# 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_1 #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H52 Dy2 N18 O5, C2 H2 Cl6, C H Cl3' _chemical_formula_sum 'C89 H55 Cl9 Dy2 N18 O5' _chemical_formula_weight 2100.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2819(5) _cell_length_b 12.6956(3) _cell_length_c 14.8559(6) _cell_angle_alpha 115.290(3) _cell_angle_beta 107.331(4) _cell_angle_gamma 91.929(3) _cell_volume 1964.27(15) _cell_formula_units_Z 1 _cell_measurement_temperature 120.00(10) _cell_measurement_reflns_used 17200 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 28.12 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 2.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120.00(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 28317 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7274 _reflns_number_gt 6585 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+13.4257P] 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 7274 _refine_ls_number_parameters 648 _refine_ls_number_restraints 2619 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.020 _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 0.15228(2) -0.02075(2) 0.49012(2) 0.02198(13) Uani 1 1 d U . . Cl1 Cl 0.7226(8) 0.4136(10) 0.8982(7) 0.247(4) Uani 1 1 d DU . . Cl2 Cl 0.6554(10) 0.2981(6) 1.0031(6) 0.262(5) Uani 1 1 d DU . . Cl3 Cl 0.5123(8) 0.4410(9) 0.9354(8) 0.255(5) Uani 1 1 d DU . . Cl4 Cl -0.3607(10) 0.2347(11) 0.1774(9) 0.170(5) Uani 0.50 1 d PDU A 2 Cl5 Cl -0.5834(12) 0.2567(13) 0.0717(12) 0.205(6) Uani 0.50 1 d PDU A 2 Cl6 Cl -0.5230(12) 0.0354(10) 0.0757(11) 0.182(4) Uani 0.50 1 d PDU . 2 N1 N 0.2619(5) 0.1465(5) 0.5032(4) 0.0265(11) Uani 1 1 d U B . N2 N 0.4495(5) 0.1653(5) 0.6313(5) 0.0302(12) Uani 1 1 d U B . N3 N 0.3523(5) -0.0406(5) 0.5318(4) 0.0258(11) Uani 1 1 d U B . N4 N 0.3289(5) -0.2558(5) 0.4585(4) 0.0265(11) Uani 1 1 d U B . N5 N 0.1675(5) -0.2034(5) 0.3545(4) 0.0243(10) Uani 1 1 d U B . N6 N 0.0069(5) -0.2253(5) 0.2005(4) 0.0275(11) Uani 1 1 d U B . N7 N 0.0764(5) -0.0164(5) 0.3237(4) 0.0232(10) Uani 1 1 d U B . N8 N 0.1193(5) 0.1948(5) 0.3804(4) 0.0254(11) Uani 1 1 d U B . N9 N -0.2430(10) -0.0941(9) 0.3091(8) 0.028(2) Uiso 0.50 1 d PDU . 1 N10 N -0.1765(8) 0.1329(9) 0.4033(7) 0.0267(19) Uiso 0.50 1 d PDU . 1 O1 O 0.0350(4) 0.1191(4) 0.5525(3) 0.0262(9) Uani 1 1 d DU . . O2 O 0.2071(9) 0.2564(9) 0.7347(8) 0.034(2) Uani 0.50 1 d PDU . 1 O3 O 0.0799(10) -0.2404(9) 0.5184(9) 0.032(2) Uani 0.50 1 d PDU . 1 O5 O 0.1937(10) 0.0286(10) 0.6692(8) 0.038(2) Uani 0.50 1 d PDU B 2 H5A H 0.2531 0.0174 0.7119 0.056 Uiso 0.50 1 d PRD B 2 H5B H 0.1526 -0.0429 0.6246 0.056 Uiso 0.50 1 d PRD B 2 C1 C 0.2137(6) 0.2206(6) 0.4637(5) 0.0250(12) Uani 1 1 d U . . C2 C 0.2878(6) 0.3367(6) 0.5220(6) 0.0275(13) Uani 1 1 d U B . C3 C 0.2797(6) 0.4398(6) 0.5100(6) 0.0299(13) Uani 1 1 d U . . H3 H 0.2146 0.4444 0.4610 0.036 Uiso 1 1 calc R B . C4 C 0.3711(7) 0.5348(6) 0.5728(6) 0.0358(15) Uani 1 1 d U B . H4 H 0.3672 0.6045 0.5664 0.043 Uiso 1 1 calc R . . C5 C 0.4700(7) 0.5277(7) 0.6464(7) 0.0393(17) Uani 1 1 d U . . H5 H 0.5301 0.5932 0.6884 0.047 Uiso 1 1 calc R B . C6 C 0.4797(7) 0.4249(6) 0.6575(6) 0.0370(16) Uani 1 1 d U B . H6 H 0.5459 0.4198 0.7051 0.044 Uiso 1 1 calc R . . C7 C 0.3870(6) 0.3296(6) 0.5951(6) 0.0291(13) Uani 1 1 d U . . C8 C 0.3689(6) 0.2079(6) 0.5797(5) 0.0273(13) Uani 1 1 d U B . C9 C 0.4424(6) 0.0507(6) 0.6056(5) 0.0269(13) Uani 1 1 d U . . C10 C 0.5373(6) 0.0041(6) 0.6548(5) 0.0284(13) Uani 1 1 d U B . C11 C 0.6463(6) 0.0583(7) 0.7332(6) 0.0315(14) Uani 1 1 d U . . H11 H 0.6728 0.1395 0.7633 0.038 Uiso 1 1 calc R B . C12 C 0.7137(6) -0.0146(7) 0.7643(6) 0.0330(15) Uani 1 1 d U B . H12 H 0.7857 0.0193 0.8181 0.040 Uiso 1 1 calc R . . C13 C 0.6769(6) -0.1349(6) 0.7177(6) 0.0305(14) Uani 1 1 d U . . H13 H 0.7243 -0.1803 0.7410 0.037 Uiso 1 1 calc R B . C14 C 0.5704(6) -0.1908(6) 0.6365(5) 0.0273(13) Uani 1 1 d U B . H14 H 0.5467 -0.2727 0.6037 0.033 Uiso 1 1 calc R . . C15 C 0.5004(6) -0.1183(6) 0.6065(5) 0.0260(13) Uani 1 1 d U . . C16 C 0.3855(6) -0.1449(6) 0.5266(5) 0.0244(12) Uani 1 1 d U B . C17 C 0.2319(6) -0.2815(6) 0.3770(5) 0.0246(12) Uani 1 1 d U . . C18 C 0.1818(6) -0.4021(6) 0.2935(5) 0.0268(13) Uani 1 1 d U B . C19 C 0.2106(6) -0.5117(6) 0.2787(6) 0.0301(14) Uani 1 1 d U . . H19 H 0.2740 -0.5178 0.3282 0.036 Uiso 1 1 calc R B . C20 C 0.1422(7) -0.6119(6) 0.1881(6) 0.0367(16) Uani 1 1 d U B . H20 H 0.1595 -0.6861 0.1776 0.044 Uiso 1 1 calc R . . C21 C 0.0476(7) -0.6034(7) 0.1120(6) 0.0376(16) Uani 1 1 d U . . H21 H 0.0031 -0.6716 0.0517 0.045 Uiso 1 1 calc R B . C22 C 0.0201(6) -0.4920(6) 0.1268(5) 0.0319(14) Uani 1 1 d U B . H22 H -0.0419 -0.4850 0.0766 0.038 Uiso 1 1 calc R . . C23 C 0.0874(6) -0.3933(6) 0.2176(5) 0.0276(13) Uani 1 1 d U . . C24 C 0.0826(6) -0.2665(6) 0.2573(5) 0.0244(12) Uani 1 1 d U B . C25 C 0.0094(6) -0.1112(6) 0.2307(5) 0.0262(12) Uani 1 1 d U . . C26 C -0.0609(6) -0.0672(6) 0.1584(5) 0.0296(13) Uani 1 1 d U B . C27 C -0.1420(7) -0.1242(7) 0.0572(6) 0.0406(17) Uani 1 1 d U . . H27 H -0.1624 -0.2065 0.0206 0.049 Uiso 1 1 calc R B . C28 C -0.1923(9) -0.0530(8) 0.0120(7) 0.052(2) Uani 1 1 d U B . H28 H -0.2506 -0.0887 -0.0542 0.063 Uiso 1 1 calc R . . C29 C -0.1592(9) 0.0641(8) 0.0608(6) 0.051(2) Uani 1 1 d U . . H29 H -0.1945 0.1069 0.0266 0.061 Uiso 1 1 calc R B . C30 C -0.0715(7) 0.1277(7) 0.1639(6) 0.0365(15) Uani 1 1 d U B . H30 H -0.0464 0.2093 0.1966 0.044 Uiso 1 1 calc R . . C31 C -0.0271(6) 0.0562(6) 0.2110(5) 0.0296(13) Uani 1 1 d U . . C32 C 0.0616(6) 0.0855(6) 0.3149(5) 0.0251(12) Uani 1 1 d U B . C33 C -0.3011(8) -0.0304(7) 0.2541(7) 0.025(2) Uani 0.50 1 d PGDU C 1 C34 C -0.2681(7) 0.0923(7) 0.3033(6) 0.035(2) Uani 0.50 1 d PGDU C 1 C35 C -0.3314(9) 0.1585(6) 0.2600(7) 0.045(3) Uani 0.50 1 d PGU C 1 H35 H -0.3093 0.2406 0.2929 0.054 Uiso 0.50 1 calc PR C 1 C36 C -0.4277(9) 0.1021(9) 0.1676(8) 0.058(3) Uani 0.50 1 d PGU C 1 H36 H -0.4701 0.1464 0.1387 0.069 Uiso 0.50 1 calc PR C 1 C37 C -0.4607(8) -0.0206(9) 0.1184(7) 0.052(3) Uani 0.50 1 d PGU C 1 H37 H -0.5251 -0.0583 0.0566 0.062 Uiso 0.50 1 calc PR C 1 C38 C -0.3974(8) -0.0868(7) 0.1617(7) 0.046(3) Uani 0.50 1 d PGU C 1 H38 H -0.4195 -0.1689 0.1287 0.055 Uiso 0.50 1 calc PR C 1 C39 C -0.1115(13) 0.2453(11) 0.4381(11) 0.032(3) Uani 0.50 1 d PDU D 1 H39 H -0.1297 0.2831 0.3955 0.038 Uiso 0.50 1 calc PR D 1 C40 C -0.0187(8) 0.3020(7) 0.5371(7) 0.025(2) Uani 0.50 1 d PGDU . 1 C41 C 0.0490(9) 0.2476(5) 0.5914(8) 0.025(3) Uani 0.50 1 d PGDU . 1 C42 C 0.1402(9) 0.3158(8) 0.6858(7) 0.031(3) Uani 0.50 1 d PGDU . 1 C43 C 0.1637(9) 0.4382(7) 0.7259(7) 0.036(3) Uani 0.50 1 d PGU . 1 H43 H 0.2247 0.4838 0.7891 0.043 Uiso 0.50 1 calc PR . 1 C44 C 0.0960(10) 0.4926(5) 0.6717(9) 0.038(3) Uani 0.50 1 d PGU . 1 H44 H 0.1117 0.5746 0.6986 0.046 Uiso 0.50 1 calc PR . 1 C45 C 0.0048(9) 0.4245(8) 0.5773(8) 0.034(3) Uani 0.50 1 d PGU . 1 H45 H -0.0406 0.4608 0.5410 0.041 Uiso 0.50 1 calc PR . 1 C46 C 0.288(2) 0.3273(19) 0.8386(13) 0.079(6) Uani 0.50 1 d PDU E 1 H46A H 0.3179 0.2773 0.8699 0.118 Uiso 0.50 1 calc PR E 1 H46B H 0.2496 0.3817 0.8812 0.118 Uiso 0.50 1 calc PR E 1 H46C H 0.3504 0.3709 0.8351 0.118 Uiso 0.50 1 calc PR E 1 C47 C -0.2440(13) -0.2154(10) 0.2497(10) 0.029(2) Uani 0.50 1 d PDU F 1 H47 H -0.2882 -0.2545 0.1779 0.034 Uiso 0.50 1 calc PR F 1 C48 C -0.1757(8) -0.2808(7) 0.3001(7) 0.025(3) Uani 0.50 1 d PGDU . 1 C49 C -0.0786(8) -0.2294(6) 0.3922(7) 0.022(2) Uani 0.50 1 d PGU . 1 C50 C -0.0172(8) -0.3004(8) 0.4303(7) 0.025(3) Uani 0.50 1 d PGU . 1 C51 C -0.0529(9) -0.4229(8) 0.3764(8) 0.030(3) Uani 0.50 1 d PGU . 1 H51 H -0.0118 -0.4704 0.4019 0.036 Uiso 0.50 1 calc PR . 1 C52 C -0.1500(9) -0.4743(6) 0.2843(8) 0.034(3) Uani 0.50 1 d PGU . 1 H52 H -0.1739 -0.5562 0.2483 0.041 Uiso 0.50 1 calc PR . 1 C53 C -0.2114(7) -0.4032(8) 0.2462(7) 0.034(3) Uani 0.50 1 d PGU . 1 H53 H -0.2764 -0.4376 0.1846 0.040 Uiso 0.50 1 calc PR . 1 C54 C 0.1257(15) -0.3041(15) 0.5754(13) 0.046(4) Uani 0.50 1 d PDU G 1 H54A H 0.1910 -0.2538 0.6374 0.070 Uiso 0.50 1 calc PR G 1 H54B H 0.1500 -0.3723 0.5310 0.070 Uiso 0.50 1 calc PR G 1 H54C H 0.0670 -0.3292 0.5964 0.070 Uiso 0.50 1 calc PR G 1 C55 C 0.6049(11) 0.3422(12) 0.9031(11) 0.133(5) Uani 1 1 d DU . . H55 H 0.5650 0.2729 0.8345 0.200 Uiso 1 1 d R . . C56 C -0.5059(12) 0.1873(13) 0.1420(15) 0.122(6) Uani 0.50 1 d PDU A 2 H56 H -0.5243 0.2123 0.2071 0.182 Uiso 0.50 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02657(19) 0.02176(19) 0.01868(18) 0.00994(13) 0.00821(13) 0.00468(12) Cl1 0.255(10) 0.295(10) 0.141(6) 0.090(7) 0.021(6) -0.014(8) Cl2 0.385(13) 0.136(5) 0.132(5) 0.025(4) -0.032(7) 0.035(7) Cl3 0.227(8) 0.220(8) 0.215(8) 0.031(6) 0.042(7) 0.039(7) Cl4 0.157(8) 0.163(8) 0.113(7) 0.030(6) -0.007(6) 0.048(7) Cl5 0.166(10) 0.234(12) 0.145(9) 0.072(9) -0.014(8) 0.030(10) Cl6 0.147(6) 0.175(6) 0.139(6) 0.020(6) 0.015(5) 0.014(6) N1 0.029(2) 0.025(2) 0.026(2) 0.0127(19) 0.009(2) 0.008(2) N2 0.037(3) 0.026(2) 0.026(2) 0.014(2) 0.006(2) 0.004(2) N3 0.030(3) 0.026(2) 0.022(2) 0.014(2) 0.005(2) 0.005(2) N4 0.032(3) 0.027(2) 0.025(2) 0.016(2) 0.009(2) 0.007(2) N5 0.029(2) 0.024(2) 0.022(2) 0.0112(19) 0.0098(19) 0.007(2) N6 0.032(3) 0.030(2) 0.020(2) 0.011(2) 0.009(2) 0.009(2) N7 0.028(2) 0.028(2) 0.018(2) 0.0140(19) 0.0080(19) 0.009(2) N8 0.030(2) 0.028(2) 0.027(2) 0.018(2) 0.013(2) 0.010(2) O1 0.026(2) 0.027(2) 0.023(2) 0.0118(17) 0.0058(17) -0.0002(17) O2 0.030(4) 0.031(4) 0.032(4) 0.016(3) -0.001(3) 0.002(4) O3 0.035(4) 0.031(4) 0.030(4) 0.014(3) 0.010(3) 0.016(3) O5 0.039(5) 0.046(6) 0.025(5) 0.018(4) 0.006(4) 0.009(5) C1 0.029(3) 0.026(3) 0.028(3) 0.015(2) 0.015(2) 0.007(2) C2 0.029(3) 0.028(3) 0.031(3) 0.015(2) 0.015(2) 0.010(2) C3 0.034(3) 0.027(3) 0.036(3) 0.018(3) 0.016(3) 0.011(2) C4 0.037(3) 0.026(3) 0.049(4) 0.021(3) 0.014(3) 0.009(3) C5 0.036(4) 0.030(3) 0.047(4) 0.018(3) 0.009(3) 0.001(3) C6 0.034(3) 0.029(3) 0.042(3) 0.018(3) 0.005(3) 0.004(3) C7 0.035(3) 0.027(3) 0.029(3) 0.016(2) 0.012(2) 0.009(2) C8 0.032(3) 0.026(3) 0.024(3) 0.013(2) 0.008(2) 0.005(2) C9 0.033(3) 0.029(3) 0.023(3) 0.016(2) 0.008(2) 0.005(2) C10 0.034(3) 0.029(3) 0.022(3) 0.015(2) 0.005(2) 0.002(2) C11 0.038(3) 0.033(3) 0.027(3) 0.018(3) 0.010(3) 0.003(3) C12 0.030(3) 0.045(4) 0.024(3) 0.019(3) 0.005(3) 0.004(3) C13 0.032(3) 0.040(3) 0.029(3) 0.024(3) 0.011(3) 0.013(3) C14 0.031(3) 0.030(3) 0.024(3) 0.016(2) 0.010(2) 0.006(2) C15 0.031(3) 0.030(3) 0.023(3) 0.017(2) 0.009(2) 0.006(2) C16 0.029(3) 0.027(3) 0.020(3) 0.015(2) 0.007(2) 0.006(2) C17 0.029(3) 0.026(3) 0.022(3) 0.014(2) 0.009(2) 0.007(2) C18 0.033(3) 0.027(3) 0.023(3) 0.013(2) 0.010(2) 0.008(2) C19 0.036(3) 0.028(3) 0.026(3) 0.013(2) 0.010(3) 0.009(3) C20 0.047(4) 0.026(3) 0.033(3) 0.011(3) 0.011(3) 0.007(3) C21 0.042(4) 0.030(3) 0.031(3) 0.008(3) 0.009(3) 0.007(3) C22 0.037(3) 0.030(3) 0.022(3) 0.008(2) 0.008(2) 0.009(3) C23 0.033(3) 0.025(3) 0.024(3) 0.010(2) 0.011(2) 0.006(2) C24 0.029(3) 0.026(3) 0.020(2) 0.011(2) 0.010(2) 0.007(2) C25 0.032(3) 0.031(3) 0.022(3) 0.016(2) 0.010(2) 0.011(2) C26 0.038(3) 0.037(3) 0.020(3) 0.016(2) 0.012(2) 0.014(3) C27 0.051(4) 0.041(3) 0.023(3) 0.012(3) 0.005(3) 0.016(3) C28 0.069(5) 0.053(4) 0.028(4) 0.021(3) 0.003(4) 0.015(4) C29 0.072(5) 0.059(4) 0.025(3) 0.026(3) 0.010(3) 0.032(4) C30 0.048(4) 0.041(3) 0.026(3) 0.020(3) 0.012(3) 0.018(3) C31 0.039(3) 0.035(3) 0.023(3) 0.017(2) 0.015(2) 0.017(2) C32 0.027(3) 0.029(3) 0.025(3) 0.015(2) 0.012(2) 0.011(2) C33 0.025(2) 0.026(2) 0.024(2) 0.0117(12) 0.0082(11) 0.0067(10) C34 0.039(4) 0.058(5) 0.030(4) 0.033(4) 0.021(4) 0.025(4) C35 0.050(5) 0.064(5) 0.037(5) 0.033(4) 0.022(4) 0.026(5) C36 0.059(6) 0.079(6) 0.043(5) 0.032(5) 0.023(5) 0.017(6) C37 0.057(6) 0.074(6) 0.037(5) 0.036(5) 0.012(5) 0.033(5) C38 0.050(5) 0.062(6) 0.036(5) 0.028(4) 0.016(5) 0.024(5) C39 0.039(5) 0.037(5) 0.031(4) 0.023(4) 0.015(4) 0.013(4) C40 0.028(4) 0.026(4) 0.031(4) 0.019(4) 0.014(4) 0.010(4) C41 0.031(4) 0.025(4) 0.026(4) 0.015(4) 0.013(4) 0.006(4) C42 0.035(5) 0.029(4) 0.030(4) 0.015(4) 0.009(4) 0.008(4) C43 0.038(5) 0.031(5) 0.035(5) 0.012(5) 0.012(5) 0.003(5) C44 0.039(5) 0.033(5) 0.040(5) 0.014(5) 0.016(5) 0.002(5) C45 0.040(5) 0.031(5) 0.038(5) 0.018(4) 0.020(5) 0.012(5) C46 0.064(10) 0.073(10) 0.062(10) 0.028(8) -0.022(9) 0.007(9) C47 0.031(5) 0.032(4) 0.027(4) 0.015(4) 0.013(4) 0.018(4) C48 0.025(5) 0.025(5) 0.025(5) 0.009(4) 0.013(4) 0.013(4) C49 0.030(4) 0.019(4) 0.024(4) 0.011(3) 0.018(4) 0.007(4) C50 0.030(5) 0.025(4) 0.025(4) 0.014(4) 0.011(4) 0.007(4) C51 0.033(5) 0.025(5) 0.029(5) 0.007(4) 0.012(4) 0.005(4) C52 0.036(5) 0.020(5) 0.036(5) 0.003(5) 0.015(5) 0.006(5) C53 0.028(5) 0.027(5) 0.033(5) 0.002(4) 0.012(4) 0.005(4) C54 0.047(4) 0.046(4) 0.046(4) 0.0215(19) 0.0155(15) 0.0093(12) C55 0.132(9) 0.115(8) 0.117(8) 0.025(7) 0.038(8) 0.025(8) C56 0.107(8) 0.122(8) 0.087(8) 0.017(8) 0.017(8) 0.008(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 Dy1 O5 2.340(10) . ? Dy1 O1 2.348(4) 2_556 ? Dy1 O1 2.376(5) . ? Dy1 N1 2.379(6) . ? Dy1 N7 2.394(5) . ? Dy1 