# 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_zt6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H47 Cl4 Gd2 N4 O9' _chemical_formula_sum 'C52 H47 Cl4 Gd2 N4 O9' _chemical_formula_weight 1328.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.4707(6) _cell_length_b 19.5166(8) _cell_length_c 17.8732(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.0720(10) _cell_angle_gamma 90.00 _cell_volume 5395.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7306 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2620 _exptl_absorpt_coefficient_mu 2.692 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6151 _exptl_absorpt_correction_T_max 0.7746 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39320 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.29 _reflns_number_total 13360 _reflns_number_gt 8427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT-plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0323P)^2^+4.8441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13360 _refine_ls_number_parameters 643 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Gd1 Gd 0.126147(12) 0.861510(11) 0.247053(11) 0.03433(6) Uani 1 1 d . . . Gd2 Gd -0.021146(12) 0.863923(11) 0.067768(11) 0.03503(6) Uani 1 1 d . . . O1 O -0.00978(17) 0.89414(15) 0.19560(15) 0.0395(7) Uani 1 1 d . . . O2 O 0.11136(17) 0.82605(15) 0.12079(15) 0.0387(7) Uani 1 1 d . . . O3 O -0.13256(19) 0.93403(16) 0.03667(18) 0.0495(8) Uani 1 1 d . . . N2 N 0.1196(2) 0.7300(2) 0.2391(2) 0.0444(9) Uani 1 1 d . . . N3 N -0.1538(2) 0.8098(2) 0.1180(2) 0.0436(9) Uani 1 1 d . . . O7 O 0.20536(19) 0.81799(16) 0.34969(16) 0.0467(8) Uani 1 1 d . . . O9 O 0.0653(2) 0.96663(17) 0.05706(18) 0.0522(8) Uani 1 1 d D . . Cl1 Cl 0.0671(2) 0.79861(17) 0.57762(16) 0.1861(13) Uani 1 1 d . . . O6 O 0.1510(2) 0.97235(16) 0.19484(17) 0.0483(8) Uani 1 1 d . . . O5 O 0.1003(2) 0.94082(17) 0.34125(18) 0.0560(9) Uani 1 1 d . . . O8 O 0.2686(2) 0.85154(18) 0.21069(18) 0.0548(9) Uani 1 1 d . . . N1 N 0.0042(2) 0.8014(2) 0.3158(2) 0.0456(9) Uani 1 1 d . . . N4 N -0.0321(2) 0.7367(2) 0.0520(2) 0.0478(10) Uani 1 1 d . . . C14 C -0.0015(3) 0.6988(3) -0.0007(3) 0.0618(15) Uani 1 1 d . . . H14A H -0.0044 0.6517 0.0066 0.074 Uiso 1 1 calc R . . C15 C -0.2625(3) 0.8982(3) 0.0958(3) 0.0505(12) Uani 1 1 d . . . O4 O 0.0101(2) 0.84049(18) -0.04920(18) 0.0541(9) Uani 1 1 d . . . C17 C -0.2136(3) 0.9454(3) 0.0548(3) 0.0503(12) Uani 1 1 d . . . C18 C 0.3377(3) 0.7818(3) 0.3001(3) 0.0580(14) Uani 1 1 d . . . H18A H 0.3870 0.7557 0.3097 0.070 Uiso 1 1 calc R . . C19 C -0.0736(3) 0.9222(3) 0.2356(2) 0.0444(11) Uani 1 1 d . . . C20 C 0.1533(3) 0.6937(3) 0.1876(3) 0.0548(13) Uani 1 1 d . . . H20A H 0.1553 0.6466 0.1952 0.066 Uiso 1 1 calc R . . C21 C 0.0878(3) 0.6983(2) 0.3055(3) 0.0495(12) Uani 1 1 d . . . C22 C -0.2314(3) 0.8329(3) 0.1215(3) 0.0524(13) Uani 1 1 d . . . H22A H -0.2718 0.8041 0.1431 0.063 Uiso 1 1 calc R . . C23 C 0.2758(3) 0.7842(2) 0.3551(3) 0.0460(11) Uani 1 1 d . . . C24 C 0.1679(3) 0.7841(2) 0.0882(3) 0.0425(11) Uani 1 1 d . . . C25 C 0.1880(3) 0.7190(3) 0.1195(3) 0.0506(12) Uani 1 1 d . . . C26 C -0.0708(3) 0.7056(3) 0.1154(3) 0.0543(13) Uani 1 1 d . . . C27 C -0.0717(3) 0.8247(3) 0.3269(3) 0.0552(13) Uani 1 1 d . . . H27A H -0.1075 0.7983 0.3565 0.066 Uiso 1 1 calc R . . C28 C 0.0386(3) 0.7910(3) -0.0913(3) 0.0537(13) Uani 1 1 d . . . C29 C -0.1072(3) 0.8881(3) 0.2979(3) 0.0501(12) Uani 1 1 d . . . Cl2 Cl 0.2029(3) 0.8889(2) 0.5493(2) 0.2290(18) Uani 1 1 d . . . C31 C 0.2628(4) 0.7601(3) -0.0143(3) 0.0722(17) Uani 1 1 d . . . H31A H 0.2876 0.7741 -0.0588 0.087 Uiso 1 1 calc R . . C32 C 0.1424(3) 1.0335(3) 0.2187(3) 0.0516(12) Uani 1 1 d . . . C33 C 0.2057(3) 0.8029(3) 0.0210(3) 0.0518(13) Uani 1 1 d . . . H33A H 0.1921 0.8451 -0.0003 0.062 Uiso 1 1 calc R . . C34 C 0.0282(3) 0.7358(3) 0.3457(3) 0.0538(13) Uani 1 1 d . . . C35 C -0.0495(4) 0.6419(3) 0.1449(4) 0.0701(17) Uani 1 1 d . . . H35A H -0.0080 0.6150 0.1219 0.084 Uiso 1 1 calc R . . C36 C 0.0717(3) 0.8058(4) -0.1622(3) 0.0726(18) Uani 1 1 d . . . H36A H 0.0715 0.8509 -0.1790 0.087 Uiso 1 1 calc R . . C37 C 0.0368(3) 0.7216(3) -0.0693(3) 0.0593(15) Uani 1 1 d . . . C38 C 0.0259(4) 0.6486(4) 0.4397(4) 0.091(2) Uani 1 1 d . . . H38A H 0.0062 0.6321 0.4852 0.110 Uiso 1 1 calc R . . C39 C -0.3495(3) 0.9140(4) 0.1135(3) 0.0733(17) Uani 1 1 d . . . H39A H -0.3824 0.8820 0.1390 0.088 Uiso 1 1 calc R . . C40 C 0.3317(3) 0.8153(3) 0.2318(3) 0.0562(13) Uani 1 1 d . . . C41 C -0.1730(4) 0.7200(3) 0.2149(3) 0.0698(16) Uani 1 1 d . . . H41A H -0.2139 0.7465 0.2390 0.084 Uiso 1 1 calc R . . C42 C 0.0830(5) 0.6104(4) 0.3990(4) 0.091(2) Uani 1 1 d . . . H42A H 0.1005 0.5676 0.4166 0.110 Uiso 1 1 calc R . . C43 C -0.1802(4) 0.9152(4) 0.3318(3) 0.0767(18) Uani 1 1 d . . . H43A H -0.2053 0.8913 0.3708 0.092 Uiso 1 1 calc R . . C44 C -0.1103(3) 0.9840(3) 0.2133(3) 0.0582(14) Uani 1 1 d . . . H44A H -0.0877 1.0076 0.1729 0.070 Uiso 1 1 calc R . . C45 C -0.1505(5) 0.6570(4) 0.2431(4) 0.083(2) Uani 1 1 d . . . H45A H -0.1766 0.6407 0.2861 0.100 Uiso 1 1 calc R . . C46 C -0.1345(3) 0.7445(3) 0.1501(3) 0.0500(12) Uani 1 1 d . . . Cl3 Cl 0.3986(4) 0.98525(19) 0.3029(3) 0.283(3) Uani 1 1 d . . . C48 C -0.1794(4) 1.0105(3) 0.2503(4) 0.0809(19) Uani 1 1 d . . . H48A H -0.2021 1.0526 0.2354 0.097 Uiso 1 1 calc R . . C49 C 0.1151(4) 0.6350(3) 0.3317(4) 0.0701(16) Uani 1 1 d . . . H49A H 0.1544 0.6092 0.3048 0.084 Uiso 1 1 calc R . . C50 C 0.2454(4) 0.6774(3) 0.0798(3) 0.0726(17) Uani 1 1 d . . . H50A H 0.2581 0.6341 0.0986 0.087 Uiso 1 1 calc R . . C51 C -0.0901(5) 0.6181(3) 0.2084(4) 0.092(2) Uani 1 1 d . . . H51A H -0.0758 0.5752 0.2274 0.110 Uiso 1 1 calc R . . C52 C 0.4055(4) 0.8115(4) 0.1773(4) 0.105(3) Uani 1 1 d . . . H52A H 0.3905 0.8368 0.1329 0.158 Uiso 1 1 calc R . . H52B H 0.4161 0.7645 0.1644 0.158 Uiso 1 1 calc R . . H52C H 0.4566 0.8308 0.2000 0.158 Uiso 1 1 calc R . . C53 C -0.0019(4) 0.7106(3) 0.4134(3) 0.0719(17) Uani 1 1 d . . . H53A H -0.0411 0.7362 0.4407 0.086 Uiso 1 1 calc R . . C54 C 0.1561(4) 1.0889(3) 0.1622(3) 0.0730(17) Uani 1 1 d . . . H54A H 0.1717 1.0687 0.1154 0.110 Uiso 1 1 calc R . . H54B H 0.2017 1.1187 0.1794 0.110 Uiso 1 1 calc R . . H54C H 0.1038 1.1148 0.1557 0.110 Uiso 1 1 calc R . . C55 C 0.2903(4) 0.7459(3) 0.4274(3) 0.0648(15) Uani 1 1 d . . . H55A H 0.2416 0.7526 0.4591 0.097 Uiso 1 1 calc R . . H55B H 0.3416 0.7627 0.4521 0.097 Uiso 1 1 calc R . . H55C H 0.2968 0.6979 0.4171 0.097 Uiso 1 1 calc R . . C56 C -0.2543(4) 1.0066(3) 0.0331(4) 0.0796(19) Uani 1 1 d . . . H56A H -0.2243 1.0379 0.0042 0.096 Uiso 1 1 calc R . . C57 C 0.0968(4) 1.0057(3) 0.3464(3) 0.0624(14) Uani 1 1 d . . . C58 C 0.2835(4) 0.6974(4) 0.0151(4) 0.083(2) Uani 1 1 d . . . H58A H 0.3228 0.6689 -0.0085 0.100 Uiso 1 1 calc R . . C59 C -0.3371(4) 1.0213(4) 0.0534(5) 0.097(2) Uani 1 1 d . . . H59A H -0.3611 1.0633 0.0399 0.116 Uiso 1 1 calc R . . C60 C 0.1041(4) 0.7560(5) -0.2071(4) 0.092(2) Uani 1 1 d . . . H60A H 0.1261 0.7678 -0.2535 0.110 Uiso 1 1 calc R . . C61 C 0.1047(5) 0.6891(5) -0.1851(4) 0.107(3) Uani 1 1 d . . . H61A H 0.1282 0.6556 -0.2157 0.128 Uiso 1 1 calc R . . Cl4 Cl 0.3785(4) 0.9965(2) 0.4569(3) 0.295(3) Uani 1 1 d . . . C63 C 0.0702(4) 0.6716(4) -0.1172(4) 0.092(2) Uani 1 1 d . . . H63A H 0.0690 0.6258 -0.1029 0.110 Uiso 1 1 calc R . . C64 C 0.1191(4) 1.0505(3) 0.2904(3) 0.0668(15) Uani 1 1 d . . . H64A H 0.1183 1.0969 0.3022 0.080 Uiso 1 1 calc R . . C65 C -0.2160(4) 0.9764(4) 0.3091(4) 0.090(2) Uani 1 1 d . . . H65A H -0.2639 0.9943 0.3330 0.108 Uiso 1 1 calc R . . C66 C -0.3856(4) 0.9756(4) 0.0934(4) 0.087(2) Uani 1 1 d . . . H66A H -0.4419 0.9863 0.1066 0.105 Uiso 1 1 calc R . . C71 C 0.3440(9) 0.9558(6) 0.3796(11) 0.277(10) Uani 1 1 d . . . H71A H 0.2825 0.9634 0.3723 0.332 Uiso 1 1 calc R . . H71B H 0.3535 0.9069 0.3852 0.332 Uiso 1 1 calc R . . C72 C 0.1162(5) 0.8487(5) 0.5114(4) 0.123(3) Uani 1 1 d . . . H72A H 0.1342 0.8203 0.4700 0.148 Uiso 1 1 calc R . . H72B H 0.0754 0.8824 0.4922 0.148 Uiso 1 1 calc R . . C74 C 0.0655(6) 1.0323(4) 0.4199(4) 0.129(3) Uani 1 1 d . . . H74A H 0.0526 0.9945 0.4522 0.193 Uiso 1 1 calc R . . H74B H 0.0142 1.0592 0.4115 0.193 Uiso 1 1 calc R . . H74C H 0.1095 1.0603 0.4429 0.193 Uiso 1 1 calc R . . H9 H 0.103(4) 0.968(5) 0.091(4) 0.193 Uiso 1 1 d 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 Gd1 0.03254(11) 0.03719(12) 0.03316(11) 0.00360(9) -0.00161(8) 0.00061(9) Gd2 