# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jinkui Tang' _publ_contact_author_email tang@ciac.jl.cn loop_ _publ_author_name 'Shuang-Yan Lin' 'Gong-Feng Xu' 'Lang Zhao' 'Yun-Nan Guo' 'Yang Guo' ; Jinkui Tang ; data_1 _database_code_depnum_ccdc_archive 'CCDC 772951' #TrackingRef 'web_deposit_cif_file_0_JinkuiTang_1303180583.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H81 Cl3 Dy2 N12 O27' _chemical_formula_weight 2013.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.5685(18) _cell_length_b 16.6655(13) _cell_length_c 19.9516(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.2240(10) _cell_angle_gamma 90.00 _cell_volume 8167.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.32 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 2.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7534 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44380 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.37 _reflns_number_total 16489 _reflns_number_gt 12287 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+4.8395P] 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 16489 _refine_ls_number_parameters 1081 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Dy1 Dy 0.190534(7) -0.028757(12) 0.162730(9) 0.01901(6) Uani 1 1 d . . . Dy2 Dy 0.326049(7) 0.033558(12) 0.157548(9) 0.01817(6) Uani 1 1 d . . . Cl1 Cl 0.11918(6) 0.85151(9) 0.45919(7) 0.0454(3) Uani 1 1 d . . . Cl2 Cl 0.40911(5) 0.24103(8) 0.91544(6) 0.0409(3) Uani 1 1 d . . . Cl3 Cl 0.25388(5) 0.09950(10) 0.47779(6) 0.0470(3) Uani 1 1 d . . . N1 N 0.30442(13) 0.1312(2) 0.06114(17) 0.0225(8) Uani 1 1 d . . . N2 N 0.31676(14) 0.2096(2) 0.07659(17) 0.0235(8) Uani 1 1 d . . . H2 H 0.3053 0.2495 0.0511 0.028 Uiso 1 1 calc R . . N3 N 0.20882(14) -0.1558(2) 0.09243(17) 0.0216(8) Uani 1 1 d . . . N4 N 0.19137(14) -0.2255(2) 0.12262(18) 0.0252(8) Uani 1 1 d . . . H4 H 0.1974 -0.2731 0.1052 0.030 Uiso 1 1 calc R . . N5 N 0.36335(13) -0.1103(2) 0.13751(17) 0.0211(8) Uani 1 1 d . . . N6 N 0.39451(14) -0.1176(2) 0.08123(17) 0.0265(9) Uani 1 1 d . . . H6 H 0.4079 -0.1641 0.0686 0.032 Uiso 1 1 calc R . . N7 N 0.19538(14) -0.0310(2) 0.29367(17) 0.0233(8) Uani 1 1 d . . . N8 N 0.15532(14) 0.0156(2) 0.32214(18) 0.0269(9) Uani 1 1 d . . . H8A H 0.1549 0.0238 0.3657 0.032 Uiso 1 1 calc R . . N9 N 0.31905(13) 0.0873(2) 0.28016(17) 0.0215(8) Uani 1 1 d . . . N10 N 0.35486(14) 0.0503(2) 0.32471(18) 0.0244(8) Uani 1 1 d . . . H10A H 0.3524 0.0570 0.3683 0.029 Uiso 1 1 calc R . . N11 N 0.15595(13) 0.0958(2) 0.09780(17) 0.0254(8) Uani 1 1 d . . . N12 N 0.12381(14) 0.0781(3) 0.04176(18) 0.0290(9) Uani 1 1 d . . . H12 H 0.1140 0.1150 0.0124 0.035 Uiso 1 1 calc R . . O1 O 0.25791(11) -0.01249(18) 0.08446(13) 0.0209(6) Uani 1 1 d . . . O2 O 0.36078(12) 0.16460(19) 0.16799(15) 0.0279(7) Uani 1 1 d . . . O3 O 0.15632(12) -0.14929(19) 0.20347(15) 0.0301(7) Uani 1 1 d . . . O4 O 0.27484(11) -0.06748(18) 0.20749(14) 0.0214(6) Uani 1 1 d . . . O5 O 0.38345(11) 0.01401(18) 0.06603(14) 0.0231(7) Uani 1 1 d . . . O6 O 0.11847(11) 0.03677(18) 0.22007(14) 0.0250(7) Uani 1 1 d . . . O7 O 0.24134(10) 0.08454(18) 0.18540(13) 0.0209(6) Uani 1 1 d . . . O8 O 0.39662(11) -0.00241(19) 0.23645(14) 0.0246(7) Uani 1 1 d . . . O9 O 0.12496(12) -0.0492(2) 0.07599(16) 0.0301(7) Uani 1 1 d . . . O10 O 0.4852(2) 0.6294(4) 0.1372(3) 0.107(2) Uani 1 1 d . . . H10 H 0.5064 0.6580 0.1149 0.080 Uiso 1 1 calc R . . O11 O 0.41685(16) 0.7204(2) 0.0630(2) 0.0515(10) Uani 1 1 d . . . H11 H 0.4393 0.7031 0.0920 0.077 Uiso 1 1 calc R . . O12 O 0.23298(15) 0.6316(2) 0.07145(19) 0.0500(10) Uani 1 1 d . . . H12A H 0.2580 0.6600 0.0559 0.080 Uiso 1 1 calc R . . O13 O 0.0021(3) 0.3906(6) 0.2066(5) 0.184(4) Uani 1 1 d . . . H13 H 0.0026 0.4352 0.1870 0.276 Uiso 1 1 calc R . . O14 O 0.07822(18) 0.3335(3) 0.0643(2) 0.0643(12) Uani 1 1 d . . . H14 H 0.0459 0.3333 0.0772 0.096 Uiso 1 1 calc R . . O15 O 0.09523(16) 0.2162(3) 0.97212(18) 0.0548(11) Uani 1 1 d . . . H15 H 0.0699 0.1924 0.9513 0.082 Uiso 1 1 calc R . . O16 O 0.0927(4) 0.8085(5) 0.5023(4) 0.197(4) Uani 1 1 d . . . O17 O 0.1452(2) 0.9224(3) 0.4810(3) 0.1032(19) Uani 1 1 d . . . O18 O 0.1630(3) 0.8003(4) 0.4405(3) 0.128(2) Uani 1 1 d . . . O19 O 0.0993(3) 0.8729(5) 0.3969(3) 0.151(3) Uani 1 1 d . . . O20 O 0.45658(16) 0.2060(3) 0.8861(2) 0.0620(12) Uani 1 1 d . . . O21 O 0.40994(16) 0.2226(3) 0.98496(18) 0.0581(11) Uani 1 1 d . . . O22 O 0.41020(17) 0.3254(3) 0.9062(2) 0.0688(13) Uani 1 1 d . . . O23 O 0.36151(16) 0.2074(3) 0.8843(2) 0.0621(12) Uani 1 1 d . . . O24 O 0.29786(18) 0.0500(3) 0.4596(2) 0.0642(12) Uani 1 1 d . . . O25 O 0.23765(19) 0.0814(5) 0.5427(2) 0.105(2) Uani 1 1 d . . . O26 O 0.27185(18) 0.1812(3) 0.4747(2) 0.0700(13) Uani 1 1 d . . . O27 O 0.21009(18) 0.0914(3) 0.4306(2) 0.0731(14) Uani 1 1 d . . . C1 C 0.25875(16) -0.0236(3) 0.0188(2) 0.0198(9) Uani 1 1 d . . . C2 C 0.27588(16) 0.0373(3) -0.0239(2) 0.0215(9) Uani 1 1 d . . . C3 C 0.27826(17) 0.0223(3) -0.0928(2) 0.0266(10) Uani 1 1 d . . . H3 H 0.2898 0.0642 -0.1215 0.032 Uiso 1 1 calc R . . C4 C 0.26459(19) -0.0507(3) -0.1205(2) 0.0290(11) Uani 1 1 d . . . C5 C 0.24668(18) -0.1103(3) -0.0774(2) 0.0291(10) Uani 1 1 d . . . H5 H 0.2367 -0.1611 -0.0955 0.035 Uiso 1 1 calc R . . C6 C 0.24296(17) -0.0978(3) -0.0089(2) 0.0229(9) Uani 1 1 d . . . C7 C 0.2705(2) -0.0672(3) -0.1944(2) 0.0416(13) Uani 1 1 d . . . H7A H 0.2837 -0.0189 -0.2167 0.062 Uiso 1 1 calc R . . H7B H 0.2350 -0.0825 -0.2139 0.062 Uiso 1 1 calc R . . H7C H 0.2965 -0.1111 -0.2004 0.062 Uiso 1 1 calc R . . C8 C 0.29039(17) 0.1171(3) -0.0002(2) 0.0263(10) Uani 1 1 d . . . H8 H 0.2895 0.1604 -0.0311 0.032 Uiso 1 1 calc R . . C9 C 0.22394(17) -0.1639(3) 0.0314(2) 0.0257(10) Uani 1 1 d . . . H9 H 0.2225 -0.2158 0.0118 0.031 Uiso 1 1 calc R . . C10 C 0.34659(16) 0.2222(3) 0.1314(2) 0.0236(10) Uani 1 1 d . . . C11 C 0.36044(17) 0.3055(3) 0.1495(2) 0.0273(10) Uani 1 1 d . . . C12 C 0.36553(18) 0.3654(3) 0.1020(3) 0.0314(11) Uani 1 1 d . . . H12B H 0.3604 0.3536 0.0557 0.038 Uiso 1 1 calc R . . C13 C 0.3780(2) 0.4420(3) 0.1221(3) 0.0446(14) Uani 1 1 d . . . H13A H 0.3819 0.4830 0.0895 0.054 Uiso 1 1 calc R . . C14 C 0.3848(2) 0.4600(3) 0.1886(4) 0.0528(16) Uani 1 1 d . . . H14A H 0.3935 0.5133 0.2020 0.063 Uiso 1 1 calc R . . C15 C 0.3792(2) 0.4011(4) 0.2362(3) 0.0461(14) Uani 1 1 d . . . H15A H 0.3832 0.4140 0.2824 0.055 Uiso 1 1 calc R . . C16 C 0.36789(19) 0.3236(3) 0.2172(2) 0.0354(12) Uani 1 1 d . . . H16 H 0.3651 0.2826 0.2500 0.042 Uiso 1 1 calc R . . C17 C 0.16492(17) -0.2164(3) 0.1797(2) 0.0245(10) Uani 1 1 d . . . C18 C 0.14626(17) -0.2889(3) 0.2147(2) 0.0283(10) Uani 1 1 d . . . C19 C 0.1322(2) -0.3592(3) 0.1814(3) 0.0380(12) Uani 1 1 d . . . H19 H 0.1339 -0.3625 0.1339 0.046 Uiso 1 1 calc R . . C20 C 0.1155(2) -0.4243(3) 0.2185(3) 0.0558(17) Uani 1 1 d . . . H20 H 0.1057 -0.4728 0.1964 0.067 Uiso 1 1 calc R . . C21 C 0.1129(2) -0.4195(4) 0.2872(3) 0.061(2) Uani 1 1 d . . . H21 H 0.1015 -0.4647 0.3122 0.074 Uiso 1 1 calc R . . C22 C 0.1267(2) -0.3504(4) 0.3192(3) 0.0558(17) Uani 1 1 d . . . H22 H 0.1252 -0.3477 0.3667 0.067 Uiso 1 1 calc R . . C23 C 0.1429(2) -0.2846(3) 0.2837(2) 0.0399(13) Uani 1 1 d . . . H23 H 0.1518 -0.2361 0.3064 0.048 Uiso 1 1 calc R . . C24 C 0.29231(16) -0.1186(3) 0.2535(2) 0.0205(9) Uani 1 1 d . . . C25 C 0.33553(16) -0.1712(3) 0.2404(2) 0.0236(10) Uani 1 1 d . . . C26 C 0.35424(18) -0.2235(3) 0.2896(2) 0.0307(11) Uani 1 1 d . . . H26 H 0.3820 -0.2606 0.2787 0.037 Uiso 1 1 calc R . . C27 C 0.33420(18) -0.2239(3) 0.3538(2) 0.0299(11) Uani 1 1 d . . . C28 C 0.29154(17) -0.1720(3) 0.3664(2) 0.0287(11) Uani 1 1 d . . . H28 H 0.2767 -0.1710 0.4100 0.034 Uiso 1 1 calc R . . C29 C 0.26963(16) -0.1214(3) 0.3174(2) 0.0225(9) Uani 1 1 d . . . C30 C 0.3597(2) -0.2764(3) 0.4072(3) 0.0412(13) Uani 1 1 d . . . H30A H 0.3686 -0.3288 0.3880 0.062 Uiso 1 1 calc R . . H30B H 0.3341 -0.2836 0.4437 0.062 Uiso 1 1 calc R . . H30C H 0.3931 -0.2510 0.4247 0.062 Uiso 1 1 calc R . . C31 C 0.36430(17) -0.1700(3) 0.1775(2) 0.0269(10) Uani 1 1 d . . . H31 H 0.3848 -0.2160 0.1655 0.032 Uiso 1 1 calc R . . C32 C 0.22510(17) -0.0694(3) 0.3359(2) 0.0247(10) Uani 1 1 d . . . H32 H 0.2176 -0.0637 0.3822 0.030 Uiso 1 1 calc R . . C33 C 0.40324(16) -0.0502(3) 0.0469(2) 0.0205(9) Uani 1 1 d . . . C34 C 0.43635(16) -0.0552(3) -0.0141(2) 0.0234(10) Uani 1 1 d . . . C35 C 0.47159(17) -0.1179(3) -0.0257(2) 0.0277(10) Uani 1 1 d . . . H35 H 0.4745 -0.1609 0.0054 0.033 Uiso 1 1 calc R . . C36 C 0.50266(18) -0.1180(3) -0.0827(2) 0.0332(12) Uani 1 1 d . . . H36 H 0.5270 -0.1611 -0.0906 0.040 Uiso 1 1 calc R . . C37 C 0.49853(18) -0.0564(3) -0.1276(2) 0.0342(12) Uani 1 1 d . . . H37 H 0.5198 -0.0568 -0.1668 0.041 Uiso 1 1 calc R . . C38 C 0.46343(19) 0.0064(4) -0.1160(2) 0.0387(13) Uani 1 1 d . . . H38 H 0.4602 0.0488 -0.1476 0.046 Uiso 1 1 calc R . . C39 C 0.43315(18) 0.0079(3) -0.0590(2) 0.0308(11) Uani 1 1 d . . . H39 H 0.4100 0.0522 -0.0503 0.037 Uiso 1 1 calc R . . C40 C 0.11762(17) 0.0474(3) 0.2815(2) 0.0232(10) Uani 1 1 d . . . C41 C 0.07528(17) 0.0969(3) 0.3132(2) 0.0272(10) Uani 1 1 d . . . C42 C 0.05769(19) 0.0795(3) 0.3777(2) 0.0370(12) Uani 1 1 d . . . H42 H 0.0731 0.0363 0.4026 0.044 Uiso 1 1 calc R . . C43 C 0.0170(2) 0.1272(4) 0.4046(3) 0.0445(14) Uani 1 1 d . . . H43 H 0.0040 0.1157 0.4481 0.053 Uiso 1 1 calc R . . C44 C -0.0044(2) 0.1897(4) 0.3695(3) 0.0481(15) Uani 1 1 d . . . H44 H -0.0313 0.2226 0.3891 0.058 Uiso 1 1 calc R . . C45 C 0.0125(2) 0.2057(4) 0.3056(3) 0.0490(15) Uani 1 1 d . . . H45 H -0.0032 0.2488 0.2808 0.059 Uiso 1 1 calc R . . C46 C 0.05244(19) 0.1589(3) 0.2777(2) 0.0347(12) Uani 1 1 d . . . H46 H 0.0641 0.1698 0.2336 0.042 Uiso 1 1 calc R . . C47 C 0.22726(16) 0.1555(3) 0.2073(2) 0.0215(9) Uani 1 1 d . . . C48 C 0.25101(17) 0.1886(3) 0.2653(2) 0.0231(9) Uani 1 1 d . . . C49 C 0.23450(19) 0.2631(3) 0.2875(3) 0.0367(12) Uani 1 1 d . . . H49 H 0.2506 0.2840 0.3275 0.044 Uiso 1 1 calc R . . C50 C 0.1954(2) 0.3087(3) 0.2537(3) 0.0434(13) Uani 1 1 d . . . C51 C 0.1726(2) 0.2753(3) 0.1955(3) 0.0378(12) Uani 1 1 d . . . H51 H 0.1463 0.3054 0.1707 0.045 Uiso 1 1 calc R . . C52 C 0.18670(17) 0.2005(3) 0.1726(2) 0.0260(10) Uani 1 1 d . . . C53 C 0.1788(3) 0.3901(4) 0.2768(4) 0.073(2) Uani 1 1 d . . . H53A H 0.1951 0.4007 0.3212 0.110 Uiso 1 1 calc R . . H53B H 0.1390 0.3925 0.2794 0.110 Uiso 1 1 calc R . . H53C H 0.1912 0.4305 0.2450 0.110 Uiso 1 1 calc R . . C54 C 0.29228(17) 0.1456(3) 0.3040(2) 0.0229(9) Uani 1 1 d . . . H54 H 0.2996 0.1617 0.3489 0.027 Uiso 1 1 calc R . . C55 C 0.15758(17) 0.1699(3) 0.1140(2) 0.0280(10) Uani 1 1 d . . . H55 H 0.1386 0.2071 0.0861 0.034 Uiso 1 1 calc R . . C56 C 0.39335(17) 0.0041(3) 0.2986(2) 0.0235(9) Uani 1 1 d . . . C57 C 0.42956(17) -0.0418(3) 0.3447(2) 0.0245(10) Uani 1 1 d . . . C58 C 0.4302(2) -0.0299(3) 0.4142(2) 0.0379(12) Uani 1 1 d . . . H58 H 0.4081 0.0105 0.4334 0.045 Uiso 1 1 calc R . . C59 C 0.4631(2) -0.0775(4) 0.4543(3) 0.0453(14) Uani 1 1 d . . . H59 H 0.4642 -0.0694 0.5015 0.054 Uiso 1 1 calc R . . C60 C 0.49420(19) -0.1365(4) 0.4267(3) 0.0443(14) Uani 1 1 d . . . H60 H 0.5160 -0.1700 0.4549 0.053 Uiso 1 1 calc R . . C61 C 0.4942(2) -0.1476(4) 0.3588(3) 0.0451(14) Uani 1 1 d . . . H61 H 0.5163 -0.1882 0.3399 0.054 Uiso 1 1 calc R . . C62 C 0.46190(17) -0.0993(3) 0.3175(3) 0.0348(12) Uani 1 1 d . . . H62 H 0.4623 -0.1062 0.2703 0.042 Uiso 1 1 calc R . . C63 C 0.10872(17) 0.0019(3) 0.0353(2) 0.0278(11) Uani 1 1 d . . . C64 C 0.07114(17) -0.0214(4) -0.0206(2) 0.0350(13) Uani 1 1 d . . . C65 C 0.04746(19) 0.0357(4) -0.0639(2) 0.0438(15) Uani 1 1 d . . . H65 H 0.0572 0.0908 -0.0608 0.053 Uiso 1 1 calc R . . C66 C 0.0095(2) 0.0095(6) -0.1114(3) 0.062(2) Uani 1 1 d . . . H66 H -0.0073 0.0474 -0.1409 0.074 Uiso 1 1 calc R . . C67 C -0.0042(2) -0.0699(6) -0.1167(3) 0.072(3) Uani 1 1 d . . . H67 H -0.0306 -0.0865 -0.1494 0.086 Uiso 1 1 calc R . . C68 C 0.0196(2) -0.1250(5) -0.0757(3) 0.062(2) Uani 1 1 d . . . H68 H 0.0103 -0.1800 -0.0804 0.074 Uiso 1 1 calc R . . C69 C 0.05773(19) -0.1015(4) -0.0267(3) 0.0430(14) Uani 1 1 d . . . H69 H 0.0742 -0.1402 0.0022 0.052 Uiso 1 1 calc R . . C70 C 0.4891(3) 0.6520(7) 0.2069(4) 0.123(4) Uani 1 1 d . . . H70A H 0.5263 0.6427 0.2238 0.184 Uiso 1 1 calc R . . H70B H 0.4637 0.6196 0.2327 0.184 Uiso 1 1 calc R . . H70C H 0.4800 0.7089 0.2115 0.184 Uiso 1 1 calc R . . C71 C 0.3685(3) 0.6723(4) 0.0637(4) 0.076(2) Uani 1 1 d . . . H71A H 0.3696 0.6370 0.1030 0.114 Uiso 1 1 calc R . . H71B H 0.3662 0.6397 0.0229 0.114 Uiso 1 1 calc R . . H71C H 0.3365 0.7073 0.0658 0.114 Uiso 1 1 calc R . . C72 C 0.2553(3) 0.5785(5) 0.1217(4) 0.078(2) Uani 1 1 d . . . H72A H 0.2702 0.6101 0.1592 0.116 Uiso 1 1 calc R . . H72B H 0.2844 0.5462 0.1023 0.116 Uiso 1 1 calc R . . H72C H 0.2266 0.5430 0.1378 0.116 Uiso 1 1 calc R . . C73 C 0.0002(2) 0.3305(4) 0.1601(3) 0.0395(13) Uani 1 1 d . . . H73A H 0.0321 0.3341 0.1316 0.059 Uiso 1 1 calc . . . H73B H -0.0330 0.3359 0.1323 0.059 Uiso 1 1 calc . . . H73C H 0.0001 0.2785 0.1829 0.059 Uiso 1 1 calc . . . C74 C 0.0966(3) 0.4140(5) 0.0586(3) 0.075(2) Uani 1 1 d . . . H74A H 0.0656 0.4491 0.0481 0.112 Uiso 1 1 calc R . . H74B H 0.1231 0.4176 0.0227 0.112 Uiso 1 1 calc R . . H74C H 0.1138 0.4309 0.1011 0.112 Uiso 1 1 calc R . . C75 C 0.1359(3) 0.2362(5) 0.9278(4) 0.089(3) Uani 1 1 d . . . H75A H 0.1212 0.2728 0.8935 0.134 Uiso 1 1 calc R . . H75B H 0.1494 0.1875 0.9063 0.134 Uiso 1 1 calc R . . H75C H 0.1659 0.2626 0.9523 0.134 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 Dy1 0.01755(10) 0.02255(11) 0.01691(11) -0.00160(9) -0.00012(7) -0.00187(8) Dy2 0.01685(10) 0.02084(11) 0.01679(10) 0.00164(8) -0.00065(7) -0.00062(8) Cl1 0.0491(8) 0.0473(8) 0.0397(7) 0.0052(7) -0.0025(6) -0.0043(7) Cl2 0.0404(7) 0.0438(8) 0.0389(7) 0.0120(6) 0.0054(6) 0.0037(6) Cl3 0.0462(8) 0.0661(10) 0.0285(7) -0.0053(7) -0.0051(5) -0.0097(7) N1 0.0200(18) 0.024(2) 0.0232(19) -0.0008(16) 0.0007(15) -0.0003(15) N2 0.0248(19) 0.0213(19) 0.0242(19) 0.0033(16) -0.0013(15) -0.0004(16) N3 0.0239(19) 0.0216(19) 0.0194(18) 0.0021(16) 0.0015(14) -0.0014(15) N4 0.029(2) 0.0200(19) 0.027(2) 0.0009(17) 0.0058(16) -0.0030(16) N5 0.0215(18) 0.024(2) 0.0181(18) 0.0006(16) 0.0039(14) 0.0000(15) N6 0.028(2) 0.028(2) 0.024(2) -0.0010(17) 0.0079(16) 0.0032(17) N7 0.0188(18) 0.030(2) 0.0212(18) -0.0057(17) 0.0011(15) -0.0006(16) N8 0.0227(19) 0.037(2) 0.0205(19) -0.0034(17) 0.0025(15) 0.0076(17) N9 0.0224(18) 0.0221(19) 0.0198(18) 0.0021(16) -0.0064(14) -0.0019(16) N10 0.0235(19) 0.032(2) 0.0172(18) -0.0007(16) -0.0046(15) 0.0027(16) N11 0.0181(18) 0.035(2) 0.0225(19) 0.0004(18) -0.0024(14) -0.0019(17) N12 0.024(2) 0.042(3) 0.0203(19) -0.0018(19) -0.0064(15) 0.0025(18) O1 0.0229(15) 0.0249(16) 0.0147(14) 0.0001(13) -0.0020(11) -0.0039(13) O2 0.0280(17) 0.0298(18) 0.0256(16) 0.0016(15) -0.0061(13) -0.0046(14) O3 0.0338(18) 0.0275(18) 0.0294(17) -0.0049(15) 0.0078(14) -0.0064(15) O4 0.0216(15) 0.0231(16) 0.0197(15) 0.0021(13) 0.0017(12) 0.0008(13) O5 0.0222(15) 0.0253(17) 0.0220(16) 0.0008(14) 0.0033(12) 0.0010(13) O6 0.0237(16) 0.0340(18) 0.0173(15) -0.0050(14) -0.0015(12) 0.0020(14) O7 0.0170(14) 0.0242(16) 0.0214(15) 0.0010(13) -0.0019(11) 0.0000(12) O8 0.0206(15) 0.0292(17) 0.0238(17) 0.0019(14) -0.0028(12) 0.0028(13) O9 0.0273(17) 0.0336(19) 0.0292(18) -0.0096(16) -0.0065(14) -0.0005(15) O10 0.075(4) 0.101(5) 0.148(6) 0.042(4) 0.013(4) -0.014(3) O11 0.061(3) 0.037(2) 0.057(3) -0.001(2) 0.010(2) 0.002(2) O12 0.048(2) 0.044(2) 0.058(2) 0.000(2) 0.0085(19) 0.0108(19) O13 0.167(8) 0.164(9) 0.221(10) 0.075(8) -0.008(7) 0.019(7) O14 0.070(3) 0.067(3) 0.056(3) 0.002(2) -0.002(2) 0.015(3) O15 0.059(3) 0.062(3) 0.043(2) 0.015(2) -0.0135(19) 0.003(2) O16 0.258(9) 0.135(7) 0.206(8) 0.013(6) 0.182(8) -0.033(7) O17 0.117(5) 0.064(4) 0.127(5) -0.024(4) -0.037(4) 0.005(3) O18 0.128(5) 0.112(5) 0.144(6) 0.012(4) 0.054(4) 0.052(4) O19 0.135(6) 0.192(9) 0.123(5) 0.033(6) -0.064(4) -0.011(6) O20 0.059(3) 0.061(3) 0.067(3) 0.009(2) 0.025(2) 0.017(2) O21 0.065(3) 0.077(3) 0.032(2) 0.009(2) 0.0010(19) 0.003(2) O22 0.057(3) 0.048(3) 0.102(4) 0.025(3) 0.013(2) 0.011(2) O23 0.052(2) 0.087(4) 0.047(2) 0.003(2) -0.0086(19) -0.009(2) O24 0.077(3) 0.061(3) 0.055(3) -0.004(2) 0.008(2) 0.016(2) O25 0.064(3) 0.209(7) 0.042(3) 0.022(4) 0.007(2) -0.008(4) O26 0.076(3) 0.057(3) 0.077(3) -0.027(3) -0.029(2) -0.003(2) O27 0.077(3) 0.078(3) 0.063(3) -0.006(3) -0.040(2) -0.020(3) C1 0.017(2) 0.026(2) 