N5 2.394(5) . ? Dy1 N3 2.398(6) . ? Dy1 N10 2.509(10) 2_556 ? Dy1 N9 2.541(11) 2_556 ? Dy1 H5B 2.1323 . ? Cl1 C55 1.718(9) . ? Cl2 C55 1.757(9) . ? Cl3 C55 1.734(9) . ? Cl3 Cl3 1.985(19) 2_667 ? Cl4 C56 1.708(10) . ? Cl5 C56 1.739(9) . ? Cl6 C56 1.721(9) . ? Cl6 Cl6 2.29(3) 2_455 ? N1 C1 1.372(8) . ? N1 C8 1.383(9) . ? N2 C9 1.331(9) . ? N2 C8 1.340(9) . ? N3 C9 1.369(9) . ? N3 C16 1.377(8) . ? N4 C17 1.329(9) . ? N4 C16 1.337(9) . ? N5 C24 1.369(8) . ? N5 C17 1.379(8) . ? N6 C25 1.317(9) . ? N6 C24 1.339(9) . ? N7 C32 1.368(8) . ? N7 C25 1.368(9) . ? N8 C32 1.321(9) . ? N8 C1 1.325(9) . ? N9 C47 1.408(9) . ? N9 C33 1.445(8) . ? N9 Dy1 2.541(10) 2_556 ? N10 C39 1.410(9) . ? N10 C34 1.432(8) . ? N10 O3 1.529(15) 2_556 ? N10 Dy1 2.509(10) 2_556 ? O1 C49 1.275(8) 2_556 ? O1 C41 1.464(6) . ? O1 Dy1 2.348(4) 2_556 ? O2 C48 0.734(9) 2_556 ? O2 C47 0.765(12) 2_556 ? O2 C42 1.388(8) . ? O2 C46 1.420(9) . ? O2 C53 1.76(3) 2_556 ? O3 C40 0.947(13) 2_556 ? O3 C50 1.368(13) . ? O3 C54 1.421(7) . ? O3 N10 1.529(15) 2_556 ? O3 C41 1.87(4) 2_556 ? O5 H5A 0.8740 . ? O5 H5B 0.8791 . ? C1 C2 1.448(10) . ? C2 C3 1.399(9) . ? C2 C7 1.406(10) . ? C3 C4 1.381(10) . ? C3 H3 0.9300 . ? C4 C5 1.407(11) . ? C4 H4 0.9300 . ? C5 C6 1.389(11) . ? C5 H5 0.9300 . ? C6 C7 1.392(10) . ? C6 H6 0.9300 . ? C7 C8 1.460(9) . ? C9 C10 1.466(9) . ? C10 C15 1.393(10) . ? C10 C11 1.395(10) . ? C11 C12 1.395(10) . ? C11 H11 0.9300 . ? C12 C13 1.371(11) . ? C12 H12 0.9300 . ? C13 C14 1.391(10) . ? C13 H13 0.9300 . ? C14 C15 1.401(9) . ? C14 H14 0.9300 . ? C15 C16 1.463(9) . ? C17 C18 1.457(9) . ? C18 C19 1.388(9) . ? C18 C23 1.401(9) . ? C19 C20 1.389(10) . ? C19 H19 0.9300 . ? C20 C21 1.404(11) . ? C20 H20 0.9300 . ? C21 C22 1.405(10) . ? C21 H21 0.9300 . ? C22 C23 1.376(10) . ? C22 H22 0.9300 . ? C23 C24 1.469(9) . ? C25 C26 1.484(9) . ? C26 C27 1.381(10) . ? C26 C31 1.397(10) . ? C27 C28 1.400(11) . ? C27 H27 0.9300 . ? C28 C29 1.328(13) . ? C28 H28 0.9300 . ? C29 C30 1.435(11) . ? C29 H29 0.9300 . ? C30 C31 1.399(10) . ? C30 H30 0.9300 . ? C31 C32 1.479(9) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.422(13) . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C40 C54 1.804(15) 2_556 ? C40 C49 1.88(3) 2_556 ? C41 C49 0.50(3) 2_556 ? C41 C50 0.91(3) 2_556 ? C41 C42 1.3900 . ? C41 C48 1.755(11) 2_556 ? C41 O3 1.871(14) 2_556 ? C42 C43 1.3900 . ? C42 C50 1.85(4) 2_556 ? C42 C52 1.86(2) 2_556 ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.468(12) . ? C47 H47 0.9300 . ? C48 C42 0.69(4) 2_556 ? C48 O2 0.734(9) 2_556 ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C48 C41 1.75(4) 2_556 ? C48 C43 1.89(2) 2_556 ? C48 C46 1.925(15) 2_556 ? C49 C41 0.50(3) 2_556 ? C49 C42 1.21(2) 2_556 ? C49 O1 1.275(8) 2_556 ? C49 C50 1.3900 . ? C49 C40 1.880(11) 2_556 ? C50 C51 1.3900 . ? C50 C45 1.546(16) 2_556 ? C50 C42 1.85(4) 2_556 ? C50 C39 1.930(15) 2_556 ? C51 C52 1.3900 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55 0.9800 . ? C56 H56 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Dy1 O1 90.6(3) . 2_556 ? O5 Dy1 O1 73.5(3) . . ? O1 Dy1 O1 69.83(17) 2_556 . ? O5 Dy1 N1 101.4(3) . . ? O1 Dy1 N1 145.17(17) 2_556 . ? O1 Dy1 N1 82.31(17) . . ? O5 Dy1 N7 160.6(3) . . ? O1 Dy1 N7 85.59(17) 2_556 . ? O1 Dy1 N7 87.41(17) . . ? N1 Dy1 N7 72.30(19) . . ? O5 Dy1 N5 126.7(3) . . ? O1 Dy1 N5 84.68(17) 2_556 . ? O1 Dy1 N5 148.43(17) . . ? N1 Dy1 N5 112.21(19) . . ? N7 Dy1 N5 71.89(18) . . ? O5 Dy1 N3 82.1(3) . . ? O1 Dy1 N3 142.96(17) 2_556 . ? O1 Dy1 N3 139.80(17) . . ? N1 Dy1 N3 71.63(18) . . ? N7 Dy1 N3 111.96(18) . . ? N5 Dy1 N3 71.45(19) . . ? O5 Dy1 N10 44.2(4) . 2_556 ? O1 Dy1 N10 74.3(2) 2_556 2_556 ? O1 Dy1 N10 105.7(3) . 2_556 ? N1 Dy1 N10 135.3(2) . 2_556 ? N7 Dy1 N10 149.9(2) . 2_556 ? N5 Dy1 N10 84.0(3) . 2_556 ? N3 Dy1 N10 75.3(3) . 2_556 ? O5 Dy1 N9 20.4(3) . 2_556 ? O1 Dy1 N9 108.3(3) 2_556 2_556 ? O1 Dy1 N9 71.8(2) . 2_556 ? N1 Dy1 N9 81.0(3) . 2_556 ? N7 Dy1 N9 148.2(2) . 2_556 ? N5 Dy1 N9 136.2(2) . 2_556 ? N3 Dy1 N9 74.3(3) . 2_556 ? N10 Dy1 N9 61.4(3) 2_556 2_556 ? O5 Dy1 Dy1 80.3(3) . 2_556 ? O1 Dy1 Dy1 35.15(11) 2_556 2_556 ? O1 Dy1 Dy1 34.68(10) . 2_556 ? N1 Dy1 Dy1 114.55(13) . 2_556 ? N7 Dy1 Dy1 85.74(13) . 2_556 ? N5 Dy1 Dy1 117.80(13) . 2_556 ? N3 Dy1 Dy1 162.24(13) . 2_556 ? N10 Dy1 Dy1 90.1(2) 2_556 2_556 ? N9 Dy1 Dy1 89.9(3) 2_556 2_556 ? O5 Dy1 H5B 22.0 . . ? O1 Dy1 H5B 73.6 2_556 . ? O1 Dy1 H5B 81.1 . . ? N1 Dy1 H5B 123.3 . . ? N7 Dy1 H5B 158.7 . . ? N5 Dy1 H5B 110.0 . . ? N3 Dy1 H5B 88.1 . . ? N10 Dy1 H5B 26.4 2_556 . ? N9 Dy1 H5B 42.2 2_556 . ? Dy1 Dy1 H5B 74.6 2_556 . ? C55 Cl3 Cl3 138.3(10) . 2_667 ? C56 Cl6 Cl6 114.8(13) . 2_455 ? C1 N1 C8 107.5(5) . . ? C1 N1 Dy1 123.7(4) . . ? C8 N1 Dy1 125.0(4) . . ? C9 N2 C8 123.2(6) . . ? C9 N3 C16 108.0(5) . . ? C9 N3 Dy1 123.8(4) . . ? C16 N3 Dy1 121.5(4) . . ? C17 N4 C16 123.1(6) . . ? C24 N5 C17 107.9(5) . . ? C24 N5 Dy1 123.9(4) . . ? C17 N5 Dy1 122.6(4) . . ? C25 N6 C24 122.6(6) . . ? C32 N7 C25 109.0(5) . . ? C32 N7 Dy1 123.5(4) . . ? C25 N7 Dy1 124.5(4) . . ? C32 N8 C1 123.0(6) . . ? C47 N9 C33 118.7(10) . . ? C47 N9 Dy1 124.3(7) . 2_556 ? C33 N9 Dy1 117.0(6) . 2_556 ? C39 N10 C34 113.0(9) . . ? C34 N10 O3 139.2(9) . 2_556 ? C39 N10 Dy1 124.9(8) . 2_556 ? C34 N10 Dy1 121.9(6) . 2_556 ? O3 N10 Dy1 98.8(6) 2_556 2_556 ? C49 O1 Dy1 129.1(18) 2_556 2_556 ? C41 O1 Dy1 115.6(5) . 2_556 ? C49 O1 Dy1 120.5(18) 2_556 . ? C41 O1 Dy1 133.0(5) . . ? Dy1 O1 Dy1 110.17(17) 2_556 . ? C48 O2 C47 157(2) 2_556 2_556 ? C47 O2 C42 168.2(17) 2_556 . ? C48 O2 C46 123.6(16) 2_556 . ? C47 O2 C46 73.0(15) 2_556 . ? C42 O2 C46 116.6(12) . . ? C47 O2 C53 143(2) 2_556 2_556 ? C40 O3 C54 97.3(12) 2_556 . ? C50 O3 C54 115.6(11) . . ? C40 O3 N10 171.3(13) 2_556 2_556 ? C50 O3 N10 153.6(10) . 2_556 ? C54 O3 N10 90.8(11) . 2_556 ? C54 O3 C41 142.1(12) . 2_556 ? N10 O3 C41 126.5(8) 2_556 2_556 ? H5A O5 H5B 104.7 . . ? N8 C1 N1 128.3(6) . . ? N8 C1 C2 121.7(6) . . ? N1 C1 C2 109.8(6) . . ? C3 C2 C7 120.7(6) . . ? C3 C2 C1 131.8(7) . . ? C7 C2 C1 107.2(6) . . ? C4 C3 C2 118.2(7) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 120.9(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 121.2(7) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 117.9(7) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C6 C7 C2 121.0(6) . . ? C6 C7 C8 133.4(7) . . ? C2 C7 C8 105.4(6) . . ? N2 C8 N1 127.2(6) . . ? N2 C8 C7 122.7(6) . . ? N1 C8 C7 110.0(6) . . ? N2 C9 N3 127.9(6) . . ? N2 C9 C10 122.4(6) . . ? N3 C9 C10 109.7(6) . . ? C15 C10 C11 121.1(6) . . ? C15 C10 C9 106.2(6) . . ? C11 C10 C9 132.7(7) . . ? C10 C11 C12 117.1(7) . . ? C10 C11 H11 121.5 . . ? C12 C11 H11 121.5 . . ? C13 C12 C11 121.8(7) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C12 C13 C14 121.7(6) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 117.0(6) . . ? C13 C14 H14 121.5 . . ? C15 C14 H14 121.5 . . ? C10 C15 C14 121.2(6) . . ? C10 C15 C16 106.7(6) . . ? C14 C15 C16 132.1(6) . . ? N4 C16 N3 128.1(6) . . ? N4 C16 C15 122.6(6) . . ? N3 C16 C15 109.3(6) . . ? N4 C17 N5 127.5(6) . . ? N4 C17 C18 122.5(6) . . ? N5 C17 C18 109.9(5) . . ? C19 C18 C23 120.6(6) . . ? C19 C18 C17 133.1(6) . . ? C23 C18 C17 106.2(6) . . ? C18 C19 C20 118.2(7) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C19 C20 C21 121.3(7) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C22 120.1(7) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 118.2(7) . . ? C23 C22 H22 120.9 . . ? C21 C22 H22 120.9 . . ? C22 C23 C18 121.6(6) . . ? C22 C23 C24 132.1(6) . . ? C18 C23 C24 106.3(6) . . ? N6 C24 N5 128.2(6) . . ? N6 C24 C23 122.2(6) . . ? N5 C24 C23 109.5(6) . . ? N6 C25 N7 129.2(6) . . ? N6 C25 C26 121.7(6) . . ? N7 C25 C26 109.0(6) . . ? C27 C26 C31 121.0(7) . . ? C27 C26 C25 132.6(7) . . ? C31 C26 C25 106.3(6) . . ? C26 C27 C28 117.1(8) . . ? C26 C27 H27 121.4 . . ? C28 C27 H27 121.4 . . ? C29 C28 C27 122.0(8) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 123.2(7) . . ? C28 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C31 C30 C29 114.2(7) . . ? C31 C30 H30 122.9 . . ? C29 C30 H30 122.9 . . ? C26 C31 C30 122.2(7) . . ? C26 C31 C32 106.2(6) . . ? C30 C31 C32 131.5(7) . . ? N8 C32 N7 129.0(6) . . ? N8 C32 C31 121.5(6) . . ? N7 C32 C31 109.4(6) . . ? C34 C33 C38 120.0 . . ? C34 C33 N9 118.1(7) . . ? C38 C33 N9 121.4(7) . . ? C35 C34 C33 120.0 . . ? C35 C34 N10 128.8(7) . . ? C33 C34 N10 110.7(7) . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? N10 C39 C40 121.3(12) . . ? N10 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 127.0(8) . . ? C45 C40 C39 112.9(8) . . ? C41 C40 C54 154.5(8) . 2_556 ? C45 C40 C49 119.4(4) . 2_556 ? C39 C40 C49 127.4(9) . 2_556 ? C54 C40 C49 154.3(10) 2_556 2_556 ? C49 C41 C50 160(5) 2_556 2_556 ? C50 C41 C42 105.3(17) 2_556 . ? C49 C41 C40 169(6) 2_556 . ? C42 C41 C40 120.0 . . ? C50 C41 O1 138.5(18) 2_556 . ? C42 C41 O1 116.0(6) . . ? C40 C41 O1 123.9(6) . . ? C50 C41 C48 126.0(19) 2_556 2_556 ? C40 C41 C48 140.6(4) . 2_556 ? C49 C41 O3 152(2) 2_556 2_556 ? C42 C41 O3 148.9(5) . 2_556 ? O1 C41 O3 95.0(5) . 2_556 ? C48 C41 O3 169.9(6) 2_556 2_556 ? O2 C42 C41 117.5(7) . . ? O2 C42 C43 122.5(7) . . ? C41 C42 C43 120.0 . . ? O2 C42 C50 145.8(8) . 2_556 ? O2 C42 C52 133.2(15) . 2_556 ? C41 C42 C52 109.2(14) . 2_556 ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? O2 C46 H46A 109.5 . . ? O2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N9 C47 C48 120.6(10) . . ? N9 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C42 C48 O2 156(5) 2_556 2_556 ? O2 C48 C49 130.7(12) 2_556 . ? O2 C48 C53 107.7(12) 2_556 . ? C49 C48 C53 120.0 . . ? C42 C48 C47 168(5) 2_556 . ? C49 C48 C47 124.8(8) . . ? C53 C48 C47 115.1(8) . . ? O2 C48 C41 141.7(15) 2_556 2_556 ? C53 C48 C41 107.7(4) . 2_556 ? C47 C48 C41 136.9(9) . 2_556 ? O2 C48 C43 131.4(18) 2_556 2_556 ? C47 C48 C43 139.9(14) . 2_556 ? C42 C48 C46 125(3) 2_556 2_556 ? C49 C48 C46 164.5(10) . 2_556 ? C41 C48 C46 165(2) 2_556 2_556 ? C43 C48 C46 93.8(15) 2_556 2_556 ? C41 C49 C42 101.2(16) 2_556 2_556 ? C41 C49 O1 102(2) 2_556 2_556 ? C42 C49 O1 155(2) 2_556 2_556 ? C42 C49 C50 90.9(17) 2_556 . ? O1 C49 C50 113.6(7) 2_556 . ? C41 C49 C48 131(2) 2_556 . ? O1 C49 C48 126.4(7) 2_556 . ? C50 C49 C48 120.0 . . ? C42 C49 C40 100.3(19) 2_556 2_556 ? O1 C49 C40 104.3(6) 2_556 2_556 ? C48 C49 C40 129.3(4) . 2_556 ? O3 C50 C51 125.2(7) . . ? O3 C50 C49 114.7(7) . . ? C51 C50 C49 120.0 . . ? C49 C50 C45 149.6(18) . 2_556 ? O3 C50 C42 154.5(10) . 2_556 ? C45 C50 C42 109.4(15) 2_556 2_556 ? C51 C50 C39 113.8(7) . 2_556 ? C49 C50 C39 126.0(7) . 2_556 ? C42 C50 C39 166.5(8) 2_556 2_556 ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C48 120.0 . . ? C52 C53 H53 120.0 . . ? C48 C53 H53 120.0 . . ? O3 C54 H54A 109.5 . . ? O3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Cl1 C55 Cl3 108.6(8) . . ? Cl1 C55 Cl2 108.0(8) . . ? Cl3 C55 Cl2 109.3(8) . . ? Cl1 C55 H55 110.1 . . ? Cl3 C55 H55 110.5 . . ? Cl2 C55 H55 110.3 . . ? Cl4 C56 Cl6 103.6(9) . . ? Cl4 C56 Cl5 109.2(9) . . ? Cl6 C56 Cl5 117.1(11) . . ? Cl4 C56 H56 107.9 . . ? Cl6 C56 H56 111.0 . . ? Cl5 C56 H56 107.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.927 _refine_diff_density_min -2.719 _refine_diff_density_rms 0.198 _database_code_depnum_ccdc_archive 'CCDC 903254' ####################################################################### # # 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_2 #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H52 Gd2 N18 O5, C2 H2 Cl6, C H Cl3' _chemical_formula_sum 'C89 H55 Cl9 Gd2 N18 O5' _chemical_formula_weight 2090.06 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3447(9) _cell_length_b 12.6876(4) _cell_length_c 14.8992(11) _cell_angle_alpha 115.119(6) _cell_angle_beta 107.452(6) _cell_angle_gamma 91.663(5) _cell_volume 1982.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 120 _cell_measurement_reflns_used 6788 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 29.0 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 2.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 15418 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7352 _reflns_number_gt 6285 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1343P)^2^+3.6195P] 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 7352 _refine_ls_number_parameters 648 _refine_ls_number_restraints 2595 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1898 _refine_ls_wR_factor_gt 0.1792 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.15281(3) -0.02143(3) 0.49115(2) 0.02050(15) Uani 1 1 d U . . Cl1 Cl 0.7241(6) 0.4058(8) 0.8972(5) 0.203(3) Uani 1 1 d DU . . Cl2 Cl 0.6509(8) 0.2953(5) 1.0033(5) 0.212(4) Uani 1 1 d DU . . Cl3 Cl 0.5124(6) 0.4378(7) 0.9358(7) 0.204(3) Uani 1 1 d DU . . Cl4 Cl -0.3587(9) 0.2403(10) 0.1758(9) 0.165(5) Uani 0.50 1 d PDU A 2 Cl5 Cl -0.5893(8) 0.2535(10) 0.0713(9) 0.147(4) Uani 0.50 1 d PDU A 2 Cl6 Cl -0.5215(11) 0.0369(10) 0.0656(11) 0.181(4) Uani 0.50 1 d PDU . 