0.03123(11) 0.04125(13) 0.03256(11) 0.00483(10) -0.00045(8) 0.00066(9) O1 0.0338(15) 0.0493(19) 0.0354(16) 0.0021(14) 0.0029(12) 0.0071(13) O2 0.0359(16) 0.0422(18) 0.0379(16) 0.0004(14) -0.0013(13) 0.0061(13) O3 0.0380(17) 0.052(2) 0.059(2) 0.0128(16) 0.0030(15) 0.0055(14) N2 0.044(2) 0.040(2) 0.048(2) 0.0072(19) -0.0079(18) -0.0046(18) N3 0.040(2) 0.050(2) 0.041(2) 0.0049(18) 0.0013(17) -0.0084(18) O7 0.0449(18) 0.055(2) 0.0401(18) 0.0015(15) -0.0074(14) 0.0047(15) O9 0.055(2) 0.049(2) 0.052(2) 0.0118(16) -0.0104(16) -0.0118(16) Cl1 0.263(4) 0.177(3) 0.119(2) 0.029(2) 0.037(2) 0.017(3) O6 0.056(2) 0.0401(19) 0.0481(19) 0.0051(15) -0.0021(15) -0.0071(15) O5 0.073(2) 0.044(2) 0.051(2) -0.0024(16) 0.0102(17) 0.0038(17) O8 0.0388(18) 0.072(2) 0.054(2) 0.0081(18) 0.0001(15) 0.0033(17) N1 0.045(2) 0.053(3) 0.039(2) 0.0083(18) -0.0003(17) -0.0078(19) N4 0.045(2) 0.046(2) 0.052(2) -0.002(2) -0.0087(18) -0.0009(19) C14 0.056(3) 0.050(3) 0.079(4) -0.008(3) -0.018(3) 0.002(3) C15 0.038(3) 0.067(4) 0.046(3) -0.008(3) 0.001(2) 0.002(2) O4 0.057(2) 0.064(2) 0.0414(18) -0.0015(16) 0.0067(16) 0.0035(17) C17 0.038(3) 0.059(3) 0.054(3) -0.001(2) -0.002(2) 0.006(2) C18 0.045(3) 0.065(4) 0.063(4) -0.006(3) -0.004(3) 0.013(3) C19 0.033(2) 0.059(3) 0.041(3) -0.005(2) 0.0009(19) 0.005(2) C20 0.058(3) 0.036(3) 0.070(4) 0.000(3) -0.011(3) 0.010(2) C21 0.045(3) 0.046(3) 0.057(3) 0.017(2) -0.013(2) -0.014(2) C22 0.039(3) 0.067(3) 0.051(3) 0.003(3) 0.004(2) -0.013(2) C23 0.045(3) 0.038(3) 0.054(3) -0.004(2) -0.022(2) 0.001(2) C24 0.032(2) 0.049(3) 0.046(3) -0.011(2) -0.0032(19) 0.005(2) C25 0.055(3) 0.046(3) 0.050(3) -0.008(2) -0.006(2) 0.016(2) C26 0.054(3) 0.051(3) 0.058(3) 0.006(3) -0.016(3) -0.013(3) C27 0.043(3) 0.081(4) 0.042(3) 0.013(3) 0.012(2) -0.007(3) C28 0.039(3) 0.077(4) 0.045(3) -0.016(3) -0.005(2) 0.003(3) C29 0.043(3) 0.068(3) 0.040(3) -0.003(2) 0.002(2) 0.006(2) Cl2 0.227(4) 0.255(4) 0.204(4) -0.117(3) -0.019(3) -0.032(3) C31 0.063(4) 0.103(5) 0.051(3) -0.011(3) 0.008(3) 0.021(3) C32 0.048(3) 0.044(3) 0.062(3) 0.008(3) -0.013(2) -0.010(2) C33 0.040(3) 0.068(4) 0.048(3) -0.005(2) 0.003(2) 0.009(2) C34 0.048(3) 0.061(3) 0.052(3) 0.019(3) -0.010(2) -0.014(3) C35 0.065(4) 0.050(3) 0.094(5) 0.012(3) -0.026(3) -0.005(3) C36 0.056(3) 0.117(5) 0.045(3) -0.016(3) 0.008(3) -0.002(3) C37 0.047(3) 0.075(4) 0.056(3) -0.024(3) -0.002(2) 0.010(3) C38 0.073(5) 0.116(6) 0.085(5) 0.059(5) -0.008(4) -0.029(4) C39 0.044(3) 0.099(5) 0.077(4) -0.009(4) 0.010(3) 0.003(3) C40 0.036(3) 0.072(4) 0.060(3) -0.007(3) -0.008(2) 0.001(3) C41 0.060(3) 0.080(4) 0.069(4) 0.017(3) -0.004(3) -0.032(3) C42 0.087(5) 0.073(5) 0.114(6) 0.062(4) -0.031(4) -0.029(4) C43 0.060(4) 0.114(5) 0.057(4) 0.000(4) 0.020(3) 0.015(4) C44 0.057(3) 0.065(4) 0.053(3) -0.002(3) 0.000(2) 0.021(3) C45 0.091(5) 0.080(5) 0.079(5) 0.032(4) -0.012(4) -0.037(4) C46 0.043(3) 0.056(3) 0.050(3) 0.009(2) -0.010(2) -0.018(2) Cl3 0.386(7) 0.118(3) 0.340(6) 0.032(3) -0.123(5) -0.077(4) C48 0.077(4) 0.079(5) 0.087(5) -0.012(4) 0.009(4) 0.038(4) C49 0.068(4) 0.055(3) 0.086(4) 0.025(3) -0.017(3) -0.010(3) C50 0.080(4) 0.066(4) 0.072(4) -0.012(3) -0.004(3) 0.030(3) C51 0.106(6) 0.062(4) 0.106(6) 0.044(4) -0.042(5) -0.032(4) C52 0.051(4) 0.179(8) 0.086(5) -0.003(5) 0.017(3) 0.031(4) C53 0.059(3) 0.091(5) 0.065(4) 0.036(3) -0.005(3) -0.016(3) C54 0.095(4) 0.046(3) 0.078(4) 0.015(3) -0.016(3) -0.020(3) C55 0.077(4) 0.055(3) 0.061(4) 0.005(3) -0.023(3) 0.014(3) C56 0.052(3) 0.065(4) 0.122(6) 0.018(4) 0.006(3) 0.016(3) C57 0.073(4) 0.060(4) 0.054(3) -0.010(3) 0.011(3) 0.004(3) C58 0.086(5) 0.093(5) 0.071(4) -0.016(4) 0.009(4) 0.045(4) C59 0.057(4) 0.077(5) 0.158(7) -0.001(5) 0.004(4) 0.031(4) C60 0.065(4) 0.144(7) 0.067(5) -0.025(5) 0.010(3) 0.013(5) C61 0.082(5) 0.165(9) 0.074(5) -0.057(6) 0.005(4) 0.034(6) Cl4 0.327(6) 0.177(4) 0.379(7) -0.005(4) -0.053(5) -0.092(4) C63 0.083(5) 0.096(5) 0.096(5) -0.040(4) -0.015(4) 0.015(4) C64 0.088(4) 0.044(3) 0.069(4) -0.009(3) 0.000(3) 0.003(3) C65 0.072(4) 0.120(6) 0.079(5) -0.014(4) 0.024(4) 0.038(4) C66 0.046(3) 0.105(6) 0.111(6) -0.015(5) 0.012(3) 0.017(4) C71 0.210(14) 0.087(8) 0.53(3) 0.010(13) -0.085(17) -0.083(9) C72 0.123(7) 0.169(9) 0.078(5) -0.013(5) 0.010(5) 0.022(6) C74 0.202(9) 0.072(5) 0.116(6) -0.028(4) 0.089(6) -0.005(5) _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 O8 2.317(3) . ? Gd1 O5 2.327(3) . ? Gd1 O7 2.346(3) . ? Gd1 O1 2.367(3) . ? Gd1 O2 2.367(3) . ? Gd1 O6 2.390(3) . ? Gd1 N1 2.555(4) . ? Gd1 N2 2.572(4) . ? Gd1 Gd2 3.8974(3) . ? Gd2 O4 2.202(3) . ? Gd2 O3 2.262(3) . ? Gd2 O2 2.361(3) . ? Gd2 O1 2.363(3) . ? Gd2 O9 2.419(3) . ? Gd2 N3 2.490(3) . ? Gd2 N4 2.504(4) . ? O1 C19 1.347(5) . ? O2 C24 1.339(5) . ? O3 C17 1.320(5) . ? N2 C20 1.279(6) . ? N2 C21 1.434(6) . ? N3 C22 1.285(6) . ? N3 C46 1.428(6) . ? O7 C23 1.275(5) . ? O9 H9 0.841(10) . ? Cl1 C72 1.723(8) . ? O6 C32 1.275(6) . ? O5 C57 1.270(6) . ? O8 C40 1.258(6) . ? N1 C27 1.278(6) . ? N1 C34 1.434(6) . ? N4 C14 1.294(6) . ? N4 C26 1.427(6) . ? C14 C37 1.443(8) . ? C14 H14A 0.9300 . ? C15 C17 1.406(7) . ? C15 C39 1.422(7) . ? C15 C22 1.435(7) . ? O4 C28 1.305(6) . ? C17 C56 1.400(7) . ? C18 C40 1.385(7) . ? C18 C23 1.387(7) . ? C18 H18A 0.9300 . ? C19 C44 1.388(7) . ? C19 C29 1.405(6) . ? C20 C25 1.427(7) . ? C20 H20A 0.9300 . ? C21 C49 1.385(7) . ? C21 C34 1.387(7) . ? C22 H22A 0.9300 . ? C23 C55 1.506(6) . ? C24 C33 1.395(6) . ? C24 C25 1.420(7) . ? C25 C50 1.405(7) . ? C26 C35 1.388(7) . ? C26 C46 1.398(7) . ? C27 C29 1.446(7) . ? C27 H27A 0.9300 . ? C28 C36 1.406(7) . ? C28 C37 1.412(8) . ? C29 C43 1.397(7) . ? Cl2 C72 1.684(9) . ? C31 C58 1.368(8) . ? C31 C33 1.378(7) . ? C31 H31A 0.9300 . ? C32 C64 1.378(7) . ? C32 C54 1.497(7) . ? C33 H33A 0.9300 . ? C34 C53 1.394(7) . ? C35 C51 1.387(9) . ? C35 H35A 0.9300 . ? C36 C60 1.362(9) . ? C36 H36A 0.9300 . ? C37 C63 1.403(8) . ? C38 C53 1.366(9) . ? C38 C42 1.375(10) . ? C38 H38A 0.9300 . ? C39 C66 1.372(9) . ? C39 H39A 0.9300 . ? C40 C52 1.517(7) . ? C41 C45 1.372(8) . ? C41 C46 1.396(7) . ? C41 H41A 0.9300 . ? C42 C49 1.395(9) . ? C42 H42A 0.9300 . ? C43 C65 1.374(9) . ? C43 H43A 0.9300 . ? C44 C48 1.369(7) . ? C44 H44A 0.9300 . ? C45 C51 1.363(10) . ? C45 H45A 0.9300 . ? Cl3 C71 1.723(18) . ? C48 C65 1.375(9) . ? C48 H48A 0.9300 . ? C49 H49A 0.9300 . ? C50 C58 1.365(8) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9300 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 C59 1.369(8) . ? C56 H56A 0.9300 . ? C57 C64 1.379(7) . ? C57 C74 1.501(8) . ? C58 H58A 0.9300 . ? C59 C66 1.375(9) . ? C59 H59A 0.9300 . ? C60 C61 1.364(10) . ? C60 H60A 0.9300 . ? C61 C63 1.379(10) . ? C61 H61A 0.9300 . ? Cl4 C71 1.672(17) . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? 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 O8 Gd1 O5 115.85(12) . . ? O8 Gd1 O7 72.75(11) . . ? O5 Gd1 O7 76.68(11) . . ? O8 Gd1 O1 139.14(10) . . ? O5 Gd1 O1 86.48(11) . . ? O7 Gd1 O1 148.06(10) . . ? O8 Gd1 O2 77.50(11) . . ? O5 Gd1 O2 150.36(11) . . ? O7 Gd1 O2 132.79(10) . . ? O1 Gd1 O2 68.83(9) . . ? O8 Gd1 O6 78.81(11) . . ? O5 Gd1 O6 73.23(11) . . ? O7 Gd1 O6 123.21(11) . . ? O1 Gd1 O6 75.69(10) . . ? O2 Gd1 O6 84.59(10) . . ? O8 Gd1 N1 144.18(12) . . ? O5 Gd1 N1 79.57(12) . . ? O7 Gd1 N1 80.65(11) . . ? O1 Gd1 N1 69.61(11) . . ? O2 Gd1 N1 105.37(11) . . ? O6 Gd1 N1 136.76(12) . . ? O8 Gd1 N2 86.40(12) . . ? O5 Gd1 N2 134.16(12) . . ? O7 Gd1 N2 72.64(11) . . ? O1 Gd1 N2 102.31(11) . . ? O2 Gd1 N2 69.67(11) . . ? O6 Gd1 N2 152.61(11) . . ? N1 Gd1 N2 62.63(12) . . ? O8 Gd1 Gd2 108.35(8) . . ? O5 Gd1 Gd2 118.75(9) . . ? O7 Gd1 Gd2 159.40(8) . . ? O1 Gd1 Gd2 34.48(7) . . ? O2 Gd1 Gd2 34.43(7) . . ? O6 Gd1 Gd2 76.33(8) . . ? N1 Gd1 Gd2 88.58(8) . . ? N2 Gd1 Gd2 86.83(8) . . ? O4 Gd2 O3 94.13(12) . . ? O4 Gd2 O2 96.41(11) . . ? O3 Gd2 O2 160.05(11) . . ? O4 Gd2 O1 162.92(11) . . ? O3 Gd2 O1 97.43(11) . . ? O2 Gd2 O1 69.00(9) . . ? O4 Gd2 O9 88.03(12) . . ? O3 Gd2 O9 84.21(11) . . ? O2 Gd2 O9 79.29(10) . . ? O1 Gd2 O9 80.71(11) . . ? O4 Gd2 N3 116.80(12) . . ? O3 Gd2 N3 73.47(12) . . ? O2 Gd2 N3 115.98(11) . . ? O1 Gd2 N3 78.72(11) . . ? O9 Gd2 N3 147.17(13) . . ? O4 Gd2 N4 72.72(13) . . ? O3 Gd2 N4 121.50(12) . . ? O2 Gd2 N4 77.94(11) . . ? O1 Gd2 N4 111.08(12) . . ? O9 Gd2 N4 148.10(12) . . ? N3 Gd2 N4 64.26(13) . . ? O4 Gd2 Gd1 129.99(9) . . ? O3 Gd2 Gd1 129.83(8) . . ? O2 Gd2 Gd1 34.54(7) . . ? O1 Gd2 Gd1 34.54(7) . . ? O9 Gd2 Gd1 76.09(7) . . ? N3 Gd2 Gd1 