0.017(2) -0.0047(19) -0.0026(16) 0.0000(18) C2 0.021(2) 0.026(2) 0.017(2) 0.0000(19) 0.0001(16) 0.0022(18) C3 0.026(2) 0.037(3) 0.017(2) 0.004(2) -0.0030(17) -0.002(2) C4 0.033(3) 0.034(3) 0.019(2) 0.001(2) 0.0022(19) 0.003(2) C5 0.036(3) 0.030(3) 0.022(2) -0.006(2) -0.0002(19) 0.001(2) C6 0.024(2) 0.027(2) 0.018(2) 0.001(2) 0.0005(17) 0.0027(19) C7 0.060(4) 0.047(3) 0.019(2) -0.006(2) 0.004(2) -0.003(3) C8 0.024(2) 0.031(3) 0.024(2) 0.004(2) 0.0006(18) 0.001(2) C9 0.026(2) 0.024(2) 0.026(2) -0.004(2) -0.0025(18) 0.0008(19) C10 0.019(2) 0.028(2) 0.024(2) 0.002(2) 0.0011(18) -0.0019(19) C11 0.019(2) 0.028(3) 0.034(3) 0.002(2) -0.0019(19) -0.0030(19) C12 0.028(2) 0.028(3) 0.038(3) 0.005(2) -0.005(2) -0.002(2) C13 0.044(3) 0.028(3) 0.061(4) 0.009(3) -0.007(3) -0.005(2) C14 0.046(3) 0.028(3) 0.084(5) -0.012(3) -0.005(3) -0.005(3) C15 0.046(3) 0.046(3) 0.046(3) -0.017(3) -0.002(3) -0.002(3) C16 0.035(3) 0.037(3) 0.034(3) -0.008(2) 0.001(2) -0.010(2) C17 0.021(2) 0.030(3) 0.023(2) 0.006(2) -0.0021(18) -0.0006(19) C18 0.020(2) 0.031(3) 0.035(3) 0.005(2) 0.0065(19) -0.0003(19) C19 0.036(3) 0.033(3) 0.046(3) 0.005(3) 0.012(2) 0.000(2) C20 0.053(4) 0.027(3) 0.089(5) 0.003(3) 0.032(3) -0.003(3) C21 0.061(4) 0.041(4) 0.083(5) 0.029(4) 0.044(4) 0.013(3) C22 0.060(4) 0.059(4) 0.050(4) 0.023(3) 0.031(3) 0.016(3) C23 0.039(3) 0.046(3) 0.035(3) 0.009(3) 0.016(2) 0.003(2) C24 0.020(2) 0.021(2) 0.020(2) 0.0043(19) -0.0006(17) -0.0032(17) C25 0.021(2) 0.026(2) 0.024(2) 0.005(2) 0.0041(18) -0.0004(18) C26 0.025(2) 0.030(3) 0.038(3) 0.009(2) 0.002(2) 0.004(2) C27 0.026(2) 0.032(3) 0.031(3) 0.014(2) -0.002(2) -0.002(2) C28 0.026(2) 0.039(3) 0.021(2) 0.009(2) 0.0017(18) -0.005(2) C29 0.019(2) 0.026(2) 0.023(2) 0.0044(19) -0.0016(17) 0.0011(18) C30 0.031(3) 0.052(3) 0.040(3) 0.022(3) -0.003(2) 0.001(2) C31 0.025(2) 0.025(2) 0.031(3) -0.003(2) 0.0016(19) 0.0035(19) C32 0.024(2) 0.033(3) 0.018(2) 0.000(2) 0.0016(18) -0.001(2) C33 0.017(2) 0.024(2) 0.020(2) -0.0029(19) -0.0040(17) -0.0019(18) C34 0.016(2) 0.032(2) 0.022(2) -0.002(2) -0.0017(17) -0.0046(18) C35 0.024(2) 0.030(3) 0.030(2) 0.002(2) 0.0015(19) -0.002(2) C36 0.024(2) 0.044(3) 0.033(3) -0.009(2) 0.007(2) -0.003(2) C37 0.026(2) 0.055(3) 0.022(2) -0.006(2) 0.0046(19) -0.010(2) C38 0.031(3) 0.057(4) 0.028(3) 0.014(3) 0.003(2) -0.005(3) C39 0.024(2) 0.041(3) 0.027(2) 0.004(2) -0.0021(19) 0.000(2) C40 0.021(2) 0.025(2) 0.024(2) -0.0038(19) -0.0008(18) -0.0028(18) C41 0.020(2) 0.036(3) 0.025(2) -0.011(2) -0.0054(18) 0.002(2) C42 0.033(3) 0.049(3) 0.029(3) -0.009(2) 0.000(2) 0.005(2) C43 0.033(3) 0.069(4) 0.032(3) -0.015(3) 0.003(2) 0.004(3) C44 0.035(3) 0.064(4) 0.045(3) -0.019(3) 0.004(2) 0.012(3) C45 0.038(3) 0.053(4) 0.055(4) -0.005(3) -0.008(3) 0.017(3) C46 0.030(3) 0.045(3) 0.029(3) -0.006(2) -0.003(2) 0.002(2) C47 0.016(2) 0.023(2) 0.025(2) 0.0000(19) -0.0026(17) -0.0017(18) C48 0.022(2) 0.024(2) 0.023(2) -0.002(2) -0.0024(17) -0.0011(18) C49 0.030(3) 0.035(3) 0.044(3) -0.011(2) -0.013(2) 0.001(2) C50 0.040(3) 0.030(3) 0.060(4) -0.013(3) -0.018(3) 0.009(2) C51 0.034(3) 0.025(3) 0.053(3) 0.000(3) -0.016(2) 0.005(2) C52 0.025(2) 0.022(2) 0.030(2) 0.001(2) -0.0036(19) -0.0025(19) C53 0.075(5) 0.044(4) 0.099(5) -0.029(4) -0.049(4) 0.022(3) C54 0.024(2) 0.027(2) 0.017(2) -0.0011(19) -0.0033(17) -0.0023(19) C55 0.025(2) 0.029(3) 0.029(2) 0.005(2) -0.0059(19) 0.002(2) C56 0.023(2) 0.022(2) 0.026(2) -0.001(2) -0.0020(18) -0.0059(19) C57 0.018(2) 0.027(2) 0.028(2) 0.009(2) -0.0055(18) -0.0028(18) C58 0.038(3) 0.045(3) 0.031(3) 0.006(2) -0.008(2) 0.005(2) C59 0.045(3) 0.062(4) 0.028(3) 0.014(3) -0.011(2) -0.003(3) C60 0.025(3) 0.055(4) 0.052(3) 0.027(3) -0.012(2) 0.005(2) C61 0.026(3) 0.050(4) 0.059(4) 0.011(3) 0.000(2) 0.015(2) C62 0.021(2) 0.044(3) 0.038(3) 0.004(3) -0.005(2) 0.004(2) C63 0.017(2) 0.046(3) 0.021(2) -0.009(2) -0.0026(18) 0.003(2) C64 0.017(2) 0.066(4) 0.022(2) -0.015(3) 0.0008(18) 0.002(2) C65 0.023(2) 0.085(5) 0.024(2) -0.015(3) -0.003(2) 0.007(3) C66 0.024(3) 0.135(7) 0.027(3) -0.019(4) -0.006(2) 0.015(4) C67 0.030(3) 0.151(8) 0.035(3) -0.045(5) -0.006(3) 0.011(4) C68 0.032(3) 0.093(5) 0.061(4) -0.052(4) 0.008(3) -0.011(3) C69 0.026(3) 0.066(4) 0.037(3) -0.030(3) 0.002(2) 0.002(3) C70 0.067(5) 0.224(13) 0.078(6) 0.051(7) 0.029(5) 0.027(6) C71 0.075(5) 0.062(5) 0.092(6) -0.001(4) 0.011(4) -0.019(4) C72 0.067(5) 0.067(5) 0.099(6) 0.023(5) 0.006(4) 0.021(4) C73 0.040(3) 0.050(3) 0.028(3) -0.011(3) -0.001(2) 0.004(3) C74 0.093(5) 0.078(6) 0.053(4) 0.012(4) 0.002(4) 0.016(5) C75 0.070(5) 0.084(6) 0.114(7) 0.037(5) 0.006(5) 0.003(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 Dy1 O7 2.303(3) . ? Dy1 O1 2.316(3) . ? Dy1 O4 2.329(3) . ? Dy1 O3 2.331(3) . ? Dy1 O9 2.364(3) . ? Dy1 O6 2.392(3) . ? Dy1 N11 2.581(4) . ? Dy1 N3 2.584(4) . ? Dy1 N7 2.613(3) . ? Dy2 O7 2.326(3) . ? Dy2 O1 2.327(3) . ? Dy2 O4 2.338(3) . ? Dy2 O2 2.352(3) . ? Dy2 O5 2.353(3) . ? Dy2 O8 2.393(3) . ? Dy2 N1 2.567(4) . ? Dy2 N5 2.601(4) . ? Dy2 N9 2.614(3) . ? Cl1 O16 1.303(6) . ? Cl1 O19 1.373(6) . ? Cl1 O17 1.407(6) . ? Cl1 O18 1.429(6) . ? Cl2 O22 1.418(4) . ? Cl2 O21 1.420(4) . ? Cl2 O23 1.427(4) . ? Cl2 O20 1.440(4) . ? Cl3 O25 1.396(4) . ? Cl3 O24 1.413(4) . ? Cl3 O27 1.421(4) . ? Cl3 O26 1.433(5) . ? N1 C8 1.285(5) . ? N1 N2 1.374(5) . ? N2 C10 1.320(5) . ? N2 H2 0.8800 . ? N3 C9 1.289(5) . ? N3 N4 1.381(5) . ? N4 C17 1.332(5) . ? N4 H4 0.8800 . ? N5 C31 1.275(6) . ? N5 N6 1.378(4) . ? N6 C33 1.335(5) . ? N6 H6 0.8800 . ? N7 C32 1.276(5) . ? N7 N8 1.385(5) . ? N8 C40 1.328(6) . ? N8 H8A 0.8800 . ? N9 C54 1.272(5) . ? N9 N10 1.382(5) . ? N10 C56 1.334(6) . ? N10 H10A 0.8800 . ? N11 C55 1.277(6) . ? N11 N12 1.387(5) . ? N12 C63 1.328(6) . ? N12 H12 0.8800 . ? O1 C1 1.324(5) . ? O2 C10 1.252(5) . ? O3 C17 1.234(5) . ? O4 C24 1.317(5) . ? O5 C33 1.239(5) . ? O6 C40 1.240(5) . ? O7 C47 1.310(5) . ? O8 C56 1.249(5) . ? O9 C63 1.237(6) . ? O10 C70 1.441(10) . ? O10 H10 0.8400 . ? O11 C71 1.433(7) . ? O11 H11 0.8400 . ? O12 C72 1.436(7) . ? O12 H12A 0.8400 . ? O13 C73 1.367(11) . ? O13 H13 0.8400 . ? O14 C74 1.421(8) . ? O14 H14 0.8400 . ? O15 C75 1.390(7) . ? O15 H15 0.8400 . ? C1 C2 1.396(6) . ? C1 C6 1.406(6) . ? C2 C3 1.398(6) . ? C2 C8 1.454(6) . ? C3 C4 1.375(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 C7 1.510(6) . ? C5 C6 1.387(6) . ? C5 H5 0.9500 . ? C6 C9 1.447(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.472(6) . ? C11 C12 1.386(6) . ? C11 C16 1.391(6) . ? C12 C13 1.370(7) . ? C12 H12B 0.9500 . ? C13 C14 1.368(8) . ? C13 H13A 0.9500 . ? C14 C15 1.374(8) . ? C14 H14A 0.9500 . ? C15 C16 1.372(7) . ? C15 H15A 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.474(6) . ? C18 C23 1.382(6) . ? C18 C19 1.388(7) . ? C19 C20 1.380(7) . ? C19 H19 0.9500 . ? C20 C21 1.376(9) . ? C20 H20 0.9500 . ? C21 C22 1.357(9) . ? C21 H21 0.9500 . ? C22 C23 1.370(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.404(5) . ? C24 C25 1.405(6) . ? C25 C26 1.382(6) . ? C25 C31 1.455(6) . ? C26 C27 1.382(6) . ? C26 H26 0.9500 . ? C27 C28 1.386(6) . ? C27 C30 1.506(6) . ? C28 C29 1.391(6) . ? C28 H28 0.9500 . ? C29 C32 1.449(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.481(6) . ? C34 C35 1.380(6) . ? C34 C39 1.382(7) . ? C35 C36 1.383(6) . ? C35 H35 0.9500 . ? C36 C37 1.366(7) . ? C36 H36 0.9500 . ? C37 C38 1.378(7) . ? C37 H37 0.9500 . ? C38 C39 1.373(6) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.479(6) . ? C41 C46 1.367(7) . ? C41 C42 1.396(6) . ? C42 C43 1.393(7) . ? C42 H42 0.9500 . ? C43 C44 1.356(8) . ? C43 H43 0.9500 . ? C44 C45 1.375(8) . ? C44 H44 0.9500 . ? C45 C46 1.379(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.398(6) . ? C47 C52 1.416(6) . ? C48 C49 1.382(6) . ? C48 C54 1.450(6) . ? C49 C50 1.388(7) . ? C49 H49 0.9500 . ? C50 C51 1.393(7) . ? C50 C53 1.493(7) . ? C51 C52 1.374(6) . ? C51 H51 0.9500 . ? C52 C55 1.450(6) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.480(6) . ? C57 C62 1.364(6) . ? C57 C58 1.400(6) . ? C58 C59 1.378(7) . ? C58 H58 0.9500 . ? C59 C60 1.368(8) . ? C59 H59 0.9500 . ? C60 C61 1.368(8) . ? C60 H60 0.9500 . ? C61 C62 1.389(7) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C64 1.484(6) . ? C64 C69 1.380(8) . ? C64 C65 1.404(8) . ? C65 C66 1.386(7) . ? C65 H65 0.9500 . ? C66 C67 1.370(11) . ? C66 H66 0.9500 . ? C67 C68 1.354(10) . ? C67 H67 0.9500 . ? C68 C69 1.396(7) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? 