2 N1 N 0.2629(5) 0.1460(5) 0.5036(5) 0.0248(11) Uani 1 1 d U B . N2 N 0.4491(6) 0.1641(5) 0.6313(5) 0.0299(13) Uani 1 1 d U B . N3 N 0.3531(5) -0.0421(5) 0.5322(4) 0.0243(12) Uani 1 1 d U B . N4 N 0.3293(5) -0.2569(5) 0.4576(5) 0.0266(12) Uani 1 1 d U B . N5 N 0.1694(5) -0.2038(5) 0.3537(5) 0.0241(11) Uani 1 1 d U B . N6 N 0.0095(5) -0.2248(5) 0.2005(4) 0.0265(12) Uani 1 1 d U B . N7 N 0.0798(5) -0.0156(5) 0.3238(4) 0.0231(11) Uani 1 1 d U B . N8 N 0.1213(5) 0.1958(5) 0.3819(5) 0.0246(11) Uani 1 1 d U B . N9 N -0.2428(11) -0.0935(9) 0.3075(8) 0.026(2) Uiso 0.50 1 d PDU . 1 N10 N -0.1760(9) 0.1345(9) 0.4023(7) 0.0245(19) Uiso 0.50 1 d PDU . 1 O1 O 0.0355(4) 0.1196(4) 0.5538(4) 0.0275(10) Uani 1 1 d DU . . O2 O 0.2058(9) 0.2562(9) 0.7350(8) 0.034(2) Uani 0.50 1 d PDU . 1 O3 O 0.0810(10) -0.2409(9) 0.5169(10) 0.034(2) Uani 0.50 1 d PDU . 1 O5 O 0.1969(10) 0.0305(11) 0.6743(9) 0.037(2) Uani 0.50 1 d PDU B 2 H5A H 0.2564 0.0193 0.7170 0.056 Uiso 0.50 1 d PRD B 2 H5B H 0.1559 -0.0410 0.6298 0.056 Uiso 0.50 1 d PRD B 2 C1 C 0.2158(6) 0.2222(6) 0.4655(6) 0.0234(13) Uani 1 1 d U . . C2 C 0.2889(6) 0.3361(6) 0.5233(6) 0.0242(13) Uani 1 1 d U B . C3 C 0.2803(6) 0.4393(6) 0.5114(6) 0.0286(14) Uani 1 1 d U . . H3 H 0.2155 0.4443 0.4627 0.034 Uiso 1 1 calc R B . C4 C 0.3718(7) 0.5346(6) 0.5747(7) 0.0330(16) Uani 1 1 d U B . H4 H 0.3686 0.6042 0.5681 0.040 Uiso 1 1 calc R . . C5 C 0.4682(7) 0.5262(7) 0.6477(7) 0.0378(18) Uani 1 1 d U . . H5 H 0.5273 0.5916 0.6902 0.045 Uiso 1 1 calc R B . C6 C 0.4792(7) 0.4238(7) 0.6593(6) 0.0340(16) Uani 1 1 d U B . H6 H 0.5446 0.4183 0.7071 0.041 Uiso 1 1 calc R . . C7 C 0.3856(6) 0.3286(6) 0.5946(6) 0.0274(14) Uani 1 1 d U . . C8 C 0.3682(6) 0.2055(6) 0.5797(6) 0.0253(13) Uani 1 1 d U B . C9 C 0.4430(6) 0.0479(6) 0.6054(5) 0.0253(13) Uani 1 1 d U . . C10 C 0.5363(7) 0.0009(6) 0.6548(6) 0.0268(14) Uani 1 1 d U B . C11 C 0.6452(6) 0.0551(7) 0.7330(6) 0.0296(15) Uani 1 1 d U . . H11 H 0.6711 0.1362 0.7631 0.035 Uiso 1 1 calc R B . C12 C 0.7127(7) -0.0180(7) 0.7633(6) 0.0320(16) Uani 1 1 d U B . H12 H 0.7846 0.0153 0.8163 0.038 Uiso 1 1 calc R . . C13 C 0.6750(6) -0.1407(6) 0.7160(6) 0.0270(14) Uani 1 1 d U . . H13 H 0.7217 -0.1865 0.7395 0.032 Uiso 1 1 calc R B . C14 C 0.5701(6) -0.1952(7) 0.6352(6) 0.0264(14) Uani 1 1 d U B . H14 H 0.5470 -0.2769 0.6023 0.032 Uiso 1 1 calc R . . C15 C 0.4993(6) -0.1226(6) 0.6044(5) 0.0256(14) Uani 1 1 d U . . C16 C 0.3851(6) -0.1465(6) 0.5258(5) 0.0244(13) Uani 1 1 d U B . C17 C 0.2338(6) -0.2824(6) 0.3757(5) 0.0240(13) Uani 1 1 d U . . C18 C 0.1816(7) -0.4033(6) 0.2927(6) 0.0267(14) Uani 1 1 d U B . C19 C 0.2102(7) -0.5135(6) 0.2780(6) 0.0299(15) Uani 1 1 d U . . H19 H 0.2729 -0.5203 0.3275 0.036 Uiso 1 1 calc R B . C20 C 0.1432(7) -0.6115(6) 0.1888(6) 0.0327(16) Uani 1 1 d U B . H20 H 0.1615 -0.6855 0.1781 0.039 Uiso 1 1 calc R . . C21 C 0.0487(7) -0.6042(7) 0.1136(6) 0.0366(17) Uani 1 1 d U . . H21 H 0.0038 -0.6726 0.0547 0.044 Uiso 1 1 calc R B . C22 C 0.0211(7) -0.4916(6) 0.1271(6) 0.0292(14) Uani 1 1 d U B . H22 H -0.0405 -0.4845 0.0769 0.035 Uiso 1 1 calc R . . C23 C 0.0891(6) -0.3934(6) 0.2174(6) 0.0255(13) Uani 1 1 d U . . C24 C 0.0838(6) -0.2663(6) 0.2566(5) 0.0235(13) Uani 1 1 d U B . C25 C 0.0128(6) -0.1099(6) 0.2301(5) 0.0243(13) Uani 1 1 d U . . C26 C -0.0569(6) -0.0642(7) 0.1598(5) 0.0280(14) Uani 1 1 d U B . C27 C -0.1375(8) -0.1211(7) 0.0586(6) 0.0395(18) Uani 1 1 d U . . H27 H -0.1583 -0.2032 0.0219 0.047 Uiso 1 1 calc R B . C28 C -0.1866(9) -0.0466(8) 0.0139(7) 0.047(2) Uani 1 1 d U B . H28 H -0.2441 -0.0813 -0.0523 0.056 Uiso 1 1 calc R . . C29 C -0.1544(9) 0.0688(8) 0.0619(6) 0.046(2) Uani 1 1 d U . . H29 H -0.1885 0.1124 0.0279 0.056 Uiso 1 1 calc R B . C30 C -0.0677(7) 0.1303(7) 0.1658(6) 0.0354(16) Uani 1 1 d U B . H30 H -0.0435 0.2120 0.1994 0.042 Uiso 1 1 calc R . . C31 C -0.0232(7) 0.0588(6) 0.2119(6) 0.0278(14) Uani 1 1 d U . . C32 C 0.0643(6) 0.0870(6) 0.3149(5) 0.0218(12) Uani 1 1 d U B . C33 C -0.2998(8) -0.0294(7) 0.2524(7) 0.022(2) Uani 0.50 1 d PGDU C 1 C34 C -0.2676(7) 0.0931(8) 0.3022(6) 0.034(2) Uani 0.50 1 d PGDU C 1 C35 C -0.3308(9) 0.1601(6) 0.2597(8) 0.041(3) Uani 0.50 1 d PGU C 1 H35 H -0.3093 0.2421 0.2931 0.050 Uiso 0.50 1 calc PR C 1 C36 C -0.4262(9) 0.1047(9) 0.1674(8) 0.052(3) Uani 0.50 1 d PGU C 1 H36 H -0.4685 0.1495 0.1390 0.062 Uiso 0.50 1 calc PR C 1 C37 C -0.4584(8) -0.0178(9) 0.1176(7) 0.047(3) Uani 0.50 1 d PGU C 1 H37 H -0.5222 -0.0549 0.0558 0.056 Uiso 0.50 1 calc PR C 1 C38 C -0.3952(9) -0.0849(6) 0.1601(7) 0.044(3) Uani 0.50 1 d PGU C 1 H38 H -0.4168 -0.1668 0.1267 0.053 Uiso 0.50 1 calc PR C 1 C39 C -0.1133(13) 0.2478(11) 0.4366(11) 0.031(3) Uani 0.50 1 d PDU D 1 H39 H -0.1322 0.2869 0.3950 0.037 Uiso 0.50 1 calc PR D 1 C40 C -0.0194(8) 0.3023(7) 0.5373(7) 0.023(2) Uani 0.50 1 d PGDU . 1 C41 C 0.0478(9) 0.2479(5) 0.5918(7) 0.025(3) Uani 0.50 1 d PGDU . 1 C42 C 0.1381(9) 0.3156(8) 0.6859(7) 0.029(3) Uani 0.50 1 d PGDU . 1 C43 C 0.1614(9) 0.4378(7) 0.7255(7) 0.036(3) Uani 0.50 1 d PGU . 1 H43 H 0.2219 0.4832 0.7884 0.043 Uiso 0.50 1 calc PR . 1 C44 C 0.0943(10) 0.4923(5) 0.6709(9) 0.037(3) Uani 0.50 1 d PGU . 1 H44 H 0.1098 0.5741 0.6973 0.044 Uiso 0.50 1 calc PR . 1 C45 C 0.0039(9) 0.4246(8) 0.5768(8) 0.030(3) Uani 0.50 1 d PGU . 1 H45 H -0.0410 0.4610 0.5403 0.037 Uiso 0.50 1 calc PR . 1 C46 C 0.282(2) 0.3268(19) 0.8394(13) 0.079(6) Uani 0.50 1 d PDU E 1 H46A H 0.3126 0.2768 0.8707 0.119 Uiso 0.50 1 calc PR E 1 H46B H 0.2418 0.3792 0.8802 0.119 Uiso 0.50 1 calc PR E 1 H46C H 0.3448 0.3725 0.8381 0.119 Uiso 0.50 1 calc PR E 1 C47 C -0.2423(13) -0.2144(10) 0.2480(11) 0.026(2) Uani 0.50 1 d PDU F 1 H47 H -0.2846 -0.2524 0.1760 0.031 Uiso 0.50 1 calc PR F 1 C48 C -0.1766(8) -0.2804(8) 0.2975(8) 0.024(3) Uani 0.50 1 d PGDU . 1 C49 C -0.0801(9) -0.2297(6) 0.3892(8) 0.024(3) Uani 0.50 1 d PGU . 1 C50 C -0.0191(8) -0.3012(8) 0.4273(7) 0.021(2) Uani 0.50 1 d PGU . 1 C51 C -0.0546(9) -0.4234(8) 0.3737(8) 0.032(3) Uani 0.50 1 d PGU . 1 H51 H -0.0137 -0.4712 0.3992 0.039 Uiso 0.50 1 calc PR . 1 C52 C -0.1510(10) -0.4740(6) 0.2820(8) 0.035(3) Uani 0.50 1 d PGU . 1 H52 H -0.1748 -0.5558 0.2462 0.042 Uiso 0.50 1 calc PR . 1 C53 C -0.2121(8) -0.4026(8) 0.2439(7) 0.031(3) Uani 0.50 1 d PGU . 1 H53 H -0.2766 -0.4365 0.1826 0.037 Uiso 0.50 1 calc PR . 1 C54 C 0.1233(17) -0.3069(16) 0.5729(14) 0.049(4) Uani 0.50 1 d PDU G 1 H54A H 0.1885 -0.2586 0.6350 0.074 Uiso 0.50 1 calc PR G 1 H54B H 0.1465 -0.3758 0.5284 0.074 Uiso 0.50 1 calc PR G 1 H54C H 0.0636 -0.3307 0.5930 0.074 Uiso 0.50 1 calc PR G 1 C55 C 0.6038(9) 0.3378(11) 0.9020(10) 0.113(5) Uani 1 1 d DU . . H55 H 0.5638 0.2686 0.8333 0.169 Uiso 1 1 d R . . C56 C -0.5028(11) 0.1875(12) 0.1397(14) 0.112(6) Uani 0.50 1 d PDU A 2 H56 H -0.5212 0.2124 0.2048 0.168 Uiso 0.50 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0235(2) 0.0208(2) 0.0202(2) 0.01187(15) 0.00784(14) 0.00325(13) Cl1 0.172(7) 0.266(8) 0.127(5) 0.077(5) 0.018(4) -0.023(6) Cl2 0.295(9) 0.111(4) 0.120(4) 0.031(3) -0.040(5) 0.012(5) Cl3 0.145(6) 0.175(6) 0.211(7) 0.031(5) 0.042(5) 0.018(5) Cl4 0.117(7) 0.155(8) 0.119(7) 0.003(6) -0.010(6) 0.043(6) Cl5 0.075(5) 0.195(9) 0.137(8) 0.077(7) -0.011(5) 0.006(6) Cl6 0.136(6) 0.167(6) 0.144(6) 0.011(6) 0.011(5) 0.008(6) N1 0.029(3) 0.022(2) 0.028(2) 0.014(2) 0.012(2) 0.008(2) N2 0.032(3) 0.028(3) 0.032(3) 0.019(2) 0.007(2) 0.004(2) N3 0.025(3) 0.025(2) 0.025(2) 0.017(2) 0.002(2) 0.002(2) N4 0.029(3) 0.025(3) 0.030(3) 0.017(2) 0.009(2) 0.006(2) N5 0.025(3) 0.020(2) 0.028(2) 0.011(2) 0.009(2) 0.004(2) N6 0.029(3) 0.029(3) 0.023(2) 0.013(2) 0.008(2) 0.006(2) N7 0.022(3) 0.026(3) 0.024(2) 0.014(2) 0.009(2) 0.007(2) N8 0.025(3) 0.030(3) 0.026(2) 0.018(2) 0.011(2) 0.011(2) O1 0.026(2) 0.027(2) 0.028(2) 0.0114(18) 0.0086(18) -0.0021(18) O2 0.026(4) 0.033(4) 0.035(4) 0.018(4) -0.002(4) 0.001(4) O3 0.035(4) 0.029(4) 0.036(4) 0.015(4) 0.010(4) 0.014(3) O5 0.028(5) 0.039(6) 0.042(6) 0.020(5) 0.005(4) 0.014(4) C1 0.025(3) 0.026(3) 0.028(3) 0.016(2) 0.016(2) 0.005(2) C2 0.023(3) 0.024(3) 0.032(3) 0.017(2) 0.014(2) 0.005(2) C3 0.025(3) 0.031(3) 0.035(3) 0.018(3) 0.013(3) 0.008(3) C4 0.029(3) 0.025(3) 0.052(4) 0.023(3) 0.015(3) 0.007(3) C5 0.033(4) 0.029(4) 0.048(4) 0.019(3) 0.009(3) -0.001(3) C6 0.033(3) 0.029(3) 0.038(3) 0.017(3) 0.006(3) -0.001(3) C7 0.030(3) 0.028(3) 0.030(3) 0.018(2) 0.012(3) 0.006(3) C8 0.026(3) 0.026(3) 0.026(3) 0.015(2) 0.007(2) 0.001(2) C9 0.026(3) 0.027(3) 0.027(3) 0.018(2) 0.006(2) 0.005(2) C10 0.030(3) 0.028(3) 0.024(3) 0.016(2) 0.006(3) 0.005(3) C11 0.027(3) 0.031(3) 0.033(3) 0.019(3) 0.008(3) 0.004(3) C12 0.027(4) 0.043(4) 0.025(3) 0.016(3) 0.007(3) 0.006(3) C13 0.024(3) 0.038(4) 0.032(3) 0.026(3) 0.011(3) 0.011(3) C14 0.027(3) 0.034(3) 0.026(3) 0.020(3) 0.010(3) 0.006(3) C15 0.024(3) 0.035(3) 0.024(3) 0.019(2) 0.008(2) 0.007(3) C16 0.026(3) 0.025(3) 0.028(3) 0.020(2) 0.005(2) 0.005(2) C17 0.028(3) 0.024(3) 0.025(3) 0.016(2) 0.009(2) 0.005(2) C18 0.033(3) 0.026(3) 0.026(3) 0.015(2) 0.011(2) 0.008(2) C19 0.037(3) 0.027(3) 0.029(3) 0.015(3) 0.012(3) 0.010(3) C20 0.042(4) 0.019(3) 0.034(4) 0.013(3) 0.008(3) 0.006(3) C21 0.042(4) 0.027(3) 0.035(4) 0.010(3) 0.011(3) 0.007(3) C22 0.031(3) 0.029(3) 0.026(3) 0.011(2) 0.011(3) 0.006(3) C23 0.027(3) 0.024(3) 0.028(3) 0.012(2) 0.014(2) 0.005(2) C24 0.028(3) 0.023(3) 0.027(3) 0.015(2) 0.013(2) 0.005(2) C25 0.028(3) 0.026(3) 0.027(3) 0.017(2) 0.011(2) 0.010(2) C26 0.031(3) 0.037(3) 0.021(3) 0.017(2) 0.010(2) 0.014(3) C27 0.051(4) 0.039(4) 0.021(3) 0.011(3) 0.004(3) 0.012(3) C28 0.059(5) 0.048(4) 0.028(4) 0.025(3) -0.004(3) 0.008(4) C29 0.066(5) 0.052(4) 0.025(4) 0.024(3) 0.009(3) 0.026(4) C30 0.043(4) 0.039(3) 0.027(3) 0.019(3) 0.009(3) 0.016(3) C31 0.036(3) 0.031(3) 0.024(3) 0.016(2) 0.014(2) 0.012(3) C32 0.026(3) 0.026(3) 0.023(3) 0.016(2) 0.013(2) 0.008(2) C33 0.022(2) 0.023(2) 0.022(2) 0.0106(12) 0.0076(11) 0.0055(10) C34 0.038(4) 0.056(5) 0.029(4) 0.032(4) 0.021(4) 0.020(4) C35 0.043(5) 0.060(5) 0.034(5) 0.029(4) 0.020(4) 0.021(5) C36 0.052(6) 0.072(6) 0.043(5) 0.032(5) 0.022(5) 0.010(5) C37 0.052(6) 0.064(6) 0.037(5) 0.037(5) 0.011(5) 0.019(5) C38 0.044(5) 0.056(6) 0.034(5) 0.020(5) 0.016(5) 0.016(5) C39 0.033(5) 0.038(5) 0.030(4) 0.020(4) 0.016(4) 0.007(4) C40 0.027(5) 0.026(4) 0.032(4) 0.023(4) 0.015(4) 0.009(4) C41 0.027(4) 0.024(4) 0.027(4) 0.014(4) 0.012(4) 0.003(4) C42 0.031(5) 0.027(4) 0.031(4) 0.017(4) 0.010(4) 0.001(4) C43 0.032(6) 0.030(5) 0.041(5) 0.011(5) 0.016(5) 0.001(5) C44 0.033(5) 0.034(5) 0.040(5) 0.012(5) 0.015(5) -0.003(5) C45 0.030(5) 0.028(5) 0.041(5) 0.018(4) 0.019(5) 0.009(4) C46 0.054(10) 0.074(10) 0.071(10) 0.030(9) -0.023(9) 0.002(9) C47 0.027(5) 0.029(4) 0.029(4) 0.017(4) 0.013(4) 0.017(4) C48 0.025(5) 0.022(5) 0.026(5) 0.010(4) 0.011(4) 0.011(4) C49 0.028(4) 0.021(4) 0.028(4) 0.011(4) 0.015(4) 0.006(4) C50 0.027(5) 0.020(4) 0.024(4) 0.015(4) 0.011(4) 0.003(4) C51 0.033(5) 0.027(5) 0.030(5) 0.007(5) 0.012(5) 0.000(5) C52 0.034(5) 0.021(5) 0.039(5) 0.003(5) 0.014(5) 0.003(5) C53 0.029(5) 0.025(5) 0.029(5) 0.003(4) 0.010(4) 0.003(4) C54 0.049(4) 0.049(4) 0.049(4) 0.023(2) 0.0166(17) 0.0093(12) C55 0.103(8) 0.102(8) 0.118(8) 0.031(7) 0.046(7) 0.019(7) C56 0.092(8) 0.115(8) 0.086(8) 0.019(8) 0.015(8) 0.004(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 Gd1 O1 2.365(5) 2_556 ? Gd1 O1 2.390(5) . ? Gd1 O5 2.396(12) . ? Gd1 N1 2.396(6) . ? Gd1 N3 2.413(6) . ? Gd1 N5 2.418(6) . ? Gd1 N7 2.418(6) . ? Gd1 N10 2.518(10) 2_556 ? Gd1 N9 2.560(11) 2_556 ? Gd1 Gd1 3.8978(7) 2_556 ? Gd1 H5B 2.1719 . ? Cl1 C55 1.732(9) . ? Cl2 C55 1.758(9) . ? Cl3 C55 1.736(8) . ? Cl3 Cl3 2.016(16) 2_667 ? Cl4 C56 1.720(9) . ? Cl5 C56 1.733(9) . ? Cl6 C56 1.718(9) . ? Cl6 Cl6 2.02(3) 2_455 ? N1 C8 1.369(9) . ? N1 C1 1.378(9) . ? N2 C8 1.334(9) . ? N2 C9 1.350(9) . ? N3 C16 1.366(9) . ? N3 C9 1.367(9) . ? N4 C17 1.328(9) . ? N4 C16 1.336(9) . ? N5 C24 1.378(9) . ? N5 C17 1.379(9) . ? N6 C24 1.326(9) . ? N6 C25 1.327(9) . ? N7 C32 1.376(9) . ? N7 C25 1.377(9) . ? N8 C32 1.323(9) . ? N8 C1 1.333(9) . ? N9 C47 1.410(9) . ? N9 C33 1.444(8) . ? N9 Gd1 2.560(11) 2_556 ? N10 C39 1.414(9) . ? N10 C34 1.438(8) . ? N10 O3 1.526(15) 2_556 ? N10 Gd1 2.518(10) 2_556 ? O1 C49 1.282(8) 2_556 ? O1 C41 1.464(6) . ? O1 Gd1 2.365(5) 2_556 ? O2 C48 0.698(9) 2_556 ? O2 C47 0.780(12) 2_556 ? O2 C42 1.392(8) . ? O2 C46 1.415(9) . ? O2 C53 1.74(3) 2_556 ? O2 C49 1.91(3) 2_556 ? O3 C40 0.949(13) 2_556 ? O3 C50 1.408(14) . ? O3 C54 1.424(7) . ? O3 N10 1.526(15) 2_556 ? O3 C41 1.87(4) 2_556 ? O5 H5A 0.8754 . ? O5 H5B 0.8833 . ? C1 C2 1.430(10) . ? C2 C7 1.377(10) . ? C2 C3 1.396(10) . ? C3 C4 1.393(10) . ? C3 H3 0.9300 . ? C4 C5 1.392(11) . ? C4 H4 0.9300 . ? C5 C6 1.387(11) . ? C5 H5 0.9300 . ? C6 C7 1.409(10) . ? C6 H6 0.9300 . ? C7 C8 1.480(10) . ? C9 C10 1.460(10) . ? C10 C11 1.401(10) . ? C10 C15 1.407(10) . ? C11 C12 1.391(11) . ? C11 H11 0.9300 . ? C12 C13 1.402(11) . ? C12 H12 0.9300 . ? C13 C14 1.381(10) . ? C13 H13 0.9300 . ? C14 C15 1.410(10) . ? C14 H14 0.9300 . ? C15 C16 1.461(10) . ? C17 C18 1.467(10) . ? C18 C23 1.392(10) . ? C18 C19 1.395(10) . ? C19 C20 1.369(10) . ? C19 H19 0.9300 . ? C20 C21 1.391(11) . ? C20 H20 0.9300 . ? C21 C22 1.422(11) . ? C21 H21 0.9300 . ? C22 C23 1.381(10) . ? C22 H22 0.9300 . ? C23 C24 1.476(9) . ? C25 C26 1.475(9) . ? C26 C27 1.385(10) . ? C26 C31 1.397(10) . ? C27 C28 1.425(11) . ? C27 H27 0.9300 . ? C28 C29 1.311(13) . ? C28 H28 0.9300 . ? C29 C30 1.442(11) . ? C29 H29 0.9300 . ? C30 C31 1.390(10) . ? C30 H30 0.9300 . ? C31 C32 1.472(10) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.450(14) . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C40 C54 1.779(16) 2_556 ? C40 C49 1.92(3) 2_556 ? C41 C49 0.53(3) 2_556 ? C41 C50 0.88(3) 2_556 ? C41 C42 1.3900 . ? C41 C48 1.797(11) 2_556 ? C41 O3 1.867(14) 2_556 ? C42 C43 1.3900 . ? C42 C50 1.81(4) 2_556 ? C42 C52 1.85(2) 2_556 ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.452(12) . ? C47 H47 0.9300 . ? C48 O2 0.698(9) 2_556 ? C48 C42 0.72(4) 2_556 ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C48 C41 1.80(4) 2_556 ? C48 C46 1.885(16) 2_556 ? C48 C43 1.90(2) 2_556 ? C49 C41 0.53(3) 2_556 ? C49 C42 1.18(2) 2_556 ? C49 O1 1.282(8) 2_556 ? C49 C50 1.3900 . ? C49 O2 1.914(12) 2_556 ? C49 C40 1.916(11) 2_556 ? C50 C51 1.3900 . ? C50 C45 1.560(16) 2_556 ? C50 C42 1.81(4) 2_556 ? C50 C39 2.006(16) 2_556 ? C51 C52 1.3900 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55 0.9852 . ? C56 H56 0.9842 . ? 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 O1 Gd1 O1 69.89(17) 2_556 . ? O1 Gd1 O5 92.1(3) 2_556 . ? O1 Gd1 O5 73.4(3) . . ? O1 Gd1 N1 144.84(18) 2_556 . ? O1 Gd1 N1 82.57(18) . . ? O5 Gd1 N1 100.7(3) . . ? O1 Gd1 N3 143.49(17) 2_556 . ? O1 Gd1 N3 139.81(18) . . ? O5 Gd1 N3 82.0(3) . . ? N1 Gd1 N3 71.26(19) . . ? O1 Gd1 N5 84.98(18) 2_556 . ? O1 Gd1 N5 148.57(18) . . ? O5 Gd1 N5 127.8(3) . . ? N1 Gd1 N5 111.1(2) . . ? N3 Gd1 N5 71.2(2) . . ? O1 Gd1 N7 85.68(18) 2_556 . ? O1 Gd1 N7 88.08(18) . . ? O5 Gd1 N7 160.9(3) . . ? N1 Gd1 N7 71.6(2) . . ? N3 Gd1 N7 110.76(19) . . ? N5 Gd1 N7 70.98(19) . . ? O1 Gd1 N10 74.8(2) 2_556 2_556 ? O1 Gd1 N10 105.4(3) . 2_556 ? O5 Gd1 N10 44.8(4) . 2_556 ? N1 Gd1 N10 135.5(2) . 2_556 ? N3 Gd1 N10 75.9(3) . 2_556 ? N5 Gd1 N10 84.9(3) . 2_556 ? N7 Gd1 N10 150.2(2) . 2_556 ? O1 Gd1 N9 108.8(3) 2_556 2_556 ? O1 Gd1 N9 71.5(3) . 2_556 ? O5 Gd1 N9 19.5(3) . 2_556 ? N1 Gd1 N9 81.2(3) . 2_556 ? N3 Gd1 N9 74.7(3) . 2_556 ? N5 Gd1 N9 136.8(2) . 2_556 ? N7 Gd1 N9 147.9(3) . 2_556 ? N10 Gd1 N9 61.5(3) 2_556 2_556 ? O1 Gd1 Gd1 35.16(12) 2_556 2_556 ? O1 Gd1 Gd1 34.73(11) . 2_556 ? O5 Gd1 Gd1 81.2(3) . 2_556 ? N1 Gd1 Gd1 114.63(14) . 2_556 ? N3 Gd1 Gd1 162.96(14) . 2_556 ? N5 Gd1 Gd1 118.05(14) . 2_556 ? N7 Gd1 Gd1 86.20(14) . 2_556 ? N10 Gd1 Gd1 90.2(3) 2_556 2_556 ? N9 Gd1 Gd1 90.1(3) 2_556 2_556 ? O1 Gd1 H5B 75.5 2_556 . ? O1 Gd1 H5B 80.8 . . ? O5 Gd1 H5B 21.6 . . ? N1 Gd1 H5B 122.2 . . ? N3 Gd1 H5B 87.9 . . ? N5 Gd1 H5B 111.6 . . ? N7 Gd1 H5B 160.5 . . ? N10 Gd1 H5B 26.9 2_556 . ? N9 Gd1 H5B 41.0 2_556 . ? Gd1 Gd1 H5B 75.5 2_556 . ? C55 Cl3 Cl3 140.5(8) . 2_667 ? C56 Cl6 Cl6 122.5(14) . 2_455 ? C8 N1 C1 107.2(6) . . ? C8 N1 Gd1 124.4(4) . . ? C1 N1 Gd1 124.2(5) . . ? C8 N2 C9 122.7(6) . . ? C16 N3 C9 108.3(6) . . ? C16 N3 Gd1 121.0(4) . . ? C9 N3 Gd1 124.1(5) . . ? C17 N4 C16 123.2(6) . . ? C24 N5 C17 108.1(5) . . ? C24 N5 Gd1 123.6(5) . . ? C17 N5 Gd1 122.3(4) . . ? C24 N6 C25 122.7(6) . . ? C32 N7 C25 108.4(5) . . ? C32 N7 Gd1 123.5(4) . . ? C25 N7 Gd1 124.6(4) . . ? C32 N8 C1 124.1(6) . . ? C47 N9 C33 118.4(10) . . ? C47 N9 Gd1 124.6(7) . 2_556 ? C33 N9 Gd1 117.0(7) . 2_556 ? C39 N10 C34 112.9(10) . . ? C39 N10 O3 28.5(6) . 2_556 ? C34 N10 O3 141.3(9) . 2_556 ? C39 N10 Gd1 125.7(8) . 2_556 ? C34 N10 Gd1 121.1(6) . 2_556 ? O3 N10 Gd1 97.3(6) 2_556 2_556 ? C49 O1 C41 21.1(15) 2_556 . ? C49 O1 Gd1 129(2) 2_556 2_556 ? C41 O1 Gd1 114.9(5) . 2_556 ? C49 O1 Gd1 120.2(19) 2_556 . ? C41 O1 Gd1 133.5(5) . . ? Gd1 O1 Gd1 110.11(17) 2_556 . ? C48 O2 C47 159(2) 2_556 2_556 ? C48 O2 C42 11.5(13) 2_556 . ? C47 O2 C42 169.6(17) 2_556 . ? C48 O2 C46 122.6(18) 2_556 . ? C47 O2 C46 73.1(15) 2_556 . ? C42 O2 C46 116.3(13) . . ? C48 O2 C53 49.2(11) 2_556 2_556 ? C47 O2 C53 142(2) 2_556 2_556 ? C42 O2 C53 44.8(13) . 2_556 ? C46 O2 C53 73.5(18) . 2_556 ? C48 O2 C49 33.8(12) 2_556 2_556 ? C47 O2 C49 133.2(15) 2_556 2_556 ? C42 O2 C49 37.8(6) . 2_556 ? C46 O2 C49 153.5(14) . 2_556 ? C53 O2 C49 82.2(16) 2_556 2_556 ? C40 O3 C50 19.3(7) 2_556 . ? C40 O3 C54 95.0(12) 2_556 . ? C50 O3 C54 114.2(12) . . ? C40 O3 N10 174.0(12) 2_556 2_556 ? C50 O3 N10 154.7(10) . 2_556 ? C54 O3 N10 91.0(11) . 2_556 ? C40 O3 C41 46.2(7) 2_556 2_556 ? C50 O3 C41 27.0(5) . 2_556 ? C54 O3 C41 140.1(13) . 2_556 ? N10 O3 C41 127.9(8) 2_556 2_556 ? Gd1 O5 H5A 128.8 . . ? Gd1 O5 H5B 64.8 . . ? H5A O5 H5B 105.1 . . ? N8 C1 N1 127.0(6) . . ? N8 C1 C2 122.6(6) . . ? N1 C1 C2 110.3(6) . . ? C7 C2 C3 120.9(6) . . ? C7 C2 C1 107.5(6) . . ? C3 C2 C1 131.4(7) . . ? C4 C3 C2 118.0(7) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C5 C4 C3 120.4(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 122.4(7) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 116.2(7) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? C2 C7 C6 122.1(7) . . ? C2 C7 C8 105.8(6) . . ? C6 C7 C8 132.1(7) . . ? N2 C8 N1 128.5(6) . . ? N2 C8 C7 122.2(6) . . ? N1 C8 C7 109.2(6) . . ? N2 C9 N3 127.2(6) . . ? N2 C9 C10 122.9(6) . . ? N3 C9 C10 109.9(6) . . ? C11 C10 C15 121.9(7) . . ? C11 C10 C9 132.3(7) . . ? C15 C10 C9 105.8(6) . . ? C12 C11 C10 116.9(7) . . ? C12 C11 H11 121.6 . . ? C10 C11 H11 121.6 . . ? C11 C12 C13 121.6(7) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 121.7(7) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 117.7(7) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C10 C15 C14 120.2(7) . . ? C10 C15 C16 106.3(6) . . ? C14 C15 C16 133.5(7) . . ? N4 C16 N3 128.8(6) . . ? N4 C16 C15 121.6(6) . . ? N3 C16 C15 109.5(6) . . ? N4 C17 N5 127.2(6) . . ? N4 C17 C18 123.3(6) . . ? N5 C17 C18 109.5(6) . . ? C23 C18 C19 120.7(7) . . ? C23 C18 C17 106.5(6) . . ? C19 C18 C17 132.8(7) . . ? C20 C19 C18 118.0(7) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C19 C20 C21 122.3(7) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C20 C21 C22 119.8(7) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 117.5(7) . . ? C23 C22 H22 121.3 . . ? C21 C22 H22 121.3 . . ? C22 C23 C18 121.7(7) . . ? C22 C23 C24 131.6(7) . . ? C18 C23 C24 106.7(6) . . ? N6 C24 N5 128.4(6) . . ? N6 C24 C23 122.5(6) . . ? N5 C24 C23 109.0(6) . . ? N6 C25 N7 128.7(6) . . ? N6 C25 C26 122.4(6) . . ? N7 C25 C26 108.8(6) . . ? C27 C26 C31 121.1(7) . . ? C27 C26 C25 131.9(7) . . ? C31 C26 C25 106.9(6) . . ? C26 C27 C28 116.0(8) . . ? C26 C27 H27 122.0 . . ? C28 C27 H27 122.0 . . ? C29 C28 C27 123.0(8) . . ? C29 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C28 C29 C30 122.2(7) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 115.1(7) . . ? C31 C30 H30 122.4 . . ? C29 C30 H30 122.4 . . ? C30 C31 C26 122.3(7) . . ? C30 C31 C32 131.6(7) . . ? C26 C31 C32 106.1(6) . . ? N8 C32 N7 128.1(6) . . ? N8 C32 C31 122.2(6) . . ? N7 C32 C31 109.6(6) . . ? C34 C33 C38 120.0 . . ? C34 C33 N9 117.8(7) . . ? C38 C33 N9 121.5(8) . . ? C33 C34 C35 120.0 . . ? C33 C34 N10 111.6(7) . . ? C35 C34 N10 127.9(7) . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? N10 C39 C40 119.3(12) . . ? N10 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 128.5(8) . . ? C45 C40 C39 111.5(8) . . ? C41 C40 C54 155.2(8) . 2_556 ? C45 C40 C54 84.3(8) . 2_556 ? C39 C40 C54 27.3(7) . 2_556 ? C41 C40 C49 3.1(15) . 2_556 ? C45 C40 C49 118.8(4) . 2_556 ? C39 C40 C49 129.5(9) . 2_556 ? C54 C40 C49 155.6(10) 2_556 2_556 ? C49 C41 C50 156(5) 2_556 2_556 ? C49 C41 C40 169(5) 2_556 . ? C50 C41 C40 16.8(18) 2_556 . ? C49 C41 C42 56.2(15) 2_556 . ? C50 C41 C42 103.2(18) 2_556 . ? C40 C41 C42 120.0 . . ? C49 C41 O1 59.9(12) 2_556 . ? C50 C41 O1 141.1(19) 2_556 . ? C40 C41 O1 124.4(6) . . ? C42 C41 O1 115.5(6) . . ? C49 C41 C48 34.5(12) 2_556 2_556 ? C50 C41 C48 124(2) 2_556 2_556 ? C40 C41 C48 140.9(4) . 2_556 ? C42 C41 C48 21.8(4) . 2_556 ? O1 C41 C48 94.1(5) . 2_556 ? C49 C41 O3 154.6(19) 2_556 2_556 ? C50 C41 O3 46.2(18) 2_556 2_556 ? C40 C41 O3 29.5(5) . 2_556 ? C42 C41 O3 149.0(5) . 2_556 ? O1 C41 O3 95.4(6) . 2_556 ? C48 C41 O3 170.4(6) 2_556 2_556 ? C43 C42 C41 120.0 . . ? C43 C42 O2 122.3(7) . . ? C41 C42 O2 117.7(7) . . ? C43 C42 C50 91.6(3) . 2_556 ? C41 C42 C50 28.4(3) . 2_556 ? O2 C42 C50 146.0(8) . 2_556 ? C43 C42 C52 9.3(15) . 2_556 ? C41 C42 C52 110.7(14) . 2_556 ? O2 C42 C52 131.5(15) . 2_556 ? C50 C42 C52 82.3(15) 2_556 2_556 ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? O2 C46 H46A 109.5 . . ? O2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N9 C47 C48 120.9(11) . . ? N9 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? O2 C48 C42 157(5) 2_556 2_556 ? O2 C48 C49 129.9(13) 2_556 . ? C42 C48 C49 58.1(16) 2_556 . ? O2 C48 C53 108.5(13) 2_556 . ? C42 C48 C53 62.7(16) 2_556 . ? C49 C48 C53 120.0 . . ? O2 C48 C47 11.3(13) 2_556 . ? C42 C48 C47 168(5) 2_556 . ? C49 C48 C47 124.3(8) . . ? C53 C48 C47 115.6(8) . . ? O2 C48 C41 141.1(16) 2_556 2_556 ? C42 C48 C41 45.5(17) 2_556 2_556 ? C49 C48 C41 12.6(4) . 2_556 ? C53 C48 C41 107.6(4) . 2_556 ? C47 C48 C41 136.5(9) . 2_556 ? O2 C48 C46 39.3(13) 2_556 2_556 ? C42 C48 C46 126(3) 2_556 2_556 ? C49 C48 C46 163.7(11) . 2_556 ? C53 C48 C46 69.3(9) . 2_556 ? C47 C48 C46 47.6(9) . 2_556 ? C41 C48 C46 164(2) 2_556 2_556 ? O2 C48 C43 133.5(19) 2_556 2_556 ? C42 C48 C43 36.4(7) 2_556 2_556 ? C49 C48 C43 93.6(13) . 2_556 ? C53 C48 C43 26.5(13) . 2_556 ? C47 C48 C43 141.7(14) . 2_556 ? C41 C48 C43 81.1(15) 2_556 2_556 ? C46 C48 C43 94.4(15) 2_556 2_556 ? C41 C49 C42 101.7(15) 2_556 2_556 ? C41 C49 O1 99.0(19) 2_556 2_556 ? C42 C49 O1 157(2) 2_556 2_556 ? C41 C49 C48 132.9(19) 2_556 . ? C42 C49 C48 31.3(18) 2_556 . ? O1 C49 C48 127.5(7) 2_556 . ? C41 C49 C50 15(3) 2_556 . ? C42 C49 C50 89.1(17) 2_556 . ? O1 C49 C50 112.5(7) 2_556 . ? C48 C49 C50 120.0 . . ? C41 C49 O2 147(3) 2_556 2_556 ? C42 C49 O2 46.3(17) 2_556 2_556 ? O1 C49 O2 111.7(6) 2_556 2_556 ? C48 C49 O2 16.2(4) . 2_556 ? C50 C49 O2 135.5(4) . 2_556 ? C41 C49 C40 8(5) 2_556 2_556 ? C42 C49 C40 99.3(19) 2_556 2_556 ? O1 C49 C40 102.4(6) 2_556 2_556 ? C48 C49 C40 130.1(4) . 2_556 ? C50 C49 C40 10.2(4) . 2_556 ? O2 C49 C40 145.6(5) 2_556 2_556 ? C51 C50 C49 120.0 . . ? C51 C50 O3 124.9(8) . . ? C49 C50 O3 115.0(8) . . ? C51 C50 C45 31.5(17) . 2_556 ? C49 C50 C45 151.3(18) . 2_556 ? O3 C50 C45 93.7(17) . 2_556 ? C51 C50 C42 79.5(4) . 2_556 ? C49 C50 C42 40.7(4) . 2_556 ? O3 C50 C42 154.7(10) . 2_556 ? C45 C50 C42 111.0(15) 2_556 2_556 ? C51 C50 C39 112.8(7) . 2_556 ? C49 C50 C39 127.0(7) . 2_556 ? O3 C50 C39 14.4(5) . 2_556 ? C45 C50 C39 81.3(17) 2_556 2_556 ? C42 C50 C39 167.7(8) 2_556 2_556 ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C48 120.0 . . ? C52 C53 H53 120.0 . . ? C48 C53 H53 120.0 . . ? O3 C54 H54A 109.5 . . ? O3 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O3 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Cl1 C55 Cl3 110.2(8) . . ? Cl1 C55 Cl2 107.8(7) . . ? Cl3 C55 Cl2 107.0(7) . . ? Cl1 C55 H55 109.7 . . ? Cl3 C55 H55 111.1 . . ? Cl2 C55 H55 110.9 . . ? Cl6 C56 Cl4 105.8(9) . . ? Cl6 C56 Cl5 112.5(10) . . ? Cl4 C56 Cl5 111.5(9) . . ? Cl6 C56 H56 114.7 . . ? Cl4 C56 H56 107.6 . . ? Cl5 C56 H56 104.7 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.489 _refine_diff_density_min -2.872 _refine_diff_density_rms 0.211 _database_code_depnum_ccdc_archive 'CCDC 931252' ####################################################################### # # 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_3 #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H60 Dy2 N6 O15' _chemical_formula_weight 1502.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.773(10) _cell_length_b 12.4264(8) _cell_length_c 23.7209(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6418(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4435 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3000 _exptl_absorpt_coefficient_mu 2.