99.90(8) . . ? N4 Gd2 Gd1 96.76(9) . . ? C19 O1 Gd2 125.0(3) . . ? C19 O1 Gd1 123.9(3) . . ? Gd2 O1 Gd1 110.98(11) . . ? C24 O2 Gd2 125.9(3) . . ? C24 O2 Gd1 122.7(2) . . ? Gd2 O2 Gd1 111.03(11) . . ? C17 O3 Gd2 139.9(3) . . ? C20 N2 C21 120.5(4) . . ? C20 N2 Gd1 125.2(3) . . ? C21 N2 Gd1 113.4(3) . . ? C22 N3 C46 118.8(4) . . ? C22 N3 Gd2 130.3(3) . . ? C46 N3 Gd2 110.9(3) . . ? C23 O7 Gd1 132.8(3) . . ? Gd2 O9 H9 110(6) . . ? C32 O6 Gd1 134.3(3) . . ? C57 O5 Gd1 136.3(3) . . ? C40 O8 Gd1 134.4(3) . . ? C27 N1 C34 119.4(4) . . ? C27 N1 Gd1 126.9(3) . . ? C34 N1 Gd1 113.6(3) . . ? C14 N4 C26 120.0(5) . . ? C14 N4 Gd2 128.6(4) . . ? C26 N4 Gd2 111.2(3) . . ? N4 C14 C37 127.2(5) . . ? N4 C14 H14A 116.4 . . ? C37 C14 H14A 116.4 . . ? C17 C15 C39 119.7(5) . . ? C17 C15 C22 124.6(4) . . ? C39 C15 C22 115.7(5) . . ? C28 O4 Gd2 141.5(3) . . ? O3 C17 C56 120.0(5) . . ? O3 C17 C15 122.7(4) . . ? C56 C17 C15 117.3(5) . . ? C40 C18 C23 124.9(5) . . ? C40 C18 H18A 117.6 . . ? C23 C18 H18A 117.6 . . ? O1 C19 C44 120.1(4) . . ? O1 C19 C29 120.9(4) . . ? C44 C19 C29 119.0(4) . . ? N2 C20 C25 125.9(5) . . ? N2 C20 H20A 117.0 . . ? C25 C20 H20A 117.0 . . ? C49 C21 C34 119.8(5) . . ? C49 C21 N2 123.9(5) . . ? C34 C21 N2 116.3(4) . . ? N3 C22 C15 127.1(4) . . ? N3 C22 H22A 116.4 . . ? C15 C22 H22A 116.4 . . ? O7 C23 C18 124.4(5) . . ? O7 C23 C55 115.8(5) . . ? C18 C23 C55 119.8(4) . . ? O2 C24 C33 120.0(4) . . ? O2 C24 C25 121.1(4) . . ? C33 C24 C25 118.9(4) . . ? C50 C25 C24 117.0(5) . . ? C50 C25 C20 118.9(5) . . ? C24 C25 C20 124.2(4) . . ? C35 C26 C46 118.8(5) . . ? C35 C26 N4 125.6(5) . . ? C46 C26 N4 115.6(4) . . ? N1 C27 C29 126.3(4) . . ? N1 C27 H27A 116.8 . . ? C29 C27 H27A 116.8 . . ? O4 C28 C36 120.0(6) . . ? O4 C28 C37 122.8(5) . . ? C36 C28 C37 117.1(5) . . ? C43 C29 C19 118.6(5) . . ? C43 C29 C27 118.3(5) . . ? C19 C29 C27 123.1(4) . . ? C58 C31 C33 121.0(6) . . ? C58 C31 H31A 119.5 . . ? C33 C31 H31A 119.5 . . ? O6 C32 C64 124.6(5) . . ? O6 C32 C54 115.7(5) . . ? C64 C32 C54 119.7(5) . . ? C31 C33 C24 121.2(5) . . ? C31 C33 H33A 119.4 . . ? C24 C33 H33A 119.4 . . ? C21 C34 C53 120.0(5) . . ? C21 C34 N1 116.6(4) . . ? C53 C34 N1 123.4(5) . . ? C51 C35 C26 120.1(6) . . ? C51 C35 H35A 119.9 . . ? C26 C35 H35A 119.9 . . ? C60 C36 C28 122.0(7) . . ? C60 C36 H36A 119.0 . . ? C28 C36 H36A 119.0 . . ? C63 C37 C28 119.3(6) . . ? C63 C37 C14 117.8(6) . . ? C28 C37 C14 122.8(5) . . ? C53 C38 C42 119.9(6) . . ? C53 C38 H38A 120.0 . . ? C42 C38 H38A 120.0 . . ? C66 C39 C15 120.9(6) . . ? C66 C39 H39A 119.5 . . ? C15 C39 H39A 119.5 . . ? O8 C40 C18 124.7(5) . . ? O8 C40 C52 115.0(5) . . ? C18 C40 C52 120.2(5) . . ? C45 C41 C46 120.2(6) . . ? C45 C41 H41A 119.9 . . ? C46 C41 H41A 119.9 . . ? C38 C42 C49 120.8(6) . . ? C38 C42 H42A 119.6 . . ? C49 C42 H42A 119.6 . . ? C65 C43 C29 121.7(6) . . ? C65 C43 H43A 119.1 . . ? C29 C43 H43A 119.1 . . ? C48 C44 C19 120.5(5) . . ? C48 C44 H44A 119.8 . . ? C19 C44 H44A 119.8 . . ? C51 C45 C41 120.2(6) . . ? C51 C45 H45A 119.9 . . ? C41 C45 H45A 119.9 . . ? C41 C46 C26 119.8(5) . . ? C41 C46 N3 123.4(5) . . ? C26 C46 N3 116.7(4) . . ? C44 C48 C65 121.6(6) . . ? C44 C48 H48A 119.2 . . ? C65 C48 H48A 119.2 . . ? C21 C49 C42 119.2(6) . . ? C21 C49 H49A 120.4 . . ? C42 C49 H49A 120.4 . . ? C58 C50 C25 123.4(6) . . ? C58 C50 H50A 118.3 . . ? C25 C50 H50A 118.3 . . ? C45 C51 C35 120.8(6) . . ? C45 C51 H51A 119.6 . . ? C35 C51 H51A 119.6 . . ? C40 C52 H52A 109.5 . . ? C40 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C40 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C38 C53 C34 120.3(6) . . ? C38 C53 H53A 119.9 . . ? C34 C53 H53A 119.9 . . ? C32 C54 H54A 109.5 . . ? C32 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C32 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C23 C55 H55A 109.5 . . ? C23 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C23 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C59 C56 C17 121.6(6) . . ? C59 C56 H56A 119.2 . . ? C17 C56 H56A 119.2 . . ? O5 C57 C64 124.6(5) . . ? O5 C57 C74 115.1(5) . . ? C64 C57 C74 120.3(5) . . ? C50 C58 C31 118.6(5) . . ? C50 C58 H58A 120.7 . . ? C31 C58 H58A 120.7 . . ? C56 C59 C66 121.6(6) . . ? C56 C59 H59A 119.2 . . ? C66 C59 H59A 119.2 . . ? C36 C60 C61 120.9(7) . . ? C36 C60 H60A 119.6 . . ? C61 C60 H60A 119.6 . . ? C60 C61 C63 119.5(7) . . ? C60 C61 H61A 120.3 . . ? C63 C61 H61A 120.3 . . ? C61 C63 C37 121.1(8) . . ? C61 C63 H63A 119.4 . . ? C37 C63 H63A 119.4 . . ? C32 C64 C57 126.6(5) . . ? C32 C64 H64A 116.7 . . ? C57 C64 H64A 116.7 . . ? C48 C65 C43 118.5(5) . . ? C48 C65 H65A 120.8 . . ? C43 C65 H65A 120.8 . . ? C39 C66 C59 118.8(6) . . ? C39 C66 H66A 120.6 . . ? C59 C66 H66A 120.6 . . ? Cl4 C71 Cl3 110.2(6) . . ? Cl4 C71 H71A 109.6 . . ? Cl3 C71 H71A 109.6 . . ? Cl4 C71 H71B 109.6 . . ? Cl3 C71 H71B 109.6 . . ? H71A C71 H71B 108.1 . . ? Cl2 C72 Cl1 110.3(5) . . ? Cl2 C72 H72A 109.6 . . ? Cl1 C72 H72A 109.6 . . ? Cl2 C72 H72B 109.6 . . ? Cl1 C72 H72B 109.6 . . ? H72A C72 H72B 108.1 . . ? C57 C74 H74A 109.5 . . ? C57 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C57 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Gd1 Gd2 O4 11.49(15) . . . . ? O5 Gd1 Gd2 O4 146.40(15) . . . . ? O7 Gd1 Gd2 O4 -78.2(2) . . . . ? O1 Gd1 Gd2 O4 169.09(17) . . . . ? O2 Gd1 Gd2 O4 -15.99(17) . . . . ? O6 Gd1 Gd2 O4 84.56(14) . . . . ? N1 Gd1 Gd2 O4 -136.32(15) . . . . ? N2 Gd1 Gd2 O4 -73.66(15) . . . . ? O8 Gd1 Gd2 O3 -133.80(13) . . . . ? O5 Gd1 Gd2 O3 1.11(14) . . . . ? O7 Gd1 Gd2 O3 136.5(2) . . . . ? O1 Gd1 Gd2 O3 23.81(16) . . . . ? O2 Gd1 Gd2 O3 -161.27(16) . . . . ? O6 Gd1 Gd2 O3 -60.72(13) . . . . ? N1 Gd1 Gd2 O3 78.39(13) . . . . ? N2 Gd1 Gd2 O3 141.05(13) . . . . ? O8 Gd1 Gd2 O2 27.47(15) . . . . ? O5 Gd1 Gd2 O2 162.38(16) . . . . ? O7 Gd1 Gd2 O2 -62.2(2) . . . . ? O1 Gd1 Gd2 O2 -174.92(17) . . . . ? O6 Gd1 Gd2 O2 100.55(15) . . . . ? N1 Gd1 Gd2 O2 -120.34(15) . . . . ? N2 Gd1 Gd2 O2 -57.68(15) . . . . ? O8 Gd1 Gd2 O1 -157.61(16) . . . . ? O5 Gd1 Gd2 O1 -22.70(16) . . . . ? O7 Gd1 Gd2 O1 112.7(2) . . . . ? O2 Gd1 Gd2 O1 174.92(17) . . . . ? O6 Gd1 Gd2 O1 -84.53(15) . . . . ? N1 Gd1 Gd2 O1 54.58(16) . . . . ? N2 Gd1 Gd2 O1 117.24(15) . . . . ? O8 Gd1 Gd2 O9 -63.79(13) . . . . ? O5 Gd1 Gd2 O9 71.11(13) . . . . ? O7 Gd1 Gd2 O9 -153.5(2) . . . . ? O1 Gd1 Gd2 O9 93.81(16) . . . . ? O2 Gd1 Gd2 O9 -91.27(15) . . . . ? O6 Gd1 Gd2 O9 9.28(12) . . . . ? N1 Gd1 Gd2 O9 148.40(13) . . . . ? N2 Gd1 Gd2 O9 -148.94(12) . . . . ? O8 Gd1 Gd2 N3 149.53(13) . . . . ? O5 Gd1 Gd2 N3 -75.56(13) . . . . ? O7 Gd1 Gd2 N3 59.9(2) . . . . ? O1 Gd1 Gd2 N3 -52.86(16) . . . . ? O2 Gd1 Gd2 N3 122.06(15) . . . . ? O6 Gd1 Gd2 N3 -137.39(12) . . . . ? N1 Gd1 Gd2 N3 1.72(12) . . . . ? N2 Gd1 Gd2 N3 64.38(12) . . . . ? O8 Gd1 Gd2 N4 84.57(13) . . . . ? O5 Gd1 Gd2 N4 -140.52(13) . . . . ? O7 Gd1 Gd2 N4 -5.1(2) . . . . ? O1 Gd1 Gd2 N4 -117.82(16) . . . . ? O2 Gd1 Gd2 N4 57.10(15) . . . . ? O6 Gd1 Gd2 N4 157.65(12) . . . . ? N1 Gd1 Gd2 N4 -63.24(13) . . . . ? N2 Gd1 Gd2 N4 -0.58(13) . . . . ? O4 Gd2 O1 C19 154.3(4) . . . . ? O3 Gd2 O1 C19 22.1(3) . . . . ? O2 Gd2 O1 C19 -173.0(4) . . . . ? O9 Gd2 O1 C19 105.0(3) . . . . ? N3 Gd2 O1 C19 -49.3(3) . . . . ? N4 Gd2 O1 C19 -105.8(3) . . . . ? Gd1 Gd2 O1 C19 -176.1(4) . . . . ? O4 Gd2 O1 Gd1 -29.6(4) . . . . ? O3 Gd2 O1 Gd1 -161.78(12) . . . . ? O2 Gd2 O1 Gd1 3.08(10) . . . . ? O9 Gd2 O1 Gd1 -78.93(13) . . . . ? N3 Gd2 O1 Gd1 126.79(15) . . . . ? N4 Gd2 O1 Gd1 70.26(15) . . . . ? O8 Gd1 O1 C19 -150.3(3) . . . . ? O5 Gd1 O1 C19 -23.7(3) . . . . ? O7 Gd1 O1 C19 34.0(4) . . . . ? O2 Gd1 O1 C19 173.1(4) . . . . ? O6 Gd1 O1 C19 -97.2(3) . . . . ? N1 Gd1 O1 C19 56.5(3) . . . . ? N2 Gd1 O1 C19 110.8(3) . . . . ? Gd2 Gd1 O1 C19 176.2(4) . . . . ? O8 Gd1 O1 Gd2 33.6(2) . . . . ? O5 Gd1 O1 Gd2 160.19(14) . . . . ? O7 Gd1 O1 Gd2 -142.17(16) . . . . ? O2 Gd1 O1 Gd2 -3.08(10) . . . . ? O6 Gd1 O1 Gd2 86.60(13) . . . . ? N1 Gd1 O1 Gd2 -119.64(15) . . . . ? N2 Gd1 O1 Gd2 -65.31(14) . . . . ? O4 Gd2 O2 C24 -18.9(3) . . . . ? O3 Gd2 O2 C24 -140.4(4) . . . . ? O1 Gd2 O2 C24 170.3(4) . . . . ? O9 Gd2 O2 C24 -105.7(3) . . . . ? N3 Gd2 O2 C24 105.1(3) . . . . ? N4 Gd2 O2 C24 51.8(3) . . . . ? Gd1 Gd2 O2 C24 173.4(4) . . . . ? O4 Gd2 O2 Gd1 167.74(13) . . . . ? O3 Gd2 O2 Gd1 46.3(3) . . . . ? O1 Gd2 O2 Gd1 -3.08(10) . . . . ? O9 Gd2 O2 Gd1 80.98(13) . . . . ? N3 Gd2 O2 Gd1 -68.24(15) . . . . ? N4 Gd2 O2 Gd1 -121.51(15) . . . . ? O8 Gd1 O2 C24 33.0(3) . . . . ? O5 