# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_xuesfy11113005_111215_0m _database_code_depnum_ccdc_archive 'CCDC 881629' #TrackingRef 'web_deposit_cif_file_0_JinkuiTang_1336725020.xuesfy11113005_111215_0m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C136 H154 Dy6 N40 O40 S2' _chemical_formula_weight 4028.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.3269(8) _cell_length_b 27.9952(13) _cell_length_c 18.0851(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.4970(10) _cell_angle_gamma 90.00 _cell_volume 7757.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used 9971 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.05 _exptl_crystal_description rectangle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3996 _exptl_absorpt_coefficient_mu 2.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4901 _exptl_absorpt_correction_T_max 0.6022 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _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 39361 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.08 _reflns_number_total 13772 _reflns_number_gt 9538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+29.3800P] 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 13772 _refine_ls_number_parameters 1019 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Dy1 Dy 0.89958(3) 0.094973(16) 0.41777(2) 0.02887(13) Uani 1 1 d . . . Dy2 Dy 0.83363(3) 0.023038(16) 0.26074(2) 0.02909(13) Uani 1 1 d . . . Dy3 Dy 0.58427(3) 0.029268(17) 0.27013(3) 0.03278(14) Uani 1 1 d . . . N1 N 0.9306(5) 0.1651(3) 0.5115(4) 0.0333(19) Uani 1 1 d . . . N2 N 0.8756(6) 0.1769(3) 0.3737(4) 0.036(2) Uani 1 1 d . . . N3 N 0.8319(5) 0.1852(3) 0.3049(4) 0.036(2) Uani 1 1 d . . . N4 N 0.8802(7) 0.2588(3) 0.3821(6) 0.063(3) Uani 1 1 d . . . H4A H 0.8566 0.2624 0.3375 0.075 Uiso 1 1 calc R . . H4B H 0.8944 0.2840 0.4088 0.075 Uiso 1 1 calc R . . N5 N 1.0510(5) 0.1234(3) 0.3820(4) 0.0330(19) Uani 1 1 d . . . N6 N 1.0284(5) 0.0688(3) 0.4952(4) 0.0289(18) Uani 1 1 d . . . N7 N 1.0087(5) 0.0422(3) 0.5576(4) 0.0285(18) Uani 1 1 d . . . H7 H 1.0497 0.0318 0.5885 0.034 Uiso 1 1 calc R . . N8 N 1.1618(5) 0.0888(3) 0.5524(5) 0.040(2) Uani 1 1 d . . . H8A H 1.1519 0.0716 0.5921 0.048 Uiso 1 1 calc R . . H8B H 1.2109 0.1048 0.5491 0.048 Uiso 1 1 calc R . . N9 N 0.4719(5) 0.0219(3) 0.3708(4) 0.038(2) Uani 1 1 d . . . N10 N 0.5774(5) -0.0470(3) 0.3376(4) 0.0319(19) Uani 1 1 d . . . N11 N 0.6339(5) -0.0846(3) 0.3174(4) 0.0340(19) Uani 1 1 d . . . N12 N 0.4844(6) -0.1058(3) 0.3844(5) 0.044(2) Uani 1 1 d . . . H12A H 0.5164 -0.1296 0.3684 0.052 Uiso 1 1 calc R . . H12B H 0.4364 -0.1118 0.4084 0.052 Uiso 1 1 calc R . . N13 N 0.5377(5) 0.1196(3) 0.2732(5) 0.041(2) Uani 1 1 d . . . N14 N 0.4452(6) 0.0514(3) 0.2095(5) 0.043(2) Uani 1 1 d . . . N15 N 0.3926(6) 0.0170(4) 0.1763(5) 0.047(2) Uani 1 1 d . . . N16 N 0.3357(6) 0.1031(4) 0.1674(6) 0.063(3) Uani 1 1 d . . . H16A H 0.3076 0.0795 0.1453 0.076 Uiso 1 1 calc R . . H16B H 0.3144 0.1323 0.1651 0.076 Uiso 1 1 calc R . . N17 N 0.8395(6) 0.0078(4) 0.1310(5) 0.052(3) Uani 1 1 d . . . N18 N 0.2062(14) 0.1762(7) 0.1150(10) 0.147(8) Uani 1 1 d . . . N19 N 0.6187(10) 0.8545(4) 0.0331(6) 0.086(4) Uani 1 1 d . . . N20 N 0.2110(12) 0.7771(7) 0.2580(11) 0.141(7) Uani 1 1 d . . . O1 O 0.8589(4) 0.1044(2) 0.2913(3) 0.0338(16) Uani 1 1 d . . . O2 O 0.7112(4) 0.0670(2) 0.2316(3) 0.0332(16) Uani 1 1 d . . . O3 O 0.6031(4) 0.0661(2) 0.1214(4) 0.0380(17) Uani 1 1 d . . . O4 O 0.8673(4) 0.0508(2) 0.5267(3) 0.0335(16) Uani 1 1 d . . . O5 O 0.9527(4) 0.0286(2) 0.3483(3) 0.0286(14) Uani 1 1 d . . . O6 O 0.9829(4) 0.0543(2) 0.2139(3) 0.0381(17) Uani 1 1 d . . . O7 O 0.7047(4) -0.0239(2) 0.2570(3) 0.0326(15) Uani 1 1 d . . . O8 O 0.8779(4) -0.0504(2) 0.2867(4) 0.0349(16) Uani 