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.658 _exptl_absorpt_correction_T_max 0.788 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 16420 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8657 _reflns_number_gt 7470 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(13) _refine_ls_number_reflns 8657 _refine_ls_number_parameters 802 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1103 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _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 C1 C 0.4144(6) 0.4317(9) 0.4411(9) 0.074(6) Uani 1 1 d . . . H1A H 0.3834 0.4382 0.4696 0.111 Uiso 1 1 calc R . . H1B H 0.3962 0.4046 0.4070 0.111 Uiso 1 1 calc R . . H1C H 0.4323 0.5010 0.4339 0.111 Uiso 1 1 calc R . . C2 C 0.5110(5) 0.3386(7) 0.4246(6) 0.040(3) Uani 1 1 d . . . C3 C 0.5198(5) 0.3824(8) 0.3728(6) 0.044(3) Uani 1 1 d . . . H3 H 0.4908 0.4296 0.3582 0.053 Uiso 1 1 calc R . . C4 C 0.5715(7) 0.3575(10) 0.3413(7) 0.062(4) Uani 1 1 d . . . H4 H 0.5766 0.3861 0.3054 0.075 Uiso 1 1 calc R . . C5 C 0.6152(6) 0.2902(9) 0.3637(5) 0.046(3) Uani 1 1 d . . . H5 H 0.6512 0.2772 0.3437 0.055 Uiso 1 1 calc R . . C6 C 0.6062(5) 0.2408(8) 0.4162(5) 0.039(3) Uani 1 1 d . . . C7 C 0.5535(5) 0.2632(8) 0.4472(5) 0.034(2) Uani 1 1 d . . . C8 C 0.6550(5) 0.1704(9) 0.4360(5) 0.042(3) Uani 1 1 d . . . H8 H 0.6921 0.1729 0.4166 0.050 Uiso 1 1 calc R . . C9 C 0.7029(5) 0.0405(8) 0.4917(5) 0.036(3) Uani 1 1 d . . . C10 C 0.7473(5) 0.0036(9) 0.4539(6) 0.051(3) Uani 1 1 d . . . H10 H 0.7487 0.0318 0.4176 0.061 Uiso 1 1 calc R . . C11 C 0.7896(5) -0.0748(10) 0.4700(7) 0.056(4) Uani 1 1 d . . . H11 H 0.8185 -0.0992 0.4441 0.068 Uiso 1 1 calc R . . C12 C 0.7888(5) -0.1156(10) 0.5227(8) 0.059(4) Uani 1 1 d . . . H12 H 0.8171 -0.1682 0.5328 0.071 Uiso 1 1 calc R . . C13 C 0.7469(5) -0.0809(10) 0.5615(7) 0.059(4) Uani 1 1 d . . . H13 H 0.7470 -0.1092 0.5978 0.071 Uiso 1 1 calc R . . C14 C 0.7029(4) -0.0004(8) 0.5457(5) 0.041(3) Uani 1 1 d . . . C15 C 0.6624(6) 0.0328(10) 0.6347(7) 0.050(3) Uani 1 1 d . . . H15 H 0.7013 0.0112 0.6464 0.060 Uiso 1 1 calc R . . C16 C 0.6217(5) 0.0650(8) 0.6793(5) 0.041(3) Uani 1 1 d . . . C17 C 0.6388(6) 0.0538(10) 0.7359(6) 0.054(3) Uani 1 1 d . . . H17 H 0.6748 0.0169 0.7444 0.065 Uiso 1 1 calc R . . C18 C 0.6045(7) 0.0953(13) 0.7792(6) 0.067(4) Uani 1 1 d . . . H18 H 0.6173 0.0866 0.8164 0.080 Uiso 1 1 calc R . . C19 C 0.5515(7) 0.1496(13) 0.7675(6) 0.066(4) Uani 1 1 d . . . H19 H 0.5288 0.1794 0.7968 0.080 Uiso 1 1 calc R . . C20 C 0.5315(5) 0.1608(8) 0.7128(5) 0.040(3) Uani 1 1 d . . . C21 C 0.5644(5) 0.1159(8) 0.6655(5) 0.038(3) Uani 1 1 d . . . C22 C 0.4505(8) 0.2819(15) 0.7383(7) 0.094(6) Uani 1 1 d . . . H22A H 0.4148 0.3157 0.7224 0.141 Uiso 1 1 calc R . . H22B H 0.4791 0.3361 0.7502 0.141 Uiso 1 1 calc R . . H22C H 0.4386 0.2389 0.7701 0.141 Uiso 1 1 calc R . . C23 C 0.3237(6) 0.2609(9) 0.5939(8) 0.071(5) Uani 1 1 d . . . H23A H 0.3280 0.2603 0.6342 0.106 Uiso 1 1 calc R . . H23B H 0.2822 0.2434 0.5840 0.106 Uiso 1 1 calc R . . H23C H 0.3337 0.3311 0.5797 0.106 Uiso 1 1 calc R . . C24 C 0.3656(5) 0.1695(8) 0.5132(5) 0.037(3) Uani 1 1 d . . . C25 C 0.3253(5) 0.2146(9) 0.4750(6) 0.049(3) Uani 1 1 d . . . H25 H 0.2937 0.2579 0.4885 0.059 Uiso 1 1 calc R . . C26 C 0.3297(6) 0.1987(10) 0.4193(6) 0.054(3) Uani 1 1 d . . . H26 H 0.2996 0.2263 0.3955 0.065 Uiso 1 1 calc R . . C27 C 0.3775(5) 0.1427(9) 0.3970(6) 0.047(3) Uani 1 1 d . . . H27 H 0.3823 0.1362 0.3582 0.056 Uiso 1 1 calc R . . C28 C 0.4196(5) 0.0948(7) 0.4347(5) 0.034(3) Uani 1 1 d . . . C29 C 0.4131(4) 0.1033(7) 0.4925(5) 0.028(2) Uani 1 1 d . . . C30 C 0.4710(5) 0.0401(8) 0.4071(5) 0.040(3) Uani 1 1 d . . . H30 H 0.4658 0.0229 0.3692 0.048 Uiso 1 1 calc R . . C31 C 0.5706(5) -0.0347(9) 0.3957(5) 0.037(3) Uani 1 1 d . . . C32 C 0.5793(6) -0.0078(12) 0.3398(6) 0.060(4) Uani 1 1 d . . . H32 H 0.5531 0.0408 0.3222 0.072 Uiso 1 1 calc R . . C33 C 0.6280(8) -0.0548(13) 0.3099(7) 0.076(5) Uani 1 1 d . . . H33 H 0.6356 -0.0344 0.2729 0.091 Uiso 1 1 calc R . . C34 C 0.6630(7) -0.1274(13) 0.3341(6) 0.068(4) Uani 1 1 d . . . H34 H 0.6934 -0.1617 0.3132 0.082 Uiso 1 1 calc R . . C35 C 0.6549(6) -0.1540(10) 0.3917(6) 0.054(3) Uani 1 1 d . . . H35 H 0.6809 -0.2045 0.4080 0.065 Uiso 1 1 calc R . . C36 C 0.6096(5) -0.1073(7) 0.4244(5) 0.034(2) Uani 1 1 d . . . C37 C 0.6196(5) -0.2009(8) 0.5079(5) 0.034(2) Uani 1 1 d . . . H37 H 0.6423 -0.2516 0.4879 0.041 Uiso 1 1 calc R . . C38 C 0.6078(5) -0.2191(8) 0.5675(5) 0.037(3) Uani 1 1 d . . . C39 C 0.6457(5) -0.2927(9) 0.5961(6) 0.047(3) Uani 1 1 d . . . H39 H 0.6793 -0.3230 0.5779 0.056 Uiso 1 1 calc R . . C40 C 0.6332(6) -0.3198(10) 0.6504(6) 0.060(4) Uani 1 1 d . . . H40 H 0.6590 -0.3682 0.6687 0.072 Uiso 1 1 calc R . . C41 C 0.5837(6) -0.2779(11) 0.6792(6) 0.059(4) Uani 1 1 d . . . H41 H 0.5765 -0.2959 0.7167 0.071 Uiso 1 1 calc R . . C42 C 0.5450(5) -0.2079(8) 0.6504(5) 0.037(3) Uani 1 1 d . . . C43 C 0.5580(4) -0.1756(7) 0.5963(5) 0.030(2) Uani 1 1 d . . . C44 C 0.4782(8) -0.1715(15) 0.7283(6) 0.078(5) Uani 1 1 d . . . H44A H 0.4394 -0.1376 0.7357 0.117 Uiso 1 1 calc R . . H44B H 0.5098 -0.1358 0.7494 0.117 Uiso 1 1 calc R . . H44C H 0.4762 -0.2457 0.7394 0.117 Uiso 1 1 calc R . . C45 C 0.1631(6) 0.1128(12) 0.5572(7) 0.069(4) Uani 1 1 d . . . H45A H 0.1589 0.1420 0.5944 0.104 Uiso 1 1 calc R . . H45B H 0.1294 0.0651 0.5496 0.104 Uiso 1 1 calc R . . H45C H 0.1629 0.1704 0.5301 0.104 Uiso 1 1 calc R . . C46 C 0.2325(5) 0.0076(8) 0.5030(5) 0.036(2) Uani 1 1 d . . . C47 C 0.1974(6) 0.0190(10) 0.4555(6) 0.051(3) Uani 1 1 d . . . H47 H 0.1626 0.0624 0.4557 0.061 Uiso 1 1 calc R . . C48 C 0.2149(6) -0.0358(11) 0.4069(8) 0.069(5) Uani 1 1 d . . . H48 H 0.1896 -0.0314 0.3753 0.083 Uiso 1 1 calc R . . C49 C 0.2670(5) -0.0953(10) 0.4034(6) 0.051(3) Uani 1 1 d . . . H49 H 0.2778 -0.1304 0.3702 0.061 Uiso 1 1 calc R . . C50 C 0.3050(5) -0.1022(8) 0.4529(6) 0.041(3) Uani 1 1 d . . . C51 C 0.2884(5) -0.0513(8) 0.5038(5) 0.032(2) Uani 1 1 d . . . C52 C 0.3588(5) -0.1705(8) 0.4471(5) 0.033(2) Uani 1 1 d . . . H52 H 0.3632 -0.2088 0.4136 0.040 Uiso 1 1 calc R . . C53 C 0.4502(4) -0.2573(7) 0.4753(5) 0.029(2) Uani 1 1 d . . . C54 C 0.4788(5) -0.2668(8) 0.4230(5) 0.040(3) Uani 1 1 d . . . H54 H 0.4663 -0.2238 0.3930 0.049 Uiso 1 1 calc R . . C55 C 0.5268(6) -0.3422(10) 0.4157(6) 0.052(3) Uani 1 1 d . . . H55 H 0.5466 -0.3498 0.3812 0.062 Uiso 1 1 calc R . . C56 C 0.5433(5) -0.4039(9) 0.4614(7) 0.052(4) Uani 1 1 d . . . H56 H 0.5751 -0.4532 0.4573 0.062 Uiso 1 1 calc R . . C57 C 0.5143(5) -0.3957(8) 0.5143(6) 0.047(3) Uani 1 1 d . . . H57 H 0.5263 -0.4387 0.5444 0.056 Uiso 1 1 calc R . . C58 C 0.4669(4) -0.3209(7) 0.5200(5) 0.031(2) Uani 1 1 d . . . C59 C 0.4188(5) -0.3821(8) 0.6019(5) 0.038(3) Uani 1 1 d . . . H59 H 0.4332 -0.4495 0.5911 0.046 Uiso 1 1 calc R . . C60 C 0.3802(6) -0.3772(8) 0.6512(5) 0.045(3) Uani 1 1 d . . . C61 C 0.3682(7) -0.4794(10) 0.6787(6) 0.063(4) Uani 1 1 d . . . H61 H 0.3874 -0.5412 0.6655 0.075 Uiso 1 1 calc R . . C62 C 0.3297(7) -0.4861(12) 0.7228(6) 0.068(4) Uani 1 1 d . . . H62 H 0.3238 -0.5513 0.7413 0.082 Uiso 1 1 calc R . . C63 C 0.2983(6) -0.3928(11) 0.7407(5) 0.058(4) Uani 1 1 d . . . H63 H 0.2707 -0.3978 0.7705 0.070 Uiso 1 1 calc R . . C64 C 0.3075(5) -0.2948(10) 0.7154(5) 0.043(3) Uani 1 1 d . . . C65 C 0.3493(5) -0.2850(9) 0.6690(5) 0.038(3) Uani 1 1 d . . . C66 C 0.2341(7) -0.2020(14) 0.7721(6) 0.076(5) Uani 1 1 d . . . H66A H 0.2192 -0.1303 0.7786 0.114 Uiso 1 1 calc R . . H66B H 0.2510 -0.2302 0.8065 0.114 Uiso 1 1 calc R . . H66C H 0.2009 -0.2470 0.7598 0.114 Uiso 1 1 calc R . . O1 O 0.4624(4) 0.3570(6) 0.4603(4) 0.054(2) Uani 1 1 d . . . O2 O 0.5434(3) 0.2215(5) 0.4963(3) 0.0348(17) Uani 1 1 d . . . O3 O 0.5426(4) 0.1271(6) 0.6149(4) 0.0428(19) Uani 1 1 d . . . O4 O 0.4785(4) 0.2152(6) 0.6971(4) 0.056(2) Uani 1 1 d . . . O5 O 0.3646(4) 0.1828(6) 0.5697(4) 0.051(2) Uani 1 1 d . . . O6 O 0.4484(3) 0.0486(4) 0.5289(5) 0.0304(14) Uani 1 1 d . . . O7 O 0.5195(3) -0.1058(4) 0.5714(3) 0.0295(18) Uani 1 1 d . . . O8 O 0.4913(4) -0.1649(6) 0.6709(4) 0.048(2) Uani 1 1 d . . . O9 O 0.2199(4) 0.0545(6) 0.5531(4) 0.051(2) Uani 1 1 d . . . O10 O 0.3213(3) -0.0581(5) 0.5492(3) 0.0375(19) Uani 1 1 d . . . O11 O 0.3566(3) -0.1902(6) 0.6462(3) 0.0410(18) Uani 1 1 d . . . O12 O 0.2799(4) -0.1996(8) 0.7304(4) 0.062(2) Uani 1 1 d . . . O13 O 0.4085(4) 0.0285(6) 0.6539(4) 0.051(2) Uani 1 1 d D . . H13A H 0.3817 0.0422 0.6286 0.077 Uiso 1 1 d RD . . H13B H 0.3927 0.0086 0.6851 0.077 Uiso 1 1 d RD . . O14 O 0.2813(4) 0.0090(8) 0.6646(5) 0.075(3) Uani 1 1 d D . . H14B H 0.2717 0.0531 0.6386 0.113 Uiso 1 1 d RD . . H14A H 0.3088 -0.0384 0.6501 0.113 Uiso 1 1 d RD . . O15 O 0.4843(6) 0.3570(7) 0.5889(6) 0.091(4) Uani 1 1 d D . . H15A H 0.4818 0.3351 0.5539 0.137 Uiso 1 1 d RD . . H15B H 0.4700 0.3146 0.6103 0.137 Uiso 1 1 d RD . . Dy1 Dy 0.555262(17) 0.05360(3) 0.52937(2) 0.02523(11) Uani 1 1 d . . . Dy2 Dy 0.413320(18) -0.10587(3) 0.58191(2) 0.02699(12) Uani 1 1 d . . . N1 N 0.6517(4) 0.1061(6) 0.4774(4) 0.0310(19) Uani 1 1 d . . . N2 N 0.6537(3) 0.0295(6) 0.5833(5) 0.0319(18) Uani 1 1 d . . . N3 N 0.5235(4) 0.0128(6) 0.4297(4) 0.033(2) Uani 1 1 d . . . N4 N 0.5997(4) -0.1172(6) 0.4821(4) 0.032(2) Uani 1 1 d . . . N5 N 0.4014(4) -0.1820(6) 0.4854(4) 0.0317(19) Uani 1 1 d . . . N6 N 0.4351(4) -0.3018(6) 0.5715(4) 0.034(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.046(8) 0.039(6) 0.136(18) 0.021(9) -0.014(9) 0.007(6) C2 0.042(6) 0.026(5) 0.051(7) 0.003(5) -0.001(6) 0.001(5) C3 0.041(6) 0.036(6) 0.055(8) 0.007(6) -0.003(6) 0.002(5) C4 0.086(11) 0.052(7) 0.049(8) 0.003(7) -0.006(8) -0.020(7) C5 0.049(7) 0.046(6) 0.043(7) 0.002(6) 0.002(6) -0.001(6) C6 0.045(6) 0.028(5) 0.044(7) -0.001(5) 0.005(6) -0.011(5) C7 0.038(6) 0.026(5) 0.037(6) -0.001(5) -0.002(5) -0.014(4) C8 0.037(6) 0.049(6) 0.040(7) -0.013(6) 0.008(5) -0.019(5) C9 0.024(5) 0.040(6) 0.044(7) -0.012(5) 0.004(5) -0.003(4) C10 0.044(7) 0.048(6) 0.060(8) -0.012(6) -0.004(6) -0.010(6) C11 0.026(6) 0.049(7) 0.094(12) -0.033(8) 0.001(7) -0.005(5) C12 0.031(6) 0.062(7) 0.084(12) -0.014(9) 0.000(8) 0.017(5) C13 0.028(6) 0.060(7) 0.090(12) -0.026(7) -0.007(6) 0.003(5) C14 0.019(5) 0.040(5) 0.065(9) -0.021(6) -0.002(5) -0.002(4) C15 0.035(6) 0.053(7) 0.064(9) -0.007(7) -0.014(7) 0.015(5) C16 0.044(7) 0.039(6) 0.039(7) -0.012(5) -0.018(6) 0.000(5) C17 0.058(8) 0.069(8) 0.037(7) 0.002(6) -0.017(7) 0.010(7) C18 0.065(9) 0.104(12) 0.032(7) 0.004(8) -0.003(7) -0.012(9) C19 0.067(10) 0.092(11) 0.040(8) -0.007(8) 0.008(7) -0.007(8) C20 0.044(6) 0.036(5) 0.041(7) 0.001(5) 0.001(6) -0.002(5) C21 0.046(6) 0.028(5) 0.039(7) -0.005(5) 0.002(6) -0.004(5) C22 0.101(13) 0.119(14) 0.063(11) 0.011(11) 0.033(10) 0.055(11) C23 0.067(8) 0.057(7) 0.088(14) -0.019(9) 0.009(9) 0.031(7) C24 0.027(5) 0.027(5) 0.058(8) 0.011(5) -0.001(5) 0.005(4) C25 0.035(6) 0.037(6) 0.075(10) 0.028(7) -0.007(7) 0.010(5) C26 0.048(7) 0.058(7) 0.055(9) 0.025(7) -0.017(7) 0.005(6) C27 0.041(7) 0.052(6) 0.048(7) 0.015(6) -0.014(6) 0.002(6) C28 0.034(6) 0.024(5) 0.044(7) -0.001(5) -0.009(5) -0.004(4) C29 0.022(5) 0.020(4) 0.042(7) 0.007(5) -0.004(5) -0.003(4) C30 0.046(7) 0.032(5) 0.042(7) 0.010(5) -0.004(6) -0.002(5) C31 0.040(6) 0.040(5) 0.033(6) -0.009(5) 0.008(5) -0.007(5) C32 0.055(8) 0.075(9) 0.050(8) 0.013(8) 0.010(7) 0.004(7) C33 0.081(12) 0.104(13) 0.042(8) 0.015(8) 0.014(8) 0.015(10) C34 0.054(8) 0.098(11) 0.052(9) -0.022(8) 0.023(8) -0.007(8) C35 0.043(7) 0.059(7) 0.061(9) -0.016(7) 0.006(7) -0.002(6) C36 0.030(5) 0.032(5) 0.039(6) 0.002(5) 0.004(5) -0.007(4) C37 0.022(5) 0.039(5) 0.041(6) -0.009(5) 0.003(5) -0.003(4) C38 0.029(5) 0.034(5) 0.049(8) 0.002(5) -0.008(5) -0.002(4) C39 0.041(6) 0.044(5) 0.056(9) 0.018(6) 0.005(6) 0.012(5) C40 0.055(8) 0.068(8) 0.056(9) 0.019(7) 0.000(7) 0.040(7) C41 0.070(9) 0.067(8) 0.040(7) 0.020(7) -0.019(7) 0.010(7) C42 0.033(6) 0.036(5) 0.043(7) 0.012(5) -0.004(5) 0.001(4) C43 0.024(5) 0.022(4) 0.045(7) 0.000(5) -0.006(5) 0.001(4) C44 0.074(10) 0.130(14) 0.031(7) -0.002(9) 0.001(8) 0.007(10) C45 0.044(7) 0.087(10) 0.077(11) -0.001(8) 0.000(7) 0.025(7) C46 0.033(6) 0.036(5) 0.038(6) 0.003(5) -0.011(5) -0.003(5) C47 0.042(7) 0.053(7) 0.058(8) 0.012(7) -0.001(7) -0.010(6) C48 0.053(8) 0.069(8) 0.086(12) 0.026(9) -0.038(9) -0.003(7) C49 0.041(7) 0.070(7) 0.042(7) 0.002(6) -0.018(6) -0.001(6) C50 0.036(6) 0.038(6) 0.050(7) 0.019(6) -0.014(6) -0.013(5) C51 0.036(6) 0.031(5) 0.029(5) 0.006(5) 0.005(5) -0.008(4) C52 0.028(5) 0.042(5) 0.031(6) 0.007(5) -0.007(5) -0.002(5) C53 0.027(5) 0.022(4) 0.038(6) -0.005(5) 0.000(5) 0.000(4) C54 0.038(6) 0.042(5) 0.042(7) -0.002(6) 0.010(6) -0.004(5) C55 0.050(7) 0.052(7) 0.053(8) -0.017(7) 0.010(7) -0.013(6) C56 0.034(6) 0.039(6) 0.083(11) -0.019(7) 0.003(7) 0.001(5) C57 0.036(6) 0.036(5) 0.068(10) -0.005(6) -0.016(6) -0.011(5) C58 0.027(5) 0.025(4) 0.041(7) -0.010(5) 0.005(5) -0.002(4) C59 0.052(7) 0.027(5) 0.036(6) -0.011(5) -0.007(5) 0.003(5) C60 0.053(7) 0.039(6) 0.044(7) 0.016(6) -0.009(6) -0.015(5) C61 0.090(11) 0.042(6) 0.056(9) 0.018(7) -0.011(8) -0.018(7) C62 0.092(11) 0.064(8) 0.050(9) 0.018(8) -0.002(9) -0.020(8) C63 0.057(8) 0.091(10) 0.027(6) 0.021(7) -0.001(6) -0.034(7) C64 0.042(6) 0.059(7) 0.028(6) 0.014(6) -0.004(5) -0.018(6) C65 0.031(5) 0.047(6) 0.036(6) 0.020(5) -0.001(5) -0.005(5) C66 0.063(9) 0.120(13) 0.045(8) 0.017(9) 0.028(8) 0.019(9) O1 0.056(5) 0.037(4) 0.067(6) 0.015(4) 0.001(5) 0.016(4) O2 0.041(4) 0.026(3) 0.037(4) 0.008(3) 0.004(4) 0.005(3) O3 0.044(4) 0.048(4) 0.036(5) 0.000(4) -0.009(4) 0.011(4) O4 0.058(5) 0.062(5) 0.047(5) -0.003(5) 0.007(5) 0.019(4) O5 0.042(4) 0.047(4) 0.063(7) -0.002(5) 0.010(4) 0.014(4) O6 0.025(3) 0.032(3) 0.034(4) 0.005(4) 0.001(4) 0.002(3) O7 0.021(3) 0.028(3) 0.039(5) 0.010(3) -0.002(3) 0.007(3) O8 0.053(5) 0.056(5) 0.036(5) 0.007(4) 0.003(4) 0.012(4) O9 0.032(4) 0.058(5) 0.064(6) 0.004(4) -0.006(4) 0.015(4) O10 0.022(3) 0.043(4) 0.048(5) 0.009(3) -0.004(3) 0.001(3) O11 0.034(4) 0.045(4) 0.044(5) 0.008(4) 