# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ic15715 _database_code_depnum_ccdc_archive 'CCDC 910493' #TrackingRef '15357_web_deposit_cif_file_0_En-CheYang_1352708909.complex 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H65 Cl Dy2 N4 Ni2 O22' _chemical_formula_weight 1708.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.1004(8) _cell_length_b 14.7275(6) _cell_length_c 23.5622(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.9021(10) _cell_angle_gamma 90.00 _cell_volume 6529.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8265 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.15 _exptl_crystal_description block _exptl_crystal_colour light-blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 2.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4248 _exptl_absorpt_correction_T_max 0.5257 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49539 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14997 _reflns_number_gt 12141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+5.2412P] 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 14997 _refine_ls_number_parameters 853 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.171613(10) 0.020608(13) 0.162465(8) 0.01860(5) Uani 1 1 d . . . Dy2 Dy 0.280075(10) 0.152179(13) 0.063095(8) 0.01983(5) Uani 1 1 d . . . Ni1 Ni 0.35476(3) 0.02013(3) 0.17246(2) 0.01941(11) Uani 1 1 d . . . Ni2 Ni 0.25752(3) -0.07851(3) 0.06891(2) 0.01954(11) Uani 1 1 d . . . O1 O 0.27498(14) 0.11481(18) 0.16022(11) 0.0194(6) Uani 1 1 d . . . O2 O 0.27190(14) -0.07107(18) 0.15943(11) 0.0200(6) Uani 1 1 d . . . O3 O 0.33941(14) 0.01241(18) 0.08066(11) 0.0191(6) Uani 1 1 d . . . O4 O 0.19245(14) 0.03356(18) 0.06777(11) 0.0194(6) Uani 1 1 d . . . O5 O 0.19048(15) 0.0720(2) 0.25939(12) 0.0254(6) Uani 1 1 d . . . O6 O 0.17531(15) -0.07497(19) 0.24934(12) 0.0248(6) Uani 1 1 d . . . O7 O 0.21592(15) 0.1597(2) -0.03434(12) 0.0292(7) Uani 1 1 d . . . O8 O 0.32995(16) 0.1289(2) -0.02345(12) 0.0295(7) Uani 1 1 d . . . O9 O 0.12187(15) 0.16243(19) 0.13841(12) 0.0254(6) Uani 1 1 d . . . O10 O 0.18896(15) 0.23730(19) 0.08540(12) 0.0270(7) Uani 1 1 d . . . O11 O 0.11319(15) -0.10560(19) 0.12093(12) 0.0262(7) Uani 1 1 d . . . O12 O 0.18342(15) -0.17808(19) 0.06897(12) 0.0258(6) Uani 1 1 d . . . O13 O 0.39261(15) 0.19775(19) 0.10487(12) 0.0274(7) Uani 1 1 d . . . O14 O 0.44193(14) 0.09682(19) 0.17057(12) 0.0249(6) Uani 1 1 d . . . O15 O 0.05088(15) 0.02742(18) 0.18132(12) 0.0243(6) Uani 1 1 d . . . H15 H 0.0406 0.0797 0.2002 0.037 Uiso 1 1 d R . . O16 O 0.29913(16) 0.3105(2) 0.03842(13) 0.0308(7) Uani 1 1 d . . . H16 H 0.3050 0.3482 0.0695 0.046 Uiso 1 1 d R . . N1 N 0.36040(18) 0.0664(2) 0.25628(15) 0.0251(8) Uani 1 1 d . . . N2 N 0.41186(18) -0.0946(2) 0.19296(14) 0.0237(8) Uani 1 1 d . . . N3 N 0.33757(18) -0.1649(2) 0.05885(15) 0.0247(8) Uani 1 1 d . . . N4 N 0.21463(17) -0.0682(2) -0.01891(14) 0.0226(7) Uani 1 1 d . . . C1 C 0.4011(3) 0.0344(3) 0.3042(2) 0.0378(12) Uani 1 1 d . . . H1 H 0.4226 -0.0236 0.3030 0.045 Uiso 1 1 calc R . . C2 C 0.4127(3) 0.0821(4) 0.3549(2) 0.0483(14) Uani 1 1 d . . . H2 H 0.4430 0.0586 0.3878 0.058 Uiso 1 1 calc R . . C3 C 0.3797(3) 0.1648(4) 0.3573(2) 0.0417(13) Uani 1 1 d . . . H3 H 0.3866 0.1988 0.3920 0.050 Uiso 1 1 calc R . . C4 C 0.3367(2) 0.1975(3) 0.30884(18) 0.0310(10) Uani 1 1 d . . . H4 H 0.3122 0.2534 0.3099 0.037 Uiso 1 1 calc R . . C5 C 0.3296(2) 0.1475(3) 0.25842(17) 0.0229(9) Uani 1 1 d . . . C6 C 0.2888(2) 0.1843(3) 0.20270(17) 0.0218(9) Uani 1 1 d . . . H6A H 0.2432 0.2103 0.2096 0.026 Uiso 1 1 calc R . . H6B H 0.3165 0.2335 0.1884 0.026 Uiso 1 1 calc R . . C7 C 0.4831(2) -0.1009(3) 0.20541(19) 0.0299(10) Uani 1 1 d . . . H7 H 0.5110 -0.0478 0.2045 0.036 Uiso 1 1 calc R . . C8 C 0.5165(2) -0.1831(3) 0.2195(2) 0.0381(12) Uani 1 1 d . . . H8 H 0.5668 -0.1862 0.2294 0.046 Uiso 1 1 calc R . . C9 C 0.4761(3) -0.2604(3) 0.2191(2) 0.0376(12) Uani 1 1 d . . . H9 H 0.4981 -0.3178 0.2274 0.045 Uiso 1 1 calc R . . C10 C 0.4030(2) -0.2533(3) 0.20624(19) 0.0307(10) Uani 1 1 d . . . H10 H 0.3742 -0.3060 0.2053 0.037 Uiso 1 1 calc R . . C11 C 0.3725(2) -0.1695(3) 0.19481(17) 0.0225(9) Uani 1 1 d . . . C12 C 0.2929(2) -0.1554(3) 0.18627(18) 0.0222(9) Uani 1 1 d . . . H12A H 0.2690 -0.2053 0.1623 0.027 Uiso 1 1 calc R . . H12B H 0.2772 -0.1579 0.2242 0.027 Uiso 1 1 calc R . . C13 C 0.3336(2) -0.2559(3) 0.05390(19) 0.0301(10) Uani 1 1 d . . . H13 H 0.2912 -0.2858 0.0594 0.036 Uiso 1 1 calc R . . C14 C 0.3892(3) -0.3069(3) 0.0412(2) 0.0387(12) Uani 1 1 d . . . H14 H 0.3852 -0.3710 0.0378 0.046 Uiso 1 1 calc R . . C15 C 0.4510(3) -0.2630(3) 0.0335(2) 0.0421(13) Uani 1 1 d . . . H15A H 0.4900 -0.2968 0.0244 0.051 Uiso 1 1 calc R . . C16 C 0.4554(2) -0.1701(3) 0.0392(2) 0.0346(11) Uani 1 1 d . . . H16A H 0.4976 -0.1389 0.0345 0.042 Uiso 1 1 calc R . . C17 C 0.3969(2) -0.1221(3) 0.05207(17) 0.0247(9) Uani 1 1 d . . . C18 C 0.3977(2) -0.0209(3) 0.05689(19) 0.0263(9) Uani 1 1 d . . . H18A H 0.4426 -0.0016 0.0815 0.032 Uiso 1 1 calc R . . H18B H 0.3964 0.0058 0.0182 0.032 Uiso 1 1 calc R . . C19 C 0.2320(2) -0.1194(3) -0.06154(18) 0.0287(10) Uani 1 1 d . . . H19 H 0.2778 -0.1466 -0.0563 0.034 Uiso 1 1 calc R . . C20 C 0.1866(2) -0.1339(3) -0.11227(19) 0.0325(11) Uani 1 1 d . . . H20 H 0.2007 -0.1699 -0.1418 0.039 Uiso 1 1 calc R . . C21 C 0.1204(3) -0.0956(3) -0.1197(2) 0.0380(12) Uani 1 1 d . . . H21 H 0.0874 -0.1064 -0.1541 0.046 Uiso 1 1 calc R . . C22 C 0.1019(2) -0.0412(3) -0.0769(2) 0.0335(11) Uani 1 1 d . . . H22 H 0.0566 -0.0127 -0.0816 0.040 Uiso 1 1 calc R . . C23 C 0.1509(2) -0.0290(3) -0.02687(18) 0.0236(9) Uani 1 1 d . . . C24 C 0.1335(2) 0.0287(3) 0.02192(17) 0.0231(9) Uani 1 1 d . . . H24A H 0.1204 0.0906 0.0075 0.028 Uiso 1 1 calc R . . H24B H 0.0922 0.0024 0.0363 0.028 Uiso 1 1 calc R . . C25 C 0.1906(2) -0.0137(3) 0.34494(18) 0.0256(9) Uani 1 1 d . . . C26 C 0.1979(2) 0.0641(3) 0.37920(19) 0.0338(11) Uani 1 1 d . . . H26 H 0.1992 0.1223 0.3619 0.041 Uiso 1 1 calc R . . C27 C 0.2032(3) 0.0567(4) 0.4381(2) 0.0425(13) Uani 1 1 d . . . H27 H 0.2073 0.1098 0.4613 0.051 Uiso 1 1 calc R . . C28 C 0.2025(3) -0.0274(4) 0.4633(2) 0.0444(14) Uani 1 1 d . . . H28 H 0.2078 -0.0325 0.5040 0.053 Uiso 1 1 calc R . . C29 C 0.1941(3) -0.1047(4) 0.4295(2) 0.0440(13) Uani 1 1 d . . . H29 H 0.1925 -0.1625 0.4470 0.053 Uiso 1 1 calc R . . C30 C 0.1880(2) -0.0984(3) 0.37061(19) 0.0315(10) Uani 1 1 d . . . H30 H 0.1821 -0.1517 0.3476 0.038 Uiso 1 1 calc R . . C31 C 0.1853(2) -0.0052(3) 0.28124(18) 0.0245(9) Uani 1 1 d . . . C32 C 0.2614(2) 0.1122(3) -0.11746(17) 0.0232(9) Uani 1 1 d . . . C33 C 0.1977(2) 0.1281(3) -0.15445(18) 0.0313(10) Uani 1 1 d . . . H33 H 0.1588 0.1544 -0.1401 0.038 Uiso 1 1 calc R . . C34 C 0.1907(3) 0.1057(4) -0.2122(2) 0.0390(12) Uani 1 1 d . . . H34 H 0.1469 0.1165 -0.2373 0.047 Uiso 1 1 calc R . . C35 C 0.2469(3) 0.0680(3) -0.2334(2) 0.0362(11) Uani 1 1 d . . . H35 H 0.2419 0.0530 -0.2731 0.043 Uiso 1 1 calc R . . C36 C 0.3104(3) 0.0518(3) -0.19707(19) 0.0332(11) Uani 1 1 d . . . H36 H 0.3490 0.0253 -0.2117 0.040 Uiso 1 1 calc R . . C37 C 0.3178(2) 0.0741(3) -0.13945(19) 0.0297(10) Uani 1 1 d . . . H37 H 0.3617 0.0633 -0.1146 0.036 Uiso 1 1 calc R . . C38 C 0.2695(2) 0.1350(3) -0.05520(18) 0.0254(9) Uani 1 1 d . . . C39 C 0.1055(2) 0.3216(3) 0.12528(17) 0.0251(9) Uani 1 1 d . . . C40 C 0.0384(2) 0.3217(3) 0.1398(2) 0.0358(11) Uani 1 1 d . . . H40 H 0.0150 0.2663 0.1452 0.043 Uiso 1 1 calc R . . C41 C 0.0057(3) 0.4046(4) 0.1462(2) 0.0483(15) Uani 1 1 d . . . H41 H -0.0409 0.4056 0.1552 0.058 Uiso 1 1 calc R . . C42 C 0.0399(4) 0.4849(4) 0.1396(2) 0.0542(16) Uani 1 1 d . . . H42 H 0.0169 0.5410 0.1440 0.065 Uiso 1 1 calc R . . C43 C 0.1072(3) 0.4844(4) 0.1268(2) 0.0492(14) Uani 1 1 d . . . H43 H 0.1314 0.5400 0.1234 0.059 Uiso 1 1 calc R . . C44 C 0.1398(3) 0.4028(3) 0.11871(18) 0.0328(11) Uani 1 1 d . . . H44 H 0.1859 0.4024 0.1086 0.039 Uiso 1 1 calc R . . C45 C 0.1410(2) 0.2334(3) 0.11574(17) 0.0233(9) Uani 1 1 d . . . C46 C 0.0672(2) -0.2335(3) 0.06499(17) 0.0231(9) Uani 1 1 d . . . C47 C -0.0018(2) -0.2162(3) 0.07277(19) 0.0302(10) Uani 1 1 d . . . H47 H -0.0118 -0.1639 0.0935 0.036 Uiso 1 1 calc R . . C48 C -0.0562(2) -0.2747(3) 0.0505(2) 0.0341(11) Uani 1 1 d . . . H48 H -0.1034 -0.2624 0.0559 0.041 Uiso 1 1 calc R . . C49 C -0.0419(2) -0.3504(3) 0.02069(19) 0.0317(10) Uani 1 1 d . . . H49 H -0.0793 -0.3908 0.0056 0.038 Uiso 1 1 calc R . . C50 C 0.0263(3) -0.3680(3) 0.0125(2) 0.0372(12) Uani 1 1 d . . . H50 H 0.0359 -0.4207 -0.0081 0.045 Uiso 1 1 calc R . . C51 C 0.0810(2) -0.3092(3) 0.03423(19) 0.0293(10) Uani 1 1 d . . . H51 H 0.1279 -0.3210 0.0279 0.035 Uiso 1 1 calc R . . C52 C 0.1257(2) -0.1681(3) 0.08659(17) 0.0235(9) Uani 1 1 d . . . C53 C 0.5169(2) 0.2030(3) 0.13681(18) 0.0272(9) Uani 1 1 d . . . C54 C 0.5762(2) 0.1517(3) 0.1563(2) 0.0395(12) Uani 1 1 d . . . H54 H 0.5710 0.0918 0.1700 0.047 Uiso 1 1 calc R . . C55 C 0.6435(3) 0.1864(4) 0.1563(3) 0.0538(15) Uani 1 1 d . . . H55 H 0.6843 0.1502 0.1694 0.065 Uiso 1 1 calc R . . C56 C 0.6513(3) 0.2734(4) 0.1373(3) 0.0518(15) Uani 1 1 d . . . H56 H 0.6974 0.2979 0.1379 0.062 Uiso 1 1 calc R . . C57 C 0.5924(3) 0.3246(4) 0.1176(2) 0.0474(14) Uani 1 1 d . . . H57 H 0.5979 0.3845 0.1041 0.057 Uiso 1 1 calc R . . C58 C 0.5247(3) 0.2902(3) 0.1172(2) 0.0371(11) Uani 1 1 d . . . H58 H 0.4841 0.3263 0.1035 0.045 Uiso 1 1 calc R . . C59 C 0.4449(2) 0.1631(3) 0.13760(18) 0.0239(9) Uani 1 1 d . . . C60 C 0.0134(2) -0.0424(3) 0.2056(2) 0.0333(11) Uani 1 1 d . . . H60A H 0.0299 -0.1019 0.1948 0.050 Uiso 1 1 calc R . . H60B H -0.0377 -0.0366 0.1910 0.050 Uiso 1 1 calc R . . H60C H 0.0221 -0.0367 0.2477 0.050 Uiso 1 1 calc R . . C61 C 0.3509(3) 0.3370(4) 0.0046(3) 0.0614(17) Uani 1 1 d . . . H61A H 0.3927 0.2976 0.0137 0.092 Uiso 1 1 calc R . . H61B H 0.3650 0.4001 0.0134 0.092 Uiso 1 1 calc R . . H61C H 0.3307 0.3316 -0.0363 0.092 Uiso 1 1 calc R . . Cl1 Cl 0.36002(8) 0.49023(9) 0.14291(6) 0.0426(3) Uani 1 1 d . . . O17 O 0.3339(2) 0.4002(3) 0.14730(18) 0.0624(12) Uani 1 1 d . . . O18 O 0.3969(3) 0.5165(3) 0.1979(2) 0.0980(19) Uani 1 1 d . . . O19 O 0.4113(3) 0.4923(3) 0.1061(2) 0.0908(17) Uani 1 1 d . . . O20 O 0.3051(3) 0.5497(3) 0.1257(3) 0.106(2) Uani 1 1 d . . . O21 O 0.00023(18) 0.1665(2) 0.23888(15) 0.0413(8) Uani 1 1 d . . . H21A H -0.0381 0.1956 0.2354 0.062 Uiso 1 1 calc R . . C62 C 0.0524(3) 0.2102(4) 0.2797(2) 0.0528(15) Uani 1 1 d . . . H62A H 0.0556 0.2743 0.2692 0.079 Uiso 1 1 calc R . . H62B H 0.0986 0.1809 0.2801 0.079 Uiso 1 1 calc R . . H62C H 0.0393 0.2057 0.3180 0.079 Uiso 1 1 calc R . . O22 O 0.13033(19) 0.7435(2) 0.25864(15) 0.0398(8) Uani 1 1 d . . . H22A H 0.1490 0.7951 0.2582 0.060 Uiso 1 1 calc R . . C63 C 0.1619(3) 0.6832(3) 0.2231(2) 0.0473(14) Uani 1 1 d . . . H63A H 0.2138 0.6857 0.2340 0.071 Uiso 1 1 calc R . . H63B H 0.1483 0.7013 0.1827 0.071 Uiso 1 1 calc R . . H63C H 0.1454 0.6212 0.2281 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01950(10) 0.01769(10) 0.01920(10) -0.00213(7) 0.00496(7) -0.00054(7) Dy2 0.02002(10) 0.02095(10) 0.01888(10) 0.00145(8) 0.00437(7) 0.00220(8) Ni1 0.0188(2) 0.0181(3) 0.0209(3) 0.0002(2) 0.0022(2) -0.0001(2) Ni2 0.0183(2) 0.0200(3) 0.0203(3) -0.0032(2) 0.0036(2) 0.0011(2) O1 0.0202(14) 0.0190(14) 0.0183(14) -0.0031(11) 0.0015(11) -0.0005(11) O2 0.0231(14) 0.0153(14) 0.0215(15) 0.0010(11) 0.0035(12) 0.0002(11) O3 0.0166(13) 0.0221(15) 0.0194(14) -0.0010(11) 0.0055(11) 0.0009(11) O4 0.0179(14) 0.0218(15) 0.0176(14) -0.0027(11) 0.0005(11) 0.0005(11) O5 0.0288(16) 0.0252(16) 0.0236(16) -0.0021(13) 0.0084(13) -0.0075(13) O6 0.0295(16) 0.0217(16) 0.0242(16) -0.0008(12) 0.0071(13) 0.0006(12) O7 0.0262(16) 0.0386(19) 0.0237(16) 0.0020(13) 0.0072(13) 0.0064(14) O8 0.0293(16) 0.0363(18) 0.0228(16) -0.0030(13) 0.0042(13) 0.0062(14) O9 0.0259(15) 0.0225(16) 0.0292(16) 0.0027(13) 0.0087(13) 0.0017(12) O10 0.0298(16) 0.0268(17) 0.0269(16) 0.0049(13) 0.0117(13) 0.0069(13) O11 0.0286(16) 0.0226(16) 0.0287(16) -0.0083(13) 0.0087(13) -0.0051(13) O12 0.0231(15) 0.0239(16) 0.0308(17) -0.0051(13) 0.0061(13) -0.0031(12) O13 0.0253(16) 0.0250(16) 0.0306(17) 0.0046(13) 0.0014(13) -0.0002(13) O14 0.0223(15) 0.0245(16) 0.0267(16) 0.0030(13) 0.0010(12) -0.0016(12) O15 0.0243(15) 0.0211(15) 0.0292(17) -0.0053(12) 0.0089(13) -0.0039(12) O16 0.0350(17) 0.0276(17) 0.0312(17) 0.0057(14) 0.0098(14) 0.0004(14) N1 0.0291(19) 0.0236(19) 0.0231(19) 0.0017(15) 0.0055(15) -0.0036(15) N2 0.0233(18) 0.0249(19) 0.0221(18) 0.0028(15) 0.0013(14) -0.0008(15) N3 0.0265(19) 0.026(2) 0.0223(19) -0.0006(15) 0.0049(15) 0.0042(15) N4 0.0219(17) 0.0250(19) 0.0213(18) -0.0045(15) 0.0046(14) 0.0006(15) C1 0.047(3) 0.038(3) 0.027(3) 0.009(2) 0.001(2) 0.002(2) C2 0.065(4) 0.053(4) 0.023(3) -0.001(2) -0.006(2) 0.002(3) C3 0.054(3) 0.050(3) 0.020(2) -0.009(2) 0.002(2) -0.007(3) C4 0.039(3) 0.029(3) 0.026(2) -0.0108(19) 0.009(2) -0.009(2) C5 0.025(2) 0.024(2) 0.020(2) -0.0001(17) 0.0061(17) -0.0076(17) C6 0.024(2) 0.018(2) 0.025(2) -0.0050(17) 0.0070(17) -0.0028(16) C7 0.023(2) 0.032(3) 0.033(3) 0.002(2) -0.0003(18) 0.0015(19) C8 0.025(2) 0.039(3) 0.049(3) 0.008(2) 0.002(2) 0.014(2) C9 0.041(3) 0.030(3) 0.041(3) 0.006(2) 0.003(2) 0.014(2) C10 0.038(3) 0.023(2) 0.032(3) 0.0054(19) 0.008(2) 0.004(2) C11 0.027(2) 0.023(2) 0.017(2) 0.0001(17) 0.0028(17) 0.0016(17) C12 0.024(2) 0.017(2) 0.024(2) -0.0010(17) 0.0023(17) -0.0008(17) C13 0.036(3) 0.022(2) 0.032(3) -0.0037(19) 0.007(2) 0.0030(19) C14 0.047(3) 0.028(3) 0.043(3) -0.006(2) 0.012(2) 0.011(2) C15 0.039(3) 0.040(3) 0.050(3) -0.007(2) 0.015(2) 0.018(2) C16 0.028(2) 0.040(3) 0.038(3) -0.004(2) 0.013(2) 0.007(2) C17 0.029(2) 0.027(2) 0.018(2) -0.0026(17) 0.0063(17) 0.0033(18) C18 0.022(2) 0.028(2) 0.030(2) -0.0024(19) 0.0074(18) 0.0037(18) C19 0.028(2) 0.029(2) 0.029(2) -0.0029(19) 0.0056(19) 0.0031(19) C20 0.038(3) 0.033(3) 0.027(2) -0.011(2) 0.007(2) 0.000(2) C21 0.040(3) 0.042(3) 0.027(3) -0.008(2) -0.006(2) 0.001(2) C22 0.027(2) 0.035(3) 0.034(3) -0.008(2) -0.005(2) 0.006(2) C23 0.024(2) 0.023(2) 0.025(2) -0.0013(17) 0.0059(17) 0.0003(17) C24 0.019(2) 0.030(2) 0.020(2) -0.0009(17) 0.0030(16) 0.0024(17) C25 0.017(2) 0.036(3) 0.023(2) -0.0028(19) 0.0025(17) 0.0004(18) C26 0.033(3) 0.041(3) 0.028(3) -0.006(2) 0.007(2) -0.005(2) C27 0.041(3) 0.057(4) 0.030(3) -0.017(2) 0.006(2) -0.005(3) C28 0.045(3) 0.069(4) 0.019(2) 0.003(2) 0.005(2) 0.006(3) C29 0.049(3) 0.051(3) 0.035(3) 0.010(3) 0.016(2) 0.009(3) C30 0.033(2) 0.038(3) 0.024(2) 0.001(2) 0.0086(19) 0.007(2) C31 0.017(2) 0.033(3) 0.024(2) -0.0032(19) 0.0041(17) 0.0037(17) C32 0.029(2) 0.023(2) 0.019(2) 0.0025(17) 0.0073(17) -0.0027(18) C33 0.030(2) 0.041(3) 0.023(2) 0.001(2) 0.0043(19) 0.001(2) C34 0.033(3) 0.057(3) 0.024(2) -0.006(2) -0.003(2) -0.005(2) C35 0.045(3) 0.040(3) 0.024(2) -0.005(2) 0.007(2) -0.003(2) C36 0.039(3) 0.035(3) 0.027(3) -0.001(2) 0.011(2) 0.005(2) C37 0.033(2) 0.028(2) 0.028(2) 0.0024(19) 0.0046(19) 0.0067(19) C38 0.029(2) 0.024(2) 0.023(2) 0.0056(18) 0.0039(18) -0.0022(18) C39 0.030(2) 0.025(2) 0.019(2) 0.0011(17) 0.0021(17) 0.0072(18) C40 0.032(3) 0.043(3) 0.033(3) -0.002(2) 0.007(2) 0.011(2) C41 0.041(3) 0.066(4) 0.038(3) -0.011(3) 0.005(2) 