1 1 d . . . O9 O 0.9995(5) -0.1148(3) 0.2351(4) 0.0498(19) Uani 1 1 d . . . O10 O 0.5170(5) -0.0290(3) 0.1956(4) 0.0443(18) Uani 1 1 d . . . O11 O 0.5017(5) -0.1192(3) 0.1866(5) 0.057(2) Uani 1 1 d . . . H11 H 0.5275 -0.0933 0.1961 0.086 Uiso 1 1 calc . . . O12 O 0.4200(6) -0.1932(3) 0.1382(5) 0.070(3) Uani 1 1 d . . . O13 O 0.7484(4) 0.1058(2) 0.4317(3) 0.0332(15) Uani 1 1 d . . . O14 O 0.7865(4) 0.0384(2) 0.3807(3) 0.0285(14) Uani 1 1 d . . . O15 O 0.6457(4) 0.0593(2) 0.3784(3) 0.0329(15) Uani 1 1 d . . . O16 O 0.6874(5) 0.8519(3) 0.4247(4) 0.051(2) Uani 1 1 d . . . H16 H 0.6541 0.8490 0.4606 0.076 Uiso 1 1 calc . . . O17 O 0.5302(6) 0.8055(3) 0.2958(5) 0.073(3) Uani 1 1 d . . . H17 H 0.5118 0.8190 0.2569 0.110 Uiso 1 1 calc . . . O18 O 0.4747(14) 0.2697(7) 0.4503(10) 0.200(8) Uani 1 1 d . . . H18 H 0.4966 0.2644 0.4926 0.300 Uiso 1 1 calc . . . O19 O 0.6379(7) 0.1530(3) 0.5150(6) 0.097(4) Uani 1 1 d . . . H19 H 0.6645 0.1371 0.4832 0.145 Uiso 1 1 calc . . . O20 O 0.4522(9) 0.1780(5) 0.4705(7) 0.131(5) Uani 1 1 d . . . S1 S 0.8634(4) -0.0141(3) -0.0154(2) 0.141(3) Uani 1 1 d . . . C1 C 0.9319(7) 0.2095(3) 0.4855(5) 0.034(2) Uani 1 1 d . . . C2 C 0.9644(8) 0.2476(4) 0.5255(6) 0.053(3) Uani 1 1 d . . . H2 H 0.9636 0.2788 0.5049 0.063 Uiso 1 1 calc R . . C3 C 0.9975(10) 0.2401(4) 0.5945(7) 0.068(4) Uani 1 1 d . . . H3A H 1.0223 0.2658 0.6221 0.081 Uiso 1 1 calc R . . C4 C 0.9952(9) 0.1948(4) 0.6247(6) 0.058(3) Uani 1 1 d . . . H4 H 1.0157 0.1886 0.6738 0.070 Uiso 1 1 calc R . . C5 C 0.9617(7) 0.1594(4) 0.5804(5) 0.038(2) Uani 1 1 d . . . H5 H 0.9606 0.1280 0.6005 0.046 Uiso 1 1 calc R . . C6 C 0.8944(6) 0.2151(4) 0.4090(5) 0.035(2) Uani 1 1 d . . . C7 C 0.8238(7) 0.1444(4) 0.2693(6) 0.041(3) Uani 1 1 d . . . C8 C 0.7671(7) 0.1444(3) 0.2008(6) 0.040(3) Uani 1 1 d . . . C9 C 0.7132(6) 0.1056(3) 0.1879(5) 0.032(2) Uani 1 1 d . . . C10 C 0.6537(7) 0.1062(4) 0.1260(6) 0.043(3) Uani 1 1 d . . . C11 C 0.6492(9) 0.1451(4) 0.0813(6) 0.062(4) Uani 1 1 d . . . H11A H 0.6097 0.1455 0.0400 0.074 Uiso 1 1 calc R . . C12 C 0.7027(10) 0.1843(4) 0.0960(7) 0.077(5) Uani 1 1 d . . . H12 H 0.6984 0.2116 0.0649 0.092 Uiso 1 1 calc R . . C13 C 0.7618(9) 0.1843(4) 0.1548(7) 0.064(4) Uani 1 1 d . . . H13 H 0.7985 0.2111 0.1639 0.077 Uiso 1 1 calc R . . C14 C 0.5437(8) 0.0632(4) 0.0590(6) 0.054(3) Uani 1 1 d . . . H14A H 0.5031 0.0902 0.0599 0.081 Uiso 1 1 calc R . . H14B H 0.5109 0.0332 0.0611 0.081 Uiso 1 1 calc R . . H14C H 0.5766 0.0643 0.0132 0.081 Uiso 1 1 calc R . . C15 C 1.1207(7) 0.1180(3) 0.4281(6) 0.036(2) Uani 1 1 d . . . C16 C 1.2024(7) 0.1360(4) 0.4135(6) 0.045(3) Uani 1 1 d . . . H16C H 1.2486 0.1340 0.4494 0.054 Uiso 1 1 calc R . . C17 C 1.2152(8) 0.1567(5) 0.3460(6) 0.055(3) Uani 1 1 d . . . H17A H 1.2715 0.1681 0.3340 0.066 Uiso 1 1 calc R . . C18 C 1.1472(8) 0.1610(4) 0.2955(6) 0.051(3) Uani 1 1 d . . . H18A H 1.1554 0.1743 0.2478 0.061 Uiso 1 1 calc R . . C19 C 1.0653(7) 0.1450(4) 0.3173(6) 0.044(3) Uani 1 1 d . . . H19A H 1.0169 0.1496 0.2842 0.053 Uiso 1 1 calc R . . C20 C 1.1023(6) 0.0904(3) 0.4972(5) 0.029(2) Uani 1 1 d . . . C21 C 0.9244(6) 0.0333(3) 0.5682(5) 0.030(2) Uani 1 1 d . . . C22 C 1.0972(6) -0.0056(3) 0.3654(5) 0.032(2) Uani 1 1 d . . . C23 C 1.0328(6) 0.0196(3) 0.3248(5) 0.025(2) Uani 1 1 d . . . C24 C 1.0565(7) 0.0349(4) 0.2523(5) 0.039(3) Uani 1 1 d . . . C25 C 1.1385(7) 0.0318(4) 0.2268(6) 0.044(3) Uani 1 1 d . . . H25 H 1.1521 0.0441 0.1795 0.053 Uiso 1 1 calc R . . C26 C 1.2031(7) 0.0100(4) 0.2719(6) 0.045(3) Uani 1 1 d . . . H26 H 1.2615 0.0081 0.2559 0.054 Uiso 1 1 calc R . . C27 C 1.1813(7) -0.0087(4) 0.3395(5) 0.037(2) Uani 1 1 d . . . H27 H 1.2250 -0.0242 0.3690 0.044 Uiso 1 1 calc R . . C28 C 0.9979(8) 0.0791(4) 0.1466(6) 0.048(3) Uani 1 1 d . . . H28A