# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef 'complexes.cif' # SUBMISSION DETAILS _publ_contact_author_name 'Jianzhuang Jiang' _publ_contact_author_address ; Department of Chemistry, University of Science and Technology Beijing, Beijing 100083, China ; _publ_contact_author_email xiaolongz@126.com _publ_contact_author_fax ? _publ_contact_author_phone ? # TITLE AND AUTHOR LIST _publ_section_title ; xxx ; _publ_author_name 'Hailong Wang' #======================================================================= data_1a _database_code_depnum_ccdc_archive 'CCDC 849698' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H46 Cl10 Dy N12 O5' _chemical_formula_weight 1760.28 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' Dy Dy -0.1892 4.4098 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.436(5) _cell_length_b 19.024(2) _cell_length_c 26.273(3) _cell_angle_alpha 90.00 _cell_angle_beta 127.986(3) _cell_angle_gamma 90.00 _cell_volume 15141(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8526 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7040 _exptl_absorpt_coefficient_mu 1.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7670 _exptl_absorpt_correction_T_max 0.8499 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 36641 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13255 _reflns_number_gt 10763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXL97 _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^)+(0.1012P)^2^+10.3956P] 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 13255 _refine_ls_number_parameters 966 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.26921(15) 0.1812(2) 0.1055(2) 0.0349(10) Uani 1 1 d . . . C2 C 0.24037(15) 0.2389(2) 0.0957(2) 0.0357(10) Uani 1 1 d . . . C3 C 0.24183(18) 0.2869(3) 0.1366(3) 0.0460(12) Uani 1 1 d . . . H3 H 0.2648 0.2862 0.1808 0.055 Uiso 1 1 calc R . . C4 C 0.20867(19) 0.3351(3) 0.1104(3) 0.0516(13) Uani 1 1 d . . . H4 H 0.2085 0.3664 0.1375 0.062 Uiso 1 1 calc R . . C5 C 0.17539(18) 0.3385(3) 0.0448(3) 0.0489(12) Uani 1 1 d . . . H5 H 0.1534 0.3722 0.0286 0.059 Uiso 1 1 calc R . . C6 C 0.17392(18) 0.2928(2) 0.0022(3) 0.0454(12) Uani 1 1 d . . . H6 H 0.1522 0.2962 -0.0423 0.055 Uiso 1 1 calc R . . C7 C 0.20663(16) 0.2420(2) 0.0298(2) 0.0375(10) Uani 1 1 d . . . C8 C 0.21449(15) 0.1833(2) 0.0013(2) 0.0332(9) Uani 1 1 d . . . C9 C 0.19823(15) 0.1259(2) -0.0896(2) 0.0350(10) Uani 1 1 d . . . C10 C 0.17342(16) 0.1235(2) -0.1593(2) 0.0390(10) Uani 1 1 d . . . C11 C 0.13688(18) 0.1624(3) -0.2097(2) 0.0498(13) Uani 1 1 d . . . H11 H 0.1234 0.1968 -0.2022 0.060 Uiso 1 1 calc R . . C12 C 0.1222(2) 0.1454(3) -0.2722(2) 0.0597(15) Uani 1 1 d . . . H12 H 0.0978 0.1688 -0.3074 0.072 Uiso 1 1 calc R . . C13 C 0.1426(2) 0.0962(3) -0.2828(3) 0.0609(15) Uani 1 1 d . . . H13 H 0.1316 0.0868 -0.3250 0.073 Uiso 1 1 calc R . . C14 C 0.17960(19) 0.0588(3) -0.2323(2) 0.0524(13) Uani 1 1 d . . . H14 H 0.1938 0.0258 -0.2399 0.063 Uiso 1 1 calc R . . C15 C 0.19373(16) 0.0737(2) -0.1709(2) 0.0393(10) Uani 1 1 d . . . C16 C 0.23143(16) 0.0483(2) -0.1076(2) 0.0356(10) Uani 1 1 d . . . C17 C 0.30085(16) -0.0045(2) -0.0441(2) 0.0352(10) Uani 1 1 d . . . C18 C 0.33809(17) -0.0340(2) -0.0399(2) 0.0402(11) Uani 1 1 d . . . C19 C 0.34020(19) -0.0629(3) -0.0857(3) 0.0525(13) Uani 1 1 d . . . H19 H 0.3151 -0.0685 -0.1283 0.063 Uiso 1 1 calc R . . C20 C 0.3820(2) -0.0838(3) -0.0652(3) 0.0669(17) Uani 1 1 d . . . H20 H 0.3849 -0.1046 -0.0944 0.080 Uiso 1 1 calc R . . C21 C 0.4189(2) -0.0737(3) -0.0021(3) 0.0626(15) Uani 1 1 d . . . H21 H 0.4463 -0.0871 0.0101 0.075 Uiso 1 1 calc R . . C22 C 0.41645(19) -0.0445(3) 0.0434(3) 0.0545(13) Uani 1 1 d . . . H22 H 0.4417 -0.0375 0.0857 0.065 Uiso 1 1 calc R . . C23 C 0.37504(18) -0.0257(2) 0.0241(3) 0.0422(11) Uani 1 1 d . . . C24 C 0.35916(16) 0.0048(3) 0.0574(2) 0.0385(10) Uani 1 1 d . . . C25 C 0.37503(15) 0.0602(3) 0.1490(2) 0.0408(11) Uani 1 1 d . . . C26 C 0.40742(15) 0.0870(3) 0.2146(2) 0.0452(12) Uani 1 1 d . . . C27 C 0.45324(18) 0.0797(3) 0.2595(3) 0.0625(15) Uani 1 1 d . . . H27 H 0.4693 0.0534 0.2505 0.075 Uiso 1 1 calc R . . C28 C 0.4736(2) 0.1135(4) 0.3183(3) 0.076(2) Uani 1 1 d . . . H28 H 0.5040 0.1093 0.3496 0.091 Uiso 1 1 calc R . . C29 C 0.4499(2) 0.1537(4) 0.3321(3) 0.0713(18) Uani 1 1 d . . . H29 H 0.4649 0.1754 0.3722 0.086 Uiso 1 1 calc R . . C30 C 0.40502(19) 0.1618(3) 0.2875(2) 0.0570(14) Uani 1 1 d . . . H30 H 0.3892 0.1887 0.2965 0.068 Uiso 1 1 calc R . . C31 C 0.38409(16) 0.1280(3) 0.2280(2) 0.0452(12) Uani 1 1 d . . . C32 C 0.33773(16) 0.1272(2) 0.1690(2) 0.0377(10) Uani 1 1 d . . . C33 C 0.23491(15) 0.0544(2) 0.1394(2) 0.0352(10) Uani 1 1 d . . . C34 C 0.25646(17) 0.0713(3) 0.2059(2) 0.0439(11) Uani 1 1 d . . . H34 H 0.2450 0.0986 0.2218 0.053 Uiso 1 1 calc R . . C35 C 0.29605(17) 0.0405(3) 0.2406(2) 0.0478(12) Uani 1 1 d . . . H35 H 0.3174 0.0431 0.2852 0.057 Uiso 1 1 calc R . . C36 C 0.29983(15) 0.0030(3) 0.1973(2) 0.0358(10) Uani 1 1 d . . . C37 C 0.33409(15) -0.0443(3) 0.2160(2) 0.0396(10) Uani 1 1 d . . . C38 C 0.33700(15) -0.0847(2) 0.1745(2) 0.0365(10) Uani 1 1 d . . . C39 C 0.36662(18) -0.1437(3) 0.1949(3) 0.0555(14) Uani 1 1 d . . . H39 H 0.3881 -0.1580 0.2373 0.067 Uiso 1 1 calc R . . C40 C 0.35757(18) -0.1741(3) 0.1418(3) 0.0527(13) Uani 1 1 d . . . H40 H 0.3719 -0.2127 0.1405 0.063 Uiso 1 1 calc R . . C41 C 0.32114(15) -0.1352(2) 0.0869(2) 0.0380(10) Uani 1 1 d . . . C42 C 0.29871(15) -0.1563(2) 0.0220(2) 0.0368(10) Uani 1 1 d . . . C43 C 0.25761(15) -0.1304(2) -0.0304(2) 0.0354(10) Uani 1 1 d . . . C44 C 0.23229(17) -0.1585(3) -0.0955(2) 0.0442(11) Uani 1 1 d . . . H44 H 0.2420 -0.1912 -0.1106 0.053 Uiso 1 1 calc R . . C45 C 0.19202(17) -0.1285(3) -0.1300(2) 0.0443(11) Uani 1 1 d . . . H45 H 0.1686 -0.1371 -0.1731 0.053 Uiso 1 1 calc R . . C46 C 0.19208(14) -0.0806(2) -0.0876(2) 0.0332(9) Uani 1 1 d . . . C47 C 0.15488(14) -0.0434(2) -0.1048(2) 0.0355(10) Uani 1 1 d . . . C48 C 0.15251(15) 0.0007(3) -0.0639(2) 0.0352(10) Uani 1 1 d . . . C49 C 0.11157(17) 0.0282(3) -0.0804(3) 0.0455(12) Uani 1 1 d . . . H49 H 0.0838 0.0246 -0.1202 0.055 Uiso 1 1 calc R . . C50 C 0.12148(16) 0.0606(3) -0.0265(2) 0.0418(11) Uani 1 1 d . . . H50 H 0.1019 0.0831 -0.0224 0.050 Uiso 1 1 calc R . . C51 C 0.16894(14) 0.0527(2) 0.0232(2) 0.0336(9) Uani 1 1 d . . . C52 C 0.19120(15) 0.0716(2) 0.0882(2) 0.0346(10) Uani 1 1 d . . . C53 C 0.36871(15) -0.0564(3) 0.2875(2) 0.0392(10) Uani 1 1 d . . . C58 C 0.41215(19) -0.0394(4) 0.3177(3) 0.0617(15) Uani 1 1 d . . . H58 H 0.4202 -0.0210 0.2935 0.074 Uiso 1 1 calc R . . C57 C 0.44471(19) -0.0494(4) 0.3844(3) 0.0687(17) Uani 1 1 d . . . H57 H 0.4739 -0.0364 0.4049 0.082 Uiso 1 1 calc R . . C56 C 0.43182(18) -0.0794(3) 0.4187(2) 0.0544(14) Uani 1 1 d . . . C55 C 0.3891(2) -0.0962(3) 0.3893(3) 0.0572(14) Uani 1 1 d . . . H55 H 0.3810 -0.1150 0.4133 0.069 Uiso 1 1 calc R . . C54 C 0.35776(18) -0.0854(3) 0.3241(2) 0.0523(13) Uani 1 1 d . . . H54 H 0.3286 -0.0979 0.3043 0.063 Uiso 1 1 calc R . . C59 C 0.31884(16) -0.2152(2) 0.0111(2) 0.0397(10) Uani 1 1 d . . . C60 C 0.29844(17) -0.2796(2) -0.0127(3) 0.0437(11) Uani 1 1 d . . . H60 H 0.2710 -0.2863 -0.0221 0.052 Uiso 1 1 calc R . . C61 C 0.31699(17) -0.3344(3) -0.0229(3) 0.0456(12) Uani 1 1 d . . . H61 H 0.3025 -0.3774 -0.0385 0.055 Uiso 1 1 calc R . . C62 C 0.35771(18) -0.3242(3) -0.0095(2) 0.0471(12) Uani 1 1 d . . . C63 C 0.37954(17) -0.2611(3) 0.0157(3) 0.0513(13) Uani 1 1 d . . . H63 H 0.4071 -0.2548 0.0257 0.062 Uiso 1 1 calc R . . C64 C 0.36047(16) -0.2075(3) 0.0259(3) 0.0454(11) Uani 1 1 d . . . H64 H 0.3755 -0.1652 0.0430 0.055 Uiso 1 1 calc R . . C65 C 0.11210(15) -0.0588(3) -0.1698(2) 0.0405(10) Uani 1 1 d . . . C66 C 0.09079(19) -0.1220(3) -0.1822(3) 0.0622(15) Uani 1 1 d . . . H66 H 0.1033 -0.1555 -0.1495 0.075 Uiso 1 1 calc R . . C67 C 0.0518(2) -0.1372(4) -0.2409(3) 0.0722(18) Uani 1 1 d . . . H67 H 0.0379 -0.1800 -0.2477 0.087 Uiso 1 1 calc R . . C68 C 0.03362(18) -0.0896(4) -0.2890(3) 0.0625(16) Uani 1 1 d . . . C69 C 0.0529(2) -0.0267(4) -0.2794(3) 0.078(2) Uani 1 1 d . . . H69 H 0.0399 0.0060 -0.3127 0.093 Uiso 1 1 calc R . . C70 C 0.0920(2) -0.0112(3) -0.2198(3) 0.071(2) Uani 1 1 d . . . H70 H 0.1051 0.0324 -0.2133 0.086 Uiso 1 1 calc R . . C71 C 0.16487(15) 0.1049(2) 0.1064(2) 0.0373(10) Uani 1 1 d . . . C76 C 0.14890(19) 0.1728(3) 0.0876(3) 0.0555(14) Uani 1 1 d . . . H76 H 0.1536 0.1980 0.0620 0.067 Uiso 1 1 calc R . . C75 C 0.1255(2) 0.2036(3) 0.1072(4) 0.0727(19) Uani 1 1 d . . . H75 H 0.1144 0.2489 0.0944 0.087 Uiso 1 1 calc R . . C74 C 0.1196(2) 0.1653(3) 0.1455(3) 0.0642(16) Uani 1 1 d . . . C73 C 0.1332(2) 0.0986(4) 0.1620(3) 0.0679(17) Uani 1 1 d . . . H73 H 0.1274 0.0729 0.1862 0.081 Uiso 1 1 calc R . . C72 C 0.1560(2) 0.0684(3) 0.1421(3) 0.0565(14) Uani 1 1 d . . . H72 H 0.1656 0.0221 0.1535 0.068 Uiso 1 1 calc R . . C77 C 0.2278(3) -0.2174(6) 0.1784(4) 0.119(4) Uani 1 1 d . . . H77 H 0.2204 -0.2219 0.1356 0.143 Uiso 1 1 calc R . . C78 C 0.0636(4) 0.2084(6) -0.1343(8) 0.239(11) Uani 1 1 d . . . H78 H 0.0908 0.1811 -0.1143 0.287 Uiso 1 1 calc R . . C79 C -0.0112(3) -0.3238(5) -0.1950(4) 0.095(2) Uani 1 1 d . . . H79A H -0.0090 -0.3174 -0.1569 0.143 Uiso 1 1 calc R . . H79B H -0.0165 -0.3725 -0.2071 0.143 Uiso 1 1 calc R . . H79C H -0.0352 -0.2960 -0.2295 0.143 Uiso 1 1 calc R . . N8 N 0.30810(12) 0.1699(2) 0.16232(17) 0.0370(8) Uani 1 1 d . . . N1 N 0.25137(12) 0.14650(18) 0.04841(17) 0.0342(8) Uani 1 1 d . . . N2 N 0.18874(13) 0.1729(2) -0.06214(18) 0.0387(9) Uani 1 1 d . . . N3 N 0.23173(12) 0.07848(19) -0.06047(18) 0.0348(8) Uani 1 1 d . . . N4 N 0.26185(14) 0.0069(2) -0.10074(19) 0.0382(9) Uani 1 1 d . . . N5 N 0.31482(13) 0.01512(19) 0.01606(19) 0.0353(9) Uani 1 1 d . . . N6 N 0.38725(14) 0.0229(2) 0.1198(2) 0.0430(10) Uani 1 1 d . . . N7 N 0.33360(12) 0.08345(19) 0.12435(17) 0.0358(8) Uani 1 1 d . . . N9 N 0.26285(12) 0.01518(18) 0.13458(18) 0.0327(8) Uani 1 1 d . . . N10 N 0.30948(12) -0.08013(19) 0.10773(17) 0.0349(8) Uani 1 1 d . . . N11 N 0.23319(12) -0.08067(18) -0.02758(17) 0.0327(8) Uani 1 1 d . . . N12 N 0.18671(12) 0.01826(17) -0.00167(18) 0.0317(8) Uani 1 1 d . . . Dy1 Dy 0.264353(6) 0.020422(10) 0.043905(9) 0.02854(10) Uani 1 1 d . . . Cl1 Cl 0.47206(6) -0.09268(12) 0.50116(7) 0.0923(6) Uani 1 1 d . . . Cl4 Cl 0.09288(10) 0.20461(13) 0.17308(15) 0.1260(10) Uani 1 1 d . . . Cl3 Cl -0.01617(6) -0.10830(14) -0.36485(9) 0.1018(7) Uani 1 1 d . . . Cl2 Cl 0.38083(5) -0.39113(8) -0.02459(8) 0.0702(4) Uani 1 1 d . . . Cl5 Cl 0.18744(12) -0.25827(18) 0.17896(17) 0.1636(14) Uani 1 1 d . . . Cl6 Cl 0.27978(10) -0.25668(19) 0.23738(14) 0.1493(12) Uani 1 1 d . . . Cl7 Cl 0.23084(8) -0.12809(12) 0.19796(12) 0.1084(7) Uani 1 1 d . . . Cl8 Cl 0.06115(12) 0.2554(3) -0.06615(18) 0.1919(18) Uani 1 1 d . . . Cl9 Cl 0.06146(11) 0.27014(19) -0.17314(16) 0.1491(11) Uani 1 1 d . . . Cl10 Cl 0.01712(16) 0.1527(3) -0.1650(3) 0.264(3) Uani 1 1 d . . . O1 O 0.0291(2) -0.3021(3) -0.1824(3) 0.113(2) Uani 1 1 d . . . H1 H 0.0501 -0.3179 -0.1475 0.170 Uiso 1 1 calc R . . O2 O -0.0254(2) -0.4173(4) -0.2670(6) 0.202(5) Uani 1 1 d . . . O3 O 0.0691(3) 0.2395(5) -0.4328(3) 0.156(3) Uani 1 1 d . . . O4 O 0.0479(2) 0.0078(6) -0.4576(7) 0.245(7) Uani 1 1 d . . . O5 O 0.0060(4) -0.2751(6) -0.0618(6) 0.223(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(2) 0.038(2) 0.033(2) -0.0034(18) 0.025(2) -0.0089(19) C2 0.044(3) 0.033(2) 0.034(2) -0.0039(18) 0.026(2) -0.0068(19) C3 0.055(3) 0.046(3) 0.042(3) -0.006(2) 0.033(3) -0.008(2) C4 0.072(4) 0.041(3) 0.061(4) -0.005(2) 0.051(3) -0.002(3) C5 0.058(3) 0.039(3) 0.066(4) 0.004(2) 0.047(3) 0.003(2) C6 0.057(3) 0.039(3) 0.050(3) 0.004(2) 0.038(3) 0.003(2) C7 0.046(3) 0.034(2) 0.041(3) -0.0006(19) 0.031(2) -0.005(2) C8 0.040(2) 0.034(2) 0.028(2) 0.0004(18) 0.022(2) -0.0012(19) C9 0.038(2) 0.034(2) 0.028(2) 0.0016(18) 0.018(2) -0.0016(19) C10 0.043(3) 0.038(2) 0.029(2) 0.0005(19) 0.018(2) -0.003(2) C11 0.061(3) 0.040(3) 0.034(3) 0.008(2) 0.022(3) 0.004(2) C12 0.066(4) 0.058(3) 0.026(3) 0.008(2) 0.014(3) 0.008(3) C13 0.076(4) 0.062(3) 0.028(3) 0.001(2) 0.023(3) 0.004(3) C14 0.067(3) 0.052(3) 0.030(3) -0.003(2) 0.025(3) 0.003(3) C15 0.047(3) 0.039(2) 0.029(2) 0.0003(19) 0.022(2) -0.004(2) C16 0.047(3) 0.035(2) 0.025(2) 0.0002(18) 0.022(2) -0.004(2) C17 0.045(3) 0.034(2) 0.038(3) 0.001(2) 0.031(2) -0.002(2) C18 0.052(3) 0.039(2) 0.045(3) 0.004(2) 0.038(3) 0.000(2) C19 0.060(3) 0.060(3) 0.054(3) 0.000(3) 