0.011(4) -0.003(3) O12 0.046(5) 0.089(6) 0.053(6) 0.008(5) 0.018(5) -0.002(5) O13 0.073(6) 0.049(4) 0.032(5) -0.010(4) -0.005(5) 0.003(4) O14 0.071(6) 0.075(6) 0.080(8) 0.008(6) 0.023(6) 0.027(5) O15 0.137(10) 0.055(5) 0.082(8) 0.002(7) 0.006(9) 0.010(6) Dy1 0.02098(19) 0.02524(19) 0.0295(2) 0.0002(2) -0.0019(2) -0.00125(17) Dy2 0.0234(2) 0.0280(2) 0.0296(2) 0.0026(2) 0.0008(2) -0.00032(17) N1 0.025(4) 0.032(4) 0.036(5) 0.001(4) 0.001(4) -0.005(4) N2 0.023(4) 0.033(4) 0.039(5) -0.005(5) -0.005(5) 0.005(3) N3 0.041(5) 0.027(4) 0.031(5) 0.002(4) -0.003(4) -0.007(4) N4 0.023(4) 0.036(4) 0.037(5) 0.007(4) -0.002(4) 0.002(3) N5 0.041(5) 0.022(4) 0.033(5) 0.006(4) 0.008(4) -0.005(4) N6 0.030(4) 0.024(4) 0.048(7) 0.002(4) -0.004(4) -0.003(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 C1 O1 1.470(14) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.359(17) . ? C2 O1 1.376(14) . ? C2 C7 1.421(15) . ? C3 C4 1.385(19) . ? C3 H3 0.9300 . ? C4 C5 1.373(18) . ? C4 H4 0.9300 . ? C5 C6 1.402(16) . ? C5 H5 0.9300 . ? C6 C7 1.391(15) . ? C6 C8 1.456(16) . ? C7 O2 1.293(13) . ? C8 N1 1.267(14) . ? C8 H8 0.9300 . ? C9 C14 1.378(17) . ? C9 C10 1.396(16) . ? C9 N1 1.423(13) . ? C10 C11 1.392(17) . ? C10 H10 0.9300 . ? C11 C12 1.35(2) . ? C11 H11 0.9300 . ? C12 C13 1.364(19) . ? C12 H12 0.9300 . ? C13 C14 1.436(16) . ? C13 H13 0.9300 . ? C14 N2 1.443(14) . ? C15 N2 1.235(18) . ? C15 C16 1.438(18) . ? C15 H15 0.9300 . ? C16 C17 1.401(16) . ? C16 C21 1.435(16) . ? C17 C18 1.37(2) . ? C17 H17 0.9300 . ? C18 C19 1.36(2) . ? C18 H18 0.9300 . ? C19 C20 1.377(19) . ? C19 H19 0.9300 . ? C20 O4 1.387(13) . ? C20 C21 1.444(17) . ? C21 O3 1.299(14) . ? C22 O4 1.419(17) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O5 1.435(13) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O5 1.350(15) . ? C24 C25 1.381(16) . ? C24 C29 1.410(14) . ? C25 C26 1.34(2) . ? C25 H25 0.9300 . ? C26 C27 1.358(18) . ? C26 H26 0.9300 . ? C27 C28 1.412(15) . ? C27 H27 0.9300 . ? C28 C29 1.382(16) . ? C28 C30 1.465(16) . ? C29 O6 1.340(13) . ? C30 N3 1.307(14) . ? C30 H30 0.9300 . ? C31 C32 1.380(18) . ? C31 C36 1.414(16) . ? C31 N3 1.431(14) . ? C32 C33 1.40(2) . ? C32 H32 0.9300 . ? C33 C34 1.31(2) . ? C33 H33 0.9300 . ? C34 C35 1.42(2) . ? C34 H34 0.9300 . ? C35 C36 1.384(16) . ? C35 H35 0.9300 . ? C36 N4 1.389(14) . ? C37 N4 1.283(13) . ? C37 C38 1.453(15) . ? C37 H37 0.9300 . ? C38 C43 1.392(14) . ? C38 C39 1.407(15) . ? C39 C40 1.357(18) . ? C39 H39 0.9300 . ? C40 C41 1.378(18) . ? C40 H40 0.9300 . ? C41 C42 1.391(15) . ? C41 H41 0.9300 . ? C42 C43 1.372(16) . ? C42 O8 1.375(13) . ? C43 O7 1.342(11) . ? C44 O8 1.393(16) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 O9 1.438(14) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 O9 1.352(14) . ? C46 C47 1.370(17) . ? C46 C51 1.420(15) . ? C47 C48 1.39(2) . ? C47 H47 0.9300 . ? C48 C49 1.358(19) . ? C48 H48 0.9300 . ? C49 C50 1.439(16) . ? C49 H49 0.9300 . ? C50 C51 1.410(17) . ? C50 C52 1.452(15) . ? C51 O10 1.296(12) . ? C52 N5 1.307(13) . ? C52 H52 0.9300 . ? C53 C58 1.372(15) . ? C53 C54 1.393(16) . ? C53 N5 1.435(12) . ? C54 C55 1.416(16) . ? C54 H54 0.9300 . ? C55 C56 1.38(2) . ? C55 H55 0.9300 . ? C56 C57 1.41(2) . ? C56 H56 0.9300 . ? C57 C58 1.395(14) . ? C57 H57 0.9300 . ? C58 N6 1.424(14) . ? C59 N6 1.280(14) . ? C59 C60 1.444(17) . ? C59 H59 0.9300 . ? C60 C65 1.394(16) . ? C60 C61 1.450(16) . ? C61 C62 1.34(2) . ? C61 H61 0.9300 . ? C62 C63 1.41(2) . ? C62 H62 0.9300 . ? C63 C64 1.373(16) . ? C63 H63 0.9300 . ? C64 O12 1.374(15) . ? C64 C65 1.433(15) . ? C65 O11 1.306(12) . ? C66 O12 1.405(15) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? O2 Dy1 2.244(6) . ? O3 Dy1 2.242(8) . ? O6 Dy1 2.328(6) . ? O6 Dy2 2.419(7) . ? O7 Dy2 2.326(6) . ? O7 Dy1 2.350(6) . ? O8 Dy2 2.807(8) . ? O10 Dy2 2.229(7) . ? O11 Dy2 2.224(7) . ? O13 Dy2 2.391(8) . ? O13 H13A 0.8559 . ? O13 H13B 0.8513 . ? O14 H14B 0.8519 . ? O14 H14A 0.9084 . ? O15 H15A 0.8757 . ? O15 H15B 0.7950 . ? Dy1 N2 2.514(9) . ? Dy1 N3 2.516(9) . ? Dy1 N1 2.520(9) . ? Dy1 N4 2.589(9) . ? Dy1 Dy2 3.8770(13) . ? Dy2 N5 2.490(9) . ? Dy2 N6 2.492(8) . ? Dy2 H13A 2.2552 . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 126.8(10) . . ? C3 C2 C7 120.9(11) . . ? O1 C2 C7 112.2(10) . . ? C2 C3 C4 120.8(11) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.4(13) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.8(12) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 119.9(10) . . ? C7 C6 C8 123.5(11) . . ? C5 C6 C8 116.6(10) . . ? O2 C7 C6 122.5(10) . . ? O2 C7 C2 119.6(10) . . ? C6 C7 C2 117.9(11) . . ? N1 C8 C6 125.9(10) . . ? N1 C8 H8 117.0 . . ? C6 C8 H8 117.0 . . ? C14 C9 C10 118.4(11) . . ? C14 C9 N1 115.7(10) . . ? C10 C9 N1 125.3(11) . . ? C11 C10 C9 120.8(14) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.5(13) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.9(12) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 119.4(15) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C9 C14 C13 119.9(11) . . ? C9 C14 N2 118.7(10) . . ? C13 C14 N2 121.0(12) . . ? N2 C15 C16 129.9(11) . . ? N2 C15 H15 115.1 . . ? C16 C15 H15 115.1 . . ? C17 C16 C21 119.7(12) . . ? C17 C16 C15 120.9(11) . . ? C21 C16 C15 119.3(11) . . ? C18 C17 C16 122.4(12) . . ? C18 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? C19 C18 C17 119.6(13) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.7(14) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 O4 124.5(12) . . ? C19 C20 C21 122.4(12) . . ? O4 C20 C21 113.1(10) . . ? O3 C21 C16 125.3(11) . . ? O3 C21 C20 119.6(10) . . ? C16 C21 C20 115.1(11) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C25 126.2(11) . . ? O5 C24 C29 115.5(10) . . ? C25 C24 C29 118.3(12) . . ? C26 C25 C24 122.9(12) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C25 C26 C27 120.9(12) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C28 117.9(12) . . ? C26 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C29 C28 C27 122.0(10) . . ? C29 C28 C30 123.9(10) . . ? C27 C28 C30 114.1(11) . . ? O6 C29 C28 122.8(9) . . ? O6 C29 C24 119.4(11) . . ? C28 C29 C24 117.7(10) . . ? N3 C30 C28 127.3(12) . . ? N3 C30 H30 116.4 . . ? C28 C30 H30 116.4 . . ? C32 C31 C36 122.4(11) . . ? C32 C31 N3 122.6(11) . . ? C36 C31 N3 114.9(10) . . ? C31 C32 C33 119.2(13) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 120.3(15) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.6(14) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 122.2(13) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C35 C36 N4 128.7(11) . . ? C35 C36 C31 115.2(12) . . ? N4 C36 C31 116.0(9) . . ? N4 C37 C38 122.1(11) . . ? N4 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C43 C38 C39 118.1(11) . . ? C43 C38 C37 123.8(10) . . ? C39 C38 C37 117.8(11) . . ? C40 C39 C38 120.2(11) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 122.2(11) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C40 C41 C42 117.8(12) . . ? C40 C41 H41 121.1 . . ? C42 C41 H41 121.1 . . ? C43 C42 O8 113.1(9) . . ? C43 C42 C41 121.2(11) . . ? O8 C42 C41 125.7(11) . . ? O7 C43 C42 118.2(9) . . ? O7 C43 C38 121.3(10) . . ? C42 C43 C38 120.4(9) . . ? O8 C44 H44A 109.5 . . ? O8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O9 C45 H45A 109.5 . . ? O9 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O9 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O9 C46 C47 124.4(11) . . ? O9 C46 C51 112.6(9) . . ? C47 C46 C51 122.9(12) . . ? C46 C47 C48 118.6(12) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C49 C48 C47 123.1(14) . . ? C49 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C48 C49 C50 117.6(13) . . ? C48 C49 H49 121.2 . . ? C50 C49 H49 121.2 . . ? C51 C50 C49 121.6(11) . . ? C51 C50 C52 123.4(10) . . ? C49 C50 C52 114.9(12) . . ? O10 C51 C50 122.8(10) . . ? O10 C51 C46 121.2(10) . . ? C50 C51 C46 116.1(10) . . ? N5 C52 C50 124.8(11) . . ? N5 C52 H52 117.6 . . ? C50 C52 H52 117.6 . . ? C58 C53 C54 121.4(9) . . ? C58 C53 N5 116.3(9) . . ? C54 C53 N5 122.3(10) . . ? C53 C54 C55 119.6(11) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 117.8(12) . . ? C56 C55 H55 121.1 . . ? C54 C55 H55 121.1 . . ? C55 C56 C57 123.0(11) . . ? C55 C56 H56 118.5 . . ? C57 C56 H56 118.5 . . ? C58 C57 C56 117.8(12) . . ? C58 C57 H57 121.1 . . ? C56 C57 H57 121.1 . . ? C53 C58 C57 120.4(11) . . ? C53 C58 N6 116.0(8) . . ? C57 C58 N6 123.6(11) . . ? N6 C59 C60 125.8(10) . . ? N6 C59 H59 117.1 . . ? C60 C59 H59 117.1 . . ? C65 C60 C59 124.1(10) . . ? C65 C60 C61 119.8(12) . . ? C59 C60 C61 115.7(12) . . ? C62 C61 C60 121.1(14) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? C61 C62 C63 119.0(13) . . ? C61 C62 H62 120.5 . . ? C63 C62 H62 120.5 . . ? C64 C63 C62 121.8(13) . . ? C64 C63 H63 119.1 . . ? C62 C63 H63 119.1 . . ? C63 C64 O12 125.9(11) . . ? C63 C64 C65 120.3(12) . . ? O12 C64 C65 113.8(9) . . ? O11 C65 C60 123.9(10) . . ? O11 C65 C64 118.2(10) . . ? C60 C65 C64 117.9(10) . . ? O12 C66 H66A 109.5 . . ? O12 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O12 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C2 O1 C1 117.4(11) . . ? C7 O2 Dy1 131.9(6) . . ? C21 O3 Dy1 138.3(7) . . ? C20 O4 C22 117.2(11) . . ? C24 O5 C23 119.3(11) . . ? C29 O6 Dy1 124.2(6) . . ? C29 O6 Dy2 123.8(5) . . ? Dy1 O6 Dy2 109.5(3) . . ? C43 O7 Dy2 124.9(6) . . ? C43 O7 Dy1 121.7(5) . . ? Dy2 O7 Dy1 112.0(2) . . ? C42 O8 C44 119.9(10) . . ? C42 O8 Dy2 110.4(7) . . ? C44 O8 Dy2 128.8(8) . . ? C46 O9 C45 116.8(10) . . ? C51 O10 Dy2 143.4(7) . . ? C65 O11 Dy2 140.9(7) . . ? C64 O12 C66 118.4(10) . . ? Dy2 O13 H13A 70.5 . . ? Dy2 O13 H13B 115.7 . . ? H13A O13 H13B 113.1 . . ? H14B O14 H14A 107.7 . . ? H15A O15 H15B 112.1 . . ? O3 Dy1 O2 85.6(3) . . ? O3 Dy1 O6 83.8(3) . . ? O2 Dy1 O6 84.7(2) . . ? O3 Dy1 O7 85.3(3) . . ? O2 Dy1 O7 153.4(2) . . ? O6 Dy1 O7 69.4(2) . . ? O3 Dy1 N2 72.1(3) . . ? O2 Dy1 N2 112.8(3) . . ? O6 Dy1 N2 148.4(3) . . ? O7 Dy1 N2 88.0(2) . . ? O3 Dy1 N3 154.0(3) . . ? O2 Dy1 N3 80.0(3) . . ? O6 Dy1 N3 73.5(3) . . ? O7 Dy1 N3 97.9(3) . . ? N2 Dy1 N3 133.5(3) . . ? O3 Dy1 N1 116.1(3) . . ? O2 Dy1 N1 71.6(3) . . ? O6 Dy1 N1 146.8(3) . . ? O7 Dy1 N1 134.6(2) . . ? N2 Dy1 N1 64.5(3) . . ? N3 Dy1 N1 79.7(3) . . ? O3 Dy1 N4 140.6(3) . . ? O2 Dy1 N4 130.8(3) . . ? O6 Dy1 N4 110.5(3) . . ? O7 Dy1 N4 67.5(2) . . ? N2 Dy1 N4 78.7(3) . . ? N3 Dy1 N4 61.9(3) . . ? N1 Dy1 N4 71.9(3) . . ? O3 Dy1 Dy2 79.6(2) . . ? O2 Dy1 Dy2 119.71(18) . . ? O6 Dy1 Dy2 36.02(19) . . ? O7 Dy1 Dy2 33.79(14) . . ? N2 Dy1 Dy2 117.1(2) . . ? N3 Dy1 Dy2 88.85(19) . . ? N1 Dy1 Dy2 162.46(18) . . ? N4 Dy1 Dy2 91.04(18) . . ? O11 Dy2 O10 82.2(3) . . ? O11 Dy2 O7 128.7(3) . . ? O10 Dy2 O7 148.9(3) . . ? O11 Dy2 O13 79.3(3) . . ? O10 Dy2 O13 91.3(3) . . ? O7 Dy2 O13 96.9(3) . . ? O11 Dy2 O6 154.9(3) . . ? O10 Dy2 O6 83.8(2) . . ? O7 Dy2 O6 68.3(2) . . ? O13 Dy2 O6 80.3(3) . . ? O11 Dy2 N5 113.2(3) . . ? O10 Dy2 N5 71.8(3) . . ? O7 Dy2 N5 90.3(3) . . ? O13 Dy2 N5 156.5(3) . . ? O6 Dy2 N5 81.7(3) . . ? O11 Dy2 N6 73.3(3) . . ? O10 Dy2 N6 113.4(3) . . ? O7 Dy2 N6 78.5(2) . . ? O13 Dy2 N6 139.6(3) . . ? O6 Dy2 N6 131.6(3) . . ? N5 Dy2 N6 63.8(3) . . ? O11 Dy2 O8 72.4(3) . . ? O10 Dy2 O8 151.0(3) . . ? O7 Dy2 O8 58.6(2) . . ? O13 Dy2 O8 70.8(3) . . ? O6 Dy2 O8 114.0(3) . . ? N5 Dy2 O8 130.9(3) . . ? N6 Dy2 O8 72.8(3) . . ? O11 Dy2 Dy1 154.6(2) . . ? O10 Dy2 Dy1 117.95(18) . . ? O7 Dy2 Dy1 34.19(14) . . ? O13 Dy2 Dy1 84.7(2) . . ? O6 Dy2 Dy1 34.47(14) . . ? N5 Dy2 Dy1 88.95(18) . . ? N6 Dy2 Dy1 108.41(19) . . ? O8 Dy2 Dy1 83.86(17) . . ? O11 Dy2 H13A 83.0 . . ? O10 Dy2 H13A 71.3 . . ? O7 Dy2 H13A 110.9 . . ? O13 Dy2 H13A 21.0 . . ? O6 Dy2 H13A 72.8 . . ? N5 Dy2 H13A 136.8 . . ? N6 Dy2 H13A 154.7 . . ? O8 Dy2 H13A 91.7 . . ? Dy1 Dy2 H13A 89.1 . . ? C8 N1 C9 120.0(10) . . ? C8 N1 Dy1 126.2(7) . . ? C9 N1 Dy1 112.8(6) . . ? C15 N2 C14 120.4(10) . . ? C15 N2 Dy1 129.0(8) . . ? C14 N2 Dy1 110.4(7) . . ? C30 N3 C31 120.2(10) . . ? C30 N3 Dy1 125.0(8) . . ? C31 N3 Dy1 114.5(7) . . ? C37 N4 C36 119.4(9) . . ? C37 N4 Dy1 125.7(8) . . ? C36 N4 Dy1 114.3(6) . . ? C52 N5 C53 118.7(9) . . ? C52 N5 Dy2 132.2(7) . . ? C53 N5 Dy2 108.9(7) . . ? C59 N6 C58 119.1(9) . . ? C59 N6 Dy2 130.8(8) . . ? C58 N6 Dy2 109.9(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.191 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 931253' ####################################################################### # # 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_4 #TrackingRef 'complexes.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H60 Gd2 N6 O15' _chemical_formula_weight 1491.70 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.8735(13) _cell_length_b 12.4022(7) _cell_length_c 23.7390(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6439.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6678 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.57 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 2.