H 1.0399 0.1049 0.1558 0.071 Uiso 1 1 calc R . . H28B H 0.9428 0.0925 0.1275 0.071 Uiso 1 1 calc R . . H28C H 1.0212 0.0568 0.1103 0.071 Uiso 1 1 calc R . . C29 C 0.4543(6) -0.0212(3) 0.3992(5) 0.031(2) Uani 1 1 d . . . C30 C 0.3980(7) -0.0269(4) 0.4568(6) 0.041(3) Uani 1 1 d . . . H30 H 0.3869 -0.0579 0.4757 0.049 Uiso 1 1 calc R . . C31 C 0.3576(7) 0.0124(4) 0.4868(6) 0.040(3) Uani 1 1 d . . . H31 H 0.3169 0.0088 0.5252 0.048 Uiso 1 1 calc R . . C32 C 0.3778(7) 0.0566(4) 0.4598(6) 0.042(3) Uani 1 1 d . . . H32 H 0.3536 0.0846 0.4806 0.050 Uiso 1 1 calc R . . C33 C 0.4327(7) 0.0596(4) 0.4028(6) 0.042(3) Uani 1 1 d . . . H33 H 0.4447 0.0904 0.3837 0.050 Uiso 1 1 calc R . . C34 C 0.5089(7) -0.0603(3) 0.3720(5) 0.034(2) Uani 1 1 d . . . C35 C 0.6967(6) -0.0685(4) 0.2769(5) 0.031(2) Uani 1 1 d . . . C36 C 0.7629(6) -0.1038(3) 0.2534(5) 0.033(2) Uani 1 1 d . . . C37 C 0.8511(6) -0.0917(3) 0.2560(5) 0.033(2) Uani 1 1 d . . . C38 C 0.9120(7) -0.1245(4) 0.2286(6) 0.044(3) Uani 1 1 d . . . C39 C 0.8847(8) -0.1685(4) 0.2033(7) 0.053(3) Uani 1 1 d . . . H39 H 0.9265 -0.1908 0.1863 0.064 Uiso 1 1 calc R . . C40 C 0.7964(8) -0.1810(4) 0.2022(7) 0.057(3) Uani 1 1 d . . . H40 H 0.7779 -0.2116 0.1851 0.068 Uiso 1 1 calc R . . C41 C 0.7369(7) -0.1483(4) 0.2263(6) 0.047(3) Uani 1 1 d . . . H41 H 0.6766 -0.1562 0.2244 0.057 Uiso 1 1 calc R . . C42 C 1.0258(9) -0.0820(5) 0.1813(8) 0.076(4) Uani 1 1 d . . . H42A H 1.0295 -0.0982 0.1334 0.113 Uiso 1 1 calc R . . H42B H 1.0831 -0.0689 0.1955 0.113 Uiso 1 1 calc R . . H42C H 0.9831 -0.0561 0.1773 0.113 Uiso 1 1 calc R . . C43 C 0.4606(8) 0.1328(4) 0.2404(6) 0.047(3) Uani 1 1 d . . . C44 C 0.4331(8) 0.1804(4) 0.2418(6) 0.053(3) Uani 1 1 d . . . H44 H 0.3795 0.1893 0.2181 0.063 Uiso 1 1 calc R . . C45 C 0.4825(9) 0.2137(5) 0.2770(8) 0.068(4) Uani 1 1 d . . . H45 H 0.4630 0.2459 0.2801 0.081 Uiso 1 1 calc R . . C46 C 0.5617(9) 0.2003(4) 0.3083(8) 0.066(4) Uani 1 1 d . . . H46 H 0.5988 0.2233 0.3318 0.080 Uiso 1 1 calc R . . C47 C 0.5858(8) 0.1535(4) 0.3050(6) 0.050(3) Uani 1 1 d . . . H47 H 0.6405 0.1447 0.3268 0.060 Uiso 1 1 calc R . . C48 C 0.4125(7) 0.0946(4) 0.2054(6) 0.046(3) Uani 1 1 d . . . C49 C 0.4332(7) -0.0229(4) 0.1733(6) 0.042(3) Uani 1 1 d . . . C50 C 0.3893(8) -0.0652(4) 0.1453(6) 0.048(3) Uani 1 1 d . . . C51 C 0.4238(7) -0.1099(4) 0.1537(6) 0.044(3) Uani 1 1 d . . . C52 C 0.3770(9) -0.1509(5) 0.1286(7) 0.058(3) Uani 1 1 d . . . C53 C 0.2956(9) -0.1455(5) 0.0957(9) 0.075(4) Uani 1 1 d . . . H53 H 0.2627 -0.1726 0.0803 0.090 Uiso 1 1 calc R . . C54 C 0.2619(9) -0.0994(5) 0.0850(8) 0.072(4) Uani 1 1 d . . . H54 H 0.2078 -0.0953 0.0590 0.087 Uiso 1 1 calc R . . C55 C 0.3050(8) -0.0606(5) 0.1110(7) 0.062(4) Uani 1 1 d . . . H55 H 0.2789 -0.0299 0.1064 0.075 Uiso 1 1 calc R . . C56 C 0.3746(10) -0.2347(4) 0.1137(9) 0.080(4) Uani 1 1 d . . . H56A H 0.3161 -0.2350 0.1344 0.121 Uiso 1 1 calc R . . H56B H 0.4066 -0.2632 0.1302 0.121 Uiso 1 1 calc R . . H56C H 0.3695 -0.2345 0.0596 0.121 Uiso 1 1 calc R . . C57 C 0.7246(6) 0.0672(3) 0.3972(5) 0.031(2) Uani 1 1 d . . . C58 C 0.8491(9) -0.0008(6) 0.0706(7) 0.069(4) Uani 1 1 d . . . C59 C 0.1439(18) 0.1553(11) -0.0161(12) 0.220(17) Uani 1 1 d . . . H59A H 0.0843 0.1675 -0.0233 0.330 Uiso 1 1 calc R . . H59B H 0.1438 0.1205 -0.0218 0.330 Uiso 1 1 calc R . . H59C H 0.1817 0.1696 -0.0529 0.330 Uiso 1 1 calc R . . C60 C 0.1765(14) 0.1678(8) 0.0584(12) 0.121(8) Uani 1 1 d . . . C61 C 0.6556(10) 0.9412(5) 0.0671(7) 0.071(4) Uani 1 1 d . . . H61A H 0.6089 0.9545 0.0969 0.107 Uiso 1 1 calc R . . H61B H 0.6617 0.9605 0.0223 0.107 Uiso 1 1 calc R . . H61C H 0.7107 0.9418 0.0960 0.107 Uiso 1 1 calc R . . C62 C 0.6343(9) 0.8923(5) 0.0468(7) 0.060(3) Uani 1 1 d . . . C63 C 0.2345(13) 0.8657(6) 0.2947(12) 0.124(7) Uani 