0.024(3) C42 0.079(4) 0.040(3) 0.042(3) -0.007(3) 0.005(3) 0.031(3) C43 0.076(4) 0.031(3) 0.040(3) -0.001(2) 0.010(3) 0.013(3) C44 0.044(3) 0.030(3) 0.024(2) -0.0005(19) 0.004(2) 0.004(2) C45 0.022(2) 0.024(2) 0.023(2) -0.0005(18) 0.0005(17) -0.0005(17) C46 0.025(2) 0.024(2) 0.020(2) 0.0020(17) 0.0018(17) -0.0015(17) C47 0.032(2) 0.023(2) 0.035(3) -0.009(2) 0.006(2) 0.0002(19) C48 0.024(2) 0.035(3) 0.042(3) -0.001(2) 0.003(2) -0.001(2) C49 0.032(2) 0.033(3) 0.028(2) 0.000(2) -0.0022(19) -0.012(2) C50 0.048(3) 0.029(3) 0.036(3) -0.010(2) 0.011(2) -0.013(2) C51 0.033(2) 0.026(2) 0.032(2) -0.0041(19) 0.012(2) -0.0042(19) C52 0.027(2) 0.024(2) 0.017(2) -0.0006(17) 0.0000(17) -0.0032(18) C53 0.027(2) 0.028(2) 0.028(2) -0.0039(19) 0.0094(18) -0.0048(19) C54 0.028(2) 0.037(3) 0.055(3) 0.003(2) 0.009(2) -0.003(2) C55 0.024(3) 0.054(4) 0.086(5) 0.006(3) 0.016(3) 0.002(2) C56 0.036(3) 0.052(4) 0.073(4) -0.006(3) 0.026(3) -0.012(3) C57 0.057(4) 0.030(3) 0.061(4) -0.006(3) 0.026(3) -0.019(3) C58 0.037(3) 0.028(3) 0.048(3) 0.003(2) 0.012(2) -0.004(2) C59 0.020(2) 0.029(2) 0.024(2) -0.0060(18) 0.0045(17) -0.0030(17) C60 0.031(2) 0.031(3) 0.040(3) 0.005(2) 0.012(2) -0.004(2) C61 0.066(4) 0.062(4) 0.062(4) 0.017(3) 0.028(3) 0.004(3) Cl1 0.0600(8) 0.0327(7) 0.0371(7) 0.0005(5) 0.0135(6) -0.0079(6) O17 0.088(3) 0.037(2) 0.068(3) -0.007(2) 0.031(2) -0.021(2) O18 0.147(5) 0.072(3) 0.067(3) -0.006(3) -0.004(3) -0.044(3) O19 0.108(4) 0.068(3) 0.114(4) 0.016(3) 0.069(4) 0.001(3) O20 0.056(3) 0.065(3) 0.193(6) 0.037(4) 0.013(4) 0.002(3) O21 0.0376(19) 0.042(2) 0.046(2) -0.0139(17) 0.0114(17) 0.0059(16) C62 0.049(3) 0.052(4) 0.054(4) -0.022(3) -0.001(3) 0.015(3) O22 0.050(2) 0.0276(18) 0.042(2) 0.0016(16) 0.0100(16) -0.0116(16) C63 0.053(3) 0.033(3) 0.059(4) -0.001(3) 0.019(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O11 2.298(3) . ? Dy1 O9 2.324(3) . ? Dy1 O4 2.341(3) . ? Dy1 O2 2.355(3) . ? Dy1 O5 2.374(3) . ? Dy1 O1 2.421(3) . ? Dy1 O15 2.424(3) . ? Dy1 O6 2.475(3) . ? Dy1 Ni2 3.3055(5) . ? Dy1 Ni1 3.4655(5) . ? Dy1 Dy2 3.8983(3) . ? Dy2 O10 2.278(3) . ? Dy2 O13 2.305(3) . ? Dy2 O3 2.352(3) . ? Dy2 O1 2.372(3) . ? Dy2 O7 2.412(3) . ? Dy2 O8 2.419(3) . ? Dy2 O4 2.435(3) . ? Dy2 O16 2.445(3) . ? Dy2 Ni1 3.3456(5) . ? Dy2 Ni2 3.4303(6) . ? Ni1 O14 2.019(3) . ? Ni1 N2 2.024(3) . ? Ni1 O1 2.049(3) . ? Ni1 O2 2.058(3) . ? Ni1 N1 2.074(3) . ? Ni1 O3 2.135(3) . ? Ni2 N3 2.034(3) . ? Ni2 O12 2.038(3) . ? Ni2 O3 2.041(3) . ? Ni2 O4 2.063(3) . ? Ni2 N4 2.096(3) . ? Ni2 O2 2.106(3) . ? O1 C6 1.424(4) . ? O2 C12 1.420(5) . ? O3 C18 1.418(5) . ? O4 C24 1.422(5) . ? O5 C31 1.259(5) . ? O6 C31 1.269(5) . ? O7 C38 1.263(5) . ? O8 C38 1.266(5) . ? O9 C45 1.257(5) . ? O10 C45 1.256(5) . ? O11 C52 1.275(5) . ? O12 C52 1.253(5) . ? O13 C59 1.260(5) . ? O14 C59 1.254(5) . ? O15 C60 1.429(5) . ? O16 C61 1.427(6) . ? N1 C5 1.337(5) . ? N1 C1 1.342(6) . ? N2 C11 1.339(5) . ? N2 C7 1.345(5) . ? N3 C17 1.329(5) . ? N3 C13 1.347(5) . ? N4 C23 1.331(5) . ? N4 C19 1.343(5) . ? C1 C2 1.369(7) . ? C2 C3 1.376(7) . ? C3 C4 1.374(7) . ? C4 C5 1.384(6) . ? C5 C6 1.507(6) . ? C7 C8 1.382(6) . ? C8 C9 1.374(7) . ? C9 C10 1.379(6) . ? C10 C11 1.373(6) . ? C11 C12 1.514(5) . ? C13 C14 1.374(6) . ? C14 C15 1.385(7) . ? C15 C16 1.377(7) . ? C16 C17 1.399(6) . ? C17 C18 1.495(6) . ? C19 C20 1.368(6) . ? C20 C21 1.368(6) . ? C21 C22 1.382(6) . ? C22 C23 1.385(6) . ? C23 C24 1.512(6) . ? C25 C30 1.390(6) . ? C25 C26 1.396(6) . ? C25 C31 1.492(6) . ? C26 C27 1.379(6) . ? C27 C28 1.375(7) . ? C28 C29 1.383(7) . ? C29 C30 1.375(6) . ? C32 C33 1.389(6) . ? C32 C37 1.391(6) . ? C32 C38 1.487(6) . ? C33 C34 1.384(6) . ? C34 C35 1.377(7) . ? C35 C36 1.380(7) . ? C36 C37 1.380(6) . ? C39 C40 1.383(6) . ? C39 C44 1.385(6) . ? C39 C45 1.499(6) . ? C40 C41 1.390(7) . ? C41 C42 1.374(8) . ? C42 C43 1.371(8) . ? C43 C44 1.381(7) . ? C46 C51 1.379(6) . ? C46 C47 1.385(6) . ? C46 C52 1.496(6) . ? C47 C48 1.381(6) . ? C48 C49 1.370(6) . ? C49 C50 1.374(7) . ? C50 C51 1.386(6) . ? C53 C54 1.374(6) . ? C53 C58 1.382(6) . ? C53 C59 1.500(6) . ? C54 C55 1.384(7) . ? C55 C56 1.373(8) . ? C56 C57 1.368(8) . ? C57 C58 1.386(7) . ? Cl1 O20 1.373(5) . ? Cl1 O19 1.416(5) . ? Cl1 O18 1.417(5) . ? Cl1 O17 1.427(4) . ? O21 C62 1.416(6) . ? O22 C63 1.425(6) . ? 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 O11 Dy1 O9 118.35(10) . . ? O11 Dy1 O4 79.03(9) . . ? O9 Dy1 O4 79.84(9) . . ? O11 Dy1 O2 82.03(10) . . ? O9 Dy1 O2 143.95(9) . . ? O4 Dy1 O2 75.24(9) . . ? O11 Dy1 O5 130.53(10) . . ? O9 Dy1 O5 86.33(10) . . ? O4 Dy1 O5 150.28(9) . . ? O2 Dy1 O5 102.85(10) . . ? O11 Dy1 O1 142.39(9) . . ? O9 Dy1 O1 77.31(9) . . ? O4 Dy1 O1 70.09(9) . . ? O2 Dy1 O1 69.95(9) . . ? O5 Dy1 O1 81.31(9) . . ? O11 Dy1 O15 72.78(9) . . ? O9 Dy1 O15 69.25(9) . . ? O4 Dy1 O15 119.63(9) . . ? O2 Dy1 O15 146.48(9) . . ? O5 Dy1 O15 78.60(9) . . ? O1 Dy1 O15 141.74(9) . . ? O11 Dy1 O6 80.50(10) . . ? O9 Dy1 O6 131.69(9) . . ? O4 Dy1 O6 148.14(9) . . ? O2 Dy1 O6 77.96(9) . . ? O5 Dy1 O6 53.69(9) . . ? O1 Dy1 O6 115.89(9) . . ? O15 Dy1 O6 76.39(9) . . ? O11 Dy1 Ni2 67.62(7) . . ? O9 Dy1 Ni2 117.60(7) . . ? O4 Dy1 Ni2 38.28(6) . . ? O2 Dy1 Ni2 39.36(6) . . ? O5 Dy1 Ni2 140.51(7) . . ? O1 Dy1 Ni2 74.83(6) . . ? O15 Dy1 Ni2 137.51(7) . . ? O6 Dy1 Ni2 110.70(6) . . ? O11 Dy1 Ni1 115.96(7) . . ? O9 Dy1 Ni1 112.58(7) . . ? O4 Dy1 Ni1 74.32(6) . . ? O2 Dy1 Ni1 35.31(6) . . ? O5 Dy1 Ni1 87.18(7) . . ? O1 Dy1 Ni1 35.43(6) . . ? O15 Dy1 Ni1 165.58(7) . . ? O6 Dy1 Ni1 93.31(7) . . ? Ni2 Dy1 Ni1 55.485(12) . . ? O11 Dy1 Dy2 114.55(7) . . ? O9 Dy1 Dy2 69.14(7) . . ? O4 Dy1 Dy2 36.09(6) . . ? O2 Dy1 Dy2 75.38(6) . . ? O5 Dy1 Dy2 114.26(7) . . ? O1 Dy1 Dy2 35.16(6) . . ? O15 Dy1 Dy2 135.23(7) . . ? O6 Dy1 Dy2 146.81(7) . . ? Ni2 Dy1 Dy2 56.148(10) . . ? Ni1 Dy1 Dy2 53.653(9) . . ? O10 Dy2 O13 115.75(11) . . ? O10 Dy2 O3 143.62(9) . . ? O13 Dy2 O3 78.11(10) . . ? O10 Dy2 O1 75.25(9) . . ? O13 Dy2 O1 81.11(9) . . ? O3 Dy2 O1 74.07(9) . . ? O10 Dy2 O7 84.90(10) . . ? O13 Dy2 O7 132.62(10) . . ? O3 Dy2 O7 110.98(10) . . ? O1 Dy2 O7 146.16(9) . . ? O10 Dy2 O8 134.39(10) . . ? O13 Dy2 O8 85.86(10) . . ? O3 Dy2 O8 77.09(9) . . ? O1 Dy2 O8 150.21(10) . . ? O7 Dy2 O8 54.08(10) . . ? O10 Dy2 O4 79.98(10) . . ? O13 Dy2 O4 141.94(9) . . ? O3 Dy2 O4 71.23(9) . . ? O1 Dy2 O4 69.34(9) . . ? O7 Dy2 O4 80.51(9) . . ? O8 Dy2 O4 108.05(10) . . ? O10 Dy2 O16 71.40(10) . . ? O13 Dy2 O16 70.00(10) . . ? O3 Dy2 O16 142.13(9) . . ? O1 Dy2 O16 118.89(10) . . ? O7 Dy2 O16 78.59(10) . . ? O8 Dy2 O16 80.70(10) . . ? O4 Dy2 O16 145.74(9) . . ? O10 Dy2 Ni1 112.56(7) . . ? O13 Dy2 Ni1 66.26(7) . . ? O3 Dy2 Ni1 39.37(6) . . ? O1 Dy2 Ni1 37.33(6) . . ? O7 Dy2 Ni1 147.06(7) . . ? O8 Dy2 Ni1 112.91(7) . . ? O4 Dy2 Ni1 75.73(6) . . ? O16 Dy2 Ni1 132.55(7) . . ? O10 Dy2 Ni2 115.44(7) . . ? O13 Dy2 Ni2 112.69(7) . . ? O3 Dy2 Ni2 35.53(6) . . ? O1 Dy2 Ni2 72.86(6) . . ? O7 Dy2 Ni2 92.09(7) . . ? O8 Dy2 Ni2 87.92(7) . . ? O4 Dy2 Ni2 36.44(6) . . ? O16 Dy2 Ni2 168.15(7) . . ? Ni1 Dy2 Ni2 55.485(12) . . ? O10 Dy2 Dy1 68.23(7) . . ? O13 Dy2 Dy1 116.17(7) . . ? O3 Dy2 Dy1 75.47(6) . . ? O1 Dy2 Dy1 36.00(6) . . ? O7 Dy2 Dy1 111.03(7) . . ? O8 Dy2 Dy1 139.72(7) . . ? O4 Dy2 Dy1 34.49(6) . . ? O16 Dy2 Dy1 137.14(7) . . ? Ni1 Dy2 Dy1 56.545(10) . . ? Ni2 Dy2 Dy1 53.155(9) . . ? O14 Ni1 N2 93.44(12) . . ? O14 Ni1 O1 102.26(11) . . ? N2 Ni1 O1 163.50(12) . . ? O14 Ni1 O2 167.91(11) . . ? N2 Ni1 O2 81.93(12) . . ? O1 Ni1 O2 83.62(11) . . ? O14 Ni1 N1 85.94(12) . . ? N2 Ni1 N1 96.28(14) . . ? O1 Ni1 N1 79.98(12) . . ? O2 Ni1 N1 105.61(12) . . ? O14 Ni1 O3 88.71(11) . . ? N2 Ni1 O3 99.90(12) . . ? O1 Ni1 O3 85.66(10) . . ? O2 Ni1 O3 81.14(10) . . ? N1 Ni1 O3 163.23(12) . . ? O14 Ni1 Dy2 84.36(8) . . ? N2 Ni1 Dy2 144.10(10) . . ? O1 Ni1 Dy2 44.58(7) . . ? O2 Ni1 Dy2 92.83(7) . . ? N1 Ni1 Dy2 119.19(10) . . ? O3 Ni1 Dy2 44.32(7) . . ? O14 Ni1 Dy1 145.49(8) . . ? N2 Ni1 Dy1 120.93(10) . . ? O1 Ni1 Dy1 43.23(7) . . ? O2 Ni1 Dy1 41.39(7) . . ? N1 Ni1 Dy1 87.16(10) . . ? O3 Ni1 Dy1 88.29(7) . . ? Dy2 Ni1 Dy1 69.802(11) . . ? N3 Ni2 O12 94.93(13) . . ? N3 Ni2 O3 81.51(12) . . ? O12 Ni2 O3 171.04(11) . . ? N3 Ni2 O4 164.14(13) . . ? O12 Ni2 O4 99.14(11) . . ? O3 Ni2 O4 85.57(10) . . ? N3 Ni2 N4 96.00(13) . . ? O12 Ni2 N4 84.23(12) . . ? O3 Ni2 N4 104.27(12) . . ? O4 Ni2 N4 78.27(12) . . ? N3 Ni2 O2 100.41(12) . . ? O12 Ni2 O2 90.37(11) . . ? O3 Ni2 O2 82.24(10) . . ? O4 Ni2 O2 86.84(10) . . ? N4 Ni2 O2 163.11(12) . . ? N3 Ni2 Dy1 145.40(10) . . ? O12 Ni2 Dy1 83.85(8) . . ? O3 Ni2 Dy1 94.39(7) . . ? O4 Ni2 Dy1 44.64(7) . . ? N4 Ni2 Dy1 118.14(9) . . ? O2 Ni2 Dy1 45.16(7) . . ? N3 Ni2 Dy2 120.85(10) . . ? O12 Ni2 Dy2 143.58(8) . . ? O3 Ni2 Dy2 42.03(7) . . ? O4 Ni2 Dy2 44.50(7) . . ? N4 Ni2 Dy2 85.35(9) . . ? O2 Ni2 Dy2 89.63(7) . . ? Dy1 Ni2 Dy2 70.697(11) . . ? C6 O1 Ni1 110.3(2) . . ? C6 O1 Dy2 118.6(2) . . ? Ni1 O1 Dy2 98.10(10) . . ? C6 O1 Dy1 116.7(2) . . ? Ni1 O1 Dy1 101.33(11) . . ? Dy2 O1 Dy1 108.85(10) . . ? C12 O2 Ni1 110.7(2) . . ? C12 O2 Ni2 112.5(2) . . ? Ni1 O2 Ni2 98.51(11) . . ? C12 O2 Dy1 131.1(2) . . ? Ni1 O2 Dy1 103.30(11) . . ? Ni2 O2 Dy1 95.48(10) . . ? C18 O3 Ni2 110.8(2) . . ? C18 O3 Ni1 116.0(2) . . ? Ni2 O3 Ni1 98.10(11) . . ? C18 O3 Dy2 128.4(2) . . ? Ni2 O3 Dy2 102.44(11) . . ? Ni1 O3 Dy2 96.30(10) . . ? C24 O4 Ni2 111.5(2) . . ? C24 O4 Dy1 118.5(2) . . ? Ni2 O4 Dy1 97.08(10) . . ? C24 O4 Dy2 117.6(2) . . ? Ni2 O4 Dy2 99.05(10) . . ? Dy1 O4 Dy2 109.42(10) . . ? C31 O5 Dy1 95.5(2) . . ? C31 O6 Dy1 90.5(2) . . ? C38 O7 Dy2 92.5(2) . . ? C38 O8 Dy2 92.1(2) . . ? C45 O9 Dy1 135.6(3) . . ? C45 O10 Dy2 140.0(3) . . ? C52 O11 Dy1 136.4(3) . . ? C52 O12 Ni2 124.5(3) . . ? C59 O13 Dy2 136.5(3) . . ? C59 O14 Ni1 125.0(3) . . ? C60 O15 Dy1 127.0(3) . . ? C61 O16 Dy2 122.7(3) . . ? C5 N1 C1 118.5(4) . . ? C5 N1 Ni1 112.2(3) . . ? C1 N1 Ni1 127.9(3) . . ? C11 N2 C7 119.2(4) . . ? C11 N2 Ni1 114.4(3) . . ? C7 N2 Ni1 126.4(3) . . ? C17 N3 C13 119.8(4) . . ? C17 N3 Ni2 113.0(3) . . ? C13 N3 Ni2 126.9(3) . . ? C23 N4 C19 118.4(4) . . ? C23 N4 Ni2 111.3(3) . . ? C19 N4 Ni2 126.3(3) . . ? N1 C1 C2 122.5(5) . . ? C1 C2 C3 118.9(5) . . ? C4 C3 C2 119.2(4) . . ? C3 C4 C5 118.9(5) . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 117.0(3) . . ? C4 C5 C6 121.1(4) . . ? O1 C6 C5 111.1(3) . . ? N2 C7 C8 121.4(4) . . ? C9 C8 C7 119.2(4) . . ? C8 C9 C10 119.0(4) . . ? C11 C10 C9 119.3(4) . . ? N2 C11 C10 121.7(4) . . ? N2 C11 C12 116.1(4) . . ? C10 C11 C12 122.1(4) . . ? O2 C12 C11 112.3(3) . . ? N3 C13 C14 121.9(4) . . ? C13 C14 C15 118.8(5) . . ? C16 C15 C14 119.4(4) . . ? C15 C16 C17 119.0(4) . . ? N3 C17 C16 121.1(4) . . ? N3 C17 C18 117.5(4) . . ? C16 C17 C18 121.4(4) . . ? O3 C18 C17 112.1(3) . . ? N4 C19 C20 122.7(4) . . ? C21 C20 C19 118.8(4) . . ? C20 C21 C22 119.5(4) . . ? C21 C22 C23 118.4(4) . . ? N4 C23 C22 122.2(4) . . ? N4 C23 C24 116.9(4) . . ? C22 C23 C24 121.0(4) . . ? O4 C24 C23 110.9(3) . . ? C30 C25 C26 119.5(4) . . ? C30 C25 C31 120.8(4) . . ? C26 C25 C31 119.7(4) . . ? C27 C26 C25 120.0(5) . . ? C28 C27 C26 120.1(5) . . ? C27 C28 C29 120.1(5) . . ? C30 C29 C28 120.5(5) . . ? C29 C30 C25 119.7(5) . . ? O5 C31 O6 120.3(4) . . ? O5 C31 C25 119.4(4) . . ? O6 C31 C25 120.3(4) . . ? C33 C32 C37 119.0(4) . . ? C33 C32 C38 120.8(4) . . ? C37 C32 C38 120.2(4) . . ? C34 C33 C32 120.2(4) . . ? C35 C34 C33 120.2(4) . . ? C34 C35 C36 120.1(4) . . ? C35 C36 C37 119.9(4) . . ? C36 C37 C32 120.5(4) . . ? O7 C38 O8 120.5(4) . . ? O7 C38 C32 119.7(4) . . ? O8 C38 C32 119.8(4) . . ? C40 C39 C44 120.2(4) . . ? C40 C39 C45 120.1(4) . . ? C44 C39 C45 119.8(4) . . ? C39 C40 C41 118.7(5) . . ? C42 C41 C40 120.8(5) . . ? C43 C42 C41 120.2(5) . . ? C42 C43 C44 119.8(5) . . ? C43 C44 C39 120.2(5) . . ? O10 C45 O9 125.0(4) . . ? O10 C45 C39 116.0(4) . . ? O9 C45 C39 119.0(4) . . ? C51 C46 C47 119.3(4) . . ? C51 C46 C52 120.1(4) . . ? C47 C46 C52 120.5(4) . . ? C48 C47 C46 120.4(4) . . ? C49 C48 C47 119.9(4) . . ? C48 C49 C50 120.2(4) . . ? C49 C50 C51 120.2(4) . . ? C46 C51 C50 120.0(4) . . ? O12 C52 O11 124.5(4) . . ? O12 C52 C46 117.4(4) . . ? O11 C52 C46 118.1(4) . . ? C54 C53 C58 119.5(4) . . ? C54 C53 C59 119.0(4) . . ? C58 C53 C59 121.4(4) . . ? C53 C54 C55 120.6(5) . . ? C56 C55 C54 119.8(5) . . ? C57 C56 C55 119.8(5) . . ? C56 C57 C58 120.8(5) . . ? C53 C58 C57 119.4(5) . . ? O14 C59 O13 125.4(4) . . ? O14 C59 C53 116.9(4) . . ? O13 C59 C53 117.7(4) . . ? O20 Cl1 O19 112.2(3) . . ? O20 Cl1 O18 109.3(4) . . ? O19 Cl1 O18 105.5(4) . . ? O20 Cl1 O17 110.8(3) . . ? O19 Cl1 O17 110.6(3) . . ? O18 Cl1 O17 108.2(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.433 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.127 data_ic15717 _database_code_depnum_ccdc_archive 'CCDC 910494' #TrackingRef '15358_web_deposit_cif_file_1_En-CheYang_1352708909.complex 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H65 Cl Dy2 N4 O22 Zn2' _chemical_formula_weight 1721.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.1917(8) _cell_length_b 14.7897(6) _cell_length_c 23.5660(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.3505(10) _cell_angle_gamma 90.00 _cell_volume 6600.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3823 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 20.82 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.732 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 3.