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6203 _exptl_absorpt_correction_T_max 0.6774 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2141 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 36201 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.57 _reflns_number_total 13994 _reflns_number_gt 12689 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+7.3532P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.938(13) _refine_ls_number_reflns 13994 _refine_ls_number_parameters 808 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 C1 C 1.2668(5) -0.2079(12) 0.1198(4) 0.086(4) Uani 1 1 d . . . H1A H 1.3013 -0.2473 0.1340 0.129 Uiso 1 1 calc R . . H1B H 1.2792 -0.1358 0.1105 0.129 Uiso 1 1 calc R . . H1C H 1.2515 -0.2430 0.0867 0.129 Uiso 1 1 calc R . . C2 C 1.1927(4) -0.3000(8) 0.1760(3) 0.053(2) Uani 1 1 d . . . C3 C 1.2008(5) -0.4012(10) 0.1513(4) 0.072(3) Uani 1 1 d . . . H3 H 1.2287 -0.4077 0.1219 0.086 Uiso 1 1 calc R . . C4 C 1.1693(5) -0.4918(9) 0.1686(4) 0.066(3) Uani 1 1 d . . . H4 H 1.1741 -0.5572 0.1499 0.079 Uiso 1 1 calc R . . C5 C 1.1322(5) -0.4829(8) 0.2124(4) 0.062(2) Uani 1 1 d . . . H5 H 1.1123 -0.5444 0.2252 0.074 Uiso 1 1 calc R . . C6 C 1.1508(3) -0.2883(6) 0.2221(3) 0.0398(16) Uani 1 1 d . . . C7 C 1.1210(4) -0.3822(6) 0.2413(3) 0.0444(18) Uani 1 1 d . . . C8 C 1.0819(3) -0.3847(6) 0.2900(3) 0.0405(17) Uani 1 1 d . . . H8 H 1.0661 -0.4513 0.3005 0.049 Uiso 1 1 calc R . . C9 C 1.0351(3) -0.3223(6) 0.3709(3) 0.0375(15) Uani 1 1 d . . . C10 C 0.9877(4) -0.3961(6) 0.3774(4) 0.0472(19) Uani 1 1 d . . . H10 H 0.9757 -0.4398 0.3475 0.057 Uiso 1 1 calc R . . C11 C 0.9583(4) -0.4033(7) 0.4301(5) 0.054(2) Uani 1 1 d . . . H11 H 0.9260 -0.4514 0.4345 0.065 Uiso 1 1 calc R . . C12 C 0.9760(4) -0.3418(8) 0.4747(4) 0.055(2) Uani 1 1 d . . . H12 H 0.9567 -0.3498 0.5093 0.066 Uiso 1 1 calc R . . C13 C 1.0228(4) -0.2672(7) 0.4685(3) 0.0450(17) Uani 1 1 d . . . H13 H 1.0341 -0.2236 0.4987 0.054 Uiso 1 1 calc R . . C14 C 1.0528(3) -0.2579(6) 0.4167(3) 0.0369(14) Uani 1 1 d . . . C15 C 1.1430(4) -0.1718(6) 0.4439(3) 0.0408(16) Uani 1 1 d . . . H15 H 1.1384 -0.2090 0.4777 0.049 Uiso 1 1 calc R . . C16 C 1.1962(4) -0.1054(6) 0.4383(4) 0.0446(18) Uani 1 1 d . . . C17 C 1.2350(4) -0.0957(9) 0.4877(4) 0.058(2) Uani 1 1 d . . . H17 H 1.2239 -0.1304 0.5209 0.070 Uiso 1 1 calc R . . C18 C 1.2864(4) -0.0377(8) 0.4861(5) 0.062(2) Uani 1 1 d . . . H18 H 1.3106 -0.0323 0.5182 0.074 Uiso 1 1 calc R . . C19 C 1.3043(4) 0.0151(8) 0.4366(4) 0.056(2) Uani 1 1 d . . . H19 H 1.3400 0.0558 0.4361 0.068 Uiso 1 1 calc R . . C20 C 1.2687(3) 0.0066(6) 0.3884(3) 0.0427(17) Uani 1 1 d . . . C21 C 1.2136(3) -0.0535(6) 0.3884(3) 0.0375(16) Uani 1 1 d . . . C22 C 1.3383(5) 0.1122(10) 0.3332(6) 0.081(4) Uani 1 1 d . . . H22A H 1.3396 0.1680 0.3612 0.121 Uiso 1 1 calc R . . H22B H 1.3407 0.1439 0.2964 0.121 Uiso 1 1 calc R . . H22C H 1.3721 0.0640 0.3386 0.121 Uiso 1 1 calc R . . C23 C 1.0228(6) -0.1772(13) 0.1641(4) 0.084(4) Uani 1 1 d . . . H23A H 1.0216 -0.2522 0.1542 0.126 Uiso 1 1 calc R . . H23B H 1.0629 -0.1490 0.1569 0.126 Uiso 1 1 calc R . . H23C H 0.9934 -0.1384 0.1421 0.126 Uiso 1 1 calc R . . C24 C 0.9558(4) -0.2060(7) 0.2418(3) 0.0451(18) Uani 1 1 d . . . C25 C 0.9178(5) -0.2783(9) 0.2134(4) 0.061(2) Uani 1 1 d . . . H25 H 0.9265 -0.2986 0.1765 0.074 Uiso 1 1 calc R . . C26 C 0.8667(4) -0.3197(9) 0.2409(4) 0.068(3) Uani 1 1 d . . . H26 H 0.8407 -0.3668 0.2221 0.082 Uiso 1 1 calc R . . C27 C 0.8547(4) -0.2916(7) 0.2952(4) 0.052(2) Uani 1 1 d . . . H27 H 0.8208 -0.3208 0.3133 0.062 Uiso 1 1 calc R . . C28 C 0.8927(4) -0.2191(6) 0.3243(3) 0.0427(18) Uani 1 1 d . . . C29 C 0.9431(3) -0.1735(5) 0.2970(3) 0.0351(15) Uani 1 1 d . . . C30 C 0.8819(3) -0.1997(6) 0.3837(3) 0.0390(16) Uani 1 1 d . . . H30 H 0.8597 -0.2507 0.4038 0.047 Uiso 1 1 calc R . . C31 C 0.8915(4) -0.1048(6) 0.4688(3) 0.0387(15) Uani 1 1 d . . . C32 C 0.8451(4) -0.1523(8) 0.4988(4) 0.056(2) Uani 1 1 d . . . H32 H 0.8199 -0.2027 0.4815 0.067 Uiso 1 1 calc R . . C33 C 0.8358(5) -0.1255(11) 0.5552(4) 0.076(3) Uani 1 1 d . . . H33 H 0.8041 -0.1574 0.5752 0.091 Uiso 1 1 calc R . . C34 C 0.8727(7) -0.0531(12) 0.5810(4) 0.089(4) Uani 1 1 d . . . H34 H 0.8651 -0.0333 0.6181 0.107 Uiso 1 1 calc R . . C35 C 0.9227(5) -0.0074(10) 0.5521(4) 0.062(2) Uani 1 1 d . . . H35 H 0.9490 0.0398 0.5705 0.075 Uiso 1 1 calc R . . C36 C 0.9321(4) -0.0338(7) 0.4960(3) 0.0429(17) Uani 1 1 d . . . C37 C 1.0309(4) 0.0386(6) 0.4852(3) 0.0405(16) Uani 1 1 d . . . H37 H 1.0368 0.0187 0.5226 0.049 Uiso 1 1 calc R . . C38 C 1.0808(4) 0.0939(6) 0.4579(4) 0.0420(17) Uani 1 1 d . . . C39 C 1.1246(4) 0.1416(8) 0.4947(4) 0.055(2) Uani 1 1 d . . . H39 H 1.1210 0.1331 0.5335 0.066 Uiso 1 1 calc R . . C40 C 1.1717(4) 0.1992(8) 0.4731(4) 0.061(2) Uani 1 1 d . . . H40 H 1.2007 0.2287 0.4972 0.074 Uiso 1 1 calc R . . C41 C 1.1773(4) 0.2148(7) 0.4163(5) 0.056(2) Uani 1 1 d . . . H41 H 1.2092 0.2568 0.4024 0.068 Uiso 1 1 calc R . . C42 C 1.1357(3) 0.1684(6) 0.3792(3) 0.0408(17) Uani 1 1 d . . . C43 C 1.0882(3) 0.1032(5) 0.3997(4) 0.0373(16) Uani 1 1 d . . . C44 C 1.1785(5) 0.2578(8) 0.2988(6) 0.076(3) Uani 1 1 d . . . H44A H 1.1750 0.3246 0.3190 0.114 Uiso 1 1 calc R . . H44B H 1.1683 0.2694 0.2599 0.114 Uiso 1 1 calc R . . H44C H 1.2197 0.2316 0.3015 0.114 Uiso 1 1 calc R . . C45 C 1.0523(7) 0.2781(13) 0.1515(5) 0.098(5) Uani 1 1 d . . . H45A H 1.0727 0.2317 0.1251 0.147 Uiso 1 1 calc R . . H45B H 1.0818 0.3239 0.1695 0.147 Uiso 1 1 calc R . . H45C H 1.0228 0.3216 0.1320 0.147 Uiso 1 1 calc R . . C46 C 0.9681(4) 0.1611(7) 0.1779(4) 0.0515(19) Uani 1 1 d . . . C47 C 0.9477(5) 0.1479(11) 0.1232(4) 0.070(3) Uani 1 1 d . . . H47 H 0.9713 0.1733 0.0934 0.084 Uiso 1 1 calc R . . C48 C 0.8925(6) 0.0975(12) 0.1122(4) 0.083(4) Uani 1 1 d . . . H48 H 0.8786 0.0894 0.0754 0.100 Uiso 1 1 calc R . . C49 C 0.8590(5) 0.0598(9) 0.1566(4) 0.070(3) Uani 1 1 d . . . H49 H 0.8218 0.0263 0.1493 0.084 Uiso 1 1 calc R . . C50 C 0.8785(4) 0.0695(7) 0.2126(4) 0.053(2) Uani 1 1 d . . . C51 C 0.9353(4) 0.1185(6) 0.2243(3) 0.0429(17) Uani 1 1 d . . . C52 C 0.8374(4) 0.0386(8) 0.2556(4) 0.056(2) Uani 1 1 d . . . H52 H 0.7983 0.0198 0.2437 0.067 Uiso 1 1 calc R . . C53 C 0.7973(3) 0.0022(7) 0.3453(4) 0.0472(19) Uani 1 1 d . . . C54 C 0.7539(4) -0.0776(8) 0.3302(5) 0.059(2) Uani 1 1 d . . . H54 H 0.7537 -0.1062 0.2940 0.071 Uiso 1 1 calc R . . C55 C 0.7127(4) -0.1118(8) 0.3688(6) 0.069(3) Uani 1 1 d . . . H55 H 0.6846 -0.1648 0.3590 0.083 Uiso 1 1 calc R . . C56 C 0.7116(4) -0.0690(9) 0.4231(6) 0.067(3) Uani 1 1 d . . . H56 H 0.6825 -0.0920 0.4490 0.080 Uiso 1 1 calc R . . C57 C 0.7535(4) 0.0065(8) 0.4379(5) 0.061(2) Uani 1 1 d . . . H57 H 0.7525 0.0347 0.4742 0.073 Uiso 1 1 calc R . . C58 C 0.7983(4) 0.0434(6) 0.4001(4) 0.049(2) Uani 1 1 d . . . C59 C 0.8462(4) 0.1738(7) 0.4561(3) 0.0457(18) Uani 1 1 d . . . H59 H 0.8092 0.1773 0.4754 0.055 Uiso 1 1 calc R . . C60 C 0.8948(4) 0.2418(6) 0.4767(3) 0.0447(17) Uani 1 1 d . . . C61 C 0.8857(5) 0.2923(8) 0.5298(4) 0.060(2) Uani 1 1 d . . . H61 H 0.8497 0.2802 0.5497 0.072 Uiso 1 1 calc R . . C62 C 0.9295(6) 0.3585(9) 0.5517(4) 0.066(3) Uani 1 1 d . . . H62 H 0.9245 0.3878 0.5874 0.079 Uiso 1 1 calc R . . C63 C 0.9805(5) 0.3817(7) 0.5211(4) 0.060(2) Uani 1 1 d . . . H63 H 1.0096 0.4284 0.5360 0.072 Uiso 1 1 calc R . . C64 C 0.9899(4) 0.3375(6) 0.4687(4) 0.0477(18) Uani 1 1 d . . . C65 C 0.9473(3) 0.2656(6) 0.4453(3) 0.0399(16) Uani 1 1 d . . . C66 C 1.0852(5) 0.4310(8) 0.4538(6) 0.075(3) Uani 1 1 d . . . H66A H 1.0680 0.5013 0.4596 0.112 Uiso 1 1 calc R . . H66B H 1.1172 0.4353 0.4261 0.112 Uiso 1 1 calc R . . H66C H 1.1017 0.4045 0.4886 0.112 Uiso 1 1 calc R . . N1 N 1.0670(3) -0.3033(5) 0.3202(3) 0.0348(13) Uani 1 1 d . . . N2 N 1.1008(3) -0.1847(5) 0.4062(2) 0.0346(12) Uani 1 1 d . . . N3 N 0.9012(3) -0.1165(5) 0.4098(3) 0.0364(13) Uani 1 1 d . . . N4 N 0.9785(3) 0.0136(5) 0.4627(2) 0.0381(13) Uani 1 1 d . . . N5 N 0.8469(3) 0.0331(5) 0.3091(3) 0.0423(12) Uani 1 1 d . . . N6 N 0.8487(3) 0.1089(5) 0.4140(3) 0.0419(14) Uani 1 1 d . . . O1 O 1.2211(3) -0.2045(6) 0.1607(3) 0.0669(18) Uani 1 1 d . . . O2 O 1.1440(3) -0.1939(4) 0.2445(2) 0.0485(13) Uani 1 1 d . . . O3 O 1.1812(2) -0.0593(4) 0.3420(2) 0.0394(11) Uani 1 1 d . . . O4 O 1.2823(3) 0.0537(5) 0.3384(3) 0.0575(16) Uani 1 1 d . . . O5 O 1.0092(3) -0.1655(5) 0.2208(2) 0.0512(14) Uani 1 1 d . . . O6 O 0.9817(2) -0.1059(4) 0.3207(2) 0.0356(12) Uani 1 1 d . . . O7 O 1.05333(19) 0.0495(3) 0.3629(3) 0.0344(9) Uani 1 1 d . . . O8 O 1.1378(3) 0.1809(5) 0.3224(3) 0.0535(15) Uani 1 1 d . . . O9 O 1.0220(3) 0.2140(6) 0.1931(3) 0.0639(17) Uani 1 1 d . . . O10 O 0.9586(3) 0.1271(5) 0.2746(2) 0.0504(14) Uani 1 1 d . . . O11 O 0.9576(2) 0.2246(4) 0.3957(2) 0.0427(11) Uani 1 1 d . . . O12 O 1.0383(3) 0.3587(5) 0.4341(4) 0.0652(18) Uani 1 1 d . . . O13 O 1.0948(3) 0.0305(6) 0.2371(3) 0.0614(17) Uani 1 1 d D . . H13A H 1.0772 0.0851 0.2227 0.092 Uiso 1 1 d RD . . H13B H 1.1261 0.0166 0.2172 0.092 Uiso 1 1 d RD . . O14 O 1.0184(5) 0.3524(6) 0.3034(5) 0.095(3) Uani 1 1 d D . . H14A H 1.0033 0.3142 0.3297 0.143 Uiso 1 1 d RD . . H14B H 1.0185 0.3144 0.2736 0.143 Uiso 1 1 d RD . . O15 O 1.2206(4) 0.0054(7) 0.2276(3) 0.081(2) Uani 1 1 d D . . H15A H 1.2227 -0.0546 0.2103 0.122 Uiso 1 1 d RD . . H15B H 1.1877 0.0056 0.2466 0.122 Uiso 1 1 d RD . . Gd1 Gd 0.945852(12) 0.05565(2) 0.361619(14) 0.02859(8) Uani 1 1 d . . . Gd2 Gd 1.088201(12) -0.10601(2) 0.308267(14) 0.02908(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.064(6) 0.140(12) 0.054(6) -0.024(7) 0.019(5) -0.025(7) C2 0.046(4) 0.081(6) 0.032(4) -0.011(4) -0.006(3) 0.018(4) C3 0.062(6) 0.114(9) 0.041(5) -0.027(5) -0.004(4) 0.039(6) C4 0.084(7) 0.064(6) 0.050(5) -0.025(5) 0.001(5) 0.017(5) C5 0.076(6) 0.047(4) 0.063(6) -0.021(4) -0.013(5) 0.015(4) C6 0.032(3) 0.049(4) 0.039(4) -0.010(3) -0.006(3) 0.011(3) C7 0.049(4) 0.047(4) 0.037(4) -0.011(3) -0.002(3) 0.012(3) C8 0.037(4) 0.038(4) 0.047(4) -0.002(3) -0.005(3) 0.002(3) C9 0.037(3) 0.035(3) 0.040(4) 0.004(3) 0.001(3) 0.003(3) C10 0.043(4) 0.043(4) 0.056(5) 0.002(3) -0.005(4) -0.002(3) C11 0.041(4) 0.050(4) 0.071(6) 0.019(4) 0.005(4) -0.004(4) C12 0.055(5) 0.062(5) 0.048(5) 0.019(4) 0.013(4) 0.005(4) C13 0.051(4) 0.049(4) 0.035(4) -0.001(3) 0.007(3) 0.009(4) C14 0.040(4) 0.034(3) 0.037(3) 0.001(3) 0.001(3) 0.004(3) C15 0.044(4) 0.045(4) 0.033(3) -0.008(3) -0.006(3) 0.007(3) C16 0.034(4) 0.052(4) 0.048(4) -0.011(3) -0.009(3) 0.008(3) C17 0.042(4) 0.086(6) 0.047(5) -0.010(4) -0.017(4) 0.002(4) C18 0.053(5) 0.073(6) 0.060(6) -0.014(5) -0.026(4) 0.005(4) C19 0.028(4) 0.062(5) 0.080(6) -0.022(5) -0.009(4) 0.007(4) C20 0.035(4) 0.043(4) 0.050(4) -0.010(3) -0.003(3) 0.004(3) C21 0.025(3) 0.043(4) 0.044(4) -0.011(3) -0.008(3) 0.006(3) C22 0.056(6) 0.092(8) 0.095(8) -0.002(6) 0.002(6) -0.031(6) C23 0.080(7) 0.131(11) 0.041(5) 0.001(6) 0.008(5) -0.016(8) C24 0.041(4) 0.051(4) 0.044(4) -0.009(4) -0.008(3) -0.002(3) C25 0.068(6) 0.072(6) 0.044(5) -0.016(4) -0.017(4) -0.009(5) C26 0.055(5) 0.087(7) 0.063(6) -0.012(5) -0.014(4) -0.033(5) C27 0.044(4) 0.050(4) 0.061(6) -0.005(4) -0.008(4) -0.018(4) C28 0.036(4) 0.041(4) 0.052(5) -0.001(3) -0.007(3) 0.000(3) C29 0.028(3) 0.033(3) 0.044(4) -0.003(3) -0.003(3) 0.000(2) C30 0.030(3) 0.040(4) 0.047(4) 0.004(3) 0.002(3) -0.003(3) C31 0.040(4) 0.042(4) 0.034(3) 0.006(3) 0.004(3) 0.006(3) C32 0.048(5) 0.067(5) 0.052(5) 0.015(4) 0.009(4) -0.006(4) C33 0.065(6) 0.116(9) 0.045(5) 0.018(6) 0.015(5) -0.005(6) C34 0.109(10) 0.125(11) 0.033(5) 0.009(6) 0.025(6) 0.013(8) C35 0.061(5) 0.085(7) 0.041(4) -0.001(5) 0.006(4) -0.002(5) C36 0.048(4) 0.047(4) 0.034(4) 0.002(3) 0.003(3) 0.005(3) C37 0.047(4) 0.042(4) 0.032(3) -0.007(3) -0.008(3) 0.000(3) C38 0.043(4) 0.038(4) 0.045(4) -0.005(3) -0.014(3) 0.002(3) C39 0.052(5) 0.061(5) 0.053(5) -0.013(4) -0.021(4) 0.001(4) C40 0.053(5) 0.064(5) 0.068(6) -0.021(5) -0.021(5) -0.009(4) C41 0.041(4) 0.053(5) 0.076(6) -0.023(5) -0.003(4) -0.009(4) C42 0.035(4) 0.032(3) 0.055(4) -0.009(3) -0.011(3) 0.000(3) C43 0.029(3) 0.032(3) 0.051(4) -0.009(3) -0.011(3) 0.005(3) C44 0.073(6) 0.074(6) 0.082(8) 0.024(6) -0.004(6) -0.027(5) C45 0.119(11) 0.109(10) 0.066(7) -0.013(7) 0.020(7) -0.053(9) C46 0.059(5) 0.055(5) 0.041(4) 0.004(4) 0.000(4) 0.012(4) C47 0.079(7) 0.090(8) 0.041(5) 0.002(5) 0.007(4) 0.001(6) C48 0.080(7) 0.133(11) 0.037(5) -0.005(6) -0.009(5) -0.014(7) C49 0.064(6) 0.093(8) 0.054(6) -0.003(5) -0.020(5) -0.011(5) C50 0.058(5) 0.055(5) 0.046(5) -0.002(4) -0.012(4) -0.003(4) C51 0.057(5) 0.039(4) 0.034(4) 0.004(3) -0.006(3) 0.002(3) C52 0.041(4) 0.064(5) 0.062(5) 0.013(5) -0.017(4) -0.007(4) C53 0.031(3) 0.048(4) 0.063(5) 0.010(4) -0.012(3) 0.001(3) C54 0.031(4) 0.070(5) 0.077(6) 0.013(5) -0.018(4) -0.007(4) C55 0.039(4) 0.071(6) 0.096(8) 0.028(6) -0.006(5) -0.016(4) C56 0.033(4) 0.071(6) 0.097(9) 0.034(6) 0.000(5) -0.004(4) C57 0.047(5) 0.061(5) 0.075(6) 0.014(5) 0.013(4) 0.015(4) C58 0.031(4) 0.045(4) 0.070(6) 0.012(4) 0.006(4) 0.003(3) C59 0.034(4) 0.054(4) 0.049(4) 0.004(4) 0.010(3) 0.013(3) C60 0.044(4) 0.043(4) 0.046(4) 0.004(3) 0.006(3) 0.012(3) C61 0.068(6) 0.063(5) 0.048(5) -0.002(4) 