1 1 d . . . H63A H 0.2377 0.8849 0.2495 0.186 Uiso 1 1 calc R . . H63B H 0.2886 0.8694 0.3241 0.186 Uiso 1 1 calc R . . H63C H 0.1850 0.8764 0.3236 0.186 Uiso 1 1 calc R . . C64 C 0.2227(12) 0.8157(8) 0.2751(12) 0.106(6) Uani 1 1 d . . . C65 C 0.7194(10) 0.8062(4) 0.4043(8) 0.072(4) Uani 1 1 d . . . H65A H 0.7729 0.8100 0.3764 0.108 Uiso 1 1 calc R . . H65B H 0.6753 0.7897 0.3735 0.108 Uiso 1 1 calc R . . H65C H 0.7320 0.7873 0.4489 0.108 Uiso 1 1 calc R . . C66 C 0.4857(10) 0.7617(5) 0.3047(9) 0.084(5) Uani 1 1 d . . . H66A H 0.5026 0.7476 0.3526 0.126 Uiso 1 1 calc R . . H66B H 0.5011 0.7398 0.2649 0.126 Uiso 1 1 calc R . . H66C H 0.4226 0.7674 0.3028 0.126 Uiso 1 1 calc R . . C67 C 0.403(3) 0.298(2) 0.456(3) 0.47(5) Uani 1 1 d . . . H67A H 0.3672 0.2955 0.4109 0.698 Uiso 1 1 calc . . . H67B H 0.4212 0.3309 0.4644 0.698 Uiso 1 1 calc . . . H67C H 0.3690 0.2869 0.4984 0.698 Uiso 1 1 calc . . . C68 C 0.6773(13) 0.1984(5) 0.5230(11) 0.119(7) Uani 1 1 d . . . H68A H 0.6505 0.2156 0.5638 0.179 Uiso 1 1 calc R . . H68B H 0.6688 0.2166 0.4771 0.179 Uiso 1 1 calc R . . H68C H 0.7399 0.1944 0.5338 0.179 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 0.0308(3) 0.0250(3) 0.0301(3) 0.00311(19) -0.01160(19) 0.0000(2) Dy2 0.0296(3) 0.0300(3) 0.0271(3) 0.00201(19) -0.00941(18) -0.0002(2) Dy3 0.0285(3) 0.0346(3) 0.0348(3) 0.0045(2) -0.00935(19) 0.0011(2) N1 0.035(5) 0.032(5) 0.032(5) -0.001(4) -0.008(4) 0.001(4) N2 0.046(5) 0.026(5) 0.037(5) 0.003(4) -0.020(4) -0.004(4) N3 0.040(5) 0.028(5) 0.038(5) 0.006(4) -0.010(4) -0.001(4) N4 0.087(8) 0.035(6) 0.064(7) 0.012(5) -0.036(6) -0.002(5) N5 0.044(5) 0.027(4) 0.027(4) 0.005(3) -0.002(4) 0.000(4) N6 0.031(5) 0.025(4) 0.030(4) -0.001(3) -0.011(3) -0.001(4) N7 0.029(5) 0.029(4) 0.027(4) 0.007(3) -0.009(3) 0.002(4) N8 0.030(5) 0.045(5) 0.043(5) 0.013(4) -0.006(4) -0.009(4) N9 0.039(5) 0.034(5) 0.038(5) 0.002(4) -0.012(4) 0.002(4) N10 0.030(5) 0.035(5) 0.031(5) 0.000(4) -0.011(4) 0.000(4) N11 0.032(5) 0.033(5) 0.037(5) -0.002(4) -0.010(4) -0.001(4) N12 0.042(6) 0.030(5) 0.060(6) 0.004(4) 0.005(4) -0.004(4) N13 0.031(5) 0.044(5) 0.047(5) 0.013(4) -0.005(4) 0.011(4) N14 0.038(5) 0.047(6) 0.043(5) 0.005(4) -0.001(4) 0.001(5) N15 0.036(5) 0.059(7) 0.046(6) -0.005(5) 0.000(4) 0.002(5) N16 0.039(6) 0.065(7) 0.084(8) 0.021(6) -0.016(5) 0.010(5) N17 0.048(6) 0.070(7) 0.038(6) -0.002(5) -0.002(5) -0.006(5) N18 0.18(2) 0.162(17) 0.094(13) 0.026(12) -0.017(13) 0.094(14) N19 0.152(14) 0.042(7) 0.064(8) 0.011(6) -0.001(8) -0.011(8) N20 0.115(15) 0.110(15) 0.20(2) -0.019(14) 0.017(13) -0.024(12) O1 0.043(4) 0.026(4) 0.032(4) 0.004(3) -0.017(3) 0.001(3) O2 0.028(4) 0.033(4) 0.038(4) 0.011(3) -0.013(3) 0.001(3) O3 0.042(4) 0.035(4) 0.037(4) 0.008(3) -0.016(3) -0.006(3) O4 0.024(4) 0.042(4) 0.034(4) 0.008(3) -0.011(3) 0.002(3) O5 0.029(4) 0.030(4) 0.027(3) 0.003(3) -0.008(3) -0.005(3) O6 0.036(4) 0.046(4) 0.031(4) 0.012(3) -0.003(3) 0.001(3) O7 0.030(4) 0.030(4) 0.037(4) 0.004(3) -0.010(3) -0.001(3) O8 0.032(4) 0.026(4) 0.045(4) -0.005(3) -0.017(3) 0.003(3) O9 0.035(5) 0.046(5) 0.068(5) 0.000(4) -0.007(4) 0.004(4) O10 0.039(4) 0.054(5) 0.039(4) 0.000(3) -0.011(3) -0.008(4) O11 0.051(5) 0.048(5) 0.072(6) 0.008(4) -0.016(4) -0.003(4) O12 0.074(6) 0.038(5) 0.098(7) -0.004(5) -0.022(5) -0.009(5) O13 0.036(4) 0.026(4) 0.037(4) -0.002(3) -0.008(3) -0.001(3) O14 0.027(4) 0.024(3) 0.033(4) 0.001(3) -0.012(3) 0.002(3) O15 0.027(4) 0.036(4) 0.035(4) 0.002(3) -0.004(3) -0.001(3) O16 0.059(5) 0.036(4) 0.057(5) -0.006(4) -0.003(4) 0.004(4) O17 0.093(7) 0.043(5) 0.082(7) 0.001(4) -0.021(5) -0.003(5) O18 0.20(2) 0.22(2) 0.185(18) -0.012(15) 0.041(15) -0.021(16) O19 0.105(9) 0.045(6) 0.145(10) -0.017(6) 0.075(7) -0.017(6) O20 0.122(11) 0.136(12) 0.134(11) 0.020(9) 