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 O7 Dy1 O1 69.16(10) . . ? O7 Dy1 O4 71.22(10) . . ? O1 Dy1 O4 69.41(10) . . ? O7 Dy1 O3 146.74(10) . . ? O1 Dy1 O3 127.19(10) . . ? O4 Dy1 O3 87.24(11) . . ? O7 Dy1 O9 128.33(11) . . ? O1 Dy1 O9 90.52(10) . . ? O4 Dy1 O9 145.83(10) . . ? O3 Dy1 O9 83.44(11) . . ? O7 Dy1 O6 86.29(10) . . ? O1 Dy1 O6 144.69(10) . . ? O4 Dy1 O6 127.17(10) . . ? O3 Dy1 O6 87.17(10) . . ? O9 Dy1 O6 85.19(10) . . ? O7 Dy1 N11 67.08(11) . . ? O1 Dy1 N11 78.45(10) . . ? O4 Dy1 N11 134.09(10) . . ? O3 Dy1 N11 138.67(11) . . ? O9 Dy1 N11 62.39(11) . . ? O6 Dy1 N11 68.52(10) . . ? O7 Dy1 N3 132.72(10) . . ? O1 Dy1 N3 66.10(10) . . ? O4 Dy1 N3 79.49(10) . . ? O3 Dy1 N3 63.34(10) . . ? O9 Dy1 N3 66.93(11) . . ? O6 Dy1 N3 140.59(10) . . ? N11 Dy1 N3 116.45(11) . . ? O7 Dy1 N7 78.59(10) . . ? O1 Dy1 N7 131.14(10) . . ? O4 Dy1 N7 65.89(10) . . ? O3 Dy1 N7 69.40(11) . . ? O9 Dy1 N7 138.23(11) . . ? O6 Dy1 N7 63.04(10) . . ? N11 Dy1 N7 121.38(11) . . ? N3 Dy1 N7 121.76(11) . . ? O7 Dy2 O1 68.58(10) . . ? O7 Dy2 O4 70.66(10) . . ? O1 Dy2 O4 69.08(10) . . ? O7 Dy2 O2 87.96(10) . . ? O1 Dy2 O2 128.06(10) . . ? O4 Dy2 O2 145.94(10) . . ? O7 Dy2 O5 142.18(10) . . ? O1 Dy2 O5 84.44(10) . . ? O4 Dy2 O5 124.60(10) . . ? O2 Dy2 O5 88.57(10) . . ? O7 Dy2 O8 125.00(9) . . ? O1 Dy2 O8 146.21(11) . . ? O4 Dy2 O8 85.88(10) . . ? O2 Dy2 O8 85.30(11) . . ? O5 Dy2 O8 92.18(10) . . ? O7 Dy2 N1 77.02(10) . . ? O1 Dy2 N1 66.72(11) . . ? O4 Dy2 N1 132.18(10) . . ? O2 Dy2 N1 63.03(11) . . ? O5 Dy2 N1 67.93(10) . . ? O8 Dy2 N1 141.94(11) . . ? O7 Dy2 N5 133.90(10) . . ? O1 Dy2 N5 81.42(11) . . ? O4 Dy2 N5 66.18(10) . . ? O2 Dy2 N5 137.83(10) . . ? O5 Dy2 N5 62.23(10) . . ? O8 Dy2 N5 67.51(11) . . ? N1 Dy2 N5 122.51(11) . . ? O7 Dy2 N9 64.81(10) . . ? O1 Dy2 N9 129.69(10) . . ? O4 Dy2 N9 78.52(10) . . ? O2 Dy2 N9 68.30(10) . . ? O5 Dy2 N9 145.68(10) . . ? O8 Dy2 N9 62.05(10) . . ? N1 Dy2 N9 117.87(11) . . ? N5 Dy2 N9 119.34(11) . . ? O16 Cl1 O19 124.6(6) . . ? O16 Cl1 O17 119.1(5) . . ? O19 Cl1 O17 102.3(4) . . ? O16 Cl1 O18 103.5(5) . . ? O19 Cl1 O18 100.0(5) . . ? O17 Cl1 O18 104.0(4) . . ? O22 Cl2 O21 110.0(3) . . ? O22 Cl2 O23 110.5(3) . . ? O21 Cl2 O23 109.5(3) . . ? O22 Cl2 O20 109.3(3) . . ? O21 Cl2 O20 108.3(3) . . ? O23 Cl2 O20 109.1(3) . . ? O25 Cl3 O24 110.4(3) . . ? O25 Cl3 O27 111.5(3) . . ? O24 Cl3 O27 110.3(3) . . ? O25 Cl3 O26 109.8(4) . . ? O24 Cl3 O26 107.8(3) . . ? O27 Cl3 O26 107.0(3) . . ? C8 N1 N2 116.2(4) . . ? C8 N1 Dy2 130.0(3) . . ? N2 N1 Dy2 113.2(2) . . ? C10 N2 N1 117.0(4) . . ? C10 N2 H2 121.5 . . ? N1 N2 H2 121.5 . . ? C9 N3 N4 115.0(4) . . ? C9 N3 Dy1 131.0(3) . . ? N4 N3 Dy1 113.1(2) . . ? C17 N4 N3 116.0(4) . . ? C17 N4 H4 122.0 . . ? N3 N4 H4 122.0 . . ? C31 N5 N6 115.9(4) . . ? C31 N5 Dy2 128.7(3) . . ? N6 N5 Dy2 114.2(2) . . ? C33 N6 N5 116.2(4) . . ? C33 N6 H6 121.9 . . ? N5 N6 H6 121.9 . . ? C32 N7 N8 114.3(4) . . ? C32 N7 Dy1 132.9(3) . . ? N8 N7 Dy1 112.6(3) . . ? C40 N8 N7 117.8(4) . . ? C40 N8 H8A 121.1 . . ? N7 N8 H8A 121.1 . . ? C54 N9 N10 115.3(4) . . ? C54 N9 Dy2 131.0(3) . . ? N10 N9 Dy2 113.3(2) . . ? C56 N10 N9 116.9(4) . . ? C56 N10 H10A 121.5 . . ? N9 N10 H10A 121.5 . . ? C55 N11 N12 115.1(4) . . ? C55 N11 Dy1 130.0(3) . . ? N12 N11 Dy1 114.2(3) . . ? C63 N12 N11 115.8(4) . . ? C63 N12 H12 122.1 . . ? N11 N12 H12 122.1 . . ? C1 O1 Dy1 132.6(2) . . ? C1 O1 Dy2 129.8(2) . . ? Dy1 O1 Dy2 97.53(10) . . ? C10 O2 Dy2 124.4(3) . . ? C17 O3 Dy1 125.5(3) . . ? C24 O4 Dy1 136.1(2) . . ? C24 O4 Dy2 126.3(2) . . ? Dy1 O4 Dy2 96.85(11) . . ? C33 O5 Dy2 127.1(3) . . ? C40 O6 Dy1 124.5(3) . . ? C47 O7 Dy1 131.3(2) . . ? C47 O7 Dy2 130.8(2) . . ? Dy1 O7 Dy2 97.91(11) . . ? C56 O8 Dy2 124.8(3) . . ? C63 O9 Dy1 125.9(3) . . ? C70 O10 H10 109.5 . . ? C71 O11 H11 109.5 . . ? C72 O12 H12A 109.5 . . ? C73 O13 H13 109.5 . . ? C74 O14 H14 109.5 . . ? C75 O15 H15 109.5 . . ? O1 C1 C2 120.9(4) . . ? O1 C1 C6 120.2(4) . . ? C2 C1 C6 118.9(4) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 C8 122.7(4) . . ? C3 C2 C8 117.9(4) . . ? C4 C3 C2 122.5(4) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 117.5(4) . . ? C3 C4 C7 121.8(4) . . ? C5 C4 C7 120.7(4) . . ? C6 C5 C4 121.9(4) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C1 119.8(4) . . ? C5 C6 C9 117.5(4) . . ? C1 C6 C9 122.7(4) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C2 122.5(4) . . ? N1 C8 H8 118.7 . . ? C2 C8 H8 118.7 . . ? N3 C9 C6 123.3(4) . . ? N3 C9 H9 118.4 . . ? C6 C9 H9 118.4 . . ? O2 C10 N2 120.2(4) . . ? O2 C10 C11 121.3(4) . . ? N2 C10 C11 118.4(4) . . ? C12 C11 C16 119.7(5) . . ? C12 C11 C10 122.3(4) . . ? C16 C11 C10 117.9(4) . . ? C13 C12 C11 119.6(5) . . ? C13 C12 H12B 120.2 . . ? C11 C12 H12B 120.2 . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C11 119.6(5) . . ? C15 C16 H16 120.2 . . ? C11 C16 H16 120.2 . . ? O3 C17 N4 121.4(4) . . ? O3 C17 C18 120.3(4) . . ? N4 C17 C18 118.3(4) . . ? C23 C18 C19 120.1(5) . . ? C23 C18 C17 117.0(5) . . ? C19 C18 C17 122.9(4) . . ? C20 C19 C18 118.7(5) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C21 C20 C19 120.7(6) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.1(5) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.6(6) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.8(6) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? O4 C24 C29 121.6(4) . . ? O4 C24 C25 120.7(4) . . ? C29 C24 C25 117.6(4) . . ? C26 C25 C24 120.2(4) . . ? C26 C25 C31 117.4(4) . . ? C24 C25 C31 122.3(4) . . ? C27 C26 C25 122.7(4) . . ? C27 C26 H26 118.6 . . ? C25 C26 H26 118.6 . . ? C26 C27 C28 116.8(4) . . ? C26 C27 C30 120.5(4) . . ? C28 C27 C30 122.6(4) . . ? C27 C28 C29 122.3(4) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C28 C29 C24 120.2(4) . . ? C28 C29 C32 117.8(4) . . ? C24 C29 C32 121.9(4) . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 C25 123.2(4) . . ? N5 C31 H31 118.4 . . ? C25 C31 H31 118.4 . . ? N7 C32 C29 123.8(4) . . ? N7 C32 H32 118.1 . . ? C29 C32 H32 118.1 . . ? O5 C33 N6 120.0(4) . . ? O5 C33 C34 121.8(4) . . ? N6 C33 C34 118.1(4) . . ? C35 C34 C39 119.7(4) . . ? C35 C34 C33 122.5(4) . . ? C39 C34 C33 117.7(4) . . ? C34 C35 C36 119.8(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C37 C36 C35 120.3(5) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 120.4(5) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C34 119.9(5) . . ? C38 C39 H39 120.1 . . ? C34 C39 H39 120.1 . . ? O6 C40 N8 121.3(4) . . ? O6 C40 C41 122.0(4) . . ? N8 C40 C41 116.7(4) . . ? C46 C41 C42 120.2(4) . . ? C46 C41 C40 119.0(4) . . ? C42 C41 C40 120.8(4) . . ? C43 C42 C41 118.4(5) . . ? C43 C42 H42 120.8 . . ? C41 C42 H42 120.8 . . ? C44 C43 C42 120.8(5) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 120.4(5) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C41 C46 C45 120.4(5) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? O7 C47 C48 121.5(4) . . ? O7 C47 C52 120.2(4) . . ? C48 C47 C52 118.3(4) . . ? C49 C48 C47 119.9(4) . . ? C49 C48 C54 118.7(4) . . ? C47 C48 C54 121.4(4) . . ? C48 C49 C50 122.7(5) . . ? C48 C49 H49 118.6 . . ? C50 C49 H49 118.6 . . ? C49 C50 C51 116.6(5) . . ? C49 C50 C53 122.6(5) . . ? C51 C50 C53 120.8(5) . . ? C52 C51 C50 122.7(5) . . ? C52 C51 H51 118.6 . . ? C50 C51 H51 118.6 . . ? C51 C52 C47 119.7(4) . . ? C51 C52 C55 117.7(4) . . ? C47 C52 C55 122.5(4) . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N9 C54 C48 122.7(4) . . ? N9 C54 H54 118.6 . . ? C48 C54 H54 118.6 . . ? N11 C55 C52 123.9(4) . . ? N11 C55 H55 118.1 . . ? C52 C55 H55 118.1 . . ? O8 C56 N10 120.0(4) . . ? O8 C56 C57 121.4(4) . . ? N10 C56 C57 118.5(4) . . ? C62 C57 C58 120.0(4) . . ? C62 C57 C56 117.6(4) . . ? C58 C57 C56 122.4(4) . . ? C59 C58 C57 119.2(5) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C60 C59 C58 120.4(5) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C61 120.6(5) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C60 C61 C62 119.8(5) . . ? C60 C61 H61 120.1 . . ? C62 C61 H61 120.1 . . ? C57 C62 C61 120.1(5) . . ? C57 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? O9 C63 N12 120.6(4) . . ? O9 C63 C64 120.0(5) . . ? N12 C63 C64 119.5(5) . . ? C69 C64 C65 120.5(5) . . ? C69 C64 C63 117.6(5) . . ? C65 C64 C63 121.9(5) . . ? C66 C65 C64 118.2(6) . . ? C66 C65 H65 120.9 . . ? C64 C65 H65 120.9 . . ? C67 C66 C65 121.2(7) . . ? C67 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? C68 C67 C66 120.4(6) . . ? C68 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C67 C68 C69 120.6(7) . . ? C67 C68 H68 119.7 . . ? C69 C68 H68 119.7 . . ? C64 C69 C68 119.2(6) . . ? C64 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? O10 C70 H70A 109.5 . . ? O10 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O10 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O11 C71 H71A 109.5 . . ? O11 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O11 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O12 C72 H72A 109.5 . . ? O12 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? O12 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O13 C73 H73A 109.5 . . ? O13 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? O13 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? O14 C74 H74A 109.5 . . ? O14 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? O14 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O15 C75 H75A 109.5 . . ? O15 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? O15 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.574 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.120 # Attachment 'web_deposit_cif_file_1_JinkuiTang_1303180583.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 772952' #TrackingRef 'web_deposit_cif_file_1_JinkuiTang_1303180583.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H81 Cl3 N12 O27 Tb2' _chemical_formula_weight 2006.71 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.6371(9) _cell_length_b 16.7291(6) _cell_length_c 19.9998(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.2000(10) _cell_angle_gamma 90.00 _cell_volume 8241.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.07 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4048 _exptl_absorpt_coefficient_mu 1.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7158 _exptl_absorpt_correction_T_max 0.8053 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45300 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.83 _diffrn_reflns_theta_max 26.07 _reflns_number_total 16290 _reflns_number_gt 13255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+16.8816P] 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 16290 _refine_ls_number_parameters 1085 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.003 _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 Tb1 Tb 0.309796(6) 0.470923(10) 0.337841(7) 0.01867(5) Uani 1 1 d . . . Tb2 Tb 0.173586(6) 0.533478(9) 0.342600(7) 0.01801(5) Uani 1 1 d . . . Cl1 Cl 0.09136(4) 0.76015(6) 0.08568(5) 0.0396(2) Uani 1 1 d . . . Cl2 Cl 0.24671(5) 0.59971(8) 0.02198(5) 0.0476(3) Uani 1 1 d . . . Cl3 Cl 0.38161(5) 0.35095(7) 0.04179(5) 0.0446(3) Uani 1 1 d . . . N1 N 0.19545(11) 0.63115(17) 0.43963(14) 0.0219(6) Uani 1 1 d . . . N2 N 0.18347(11) 0.71002(17) 0.42427(14) 0.0230(6) Uani 1 1 d . . . H2H H 0.1950 0.7497 0.4497 0.028 Uiso 1 1 calc R . . N3 N 0.29125(11) 0.34334(17) 0.40917(14) 0.0217(6) Uani 1 1 d . . . N4 N 0.30871(12) 0.27357(17) 0.37849(14) 0.0249(6) Uani 1 1 d . . . H4H H 0.3026 0.2262 0.3958 0.030 Uiso 1 1 calc R . . N6 N 0.37648(12) 0.5788(2) 0.45876(14) 0.0290(7) Uani 1 1 d . . . H6H H 0.3864 0.6158 0.4878 0.035 Uiso 1 1 calc R . . N5 N 0.34438(11) 0.59655(18) 0.40271(14) 0.0238(6) Uani 1 1 d . . . N8 N 0.14547(11) 0.55074(18) 0.17461(14) 0.0245(6) Uani 1 1 d . . . H8H H 0.1480 0.5577 0.1312 0.029 Uiso 1 1 calc R . . N7 N 0.18102(11) 0.58712(17) 0.21937(13) 0.0213(6) Uani 1 1 d . . . N10 N 0.34538(12) 0.51476(19) 0.17779(15) 0.0272(7) Uani 1 1 d . . . H10H H 0.3459 0.5224 0.1343 0.033 Uiso 1 1 calc R . . N9 N 0.30538(11) 0.46838(18) 0.20655(14) 0.0237(6) Uani 1 1 d . . . N12 N 0.10446(12) 0.38127(18) 0.41858(14) 0.0255(6) Uani 1 1 d . . . H12H H 0.0908 0.3349 0.4305 0.031 Uiso 1 1 calc R . . N11 N 0.13575(11) 0.38947(17) 0.36231(14) 0.0233(6) Uani 1 1 d . . . O1 O 0.24196(9) 0.48724(14) 0.41637(11) 0.0210(5) Uani 1 1 d . . . O2 O 0.34359(10) 0.34964(15) 0.29729(12) 0.0295(6) Uani 1 1 d . . . O3 O 0.13929(10) 0.66578(15) 0.33227(12) 0.0271(5) Uani 1 1 d . . . O4 O 0.25868(9) 0.58449(14) 0.31483(11) 0.0212(5) Uani 1 1 d . . . O5 O 0.37486(10) 0.45116(16) 0.42565(13) 0.0290(6) Uani 1 1 d . . . O6 O 0.10326(9) 0.49790(15) 0.26257(12) 0.0253(5) Uani 1 1 d . . . O7 O 0.22520(9) 0.43203(14) 0.29262(11) 0.0210(5) Uani 1 1 d . . . O8 O 0.38174(10) 0.53694(15) 0.28002(12) 0.0262(5) Uani 1 1 d . . . O9 O 0.11653(9) 0.51252(14) 0.43511(12) 0.0238(5) Uani 1 1 d . . . O11 O 0.42209(16) 0.8338(2) 0.43558(19) 0.0666(10) Uani 1 1 d . . . H11 H 0.4521 0.8322 0.4165 0.100 Uiso 1 1 calc R . . O12 O 0.49887(17) 0.8313(3) 0.3386(2) 0.0804(12) Uani 1 1 d . . . H12 H 0.5265 0.8356 0.3637 0.121 Uiso 1 1 calc R . . O13 O 0.9868(2) 0.6295(3) 0.1364(3) 0.0997(16) Uani 1 1 d . . . H13 H 0.9680 0.6634 0.1155 0.150 Uiso 1 1 calc R . . O14 O 0.08297(14) 0.2199(2) 0.43579(18) 0.0561(9) Uani 1 1 d . . . H14 H 0.0624 0.2046 0.4043 0.084 Uiso 1 1 calc R . . O15 O 0.26607(13) 0.13277(18) 0.43099(17) 0.0493(8) Uani 1 1 d . . . H15H H 0.2864 0.1076 0.4579 0.074 Uiso 1 1 calc R . . O16 O 0.09028(14) 0.7790(2) 0.01611(15) 0.0562(9) Uani 1 1 d . . . O17 O 0.13881(14) 0.7930(2) 0.11699(16) 0.0602(9) Uani 1 1 d . . . O18 O 0.08983(14) 0.6754(2) 0.0944(2) 0.0659(10) Uani 1 1 d . . . O19 O 0.04385(15) 0.7949(2) 0.11547(18) 0.0635(10) Uani 1 1 d . . . O20 O 0.20271(16) 0.5491(2) 0.03997(17) 0.0606(9) Uani 1 1 d . . . O21 O 0.22859(16) 0.6818(2) 0.02529(19) 0.0706(11) Uani 1 1 d . . . O22 O 0.26347(17) 0.5825(4) -0.04310(19) 0.1052(18) Uani 1 1 d . . . O23 O 0.29067(16) 0.5909(2) 0.06937(18) 0.0706(11) Uani 1 1 d . . . O24 O 0.3378(2) 0.2992(3) 0.0620(3) 0.1144(18) Uani 1 1 d . . . O25 O 0.3558(2) 0.4213(3) 0.0198(3) 0.0986(16) Uani 1 1 d . . . O26 O 0.4073(3) 0.3076(4) -0.0018(4) 0.193(4) Uani 1 1 d . . . O27 O 0.4040(3) 0.3719(4) 0.1021(4) 0.171(3) Uani 1 1 d . . . C70 C 0.3648(3) 0.7361(4) 0.5728(3) 0.084(2) Uani 1 1 d . . . H70A H 0.3795 0.7722 0.6072 0.125 Uiso 1 1 calc R . . H70B H 0.3509 0.6876 0.5940 0.125 Uiso 1 1 calc R . . H70C H 0.3352 0.7628 0.5480 0.125 Uiso 1 1 calc R . . C1 C 0.24102(13) 0.4761(2) 0.48176(16) 0.0212(7) Uani 1 1 d . . . C2 C 0.25694(14) 0.4024(2) 0.50982(16) 0.0229(7) Uani 1 1 d . . . C3 C 0.25292(15) 0.3900(2) 0.57889(17) 0.0274(8) Uani 1 1 d . . . H3 H 0.2628 0.3394 0.5971 0.033 Uiso 1 1 calc R . . C4 C 0.23489(15) 0.4495(2) 0.62149(17) 0.0290(8) Uani 1 1 d . . . C5 C 0.22152(15) 0.5228(2) 0.59391(17) 0.0270(8) Uani 1 1 d . . . H5 H 0.2101 0.5645 0.6226 0.032 Uiso 1 1 calc R . . C6 C 0.22421(14) 0.5376(2) 0.52519(17) 0.0233(7) Uani 1 1 d . . . C7 C 0.22904(19) 0.4331(3) 0.69548(18) 0.0403(10) Uani 1 1 d . . . H7A H 0.2157 0.4813 0.7177 0.060 Uiso 1 1 calc R . . H7B H 0.2644 0.4182 0.7150 0.060 Uiso 1 1 calc R . . H7C H 0.2032 0.3893 0.7016 0.060 Uiso 1 1 calc R . . C8 C 0.27599(14) 0.3358(2) 0.46968(17) 0.0250(7) Uani 1 1 d . . . H8 H 0.2772 0.2842 0.4894 0.030 Uiso 1 1 calc R . . C9 C 0.20935(14) 0.6170(2) 0.50104(17) 0.0247(7) Uani 1 1 d . . . H9 H 0.2099 0.6602 0.5319 0.030 Uiso 1 1 calc R . . C11 C 0.35348(15) 0.2095(2) 0.28645(19) 0.0301(8) Uani 1 1 d . . . C12 C 0.36753(17) 0.1394(2) 0.3198(2) 0.0394(10) Uani 1 1 d . . . H12A H 0.3657 0.1362 0.3671 0.047 Uiso 1 1 calc R . . C13 C 0.3843(2) 0.0744(3) 0.2826(3) 0.0541(13) Uani 1 1 d . . . H13A H 0.3943 0.0262 0.3047 0.065 Uiso 1 1 calc R . . C14 C 0.3867(2) 0.0792(3) 0.2142(3) 0.0598(15) Uani 1 1 d . . . H14A H 0.3979 0.0340 0.1894 0.072 Uiso 1 1 calc R . . C15 C 0.3731(2) 0.1479(3) 0.1815(2) 0.0538(13) Uani 1 1 d . . . H15 H 0.3750 0.1504 0.1342 0.065 Uiso 1 1 calc R . . C16 C 0.35665(17) 0.2142(3) 0.2173(2) 0.0404(10) Uani 1 1 d . . . H16 H 0.3476 0.2625 0.1947 0.049 Uiso 1 1 calc R . . C10 C 0.33526(14) 0.2822(2) 0.32135(17) 0.0248(7) Uani 1 1 d . . . C18 C 0.13980(14) 0.8061(2) 