0.012(4) 0.011(5) C62 0.091(7) 0.064(6) 0.044(5) -0.011(4) -0.002(5) 0.013(6) C63 0.073(6) 0.049(5) 0.058(5) -0.013(4) -0.017(5) 0.004(4) C64 0.045(4) 0.038(4) 0.060(5) 0.000(4) -0.003(4) 0.005(3) C65 0.043(4) 0.030(3) 0.047(4) 0.005(3) -0.002(3) 0.010(3) C66 0.054(6) 0.050(5) 0.121(11) -0.017(6) -0.012(6) 0.002(4) N1 0.030(3) 0.035(3) 0.040(3) 0.000(2) -0.002(2) 0.000(2) N2 0.040(3) 0.033(3) 0.030(3) 0.000(2) 0.005(2) 0.004(2) N3 0.031(3) 0.039(3) 0.039(3) 0.001(2) -0.001(2) 0.000(2) N4 0.046(3) 0.039(3) 0.029(3) 0.001(2) -0.002(3) 0.001(3) N5 0.033(3) 0.049(3) 0.045(3) 0.005(3) -0.001(3) 0.002(2) N6 0.036(3) 0.037(3) 0.052(4) 0.003(3) 0.007(3) 0.006(3) O1 0.056(4) 0.095(5) 0.049(3) -0.012(3) 0.021(3) -0.004(4) O2 0.051(3) 0.050(3) 0.045(3) -0.012(2) 0.012(2) -0.005(3) O3 0.033(3) 0.046(3) 0.039(3) -0.006(2) -0.002(2) -0.001(2) O4 0.039(3) 0.063(4) 0.070(4) -0.011(3) -0.003(3) -0.015(3) O5 0.050(3) 0.061(3) 0.043(3) -0.004(3) 0.003(2) -0.011(3) O6 0.026(2) 0.034(2) 0.047(3) -0.006(2) -0.002(2) -0.0058(18) O7 0.030(2) 0.035(2) 0.039(2) -0.009(2) -0.002(2) 0.0011(18) O8 0.046(3) 0.050(3) 0.064(4) 0.000(3) 0.001(3) -0.009(3) O9 0.071(4) 0.072(4) 0.049(3) 0.011(3) 0.003(3) -0.018(4) O10 0.053(3) 0.063(4) 0.036(3) 0.013(3) -0.009(2) -0.010(3) O11 0.046(3) 0.037(2) 0.045(3) -0.007(2) 0.006(2) -0.001(2) O12 0.057(4) 0.050(3) 0.089(5) -0.021(3) 0.007(4) -0.009(3) O13 0.077(5) 0.059(4) 0.048(4) 0.012(3) 0.004(3) -0.005(3) O14 0.136(8) 0.062(4) 0.087(6) -0.003(5) 0.020(6) -0.019(5) O15 0.076(5) 0.089(5) 0.078(5) -0.006(5) 0.017(4) -0.023(4) Gd1 0.02515(13) 0.03078(13) 0.02985(14) 0.00052(14) -0.00177(14) 0.00214(11) Gd2 0.02657(14) 0.03194(14) 0.02873(14) -0.00289(14) 0.00093(14) -0.00008(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.396(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.387(13) . ? C2 C3 1.396(14) . ? C2 C6 1.434(11) . ? C3 C4 1.380(17) . ? C3 H3 0.9300 . ? C4 C5 1.326(15) . ? C4 H4 0.9300 . ? C5 C7 1.445(11) . ? C5 H5 0.9300 . ? C6 O2 1.293(9) . ? C6 C7 1.411(12) . ? C7 C8 1.438(11) . ? C8 N1 1.281(10) . ? C8 H8 0.9300 . ? C9 C10 1.390(11) . ? C9 C14 1.403(10) . ? C9 N1 1.411(9) . ? C10 C11 1.410(13) . ? C10 H10 0.9300 . ? C11 C12 1.361(15) . ? C11 H11 0.9300 . ? C12 C13 1.387(13) . ? C12 H12 0.9300 . ? C13 C14 1.399(11) . ? C13 H13 0.9300 . ? C14 N2 1.409(9) . ? C15 N2 1.297(9) . ? C15 C16 1.430(12) . ? C15 H15 0.9300 . ? C16 C21 1.401(12) . ? C16 C17 1.453(11) . ? C17 C18 1.335(14) . ? C17 H17 0.9300 . ? C18 C19 1.401(15) . ? C18 H18 0.9300 . ? C19 C20 1.389(12) . ? C19 H19 0.9300 . ? C20 O4 1.357(11) . ? C20 C21 1.417(11) . ? C21 O3 1.312(8) . ? C22 O4 1.428(12) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O5 1.386(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O5 1.366(10) . ? C24 C25 1.397(12) . ? C24 C29 1.399(11) . ? C25 C26 1.392(14) . ? C25 H25 0.9300 . ? C26 C27 1.361(14) . ? C26 H26 0.9300 . ? C27 C28 1.407(11) . ? C27 H27 0.9300 . ? C28 C29 1.397(11) . ? C28 C30 1.450(11) . ? C29 O6 1.317(8) . ? C30 N3 1.276(10) . ? C30 H30 0.9300 . ? C31 C32 1.372(11) . ? C31 C36 1.406(12) . ? C31 N3 1.424(10) . ? C32 C33 1.394(14) . ? C32 H32 0.9300 . ? C33 C34 1.354(19) . ? C33 H33 0.9300 . ? C34 C35 1.409(16) . ? C34 H34 0.9300 . ? C35 C36 1.388(12) . ? C35 H35 0.9300 . ? C36 N4 1.415(10) . ? C37 N4 1.303(10) . ? C37 C38 1.442(12) . ? C37 H37 0.9300 . ? C38 C43 1.397(12) . ? C38 C39 1.426(11) . ? C39 C40 1.355(14) . ? C39 H39 0.9300 . ? C40 C41 1.366(15) . ? C40 H40 0.9300 . ? C41 C42 1.391(11) . ? C41 H41 0.9300 . ? C42 O8 1.360(10) . ? C42 C43 1.403(11) . ? C43 O7 1.337(9) . ? C44 O8 1.420(11) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 O9 1.430(13) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.383(14) . ? C46 O9 1.396(11) . ? C46 C51 1.416(12) . ? C47 C48 1.383(17) . ? C47 H47 0.9300 . ? C48 C49 1.366(17) . ? C48 H48 0.9300 . ? C49 C50 1.401(13) . ? C49 H49 0.9300 . ? C50 C51 1.411(13) . ? C50 C52 1.414(14) . ? C51 O10 1.302(10) . ? C52 N5 1.289(12) . ? C52 H52 0.9300 . ? C53 C58 1.397(13) . ? C53 C54 1.417(12) . ? C53 N5 1.436(11) . ? C54 C55 1.354(15) . ? C54 H54 0.9300 . ? C55 C56 1.394(19) . ? C55 H55 0.9300 . ? C56 C57 1.355(15) . ? C56 H56 0.9300 . ? C57 C58 1.405(12) . ? C57 H57 0.9300 . ? C58 N6 1.409(11) . ? C59 N6 1.285(11) . ? C59 C60 1.441(12) . ? C59 H59 0.9300 . ? C60 C65 1.401(11) . ? C60 C61 1.421(12) . ? C61 C62 1.365(15) . ? C61 H61 0.9300 . ? C62 C63 1.362(16) . ? C62 H62 0.9300 . ? C63 C64 1.374(13) . ? C63 H63 0.9300 . ? C64 O12 1.365(11) . ? C64 C65 1.406(11) . ? C65 O11 1.301(9) . ? C66 O12 1.440(12) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? N1 Gd2 2.506(6) . ? N2 Gd2 2.538(6) . ? N3 Gd1 2.612(6) . ? N4 Gd1 2.556(6) . ? N5 Gd1 2.514(6) . ? N6 Gd1 2.550(6) . ? O2 Gd2 2.230(5) . ? O3 Gd2 2.262(5) . ? O5 Gd2 2.799(6) . ? O6 Gd2 2.348(5) . ? O6 Gd1 2.360(5) . ? O7 Gd1 2.352(4) . ? O7 Gd2 2.447(5) . ? O10 Gd1 2.266(6) . ? O11 Gd1 2.262(5) . ? O13 Gd2 2.396(6) . ? O13 H13A 0.8501 . ? O13 H13B 0.8501 . ? O14 H14A 0.8499 . ? O14 H14B 0.8499 . ? O15 H15A 0.8501 . ? O15 H15B 0.8502 . ? Gd1 Gd2 3.9140(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 126.9(8) . . ? O1 C2 C6 113.5(7) . . ? C3 C2 C6 119.6(10) . . ? C4 C3 C2 122.9(9) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C5 C4 C3 118.1(9) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C7 123.2(10) . . ? C4 C5 H5 118.4 . . ? C7 C5 H5 118.4 . . ? O2 C6 C7 124.1(7) . . ? O2 C6 C2 118.6(8) . . ? C7 C6 C2 117.2(7) . . ? C6 C7 C8 123.5(7) . . ? C6 C7 C5 118.8(8) . . ? C8 C7 C5 117.6(8) . . ? N1 C8 C7 125.8(7) . . ? N1 C8 H8 117.1 . . ? C7 C8 H8 117.1 . . ? C10 C9 C14 119.7(7) . . ? C10 C9 N1 124.9(7) . . ? C14 C9 N1 115.4(6) . . ? C9 C10 C11 118.6(8) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 121.7(8) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 120.2(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 119.5(8) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C9 120.3(7) . . ? C13 C14 N2 123.9(7) . . ? C9 C14 N2 115.8(6) . . ? N2 C15 C16 125.9(7) . . ? N2 C15 H15 117.0 . . ? C16 C15 H15 117.0 . . ? C21 C16 C15 124.3(7) . . ? C21 C16 C17 119.0(8) . . ? C15 C16 C17 116.6(8) . . ? C18 C17 C16 120.9(10) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.7(9) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C20 C19 C18 120.0(8) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? O4 C20 C19 124.5(8) . . ? O4 C20 C21 114.4(7) . . ? C19 C20 C21 121.1(8) . . ? O3 C21 C16 122.6(6) . . ? O3 C21 C20 119.2(7) . . ? C16 C21 C20 118.3(7) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C25 124.8(8) . . ? O5 C24 C29 113.9(7) . . ? C25 C24 C29 121.2(8) . . ? C26 C25 C24 119.2(9) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C27 C26 C25 120.3(8) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 120.9(8) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 119.9(7) . . ? C29 C28 C30 120.8(7) . . ? C27 C28 C30 119.1(8) . . ? O6 C29 C28 124.4(7) . . ? O6 C29 C24 117.1(6) . . ? C28 C29 C24 118.3(7) . . ? N3 C30 C28 123.6(7) . . ? N3 C30 H30 118.2 . . ? C28 C30 H30 118.2 . . ? C32 C31 C36 119.8(8) . . ? C32 C31 N3 125.2(8) . . ? C36 C31 N3 114.9(7) . . ? C31 C32 C33 120.2(10) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 120.3(10) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.6(10) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 119.2(10) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C31 119.6(8) . . ? C35 C36 N4 123.0(8) . . ? C31 C36 N4 117.2(7) . . ? N4 C37 C38 126.4(7) . . ? N4 C37 H37 116.8 . . ? C38 C37 H37 116.8 . . ? C43 C38 C39 119.6(8) . . ? C43 C38 C37 124.9(7) . . ? C39 C38 C37 115.5(8) . . ? C40 C39 C38 119.8(9) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 121.2(8) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C42 120.4(9) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? O8 C42 C41 124.0(8) . . ? O8 C42 C43 115.7(7) . . ? C41 C42 C43 120.3(8) . . ? O7 C43 C38 122.5(7) . . ? O7 C43 C42 118.9(8) . . ? C38 C43 C42 118.5(7) . . ? O8 C44 H44A 109.5 . . ? O8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O9 C45 H45A 109.5 . . ? O9 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O9 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 O9 124.8(9) . . ? C47 C46 C51 121.5(9) . . ? O9 C46 C51 113.7(7) . . ? C48 C47 C46 120.8(10) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C49 C48 C47 118.5(9) . . ? C49 C48 H48 120.7 . . ? C47 C48 H48 120.7 . . ? C48 C49 C50 122.6(10) . . ? C48 C49 H49 118.7 . . ? C50 C49 H49 118.7 . . ? C49 C50 C51 119.5(9) . . ? C49 C50 C52 118.0(9) . . ? C51 C50 C52 122.2(8) . . ? O10 C51 C50 124.1(8) . . ? O10 C51 C46 119.0(8) . . ? C50 C51 C46 116.9(8) . . ? N5 C52 C50 128.7(8) . . ? N5 C52 H52 115.7 . . ? C50 C52 H52 115.7 . . ? C58 C53 C54 120.1(8) . . ? C58 C53 N5 116.6(7) . . ? C54 C53 N5 122.7(8) . . ? C55 C54 C53 119.5(10) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 121.2(9) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C57 C56 C55 119.4(10) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C56 C57 C58 122.0(11) . . ? C56 C57 H57 119.0 . . ? C58 C57 H57 119.0 . . ? C53 C58 C57 117.7(8) . . ? C53 C58 N6 116.2(8) . . ? C57 C58 N6 125.7(9) . . ? N6 C59 C60 126.9(7) . . ? N6 C59 H59 116.6 . . ? C60 C59 H59 116.6 . . ? C65 C60 C61 119.6(8) . . ? C65 C60 C59 123.1(7) . . ? C61 C60 C59 117.1(8) . . ? C62 C61 C60 120.2(9) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C63 C62 C61 120.0(9) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C62 C63 C64 121.3(9) . . ? C62 C63 H63 119.3 . . ? C64 C63 H63 119.3 . . ? O12 C64 C63 125.7(8) . . ? O12 C64 C65 113.5(8) . . ? C63 C64 C65 120.8(9) . . ? O11 C65 C60 122.8(7) . . ? O11 C65 C64 119.4(7) . . ? C60 C65 C64 117.8(8) . . ? O12 C66 H66A 109.5 . . ? O12 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O12 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C8 N1 C9 118.2(6) . . ? C8 N1 Gd2 131.2(5) . . ? C9 N1 Gd2 110.6(4) . . ? C15 N2 C14 119.3(6) . . ? C15 N2 Gd2 131.5(5) . . ? C14 N2 Gd2 109.2(4) . . ? C30 N3 C31 120.8(7) . . ? C30 N3 Gd1 124.8(5) . . ? C31 N3 Gd1 113.8(4) . . ? C37 N4 C36 120.0(7) . . ? C37 N4 Gd1 125.7(5) . . ? C36 N4 Gd1 114.1(5) . . ? C52 N5 C53 118.9(7) . . ? C52 N5 Gd1 128.4(6) . . ? C53 N5 Gd1 112.6(5) . . ? C59 N6 C58 120.7(7) . . ? C59 N6 Gd1 125.2(5) . . ? C58 N6 Gd1 112.9(5) . . ? C2 O1 C1 118.5(9) . . ? C6 O2 Gd2 141.7(5) . . ? C21 O3 Gd2 142.8(5) . . ? C20 O4 C22 118.7(8) . . ? C24 O5 C23 119.9(8) . . ? C24 O5 Gd2 110.8(4) . . ? C23 O5 Gd2 128.0(6) . . ? C29 O6 Gd2 125.6(4) . . ? C29 O6 Gd1 120.2(4) . . ? Gd2 O6 Gd1 112.48(17) . . ? C43 O7 Gd1 124.3(4) . . ? C43 O7 Gd2 124.1(4) . . ? Gd1 O7 Gd2 109.28(19) . . ? C42 O8 C44 119.2(8) . . ? C46 O9 C45 118.3(8) . . ? C51 O10 Gd1 139.1(5) . . ? C65 O11 Gd1 131.7(5) . . ? C64 O12 C66 118.6(9) . . ? Gd2 O13 H13A 144.9 . . ? Gd2 O13 H13B 107.3 . . ? H13A O13 H13B 107.7 . . ? H14A O14 H14B 107.7 . . ? H15A O15 H15B 107.7 . . ? O11 Gd1 O10 87.1(2) . . ? O11 Gd1 O7 84.93(18) . . ? O10 Gd1 O7 84.4(2) . . ? O11 Gd1 O6 153.63(17) . . ? O10 Gd1 O6 85.2(2) . . ? O7 Gd1 O6 69.25(16) . . ? O11 Gd1 N5 112.3(2) . . ? O10 Gd1 N5 72.4(2) . . ? O7 Gd1 N5 149.7(2) . . ? O6 Gd1 N5 89.30(19) . . ? O11 Gd1 N6 71.3(2) . . ? O10 Gd1 N6 116.5(2) . . ? O7 Gd1 N6 146.6(2) . . ? O6 Gd1 N6 134.25(18) . . ? N5 Gd1 N6 63.4(2) . . ? O11 Gd1 N4 79.7(2) . . ? O10 Gd1 N4 154.3(2) . . ? O7 Gd1 N4 72.6(2) . . ? O6 Gd1 N4 96.90(18) . . ? N5 Gd1 N4 133.1(2) . . ? N6 Gd1 N4 80.1(2) . . ? O11 Gd1 N3 130.0(2) . . ? O10 Gd1 N3 139.9(2) . . ? O7 Gd1 N3 109.94(18) . . ? O6 Gd1 N3 67.09(18) . . ? N5 Gd1 N3 78.7(2) . . ? N6 Gd1 N3 71.74(19) . . ? N4 Gd1 N3 61.7(2) . . ? O11 Gd1 Gd2 120.01(13) . . ? O10 Gd1 Gd2 78.91(17) . . ? O7 Gd1 Gd2 36.16(12) . . ? O6 Gd1 Gd2 33.66(11) . . ? N5 Gd1 Gd2 117.89(16) . . ? N6 Gd1 Gd2 162.51(14) . . ? N4 Gd1 Gd2 88.67(14) . . ? N3 Gd1 Gd2 91.16(13) . . ? O2 Gd2 O3 82.7(2) . . ? O2 Gd2 O6 128.98(19) . . ? O3 Gd2 O6 147.96(17) . . ? O2 Gd2 O13 80.4(2) . . ? O3 Gd2 O13 90.8(2) . . ? O6 Gd2 O13 98.5(2) . . ? O2 Gd2 O7 156.40(19) . . ? O3 Gd2 O7 83.74(16) . . ? O6 Gd2 O7 67.87(15) . . ? O13 Gd2 O7 80.5(2) . . ? O2 Gd2 N1 72.6(2) . . ? O3 Gd2 N1 112.10(19) . . ? O6 Gd2 N1 78.64(17) . . ? O13 Gd2 N1 141.3(2) . . ? O7 Gd2 N1 130.67(19) . . ? O2 Gd2 N2 112.0(2) . . ? O3 Gd2 N2 71.14(19) . . ? O6 Gd2 N2 89.57(18) . . ? O13 Gd2 N2 155.7(2) . . ? O7 Gd2 N2 81.4(2) . . ? N1 Gd2 N2 62.64(19) . . ? O2 Gd2 O5 72.9(2) . . ? O3 Gd2 O5 152.24(18) . . ? O6 Gd2 O5 58.76(17) . . ? O13 Gd2 O5 72.6(2) . . ? O7 Gd2 O5 114.12(18) . . ? N1 Gd2 O5 73.31(19) . . ? N2 Gd2 O5 130.18(19) . . ? O2 Gd2 Gd1 154.93(16) . . ? O3 Gd2 Gd1 118.03(13) . . ? O6 Gd2 Gd1 33.86(11) . . ? O13 Gd2 Gd1 85.08(17) . . ? O7 Gd2 Gd1 34.56(10) . . ? N1 Gd2 Gd1 108.43(14) . . ? N2 Gd2 Gd1 89.24(13) . . ? O5 Gd2 Gd1 83.34(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.337 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.115 #===END _database_code_depnum_ccdc_archive 'CCDC 931254'