0.015(9) -0.004(9) S1 0.109(4) 0.260(7) 0.053(3) -0.046(4) -0.003(2) 0.066(4) C1 0.039(6) 0.025(5) 0.037(6) 0.000(4) 0.002(5) 0.002(5) C2 0.076(9) 0.028(6) 0.053(8) -0.001(5) -0.018(6) -0.014(6) C3 0.102(11) 0.038(7) 0.061(9) -0.014(6) -0.033(8) 0.007(7) C4 0.099(11) 0.046(7) 0.029(6) -0.008(5) -0.016(6) -0.009(7) C5 0.042(6) 0.039(6) 0.034(6) -0.003(5) 0.005(5) 0.008(5) C6 0.032(6) 0.032(6) 0.041(6) 0.007(5) -0.014(4) 0.007(5) C7 0.043(7) 0.037(6) 0.040(6) 0.017(5) -0.012(5) -0.003(5) C8 0.044(7) 0.027(6) 0.048(7) 0.015(5) -0.020(5) -0.002(5) C9 0.038(6) 0.037(6) 0.021(5) 0.009(4) -0.006(4) 0.008(5) C10 0.043(7) 0.050(7) 0.035(6) 0.011(5) -0.012(5) -0.005(5) C11 0.075(9) 0.059(8) 0.048(7) 0.028(6) -0.039(6) -0.008(7) C12 0.111(12) 0.049(8) 0.068(9) 0.036(7) -0.062(8) -0.030(8) C13 0.081(10) 0.037(7) 0.074(9) 0.024(6) -0.039(7) -0.016(6) C14 0.052(8) 0.069(8) 0.040(7) 0.010(6) -0.021(5) -0.016(6) C15 0.039(6) 0.027(5) 0.043(6) 0.013(4) -0.005(5) -0.010(5) C16 0.043(7) 0.046(7) 0.045(7) 0.019(5) -0.002(5) -0.004(5) C17 0.034(7) 0.076(9) 0.055(8) 0.013(7) 0.001(6) 0.004(6) C18 0.055(8) 0.057(8) 0.042(7) 0.011(6) 0.013(6) -0.009(6) C19 0.051(7) 0.046(7) 0.035(6) 0.001(5) -0.003(5) -0.002(6) C20 0.026(5) 0.029(5) 0.032(5) 0.002(4) -0.011(4) 0.005(4) C21 0.028(5) 0.027(5) 0.035(6) 0.003(4) -0.009(4) -0.001(4) C22 0.031(6) 0.029(5) 0.036(6) 0.002(4) -0.005(4) -0.006(4) C23 0.020(5) 0.026(5) 0.029(5) -0.001(4) 0.000(4) -0.001(4) C24 0.052(7) 0.039(6) 0.025(5) 0.010(4) -0.011(5) -0.025(5) C25 0.040(7) 0.054(7) 0.038(6) 0.006(5) 0.006(5) -0.011(5) C26 0.029(6) 0.061(8) 0.044(7) 0.002(6) -0.003(5) -0.005(5) C27 0.035(6) 0.040(6) 0.035(6) 0.003(5) -0.007(5) -0.005(5) C28 0.053(7) 0.053(7) 0.036(6) 0.012(5) -0.004(5) -0.005(6) C29 0.029(5) 0.030(5) 0.033(6) 0.000(4) -0.009(4) -0.001(4) C30 0.035(6) 0.043(6) 0.045(7) -0.003(5) -0.004(5) 0.002(5) C31 0.040(6) 0.040(6) 0.042(6) 0.005(5) 0.004(5) 0.001(5) C32 0.044(7) 0.041(7) 0.041(6) 0.001(5) -0.007(5) 0.012(5) C33 0.039(6) 0.045(7) 0.041(6) 0.011(5) -0.006(5) -0.001(5) C34 0.040(6) 0.028(6) 0.033(6) 0.002(4) -0.012(5) -0.002(5) C35 0.032(6) 0.034(6) 0.027(5) -0.004(4) -0.010(4) 0.001(5) C36 0.035(6) 0.027(5) 0.036(6) -0.004(4) -0.009(4) 0.009(4) C37 0.028(5) 0.031(6) 0.040(6) -0.004(4) -0.014(4) 0.000(4) C38 0.036(6) 0.039(6) 0.055(7) -0.011(5) -0.018(5) 0.003(5) C39 0.050(8) 0.044(7) 0.066(8) -0.015(6) -0.008(6) 0.008(6) C40 0.048(8) 0.049(8) 0.071(8) -0.024(6) -0.022(6) 0.004(6) C41 0.038(7) 0.044(7) 0.060(8) -0.012(6) -0.006(5) 0.004(5) C42 0.061(10) 0.058(9) 0.107(12) -0.010(8) 0.002(8) 0.004(7) C43 0.045(7) 0.057(8) 0.040(7) 0.010(5) 0.002(5) 0.004(6) C44 0.052(8) 0.045(7) 0.060(8) 0.022(6) -0.003(6) 0.018(6) C45 0.065(9) 0.044(8) 0.093(11) 0.007(7) -0.014(8) 0.006(7) C46 0.074(10) 0.027(7) 0.096(11) 0.007(6) -0.019(8) 0.010(6) C47 0.047(7) 0.040(7) 0.062(8) 0.017(6) -0.011(6) -0.007(6) C48 0.035(6) 0.060(8) 0.044(7) 0.022(6) 0.001(5) 0.016(6) C49 0.043(7) 0.049(7) 0.031(6) 0.004(5) -0.012(5) -0.013(6) C50 0.046(7) 0.059(8) 0.039(7) 0.000(5) -0.004(5) 0.004(6) C51 0.040(7) 0.054(7) 0.036(6) -0.002(5) -0.011(5) -0.005(6) C52 0.060(9) 0.054(8) 0.060(8) -0.003(6) -0.013(6) 0.002(7) C53 0.046(8) 0.062(9) 0.117(13) -0.020(8) -0.018(8) -0.012(7) C54 0.054(9) 0.079(11) 0.083(10) -0.014(8) -0.018(7) 0.005(8) C55 0.042(7) 0.066(9) 0.078(9) -0.018(7) -0.025(6) -0.011(6) C56 0.082(11) 0.043(8) 0.115(13) -0.023(8) -0.004(9) -0.003(7) C57 0.031(6) 0.035(6) 0.026(5) 0.007(4) -0.008(4) 0.004(5) C58 0.056(9) 0.108(12) 0.043(8) -0.016(8) -0.006(6) 0.013(8) C59 0.23(3) 0.34(4) 0.089(17) -0.04(2) -0.034(18) 0.17(3) C60 0.126(18) 0.16(2) 0.078(13) 0.032(14) -0.006(12) 0.062(15) C61 0.084(11) 0.061(9) 0.067(9) -0.018(7) 0.002(8) -0.005(8) C62 0.072(9) 0.051(9) 0.056(8) 