0.35128(18) 0.0249(8) Uani 1 1 d . . . C19 C 0.13461(15) 0.8661(2) 0.3992(2) 0.0315(8) Uani 1 1 d . . . H19 H 0.1396 0.8539 0.4453 0.038 Uiso 1 1 calc R . . C20 C 0.12219(17) 0.9430(3) 0.3795(2) 0.0421(10) Uani 1 1 d . . . H20 H 0.1184 0.9838 0.4121 0.050 Uiso 1 1 calc R . . C21 C 0.11531(19) 0.9609(3) 0.3125(3) 0.0486(12) Uani 1 1 d . . . H21 H 0.1070 1.0141 0.2992 0.058 Uiso 1 1 calc R . . C22 C 0.12042(18) 0.9019(3) 0.2646(2) 0.0435(10) Uani 1 1 d . . . H22 H 0.1158 0.9146 0.2185 0.052 Uiso 1 1 calc R . . C23 C 0.13217(16) 0.8248(2) 0.2839(2) 0.0337(9) Uani 1 1 d . . . H23 H 0.1351 0.7841 0.2511 0.040 Uiso 1 1 calc R . . C17 C 0.15353(13) 0.7230(2) 0.36897(17) 0.0225(7) Uani 1 1 d . . . C24 C 0.27319(13) 0.6558(2) 0.29293(17) 0.0216(7) Uani 1 1 d . . . C25 C 0.31347(14) 0.7010(2) 0.32746(18) 0.0262(8) Uani 1 1 d . . . C26 C 0.32755(16) 0.7761(2) 0.3040(2) 0.0391(10) Uani 1 1 d . . . H26 H 0.3537 0.8065 0.3285 0.047 Uiso 1 1 calc R . . C27 C 0.30476(17) 0.8086(2) 0.2458(2) 0.0419(11) Uani 1 1 d . . . C28 C 0.26610(16) 0.7635(2) 0.2122(2) 0.0360(9) Uani 1 1 d . . . H28 H 0.2503 0.7842 0.1721 0.043 Uiso 1 1 calc R . . C29 C 0.24918(14) 0.6887(2) 0.23449(17) 0.0241(7) Uani 1 1 d . . . C30 C 0.3221(2) 0.8901(3) 0.2221(3) 0.0747(19) Uani 1 1 d . . . H30A H 0.3048 0.9014 0.1785 0.112 Uiso 1 1 calc R . . H30B H 0.3616 0.8914 0.2180 0.112 Uiso 1 1 calc R . . H30C H 0.3110 0.9306 0.2545 0.112 Uiso 1 1 calc R . . C31 C 0.34246(14) 0.6705(2) 0.38608(18) 0.0276(8) Uani 1 1 d . . . H31 H 0.3612 0.7078 0.4139 0.033 Uiso 1 1 calc R . . C32 C 0.20811(14) 0.6459(2) 0.19569(17) 0.0238(7) Uani 1 1 d . . . H32 H 0.2010 0.6620 0.1508 0.029 Uiso 1 1 calc R . . C34 C 0.42914(14) 0.4803(3) 0.52225(19) 0.0347(10) Uani 1 1 d . . . C35 C 0.45313(16) 0.5369(3) 0.5648(2) 0.0436(11) Uani 1 1 d . . . H35 H 0.4437 0.5919 0.5611 0.052 Uiso 1 1 calc R . . C36 C 0.49108(17) 0.5115(4) 0.6127(2) 0.0594(16) Uani 1 1 d . . . H36 H 0.5079 0.5495 0.6418 0.071 Uiso 1 1 calc R . . C37 C 0.50447(18) 0.4326(4) 0.6184(2) 0.0671(19) Uani 1 1 d . . . H37 H 0.5307 0.4162 0.6511 0.080 Uiso 1 1 calc R . . C38 C 0.48055(18) 0.3771(4) 0.5777(2) 0.0572(15) Uani 1 1 d . . . H38 H 0.4898 0.3223 0.5826 0.069 Uiso 1 1 calc R . . C39 C 0.44241(16) 0.4003(3) 0.5287(2) 0.0428(11) Uani 1 1 d . . . H39 H 0.4258 0.3616 0.5001 0.051 Uiso 1 1 calc R . . C33 C 0.39133(14) 0.5027(2) 0.46611(17) 0.0270(8) Uani 1 1 d . . . C41 C 0.07091(14) 0.4587(2) 0.15411(18) 0.0261(8) Uani 1 1 d . . . C42 C 0.07079(17) 0.4705(3) 0.0849(2) 0.0388(10) Uani 1 1 d . . . H42 H 0.0931 0.5105 0.0660 0.047 Uiso 1 1 calc R . . C43 C 0.03774(18) 0.4230(3) 0.0441(2) 0.0465(11) Uani 1 1 d . . . H43 H 0.0369 0.4313 -0.0029 0.056 Uiso 1 1 calc R . . C44 C 0.00616(17) 0.3639(3) 0.0715(2) 0.0445(11) Uani 1 1 d . . . H44 H -0.0152 0.3304 0.0431 0.053 Uiso 1 1 calc R . . C45 C 0.00544(16) 0.3532(3) 0.1397(2) 0.0436(11) Uani 1 1 d . . . H45 H -0.0170 0.3133 0.1584 0.052 Uiso 1 1 calc R . . C46 C 0.03769(15) 0.4010(3) 0.1809(2) 0.0345(9) Uani 1 1 d . . . H46 H 0.0369 0.3940 0.2280 0.041 Uiso 1 1 calc R . . C40 C 0.10702(13) 0.5044(2) 0.20035(17) 0.0233(7) Uani 1 1 d . . . C47 C 0.20766(13) 0.3814(2) 0.24640(16) 0.0217(7) Uani 1 1 d . . . C48 C 0.23075(13) 0.3783(2) 0.18225(17) 0.0226(7) Uani 1 1 d . . . C49 C 0.20882(15) 0.3277(2) 0.13317(18) 0.0290(8) Uani 1 1 d . . . H49 H 0.2237 0.3286 0.0898 0.035 Uiso 1 1 calc R . . C50 C 0.16605(14) 0.2761(2) 0.14544(18) 0.0282(8) Uani 1 1 d . . . C51 C 0.14539(14) 0.2767(2) 0.20952(19) 0.0294(8) Uani 1 1 d . . . H51 H 0.1173 0.2400 0.2198 0.035 Uiso 1 1 calc R . . C52 C 0.16393(14) 0.3287(2) 0.25931(18) 0.0248(7) Uani 1 1 d . . . C53 C 0.14061(16) 0.2242(3) 0.0914(2) 0.0409(10) Uani 1 1 d . . . H53A H 0.1060 0.2478 0.0764 0.061 Uiso 1 1 calc R . . H53B H 0.1341 0.1706 0.1093 0.061 Uiso 1 1 calc R . . H53C H 0.1651 0.2207 0.0536 0.061 Uiso 1 1 calc R . . C54 C 0.27531(14) 0.4302(2) 0.16414(17) 0.0247(7) Uani 1 1 d . . . H54 H 0.2827 0.4362 0.1180 0.030 Uiso 1 1 calc R . . C55 C 0.13507(14) 0.3297(2) 0.32169(18) 0.0261(8) Uani 1 1 d . . . H55 H 0.1146 0.2838 0.3333 0.031 Uiso 1 1 calc R . . C57 C 0.42515(14) 0.5963(2) 0.18670(18) 0.0281(8) Uani 1 1 d . . . C58 C 0.44344(16) 0.5794(3) 0.1222(2) 0.0379(10) Uani 1 1 d . . . H58 H 0.4284 0.5361 0.0974 0.045 Uiso 1 1 calc R . . C59 C 0.48365(17) 0.6265(3) 0.0952(2) 0.0444(11) Uani 1 1 d . . . H59 H 0.4964 0.6148 0.0517 0.053 Uiso 1 1 calc R . . C60 C 0.50538(18) 0.6898(3) 0.1302(2) 0.0486(12) Uani 1 1 d . . . H60 H 0.5325 0.7222 0.1107 0.058 Uiso 1 1 calc R . . C61 C 0.48774(18) 0.7063(3) 0.1937(2) 0.0480(12) Uani 1 1 d . . . H61 H 0.5030 0.7498 0.2181 0.058 Uiso 1 1 calc R . . C62 C 0.44778(16) 0.6595(3) 0.2222(2) 0.0356(9) Uani 1 1 d . . . H62 H 0.4360 0.6709 0.2661 0.043 Uiso 1 1 calc R . . C56 C 0.38288(14) 0.5472(2) 0.21831(17) 0.0240(7) Uani 1 1 d . . . C64 C 0.06280(13) 0.4432(2) 0.51436(17) 0.0237(7) Uani 1 1 d . . . C65 C 0.02761(14) 0.3801(2) 0.52599(19) 0.0287(8) Uani 1 1 d . . . H65 H 0.0248 0.3372 0.4950 0.034 Uiso 1 1 calc R . . C66 C -0.00339(15) 0.3799(3) 0.5829(2) 0.0343(9) Uani 1 1 d . . . H66 H -0.0276 0.3370 0.5908 0.041 Uiso 1 1 calc R . . C67 C 0.00076(15) 0.4418(3) 0.62822(19) 0.0350(9) Uani 1 1 d . . . H67 H -0.0205 0.4412 0.6673 0.042 Uiso 1 1 calc R . . C68 C 0.03581(16) 0.5048(3) 0.61680(19) 0.0361(9) Uani 1 1 d . . . H68 H 0.0388 0.5472 0.6483 0.043 Uiso 1 1 calc R . . C69 C 0.06647(15) 0.5063(2) 0.55967(19) 0.0311(8) Uani 1 1 d . . . H69 H 0.0899 0.5501 0.5514 0.037 Uiso 1 1 calc R . . C63 C 0.09612(13) 0.4483(2) 0.45383(17) 0.0229(7) Uani 1 1 d . . . O10 O 0.40551(15) 0.7157(2) 0.52910(16) 0.0543(9) Uani 1 1 d . . . H10 H 0.4155 0.7566 0.5084 0.081 Uiso 1 1 calc R . . C71 C 0.4051(3) 0.9146(4) 0.4415(3) 0.0725(17) Uani 1 1 d . . . H71A H 0.3804 0.9196 0.4791 0.109 Uiso 1 1 calc R . . H71B H 0.3863 0.9312 0.4002 0.109 Uiso 1 1 calc R . . H71C H 0.4369 0.9488 0.4495 0.109 Uiso 1 1 calc R . . C72 C 0.4984(3) 0.8948(4) 0.2904(3) 0.087(2) Uani 1 1 d . . . H72A H 0.4952 0.9462 0.3135 0.131 Uiso 1 1 calc R . . H72B H 0.4675 0.8878 0.2594 0.131 Uiso 1 1 calc R . . H72C H 0.5322 0.8937 0.2655 0.131 Uiso 1 1 calc R . . C73 C 0.9899(3) 0.6508(6) 0.2064(4) 0.122(3) Uani 1 1 d . . . H73A H 1.0253 0.6350 0.2253 0.182 Uiso 1 1 calc R . . H73B H 0.9611 0.6232 0.2303 0.182 Uiso 1 1 calc R . . H73C H 0.9853 0.7087 0.2111 0.182 Uiso 1 1 calc R . . C74 C 0.1324(2) 0.1736(4) 0.4360(3) 0.0793(18) Uani 1 1 d . . . H74A H 0.1637 0.2098 0.4361 0.119 Uiso 1 1 calc R . . H74B H 0.1329 0.1398 0.3961 0.119 Uiso 1 1 calc R . . H74C H 0.1341 0.1399 0.4761 0.119 Uiso 1 1 calc R . . C75 C 0.2446(3) 0.0785(4) 0.3811(3) 0.0818(19) Uani 1 1 d . . . H75A H 0.2158 0.0460 0.4004 0.123 Uiso 1 1 calc R . . H75B H 0.2737 0.0435 0.3657 0.123 Uiso 1 1 calc R . . H75C H 0.2298 0.1091 0.3431 0.123 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 Tb1 0.01847(8) 0.02144(9) 0.01608(8) 0.00161(6) -0.00049(6) 0.00167(6) Tb2 0.01811(8) 0.01957(9) 0.01628(8) -0.00194(6) -0.00146(6) 0.00061(6) Cl1 0.0418(6) 0.0387(6) 0.0385(5) 0.0101(4) 0.0055(4) 0.0014(4) Cl2 0.0500(6) 0.0616(7) 0.0307(5) 0.0085(5) -0.0079(5) 0.0083(6) Cl3 0.0509(6) 0.0441(6) 0.0387(6) -0.0066(5) -0.0012(5) 0.0014(5) N1 0.0221(14) 0.0214(15) 0.0221(15) -0.0033(12) -0.0008(12) -0.0001(12) N2 0.0257(15) 0.0177(15) 0.0254(15) -0.0043(12) -0.0034(12) 0.0014(12) N3 0.0237(15) 0.0219(15) 0.0197(15) -0.0011(11) 0.0021(11) 0.0030(12) N4 0.0299(16) 0.0190(15) 0.0261(16) -0.0004(12) 0.0037(13) 0.0025(12) N6 0.0256(16) 0.041(2) 0.0197(15) 0.0003(13) -0.0084(12) -0.0040(14) N5 0.0199(14) 0.0311(17) 0.0203(14) -0.0017(12) -0.0043(11) 0.0001(13) N8 0.0267(16) 0.0286(17) 0.0180(14) -0.0001(12) -0.0072(12) -0.0027(13) N7 0.0220(14) 0.0218(15) 0.0198(14) -0.0018(11) -0.0048(11) 0.0003(12) N10 0.0251(15) 0.0381(19) 0.0184(15) 0.0052(13) 0.0015(12) -0.0053(13) N9 0.0218(14) 0.0287(16) 0.0206(15) 0.0039(12) 0.0024(12) -0.0007(12) N12 0.0285(16) 0.0247(16) 0.0236(15) 0.0002(12) 0.0076(12) -0.0017(13) N11 0.0232(15) 0.0259(16) 0.0208(15) -0.0013(12) 0.0030(12) 0.0006(12) O1 0.0226(12) 0.0240(13) 0.0164(11) 0.0018(9) 0.0000(9) 0.0038(10) O2 0.0361(14) 0.0267(14) 0.0260(13) 0.0029(11) 0.0065(11) 0.0087(11) O3 