258(3) -0.12633(17) 0.0606(12) Uani 1 1 d . . . H63A H 0.1900 0.3504 -0.1040 0.073 Uiso 1 1 calc R . . H63B H 0.1695 0.2728 -0.1269 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03008(11) 0.03438(11) 0.03057(13) -0.00727(10) -0.00535(11) 0.01613(9) Cd2 0.03184(11) 0.03559(12) 0.02820(16) -0.00085(10) -0.00501(9) 0.01655(9) Cd3 0.03198(11) 0.02980(11) 0.02559(12) -0.00210(9) 0.00056(10) 0.01546(9) K1 0.0482(5) 0.0430(4) 0.0472(5) 0.0072(4) 0.0134(4) 0.0206(4) K2 0.0526(5) 0.0563(5) 0.0821(8) 0.0180(5) 0.0234(5) 0.0290(5) K3 0.0479(5) 0.0524(5) 0.0515(5) 0.0182(4) 0.0130(4) 0.0273(4) N1 0.0420(17) 0.0541(19) 0.046(2) -0.0104(16) -0.0038(15) 0.0192(15) N2 0.057(2) 0.054(2) 0.053(2) -0.0135(17) -0.0163(17) 0.0224(18) N3 0.075(3) 0.081(3) 0.060(3) 0.009(2) -0.015(2) 0.042(2) O1 0.0468(15) 0.0496(15) 0.0450(16) -0.0205(13) -0.0150(13) 0.0225(13) O2 0.0458(14) 0.0294(12) 0.0380(15) -0.0064(10) 0.0001(11) 0.0131(11) O3 0.0439(14) 0.0268(12) 0.0464(15) -0.0040(11) -0.0169(12) 0.0094(11) O4 0.0426(14) 0.0344(12) 0.0323(13) -0.0004(10) -0.0077(11) 0.0132(11) O5 0.0431(14) 0.0485(14) 0.0417(15) 0.0015(12) 0.0077(11) 0.0286(12) O6 0.0436(14) 0.0586(16) 0.0323(14) 0.0104(12) 0.0043(11) 0.0272(13) O7 0.0427(14) 0.0494(15) 0.0455(16) -0.0061(12) 0.0137(12) 0.0206(12) O8 0.0540(16) 0.0538(16) 0.0364(14) -0.0066(12) -0.0058(12) 0.0389(14) O9 0.0428(14) 0.0349(13) 0.0463(16) -0.0061(11) 0.0036(12) 0.0185(11) O10 0.0525(16) 0.0431(14) 0.0432(16) -0.0012(12) 0.0071(13) 0.0263(13) O11 0.096(3) 0.0572(19) 0.055(2) -0.0179(15) -0.0029(18) 0.0482(19) O12 0.0546(17) 0.0406(14) 0.0481(17) -0.0101(13) -0.0102(14) 0.0178(13) O13 0.0522(17) 0.0423(15) 0.065(2) -0.0130(14) -0.0152(15) 0.0205(13) O14 0.0631(18) 0.0342(13) 0.0453(16) 0.0012(12) 0.0045(14) 0.0228(13) O15 0.0382(13) 0.0388(13) 0.0311(13) -0.0022(10) -0.0032(10) 0.0173(11) O16 0.0450(15) 0.0525(16) 0.0309(14) 0.0093(12) -0.0049(11) 0.0171(13) O17 0.0477(14) 0.0326(12) 0.0366(14) -0.0033(10) 0.0038(11) 0.0223(11) O18 0.0606(17) 0.0457(14) 0.0313(13) 0.0013(11) 0.0128(12) 0.0302(13) O19 0.0671(18) 0.0372(14) 0.0478(17) -0.0105(12) 0.0006(14) 0.0289(13) O20 0.0430(14) 0.0317(13) 0.0470(16) -0.0038(11) 0.0056(12) 0.0100(11) O21 0.0410(14) 0.0589(17) 0.0491(17) -0.0039(13) -0.0076(12) 0.0293(13) O22 0.0381(14) 0.0440(15) 0.0477(16) -0.0005(13) -0.0065(12) 0.0082(12) O23 0.0608(17) 0.0651(18) 0.0329(14) 0.0139(13) 0.0050(13) 0.0391(15) O24 0.0405(14) 0.0506(16) 0.0483(16) 0.0052(13) -0.0089(12) 0.0224(12) O25 0.0505(18) 0.106(3) 0.055(2) 0.0186(19) 0.0173(15) 0.0463(19) O26 0.0542(17) 0.0551(17) 0.0435(17) -0.0006(14) -0.0039(13) 0.0195(14) O27 0.127(3) 0.073(2) 0.077(3) 0.036(2) 0.040(2) 0.071(3) O28 0.0521(17) 0.0540(17) 0.0569(19) -0.0041(14) 0.0015(14) 0.0236(14) O29 0.180(4) 0.084(3) 0.098(3) 0.035(2) 0.051(3) 0.081(3) O30 0.088(3) 0.083(2) 0.0482(19) 0.0001(17) -0.0027(18) 0.048(2) C1 0.0306(16) 0.0337(17) 0.0327(18) -0.0021(14) -0.0047(13) 0.0116(14) C2 0.0351(16) 0.0305(15) 0.0361(19) -0.0040(15) -0.0054(15) 0.0147(13) C3 0.049(2) 0.047(2) 0.034(2) -0.0052(16) -0.0152(16) 0.0237(18) C4 0.063(3) 0.043(2) 0.044(2) 0.0064(18) -0.012(2) 0.027(2) C5 0.053(2) 0.0359(18) 0.049(2) -0.0017(16) -0.0184(18) 0.0229(17) C6 0.0353(17) 0.0307(16) 0.0357(19) -0.0028(14) -0.0079(14) 0.0161(14) C7 0.0295(15) 0.0348(16) 0.0379(18) -0.0126(16) -0.0080(15) 0.0152(13) C8 0.0309(16) 0.0294(15) 0.0357(18) -0.0041(13) -0.0040(14) 0.0130(13) C9 0.0392(18) 0.0359(17) 0.0304(18) 0.0028(14) -0.0015(14) 0.0182(15) C10 0.0321(16) 0.0319(16) 0.0304(17) -0.0006(13) 0.0043(13) 0.0145(13) C11 0.0440(19) 0.0388(18) 0.038(2) 0.0012(15) 0.0041(15) 0.0221(16) C12 0.056(2) 0.044(2) 0.037(2) 0.0110(16) 0.0074(17) 0.0286(18) C13 0.043(2) 0.0387(18) 0.037(2) 0.0045(15) 0.0088(16) 0.0184(16) C14 0.0328(15) 0.0341(16) 0.0308(17) -0.0014(14) -0.0007(14) 0.0145(13) C15 0.0361(17) 0.0291(15) 0.0341(18) -0.0024(13) 0.0039(14) 0.0138(14) C16 0.0295(15) 0.0353(16) 0.040(2) -0.0100(15) -0.0045(15) 0.0127(13) C17 0.0336(17) 0.0377(18) 0.043(2) -0.0055(15) -0.0011(15) 0.0190(15) C18 0.0318(16) 0.0364(17) 0.041(2) -0.0047(15) -0.0005(14) 0.0179(14) C19 0.0377(19) 0.045(2) 0.058(3) -0.0076(19) 0.0062(18) 0.0148(17) C20 0.047(2) 0.053(2) 0.060(3) -0.004(2) 0.022(2) 0.0168(19) C21 0.046(2) 0.056(2) 0.055(3) -0.017(2) 0.0059(19) 0.0241(19) C22 0.0416(19) 0.048(2) 0.046(2) -0.0104(17) -0.0042(16) 0.0269(17) C23 0.0303(16) 0.0421(18) 0.0335(18) -0.0094(15) -0.0062(14) 0.0198(14) C24 0.055(2) 0.049(2) 0.050(2) -0.016(2) -0.015(2) 0.0344(19) C25 0.0399(18) 0.0351(17) 0.0320(18) 0.0072(14) -0.0002(14) 0.0198(15) C26 0.0333(16) 0.0347(16) 0.0376(19) 0.0003(14) 0.0010(14) 0.0158(14) C27 0.0364(18) 0.045(2) 0.040(2) -0.0038(17) -0.0106(16) 0.0175(16) C28 0.051(2) 0.045(2) 0.042(2) 0.0068(17) -0.0117(18) 0.0219(18) C29 0.0374(18) 0.0315(16) 0.039(2) 0.0027(14) -0.0021(15) 0.0117(14) C30 0.0308(16) 0.0341(16) 0.0276(16) 0.0016(13) -0.0021(13) 0.0160(13) C31 0.0397(18) 0.0373(17) 0.042(2) 0.0005(16) 0.0032(16) 0.0167(15) C32 0.0342(16) 0.0398(18) 0.0306(17) -0.0019(14) -0.0001(14) 0.0215(15) C33 0.0392(18) 0.0307(16) 0.0303(17) -0.0002(13) 0.0084(14) 0.0144(14) C34 0.0332(16) 0.0311(16) 0.0286(17) -0.0018(13) 0.0047(13) 0.0139(13) C35 0.0435(19) 0.0292(16) 0.039(2) -0.0010(15) 0.0093(16) 0.0126(15) C36 0.048(2) 0.0414(19) 0.044(2) 0.0021(17) 0.0214(18) 0.0138(16) C37 0.048(2) 0.047(2) 0.038(2) -0.0055(17) 0.0095(17) 0.0237(17) C38 0.0367(17) 0.0318(16) 0.0328(18) -0.0052(14) 0.0016(14) 0.0149(14) C39 0.0311(16) 0.0345(16) 0.0304(17) -0.0025(14) 0.0027(13) 0.0132(14) C40 0.050(2) 0.0315(16) 0.0379(19) -0.0064(14) -0.0078(16) 0.0248(16) C41 0.0384(18) 0.0335(17) 0.0345(19) 0.0044(14) 0.0007(15) 0.0167(15) C42 0.0351(17) 0.0336(17) 0.042(2) -0.0013(15) -0.0051(15) 0.0183(14) C43 0.050(2) 0.0442(19) 0.036(2) 0.0073(16) -0.0078(17) 0.0234(17) C44 0.049(2) 0.0416(19) 0.046(2) 0.0186(18) 0.002(2) 0.0127(17) C45 0.0361(18) 0.0366(18) 0.047(2) 0.0035(16) -0.0066(16) 0.0119(15) C46 0.0378(17) 0.0340(16) 0.0326(18) 0.0002(14) -0.0036(14) 0.0191(14) C47 0.0379(18) 0.0438(19) 0.0369(19) -0.0105(15) -0.0043(15) 0.0228(16) C48 0.0419(19) 0.0325(16) 0.039(2) -0.0027(14) -0.0071(15) 0.0212(15) C49 0.062(3) 0.082(3) 0.052(3) -0.028(2) 0.000(2) 0.041(3) C50 0.046(2) 0.061(2) 0.040(2) -0.0125(18) -0.0073(17) 0.0322(19) C51 0.062(3) 0.066(3) 0.036(2) 0.0012(19) -0.0023(19) 0.038(2) C52 0.058(3) 0.081(3) 0.051(3) -0.006(2) 0.000(2) 0.038(3) C53 0.043(2) 0.052(2) 0.045(2) 0.0025(19) -0.0097(18) 0.0174(18) C54 0.092(4) 0.057(3) 0.068(3) 0.007(2) -0.029(3) 0.036(3) C55 0.061(3) 0.047(2) 0.061(3) -0.013(2) -0.016(2) 0.035(2) C56 0.067(3) 0.083(3) 0.039(2) 0.001(2) 0.003(2) 0.047(3) C57 0.079(3) 0.066(3) 0.065(3) 0.001(3) -0.005(3) 0.041(3) C58 0.057(3) 0.055(2) 0.060(3) -0.001(2) 0.007(2) 0.028(2) C59 0.102(5) 0.076(4) 0.072(4) -0.008(3) -0.027(3) 0.045(3) C60 0.081(3) 0.052(3) 0.061(3) -0.005(2) -0.006(3) 0.039(3) C61 0.121(4) 0.075(3) 0.070(4) 0.007(3) 0.025(3) 0.064(3) C62 0.096(4) 0.063(3) 0.061(3) -0.005(3) -0.006(3) 0.038(3) C63 0.068(3) 0.054(3) 0.049(3) -0.006(2) 0.001(2) 0.023(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O2 2.283(2) 5_665 ? Cd1 O8 2.285(2) . ? Cd1 O9 2.305(3) . ? Cd1 O3 2.309(3) . ? Cd1 O4 2.517(2) . ? Cd1 O10 2.526(3) . ? Cd1 O1 2.701(3) 5_665 ? Cd1 O7 2.751(3) . ? Cd1 K3 3.9182(10) 6_654 ? Cd1 K1 3.9192(10) . ? Cd2 O12 2.309(3) . ? Cd2 O14 2.337(3) 3_665 ? Cd2 O5 2.337(3) 3_775 ? Cd2 O24 2.354(3) . ? Cd2 O23 2.432(3) . ? Cd2 O6 2.459(3) 3_775 ? Cd2 O13 2.511(3) 3_665 ? Cd2 C48 2.723(3) . ? Cd2 C15 2.735(3) 3_775 ? Cd2 C31 2.758(4) 3_665 ? Cd2 O11 2.761(4) . ? Cd2 K2 3.8246(10) 5_565 ? Cd3 O22 2.358(3) . ? Cd3 O20 2.363(3) 6_654 ? Cd3 O18 2.374(3) . ? Cd3 O16 2.395(3) . ? Cd3 O15 2.401(2) . ? Cd3 O17 2.436(2) . ? Cd3 O21 2.494(3) . ? Cd3 O19 2.510(3) 6_654 ? Cd3 C39 2.742(3) . ? Cd3 C32 2.743(3) . ? Cd3 K3 3.6668(9) . ? Cd3 K1 3.7358(9) 6_554 ? K1 O18 2.710(3) 5 ? K1 O9 2.713(3) . ? K1 O21 2.718(3) 5 ? K1 O25 2.831(4) . ? K1 O7 2.833(3) . ? K1 O26 2.958(3) . ? K1 O15 3.255(3) 5 ? K1 Cd3 3.7358(9) 5 ? K2 O24 2.611(3) . ? K2 O23 2.634(3) 6_654 ? K2 O11 2.689(3) 6_654 ? K2 O27 2.787(4) . ? K2 O28 2.914(3) . ? K2 O13 3.037(3) 3_665 ? K2 Cd2 3.8246(10) 6_654 ? K3 O3 2.662(3) 5_565 ? K3 O16 2.730(3) . ? K3 O19 2.746(3) 6_654 ? K3 O1 2.786(3) 3_665 ? K3 O29 2.809(5) . ? K3 O30 3.026(4) . ? K3 O17 3.035(3) . ? K3 Cd1 3.9182(10) 5_565 ? N1 C50 1.493(5) . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N2 C55 1.514(6) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 C60 1.491(7) . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? O1 C7 1.251(4) . ? O1 K3 2.786(3) 2_654 ? O2 C7 1.265(4) . ? O2 Cd1 2.283(2) 6_544 ? O3 C8 1.271(4) . ? O3 K3 2.662(3) 6_654 ? O4 C8 1.255(4) . ? O5 C15 1.271(4) . ? O5 Cd2 2.337(3) 2_754 ? O6 C15 1.248(4) . ? O6 Cd2 2.459(3) 2_754 ? O7 C16 1.250(5) . ? O8 C16 1.267(5) . ? O9 C23 1.266(4) . ? O10 C23 1.251(4) . ? O11 C24 1.240(5) . ? O11 K2 2.689(3) 5_565 ? O12 C24 1.254(5) . ? O13 C31 1.253(5) . ? O13 Cd2 2.511(3) 2_654 ? O13 K2 3.037(3) 2_654 ? O14 C31 1.259(5) . ? O14 Cd2 2.337(3) 2_654 ? O15 C32 1.272(4) . ? O15 K1 3.255(3) 6_554 ? O16 C32 1.251(4) . ? O17 C39 1.264(4) . ? O18 C39 1.264(4) . ? O18 K1 2.710(3) 6_554 ? O19 C40 1.258(4) . ? O19 Cd3 2.510(3) 5_565 ? O19 K3 2.746(3) 5_565 ? O20 C40 1.253(5) . ? O20 Cd3 2.363(3) 5_565 ? O21 C47 1.263(5) . ? O21 K1 2.718(3) 6_554 ? O22 C47 1.252(5) . ? O23 C48 1.232(5) . ? O23 K2 2.634(3) 5_565 ? O24 C48 1.256(4) . ? O25 C51 1.399(5) . ? O25 H25B 0.9300 . ? O26 C53 1.436(5) . ? O26 H26A 0.9300 . ? O27 C56 1.381(6) . ? O27 H27B 0.9300 . ? O28 C58 1.452(6) . ? O28 H28B 0.9300 . ? O29 C61 1.393(7) . ? O29 H29B 0.9300 . ? O30 C63 1.429(6) . ? O30 H30A 0.9300 . ? C1 C6 1.385(5) . ? C1 C2 1.399(5) . ? C1 H1A 0.9300 . ? C2 C3 1.382(5) . ? C2 C7 1.503(4) . ? C3 C4 1.382(5) . ? C3 H3A 0.9300 . ? C4 C5 1.379(6) . ? C4 H4A 0.9300 . ? C5 C6 1.410(5) . ? C5 H5A 0.9300 . ? C6 C8 1.498(5) . ? C9 C10 1.384(5) . ? C9 C14 1.391(5) . ? C9 H9A 0.9300 . ? C10 C11 1.393(5) . ? C10 C15 1.516(5) . ? C11 C12 1.394(5) . ? C11 H11A 0.9300 . ? C12 C13 1.380(5) . ? C12 H12A 0.9300 . ? C13 C14 1.397(5) . ? C13 H13A 0.9300 . ? C14 C16 1.506(5) . ? C15 Cd2 2.735(3) 2_754 ? C17 C22 1.382(5) . ? C17 C18 1.394(5) . ? C17 H17A 0.9300 . ? C18 C19 1.382(5) . ? C18 C23 1.505(5) . ? C19 C20 1.384(6) . ? C19 H19A 0.9300 . ? C20 C21 1.398(6) . ? C20 H20A 0.9300 . ? C21 C22 1.386(6) . ? C21 H21A 0.9300 . ? C22 C24 1.521(5) . ? C25 C26 1.390(5) . ? C25 C30 1.394(5) . ? C25 H25A 0.9300 . ? C26 C27 1.392(5) . ? C26 C31 1.496(5) . ? C27 C28 1.390(5) . ? C27 H27A 0.9300 . ? C28 C29 1.387(5) . ? C28 H28A 0.9300 . ? C29 C30 1.378(5) . ? C29 H29A 0.9300 . ? C30 C32 1.496(5) . ? C31 Cd2 2.758(4) 2_654 ? C33 C38 1.379(5) . ? C33 C34 1.393(5) . ? C33 H33A 0.9300 . ? C34 C35 1.385(5) . ? C34 C39 1.494(5) . ? C35 C36 1.397(5) . ? C35 H35A 0.9300 . ? C36 C37 1.389(5) . ? C36 H36A 0.9300 . ? C37 C38 1.384(5) . ? C37 H37A 0.9300 . ? C38 C40 1.507(5) . ? C41 C46 1.387(5) . ? C41 C42 1.394(5) . ? C41 H41A 0.848(19) . ? C42 C43 1.384(5) . ? C42 C47 1.505(5) . ? C43 C44 1.387(5) . ? C43 H43A 0.9300 . ? C44 C45 1.387(5) . ? C44 H44A 0.9300 . ? C45 C46 1.389(5) . ? C45 H45A 0.9300 . ? C46 C48 1.500(5) . ? C49 C50 1.524(6) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.499(6) . ? C50 H50A 0.9800 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.497(6) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.513(6) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.483(7) . ? C55 H55A 0.9800 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.483(6) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.519(7) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.491(7) . ? C60 H60A 0.9800 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.520(7) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cd1 O8 82.02(9) 5_665 . ? O2 Cd1 O9 96.23(9) 5_665 . ? O8 Cd1 O9 138.39(10) . . ? O2 Cd1 O3 137.25(9) 5_665 . ? O8 Cd1 O3 96.56(10) . . ? O9 Cd1 O3 111.21(10) . . ? O2 Cd1 O4 161.13(9) 5_665 . ? O8 Cd1 O4 81.38(9) . . ? O9 Cd1 O4 90.27(9) . . ? O3 Cd1 O4 54.11(8) . . ? O2 Cd1 O10 79.47(9) 5_665 . ? O8 Cd1 O10 159.20(10) . . ? O9 Cd1 O10 53.88(9) . . ? O3 Cd1 O10 90.67(9) . . ? O4 Cd1 O10 118.27(9) . . ? O2 Cd1 O1 51.78(9) 5_665 5_665 ? O8 Cd1 O1 75.41(10) . 5_665 ? O9 Cd1 O1 134.49(9) . 5_665 ? O3 Cd1 O1 86.30(9) . 5_665 ? O4 Cd1 O1 131.04(9) . 5_665 ? O10 Cd1 O1 85.68(9) . 5_665 ? O2 Cd1 O7 74.61(9) 5_665 . ? O8 Cd1 O7 51.03(9) . . ? O9 Cd1 O7 88.21(9) . . ? O3 Cd1 O7 135.70(9) . . ? O4 Cd1 O7 87.95(8) . . ? O10 Cd1 O7 130.86(9) . . ? O1 Cd1 O7 108.43(8) 5_665 . ? O2 Cd1 K3 97.03(7) 5_665 6_654 ? O8 Cd1 K3 81.35(7) . 6_654 ? O9 Cd1 K3 139.57(7) . 6_654 ? O3 Cd1 K3 41.28(7) . 6_654 ? O4 Cd1 K3 89.29(6) . 6_654 ? O10 Cd1 K3 91.56(7) . 6_654 ? O1 Cd1 K3 45.31(6) 5_665 6_654 ? O7 Cd1 K3 132.16(6) . 6_654 ? O2 Cd1 K1 78.72(7) 5_665 . ? O8 Cd1 K1 97.30(7) . . ? O9 Cd1 K1 42.53(7) . . ? O3 Cd1 K1 143.02(7) . . ? O4 Cd1 K1 94.56(6) . . ? O10 Cd1 K1 88.32(7) . . ? O1 Cd1 K1 130.41(6) 5_665 . ? O7 Cd1 K1 46.27(6) . . ? K3 Cd1 K1 175.69(2) 6_654 . ? O12 Cd2 O14 84.19(11) . 3_665 ? O12 Cd2 O5 135.75(10) . 3_775 ? O14 Cd2 O5 87.71(10) 3_665 3_775 ? O12 Cd2 O24 93.41(10) . . ? O14 Cd2 O24 143.04(10) 3_665 . ? O5 Cd2 O24 117.47(10) 3_775 . ? O12 Cd2 O23 85.15(11) . . ? O14 Cd2 O23 160.34(10) 3_665 . ? O5 Cd2 O23 88.47(9) 3_775 . ? O24 Cd2 O23 54.13(9) . . ? O12 Cd2 O6 165.99(10) . 3_775 ? O14 Cd2 O6 87.45(10) 3_665 3_775 ? O5 Cd2 O6 54.76(8) 3_775 3_775 ? O24 Cd2 O6 86.54(10) . 3_775 ? O23 Cd2 O6 105.93(10) . 3_775 ? O12 Cd2 O13 79.92(11) . 3_665 ? O14 Cd2 O13 54.01(10) 3_665 3_665 ? O5 Cd2 O13 127.72(10) 3_775 3_665 ? O24 Cd2 O13 89.20(10) . 3_665 ? O23 Cd2 O13 139.43(10) . 3_665 ? O6 Cd2 O13 86.07(10) 3_775 3_665 ? O12 Cd2 C48 86.67(10) . . ? O14 Cd2 C48 166.17(10) 3_665 . ? O5 Cd2 C48 106.06(10) 3_775 . ? O24 Cd2 C48 27.44(10) . . ? O23 Cd2 C48 26.91(10) . . ? O6 Cd2 C48 99.33(10) 3_775 . ? O13 Cd2 C48 114.09(11) 3_665 . ? O12 Cd2 C15 161.81(11) . 3_775 ? O14 Cd2 C15 86.98(10) 3_665 3_775 ? O5 Cd2 C15 27.61(9) 3_775 3_775 ? O24 Cd2 C15 103.14(10) . 3_775 ? O23 Cd2 C15 98.37(10) . 3_775 ? O6 Cd2 C15 27.15(9) 3_775 3_775 ? O13 Cd2 C15 107.45(10) 3_665 3_775 ? C48 Cd2 C15 104.56(10) . 3_775 ? O12 Cd2 C31 80.42(11) . 3_665 ? O14 Cd2 C31 27.02(11) 3_665 3_665 ? O5 Cd2 C31 109.16(10) 3_775 3_665 ? O24 Cd2 C31 116.17(11) . 3_665 ? O23 Cd2 C31 162.19(11) . 3_665 ? O6 Cd2 C31 87.03(10) 3_775 3_665 ? O13 Cd2 C31 27.00(10) 3_665 3_665 ? C48 Cd2 C31 140.56(12) . 3_665 ? C15 Cd2 C31 98.59(10) 3_775 3_665 ? O12 Cd2 O11 50.11(10) . . ? O14 Cd2 O11 81.07(10) 3_665 . ? O5 Cd2 O11 85.68(9) 3_775 . ? O24 Cd2 O11 124.63(10) . . ? O23 Cd2 O11 79.42(10) . . ? O6 Cd2 O11 139.27(9) 3_775 . ? O13 Cd2 O11 116.48(9) 3_665 . ? C48 Cd2 O11 100.90(11) . . ? C15 Cd2 O11 112.77(10) 3_775 . ? C31 Cd2 O11 98.90(10) 3_665 . ? O12 Cd2 K2 80.27(8) . 5_565 ? O14 Cd2 K2 118.58(8) 3_665 5_565 ? O5 Cd2 K2 65.91(6) 3_775 5_565 ? O24 Cd2 K2 97.13(7) . 5_565 ? O23 Cd2 K2 43.00(7) . 5_565 ? O6 Cd2 K2 113.66(7) 3_775 5_565 ? O13 Cd2 K2 159.52(8) 3_665 5_565 ? C48 Cd2 K2 69.78(8) . 5_565 ? C15 Cd2 K2 90.12(7) 3_775 5_565 ? C31 Cd2 K2 142.21(8) 3_665 5_565 ? O11 Cd2 K2 44.67(7) . 5_565 ? O22 Cd3 O20 87.65(10) . 6_654 ? O22 Cd3 O18 91.42(10) . . ? O20 Cd3 O18 165.00(9) 6_654 . ? O22 Cd3 O16 164.28(9) . . ? O20 Cd3 O16 93.80(10) 6_654 . ? O18 Cd3 O16 91.14(10) . . ? O22 Cd3 O15 141.11(9) . . ? O20 Cd3 O15 86.56(9) 6_654 . ? O18 Cd3 O15 84.79(9) . . ? O16 Cd3 O15 54.60(8) . . ? O22 Cd3 O17 84.74(10) . . ? O20 Cd3 O17 139.93(9) 6_654 . ? O18 Cd3 O17 54.71(8) . . ? O16 Cd3 O17 84.10(9) . . ? O15 Cd3 O17 122.31(8) . . ? O22 Cd3 O21 53.92(9) . . ? O20 Cd3 O21 86.73(9) 6_654 . ? O18 Cd3 O21 80.67(9) . . ? O16 Cd3 O21 141.77(9) . . ? O15 Cd3 O21 87.36(9) . . ? O17 Cd3 O21 118.79(9) . . ? O22 Cd3 O19 87.16(10) . 6_654 ? O20 Cd3 O19 53.43(9) 6_654 6_654 ? O18 Cd3 O19 141.50(9) . 6_654 ? O16 Cd3 O19 81.20(10) . 6_654 ? O15 Cd3 O19 118.83(9) . 6_654 ? O17 Cd3 O19 86.88(8) . 6_654 ? O21 Cd3 O19 126.83(8) . 6_654 ? O22 Cd3 C39 85.75(10) . . ? O20 Cd3 C39 166.44(10) 6_654 . ? O18 Cd3 C39 27.41(9) . . ? O16 Cd3 C39 89.43(10) . . ? O15 Cd3 C39 105.95(10) . . ? O17 Cd3 C39 27.45(9) . . ? O21 Cd3 C39 98.86(9) . . ? O19 Cd3 C39 114.33(10) 6_654 . ? O22 Cd3 C32 168.37(10) . . ? O20 Cd3 C32 88.24(10) 6_654 . ? O18 Cd3 C32 89.74(10) . . ? O16 Cd3 C32 27.12(9) . . ? O15 Cd3 C32 27.61(9) . . ? O17 Cd3 C32 105.28(9) . . ? O21 Cd3 C32 114.97(10) . . ? O19 Cd3 C32 99.07(10) 6_654 . ? C39 Cd3 C32 100.40(10) . . ? O22 Cd3 K3 116.18(7) . . ? O20 Cd3 K3 94.30(7) 6_654 . ? O18 Cd3 K3 99.52(7) . . ? O16 Cd3 K3 48.10(6) . . ? O15 Cd3 K3 102.59(6) . . ? O17 Cd3 K3 55.30(6) . . ? O21 Cd3 K3 170.04(7) . . ? O19 Cd3 K3 48.46(6) 6_654 . ? C39 Cd3 K3 78.09(7) . . ? C32 Cd3 K3 74.98(8) . . ? O22 Cd3 K1 90.60(7) . 