Gd1 O2 C24 153.9(3) . . . . ? O7 Gd1 O2 C24 -18.7(4) . . . . ? O1 Gd1 O2 C24 -170.5(3) . . . . ? O6 Gd1 O2 C24 112.8(3) . . . . ? N1 Gd1 O2 C24 -110.1(3) . . . . ? N2 Gd1 O2 C24 -57.7(3) . . . . ? Gd2 Gd1 O2 C24 -173.6(4) . . . . ? O8 Gd1 O2 Gd2 -153.35(14) . . . . ? O5 Gd1 O2 Gd2 -32.5(3) . . . . ? O7 Gd1 O2 Gd2 154.91(11) . . . . ? O1 Gd1 O2 Gd2 3.08(10) . . . . ? O6 Gd1 O2 Gd2 -73.64(13) . . . . ? N1 Gd1 O2 Gd2 63.48(15) . . . . ? N2 Gd1 O2 Gd2 115.87(14) . . . . ? O4 Gd2 O3 C17 133.1(5) . . . . ? O2 Gd2 O3 C17 -105.1(5) . . . . ? O1 Gd2 O3 C17 -59.5(5) . . . . ? O9 Gd2 O3 C17 -139.3(5) . . . . ? N3 Gd2 O3 C17 16.4(5) . . . . ? N4 Gd2 O3 C17 60.9(5) . . . . ? Gd1 Gd2 O3 C17 -72.8(5) . . . . ? O8 Gd1 N2 C20 -41.2(4) . . . . ? O5 Gd1 N2 C20 -164.4(4) . . . . ? O7 Gd1 N2 C20 -114.2(4) . . . . ? O1 Gd1 N2 C20 98.5(4) . . . . ? O2 Gd1 N2 C20 36.8(4) . . . . ? O6 Gd1 N2 C20 15.9(5) . . . . ? N1 Gd1 N2 C20 157.5(4) . . . . ? Gd2 Gd1 N2 C20 67.4(4) . . . . ? O8 Gd1 N2 C21 128.0(3) . . . . ? O5 Gd1 N2 C21 4.8(4) . . . . ? O7 Gd1 N2 C21 55.0(3) . . . . ? O1 Gd1 N2 C21 -92.3(3) . . . . ? O2 Gd1 N2 C21 -154.0(3) . . . . ? O6 Gd1 N2 C21 -174.9(3) . . . . ? N1 Gd1 N2 C21 -33.3(3) . . . . ? Gd2 Gd1 N2 C21 -123.3(3) . . . . ? O4 Gd2 N3 C22 -94.2(4) . . . . ? O3 Gd2 N3 C22 -8.0(4) . . . . ? O2 Gd2 N3 C22 153.2(4) . . . . ? O1 Gd2 N3 C22 93.4(4) . . . . ? O9 Gd2 N3 C22 41.2(5) . . . . ? N4 Gd2 N3 C22 -146.4(4) . . . . ? Gd1 Gd2 N3 C22 120.8(4) . . . . ? O4 Gd2 N3 C46 89.2(3) . . . . ? O3 Gd2 N3 C46 175.4(3) . . . . ? O2 Gd2 N3 C46 -23.5(3) . . . . ? O1 Gd2 N3 C46 -83.3(3) . . . . ? O9 Gd2 N3 C46 -135.4(3) . . . . ? N4 Gd2 N3 C46 37.0(3) . . . . ? Gd1 Gd2 N3 C46 -55.8(3) . . . . ? O8 Gd1 O7 C23 -24.9(4) . . . . ? O5 Gd1 O7 C23 -147.7(4) . . . . ? O1 Gd1 O7 C23 152.2(4) . . . . ? O2 Gd1 O7 C23 28.5(4) . . . . ? O6 Gd1 O7 C23 -88.4(4) . . . . ? N1 Gd1 O7 C23 130.9(4) . . . . ? N2 Gd1 O7 C23 66.8(4) . . . . ? Gd2 Gd1 O7 C23 71.5(5) . . . . ? O8 Gd1 O6 C32 -126.0(4) . . . . ? O5 Gd1 O6 C32 -4.4(4) . . . . ? O7 Gd1 O6 C32 -65.4(4) . . . . ? O1 Gd1 O6 C32 86.2(4) . . . . ? O2 Gd1 O6 C32 155.7(4) . . . . ? N1 Gd1 O6 C32 49.0(5) . . . . ? N2 Gd1 O6 C32 175.4(4) . . . . ? Gd2 Gd1 O6 C32 121.8(4) . . . . ? O8 Gd1 O5 C57 74.1(5) . . . . ? O7 Gd1 O5 C57 137.2(5) . . . . ? O1 Gd1 O5 C57 -70.2(5) . . . . ? O2 Gd1 O5 C57 -37.3(6) . . . . ? O6 Gd1 O5 C57 5.9(5) . . . . ? N1 Gd1 O5 C57 -140.1(5) . . . . ? N2 Gd1 O5 C57 -173.9(5) . . . . ? Gd2 Gd1 O5 C57 -57.5(5) . . . . ? O5 Gd1 O8 C40 89.6(5) . . . . ? O7 Gd1 O8 C40 24.3(5) . . . . ? O1 Gd1 O8 C40 -153.3(4) . . . . ? O2 Gd1 O8 C40 -118.6(5) . . . . ? O6 Gd1 O8 C40 154.5(5) . . . . ? N1 Gd1 O8 C40 -19.6(6) . . . . ? N2 Gd1 O8 C40 -48.6(5) . . . . ? Gd2 Gd1 O8 C40 -134.1(5) . . . . ? O8 Gd1 N1 C27 178.6(4) . . . . ? O5 Gd1 N1 C27 58.5(4) . . . . ? O7 Gd1 N1 C27 136.5(4) . . . . ? O1 Gd1 N1 C27 -31.6(4) . . . . ? O2 Gd1 N1 C27 -91.5(4) . . . . ? O6 Gd1 N1 C27 7.1(5) . . . . ? N2 Gd1 N1 C27 -148.3(4) . . . . ? Gd2 Gd1 N1 C27 -61.1(4) . . . . ? O8 Gd1 N1 C34 0.7(4) . . . . ? O5 Gd1 N1 C34 -119.5(3) . . . . ? O7 Gd1 N1 C34 -41.4(3) . . . . ? O1 Gd1 N1 C34 150.4(3) . . . . ? O2 Gd1 N1 C34 90.5(3) . . . . ? O6 Gd1 N1 C34 -170.9(3) . . . . ? N2 Gd1 N1 C34 33.8(3) . . . . ? Gd2 Gd1 N1 C34 120.9(3) . . . . ? O4 Gd2 N4 C14 17.0(4) . . . . ? O3 Gd2 N4 C14 101.1(4) . . . . ? O2 Gd2 N4 C14 -83.7(4) . . . . ? O1 Gd2 N4 C14 -145.4(4) . . . . ? O9 Gd2 N4 C14 -38.4(5) . . . . ? N3 Gd2 N4 C14 149.4(4) . . . . ? Gd1 Gd2 N4 C14 -112.9(4) . . . . ? O4 Gd2 N4 C26 -169.4(3) . . . . ? O3 Gd2 N4 C26 -85.3(3) . . . . ? O2 Gd2 N4 C26 89.8(3) . . . . ? O1 Gd2 N4 C26 28.2(3) . . . . ? O9 Gd2 N4 C26 135.2(3) . . . . ? N3 Gd2 N4 C26 -37.1(3) . . . . ? Gd1 Gd2 N4 C26 60.7(3) . . . . ? C26 N4 C14 C37 177.7(5) . . . . ? Gd2 N4 C14 C37 -9.2(8) . . . . ? O3 Gd2 O4 C28 -145.8(5) . . . . ? O2 Gd2 O4 C28 51.1(5) . . . . ? O1 Gd2 O4 C28 81.6(6) . . . . ? O9 Gd2 O4 C28 130.1(5) . . . . ? N3 Gd2 O4 C28 -72.3(5) . . . . ? N4 Gd2 O4 C28 -24.1(5) . . . . ? Gd1 Gd2 O4 C28 60.2(5) . . . . ? Gd2 O3 C17 C56 164.4(4) . . . . ? Gd2 O3 C17 C15 -15.6(8) . . . . ? C39 C15 C17 O3 179.9(5) . . . . ? C22 C15 C17 O3 -0.9(8) . . . . ? C39 C15 C17 C56 -0.1(8) . . . . ? C22 C15 C17 C56 179.2(5) . . . . ? Gd2 O1 C19 C44 -58.5(6) . . . . ? Gd1 O1 C19 C44 125.9(4) . . . . ? Gd2 O1 C19 C29 118.1(4) . . . . ? Gd1 O1 C19 C29 -57.5(5) . . . . ? C21 N2 C20 C25 -179.3(4) . . . . ? Gd1 N2 C20 C25 -10.8(7) . . . . ? C20 N2 C21 C49 22.9(7) . . . . ? Gd1 N2 C21 C49 -146.9(4) . . . . ? C20 N2 C21 C34 -159.3(5) . . . . ? Gd1 N2 C21 C34 30.9(5) . . . . ? C46 N3 C22 C15 176.9(5) . . . . ? Gd2 N3 C22 C15 0.5(8) . . . . ? C17 C15 C22 N3 7.0(8) . . . . ? C39 C15 C22 N3 -173.7(5) . . . . ? Gd1 O7 C23 C18 20.4(7) . . . . ? Gd1 O7 C23 C55 -160.4(3) . . . . ? C40 C18 C23 O7 -0.3(8) . . . . ? C40 C18 C23 C55 -179.5(5) . . . . ? Gd2 O2 C24 C33 60.4(5) . . . . ? Gd1 O2 C24 C33 -127.0(4) . . . . ? Gd2 O2 C24 C25 -117.3(4) . . . . ? Gd1 O2 C24 C25 55.4(5) . . . . ? O2 C24 C25 C50 177.5(4) . . . . ? C33 C24 C25 C50 -0.2(7) . . . . ? O2 C24 C25 C20 -2.0(7) . . . . ? C33 C24 C25 C20 -179.6(5) . . . . ? N2 C20 C25 C50 160.7(5) . . . . ? N2 C20 C25 C24 -19.8(8) . . . . ? C14 N4 C26 C35 29.2(7) . . . . ? Gd2 N4 C26 C35 -145.0(4) . . . . ? C14 N4 C26 C46 -151.7(5) . . . . ? Gd2 N4 C26 C46 34.1(5) . . . . ? C34 N1 C27 C29 -177.0(5) . . . . ? Gd1 N1 C27 C29 5.1(7) . . . . ? Gd2 O4 C28 C36 -161.7(4) . . . . ? Gd2 O4 C28 C37 19.3(8) . . . . ? O1 C19 C29 C43 -172.2(5) . . . . ? C44 C19 C29 C43 4.5(7) . . . . ? O1 C19 C29 C27 5.4(7) . . . . ? C44 C19 C29 C27 -177.9(5) . . . . ? N1 C27 C29 C43 -162.0(5) . . . . ? N1 C27 C29 C19 20.4(8) . . . . ? Gd1 O6 C32 C64 4.7(8) . . . . ? Gd1 O6 C32 C54 -172.9(3) . . . . ? C58 C31 C33 C24 0.7(9) . . . . ? O2 C24 C33 C31 -178.8(4) . . . . ? C25 C24 C33 C31 -1.1(7) . . . . ? C49 C21 C34 C53 1.9(7) . . . . ? N2 C21 C34 C53 -176.0(4) . . . . ? C49 C21 C34 N1 178.9(4) . . . . ? N2 C21 C34 N1 1.0(6) . . . . ? C27 N1 C34 C21 149.2(5) . . . . ? Gd1 N1 C34 C21 -32.7(5) . . . . ? C27 N1 C34 C53 -33.9(7) . . . . ? Gd1 N1 C34 C53 144.2(4) . . . . ? C46 C26 C35 C51 -1.2(8) . . . . ? N4 C26 C35 C51 178.0(5) . . . . ? O4 C28 C36 C60 178.3(5) . . . . ? C37 C28 C36 C60 -2.6(8) . . . . ? O4 C28 C37 C63 -178.8(5) . . . . ? C36 C28 C37 C63 2.2(7) . . . . ? O4 C28 C37 C14 3.9(8) . . . . ? C36 C28 C37 C14 -175.1(5) . . . . ? N4 C14 C37 C63 176.7(5) . . . . ? N4 C14 C37 C28 -6.0(8) . . . . ? C17 C15 C39 C66 -2.3(8) . . . . ? C22 C15 C39 C66 178.4(6) . . . . ? Gd1 O8 C40 C18 -18.7(8) . . . . ? Gd1 O8 C40 C52 163.1(4) . . . . ? C23 C18 C40 O8 -0.9(9) . . . . ? C23 C18 C40 C52 177.2(6) . . . . ? C53 C38 C42 C49 1.8(11) . . . . ? C19 C29 C43 C65 -4.5(9) . . . . ? C27 C29 C43 C65 177.8(6) . . . . ? O1 C19 C44 C48 175.2(5) . . . . ? C29 C19 C44 C48 -1.5(8) . . . . ? C46 C41 C45 C51 0.5(9) . . . . ? C45 C41 C46 C26 -2.2(8) . . . . ? C45 C41 C46 N3 -179.2(5) . . . . ? C35 C26 C46 C41 2.5(7) . . . . ? N4 C26 C46 C41 -176.7(4) . . . . ? C35 C26 C46 N3 179.7(4) . . . . ? N4 C26 C46 N3 0.5(6) . . . . ? C22 N3 C46 C41 -35.1(7) . . . . ? Gd2 N3 C46 C41 142.0(4) . . . . ? C22 N3 C46 C26 147.9(4) . . . . ? Gd2 N3 C46 C26 -35.1(5) . . . . ? C19 C44 C48 C65 -1.7(10) . . . . ? C34 C21 C49 C42 -0.9(8) . . . . ? N2 C21 C49 C42 176.9(5) . . . . ? C38 C42 C49 C21 -0.9(9) . . . . ? C24 C25 C50 C58 1.9(9) . . . . ? C20 C25 C50 C58 -178.6(6) . . . . ? C41 C45 C51 C35 0.9(10) . . . . ? C26 C35 C51 C45 -0.6(9) . . . . ? C42 C38 C53 C34 -0.7(10) . . . . ? C21 C34 C53 C38 -1.1(8) . . . . ? N1 C34 C53 C38 -177.9(5) . . . . ? O3 C17 C56 C59 -177.4(6) . . . . ? C15 C17 C56 C59 2.6(9) . . . . ? Gd1 O5 C57 C64 -7.6(9) . . . . ? Gd1 O5 C57 C74 172.1(5) . . . . ? C25 C50 C58 C31 -2.3(10) . . . . ? C33 C31 C58 C50 1.0(10) . . . . ? C17 C56 C59 C66 -2.8(12) . . . . ? C28 C36 C60 C61 0.8(10) . . . . ? C36 C60 C61 C63 1.5(11) . . . . ? C60 C61 C63 C37 -1.9(11) . . . . ? C28 C37 C63 C61 0.0(9) . . . . ? C14 C37 C63 C61 177.5(6) . . . . ? O6 C32 C64 C57 -3.7(9) . . . . ? C54 C32 C64 C57 173.8(6) . . . . ? O5 C57 C64 C32 5.0(10) . . . . ? C74 C57 C64 C32 -174.7(6) . . . . ? C44 C48 C65 C43 1.7(11) . . . . ? C29 C43 C65 C48 1.4(10) . . . . ? C15 C39 C66 C59 2.2(10) . . . . ? C56 C59 C66 C39 0.