0.044(3) 0.001(3) C20 0.082(5) 0.070(4) 0.081(5) 0.005(3) 0.067(4) 0.012(3) C21 0.056(3) 0.078(4) 0.076(4) 0.001(3) 0.052(4) 0.005(3) C22 0.048(3) 0.064(3) 0.058(3) -0.003(3) 0.036(3) -0.003(3) C23 0.047(3) 0.042(3) 0.049(3) 0.001(2) 0.036(3) -0.002(2) C24 0.039(3) 0.043(2) 0.040(3) 0.002(2) 0.027(2) -0.003(2) C25 0.039(3) 0.049(3) 0.035(2) -0.002(2) 0.023(2) -0.006(2) C26 0.034(2) 0.062(3) 0.034(3) -0.001(2) 0.018(2) -0.005(2) C27 0.037(3) 0.087(4) 0.048(3) -0.004(3) 0.018(3) -0.009(3) C28 0.044(3) 0.100(5) 0.048(4) -0.007(3) 0.010(3) -0.018(3) C29 0.057(4) 0.085(4) 0.032(3) -0.011(3) 0.007(3) -0.011(3) C30 0.061(3) 0.057(3) 0.034(3) -0.006(2) 0.019(3) -0.002(3) C31 0.044(3) 0.046(3) 0.034(3) 0.000(2) 0.018(2) -0.006(2) C32 0.039(2) 0.041(2) 0.028(2) -0.0003(19) 0.018(2) -0.006(2) C33 0.044(3) 0.034(2) 0.033(2) 0.0002(18) 0.027(2) -0.002(2) C34 0.049(3) 0.052(3) 0.033(2) -0.001(2) 0.026(2) 0.008(2) C35 0.047(3) 0.063(3) 0.026(2) -0.002(2) 0.019(2) 0.007(3) C36 0.032(2) 0.048(2) 0.026(2) 0.004(2) 0.017(2) -0.001(2) C37 0.037(2) 0.053(3) 0.023(2) 0.006(2) 0.015(2) -0.001(2) C38 0.034(2) 0.046(3) 0.027(2) 0.0055(19) 0.017(2) 0.004(2) C39 0.056(3) 0.065(3) 0.033(3) 0.016(2) 0.021(3) 0.026(3) C40 0.059(3) 0.052(3) 0.046(3) 0.008(2) 0.031(3) 0.023(3) C41 0.044(3) 0.038(2) 0.037(3) 0.0058(19) 0.027(2) 0.006(2) C42 0.041(2) 0.035(2) 0.040(3) 0.0017(19) 0.028(2) -0.0014(19) C43 0.038(2) 0.036(2) 0.033(2) -0.0023(19) 0.023(2) -0.0025(19) C44 0.053(3) 0.045(3) 0.039(3) -0.006(2) 0.030(2) 0.004(2) C45 0.046(3) 0.047(3) 0.033(3) -0.006(2) 0.021(2) -0.003(2) C46 0.034(2) 0.035(2) 0.029(2) -0.0006(18) 0.018(2) -0.0038(18) C47 0.033(2) 0.037(2) 0.029(2) -0.0003(19) 0.015(2) -0.0044(19) C48 0.036(2) 0.036(2) 0.035(3) -0.001(2) 0.022(2) 0.000(2) C49 0.035(3) 0.051(3) 0.036(3) -0.001(2) 0.014(2) 0.004(2) C50 0.039(2) 0.047(3) 0.038(3) -0.001(2) 0.023(2) 0.003(2) C51 0.034(2) 0.033(2) 0.031(2) 0.0018(18) 0.019(2) -0.0019(19) C52 0.041(2) 0.033(2) 0.036(2) 0.0016(18) 0.027(2) -0.0006(19) C53 0.041(3) 0.047(3) 0.029(2) 0.007(2) 0.021(2) 0.007(2) C58 0.045(3) 0.093(4) 0.038(3) 0.021(3) 0.022(3) 0.004(3) C57 0.037(3) 0.108(5) 0.040(3) 0.015(3) 0.013(3) 0.000(3) C56 0.050(3) 0.065(3) 0.028(3) 0.009(2) 0.014(2) 0.010(3) C55 0.066(4) 0.074(4) 0.034(3) 0.011(3) 0.032(3) 0.011(3) C54 0.045(3) 0.070(4) 0.037(3) 0.010(2) 0.023(2) 0.000(3) C59 0.047(3) 0.039(2) 0.036(3) 0.0019(19) 0.027(2) 0.002(2) C60 0.051(3) 0.041(3) 0.054(3) 0.005(2) 0.040(3) -0.002(2) C61 0.057(3) 0.032(2) 0.055(3) 0.003(2) 0.039(3) 0.000(2) C62 0.057(3) 0.044(3) 0.043(3) 0.007(2) 0.032(3) 0.016(2) C63 0.044(3) 0.048(3) 0.068(4) 0.002(3) 0.037(3) 0.006(2) C64 0.043(3) 0.038(3) 0.054(3) -0.006(2) 0.029(3) -0.003(2) C65 0.037(2) 0.049(3) 0.030(2) -0.006(2) 0.017(2) -0.002(2) C66 0.053(3) 0.064(4) 0.047(3) 0.001(3) 0.020(3) -0.011(3) C67 0.056(4) 0.069(4) 0.063(4) -0.020(3) 0.022(3) -0.030(3) C68 0.035(3) 0.095(5) 0.040(3) -0.017(3) 0.014(3) -0.007(3) C69 0.055(4) 0.095(5) 0.036(3) 0.014(3) 0.005(3) 0.001(3) C70 0.063(4) 0.065(4) 0.045(4) 0.010(3) 0.012(3) -0.013(3) C71 0.037(2) 0.041(2) 0.035(2) -0.0009(19) 0.022(2) -0.001(2) C76 0.071(4) 0.044(3) 0.074(4) 0.002(3) 0.056(3) -0.002(3) C75 0.096(5) 0.044(3) 0.125(6) -0.005(3) 0.092(5) 0.006(3) C74 0.070(4) 0.071(4) 0.085(4) -0.013(3) 0.065(4) -0.001(3) C73 0.090(5) 0.072(4) 0.080(4) 0.008(3) 0.072(4) 0.003(3) C72 0.069(4) 0.058(3) 0.062(4) 0.015(3) 0.051(3) 0.013(3) C77 0.130(8) 0.166(9) 0.060(5) 0.022(5) 0.058(5) 0.062(7) C78 0.132(10) 0.072(6) 0.228(16) 0.052(8) -0.033(10) -0.001(6) C79 0.073(5) 0.116(6) 0.073(5) 0.035(5) 0.033(4) 0.025(5) N8 0.037(2) 0.040(2) 0.030(2) -0.0030(16) 0.0178(18) -0.0041(17) N1 0.040(2) 0.0330(19) 0.0299(19) -0.0004(15) 0.0213(17) -0.0029(16) N2 0.046(2) 0.036(2) 0.034(2) 0.0010(16) 0.0247(19) 0.0000(17) N3 0.040(2) 0.034(2) 0.0295(19) -0.0003(15) 0.0215(17) -0.0028(16) N4 0.046(2) 0.042(2) 0.030(2) 0.0005(17) 0.025(2) -0.0023(18) N5 0.039(2) 0.039(2) 0.032(2) 0.0019(15) 0.0241(19) -0.0006(16) N6 0.031(2) 0.059(3) 0.036(2) 0.0008(18) 0.020(2) -0.0015(17) N7 0.036(2) 0.039(2) 0.030(2) -0.0031(16) 0.0191(17) -0.0050(16) N9 0.032(2) 0.034(2) 0.029(2) 0.0038(14) 0.0170(17) 0.0038(15) N10 0.037(2) 0.040(2) 0.0260(19) 0.0027(15) 0.0184(17) 0.0035(16) N11 0.036(2) 0.0333(19) 0.0292(19) -0.0011(15) 0.0205(17) -0.0013(15) N12 0.033(2) 0.034(2) 0.027(2) 0.0003(14) 0.0175(17) 0.0007(14) Dy1 0.03053(14) 0.03153(14) 0.02292(14) 0.00021(7) 0.01612(11) -0.00086(8) Cl1 0.0771(11) 0.1302(16) 0.0309(8) 0.0217(9) 0.0138(8) 0.0219(11) Cl4 0.168(2) 0.1170(17) 0.199(3) -0.0222(17) 0.167(2) 0.0067(16) Cl3 0.0504(9) 0.156(2) 0.0504(10) -0.0303(11) 0.0066(8) -0.0187(11) Cl2 0.0739(10) 0.0578(8) 0.0833(11) -0.0009(8) 0.0506(9) 0.0221(7) Cl5 0.149(3) 0.136(2) 0.136(3) -0.025(2) 0.053(2) -0.050(2) Cl6 0.139(2) 0.178(3) 0.105(2) 0.0185(19) 0.0619(18) 0.073(2) Cl7 0.0921(14) 0.0939(14) 0.1147(18) 0.0080(13) 0.0513(13) 0.0062(12) Cl8 0.129(2) 0.307(5) 0.120(3) 0.064(3) 0.067(2) 0.058(3) Cl9 0.139(2) 0.167(3) 0.130(2) 0.046(2) 0.078(2) 0.021(2) Cl10 0.182(4) 0.168(4) 0.287(6) 0.073(4) 0.067(4) -0.014(3) O1 0.129(5) 0.092(4) 0.067(4) 0.013(3) 0.035(4) 0.031(4) O2 0.121(6) 0.091(5) 0.417(16) -0.033(7) 0.177(9) -0.031(4) O3 0.169(7) 0.216(9) 0.100(5) 0.006(5) 0.092(5) 0.034(6) O4 0.047(4) 0.299(12) 0.302(14) 0.156(11) 0.064(6) 0.025(5) O5 0.191(9) 0.173(9) 0.226(12) 0.006(8) 0.088(9) -0.020(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N8 1.327(6) . ? C1 N1 1.375(6) . ? C1 C2 1.467(6) . ? C2 C7 1.385(7) . ? C2 C3 1.386(7) . ? C3 C4 1.364(7) . ? C3 H3 0.9300 . ? C4 C5 1.378(8) . ? C4 H4 0.9300 . ? C5 C6 1.391(7) . ? C5 H5 0.9300 . ? C6 C7 1.385(7) . ? C6 H6 0.9300 . ? C7 C8 1.476(6) . ? C8 N2 1.329(6) . ? C8 N1 1.368(6) . ? C9 N2 1.334(6) . ? C9 N3 1.358(6) . ? C9 C10 1.454(6) . ? C10 C15 1.376(7) . ? C10 C11 1.408(7) . ? C11 C12 1.407(7) . ? C11 H11 0.9300 . ? C12 C13 1.354(8) . ? C12 H12 0.9300 . ? C13 C14 1.402(8) . ? C13 H13 0.9300 . ? C14 C15 1.378(7) . ? C14 H14 0.9300 . ? C15 C16 1.460(6) . ? C16 N4 1.327(6) . ? C16 N3 1.359(6) . ? C17 N4 1.328(6) . ? C17 N5 1.371(6) . ? C17 C18 1.478(7) . ? C18 C19 1.369(7) . ? C18 C23 1.389(7) . ? C19 C20 1.402(8) . ? C19 H19 0.9300 . ? C20 C21 1.379(9) . ? C20 H20 0.9300 . ? C21 C22 1.372(8) . ? C21 H21 0.9300 . ? C22 C23 1.387(7) . ? C22 H22 0.9300 . ? C23 C24 1.461(7) . ? C24 N6 1.340(7) . ? C24 N5 1.358(6) . ? C25 N6 1.324(6) . ? C25 N7 1.371(6) . ? C25 C26 1.462(7) . ? C26 C31 1.387(7) . ? C26 C27 1.398(7) . ? C27 C28 1.387(9) . ? C27 H27 0.9300 . ? C28 C29 1.395(10) . ? C28 H28 0.9300 . ? C29 C30 1.374(8) . ? C29 H29 0.9300 . ? C30 C31 1.399(7) . ? C30 H30 0.9300 . ? C31 C32 1.476(7) . ? C32 N8 1.321(6) . ? C32 N7 1.365(6) . ? C33 N9 1.376(6) . ? C33 C52 1.399(6) . ? C33 C34 1.436(6) . ? C34 C35 1.335(7) . ? C34 H34 0.9300 . ? C35 C36 1.427(7) . ? C35 H35 0.9300 . ? C36 N9 1.380(6) . ? C36 C37 1.410(7) . ? C37 C38 1.395(7) . ? C37 C53 1.507(6) . ? C38 N10 1.385(6) . ? C38 C39 1.446(7) . ? C39 C40 1.343(7) . ? C39 H39 0.9300 . ? C40 C41 1.450(7) . ? C40 H40 0.9300 . ? C41 N10 1.379(6) . ? C41 C42 1.415(6) . ? C42 C43 1.398(6) . ? C42 C59 1.486(6) . ? C43 N11 1.367(6) . ? C43 C44 1.453(6) . ? C44 C45 1.348(7) . ? C44 H44 0.9300 . ? C45 C46 1.438(6) . ? C45 H45 0.9300 . ? C46 N11 1.385(6) . ? C46 C47 1.398(6) . ? C47 C48 1.408(7) . ? C47 C65 1.500(6) . ? C48 N12 1.367(6) . ? C48 C49 1.449(7) . ? C49 C50 1.366(7) . ? C49 H49 0.9300 . ? C50 C51 1.457(6) . ? C50 H50 0.9300 . ? C51 N12 1.367(6) . ? C51 C52 1.407(6) . ? C52 C71 1.500(6) . ? C53 C58 1.375(8) . ? C53 C54 1.380(7) . ? C58 C57 1.405(8) . ? C58 H58 0.9300 . ? C57 C56 1.389(8) . ? C57 H57 0.9300 . ? C56 C55 1.353(8) . ? C56 Cl1 1.740(5) . ? C55 C54 1.374(7) . ? C55 H55 0.9300 . ? C54 H54 0.9300 . ? C59 C60 1.379(7) . ? C59 C64 1.403(7) . ? C60 C61 1.381(7) . ? C60 H60 0.9300 . ? C61 C62 1.390(7) . ? C61 H61 0.9300 . ? C62 C63 1.378(7) . ? C62 Cl2 1.733(5) . ? C63 C64 1.375(7) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C66 1.376(7) . ? C65 C70 1.377(8) . ? C66 C67 1.365(8) . ? C66 H66 0.9300 . ? C67 C68 1.348(9) . ? C67 H67 0.9300 . ? C68 C69 1.346(9) . ? C68 Cl3 1.751(6) . ? C69 C70 1.379(9) . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C72 1.368(7) . ? C71 C76 1.384(7) . ? C76 C75 1.410(8) . ? C76 H76 0.9300 . ? C75 C74 1.371(9) . ? C75 H75 0.9300 . ? C74 C73 1.339(9) . ? C74 Cl4 1.746(5) . ? C73 C72 1.392(8) . ? C73 H73 0.9300 . ? C72 H72 0.9300 . ? C77 Cl5 1.742(12) . ? C77 Cl7 1.757(11) . ? C77 Cl6 1.773(9) . ? C77 H77 0.9800 . ? C78 Cl9 1.524(15) . ? C78 Cl10 1.787(14) . ? C78 Cl8 2.06(2) . ? C78 H78 0.9800 . ? C79 O1 1.429(10) . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? N1 Dy1 2.468(4) . ? N3 Dy1 2.466(4) . ? N5 Dy1 2.461(4) . ? N7 Dy1 2.463(4) . ? N9 Dy1 2.420(4) . ? N10 Dy1 2.429(4) . ? N11 Dy1 2.427(4) . ? N12 Dy1 2.438(4) . ? O1 H1 0.8200 . ? O2 O2 1.567(13) 2_554 ? 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 N8 C1 N1 127.6(4) . . ? N8 C1 C2 121.7(4) . . ? N1 C1 C2 110.6(4) . . ? C7 C2 C3 120.1(5) . . ? C7 C2 C1 106.1(4) . . ? C3 C2 C1 133.8(5) . . ? C4 C3 C2 118.2(5) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 121.5(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 121.6(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 116.2(5) . . ? C7 C6 H6 121.9 . . ? C5 C6 H6 121.9 . . ? C2 C7 C6 122.2(4) . . ? C2 C7 C8 106.0(4) . . ? C6 C7 C8 131.8(4) . . ? N2 C8 N1 128.1(4) . . ? N2 C8 C7 121.4(4) . . ? N1 C8 C7 110.5(4) . . ? N2 C9 N3 128.3(4) . . ? N2 C9 C10 121.1(4) . . ? N3 C9 C10 110.5(4) . . ? C15 C10 C11 121.8(4) . . ? C15 C10 C9 106.2(4) . . ? C11 C10 C9 132.0(5) . . ? C12 C11 C10 115.4(5) . . ? C12 C11 H11 122.3 . . ? C10 C11 H11 122.3 . . ? C13 C12 C11 122.1(5) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 122.4(5) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C15 C14 C13 116.2(5) . . ? C15 C14 H14 121.9 . . ? C13 C14 H14 121.9 . . ? C10 C15 C14 122.2(5) . . ? C10 C15 C16 106.0(4) . . ? C14 C15 C16 131.7(5) . . ? N4 C16 N3 127.9(4) . . ? N4 C16 C15 121.7(4) . . ? N3 C16 C15 110.2(4) . . ? N4 C17 N5 128.2(4) . . ? N4 C17 C18 121.2(4) . . ? N5 C17 C18 110.1(4) . . ? C19 C18 C23 122.6(5) . . ? C19 C18 C17 131.8(5) . . ? C23 C18 C17 105.6(4) . . ? C18 C19 C20 116.7(6) . . ? C18 C19 H19 121.6 . . ? C20 C19 H19 121.6 . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 122.2(5) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 117.6(6) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? C22 C23 C18 120.2(5) . . ? C22 C23 C24 133.7(5) . . ? C18 C23 C24 106.1(4) . . ? N6 C24 N5 127.7(4) . . ? N6 C24 C23 121.1(4) . . ? N5 C24 C23 111.1(4) . . ? N6 C25 N7 128.4(4) . . ? N6 C25 C26 121.4(4) . . ? N7 C25 C26 110.1(4) . . ? C31 C26 C27 121.1(5) . . ? C31 C26 C25 106.3(4) . . ? C27 C26 C25 132.6(5) . . ? C28 C27 C26 116.6(6) . . ? C28 C27 H27 121.7 . . ? C26 C27 H27 121.7 . . ? C27 C28 C29 122.2(6) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C30 C29 C28 121.2(6) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 117.3(6) . . ? C29 C30 H30 121.4 . . ? C31 C30 H30 121.4 . . ? C26 C31 C30 121.7(5) . . ? C26 C31 C32 106.2(4) . . ? C30 C31 C32 132.1(5) . . ? N8 C32 N7 128.8(4) . . ? N8 C32 C31 121.2(4) . . ? N7 C32 C31 109.6(4) . . ? N9 C33 C52 125.6(4) . . ? N9 C33 C34 109.6(4) . . ? C52 C33 C34 124.7(4) . . ? C35 C34 C33 107.2(4) . . ? C35 C34 H34 126.4 . . ? C33 C34 H34 126.4 . . ? C34 C35 C36 107.9(4) . . ? C34 C35 H35 126.1 . . ? C36 C35 H35 126.1 . . ? N9 C36 C37 125.4(4) . . ? N9 C36 C35 109.4(4) . . ? C37 C36 C35 124.9(4) . . ? C38 C37 C36 125.8(4) . . ? C38 C37 C53 117.2(4) . . ? C36 C37 C53 116.9(4) . . ? N10 C38 C37 126.2(4) . . ? N10 C38 C39 109.4(4) . . ? C37 C38 C39 124.1(4) . . ? C40 C39 C38 107.9(4) . . ? C40 C39 H39 126.0 . . ? C38 C39 H39 126.0 . . ? C39 C40 C41 106.7(4) . . ? C39 C40 H40 126.6 . . ? C41 C40 H40 126.6 . . ? N10 C41 C42 126.0(4) . . ? N10 C41 C40 110.1(4) . . ? C42 C41 C40 123.6(4) . . ? C43 C42 C41 124.6(4) . . ? C43 C42 C59 118.8(4) . . ? C41 C42 C59 116.3(4) . . ? N11 C43 C42 126.0(4) . . ? N11 C43 C44 109.5(4) . . ? C42 C43 C44 124.2(4) . . ? C45 C44 C43 107.2(4) . . ? C45 C44 H44 126.4 . . ? C43 C44 H44 126.4 . . ? C44 C45 C46 107.1(4) . . ? C44 C45 H45 126.4 . . ? C46 C45 H45 126.4 . . ? N11 C46 C47 126.2(4) . . ? N11 C46 C45 109.8(4) . . ? C47 C46 C45 123.9(4) . . ? C46 C47 C48 126.1(4) . . ? C46 C47 C65 117.1(4) . . ? C48 C47 C65 