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5135 _exptl_absorpt_correction_T_max 0.6555 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42411 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15116 _reflns_number_gt 10917 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+4.3710P] 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 15116 _refine_ls_number_parameters 853 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.281792(14) 0.152370(17) 0.563583(10) 0.02082(7) Uani 1 1 d . . . Dy2 Dy 0.173013(14) 0.021662(17) 0.663193(10) 0.01946(7) Uani 1 1 d . . . Zn1 Zn 0.25978(3) -0.08180(4) 0.56965(3) 0.02187(15) Uani 1 1 d . . . Zn2 Zn 0.35937(4) 0.02309(4) 0.67539(3) 0.02254(15) Uani 1 1 d . . . O1 O 0.1951(2) 0.0349(2) 0.56832(15) 0.0220(8) Uani 1 1 d . . . O2 O 0.3412(2) 0.0143(2) 0.57936(15) 0.0222(8) Uani 1 1 d . . . O3 O 0.2727(2) -0.0698(2) 0.66173(15) 0.0223(9) Uani 1 1 d . . . O4 O 0.27612(19) 0.1160(2) 0.66175(14) 0.0217(8) Uani 1 1 d . . . O5 O 0.2171(2) 0.1578(3) 0.46697(16) 0.0311(10) Uani 1 1 d . . . O6 O 0.3312(2) 0.1320(3) 0.47571(16) 0.0321(10) Uani 1 1 d . . . O7 O 0.1927(2) 0.0729(3) 0.75990(15) 0.0274(9) Uani 1 1 d . . . O8 O 0.1735(2) -0.0731(3) 0.75037(15) 0.0275(9) Uani 1 1 d . . . O9 O 0.1909(2) 0.2377(2) 0.58583(16) 0.0291(10) Uani 1 1 d . . . O10 O 0.1234(2) 0.1634(2) 0.63902(16) 0.0280(9) Uani 1 1 d . . . O11 O 0.3938(2) 0.1984(3) 0.60605(16) 0.0277(9) Uani 1 1 d . . . O12 O 0.4478(2) 0.0956(3) 0.66721(16) 0.0306(10) Uani 1 1 d . . . O13 O 0.1155(2) -0.1054(2) 0.62140(16) 0.0290(9) Uani 1 1 d . . . O14 O 0.1869(2) -0.1843(2) 0.57341(17) 0.0303(10) Uani 1 1 d . . . O15 O 0.3000(2) 0.3101(3) 0.53888(16) 0.0337(10) Uani 1 1 d . . . H15 H 0.2967 0.3397 0.5618 0.051 Uiso 1 1 d R . . O16 O 0.0529(2) 0.0290(2) 0.68193(16) 0.0282(9) Uani 1 1 d . . . H16 H 0.0369 0.0732 0.6977 0.042 Uiso 1 1 d R . . N1 N 0.2107(3) -0.0718(3) 0.48066(19) 0.0300(12) Uani 1 1 d . . . N2 N 0.3432(3) -0.1639(3) 0.55724(18) 0.0242(11) Uani 1 1 d . . . N3 N 0.4116(3) -0.0951(3) 0.69827(19) 0.0260(11) Uani 1 1 d . . . N4 N 0.3641(3) 0.0797(3) 0.7588(2) 0.0313(12) Uani 1 1 d . . . C1 C 0.2234(4) -0.1254(4) 0.4383(3) 0.0415(17) Uani 1 1 d . . . H1 H 0.2679 -0.1549 0.4423 0.050 Uiso 1 1 calc R . . C2 C 0.1760(4) -0.1405(4) 0.3894(3) 0.0456(18) Uani 1 1 d . . . H2 H 0.1881 -0.1778 0.3596 0.055 Uiso 1 1 calc R . . C3 C 0.1104(4) -0.1006(5) 0.3841(3) 0.051(2) Uani 1 1 d . . . H3 H 0.0758 -0.1119 0.3512 0.061 Uiso 1 1 calc R . . C4 C 0.0957(4) -0.0441(4) 0.4271(3) 0.0401(17) Uani 1 1 d . . . H4 H 0.0512 -0.0148 0.4241 0.048 Uiso 1 1 calc R . . C5 C 0.1472(3) -0.0308(4) 0.4750(2) 0.0316(14) Uani 1 1 d . . . C6 C 0.1339(3) 0.0299(4) 0.5242(2) 0.0279(13) Uani 1 1 d . . . H6A H 0.1214 0.0913 0.5092 0.033 Uiso 1 1 calc R . . H6B H 0.0934 0.0059 0.5408 0.033 Uiso 1 1 calc R . . C7 C 0.3421(3) -0.2537(4) 0.5530(2) 0.0334(15) Uani 1 1 d . . . H7 H 0.3010 -0.2853 0.5597 0.040 Uiso 1 1 calc R . . C8 C 0.3979(4) -0.3023(4) 0.5394(3) 0.0406(17) Uani 1 1 d . . . H8 H 0.3954 -0.3663 0.5361 0.049 Uiso 1 1 calc R . . C9 C 0.4579(4) -0.2564(4) 0.5306(3) 0.0442(18) Uani 1 1 d . . . H9 H 0.4973 -0.2885 0.5210 0.053 Uiso 1 1 calc R . . C10 C 0.4601(4) -0.1640(4) 0.5357(3) 0.0382(16) Uani 1 1 d . . . H10 H 0.5010 -0.1310 0.5303 0.046 Uiso 1 1 calc R . . C11 C 0.4003(3) -0.1197(4) 0.5492(2) 0.0284(14) Uani 1 1 d . . . C12 C 0.3999(3) -0.0175(4) 0.5550(2) 0.0298(14) Uani 1 1 d . . . H12A H 0.4441 0.0021 0.5795 0.036 Uiso 1 1 calc R . . H12B H 0.3985 0.0100 0.5166 0.036 Uiso 1 1 calc R . . C13 C 0.4822(3) -0.1043(5) 0.7120(3) 0.0383(16) Uani 1 1 d . . . H13 H 0.5113 -0.0524 0.7116 0.046 Uiso 1 1 calc R . . C14 C 0.5135(4) -0.1866(4) 0.7264(3) 0.0407(17) Uani 1 1 d . . . H14 H 0.5633 -0.1912 0.7373 0.049 Uiso 1 1 calc R . . C15 C 0.4718(4) -0.2611(4) 0.7247(3) 0.0440(18) Uani 1 1 d . . . H15A H 0.4926 -0.3188 0.7331 0.053 Uiso 1 1 calc R . . C16 C 0.3993(4) -0.2534(4) 0.7108(3) 0.0354(15) Uani 1 1 d . . . H16A H 0.3698 -0.3052 0.7095 0.042 Uiso 1 1 calc R . . C17 C 0.3711(3) -0.1690(4) 0.6991(2) 0.0249(13) Uani 1 1 d . . . C18 C 0.2919(3) -0.1531(4) 0.6890(2) 0.0254(13) Uani 1 1 d . . . H18A H 0.2684 -0.2027 0.6649 0.030 Uiso 1 1 calc R . . H18B H 0.2747 -0.1546 0.7264 0.030 Uiso 1 1 calc R . . C19 C 0.4060(4) 0.0548(4) 0.8076(3) 0.0403(17) Uani 1 1 d . . . H19 H 0.4316 -0.0002 0.8078 0.048 Uiso 1 1 calc R . . C20 C 0.4136(4) 0.1048(5) 0.8571(3) 0.052(2) Uani 1 1 d . . . H20 H 0.4438 0.0851 0.8908 0.062 Uiso 1 1 calc R . . C21 C 0.3760(4) 0.1852(5) 0.8570(3) 0.0467(19) Uani 1 1 d . . . H21 H 0.3807 0.2219 0.8905 0.056 Uiso 1 1 calc R . . C22 C 0.3321(3) 0.2107(4) 0.8078(2) 0.0364(16) Uani 1 1 d . . . H22 H 0.3042 0.2639 0.8071 0.044 Uiso 1 1 calc R . . C23 C 0.3290(3) 0.1578(4) 0.7592(2) 0.0267(13) Uani 1 1 d . . . C24 C 0.2871(3) 0.1887(3) 0.7023(2) 0.0236(13) Uani 1 1 d . . . H24A H 0.2408 0.2126 0.7087 0.028 Uiso 1 1 calc R . . H24B H 0.3128 0.2382 0.6864 0.028 Uiso 1 1 calc R . . C25 C 0.2617(3) 0.1067(4) 0.3833(2) 0.0226(12) Uani 1 1 d . . . C26 C 0.1977(3) 0.1199(4) 0.3471(2) 0.0344(15) Uani 1 1 d . . . H26 H 0.1591 0.1461 0.3618 0.041 Uiso 1 1 calc R . . C27 C 0.1901(4) 0.0949(5) 0.2899(3) 0.0425(17) Uani 1 1 d . . . H27 H 0.1462 0.1040 0.2655 0.051 Uiso 1 1 calc R . . C28 C 0.2454(4) 0.0569(4) 0.2682(3) 0.0423(18) Uani 1 1 d . . . H28 H 0.2400 0.0396 0.2289 0.051 Uiso 1 1 calc R . . C29 C 0.3090(4) 0.0441(4) 0.3041(3) 0.0391(17) Uani 1 1 d . . . H29 H 0.3474 0.0182 0.2891 0.047 Uiso 1 1 calc R . . C30 C 0.3180(3) 0.0682(4) 0.3614(2) 0.0318(15) Uani 1 1 d . . . H30 H 0.3620 0.0587 0.3856 0.038 Uiso 1 1 calc R . . C31 C 0.2708(3) 0.1344(4) 0.4453(2) 0.0270(13) Uani 1 1 d . . . C32 C 0.1900(3) -0.0104(4) 0.8458(2) 0.0289(14) Uani 1 1 d . . . C33 C 0.1862(3) -0.0945(4) 0.8716(2) 0.0338(15) Uani 1 1 d . . . H33 H 0.1797 -0.1476 0.8486 0.041 Uiso 1 1 calc R . . C34 C 0.1918(4) -0.1011(5) 0.9311(3) 0.0473(19) Uani 1 1 d . . . H34 H 0.1896 -0.1585 0.9489 0.057 Uiso 1 1 calc R . . C35 C 0.2008(4) -0.0232(6) 0.9640(3) 0.051(2) Uani 1 1 d . . . H35 H 0.2054 -0.0275 1.0047 0.061 Uiso 1 1 calc R . . C36 C 0.2030(4) 0.0607(5) 0.9386(3) 0.0462(19) Uani 1 1 d . . . H36 H 0.2083 0.1137 0.9617 0.055 Uiso 1 1 calc R . . C37 C 0.1976(4) 0.0677(5) 0.8793(3) 0.0402(17) Uani 1 1 d . . . H37 H 0.1990 0.1253 0.8617 0.048 Uiso 1 1 calc R . . C38 C 0.1852(3) -0.0031(4) 0.7818(2) 0.0255(13) Uani 1 1 d . . . C39 C 0.1069(3) 0.3217(4) 0.6259(2) 0.0269(13) Uani 1 1 d . . . C40 C 0.1416(4) 0.4024(4) 0.6198(2) 0.0328(15) Uani 1 1 d . . . H40 H 0.1879 0.4015 0.6103 0.039 Uiso 1 1 calc R . . C41 C 0.1090(5) 0.4849(5) 0.6274(3) 0.050(2) Uani 1 1 d . . . H41 H 0.1331 0.5403 0.6239 0.061 Uiso 1 1 calc R . . C42 C 0.0416(5) 0.4849(5) 0.6401(3) 0.058(2) Uani 1 1 d . . . H42 H 0.0185 0.5406 0.6446 0.069 Uiso 1 1 calc R . . C43 C 0.0076(4) 0.4052(5) 0.6464(3) 0.0485(19) Uani 1 1 d . . . H43 H -0.0388 0.4065 0.6555 0.058 Uiso 1 1 calc R . . C44 C 0.0393(3) 0.3227(4) 0.6397(3) 0.0375(16) Uani 1 1 d . . . H44 H 0.0152 0.2678 0.6445 0.045 Uiso 1 1 calc R . . C45 C 0.1424(3) 0.2345(4) 0.6162(2) 0.0254(13) Uani 1 1 d . . . C46 C 0.5182(3) 0.2075(4) 0.6339(2) 0.0305(14) Uani 1 1 d . . . C47 C 0.5229(4) 0.2975(5) 0.6184(3) 0.0436(17) Uani 1 1 d . . . H47 H 0.4815 0.3330 0.6080 0.052 Uiso 1 1 calc R . . C48 C 0.5900(5) 0.3351(5) 0.6184(3) 0.063(2) Uani 1 1 d . . . H48 H 0.5942 0.3966 0.6078 0.076 Uiso 1 1 calc R . . C49 C 0.6501(5) 0.2834(6) 0.6338(4) 0.067(3) Uani 1 1 d . . . H49 H 0.6953 0.3098 0.6343 0.081 Uiso 1 1 calc R . . C50 C 0.6450(4) 0.1957(6) 0.6480(4) 0.067(2) Uani 1 1 d . . . H50 H 0.6865 0.1602 0.6576 0.080 Uiso 1 1 calc R . . C51 C 0.5795(4) 0.1572(5) 0.6485(3) 0.0429(17) Uani 1 1 d . . . H51 H 0.5764 0.0955 0.6591 0.051 Uiso 1 1 calc R . . C52 C 0.4477(3) 0.1637(4) 0.6356(2) 0.0246(13) Uani 1 1 d . . . C53 C 0.0688(3) -0.2326(4) 0.5665(2) 0.0268(14) Uani 1 1 d . . . C54 C -0.0002(3) -0.2125(4) 0.5735(2) 0.0328(15) Uani 1 1 d . . . H54 H -0.0099 -0.1600 0.5942 0.039 Uiso 1 1 calc R . . C55 C -0.0548(3) -0.2696(4) 0.5500(3) 0.0370(16) Uani 1 1 d . . . H55 H -0.1020 -0.2557 0.5542 0.044 Uiso 1 1 calc R . . C56 C -0.0408(4) -0.3463(4) 0.5207(3) 0.0380(16) Uani 1 1 d . . . H56 H -0.0784 -0.3854 0.5052 0.046 Uiso 1 1 calc R . . C57 C 0.0270(4) -0.3666(4) 0.5137(3) 0.0372(16) Uani 1 1 d . . . H57 H 0.0364 -0.4196 0.4934 0.045 Uiso 1 1 calc R . . C58 C 0.0818(3) -0.3093(4) 0.5363(2) 0.0303(14) Uani 1 1 d . . . H58 H 0.1286 -0.3229 0.5309 0.036 Uiso 1 1 calc R . . C59 C 0.1276(3) -0.1698(4) 0.5888(2) 0.0240(13) Uani 1 1 d . . . C60 C 0.3518(5) 0.3405(5) 0.5058(3) 0.068(2) Uani 1 1 d . . . H60A H 0.3983 0.3167 0.5226 0.102 Uiso 1 1 calc R . . H60B H 0.3534 0.4068 0.5060 0.102 Uiso 1 1 calc R . . H60C H 0.3394 0.3189 0.4661 0.102 Uiso 1 1 calc R . . C61 C 0.0136(3) -0.0410(4) 0.7044(3) 0.0360(16) Uani 1 1 d . . . H61A H 0.0193 -0.0355 0.7463 0.054 Uiso 1 1 calc R . . H61B H 0.0311 -0.1001 0.6942 0.054 Uiso 1 1 calc R . . H61C H -0.0365 -0.0353 0.6879 0.054 Uiso 1 1 calc R . . Cl1 Cl 0.36067(11) 0.49432(11) 0.64231(7) 0.0462(5) Uani 1 1 d . . . O17 O 0.3948(4) 0.5204(4) 0.6979(3) 0.093(2) Uani 1 1 d . . . O18 O 0.4131(4) 0.4983(4) 0.6068(3) 0.108(3) Uani 1 1 d . . . O19 O 0.3064(4) 0.5537(4) 0.6250(4) 0.119(3) Uani 1 1 d . . . O20 O 0.3344(3) 0.4047(3) 0.6455(2) 0.0658(16) Uani 1 1 d . . . O21 O 0.0035(2) 0.1681(3) 0.7404(2) 0.0435(12) Uani 1 1 d . . . H21A H -0.0342 0.1980 0.7360 0.065 Uiso 1 1 calc R . . C62 C 0.0548(4) 0.2130(5) 0.7786(3) 0.062(2) Uani 1 1 d . . . H62A H 0.1016 0.1904 0.7742 0.093 Uiso 1 1 calc R . . H62B H 0.0468 0.2023 0.8181 0.093 Uiso 1 1 calc R . . H62C H 0.0522 0.2781 0.7705 0.093 Uiso 1 1 calc R . . O22 O 0.1261(3) 0.7470(3) 0.75966(19) 0.0435(12) Uani 1 1 d . . . H22A H 0.1298 0.7998 0.7474 0.065 Uiso 1 1 calc R . . C63 C 0.1603(4) 0.6861(4) 0.7271(3) 0.0483(19) Uani 1 1 d . . . H63A H 0.1443 0.6244 0.7328 0.072 Uiso 1 1 calc R . . H63B H 0.2115 0.6898 0.7395 0.072 Uiso 1 1 calc R . . H63C H 0.1490 0.7019 0.6862 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01991(15) 0.02376(14) 0.01922(13) 0.00166(10) 0.00444(10) 0.00193(12) Dy2 0.01944(15) 0.01983(13) 0.01964(13) -0.00209(10) 0.00472(10) -0.00079(11) Zn1 0.0197(4) 0.0231(3) 0.0232(3) -0.0039(3) 0.0048(3) 0.0017(3) Zn2 0.0196(4) 0.0227(3) 0.0245(3) 0.0011(3) 0.0012(3) 0.0006(3) O1 0.020(2) 0.025(2) 0.0204(18) -0.0034(15) 0.0011(16) 0.0003(17) O2 0.020(2) 0.022(2) 0.026(2) -0.0030(16) 0.0081(16) 0.0024(17) O3 0.025(2) 0.0163(19) 0.025(2) -0.0007(15) 0.0024(17) -0.0007(16) O4 0.018(2) 0.024(2) 0.0227(19) -0.0040(16) 0.0024(16) 0.0010(17) O5 0.028(3) 0.041(2) 0.026(2) 0.0035(18) 0.0075(18) 0.005(2) O6 0.023(3) 0.046(3) 0.027(2) -0.0041(18) 0.0016(18) 0.002(2) O7 0.029(3) 0.029(2) 0.025(2) -0.0011(17) 0.0065(18) -0.0074(18) O8 0.032(3) 0.029(2) 0.022(2) -0.0008(17) 0.0084(18) 0.0033(19) O9 0.031(3) 0.028(2) 0.031(2) 0.0063(17) 0.0141(19) 0.0066(19) O10 0.026(2) 0.026(2) 0.033(2) 0.0028(17) 0.0075(18) 0.0037(18) O11 0.024(2) 0.028(2) 0.031(2) 0.0049(17) 0.0017(18) -0.0010(18) O12 0.021(2) 0.036(2) 0.034(2) 0.0069(19) 0.0000(18) -0.0007(19) O13 0.031(3) 0.024(2) 0.033(2) -0.0096(17) 0.0101(19) -0.0039(19) O14 0.027(3) 0.024(2) 0.041(2) -0.0134(18) 0.0080(19) -0.0025(18) O15 0.036(3) 0.037(2) 0.030(2) 0.0104(19) 0.014(2) 0.003(2) O16 0.029(3) 0.021(2) 0.037(2) -0.0059(17) 0.0127(19) -0.0011(18) N1 0.031(3) 0.030(3) 0.027(3) -0.005(2) -0.001(2) 0.000(2) N2 0.025(3) 0.026(3) 0.023(2) -0.002(2) 0.006(2) 0.001(2) N3 0.023(3) 0.028(3) 0.026(2) 0.002(2) 0.000(2) 0.006(2) N4 0.032(3) 0.031(3) 0.029(3) 0.002(2) 0.000(2) 0.003(2) C1 0.051(5) 0.038(4) 0.034(3) -0.009(3) 0.004(3) 0.011(3) C2 0.046(5) 0.046(4) 0.043(4) -0.013(3) 0.002(3) 0.011(4) C3 0.046(5) 0.065(5) 0.036(4) -0.014(4) -0.012(3) 0.004(4) C4 0.030(4) 0.047(4) 0.039(4) -0.006(3) -0.009(3) 0.006(3) C5 0.032(4) 0.031(3) 0.030(3) 0.001(3) 0.002(3) 0.000(3) C6 0.022(3) 0.034(3) 0.029(3) -0.009(3) 0.005(3) 0.000(3) C7 0.033(4) 0.037(4) 0.032(3) -0.002(3) 0.011(3) 0.006(3) C8 0.051(5) 0.027(3) 0.047(4) -0.003(3) 0.019(4) 0.012(3) C9 0.041(5) 0.042(4) 0.055(4) 0.003(3) 0.023(4) 0.022(3) C10 0.028(4) 0.042(4) 0.047(4) -0.002(3) 0.013(3) 0.008(3) C11 0.031(4) 0.032(3) 0.023(3) -0.001(2) 0.005(3) 0.010(3) C12 0.026(4) 0.035(3) 0.031(3) 0.001(3) 0.013(3) 0.003(3) C13 0.026(4) 0.046(4) 0.042(4) 0.004(3) 0.002(3) 0.005(3) C14 0.028(4) 0.044(4) 0.048(4) 0.012(3) 0.000(3) 0.014(3) C15 0.052(5) 0.036(4) 0.044(4) 0.004(3) 0.006(3) 0.027(4) C16 0.035(4) 0.031(3) 0.040(4) 0.009(3) 0.008(3) 0.009(3) C17 0.031(4) 0.032(3) 0.013(2) 0.004(2) 0.005(2) 0.007(3) C18 0.029(4) 0.021(3) 0.027(3) -0.001(2) 0.007(3) -0.002(3) C19 0.048(5) 0.037(4) 0.034(4) 0.005(3) 0.001(3) 0.004(3) C20 0.062(6) 0.061(5) 0.026(3) 0.002(3) -0.009(3) 0.006(4) C21 0.060(5) 0.055(5) 0.024(3) -0.009(3) 0.002(3) -0.003(4) C22 0.037(4) 0.043(4) 0.028(3) -0.011(3) 0.004(3) -0.005(3) C23 0.025(4) 0.027(3) 0.029(3) -0.002(2) 0.008(3) -0.006(3) C24 0.025(3) 0.020(3) 0.025(3) -0.003(2) 0.004(2) -0.003(2) C25 0.028(4) 0.021(3) 0.019(3) 0.005(2) 0.008(2) -0.001(3) C26 0.023(4) 0.051(4) 0.031(3) -0.004(3) 0.009(3) -0.001(3) C27 0.037(4) 0.065(5) 0.025(3) -0.002(3) 0.004(3) -0.007(4) C28 0.061(5) 0.045(4) 0.020(3) -0.010(3) 0.006(3) -0.008(4) C29 0.050(5) 0.039(4) 0.030(3) -0.003(3) 0.013(3) 0.012(3) C30 0.036(4) 0.034(3) 0.025(3) 0.002(3) 0.004(3) 0.008(3) C31 0.031(4) 0.025(3) 0.025(3) 0.003(2) 0.003(3) -0.002(3) C32 0.018(3) 0.042(4) 0.027(3) 0.000(3) 0.004(2) -0.005(3) C33 0.032(4) 0.038(4) 0.032(3) 0.004(3) 0.007(3) 0.009(3) C34 0.045(5) 0.067(5) 0.033(4) 0.014(3) 0.014(3) 0.021(4) C35 0.040(5) 0.091(6) 0.022(3) -0.002(4) 0.005(3) -0.001(4) C36 0.034(4) 0.070(5) 0.034(4) -0.015(4) 0.003(3) -0.010(4) C37 0.037(4) 0.051(4) 0.032(3) -0.009(3) 0.004(3) -0.009(3) C38 0.007(3) 0.040(4) 0.029(3) -0.003(3) 0.000(2) -0.002(2) C39 0.029(4) 0.032(3) 0.021(3) -0.001(2) 0.005(2) 0.005(3) C40 0.044(4) 0.028(3) 0.027(3) 0.001(3) 0.006(3) 0.008(3) C41 0.083(7) 0.032(4) 0.038(4) 0.003(3) 0.012(4) 0.014(4) C42 0.083(7) 0.043(5) 0.046(4) -0.001(4) 0.009(4) 0.040(5) C43 0.032(4) 0.065(5) 0.051(4) -0.007(4) 0.013(3) 0.023(4) C44 0.029(4) 0.046(4) 0.038(4) -0.003(3) 0.009(3) 0.012(3) C45 0.031(4) 0.023(3) 0.020(3) 0.003(2) -0.002(3) 0.003(3) C46 0.027(4) 0.039(4) 0.027(3) -0.006(3) 0.008(3) -0.007(3) C47 0.047(5) 0.040(4) 0.045(4) -0.006(3) 0.009(3) -0.009(3) C48 0.078(7) 0.050(5) 0.069(5) -0.010(4) 0.032(5) -0.033(5) C49 0.044(6) 0.085(7) 0.081(6) -0.021(5) 0.035(5) -0.031(5) C50 0.032(5) 0.087(7) 0.083(6) -0.002(5) 0.015(4) -0.015(5) C51 0.027(4) 0.053(4) 0.050(4) -0.004(3) 0.010(3) -0.005(3) C52 0.024(4) 0.023(3) 0.026(3) -0.003(2) 0.003(3) -0.004(3) C53 0.035(4) 0.026(3) 0.020(3) -0.003(2) 0.004(3) -0.005(3) C54 0.031(4) 0.033(3) 0.034(3) -0.010(3) 0.003(3) -0.003(3) C55 0.022(4) 0.043(4) 0.046(4) -0.008(3) 0.006(3) -0.006(3) C56 0.038(4) 0.041(4) 0.035(3) -0.009(3) 0.004(3) -0.016(3) C57 0.046(5) 0.029(3) 0.037(3) -0.016(3) 0.006(3) -0.007(3) C58 0.033(4) 0.024(3) 0.035(3) -0.003(3) 0.010(3) 0.001(3) C59 0.026(4) 0.024(3) 0.021(3) 0.001(2) 0.002(2) -0.002(3) C60 0.077(7) 0.071(6) 0.062(5) 0.014(4) 0.027(5) 0.008(5) C61 0.030(4) 0.039(4) 0.041(4) 0.003(3) 0.014(3) -0.006(3) Cl1 0.0688(14) 0.0323(9) 0.0405(9) -0.0013(7) 0.0173(9) -0.0077(9) O17 0.130(6) 0.078(4) 0.063(4) -0.003(3) -0.005(4) -0.031(4) O18 0.142(7) 0.062(4) 0.144(6) 0.009(4) 0.097(6) -0.011(4) O19 0.063(5) 0.068(4) 0.213(9) 0.042(5) -0.015(5) 0.002(4) O20 0.094(5) 0.038(3) 0.069(4) -0.009(3) 0.026(3) -0.022(3) O21 0.042(3) 0.042(3) 0.050(3) -0.017(2) 0.015(2) 0.005(2) C62 0.060(6) 0.064(5) 0.059(5) -0.025(4) -0.005(4) 0.016(4) O22 0.053(3) 0.035(3) 0.043(3) 0.002(2) 0.009(2) -0.008(2) C63 0.056(5) 0.033(4) 0.058(5) 0.004(3) 0.018(4) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O9 2.282(4) . ? Dy1 O11 2.320(4) . ? Dy1 O2 2.339(4) . ? Dy1 O4 2.395(3) . ? Dy1 O5 2.411(4) . ? Dy1 O1 2.421(4) . ? Dy1 O6 2.432(4) . ? Dy1 O15 2.444(4) . ? Dy1 Zn2 3.3970(7) . ? Dy1 Zn1 3.4947(7) . ? Dy1 Dy2 3.8985(4) . ? Dy2 O13 2.317(4) . ? Dy2 O10 2.335(4) . ? Dy2 O3 2.348(4) . ? Dy2 O1 2.350(3) . ? Dy2 O7 2.373(4) . ? Dy2 O16 2.420(4) . ? Dy2 O4 2.426(4) . ? Dy2 O8 2.485(4) . ? Dy2 Zn1 3.3417(7) . ? Dy2 Zn2 3.5412(7) . ? Zn1 N2 2.068(5) . ? Zn1 O14 2.075(4) . ? Zn1 O2 2.096(4) . ? Zn1 O1 2.123(4) . ? Zn1 O3 2.151(3) . ? Zn1 N1 2.160(5) . ? Zn2 O12 2.043(4) . ? Zn2 N3 2.044(5) . ? Zn2 O4 2.092(4) . ? Zn2 N4 2.126(5) . ? Zn2 O3 2.141(4) . ? Zn2 O2 2.237(3) . ? O1 C6 1.440(6) . ? O2 C12 1.424(6) . ? O3 C18 1.410(6) . ? O4 C24 1.430(6) . ? O5 C31 1.270(7) . ? O6 C31 1.260(7) . ? O7 C38 1.256(7) . ? O8 C38 1.272(6) . ? O9 C45 1.264(6) . ? O10 C45 1.262(6) . ? O11 C52 1.258(7) . ? O12 C52 1.253(6) . ? O13 C59 1.268(6) . ? O14 C59 1.268(6) . ? O15 C60 1.433(8) . ? O16 C61 1.432(6) . ? N1 C1 1.328(7) . ? N1 C5 1.349(8) . ? N2 C11 1.316(7) . ? N2 C7 1.332(7) . ? N3 C17 1.343(7) . ? N3 C13 1.348(7) . ? N4 C23 1.337(7) . ? N4 C19 1.344(8) . ? C1 C2 1.366(9) . ? C2 C3 1.378(9) . ? C3 C4 1.379(9) . ? C4 C5 1.386(8) . ? C5 C6 1.520(8) . ? C7 C8 1.371(8) . ? C8 C9 1.382(9) . ? C9 C10 1.371(9) . ? C10 C11 1.403(8) . ? C11 C12 1.518(8) . ? C13 C14 1.375(8) . ? C14 C15 1.360(9) . ? C15 C16 1.381(9) . ? C16 C17 1.371(8) . ? C17 C18 1.520(8) . ? C19 C20 1.370(9) . ? C20 C21 1.390(10) . ? C21 C22 1.372(9) . ? C22 C23 1.380(7) . ? C23 C24 1.518(7) . ? C25 C30 1.391(8) . ? C25 C26 1.391(8) . ? C25 C31 1.500(7) . ? C26 C27 1.382(8) . ? C27 C28 1.372(9) . ? C28 C29 1.381(9) . ? C29 C30 1.379(8) . ? C32 C33 1.392(8) . ? C32 C37 1.393(8) . ? C32 C38 1.498(8) . ? C33 C34 1.393(8) . ? C34 C35 1.384(10) . ? C35 C36 1.382(10) . ? C36 C37 1.387(8) . ? C39 C40 1.386(8) . ? C39 C44 1.387(8) . ? C39 C45 1.493(8) . ? C40 C41 1.397(8) . ? C41 C42 1.375(11) . ? C42 C43 1.366(10) . ? C43 C44 1.384(9) . ? C46 C47 1.387(8) . ? C46 C51 1.387(9) . ? C46 C52 1.507(8) . ? C47 C48 1.404(10) . ? C48 C49 1.381(11) . ? C49 C50 1.347(11) . ? C50 C51 1.382(9) . ? C53 C58 1.383(7) . ? C53 C54 1.394(8) . ? C53 C59 1.489(8) . ? C54 C55 1.388(8) . ? C55 C56 1.377(8) . ? C56 C57 1.372(9) . ? C57 C58 1.388(8) . ? Cl1 O19 1.373(6) . ? Cl1 O18 1.412(6) . ? Cl1 O17 1.420(6) . ? Cl1 O20 1.425(5) . ? O21 C62 1.391(8) . ? O22 C63 1.413(7) . ? 