0.013(6) -0.018(7) 0.011(7) C63 0.128(18) 0.083(14) 0.163(19) 0.006(13) 0.046(14) -0.017(12) C64 0.082(14) 0.095(15) 0.142(18) -0.001(13) 0.041(12) -0.025(12) C65 0.100(12) 0.040(7) 0.075(10) -0.004(7) -0.010(8) 0.009(7) C66 0.071(11) 0.064(10) 0.117(13) -0.017(9) 0.007(9) -0.018(8) C67 0.24(4) 0.58(8) 0.59(8) 0.40(7) 0.29(5) 0.33(5) C68 0.129(17) 0.046(9) 0.19(2) -0.026(11) 0.054(14) -0.004(10) _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 O13 2.358(7) . ? Dy1 O1 2.369(6) . ? Dy1 O4 2.387(6) . ? Dy1 O5 2.398(6) . ? Dy1 O14 2.429(6) . ? Dy1 N2 2.453(8) . ? Dy1 N6 2.501(7) . ? Dy1 N5 2.553(8) . ? Dy1 N1 2.629(8) . ? Dy1 Dy2 3.6046(6) . ? Dy2 O8 2.211(6) . ? Dy2 O2 2.294(6) . ? Dy2 O14 2.345(6) . ? Dy2 O1 2.372(6) . ? Dy2 O7 2.372(6) . ? Dy2 N17 2.389(10) . ? Dy2 O5 2.390(6) . ? Dy2 O6 2.612(7) . ? Dy2 Dy3 3.8340(7) . ? Dy3 O15 2.308(6) . ? Dy3 O2 2.335(6) . ? Dy3 O10 2.338(7) . ? Dy3 O7 2.387(6) . ? Dy3 N14 2.451(9) . ? Dy3 N10 2.463(8) . ? Dy3 N9 2.547(9) . ? Dy3 N13 2.628(8) . ? Dy3 O3 2.903(6) . ? N1 C1 1.330(12) . ? N1 C5 1.333(12) . ? N2 C6 1.274(12) . ? N2 N3 1.416(10) . ? N3 C7 1.317(13) . ? N4 C6 1.334(12) . ? N5 C19 1.341(12) . ? N5 C15 1.345(12) . ? N6 C20 1.285(12) . ? N6 N7 1.390(10) . ? N7 C21 1.334(12) . ? N8 C20 1.334(11) . ? N9 C29 1.342(12) . ? N9 C33 1.351(13) . ? N10 C34 1.289(12) . ? N10 N11 1.415(11) . ? N11 C35 1.304(12) . ? N12 C34 1.349(12) . ? N13 C47 1.323(13) . ? N13 C43 1.360(13) . ? N14 C48 1.311(13) . ? N14 N15 1.382(12) . ? N15 C49 1.283(13) . ? N16 C48 1.368(13) . ? N17 C58 1.131(14) . ? N18 C60 1.13(2) . ? N19 C62 1.110(15) . ? N20 C64 1.14(2) . ? O1 C7 1.301(11) . ? O2 C9 1.341(11) . ? O3 C10 1.367(12) . ? O3 C14 1.433(12) . ? O4 C21 1.239(11) . ? O5 C23 1.334(10) . ? O6 C24 1.418(12) . ? O6 C28 1.424(11) . ? O7 C35 1.307(11) . ? O8 C37 1.343(11) . ? O9 C38 1.371(12) . ? O9 C42 1.404(15) . ? O10 C49 1.346(12) . ? O11 C51 1.345(12) . ? O12 C52 1.365(14) . ? O12 C56 1.419(14) . ? O13 C57 1.295(11) . ? O14 C57 1.287(11) . ? O15 C57 1.267(11) . ? O16 C65 1.423(13) . ? O17 C66 1.412(15) . ? O18 C67 1.36(3) . ? O19 C68 1.412(17) . ? S1 C58 1.621(13) . ? C1 C2 1.375(14) . ? C1 C6 1.491(13) . ? C2 C3 1.351(15) . ? C3 C4 1.381(16) . ? C4 C5 1.365(14) . ? C7 C8 1.494(14) . ? C8 C9 1.381(14) . ? C8 C13 1.392(14) . ? C9 C10 1.426(13) . ? C10 C11 1.355(14) . ? C11 C12 1.392(16) . ? C12 C13 1.379(16) . ? C15 C16 1.381(14) . ? C15 C20 1.504(13) . ? C16 C17 1.371(15) . ? C17 C18 1.373(16) . ? C18 C19 1.400(15) . ? C21 C22 1.476(13) 3_756 ? C22 C27 1.385(13) . ? C22 C23 1.405(13) . ? C22 C21 1.476(13) 3_756 ? C23 C24 1.433(13) . ? C24 C25 1.354(15) . ? C25 C26 1.406(15) . ? C26 C27 1.379(14) . ? C29 C30 1.378(14) . ? C29 C34 1.471(13) . ? C30 C31 1.381(14) . ? C31 C32 1.369(14) . ? C32 C33 1.351(15) . ? C35 C36 1.485(13) . ? C36 C37 1.394(13) . ? C36 C41 1.395(14) . ? C37 C38 1.409(14) . ? C38 C39 1.376(15) . ? C39 C40 1.398(16) . ? C40 C41 1.371(15) . ? C43 C44 1.397(15) . ? C43 C48 1.439(16) . ? C44 C45 1.350(17) . ? C45 C46 1.378(17) . ? C46 C47 1.364(15) . ? C49 C50 1.448(15) . ? C50 C51 1.366(16) . ? C50 C55 1.423(15) . ? C51 C52 1.421(16) . ? C52 C53 1.377(17) . ? C53 C54 1.401(18) . ? C54 C55 1.349(17) . ? C59 C60 1.47(3) . ? C61 C62 1.454(18) . ? C63 C64 1.45(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Dy1 O1 81.6(2) . . ? O13 Dy1 O4 75.7(2) . . ? O1 Dy1 O4 143.0(2) . . ? O13 Dy1 O5 120.3(2) . . ? O1 Dy1 O5 70.4(2) . . ? O4 Dy1 O5 96.4(2) . . ? O13 Dy1 O14 54.3(2) . . ? O1 Dy1 O14 68.8(2) . . ? O4 Dy1 O14 74.2(2) . . ? O5 Dy1 O14 66.4(2) . . ? O13 Dy1 N2 77.0(3) . . ? O1 Dy1 N2 63.2(2) . . ? O4 Dy1 N2 136.0(3) . . ? O5 Dy1 N2 127.2(2) . . ? O14 Dy1 N2 114.8(2) . . ? O13 Dy1 N6 137.9(2) . . ? O1 Dy1 N6 139.2(2) . . ? O4 Dy1 N6 64.1(2) . . ? O5 