6_554 ? O20 Cd3 K1 118.68(7) 6_654 6_554 ? O18 Cd3 K1 46.34(6) . 6_554 ? O16 Cd3 K1 102.34(7) . 6_554 ? O15 Cd3 K1 59.42(6) . 6_554 ? O17 Cd3 K1 100.71(6) . 6_554 ? O21 Cd3 K1 46.66(6) . 6_554 ? O19 Cd3 K1 171.86(6) 6_654 6_554 ? C39 Cd3 K1 73.26(7) . 6_554 ? C32 Cd3 K1 81.86(7) . 6_554 ? K3 Cd3 K1 138.91(2) . 6_554 ? O18 K1 O9 102.32(9) 5 . ? O18 K1 O21 70.99(9) 5 5 ? O9 K1 O21 136.59(9) . 5 ? O18 K1 O25 83.17(9) 5 . ? O9 K1 O25 138.40(10) . . ? O21 K1 O25 84.51(10) 5 . ? O18 K1 O7 157.81(8) 5 . ? O9 K1 O7 79.12(9) . . ? O21 K1 O7 92.55(9) 5 . ? O25 K1 O7 110.70(9) . . ? O18 K1 O26 119.31(9) 5 . ? O9 K1 O26 74.87(8) . . ? O21 K1 O26 146.80(9) 5 . ? O25 K1 O26 66.96(10) . . ? O7 K1 O26 82.63(9) . . ? O18 K1 O15 64.57(7) 5 5 ? O9 K1 O15 70.35(7) . 5 ? O21 K1 O15 68.28(8) 5 5 ? O25 K1 O15 142.77(8) . 5 ? O7 K1 O15 95.94(8) . 5 ? O26 K1 O15 144.78(8) . 5 ? O18 K1 Cd3 39.31(5) 5 5 ? O9 K1 Cd3 106.26(6) . 5 ? O21 K1 Cd3 41.86(6) 5 5 ? O25 K1 Cd3 103.51(7) . 5 ? O7 K1 Cd3 118.71(6) . 5 ? O26 K1 Cd3 158.62(7) . 5 ? O15 K1 Cd3 39.43(4) 5 5 ? O18 K1 Cd1 135.95(7) 5 . ? O9 K1 Cd1 35.05(6) . . ? O21 K1 Cd1 126.76(7) 5 . ? O25 K1 Cd1 133.02(7) . . ? O7 K1 Cd1 44.57(6) . . ? O26 K1 Cd1 70.11(6) . . ? O15 K1 Cd1 84.21(5) 5 . ? Cd3 K1 Cd1 123.26(3) 5 . ? O24 K2 O23 98.63(10) . 6_654 ? O24 K2 O11 125.15(10) . 6_654 ? O23 K2 O11 77.36(10) 6_654 6_654 ? O24 K2 O27 147.85(12) . . ? O23 K2 O27 79.88(10) 6_654 . ? O11 K2 O27 86.18(12) 6_654 . ? O24 K2 O28 81.87(9) . . ? O23 K2 O28 114.08(10) 6_654 . ? O11 K2 O28 150.14(11) 6_654 . ? O27 K2 O28 69.94(11) . . ? O24 K2 O13 74.03(9) . 3_665 ? O23 K2 O13 154.15(10) 6_654 3_665 ? O11 K2 O13 86.68(10) 6_654 3_665 ? O27 K2 O13 119.61(10) . 3_665 ? O28 K2 O13 89.79(9) . 3_665 ? O24 K2 Cd2 98.23(7) . 6_654 ? O23 K2 Cd2 39.03(6) 6_654 6_654 ? O11 K2 Cd2 46.20(8) 6_654 6_654 ? O27 K2 Cd2 100.06(8) . 6_654 ? O28 K2 Cd2 153.03(8) . 6_654 ? O13 K2 Cd2 116.32(7) 3_665 6_654 ? O24 K2 Cd2 36.15(6) . . ? O23 K2 Cd2 134.31(8) 6_654 . ? O11 K2 Cd2 118.41(8) 6_654 . ? O27 K2 Cd2 139.17(8) . . ? O28 K2 Cd2 74.54(7) . . ? O13 K2 Cd2 40.20(6) 3_665 . ? Cd2 K2 Cd2 120.60(3) 6_654 . ? O3 K3 O16 105.22(9) 5_565 . ? O3 K3 O19 142.12(9) 5_565 6_654 ? O16 K3 O19 71.34(9) . 6_654 ? O3 K3 O1 78.22(9) 5_565 3_665 ? O16 K3 O1 162.36(9) . 3_665 ? O19 K3 O1 95.14(9) 6_654 3_665 ? O3 K3 O29 132.54(14) 5_565 . ? O16 K3 O29 79.40(11) . . ? O19 K3 O29 84.82(14) 6_654 . ? O1 K3 O29 111.39(11) 3_665 . ? O3 K3 O30 73.77(9) 5_565 . ? O16 K3 O30 118.89(9) . . ? O19 K3 O30 142.12(10) 6_654 . ? O1 K3 O30 78.75(9) 3_665 . ? O29 K3 O30 63.73(12) . . ? O3 K3 O17 72.10(8) 5_565 . ? O16 K3 O17 68.05(8) . . ? O19 K3 O17 71.89(8) 6_654 . ? O1 K3 O17 97.40(8) 3_665 . ? O29 K3 O17 144.48(10) . . ? O30 K3 O17 145.70(9) . . ? O3 K3 Cd3 109.53(6) 5_565 . ? O16 K3 Cd3 40.76(6) . . ? O19 K3 Cd3 43.17(6) 6_654 . ? O1 K3 Cd3 121.61(7) 3_665 . ? O29 K3 Cd3 103.84(10) . . ? O30 K3 Cd3 159.59(7) . . ? O17 K3 Cd3 41.29(5) . . ? O3 K3 Cd1 34.91(6) 5_565 5_565 ? O16 K3 Cd1 139.08(7) . 5_565 ? O19 K3 Cd1 129.90(7) 6_654 5_565 ? O1 K3 Cd1 43.56(6) 3_665 5_565 ? O29 K3 Cd1 130.17(10) . 5_565 ? O30 K3 Cd1 68.57(7) . 5_565 ? O17 K3 Cd1 85.07(5) . 5_565 ? Cd3 K3 Cd1 125.98(3) . 5_565 ? C50 N1 H1B 109.5 . . ? C50 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C50 N1 H1D 109.5 . . ? H1B N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C55 N2 H2A 109.5 . . ? C55 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C55 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C60 N3 H3B 109.5 . . ? C60 N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C60 N3 H3D 109.5 . . ? H3B N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C7 O1 K3 173.8(3) . 2_654 ? C7 O2 Cd1 102.0(2) . 6_544 ? C8 O3 Cd1 96.7(2) . . ? C8 O3 K3 135.6(2) . 6_654 ? Cd1 O3 K3 103.81(10) . 6_654 ? C8 O4 Cd1 87.51(19) . . ? C15 O5 Cd2 93.9(2) . 2_754 ? C15 O6 Cd2 88.9(2) . 2_754 ? C16 O7 Cd1 82.0(2) . . ? C16 O7 K1 170.4(3) . . ? Cd1 O7 K1 89.15(8) . . ? C16 O8 Cd1 103.5(2) . . ? C23 O9 Cd1 97.1(2) . . ? C23 O9 K1 131.2(2) . . ? Cd1 O9 K1 102.42(10) . . ? C23 O10 Cd1 87.2(2) . . ? C24 O11 K2 128.8(3) . 5_565 ? C24 O11 Cd2 82.4(3) . . ? K2 O11 Cd2 89.13(10) 5_565 . ? C24 O12 Cd2 103.5(2) . . ? C31 O13 Cd2 87.6(2) . 2_654 ? C31 O13 K2 164.9(3) . 2_654 ? Cd2 O13 K2 88.46(8) 2_654 2_654 ? C31 O14 Cd2 95.5(2) . 2_654 ? C32 O15 Cd3 91.3(2) . . ? C32 O15 K1 140.2(2) . 6_554 ? Cd3 O15 K1 81.15(7) . 6_554 ? C32 O16 Cd3 92.1(2) . . ? C32 O16 K3 170.4(3) . . ? Cd3 O16 K3 91.13(8) . . ? C39 O17 Cd3 89.9(2) . . ? C39 O17 K3 141.5(2) . . ? Cd3 O17 K3 83.41(7) . . ? C39 O18 Cd3 92.7(2) . . ? C39 O18 K1 165.5(2) . 6_554 ? Cd3 O18 K1 94.35(9) . 6_554 ? C40 O19 Cd3 88.6(2) . 5_565 ? C40 O19 K3 145.5(3) . 5_565 ? Cd3 O19 K3 88.37(8) 5_565 5_565 ? C40 O20 Cd3 95.6(2) . 5_565 ? C47 O21 Cd3 88.3(2) . . ? C47 O21 K1 139.2(2) . 6_554 ? Cd3 O21 K1 91.48(9) . 6_554 ? C47 O22 Cd3 94.9(2) . . ? C48 O23 Cd2 89.8(2) . . ? C48 O23 K2 169.6(3) . 5_565 ? Cd2 O23 K2 97.97(9) . 5_565 ? C48 O24 Cd2 92.9(2) . . ? C48 O24 K2 133.3(2) . . ? Cd2 O24 K2 102.98(10) . . ? C51 O25 K1 135.6(3) . . ? C51 O25 H25B 112.2 . . ? K1 O25 H25B 112.2 . . ? C53 O26 K1 132.7(2) . . ? C53 O26 H26A 113.7 . . ? K1 O26 H26A 113.7 . . ? C56 O27 K2 132.7(3) . . ? C56 O27 H27B 113.6 . . ? K2 O27 H27B 113.6 . . ? C58 O28 K2 137.1(3) . . ? C58 O28 H28B 111.5 . . ? K2 O28 H28B 111.5 . . ? C61 O29 K3 134.6(5) . . ? C61 O29 H29B 112.7 . . ? K3 O29 H29B 112.7 . . ? C63 O30 K3 126.1(3) . . ? C63 O30 H30A 117.0 . . ? K3 O30 H30A 117.0 . . ? C6 C1 C2 121.1(3) . . ? C6 C1 H1A 119.4 . . ? C2 C1 H1A 119.4 . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C7 122.0(3) . . ? C1 C2 C7 119.5(3) . . ? C2 C3 C4 121.3(3) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 120.2(4) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C1 C6 C5 119.0(3) . . ? C1 C6 C8 120.0(3) . . ? C5 C6 C8 120.9(3) . . ? O1 C7 O2 122.7(3) . . ? O1 C7 C2 119.6(3) . . ? O2 C7 C2 117.6(3) . . ? O4 C8 O3 121.4(3) . . ? O4 C8 C6 120.2(3) . . ? O3 C8 C6 118.3(3) . . ? C10 C9 C14 121.0(3) . . ? C10 C9 H9A 119.5 . . ? C14 C9 H9A 119.5 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 C15 119.7(3) . . ? C11 C10 C15 120.0(3) . . ? C10 C11 C12 118.9(3) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C9 C14 C13 118.5(3) . . ? C9 C14 C16 120.7(3) . . ? C13 C14 C16 120.8(3) . . ? O6 C15 O5 122.5(3) . . ? O6 C15 C10 119.2(3) . . ? O5 C15 C10 118.4(3) . . ? O6 C15 Cd2 64.00(18) . 2_754 ? O5 C15 Cd2 58.48(18) . 2_754 ? C10 C15 Cd2 176.3(2) . 2_754 ? O7 C16 O8 122.7(3) . . ? O7 C16 C14 120.3(4) . . ? O8 C16 C14 117.0(3) . . ? C22 C17 C18 120.9(4) . . ? C22 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 C23 120.8(3) . . ? C17 C18 C23 119.4(3) . . ? C18 C19 C20 119.6(4) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C19 C20 C21 120.5(4) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C22 C21 C20 119.8(4) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C17 C22 C21 119.3(4) . . ? C17 C22 C24 120.7(4) . . ? C21 C22 C24 119.9(4) . . ? O10 C23 O9 121.6(3) . . ? O10 C23 C18 120.2(3) . . ? O9 C23 C18 118.2(3) . . ? O11 C24 O12 122.4(4) . . ? O11 C24 C22 119.8(4) . . ? O12 C24 C22 117.6(4) . . ? C26 C25 C30 121.6(3) . . ? C26 C25 H25A 119.2 . . ? C30 C25 H25A 119.2 . . ? C25 C26 C27 118.3(3) . . ? C25 C26 C31 120.0(3) . . ? C27 C26 C31 121.6(3) . . ? C28 C27 C26 120.5(3) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C29 C28 C27 120.2(4) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C25 119.1(3) . . ? C29 C30 C32 122.5(3) . . ? C25 C30 C32 118.2(3) . . ? O13 C31 O14 122.9(3) . . ? O13 C31 C26 119.6(3) . . ? O14 C31 C26 117.5(3) . . ? O13 C31 Cd2 65.4(2) . 2_654 ? O14 C31 Cd2 57.50(19) . 2_654 ? C26 C31 Cd2 173.9(3) . 2_654 ? O16 C32 O15 121.3(3) . . ? O16 C32 C30 119.5(3) . . ? O15 C32 C30 119.1(3) . . ? O16 C32 Cd3 60.74(18) . . ? O15 C32 Cd3 61.06(17) . . ? C30 C32 Cd3 170.9(2) . . ? C38 C33 C34 121.6(3) . . ? C38 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C35 C34 C33 119.5(3) . . ? C35 C34 C39 122.0(3) . . ? C33 C34 C39 118.4(3) . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C33 C38 C37 118.6(3) . . ? C33 C38 C40 119.9(3) . . ? C37 C38 C40 121.4(3) . . ? O18 C39 O17 122.0(3) . . ? O18 C39 C34 117.8(3) . . ? O17 C39 C34 120.1(3) . . ? O18 C39 Cd3 59.85(18) . . ? O17 C39 Cd3 62.67(18) . . ? C34 C39 Cd3 169.8(2) . . ? O20 C40 O19 121.8(3) . . ? O20 C40 C38 118.7(3) . . ? O19 C40 C38 119.3(3) . . ? C46 C41 C42 121.5(3) . . ? C46 C41 H41A 115(3) . . ? C42 C41 H41A 123(3) . . ? C43 C42 C41 118.5(3) . . ? C43 C42 C47 122.0(3) . . ? C41 C42 C47 119.1(3) . . ? C42 C43 C44 120.5(3) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? C43 C44 C45 120.4(4) . . ? C43 C44 H44A 119.8 . . ? C45 C44 H44A 119.8 . . ? C44 C45 C46 119.9(3) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? C41 C46 C45 119.1(3) . . ? C41 C46 C48 117.9(3) . . ? C45 C46 C48 122.7(3) . . ? O22 C47 O21 122.3(3) . . ? O22 C47 C42 119.2(3) . . ? O21 C47 C42 118.4(3) . . ? O23 C48 O24 122.2(3) . . ? O23 C48 C46 119.8(3) . . ? O24 C48 C46 117.9(3) . . ? O23 C48 Cd2 63.3(2) . . ? O24 C48 Cd2 59.70(19) . . ? C46 C48 Cd2 167.7(2) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N1 C50 C51 110.3(3) . . ? N1 C50 C49 108.0(4) . . ? C51 C50 C49 114.3(4) . . ? N1 C50 H50A 108.1 . . ? C51 C50 H50A 108.1 . . ? C49 C50 H50A 108.1 . . ? O25 C51 C50 111.0(4) . . ? O25 C51 H51A 109.4 . . ? C50 C51 H51A 109.4 . . ? O25 C51 H51B 109.4 . . ? C50 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O26 C53 C52 109.0(4) . . ? O26 C53 H53A 109.9 . . ? C52 C53 H53A 109.9 . . ? O26 C53 H53B 109.9 . . ? C52 C53 H53B 109.9 . . ? H53A C53 H53B 108.3 . . ? 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 C54 114.3(4) . . ? C56 C55 N2 109.8(4) . . ? C54 C55 N2 107.1(4) . . ? C56 C55 H55A 108.5 . . ? C54 C55 H55A 108.5 . . ? N2 C55 H55A 108.5 . . ? O27 C56 C55 111.8(4) . . ? O27 C56 H56A 109.3 . . ? C55 C56 H56A 109.3 . . ? O27 C56 H56B 109.3 . . ? C55 C56 H56B 109.3 . . ? H56A C56 H56B 107.9 . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? O28 C58 C57 108.7(4) . . ? O28 C58 H58A 110.0 . . ? C57 C58 H58A 110.0 . . ? O28 C58 H58B 110.0 . . ? C57 C58 H58B 110.0 . . ? H58A C58 H58B 108.3 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N3 C60 C61 113.2(4) . . ? N3 C60 C59 107.7(5) . . ? C61 C60 C59 112.5(5) . . ? N3 C60 H60A 107.7 . . ? C61 C60 H60A 107.7 . . ? C59 C60 H60A 107.7 . . ? O29 C61 C60 111.3(5) . . ? O29 C61 H61A 109.4 . . ? C60 C61 H61A 109.4 . . ? O29 C61 H61B 109.4 . . ? C60 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O30 C63 C62 108.3(4) . . ? O30 C63 H63A 110.0 . . ? C62 C63 H63A 110.0 . . ? O30 C63 H63B 110.0 . . ? C62 C63 H63B 110.0 . . ? H63A C63 H63B 108.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.669 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.063 data_complex_1L _database_code_depnum_ccdc_archive 'CCDC 926654' #TrackingRef '926654-new.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H72 Cd3 K3 N3 O30' _chemical_formula_weight 1805.74 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/6' '-y, x-y, z+1/3' '-x, -y, z+1/2' '-x+y, -x, z+2/3' 'y, -x+y, z+5/6' _cell_length_a 20.609(3) _cell_length_b 20.609(3) _cell_length_c 28.314(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10414(2) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35084 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .11 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5472 _exptl_absorpt_coefficient_mu 1.181 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7951 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _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 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 90167 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.49 _reflns_number_total 15851 _reflns_number_gt 15379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+52.8281P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(3) _Chemical_absolute_configuration ad _refine_ls_number_reflns 15851 _refine_ls_number_parameters 922 _refine_ls_number_restraints 32 _refine_ls_R_factor_ref 0.0722 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.108 _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 Cd1 Cd -0.66700(3) 0.44366(3) 1.17511(2) 0.03280(13) Uani 1 1 d . . . Cd2 Cd -0.23198(4) 0.76915(4) 1.001722(16) 0.03844(17) Uani 1 1 d . . . Cd3 Cd -0.33411(3) 1.09013(3) 1.17523(2) 0.03389(13) Uani 1 1 d . . . K1 K -0.75283(12) 0.39516(12) 1.04783(8) 0.0519(5) Uani 1 1 d . . . K2 K -0.19305(18) 0.72914(16) 1.12998(12) 0.0774(8) Uani 1 1 d . . . K3 K -0.51722(14) 1.05898(14) 1.13314(9) 0.0592(6) Uani 1 1 d . . . N1 N -0.6288(4) 0.2799(5) 0.9917(3) 0.057(2) Uani 1 1 d . . . H1B H -0.6097 0.2915 0.9627 0.086 Uiso 1 1 calc R . . H1C H -0.6061 0.2599 1.0079 0.086 Uiso 1 1 calc R . . H1D H -0.6218 0.3212 1.0063 0.086 Uiso 1 1 calc R . . N2 N -0.4285(6) 0.6154(6) 1.1912(4) 0.082(3) Uani 1 1 d U . . H2A H -0.4373 0.6241 1.2206 0.124 Uiso 1 1 calc R . . H2B H -0.4709 0.5952 1.1747 0.124 Uiso 1 1 calc R . . H2C H -0.3951 0.6584 1.1778 0.124 Uiso 1 1 calc R . . N3 N -0.7654(7) 0.9354(7) 1.1880(4) 0.086(3) Uani 1 1 d U . . H3B H -0.7733 0.9466 1.2170 0.129 Uiso 1 1 calc R . . H3C H -0.8089 0.9108 1.1727 0.129 Uiso 1 1 calc R . . H3D H -0.7350 0.9774 1.1725 0.129 Uiso 1 1 calc R . . O1 O -0.9826(5) 0.4395(5) 1.3815(3) 0.065(2) Uani 1 1 d . . . O2 O -0.9954(3) 0.4020(3) 1.3069(2) 0.0380(13) Uani 1 1 d . . . O3 O -0.6644(3) 0.5047(4) 1.2439(3) 0.062(2) Uani 1 1 d . . . O4 O -0.7758(3) 0.4502(4) 1.2097(2) 0.0461(16) Uani 1 1 d . . . O5 O -0.8194(4) -0.0054(3) 1.2607(2) 0.0509(17) Uani 1 1 d . . . O6 O -0.7815(4) 0.1013(4) 1.2997(2) 0.0451(15) Uani 1 1 d . . . O7 O -0.7702(4) 0.3142(4) 1.1322(2) 0.0472(16) Uani 1 1 d . . . O8 O -0.7306(4) 0.3260(3) 1.2053(2) 0.0501(17) Uani 1 1 d . . . O9 O -0.6716(3) 0.5069(3) 1.1100(2) 0.0438(14) Uani 1 1 d . . . O10 O -0.5590(4) 0.5632(4) 1.1420(3) 0.0581(19) Uani 1 1 d . . . O11 O -0.3563(5) 0.7727(5) 0.9762(4) 0.085(3) Uani 1 1 d . . . O12 O -0.3415(4) 0.7319(5) 1.0430(3) 0.063(2) Uani 1 1 d . . . O13 O -0.6470(4) 1.1007(5) 1.3695(4) 0.077(3) Uani 1 1 d . . . O14 O -0.6510(4) 1.0506(4) 1.2989(3) 0.0584(19) Uani 1 1 d . . . O15 O -0.3216(3) 1.1502(3) 1.2499(2) 0.0401(13) Uani 1 1 d . . . O16 O -0.4193(4) 1.1248(5) 1.2070(3) 0.062(2) Uani 1 1 d . . . O17 O -0.3523(4) 1.1393(4) 1.1023(3) 0.0547(18) Uani 1 1 d . . . O18 O -0.2516(4) 1.2142(4) 1.1466(2) 0.0561(18) Uani 1 1 d . . . O19 O -0.0269(4) 1.4263(4) 0.9889(3) 0.061(2) Uani 1 1 d . . . O20 O -0.0234(3) 1.3647(4) 1.0513(2) 0.0474(15) Uani 1 1 d . . . O21 O -0.2100(4) 1.0989(4) 1.1923(3) 0.0577(19) Uani 1 1 d . . . O22 O -0.2751(4) 1.0402(5) 1.1284(3) 0.063(2) Uani 1 1 d . . . O23 O -0.1974(4) 0.8947(4) 1.0289(3) 0.062(2) Uani 1 1 d . . . O24 O -0.1569(4) 0.8333(4) 1.0679(2) 0.0562(19) Uani 1 1 d . . . O25 O -0.7318(6) 0.3249(5) 0.9706(3) 0.083(3) Uani 1 1 d . . . H25B H -0.7061 0.3597 0.9469 0.100 Uiso 1 1 calc R . . O26 O -0.6016(5) 0.4097(5) 1.0464(3) 0.0623(19) Uani 1 1 d . . . H26A H -0.6014 0.3674 1.0576 0.075 Uiso 1 1 calc R . . O27 O -0.2770(6) 0.6606(6) 1.2119(4) 0.103(4) Uani 1 1 d . . . H27B H -0.2657 0.6937 1.2369 0.123 Uiso 1 1 calc R . . O28 O -0.3222(4) 0.7502(5) 1.1352(3) 0.067(2) Uani 1 1 d . . . H28B H -0.3653 0.7070 1.1256 0.080 Uiso 1 1 calc R . . O29 O -0.6125(6) 0.9883(6) 1.2106(4) 0.103(3) Uani 1 1 d U . . H29B H -0.6101 1.0215 1.2337 0.124 Uiso 1 1 calc R . . O30 O -0.6612(5) 1.0620(5) 1.1316(3) 0.075(2) Uani 1 1 d . . . H30A H -0.7034 1.0188 1.1210 0.090 Uiso 1 1 calc R . . C1 C -0.8410(5) 0.4692(5) 1.2937(3) 0.045(2) Uani 1 1 d . . . H1A H -0.8726 0.4386 1.2700 0.053 Uiso 1 1 calc R . . C2 C -0.8728(4) 0.4782(6) 1.3357(3) 0.050(2) Uani 1 1 d . . . C3 C -0.8238(6) 0.5242(6) 1.3712(3) 0.053(3) Uani 1 1 d . . . H3A H -0.8432 0.5299 1.3996 0.064 Uiso 1 1 calc R . . C4 C -0.7467(7) 0.5614(6) 1.3644(4) 0.067(3) Uani 1 1 d . . . H4A H -0.7156 0.5940 1.3876 0.081 Uiso 1 1 calc R . . C5 C -0.7146(5) 0.5512(6) 1.3236(4) 0.059(3) Uani 1 1 d . . . H5A H -0.6629 0.5736 1.3201 0.071 Uiso 1 1 calc R . . C6 C -0.7653(5) 0.5041(5) 1.2870(4) 0.049(2) Uani 1 1 d . . . C7 C -0.9549(4) 0.4398(5) 1.3417(3) 0.0386(18) Uani 1 1 d . . . C8 C -0.7343(4) 0.4857(5) 1.2438(3) 0.0402(19) Uani 1 1 d . . . C9 C -0.7954(4) 0.1697(5) 1.2180(3) 0.0357(17) Uani 1 1 d . . . H9A H -0.7658 0.2002 1.2425 0.043 Uiso 1 1 calc R . . C10 C -0.8287(4) 0.0928(5) 1.2219(3) 