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 O9 Dy1 O11 115.32(14) . . ? O9 Dy1 O2 144.81(13) . . ? O11 Dy1 O2 78.13(13) . . ? O9 Dy1 O4 75.29(12) . . ? O11 Dy1 O4 80.41(13) . . ? O2 Dy1 O4 75.38(12) . . ? O9 Dy1 O5 84.45(13) . . ? O11 Dy1 O5 134.12(13) . . ? O2 Dy1 O5 109.98(13) . . ? O4 Dy1 O5 145.34(13) . . ? O9 Dy1 O1 80.19(13) . . ? O11 Dy1 O1 141.80(12) . . ? O2 Dy1 O1 71.74(13) . . ? O4 Dy1 O1 69.80(12) . . ? O5 Dy1 O1 79.35(13) . . ? O9 Dy1 O6 133.02(13) . . ? O11 Dy1 O6 86.66(13) . . ? O2 Dy1 O6 77.29(13) . . ? O4 Dy1 O6 151.62(13) . . ? O5 Dy1 O6 53.99(13) . . ? O1 Dy1 O6 108.44(13) . . ? O9 Dy1 O15 70.79(13) . . ? O11 Dy1 O15 70.40(13) . . ? O2 Dy1 O15 141.88(13) . . ? O4 Dy1 O15 118.39(12) . . ? O5 Dy1 O15 79.34(13) . . ? O1 Dy1 O15 145.32(13) . . ? O6 Dy1 O15 79.91(13) . . ? O9 Dy1 Zn2 112.84(9) . . ? O11 Dy1 Zn2 64.66(9) . . ? O2 Dy1 Zn2 40.92(8) . . ? O4 Dy1 Zn2 37.55(9) . . ? O5 Dy1 Zn2 147.63(10) . . ? O1 Dy1 Zn2 77.18(9) . . ? O6 Dy1 Zn2 114.10(10) . . ? O15 Dy1 Zn2 131.34(10) . . ? O9 Dy1 Zn1 115.89(10) . . ? O11 Dy1 Zn1 112.49(9) . . ? O2 Dy1 Zn1 35.62(9) . . ? O4 Dy1 Zn1 73.32(9) . . ? O5 Dy1 Zn1 91.40(10) . . ? O1 Dy1 Zn1 36.70(9) . . ? O6 Dy1 Zn1 88.77(10) . . ? O15 Dy1 Zn1 168.21(9) . . ? Zn2 Dy1 Zn1 56.711(15) . . ? O9 Dy1 Dy2 68.39(9) . . ? O11 Dy1 Dy2 115.77(9) . . ? O2 Dy1 Dy2 76.47(9) . . ? O4 Dy1 Dy2 36.30(9) . . ? O5 Dy1 Dy2 109.95(10) . . ? O1 Dy1 Dy2 34.61(8) . . ? O6 Dy1 Dy2 140.55(10) . . ? O15 Dy1 Dy2 136.74(9) . . ? Zn2 Dy1 Dy2 57.586(13) . . ? Zn1 Dy1 Dy2 53.404(11) . . ? O13 Dy2 O10 118.54(14) . . ? O13 Dy2 O3 81.91(13) . . ? O10 Dy2 O3 144.57(13) . . ? O13 Dy2 O1 79.05(13) . . ? O10 Dy2 O1 79.79(12) . . ? O3 Dy2 O1 76.15(12) . . ? O13 Dy2 O7 131.15(13) . . ? O10 Dy2 O7 86.69(13) . . ? O3 Dy2 O7 101.25(13) . . ? O1 Dy2 O7 149.51(13) . . ? O13 Dy2 O16 73.24(13) . . ? O10 Dy2 O16 68.98(13) . . ? O3 Dy2 O16 146.25(12) . . ? O1 Dy2 O16 119.62(13) . . ? O7 Dy2 O16 79.53(13) . . ? O13 Dy2 O4 142.55(12) . . ? O10 Dy2 O4 77.37(13) . . ? O3 Dy2 O4 70.28(12) . . ? O1 Dy2 O4 70.45(12) . . ? O7 Dy2 O4 80.01(12) . . ? O16 Dy2 O4 141.31(12) . . ? O13 Dy2 O8 80.30(13) . . ? O10 Dy2 O8 130.89(12) . . ? O3 Dy2 O8 78.09(12) . . ? O1 Dy2 O8 148.87(12) . . ? O7 Dy2 O8 53.69(12) . . ? O16 Dy2 O8 75.54(13) . . ? O4 Dy2 O8 116.24(12) . . ? O13 Dy2 Zn1 66.55(9) . . ? O10 Dy2 Zn1 118.52(9) . . ? O3 Dy2 Zn1 39.82(8) . . ? O1 Dy2 Zn1 39.14(9) . . ? O7 Dy2 Zn1 139.56(10) . . ? O16 Dy2 Zn1 137.12(9) . . ? O4 Dy2 Zn1 76.05(8) . . ? O8 Dy2 Zn1 110.59(9) . . ? O13 Dy2 Zn2 116.38(10) . . ? O10 Dy2 Zn2 112.38(10) . . ? O3 Dy2 Zn2 35.91(9) . . ? O1 Dy2 Zn2 74.98(9) . . ? O7 Dy2 Zn2 85.35(10) . . ? O16 Dy2 Zn2 164.75(9) . . ? O4 Dy2 Zn2 35.14(8) . . ? O8 Dy2 Zn2 93.90(9) . . ? Zn1 Dy2 Zn2 56.723(16) . . ? O13 Dy2 Dy1 114.27(9) . . ? O10 Dy2 Dy1 69.19(9) . . ? O3 Dy2 Dy1 76.09(9) . . ? O1 Dy2 Dy1 35.82(9) . . ? O7 Dy2 Dy1 113.73(9) . . ? O16 Dy2 Dy1 135.00(9) . . ? O4 Dy2 Dy1 35.77(8) . . ? O8 Dy2 Dy1 147.86(9) . . ? Zn1 Dy2 Dy1 57.102(12) . . ? Zn2 Dy2 Dy1 54.078(11) . . ? N2 Zn1 O14 96.87(17) . . ? N2 Zn1 O2 80.40(16) . . ? O14 Zn1 O2 170.50(15) . . ? N2 Zn1 O1 159.99(16) . . ? O14 Zn1 O1 101.41(15) . . ? O2 Zn1 O1 82.78(14) . . ? N2 Zn1 O3 103.08(15) . . ? O14 Zn1 O3 89.15(15) . . ? O2 Zn1 O3 82.67(14) . . ? O1 Zn1 O3 85.35(13) . . ? N2 Zn1 N1 97.38(18) . . ? O14 Zn1 N1 84.32(17) . . ? O2 Zn1 N1 105.02(16) . . ? O1 Zn1 N1 76.60(16) . . ? O3 Zn1 N1 159.13(17) . . ? N2 Zn1 Dy2 147.40(12) . . ? O14 Zn1 Dy2 83.96(10) . . ? O2 Zn1 Dy2 93.44(9) . . ? O1 Zn1 Dy2 44.33(9) . . ? O3 Zn1 Dy2 44.34(10) . . ? N1 Zn1 Dy2 115.06(14) . . ? N2 Zn1 Dy1 118.34(13) . . ? O14 Zn1 Dy1 144.38(11) . . ? O2 Zn1 Dy1 40.53(10) . . ? O1 Zn1 Dy1 42.97(10) . . ? O3 Zn1 Dy1 87.97(9) . . ? N1 Zn1 Dy1 85.92(13) . . ? Dy2 Zn1 Dy1 69.494(13) . . ? O12 Zn2 N3 95.42(18) . . ? O12 Zn2 O4 105.43(15) . . ? N3 Zn2 O4 158.75(17) . . ? O12 Zn2 N4 88.21(18) . . ? N3 Zn2 N4 98.48(18) . . ? O4 Zn2 N4 78.48(16) . . ? O12 Zn2 O3 163.68(15) . . ? N3 Zn2 O3 80.03(17) . . ? O4 Zn2 O3 80.96(14) . . ? N4 Zn2 O3 107.91(17) . . ? O12 Zn2 O2 86.03(14) . . ? N3 Zn2 O2 101.90(15) . . ? O4 Zn2 O2 83.87(13) . . ? N4 Zn2 O2 159.24(16) . . ? O3 Zn2 O2 79.67(13) . . ? O12 Zn2 Dy1 84.11(11) . . ? N3 Zn2 Dy1 145.14(13) . . ? O4 Zn2 Dy1 44.25(9) . . ? N4 Zn2 Dy1 116.31(13) . . ? O3 Zn2 Dy1 90.73(10) . . ? O2 Zn2 Dy1 43.23(9) . . ? O12 Zn2 Dy2 147.03(11) . . ? N3 Zn2 Dy2 117.52(14) . . ? O4 Zn2 Dy2 41.87(10) . . ? N4 Zn2 Dy2 88.20(14) . . ? O3 Zn2 Dy2 40.02(10) . . ? O2 Zn2 Dy2 85.87(10) . . ? Dy1 Zn2 Dy2 68.337(14) . . ? C6 O1 Zn1 112.1(3) . . ? C6 O1 Dy2 115.6(3) . . ? Zn1 O1 Dy2 96.54(14) . . ? C6 O1 Dy1 119.3(3) . . ? Zn1 O1 Dy1 100.33(15) . . ? Dy2 O1 Dy1 109.57(14) . . ? C12 O2 Zn1 110.9(3) . . ? C12 O2 Zn2 115.0(3) . . ? Zn1 O2 Zn2 98.10(14) . . ? C12 O2 Dy1 128.4(3) . . ? Zn1 O2 Dy1 103.85(15) . . ? Zn2 O2 Dy1 95.84(13) . . ? C18 O3 Zn2 110.7(3) . . ? C18 O3 Zn1 111.5(3) . . ? Zn2 O3 Zn1 99.43(14) . . ? C18 O3 Dy2 130.5(3) . . ? Zn2 O3 Dy2 104.07(14) . . ? Zn1 O3 Dy2 95.85(14) . . ? C24 O4 Zn2 111.4(3) . . ? C24 O4 Dy1 116.8(3) . . ? Zn2 O4 Dy1 98.20(13) . . ? C24 O4 Dy2 117.1(3) . . ? Zn2 O4 Dy2 102.99(14) . . ? Dy1 O4 Dy2 107.94(13) . . ? C31 O5 Dy1 92.5(3) . . ? C31 O6 Dy1 91.8(3) . . ? C38 O7 Dy2 95.6(3) . . ? C38 O8 Dy2 90.0(3) . . ? C45 O9 Dy1 140.4(3) . . ? C45 O10 Dy2 135.9(4) . . ? C52 O11 Dy1 137.7(4) . . ? C52 O12 Zn2 123.8(4) . . ? C59 O13 Dy2 138.2(4) . . ? C59 O14 Zn1 122.1(3) . . ? C60 O15 Dy1 124.6(4) . . ? C61 O16 Dy2 127.6(3) . . ? C1 N1 C5 117.8(5) . . ? C1 N1 Zn1 125.8(4) . . ? C5 N1 Zn1 111.9(4) . . ? C11 N2 C7 119.3(5) . . ? C11 N2 Zn1 114.2(4) . . ? C7 N2 Zn1 126.3(4) . . ? C17 N3 C13 118.4(5) . . ? C17 N3 Zn2 116.1(4) . . ? C13 N3 Zn2 125.5(4) . . ? C23 N4 C19 117.7(5) . . ? C23 N4 Zn2 113.6(4) . . ? C19 N4 Zn2 127.8(4) . . ? N1 C1 C2 123.6(7) . . ? C1 C2 C3 118.6(6) . . ? C2 C3 C4 119.1(6) . . ? C3 C4 C5 118.7(6) . . ? N1 C5 C4 122.0(6) . . ? N1 C5 C6 116.8(5) . . ? C4 C5 C6 121.2(6) . . ? O1 C6 C5 111.3(5) . . ? N2 C7 C8 122.4(6) . . ? C7 C8 C9 118.8(6) . . ? C10 C9 C8 119.3(6) . . ? C9 C10 C11 118.1(6) . . ? N2 C11 C10 122.1(6) . . ? N2 C11 C12 117.7(5) . . ? C10 C11 C12 120.2(6) . . ? O2 C12 C11 112.4(5) . . ? N3 C13 C14 122.1(6) . . ? C15 C14 C13 118.6(6) . . ? C14 C15 C16 120.5(6) . . ? C17 C16 C15 118.1(6) . . ? N3 C17 C16 122.3(6) . . ? N3 C17 C18 116.0(5) . . ? C16 C17 C18 121.7(5) . . ? O3 C18 C17 112.8(4) . . ? N4 C19 C20 123.1(6) . . ? C19 C20 C21 118.5(6) . . ? C22 C21 C20 119.0(6) . . ? C21 C22 C23 118.9(6) . . ? N4 C23 C22 122.7(6) . . ? N4 C23 C24 116.7(5) . . ? C22 C23 C24 120.5(5) . . ? O4 C24 C23 111.3(4) . . ? C30 C25 C26 119.4(5) . . ? C30 C25 C31 119.9(5) . . ? C26 C25 C31 120.6(5) . . ? C27 C26 C25 120.2(6) . . ? C28 C27 C26 120.5(6) . . ? C27 C28 C29 119.2(6) . . ? C30 C29 C28 121.5(6) . . ? C29 C30 C25 119.2(6) . . ? O6 C31 O5 120.7(5) . . ? O6 C31 C25 119.8(5) . . ? O5 C31 C25 119.5(5) . . ? C33 C32 C37 120.0(5) . . ? C33 C32 C38 120.4(5) . . ? C37 C32 C38 119.6(5) . . ? C32 C33 C34 120.1(6) . . ? C35 C34 C33 119.2(7) . . ? C36 C35 C34 120.9(6) . . ? C35 C36 C37 120.1(7) . . ? C36 C37 C32 119.6(7) . . ? O7 C38 O8 120.7(5) . . ? O7 C38 C32 119.1(5) . . ? O8 C38 C32 120.2(5) . . ? C40 C39 C44 119.9(6) . . ? C40 C39 C45 119.2(5) . . ? C44 C39 C45 120.9(6) . . ? C39 C40 C41 120.4(7) . . ? C42 C41 C40 119.0(7) . . ? C43 C42 C41 120.4(6) . . ? C42 C43 C44 121.4(7) . . ? C43 C44 C39 118.7(7) . . ? O10 C45 O9 124.2(5) . . ? O10 C45 C39 118.9(5) . . ? O9 C45 C39 116.9(5) . . ? C47 C46 C51 119.5(6) . . ? C47 C46 C52 121.1(6) . . ? C51 C46 C52 119.4(6) . . ? C46 C47 C48 118.6(7) . . ? C49 C48 C47 120.5(8) . . ? C50 C49 C48 120.5(8) . . ? C49 C50 C51 120.1(8) . . ? C50 C51 C46 120.8(7) . . ? O12 C52 O11 125.4(5) . . ? O12 C52 C46 116.5(5) . . ? O11 C52 C46 118.1(5) . . ? C58 C53 C54 119.3(6) . . ? C58 C53 C59 120.3(6) . . ? C54 C53 C59 120.3(5) . . ? C55 C54 C53 119.5(6) . . ? C56 C55 C54 120.3(6) . . ? C57 C56 C55 120.5(6) . . ? C56 C57 C58 119.6(6) . . ? C53 C58 C57 120.7(6) . . ? O14 C59 O13 124.2(5) . . ? O14 C59 C53 117.2(5) . . ? O13 C59 C53 118.7(5) . . ? O19 Cl1 O18 112.1(5) . . ? O19 Cl1 O17 108.3(5) . . ? O18 Cl1 O17 105.6(5) . . ? O19 Cl1 O20 110.7(4) . . ? O18 Cl1 O20 111.3(3) . . ? O17 Cl1 O20 108.5(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.071 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.147 data_ic15776 _database_code_depnum_ccdc_archive 'CCDC 910495' #TrackingRef '15359_web_deposit_cif_file_2_En-CheYang_1352708909.complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H65 Cl N4 Ni2 O22 Y2' _chemical_formula_weight 1560.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.127(2) _cell_length_b 14.7562(18) _cell_length_c 23.539(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.939(3) _cell_angle_gamma 90.00 _cell_volume 6544.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3917 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.75 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3192 _exptl_absorpt_coefficient_mu 2.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5276 _exptl_absorpt_correction_T_max 0.6034 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44498 _diffrn_reflns_av_R_equivalents 0.0888 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15013 _reflns_number_gt 9925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.7866P] 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 15013 _refine_ls_number_parameters 853 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.17193(2) 0.01945(3) 0.162696(17) 0.01909(10) Uani 1 1 d . . . Y2 Y 0.27974(2) 0.15045(3) 0.063722(17) 0.02015(10) Uani 1 1 d . . . Ni1 Ni 0.35461(3) 0.01896(4) 0.17301(2) 0.01974(13) Uani 1 1 d . . . Ni2 Ni 0.25729(3) -0.07941(4) 0.06926(2) 0.02009(13) Uani 1 1 d . . . O1 O 0.27485(14) 0.11327(19) 0.16073(11) 0.0199(6) Uani 1 1 d . . . O2 O 0.27152(14) -0.07223(19) 0.15979(12) 0.0212(6) Uani 1 1 d . . . O3 O 0.33902(14) 0.01131(19) 0.08125(12) 0.0216(6) Uani 1 1 d . . . O4 O 0.19293(14) 0.03291(19) 0.06860(12) 0.0205(6) Uani 1 1 d . . . O5 O 0.19115(14) 0.0711(2) 0.25924(12) 0.0242(7) Uani 1 1 d . . . O6 O 0.17509(15) -0.0764(2) 0.24914(12) 0.0262(7) Uani 1 1 d . . . O7 O 0.21571(15) 0.1576(2) -0.03326(12) 0.0283(7) Uani 1 1 d . . . O8 O 0.33020(15) 0.1283(2) -0.02218(12) 0.0287(7) Uani 1 1 d . . . O9 O 0.12196(14) 0.1603(2) 0.13880(13) 0.0257(7) Uani 1 1 d . . . O10 O 0.18943(15) 0.2356(2) 0.08624(12) 0.0260(7) Uani 1 1 d . . . O11 O 0.11348(15) -0.1059(2) 0.12094(12) 0.0251(7) Uani 1 1 d . . . O12 O 0.18311(14) -0.1788(2) 0.06913(12) 0.0251(7) Uani 1 1 d . . . O13 O 0.39140(15) 0.1964(2) 0.10556(13) 0.0275(7) Uani 1 1 d . . . O14 O 0.44179(14) 0.0958(2) 0.17095(13) 0.0253(7) Uani 1 1 d . . . O15 O 0.05182(14) 0.0263(2) 0.18129(12) 0.0246(7) Uani 1 1 d . . . H15 H 0.0415 0.0786 0.2001 0.037 Uiso 1 1 d R . . O16 O 0.29822(15) 0.3070(2) 0.03854(13) 0.0303(7) Uani 1 1 d . . . H16 H 0.3041 0.3447 0.0696 0.045 Uiso 1 1 d R . . N1 N 0.36051(18) 0.0659(3) 0.25693(15) 0.0250(8) Uani 1 1 d . . . N2 N 0.41139(17) -0.0951(2) 0.19347(15) 0.0232(8) Uani 1 1 d . . . N3 N 0.33711(18) -0.1654(2) 0.05932(14) 0.0237(8) Uani 1 1 d . . . N4 N 0.21450(18) -0.0691(2) -0.01846(15) 0.0230(8) Uani 1 1 d . . . C1 C 0.4021(3) 0.0339(3) 0.3046(2) 0.0366(12) Uani 1 1 d . . . H1 H 0.4239 -0.0237 0.3033 0.044 Uiso 1 1 calc R . . C2 C 0.4141(3) 0.0825(4) 0.3557(2) 0.0491(15) Uani 1 1 d . . . H2 H 0.4448 0.0595 0.3886 0.059 Uiso 1 1 calc R . . C3 C 0.3806(3) 0.1647(4) 0.3579(2) 0.0432(14) Uani 1 1 d . . . H3 H 0.3873 0.1988 0.3927 0.052 Uiso 1 1 calc R . . C4 C 0.3372(2) 0.1972(3) 0.30917(19) 0.0308(11) Uani 1 1 d . . . H4 H 0.3131 0.2533 0.3100 0.037 Uiso 1 1 calc R . . C5 C 0.3298(2) 0.1465(3) 0.25939(18) 0.0217(9) Uani 1 1 d . . . C6 C 0.2881(2) 0.1826(3) 0.20311(17) 0.0216(9) Uani 1 1 d . . . H6A H 0.2424 0.2079 0.2101 0.026 Uiso 1 1 calc R . . H6B H 0.3153 0.2322 0.1887 0.026 Uiso 1 1 calc R . . C7 C 0.4825(2) -0.1030(3) 0.2062(2) 0.0311(11) Uani 1 1 d . . . H7 H 0.5107 -0.0501 0.2056 0.037 Uiso 1 1 calc R . . C8 C 0.5159(3) -0.1839(4) 0.2201(2) 0.0390(13) Uani 1 1 d . . . H8 H 0.5661 -0.1866 0.2304 0.047 Uiso 1 1 calc R . . C9 C 0.4756(3) -0.2613(3) 0.2190(2) 0.0370(12) Uani 1 1 d . . . H9 H 0.4978 -0.3188 0.2264 0.044 Uiso 1 1 calc R . . C10 C 0.4025(2) -0.2543(3) 0.20689(19) 0.0320(11) Uani 1 1 d . . . H10 H 0.3736 -0.3068 0.2065 0.038 Uiso 1 1 calc R . . C11 C 0.3719(2) -0.1698(3) 0.19533(17) 0.0237(10) Uani 1 1 d . . . C12 C 0.2926(2) -0.1561(3) 0.18678(19) 0.0234(9) Uani 1 1 d . . . H12A H 0.2688 -0.2061 0.1628 0.028 Uiso 1 1 calc R . . H12B H 0.2769 -0.1585 0.2247 0.028 Uiso 1 1 calc R . . C13 C 0.3338(2) -0.2564(3) 0.05434(19) 0.0299(11) Uani 1 1 d . . . H13 H 0.2915 -0.2863 0.0601 0.036 Uiso 1 1 calc R . . C14 C 0.3884(3) -0.3075(3) 0.0414(2) 0.0359(12) Uani 1 1 d . . . H14 H 0.3845 -0.3716 0.0381 0.043 Uiso 1 1 calc R . . C15 C 0.4497(3) -0.2631(4) 0.0333(2) 0.0415(13) Uani 1 1 d . . . H15A H 0.4885 -0.2967 0.0238 0.050 Uiso 1 1 calc R . . C16 C 0.4545(2) -0.1709(3) 0.0388(2) 0.0336(11) Uani 1 1 d . . . H16A H 0.4966 -0.1401 0.0337 0.040 Uiso 1 1 calc R . . C17 C 0.3970(2) -0.1230(3) 0.05195(18) 0.0235(10) Uani 1 1 d . . . C18 C 0.3972(2) -0.0213(3) 0.05674(19) 0.0249(10) Uani 1 1 d . . . H18A H 0.4421 -0.0014 0.0809 0.030 Uiso 1 1 calc R . . H18B H 0.3950 0.0054 0.0179 0.030 Uiso 1 1 calc R . . C19 C 0.2314(2) -0.1198(3) -0.06169(19) 0.0280(10) Uani 1 1 d . . . H19 H 0.2771 -0.1469 -0.0565 0.034 Uiso 1 1 calc R . . C20 C 0.1863(2) -0.1343(3) -0.11264(19) 0.0316(11) Uani 1 1 d . . . H20 H 0.2006 -0.1699 -0.1422 0.038 Uiso 1 1 calc R . . C21 C 0.1193(3) -0.0959(3) -0.1200(2) 0.0388(13) Uani 1 1 d . . . H21 H 0.0860 -0.1066 -0.1542 0.047 Uiso 1 1 calc R . . C22 C 0.1018(2) -0.0419(3) -0.0767(2) 0.0324(11) Uani 1 1 d . . . H22 H 0.0567 -0.0132 -0.0814 0.039 Uiso 1 1 calc R . . C23 C 