Dy1 N6 78.0(2) . . ? O14 Dy1 N6 120.7(2) . . ? N2 Dy1 N6 124.5(3) . . ? O13 Dy1 N5 152.9(2) . . ? O1 Dy1 N5 86.5(2) . . ? O4 Dy1 N5 125.4(2) . . ? O5 Dy1 N5 77.6(2) . . ? O14 Dy1 N5 141.3(2) . . ? N2 Dy1 N5 75.8(3) . . ? N6 Dy1 N5 61.6(2) . . ? O13 Dy1 N1 89.8(2) . . ? O1 Dy1 N1 125.3(2) . . ? O4 Dy1 N1 83.8(2) . . ? O5 Dy1 N1 149.2(2) . . ? O14 Dy1 N1 141.3(2) . . ? N2 Dy1 N1 62.3(2) . . ? N6 Dy1 N1 74.4(2) . . ? N5 Dy1 N1 77.3(2) . . ? O13 Dy1 Dy2 84.25(15) . . ? O1 Dy1 Dy2 40.54(15) . . ? O4 Dy1 Dy2 107.51(16) . . ? O5 Dy1 Dy2 41.08(14) . . ? O14 Dy1 Dy2 40.09(15) . . ? N2 Dy1 Dy2 103.28(18) . . ? N6 Dy1 Dy2 118.58(17) . . ? N5 Dy1 Dy2 102.30(17) . . ? N1 Dy1 Dy2 165.36(17) . . ? O8 Dy2 O2 142.4(2) . . ? O8 Dy2 O14 94.2(2) . . ? O2 Dy2 O14 81.0(2) . . ? O8 Dy2 O1 142.7(2) . . ? O2 Dy2 O1 70.5(2) . . ? O14 Dy2 O1 70.2(2) . . ? O8 Dy2 O7 75.1(2) . . ? O2 Dy2 O7 67.3(2) . . ? O14 Dy2 O7 81.4(2) . . ? O1 Dy2 O7 132.0(2) . . ? O8 Dy2 N17 91.4(3) . . ? O2 Dy2 N17 85.5(3) . . ? O14 Dy2 N17 164.2(3) . . ? O1 Dy2 N17 112.9(3) . . ? O7 Dy2 N17 85.8(3) . . ? O8 Dy2 O5 72.2(2) . . ? O2 Dy2 O5 136.3(2) . . ? O14 Dy2 O5 67.9(2) . . ? O1 Dy2 O5 70.5(2) . . ? O7 Dy2 O5 132.5(2) . . ? N17 Dy2 O5 127.9(3) . . ? O8 Dy2 O6 96.5(2) . . ? O2 Dy2 O6 117.7(2) . . ? O14 Dy2 O6 122.2(2) . . ? O1 Dy2 O6 67.3(2) . . ? O7 Dy2 O6 155.9(2) . . ? N17 Dy2 O6 71.7(3) . . ? O5 Dy2 O6 62.1(2) . . ? O8 Dy2 Dy1 105.88(16) . . ? O2 Dy2 Dy1 95.29(16) . . ? O14 Dy2 Dy1 41.86(15) . . ? O1 Dy2 Dy1 40.49(14) . . ? O7 Dy2 Dy1 123.22(15) . . ? N17 Dy2 Dy1 148.9(2) . . ? O5 Dy2 Dy1 41.25(15) . . ? O6 Dy2 Dy1 80.68(15) . . ? O8 Dy2 Dy3 109.51(17) . . ? O2 Dy2 Dy3 34.43(16) . . ? O14 Dy2 Dy3 67.61(14) . . ? O1 Dy2 Dy3 95.91(16) . . ? O7 Dy2 Dy3 36.47(15) . . ? N17 Dy2 Dy3 96.6(2) . . ? O5 Dy2 Dy3 135.44(15) . . ? O6 Dy2 Dy3 151.87(14) . . ? Dy1 Dy2 Dy3 101.479(15) . . ? O15 Dy3 O2 76.3(2) . . ? O15 Dy3 O10 155.0(2) . . ? O2 Dy3 O10 120.1(2) . . ? O15 Dy3 O7 90.7(2) . . ? O2 Dy3 O7 66.4(2) . . ? O10 Dy3 O7 80.7(2) . . ? O15 Dy3 N14 128.2(3) . . ? O2 Dy3 N14 118.3(2) . . ? O10 Dy3 N14 63.4(3) . . ? O7 Dy3 N14 141.1(3) . . ? O15 Dy3 N10 85.3(2) . . ? O2 Dy3 N10 125.9(2) . . ? O10 Dy3 N10 69.9(2) . . ? O7 Dy3 N10 63.4(2) . . ? N14 Dy3 N10 113.1(3) . . ? O15 Dy3 N9 72.0(2) . . ? O2 Dy3 N9 146.5(2) . . ? O10 Dy3 N9 93.4(3) . . ? O7 Dy3 N9 124.0(2) . . ? N14 Dy3 N9 75.2(3) . . ? N10 Dy3 N9 62.4(3) . . ? O15 Dy3 N13 74.8(2) . . ? O2 Dy3 N13 78.5(2) . . ? O10 Dy3 N13 124.6(3) . . ? O7 Dy3 N13 144.4(2) . . ? N14 Dy3 N13 62.2(3) . . ? N10 Dy3 N13 144.0(3) . . ? N9 Dy3 N13 82.8(3) . . ? O15 Dy3 O3 127.5(2) . . ? O2 Dy3 O3 57.27(19) . . ? O10 Dy3 O3 76.5(2) . . ? O7 Dy3 O3 91.9(2) . . ? N14 Dy3 O3 66.5(2) . . ? N10 Dy3 O3 140.7(2) . . ? N9 Dy3 O3 141.0(2) . . ? N13 Dy3 O3 73.2(2) . . ? O15 Dy3 Dy2 70.67(16) . . ? O2 Dy3 Dy2 33.73(15) . . ? O10 Dy3 Dy2 111.60(18) . . ? O7 Dy3 Dy2 36.20(15) . . ? N14 Dy3 Dy2 148.0(2) . . ? N10 Dy3 Dy2 92.18(19) . . ? N9 Dy3 Dy2 136.15(18) . . ? N13 Dy3 Dy2 108.43(19) . . ? O3 Dy3 Dy2 81.48(13) . . ? C1 N1 C5 115.8(8) . . ? C1 N1 Dy1 118.3(6) . . ? C5 N1 Dy1 124.6(6) . . ? C6 N2 N3 113.5(8) . . ? C6 N2 Dy1 126.2(6) . . ? N3 N2 Dy1 120.2(5) . . ? C7 N3 N2 108.9(8) . . ? C19 N5 C15 116.5(9) . . ? C19 N5 Dy1 122.1(7) . . ? C15 N5 Dy1 121.4(6) . . ? C20 N6 N7 116.1(7) . . ? C20 N6 Dy1 124.1(6) . . ? N7 N6 Dy1 115.2(5) . . ? C21 N7 N6 116.6(7) . . ? C29 N9 C33 116.2(9) . . ? C29 N9 Dy3 119.6(6) . . ? C33 N9 Dy3 124.0(7) . . ? C34 N10 N11 115.0(8) . . ? C34 N10 Dy3 122.3(6) . . ? N11 N10 Dy3 118.8(6) . . ? C35 N11 N10 110.8(8) . . ? C47 N13 C43 117.5(10) . . ? C47 N13 Dy3 123.4(7) . . ? C43 N13 Dy3 119.1(7) . . ? C48 N14 N15 113.5(9) . . ? C48 N14 Dy3 125.9(8) . . ? N15 N14 Dy3 120.7(7) . . ? C49 N15 N14 