116.4(4) . . ? N12 C48 C47 126.3(4) . . ? N12 C48 C49 109.7(4) . . ? C47 C48 C49 123.7(4) . . ? C50 C49 C48 107.1(4) . . ? C50 C49 H49 126.4 . . ? C48 C49 H49 126.4 . . ? C49 C50 C51 106.2(4) . . ? C49 C50 H50 126.9 . . ? C51 C50 H50 126.9 . . ? N12 C51 C52 126.4(4) . . ? N12 C51 C50 109.8(4) . . ? C52 C51 C50 123.5(4) . . ? C33 C52 C51 125.5(4) . . ? C33 C52 C71 116.0(4) . . ? C51 C52 C71 118.0(4) . . ? C58 C53 C54 118.3(5) . . ? C58 C53 C37 120.8(4) . . ? C54 C53 C37 121.0(4) . . ? C53 C58 C57 121.5(5) . . ? C53 C58 H58 119.3 . . ? C57 C58 H58 119.3 . . ? C56 C57 C58 117.7(5) . . ? C56 C57 H57 121.2 . . ? C58 C57 H57 121.2 . . ? C55 C56 C57 121.2(5) . . ? C55 C56 Cl1 120.8(4) . . ? C57 C56 Cl1 117.9(4) . . ? C56 C55 C54 120.1(5) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C54 C53 121.2(5) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C60 C59 C64 116.9(4) . . ? C60 C59 C42 122.5(4) . . ? C64 C59 C42 120.6(4) . . ? C59 C60 C61 122.8(5) . . ? C59 C60 H60 118.6 . . ? C61 C60 H60 118.6 . . ? C60 C61 C62 118.7(5) . . ? C60 C61 H61 120.6 . . ? C62 C61 H61 120.6 . . ? C63 C62 C61 120.1(4) . . ? C63 C62 Cl2 120.2(4) . . ? C61 C62 Cl2 119.7(4) . . ? C64 C63 C62 119.9(5) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C59 121.5(5) . . ? C63 C64 H64 119.2 . . ? C59 C64 H64 119.2 . . ? C66 C65 C70 116.5(5) . . ? C66 C65 C47 121.1(4) . . ? C70 C65 C47 122.4(5) . . ? C67 C66 C65 122.1(6) . . ? C67 C66 H66 119.0 . . ? C65 C66 H66 119.0 . . ? C68 C67 C66 119.5(6) . . ? C68 C67 H67 120.2 . . ? C66 C67 H67 120.2 . . ? C69 C68 C67 120.8(5) . . ? C69 C68 Cl3 119.0(5) . . ? C67 C68 Cl3 120.2(5) . . ? C68 C69 C70 119.6(6) . . ? C68 C69 H69 120.2 . . ? C70 C69 H69 120.2 . . ? C65 C70 C69 121.4(6) . . ? C65 C70 H70 119.3 . . ? C69 C70 H70 119.3 . . ? C72 C71 C76 118.4(5) . . ? C72 C71 C52 120.4(4) . . ? C76 C71 C52 121.2(4) . . ? C71 C76 C75 120.0(5) . . ? C71 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C74 C75 C76 118.7(6) . . ? C74 C75 H75 120.7 . . ? C76 C75 H75 120.7 . . ? C73 C74 C75 122.2(5) . . ? C73 C74 Cl4 119.0(5) . . ? C75 C74 Cl4 118.9(5) . . ? C74 C73 C72 118.7(5) . . ? C74 C73 H73 120.6 . . ? C72 C73 H73 120.6 . . ? C71 C72 C73 121.9(5) . . ? C71 C72 H72 119.0 . . ? C73 C72 H72 119.0 . . ? Cl5 C77 Cl7 109.3(5) . . ? Cl5 C77 Cl6 109.6(6) . . ? Cl7 C77 Cl6 108.4(6) . . ? Cl5 C77 H77 109.9 . . ? Cl7 C77 H77 109.9 . . ? Cl6 C77 H77 109.9 . . ? Cl9 C78 Cl10 121.8(7) . . ? Cl9 C78 Cl8 103.5(8) . . ? Cl10 C78 Cl8 94.6(11) . . ? Cl9 C78 H78 111.6 . . ? Cl10 C78 H78 111.6 . . ? Cl8 C78 H78 111.6 . . ? O1 C79 H79A 109.5 . . ? O1 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? O1 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C32 N8 C1 122.1(4) . . ? C8 N1 C1 106.6(4) . . ? C8 N1 Dy1 125.5(3) . . ? C1 N1 Dy1 122.6(3) . . ? C8 N2 C9 122.5(4) . . ? C9 N3 C16 107.0(4) . . ? C9 N3 Dy1 125.6(3) . . ? C16 N3 Dy1 122.6(3) . . ? C16 N4 C17 122.8(4) . . ? C24 N5 C17 106.9(4) . . ? C24 N5 Dy1 126.8(3) . . ? C17 N5 Dy1 122.2(3) . . ? C25 N6 C24 122.7(4) . . ? C32 N7 C25 107.7(4) . . ? C32 N7 Dy1 121.8(3) . . ? C25 N7 Dy1 125.2(3) . . ? C33 N9 C36 105.7(4) . . ? C33 N9 Dy1 124.1(3) . . ? C36 N9 Dy1 123.4(3) . . ? C41 N10 C38 105.9(4) . . ? C41 N10 Dy1 126.4(3) . . ? C38 N10 Dy1 126.0(3) . . ? C43 N11 C46 106.2(3) . . ? C43 N11 Dy1 124.2(3) . . ? C46 N11 Dy1 123.7(3) . . ? C48 N12 C51 107.1(4) . . ? C48 N12 Dy1 125.2(3) . . ? C51 N12 Dy1 125.3(3) . . ? N9 Dy1 N11 115.44(12) . . ? N9 Dy1 N10 74.19(12) . . ? N11 Dy1 N10 73.31(13) . . ? N9 Dy1 N12 73.69(12) . . ? N11 Dy1 N12 74.61(12) . . ? N10 Dy1 N12 117.65(12) . . ? N9 Dy1 N5 142.34(13) . . ? N11 Dy1 N5 80.88(12) . . ? N10 Dy1 N5 79.30(12) . . ? N12 Dy1 N5 143.51(13) . . ? N9 Dy1 N7 80.98(12) . . ? N11 Dy1 N7 143.89(12) . . ? N10 Dy1 N7 81.70(12) . . ? N12 Dy1 N7 141.22(12) . . ? N5 Dy1 N7 69.01(12) . . ? N9 Dy1 N3 144.02(12) . . ? N11 Dy1 N3 79.83(12) . . ? N10 Dy1 N3 141.16(12) . . ? N12 Dy1 N3 80.23(12) . . ? N5 Dy1 N3 69.03(12) . . ? N7 Dy1 N3 106.12(12) . . ? N9 Dy1 N1 82.23(11) . . ? N11 Dy1 N1 142.11(12) . . ? N10 Dy1 N1 144.30(12) . . ? N12 Dy1 N1 79.47(12) . . ? N5 Dy1 N1 105.89(12) . . ? N7 Dy1 N1 68.24(12) . . ? N3 Dy1 N1 68.81(12) . . ? C79 O1 H1 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.538 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.123 #===END data_2a _database_code_depnum_ccdc_archive 'CCDC 849699' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H81 Cl7 Dy N12 O4' _chemical_formula_weight 1889.39 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' Dy Dy -0.1892 4.4098 '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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0680(5) _cell_length_b 17.6605(7) _cell_length_c 18.6659(7) _cell_angle_alpha 112.931(4) _cell_angle_beta 96.166(3) _cell_angle_gamma 97.426(3) _cell_volume 4171.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6986 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 27.96 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 29700 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.1121 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14580 _reflns_number_gt 11089 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0636P)^2^+8.9288P] 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 14580 _refine_ls_number_parameters 1090 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1527 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6452(5) 0.5884(4) 0.7841(4) 0.0151(14) Uani 1 1 d . . . C2 C 0.7322(5) 0.5893(4) 0.8349(4) 0.0193(15) Uani 1 1 d . . . C13 C 0.8942(5) 0.9560(4) 0.6516(4) 0.0287(17) Uani 1 1 d . . . H2A H 0.9211 0.9923 0.6309 0.034 Uiso 1 1 calc R . . C3 C 0.7577(5) 0.5343(4) 0.8669(4) 0.0247(16) Uani 1 1 d . . . H3 H 0.7156 0.4849 0.8571 0.030 Uiso 1 1 calc R . . C4 C 0.8482(5) 0.5558(5) 0.9140(4) 0.0298(18) Uani 1 1 d . . . H4 H 0.8674 0.5199 0.9360 0.036 Uiso 1 1 calc R . . C5 C 0.9111(5) 0.6298(5) 0.9291(4) 0.0288(18) Uani 1 1 d . . . H5 H 0.9704 0.6432 0.9626 0.035 Uiso 1 1 calc R . . C6 C 0.8877(5) 0.6846(4) 0.8954(4) 0.0250(17) Uani 1 1 d . . . C7 C 0.7966(5) 0.6618(4) 0.8472(4) 0.0204(15) Uani 1 1 d . . . C8 C 0.7478(5) 0.7009(4) 0.8007(4) 0.0186(15) Uani 1 1 d . . . C9 C 0.7571(5) 0.7908(4) 0.7364(4) 0.0152(14) Uani 1 1 d . . . C32 C 0.4982(5) 0.5111(4) 0.7005(4) 0.0198(15) Uani 1 1 d . . . C10 C 0.8166(5) 0.8507(4) 0.7159(4) 0.0205(15) Uani 1 1 d . . . C11 C 0.9123(5) 0.8932(4) 0.7464(4) 0.0273(17) Uani 1 1 d . . . H11 H 0.9492 0.8874 0.7877 0.033 Uiso 1 1 calc R . . C12 C 0.9499(5) 0.9450(5) 0.7116(4) 0.0316(18) Uani 1 1 d . . . H12 H 1.0142 0.9729 0.7292 0.038 Uiso 1 1 calc R . . C14 C 0.7975(5) 0.9128(4) 0.6218(4) 0.0263(17) Uani 1 1 d . . . C15 C 0.7598(5) 0.8592(4) 0.6551(4) 0.0191(15) Uani 1 1 d . . . C16 C 0.6675(5) 0.8035(4) 0.6392(4) 0.0195(15) Uani 1 1 d . . . C17 C 0.5219(5) 0.7269(4) 0.5551(4) 0.0188(15) Uani 1 1 d . . . C18 C 0.4580(5) 0.7035(4) 0.4794(4) 0.0203(15) Uani 1 1 d . . . C19 C 0.4576(5) 0.7425(4) 0.4283(4) 0.0208(15) Uani 1 1 d . . . H19 H 0.5009 0.7919 0.4398 0.025 Uiso 1 1 calc R . . C20 C 0.3900(5) 0.7050(4) 0.3591(4) 0.0229(16) Uani 1 1 d . . . H20 H 0.3864 0.7302 0.3237 0.028 Uiso 1 1 calc R . . C21 C 0.3274(5) 0.6302(5) 0.3416(4) 0.0262(17) Uani 1 1 d . . . H21 H 0.2833 0.6060 0.2944 0.031 Uiso 1 1 calc R . . C22 C 0.3291(5) 0.5902(4) 0.3940(4) 0.0214(16) Uani 1 1 d . . . C24 C 0.4232(5) 0.6105(4) 0.5339(4) 0.0172(15) Uani 1 1 d . . . C25 C 0.4156(5) 0.5198(4) 0.5981(4) 0.0173(15) Uani 1 1 d . . . C26 C 0.3737(5) 0.4381(4) 0.5969(4) 0.0181(15) Uani 1 1 d . . . C27 C 0.2993(5) 0.3754(4) 0.5453(4) 0.0246(16) Uani 1 1 d . . . H27 H 0.2668 0.3794 0.5011 0.030 Uiso 1 1 calc R . . C28 C 0.2751(5) 0.3065(4) 0.5619(4) 0.0253(16) Uani 1 1 d . . . H28 H 0.2251 0.2632 0.5283 0.030 Uiso 1 1 calc R . . C23 C 0.3954(5) 0.6284(4) 0.4649(4) 0.0180(15) Uani 1 1 d . . . C30 C 0.4007(5) 0.3629(4) 0.6784(4) 0.0210(16) Uani 1 1 d . . . C29 C 0.3233(5) 0.3004(4) 0.6270(4) 0.0243(16) Uani 1 1 d . . . H29 H 0.3040 0.2537 0.6371 0.029 Uiso 1 1 calc R . . C31 C 0.4246(5) 0.4324(4) 0.6622(4) 0.0174(15) Uani 1 1 d . . . C33 C 0.5410(5) 0.7172(4) 0.9165(4) 0.0159(14) Uani 1 1 d . . . C34 C 0.5047(5) 0.6710(4) 0.9599(4) 0.0202(15) Uani 1 1 d . . . H34 H 0.5350 0.6739 1.0079 0.024 Uiso 1 1 calc R . . C35 C 0.4188(5) 0.6229(4) 0.9178(4) 0.0187(15) Uani 1 1 d . . . H35 H 0.3785 0.5865 0.9315 0.022 Uiso 1 1 calc R . . C36 C 0.4007(5) 0.6385(4) 0.8474(4) 0.0193(15) Uani 1 1 d . . . C37 C 0.3144(5) 0.6039(4) 0.7913(4) 0.0170(14) Uani 1 1 d . . . C38 C 0.2901(5) 0.6255(4) 0.7274(4) 0.0181(15) Uani 1 1 d . . . C39 C 0.1979(5) 0.5924(4) 0.6733(4) 0.0224(16) Uani 1 1 d . . . H39 H 0.1498 0.5493 0.6704 0.027 Uiso 1 1 calc R . . C40 C 0.1951(5) 0.6359(4) 0.6283(4) 0.0241(16) Uani 1 1 d . . . H40 H 0.1455 0.6276 0.5874 0.029 Uiso 1 1 calc R . . C41 C 0.2836(5) 0.6981(4) 0.6553(4) 0.0173(15) Uani 1 1 d . . . C42 C 0.3008(4) 0.7654(4) 0.6332(4) 0.0165(14) Uani 1 1 d . . . C43 C 0.3825(5) 0.8303(4) 0.6648(4) 0.0185(15) Uani 1 1 d . . . C44 C 0.3893(5) 0.9073(4) 0.6533(4) 0.0244(16) Uani 1 1 d . . . H44 H 0.3442 0.9196 0.6211 0.029 Uiso 1 1 calc R . . C45 C 0.4729(5) 0.9578(4) 0.6978(4) 0.0262(17) Uani 1 1 d . . . H45 H 0.4971 1.0110 0.7016 0.031 Uiso 1 1 calc R . . C46 C 0.5183(5) 0.9132(4) 0.7391(4) 0.0176(15) Uani 1 1 d . . . C47 C 0.6033(5) 0.9506(4) 0.7975(4) 0.0174(14) Uani 1 1 d . . . C48 C 0.6404(5) 0.9159(4) 0.8472(4) 0.0174(15) Uani 1 1 d . . . C49 C 0.7239(5) 0.9566(4) 0.9099(4) 0.0183(15) Uani 1 1 d . . . H49 H 0.7652 1.0065 0.9198 0.022 Uiso 1 1 calc R . . C50 C 0.7308(5) 0.9093(4) 0.9511(4) 0.0194(15) Uani 1 1 d . . . H50 H 0.7778 0.9201 0.9946 0.023 Uiso 1 1 calc R . . C51 C 0.6523(5) 0.8390(4) 0.9153(4) 0.0192(15) Uani 1 1 d . . . C52 C 0.6250(5) 0.7806(4) 0.9464(4) 0.0181(15) Uani 1 1 d . . . C53 C 1.0941(10) 0.7753(7) 0.8140(6) 0.086(4) Uani 1 1 d . . . H53A H 1.1261 0.8102 0.7918 0.130 Uiso 1 1 calc R . . H53B H 1.0284 0.7528 0.7864 0.130 Uiso 1 1 calc R . . H53C H 1.1283 0.7304 0.8091 0.130 Uiso 1 1 calc R . . C54 C 1.0934(7) 0.8281(7) 0.9024(6) 0.067(3) Uani 1 1 d . . . H54A H 1.1601 0.8508 0.9297 0.080 Uiso 1 1 calc R . . H54B H 1.0614 0.8748 0.9069 0.080 Uiso 1 1 calc R . . C55 C 1.0427(5) 0.7793(5) 0.9428(5) 0.039(2) Uani 1 1 d . . . H55 H 1.0687 0.7278 0.9315 0.047 Uiso 1 1 calc R . . C56 C 1.0526(7) 0.8252(7) 1.0311(5) 0.061(3) Uani 1 1 d . . . H56A H 1.1212 0.8417 1.0540 0.073 Uiso 1 1 calc R . . H56B H 1.0228 0.7874 1.0519 0.073 Uiso 1 1 calc R . . C57 C 1.0067(9) 0.9021(8) 1.0561(6) 0.099(5) Uani 1 1 d . . . H57A H 1.0152 0.9281 1.1127 0.148 Uiso 1 1 calc R . . H57B H 0.9385 0.8863 1.0345 0.148 Uiso 1 1 calc R . . H57C H 1.0372 0.9408 1.0371 0.148 Uiso 1 1 calc R . . C58 C 0.8768(7) 1.0024(5) 0.4428(5) 0.052(2) Uani 1 1 d . . . H58A H 0.9122 0.9739 0.4023 0.077 Uiso 1 1 calc R . . H58B H 0.9213 1.0452 0.4868 0.077 Uiso 1 1 calc R . . H58C H 0.8304 1.0275 0.4223 0.077 Uiso 1 1 calc R . . C59 C 0.8248(6) 0.9415(5) 0.4691(5) 0.042(2) Uani 1 1 d . . . H59A H 0.8721 0.9154 0.4884 0.051 Uiso 1 1 calc R . . H59B H 0.7811 0.8978 0.4241 0.051 Uiso 1 1 calc R . . C60 C 0.7661(5) 0.9815(5) 0.5343(4) 0.0276(17) Uani 1 1 d . . . H60 H 0.8075 1.0314 0.5763 0.033 Uiso 1 1 calc R . . C61 C 0.6767(6) 1.0051(5) 0.5054(5) 0.044(2) Uani 1 1 d . . . H61A H 0.6334 0.9547 0.4674 0.053 Uiso 1 1 calc R . . H61B H 0.6945 1.0402 0.4781 0.053 Uiso 1 1 calc R . . C62 C 0.6219(7) 1.0513(6) 0.5705(6) 0.059(3) Uani 1 1 d . . . H62A H 0.5649 1.0640 0.5477 0.089 Uiso 1 1 calc R . . H62B H 0.6634 1.1023 0.6075 0.089 Uiso 1 1 calc R . . H62C H 0.6030 1.0166 0.5974 0.089 Uiso 1 1 calc R . . C63 C 0.0651(6) 0.5170(6) 0.3123(6) 0.056(3) Uani 1 1 d . . . H63A H 0.0147 0.5487 0.3117 0.084 Uiso 1 1 calc R . . H63B H 0.0369 0.4585 0.2903 0.084 Uiso 1 1 calc R . . H63C H 0.1116 0.5269 0.2814 0.084 Uiso 1 1 calc R . . C64 C 0.1145(6) 0.5431(5) 0.3950(5) 0.041(2) Uani 1 1 d . . . H64A H 0.0661 0.5344 0.4257 0.049 Uiso 1 1 calc R . . H64B H 0.1406 0.6027 0.4168 0.049 Uiso 1 1 calc R . . C65 C 0.1977(5) 0.4975(4) 0.4058(4) 0.0270(17) Uani 1 1 d . . . H65 H 0.2234 0.5173 0.4622 0.032 Uiso 1 1 calc R . . C66 C 0.1660(5) 0.4031(4) 0.3703(4) 0.0312(18) Uani 1 1 d . . . H66A H 0.2223 0.3785 0.3771 0.037 Uiso 1 1 calc R . . H66B H 0.1442 0.3842 0.3140 0.037 Uiso 1 1 calc R . . C67 C 0.0857(6) 0.3698(6) 0.4045(6) 0.048(2) Uani 1 1 d . . . H67A H 0.0706 0.3098 0.3782 0.072 Uiso 1 1 calc R . . H67B