0.1502(2) -0.0295(3) -0.02663(19) 0.0247(10) Uani 1 1 d . . . C24 C 0.1336(2) 0.0275(3) 0.02235(17) 0.0239(10) Uani 1 1 d . . . H24A H 0.1203 0.0893 0.0080 0.029 Uiso 1 1 calc R . . H24B H 0.0925 0.0010 0.0369 0.029 Uiso 1 1 calc R . . C25 C 0.1905(2) -0.0139(3) 0.34500(19) 0.0245(10) Uani 1 1 d . . . C26 C 0.1984(2) 0.0634(4) 0.37925(19) 0.0320(11) Uani 1 1 d . . . H26 H 0.2000 0.1214 0.3620 0.038 Uiso 1 1 calc R . . C27 C 0.2041(3) 0.0559(4) 0.4387(2) 0.0427(14) Uani 1 1 d . . . H27 H 0.2086 0.1088 0.4620 0.051 Uiso 1 1 calc R . . C28 C 0.2031(3) -0.0286(4) 0.4640(2) 0.0458(14) Uani 1 1 d . . . H28 H 0.2080 -0.0338 0.5047 0.055 Uiso 1 1 calc R . . C29 C 0.1949(3) -0.1057(4) 0.4298(2) 0.0424(13) Uani 1 1 d . . . H29 H 0.1935 -0.1636 0.4472 0.051 Uiso 1 1 calc R . . C30 C 0.1887(2) -0.0990(3) 0.37085(19) 0.0306(11) Uani 1 1 d . . . H30 H 0.1833 -0.1521 0.3477 0.037 Uiso 1 1 calc R . . C31 C 0.1856(2) -0.0063(3) 0.28138(19) 0.0232(10) Uani 1 1 d . . . C32 C 0.2615(2) 0.1119(3) -0.11670(18) 0.0255(10) Uani 1 1 d . . . C33 C 0.1981(2) 0.1271(3) -0.15378(19) 0.0326(11) Uani 1 1 d . . . H33 H 0.1591 0.1525 -0.1392 0.039 Uiso 1 1 calc R . . C34 C 0.1906(3) 0.1058(4) -0.2118(2) 0.0405(13) Uani 1 1 d . . . H34 H 0.1469 0.1167 -0.2368 0.049 Uiso 1 1 calc R . . C35 C 0.2470(3) 0.0686(4) -0.2332(2) 0.0397(13) Uani 1 1 d . . . H35 H 0.2423 0.0543 -0.2730 0.048 Uiso 1 1 calc R . . C36 C 0.3104(3) 0.0521(3) -0.1964(2) 0.0331(11) Uani 1 1 d . . . H36 H 0.3490 0.0256 -0.2109 0.040 Uiso 1 1 calc R . . C37 C 0.3175(2) 0.0740(3) -0.13908(19) 0.0295(11) Uani 1 1 d . . . H37 H 0.3613 0.0630 -0.1143 0.035 Uiso 1 1 calc R . . C38 C 0.2700(2) 0.1347(3) -0.05416(19) 0.0255(10) Uani 1 1 d . . . C39 C 0.1054(2) 0.3189(3) 0.12515(17) 0.0242(10) Uani 1 1 d . . . C40 C 0.0376(2) 0.3193(4) 0.1392(2) 0.0354(12) Uani 1 1 d . . . H40 H 0.0142 0.2638 0.1442 0.043 Uiso 1 1 calc R . . C41 C 0.0045(3) 0.4010(4) 0.1460(2) 0.0480(15) Uani 1 1 d . . . H41 H -0.0421 0.4017 0.1549 0.058 Uiso 1 1 calc R . . C42 C 0.0392(3) 0.4816(4) 0.1397(2) 0.0549(17) Uani 1 1 d . . . H42 H 0.0163 0.5375 0.1447 0.066 Uiso 1 1 calc R . . C43 C 0.1068(3) 0.4820(4) 0.1264(2) 0.0466(14) Uani 1 1 d . . . H43 H 0.1307 0.5375 0.1227 0.056 Uiso 1 1 calc R . . C44 C 0.1389(3) 0.4003(3) 0.11856(19) 0.0321(11) Uani 1 1 d . . . H44 H 0.1849 0.3999 0.1084 0.038 Uiso 1 1 calc R . . C45 C 0.1414(2) 0.2314(3) 0.11612(18) 0.0240(10) Uani 1 1 d . . . C46 C 0.0669(2) -0.2332(3) 0.06519(18) 0.0223(9) Uani 1 1 d . . . C47 C -0.0023(2) -0.2153(3) 0.0727(2) 0.0311(11) Uani 1 1 d . . . H47 H -0.0122 -0.1628 0.0934 0.037 Uiso 1 1 calc R . . C48 C -0.0569(2) -0.2738(3) 0.0502(2) 0.0357(12) Uani 1 1 d . . . H48 H -0.1042 -0.2612 0.0551 0.043 Uiso 1 1 calc R . . C49 C -0.0423(2) -0.3503(3) 0.0207(2) 0.0342(12) Uani 1 1 d . . . H49 H -0.0796 -0.3906 0.0055 0.041 Uiso 1 1 calc R . . C50 C 0.0258(3) -0.3683(3) 0.0131(2) 0.0363(12) Uani 1 1 d . . . H50 H 0.0356 -0.4211 -0.0072 0.044 Uiso 1 1 calc R . . C51 C 0.0804(2) -0.3097(3) 0.03507(19) 0.0304(11) Uani 1 1 d . . . H51 H 0.1274 -0.3222 0.0294 0.037 Uiso 1 1 calc R . . C52 C 0.1253(2) -0.1688(3) 0.08697(18) 0.0237(10) Uani 1 1 d . . . C53 C 0.5158(2) 0.2019(3) 0.13660(19) 0.0274(10) Uani 1 1 d . . . C54 C 0.5761(2) 0.1503(4) 0.1553(2) 0.0391(13) Uani 1 1 d . . . H54 H 0.5713 0.0901 0.1685 0.047 Uiso 1 1 calc R . . C55 C 0.6428(3) 0.1853(4) 0.1551(3) 0.0536(16) Uani 1 1 d . . . H55 H 0.6836 0.1493 0.1679 0.064 Uiso 1 1 calc R . . C56 C 0.6500(3) 0.2719(4) 0.1363(3) 0.0510(16) Uani 1 1 d . . . H56 H 0.6960 0.2961 0.1363 0.061 Uiso 1 1 calc R . . C57 C 0.5907(3) 0.3243(4) 0.1171(2) 0.0459(14) Uani 1 1 d . . . H57 H 0.5960 0.3844 0.1040 0.055 Uiso 1 1 calc R . . C58 C 0.5230(2) 0.2889(3) 0.1172(2) 0.0351(12) Uani 1 1 d . . . H58 H 0.4821 0.3246 0.1039 0.042 Uiso 1 1 calc R . . C59 C 0.4441(2) 0.1620(3) 0.13804(19) 0.0242(10) Uani 1 1 d . . . C60 C 0.0144(2) -0.0433(3) 0.2059(2) 0.0328(11) Uani 1 1 d . . . H60A H 0.0307 -0.1027 0.1950 0.049 Uiso 1 1 calc R . . H60B H -0.0366 -0.0373 0.1916 0.049 Uiso 1 1 calc R . . H60C H 0.0235 -0.0375 0.2480 0.049 Uiso 1 1 calc R . . C61 C 0.3497(3) 0.3338(4) 0.0042(3) 0.0593(17) Uani 1 1 d . . . H61A H 0.3933 0.2986 0.0157 0.089 Uiso 1 1 calc R . . H61B H 0.3602 0.3984 0.0101 0.089 Uiso 1 1 calc R . . H61C H 0.3309 0.3226 -0.0366 0.089 Uiso 1 1 calc R . . Cl1 Cl 0.35931(8) 0.48916(9) 0.14247(6) 0.0426(3) Uani 1 1 d . . . O17 O 0.3334(2) 0.3988(3) 0.14684(18) 0.0635(12) Uani 1 1 d . . . O18 O 0.3963(3) 0.5153(3) 0.1973(2) 0.0979(18) Uani 1 1 d . . . O19 O 0.4114(3) 0.4912(3) 0.1055(3) 0.0989(19) Uani 1 1 d . . . O20 O 0.3046(3) 0.5486(3) 0.1243(3) 0.107(2) Uani 1 1 d . . . O21 O 0.00069(17) 0.1653(2) 0.23955(15) 0.0408(9) Uani 1 1 d . . . H21A H -0.0375 0.1946 0.2360 0.061 Uiso 1 1 calc R . . C62 C 0.0531(3) 0.2091(4) 0.2806(3) 0.0581(17) Uani 1 1 d . . . H62A H 0.0539 0.2739 0.2717 0.087 Uiso 1 1 calc R . . H62B H 0.0997 0.1826 0.2790 0.087 Uiso 1 1 calc R . . H62C H 0.0418 0.2009 0.3193 0.087 Uiso 1 1 calc R . . O22 O 0.12997(19) -0.2573(2) 0.25836(15) 0.0399(9) Uani 1 1 d . . . H22A H 0.1432 -0.2041 0.2532 0.060 Uiso 1 1 calc R . . C63 C 0.1617(3) -0.3170(4) 0.2242(2) 0.0455(14) Uani 1 1 d . . . H63A H 0.2135 -0.3133 0.2351 0.068 Uiso 1 1 calc R . . H63B H 0.1479 -0.3003 0.1835 0.068 Uiso 1 1 calc R . . H63C H 0.1461 -0.3790 0.2300 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.0202(2) 0.0178(2) 0.0194(2) -0.00253(18) 0.00364(16) -0.00078(17) Y2 0.0203(2) 0.0212(2) 0.0188(2) 0.00126(18) 0.00281(16) 0.00224(17) Ni1 0.0195(3) 0.0180(3) 0.0206(3) 0.0003(2) 0.0005(2) -0.0002(2) Ni2 0.0196(3) 0.0203(3) 0.0199(3) -0.0030(2) 0.0023(2) 0.0009(2) O1 0.0215(14) 0.0178(16) 0.0199(16) -0.0028(12) 0.0020(12) 0.0010(12) O2 0.0211(14) 0.0186(16) 0.0237(16) 0.0027(13) 0.0027(12) 0.0012(12) O3 0.0177(14) 0.0242(17) 0.0238(16) -0.0008(13) 0.0062(12) 0.0001(12) O4 0.0184(14) 0.0203(17) 0.0217(16) -0.0043(13) 0.0000(12) 0.0009(12) O5 0.0282(16) 0.0237(18) 0.0210(16) -0.0023(13) 0.0053(13) -0.0047(13) O6 0.0309(16) 0.0238(18) 0.0234(16) -0.0018(14) 0.0032(13) -0.0020(14) O7 0.0278(16) 0.036(2) 0.0215(16) 0.0012(14) 0.0045(13) 0.0051(14) O8 0.0274(16) 0.039(2) 0.0183(16) 0.0000(14) 0.0003(13) 0.0047(14) O9 0.0236(15) 0.0238(18) 0.0310(18) 0.0041(14) 0.0086(13) 0.0027(13) O10 0.0276(16) 0.0240(18) 0.0280(17) 0.0034(14) 0.0093(13) 0.0069(13) O11 0.0284(16) 0.0238(17) 0.0243(17) -0.0073(14) 0.0078(13) -0.0061(13) O12 0.0239(15) 0.0231(17) 0.0283(17) -0.0052(14) 0.0048(13) -0.0023(13) O13 0.0263(16) 0.0254(18) 0.0291(18) 0.0042(14) 0.0001(13) -0.0005(13) O14 0.0209(15) 0.0251(18) 0.0278(17) 0.0034(14) -0.0017(13) -0.0040(13) O15 0.0207(15) 0.0251(18) 0.0289(17) -0.0055(14) 0.0070(13) -0.0029(13) O16 0.0352(17) 0.0285(19) 0.0286(18) 0.0066(15) 0.0090(14) 0.0023(14) N1 0.0268(19) 0.024(2) 0.024(2) -0.0001(17) 0.0039(16) -0.0022(16) N2 0.0216(18) 0.024(2) 0.023(2) 0.0035(16) 0.0016(15) 0.0014(15) N3 0.0278(19) 0.022(2) 0.0198(19) -0.0036(16) 0.0002(15) 0.0042(16) N4 0.0259(19) 0.021(2) 0.022(2) -0.0043(16) 0.0031(15) 0.0002(15) C1 0.042(3) 0.035(3) 0.029(3) 0.006(2) -0.003(2) 0.002(2) C2 0.063(4) 0.051(4) 0.027(3) 0.001(3) -0.010(3) 0.001(3) C3 0.058(3) 0.050(4) 0.021(3) -0.010(3) 0.004(2) -0.009(3) C4 0.036(3) 0.030(3) 0.026(3) -0.009(2) 0.005(2) -0.007(2) C5 0.022(2) 0.022(2) 0.021(2) -0.0012(19) 0.0043(17) -0.0057(18) C6 0.025(2) 0.015(2) 0.024(2) -0.0013(18) 0.0003(18) -0.0014(17) C7 0.021(2) 0.034(3) 0.037(3) 0.003(2) 0.000(2) 0.006(2) C8 0.028(3) 0.045(3) 0.043(3) 0.010(3) 0.001(2) 0.011(2) C9 0.036(3) 0.032(3) 0.041(3) 0.006(2) 0.002(2) 0.013(2) C10 0.042(3) 0.024(3) 0.030(3) 0.002(2) 0.006(2) 0.005(2) C11 0.030(2) 0.027(3) 0.013(2) 0.0025(19) 0.0025(18) 0.0017(19) C12 0.026(2) 0.018(2) 0.027(2) 0.0015(19) 0.0037(18) 0.0018(18) C13 0.036(3) 0.026(3) 0.029(3) -0.002(2) 0.007(2) 0.003(2) C14 0.048(3) 0.024(3) 0.036(3) -0.003(2) 0.009(2) 0.012(2) C15 0.041(3) 0.042(3) 0.043(3) -0.006(3) 0.012(2) 0.018(3) C16 0.028(2) 0.033(3) 0.041(3) -0.001(2) 0.008(2) 0.007(2) C17 0.024(2) 0.027(3) 0.018(2) -0.0042(19) 0.0012(17) 0.0048(19) C18 0.022(2) 0.028(3) 0.027(2) 0.000(2) 0.0090(18) 0.0058(19) C19 0.028(2) 0.030(3) 0.027(3) -0.005(2) 0.005(2) 0.003(2) C20 0.040(3) 0.034(3) 0.020(2) -0.008(2) 0.001(2) 0.003(2) C21 0.040(3) 0.039(3) 0.032(3) -0.011(2) -0.010(2) 0.006(2) C22 0.028(2) 0.036(3) 0.031(3) -0.006(2) 0.000(2) 0.006(2) C23 0.023(2) 0.025(3) 0.026(2) 0.000(2) 0.0014(18) -0.0012(19) C24 0.024(2) 0.029(3) 0.018(2) 0.0003(19) -0.0002(17) 0.0018(19) C25 0.015(2) 0.035(3) 0.023(2) 0.002(2) 0.0028(17) 0.0024(19) C26 0.030(2) 0.041(3) 0.024(3) -0.006(2) 0.000(2) -0.004(2) C27 0.036(3) 0.059(4) 0.031(3) -0.016(3) 0.004(2) -0.001(3) C28 0.048(3) 0.068(4) 0.022(3) 0.002(3) 0.007(2) 0.006(3) C29 0.049(3) 0.048(4) 0.030(3) 0.012(3) 0.009(2) 0.011(3) C30 0.027(2) 0.038(3) 0.027(3) 0.003(2) 0.0050(19) 0.009(2) C31 0.015(2) 0.029(3) 0.026(2) -0.002(2) 0.0041(17) -0.0005(18) C32 0.027(2) 0.024(3) 0.024(2) 0.000(2) 0.0033(19) -0.0020(19) C33 0.026(2) 0.044(3) 0.027(3) 0.003(2) 0.005(2) 0.005(2) C34 0.031(3) 0.063(4) 0.024(3) -0.002(3) -0.004(2) -0.002(3) C35 0.046(3) 0.047(3) 0.025(3) -0.002(2) 0.005(2) -0.006(3) C36 0.038(3) 0.034(3) 0.028(3) -0.004(2) 0.008(2) 0.004(2) C37 0.031(2) 0.028(3) 0.028(3) 0.007(2) 0.002(2) 0.003(2) C38 0.029(2) 0.020(3) 0.026(2) 0.0057(19) 0.0008(19) -0.0008(19) C39 0.029(2) 0.027(3) 0.015(2) 0.0030(19) 0.0002(18) 0.0066(19) C40 0.033(3) 0.040(3) 0.032(3) 0.000(2) 0.004(2) 0.008(2) C41 0.045(3) 0.061(4) 0.038(3) -0.004(3) 0.007(2) 0.026(3) C42 0.081(5) 0.039(4) 0.040(3) -0.008(3) 0.001(3) 0.038(3) C43 0.069(4) 0.034(3) 0.037(3) 0.000(3) 0.007(3) 0.012(3) C44 0.044(3) 0.025(3) 0.027(3) -0.002(2) 0.005(2) 0.009(2) C45 0.020(2) 0.028(3) 0.023(2) -0.001(2) -0.0009(18) 0.0013(18) C46 0.023(2) 0.022(2) 0.020(2) -0.0050(19) 0.0017(17) -0.0031(18) C47 0.029(2) 0.028(3) 0.036(3) -0.007(2) 0.004(2) -0.004(2) C48 0.027(2) 0.035(3) 0.044(3) 0.002(2) 0.003(2) -0.002(2) C49 0.034(3) 0.032(3) 0.033(3) -0.004(2) -0.004(2) -0.013(2) C50 0.049(3) 0.028(3) 0.032(3) -0.011(2) 0.008(2) -0.010(2) C51 0.033(2) 0.027(3) 0.032(3) -0.009(2) 0.007(2) -0.003(2) C52 0.025(2) 0.025(3) 0.020(2) -0.0030(19) 0.0014(18) -0.0014(19) C53 0.028(2) 0.029(3) 0.025(2) -0.001(2) 0.0048(19) -0.003(2) C54 0.028(3) 0.035(3) 0.054(3) 0.004(3) 0.006(2) -0.006(2) C55 0.030(3) 0.060(4) 0.074(4) 0.005(3) 0.015(3) -0.003(3) C56 0.031(3) 0.057(4) 0.070(4) -0.010(3) 0.022(3) -0.013(3) C57 0.058(4) 0.033(3) 0.052(4) -0.006(3) 0.021(3) -0.015(3) C58 0.034(3) 0.032(3) 0.042(3) 0.002(2) 0.011(2) -0.003(2) C59 0.023(2) 0.024(3) 0.025(2) -0.006(2) 0.0036(18) -0.0038(19) C60 0.031(3) 0.032(3) 0.037(3) 0.005(2) 0.009(2) -0.003(2) C61 0.061(4) 0.063(4) 0.059(4) 0.018(3) 0.025(3) 0.000(3) Cl1 0.0598(9) 0.0312(7) 0.0376(7) -0.0009(6) 0.0110(6) -0.0063(6) O17 0.094(3) 0.035(2) 0.068(3) -0.009(2) 0.031(2) -0.023(2) O18 0.144(5) 0.073(4) 0.066(3) -0.005(3) -0.011(3) -0.038(3) O19 0.116(4) 0.067(3) 0.135(5) 0.019(3) 0.081(4) 0.000(3) O20 0.062(3) 0.069(4) 0.187(6) 0.037(4) 0.013(3) 0.008(3) O21 0.0371(19) 0.042(2) 0.045(2) -0.0145(18) 0.0113(17) 0.0037(16) C62 0.052(4) 0.055(4) 0.061(4) -0.029(3) -0.008(3) 0.015(3) O22 0.054(2) 0.026(2) 0.040(2) 0.0025(17) 0.0089(17) -0.0068(17) C63 0.054(3) 0.033(3) 0.050(4) 0.003(3) 0.012(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O11 2.294(3) . ? Y1 O9 2.316(3) . ? Y1 O4 2.327(3) . ? Y1 O2 2.347(3) . ? Y1 O5 2.365(3) . ? Y1 O1 2.414(3) . ? Y1 O15 2.414(3) . ? Y1 O6 2.470(3) . ? Y1 Ni2 3.2969(7) . ? Y1 Ni1 3.4605(8) . ? Y1 Y2 3.8826(6) . ? Y2 O10 2.271(3) . ? Y2 O13 2.294(3) . ? Y2 O3 2.347(3) . ? Y2 O1 2.366(3) . ? Y2 O7 2.399(3) . ? Y2 O8 2.408(3) . ? Y2 O4 2.418(3) . ? Y2 O16 2.425(3) . ? Y2 Ni1 3.3409(7) . ? Y2 Ni2 3.4243(8) . ? Ni1 N2 2.016(3) . ? Ni1 O14 2.024(3) . ? Ni1 O1 2.048(3) . ? Ni1 O2 2.065(3) . ? Ni1 N1 2.078(4) . ? Ni1 O3 2.132(3) . ? Ni2 N3 2.030(3) . ? Ni2 O12 2.040(3) . ? Ni2 O3 2.040(3) . ? Ni2 O4 2.063(3) . ? Ni2 N4 2.091(3) . ? Ni2 O2 2.104(3) . ? O1 C6 1.421(5) . ? O2 C12 1.418(5) . ? O3 C18 1.423(5) . ? O4 C24 1.433(5) . ? O5 C31 1.269(5) . ? O6 C31 1.277(5) . ? O7 C38 1.269(5) . ? O8 C38 1.266(5) . ? O9 C45 1.262(5) . ? O10 C45 1.252(5) . ? O11 C52 1.269(5) . ? O12 C52 1.258(5) . ? O13 C59 1.262(5) . ? O14 C59 1.252(5) . ? O15 C60 1.431(5) . ? O16 C61 1.433(6) . ? N1 C5 1.332(5) . ? N1 C1 1.345(6) . ? N2 C11 1.341(5) . ? N2 C7 1.347(5) . ? N3 C17 1.342(5) . ? N3 C13 1.348(5) . ? N4 C23 1.345(5) . ? N4 C19 1.346(5) . ? C1 C2 1.384(7) . ? C2 C3 1.377(7) . ? C3 C4 1.381(7) . ? C4 C5 1.377(6) . ? C5 C6 1.520(6) . ? C7 C8 1.366(6) . ? C8 C9 1.376(7) . ? C9 C10 1.383(6) . ? C10 C11 1.384(6) . ? C11 C12 1.509(6) . ? C13 C14 1.365(6) . ? C14 C15 1.385(7) . ? C15 C16 1.369(7) . ? C16 C17 1.386(6) . ? C17 C18 1.506(6) . ? C19 C20 1.368(6) . ? C20 C21 1.384(6) . ? C21 C22 1.380(6) . ? C22 C23 1.379(6) . ? C23 C24 1.505(6) . ? C25 C26 1.390(6) . ? C25 C30 1.398(6) . ? C25 C31 1.489(6) . ? C26 C27 1.389(7) . ? C27 C28 1.383(8) . ? C28 C29 1.387(7) . ? C29 C30 1.376(6) . ? C32 C33 1.385(6) . ? C32 C37 1.390(6) . ? C32 C38 1.491(6) . ? C33 C34 1.385(6) . ? C34 C35 1.380(7) . ? C35 C36 1.384(6) . ? C36 C37 1.372(6) . ? C39 C44 1.382(6) . ? C39 C40 1.394(6) . ? C39 C45 1.496(6) . ? C40 C41 1.383(7) . ? C41 C42 1.383(8) . ? C42 C43 1.381(8) . ? C43 C44 1.381(7) . ? C46 C51 1.381(6) . ? C46 C47 1.392(6) . ? C46 C52 1.488(6) . ? C47 C48 1.388(6) . ? C48 C49 1.379(7) . ? C49 C50 1.371(7) . ? C50 C51 1.385(6) . ? C53 C58 1.378(6) . ? C53 C54 1.388(6) . ? C53 C59 1.498(6) . ? C54 C55 1.377(6) . ? C55 C56 1.367(8) . ? C56 C57 1.383(7) . ? C57 C58 1.396(6) . ? Cl1 O20 1.376(5) . ? Cl1 O18 1.413(5) . ? Cl1 O17 1.432(4) . ? Cl1 O19 1.432(5) . ? O21 C62 1.421(6) . ? O22 C63 1.400(6) . ? 