110.3(9) . . ? C58 N17 Dy2 174.2(10) . . ? C7 O1 Dy1 119.1(6) . . ? C7 O1 Dy2 133.7(6) . . ? Dy1 O1 Dy2 99.0(2) . . ? C9 O2 Dy2 122.5(6) . . ? C9 O2 Dy3 124.9(6) . . ? Dy2 O2 Dy3 111.8(2) . . ? C10 O3 C14 116.2(8) . . ? C10 O3 Dy3 107.8(5) . . ? C14 O3 Dy3 129.3(6) . . ? C21 O4 Dy1 123.1(6) . . ? C23 O5 Dy2 118.0(5) . . ? C23 O5 Dy1 129.9(5) . . ? Dy2 O5 Dy1 97.7(2) . . ? C24 O6 C28 117.5(8) . . ? C24 O6 Dy2 113.9(5) . . ? C28 O6 Dy2 127.0(6) . . ? C35 O7 Dy2 127.3(6) . . ? C35 O7 Dy3 119.4(6) . . ? Dy2 O7 Dy3 107.3(2) . . ? C37 O8 Dy2 128.6(5) . . ? C38 O9 C42 111.6(9) . . ? C49 O10 Dy3 119.2(7) . . ? C52 O12 C56 116.0(10) . . ? C57 O13 Dy1 96.1(5) . . ? C57 O14 Dy2 125.2(5) . . ? C57 O14 Dy1 93.0(5) . . ? Dy2 O14 Dy1 98.0(2) . . ? C57 O15 Dy3 131.1(6) . . ? N1 C1 C2 123.2(9) . . ? N1 C1 C6 114.6(8) . . ? C2 C1 C6 122.2(9) . . ? C3 C2 C1 119.2(10) . . ? C2 C3 C4 119.7(11) . . ? C5 C4 C3 116.6(11) . . ? N1 C5 C4 125.5(10) . . ? N2 C6 N4 123.6(9) . . ? N2 C6 C1 117.0(8) . . ? N4 C6 C1 119.3(9) . . ? O1 C7 N3 124.4(9) . . ? O1 C7 C8 118.8(9) . . ? N3 C7 C8 116.8(9) . . ? C9 C8 C13 120.3(9) . . ? C9 C8 C7 118.1(8) . . ? C13 C8 C7 121.3(10) . . ? O2 C9 C8 123.9(8) . . ? O2 C9 C10 116.7(9) . . ? C8 C9 C10 119.4(9) . . ? C11 C10 O3 127.1(9) . . ? C11 C10 C9 120.0(10) . . ? O3 C10 C9 112.8(8) . . ? C10 C11 C12 119.9(10) . . ? C13 C12 C11 121.3(10) . . ? C12 C13 C8 119.1(11) . . ? N5 C15 C16 123.4(9) . . ? N5 C15 C20 114.1(8) . . ? C16 C15 C20 122.4(9) . . ? C17 C16 C15 118.4(10) . . ? C16 C17 C18 120.4(11) . . ? C17 C18 C19 117.1(10) . . ? N5 C19 C18 123.9(10) . . ? N6 C20 N8 126.1(9) . . ? N6 C20 C15 113.8(8) . . ? N8 C20 C15 120.0(9) . . ? O4 C21 N7 120.7(9) . . ? O4 C21 C22 122.1(9) . 3_756 ? N7 C21 C22 117.0(8) . 3_756 ? C27 C22 C23 120.1(9) . . ? C27 C22 C21 118.2(9) . 3_756 ? C23 C22 C21 121.3(9) . 3_756 ? O5 C23 C22 124.6(8) . . ? O5 C23 C24 119.5(8) . . ? C22 C23 C24 115.9(9) . . ? C25 C24 O6 126.2(9) . . ? C25 C24 C23 123.5(10) . . ? O6 C24 C23 110.2(9) . . ? C24 C25 C26 118.4(10) . . ? C27 C26 C25 119.8(10) . . ? C26 C27 C22 121.6(10) . . ? N9 C29 C30 122.0(9) . . ? N9 C29 C34 114.7(9) . . ? C30 C29 C34 122.7(9) . . ? C29 C30 C31 120.1(10) . . ? C32 C31 C30 118.1(10) . . ? C33 C32 C31 118.7(10) . . ? C32 C33 N9 124.8(10) . . ? N10 C34 N12 125.9(10) . . ? N10 C34 C29 115.2(9) . . ? N12 C34 C29 118.9(9) . . ? N11 C35 O7 124.0(9) . . ? N11 C35 C36 116.8(9) . . ? O7 C35 C36 119.2(9) . . ? C37 C36 C41 119.8(9) . . ? C37 C36 C35 119.9(9) . . ? C41 C36 C35 120.3(9) . . ? O8 C37 C36 120.6(9) . . ? O8 C37 C38 120.6(9) . . ? C36 C37 C38 118.7(9) . . ? O9 C38 C39 119.6(10) . . ? O9 C38 C37 119.8(9) . . ? C39 C38 C37 120.2(10) . . ? C38 C39 C40 121.0(11) . . ? C41 C40 C39 118.7(11) . . ? C40 C41 C36 121.5(11) . . ? N13 C43 C44 120.7(11) . . ? N13 C43 C48 114.8(10) . . ? C44 C43 C48 124.5(11) . . ? C45 C44 C43 120.1(11) . . ? C44 C45 C46 118.9(12) . . ? C47 C46 C45 118.7(13) . . ? N13 C47 C46 124.1(11) . . ? N14 C48 N16 120.9(12) . . ? N14 C48 C43 118.1(10) . . ? N16 C48 C43 121.0(11) . . ? N15 C49 O10 123.9(10) . . ? N15 C49 C50 120.4(10) . . ? O10 C49 C50 115.7(10) . . ? C51 C50 C55 118.5(11) . . ? C51 C50 C49 122.3(10) . . ? C55 C50 C49 119.1(11) . . ? O11 C51 C50 124.2(10) . . ? O11 C51 C52 114.9(10) . . ? C50 C51 C52 120.8(11) . . ? O12 C52 C53 125.5(12) . . ? O12 C52 C51 114.9(11) . . ? C53 C52 C51 119.6(12) . . ? C52 C53 C54 119.2(12) . . ? C55 C54 C53 121.2(13) . . ? C54 C55 C50 120.5(13) . . ? O15 C57 O14 122.1(9) . . ? O15 C57 O13 122.1(9) . . ? O14 C57 O13 115.8(8) . . ? N17 C58 S1 179.0(15) . . ? N18 C60 C59 176(2) . . ? N19 C62 C61 178.1(14) . . ? N20 C64 C63 177(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.656 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.263