H 0.0287 0.3922 0.3969 0.072 Uiso 1 1 calc R . . H67C H 0.1070 0.3861 0.4599 0.072 Uiso 1 1 calc R . . C68 C 0.4238(8) 0.1777(5) 0.7223(5) 0.060(3) Uani 1 1 d . . . H68A H 0.4541 0.1345 0.7289 0.091 Uiso 1 1 calc R . . H68B H 0.4466 0.1895 0.6805 0.091 Uiso 1 1 calc R . . H68C H 0.3545 0.1592 0.7095 0.091 Uiso 1 1 calc R . . C69 C 0.4492(7) 0.2560(5) 0.7983(5) 0.040(2) Uani 1 1 d . . . H69A H 0.4265 0.2434 0.8404 0.048 Uiso 1 1 calc R . . H69B H 0.5194 0.2731 0.8119 0.048 Uiso 1 1 calc R . . C70 C 0.4052(5) 0.3273(4) 0.7927(4) 0.0258(17) Uani 1 1 d . . . H70 H 0.3356 0.3079 0.7711 0.031 Uiso 1 1 calc R . . C71 C 0.4197(6) 0.4048(5) 0.8705(4) 0.0359(19) Uani 1 1 d . . . H71A H 0.3899 0.3897 0.9088 0.043 Uiso 1 1 calc R . . H71B H 0.3872 0.4466 0.8620 0.043 Uiso 1 1 calc R . . C72 C 0.5281(6) 0.4426(5) 0.9040(5) 0.045(2) Uani 1 1 d . . . H72A H 0.5342 0.4910 0.9526 0.067 Uiso 1 1 calc R . . H72B H 0.5576 0.4585 0.8666 0.067 Uiso 1 1 calc R . . H72C H 0.5602 0.4018 0.9135 0.067 Uiso 1 1 calc R . . C73 C 0.2393(5) 0.5474(4) 0.8073(4) 0.0187(15) Uani 1 1 d . . . C74 C 0.1962(5) 0.5783(4) 0.8736(4) 0.0236(16) Uani 1 1 d . . . H74 H 0.2136 0.6348 0.9069 0.028 Uiso 1 1 calc R . . C75 C 0.1284(5) 0.5281(5) 0.8919(5) 0.0318(18) Uani 1 1 d . . . H75 H 0.1011 0.5503 0.9372 0.038 Uiso 1 1 calc R . . C76 C 0.1015(5) 0.4437(5) 0.8414(5) 0.0302(18) Uani 1 1 d . . . C77 C 0.1424(5) 0.4108(4) 0.7740(4) 0.0254(17) Uani 1 1 d . . . H77 H 0.1240 0.3544 0.7401 0.030 Uiso 1 1 calc R . . C78 C 0.2103(5) 0.4622(4) 0.7579(4) 0.0222(16) Uani 1 1 d . . . H78 H 0.2379 0.4399 0.7128 0.027 Uiso 1 1 calc R . . C79 C 0.2224(5) 0.7731(4) 0.5771(4) 0.0204(15) Uani 1 1 d . . . C80 C 0.1289(5) 0.7798(4) 0.5952(4) 0.0250(16) Uani 1 1 d . . . H80 H 0.1161 0.7814 0.6436 0.030 Uiso 1 1 calc R . . C81 C 0.0549(5) 0.7842(4) 0.5422(4) 0.0288(17) Uani 1 1 d . . . H81 H -0.0068 0.7894 0.5548 0.035 Uiso 1 1 calc R . . C82 C 0.0749(5) 0.7808(4) 0.4697(4) 0.0265(17) Uani 1 1 d . . . C83 C 0.1658(5) 0.7761(4) 0.4512(4) 0.0258(17) Uani 1 1 d . . . H83 H 0.1783 0.7751 0.4029 0.031 Uiso 1 1 calc R . . C84 C 0.2390(5) 0.7729(4) 0.5047(4) 0.0203(15) Uani 1 1 d . . . H84 H 0.3011 0.7705 0.4922 0.024 Uiso 1 1 calc R . . C85 C 0.6459(4) 1.0393(4) 0.8154(4) 0.0196(15) Uani 1 1 d . . . C86 C 0.6119(7) 1.1019(5) 0.8672(7) 0.076(4) Uani 1 1 d . . . H86 H 0.5628 1.0896 0.8927 0.092 Uiso 1 1 calc R . . C87 C 0.6487(8) 1.1855(5) 0.8838(8) 0.086(4) Uani 1 1 d . . . H87 H 0.6210 1.2276 0.9176 0.103 Uiso 1 1 calc R . . C88 C 0.7225(6) 1.2056(5) 0.8518(5) 0.037(2) Uani 1 1 d . . . C89 C 0.7584(8) 1.1442(6) 0.8010(6) 0.071(3) Uani 1 1 d . . . H89 H 0.8095 1.1571 0.7774 0.085 Uiso 1 1 calc R . . C90 C 0.7200(8) 1.0611(5) 0.7829(5) 0.066(3) Uani 1 1 d . . . H90 H 0.7462 1.0192 0.7473 0.080 Uiso 1 1 calc R . . C91 C 0.6830(5) 0.7924(4) 1.0236(4) 0.0212(15) Uani 1 1 d . . . C92 C 0.6905(5) 0.8666(4) 1.0919(4) 0.0281(17) Uani 1 1 d . . . H92 H 0.6568 0.9079 1.0896 0.034 Uiso 1 1 calc R . . C93 C 0.7470(6) 0.8789(5) 1.1618(4) 0.038(2) Uani 1 1 d . . . H93 H 0.7522 0.9283 1.2065 0.046 Uiso 1 1 calc R . . C94 C 0.7959(6) 0.8169(5) 1.1649(4) 0.038(2) Uani 1 1 d . . . C95 C 0.7890(6) 0.7425(5) 1.1002(4) 0.0350(19) Uani 1 1 d . . . H95 H 0.8218 0.7012 1.1034 0.042 Uiso 1 1 calc R . . C96 C 0.7319(5) 0.7311(5) 1.0304(4) 0.0259(17) Uani 1 1 d . . . H96 H 0.7260 0.6808 0.9866 0.031 Uiso 1 1 calc R . . C97 C 0.3866(8) 0.8821(8) 0.8966(7) 0.084(4) Uani 1 1 d . . . H97 H 0.4241 0.8473 0.8598 0.100 Uiso 1 1 calc R . . N1 N 0.6553(4) 0.6566(3) 0.7667(3) 0.0150(12) Uani 1 1 d . . . N2 N 0.7941(4) 0.7651(3) 0.7898(3) 0.0180(12) Uani 1 1 d . . . N3 N 0.6666(4) 0.7660(3) 0.6908(3) 0.0173(12) Uani 1 1 d . . . N4 N 0.5973(4) 0.7904(3) 0.5794(3) 0.0176(12) Uani 1 1 d . . . N5 N 0.4955(4) 0.6717(3) 0.5872(3) 0.0161(12) Uani 1 1 d . . . N6 N 0.3826(4) 0.5402(3) 0.5392(3) 0.0178(12) Uani 1 1 d . . . N7 N 0.4852(4) 0.5627(3) 0.6626(3) 0.0153(12) Uani 1 1 d . . . N8 N 0.5711(4) 0.5237(3) 0.7588(3) 0.0177(12) Uani 1 1 d . . . N9 N 0.4776(4) 0.6946(3) 0.8473(3) 0.0159(12) Uani 1 1 d . . . N10 N 0.3424(4) 0.6873(3) 0.7129(3) 0.0150(12) Uani 1 1 d . . . N11 N 0.4632(4) 0.8352(3) 0.7164(3) 0.0167(12) Uani 1 1 d . . . N12 N 0.5996(4) 0.8413(3) 0.8500(3) 0.0159(12) Uani 1 1 d . . . O1 O 0.9429(3) 0.7575(3) 0.9070(3) 0.0359(13) Uani 1 1 d . . . O2 O 0.7365(4) 0.9224(3) 0.5657(3) 0.0341(13) Uani 1 1 d . . . O3 O 0.2739(3) 0.5126(3) 0.3661(3) 0.0268(11) Uani 1 1 d . . . O4 O 0.4539(3) 0.3561(3) 0.7400(3) 0.0262(11) Uani 1 1 d . . . Dy1 Dy 0.51993(2) 0.716360(19) 0.731684(18) 0.01371(10) Uani 1 1 d . . . Cl1 Cl 0.01324(14) 0.38080(13) 0.86234(14) 0.0434(5) Uani 1 1 d . . . Cl2 Cl -0.01842(15) 0.78482(13) 0.40208(12) 0.0426(5) Uani 1 1 d . . . Cl3 Cl 0.76920(17) 1.31046(14) 0.87428(18) 0.0669(8) Uani 1 1 d . . . Cl4 Cl 0.8681(2) 0.83203(15) 1.25362(12) 0.0634(7) Uani 1 1 d . . . Cl5 Cl 0.4681(4) 0.9777(3) 0.9668(3) 0.166(2) Uani 1 1 d . . . Cl6 Cl 0.3449(2) 0.8328(2) 0.9475(2) 0.0949(10) Uani 1 1 d . . . Cl7 Cl 0.3089(3) 0.9171(2) 0.8472(2) 0.0943(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(3) 0.016(4) 0.012(3) 0.005(3) 0.004(3) 0.007(3) C2 0.024(4) 0.016(4) 0.020(4) 0.008(3) 0.004(3) 0.007(3) C13 0.032(4) 0.027(4) 0.037(4) 0.024(4) 0.008(4) 0.002(3) C3 0.032(4) 0.016(4) 0.028(4) 0.012(3) -0.002(3) 0.004(3) C4 0.038(4) 0.029(4) 0.029(4) 0.018(4) -0.002(4) 0.016(4) C5 0.027(4) 0.034(5) 0.032(4) 0.021(4) -0.004(3) 0.011(4) C6 0.023(4) 0.023(4) 0.027(4) 0.007(3) 0.002(3) 0.006(3) C7 0.026(4) 0.018(4) 0.023(4) 0.013(3) 0.008(3) 0.007(3) C8 0.022(4) 0.017(4) 0.019(4) 0.009(3) 0.005(3) 0.004(3) C9 0.023(4) 0.010(3) 0.012(3) 0.002(3) 0.006(3) 0.006(3) C32 0.026(4) 0.021(4) 0.019(4) 0.012(3) 0.009(3) 0.010(3) C10 0.019(4) 0.021(4) 0.026(4) 0.012(3) 0.010(3) 0.007(3) C11 0.025(4) 0.027(4) 0.035(4) 0.018(4) 0.004(3) 0.005(3) C12 0.019(4) 0.035(5) 0.043(5) 0.020(4) 0.006(4) 0.000(3) C14 0.027(4) 0.026(4) 0.026(4) 0.011(3) 0.000(3) 0.005(3) C15 0.022(4) 0.019(4) 0.019(4) 0.011(3) 0.007(3) 0.001(3) C16 0.025(4) 0.015(4) 0.021(4) 0.010(3) 0.006(3) 0.003(3) C17 0.028(4) 0.013(4) 0.019(4) 0.009(3) 0.008(3) 0.011(3) C18 0.024(4) 0.027(4) 0.019(4) 0.014(3) 0.010(3) 0.017(3) C19 0.023(4) 0.026(4) 0.020(4) 0.015(3) 0.009(3) 0.005(3) C20 0.030(4) 0.025(4) 0.025(4) 0.017(3) 0.011(3) 0.013(3) C21 0.028(4) 0.033(4) 0.017(4) 0.008(3) 0.000(3) 0.015(4) C22 0.025(4) 0.017(4) 0.020(4) 0.005(3) 0.002(3) 0.008(3) C24 0.016(3) 0.017(4) 0.023(4) 0.010(3) 0.008(3) 0.006(3) C25 0.019(3) 0.019(4) 0.020(4) 0.014(3) 0.006(3) 0.007(3) C26 0.024(4) 0.016(4) 0.017(3) 0.008(3) 0.005(3) 0.004(3) C27 0.033(4) 0.023(4) 0.022(4) 0.014(3) 0.005(3) 0.004(3) C28 0.025(4) 0.017(4) 0.026(4) 0.005(3) 0.000(3) -0.007(3) C23 0.029(4) 0.012(3) 0.019(3) 0.011(3) 0.009(3) 0.007(3) C30 0.027(4) 0.021(4) 0.026(4) 0.016(3) 0.012(3) 0.014(3) C29 0.034(4) 0.013(4) 0.027(4) 0.009(3) 0.010(4) 0.002(3) C31 0.023(4) 0.011(3) 0.018(3) 0.006(3) 0.008(3) 0.001(3) C33 0.021(3) 0.012(3) 0.016(3) 0.007(3) 0.004(3) 0.007(3) C34 0.030(4) 0.013(4) 0.019(4) 0.008(3) 0.004(3) 0.004(3) C35 0.031(4) 0.013(4) 0.016(3) 0.008(3) 0.009(3) 0.006(3) C36 0.019(3) 0.015(4) 0.027(4) 0.010(3) 0.006(3) 0.008(3) C37 0.017(3) 0.011(3) 0.025(4) 0.008(3) 0.007(3) 0.003(3) C38 0.017(3) 0.020(4) 0.023(4) 0.012(3) 0.006(3) 0.009(3) C39 0.021(4) 0.018(4) 0.030(4) 0.013(3) 0.001(3) 0.000(3) C40 0.023(4) 0.023(4) 0.027(4) 0.011(3) -0.004(3) 0.006(3) C41 0.016(3) 0.022(4) 0.017(3) 0.010(3) 0.003(3) 0.005(3) C42 0.015(3) 0.014(4) 0.023(4) 0.011(3) 0.000(3) 0.005(3) C43 0.025(4) 0.019(4) 0.017(3) 0.011(3) 0.006(3) 0.009(3) C44 0.028(4) 0.023(4) 0.029(4) 0.019(3) -0.001(3) 0.009(3) C45 0.029(4) 0.017(4) 0.034(4) 0.014(3) 0.001(4) 0.000(3) C46 0.024(4) 0.014(4) 0.019(3) 0.011(3) 0.006(3) 0.001(3) C47 0.020(3) 0.016(4) 0.023(4) 0.014(3) 0.009(3) 0.002(3) C48 0.020(3) 0.010(3) 0.018(3) 0.003(3) 0.003(3) 0.001(3) C49 0.020(3) 0.012(3) 0.024(4) 0.008(3) 0.005(3) 0.003(3) C50 0.017(3) 0.024(4) 0.019(4) 0.011(3) 0.004(3) 0.002(3) C51 0.021(4) 0.015(4) 0.021(4) 0.005(3) 0.006(3) 0.005(3) C52 0.020(3) 0.020(4) 0.017(3) 0.008(3) 0.003(3) 0.008(3) C53 0.134(11) 0.085(9) 0.048(6) 0.030(6) 0.032(7) 0.023(8) C54 0.051(6) 0.082(8) 0.064(7) 0.032(6) 0.009(5) -0.006(6) C55 0.030(4) 0.044(5) 0.043(5) 0.019(4) -0.004(4) 0.010(4) C56 0.053(6) 0.073(7) 0.052(6) 0.022(6) 0.005(5) 0.008(6) C57 0.086(9) 0.118(11) 0.052(7) -0.013(7) 0.002(7) 0.048(8) C58 0.060(6) 0.040(5) 0.049(6) 0.013(5) 0.024(5) -0.005(5) C59 0.053(5) 0.025(5) 0.041(5) 0.009(4) 0.013(4) -0.005(4) C60 0.030(4) 0.023(4) 0.036(4) 0.022(4) 0.002(4) -0.006(3) C61 0.053(5) 0.037(5) 0.049(5) 0.030(4) -0.001(5) 0.002(4) C62 0.049(6) 0.062(7) 0.082(7) 0.040(6) 0.013(6) 0.024(5) C63 0.039(5) 0.080(7) 0.084(7) 0.065(6) 0.017(5) 0.020(5) C64 0.032(4) 0.038(5) 0.063(6) 0.028(5) 0.008(4) 0.015(4) C65 0.035(4) 0.029(4) 0.023(4) 0.013(3) 0.008(3) 0.012(4) C66 0.033(4) 0.022(4) 0.035(4) 0.011(4) 0.003(4) 0.000(3) C67 0.036(5) 0.048(6) 0.069(6) 0.034(5) 0.015(5) 0.002(4) C68 0.116(9) 0.029(5) 0.048(6) 0.021(4) 0.024(6) 0.030(6) C69 0.067(6) 0.028(5) 0.035(5) 0.023(4) 0.009(4) 0.011(4) C70 0.035(4) 0.023(4) 0.028(4) 0.019(3) 0.008(3) 0.004(3) C71 0.046(5) 0.027(4) 0.031(4) 0.009(4) 0.011(4) 0.002(4) C72 0.052(5) 0.043(5) 0.033(5) 0.014(4) 0.004(4) 0.000(4) C73 0.015(3) 0.016(4) 0.028(4) 0.013(3) 0.002(3) 0.002(3) C74 0.027(4) 0.019(4) 0.030(4) 0.013(3) 0.012(3) 0.004(3) C75 0.029(4) 0.042(5) 0.038(5) 0.026(4) 0.016(4) 0.013(4) C76 0.025(4) 0.032(5) 0.040(5) 0.025(4) 0.000(4) 0.001(4) C77 0.028(4) 0.014(4) 0.036(4) 0.016(3) 0.000(4) -0.002(3) C78 0.024(4) 0.021(4) 0.026(4) 0.014(3) 0.006(3) 0.005(3) C79 0.024(4) 0.012(4) 0.027(4) 0.011(3) 0.001(3) 0.002(3) C80 0.026(4) 0.029(4) 0.027(4) 0.019(3) 0.004(3) 0.006(3) C81 0.022(4) 0.030(4) 0.040(5) 0.020(4) 0.003(4) 0.005(3) C82 0.029(4) 0.023(4) 0.023(4) 0.007(3) -0.009(3) 0.010(3) C83 0.041(4) 0.026(4) 0.013(3) 0.008(3) 0.003(3) 0.016(4) C84 0.022(4) 0.018(4) 0.025(4) 0.011(3) 0.006(3) 0.010(3) C85 0.013(3) 0.020(4) 0.026(4) 0.012(3) -0.002(3) -0.001(3) C86 0.076(7) 0.018(5) 0.141(10) 0.019(6) 0.093(8) 0.011(5) C87 0.080(8) 0.016(5) 0.156(12) 0.012(6) 0.081(8) 0.012(5) C88 0.034(4) 0.016(4) 0.063(6) 0.020(4) 0.002(4) 0.000(4) C89 0.105(9) 0.040(6) 0.057(6) 0.012(5) 0.048(7) -0.022(6) C90 0.109(9) 0.018(5) 0.054(6) -0.006(4) 0.053(6) -0.017(5) C91 0.025(4) 0.021(4) 0.020(4) 0.012(3) 0.001(3) 0.003(3) C92 0.037(4) 0.020(4) 0.030(4) 0.016(3) -0.002(4) 0.002(3) C93 0.056(5) 0.028(5) 0.021(4) 0.008(4) -0.005(4) -0.006(4) C94 0.052(5) 0.043(5) 0.020(4) 0.019(4) -0.007(4) 0.007(4) C95 0.043(5) 0.037(5) 0.025(4) 0.014(4) -0.003(4) 0.015(4) C96 0.036(4) 0.029(4) 0.015(4) 0.010(3) 0.004(3) 0.012(4) C97 0.065(7) 0.105(10) 0.070(8) 0.016(7) 0.035(7) 0.024(7) N1 0.017(3) 0.013(3) 0.018(3) 0.009(2) 0.009(2) 0.004(2) N2 0.018(3) 0.021(3) 0.017(3) 0.009(3) 0.005(2) 0.005(3) N3 0.019(3) 0.016(3) 0.021(3) 0.011(2) 0.004(2) 0.005(2) N4 0.022(3) 0.014(3) 0.018(3) 0.010(2) 0.004(3) 0.000(3) N5 0.017(3) 0.014(3) 0.019(3) 0.010(2) 0.002(2) 0.002(2) N6 0.026(3) 0.013(3) 0.018(3) 0.010(2) 0.005(3) 0.003(2) N7 0.018(3) 0.015(3) 0.014(3) 0.008(2) 0.000(2) 0.004(2) N8 0.023(3) 0.015(3) 0.019(3) 0.010(2) 0.006(3) 0.005(3) N9 0.018(3) 0.016(3) 0.017(3) 0.011(2) 0.002(2) 0.001(2) N10 0.016(3) 0.013(3) 0.018(3) 0.009(2) 0.002(2) 0.003(2) N11 0.014(3) 0.019(3) 0.021(3) 0.013(2) 0.005(2) 0.003(2) N12 0.018(3) 0.012(3) 0.020(3) 0.009(2) 0.003(2) 0.005(2) O1 0.027(3) 0.030(3) 0.047(3) 0.021(3) -0.013(3) -0.005(2) O2 0.035(3) 0.031(3) 0.045(3) 0.029(3) 0.002(3) -0.004(2) O3 0.021(2) 0.026(3) 0.029(3) 0.009(2) 0.002(2) 0.000(2) O4 0.034(3) 0.026(3) 0.029(3) 0.021(2) 0.009(2) 0.005(2) Dy1 0.01516(16) 0.01301(17) 0.01592(17) 0.00943(13) 0.00151(12) 0.00234(12) Cl1 0.0296(10) 0.0457(13) 0.0708(15) 0.0411(12) 0.0158(11) 0.0000(9) Cl2 0.0412(11) 0.0391(12) 0.0402(11) 0.0143(10) -0.0189(10) 0.0100(10) Cl3 0.0516(14) 0.0233(12) 0.122(2) 0.0321(14) 0.0085(15) -0.0079(11) Cl4 0.0914(19) 0.0550(15) 0.0304(12) 0.0165(11) -0.0299(13) 0.0044(14) Cl5 0.128(4) 0.157(5) 0.153(5) 0.007(4) 0.016(3) 0.006(4) Cl6 0.085(2) 0.082(2) 0.126(3) 0.043(2) 0.024(2) 0.0367(19) Cl7 0.114(3) 0.080(2) 0.102(2) 0.041(2) 0.041(2) 0.031(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N8 1.334(8) . ? C1 N1 1.360(8) . ? C1 C2 1.460(9) . ? C2 C3 1.388(9) . ? C2 C7 1.394(9) . ? C13 C12 1.388(10) . ? C13 C14 1.408(10) . ? C13 H2A 0.9300 . ? C3 C4 