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 O11 Y1 O9 118.01(11) . . ? O11 Y1 O4 79.19(10) . . ? O9 Y1 O4 79.86(10) . . ? O11 Y1 O2 81.98(10) . . ? O9 Y1 O2 144.41(10) . . ? O4 Y1 O2 75.35(9) . . ? O11 Y1 O5 130.95(10) . . ? O9 Y1 O5 86.17(10) . . ? O4 Y1 O5 149.71(10) . . ? O2 Y1 O5 102.80(10) . . ? O11 Y1 O1 142.51(9) . . ? O9 Y1 O1 77.55(10) . . ? O4 Y1 O1 69.97(9) . . ? O2 Y1 O1 70.20(9) . . ? O5 Y1 O1 80.87(9) . . ? O11 Y1 O15 72.71(10) . . ? O9 Y1 O15 68.92(10) . . ? O4 Y1 O15 119.67(9) . . ? O2 Y1 O15 146.33(10) . . ? O5 Y1 O15 78.88(10) . . ? O1 Y1 O15 141.65(10) . . ? O11 Y1 O6 80.33(10) . . ? O9 Y1 O6 131.62(10) . . ? O4 Y1 O6 148.15(10) . . ? O2 Y1 O6 77.85(10) . . ? O5 Y1 O6 54.22(10) . . ? O1 Y1 O6 116.11(9) . . ? O15 Y1 O6 76.32(10) . . ? O11 Y1 Ni2 67.55(7) . . ? O9 Y1 Ni2 117.79(7) . . ? O4 Y1 Ni2 38.38(7) . . ? O2 Y1 Ni2 39.44(7) . . ? O5 Y1 Ni2 140.44(7) . . ? O1 Y1 Ni2 75.02(7) . . ? O15 Y1 Ni2 137.39(7) . . ? O6 Y1 Ni2 110.59(7) . . ? O11 Y1 Ni1 116.11(7) . . ? O9 Y1 Ni1 112.85(7) . . ? O4 Y1 Ni1 74.27(7) . . ? O2 Y1 Ni1 35.52(7) . . ? O5 Y1 Ni1 86.88(7) . . ? O1 Y1 Ni1 35.47(7) . . ? O15 Y1 Ni1 165.56(7) . . ? O6 Y1 Ni1 93.45(7) . . ? Ni2 Y1 Ni1 55.641(15) . . ? O11 Y1 Y2 114.50(7) . . ? O9 Y1 Y2 69.34(7) . . ? O4 Y1 Y2 35.86(7) . . ? O2 Y1 Y2 75.63(7) . . ? O5 Y1 Y2 113.92(7) . . ? O1 Y1 Y2 35.27(6) . . ? O15 Y1 Y2 135.11(7) . . ? O6 Y1 Y2 147.07(7) . . ? Ni2 Y1 Y2 56.262(15) . . ? Ni1 Y1 Y2 53.754(13) . . ? O10 Y2 O13 115.19(11) . . ? O10 Y2 O3 143.75(10) . . ? O13 Y2 O3 78.30(10) . . ? O10 Y2 O1 75.21(10) . . ? O13 Y2 O1 80.98(10) . . ? O3 Y2 O1 74.09(9) . . ? O10 Y2 O7 85.06(10) . . ? O13 Y2 O7 132.83(10) . . ? O3 Y2 O7 110.94(10) . . ? O1 Y2 O7 146.07(10) . . ? O10 Y2 O8 134.59(10) . . ? O13 Y2 O8 85.53(10) . . ? O3 Y2 O8 77.15(10) . . ? O1 Y2 O8 150.14(10) . . ? O7 Y2 O8 54.54(9) . . ? O10 Y2 O4 80.17(10) . . ? O13 Y2 O4 141.96(10) . . ? O3 Y2 O4 71.28(9) . . ? O1 Y2 O4 69.26(9) . . ? O7 Y2 O4 80.48(10) . . ? O8 Y2 O4 108.71(10) . . ? O10 Y2 O16 71.29(10) . . ? O13 Y2 O16 70.09(10) . . ? O3 Y2 O16 142.14(10) . . ? O1 Y2 O16 119.24(10) . . ? O7 Y2 O16 78.33(10) . . ? O8 Y2 O16 80.06(11) . . ? O4 Y2 O16 145.59(10) . . ? O10 Y2 Ni1 112.56(7) . . ? O13 Y2 Ni1 66.27(7) . . ? O3 Y2 Ni1 39.36(7) . . ? O1 Y2 Ni1 37.37(7) . . ? O7 Y2 Ni1 147.00(8) . . ? O8 Y2 Ni1 112.78(7) . . ? O4 Y2 Ni1 75.72(7) . . ? O16 Y2 Ni1 132.85(7) . . ? O10 Y2 Ni2 115.68(8) . . ? O13 Y2 Ni2 112.94(8) . . ? O3 Y2 Ni2 35.60(7) . . ? O1 Y2 Ni2 72.99(7) . . ? O7 Y2 Ni2 91.89(8) . . ? O8 Y2 Ni2 88.22(8) . . ? O4 Y2 Ni2 36.47(6) . . ? O16 Y2 Ni2 167.70(7) . . ? Ni1 Y2 Ni2 55.619(15) . . ? O10 Y2 Y1 68.36(7) . . ? O13 Y2 Y1 116.16(7) . . ? O3 Y2 Y1 75.49(7) . . ? O1 Y2 Y1 36.09(6) . . ? O7 Y2 Y1 110.86(7) . . ? O8 Y2 Y1 140.14(8) . . ? O4 Y2 Y1 34.31(7) . . ? O16 Y2 Y1 137.36(7) . . ? Ni1 Y2 Y1 56.651(14) . . ? Ni2 Y2 Y1 53.194(12) . . ? N2 Ni1 O14 93.53(13) . . ? N2 Ni1 O1 163.41(13) . . ? O14 Ni1 O1 102.27(12) . . ? N2 Ni1 O2 81.99(12) . . ? O14 Ni1 O2 167.81(12) . . ? O1 Ni1 O2 83.48(11) . . ? N2 Ni1 N1 96.46(14) . . ? O14 Ni1 N1 85.77(13) . . ? O1 Ni1 N1 79.90(12) . . ? O2 Ni1 N1 105.94(12) . . ? N2 Ni1 O3 99.97(13) . . ? O14 Ni1 O3 88.68(11) . . ? O1 Ni1 O3 85.56(11) . . ? O2 Ni1 O3 80.99(11) . . ? N1 Ni1 O3 162.95(13) . . ? N2 Ni1 Y2 144.14(10) . . ? O14 Ni1 Y2 84.35(8) . . ? O1 Ni1 Y2 44.51(8) . . ? O2 Ni1 Y2 92.63(8) . . ? N1 Ni1 Y2 118.96(10) . . ? O3 Ni1 Y2 44.29(8) . . ? N2 Ni1 Y1 120.94(10) . . ? O14 Ni1 Y1 145.40(9) . . ? O1 Ni1 Y1 43.14(8) . . ? O2 Ni1 Y1 41.34(8) . . ? N1 Ni1 Y1 87.40(10) . . ? O3 Ni1 Y1 88.06(7) . . ? Y2 Ni1 Y1 69.595(14) . . ? N3 Ni2 O12 94.99(13) . . ? N3 Ni2 O3 81.53(13) . . ? O12 Ni2 O3 171.06(12) . . ? N3 Ni2 O4 164.00(13) . . ? O12 Ni2 O4 99.41(11) . . ? O3 Ni2 O4 85.18(11) . . ? N3 Ni2 N4 96.07(13) . . ? O12 Ni2 N4 84.11(13) . . ? O3 Ni2 N4 104.40(13) . . ? O4 Ni2 N4 78.61(12) . . ? N3 Ni2 O2 100.36(12) . . ? O12 Ni2 O2 90.35(11) . . ? O3 Ni2 O2 82.23(11) . . ? O4 Ni2 O2 86.56(11) . . ? N4 Ni2 O2 163.06(12) . . ? N3 Ni2 Y1 145.34(10) . . ? O12 Ni2 Y1 83.96(8) . . ? O3 Ni2 Y1 94.20(8) . . ? O4 Ni2 Y1 44.44(8) . . ? N4 Ni2 Y1 118.16(10) . . ? O2 Ni2 Y1 45.13(7) . . ? N3 Ni2 Y2 120.88(10) . . ? O12 Ni2 Y2 143.49(8) . . ? O3 Ni2 Y2 42.04(8) . . ? O4 Ni2 Y2 44.15(8) . . ? N4 Ni2 Y2 85.43(10) . . ? O2 Ni2 Y2 89.63(8) . . ? Y1 Ni2 Y2 70.545(15) . . ? C6 O1 Ni1 110.6(2) . . ? C6 O1 Y2 118.6(2) . . ? Ni1 O1 Y2 98.12(11) . . ? C6 O1 Y1 116.6(2) . . ? Ni1 O1 Y1 101.40(11) . . ? Y2 O1 Y1 108.65(10) . . ? C12 O2 Ni1 110.5(2) . . ? C12 O2 Ni2 112.8(2) . . ? Ni1 O2 Ni2 98.46(12) . . ? C12 O2 Y1 131.3(2) . . ? Ni1 O2 Y1 103.14(12) . . ? Ni2 O2 Y1 95.44(10) . . ? C18 O3 Ni2 110.9(2) . . ? C18 O3 Ni1 116.5(2) . . ? Ni2 O3 Ni1 98.32(11) . . ? C18 O3 Y2 127.8(2) . . ? Ni2 O3 Y2 102.37(11) . . ? Ni1 O3 Y2 96.35(11) . . ? C24 O4 Ni2 110.7(2) . . ? C24 O4 Y1 118.3(2) . . ? Ni2 O4 Y1 97.18(11) . . ? C24 O4 Y2 117.7(2) . . ? Ni2 O4 Y2 99.37(10) . . ? Y1 O4 Y2 109.83(11) . . ? C31 O5 Y1 95.4(3) . . ? C31 O6 Y1 90.3(3) . . ? C38 O7 Y2 92.3(2) . . ? C38 O8 Y2 92.0(3) . . ? C45 O9 Y1 135.2(3) . . ? C45 O10 Y2 140.0(3) . . ? C52 O11 Y1 137.1(3) . . ? C52 O12 Ni2 124.5(3) . . ? C59 O13 Y2 136.7(3) . . ? C59 O14 Ni1 124.7(3) . . ? C60 O15 Y1 127.0(3) . . ? C61 O16 Y2 123.0(3) . . ? C5 N1 C1 118.6(4) . . ? C5 N1 Ni1 112.8(3) . . ? C1 N1 Ni1 127.2(3) . . ? C11 N2 C7 118.3(4) . . ? C11 N2 Ni1 114.3(3) . . ? C7 N2 Ni1 127.4(3) . . ? C17 N3 C13 118.8(4) . . ? C17 N3 Ni2 113.5(3) . . ? C13 N3 Ni2 127.4(3) . . ? C23 N4 C19 117.7(4) . . ? C23 N4 Ni2 111.4(3) . . ? C19 N4 Ni2 127.0(3) . . ? N1 C1 C2 122.0(5) . . ? C3 C2 C1 118.7(5) . . ? C2 C3 C4 119.4(5) . . ? C5 C4 C3 118.5(5) . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C6 116.4(4) . . ? C4 C5 C6 120.8(4) . . ? O1 C6 C5 111.3(3) . . ? N2 C7 C8 122.8(5) . . ? C7 C8 C9 118.9(4) . . ? C8 C9 C10 119.0(5) . . ? C9 C10 C11 119.1(5) . . ? N2 C11 C10 121.7(4) . . ? N2 C11 C12 116.4(4) . . ? C10 C11 C12 121.9(4) . . ? O2 C12 C11 112.2(3) . . ? N3 C13 C14 122.9(4) . . ? C13 C14 C15 117.9(5) . . ? C16 C15 C14 120.2(4) . . ? C15 C16 C17 119.0(5) . . ? N3 C17 C16 121.3(4) . . ? N3 C17 C18 116.5(4) . . ? C16 C17 C18 122.2(4) . . ? O3 C18 C17 112.0(3) . . ? N4 C19 C20 123.6(4) . . ? C19 C20 C21 118.4(4) . . ? C22 C21 C20 118.8(4) . . ? C23 C22 C21 119.7(4) . . ? N4 C23 C22 121.8(4) . . ? N4 C23 C24 116.2(4) . . ? C22 C23 C24 122.0(4) . . ? O4 C24 C23 111.7(3) . . ? C26 C25 C30 119.6(4) . . ? C26 C25 C31 120.2(4) . . ? C30 C25 C31 120.2(4) . . ? C27 C26 C25 120.0(5) . . ? C28 C27 C26 120.1(5) . . ? C27 C28 C29 119.9(5) . . ? C30 C29 C28 120.5(5) . . ? C29 C30 C25 120.0(5) . . ? O5 C31 O6 120.1(4) . . ? O5 C31 C25 119.1(4) . . ? O6 C31 C25 120.9(4) . . ? C33 C32 C37 118.3(4) . . ? C33 C32 C38 121.3(4) . . ? C37 C32 C38 120.3(4) . . ? C32 C33 C34 121.0(4) . . ? C35 C34 C33 119.7(4) . . ? C34 C35 C36 119.9(5) . . ? C37 C36 C35 120.0(5) . . ? C36 C37 C32 121.1(4) . . ? O8 C38 O7 120.7(4) . . ? O8 C38 C32 120.2(4) . . ? O7 C38 C32 119.0(4) . . ? C44 C39 C40 119.5(4) . . ? C44 C39 C45 120.0(4) . . ? C40 C39 C45 120.5(4) . . ? C41 C40 C39 119.6(5) . . ? C42 C41 C40 120.1(5) . . ? C43 C42 C41 120.8(5) . . ? C42 C43 C44 118.9(6) . . ? C43 C44 C39 121.2(5) . . ? O10 C45 O9 125.2(4) . . ? O10 C45 C39 116.0(4) . . ? O9 C45 C39 118.8(4) . . ? C51 C46 C47 119.2(4) . . ? C51 C46 C52 120.3(4) . . ? C47 C46 C52 120.5(4) . . ? C48 C47 C46 120.2(4) . . ? C49 C48 C47 119.8(4) . . ? C50 C49 C48 120.2(4) . . ? C49 C50 C51 120.2(5) . . ? C46 C51 C50 120.4(4) . . ? O12 C52 O11 123.9(4) . . ? O12 C52 C46 117.4(4) . . ? O11 C52 C46 118.7(4) . . ? C58 C53 C54 119.4(4) . . ? C58 C53 C59 121.2(4) . . ? C54 C53 C59 119.4(4) . . ? C55 C54 C53 120.8(5) . . ? C56 C55 C54 119.9(5) . . ? C55 C56 C57 120.3(5) . . ? C56 C57 C58 120.0(5) . . ? C53 C58 C57 119.6(5) . . ? O14 C59 O13 125.4(4) . . ? O14 C59 C53 116.8(4) . . ? O13 C59 C53 117.8(4) . . ? O20 Cl1 O18 110.1(4) . . ? O20 Cl1 O17 111.2(3) . . ? O18 Cl1 O17 108.2(3) . . ? O20 Cl1 O19 111.7(4) . . ? O18 Cl1 O19 105.0(4) . . ? O17 Cl1 O19 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.202 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.104 data_ic15661 _database_code_depnum_ccdc_archive 'CCDC 910496' #TrackingRef '15360_web_deposit_cif_file_3_En-CheYang_1352708909.complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H75 Cl Gd2 N4 Ni2 O26' _chemical_formula_weight 1783.65 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.2334(10) _cell_length_b 23.9758(11) _cell_length_c 17.5937(8) _cell_angle_alpha 90.00 _cell_angle_beta 121.3414(9) _cell_angle_gamma 90.00 _cell_volume 7649.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7171 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.27 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 2.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4441 _exptl_absorpt_correction_T_max 0.5962 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24781 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8788 _reflns_number_gt 7195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure restrains are applied for atosm of N1, N1', C1-C5, C1'-C5', C25-C30 and C25'-C30' by ISOR. ; _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^)+(0.0904P)^2^+34.1335P] 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 8788 _refine_ls_number_parameters 466 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Gd Gd 1.006436(14) 0.669807(12) 0.641486(16) 0.03431(11) Uani 1 1 d . . . Ni Ni 0.91350(5) 0.57393(4) 0.69433(5) 0.0452(2) Uani 1 1 d . . . O1 O 0.9242(2) 0.65915(17) 0.6998(3) 0.0367(8) Uani 1 1 d . . . O2 O 0.9987(2) 0.57373(17) 0.6718(3) 0.0420(9) Uani 1 1 d . . . O3 O 0.8934(2) 0.70516(18) 0.5131(3) 0.0439(10) Uani 1 1 d . . . O4 O 0.9396(2) 0.62811(19) 0.4937(3) 0.0485(11) Uani 1 1 d . . . O5 O 1.0065(3) 0.76051(18) 0.6912(3) 0.0489(11) Uani 1 1 d . . . O6 O 0.8407(3) 0.5666(2) 0.7357(3) 0.0596(13) Uani 1 1 d . A . O7 O 0.8839(2) 0.6326(2) 0.8394(3) 0.0501(11) Uani 1 1 d . . . O8 O 1.0531(3) 0.7317(2) 0.5731(3) 0.0621(13) Uani 1 1 d . . . H8A H 1.0747 0.7237 0.5441 0.093 Uiso 1 1 d R A . H8B H 1.0130 0.7484 0.5397 0.093 Uiso 1 1 d R . . N2 N 0.9123(4) 0.4916(3) 0.6648(4) 0.0701(19) Uani 1 1 d . A . N1 N 0.8180(9) 0.6052(6) 0.5695(12) 0.039(2) Uani 0.529(7) 1 d PU A 1 C1 C 0.7707(9) 0.5742(6) 0.4985(10) 0.047(3) Uani 0.529(7) 1 d PU A 1 H1 H 0.7845 0.5375 0.4925 0.057 Uiso 0.529(7) 1 calc PR A 1 C2 C 0.7022(9) 0.5946(9) 0.4338(11) 0.056(3) Uani 0.529(7) 1 d PU A 1 H2 H 0.6682 0.5715 0.3861 0.068 Uiso 0.529(7) 1 calc PR A 1 C3 C 0.6854(8) 0.6466(8) 0.4399(10) 0.056(3) Uani 0.529(7) 1 d PU A 1 H3 H 0.6396 0.6614 0.3944 0.067 Uiso 0.529(7) 1 calc PR A 1 C4 C 0.7326(9) 0.6801(6) 0.5107(11) 0.049(3) Uani 0.529(7) 1 d PU A 1 H4 H 0.7199 0.7174 0.5158 0.058 Uiso 0.529(7) 1 calc PR A 1 C5 C 0.7992(9) 0.6570(6) 0.5737(11) 0.034(2) Uani 0.529(7) 1 d PU A 1 N1' N 0.8272(10) 0.5859(6) 0.5739(13) 0.039(2) Uani 0.471(7) 1 d PU A 2 C1' C 0.7849(10) 0.5516(7) 0.5071(12) 0.047(3) Uani 0.471(7) 1 d PU A 2 H1' H 0.8023 0.5148 0.5088 0.057 Uiso 0.471(7) 1 calc PR A 2 C2' C 0.7175(10) 0.5665(8) 0.4358(12) 0.056(3) Uani 0.471(7) 1 d PU A 2 H2' H 0.6906 0.5415 0.3874 0.068 Uiso 0.471(7) 1 calc PR A 2 C3' C 0.6895(11) 0.6183(11) 0.4357(13) 0.056(3) Uani 0.471(7) 1 d PU A 2 H3' H 0.6415 0.6286 0.3891 0.067 Uiso 0.471(7) 1 calc PR A 2 C4' C 0.7322(10) 0.6554(7) 0.5043(13) 0.049(3) Uani 0.471(7) 1 d PU A 2 H4' H 0.7155 0.6919 0.5056 0.058 Uiso 0.471(7) 1 calc PR A 2 C5' C 0.8017(11) 0.6356(8) 0.5719(13) 0.034(2) Uani 0.471(7) 1 d PU A 2 C6 C 0.8528(3) 0.6846(3) 0.6514(4) 0.0521(16) Uani 1 1 d . . . H6A H 0.8337 0.6881 0.6919 0.062 Uiso 0.529(7) 1 calc PR A 1 H6B H 0.8587 0.7228 0.6347 0.062 Uiso 0.529(7) 1 calc PR A 1 H6C H 0.8547 0.7202 0.6241 0.062 Uiso 0.471(7) 1 d PR A 2 H6D H 0.8328 0.6917 0.6903 0.062 Uiso 0.471(7) 1 d PR A 2 C7 C 0.8716(6) 0.4512(4) 0.6722(6) 0.086(3) Uani 1 1 d . . . H7 H 0.8414 0.4604 0.6956 0.104 Uiso 1 1 calc R A . C8 C 0.8726(8) 0.3973(4) 0.6469(7) 0.110(4) Uani 1 1 d . A . H8 H 0.8436 0.3694 0.6527 0.131 Uiso 1 1 calc R . . C9 C 0.9162(8) 0.3845(4) 0.6130(8) 0.114(4) Uani 1 1 d . . . H9 H 0.9180 0.3473 0.5957 0.137 Uiso 1 1 calc R A . C10 C 0.9567(6) 0.4247(4) 0.6041(6) 0.083(3) Uani 1 1 d . A . H10 H 0.9861 0.4163 0.5793 0.099 Uiso 1 1 calc R . . C11 C 0.9544(5) 0.4788(3) 0.6322(5) 0.064(2) Uani 1 1 d . . . C12 C 0.9949(4) 0.5272(3) 0.6207(5) 0.0546(17) Uani 1 1 d . A . H12A H 1.0455 0.5153 0.6389 0.066 Uiso 1 1 calc R . . H12B H 0.9692 0.5379 0.5571 0.066 Uiso 1 1 calc R . . C13 C 0.8241(4) 0.6590(3) 0.3728(4) 0.0560(18) Uani 1 1 d . . . C14 C 0.8104(5) 0.6108(5) 0.3260(5) 0.086(3) Uani 1 1 d . A . H14 H 0.8441 0.5805 0.3504 0.104 Uiso 1 1 calc R . . C15 C 0.7462(6) 0.6060(6) 0.2414(6) 0.116(5) Uani 1 1 d . . . H15 H 0.7363 0.5721 0.2090 0.139 Uiso 1 1 calc R A . C16 C 0.6983(5) 0.6493(6) 0.2055(6) 0.113(5) Uani 1 1 d . A . H16 H 0.6552 0.6455 0.1482 0.135 Uiso 1 1 calc R . . C17 C 0.7113(6) 0.6978(7) 0.2502(6) 0.117(5) Uani 1 1 d . . . H17 H 0.6785 0.7284 0.2245 0.141 Uiso 1 1 calc R A . C18 C 0.7747(5) 0.7019(5) 0.3362(5) 0.087(3) Uani 1 1 d . A . H18 H 0.7832 0.7352 0.3693 0.104 Uiso 1 1 calc R . . C19 C 0.8896(3) 0.6644(3) 0.4646(4) 0.0430(14) Uani 1 1 d . A . C20 C 1.0000 0.8468(4) 0.7500 0.0391(17) Uani 1 2 d S . . C21 C 1.0167(4) 0.8756(3) 0.6958(5) 0.0516(16) Uani 1 1 d . A . H21 H 1.0283 0.8559 0.6579 0.062 Uiso 1 1 calc R . . C22 C 1.0169(5) 0.9337(3) 0.6957(6) 0.068(2) Uani 1 1 d . . . H22 H 1.0287 0.9537 0.6582 0.081 Uiso 1 1 calc R A . C23 C 1.0000 0.9610(5) 0.7500 0.075(4) Uani 1 2 d S . . H23 H 1.0000 1.0006 0.7500 0.090 Uiso 1 2 calc SR . . C24 C 1.0000 0.7848(3) 0.7500 0.0396(18) Uani 1 2 d S . . C25 C 0.7746(13) 0.5911(7) 0.8087(17) 0.044(3) Uani 0.529(7) 1 d PU A 1 C26 C 0.7083(10) 0.5638(8) 0.7394(13) 0.073(4) Uani 0.529(7) 1 d PU A 1 H26 H 0.7054 0.5510 0.6865 0.087 Uiso 0.529(7) 1 calc PR A 1 C27 C 0.6496(11) 0.5566(9) 0.7512(14) 0.086(4) Uani 0.529(7) 1 d PU A 1 H27 H 0.6057 0.5391 0.7065 0.103 Uiso 0.529(7) 1 calc PR A 1 C28 C 0.6557(11) 0.5754(9) 0.8301(14) 0.079(4) Uani 0.529(7) 1 d PU A 1 H28 H 0.6165 0.5697 0.8404 0.094 Uiso 0.529(7) 1 calc PR A 1 C29 C 0.7154(15) 0.6005(10) 0.8888(19) 0.078(5) Uani 0.529(7) 1 d PU A 1 H29 H 0.7194 0.6128 0.9424 0.093 Uiso 0.529(7) 1 calc PR A 1 C30 C 0.7750(16) 0.6105(9) 0.8762(18) 0.064(4) Uani 0.529(7) 1 d PU A 1 H30 H 0.8158 0.6320 0.9188 0.077 Uiso 0.529(7) 1 calc PR A 1 C25' C 0.7810(15) 0.5744(8) 0.8106(19) 0.044(3) Uani 0.471(7) 1 d PDU A 2 C26' C 0.7329(10) 0.5364(8) 0.7636(14) 0.073(4) Uani 0.471(7) 1 d PDU A 2 H26' H 0.7335 0.5199 0.7149 0.087 Uiso 0.471(7) 1 calc PR A 2 C27' C 0.6813(11) 0.5199(9) 0.7831(15) 0.086(4) Uani 0.471(7) 1 d PDU A 2 H27' H 0.6500 0.4892 0.7519 0.103 Uiso 0.471(7) 1 calc PR A 2 C28' C 0.6740(12) 0.5459(9) 0.8451(15) 0.079(4) Uani 0.471(7) 1 d PDU A 2 H28' H 0.6318 0.5390 0.8491 0.094 Uiso 0.471(7) 1 calc PR A 2 C29' C 0.7279(17) 0.5831(11) 0.904(2) 0.078(5) Uani 0.471(7) 1 d PDU A 2 H29' H 0.7260 0.5991 0.9524 0.093 Uiso 0.471(7) 1 calc PR A 2 C30' C 0.7823(18) 0.5951(10) 0.890(2) 0.064(4) Uani 0.471(7) 1 d PDU A 2 H30' H 0.8224 0.6175 0.9314 0.077 Uiso 0.471(7) 1 calc PR A 2 C31 C 0.8392(4) 0.5947(3) 0.7936(4) 0.0492(15) Uani 1 1 d . . . Cl1 Cl 1.0923(5) 0.9606(3) 0.5055(5) 0.114(2) Uani 0.50 1 d P B 1 O9 O 1.071(2) 0.9380(14) 0.556(2) 0.215(12) Uiso 0.50 1 d P B 1 O10 O 1.044(2) 0.9411(14) 0.418(2) 0.222(13) Uiso 0.50 1 d P B 1 O11 O 1.1567(18) 0.9615(13) 0.529(2) 0.195(11) Uiso 0.50 1 d P B 1 O12 O 1.084(2) 1.012(2) 0.539(3) 0.276(18) Uiso 0.50 1 d P B 1 O13 O 1.023(2) 0.9447(17) 0.475(3) 0.252(17) Uiso 0.50 1 d P C 2 O14 O 1.1877(6) 0.7715(4) 0.4999(6) 0.130(3) Uiso 1 1 d D . . C32 C 1.1504(9) 0.7345(7) 0.5199(11) 0.147(6) Uiso 1 1 d D . . O15 O 0.9947(8) 0.8310(5) 0.4910(9) 0.168(5) Uiso 1 1 d D . . C33 C 0.9129(10) 0.8413(8) 0.4518(13) 0.164(7) Uiso 1 1 d D . . O16 O 1.0768(19) 0.7435(14) 0.209(2) 0.226(13) Uiso 0.50 1 d PD D -1 C34 C 1.035(3) 0.776(2) 0.242(4) 0.26(3) Uiso 0.50 1 d PD D -1 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 Gd 0.02498(16) 0.04395(18) 0.02653(16) 0.00032(10) 0.00817(12) 0.00123(11) Ni 0.0407(4) 0.0534(5) 0.0391(4) -0.0102(3) 0.0190(4) -0.0148(4) O1 0.0220(18) 0.048(2) 0.0298(19) -0.0002(16) 0.0062(16) 0.0011(16) O2 0.046(2) 0.041(2) 0.038(2) -0.0043(17) 0.0210(19) -0.0006(18) O3 0.038(2) 0.053(2) 0.0290(19) 0.0024(17) 0.0099(18) 0.0081(19) O4 0.039(2) 0.059(3) 0.034(2) -0.0052(19) 0.0098(19) 0.010(2) O5 0.058(3) 0.046(2) 0.038(2) 