0.0359(17) Uani 1 1 d . . . C11 C -0.8746(5) 0.0464(5) 1.1860(3) 0.0398(18) Uani 1 1 d . . . H11A H -0.8968 -0.0054 1.1889 0.048 Uiso 1 1 calc R . . C12 C -0.8871(5) 0.0763(5) 1.1467(3) 0.046(2) Uani 1 1 d . . . H12A H -0.9178 0.0448 1.1229 0.055 Uiso 1 1 calc R . . C13 C -0.8543(5) 0.1540(5) 1.1417(3) 0.0404(19) Uani 1 1 d . . . H13A H -0.8643 0.1739 1.1150 0.048 Uiso 1 1 calc R . . C14 C -0.8062(5) 0.2021(5) 1.1771(3) 0.0385(17) Uani 1 1 d . . . C15 C -0.8093(5) 0.0594(5) 1.2641(3) 0.0404(19) Uani 1 1 d . . . C16 C -0.7656(5) 0.2864(5) 1.1714(4) 0.043(2) Uani 1 1 d . . . C17 C -0.4955(5) 0.6550(5) 1.0639(4) 0.048(2) Uani 1 1 d . . . H17A H -0.4639 0.6562 1.0877 0.058 Uiso 1 1 calc R . . C18 C -0.5729(5) 0.6109(5) 1.0683(4) 0.045(2) Uani 1 1 d . . . C19 C -0.6213(6) 0.6142(5) 1.0359(4) 0.056(3) Uani 1 1 d . . . H19A H -0.6728 0.5871 1.0408 0.068 Uiso 1 1 calc R . . C20 C -0.5918(6) 0.6586(6) 0.9959(4) 0.066(3) Uani 1 1 d . . . H20A H -0.6236 0.6587 0.9726 0.080 Uiso 1 1 calc R . . C21 C -0.5132(6) 0.7038(6) 0.9907(4) 0.064(3) Uani 1 1 d . . . H21A H -0.4928 0.7375 0.9658 0.077 Uiso 1 1 calc R . . C22 C -0.4672(6) 0.6966(5) 1.0238(4) 0.053(2) Uani 1 1 d . . . C23 C -0.6022(5) 0.5581(5) 1.1089(3) 0.0417(19) Uani 1 1 d . . . C24 C -0.3809(6) 0.7390(7) 1.0142(5) 0.070(4) Uani 1 1 d . . . C25 C -0.4965(5) 1.1298(5) 1.2893(3) 0.043(2) Uani 1 1 d . . . H25A H -0.5254 1.1009 1.2640 0.052 Uiso 1 1 calc R . . C26 C -0.5328(5) 1.1372(5) 1.3288(4) 0.046(2) Uani 1 1 d . . . C27 C -0.4896(6) 1.1812(6) 1.3658(4) 0.054(3) Uani 1 1 d . . . H27A H -0.5125 1.1842 1.3934 0.065 Uiso 1 1 calc R . . C28 C -0.4112(6) 1.2215(6) 1.3619(4) 0.061(3) Uani 1 1 d . . . H28A H -0.3824 1.2563 1.3849 0.074 Uiso 1 1 calc R . . C29 C -0.3770(5) 1.2087(6) 1.3233(3) 0.048(2) Uani 1 1 d . . . H29A H -0.3251 1.2305 1.3225 0.057 Uiso 1 1 calc R . . C30 C -0.4196(5) 1.1637(5) 1.2862(3) 0.0402(19) Uani 1 1 d . . . C31 C -0.6159(6) 1.0950(6) 1.3335(5) 0.062(3) Uani 1 1 d . . . C32 C -0.3849(5) 1.1459(5) 1.2458(3) 0.043(2) Uani 1 1 d . . . C33 C -0.1777(5) 1.2993(6) 1.0665(4) 0.055(3) Uani 1 1 d . . . H33A H -0.1485 1.2956 1.0903 0.066 Uiso 1 1 calc R . . C34 C -0.2566(5) 1.2563(5) 1.0699(4) 0.047(2) Uani 1 1 d . . . C35 C -0.2987(5) 1.2645(7) 1.0359(4) 0.062(3) Uani 1 1 d . . . H35A H -0.3507 1.2350 1.0368 0.074 Uiso 1 1 calc R . . C36 C -0.2641(6) 1.3171(8) 0.9997(4) 0.076(4) Uani 1 1 d . . . H36A H -0.2927 1.3262 0.9782 0.091 Uiso 1 1 calc R . . C37 C -0.1856(6) 1.3558(7) 0.9963(4) 0.066(3) Uani 1 1 d . . . H37A H -0.1623 1.3885 0.9712 0.079 Uiso 1 1 calc R . . C38 C -0.1433(5) 1.3461(6) 1.0294(4) 0.052(3) Uani 1 1 d . . . C39 C -0.2895(5) 1.2016(7) 1.1089(4) 0.055(3) Uani 1 1 d . . . C40 C -0.0589(5) 1.3824(5) 1.0229(3) 0.046(2) Uani 1 1 d . . . C41 C -0.1829(5) 0.9795(6) 1.1091(3) 0.046(2) Uani 1 1 d D . . H41A H -0.216(4) 0.975(6) 1.090(3) 0.056 Uiso 1 1 d D . . C42 C -0.1716(5) 1.0248(5) 1.1504(3) 0.0410(19) Uani 1 1 d . . . C43 C -0.1191(5) 1.0305(6) 1.1832(4) 0.052(2) Uani 1 1 d . . . H43A H -0.1092 1.0610 1.2095 0.063 Uiso 1 1 calc R . . C44 C -0.0817(5) 0.9922(6) 1.1774(4) 0.055(2) Uani 1 1 d . . . H44A H -0.0466 0.9977 1.2000 0.065 Uiso 1 1 calc R . . C45 C -0.0940(5) 0.9452(6) 1.1390(4) 0.051(2) Uani 1 1 d . . . H45A H -0.0696 0.9178 1.1361 0.062 Uiso 1 1 calc R . . C46 C -0.1461(5) 0.9415(6) 1.1042(3) 0.046(2) Uani 1 1 d . . . C47 C -0.2208(5) 1.0587(6) 1.1558(4) 0.048(2) Uani 1 1 d . . . C48 C -0.1687(5) 0.8857(5) 1.0636(4) 0.047(2) Uani 1 1 d . . . C49 C -0.7427(8) 0.2056(7) 1.0385(4) 0.068(3) Uani 1 1 d . . . H49A H -0.7954 0.1701 1.0373 0.103 Uiso 1 1 calc R . . H49B H -0.7347 0.2504 1.0540 0.103 Uiso 1 1 calc R . . H49C H -0.7176 0.1844 1.0558 0.103 Uiso 1 1 calc R . . C50 C -0.7116(6) 0.2243(7) 0.9888(4) 0.055(3) Uani 1 1 d . . . H50A H -0.7175 0.1783 0.9746 0.066 Uiso 1 1 calc R . . C51 C -0.7475(7) 0.2547(6) 0.9563(4) 0.059(3) Uani 1 1 d . . . H51A H -0.7291 0.2574 0.9244 0.071 Uiso 1 1 calc R . . H51B H -0.8013 0.2212 0.9561 0.071 Uiso 1 1 calc R . . C52 C -0.5357(8) 0.4979(8) 0.9855(4) 0.075(4) Uani 1 1 d . . . H52A H -0.4868 0.5371 0.9761 0.112 Uiso 1 1 calc R . . H52B H -0.5689 0.5177 0.9879 0.112 Uiso 1 1 calc R . . H52C H -0.5545 0.4586 0.9624 0.112 Uiso 1 1 calc R . . C53 C -0.5305(7) 0.4674(7) 1.0323(4) 0.059(3) Uani 1 1 d . . . H53A H -0.4962 0.4481 1.0302 0.071 Uiso 1 1 calc R . . H53B H -0.5111 0.5071 1.0557 0.071 Uiso 1 1 calc R . . C54 C -0.3836(9) 0.5505(11) 1.1403(5) 0.122(7) Uani 1 1 d . . . H54A H -0.3626 0.5182 1.1389 0.182 Uiso 1 1 calc R . . H54B H -0.3492 0.5981 1.1265 0.182 Uiso 1 1 calc R . . H54C H -0.4300 0.5282 1.1232 0.182 Uiso 1 1 calc R . . C55 C -0.3979(6) 0.5618(6) 1.1918(4) 0.059(3) Uani 1 1 d . . . H55A H -0.4372 0.5135 1.2041 0.070 Uiso 1 1 calc R . . C56 C -0.3314(7) 0.5883(7) 1.2227(4) 0.061(3) Uani 1 1 d . . . H56A H -0.3464 0.5861 1.2554 0.074 Uiso 1 1 calc R . . H56B H -0.3107 0.5553 1.2191 0.074 Uiso 1 1 calc R . . C57 C -0.3045(8) 0.8354(8) 1.1959(5) 0.087(4) Uani 1 1 d . . . H57A H -0.3127 0.8744 1.2077 0.131 Uiso 1 1 calc R . . H57B H -0.2517 0.8540 1.1930 0.131 Uiso 1 1 calc R . . H57C H -0.3259 0.7937 1.2174 0.131 Uiso 1 1 calc R . . C58 C -0.3403(8) 0.8107(6) 1.1491(4) 0.074(4) Uani 1 1 d . . . H58A H -0.3194 0.8518 1.1266 0.089 Uiso 1 1 calc R . . H58B H -0.3940 0.7907 1.1511 0.089 Uiso 1 1 calc R . . C59 C -0.7176(9) 0.8679(10) 1.1418(5) 0.099(5) Uani 1 1 d . . . H59A H -0.7612 0.8528 1.1226 0.148 Uiso 1 1 calc R . . H59B H -0.7075 0.8273 1.1442 0.148 Uiso 1 1 calc R . . H59C H -0.6754 0.9104 1.1277 0.148 Uiso 1 1 calc R . . C60 C -0.7313(8) 0.8888(7) 1.1908(5) 0.079(4) Uani 1 1 d . . . H60A H -0.7701 0.8415 1.2045 0.095 Uiso 1 1 calc R . . C61 C -0.6638(7) 0.9116(8) 1.2213(5) 0.077(3) Uani 1 1 d U . . H61A H -0.6775 0.9059 1.2544 0.093 Uiso 1 1 calc R . . H61B H -0.6414 0.8809 1.2145 0.093 Uiso 1 1 calc R . . C62 C -0.6385(8) 1.1458(9) 1.1954(5) 0.086(4) Uani 1 1 d . . . H62A H -0.6445 1.1863 1.2068 0.129 Uiso 1 1 calc R . . H62B H -0.5861 1.1613 1.1943 0.129 Uiso 1 1 calc R . . H62C H -0.6638 1.1036 1.2162 0.129 Uiso 1 1 calc R . . C63 C -0.6720(8) 1.1236(9) 1.1457(4) 0.078(4) Uani 1 1 d . . . H63A H -0.7248 1.1080 1.1461 0.093 Uiso 1 1 calc R . . H63B H -0.6465 1.1653 1.1241 0.093 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0372(3) 0.0291(3) 0.0342(3) 0.0000(3) 0.0087(2) 0.0182(2) Cd2 0.0489(3) 0.0514(4) 0.0270(4) -0.0042(3) 0.0017(2) 0.0340(3) Cd3 0.0344(3) 0.0371(3) 0.0315(3) 0.0071(3) 0.0020(2) 0.0188(2) K1 0.0514(12) 0.0450(11) 0.0560(13) 0.0063(9) -0.0063(10) 0.0216(9) K2 0.0827(19) 0.0644(16) 0.086(2) 0.0028(14) -0.0166(16) 0.0374(15) K3 0.0611(13) 0.0585(13) 0.0613(14) -0.0076(11) -0.0214(11) 0.0323(11) N1 0.046(4) 0.070(6) 0.060(5) 0.009(4) 0.008(4) 0.033(4) N2 0.087(6) 0.073(6) 0.097(7) -0.014(5) -0.042(5) 0.047(5) N3 0.099(7) 0.095(6) 0.080(6) -0.038(5) -0.032(5) 0.060(6) O1 0.069(5) 0.074(5) 0.056(5) 0.001(4) 0.023(4) 0.039(4) O2 0.029(3) 0.050(3) 0.035(3) 0.005(3) 0.014(2) 0.020(3) O3 0.030(3) 0.082(5) 0.064(4) -0.037(4) 0.005(3) 0.021(3) O4 0.030(3) 0.051(4) 0.047(4) -0.011(3) 0.009(3) 0.012(3) O5 0.070(4) 0.035(3) 0.036(3) 0.009(3) -0.009(3) 0.018(3) O6 0.049(4) 0.063(4) 0.023(3) -0.004(3) -0.010(3) 0.029(3) O7 0.045(4) 0.047(4) 0.049(4) 0.021(3) 0.010(3) 0.022(3) O8 0.062(4) 0.028(3) 0.040(3) -0.003(3) 0.015(3) 0.007(3) O9 0.034(3) 0.034(3) 0.060(4) 0.001(3) -0.001(3) 0.015(3) O10 0.064(4) 0.032(3) 0.062(4) 0.008(3) -0.016(4) 0.011(3) O11 0.051(5) 0.078(6) 0.092(7) 0.027(5) 0.011(5) 0.006(4) O12 0.042(4) 0.079(5) 0.077(5) -0.016(4) -0.002(4) 0.038(4) O13 0.048(4) 0.069(5) 0.121(8) -0.015(5) 0.007(5) 0.034(4) O14 0.047(4) 0.065(5) 0.048(4) 0.014(3) 0.001(3) 0.017(3) O15 0.048(3) 0.044(3) 0.034(3) -0.002(2) -0.004(3) 0.028(3) O16 0.067(5) 0.088(6) 0.057(4) -0.036(4) -0.030(4) 0.058(4) O17 0.036(3) 0.049(4) 0.062(4) 0.028(3) 0.005(3) 0.008(3) O18 0.068(5) 0.057(4) 0.037(3) 0.022(3) 0.004(3) 0.026(4) O19 0.045(4) 0.056(4) 0.054(4) 0.023(3) 0.000(3) 0.005(3) O20 0.035(3) 0.053(4) 0.046(4) 0.015(3) 0.004(3) 0.016(3) O21 0.067(5) 0.044(4) 0.069(5) 0.007(3) 0.021(4) 0.033(4) O22 0.055(4) 0.106(6) 0.052(4) 0.008(4) 0.009(3) 0.059(5) O23 0.068(5) 0.064(5) 0.042(4) -0.010(3) -0.016(4) 0.023(4) O24 0.064(4) 0.084(5) 0.040(4) -0.024(3) -0.012(3) 0.052(4) O25 0.126(8) 0.068(5) 0.083(6) -0.013(4) -0.051(6) 0.070(6) O26 