1.383(9) . ? C3 H3 0.9300 . ? C4 C5 1.389(10) . ? C4 H4 0.9300 . ? C5 C6 1.398(9) . ? C5 H5 0.9300 . ? C6 O1 1.340(8) . ? C6 C7 1.396(9) . ? C7 C8 1.470(9) . ? C8 N2 1.330(8) . ? C8 N1 1.371(8) . ? C9 N2 1.332(8) . ? C9 N3 1.367(8) . ? C9 C10 1.456(9) . ? C32 N8 1.341(8) . ? C32 N7 1.371(8) . ? C32 C31 1.486(9) . ? C10 C15 1.386(9) . ? C10 C11 1.393(9) . ? C11 C12 1.395(10) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 O2 1.359(8) . ? C14 C15 1.401(9) . ? C15 C16 1.450(9) . ? C16 N4 1.333(8) . ? C16 N3 1.364(8) . ? C17 N4 1.335(8) . ? C17 N5 1.364(8) . ? C17 C18 1.466(9) . ? C18 C19 1.378(9) . ? C18 C23 1.405(9) . ? C19 C20 1.387(9) . ? C19 H19 0.9300 . ? C20 C21 1.388(10) . ? C20 H20 0.9300 . ? C21 C22 1.412(10) . ? C21 H21 0.9300 . ? C22 O3 1.353(8) . ? C22 C23 1.398(9) . ? C24 N6 1.341(8) . ? C24 N5 1.361(8) . ? C24 C23 1.467(9) . ? C25 N6 1.340(8) . ? C25 N7 1.352(8) . ? C25 C26 1.478(9) . ? C26 C27 1.379(9) . ? C26 C31 1.392(9) . ? C27 C28 1.378(9) . ? C27 H27 0.9300 . ? C28 C29 1.376(9) . ? C28 H28 0.9300 . ? C30 O4 1.356(8) . ? C30 C31 1.385(9) . ? C30 C29 1.401(10) . ? C29 H29 0.9300 . ? C33 N9 1.373(8) . ? C33 C52 1.412(9) . ? C33 C34 1.441(9) . ? C34 C35 1.346(9) . ? C34 H34 0.9300 . ? C35 C36 1.448(9) . ? C35 H35 0.9300 . ? C36 N9 1.370(8) . ? C36 C37 1.408(9) . ? C37 C38 1.409(9) . ? C37 C73 1.492(9) . ? C38 N10 1.367(8) . ? C38 C39 1.452(9) . ? C39 C40 1.342(9) . ? C39 H39 0.9300 . ? C40 C41 1.445(9) . ? C40 H40 0.9300 . ? C41 N10 1.374(8) . ? C41 C42 1.404(9) . ? C42 C43 1.404(9) . ? C42 C79 1.494(9) . ? C43 N11 1.378(8) . ? C43 C44 1.450(9) . ? C44 C45 1.346(9) . ? C44 H44 0.9300 . ? C45 C46 1.453(9) . ? C45 H45 0.9300 . ? C46 N11 1.370(8) . ? C46 C47 1.418(9) . ? C47 C48 1.390(9) . ? C47 C85 1.492(9) . ? C48 N12 1.389(8) . ? C48 C49 1.449(9) . ? C49 C50 1.343(9) . ? C49 H49 0.9300 . ? C50 C51 1.432(9) . ? C50 H50 0.9300 . ? C51 N12 1.374(8) . ? C51 C52 1.400(9) . ? C52 C91 1.501(9) . ? C53 C54 1.548(13) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.510(12) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 O1 1.422(8) . ? C55 C56 1.507(12) . ? C55 H55 0.9800 . ? C56 C57 1.508(14) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 C59 1.491(11) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.536(11) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 O2 1.423(8) . ? C60 C61 1.486(10) . ? C60 H60 0.9800 . ? C61 C62 1.526(12) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.487(12) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 C65 1.543(10) . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 O3 1.421(8) . ? C65 C66 1.517(10) . ? C65 H65 0.9800 . ? C66 C67 1.518(10) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 C69 1.512(11) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.507(10) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 O4 1.463(8) . ? C70 C71 1.530(10) . ? C70 H70 0.9800 . ? C71 C72 1.539(11) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 C74 1.385(9) . ? C73 C78 1.400(9) . ? C74 C75 1.378(10) . ? C74 H74 0.9300 . ? C75 C76 1.392(11) . ? C75 H75 0.9300 . ? C76 C77 1.387(10) . ? C76 Cl1 1.736(8) . ? C77 C78 1.371(9) . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? C79 C84 1.396(9) . ? C79 C80 1.401(9) . ? C80 C81 1.389(9) . ? C80 H80 0.9300 . ? C81 C82 1.390(10) . ? C81 H81 0.9300 . ? C82 C83 1.365(10) . ? C82 Cl2 1.750(7) . ? C83 C84 1.378(9) . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? C85 C86 1.337(10) . ? C85 C90 1.348(11) . ? C86 C87 1.398(12) . ? C86 H86 0.9300 . ? C87 C88 1.328(12) . ? C87 H87 0.9300 . ? C88 C89 1.331(12) . ? C88 Cl3 1.749(8) . ? C89 C90 1.390(12) . ? C89 H89 0.9300 . ? C90 H90 0.9300 . ? C91 C96 1.394(9) . ? C91 C92 1.410(9) . ? C92 C93 1.377(10) . ? C92 H92 0.9300 . ? C93 C94 1.382(11) . ? C93 H93 0.9300 . ? C94 C95 1.379(10) . ? C94 Cl4 1.751(7) . ? C95 C96 1.381(9) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? C97 Cl6 1.624(13) . ? C97 Cl7 1.682(13) . ? C97 Cl5 1.827(12) . ? C97 H97 0.9800 . ? N1 Dy1 2.441(5) . ? N3 Dy1 2.450(5) . ? N5 Dy1 2.467(5) . ? N7 Dy1 2.462(5) . ? N9 Dy1 2.454(5) . ? N10 Dy1 2.442(5) . ? N11 Dy1 2.444(5) . ? N12 Dy1 2.456(5) . ? Cl5 Cl5 1.333(9) 2_677 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 C1 N1 128.9(6) . . ? N8 C1 C2 119.8(6) . . ? N1 C1 C2 111.3(6) . . ? C3 C2 C7 121.4(6) . . ? C3 C2 C1 133.1(6) . . ? C7 C2 C1 105.6(6) . . ? C12 C13 C14 120.6(7) . . ? C12 C13 H2A 119.7 . . ? C14 C13 H2A 119.7 . . ? C4 C3 C2 117.4(7) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.4(6) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 121.8(7) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? O1 C6 C7 117.5(6) . . ? O1 C6 C5 126.1(6) . . ? C7 C6 C5 116.3(7) . . ? C2 C7 C6 121.6(6) . . ? C2 C7 C8 106.1(6) . . ? C6 C7 C8 132.3(6) . . ? N2 C8 N1 127.7(6) . . ? N2 C8 C7 122.1(6) . . ? N1 C8 C7 110.0(6) . . ? N2 C9 N3 129.3(6) . . ? N2 C9 C10 120.8(6) . . ? N3 C9 C10 109.8(5) . . ? N8 C32 N7 126.6(6) . . ? N8 C32 C31 122.9(6) . . ? N7 C32 C31 110.2(6) . . ? C15 C10 C11 122.7(7) . . ? C15 C10 C9 106.6(6) . . ? C11 C10 C9 130.7(6) . . ? C10 C11 C12 116.5(7) . . ? C10 C11 H11 121.7 . . ? C12 C11 H11 121.7 . . ? C13 C12 C11 122.1(7) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? O2 C14 C15 117.5(6) . . ? O2 C14 C13 124.7(7) . . ? C15 C14 C13 117.7(6) . . ? C10 C15 C14 120.3(6) . . ? C10 C15 C16 105.8(6) . . ? C14 C15 C16 133.9(6) . . ? N4 C16 N3 127.0(6) . . ? N4 C16 C15 122.3(6) . . ? N3 C16 C15 110.6(6) . . ? N4 C17 N5 129.8(6) . . ? N4 C17 C18 120.0(6) . . ? N5 C17 C18 109.9(6) . . ? C19 C18 C23 124.1(6) . . ? C19 C18 C17 129.3(7) . . ? C23 C18 C17 106.6(6) . . ? C18 C19 C20 117.0(7) . . ? C18 C19 H19 121.5 . . ? C20 C19 H19 121.5 . . ? C19 C20 C21 121.0(6) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C22 121.5(6) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? O3 C22 C23 125.5(6) . . ? O3 C22 C21 115.9(6) . . ? C23 C22 C21 118.1(6) . . ? N6 C24 N5 126.7(6) . . ? N6 C24 C23 122.1(6) . . ? N5 C24 C23 111.2(6) . . ? N6 C25 N7 130.4(6) . . ? N6 C25 C26 119.2(6) . . ? N7 C25 C26 110.4(5) . . ? C27 C26 C31 122.3(6) . . ? C27 C26 C25 131.2(6) . . ? C31 C26 C25 106.5(5) . . ? C28 C27 C26 117.1(6) . . ? C28 C27 H27 121.4 . . ? C26 C27 H27 121.4 . . ? C29 C28 C27 121.5(6) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C22 C23 C18 118.3(6) . . ? C22 C23 C24 137.0(6) . . ? C18 C23 C24 104.7(6) . . ? O4 C30 C31 119.9(6) . . ? O4 C30 C29 123.0(6) . . ? C31 C30 C29 117.1(6) . . ? C28 C29 C30 121.6(6) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C30 C31 C26 120.4(6) . . ? C30 C31 C32 134.6(6) . . ? C26 C31 C32 105.0(6) . . ? N9 C33 C52 126.9(6) . . ? N9 C33 C34 109.6(6) . . ? C52 C33 C34 123.2(6) . . ? C35 C34 C33 107.1(6) . . ? C35 C34 H34 126.4 . . ? C33 C34 H34 126.4 . . ? C34 C35 C36 107.2(6) . . ? C34 C35 H35 126.4 . . ? C36 C35 H35 126.4 . . ? N9 C36 C37 126.6(6) . . ? N9 C36 C35 109.3(6) . . ? C37 C36 C35 124.0(6) . . ? C36 C37 C38 125.1(6) . . ? C36 C37 C73 116.1(6) . . ? C38 C37 C73 118.4(6) . . ? N10 C38 C37 125.9(6) . . ? N10 C38 C39 109.8(5) . . ? C37 C38 C39 123.8(6) . . ? C40 C39 C38 106.8(6) . . ? C40 C39 H39 126.6 . . ? C38 C39 H39 126.6 . . ? C39 C40 C41 107.3(6) . . ? C39 C40 H40 126.3 . . ? C41 C40 H40 126.3 . . ? N10 C41 C42 125.2(6) . . ? N10 C41 C40 109.6(6) . . ? C42 C41 C40 124.8(6) . . ? C43 C42 C41 125.0(6) . . ? C43 C42 C79 117.0(6) . . ? C41 C42 C79 117.8(6) . . ? N11 C43 C42 126.5(6) . . ? N11 C43 C44 109.5(6) . . ? C42 C43 C44 123.7(6) . . ? C45 C44 C43 107.3(6) . . ? C45 C44 H44 126.4 . . ? C43 C44 H44 126.4 . . ? C44 C45 C46 106.9(6) . . ? C44 C45 H45 126.5 . . ? C46 C45 H45 126.5 . . ? N11 C46 C47 127.4(6) . . ? N11 C46 C45 109.8(6) . . ? C47 C46 C45 122.6(6) . . ? C48 C47 C46 124.7(6) . . ? C48 C47 C85 117.5(6) . . ? C46 C47 C85 117.0(6) . . ? N12 C48 C47 126.3(6) . . ? N12 C48 C49 109.0(5) . . ? C47 C48 C49 124.5(6) . . ? C50 C49 C48 107.6(6) . . ? C50 C49 H49 126.2 . . ? C48 C49 H49 126.2 . . ? C49 C50 C51 107.1(6) . . ? C49 C50 H50 126.5 . . ? C51 C50 H50 126.5 . . ? N12 C51 C52 123.7(6) . . ? N12 C51 C50 110.6(6) . . ? C52 C51 C50 125.4(6) . . ? C51 C52 C33 125.6(6) . . ? C51 C52 C91 117.5(6) . . ? C33 C52 C91 116.4(6) . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C53 113.8(9) . . ? C55 C54 H54A 108.8 . . ? C53 C54 H54A 108.8 . . ? C55 C54 H54B 108.8 . . ? C53 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? O1 C55 C56 110.2(7) . . ? O1 C55 C54 106.0(7) . . ? C56 C55 C54 115.1(8) . . ? O1 C55 H55 108.5 . . ? C56 C55 H55 108.5 . . ? C54 C55 H55 108.5 . . ? C55 C56 C57 113.7(8) . . ? C55 C56 H56A 108.8 . . ? C57 C56 H56A 108.8 . . ? C55 C56 H56B 108.8 . . ? C57 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C59 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C58 C59 C60 113.3(7) . . ? C58 C59 H59A 108.9 . . ? C60 C59 H59A 108.9 . . ? C58 C59 H59B 108.9 . . ? C60 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? O2 C60 C61 107.4(6) . . ? O2 C60 C59 108.3(6) . . ? C61 C60 C59 113.4(7) . . ? O2 C60 H60 109.2 . . ? C61 C60 H60 109.2 . . ? C59 C60 H60 109.2 . . ? C60 C61 C62 114.0(7) . . ? C60 C61 H61A 108.8 . . ? C62 C61 H61A 108.8 . . ? C60 C61 H61B 108.8 . . ? C62 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C63 C64 C65 115.7(7) . . ? C63 C64 H64A 108.4 . . ? C65 C64 H64A 108.4 . . ? C63 C64 H64B 108.4 . . ? C65 C64 H64B 108.4 . . ? H64A C64 H64B 107.4 . . ? O3 C65 C66 105.0(5) . . ? O3 C65 C64 110.8(6) . . ? C66 C65 C64 112.9(6) . . ? O3 C65 H65 109.4 . . ? C66 C65 H65 109.4 . . ? C64 C65 H65 109.4 . . ? C65 C66 C67 115.7(6) . . ? C65 C66 H66A 108.4 . . ? C67 C66 H66A 108.4 . . ? C65 C66 H66B 108.4 . . ? C67 C66 H66B 108.4 . . ? H66A C66 H66B 107.4 . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 H68A 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C69 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 C68 112.8(7) . . ? C70 C69 H69A 109.0 . . ? C68 C69 H69A 109.0 . . ? C70 C69 H69B 109.0 . . ? C68 C69 H69B 109.0 . . ? H69A C69 H69B 107.8 . . ? O4 C70 C69 108.4(6) . . ? O4 C70 C71 105.0(5) . . ? C69 C70 C71 114.7(6) . . ? O4 C70 H70 109.5 . . ? C69 C70 H70 109.5 . . ? C71 C70 H70 109.5 . . ? C70 C71 C72 111.9(6) . . ? C70 C71 H71A 109.2 . . ? C72 C71 H71A 109.2 . . ? C70 C71 H71B 109.2 . . ? C72 C71 H71B 109.2 . . ? H71A C71 H71B 107.9 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C74 C73 C78 117.2(6) . . ? C74 C73 C37 120.2(6) . . ? C78 C73 C37 122.6(6) . . ? C75 C74 C73 122.3(7) . . ? C75 C74 H74 118.8 . . ? C73 C74 H74 118.8 . . ? C74 C75 C76 118.8(7) . . ? C74 C75 H75 120.6 . . ? C76 C75 H75 120.6 . . ? C77 C76 C75 120.5(7) . . ? C77 C76 Cl1 120.4(6) . . ? C75 C76 Cl1 119.0(6) . . ? C78 C77 C76 119.3(7) . . ? C78 C77 H77 120.4 . . ? C76 C77 H77 120.4 . . ? C77 C78 C73 121.9(7) . . ? C77 C78 H78 119.0 . . ? C73 C78 H78 119.0 . . ? C84 C79 C80 117.6(6) . . ? C84 C79 C42 121.4(6) . . ? C80 C79 C42 121.0(6) . . ? C81 C80 C79 121.1(7) . . ? C81 C80 H80 119.4 . . ? C79 C80 H80 119.4 . . ? C80 C81 C82 118.7(7) . . ? C80 C81 H81 120.7 . . ? C82 C81 H81 120.7 . . ? C83 C82 C81 121.5(6) . . ? C83 C82 Cl2 119.6(6) . . ? C81 C82 Cl2 118.9(6) . . ? C82 C83 C84 119.3(6) . . ? C82 C83 H83 120.3 . . ? C84 C83 H83 120.3 . . ? C83 C84 C79 121.7(6) . . ? C83 C84 H84 119.1 . . ? C79 C84 H84 119.1 . . ? C86 C85 C90 116.6(7) . . ? C86 C85 C47 120.1(6) . . ? C90 C85 C47 123.3(6) . . ? C85 C86 C87 121.5(8) . . ? C85 C86 H86 119.3 . . ? C87 C86 H86 119.3 . . ? C88 C87 C86 120.9(8) . . ? C88 C87 H87 119.6 . . ? C86 C87 H87 119.6 . . ? C87 C88 C89 118.5(8) . . ? C87 C88 Cl3 120.5(7) . . ? C89 C88 Cl3 120.9(7) . . ? C88 C89 C90 120.5(9) . . ? C88 C89 H89 119.8 . . ? C90 C89 H89 119.8 . . ? C85 C90 C89 122.0(8) . . ? C85 C90 H90 119.0 . . ? C89 C90 H90 119.0 . . ? C96 C91 C92 117.6(6) . . ? C96 C91 C52 121.6(6) . . ? C92 C91 C52 120.8(6) . . ? C93 C92 C91 120.8(7) . . ? C93 C92 H92 119.6 . . ? C91 C92 H92 119.6 . . ? C92 C93 C94 119.3(7) . . ? C92 C93 H93 120.4 . . ? C94 C93 H93 120.4 . . ? C95 C94 C93 121.9(7) . . ? C95 C94 Cl4 118.5(6) . . ? C93 C94 Cl4 119.5(6) . . ? C94 C95 C96 118.2(7) . . ? C94 C95 H95 120.9 . . ? C96 C95 H95 120.9 . . ? C95 C96 C91 122.1(7) . . ? C95 C96 H96 118.9 . . ? C91 C96 H96 118.9 . . ? Cl6 C97 Cl7 119.4(7) . . ? Cl6 C97 Cl5 106.8(7) . . ? Cl7 C97 Cl5 103.4(7) . . ? Cl6 C97 H97 108.9 . . ? Cl7 C97 H97 108.9 . . ? Cl5 C97 H97 108.9 . . ? C1 N1 C8 106.9(5) . . ? C1 N1 Dy1 