0.0003(18) 0.023(2) -0.004(2) O6 0.050(3) 0.081(3) 0.049(3) -0.014(2) 0.027(2) -0.026(3) O7 0.033(2) 0.071(3) 0.044(2) -0.003(2) 0.018(2) -0.008(2) O8 0.057(3) 0.074(3) 0.064(3) 0.013(3) 0.037(3) 0.003(3) N2 0.099(5) 0.058(4) 0.055(4) -0.017(3) 0.041(4) -0.032(4) N1 0.032(4) 0.035(6) 0.041(3) -0.001(5) 0.013(3) -0.001(5) C1 0.041(5) 0.045(6) 0.040(4) -0.005(5) 0.010(4) -0.008(5) C2 0.042(5) 0.058(6) 0.051(4) -0.010(5) 0.011(4) -0.015(5) C3 0.037(4) 0.059(6) 0.049(4) 0.000(6) 0.006(3) -0.001(5) C4 0.036(4) 0.048(6) 0.048(4) 0.003(5) 0.011(3) 0.000(5) C5 0.025(3) 0.035(6) 0.036(3) 0.000(5) 0.011(3) -0.003(5) N1' 0.032(4) 0.035(6) 0.041(3) -0.001(5) 0.013(3) -0.001(5) C1' 0.041(5) 0.045(6) 0.040(4) -0.005(5) 0.010(4) -0.008(5) C2' 0.042(5) 0.058(6) 0.051(4) -0.010(5) 0.011(4) -0.015(5) C3' 0.037(4) 0.059(6) 0.049(4) 0.000(6) 0.006(3) -0.001(5) C4' 0.036(4) 0.048(6) 0.048(4) 0.003(5) 0.011(3) 0.000(5) C5' 0.025(3) 0.035(6) 0.036(3) 0.000(5) 0.011(3) -0.003(5) C6 0.026(3) 0.086(5) 0.035(3) 0.007(3) 0.009(3) 0.014(3) C7 0.117(8) 0.078(6) 0.064(5) -0.021(4) 0.046(6) -0.049(6) C8 0.159(12) 0.061(6) 0.091(7) -0.024(5) 0.053(8) -0.051(7) C9 0.186(14) 0.058(6) 0.111(9) -0.026(6) 0.086(10) -0.027(7) C10 0.107(8) 0.057(5) 0.078(6) -0.020(4) 0.043(6) -0.009(5) C11 0.091(6) 0.050(4) 0.048(4) -0.014(3) 0.034(4) -0.015(4) C12 0.073(5) 0.044(3) 0.050(4) -0.008(3) 0.034(4) 0.001(3) C13 0.036(4) 0.091(5) 0.031(3) -0.009(3) 0.011(3) 0.007(3) C14 0.051(5) 0.136(9) 0.050(4) -0.043(5) 0.010(4) 0.010(5) C15 0.059(6) 0.196(13) 0.058(5) -0.062(7) 0.006(5) 0.019(7) C16 0.049(5) 0.214(13) 0.041(4) -0.043(6) 0.001(4) 0.033(7) C17 0.065(7) 0.186(13) 0.052(5) -0.017(7) -0.004(5) 0.039(8) C18 0.062(5) 0.121(8) 0.039(4) -0.004(4) -0.001(4) 0.034(5) C19 0.033(3) 0.063(4) 0.028(3) -0.002(3) 0.012(2) 0.002(3) C20 0.022(4) 0.045(4) 0.037(4) 0.000 0.006(3) 0.000 C21 0.036(3) 0.050(4) 0.060(4) 0.002(3) 0.018(3) 0.000(3) C22 0.062(5) 0.045(4) 0.097(6) 0.014(4) 0.041(5) 0.000(3) C23 0.060(7) 0.040(5) 0.116(11) 0.000 0.040(7) 0.000 C24 0.027(4) 0.044(4) 0.034(4) 0.000 0.006(3) 0.000 C25 0.038(4) 0.042(7) 0.051(4) 0.004(6) 0.023(3) -0.003(6) C26 0.065(6) 0.079(7) 0.080(6) 0.004(5) 0.042(5) -0.018(5) C27 0.074(6) 0.094(7) 0.100(7) -0.003(5) 0.052(5) -0.022(5) C28 0.068(6) 0.088(7) 0.090(6) 0.008(6) 0.048(5) -0.014(6) C29 0.077(7) 0.091(9) 0.087(7) 0.011(6) 0.058(6) -0.002(6) C30 0.059(5) 0.067(8) 0.071(6) 0.004(6) 0.037(5) -0.008(6) C25' 0.038(4) 0.042(7) 0.051(4) 0.004(6) 0.023(3) -0.003(6) C26' 0.065(6) 0.079(7) 0.080(6) 0.004(5) 0.042(5) -0.018(5) C27' 0.074(6) 0.094(7) 0.100(7) -0.003(5) 0.052(5) -0.022(5) C28' 0.068(6) 0.088(7) 0.090(6) 0.008(6) 0.048(5) -0.014(6) C29' 0.077(7) 0.091(9) 0.087(7) 0.011(6) 0.058(6) -0.002(6) C30' 0.059(5) 0.067(8) 0.071(6) 0.004(6) 0.037(5) -0.008(6) C31 0.033(3) 0.068(4) 0.034(3) 0.005(3) 0.009(3) -0.006(3) Cl1 0.118(5) 0.141(6) 0.088(4) 0.036(4) 0.056(4) 0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd O5 2.344(4) . ? Gd O7 2.348(4) 2_756 ? Gd O2 2.389(4) . ? Gd O1 2.399(4) 2_756 ? Gd O8 2.424(5) . ? Gd O4 2.437(4) . ? Gd O3 2.437(4) . ? Gd O1 2.455(4) . ? Gd Ni 3.3778(8) 2_756 ? Gd Ni 3.4571(8) . ? Gd Gd 3.9673(5) 2_756 ? Ni N1' 1.973(18) . ? Ni O6 2.031(5) . ? Ni N2 2.039(7) . ? Ni O2 2.045(4) . ? Ni O1 2.052(4) . ? Ni O2 2.111(4) 2_756 ? Ni N1 2.206(15) . ? Ni Gd 3.3779(8) 2_756 ? O1 C6 1.434(7) . ? O1 Gd 2.399(4) 2_756 ? O2 C12 1.409(7) . ? O2 Ni 2.111(4) 2_756 ? O3 C19 1.272(7) . ? O4 C19 1.258(7) . ? O5 C24 1.256(6) . ? O6 C31 1.235(8) . ? O7 C31 1.258(8) . ? O7 Gd 2.348(4) 2_756 ? N2 C11 1.325(11) . ? N2 C7 1.348(10) . ? N1 C5 1.318(15) . ? N1 C1 1.35(2) . ? C1 C2 1.39(2) . ? C2 C3 1.32(2) . ? C3 C4 1.38(2) . ? C4 C5 1.38(2) . ? C5 C6 1.409(17) . ? N1' C5' 1.302(18) . ? N1' C1' 1.33(2) . ? C1' C2' 1.37(2) . ? C2' C3' 1.38(3) . ? C3' C4' 1.39(3) . ? C4' C5' 1.41(3) . ? C5' C6 1.712(19) . ? C7 C8 1.371(14) . ? C8 C9 1.371(17) . ? C9 C10 1.353(15) . ? C10 C11 1.398(11) . ? C11 C12 1.520(10) . ? C13 C14 1.359(12) . ? C13 C18 1.368(12) . ? C13 C19 1.492(9) . ? C14 C15 1.406(12) . ? C15 C16 1.359(17) . ? C16 C17 1.348(18) . ? C17 C18 1.410(12) . ? C20 C21 1.364(8) . ? C20 C21 1.364(8) 2_756 ? C20 C24 1.488(12) . ? C21 C22 1.391(10) . ? C22 C23 1.352(10) . ? C23 C22 1.352(10) 2_756 ? C24 O5 1.256(6) 2_756 ? C25 C30 1.27(4) . ? C25 C26 1.45(3) . ? C25 C31 1.53(3) . ? C26 C27 1.38(2) . ? C27 C28 1.40(3) . ? C28 C29 1.30(3) . ? C29 C30 1.41(4) . ? C25' C26' 1.29(3) . ? C25' C30' 1.46(5) . ? C25' C31 1.50(3) . ? C26' C27' 1.37(3) . ? C27' C28' 1.33(3) . ? C28' C29' 1.40(4) . ? C29' C30' 1.34(5) . ? Cl1 O11 1.20(3) . ? Cl1 O9 1.30(3) . ? Cl1 O12 1.40(5) . ? Cl1 O10 1.41(4) . ? O14 C32 1.353(13) . ? O15 C33 1.518(15) . ? O16 C34 1.499(19) . ? 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 O5 Gd O7 119.38(17) . 2_756 ? O5 Gd O2 142.96(15) . . ? O7 Gd O2 77.28(16) 2_756 . ? O5 Gd O1 77.49(14) . 2_756 ? O7 Gd O1 80.26(14) 2_756 2_756 ? O2 Gd O1 73.10(14) . 2_756 ? O5 Gd O8 72.31(17) . . ? O7 Gd O8 70.87(17) 2_756 . ? O2 Gd O8 142.58(16) . . ? O1 Gd O8 118.78(16) 2_756 . ? O5 Gd O4 131.77(15) . . ? O7 Gd O4 88.86(15) 2_756 . ? O2 Gd O4 76.89(15) . . ? O1 Gd O4 149.64(14) 2_756 . ? O8 Gd O4 83.25(17) . . ? O5 Gd O3 80.36(15) . . ? O7 Gd O3 133.61(15) 2_756 . ? O2 Gd O3 113.16(15) . . ? O1 Gd O3 145.89(14) 2_756 . ? O8 Gd O3 77.70(16) . . ? O4 Gd O3 53.68(14) . . ? O5 Gd O1 78.66(15) . . ? O7 Gd O1 140.20(14) 2_756 . ? O2 Gd O1 70.15(14) . . ? O1 Gd O1 69.01(15) 2_756 . ? O8 Gd O1 146.57(16) . . ? O4 Gd O1 104.92(14) . . ? O3 Gd O1 81.47(14) . . ? O5 Gd Ni 114.19(10) . 2_756 ? O7 Gd Ni 66.35(11) 2_756 2_756 ? O2 Gd Ni 38.32(10) . 2_756 ? O1 Gd Ni 36.95(10) 2_756 2_756 ? O8 Gd Ni 133.43(13) . 2_756 ? O4 Gd Ni 112.84(11) . 2_756 ? O3 Gd Ni 147.57(11) . 2_756 ? O1 Gd Ni 73.91(9) . 2_756 ? O5 Gd Ni 113.97(11) . . ? O7 Gd Ni 111.80(12) 2_756 . ? O2 Gd Ni 35.31(10) . . ? O1 Gd Ni 72.94(10) 2_756 . ? O8 Gd Ni 168.17(13) . . ? O4 Gd Ni 85.26(12) . . ? O3 Gd Ni 93.19(11) . . ? O1 Gd Ni 35.81(9) . . ? Ni Gd Ni 54.64(3) 2_756 . ? O5 Gd Gd 68.15(10) . 2_756 ? O7 Gd Gd 114.96(11) 2_756 2_756 ? O2 Gd Gd 74.83(10) . 2_756 ? O1 Gd Gd 35.65(9) 2_756 2_756 ? O8 Gd Gd 136.77(13) . 2_756 ? O4 Gd Gd 137.22(12) . 2_756 ? O3 Gd Gd 111.35(10) . 2_756 ? O1 Gd Gd 34.72(9) . 2_756 ? Ni Gd Gd 55.454(15) 2_756 2_756 ? Ni Gd Gd 53.592(14) . 2_756 ? N1' Ni O6 86.8(7) . . ? N1' Ni N2 89.2(5) . . ? O6 Ni N2 95.5(3) . . ? N1' Ni O2 102.3(7) . . ? O6 Ni O2 170.2(2) . . ? N2 Ni O2 81.0(2) . . ? N1' Ni O1 85.6(4) . . ? O6 Ni O1 99.01(19) . . ? N2 Ni O1 164.2(2) . . ? O2 Ni O1 85.61(16) . . ? N1' Ni O2 170.7(5) . 2_756 ? O6 Ni O2 89.68(18) . 2_756 ? N2 Ni O2 99.7(2) . 2_756 ? O2 Ni O2 81.93(17) . 2_756 ? O1 Ni O2 86.44(15) . 2_756 ? N1' Ni N1 11.9(6) . . ? O6 Ni N1 84.8(5) . . ? N2 Ni N1 101.1(4) . . ? O2 Ni N1 104.8(5) . . ? O1 Ni N1 74.4(4) . . ? O2 Ni N1 158.9(4) 2_756 . ? N1' Ni Gd 126.3(4) . 2_756 ? O6 Ni Gd 83.74(14) . 2_756 ? N2 Ni Gd 144.2(2) . 2_756 ? O2 Ni Gd 93.72(11) . 2_756 ? O1 Ni Gd 44.63(11) . 2_756 ? O2 Ni Gd 44.57(11) 2_756 2_756 ? N1 Ni Gd 114.4(4) . 2_756 ? N1' Ni Gd 87.4(6) . . ? O6 Ni Gd 143.32(16) . . ? N2 Ni Gd 120.6(2) . . ? O2 Ni Gd 42.49(11) . . ? O1 Ni Gd 44.41(11) . . ? O2 Ni Gd 90.31(11) 2_756 . ? N1 Ni Gd 82.2(5) . . ? Gd Ni Gd 70.953(17) 2_756 . ? C6 O1 Ni 109.8(4) . . ? C6 O1 Gd 117.7(4) . 2_756 ? Ni O1 Gd 98.42(15) . 2_756 ? C6 O1 Gd 118.0(4) . . ? Ni O1 Gd 99.78(16) . . ? Gd O1 Gd 109.63(15) 2_756 . ? C12 O2 Ni 111.3(4) . . ? C12 O2 Ni 116.0(4) . 2_756 ? Ni O2 Ni 98.06(17) . 2_756 ? C12 O2 Gd 127.5(4) . . ? Ni O2 Gd 102.19(17) . . ? Ni O2 Gd 97.10(16) 2_756 . ? C19 O3 Gd 92.4(4) . . ? C19 O4 Gd 92.8(4) . . ? C24 O5 Gd 139.4(4) . . ? C31 O6 Ni 126.7(4) . . ? C31 O7 Gd 136.7(4) . 2_756 ? C11 N2 C7 119.2(8) . . ? C11 N2 Ni 114.4(5) . . ? C7 N2 Ni 126.4(7) . . ? C5 N1 C1 118.0(14) . . ? C5 N1 Ni 114.4(12) . . ? C1 N1 Ni 126.3(10) . . ? N1 C1 C2 121.6(14) . . ? C3 C2 C1 118.7(15) . . ? C2 C3 C4 121.7(15) . . ? C3 C4 C5 116.7(14) . . ? N1 C5 C4 123.2(15) . . ? N1 C5 C6 112.5(14) . . ? C4 C5 C6 124.3(12) . . ? C5' N1' C1' 117.6(17) . . ? C5' N1' Ni 107.6(14) . . ? C1' N1' Ni 133.0(11) . . ? N1' C1' C2' 123.4(16) . . ? C1' C2' C3' 118.7(16) . . ? C2' C3' C4' 119.4(17) . . ? C3' C4' C5' 116.2(16) . . ? N1' C5' C4' 124.6(18) . . ? N1' C5' C6 121.9(16) . . ? C4' C5' C6 113.5(13) . . ? C5 C6 O1 116.6(8) . . ? C5 C6 C5' 15.5(9) . . ? O1 C6 C5' 102.6(8) . . ? N2 C7 C8 121.7(11) . . ? C7 C8 C9 118.7(10) . . ? C10 C9 C8 120.3(10) . . ? C9 C10 C11 118.6(10) . . ? N2 C11 C10 121.5(8) . . ? N2 C11 C12 115.9(6) . . ? C10 C11 C12 122.4(8) . . ? O2 C12 C11 111.6(6) . . ? C14 C13 C18 118.9(7) . . ? C14 C13 C19 121.0(7) . . ? C18 C13 C19 120.0(7) . . ? C13 C14 C15 119.7(10) . . ? C16 C15 C14 120.5(11) . . ? C17 C16 C15 120.8(9) . . ? C16 C17 C18 118.5(11) . . ? C13 C18 C17 121.5(10) . . ? O4 C19 O3 120.9(5) . . ? O4 C19 C13 119.6(6) . . ? O3 C19 C13 119.4(6) . . ? C21 C20 C21 119.2(9) . 2_756 ? C21 C20 C24 120.4(4) . . ? C21 C20 C24 120.4(4) 2_756 . ? C20 C21 C22 120.6(8) . . ? C23 C22 C21 118.8(8) . . ? C22 C23 C22 122.0(10) . 2_756 ? O5 C24 O5 124.7(8) . 2_756 ? O5 C24 C20 117.6(4) . . ? O5 C24 C20 117.6(4) 2_756 . ? C30 C25 C26 119(3) . . ? C30 C25 C31 125(2) . . ? C26 C25 C31 116(2) . . ? C27 C26 C25 119(2) . . ? C26 C27 C28 119.0(18) . . ? C29 C28 C27 119(2) . . ? C28 C29 C30 123(3) . . ? C25 C30 C29 121(3) . . ? C26' C25' C30' 118(3) . . ? C26' C25' C31 124(3) . . ? C30' C25' C31 118(2) . . ? C25' C26' C27' 121(3) . . ? C28' C27' C26' 121(2) . . ? C27' C28' C29' 121(2) . . ? C30' C29' C28' 117(3) . . ? C29' C30' C25' 121(3) . . ? O6 C31 O7 126.1(6) . . ? O6 C31 C25' 111.4(11) . . ? O7 C31 C25' 122.2(12) . . ? O6 C31 C25 121.4(10) . . ? O7 C31 C25 112.1(10) . . ? C25' C31 C25 15.8(10) . . ? O11 Cl1 O9 120(2) . . ? O11 Cl1 O12 102(2) . . ? O9 Cl1 O12 86(2) . . ? O11 Cl1 O10 115(2) . . ? O9 Cl1 O10 107(2) . . ? O12 Cl1 O10 125(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.655 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.288 data_ic15698 _database_code_depnum_ccdc_archive 'CCDC 910497' #TrackingRef '16242_web_deposit_cif_file_0_En-CheYang_1355729215.compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H75 Cl Gd2 N4 O26 Zn2' _chemical_formula_weight 1796.97 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.1184(10) _cell_length_b 24.0124(11) _cell_length_c 17.7431(8) _cell_angle_alpha 90.00 _cell_angle_beta 121.1377(11) _cell_angle_gamma 90.00 _cell_volume 7701.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4442 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.21 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 2.426 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4082 _exptl_absorpt_correction_T_max 0.5604 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24818 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8837 _reflns_number_gt 6303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure restrains are applyied for the atoms of N1, N1', C1-C5, C1'-C5', C13-C18, C13'-C18', C25-C30 and C25'-C30' by ISOR. The perchlorate anion is used the SADI restrains to be a regular tetrahedron. ; _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^)+(0.1021P)^2^+23.0714P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8837 _refine_ls_number_parameters 483 _refine_ls_number_restraints 244 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1830 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.004 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 Gd Gd 1.008604(15) 0.668403(14) 0.644103(19) 0.04049(13) Uani 1 1 d . . . Zn Zn 0.90977(5) 0.57152(4) 0.69141(6) 0.0581(3) Uani 1 1 d . . . O1 O 0.9239(2) 0.65804(19) 0.6984(3) 0.0439(11) Uani 1 1 d . . . O2 O 0.9996(3) 0.5729(2) 0.6712(3) 0.0497(11) Uani 1 1 d . . . O3 O 0.8958(3) 0.7037(2) 0.5165(3) 0.0537(12) Uani 1 1 d . . . O4 O 0.9434(3) 0.6281(2) 0.4968(3) 0.0613(14) Uani 1 1 d . . . O5 O 1.0081(3) 0.7591(2) 0.6933(3) 0.0553(12) Uani 1 1 d . . . O6 O 0.8382(3) 0.5622(3) 0.7361(4) 0.0713(17) Uani 1 1 d . A . O7 O 0.8804(2) 0.6313(2) 0.8347(3) 0.0564(13) Uani 1 1 d . . . O8 O 1.0576(3) 0.7308(3) 0.5781(4) 0.0782(17) Uani 1 1 d . . . H8A H 1.0793 0.7228 0.5492 0.117 Uiso 1 1 d R A . H8B H 1.0176 0.7475 0.5447 0.117 Uiso 1 1 d R . . N2 N 0.9100(5) 0.4887(3) 0.6566(5) 0.082(2) Uani 1 1 d . A . N1 N 0.8106(8) 0.6097(7) 0.5682(10) 0.046(3) Uani 0.527(5) 1 d PU A 1 C1 C 0.7585(9) 0.5799(7) 0.4984(11) 0.057(3) Uani 0.527(5) 1 d PU A 1 H1 H 0.7680 0.5422 0.4914 0.068 Uiso 0.527(5) 1 calc PR A 1 C2 C 0.6914(9) 0.6039(8) 0.4374(12) 0.060(3) Uani 0.527(5) 1 d PU A 1 H2 H 0.6571 0.5838 0.3862 0.072 Uiso 0.527(5) 1 calc PR A 1 C3 C 0.6738(11) 0.6603(8) 0.4520(13) 0.078(4) Uani 0.527(5) 1 d PU A 1 H3 H 0.6258 0.6758 0.4160 0.093 Uiso 0.527(5) 1 calc PR A 1 C4 C 0.7290(8) 0.6895(7) 0.5191(11) 0.056(3) Uani 0.527(5) 1 d PU A 1 H4 H 0.7228 0.7278 0.5272 0.067 Uiso 0.527(5) 1 calc PR A 1 C5 C 0.7953(9) 0.6623(7) 0.5762(12) 0.048(3) Uani 0.527(5) 1 d PU A 1 N1' N 0.8231(9) 0.5866(6) 0.5718(12) 0.046(3) Uani 0.473(5) 1 d PU A 2 C1' C 0.7781(9) 0.5514(8) 0.5030(12) 0.057(3) Uani 0.473(5) 1 d PU A 2 H1' H 0.7936 0.5142 0.5027 0.068 Uiso 0.473(5) 1 calc PR A 2 C2' C 0.7120(9) 0.5696(8) 0.4359(11) 0.060(3) Uani 0.473(5) 1 d PU A 2 H2' H 0.6823 0.5460 0.3872 0.072 Uiso 0.473(5) 1 calc PR A 2 C3' C 0.6862(13) 0.6269(12) 0.4390(17) 0.078(4) Uani 0.473(5) 1 d PU A 2 H3' H 0.6389 0.6397 0.3943 0.093 Uiso 0.473(5) 1 calc PR A 2 C4' C 0.7320(9) 0.6601(8) 0.5072(12) 0.056(3) Uani 0.473(5) 1 d PU A 2 H4' H 0.7185 0.6975 0.5099 0.067 Uiso 0.473(5) 1 calc PR A 2 C5' C 0.8016(10) 0.6379(11) 0.5755(14) 0.048(3) Uani 0.473(5) 1 d PU A 2 C6 C 0.8537(4) 0.6869(4) 0.6521(5) 0.063(2) Uani 1 1 d U . . H6A H 0.8368 0.6928 0.6942 0.075 Uiso 0.527(5) 1 calc PR A 1 H6B H 0.8627 0.7241 0.6356 0.075 Uiso 0.527(5) 1 calc PR A 1 H6C H 0.8556 0.7224 0.6248 0.075 Uiso 0.473(5) 1 d PR A 2 H6D H 0.8337 0.6940 0.6910 0.075 Uiso 0.473(5) 1 d PR A 2 C7 C 0.8710(8) 0.4471(5) 0.6630(8) 0.113(4) Uani 1 1 d . . . H7 H 0.8402 0.4544 0.6862 0.135 Uiso 1 1 calc R A . C8 C 0.8746(11) 0.3941(6) 0.6368(11) 0.154(7) Uani 1 1 d . A . H8 H 0.8473 0.3646 0.6424 0.185 Uiso 1 1 calc R . . C9 C 0.9178(12) 0.3849(6) 0.6031(12) 0.162(8) Uani 1 1 d . . . H9 H 0.9186 0.3487 0.5822 0.194 Uiso 1 1 calc R A . C10 C 0.9602(8) 0.4251(4) 0.5976(7) 0.106(4) Uani 1 1 d . A . H10 H 0.9919 0.4178 0.5756 0.127 Uiso 1 1 calc R . . C11 C 0.9543(6) 0.4785(4) 0.6264(6) 0.079(3) Uani 1 1 d . . . C12 C 0.9971(5) 0.5266(4) 0.6210(6) 0.069(2) Uani 1 1 d . A . H12A H 1.0483 0.5143 0.6417 0.083 Uiso 1 1 calc R . . H12B H 0.9742 0.5381 0.5587 0.083 Uiso 1 1 calc R . . C13 C 0.8275(12) 0.6503(6) 0.3789(14) 0.044(3) Uani 0.527(5) 1 d PU A 1 C14 C 0.8112(10) 0.6000(8) 0.3372(12) 0.067(4) Uani 0.527(5) 1 d PU A 1 H14 H 0.8426 0.5689 0.3650 0.080 Uiso 0.527(5) 1 calc PR A 1 C15 C 0.7496(11) 0.5945(9) 0.2554(12) 0.075(4) Uani 0.527(5) 1 d PU A 1 H15 H 0.7416 0.5595 0.2268 0.090 Uiso 0.527(5) 1 calc PR A 1 C16 C 0.7028(11) 0.6323(8) 0.2151(13) 0.069(4) Uani 0.527(5) 1 d PU A 1 H16 H 0.6646 0.6271 0.1555 0.082 Uiso 0.527(5) 1 calc PR A 1 C17 C 0.7073(15) 