0.075(5) 0.077(5) 0.052(4) -0.003(4) 0.004(4) 0.050(5) O27 0.093(7) 0.079(7) 0.080(6) -0.001(5) -0.035(6) 0.000(6) O28 0.058(5) 0.066(5) 0.072(5) 0.004(4) -0.004(4) 0.027(4) O29 0.092(5) 0.094(5) 0.078(5) 0.012(4) -0.023(4) 0.012(4) O30 0.083(6) 0.082(6) 0.059(5) -0.007(4) -0.005(4) 0.040(5) C1 0.034(4) 0.057(5) 0.045(5) -0.015(4) 0.007(4) 0.025(4) C2 0.027(4) 0.074(6) 0.037(5) -0.010(5) 0.005(4) 0.017(4) C3 0.050(5) 0.063(6) 0.038(5) -0.021(4) 0.007(4) 0.021(5) C4 0.061(7) 0.064(7) 0.042(5) -0.029(5) -0.001(5) 0.005(5) C5 0.029(4) 0.056(6) 0.065(7) -0.031(5) 0.007(4) 0.001(4) C6 0.038(5) 0.050(5) 0.051(6) -0.019(4) 0.008(4) 0.015(4) C7 0.036(4) 0.053(5) 0.037(4) -0.008(4) 0.012(4) 0.031(4) C8 0.026(4) 0.044(4) 0.052(5) -0.012(4) 0.008(3) 0.019(3) C9 0.031(4) 0.035(4) 0.032(4) -0.007(3) 0.001(3) 0.011(3) C10 0.034(4) 0.041(4) 0.028(4) 0.005(3) 0.001(3) 0.015(3) C11 0.043(4) 0.044(4) 0.038(5) 0.002(4) 0.000(3) 0.026(4) C12 0.040(5) 0.041(5) 0.047(5) -0.002(4) -0.016(4) 0.013(4) C13 0.039(4) 0.035(4) 0.040(5) 0.008(3) -0.001(4) 0.012(4) C14 0.039(4) 0.040(4) 0.031(4) 0.004(4) 0.006(3) 0.015(3) C15 0.035(4) 0.039(4) 0.036(4) 0.005(3) 0.000(3) 0.011(4) C16 0.036(4) 0.039(4) 0.055(5) 0.006(4) 0.027(4) 0.021(3) C17 0.039(5) 0.030(4) 0.063(6) -0.001(4) -0.014(4) 0.009(4) C18 0.042(5) 0.029(4) 0.063(6) 0.008(4) -0.007(4) 0.016(4) C19 0.048(5) 0.040(5) 0.072(7) 0.023(5) -0.002(5) 0.016(4) C20 0.051(6) 0.062(6) 0.086(9) 0.042(6) 0.000(6) 0.028(5) C21 0.048(6) 0.049(6) 0.079(8) 0.020(5) 0.011(5) 0.011(5) C22 0.054(6) 0.033(4) 0.075(7) -0.001(4) 0.001(5) 0.023(4) C23 0.055(5) 0.036(4) 0.039(5) -0.001(3) -0.003(4) 0.026(4) C24 0.041(5) 0.060(7) 0.100(10) -0.020(7) 0.007(6) 0.018(5) C25 0.042(5) 0.044(5) 0.048(5) -0.023(4) -0.025(4) 0.024(4) C26 0.036(4) 0.054(5) 0.057(6) -0.003(4) -0.009(4) 0.029(4) C27 0.059(6) 0.058(6) 0.064(6) -0.009(5) 0.002(5) 0.044(5) C28 0.052(6) 0.068(7) 0.061(7) -0.031(6) -0.013(5) 0.028(5) C29 0.039(4) 0.059(6) 0.055(6) -0.017(5) -0.024(4) 0.032(4) C30 0.051(5) 0.039(4) 0.045(5) -0.011(4) -0.011(4) 0.034(4) C31 0.058(6) 0.054(6) 0.078(8) 0.002(6) -0.011(6) 0.031(5) C32 0.054(5) 0.039(4) 0.049(5) -0.012(4) -0.015(4) 0.033(4) C33 0.038(5) 0.067(6) 0.055(6) 0.035(5) 0.001(4) 0.022(5) C34 0.030(4) 0.056(5) 0.054(6) 0.024(4) 0.003(4) 0.022(4) C35 0.032(4) 0.085(8) 0.060(6) 0.039(6) 0.000(4) 0.023(5) C36 0.047(6) 0.120(11) 0.064(7) 0.047(7) 0.008(5) 0.044(6) C37 0.058(6) 0.086(8) 0.053(6) 0.033(6) 0.010(5) 0.036(6) C38 0.031(4) 0.068(6) 0.050(5) 0.032(5) 0.008(4) 0.020(4) C39 0.040(5) 0.079(7) 0.058(6) 0.024(5) 0.007(4) 0.037(5) C40 0.028(4) 0.050(5) 0.042(5) 0.007(4) 0.002(3) 0.005(4) C41 0.041(5) 0.067(6) 0.031(4) -0.004(4) -0.001(4) 0.027(5) C42 0.036(4) 0.044(5) 0.040(5) -0.003(4) 0.008(4) 0.018(4) C43 0.045(5) 0.054(5) 0.048(6) -0.005(4) 0.011(4) 0.018(4) C44 0.044(5) 0.076(7) 0.044(5) -0.020(5) -0.020(4) 0.031(5) C45 0.039(5) 0.060(6) 0.062(6) -0.018(5) -0.010(4) 0.030(5) C46 0.042(5) 0.062(6) 0.036(5) -0.008(4) -0.008(4) 0.027(5) C47 0.050(5) 0.049(5) 0.046(5) 0.021(4) 0.024(4) 0.025(4) C48 0.036(4) 0.050(5) 0.047(5) -0.015(4) 0.002(4) 0.016(4) C49 0.088(9) 0.071(7) 0.055(7) 0.027(6) 0.033(6) 0.046(7) C50 0.068(7) 0.069(7) 0.044(5) 0.008(5) 0.016(5) 0.046(6) C51 0.079(7) 0.050(6) 0.038(5) -0.008(4) -0.004(5) 0.024(5) C52 0.101(10) 0.109(11) 0.043(6) 0.021(6) 0.023(6) 0.074(9) C53 0.070(7) 0.067(7) 0.052(6) -0.014(5) 0.002(5) 0.043(6) C54 0.088(11) 0.161(17) 0.081(10) -0.085(11) -0.037(8) 0.036(11) C55 0.044(5) 0.041(5) 0.077(8) -0.013(5) 0.009(5) 0.012(4) C56 0.074(8) 0.066(7) 0.046(6) -0.005(5) -0.009(5) 0.037(6) C57 0.074(9) 0.082(9) 0.069(8) 0.022(7) 0.006(7) 0.012(7) C58 0.090(9) 0.044(6) 0.064(7) 0.018(5) 0.000(6) 0.016(6) C59 0.093(11) 0.125(14) 0.054(8) -0.010(8) -0.013(7) 0.036(10) C60 0.072(8) 0.060(7) 0.081(9) -0.012(6) 0.022(7) 0.015(6) C61 0.075(6) 0.072(6) 0.074(6) 0.011(5) -0.005(5) 0.029(5) C62 0.076(9) 0.119(12) 0.067(8) 0.002(8) -0.007(7) 0.052(9) C63 0.085(9) 0.106(11) 0.049(7) 0.011(7) -0.001(6) 0.054(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O8 2.269(6) . ? Cd1 O9 2.286(6) . ? Cd1 O2 2.294(5) 6_444 ? Cd1 O3 2.305(6) . ? Cd1 O4 2.512(6) . ? Cd1 O10 2.533(7) . ? Cd1 O1 2.694(9) 6_444 ? Cd1 O7 2.729(7) . ? Cd1 K3 3.887(3) 2_665 ? Cd1 K1 3.917(2) . ? Cd2 O12 2.306(7) . ? Cd2 O5 2.329(6) 5_454 ? Cd2 O14 2.348(7) 5_354 ? Cd2 O24 2.369(7) . ? Cd2 O23 2.439(8) . ? Cd2 O6 2.462(7) 5_454 ? Cd2 O13 2.531(9) 5_354 ? Cd2 O11 2.698(10) . ? Cd2 C15 2.704(9) 5_454 ? Cd2 C48 2.722(9) . ? Cd2 K2 3.781(3) 6_454 ? Cd2 K2 3.895(3) . ? Cd3 O22 2.356(7) . ? Cd3 O20 2.360(6) 2_665 ? Cd3 O16 2.379(7) . ? Cd3 O18 2.395(7) . ? Cd3 O15 2.398(6) . ? Cd3 O17 2.409(7) . ? Cd3 O19 2.497(8) 2_665 ? Cd3 O21 2.519(8) . ? Cd3 C39 2.745(10) . ? Cd3 C32 2.758(9) . ? Cd3 K3 3.695(2) . ? Cd3 K1 3.743(2) 2_675 ? K1 O18 2.697(7) 6_344 ? K1 O9 2.712(7) . ? K1 O21 2.732(7) 6_344 ? K1 O25 2.774(10) . ? K1 O7 2.831(6) . ? K1 O26 2.978(8) . ? K1 O15 3.264(7) 6_344 ? K1 Cd3 3.743(2) 6_344 ? K2 O24 2.579(9) . ? K2 O23 2.631(8) 2_665 ? K2 O11 2.703(9) 2_665 ? K2 O27 2.815(11) . ? K2 O28 2.907(9) . ? K2 O13 3.058(10) 5_354 ? K2 Cd2 3.781(3) 2_665 ? K3 O3 2.613(9) 6_454 ? K3 O16 2.748(7) . ? K3 O19 2.759(7) 2_665 ? K3 O1 2.803(7) 5_354 ? K3 O29 2.815(11) . ? K3 O30 2.998(10) . ? K3 O17 3.071(7) . ? K3 Cd1 3.887(3) 6_454 ? N1 C50 1.508(14) . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N2 C55 1.523(14) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 C60 1.450(18) . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? N3 H3D 0.8900 . ? O1 C7 1.263(11) . ? O1 K3 2.803(7) 3_575 ? O2 C7 1.275(10) . ? O2 Cd1 2.294(5) 2_565 ? O3 C8 1.291(10) . ? O3 K3 2.613(9) 2_665 ? O4 C8 1.253(11) . ? O5 C15 1.249(11) . ? O5 Cd2 2.329(6) 3_565 ? O6 C15 1.263(10) . ? O6 Cd2 2.462(7) 3_565 ? O7 C16 1.276(12) . ? O8 C16 1.231(12) . ? O9 C23 1.283(11) . ? O10 C23 1.260(11) . ? O11 C24 1.243(16) . ? O11 K2 2.703(9) 6_454 ? O12 C24 1.210(15) . ? O13 C31 1.240(15) . ? O13 Cd2 2.531(9) 3_575 ? O13 K2 3.058(10) 3_575 ? O14 C31 1.288(14) . ? O14 Cd2 2.348(7) 3_575 ? O15 C32 1.267(10) . ? O15 K1 3.264(7) 2_675 ? O16 C32 1.259(11) . ? O17 C39 1.302(13) . ? O18 C39 1.269(12) . ? O18 K1 2.697(7) 2_675 ? O19 C40 1.260(11) . ? O19 Cd3 2.497(8) 6_454 ? O19 K3 2.759(7) 6_454 ? O20 C40 1.257(11) . ? O20 Cd3 2.360(6) 6_454 ? O21 C47 1.275(12) . ? O21 K1 2.732(7) 2_675 ? O22 C47 1.253(13) . ? O23 C48 1.207(12) . ? O23 K2 2.631(8) 6_454 ? O24 C48 1.226(12) . ? O25 C51 1.376(12) . ? O25 H25B 0.9300 . ? O26 C53 1.406(14) . ? O26 H26A 0.9300 . ? O27 C56 1.378(15) . ? O27 H27B 0.9300 . ? O28 C58 1.522(16) . ? O28 H28B 0.9300 . ? O29 C61 1.427(16) . ? O29 H29B 0.9300 . ? O30 C63 1.450(17) . ? O30 H30A 0.9300 . ? C1 C6 1.366(12) . ? C1 C2 1.412(12) . ? C1 H1A 0.9300 . ? C2 C3 1.405(13) . ? C2 C7 1.477(11) . ? C3 C4 1.390(15) . ? C3 H3A 0.9300 . ? C4 C5 1.400(14) . ? C4 H4A 0.9300 . ? C5 C6 1.445(13) . ? C5 H5A 0.9300 . ? C6 C8 1.514(12) . ? C9 C10 1.381(12) . ? C9 C14 1.409(12) . ? C9 H9A 0.9300 . ? C10 C11 1.393(12) . ? C10 C15 1.529(11) . ? C11 C12 1.357(12) . ? C11 H11A 0.9300 . ? C12 C13 1.400(12) . ? C12 H12A 0.9300 . ? C13 C14 1.411(12) . ? C13 H13A 0.9300 . ? C14 C16 1.513(11) . ? C15 Cd2 2.704(9) 3_565 ? C17 C22 1.365(15) . ? C17 C18 1.391(13) . ? C17 H17A 0.9300 . ? C18 C19 1.381(13) . ? C18 C23 1.488(13) . ? C19 C20 1.393(14) . ? C19 H19A 0.9300 . ? C20 C21 1.415(14) . ? C20 H20A 0.9300 . ? C21 C22 1.392(16) . ? C21 H21A 0.9300 . ? C22 C24 1.565(15) . ? C25 C30 1.380(13) . ? C25 C26 1.396(13) . ? C25 H25A 0.9300 . ? C26 C27 1.381(14) . ? C26 C31 1.488(14) . ? C27 C28 1.403(15) . ? C27 H27A 0.9300 . ? C28 C29 1.396(14) . ? C28 H28A 0.9300 . ? C29 C30 1.386(12) . ? C29 H29A 0.9300 . ? C30 C32 1.489(12) . ? C33 C38 1.361(12) . ? C33 C34 1.413(12) . ? C33 H33A 0.9300 . ? C34 C35 1.362(12) . ? C34 C39 1.478(13) . ? C35 C36 1.402(14) . ? C35 H35A 0.9300 . ? C36 C37 1.404(15) . ? C36 H36A 0.9300 . ? C37 C38 1.362(13) . ? C37 H37A 0.9300 . ? C38 C40 1.521(12) . ? C41 C46 1.340(14) . ? C41 C42 1.440(13) . ? C41 H41A 0.84(2) . ? C42 C43 1.385(14) . ? C42 C47 1.500(13) . ? C43 C44 1.359(14) . ? C43 H43A 0.9300 . ? C44 C45 1.393(13) . ? C44 H44A 0.9300 . ? C45 C46 1.430(13) . ? C45 H45A 0.9300 . ? C46 C48 1.525(13) . ? C49 C50 1.515(14) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C51 1.500(15) . ? C50 H50A 0.9800 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.495(15) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.528(17) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 C56 1.480(15) . ? C55 H55A 0.9800 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.478(16) . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.521(18) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.499(19) . ? C60 H60A 0.9800 . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.533(16) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 Cd1 O9 138.3(2) . . ? O8 Cd1 O2 82.3(2) . 6_444 ? O9 Cd1 O2 95.7(2) . 6_444 ? O8 Cd1 O3 96.2(3) . . ? O9 Cd1 O3 111.5(3) . . ? O2 Cd1 O3 137.8(2) 6_444 . ? O8 Cd1 O4 81.7(2) . . ? O9 Cd1 O4 89.5(2) . . ? O2 Cd1 O4 161.1(2) 6_444 . ? O3 Cd1 O4 54.5(2) . . ? O8 Cd1 O10 159.4(3) . . ? O9 Cd1 O10 54.1(2) . . ? O2 Cd1 O10 79.6(2) 6_444 . ? O3 Cd1 O10 90.7(3) . . ? O4 Cd1 O10 117.8(2) . . ? O8 Cd1 O1 75.5(3) . 6_444 ? O9 Cd1 O1 134.4(2) . 6_444 ? O2 Cd1 O1 52.1(2) 6_444 6_444 ? O3 Cd1 O1 86.4(2) . 6_444 ? O4 Cd1 O1 131.9(2) . 6_444 ? O10 Cd1 O1 85.6(2) . 6_444 ? O8 Cd1 O7 51.1(2) . . ? O9 Cd1 O7 87.9(2) . . ? O2 Cd1 O7 75.2(2) 6_444 . ? O3 Cd1 O7 134.8(2) . . ? O4 Cd1 O7 86.9(2) . . ? O10 Cd1 O7 131.5(2) . . ? O1 Cd1 O7 109.0(2) 6_444 . ? O8 Cd1 K3 80.84(18) . 2_665 ? O9 Cd1 K3 140.06(16) . 2_665 ? O2 Cd1 K3 98.24(16) 6_444 2_665 ? O3 Cd1 K3 40.7(2) . 2_665 ? O4 Cd1 K3 89.10(16) . 2_665 ? O10 Cd1 K3 92.10(17) . 2_665 ? O1 Cd1 K3 46.15(15) 6_444 2_665 ? O7 Cd1 K3 131.81(14) . 2_665 ? O8 Cd1 K1 97.34(18) . . ? O9 Cd1 K1 42.43(16) . . ? O2 Cd1 K1 78.02(16) 6_444 . ? O3 Cd1 K1 143.3(2) . . ? O4 Cd1 K1 94.11(16) . . ? O10 Cd1 K1 88.44(17) . . ? O1 Cd1 K1 130.05(16) 6_444 . ? O7 Cd1 K1 46.28(13) . . ? K3 Cd1 K1 176.06(5) 2_665 . ? O12 Cd2 O5 136.0(3) . 5_454 ? O12 Cd2 O14 84.8(3) . 5_354 ? O5 Cd2 O14 87.9(3) 5_454 5_354 ? O12 Cd2 O24 92.4(3) . . ? O5 Cd2 O24 117.4(3) 5_454 . ? O14 Cd2 O24 143.4(3) 5_354 . ? O12 Cd2 O23 84.9(3) . . ? O5 Cd2 O23 88.6(3) 5_454 . ? O14 Cd2 O23 161.2(3) 5_354 . ? O24 Cd2 O23 52.8(2) . . ? O12 Cd2 O6 166.0(3) . 5_454 ? O5 Cd2 O6 55.3(2) 5_454 5_454 ? O14 Cd2 O6 87.8(2) 5_354 5_454 ? O24 Cd2 O6 86.5(2) . 5_454 ? O23 Cd2 O6 105.2(3) . 5_454 ? O12 Cd2 O13 80.0(3) . 5_354 ? O5 Cd2 O13 128.2(3) 5_454 5_354 ? O14 Cd2 O13 54.3(3) 5_354 5_354 ? O24 Cd2 O13 89.3(3) . 5_354 ? O23 Cd2 O13 138.5(3) . 5_354 ? O6 Cd2 O13 86.1(3) 5_454 5_354 ? O12 Cd2 O11 50.2(3) . . ? O5 Cd2 O11 85.8(3) 5_454 . ? O14 Cd2 O11 80.9(3) 5_354 . ? O24 Cd2 O11 124.1(3) . . ? O23 Cd2 O11 80.4(3) . . ? O6 Cd2 O11 139.9(2) 5_454 . ? O13 Cd2 O11 116.3(3) 5_354 . ? O12 Cd2 C15 162.2(3) . 5_454 ? O5 Cd2 C15 27.5(2) 5_454 5_454 ? O14 Cd2 C15 87.4(3) 5_354 5_454 ? O24 Cd2 C15 103.3(3) . 5_454 ? O23 Cd2 C15 97.9(3) . 5_454 ? O6 Cd2 C15 27.8(2) 5_454 5_454 ? O13 Cd2 C15 108.1(3) 5_354 5_454 ? O11 Cd2 C15 112.7(3) . 5_454 ? O12 Cd2 C48 85.7(3) . . ? O5 Cd2 C48 106.3(3) 5_454 . ? O14 Cd2 C48 165.7(3) 5_354 . ? O24 Cd2 C48 26.7(3) . . ? O23 Cd2 C48 26.3(3) . . ? O6 Cd2 C48 99.1(2) 5_454 . ? O13 Cd2 C48 113.5(3) 5_354 . ? O11 Cd2 C48 101.0(3) . . ? C15 Cd2 C48 104.6(3) 5_454 . ? O12 Cd2 K2 81.0(2) . 6_454 ? O5 Cd2 K2 65.03(16) 5_454 6_454 ? O14 Cd2 K2 118.8(2) 5_354 6_454 ? O24 Cd2 K2 96.53(19) . 6_454 ? O23 Cd2 K2 43.74(18) . 6_454 ? O6 Cd2 K2 112.97(15) 5_454 6_454 ? O13 Cd2 K2 160.3(2) 5_354 6_454 ? O11 Cd2 K2 45.6(2) . 6_454 ? C15 Cd2 K2 88.93(18) 5_454 6_454 ? C48 Cd2 K2 69.9(2) . 6_454 ? O12 Cd2 K2 74.2(2) . . ? O5 Cd2 K2 148.90(19) 5_454 . ? O14 Cd2 K2 105.19(19) 5_354 . ? O24 Cd2 K2 40.0(2) . . ? O23 Cd2 K2 87.04(18) . . ? O6 Cd2 K2 96.42(15) 5_454 . ? O13 Cd2 K2 51.7(2) 5_354 . ? O11 Cd2 K2 123.7(2) . . ? C15 Cd2 K2 123.4(2) 5_454 . ? C48 Cd2 K2 61.9(2) . . ? K2 Cd2 K2 126.63(9) 6_454 . ? O22 Cd3 O20 86.9(3) . 2_665 ? O22 Cd3 O16 164.6(3) . . ? O20 Cd3 O16 92.9(3) 2_665 . ? O22 Cd3 O18 91.7(3) . . ? O20 Cd3 O18 164.3(2) 2_665 . ? O16 Cd3 O18 92.5(3) . . ? O22 Cd3 O15 140.9(2) . . ? O20 Cd3 O15 86.3(2) 2_665 . ? O16 Cd3 O15 54.3(2) . . ? O18 Cd3 O15 85.0(2) . . ? O22 Cd3 O17 85.6(3) . . ? O20 Cd3 O17 139.5(2) 2_665 . ? O16 Cd3 O17 84.5(3) . . ? O18 Cd3 O17 55.8(2) . . ? O15 Cd3 O17 122.5(2) . . ? O22 Cd3 O19 85.7(3) . 2_665 ? O20 Cd3 O19 53.7(2) 2_665 2_665 ? O16 Cd3 O19 81.8(3) . 2_665 ? O18 Cd3 O19 141.8(2) . 2_665 ? O15 Cd3 O19 119.7(2) . 2_665 ? O17 Cd3 O19 86.0(2) . 2_665 ? O22 Cd3 O21 54.0(2) . . ? O20 Cd3 O21 86.0(2) 2_665 . ? O16 Cd3 O21 141.3(2) . . ? O18 Cd3 O21 80.6(2) . . ? O15 Cd3 O21 87.1(2) . . ? O17 Cd3 O21 120.0(2) . . ? O19 Cd3 O21 125.8(2) 2_665 . ? O22 Cd3 C39 87.2(3) . . ? O20 Cd3 C39 167.1(3) 2_665 . ? O16 Cd3 C39 89.8(3) . . ? O18 Cd3 C39 27.5(3) . . ? O15 Cd3 C39 105.5(3) . . ? O17 Cd3 C39 28.3(3) . . ? O19 Cd3 C39 114.3(3) 2_665 . ? O21 Cd3 C39 99.7(3) . . ? O22 Cd3 C32 167.4(3) . . ? O20 Cd3 C32 87.3(3) 2_665 . ? O16 Cd3 C32 27.1(2) . . ? O18 Cd3 C32 90.9(3) . . ? O15 Cd3 C32 27.3(2) . . ? O17 Cd3 C32 105.9(3) . . ? O19 Cd3 C32 99.7(3) 2_665 . ? O21 Cd3 C32 114.4(3) . . ? C39 Cd3 C32 100.6(3) . . ? O22 Cd3 K3 116.62(19) . . ? O20 Cd3 K3 93.40(17) 2_665 . ? O16 Cd3 K3 48.03(16) . . ? O18 Cd3 K3 101.19(18) . . ? O15 Cd3 K3 102.17(15) . . ? O17 Cd3 K3 55.73(16) . . ? O19 Cd3 K3 48.29(17) 2_665 . ? O21 Cd3 K3 170.61(18) . . ? C39 Cd3 K3 79.1(2) . . ? C32 Cd3 K3 74.85(19) . . ? O22 Cd3 K1 90.9(2) . 2_675 ? O20 Cd3 K1 118.43(16) 2_665 2_675 ? O16 Cd3 K1 102.65(19) . 2_675 ? O18 Cd3 K1 45.93(17) . 2_675 ? O15 Cd3 K1 59.52(16) . 2_675 ? O17 Cd3 K1 101.43(16) . 2_675 ? O19 Cd3 K1 171.55(16) 2_665 2_675 ? O21 Cd3 K1 46.86(16) . 2_675 ? C39 Cd3 K1 73.1(2) . 2_675 ? C32 Cd3 K1 82.1(2) . 2_675 ? K3 Cd3 K1 139.65(5) . 2_675 ? O18 K1 O9 102.7(2) 6_344 . ? O18 K1 O21 71.7(2) 6_344 6_344 ? O9 K1 O21 135.8(2) . 6_344 ? O18 K1 O25 82.4(2) 6_344 . ? O9 K1 O25 139.8(3) . . ? O21 K1 O25 84.0(3) 6_344 . ? O18 K1 O7 158.1(2) 6_344 . ? O9 K1 O7 78.2(2) . . ? O21 K1 O7 92.2(2) 6_344 . ? O25 K1 O7 111.3(2) . . ? O18 K1 O26 118.0(2) 6_344 . ? O9 K1 O26 75.7(2) . . ? O21 K1 O26 146.8(2) 6_344 . ? O25 K1 O26 67.2(2) . . ? O7 K1 O26 83.6(2) . . ? O18 K1 O15 64.99(18) 6_344 6_344 ? O9 K1 O15 69.95(17) . 6_344 ? O21 K1 O15 68.21(19) 6_344 6_344 ? O25 K1 O15 142.0(2) . 6_344 ? O7 K1 O15 95.64(18) . 6_344 ? O26 K1 O15 145.0(2) . 6_344 ? O18 K1 Cd3 39.65(14) 6_344 6_344 ? O9 K1 Cd3 105.86(14) . 6_344 ? O21 K1 Cd3 42.30(17) 6_344 6_344 ? O25 K1 Cd3 102.87(17) . 6_344 ? O7 K1 Cd3 118.69(15) . 6_344 ? O26 K1 Cd3 157.66(17) . 6_344 ? O15 K1 Cd3 39.28(11) 6_344 6_344 ? O18 K1 Cd1 136.22(19) 6_344 . ? O9 K1 Cd1 34.67(14) . . ? O21 K1 Cd1 126.35(18) 6_344 . ? O25 K1 Cd1 133.63(17) . . ? O7 K1 Cd1 44.15(15) . . ? O26 K1 Cd1 70.77(15) . . ? O15 K1 Cd1 84.35(11) 6_344 . ? Cd3 K1 Cd1 123.28(7) 6_344 . ? O24 K2 O23 100.7(3) . 2_665 ? O24 K2 O11 127.1(3) . 2_665 ? O23 K2 O11 77.1(3) 2_665 2_665 ? O24 K2 O27 145.9(3) . . ? O23 K2 O27 79.5(3) 2_665 . ? O11 K2 O27 86.5(4) 2_665 . ? O24 K2 O28 79.4(2) . . ? O23 K2 O28 113.4(3) 2_665 . ? O11 K2 O28 150.7(3) 2_665 . ? O27 K2 O28 69.7(3) . . ? O24 K2 O13 74.8(2) . 5_354 ? O23 K2 O13 156.1(3) 2_665 5_354 ? O11 K2 O13 86.9(3) 2_665 5_354 ? O27 K2 O13 117.5(3) . 5_354 ? O28 K2 O13 89.1(2) . 5_354 ? O24 K2 Cd2 100.58(18) . 2_665 ? O23 K2 Cd2 39.87(17) 2_665 2_665 ? O11 K2 Cd2 45.5(2) 2_665 2_665 ? O27 K2 Cd2 100.7(2) . 2_665 ? O28 K2 Cd2 153.2(2) . 2_665 ? O13 K2 Cd2 116.96(19) 5_354 2_665 ? O24 K2 Cd2 36.20(16) . . ? O23 K2 Cd2 136.4(2) 2_665 . ? O11 K2 Cd2 118.9(2) 2_665 . ? O27 K2 Cd2 137.2(2) . . ? O28 K2 Cd2 73.45(18) . . ? O13 K2 Cd2 40.50(17) 5_354 . ? Cd2 K2 Cd2 121.84(9) 2_665 . ? O3 K3 O16 105.5(3) 6_454 . ? O3 K3 O19 140.0(3) 6_454 2_665 ? O16 K3 O19 70.9(2) . 2_665 ? O3 K3 O1 78.6(2) 6_454 5_354 ? O16 K3 O1 160.3(2) . 5_354 ? O19 K3 O1 93.4(2) 2_665 5_354 ? O3 K3 O29 133.9(3) 6_454 . ? O16 K3 O29 79.2(3) . . ? O19 K3 O29 85.5(3) 2_665 . ? O1 K3 O29 112.2(3) 5_354 . ? O3 K3 O30 73.6(2) 6_454 . ? O16 K3 O30 119.4(2) . . ? O19 K3 O30 144.3(3) 2_665 . ? O1 K3 O30 80.3(2) 5_354 . ? O29 K3 O30 65.2(3) . . ? O3 K3 O17 72.3(2) 6_454 . ? O16 K3 O17 66.9(2) . . ? O19 K3 O17 69.9(2) 2_665 . ? O1 K3 O17 97.0(2) 5_354 . ? O29 K3 O17 142.9(3) . . ? O30 K3 O17 145.6(2) . . ? O3 K3 Cd3 109.05(19) 6_454 . ? O16 K3 Cd3 40.05(15) . . ? O19 K3 Cd3 42.52(17) 2_665 . ? O1 K3 Cd3 120.29(19) 5_354 . ? O29 K3 Cd3 103.1(2) . . ? O30 K3 Cd3 159.42(18) . . ? O17 K3 Cd3 40.42(13) . . ? O3 K3 Cd1 35.08(15) 6_454 6_454 ? O16 K3 Cd1 139.3(2) . 