124.4(4) . . ? C8 N1 Dy1 124.5(4) . . ? C8 N2 C9 122.5(6) . . ? C16 N3 C9 107.1(5) . . ? C16 N3 Dy1 124.7(4) . . ? C9 N3 Dy1 123.7(4) . . ? C16 N4 C17 121.7(6) . . ? C24 N5 C17 107.4(5) . . ? C24 N5 Dy1 125.7(4) . . ? C17 N5 Dy1 120.9(4) . . ? C25 N6 C24 121.8(6) . . ? C25 N7 C32 107.5(5) . . ? C25 N7 Dy1 123.6(4) . . ? C32 N7 Dy1 122.9(4) . . ? C1 N8 C32 122.3(6) . . ? C36 N9 C33 106.7(5) . . ? C36 N9 Dy1 126.2(4) . . ? C33 N9 Dy1 124.6(4) . . ? C38 N10 C41 106.2(5) . . ? C38 N10 Dy1 123.7(4) . . ? C41 N10 Dy1 123.3(4) . . ? C46 N11 C43 106.3(5) . . ? C46 N11 Dy1 125.7(4) . . ? C43 N11 Dy1 125.6(4) . . ? C51 N12 C48 105.6(5) . . ? C51 N12 Dy1 124.1(4) . . ? C48 N12 Dy1 123.1(4) . . ? C6 O1 C55 121.8(6) . . ? C14 O2 C60 121.1(6) . . ? C22 O3 C65 119.3(5) . . ? C30 O4 C70 120.2(5) . . ? N1 Dy1 N10 137.92(17) . . ? N1 Dy1 N11 148.44(17) . . ? N10 Dy1 N11 72.84(17) . . ? N1 Dy1 N3 69.98(17) . . ? N10 Dy1 N3 148.07(17) . . ? N11 Dy1 N3 83.67(17) . . ? N1 Dy1 N9 77.64(17) . . ? N10 Dy1 N9 73.51(17) . . ? N11 Dy1 N9 114.30(17) . . ? N3 Dy1 N9 137.34(17) . . ? N1 Dy1 N12 83.52(17) . . ? N10 Dy1 N12 115.08(17) . . ? N11 Dy1 N12 73.62(17) . . ? N3 Dy1 N12 77.03(17) . . ? N9 Dy1 N12 72.33(17) . . ? N1 Dy1 N7 69.03(17) . . ? N10 Dy1 N7 78.84(17) . . ? N11 Dy1 N7 137.81(17) . . ? N3 Dy1 N7 106.80(17) . . ? N9 Dy1 N7 85.83(17) . . ? N12 Dy1 N7 148.13(17) . . ? N1 Dy1 N5 107.10(16) . . ? N10 Dy1 N5 84.80(17) . . ? N11 Dy1 N5 77.77(17) . . ? N3 Dy1 N5 69.02(17) . . ? N9 Dy1 N5 149.62(18) . . ? N12 Dy1 N5 137.45(18) . . ? N7 Dy1 N5 68.99(17) . . ? Cl5 Cl5 C97 153.2(9) 2_677 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.051 _refine_diff_density_min -1.863 _refine_diff_density_rms 0.141 #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 849700' #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C97 H81 Cl7 Dy N12 O4' _chemical_formula_weight 1889.39 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0969(4) _cell_length_b 17.6251(5) _cell_length_c 18.9482(5) _cell_angle_alpha 111.959(2) _cell_angle_beta 97.403(2) _cell_angle_gamma 97.046(2) _cell_volume 4254.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13548 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.89 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 30362 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14890 _reflns_number_gt 12328 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0590P)^2^+6.2133P] 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 14890 _refine_ls_number_parameters 1245 _refine_ls_number_restraints 4851 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy -0.480687(16) 0.214949(12) 0.230784(12) 0.02552(8) Uani 1 1 d . . . Cl1 Cl -0.22972(13) 0.80517(9) 0.36749(14) 0.0886(6) Uani 1 1 d U . . Cl2 Cl -0.1078(5) 0.3317(4) 0.7405(3) 0.0829(11) Uani 0.405(5) 1 d PU A 1 Cl3 Cl -0.9798(3) -0.1223(2) 0.3612(3) 0.0793(12) Uani 0.656(11) 1 d PU B 1 Cl4 Cl -1.0298(6) 0.2867(3) -0.0929(4) 0.0713(16) Uani 0.694(17) 1 d PU C 1 Cl5 Cl 0.4802(2) 0.47250(19) 0.47530(18) 0.0682(11) Uani 0.503(3) 1 d PDU . 1 Cl6 Cl 0.3160(5) 0.4138(4) 0.3506(4) 0.0779(15) Uani 0.503(3) 1 d PDU . 1 Cl7 Cl 0.3441(4) 0.3230(3) 0.4453(4) 0.0669(13) Uani 0.503(3) 1 d PDU . 1 N1 N -0.5040(3) 0.1706(2) 0.0882(2) 0.0350(9) Uani 1 1 d U . . N2 N -0.6184(3) 0.0424(2) 0.0446(2) 0.0427(10) Uani 1 1 d U . . N3 N -0.5161(3) 0.0601(2) 0.1638(2) 0.0326(8) Uani 1 1 d U . . N4 N -0.4299(3) 0.0213(2) 0.2594(2) 0.0357(9) Uani 1 1 d U . . N5 N -0.3454(3) 0.1532(2) 0.2667(2) 0.0305(8) Uani 1 1 d U . . N6 N -0.2075(3) 0.2629(2) 0.2912(2) 0.0349(9) Uani 1 1 d U . . N7 N -0.3335(3) 0.2628(2) 0.1908(2) 0.0305(8) Uani 1 1 d U . . N8 N -0.4020(3) 0.2857(2) 0.0784(2) 0.0362(9) Uani 1 1 d U . . N9 N -0.5376(3) 0.3329(2) 0.2121(2) 0.0306(8) Uani 1 1 d U . . N10 N -0.4024(3) 0.3388(2) 0.3462(2) 0.0281(8) Uani 1 1 d U . . N11 N -0.5241(3) 0.1922(2) 0.3434(2) 0.0328(8) Uani 1 1 d U . . N12 N -0.6581(3) 0.1851(2) 0.2088(2) 0.0385(9) Uani 1 1 d U . . O1 O -0.7413(4) 0.0184(2) -0.0987(3) 0.0863(15) Uani 1 1 d U . . O2 O -0.5426(3) -0.1444(2) 0.2423(2) 0.0536(10) Uani 1 1 d U . . O3 O -0.0578(3) 0.2542(3) 0.4107(3) 0.0722(12) Uani 1 1 d DU . . O4 O -0.2616(3) 0.4163(2) 0.0636(2) 0.0643(11) Uani 1 1 d U . . C1 C -0.4777(4) 0.2240(3) 0.0541(3) 0.0364(10) Uani 1 1 d U . . C2 C -0.5423(4) 0.2001(3) -0.0207(3) 0.0412(11) Uani 1 1 d U . . C3 C -0.5481(4) 0.2344(3) -0.0762(3) 0.0475(13) Uani 1 1 d U . . H3 H -0.5059 0.2825 -0.0697 0.057 Uiso 1 1 calc R . . C4 C -0.6204(5) 0.1927(4) -0.1419(3) 0.0562(14) Uani 1 1 d U . . H4 H -0.6262 0.2139 -0.1801 0.067 Uiso 1 1 calc R . . C5 C -0.6834(5) 0.1218(4) -0.1531(3) 0.0595(15) Uani 1 1 d U . . H5 H -0.7302 0.0962 -0.1983 0.071 Uiso 1 1 calc R . . C6 C -0.6784(5) 0.0877(3) -0.0979(3) 0.0525(13) Uani 1 1 d U . . C7 C -0.6057(4) 0.1283(3) -0.0314(3) 0.0415(11) Uani 1 1 d U . . C8 C -0.5776(4) 0.1114(3) 0.0371(3) 0.0385(11) Uani 1 1 d U . . C9 C -0.5873(4) 0.0171(3) 0.1013(3) 0.0399(11) Uani 1 1 d U . . C10 C -0.6276(4) -0.0638(3) 0.0990(3) 0.0428(12) Uani 1 1 d U . . C11 C -0.7014(4) -0.1267(3) 0.0485(3) 0.0520(14) Uani 1 1 d U . . H11 H -0.7349 -0.1229 0.0047 0.062 Uiso 1 1 calc R . . C12 C -0.7238(5) -0.1962(3) 0.0656(3) 0.0568(15) Uani 1 1 d U . . H12 H -0.7737 -0.2395 0.0329 0.068 Uiso 1 1 calc R . . C13 C -0.6735(5) -0.2020(3) 0.1298(3) 0.0529(14) Uani 1 1 d U . . H13 H -0.6908 -0.2492 0.1398 0.064 Uiso 1 1 calc R . . C14 C -0.5975(4) -0.1394(3) 0.1806(3) 0.0477(12) Uani 1 1 d U . . C15 C -0.5744(4) -0.0692(3) 0.1638(3) 0.0396(11) Uani 1 1 d U . . C16 C -0.5020(4) 0.0083(3) 0.2022(3) 0.0353(10) Uani 1 1 d U . . C17 C -0.3557(4) 0.0856(3) 0.2856(3) 0.0337(10) Uani 1 1 d U . . C18 C -0.2698(4) 0.0883(3) 0.3384(3) 0.0403(11) Uani 1 1 d U . . C19 C -0.2457(5) 0.0320(3) 0.3713(3) 0.0538(14) Uani 1 1 d U . . H19 H -0.2876 -0.0175 0.3610 0.065 Uiso 1 1 calc R . . C20 C -0.1560(5) 0.0548(4) 0.4199(4) 0.0672(17) Uani 1 1 d U . . H20 H -0.1376 0.0197 0.4434 0.081 Uiso 1 1 calc R . . C21 C -0.0922(5) 0.1281(4) 0.4351(4) 0.0745(18) Uani 1 1 d U . . H21 H -0.0333 0.1414 0.4694 0.089 Uiso 1 1 calc R . . C22 C -0.1150(4) 0.1819(4) 0.3998(4) 0.0573(14) Uani 1 1 d U . . C23 C -0.2054(4) 0.1602(3) 0.3505(3) 0.0408(11) Uani 1 1 d U . . C24 C -0.2531(4) 0.1986(3) 0.3029(3) 0.0351(10) Uani 1 1 d U . . C25 C -0.2433(3) 0.2888(3) 0.2380(3) 0.0331(10) Uani 1 1 d U . . C26 C -0.1824(4) 0.3479(3) 0.2180(3) 0.0391(11) Uani 1 1 d U . . C27 C -0.0867(4) 0.3903(3) 0.2485(4) 0.0515(13) Uani 1 1 d U . . H27 H -0.0493 0.3846 0.2898 0.062 Uiso 1 1 calc R . . C28 C -0.0503(4) 0.4417(3) 0.2138(4) 0.0596(15) Uani 1 1 d U . . H28 H 0.0134 0.4710 0.2323 0.071 Uiso 1 1 calc R . . C29 C -0.1058(5) 0.4506(3) 0.1525(3) 0.0568(14) Uani 1 1 d U . . H29 H -0.0782 0.4860 0.1315 0.068 Uiso 1 1 calc R . . C30 C -0.2014(4) 0.4084(3) 0.1212(3) 0.0478(12) Uani 1 1 d U . . C31 C -0.2388(4) 0.3558(3) 0.1550(3) 0.0388(11) Uani 1 1 d U . . C32 C -0.3320(4) 0.3002(3) 0.1392(3) 0.0345(10) Uani 1 1 d U . . C33 C -0.6178(4) 0.3288(3) 0.1612(3) 0.0370(11) Uani 1 1 d U . . C34 C -0.6122(4) 0.4043(3) 0.1487(3) 0.0493(13) Uani 1 1 d U . . H34 H -0.6573 0.4160 0.1156 0.059 Uiso 1 1 calc R . . C35 C -0.5290(4) 0.4554(3) 0.1940(3) 0.0470(13) Uani 1 1 d U . . H35 H -0.5061 0.5089 0.1980 0.056 Uiso 1 1 calc R . . C36 C -0.4824(3) 0.4112(3) 0.2350(3) 0.0333(10) Uani 1 1 d U . . C37 C -0.3995(3) 0.4473(3) 0.2933(3) 0.0302(9) Uani 1 1 d U . . C38 C -0.3621(3) 0.4126(3) 0.3437(3) 0.0302(9) Uani 1 1 d U . . C39 C -0.2795(4) 0.4543(3) 0.4065(3) 0.0415(11) Uani 1 1 d U . . H39 H -0.2392 0.5045 0.4166 0.050 Uiso 1 1 calc R . . C40 C -0.2716(4) 0.4061(3) 0.4483(3) 0.0461(13) Uani 1 1 d U . . H40 H -0.2242 0.4162 0.4914 0.055 Uiso 1 1 calc R . . C41 C -0.3523(4) 0.3357(3) 0.4119(3) 0.0347(10) Uani 1 1 d U . . C42 C -0.3796(4) 0.2778(3) 0.4434(3) 0.0401(11) Uani 1 1 d U . . C43 C -0.4627(4) 0.2150(3) 0.4132(3) 0.0381(11) Uani 1 1 d U . . C44 C -0.5000(5) 0.1695(3) 0.4559(3) 0.0510(13) Uani 1 1 d U . . H44 H -0.4704 0.1728 0.5040 0.061 Uiso 1 1 calc R . . C45 C -0.5850(5) 0.1215(3) 0.4136(3) 0.0509(13) Uani 1 1 d U . . H45 H -0.6256 0.0854 0.4270 0.061 Uiso 1 1 calc R . . C46 C -0.6022(4) 0.1362(3) 0.3430(3) 0.0387(11) Uani 1 1 d U . . C47 C -0.6861(4) 0.1015(3) 0.2867(3) 0.0437(11) Uani 1 1 d U B . C48 C -0.7111(4) 0.1229(3) 0.2233(3) 0.0449(12) Uani 1 1 d U . . C49 C -0.8019(4) 0.0913(3) 0.1696(4) 0.0642(15) Uani 1 1 d U . . H49 H -0.8492 0.0474 0.1656 0.077 Uiso 1 1 calc R . . C50 C -0.8066(4) 0.1361(3) 0.1262(4) 0.0649(16) Uani 1 1 d U . . H50 H -0.8577 0.1293 0.0867 0.078 Uiso 1 1 calc R . . C51 C -0.7175(4) 0.1970(3) 0.1521(3) 0.0473(12) Uani 1 1 d U . . C52 C -0.7001(4) 0.2646(3) 0.1298(3) 0.0439(12) Uani 1 1 d U . . C53 C -0.9000(9) -0.1053(9) -0.0790(7) 0.090(4) Uani 0.564(8) 1 d PDU D 1 H53A H -0.9119 -0.1612 -0.0817 0.135 Uiso 0.564(8) 1 calc PR D 1 H53B H -0.9608 -0.0866 -0.0836 0.135 Uiso 0.564(8) 1 calc PR D 1 H53C H -0.8591 -0.0694 -0.0303 0.135 Uiso 0.564(8) 1 calc PR D 1 C54 C -0.8513(5) -0.1032(3) -0.1427(4) 0.0687(17) Uani 1 1 d DU . . H54A H -0.8933 -0.1410 -0.1911 0.082 Uiso 1 1 calc R D 1 H54B H -0.7922 -0.1254 -0.1385 0.082 Uiso 1 1 calc R D 1 C55 C -0.8244(5) -0.0211(4) -0.1491(5) 0.089(2) Uani 1 1 d DU D . H55 H -0.8092 -0.0339 -0.2009 0.107 Uiso 1 1 calc R . . C56 C -0.9011(6) 0.0336(4) -0.1414(5) 0.090(2) Uani 1 1 d DU . . H56A H -0.9388 0.0293 -0.1033 0.108 Uiso 1 1 calc R D 1 H56B H -0.8706 0.0914 -0.1253 0.108 Uiso 1 1 calc R D 1 C57 C -0.9644(11) 0.0037(10) -0.2183(7) 0.119(5) Uani 0.564(8) 1 d PDU D 1 H57A H -1.0145 0.0364 -0.2158 0.178 Uiso 0.564(8) 1 calc PR D 1 H57B H -0.9936 -0.0537 -0.2338 0.178 Uiso 0.564(8) 1 calc PR D 1 H57C H -0.9263 0.0088 -0.2553 0.178 Uiso 0.564(8) 1 calc PR D 1 C58 C -0.4703(6) -0.0578(5) 0.4079(4) 0.093(2) Uani 1 1 d U . . H58A H -0.4675 -0.0105 0.4552 0.139 Uiso 1 1 calc R . . H58B H -0.4407 -0.0399 0.3725 0.139 Uiso 1 1 calc R . . H58C H -0.4361 -0.0971 0.4189 0.139 Uiso 1 1 calc R . . C59 C -0.5765(6) -0.0987(4) 0.3716(4) 0.0788(19) Uani 1 1 d U . . H59A H -0.6112 -0.0581 0.3623 0.095 Uiso 1 1 calc R . . H59B H -0.6062 -0.1162 0.4078 0.095 Uiso 1 1 calc R . . C60 C -0.5872(6) -0.1755(4) 0.2939(4) 0.0692(17) Uani 1 1 d U . . H60 H -0.6560 -0.1999 0.2718 0.083 Uiso 1 1 calc R . . C61 C -0.5339(7) -0.2386(4) 0.3059(4) 0.094(2) Uani 1 1 d U . . H61A H -0.5540 -0.2518 0.3477 0.112 Uiso 1 1 calc R . . H61B H -0.4645 -0.2168 0.3200 0.112 Uiso 1 1 calc R . . C62 C -0.5567(8) -0.3185(5) 0.2296(4) 0.120(3) Uani 1 1 d U . . H62A H -0.5216 -0.3593 0.2366 0.180 Uiso 1 1 calc R . . H62B H -0.5372 -0.3049 0.1884 0.180 Uiso 1 1 calc R . . H62C H -0.6253 -0.3406 0.2168 0.180 Uiso 1 1 calc R . . C63 C 0.0438(14) 0.4233(9) 0.4717(12) 0.130(6) Uani 0.503(3) 1 d PDU . 2 H63D H 0.0938 0.4634 0.4685 0.195 Uiso 0.503(3) 1 calc PR . 2 H63E H 0.0166 0.4488 0.5169 0.195 Uiso 0.503(3) 1 calc PR . 2 H63F H -0.0064 0.4037 0.4263 0.195 Uiso 0.503(3) 1 calc PR . 2 C64 C 0.0875(9) 0.3499(9) 0.4772(10) 0.100(4) Uani 0.503(3) 1 d PDU . 2 H64C H 0.1123 0.3225 0.4305 0.121 Uiso 0.503(3) 1 calc PR . 2 H64D H 0.1414 0.3701 0.5209 0.121 Uiso 0.503(3) 1 calc PR . 2 C65 C 0.0106(9) 0.2875(8) 0.4872(5) 0.083(3) Uani 0.503(3) 1 d PDU . 2 H65A H 0.0413 0.2423 0.4919 0.100 Uiso 0.503(3) 1 calc PR . 2 C66 C -0.0283(10) 0.3299(10) 0.5617(7) 0.095(3) Uani 0.503(3) 1 d PDU . 2 H66C H -0.0512 0.3788 0.5595 0.114 Uiso 0.503(3) 1 calc PR . 2 H66D H -0.0844 0.2920 0.5618 0.114 Uiso 0.503(3) 1 calc PR . 2 C67 C 0.0414(13) 0.3563(12) 0.6379(8) 0.129(6) Uani 0.503(3) 1 d PDU . 2 H67D H 0.0082 0.3799 0.6800 0.194 Uiso 0.503(3) 1 calc PR . 2 H67E H 0.0952 0.3971 0.6408 0.194 Uiso 0.503(3) 1 calc PR . 2 H67F H 0.0649 0.3088 0.6414 0.194 Uiso 0.503(3) 1 calc PR . 