0.6828(12) 0.2593(18) 0.101(6) Uani 0.527(5) 1 d PU A 1 H17 H 0.6697 0.7104 0.2329 0.121 Uiso 0.527(5) 1 calc PR A 1 C18 C 0.7704(11) 0.6903(9) 0.3447(13) 0.071(4) Uani 0.527(5) 1 d PU A 1 H18 H 0.7741 0.7221 0.3787 0.085 Uiso 0.527(5) 1 calc PR A 1 C13' C 0.8301(13) 0.6707(7) 0.3752(16) 0.044(3) Uani 0.473(5) 1 d PU A 2 C14' C 0.8183(12) 0.6253(9) 0.3204(14) 0.067(4) Uani 0.473(5) 1 d PU A 2 H14' H 0.8524 0.5952 0.3412 0.080 Uiso 0.473(5) 1 calc PR A 2 C15' C 0.7564(13) 0.6240(10) 0.2345(15) 0.075(4) Uani 0.473(5) 1 d PU A 2 H15' H 0.7500 0.5933 0.1973 0.090 Uiso 0.473(5) 1 calc PR A 2 C16' C 0.7082(12) 0.6633(9) 0.2052(15) 0.069(4) Uani 0.473(5) 1 d PU A 2 H16' H 0.6621 0.6587 0.1519 0.082 Uiso 0.473(5) 1 calc PR A 2 C17' C 0.7224(16) 0.7062(13) 0.247(2) 0.101(6) Uani 0.473(5) 1 d PU A 2 H17' H 0.6908 0.7376 0.2221 0.121 Uiso 0.473(5) 1 calc PR A 2 C18' C 0.7888(12) 0.7095(10) 0.3351(15) 0.071(4) Uani 0.473(5) 1 d PU A 2 H18' H 0.8006 0.7447 0.3635 0.085 Uiso 0.473(5) 1 calc PR A 2 C19 C 0.8934(4) 0.6639(3) 0.4680(4) 0.0507(18) Uani 1 1 d . A . C20 C 1.0000 0.8460(4) 0.7500 0.051(3) Uani 1 2 d S . . C21 C 1.0181(4) 0.8745(3) 0.6976(6) 0.059(2) Uani 1 1 d . A . H21 H 1.0305 0.8545 0.6608 0.071 Uiso 1 1 calc R . . C22 C 1.0186(5) 0.9320(4) 0.6970(7) 0.078(3) Uani 1 1 d . . . H22 H 1.0316 0.9517 0.6605 0.094 Uiso 1 1 calc R A . C23 C 1.0000 0.9602(5) 0.7500 0.083(4) Uani 1 2 d S . . H23 H 1.0000 0.9998 0.7500 0.099 Uiso 1 2 calc SR . . C24 C 1.0000 0.7835(4) 0.7500 0.049(2) Uani 1 2 d S . . C25 C 0.7716(12) 0.5891(7) 0.8080(15) 0.049(3) Uani 0.527(5) 1 d PU A 1 C26 C 0.7043(10) 0.5639(9) 0.7413(14) 0.082(4) Uani 0.527(5) 1 d PU A 1 H26 H 0.7002 0.5520 0.6880 0.099 Uiso 0.527(5) 1 calc PR A 1 C27 C 0.6463(12) 0.5569(10) 0.7531(16) 0.097(5) Uani 0.527(5) 1 d PU A 1 H27 H 0.6010 0.5420 0.7071 0.117 Uiso 0.527(5) 1 calc PR A 1 C28 C 0.6535(11) 0.5715(9) 0.8321(14) 0.079(4) Uani 0.527(5) 1 d PU A 1 H28 H 0.6162 0.5637 0.8453 0.095 Uiso 0.527(5) 1 calc PR A 1 C29 C 0.7125(17) 0.5958(12) 0.886(2) 0.091(5) Uani 0.527(5) 1 d PU A 1 H29 H 0.7175 0.6062 0.9402 0.110 Uiso 0.527(5) 1 calc PR A 1 C30 C 0.7730(16) 0.6096(10) 0.875(2) 0.074(4) Uani 0.527(5) 1 d PU A 1 H30 H 0.8123 0.6329 0.9160 0.089 Uiso 0.527(5) 1 calc PR A 1 C25' C 0.7814(13) 0.5700(8) 0.8154(17) 0.049(3) Uani 0.473(5) 1 d PDU A 2 C26' C 0.7397(10) 0.5294(9) 0.7809(14) 0.082(4) Uani 0.473(5) 1 d PDU A 2 H26' H 0.7430 0.5100 0.7364 0.099 Uiso 0.473(5) 1 calc PR A 2 C27' C 0.6911(12) 0.5108(11) 0.8007(16) 0.097(5) Uani 0.473(5) 1 d PDU A 2 H27' H 0.6643 0.4775 0.7743 0.117 Uiso 0.473(5) 1 calc PR A 2 C28' C 0.6799(12) 0.5380(10) 0.8567(15) 0.079(4) Uani 0.473(5) 1 d PDU A 2 H28' H 0.6392 0.5286 0.8631 0.095 Uiso 0.473(5) 1 calc PR A 2 C29' C 0.7259(19) 0.5793(14) 0.905(2) 0.091(5) Uani 0.473(5) 1 d PDU A 2 H29' H 0.7214 0.5990 0.9484 0.110 Uiso 0.473(5) 1 calc PR A 2 C30' C 0.7794(18) 0.5907(11) 0.887(2) 0.074(4) Uani 0.473(5) 1 d PDU A 2 H30' H 0.8185 0.6147 0.9257 0.089 Uiso 0.473(5) 1 calc PR A 2 C31 C 0.8363(4) 0.5916(4) 0.7923(5) 0.059(2) Uani 1 1 d . . . Cl1 Cl 0.0962(6) 0.9580(5) 0.5108(5) 0.168(4) Uani 0.50 1 d PD B 1 O9 O 0.077(2) 0.9212(12) 0.554(2) 0.265(17) Uiso 0.50 1 d PD B 1 O10 O 0.0511(18) 0.9509(15) 0.4239(16) 0.30(2) Uiso 0.50 1 d PD B 1 O11 O 0.1667(15) 0.9542(16) 0.536(2) 0.37(2) Uiso 0.50 1 d PD B 1 O12 O 0.083(2) 1.0099(12) 0.534(2) 0.37(2) Uiso 0.50 1 d PD B 1 O13 O 0.017(3) 0.9273(18) 0.468(3) 0.278(18) Uiso 0.50 1 d P C 2 O14 O 0.1897(6) 0.7707(5) 0.4944(7) 0.150(4) Uiso 1 1 d D . . C32 C 0.1619(13) 0.7345(10) 0.5339(16) 0.223(10) Uiso 1 1 d D . . O15 O 0.9945(13) 0.8282(8) 0.4930(14) 0.263(9) Uiso 1 1 d D . . C33 C 0.9132(17) 0.8455(16) 0.439(3) 0.35(2) Uiso 1 1 d D . . O16 O 0.075(3) 0.7493(19) 0.216(3) 0.34(2) Uiso 0.50 1 d PD D -1 C34 C 0.032(3) 0.782(2) 0.246(5) 0.28(3) Uiso 0.50 1 d PD D -1 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 Gd 0.03004(17) 0.0503(2) 0.03271(19) 0.00080(14) 0.01027(13) 0.00155(13) Zn 0.0567(5) 0.0671(6) 0.0546(5) -0.0187(4) 0.0317(4) -0.0235(4) O1 0.027(2) 0.056(3) 0.035(2) -0.002(2) 0.0059(18) 0.0018(18) O2 0.056(3) 0.049(3) 0.050(3) -0.006(2) 0.032(2) -0.003(2) O3 0.048(3) 0.063(3) 0.036(3) -0.002(2) 0.012(2) 0.014(2) O4 0.052(3) 0.070(4) 0.042(3) -0.012(3) 0.011(2) 0.017(3) O5 0.066(3) 0.051(3) 0.041(3) -0.005(2) 0.022(2) -0.005(2) O6 0.065(3) 0.094(5) 0.062(4) -0.023(3) 0.038(3) -0.034(3) O7 0.036(2) 0.078(4) 0.051(3) -0.005(3) 0.020(2) -0.011(2) O8 0.073(4) 0.091(5) 0.078(4) 0.014(3) 0.044(3) -0.001(3) N2 0.122(7) 0.075(5) 0.069(5) -0.028(4) 0.064(5) -0.043(5) N1 0.039(4) 0.044(6) 0.043(4) -0.003(5) 0.013(3) 0.000(5) C1 0.050(5) 0.048(6) 0.052(5) -0.011(5) 0.012(4) -0.013(4) C2 0.043(5) 0.056(6) 0.056(5) -0.013(5) 0.008(4) -0.011(5) C3 0.058(6) 0.071(7) 0.075(6) -0.006(6) 0.013(5) 0.001(5) C4 0.036(4) 0.055(6) 0.056(5) -0.001(5) 0.009(4) 0.003(5) C5 0.031(4) 0.059(6) 0.050(4) 0.018(5) 0.018(3) 0.011(5) N1' 0.039(4) 0.044(6) 0.043(4) -0.003(5) 0.013(3) 0.000(5) C1' 0.050(5) 0.048(6) 0.052(5) -0.011(5) 0.012(4) -0.013(4) C2' 0.043(5) 0.056(6) 0.056(5) -0.013(5) 0.008(4) -0.011(5) C3' 0.058(6) 0.071(7) 0.075(6) -0.006(6) 0.013(5) 0.001(5) C4' 0.036(4) 0.055(6) 0.056(5) -0.001(5) 0.009(4) 0.003(5) C5' 0.031(4) 0.059(6) 0.050(4) 0.018(5) 0.018(3) 0.011(5) C6 0.026(3) 0.110(6) 0.040(4) -0.005(4) 0.008(3) 0.012(3) C7 0.158(12) 0.092(8) 0.098(8) -0.044(7) 0.072(8) -0.076(8) C8 0.24(2) 0.089(10) 0.129(13) -0.038(9) 0.088(13) -0.094(12) C9 0.25(2) 0.082(10) 0.166(17) -0.059(10) 0.118(16) -0.056(12) C10 0.164(12) 0.058(6) 0.079(7) -0.032(5) 0.052(8) -0.019(7) C11 0.114(8) 0.065(6) 0.063(6) -0.015(5) 0.048(6) -0.024(5) C12 0.096(7) 0.059(5) 0.064(5) -0.005(4) 0.050(5) 0.002(4) C13 0.043(4) 0.039(8) 0.038(4) -0.006(6) 0.013(3) 0.004(6) C14 0.064(5) 0.063(7) 0.058(6) -0.008(5) 0.021(4) -0.002(5) C15 0.075(6) 0.077(7) 0.065(6) -0.014(5) 0.030(5) -0.003(5) C16 0.063(5) 0.071(7) 0.057(5) -0.005(6) 0.021(4) -0.002(6) C17 0.092(8) 0.104(9) 0.091(7) 0.007(6) 0.036(5) -0.004(6) C18 0.066(6) 0.075(7) 0.055(5) 0.007(5) 0.019(4) -0.001(5) C13' 0.043(4) 0.039(8) 0.038(4) -0.006(6) 0.013(3) 0.004(6) C14' 0.064(5) 0.063(7) 0.058(6) -0.008(5) 0.021(4) -0.002(5) C15' 0.075(6) 0.077(7) 0.065(6) -0.014(5) 0.030(5) -0.003(5) C16' 0.063(5) 0.071(7) 0.057(5) -0.005(6) 0.021(4) -0.002(6) C17' 0.092(8) 0.104(9) 0.091(7) 0.007(6) 0.036(5) -0.004(6) C18' 0.066(6) 0.075(7) 0.055(5) 0.007(5) 0.019(4) -0.001(5) C19 0.041(4) 0.073(5) 0.030(3) 0.000(3) 0.013(3) 0.001(3) C20 0.025(4) 0.056(6) 0.047(6) 0.000 0.001(4) 0.000 C21 0.042(4) 0.051(5) 0.071(5) 0.002(4) 0.019(4) 0.001(3) C22 0.064(5) 0.059(6) 0.109(8) 0.012(5) 0.043(5) -0.007(4) C23 0.059(7) 0.048(7) 0.130(13) 0.000 0.041(8) 0.000 C24 0.039(5) 0.055(6) 0.038(5) 0.000 0.009(4) 0.000 C25 0.044(5) 0.050(8) 0.056(5) 0.004(6) 0.028(4) -0.004(6) C26 0.073(6) 0.091(7) 0.090(7) 0.003(5) 0.048(5) -0.017(5) C27 0.091(7) 0.107(8) 0.106(7) -0.006(6) 0.060(6) -0.019(5) C28 0.072(6) 0.084(7) 0.084(6) 0.004(6) 0.041(5) -0.008(5) C29 0.088(7) 0.103(9) 0.099(8) 0.008(6) 0.059(6) -0.001(6) C30 0.064(5) 0.082(9) 0.087(7) 0.006(6) 0.047(5) -0.006(6) C25' 0.044(5) 0.050(8) 0.056(5) 0.004(6) 0.028(4) -0.004(6) C26' 0.073(6) 0.091(7) 0.090(7) 0.003(5) 0.048(5) -0.017(5) C27' 0.091(7) 0.107(8) 0.106(7) -0.006(6) 0.060(6) -0.019(5) C28' 0.072(6) 0.084(7) 0.084(6) 0.004(6) 0.041(5) -0.008(5) C29' 0.088(7) 0.103(9) 0.099(8) 0.008(6) 0.059(6) -0.001(6) C30' 0.064(5) 0.082(9) 0.087(7) 0.006(6) 0.047(5) -0.006(6) C31 0.039(4) 0.084(6) 0.051(4) 0.004(4) 0.020(3) -0.008(4) Cl1 0.178(9) 0.236(11) 0.097(5) 0.058(6) 0.076(6) 0.033(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 Gd O7 2.348(5) 2_756 ? Gd O5 2.349(5) . ? Gd O2 2.372(5) . ? Gd O1 2.405(4) 2_756 ? Gd O8 2.438(6) . ? Gd O3 2.437(5) . ? Gd O4 2.438(5) . ? Gd O1 2.444(5) . ? Gd Zn 3.4203(9) 2_756 ? Gd Zn 3.5049(9) . ? Gd Gd 3.9581(6) 2_756 ? Zn N1' 1.992(16) . ? Zn O6 2.049(5) . ? Zn O1 2.093(5) . ? Zn N2 2.083(8) . ? Zn O2 2.105(5) . ? Zn O2 2.187(5) 2_756 ? Zn N1 2.295(15) . ? Zn Gd 3.4203(9) 2_756 ? O1 C6 1.446(8) . ? O1 Gd 2.405(4) 2_756 ? O2 C12 1.408(10) . ? O2 Zn 2.187(5) 2_756 ? O3 C19 1.269(9) . ? O4 C19 1.249(9) . ? O5 C24 1.251(7) . ? O6 C31 1.239(10) . ? O7 C31 1.272(9) . ? O7 Gd 2.348(4) 2_756 ? N2 C11 1.320(12) . ? N2 C7 1.335(12) . ? N1 C5 1.330(19) . ? N1 C1 1.36(2) . ? C1 C2 1.39(2) . ? C2 C3 1.46(3) . ? C3 C4 1.35(2) . ? C4 C5 1.40(2) . ? C5 C6 1.403(19) . ? N1' C5' 1.33(2) . ? N1' C1' 1.38(2) . ? C1' C2' 1.36(2) . ? C2' C3' 1.49(3) . ? C3' C4' 1.35(3) . ? C4' C5' 1.44(2) . ? C5' C6 1.70(3) . ? C7 C8 1.370(19) . ? C8 C9 1.34(2) . ? C9 C10 1.355(19) . ? C10 C11 1.409(13) . ? C11 C12 1.500(12) . ? C13 C14 1.36(3) . ? C13 C18 1.41(3) . ? C13 C19 1.50(2) . ? C14 C15 1.36(3) . ? C15 C16 1.26(3) . ? C16 C17 1.42(4) . ? C17 C18 1.42(3) . ? C13' C18' 1.22(3) . ? C13' C14' 1.40(3) . ? C13' C19 1.50(2) . ? C14' C15' 1.40(3) . ? C15' C16' 1.28(3) . ? C16' C17' 1.21(4) . ? C17' C18' 1.47(4) . ? C20 C21 1.358(10) . ? C20 C21 1.358(10) 2_756 ? C20 C24 1.501(15) . ? C21 C22 1.382(12) . ? C22 C23 1.371(12) . ? C23 C22 1.371(12) 2_756 ? C24 O5 1.250(7) 2_756 ? C25 C30 1.28(4) . ? C25 C26 1.43(3) . ? C25 C31 1.53(3) . ? C26 C27 1.36(3) . ? C27 C28 1.38(3) . ? C28 C29 1.25(4) . ? C29 C30 1.42(5) . ? C25' C26' 1.24(3) . ? C25' C30' 1.38(5) . ? C25' C31 1.51(3) . ? C26' C27' 1.32(3) . ? C27' C28' 1.31(3) . ? C28' C29' 1.34(4) . ? C29' C30' 1.36(5) . ? Cl1 O11 1.32(2) . ? Cl1 O9 1.36(2) . ? Cl1 O10 1.34(2) . ? Cl1 O12 1.38(2) . ? O14 C32 1.420(16) . ? O15 C33 1.528(19) . ? O16 C34 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Gd O5 119.26(19) 2_756 . ? O7 Gd O2 77.18(18) 2_756 . ? O5 Gd O2 143.66(17) . . ? O7 Gd O1 80.30(16) 2_756 2_756 ? O5 Gd O1 77.19(16) . 2_756 ? O2 Gd O1 74.09(16) . 2_756 ? O7 Gd O8 71.0(2) 2_756 . ? O5 Gd O8 72.1(2) . . ? O2 Gd O8 142.22(19) . . ? O1 Gd O8 118.55(19) 2_756 . ? O7 Gd O3 134.09(17) 2_756 . ? O5 Gd O3 80.36(17) . . ? O2 Gd O3 112.47(18) . . ? O1 Gd O3 145.37(16) 2_756 . ? O8 Gd O3 78.1(2) . . ? O7 Gd O4 89.12(17) 2_756 . ? O5 Gd O4 131.15(18) . . ? O2 Gd O4 76.89(18) . . ? O1 Gd O4 150.64(17) 2_756 . ? O8 Gd O4 82.7(2) . . ? O3 Gd O4 53.36(16) . . ? O7 Gd O1 140.46(17) 2_756 . ? O5 Gd O1 78.63(17) . . ? O2 Gd O1 70.72(16) . . ? O1 Gd O1 69.30(16) 2_756 . ? O8 Gd O1 146.24(19) . . ? O3 Gd O1 80.71(16) . . ? O4 Gd O1 105.05(17) . . ? O7 Gd Zn 65.42(13) 2_756 2_756 ? O5 Gd Zn 114.27(12) . 2_756 ? O2 Gd Zn 39.38(12) . 2_756 ? O1 Gd Zn 37.22(11) 2_756 2_756 ? O8 Gd Zn 132.53(15) . 2_756 ? O3 Gd Zn 148.03(13) . 2_756 ? O4 Gd Zn 113.63(13) . 2_756 ? O1 Gd Zn 75.11(10) . 2_756 ? O7 Gd Zn 112.20(14) 2_756 . ? O5 Gd Zn 114.12(13) . . ? O2 Gd Zn 35.84(11) . . ? O1 Gd Zn 73.84(11) 2_756 . ? O8 Gd Zn 167.55(15) . . ? O3 Gd Zn 92.07(13) . . ? O4 Gd Zn 85.25(15) . . ? O1 Gd Zn 35.91(11) . . ? Zn Gd Zn 56.22(3) 2_756 . ? O7 Gd Gd 114.93(12) 2_756 2_756 ? O5 Gd Gd 68.09(12) . 2_756 ? O2 Gd Gd 75.59(11) . 2_756 ? O1 Gd Gd 35.62(11) 2_756 2_756 ? O8 Gd Gd 136.59(15) . 2_756 ? O3 Gd Gd 110.89(12) . 2_756 ? O4 Gd Gd 137.71(14) . 2_756 ? O1 Gd Gd 34.96(10) . 2_756 ? Zn Gd Gd 56.153(16) 2_756 2_756 ? Zn Gd Gd 54.143(15) . 2_756 ? N1' Zn O6 88.7(6) . . ? N1' Zn O1 84.7(5) . . ? O6 Zn O1 101.3(2) . . ? N1' Zn N2 89.9(5) . . ? O6 Zn N2 97.2(3) . . ? O1 Zn N2 160.6(2) . . ? N1' Zn O2 103.2(6) . . ? O6 Zn O2 167.7(2) . . ? O1 Zn O2 83.21(18) . . ? N2 Zn O2 79.9(3) . . ? N1' Zn O2 167.8(5) . 2_756 ? O6 Zn O2 88.0(2) . 2_756 ? O1 Zn O2 84.47(17) . 2_756 ? N2 Zn O2 102.1(3) . 2_756 ? O2 Zn O2 81.0(2) . 2_756 ? N1' Zn N1 14.0(5) . . ? O6 Zn N1 85.4(5) . . ? O1 Zn N1 72.1(4) . . ? N2 Zn N1 103.8(5) . . ? O2 Zn N1 106.9(5) . . ? O2 Zn N1 153.8(4) 2_756 . ? N1' Zn Gd 124.4(4) . 2_756 ? O6 Zn Gd 83.73(16) . 2_756 ? O1 Zn Gd 44.02(12) . 2_756 ? N2 Zn Gd 145.6(3) . 2_756 ? O2 Zn Gd 91.95(13) . 2_756 ? O2 Zn Gd 43.48(13) 2_756 2_756 ? N1 Zn Gd 110.5(4) . 2_756 ? N1' Zn Gd 87.5(5) . . ? O6 Zn Gd 144.51(19) . . ? O1 Zn Gd 43.22(13) . . ? N2 Zn Gd 118.0(2) . . ? O2 Zn Gd 41.27(13) . . ? O2 Zn Gd 88.33(13) 2_756 . ? N1 Zn Gd 82.5(4) . . ? Gd Zn Gd 69.704(19) 2_756 . ? C6 O1 Zn 111.6(5) . . ? C6 O1 Gd 115.3(4) . 2_756 ? Zn O1 Gd 98.76(18) . 2_756 ? C6 O1 Gd 118.1(4) . . ? Zn O1 Gd 100.86(18) . . ? Gd O1 Gd 109.42(16) 2_756 . ? C12 O2 Zn 110.7(5) . . ? C12 O2 Zn 114.8(5) . 2_756 ? Zn O2 Zn 99.0(2) . 2_756 ? C12 O2 Gd 128.0(5) . . ? Zn O2 Gd 102.9(2) . . ? Zn O2 Gd 97.15(18) 2_756 . ? C19 O3 Gd 92.7(4) . . ? C19 O4 Gd 93.2(4) . . ? C24 O5 Gd 139.7(6) . . ? C31 O6 Zn 126.0(5) . . ? C31 O7 Gd 138.2(5) . 2_756 ? C11 N2 C7 119.5(9) . . ? C11 N2 Zn 114.1(6) . . ? C7 N2 Zn 126.4(8) . . ? C5 N1 C1 117.9(15) . . ? C5 N1 Zn 115.5(11) . . ? C1 N1 Zn 124.7(12) . . ? N1 C1 C2 120.9(16) . . ? C3 C2 C1 119.8(15) . . ? C4 C3 C2 116.9(17) . . ? C3 C4 C5 118.7(17) . . ? N1 C5 C4 125.2(16) . . ? N1 C5 C6 111.1(13) . . ? C4 C5 C6 123.6(15) . . ? C5' N1' C1' 121.0(17) . . ? C5' N1' Zn 105.4(13) . . ? C1' N1' Zn 131.5(12) . . ? C2' C1' N1' 120.2(17) . . ? C1' C2' C3' 119.7(17) . . ? C4' C3' C2' 118(2) . . ? C3' C4' C5' 119(2) . . ? N1' C5' C4' 122(2) . . ? N1' C5' C6 125.7(15) . . ? C4' C5' C6 112.0(17) . . ? C5 C6 O1 118.5(9) . . ? C5 C6 C5' 19.4(8) . . ? O1 C6 C5' 100.0(9) . . ? N2 C7 C8 121.5(13) . . ? C9 C8 C7 118.2(13) . . ? C8 C9 C10 122.9(14) . . ? C9 C10 C11 115.8(13) . . ? N2 C11 C10 122.1(10) . . ? N2 C11 C12 117.4(8) . . ? C10 C11 C12 120.5(10) . . ? O2 C12 C11 113.2(7) . . ? C14 C13 C18 116.7(18) . . ? C14 C13 C19 126.8(15) . . ? C18 C13 C19 115.1(16) . . ? C15 C14 C13 119.9(19) . . ? C16 C15 C14 125(2) . . ? C15 C16 C17 120(2) . . ? C18 C17 C16 117(2) . . ? C13 C18 C17 120(2) . . ? C18' C13' C14' 112(2) . . ? C18' C13' C19 133(2) . . ? C14' C13' C19 114.6(16) . . ? C15' C14' C13' 120(2) . . ? C16' C15' C14' 121(2) . . ? C15' C16' C17' 119(2) . . ? C16' C17' C18' 120(3) . . ? C13' C18' C17' 125(2) . . ? O4 C19 O3 120.7(6) . . ? O4 C19 C13' 127.6(11) . . ? O3 C19 C13' 111.3(10) . . ? O4 C19 C13 114.1(9) . . ? O3 C19 C13 124.6(10) . . ? C13' C19 C13 19.3(10) . . ? C21 C20 C21 119.6(11) . 2_756 ? C21 C20 C24 120.2(5) . . ? C21 C20 C24 120.2(5) 2_756 . ? C20 C21 C22 120.9(9) . . ? C23 C22 C21 118.8(10) . . ? C22 C23 C22 120.9(12) 2_756 . ? O5 C24 O5 124.0(10) 2_756 . ? O5 C24 C20 118.0(5) 2_756 . ? O5 C24 C20 118.0(5) . . ? C30 C25 C26 118(2) . . ? C30 C25 C31 124(2) . . ? C26 C25 C31 117.7(19) . . ? C27 C26 C25 121(2) . . ? C26 C27 C28 119(2) . . ? C29 C28 C27 116(2) . . ? C28 C29 C30 128(3) . . ? C25 C30 C29 116(3) . . ? C26' C25' C30' 113(3) . . ? C26' C25' C31 126(2) . . ? C30' C25' C31 121(2) . . ? C25' C26' C27' 126(3) . . ? C26' C27' C28' 120(2) . . ? C27' C28' C29' 120(3) . . ? C30' C29' C28' 115(3) . . ? C29' C30' C25' 125(3) . . ? O6 C31 O7 125.6(7) . . ? O6 C31 C25' 112.0(11) . . ? O7 C31 C25' 121.9(12) . . ? O6 C31 C25 122.0(10) . . ? O7 C31 C25 111.8(10) . . ? C25' C31 C25 18.6(10) . . ? O11 Cl1 O9 112.0(12) . . ? O11 Cl1 O10 112.6(12) . . ? O9 Cl1 O10 109.0(12) . . ? O11 Cl1 O12 109.1(12) . . ? O9 Cl1 O12 104.9(11) . . ? O10 Cl1 O12 108.9(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.413 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.220