0.0313(13) 0.0246(14) 0.0251(13) -0.0035(10) -0.0061(10) 0.0063(11) O4 0.0214(12) 0.0225(13) 0.0194(12) 0.0012(9) -0.0032(9) -0.0004(10) O5 0.0246(13) 0.0334(15) 0.0285(14) 0.0083(11) -0.0073(11) -0.0007(11) O6 0.0222(12) 0.0293(14) 0.0242(13) -0.0037(10) -0.0024(10) -0.0013(10) O7 0.0234(12) 0.0207(12) 0.0190(12) -0.0047(9) -0.0001(9) -0.0002(10) O8 0.0252(13) 0.0329(14) 0.0203(13) 0.0039(10) -0.0009(10) -0.0021(11) O9 0.0220(12) 0.0240(13) 0.0254(13) -0.0022(10) 0.0023(10) -0.0023(10) O11 0.083(3) 0.062(2) 0.055(2) -0.0035(18) -0.004(2) -0.017(2) O12 0.078(3) 0.098(3) 0.065(3) 0.009(2) -0.007(2) -0.006(2) O13 0.088(3) 0.076(3) 0.135(5) 0.042(3) 0.001(3) 0.000(3) O14 0.068(2) 0.0398(19) 0.061(2) 0.0014(16) 0.0144(18) 0.0001(17) O15 0.052(2) 0.0385(18) 0.058(2) 0.0070(15) -0.0008(15) -0.0104(15) O16 0.065(2) 0.067(2) 0.0357(17) 0.0093(16) -0.0035(15) 0.0015(18) O17 0.059(2) 0.075(3) 0.046(2) 0.0046(18) -0.0077(16) -0.0112(19) O18 0.061(2) 0.039(2) 0.098(3) 0.0204(19) 0.014(2) 0.0113(17) O19 0.069(2) 0.052(2) 0.071(2) 0.0070(18) 0.0271(19) 0.0156(18) O20 0.078(3) 0.055(2) 0.050(2) 0.0057(16) 0.0060(18) -0.0098(19) O21 0.081(3) 0.052(2) 0.078(3) 0.0284(19) -0.030(2) 0.0061(19) O22 0.067(3) 0.203(6) 0.045(2) -0.018(3) 0.007(2) 0.007(3) O23 0.080(3) 0.067(3) 0.064(2) 0.0066(19) -0.039(2) 0.021(2) O24 0.117(4) 0.088(4) 0.140(5) 0.000(3) 0.048(3) -0.037(3) O25 0.122(4) 0.055(3) 0.117(4) 0.025(3) -0.035(3) -0.008(3) O26 0.270(8) 0.099(5) 0.217(7) -0.025(4) 0.190(7) 0.019(5) O27 0.181(6) 0.159(6) 0.167(6) -0.042(5) -0.112(5) 0.003(5) C70 0.074(4) 0.072(4) 0.105(5) -0.035(4) 0.002(4) -0.006(3) C1 0.0186(16) 0.0271(19) 0.0180(16) 0.0000(14) -0.0018(13) -0.0018(14) C2 0.0246(17) 0.0243(18) 0.0199(17) 0.0003(14) 0.0012(14) -0.0023(14) C3 0.034(2) 0.028(2) 0.0202(18) 0.0043(14) 0.0011(15) -0.0004(16) C4 0.034(2) 0.035(2) 0.0175(18) 0.0020(15) 0.0000(15) -0.0025(17) C5 0.0316(19) 0.033(2) 0.0164(17) -0.0046(15) 0.0006(14) -0.0004(16) C6 0.0239(17) 0.0267(19) 0.0191(17) -0.0017(14) -0.0019(14) -0.0007(14) C7 0.061(3) 0.040(2) 0.0202(19) 0.0043(17) 0.0066(18) 0.003(2) C8 0.0277(18) 0.0236(18) 0.0235(18) 0.0032(14) -0.0029(14) -0.0008(15) C9 0.0250(18) 0.0282(19) 0.0209(17) -0.0059(14) 0.0002(14) 0.0011(15) C11 0.0250(19) 0.029(2) 0.037(2) -0.0076(16) 0.0071(16) 0.0000(15) C12 0.038(2) 0.030(2) 0.050(3) -0.0027(19) 0.0121(19) 0.0030(18) C13 0.055(3) 0.026(2) 0.082(4) -0.002(2) 0.028(3) 0.004(2) C14 0.061(3) 0.035(3) 0.085(4) -0.026(3) 0.045(3) -0.011(2) C15 0.061(3) 0.053(3) 0.049(3) -0.024(2) 0.033(2) -0.012(2) C16 0.040(2) 0.043(3) 0.039(2) -0.0076(19) 0.0160(19) -0.0001(19) C10 0.0244(18) 0.028(2) 0.0221(18) 0.0000(15) -0.0018(14) 0.0033(15) C18 0.0220(17) 0.0230(19) 0.0296(19) 0.0012(15) -0.0021(14) 0.0030(14) C19 0.030(2) 0.027(2) 0.037(2) -0.0041(16) -0.0051(16) 0.0022(16) C20 0.038(2) 0.027(2) 0.061(3) -0.007(2) -0.006(2) 0.0017(18) C21 0.050(3) 0.023(2) 0.073(3) 0.012(2) -0.005(2) 0.0041(19) C22 0.045(2) 0.041(3) 0.045(3) 0.013(2) -0.005(2) 0.006(2) C23 0.036(2) 0.032(2) 0.032(2) 0.0022(17) -0.0019(17) 0.0051(17) C17 0.0190(16) 0.0252(19) 0.0234(18) -0.0013(14) 0.0013(14) 0.0036(14) C24 0.0202(16) 0.0184(17) 0.0262(18) -0.0008(14) -0.0015(14) 0.0027(13) C25 0.0258(18) 0.0235(19) 0.0290(19) -0.0014(15) -0.0057(15) 0.0008(15) C26 0.036(2) 0.025(2) 0.056(3) -0.0011(18) -0.017(2) -0.0051(17) C27 0.042(2) 0.028(2) 0.055(3) 0.0128(19) -0.018(2) -0.0065(18) C28 0.038(2) 0.026(2) 0.043(2) 0.0105(17) -0.0143(18) -0.0009(17) C29 0.0244(18) 0.0228(18) 0.0249(18) 0.0017(14) -0.0033(14) 0.0006(14) C30 0.080(4) 0.037(3) 0.106(5) 0.031(3) -0.052(3) -0.025(3) C31 0.0256(18) 0.029(2) 0.0277(19) -0.0053(15) -0.0077(15) -0.0039(15) C32 0.0257(18) 0.0255(19) 0.0199(17) 0.0029(14) -0.0051(14) 0.0028(15) C34 0.0200(18) 0.062(3) 0.0222(19) 0.0173(18) -0.0013(15) -0.0053(18) C35 0.024(2) 0.082(4) 0.024(2) 0.011(2) -0.0029(16) -0.007(2) C36 0.027(2) 0.129(5) 0.022(2) 0.019(3) -0.0057(17) -0.015(3) C37 0.028(2) 0.138(6) 0.035(3) 0.046(3) -0.006(2) -0.005(3) C38 0.033(2) 0.087(4) 0.052(3) 0.046(3) 0.001(2) 0.005(2) C39 0.028(2) 0.066(3) 0.035(2) 0.027(2) -0.0021(17) -0.002(2) C33 0.0165(16) 0.044(2) 0.0208(18) 0.0113(16) -0.0023(14) -0.0020(16) C41 0.0196(17) 0.029(2) 0.0291(19) -0.0045(15) -0.0058(14) 0.0049(15) C42 0.041(2) 0.043(2) 0.032(2) -0.0037(18) -0.0072(18) -0.0061(19) C43 0.047(3) 0.058(3) 0.034(2) -0.013(2) -0.012(2) -0.006(2) C44 0.031(2) 0.052(3) 0.049(3) -0.022(2) -0.0136(19) -0.004(2) C45 0.029(2) 0.048(3) 0.054(3) -0.011(2) -0.0014(19) -0.0126(19) C46 0.0241(19) 0.044(2) 0.035(2) -0.0060(18) -0.0052(16) -0.0048(17) C40 0.0208(17) 0.0244(18) 0.0244(19) -0.0032(14) -0.0032(14) 0.0060(14) C47 0.0221(17) 0.0211(18) 0.0217(17) -0.0034(13) -0.0017(13) 0.0057(14) C48 0.0220(17) 0.0239(18) 0.0220(17) -0.0037(14) -0.0015(14) 0.0021(14) C49 0.031(2) 0.035(2) 0.0207(18) -0.0086(15) -0.0007(15) 0.0049(16) C50 0.0242(18) 0.031(2) 0.030(2) -0.0118(16) -0.0026(15) 0.0016(15) C51 0.0225(18) 0.028(2) 0.037(2) -0.0112(16) 0.0023(16) -0.0011(15) C52 0.0240(18) 0.0226(18) 0.0280(19) -0.0055(14) 0.0023(14) 0.0009(14) C53 0.032(2) 0.050(3) 0.041(2) -0.023(2) -0.0048(18) -0.0024(19) C54 0.0275(18) 0.030(2) 0.0165(17) -0.0010(14) -0.0001(14) 0.0021(15) C55 0.0253(18) 0.0229(19) 0.030(2) -0.0021(15) 0.0029(15) -0.0046(15) C57 0.0232(18) 0.037(2) 0.0244(18) 0.0093(16) -0.0024(14) -0.0005(16) C58 0.033(2) 0.051(3) 0.030(2) 0.0069(19) 0.0018(17) -0.0076(19) C59 0.037(2) 0.065(3) 0.032(2) 0.014(2) 0.0048(18) -0.008(2) C60 0.035(2) 0.065(3) 0.046(3) 0.021(2) 0.005(2) -0.011(2) C61 0.041(2) 0.047(3) 0.056(3) 0.007(2) -0.007(2) -0.016(2) C62 0.033(2) 0.042(2) 0.032(2) 0.0093(18) -0.0025(17) -0.0050(18) C56 0.0231(17) 0.0282(19) 0.0208(18) 0.0041(14) 0.0007(14) 0.0021(14) C64 0.0206(17) 0.0297(19) 0.0207(17) 0.0023(14) -0.0020(14) 0.0042(14) C65 0.0267(19) 0.027(2) 0.032(2) -0.0005(16) 0.0035(15) 0.0033(15) C66 0.0268(19) 0.040(2) 0.036(2) 0.0068(18) 0.0064(16) 0.0025(17) C67 0.028(2) 0.056(3) 0.0218(19) 0.0061(18) 0.0040(15) 0.0076(19) C68 0.032(2) 0.052(3) 0.024(2) -0.0104(18) 0.0006(16) 0.0013(19) C69 0.0277(19) 0.035(2) 0.030(2) -0.0059(16) -0.0009(16) 0.0001(17) C63 0.0194(16) 0.0271(19) 0.0222(17) -0.0003(14) -0.0031(14) 0.0015(14) O10 0.069(2) 0.055(2) 0.0388(18) -0.0123(15) -0.0084(16) -0.0143(18) C71 0.099(5) 0.066(4) 0.053(3) -0.005(3) -0.007(3) -0.001(3) C72 0.109(5) 0.070(4) 0.082(5) 0.002(4) -0.011(4) -0.010(4) C73 0.075(5) 0.190(10) 0.100(6) 0.073(6) 0.031(4) 0.034(5) C74 0.076(4) 0.058(4) 0.104(5) -0.002(3) 0.007(4) 0.015(3) C75 0.073(4) 0.067(4) 0.105(5) -0.009(4) 0.001(4) -0.022(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 Tb1 O4 2.320(2) . ? Tb1 O1 2.333(2) . ? Tb1 O2 2.344(2) . ? Tb1 O7 2.346(2) . ? Tb1 O5 2.376(2) . ? Tb1 O8 2.405(2) . ? Tb1 N5 2.604(3) . ? Tb1 N3 2.613(3) . ? Tb1 N9 2.626(3) . ? Tb1 Tb2 3.5184(2) . ? Tb2 O4 2.341(2) . ? Tb2 O1 2.347(2) . ? Tb2 O7 2.356(2) . ? Tb2 O9 2.373(2) . ? Tb2 O3 2.377(2) . ? Tb2 O6 2.409(2) . ? Tb2 N1 2.585(3) . ? Tb2 N11 2.616(3) . ? Tb2 N7 2.633(3) . ? Cl1 O17 1.425(3) . ? Cl1 O16 1.426(3) . ? Cl1 O18 1.429(3) . ? Cl1 O19 1.446(3) . ? Cl2 O22 1.403(4) . ? Cl2 O20 1.427(4) . ? Cl2 O23 1.432(3) . ? Cl2 O21 1.446(4) . ? Cl3 O26 1.308(5) . ? Cl3 O27 1.361(5) . ? Cl3 O25 1.405(4) . ? Cl3 O24 1.447(5) . ? N1 C9 1.290(4) . ? N1 N2 1.385(4) . ? N2 C17 1.334(4) . ? N3 C8 1.281(4) . ? N3 N4 1.391(4) . ? N4 C10 1.337(4) . ? N6 C33 1.331(5) . ? N6 N5 1.391(4) . ? N5 C31 1.281(5) . ? N8 C40 1.336(5) . ? N8 N7 1.380(4) . ? N7 C32 1.284(4) . ? N10 C56 1.332(5) . ? N10 N9 1.388(4) . ? N9 C54 1.285(4) . ? N12 C63 1.343(4) . ? N12 N11 1.384(4) . ? N11 C55 1.289(4) . ? O1 C1 1.321(4) . ? O2 C10 1.245(4) . ? O3 C17 1.251(4) . ? O4 C24 1.322(4) . ? O5 C33 1.245(5) . ? O6 C40 1.254(4) . ? O7 C47 1.320(4) . ? O8 C56 1.247(4) . ? O9 C63 1.247(4) . ? O11 C71 1.421(7) . ? O12 C72 1.433(7) . ? O13 C73 1.445(9) . ? O14 C74 1.443(6) . ? O15 C75 1.441(7) . ? C70 O10 1.387(7) . ? C1 C2 1.408(5) . ? C1 C6 1.413(5) . ? C2 C3 1.402(5) . ? C2 C8 1.456(5) . ? C3 C4 1.390(5) . ? C4 C5 1.381(5) . ? C4 C7 1.515(5) . ? C5 C6 1.399(5) . ? C6 C9 1.458(5) . ? C11 C12 1.389(6) . ? C11 C16 1.390(6) . ? C11 C10 1.477(5) . ? C12 C13 1.386(6) . ? C13 C14 1.374(7) . ? C14 C15 1.360(7) . ? C15 C16 1.385(6) . ? C18 C23 1.392(5) . ? C18 C19 1.395(5) . ? C18 C17 1.473(5) . ? C19 C20 1.379(6) . ? C20 C21 1.381(7) . ? C21 C22 1.383(7) . ? C22 C23 1.376(6) . ? C24 C29 1.411(5) . ? C24 C25 1.417(5) . ? C25 C26 1.388(5) . ? C25 C31 1.453(5) . ? C26 C27 1.393(6) . ? C27 C28 1.379(6) . ? C27 C30 1.508(6) . ? C28 C29 1.394(5) . ? C29 C32 1.452(5) . ? C34 C39 1.382(6) . ? C34 C35 1.397(6) . ? C34 C33 1.492(5) . ? C35 C36 1.392(6) . ? C36 C37 1.365(9) . ? C37 C38 1.360(8) . ? C38 C39 1.399(6) . ? C41 C46 1.380(5) . ? C41 C42 1.398(5) . ? C41 C40 1.483(5) . ? C42 C43 1.391(6) . ? C43 C44 1.378(7) . ? C44 C45 1.376(6) . ? C45 C46 1.387(5) . ? C47 C48 1.415(5) . ? C47 C52 1.420(5) . ? C48 C49 1.396(5) . ? C48 C54 1.451(5) . ? C49 C50 1.388(5) . ? C50 C51 1.389(5) . ? C50 C53 1.511(5) . ? C51 C52 1.391(5) . ? C52 C55 1.449(5) . ? C57 C62 1.384(6) . ? C57 C58 1.403(5) . ? C57 C56 1.479(5) . ? C58 C59 1.384(6) . ? C59 C60 1.373(7) . ? C60 C61 1.379(7) . ? C61 C62 1.389(6) . ? C64 C65 1.389(5) . ? C64 C69 1.393(5) . ? C64 C63 1.479(5) . ? C65 C66 1.384(5) . ? C66 C67 1.378(6) . ? C67 C68 1.385(6) . ? C68 C69 1.383(5) . ? 