2 C68 C -0.1282(7) 0.4969(4) -0.0567(4) 0.097(3) Uani 1 1 d U . . H68A H -0.0944 0.4681 -0.0967 0.145 Uiso 1 1 calc R . . H68B H -0.0823 0.5386 -0.0138 0.145 Uiso 1 1 calc R . . H68C H -0.1746 0.5230 -0.0768 0.145 Uiso 1 1 calc R . . C69 C -0.1790(6) 0.4376(4) -0.0308(4) 0.083(2) Uani 1 1 d U . . H69A H -0.1319 0.4102 -0.0124 0.099 Uiso 1 1 calc R . . H69B H -0.2244 0.3952 -0.0748 0.099 Uiso 1 1 calc R . . C70 C -0.2358(5) 0.4780(4) 0.0347(4) 0.0699(17) Uani 1 1 d U . . H70 H -0.1946 0.5277 0.0758 0.084 Uiso 1 1 calc R . . C71 C -0.3242(7) 0.4997(5) 0.0008(5) 0.094(2) Uani 1 1 d U . . H71A H -0.3682 0.4493 -0.0352 0.113 Uiso 1 1 calc R . . H71B H -0.3061 0.5333 -0.0275 0.113 Uiso 1 1 calc R . . C72 C -0.3768(7) 0.5495(6) 0.0675(5) 0.113(3) Uani 1 1 d U . . H72A H -0.4340 0.5632 0.0454 0.169 Uiso 1 1 calc R . . H72B H -0.3334 0.5997 0.1025 0.169 Uiso 1 1 calc R . . H72C H -0.3950 0.5158 0.0951 0.169 Uiso 1 1 calc R . . C73 C -0.3559(3) 0.5360(3) 0.3105(3) 0.0321(10) Uani 1 1 d U . . C78 C -0.2884(5) 0.5591(4) 0.2744(4) 0.0748(17) Uani 1 1 d U . . H78 H -0.2673 0.5178 0.2357 0.090 Uiso 1 1 calc R . . C77 C -0.2490(6) 0.6414(4) 0.2925(4) 0.087(2) Uani 1 1 d U . . H77 H -0.2014 0.6544 0.2670 0.104 Uiso 1 1 calc R . . C76 C -0.2787(4) 0.7010(3) 0.3453(4) 0.0513(14) Uani 1 1 d U . . C75 C -0.3441(5) 0.6821(3) 0.3841(4) 0.0758(19) Uani 1 1 d U . . H75 H -0.3643 0.7243 0.4226 0.091 Uiso 1 1 calc R . . C74 C -0.3820(5) 0.5990(3) 0.3669(4) 0.0665(16) Uani 1 1 d U . . H74 H -0.4266 0.5866 0.3949 0.080 Uiso 1 1 calc R . . C79 C -0.3226(5) 0.2905(3) 0.5208(3) 0.0560(14) Uani 1 1 d U A . C80 C -0.3189(6) 0.3642(4) 0.5861(3) 0.0739(18) Uani 1 1 d U . . H80 H -0.3531 0.4045 0.5814 0.089 Uiso 1 1 calc R . . C81 C -0.2648(7) 0.3769(4) 0.6573(4) 0.091(2) Uani 1 1 d U A . H81 H -0.2625 0.4256 0.7004 0.110 Uiso 1 1 calc R . . C82 C -0.2150(7) 0.3172(5) 0.6636(4) 0.098(2) Uani 1 1 d U . . C83 C -0.2189(6) 0.2434(4) 0.6012(4) 0.087(2) Uani 1 1 d U A . H83 H -0.1849 0.2034 0.6068 0.105 Uiso 1 1 calc R . . C84 C -0.2741(5) 0.2301(4) 0.5303(3) 0.0654(15) Uani 1 1 d U . . H84 H -0.2787 0.1798 0.4884 0.078 Uiso 1 1 calc R A . C85 C -0.7620(4) 0.0450(3) 0.3007(4) 0.0559(14) Uani 1 1 d DU . . C86 C -0.8041(7) 0.0792(6) 0.3739(6) 0.055(2) Uani 0.656(11) 1 d PDU B 1 H86 H -0.7880 0.1354 0.4065 0.067 Uiso 0.656(11) 1 calc PR B 1 C87 C -0.8666(6) 0.0248(5) 0.3904(6) 0.053(2) Uani 0.656(11) 1 d PDU B 1 H87 H -0.8923 0.0444 0.4353 0.063 Uiso 0.656(11) 1 calc PR B 1 C88 C -0.8922(7) -0.0585(6) 0.3416(6) 0.051(2) Uani 0.656(11) 1 d PDU B 1 C89 C -0.8553(12) -0.0913(12) 0.2782(9) 0.059(3) Uani 0.656(11) 1 d PDU B 1 H89 H -0.8736 -0.1479 0.2474 0.071 Uiso 0.656(11) 1 calc PR B 1 C90 C -0.7867(4) -0.0397(3) 0.2564(3) 0.0551(13) Uani 1 1 d DU B . H90 H -0.7595 -0.0633 0.2129 0.066 Uiso 1 1 calc R E 1 C91 C -0.7803(4) 0.2724(3) 0.0744(3) 0.0496(13) Uani 1 1 d U C . C92 C -0.8718(4) 0.2826(3) 0.0931(4) 0.0590(15) Uani 1 1 d U . . H92 H -0.8827 0.2860 0.1414 0.071 Uiso 1 1 calc R . . C93 C -0.9471(5) 0.2878(4) 0.0409(4) 0.0687(18) Uani 1 1 d U C . H93 H -1.0079 0.2943 0.0537 0.082 Uiso 1 1 calc R . . C94 C -0.9292(5) 0.2830(3) -0.0302(4) 0.0639(18) Uani 1 1 d U . . C95 C -0.8405(5) 0.2745(3) -0.0503(4) 0.0647(17) Uani 1 1 d U C . H95 H -0.8302 0.2719 -0.0986 0.078 Uiso 1 1 calc R . . C96 C -0.7649(4) 0.2697(3) 0.0030(3) 0.0550(14) Uani 1 1 d U . . H96 H -0.7038 0.2648 -0.0099 0.066 Uiso 1 1 calc R C . C97 C 0.4029(6) 0.3855(5) 0.4044(5) 0.057(3) Uani 0.503(3) 1 d PDU . 1 H97 H 0.4418 0.3526 0.3694 0.069 Uiso 0.503(3) 1 calc PR . 1 Cl2A Cl -0.1659(4) 0.3343(2) 0.75965(19) 0.0829(11) Uani 0.595(5) 1 d PU A 2 Cl3A Cl -1.0167(7) -0.1203(4) 0.3256(7) 0.081(3) Uani 0.344(11) 1 d PU B 2 Cl4A Cl -1.0008(10) 0.2912(8) -0.1145(8) 0.0713(16) Uani 0.306(17) 1 d PU C 2 Cl5A Cl 0.1804(4) 0.2969(4) 0.2937(3) 0.125(2) Uani 0.497(3) 1 d PDU . 2 Cl6A Cl 0.3368(6) 0.3466(5) 0.4254(4) 0.117(3) Uani 0.497(3) 1 d PDU . 2 Cl7A Cl 0.3315(7) 0.4363(5) 0.3330(5) 0.122(3) Uani 0.497(3) 1 d PDU . 2 C53A C -0.9498(8) -0.1587(7) -0.1993(9) 0.073(4) Uani 0.436(8) 1 d PDU D 2 H53D H -0.9638 -0.2093 -0.1915 0.109 Uiso 0.436(8) 1 calc PR D 2 H53E H -0.9429 -0.1716 -0.2520 0.109 Uiso 0.436(8) 1 calc PR D 2 H53F H -1.0021 -0.1286 -0.1884 0.109 Uiso 0.436(8) 1 calc PR D 2 C57A C -0.9485(10) 0.0534(9) -0.0707(7) 0.072(4) Uani 0.436(8) 1 d PDU D 2 H57D H -0.9956 0.0878 -0.0730 0.108 Uiso 0.436(8) 1 calc PR D 2 H57E H -0.8997 0.0823 -0.0246 0.108 Uiso 0.436(8) 1 calc PR D 2 H57F H -0.9804 0.0025 -0.0696 0.108 Uiso 0.436(8) 1 calc PR D 2 C63A C 0.0886(9) 0.2796(8) 0.3161(6) 0.072(3) Uani 0.497(3) 1 d PDU . 1 H63A H 0.1179 0.3158 0.2945 0.108 Uiso 0.497(3) 1 calc PR . 1 H63B H 0.0226 0.2561 0.2891 0.108 Uiso 0.497(3) 1 calc PR . 1 H63C H 0.1247 0.2357 0.3110 0.108 Uiso 0.497(3) 1 calc PR . 1 C64A C 0.0892(9) 0.3289(7) 0.4012(5) 0.060(3) Uani 0.497(3) 1 d PDU . 1 H64A H 0.1557 0.3539 0.4282 0.072 Uiso 0.497(3) 1 calc PR . 1 H64B H 0.0529 0.3734 0.4063 0.072 Uiso 0.497(3) 1 calc PR . 1 C65A C 0.0446(6) 0.2737(6) 0.4378(5) 0.053(2) Uani 0.497(3) 1 d PDU . 1 H65 H 0.0721 0.2228 0.4246 0.064 Uiso 0.497(3) 1 calc PR . 1 C66A C 0.0527(10) 0.3165(8) 0.5250(6) 0.070(3) Uani 0.497(3) 1 d PDU . 1 H66A H 0.0224 0.2766 0.5432 0.084 Uiso 0.497(3) 1 calc PR . 1 H66B H 0.1211 0.3318 0.5489 0.084 Uiso 0.50 1 calc PR . 1 C67A C 0.0073(11) 0.3938(8) 0.5533(7) 0.080(4) Uani 0.497(3) 1 d PDU . 1 H67A H 0.0151 0.4152 0.6087 0.120 Uiso 0.497(3) 1 calc PR . 1 H67B H -0.0607 0.3798 0.5307 0.120 Uiso 0.497(3) 1 calc PR . 1 H67C H 0.0389 0.4353 0.5383 0.120 Uiso 0.497(3) 1 calc PR . 1 C86A C -0.8228(14) 0.0700(13) 0.3398(11) 0.065(3) Uani 0.344(11) 1 d PDU B 2 H86A H -0.8103 0.1272 0.3688 0.077 Uiso 0.344(11) 1 calc PR B 2 C87A C -0.9095(14) 0.0267(11) 0.3486(12) 0.060(3) Uani 0.344(11) 1 d PDU B 2 H87A H -0.9516 0.0528 0.3796 0.072 Uiso 0.344(11) 1 calc PR B 2 C88A C -0.9243(14) -0.0564(12) 0.3072(12) 0.054(3) Uani 0.344(11) 1 d PDU B 2 C89A C -0.859(2) -0.090(3) 0.2590(16) 0.061(4) Uani 0.344(11) 1 d PDU B 2 H89A H -0.8681 -0.1467 0.2297 0.074 Uiso 0.344(11) 1 calc PR B 2 C97A C 0.3033(7) 0.3376(7) 0.3315(6) 0.082(4) Uani 0.497(3) 1 d PDU . 2 H97A H 0.3419 0.3017 0.2987 0.098 Uiso 0.497(3) 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03230(12) 0.01994(12) 0.02700(12) 0.01395(9) 0.00470(8) 0.00038(8) Cl1 0.0746(12) 0.0295(8) 0.1591(19) 0.0383(10) 0.0282(12) -0.0094(7) Cl2 0.114(3) 0.0868(15) 0.0353(15) 0.0244(13) -0.0143(16) 0.005(2) Cl3 0.046(2) 0.086(2) 0.127(3) 0.080(2) 0.002(2) -0.0187(15) Cl4 0.057(3) 0.0673(13) 0.072(3) 0.0223(17) -0.030(2) 0.0093(18) Cl5 0.060(2) 0.055(2) 0.065(2) 0.0001(14) 0.0207(16) -0.0093(15) Cl6 0.088(3) 0.065(3) 0.078(3) 0.025(2) 0.026(2) 0.005(2) Cl7 0.060(2) 0.050(2) 0.096(4) 0.031(2) 0.024(2) 0.0105(16) N1 0.055(2) 0.0213(18) 0.0311(19) 0.0156(15) 0.0040(17) 0.0025(16) N2 0.063(2) 0.0230(19) 0.043(2) 0.0188(17) 0.0010(19) 0.0023(17) N3 0.049(2) 0.0212(18) 0.0311(19) 0.0147(15) 0.0085(17) 0.0026(16) N4 0.057(2) 0.0247(19) 0.0293(19) 0.0161(16) 0.0065(18) 0.0045(17) N5 0.043(2) 0.0238(18) 0.0293(18) 0.0150(15) 0.0102(16) 0.0054(15) N6 0.037(2) 0.0256(19) 0.045(2) 0.0165(16) 0.0103(17) 0.0082(16) N7 0.042(2) 0.0243(18) 0.0305(18) 0.0140(15) 0.0150(16) 0.0077(15) N8 0.062(2) 0.0218(19) 0.0291(19) 0.0148(15) 0.0123(18) 0.0031(17) N9 0.037(2) 0.0207(18) 0.0346(19) 0.0153(15) 0.0009(16) 0.0009(15) N10 0.0355(19) 0.0240(18) 0.0308(18) 0.0166(15) 0.0102(15) 0.0044(15) N11 0.042(2) 0.0277(19) 0.035(2) 0.0187(16) 0.0130(17) 0.0006(16) N12 0.035(2) 0.0261(19) 0.055(2) 0.0207(17) 0.0011(18) 0.0002(16) O1 0.097(3) 0.034(2) 0.103(3) 0.018(2) -0.036(3) 0.009(2) O2 0.093(3) 0.0338(19) 0.0408(19) 0.0249(16) 0.0148(19) 0.0010(18) O3 0.055(2) 0.059(2) 0.096(3) 0.034(2) -0.014(2) 0.0033(19) O4 0.096(3) 0.045(2) 0.053(2) 0.0338(18) 0.007(2) -0.019(2) C1 0.062(3) 0.023(2) 0.028(2) 0.0145(18) 0.009(2) 0.008(2) C2 0.068(3) 0.026(2) 0.032(2) 0.0150(19) 0.008(2) 0.007(2) C3 0.081(3) 0.038(3) 0.032(2) 0.022(2) 0.012(2) 0.013(2) C4 0.091(4) 0.048(3) 0.034(3) 0.018(2) 0.006(3) 0.024(3) C5 0.086(4) 0.043(3) 0.040(3) 0.010(2) -0.009(3) 0.023(3) C6 0.075(3) 0.024(2) 0.051(3) 0.010(2) -0.006(3) 0.013(2) C7 0.065(3) 0.027(2) 0.034(2) 0.0144(19) 0.006(2) 0.011(2) C8 0.058(3) 0.024(2) 0.035(2) 0.0166(19) 0.004(2) 0.003(2) C9 0.054(3) 0.022(2) 0.042(2) 0.0155(19) 0.002(2) 0.001(2) C10 0.063(3) 0.020(2) 0.042(3) 0.014(2) 0.004(2) -0.003(2) C11 0.076(3) 0.025(3) 0.047(3) 0.015(2) -0.004(3) -0.007(2) C12 0.078(4) 0.021(3) 0.055(3) 0.008(2) -0.001(3) -0.012(2) C13 0.084(4) 0.022(3) 0.052(3) 0.017(2) 0.014(3) -0.004(2) C14 0.080(3) 0.024(2) 0.041(3) 0.017(2) 0.016(2) 0.001(2) C15 0.063(3) 0.020(2) 0.037(2) 0.0135(19) 0.013(2) 0.001(2) C16 0.056(3) 0.020(2) 0.035(2) 0.0141(18) 0.016(2) 0.0057(19) C17 0.050(3) 0.025(2) 0.033(2) 0.0173(18) 0.014(2) 0.0096(19) C18 0.058(3) 0.031(2) 0.038(2) 0.020(2) 0.006(2) 0.014(2) C19 0.078(4) 0.034(3) 0.052(3) 0.024(2) 0.000(3) 0.015(2) C20 0.087(4) 0.046(3) 0.069(4) 0.031(3) -0.013(3) 0.019(3) C21 0.076(4) 0.054(3) 0.086(4) 0.030(3) -0.023(3) 0.020(3) C22 0.057(3) 0.043(3) 0.071(3) 0.025(2) -0.002(3) 0.016(2) C23 0.050(3) 0.034(2) 0.045(3) 0.022(2) 0.005(2) 0.014(2) C24 0.040(2) 0.029(2) 0.041(2) 0.0166(19) 0.010(2) 0.0112(19) C25 0.041(2) 0.023(2) 0.043(2) 0.0162(18) 0.019(2) 0.0089(18) C26 0.042(3) 0.028(2) 0.053(3) 0.019(2) 0.022(2) 0.005(2) C27 0.046(3) 0.043(3) 0.068(3) 0.025(3) 0.016(3) 0.004(2) C28 0.050(3) 0.044(3) 0.083(4) 0.024(3) 0.026(3) -0.008(2) C29 0.072(4) 0.042(3) 0.061(3) 0.024(3) 0.032(3) -0.002(3) C30 0.070(3) 0.030(2) 0.049(3) 0.020(2) 0.025(2) -0.001(2) C31 0.059(3) 0.023(2) 0.041(2) 0.0158(19) 0.022(2) 0.006(2) C32 0.053(3) 0.021(2) 0.033(2) 0.0131(18) 0.018(2) 0.0028(19) C33 0.042(2) 0.025(2) 0.043(2) 0.0163(19) -0.006(2) 0.0033(19) C34 0.057(3) 0.030(3) 0.056(3) 0.023(2) -0.016(3) 0.001(2) C35 0.058(3) 0.026(2) 0.054(3) 0.020(2) -0.010(2) 0.000(2) C36 0.041(2) 0.023(2) 0.038(2) 0.0145(18) 0.009(2) 0.0042(18) C37 0.037(2) 0.021(2) 0.035(2) 0.0140(17) 0.0115(19) 0.0004(17) C38 0.035(2) 0.022(2) 0.038(2) 0.0158(18) 0.0093(19) 0.0050(17) C39 0.043(3) 0.032(2) 0.047(3) 0.018(2) -0.001(2) -0.001(2) C40 0.055(3) 0.032(3) 0.045(3) 0.019(2) -0.010(2) -0.004(2) C41 0.045(3) 0.029(2) 0.032(2) 0.0164(18) 0.002(2) 0.0037(19) C42 0.061(3) 0.028(2) 0.031(2) 0.0151(18) 0.003(2) 0.004(2) C43 0.061(3) 0.028(2) 0.029(2) 0.0149(19) 0.013(2) 0.005(2) C44 0.088(4) 0.035(3) 0.033(3) 0.019(2) 0.014(3) 0.000(3) C45 0.082(4) 0.031(3) 0.047(3) 0.021(2) 0.032(3) 0.000(2) C46 0.051(3) 0.026(2) 0.046(3) 0.020(2) 0.023(2) 0.005(2) C47 0.044(2) 0.027(2) 0.064(3) 0.022(2) 0.018(2) 0.0014(19) C48 0.038(2) 0.026(2) 0.068(3) 0.020(2) 0.003(2) -0.0016(19) C49 0.048(3) 0.038(3) 0.101(4) 0.034(3) -0.009(3) -0.010(2) C50 0.048(3) 0.041(3) 0.094(4) 0.031(3) -0.026(3) -0.006(2) C51 0.043(3) 0.028(2) 0.064(3) 0.019(2) -0.010(2) 0.000(2) C52 0.047(3) 0.027(2) 0.052(3) 0.017(2) -0.012(2) 0.0062(19) C53 0.070(8) 0.104(9) 0.109(9) 0.056(7) 0.008(7) 0.025(7) C54 0.088(4) 0.035(3) 0.074(4) 0.013(3) 0.011(3) 0.009(3) C55 0.092(5) 0.061(4) 0.103(5) 0.017(4) 0.022(4) 0.019(4) C56 0.097(5) 0.052(4) 0.127(5) 0.030(4) 0.046(4) 0.028(3) C57 0.129(11) 0.109(10) 0.110(10) 0.037(8) 0.016(9) 0.018(9) C58 0.130(7) 0.073(5) 0.071(5) 0.028(4) 0.017(5) 0.009(5) C59 0.114(5) 0.056(4) 0.058(4) 0.018(3) 0.019(4) -0.004(4) C60 0.104(4) 0.047(3) 0.068(4) 0.037(3) 0.024(3) 0.001(3) C61 0.154(6) 0.061(4) 0.071(4) 0.041(3) 0.008(4) 0.000(4) C62 0.216(10) 0.064(5) 0.069(5) 0.016(4) 0.014(6) 0.038(6) C63 0.119(10) 0.108(9) 0.134(10) 0.043(8) -0.025(9) -0.016(9) C64 0.081(6) 0.090(6) 0.103(6) 0.022(6) -0.011(6) 0.002(6) C65 0.070(6) 0.072(5) 0.093(6) 0.027(5) -0.010(5) 0.008(5) C66 0.091(5) 0.082(5) 0.080(5) 0.010(5) -0.010(5) 0.003(5) C67 0.112(10) 0.120(10) 0.116(10) 0.020(9) -0.007(9) 0.000(9) C68 0.149(7) 0.055(4) 0.078(5) 0.015(4) 0.053(5) -0.005(4) C69 0.123(5) 0.057(4) 0.057(4) 0.016(3) 0.035(4) -0.019(4) C70 0.104(5) 0.036(3) 0.072(4) 0.033(3) 0.011(3) -0.008(3) C71 0.132(6) 0.072(4) 0.090(5) 0.057(4) 0.004(4) 0.000(4) C72 0.127(7) 0.109(7) 0.118(7) 0.051(6) 0.041(6) 0.037(6) C73 0.036(2) 0.022(2) 0.041(2) 0.0170(19) 0.009(2) 0.0011(18) C78 0.096(4) 0.035(3) 0.090(4) 0.013(3) 0.058(3) -0.003(3) C77 0.112(5) 0.039(3) 0.108(5) 0.018(3) 0.073(4) -0.009(3) C76 0.047(3) 0.020(3) 0.087(4) 0.023(3) 0.015(3) -0.003(2) C75 0.084(4) 0.025(3) 0.107(4) 0.007(3) 0.050(4) -0.001(3) C74 0.074(3) 0.033(3) 0.088(4) 0.013(3) 0.047(3) -0.005(3) C79 0.092(4) 0.036(3) 0.034(3) 0.019(2) -0.007(3) -0.007(3) C80 0.129(5) 0.038(3) 0.045(3) 0.020(2) -0.015(3) 0.002(3) C81 0.160(6) 0.046(4) 0.045(3) 0.015(3) -0.022(4) -0.006(4) C82 0.158(6) 0.064(4) 0.049(3) 0.026(3) -0.042(4) -0.007(4) C83 0.134(5) 0.058(4) 0.055(3) 0.025(3) -0.030(4) 0.008(4) C84 0.099(4) 0.046(3) 0.044(3) 0.021(2) -0.016(3) 0.007(3) C85 0.050(3) 0.035(3) 0.084(3) 0.024(2) 0.028(3) -0.003(2) C86 0.060(4) 0.039(4) 0.067(4) 0.022(4) 0.019(4) -0.004(3) C87 0.049(4) 0.050(4) 0.071(5) 0.038(4) 0.020(4) -0.002(3) C88 0.048(4) 0.047(4) 0.073(5) 0.047(4) 0.009(4) -0.010(3) C89 0.064(5) 0.039(4) 0.077(6) 0.035(5) 0.009(5) -0.012(4) C90 