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.941 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 830602' ####################################################################### # # 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_37 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H44 N4 O9 Tb2' _chemical_formula_sum 'C50 H44 N4 O9 Tb2' _chemical_formula_weight 1162.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9763(5) _cell_length_b 19.4129(7) _cell_length_c 19.3280(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.2460(10) _cell_angle_gamma 90.00 _cell_volume 4674.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5975 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.27 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 3.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5149 _exptl_absorpt_correction_T_max 0.6088 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34033 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11585 _reflns_number_gt 8171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT-plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0301P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11585 _refine_ls_number_parameters 592 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.367034(15) 0.474253(11) 0.207940(10) 0.03361(6) Uani 1 1 d . . . Tb2 Tb 0.457228(14) 0.591209(10) 0.376620(10) 0.02948(6) Uani 1 1 d . . . O3 O 0.61603(19) 0.58459(14) 0.46015(14) 0.0367(7) Uani 1 1 d . . . O2 O 0.31175(19) 0.55377(15) 0.28216(14) 0.0365(7) Uani 1 1 d . . . O1 O 0.51548(19) 0.52002(14) 0.29479(13) 0.0344(6) Uani 1 1 d . . . O5 O 0.4906(2) 0.38991(16) 0.20018(15) 0.0440(7) Uani 1 1 d . . . O4 O 0.3802(2) 0.63214(15) 0.45485(15) 0.0437(7) Uani 1 1 d . . . O9 O 0.4197(3) 0.48369(16) 0.42262(16) 0.0446(8) Uani 1 1 d D . . O6 O 0.3807(2) 0.39667(16) 0.30640(15) 0.0415(7) Uani 1 1 d . . . O8 O 0.1934(2) 0.43761(17) 0.19335(16) 0.0496(8) Uani 1 1 d . . . N3 N 0.5789(3) 0.66977(19) 0.33612(18) 0.0411(9) Uani 1 1 d . . . N2 N 0.2815(3) 0.57972(19) 0.13427(19) 0.0425(9) Uani 1 1 d . . . N1 N 0.4819(3) 0.54329(19) 0.14507(18) 0.0415(9) Uani 1 1 d . . . O7 O 0.3001(2) 0.43964(17) 0.08858(16) 0.0515(8) Uani 1 1 d . . . C1 C 0.6158(3) 0.5057(2) 0.2935(2) 0.0348(9) Uani 1 1 d . . . C20 C 0.2106(3) 0.5766(2) 0.2694(2) 0.0355(10) Uani 1 1 d . . . N4 N 0.3787(3) 0.70410(19) 0.33051(18) 0.0422(9) Uani 1 1 d . . . C21 C 0.7182(3) 0.5981(2) 0.4672(2) 0.0364(10) Uani 1 1 d . . . C2 C 0.6879(3) 0.4766(2) 0.3540(2) 0.0425(11) Uani 1 1 d . . . H2A H 0.6649 0.4666 0.3943 0.051 Uiso 1 1 calc R . . C40 C 0.3081(3) 0.6771(2) 0.4614(2) 0.0418(11) Uani 1 1 d . . . C8 C 0.4243(4) 0.5734(3) 0.0782(2) 0.0458(11) Uani 1 1 d . . . C15 C 0.1551(3) 0.6056(2) 0.2024(2) 0.0408(11) Uani 1 1 d . . . C14 C 0.2014(3) 0.6129(2) 0.1428(2) 0.0480(12) Uani 1 1 d . . . H14A H 0.1695 0.6448 0.1074 0.058 Uiso 1 1 calc R . . C26 C 0.7524(3) 0.6425(2) 0.4203(2) 0.0407(10) Uani 1 1 d . . . C6 C 0.6523(3) 0.5197(3) 0.2329(2) 0.0446(11) Uani 1 1 d . . . C22 C 0.7973(3) 0.5661(3) 0.5216(2) 0.0550(13) Uani 1 1 d . . . H22A H 0.7765 0.5366 0.5532 0.066 Uiso 1 1 calc R . . C27 C 0.6815(3) 0.6775(3) 0.3602(2) 0.0498(12) Uani 1 1 d . . . H27A H 0.7128 0.7092 0.3361 0.060 Uiso 1 1 calc R . . C19 C 0.1586(3) 0.5734(3) 0.3232(3) 0.0494(12) Uani 1 1 d . . . H19A H 0.1945 0.5550 0.3678 0.059 Uiso 1 1 calc R . . C47 C 0.2058(4) 0.4340(3) 0.0468(3) 0.0602(14) Uani 1 1 d . . . C13 C 0.3183(4) 0.5923(2) 0.0723(2) 0.0462(11) Uani 1 1 d . . . C35 C 0.2660(3) 0.7280(2) 0.4094(3) 0.0465(11) Uani 1 1 d . . . C44 C 0.4379(3) 0.3440(2) 0.3305(2) 0.0408(10) Uani 1 1 d . . . C34 C 0.3079(3) 0.7411(2) 0.3492(3) 0.0510(12) Uani 1 1 d . . . H34A H 0.2819 0.7797 0.3213 0.061 Uiso 1 1 calc R . . C7 C 0.5841(3) 0.5486(3) 0.1665(2) 0.0490(12) Uani 1 1 d . . . H7A H 0.6174 0.5728 0.1373 0.059 Uiso 1 1 calc R . . C45 C 0.4241(4) 0.3123(2) 0.3982(2) 0.0531(12) Uani 1 1 d . . . H45A H 0.3696 0.3368 0.4129 0.080 Uiso 1 1 calc R . . H45B H 0.4907 0.3149 0.4356 0.080 Uiso 1 1 calc R . . H45C H 0.4033 0.2649 0.3893 0.080 Uiso 1 1 calc R . . C28 C 0.5201(4) 0.7066(3) 0.2734(3) 0.0513(12) Uani 1 1 d . . . C3 C 0.7925(4) 0.4623(3) 0.3551(3) 0.0580(14) Uani 1 1 d . . . H3A H 0.8388 0.4420 0.3956 0.070 Uiso 1 1 calc R . . C9 C 0.4645(4) 0.5795(3) 0.0191(2) 0.0540(13) Uani 1 1 d . . . H9A H 0.5347 0.5661 0.0230 0.065 Uiso 1 1 calc R . . C10 C 0.4022(4) 0.6052(3) -0.0449(3) 0.0694(16) Uani 1 1 d . . . H10A H 0.4302 0.6094 -0.0841 0.083 Uiso 1 1 calc R . . C4 C 0.8288(4) 0.4782(3) 0.2957(3) 0.0680(17) Uani 1 1 d . . . H4A H 0.8996 0.4692 0.2966 0.082 Uiso 1 1 calc R . . C24 C 0.9383(4) 0.6206(3) 0.4845(3) 0.0649(15) Uani 1 1 d . . . H24A H 1.0110 0.6278 0.4900 0.078 Uiso 1 1 calc R . . C33 C 0.4147(3) 0.7246(2) 0.2705(2) 0.0482(12) Uani 1 1 d . . . C42 C 0.5392(4) 0.3412(3) 0.2399(3) 0.0505(12) Uani 1 1 d . . . C5 C 0.7608(4) 0.5068(3) 0.2371(3) 0.0643(16) Uani 1 1 d . . . H5A H 0.7861 0.5183 0.1981 0.077 Uiso 1 1 calc R . . C17 C 0.0008(4) 0.6250(3) 0.2459(3) 0.0637(15) Uani 1 1 d . . . H17A H -0.0695 0.6402 0.2378 0.076 Uiso 1 1 calc R . . C49 C 0.1118(4) 0.4307(3) 0.1405(3) 0.0588(14) Uani 1 1 d . . . C18 C 0.0545(4) 0.5971(3) 0.3119(3) 0.0612(14) Uani 1 1 d . . . H18A H 0.0210 0.5942 0.3485 0.073 Uiso 1 1 calc R . . C25 C 0.8636(3) 0.6528(3) 0.4316(3) 0.0631(15) Uani 1 1 d . . . H25A H 0.8862 0.6830 0.4014 0.076 Uiso 1 1 calc R . . C43 C 0.5134(4) 0.3170(2) 0.3001(3) 0.0544(13) Uani 1 1 d . . . H43A H 0.5508 0.2784 0.3224 0.065 Uiso 1 1 calc R . . C16 C 0.0504(3) 0.6302(3) 0.1929(3) 0.0540(13) Uani 1 1 d . . . H16A H 0.0142 0.6505 0.1494 0.065 Uiso 1 1 calc R . . C12 C 0.2561(4) 0.6194(3) 0.0071(3) 0.0672(16) Uani 1 1 d . . . H12A H 0.1863 0.6339 0.0029 0.081 Uiso 1 1 calc R . . C23 C 0.9051(4) 0.5766(3) 0.5304(3) 0.0659(16) Uani 1 1 d . . . H23A H 0.9557 0.5542 0.5672 0.079 Uiso 1 1 calc R . . C41 C 0.6332(5) 0.3099(3) 0.2193(3) 0.086(2) Uani 1 1 d . . . H41A H 0.6410 0.3320 0.1766 0.129 Uiso 1 1 calc R . . H41B H 0.6208 0.2616 0.2103 0.129 Uiso 1 1 calc R . . H41C H 0.6975 0.3163 0.2580 0.129 Uiso 1 1 calc R . . C48 C 0.1130(4) 0.4309(3) 0.0691(3) 0.0723(17) Uani 1 1 d . . . H48A H 0.0475 0.4288 0.0338 0.087 Uiso 1 1 calc R . . C39 C 0.2707(4) 0.6754(3) 0.5232(3) 0.0576(13) Uani 1 1 d . . . H39A H 0.2997 0.6439 0.5597 0.069 Uiso 1 1 calc R . . C36 C 0.1843(4) 0.7723(3) 0.4185(4) 0.0730(17) Uani 1 1 d . . . H36A H 0.1558 0.8056 0.3838 0.088 Uiso 1 1 calc R . . C32 C 0.3519(4) 0.7600(3) 0.2106(3) 0.0722(17) Uani 1 1 d . . . H32A H 0.2825 0.7732 0.2091 0.087 Uiso 1 1 calc R . . C29 C 0.5591(4) 0.7216(3) 0.2155(3) 0.0732(18) Uani 1 1 d . . . H29A H 0.6290 0.7095 0.2169 0.088 Uiso 1 1 calc R . . C38 C 0.1919(4) 0.7198(3) 0.5303(3) 0.0750(17) Uani 1 1 d . . . H38A H 0.1687 0.7180 0.5716 0.090 Uiso 1 1 calc R . . C11 C 0.2974(5) 0.6249(3) -0.0513(3) 0.0779(19) Uani 1 1 d . . . H11A H 0.2548 0.6418 -0.0949 0.093 Uiso 1 1 calc R . . C37 C 0.1467(5) 0.7668(4) 0.4775(4) 0.091(2) Uani 1 1 d . . . H37A H 0.0908 0.7948 0.4819 0.109 Uiso 1 1 calc R . . C50 C 0.0067(4) 0.4217(4) 0.1597(3) 0.091(2) Uani 1 1 d . . . H50A H 0.0204 0.4223 0.2112 0.136 Uiso 1 1 calc R . . H50B H -0.0255 0.3786 0.1411 0.136 Uiso 1 1 calc R . . H50C H -0.0412 0.4587 0.1390 0.136 Uiso 1 1 calc R . . C31 C 0.3923(5) 0.7752(4) 0.1536(3) 0.102(3) Uani 1 1 d . . . H31A H 0.3506 0.7994 0.1141 0.122 Uiso 1 1 calc R . . C46 C 0.1977(5) 0.4284(4) -0.0335(3) 0.095(2) Uani 1 1 d . . . H46A H 0.2682 0.4309 -0.0401 0.142 Uiso 1 1 calc R . . H46B H 0.1546 0.4655 -0.0591 0.142 Uiso 1 1 calc R . . H46C H 0.1652 0.3852 -0.0517 0.142 Uiso 1 1 calc R . . C30 C 0.4944(5) 0.7547(4) 0.1551(3) 0.101(2) Uani 1 1 d . . . H30A H 0.5202 0.7630 0.1155 0.121 Uiso 1 1 calc R . . HW1 H 0.394(5) 0.460(3) 0.385(2) 0.152 Uiso 1 1 d D . . HW2 H 0.401(5) 0.467(3) 0.458(2) 0.152 Uiso 1 1 d 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 Tb1 0.02844(10) 0.04183(13) 0.02799(10) -0.00031(9) 0.00366(8) -0.00118(9) Tb2 0.02576(10) 0.03395(12) 0.02784(10) 0.00308(9) 0.00602(7) -0.00046(8) O3 0.0264(14) 0.0493(19) 0.0332(15) 0.0045(14) 0.0061(11) -0.0051(13) O2 0.0248(13) 0.0466(18) 0.0365(15) -0.0001(14) 0.0060(12) 0.0017(13) O1 0.0244(13) 0.0474(18) 0.0312(14) -0.0028(13) 0.0075(11) 0.0007(12) O5 0.0485(18) 0.046(2) 0.0377(17) -0.0012(15) 0.0127(14) 0.0043(15) O4 0.0451(17) 0.0433(19) 0.0461(18) 0.0086(15) 0.0181(14) 0.0155(14) O9 0.061(2) 0.0397(19) 0.0349(16) 0.0014(14) 0.0160(15) -0.0105(15) O6 0.0403(16) 0.046(2) 0.0379(17) 0.0031(14) 0.0097(13) 0.0007(14) O8 0.0335(16) 0.062(2) 