6_454 ? O19 K3 Cd1 128.03(18) 2_665 6_454 ? O1 K3 Cd1 43.87(18) 5_354 6_454 ? O29 K3 Cd1 131.5(2) . 6_454 ? O30 K3 Cd1 68.81(17) . 6_454 ? O17 K3 Cd1 85.40(14) . 6_454 ? Cd3 K3 Cd1 125.39(8) . 6_454 ? C50 N1 H1B 109.5 . . ? C50 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C50 N1 H1D 109.5 . . ? H1B N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? C55 N2 H2A 109.5 . . ? C55 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C55 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C60 N3 H3B 109.5 . . ? C60 N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C60 N3 H3D 109.5 . . ? H3B N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C7 O1 K3 173.3(7) . 3_575 ? C7 O2 Cd1 101.8(5) . 2_565 ? C8 O3 Cd1 96.5(5) . . ? C8 O3 K3 135.8(7) . 2_665 ? Cd1 O3 K3 104.3(3) . 2_665 ? C8 O4 Cd1 88.0(5) . . ? C15 O5 Cd2 93.2(5) . 3_565 ? C15 O6 Cd2 86.8(5) . 3_565 ? C16 O7 Cd1 81.6(5) . . ? C16 O7 K1 169.6(6) . . ? Cd1 O7 K1 89.57(19) . . ? C16 O8 Cd1 104.5(6) . . ? C23 O9 Cd1 98.1(5) . . ? C23 O9 K1 130.0(6) . . ? Cd1 O9 K1 102.9(2) . . ? C23 O10 Cd1 87.3(6) . . ? C24 O11 Cd2 83.1(8) . . ? C24 O11 K2 127.2(9) . 6_454 ? Cd2 O11 K2 88.9(3) . 6_454 ? C24 O12 Cd2 102.9(8) . . ? C31 O13 Cd2 87.3(7) . 3_575 ? C31 O13 K2 166.4(8) . 3_575 ? Cd2 O13 K2 87.8(3) 3_575 3_575 ? C31 O14 Cd2 94.5(7) . 3_575 ? C32 O15 Cd3 92.3(5) . . ? C32 O15 K1 142.1(6) . 2_675 ? Cd3 O15 K1 81.20(17) . 2_675 ? C32 O16 Cd3 93.4(5) . . ? C32 O16 K3 168.8(8) . . ? Cd3 O16 K3 91.9(2) . . ? C39 O17 Cd3 90.3(6) . . ? C39 O17 K3 141.0(7) . . ? Cd3 O17 K3 83.85(18) . . ? C39 O18 Cd3 91.8(6) . . ? C39 O18 K1 168.4(7) . 2_675 ? Cd3 O18 K1 94.4(2) . 2_675 ? C40 O19 Cd3 88.8(6) . 6_454 ? C40 O19 K3 142.5(7) . 6_454 ? Cd3 O19 K3 89.2(2) 6_454 6_454 ? C40 O20 Cd3 95.3(5) . 6_454 ? C47 O21 Cd3 87.5(6) . . ? C47 O21 K1 138.2(6) . 2_675 ? Cd3 O21 K1 90.8(2) . 2_675 ? C47 O22 Cd3 95.5(6) . . ? C48 O23 Cd2 90.0(6) . . ? C48 O23 K2 170.4(7) . 6_454 ? Cd2 O23 K2 96.4(2) . 6_454 ? C48 O24 Cd2 92.9(6) . . ? C48 O24 K2 134.4(6) . . ? Cd2 O24 K2 103.8(3) . . ? C51 O25 K1 139.9(8) . . ? C51 O25 H25B 110.1 . . ? K1 O25 H25B 110.1 . . ? C53 O26 K1 133.2(6) . . ? C53 O26 H26A 113.4 . . ? K1 O26 H26A 113.4 . . ? C56 O27 K2 133.5(8) . . ? C56 O27 H27B 113.2 . . ? K2 O27 H27B 113.2 . . ? C58 O28 K2 138.9(7) . . ? C58 O28 H28B 110.5 . . ? K2 O28 H28B 110.5 . . ? C61 O29 K3 132.7(10) . . ? C61 O29 H29B 113.7 . . ? K3 O29 H29B 113.7 . . ? C63 O30 K3 126.9(8) . . ? C63 O30 H30A 116.6 . . ? K3 O30 H30A 116.6 . . ? C6 C1 C2 122.0(9) . . ? C6 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 117.9(8) . . ? C3 C2 C7 121.5(8) . . ? C1 C2 C7 120.6(8) . . ? C4 C3 C2 120.6(8) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 121.9(9) . . ? C3 C4 H4A 119.0 . . ? C5 C4 H4A 119.0 . . ? C4 C5 C6 117.0(9) . . ? C4 C5 H5A 121.5 . . ? C6 C5 H5A 121.5 . . ? C1 C6 C5 120.4(8) . . ? C1 C6 C8 119.6(8) . . ? C5 C6 C8 119.5(8) . . ? O1 C7 O2 122.1(8) . . ? O1 C7 C2 120.0(9) . . ? O2 C7 C2 117.6(7) . . ? O4 C8 O3 120.8(7) . . ? O4 C8 C6 121.2(7) . . ? O3 C8 C6 117.9(8) . . ? C10 C9 C14 120.2(8) . . ? C10 C9 H9A 119.9 . . ? C14 C9 H9A 119.9 . . ? C9 C10 C11 120.5(8) . . ? C9 C10 C15 119.2(7) . . ? C11 C10 C15 120.1(8) . . ? C12 C11 C10 120.2(8) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.7(8) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C12 C13 C14 119.9(8) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C9 C14 C13 118.3(7) . . ? C9 C14 C16 120.2(8) . . ? C13 C14 C16 121.5(8) . . ? O5 C15 O6 124.7(8) . . ? O5 C15 C10 118.7(8) . . ? O6 C15 C10 116.5(8) . . ? O5 C15 Cd2 59.3(4) . 3_565 ? O6 C15 Cd2 65.4(5) . 3_565 ? C10 C15 Cd2 176.3(6) . 3_565 ? O8 C16 O7 122.0(8) . . ? O8 C16 C14 118.9(9) . . ? O7 C16 C14 119.0(9) . . ? C22 C17 C18 118.4(9) . . ? C22 C17 H17A 120.8 . . ? C18 C17 H17A 120.8 . . ? C19 C18 C17 121.9(9) . . ? C19 C18 C23 120.6(9) . . ? C17 C18 C23 117.5(8) . . ? C18 C19 C20 118.9(10) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C19 C20 C21 119.8(10) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C22 C21 C20 118.5(10) . . ? C22 C21 H21A 120.8 . . ? C20 C21 H21A 120.8 . . ? C17 C22 C21 121.8(10) . . ? C17 C22 C24 120.3(10) . . ? C21 C22 C24 117.9(10) . . ? O10 C23 O9 120.0(8) . . ? O10 C23 C18 120.1(9) . . ? O9 C23 C18 119.9(8) . . ? O12 C24 O11 122.7(11) . . ? O12 C24 C22 117.4(12) . . ? O11 C24 C22 119.6(12) . . ? C30 C25 C26 122.6(8) . . ? C30 C25 H25A 118.7 . . ? C26 C25 H25A 118.7 . . ? C27 C26 C25 118.4(8) . . ? C27 C26 C31 119.5(10) . . ? C25 C26 C31 122.0(9) . . ? C26 C27 C28 120.2(10) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C29 C28 C27 119.4(9) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C30 C29 C28 120.6(9) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C25 C30 C29 118.2(8) . . ? C25 C30 C32 119.8(8) . . ? C29 C30 C32 121.8(8) . . ? O13 C31 O14 123.9(11) . . ? O13 C31 C26 121.1(11) . . ? O14 C31 C26 114.9(11) . . ? O16 C32 O15 119.2(8) . . ? O16 C32 C30 119.8(8) . . ? O15 C32 C30 121.0(8) . . ? O16 C32 Cd3 59.4(5) . . ? O15 C32 Cd3 60.3(4) . . ? C30 C32 Cd3 171.2(7) . . ? C38 C33 C34 121.7(9) . . ? C38 C33 H33A 119.2 . . ? C34 C33 H33A 119.2 . . ? C35 C34 C33 118.6(8) . . ? C35 C34 C39 122.9(8) . . ? C33 C34 C39 118.4(8) . . ? C34 C35 C36 120.2(9) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C37 119.0(9) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C38 C37 C36 120.7(9) . . ? C38 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? C33 C38 C37 119.3(9) . . ? C33 C38 C40 120.2(8) . . ? C37 C38 C40 120.3(8) . . ? O18 C39 O17 121.8(9) . . ? O18 C39 C34 118.0(9) . . ? O17 C39 C34 119.8(9) . . ? O18 C39 Cd3 60.7(5) . . ? O17 C39 Cd3 61.4(5) . . ? C34 C39 Cd3 169.4(7) . . ? O20 C40 O19 121.7(8) . . ? O20 C40 C38 118.0(8) . . ? O19 C40 C38 120.3(9) . . ? C46 C41 C42 120.5(9) . . ? C46 C41 H41A 122(8) . . ? C42 C41 H41A 117(8) . . ? C43 C42 C41 117.7(8) . . ? C43 C42 C47 125.0(9) . . ? C41 C42 C47 117.2(9) . . ? C44 C43 C42 121.0(9) . . ? C44 C43 H43A 119.5 . . ? C42 C43 H43A 119.5 . . ? C43 C44 C45 122.5(9) . . ? C43 C44 H44A 118.7 . . ? C45 C44 H44A 118.7 . . ? C44 C45 C46 116.5(9) . . ? C44 C45 H45A 121.8 . . ? C46 C45 H45A 121.8 . . ? C41 C46 C45 121.7(9) . . ? C41 C46 C48 118.0(8) . . ? C45 C46 C48 119.8(9) . . ? O22 C47 O21 122.7(9) . . ? O22 C47 C42 120.3(9) . . ? O21 C47 C42 116.5(9) . . ? O23 C48 O24 123.0(9) . . ? O23 C48 C46 119.1(9) . . ? O24 C48 C46 117.9(9) . . ? O23 C48 Cd2 63.7(5) . . ? O24 C48 Cd2 60.4(5) . . ? C46 C48 Cd2 168.9(7) . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C51 C50 N1 108.8(9) . . ? C51 C50 C49 116.2(9) . . ? N1 C50 C49 108.4(10) . . ? C51 C50 H50A 107.7 . . ? N1 C50 H50A 107.7 . . ? C49 C50 H50A 107.7 . . ? O25 C51 C50 110.6(9) . . ? O25 C51 H51A 109.5 . . ? C50 C51 H51A 109.5 . . ? O25 C51 H51B 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O26 C53 C52 110.1(11) . . ? O26 C53 H53A 109.6 . . ? C52 C53 H53A 109.6 . . ? O26 C53 H53B 109.6 . . ? C52 C53 H53B 109.6 . . ? H53A C53 H53B 108.2 . . ? 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 N2 112.5(9) . . ? C56 C55 C54 113.9(10) . . ? N2 C55 C54 106.3(12) . . ? C56 C55 H55A 108.0 . . ? N2 C55 H55A 108.0 . . ? C54 C55 H55A 108.0 . . ? O27 C56 C55 111.7(10) . . ? O27 C56 H56A 109.3 . . ? C55 C56 H56A 109.3 . . ? O27 C56 H56B 109.3 . . ? C55 C56 H56B 109.3 . . ? H56A C56 H56B 107.9 . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C57 C58 O28 103.2(12) . . ? C57 C58 H58A 111.1 . . ? O28 C58 H58A 111.1 . . ? C57 C58 H58B 111.1 . . ? O28 C58 H58B 111.1 . . ? H58A C58 H58B 109.1 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N3 C60 C61 120.4(11) . . ? N3 C60 C59 110.9(13) . . ? C61 C60 C59 109.9(12) . . ? N3 C60 H60A 104.7 . . ? C61 C60 H60A 104.7 . . ? C59 C60 H60A 104.7 . . ? O29 C61 C60 106.3(11) . . ? O29 C61 H61A 110.5 . . ? C60 C61 H61A 110.5 . . ? O29 C61 H61B 110.5 . . ? C60 C61 H61B 110.5 . . ? H61A C61 H61B 108.7 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O30 C63 C62 105.7(11) . . ? O30 C63 H63A 110.6 . . ? C62 C63 H63A 110.6 . . ? O30 C63 H63B 110.6 . . ? C62 C63 H63B 110.6 . . ? H63A C63 H63B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.286 _refine_diff_density_min -1.298 _refine_diff_density_rms 0.128