0.058(3) 0.037(3) 0.069(3) 0.023(2) 0.016(3) -0.009(2) C91 0.051(3) 0.026(2) 0.060(3) 0.017(2) -0.019(2) 0.001(2) C92 0.046(3) 0.046(3) 0.077(4) 0.025(3) -0.016(3) 0.001(2) C93 0.052(3) 0.048(3) 0.092(4) 0.028(3) -0.025(3) -0.002(3) C94 0.056(4) 0.034(3) 0.080(4) 0.013(3) -0.034(3) 0.010(3) C95 0.081(4) 0.034(3) 0.059(3) 0.008(3) -0.025(3) 0.015(3) C96 0.062(3) 0.030(2) 0.063(3) 0.014(2) -0.014(3) 0.011(2) C97 0.050(6) 0.057(6) 0.057(6) 0.008(5) 0.036(5) 0.003(5) Cl2A 0.114(3) 0.0868(15) 0.0353(15) 0.0244(13) -0.0143(16) 0.005(2) Cl3A 0.056(5) 0.069(3) 0.127(7) 0.051(4) 0.036(4) -0.016(3) Cl4A 0.057(3) 0.0673(13) 0.072(3) 0.0223(17) -0.030(2) 0.0093(18) Cl5A 0.091(3) 0.158(5) 0.078(3) 0.006(3) -0.004(2) 0.006(3) Cl6A 0.130(5) 0.129(6) 0.066(3) 0.017(3) -0.006(3) 0.021(5) Cl7A 0.153(6) 0.074(5) 0.109(5) -0.008(3) 0.050(4) 0.032(4) C53A 0.053(8) 0.048(8) 0.109(10) 0.019(7) 0.026(7) 0.012(6) C57A 0.065(8) 0.054(8) 0.072(8) -0.004(7) 0.016(7) 0.011(6) C63A 0.043(6) 0.092(8) 0.072(7) 0.025(6) 0.014(6) 0.005(6) C64A 0.048(5) 0.066(5) 0.062(5) 0.026(4) 0.000(4) 0.003(4) C65A 0.043(5) 0.060(5) 0.058(5) 0.027(4) 0.001(4) 0.018(4) C66A 0.068(6) 0.075(6) 0.067(5) 0.037(5) -0.006(5) 0.006(5) C67A 0.085(8) 0.079(8) 0.061(7) 0.024(6) -0.005(6) -0.007(7) C86A 0.064(5) 0.041(5) 0.078(5) 0.013(5) 0.031(5) -0.016(5) C87A 0.053(6) 0.048(5) 0.077(6) 0.024(5) 0.026(5) -0.006(5) C88A 0.052(6) 0.043(5) 0.075(6) 0.035(5) 0.021(5) -0.010(5) C89A 0.060(6) 0.045(6) 0.077(6) 0.024(6) 0.027(6) -0.011(5) C97A 0.085(7) 0.062(7) 0.083(7) 0.015(6) 0.012(6) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N12 2.439(4) . ? Dy1 N9 2.444(3) . ? Dy1 N10 2.446(4) . ? Dy1 N11 2.450(4) . ? Dy1 N5 2.453(4) . ? Dy1 N7 2.459(4) . ? Dy1 N1 2.479(4) . ? Dy1 N3 2.494(4) . ? Cl1 C76 1.750(5) . ? Cl2 C82 1.879(9) . ? Cl3 C88 1.737(9) . ? Cl4 C94 1.754(7) . ? Cl5 Cl5 1.087(6) 2_666 ? Cl5 C97 1.737(7) . ? Cl6 C97 1.731(8) . ? Cl7 C97 1.755(8) . ? N1 C8 1.350(6) . ? N1 C1 1.369(6) . ? N2 C8 1.344(6) . ? N2 C9 1.354(6) . ? N3 C9 1.349(6) . ? N3 C16 1.381(6) . ? N4 C16 1.316(6) . ? N4 C17 1.334(6) . ? N5 C17 1.364(5) . ? N5 C24 1.382(6) . ? N6 C25 1.322(6) . ? N6 C24 1.338(6) . ? N7 C32 1.369(6) . ? N7 C25 1.372(6) . ? N8 C1 1.322(6) . ? N8 C32 1.339(6) . ? N9 C33 1.365(6) . ? N9 C36 1.379(6) . ? N10 C41 1.373(6) . ? N10 C38 1.374(5) . ? N11 C43 1.372(6) . ? N11 C46 1.383(6) . ? N12 C51 1.371(6) . ? N12 C48 1.382(6) . ? O1 C55 1.336(8) . ? O1 C6 1.412(7) . ? O2 C14 1.355(6) . ? O2 C60 1.458(7) . ? O3 C22 1.350(7) . ? O3 C65A 1.422(7) . ? O3 C65 1.496(8) . ? O4 C30 1.354(7) . ? O4 C70 1.418(6) . ? C1 C2 1.463(7) . ? C2 C7 1.387(7) . ? C2 C3 1.396(6) . ? C3 C4 1.391(8) . ? C4 C5 1.370(8) . ? C5 C6 1.387(8) . ? C6 C7 1.401(7) . ? C7 C8 1.454(6) . ? C9 C10 1.451(6) . ? C10 C11 1.377(7) . ? C10 C15 1.395(7) . ? C11 C12 1.390(7) . ? C12 C13 1.372(8) . ? C13 C14 1.394(8) . ? C14 C15 1.401(6) . ? C15 C16 1.468(7) . ? C17 C18 1.450(7) . ? C18 C23 1.388(7) . ? C18 C19 1.408(6) . ? C19 C20 1.381(8) . ? C20 C21 1.389(9) . ? C21 C22 1.395(8) . ? C22 C23 1.396(7) . ? C23 C24 1.463(6) . ? C25 C26 1.459(6) . ? C26 C27 1.393(7) . ? C26 C31 1.408(7) . ? C27 C28 1.392(8) . ? C28 C29 1.385(8) . ? C29 C30 1.394(8) . ? C30 C31 1.400(7) . ? C31 C32 1.463(7) . ? C33 C52 1.406(7) . ? C33 C34 1.431(6) . ? C34 C35 1.352(7) . ? C35 C36 1.445(6) . ? C36 C37 1.397(6) . ? C37 C38 1.397(6) . ? C37 C73 1.504(6) . ? C38 C39 1.446(7) . ? C39 C40 1.365(7) . ? C40 C41 1.456(7) . ? C41 C42 1.402(6) . ? C42 C43 1.400(7) . ? C42 C79 1.500(7) . ? C43 C44 1.436(7) . ? C44 C45 1.339(8) . ? C45 C46 1.451(7) . ? C46 C47 1.386(7) . ? C47 C48 1.405(7) . ? C47 C85 1.488(7) . ? C48 C49 1.432(7) . ? C49 C50 1.338(8) . ? C50 C51 1.446(7) . ? C51 C52 1.410(7) . ? C52 C91 1.496(7) . ? C53 C54 1.474(8) . ? C54 C55 1.503(6) . ? C54 C53A 1.591(8) . ? C55 C56 1.520(7) . ? C56 C57 1.473(8) . ? C56 C57A 1.518(8) . ? C58 C59 1.527(10) . ? C59 C60 1.558(9) . ? C60 C61 1.484(10) . ? C61 C62 1.557(10) . ? C63 C64 1.530(9) . ? C64 C65 1.528(9) . ? C65 C66 1.538(9) . ? C66 C67 1.512(9) . ? C68 C69 1.463(9) . ? C69 C70 1.557(10) . ? C70 C71 1.486(10) . ? C71 C72 1.578(11) . ? C73 C78 1.350(7) . ? C73 C74 1.350(7) . ? C78 C77 1.383(8) . ? C77 C76 1.308(8) . ? C76 C75 1.336(8) . ? C75 C74 1.394(8) . ? C79 C84 1.387(8) . ? C79 C80 1.409(8) . ? C80 C81 1.386(8) . ? C81 C82 1.367(10) . ? C82 C83 1.382(10) . ? C82 Cl2A 1.760(7) . ? C83 C84 1.385(8) . ? C85 C86A 1.22(2) . ? C85 C90 1.383(7) . ? C85 C86 1.521(12) . ? C86 C87 1.371(13) . ? C87 C88 1.382(13) . ? C88 C89 1.33(2) . ? C89 C90 1.45(2) . ? C90 C89A 1.28(4) . ? C91 C96 1.384(8) . ? C91 C92 1.396(8) . ? C92 C93 1.390(8) . ? C93 C94 1.376(10) . ? C94 C95 1.363(10) . ? C94 Cl4A 1.840(13) . ? C95 C96 1.403(7) . ? Cl3A C88A 1.771(18) . ? Cl5A C97A 1.738(8) . ? Cl6A C97A 1.723(8) . ? Cl7A C97A 1.724(8) . ? C63A C64A 1.516(8) . ? C64A C65A 1.513(8) . ? C65A C66A 1.519(8) . ? C66A C67A 1.519(9) . ? C86A C87A 1.42(3) . ? C87A C88A 1.35(2) . ? C88A C89A 1.40(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Dy1 N9 73.02(12) . . ? N12 Dy1 N10 115.28(13) . . ? N9 Dy1 N10 73.72(12) . . ? N12 Dy1 N11 73.45(13) . . ? N9 Dy1 N11 114.66(12) . . ? N10 Dy1 N11 72.63(12) . . ? N12 Dy1 N5 137.41(12) . . ? N9 Dy1 N5 149.08(12) . . ? N10 Dy1 N5 84.67(12) . . ? N11 Dy1 N5 78.13(12) . . ? N12 Dy1 N7 147.82(13) . . ? N9 Dy1 N7 84.01(12) . . ? N10 Dy1 N7 77.92(12) . . ? N11 Dy1 N7 137.97(13) . . ? N5 Dy1 N7 69.78(12) . . ? N12 Dy1 N1 84.71(14) . . ? N9 Dy1 N1 77.59(12) . . ? N10 Dy1 N1 137.40(12) . . ? N11 Dy1 N1 149.38(13) . . ? N5 Dy1 N1 106.10(12) . . ? N7 Dy1 N1 68.27(13) . . ? N12 Dy1 N3 78.30(13) . . ? N9 Dy1 N3 137.48(12) . . ? N10 Dy1 N3 148.31(12) . . ? N11 Dy1 N3 85.43(12) . . ? N5 Dy1 N3 68.31(12) . . ? N7 Dy1 N3 106.21(12) . . ? N1 Dy1 N3 69.02(12) . . ? Cl5 Cl5 C97 171.3(5) 2_666 . ? C8 N1 C1 106.5(4) . . ? C8 N1 Dy1 124.5(3) . . ? C1 N1 Dy1 122.5(3) . . ? C8 N2 C9 125.7(4) . . ? C9 N3 C16 106.8(4) . . ? C9 N3 Dy1 124.0(3) . . ? C16 N3 Dy1 122.9(3) . . ? C16 N4 C17 123.8(4) . . ? C17 N5 C24 106.8(4) . . ? C17 N5 Dy1 124.6(3) . . ? C24 N5 Dy1 123.2(3) . . ? C25 N6 C24 123.8(4) . . ? C32 N7 C25 106.9(4) . . ? C32 N7 Dy1 124.9(3) . . ? C25 N7 Dy1 122.9(3) . . ? C1 N8 C32 123.1(4) . . ? C33 N9 C36 106.3(4) . . ? C33 N9 Dy1 126.2(3) . . ? C36 N9 Dy1 125.5(3) . . ? C41 N10 C38 106.3(4) . . ? C41 N10 Dy1 123.5(3) . . ? C38 N10 Dy1 123.5(3) . . ? C43 N11 C46 106.0(4) . . ? C43 N11 Dy1 125.5(3) . . ? C46 N11 Dy1 126.5(3) . . ? C51 N12 C48 106.2(4) . . ? C51 N12 Dy1 124.0(3) . . ? C48 N12 Dy1 123.9(3) . . ? C55 O1 C6 125.7(5) . . ? C14 O2 C60 121.0(5) . . ? C22 O3 C65A 124.4(6) . . ? C22 O3 C65 110.4(6) . . ? C65A O3 C65 42.8(6) . . ? C30 O4 C70 121.7(5) . . ? N8 C1 N1 128.1(4) . . ? N8 C1 C2 121.4(4) . . ? N1 C1 C2 110.3(4) . . ? C7 C2 C3 121.2(5) . . ? C7 C2 C1 106.0(4) . . ? C3 C2 C1 132.9(5) . . ? C4 C3 C2 116.2(5) . . ? C5 C4 C3 123.2(5) . . ? C4 C5 C6 120.9(5) . . ? C5 C6 C7 117.1(5) . . ? C5 C6 O1 127.6(5) . . ? C7 C6 O1 115.2(5) . . ? C2 C7 C6 121.5(5) . . ? C2 C7 C8 105.5(4) . . ? C6 C7 C8 133.0(5) . . ? N2 C8 N1 125.8(4) . . ? N2 C8 C7 122.5(4) . . ? N1 C8 C7 111.6(4) . . ? N3 C9 N2 126.1(4) . . ? N3 C9 C10 112.1(4) . . ? N2 C9 C10 121.8(4) . . ? C11 C10 C15 122.4(5) . . ? C11 C10 C9 132.5(5) . . ? C15 C10 C9 105.1(4) . . ? C10 C11 C12 117.3(5) . . ? C13 C12 C11 121.2(5) . . ? C12 C13 C14 122.0(5) . . ? O2 C14 C13 124.0(4) . . ? O2 C14 C15 118.7(5) . . ? C13 C14 C15 117.2(5) . . ? C10 C15 C14 119.9(5) . . ? C10 C15 C16 106.6(4) . . ? C14 C15 C16 133.6(5) . . ? N4 C16 N3 126.2(4) . . ? N4 C16 C15 124.2(4) . . ? N3 C16 C15 109.3(4) . . ? N4 C17 N5 128.0(4) . . ? N4 C17 C18 121.1(4) . . ? N5 C17 C18 110.8(4) . . ? C23 C18 C19 122.1(5) . . ? C23 C18 C17 106.4(4) . . ? C19 C18 C17 131.4(5) . . ? C20 C19 C18 115.9(5) . . ? C19 C20 C21 122.7(5) . . ? C20 C21 C22 121.0(6) . . ? O3 C22 C21 125.4(6) . . ? O3 C22 C23 117.4(5) . . ? C21 C22 C23 117.2(6) . . ? C18 C23 C22 120.9(4) . . ? C18 C23 C24 106.1(4) . . ? C22 C23 C24 133.0(5) . . ? N6 C24 N5 126.7(4) . . ? N6 C24 C23 123.2(4) . . ? N5 C24 C23 109.8(4) . . ? N6 C25 N7 128.7(4) . . ? N6 C25 C26 120.7(4) . . ? N7 C25 C26 110.4(4) . . ? C27 C26 C31 122.0(5) . . ? C27 C26 C25 131.6(5) . . ? C31 C26 C25 106.4(4) . . ? C28 C27 C26 116.2(6) . . ? C29 C28 C27 122.1(6) . . ? C28 C29 C30 122.3(5) . . ? O4 C30 C29 125.9(5) . . ? O4 C30 C31 117.8(5) . . ? C29 C30 C31 116.2(5) . . ? C30 C31 C26 121.1(5) . . ? C30 C31 C32 133.7(5) . . ? C26 C31 C32 105.1(4) . . ? N8 C32 N7 126.4(4) . . ? N8 C32 C31 122.3(4) . . ? N7 C32 C31 111.1(4) . . ? N9 C33 C52 126.6(4) . . ? N9 C33 C34 110.3(4) . . ? C52 C33 C34 122.9(4) . . ? C35 C34 C33 107.1(4) . . ? C34 C35 C36 107.0(4) . . ? N9 C36 C37 126.9(4) . . ? N9 C36 C35 109.2(4) . . ? C37 C36 C35 123.7(4) . . ? C38 C37 C36 125.7(4) . . ? C38 C37 C73 117.1(4) . . ? C36 C37 C73 116.6(4) . . ? N10 C38 C37 125.8(4) . . ? N10 C38 C39 109.9(4) . . ? C37 C38 C39 123.9(4) . . ? C40 C39 C38 107.2(4) . . ? C39 C40 C41 106.2(4) . . ? N10 C41 C42 125.1(4) . . ? N10 C41 C40 110.1(4) . . ? C42 C41 C40 124.6(4) . . ? C43 C42 C41 125.2(4) . . ? C43 C42 C79 116.9(4) . . ? C41 C42 C79 117.4(5) . . ? N11 C43 C42 126.5(4) . . ? N11 C43 C44 110.1(5) . . ? C42 C43 C44 123.2(5) . . ? C45 C44 C43 107.4(5) . . ? C44 C45 C46 107.3(5) . . ? N11 C46 C47 126.5(4) . . ? N11 C46 C45 109.1(5) . . ? C47 C46 C45 124.3(5) . . ? C46 C47 C48 125.8(4) . . ? C46 C47 C85 116.6(5) . . ? C48 C47 C85 117.0(5) . . ? N12 C48 C47 125.5(5) . . ? N12 C48 C49 109.3(5) . . ? C47 C48 C49 124.8(5) . . ? C50 C49 C48 107.8(5) . . ? C49 C50 C51 107.1(5) . . ? N12 C51 C52 125.3(4) . . ? N12 C51 C50 109.3(5) . . ? C52 C51 C50 124.9(5) . . ? C33 C52 C51 125.0(4) . . ? C33 C52 C91 117.9(4) . . ? C51 C52 C91 116.9(5) . . ? C53 C54 C55 118.6(7) . . ? C53 C54 C53A 86.2(9) . . ? C55 C54 C53A 113.5(7) . . ? O1 C55 C54 106.9(6) . . ? O1 C55 C56 112.5(6) . . ? C54 C55 C56 117.5(6) . . ? C57 C56 C57A 118.4(10) . . ? C57 C56 C55 106.8(8) . . ? C57A C56 C55 117.8(8) . . ? C58 C59 C60 112.5(6) . . ? O2 C60 C61 109.0(6) . . ? O2 C60 C59 105.9(5) . . ? C61 C60 C59 110.5(6) . . ? C60 C61 C62 108.9(6) . . ? C65 C64 C63 110.5(10) . . ? O3 C65 C64 102.0(9) . . ? O3 C65 C66 119.1(9) . . ? C64 C65 C66 110.1(9) . . ? C67 C66 C65 117.2(10) . . ? C68 C69 C70 113.8(6) . . ? O4 C70 C71 110.7(6) . . ? O4 C70 C69 105.7(5) . . ? C71 C70 C69 108.8(6) . . ? C70 C71 C72 109.6(7) . . ? C78 C73 C74 115.4(5) . . ? C78 C73 C37 124.5(4) . . ? C74 C73 C37 120.0(4) . . ? C73 C78 C77 122.9(6) . . ? C76 C77 C78 120.1(6) . . ? C77 C76 C75 119.9(5) . . ? C77 C76 Cl1 120.0(5) . . ? C75 C76 Cl1 120.1(5) . . ? C76 C75 C74 119.8(6) . . ? C73 C74 C75 121.9(5) . . ? C84 C79 C80 118.5(5) . . ? C84 C79 C42 121.3(5) . . ? C80 C79 C42 120.2(5) . . ? C81 C80 C79 120.4(6) . . ? C82 C81 C80 119.3(7) . . ? C81 C82 C83 121.8(6) . . ? C81 C82 Cl2A 114.0(6) . . ? C83 C82 Cl2A 123.2(6) . . ? C81 C82 Cl2 127.0(6) . . ? C83 C82 Cl2 108.7(6) . . ? Cl2A C82 Cl2 29.6(2) . . ? C82 C83 C84 119.0(7) . . ? C83 C84 C79 121.0(6) . . ? C86A C85 C90 111.8(11) . . ? C86A C85 C47 123.0(11) . . ? C90 C85 C47 123.3(5) . . ? C86A C85 C86 22.8(6) . . ? C90 C85 C86 117.7(6) . . ? C47 C85 C86 118.4(6) . . ? C87 C86 C85 118.1(8) . . ? C86 C87 C88 121.3(9) . . ? C89 C88 C87 122.5(11) . . ? C89 C88 Cl3 118.4(10) . . ? C87 C88 Cl3 119.1(8) . . ? C88 C89 C90 120.6(14) . . ? C89A C90 C85 126.2(18) . . ? C89A C90 C89 14.0(12) . . ? C85 C90 C89 119.6(9) . . ? C96 C91 C92 118.3(5) . . ? C96 C91 C52 120.3(5) . . ? C92 C91 C52 121.4(6) . . ? C93 C92 C91 121.5(7) . . ? C94 C93 C92 118.2(7) . . ? C95 C94 C93 122.3(5) . . ? C95 C94 Cl4 123.0(7) . . ? C93 C94 Cl4 114.7(6) . . ? C95 C94 Cl4A 103.3(7) . . ? C93 C94 Cl4A 134.3(7) . . ? Cl4 C94 Cl4A 20.1(3) . . ? C94 C95 C96 119.0(7) . . ? C91 C96 C95 120.7(6) . . ? Cl6 C97 Cl5 111.2(5) . . ? Cl6 C97 Cl7 109.0(5) . . ? Cl5 C97 Cl7 111.2(5) . . ? C65A C64A C63A 111.1(8) . . ? O3 C65A C64A 108.3(8) . . ? O3 C65A C66A 102.3(7) . . ? C64A C65A C66A 114.2(8) . . ? C67A C66A C65A 116.1(9) . . ? C85 C86A C87A 131.0(19) . . ? C88A C87A C86A 113.1(18) . . ? C87A C88A C89A 119(2) . . ? C87A C88A Cl3A 118.0(15) . . ? C89A C88A Cl3A 122(2) . . ? C90 C89A C88A 118(3) . . ? Cl6A C97A Cl7A 106.5(7) . . ? Cl6A C97A Cl5A 113.0(7) . . ? Cl7A C97A Cl5A 110.3(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.358 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.094 #===END