0.0491(19) -0.0001(16) 0.0042(14) -0.0108(15) N3 0.0366(19) 0.044(2) 0.041(2) 0.0122(17) 0.0084(16) -0.0034(17) N2 0.037(2) 0.048(2) 0.040(2) 0.0076(18) 0.0061(16) -0.0007(17) N1 0.0375(19) 0.055(3) 0.0316(19) 0.0035(17) 0.0088(15) -0.0021(17) O7 0.0441(18) 0.064(2) 0.0395(18) -0.0103(16) 0.0000(14) -0.0034(16) C1 0.027(2) 0.043(3) 0.034(2) -0.0095(19) 0.0087(17) -0.0049(18) C20 0.027(2) 0.035(3) 0.041(2) 0.0000(19) 0.0025(18) 0.0015(17) N4 0.039(2) 0.042(2) 0.043(2) 0.0125(18) 0.0051(16) -0.0017(17) C21 0.029(2) 0.040(3) 0.038(2) -0.004(2) 0.0045(17) -0.0003(18) C2 0.032(2) 0.056(3) 0.038(2) 0.000(2) 0.0074(19) 0.002(2) C40 0.032(2) 0.041(3) 0.054(3) -0.003(2) 0.015(2) -0.0003(19) C8 0.046(3) 0.058(3) 0.032(2) 0.007(2) 0.008(2) -0.003(2) C15 0.030(2) 0.039(3) 0.049(3) 0.001(2) 0.0038(19) 0.0028(19) C14 0.040(3) 0.048(3) 0.047(3) 0.014(2) -0.002(2) 0.004(2) C26 0.030(2) 0.046(3) 0.046(3) 0.001(2) 0.0092(19) -0.0046(19) C6 0.029(2) 0.066(3) 0.040(2) 0.003(2) 0.0112(19) 0.000(2) C22 0.039(3) 0.077(4) 0.044(3) 0.014(3) 0.004(2) -0.006(2) C27 0.039(2) 0.057(3) 0.055(3) 0.010(2) 0.016(2) -0.015(2) C19 0.041(2) 0.060(3) 0.050(3) 0.005(2) 0.016(2) 0.003(2) C47 0.058(3) 0.069(4) 0.041(3) -0.008(3) -0.007(2) -0.003(3) C13 0.048(3) 0.055(3) 0.033(2) 0.007(2) 0.007(2) -0.007(2) C35 0.040(2) 0.034(3) 0.065(3) 0.000(2) 0.014(2) 0.008(2) C44 0.049(3) 0.037(3) 0.034(2) -0.002(2) 0.007(2) -0.009(2) C34 0.042(3) 0.035(3) 0.067(3) 0.015(2) 0.002(2) 0.005(2) C7 0.043(3) 0.067(3) 0.040(3) 0.005(2) 0.019(2) -0.005(2) C45 0.071(3) 0.043(3) 0.048(3) -0.001(2) 0.020(2) -0.009(2) C28 0.047(3) 0.052(3) 0.053(3) 0.024(2) 0.011(2) -0.003(2) C3 0.038(3) 0.082(4) 0.049(3) 0.003(3) 0.005(2) 0.010(3) C9 0.053(3) 0.073(4) 0.036(3) 0.008(2) 0.012(2) -0.009(3) C10 0.074(4) 0.097(5) 0.038(3) 0.014(3) 0.018(3) -0.011(3) C4 0.030(2) 0.114(5) 0.062(3) -0.002(3) 0.016(2) 0.003(3) C24 0.031(2) 0.092(4) 0.069(4) -0.001(3) 0.009(2) -0.006(3) C33 0.044(3) 0.045(3) 0.051(3) 0.018(2) 0.007(2) -0.004(2) C42 0.057(3) 0.046(3) 0.052(3) -0.003(2) 0.020(2) 0.008(2) C5 0.036(3) 0.109(5) 0.052(3) 0.000(3) 0.019(2) 0.001(3) C17 0.032(2) 0.067(4) 0.093(4) 0.009(3) 0.019(3) 0.016(2) C49 0.035(3) 0.057(3) 0.078(4) -0.002(3) 0.003(3) -0.003(2) C18 0.041(3) 0.067(4) 0.082(4) 0.000(3) 0.028(3) 0.006(3) C25 0.034(2) 0.083(4) 0.072(4) 0.011(3) 0.013(2) -0.013(3) C43 0.077(3) 0.041(3) 0.051(3) 0.012(2) 0.026(3) 0.019(3) C16 0.035(2) 0.061(3) 0.062(3) 0.009(3) 0.005(2) 0.010(2) C12 0.050(3) 0.099(5) 0.048(3) 0.026(3) 0.006(2) 0.004(3) C23 0.037(3) 0.096(5) 0.056(3) 0.008(3) -0.001(2) 0.002(3) C41 0.102(5) 0.088(5) 0.085(4) 0.020(4) 0.056(4) 0.050(4) C48 0.044(3) 0.103(5) 0.056(3) -0.010(3) -0.010(3) -0.010(3) C39 0.053(3) 0.057(3) 0.071(4) 0.000(3) 0.031(3) 0.010(3) C36 0.063(3) 0.050(4) 0.107(5) 0.004(3) 0.025(3) 0.021(3) C32 0.057(3) 0.083(4) 0.070(4) 0.042(3) 0.006(3) 0.004(3) C29 0.057(3) 0.105(5) 0.061(3) 0.037(3) 0.021(3) -0.003(3) C38 0.072(4) 0.071(4) 0.098(5) -0.009(4) 0.051(4) 0.010(3) C11 0.073(4) 0.117(5) 0.038(3) 0.032(3) 0.005(3) 0.000(4) C37 0.069(4) 0.080(5) 0.137(6) 0.001(5) 0.051(4) 0.026(4) C50 0.031(3) 0.135(6) 0.098(5) -0.009(4) 0.006(3) -0.019(3) C31 0.063(4) 0.157(7) 0.080(4) 0.078(5) 0.011(3) 0.001(4) C46 0.095(5) 0.134(6) 0.039(3) -0.013(4) -0.009(3) -0.010(4) C30 0.085(5) 0.147(7) 0.075(4) 0.061(5) 0.031(4) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O8 2.303(3) . ? Tb1 O7 2.325(3) . ? Tb1 O5 2.326(3) . ? Tb1 O1 2.347(2) . ? Tb1 O2 2.352(3) . ? Tb1 O6 2.394(3) . ? Tb1 N1 2.551(3) . ? Tb1 N2 2.563(4) . ? Tb1 Tb2 3.8754(3) . ? Tb2 O4 2.182(3) . ? Tb2 O3 2.238(2) . ? Tb2 O2 2.345(3) . ? Tb2 O9 2.372(3) . ? Tb2 O1 2.377(3) . ? Tb2 N3 2.475(3) . ? Tb2 N4 2.475(4) . ? O3 C21 1.321(4) . ? O2 C20 1.340(4) . ? O1 C1 1.337(4) . ? O5 C42 1.268(5) . ? O4 C40 1.311(5) . ? O9 HW1 0.847(10) . ? O9 HW2 0.845(10) . ? O6 C44 1.273(5) . ? O8 C49 1.257(5) . ? N3 C27 1.289(5) . ? N3 C28 1.430(5) . ? N2 C14 1.273(5) . ? N2 C13 1.429(5) . ? N1 C7 1.278(5) . ? N1 C8 1.425(5) . ? O7 C47 1.268(5) . ? C1 C2 1.396(6) . ? C1 C6 1.408(5) . ? C20 C19 1.391(6) . ? C20 C15 1.411(6) . ? N4 C34 1.295(5) . ? N4 C33 1.424(5) . ? C21 C22 1.394(6) . ? C21 C26 1.408(6) . ? C2 C3 1.379(6) . ? C2 H2A 0.9300 . ? C40 C35 1.406(6) . ? C40 C39 1.410(6) . ? C8 C9 1.387(6) . ? C8 C13 1.397(6) . ? C15 C16 1.403(5) . ? C15 C14 1.447(6) . ? C14 H14A 0.9300 . ? C26 C25 1.412(5) . ? C26 C27 1.436(6) . ? C6 C5 1.410(6) . ? C6 C7 1.452(6) . ? C22 C23 1.377(6) . ? C22 H22A 0.9300 . ? C27 H27A 0.9300 . ? C19 C18 1.385(6) . ? C19 H19A 0.9300 . ? C47 C48 1.390(7) . ? C47 C46 1.528(7) . ? C13 C12 1.395(6) . ? C35 C36 1.413(6) . ? C35 C34 1.438(6) . ? C44 C43 1.380(6) . ? C44 C45 1.501(6) . ? C34 H34A 0.9300 . ? C7 H7A 0.9300 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C28 C29 1.383(6) . ? C28 C33 1.397(6) . ? C3 C4 1.393(7) . ? C3 H3A 0.9300 . ? C9 C10 1.368(6) . ? C9 H9A 0.9300 . ? C10 C11 1.385(7) . ? C10 H10A 0.9300 . ? C4 C5 1.346(7) . ? C4 H4A 0.9300 . ? C24 C25 1.349(7) . ? C24 C23 1.384(7) . ? C24 H24A 0.9300 . ? C33 C32 1.395(6) . ? C42 C43 1.380(6) . ? C42 C41 1.513(6) . ? C5 H5A 0.9300 . ? C17 C16 1.357(7) . ? C17 C18 1.382(7) . ? C17 H17A 0.9300 . ? C49 C48 1.384(7) . ? C49 C50 1.521(7) . ? C18 H18A 0.9300 . ? C25 H25A 0.9300 . ? C43 H43A 0.9300 . ? C16 H16A 0.9300 . ? C12 C11 1.382(7) . ? C12 H12A 0.9300 . ? C23 H23A 0.9300 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C48 H48A 0.9300 . ? C39 C38 1.372(6) . ? C39 H39A 0.9300 . ? C36 C37 1.364(8) . ? C36 H36A 0.9300 . ? C32 C31 1.378(7) . ? C32 H32A 0.9300 . ? C29 C30 1.390(7) . ? C29 H29A 0.9300 . ? C38 C37 1.373(8) . ? C38 H38A 0.9300 . ? C11 H11A 0.9300 . ? C37 H37A 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C31 C30 1.376(8) . ? C31 H31A 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C30 H30A 0.9300 . ? 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 O8 Tb1 O7 73.03(11) . . ? O8 Tb1 O5 116.31(11) . . ? O7 Tb1 O5 78.79(10) . . ? O8 Tb1 O1 141.57(10) . . ? O7 Tb1 O1 145.40(10) . . ? O5 Tb1 O1 82.52(9) . . ? O8 Tb1 O2 79.78(10) . . ? O7 Tb1 O2 134.56(10) . . ? O5 Tb1 O2 146.60(9) . . ? O1 Tb1 O2 69.18(9) . . ? O8 Tb1 O6 75.85(10) . . ? O7 Tb1 O6 122.06(11) . . ? O5 Tb1 O6 73.10(10) . . ? O1 Tb1 O6 78.82(9) . . ? O2 Tb1 O6 84.00(10) . . ? O8 Tb1 N1 141.79(11) . . ? O7 Tb1 N1 77.60(11) . . ? O5 Tb1 N1 80.43(11) . . ? O1 Tb1 N1 70.72(10) . . ? O2 Tb1 N1 105.33(11) . . ? O6 Tb1 N1 141.79(10) . . ? O8 Tb1 N2 85.53(11) . . ? O7 Tb1 N2 72.30(12) . . ? O5 Tb1 N2 136.53(11) . . ? O1 Tb1 N2 103.66(10) . . ? O2 Tb1 N2 69.88(10) . . ? O6 Tb1 N2 150.30(11) . . ? N1 Tb1 N2 62.32(11) . . ? O8 Tb1 Tb2 109.80(8) . . ? O7 Tb1 Tb2 160.91(8) . . ? O5 Tb1 Tb2 114.53(7) . . ? O1 Tb1 Tb2 35.14(6) . . ? O2 Tb1 Tb2 34.33(6) . . ? O6 Tb1 Tb2 76.24(7) . . ? N1 Tb1 Tb2 90.79(8) . . ? N2 Tb1 Tb2 88.93(8) . . ? O4 Tb2 O3 91.66(10) . . ? O4 Tb2 O2 103.14(10) . . ? O3 Tb2 O2 157.27(10) . . ? O4 Tb2 O9 83.03(11) . . ? O3 Tb2 O9 85.60(10) . . ? O2 Tb2 O9 79.28(10) . . ? O4 Tb2 O1 164.82(10) . . ? O3 Tb2 O1 92.67(9) . . ? O2 Tb2 O1 68.80(9) . . ? O9 Tb2 O1 82.81(10) . . ? O4 Tb2 N3 116.83(12) . . ? O3 Tb2 N3 73.93(10) . . ? O2 Tb2 N3 113.00(10) . . ? O9 Tb2 N3 151.28(11) . . ? O1 Tb2 N3 78.34(11) . . ? O4 Tb2 N4 72.83(11) . . ? O3 Tb2 N4 120.92(11) . . ? O2 Tb2 N4 80.41(11) . . ? O9 Tb2 N4 143.79(11) . . ? O1 Tb2 N4 116.79(11) . . ? N3 Tb2 N4 64.88(11) . . ? O4 Tb2 Tb1 135.00(8) . . ? O3 Tb2 Tb1 125.01(7) . . ? O2 Tb2 Tb1 34.45(6) . . ? O9 Tb2 Tb1 75.79(7) . . ? O1 Tb2 Tb1 34.63(6) . . ? N3 Tb2 Tb1 99.45(8) . . ? N4 Tb2 Tb1 102.64(8) . . ? C21 O3 Tb2 139.3(2) . . ? C20 O2 Tb2 125.1(2) . . ? C20 O2 Tb1 123.7(2) . . ? Tb2 O2 Tb1 111.22(10) . . ? C1 O1 Tb1 121.1(2) . . ? C1 O1 Tb2 128.7(2) . . ? Tb1 O1 Tb2 110.23(9) . . ? C42 O5 Tb1 136.1(3) . . ? C40 O4 Tb2 141.9(3) . . ? Tb2 O9 HW1 103(4) . . ? Tb2 O9 HW2 140(5) . . ? HW1 O9 HW2 110.4(18) . . ? C44 O6 Tb1 134.6(3) . . ? C49 O8 Tb1 134.9(3) . . ? C27 N3 C28 120.0(4) . . ? C27 N3 Tb2 130.0(3) . . ? C28 N3 Tb2 109.8(2) . . ? C14 N2 C13 119.9(4) . . ? C14 N2 Tb1 125.1(3) . . ? C13 N2 Tb1 114.1(3) . . ? C7 N1 C8 119.7(4) . . ? C7 N1 Tb1 125.4(3) . . ? C8 N1 Tb1 114.8(3) . . ? C47 O7 Tb1 133.1(3) . . ? O1 C1 C2 119.8(4) . . ? O1 C1 C6 122.1(4) . . ? C2 C1 C6 118.1(4) . . ? O2 C20 C19 120.2(4) . . ? O2 C20 C15 121.5(4) . . ? C19 C20 C15 118.2(4) . . ? C34 N4 C33 119.5(4) . . ? C34 N4 Tb2 130.1(3) . . ? C33 N4 Tb2 