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 O4 Tb1 O1 69.17(8) . . ? O4 Tb1 O2 146.65(8) . . ? O1 Tb1 O2 126.78(8) . . ? O4 Tb1 O7 71.13(8) . . ? O1 Tb1 O7 69.45(8) . . ? O2 Tb1 O7 86.89(8) . . ? O4 Tb1 O5 127.99(8) . . ? O1 Tb1 O5 90.02(8) . . ? O2 Tb1 O5 84.05(9) . . ? O7 Tb1 O5 145.73(8) . . ? O4 Tb1 O8 86.04(8) . . ? O1 Tb1 O8 144.62(8) . . ? O2 Tb1 O8 87.73(9) . . ? O7 Tb1 O8 126.84(8) . . ? O5 Tb1 O8 85.80(8) . . ? O4 Tb1 N5 66.95(8) . . ? O1 Tb1 N5 78.56(8) . . ? O2 Tb1 N5 139.12(9) . . ? O7 Tb1 N5 133.99(8) . . ? O5 Tb1 N5 62.31(9) . . ? O8 Tb1 N5 68.42(9) . . ? O4 Tb1 N3 132.60(8) . . ? O1 Tb1 N3 65.93(8) . . ? O2 Tb1 N3 63.21(8) . . ? O7 Tb1 N3 79.62(8) . . ? O5 Tb1 N3 66.78(9) . . ? O8 Tb1 N3 140.96(8) . . ? N5 Tb1 N3 116.52(9) . . ? O4 Tb1 N9 78.70(8) . . ? O1 Tb1 N9 131.28(8) . . ? O2 Tb1 N9 69.37(9) . . ? O7 Tb1 N9 65.94(8) . . ? O5 Tb1 N9 138.59(9) . . ? O8 Tb1 N9 62.75(8) . . ? N5 Tb1 N9 121.17(9) . . ? N3 Tb1 N9 121.91(9) . . ? O4 Tb1 Tb2 41.22(6) . . ? O1 Tb1 Tb2 41.41(5) . . ? O2 Tb1 Tb2 127.78(6) . . ? O7 Tb1 Tb2 41.67(5) . . ? O5 Tb1 Tb2 130.58(6) . . ? O8 Tb1 Tb2 126.11(6) . . ? N5 Tb1 Tb2 92.80(6) . . ? N3 Tb1 Tb2 92.89(6) . . ? N9 Tb1 Tb2 90.71(6) . . ? O4 Tb2 O1 68.58(8) . . ? O4 Tb2 O7 70.60(8) . . ? O1 Tb2 O7 69.06(8) . . ? O4 Tb2 O9 141.89(8) . . ? O1 Tb2 O9 83.70(8) . . ? O7 Tb2 O9 123.93(8) . . ? O4 Tb2 O3 87.62(8) . . ? O1 Tb2 O3 127.65(8) . . ? O7 Tb2 O3 145.91(8) . . ? O9 Tb2 O3 89.43(8) . . ? O4 Tb2 O6 124.59(8) . . ? O1 Tb2 O6 146.42(8) . . ? O7 Tb2 O6 85.83(8) . . ? O9 Tb2 O6 92.98(8) . . ? O3 Tb2 O6 85.57(8) . . ? O4 Tb2 N1 76.95(8) . . ? O1 Tb2 N1 66.48(8) . . ? O7 Tb2 N1 131.92(8) . . ? O9 Tb2 N1 68.01(8) . . ? O3 Tb2 N1 62.92(8) . . ? O6 Tb2 N1 142.25(8) . . ? O4 Tb2 N11 134.04(8) . . ? O1 Tb2 N11 81.67(8) . . ? O7 Tb2 N11 66.28(8) . . ? O9 Tb2 N11 61.82(8) . . ? O3 Tb2 N11 138.04(9) . . ? O6 Tb2 N11 67.60(9) . . ? N1 Tb2 N11 122.57(9) . . ? O4 Tb2 N7 64.75(8) . . ? O1 Tb2 N7 129.62(8) . . ? O7 Tb2 N7 78.44(8) . . ? O9 Tb2 N7 146.53(8) . . ? O3 Tb2 N7 68.46(8) . . ? O6 Tb2 N7 61.66(8) . . ? N1 Tb2 N7 118.02(9) . . ? N11 Tb2 N7 119.14(9) . . ? O4 Tb2 Tb1 40.77(6) . . ? O1 Tb2 Tb1 41.11(5) . . ? O7 Tb2 Tb1 41.46(5) . . ? O9 Tb2 Tb1 123.92(6) . . ? O3 Tb2 Tb1 127.75(6) . . ? O6 Tb2 Tb1 125.58(6) . . ? N1 Tb2 Tb1 91.40(6) . . ? N11 Tb2 Tb1 94.20(6) . . ? N7 Tb2 Tb1 89.48(6) . . ? O17 Cl1 O16 110.0(2) . . ? O17 Cl1 O18 110.7(2) . . ? O16 Cl1 O18 109.8(2) . . ? O17 Cl1 O19 109.1(2) . . ? O16 Cl1 O19 108.3(2) . . ? O18 Cl1 O19 108.9(2) . . ? O22 Cl2 O20 110.6(3) . . ? O22 Cl2 O23 111.1(3) . . ? O20 Cl2 O23 109.9(2) . . ? O22 Cl2 O21 109.5(3) . . ? O20 Cl2 O21 108.4(2) . . ? O23 Cl2 O21 107.3(2) . . ? O26 Cl3 O27 122.7(6) . . ? O26 Cl3 O25 118.6(4) . . ? O27 Cl3 O25 103.6(4) . . ? O26 Cl3 O24 103.3(4) . . ? O27 Cl3 O24 101.3(4) . . ? O25 Cl3 O24 104.7(3) . . ? C9 N1 N2 115.9(3) . . ? C9 N1 Tb2 130.2(2) . . ? N2 N1 Tb2 113.29(19) . . ? C17 N2 N1 116.7(3) . . ? C8 N3 N4 115.7(3) . . ? C8 N3 Tb1 130.9(2) . . ? N4 N3 Tb1 112.67(19) . . ? C10 N4 N3 116.6(3) . . ? C33 N6 N5 116.3(3) . . ? C31 N5 N6 115.6(3) . . ? C31 N5 Tb1 129.8(2) . . ? N6 N5 Tb1 113.8(2) . . ? C40 N8 N7 116.8(3) . . ? C32 N7 N8 115.2(3) . . ? C32 N7 Tb2 130.8(2) . . ? N8 N7 Tb2 113.7(2) . . ? C56 N10 N9 117.7(3) . . ? C54 N9 N10 114.2(3) . . ? C54 N9 Tb1 132.8(2) . . ? N10 N9 Tb1 113.0(2) . . ? C63 N12 N11 116.0(3) . . ? C55 N11 N12 115.8(3) . . ? C55 N11 Tb2 128.3(2) . . ? N12 N11 Tb2 114.8(2) . . ? C1 O1 Tb1 132.6(2) . . ? C1 O1 Tb2 129.9(2) . . ? Tb1 O1 Tb2 97.48(8) . . ? C10 O2 Tb1 126.0(2) . . ? C17 O3 Tb2 124.5(2) . . ? C24 O4 Tb1 130.9(2) . . ? C24 O4 Tb2 131.1(2) . . ? Tb1 O4 Tb2 98.02(8) . . ? C33 O5 Tb1 126.1(2) . . ? C40 O6 Tb2 124.8(2) . . ? C47 O7 Tb1 136.3(2) . . ? C47 O7 Tb2 126.0(2) . . ? Tb1 O7 Tb2 96.87(8) . . ? C56 O8 Tb1 124.8(2) . . ? C63 O9 Tb2 127.6(2) . . ? O1 C1 C2 120.5(3) . . ? O1 C1 C6 121.2(3) . . ? C2 C1 C6 118.4(3) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 C8 117.4(3) . . ? C1 C2 C8 122.7(3) . . ? C4 C3 C2 121.9(3) . . ? C5 C4 C3 117.9(3) . . ? C5 C4 C7 121.6(3) . . ? C3 C4 C7 120.5(3) . . ? C4 C5 C6 122.2(3) . . ? C5 C6 C1 119.7(3) . . ? C5 C6 C9 118.0(3) . . ? C1 C6 C9 122.3(3) . . ? N3 C8 C2 123.4(3) . . ? N1 C9 C6 122.9(3) . . ? C12 C11 C16 120.5(4) . . ? C12 C11 C10 122.9(4) . . ? C16 C11 C10 116.6(4) . . ? C13 C12 C11 118.6(4) . . ? C14 C13 C12 120.6(5) . . ? C15 C14 C13 120.8(4) . . ? C14 C15 C16 120.1(5) . . ? C15 C16 C11 119.4(4) . . ? O2 C10 N4 121.1(3) . . ? O2 C10 C11 120.6(3) . . ? N4 C10 C11 118.3(3) . . ? C23 C18 C19 119.4(3) . . ? C23 C18 C17 118.0(3) . . ? C19 C18 C17 122.6(3) . . ? C20 C19 C18 119.9(4) . . ? C19 C20 C21 120.1(4) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 119.7(4) . . ? C22 C23 C18 120.4(4) . . ? O3 C17 N2 120.4(3) . . ? O3 C17 C18 121.4(3) . . ? N2 C17 C18 118.2(3) . . ? O4 C24 C29 121.0(3) . . ? O4 C24 C25 120.8(3) . . ? C29 C24 C25 118.2(3) . . ? C26 C25 C24 119.8(3) . . ? C26 C25 C31 118.0(3) . . ? C24 C25 C31 122.2(3) . . ? C25 C26 C27 122.5(4) . . ? C28 C27 C26 117.1(4) . . ? C28 C27 C30 122.6(4) . . ? C26 C27 C30 120.3(4) . . ? C27 C28 C29 122.9(4) . . ? C28 C29 C24 119.5(3) . . ? C28 C29 C32 118.8(3) . . ? C24 C29 C32 121.7(3) . . ? N5 C31 C25 124.3(3) . . ? N7 C32 C29 122.9(3) . . ? C39 C34 C35 120.2(4) . . ? C39 C34 C33 117.2(4) . . ? C35 C34 C33 122.5(4) . . ? C36 C35 C34 118.8(5) . . ? C37 C36 C35 120.7(5) . . ? C38 C37 C36 120.6(4) . . ? C37 C38 C39 120.4(5) . . ? C34 C39 C38 119.2(5) . . ? O5 C33 N6 120.4(3) . . ? O5 C33 C34 120.3(4) . . ? N6 C33 C34 119.3(4) . . ? C46 C41 C42 119.6(3) . . ? C46 C41 C40 118.1(3) . . ? C42 C41 C40 122.2(3) . . ? C43 C42 C41 119.4(4) . . ? C44 C43 C42 120.3(4) . . ? C45 C44 C43 120.4(4) . . ? C44 C45 C46 119.7(4) . . ? C41 C46 C45 120.6(4) . . ? O6 C40 N8 120.0(3) . . ? O6 C40 C41 121.2(3) . . ? N8 C40 C41 118.7(3) . . ? O7 C47 C48 121.7(3) . . ? O7 C47 C52 120.7(3) . . ? C48 C47 C52 117.6(3) . . ? C49 C48 C47 120.2(3) . . ? C49 C48 C54 118.1(3) . . ? C47 C48 C54 121.7(3) . . ? C50 C49 C48 122.5(3) . . ? C49 C50 C51 116.9(3) . . ? C49 C50 C53 122.4(3) . . ? C51 C50 C53 120.6(3) . . ? C50 C51 C52 122.9(3) . . ? C51 C52 C47 119.8(3) . . ? C51 C52 C55 117.6(3) . . ? C47 C52 C55 122.5(3) . . ? N9 C54 C48 124.2(3) . . ? N11 C55 C52 123.5(3) . . ? C62 C57 C58 119.5(4) . . ? C62 C57 C56 119.0(3) . . ? C58 C57 C56 121.5(4) . . ? C59 C58 C57 119.4(4) . . ? C60 C59 C58 120.9(4) . . ? C59 C60 C61 119.8(4) . . ? C60 C61 C62 120.3(4) . . ? C57 C62 C61 120.1(4) . . ? O8 C56 N10 121.1(3) . . ? O8 C56 C57 122.0(3) . . ? N10 C56 C57 116.9(3) . . ? C65 C64 C69 120.0(3) . . ? C65 C64 C63 122.7(3) . . ? C69 C64 C63 117.3(3) . . ? C66 C65 C64 119.8(4) . . ? C67 C66 C65 120.3(4) . . ? C66 C67 C68 120.1(4) . . ? C69 C68 C67 120.2(4) . . ? C68 C69 C64 119.7(4) . . ? O9 C63 N12 119.7(3) . . ? O9 C63 C64 122.0(3) . . ? N12 C63 C64 118.4(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.462 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.089