110.2(3) . . ? O3 C21 C22 119.7(4) . . ? O3 C21 C26 122.9(4) . . ? C22 C21 C26 117.4(4) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? O4 C40 C35 122.9(4) . . ? O4 C40 C39 119.4(4) . . ? C35 C40 C39 117.7(4) . . ? C9 C8 C13 120.0(4) . . ? C9 C8 N1 124.0(4) . . ? C13 C8 N1 115.8(4) . . ? C16 C15 C20 118.9(4) . . ? C16 C15 C14 117.7(4) . . ? C20 C15 C14 123.4(4) . . ? N2 C14 C15 126.1(4) . . ? N2 C14 H14A 116.9 . . ? C15 C14 H14A 116.9 . . ? C21 C26 C25 118.7(4) . . ? C21 C26 C27 124.4(4) . . ? C25 C26 C27 116.9(4) . . ? C1 C6 C5 118.8(4) . . ? C1 C6 C7 123.0(4) . . ? C5 C6 C7 118.2(4) . . ? C23 C22 C21 122.4(5) . . ? C23 C22 H22A 118.8 . . ? C21 C22 H22A 118.8 . . ? N3 C27 C26 126.8(4) . . ? N3 C27 H27A 116.6 . . ? C26 C27 H27A 116.6 . . ? C18 C19 C20 121.6(5) . . ? C18 C19 H19A 119.2 . . ? C20 C19 H19A 119.2 . . ? O7 C47 C48 124.8(5) . . ? O7 C47 C46 115.7(5) . . ? C48 C47 C46 119.5(5) . . ? C12 C13 C8 118.6(4) . . ? C12 C13 N2 125.3(4) . . ? C8 C13 N2 116.0(4) . . ? C40 C35 C36 119.6(5) . . ? C40 C35 C34 122.9(4) . . ? C36 C35 C34 117.3(5) . . ? O6 C44 C43 124.0(4) . . ? O6 C44 C45 116.7(4) . . ? C43 C44 C45 119.2(4) . . ? N4 C34 C35 125.9(4) . . ? N4 C34 H34A 117.1 . . ? C35 C34 H34A 117.1 . . ? N1 C7 C6 125.3(4) . . ? N1 C7 H7A 117.4 . . ? C6 C7 H7A 117.4 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C29 C28 C33 119.3(4) . . ? C29 C28 N3 124.2(4) . . ? C33 C28 N3 116.4(4) . . ? C2 C3 C4 120.1(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C10 C9 C8 120.9(5) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 119.8(5) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C25 C24 C23 119.1(4) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C32 C33 C28 119.7(4) . . ? C32 C33 N4 124.4(4) . . ? C28 C33 N4 115.9(4) . . ? O5 C42 C43 124.6(4) . . ? O5 C42 C41 116.1(4) . . ? C43 C42 C41 119.2(5) . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? O8 C49 C48 124.6(5) . . ? O8 C49 C50 115.0(5) . . ? C48 C49 C50 120.4(4) . . ? C17 C18 C19 119.6(5) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C24 C25 C26 122.5(5) . . ? C24 C25 H25A 118.8 . . ? C26 C25 H25A 118.8 . . ? C42 C43 C44 126.7(4) . . ? C42 C43 H43A 116.6 . . ? C44 C43 H43A 116.6 . . ? C17 C16 C15 121.5(5) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? C11 C12 C13 120.5(5) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C49 C48 C47 124.2(4) . . ? C49 C48 H48A 117.9 . . ? C47 C48 H48A 117.9 . . ? C38 C39 C40 120.8(5) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? C37 C36 C35 120.7(6) . . ? C37 C36 H36A 119.6 . . ? C35 C36 H36A 119.6 . . ? C31 C32 C33 120.3(5) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C28 C29 C30 120.4(5) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C39 C38 C37 121.2(5) . . ? C39 C38 H38A 119.4 . . ? C37 C38 H38A 119.4 . . ? C12 C11 C10 120.2(5) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C36 C37 C38 119.7(5) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C30 C31 C32 120.0(5) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Tb1 Tb2 O4 -3.30(13) . . . . ? O7 Tb1 Tb2 O4 92.0(2) . . . . ? O5 Tb1 Tb2 O4 -136.31(13) . . . . ? O1 Tb1 Tb2 O4 -162.53(15) . . . . ? O2 Tb1 Tb2 O4 27.20(16) . . . . ? O6 Tb1 Tb2 O4 -72.47(12) . . . . ? N1 Tb1 Tb2 O4 143.86(13) . . . . ? N2 Tb1 Tb2 O4 81.56(13) . . . . ? O8 Tb1 Tb2 O3 135.32(12) . . . . ? O7 Tb1 Tb2 O3 -129.4(2) . . . . ? O5 Tb1 Tb2 O3 2.31(11) . . . . ? O1 Tb1 Tb2 O3 -23.91(14) . . . . ? O2 Tb1 Tb2 O3 165.82(14) . . . . ? O6 Tb1 Tb2 O3 66.15(10) . . . . ? N1 Tb1 Tb2 O3 -77.53(11) . . . . ? N2 Tb1 Tb2 O3 -139.82(11) . . . . ? O8 Tb1 Tb2 O2 -30.50(15) . . . . ? O7 Tb1 Tb2 O2 64.8(3) . . . . ? O5 Tb1 Tb2 O2 -163.52(15) . . . . ? O1 Tb1 Tb2 O2 170.26(16) . . . . ? O6 Tb1 Tb2 O2 -99.67(14) . . . . ? N1 Tb1 Tb2 O2 116.65(14) . . . . ? N2 Tb1 Tb2 O2 54.36(14) . . . . ? O8 Tb1 Tb2 O9 61.22(12) . . . . ? O7 Tb1 Tb2 O9 156.5(2) . . . . ? O5 Tb1 Tb2 O9 -71.79(12) . . . . ? O1 Tb1 Tb2 O9 -98.01(14) . . . . ? O2 Tb1 Tb2 O9 91.72(15) . . . . ? O6 Tb1 Tb2 O9 -7.95(11) . . . . ? N1 Tb1 Tb2 O9 -151.63(12) . . . . ? N2 Tb1 Tb2 O9 146.08(11) . . . . ? O8 Tb1 Tb2 O1 159.23(14) . . . . ? O7 Tb1 Tb2 O1 -105.5(3) . . . . ? O5 Tb1 Tb2 O1 26.22(14) . . . . ? O2 Tb1 Tb2 O1 -170.26(16) . . . . ? O6 Tb1 Tb2 O1 90.07(13) . . . . ? N1 Tb1 Tb2 O1 -53.61(14) . . . . ? N2 Tb1 Tb2 O1 -115.90(14) . . . . ? O8 Tb1 Tb2 N3 -147.74(12) . . . . ? O7 Tb1 Tb2 N3 -52.5(2) . . . . ? O5 Tb1 Tb2 N3 79.25(11) . . . . ? O1 Tb1 Tb2 N3 53.03(14) . . . . ? O2 Tb1 Tb2 N3 -117.24(14) . . . . ? O6 Tb1 Tb2 N3 143.09(10) . . . . ? N1 Tb1 Tb2 N3 -0.58(11) . . . . ? N2 Tb1 Tb2 N3 -62.88(11) . . . . ? O8 Tb1 Tb2 N4 -81.55(12) . . . . ? O7 Tb1 Tb2 N4 13.7(2) . . . . ? O5 Tb1 Tb2 N4 145.44(11) . . . . ? O1 Tb1 Tb2 N4 119.22(14) . . . . ? O2 Tb1 Tb2 N4 -51.04(15) . . . . ? O6 Tb1 Tb2 N4 -150.71(11) . . . . ? N1 Tb1 Tb2 N4 65.61(11) . . . . ? N2 Tb1 Tb2 N4 3.32(11) . . . . ? O4 Tb2 O3 C21 -136.9(4) . . . . ? O2 Tb2 O3 C21 92.0(5) . . . . ? O9 Tb2 O3 C21 140.2(4) . . . . ? O1 Tb2 O3 C21 57.6(4) . . . . ? N3 Tb2 O3 C21 -19.4(4) . . . . ? N4 Tb2 O3 C21 -66.0(4) . . . . ? Tb1 Tb2 O3 C21 71.0(4) . . . . ? O4 Tb2 O2 C20 22.3(3) . . . . ? O3 Tb2 O2 C20 151.6(3) . . . . ? O9 Tb2 O2 C20 102.4(3) . . . . ? O1 Tb2 O2 C20 -171.2(3) . . . . ? N3 Tb2 O2 C20 -104.8(3) . . . . ? N4 Tb2 O2 C20 -47.4(3) . . . . ? Tb1 Tb2 O2 C20 -177.1(4) . . . . ? O4 Tb2 O2 Tb1 -160.61(11) . . . . ? O3 Tb2 O2 Tb1 -31.3(3) . . . . ? O9 Tb2 O2 Tb1 -80.45(13) . . . . ? O1 Tb2 O2 Tb1 5.92(10) . . . . ? N3 Tb2 O2 Tb1 72.33(15) . . . . ? N4 Tb2 O2 Tb1 129.69(14) . . . . ? O8 Tb1 O2 C20 -31.9(3) . . . . ? O7 Tb1 O2 C20 21.7(3) . . . . ? O5 Tb1 O2 C20 -154.9(3) . . . . ? O1 Tb1 O2 C20 171.2(3) . . . . ? O6 Tb1 O2 C20 -108.5(3) . . . . ? N1 Tb1 O2 C20 109.2(3) . . . . ? N2 Tb1 O2 C20 57.1(3) . . . . ? Tb2 Tb1 O2 C20 177.2(4) . . . . ? O8 Tb1 O2 Tb2 150.97(14) . . . . ? O7 Tb1 O2 Tb2 -155.47(12) . . . . ? O5 Tb1 O2 Tb2 28.0(2) . . . . ? O1 Tb1 O2 Tb2 -5.98(10) . . . . ? O6 Tb1 O2 Tb2 74.31(12) . . . . ? N1 Tb1 O2 Tb2 -67.91(13) . . . . ? N2 Tb1 O2 Tb2 -120.08(14) . . . . ? O8 Tb1 O1 C1 148.2(3) . . . . ? O7 Tb1 O1 C1 -33.0(4) . . . . ? O5 Tb1 O1 C1 24.6(3) . . . . ? O2 Tb1 O1 C1 -173.5(3) . . . . ? O6 Tb1 O1 C1 98.7(3) . . . . ? N1 Tb1 O1 C1 -57.8(3) . . . . ? N2 Tb1 O1 C1 -111.6(3) . . . . ? Tb2 Tb1 O1 C1 -179.3(3) . . . . ? O8 Tb1 O1 Tb2 -32.5(2) . . . . ? O7 Tb1 O1 Tb2 146.29(16) . . . . ? O5 Tb1 O1 Tb2 -156.08(13) . . . . ? O2 Tb1 O1 Tb2 5.86(10) . . . . ? O6 Tb1 O1 Tb2 -81.92(12) . . . . ? N1 Tb1 O1 Tb2 121.49(14) . . . . ? N2 Tb1 O1 Tb2 67.75(13) . . . . ? O4 Tb2 O1 C1 -126.6(4) . . . . ? O3 Tb2 O1 C1 -20.1(3) . . . . ? O2 Tb2 O1 C1 173.4(3) . . . . ? O9 Tb2 O1 C1 -105.4(3) . . . . ? N3 Tb2 O1 C1 52.8(3) . . . . ? N4 Tb2 O1 C1 106.7(3) . . . . ? Tb1 Tb2 O1 C1 179.3(4) . . . . ? O4 Tb2 O1 Tb1 54.2(4) . . . . ? O3 Tb2 O1 Tb1 160.59(11) . . . . ? O2 Tb2 O1 Tb1 -5.89(10) . . . . ? O9 Tb2 O1 Tb1 75.36(12) . . . . ? N3 Tb2 O1 Tb1 -126.42(13) . . . . ? N4 Tb2 O1 Tb1 -72.55(14) . . . . ? O8 Tb1 O5 C42 -73.9(4) . . . . ? O7 Tb1 O5 C42 -138.5(4) . . . . ? O1 Tb1 O5 C42 70.8(4) . . . . ? O2 Tb1 O5 C42 39.0(5) . . . . ? O6 Tb1 O5 C42 -9.7(4) . . . . ? N1 Tb1 O5 C42 142.4(4) . . . . ? N2 Tb1 O5 C42 172.8(4) . . . . ? Tb2 Tb1 O5 C42 55.9(4) . . . . ? O3 Tb2 O4 C40 141.6(4) . . . . ? O2 Tb2 O4 C40 -55.8(5) . . . . ? O9 Tb2 O4 C40 -133.0(5) . . . . ? O1 Tb2 O4 C40 -111.8(5) . . . . ? N3 Tb2 O4 C40 68.8(5) . . . . ? N4 Tb2 O4 C40 19.7(4) . . . . ? Tb1 Tb2 O4 C40 -71.2(5) . . . . ? O8 Tb1 O6 C44 127.3(4) . . . . ? O7 Tb1 O6 C44 68.2(4) . . . . ? O5 Tb1 O6 C44 3.7(4) . . . . ? O1 Tb1 O6 C44 -81.8(4) . . . . ? O2 Tb1 O6 C44 -151.7(4) . . . . ? N1 Tb1 O6 C44 -44.5(4) . . . . ? N2 Tb1 O6 C44 -179.8(3) . . . . ? Tb2 Tb1 O6 C44 -117.7(4) . . . . ? O7 Tb1 O8 C49 -22.1(5) . . . . ? O5 Tb1 O8 C49 -89.9(5) . . . . ? O1 Tb1 O8 C49 157.2(4) . . . . ? O2 Tb1 O8 C49 121.1(5) . . . . ? O6 Tb1 O8 C49 -152.6(5) . . . . ? N1 Tb1 O8 C49 19.3(5) . . . . ? N2 Tb1 O8 C49 50.8(5) . . . . ? Tb2 Tb1 O8 C49 138.0(4) . . . . ? O4 Tb2 N3 C27 93.7(4) . . . . ? O3 Tb2 N3 C27 10.1(4) . . . . ? O2 Tb2 N3 C27 -146.9(4) . . . . ? O9 Tb2 N3 C27 -36.2(5) . . . . ? O1 Tb2 N3 C27 -86.2(4) . . . . ? N4 Tb2 N3 C27 146.6(4) . . . . ? Tb1 Tb2 N3 C27 -113.8(4) . . . . ? O4 Tb2 N3 C28 -90.9(3) . . . . ? O3 Tb2 N3 C28 -174.4(3) . . . . ? O2 Tb2 N3 C28 28.6(3) . . . . ? O9 Tb2 N3 C28 139.3(3) . . . . ? O1 Tb2 N3 C28 89.3(3) . . . . ? N4 Tb2 N3 C28 -37.9(3) . . . . ? Tb1 Tb2 N3 C28 61.7(3) . . . . ? O8 Tb1 N2 C14 43.7(4) . . . . ? O7 Tb1 N2 C14 117.3(4) . . . . ? O5 Tb1 N2 C14 168.0(3) . . . . ? O1 Tb1 N2 C14 -98.5(4) . . . . ? O2 Tb1 N2 C14 -37.1(3) . . . . ? O6 Tb1 N2 C14 -7.1(5) . . . . ? N1 Tb1 N2 C14 -157.7(4) . . . . ? Tb2 Tb1 N2 C14 -66.3(4) . . . . ? O8 Tb1 N2 C13 -125.4(3) . . . . ? O7 Tb1 N2 C13 -51.8(3) . . . . ? O5 Tb1 N2 C13 -1.1(4) . . . . ? O1 Tb1 N2 C13 92.5(3) . . . . ? O2 Tb1 N2 C13 153.9(3) . . . . ? O6 Tb1 N2 C13 -176.2(2) . . . . ? N1 Tb1 N2 C13 33.2(3) . . . . ? Tb2 Tb1 N2 C13 124.7(3) . . . . ? O8 Tb1 N1 C7 -172.6(3) . . . . ? O7 Tb1 N1 C7 -132.3(4) . . . . ? O5 Tb1 N1 C7 -51.7(4) . . . . ? O1 Tb1 N1 C7 33.6(4) . . . . ? O2 Tb1 N1 C7 94.5(4) . . . . ? O6 Tb1 N1 C7 -5.4(5) . . . . ? N2 Tb1 N1 C7 151.4(4) . . . . ? Tb2 Tb1 N1 C7 63.0(4) . . . . ? O8 Tb1 N1 C8 2.8(4) . . . . ? O7 Tb1 N1 C8 43.1(3) . . . . ? O5 Tb1 N1 C8 123.6(3) . . . . ? O1 Tb1 N1 C8 -151.0(3) . . . . ? O2 Tb1 N1 C8 -90.1(3) . . . . ? O6 Tb1 N1 C8 169.9(3) . . . . ? N2 Tb1 N1 C8 -33.2(3) . . . . ? Tb2 Tb1 N1 C8 -121.6(3) . . . . ? O8 Tb1 O7 C47 23.4(5) . . . . ? O5 Tb1 O7 C47 145.6(5) . . . . ? O1 Tb1 O7 C47 -155.8(4) . . . . ? O2 Tb1 O7 C47 -32.5(5) . . . . ? O6 Tb1 O7 C47 83.9(5) . . . . ? N1 Tb1 O7 C47 -131.9(5) . . . . ? N2 Tb1 O7 C47 -67.3(5) . . . . ? Tb2 Tb1 O7 C47 -78.2(5) . . . . ? Tb1 O1 C1 C2 -123.7(3) . . . . ? Tb2 O1 C1 C2 57.1(5) . . . . ? Tb1 O1 C1 C6 56.9(5) . . . . ? Tb2 O1 C1 C6 -122.3(4) . . . . ? Tb2 O2 C20 C19 -55.2(5) . . . . ? Tb1 O2 C20 C19 128.0(4) . . . . ? Tb2 O2 C20 C15 123.4(4) . . . . ? Tb1 O2 C20 C15 -53.4(5) . . . . ? O4 Tb2 N4 C34 -15.7(4) . . . . ? O3 Tb2 N4 C34 -97.1(4) . . . . ? O2 Tb2 N4 C34 91.3(4) . . . . ? O9 Tb2 N4 C34 34.7(5) . . . . ? O1 Tb2 N4 C34 151.6(4) . . . . ? N3 Tb2 N4 C34 -147.5(4) . . . . ? Tb1 Tb2 N4 C34 117.8(4) . . . . ? O4 Tb2 N4 C33 170.0(3) . . . . ? O3 Tb2 N4 C33 88.6(3) . . . . ? O2 Tb2 N4 C33 -82.9(3) . . . . ? O9 Tb2 N4 C33 -139.6(3) . . . . ? O1 Tb2 N4 C33 -22.7(3) . . . . ? N3 Tb2 N4 C33 38.2(3) . . . . ? Tb1 Tb2 N4 C33 -56.5(3) . . . . ? Tb2 O3 C21 C22 -159.3(3) . . . . ? Tb2 O3 C21 C26 18.9(7) . . . . ? O1 C1 C2 C3 -178.8(4) . . . . ? C6 C1 C2 C3 0.7(7) . . . . ? Tb2 O4 C40 C35 -12.7(7) . . . . ? Tb2 O4 C40 C39 167.8(3) . . . . ? C7 N1 C8 C9 31.8(7) . . . . ? Tb1 N1 C8 C9 -143.8(4) . . . . ? C7 N1 C8 C13 -153.1(5) . . . . ? Tb1 N1 C8 C13 31.2(5) . . . . ? O2 C20 C15 C16 -178.3(4) . . . . ? C19 C20 C15 C16 0.3(6) . . . . ? O2 C20 C15 C14 0.2(7) . . . . ? C19 C20 C15 C14 178.8(4) . . . . ? C13 N2 C14 C15 179.8(4) . . . . ? Tb1 N2 C14 C15 11.4(7) . . . . ? C16 C15 C14 N2 -161.5(5) . . . . ? C20 C15 C14 N2 20.0(7) . . . . ? O3 C21 C26 C25 -179.0(4) . . . . ? C22 C21 C26 C25 -0.8(7) . . . . ? O3 C21 C26 C27 -0.3(7) . . . . ? C22 C21 C26 C27 177.9(5) . . . . ? O1 C1 C6 C5 176.5(4) . . . . ? C2 C1 C6 C5 -2.9(7) . . . . ? O1 C1 C6 C7 -1.9(7) . . . . ? C2 C1 C6 C7 178.6(4) . . . . ? O3 C21 C22 C23 178.2(5) . . . . ? C26 C21 C22 C23 -0.1(7) . . . . ? C28 N3 C27 C26 -177.3(5) . . . . ? Tb2 N3 C27 C26 -2.2(7) . . . . ? C21 C26 C27 N3 -6.4(8) . . . . ? C25 C26 C27 N3 172.4(5) . . . . ? O2 C20 C19 C18 179.4(4) . . . . ? C15 C20 C19 C18 0.8(7) . . . . ? Tb1 O7 C47 C48 -18.1(9) . . . . ? Tb1 O7 C47 C46 163.8(4) . . . . ? C9 C8 C13 C12 -2.1(7) . . . . ? N1 C8 C13 C12 -177.4(5) . . . . ? C9 C8 C13 N2 175.8(4) . . . . ? N1 C8 C13 N2 0.5(6) . . . . ? C14 N2 C13 C12 -23.6(7) . . . . ? Tb1 N2 C13 C12 146.0(4) . . . . ? C14 N2 C13 C8 158.7(4) . . . . ? Tb1 N2 C13 C8 -31.6(5) . . . . ? O4 C40 C35 C36 176.6(4) . . . . ? C39 C40 C35 C36 -3.8(7) . . . . ? O4 C40 C35 C34 -8.3(7) . . . . ? C39 C40 C35 C34 171.3(4) . . . . ? Tb1 O6 C44 C43 -0.7(7) . . . . ? Tb1 O6 C44 C45 176.5(3) . . . . ? C33 N4 C34 C35 -178.3(4) . . . . ? Tb2 N4 C34 C35 7.8(7) . . . . ? C40 C35 C34 N4 8.5(8) . . . . ? C36 C35 C34 N4 -176.3(5) . . . . ? C8 N1 C7 C6 -179.2(4) . . . . ? Tb1 N1 C7 C6 -4.1(7) . . . . ? C1 C6 C7 N1 -25.0(8) . . . . ? C5 C6 C7 N1 156.6(5) . . . . ? C27 N3 C28 C29 34.9(8) . . . . ? Tb2 N3 C28 C29 -141.1(5) . . . . ? C27 N3 C28 C33 -148.6(5) . . . . ? Tb2 N3 C28 C33 35.4(5) . . . . ? C1 C2 C3 C4 1.3(8) . . . . ? C13 C8 C9 C10 1.1(8) . . . . ? N1 C8 C9 C10 176.0(5) . . . . ? C8 C9 C10 C11 -0.4(9) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C29 C28 C33 C32 -2.6(8) . . . . ? N3 C28 C33 C32 -179.3(5) . . . . ? C29 C28 C33 N4 176.7(5) . . . . ? N3 C28 C33 N4 0.0(6) . . . . ? C34 N4 C33 C32 -31.2(7) . . . . ? Tb2 N4 C33 C32 143.8(5) . . . . ? C34 N4 C33 C28 149.6(4) . . . . ? Tb2 N4 C33 C28 -35.5(5) . . . . ? Tb1 O5 C42 C43 12.6(8) . . . . ? Tb1 O5 C42 C41 -165.8(4) . . . . ? C3 C4 C5 C6 -1.6(9) . . . . ? C1 C6 C5 C4 3.5(8) . . . . ? C7 C6 C5 C4 -178.0(5) . . . . ? Tb1 O8 C49 C48 14.8(9) . . . . ? Tb1 O8 C49 C50 -165.0(4) . . . . ? C16 C17 C18 C19 -1.1(8) . . . . ? C20 C19 C18 C17 -0.4(8) . . . . ? C23 C24 C25 C26 -1.2(9) . . . . ? C21 C26 C25 C24 1.5(8) . . . . ? C27 C26 C25 C24 -177.3(5) . . . . ? O5 C42 C43 C44 -5.4(9) . . . . ? C41 C42 C43 C44 173.0(5) . . . . ? O6 C44 C43 C42 -0.3(8) . . . . ? C45 C44 C43 C42 -177.4(5) . . . . ? C18 C17 C16 C15 2.2(8) . . . . ? C20 C15 C16 C17 -1.8(7) . . . . ? C14 C15 C16 C17 179.6(5) . . . . ? C8 C13 C12 C11 2.4(8) . . . . ? N2 C13 C12 C11 -175.2(5) . . . . ? C21 C22 C23 C24 0.4(9) . . . . ? C25 C24 C23 C22 0.3(9) . . . . ? O8 C49 C48 C47 4.7(10) . . . . ? C50 C49 C48 C47 -175.4(6) . . . . ? O7 C47 C48 C49 -2.8(10) . . . . ? C46 C47 C48 C49 175.3(6) . . . . ? O4 C40 C39 C38 -177.1(5) . . . . ? C35 C40 C39 C38 3.3(7) . . . . ? C40 C35 C36 C37 0.8(8) . . . . ? C34 C35 C36 C37 -174.5(5) . . . . ? C28 C33 C32 C31 1.9(9) . . . . ? N4 C33 C32 C31 -177.3(6) . . . . ? C33 C28 C29 C30 0.4(9) . . . . ? N3 C28 C29 C30 176.8(6) . . . . ? C40 C39 C38 C37 0.3(9) . . . . ? C13 C12 C11 C10 -1.8(10) . . . . ? C9 C10 C11 C12 0.8(10) . . . . ? C35 C36 C37 C38 2.8(10) . . . . ? C39 C38 C37 C36 -3.5(10) . . . . ? C33 C32 C31 C30 1.0(11) . . . . ? C32 C31 C30 C29 -3.2(12) . . . . ? C28 C29 C30 C31 2.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.701 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 830603' ####################################################################### # # 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_zt1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H53 Er2 N4 O10' _chemical_formula_weight 1252.52 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0195(15) _cell_length_b 19.6394(18) _cell_length_c 16.2270(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.722(2) _cell_angle_gamma 90.00 _cell_volume 5104.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4324 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 23.79 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_absorpt_coefficient_mu 3.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4901 _exptl_absorpt_correction_T_max 0.5858 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37184 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.35 _reflns_number_total 12704 _reflns_number_gt 7650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT-plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0726P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12704 _refine_ls_number_parameters 634 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.009 _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 Er1 Er -0.092087(19) 0.880895(14) 0.715455(18) 0.03099(10) Uani 1 1 d . . . Er2 Er 0.034321(19) 0.874637(14) 0.917104(17) 0.03033(10) Uani 1 1 d . . . O1 O 0.0293(3) 0.9138(2) 0.7824(3) 0.0323(10) Uani 1 1 d . . . O2 O -0.0836(3) 0.8358(2) 0.8478(3) 0.0336(10) Uani 1 1 d . . . O3 O 0.1313(3) 0.9455(2) 0.9615(3) 0.0423(12) Uani 1 1 d . . . O4 O 0.0044(3) 0.8479(2) 1.0425(3) 0.0471(13) Uani 1 1 d . . . O5 O -0.0553(3) 0.9709(2) 0.6350(3) 0.0445(13) Uani 1 1 d . . . O6 O -0.1411(3) 0.9780(2) 0.7818(3) 0.0417(12) Uani 1 1 d . . . O7 O -0.1483(3) 0.8566(3) 0.5897(3) 0.0495(13) Uani 1 1 d . . . O8 O -0.2268(3) 0.8507(2) 0.7390(3) 0.0464(12) Uani 1 1 d . . . O9 O -0.0541(3) 0.9683(2) 0.9322(3) 0.0460(13) Uani 1 1 d D . . H9 H -0.085(4) 0.971(4) 0.890(3) 0.069 Uiso 1 1 d D . . O10 O 0.3800(15) 1.0058(11) 0.3194(16) 0.299(11) Uani 1 1 d . . . N1 N 0.0308(4) 0.8334(3) 0.6391(3) 0.0359(13) Uani 1 1 d . . . N2 N -0.0810(4) 0.7527(3) 0.7055(3) 0.0351(13) Uani 1 1 d . . . N3 N 0.1648(4) 0.8324(3) 0.8614(3) 0.0367(13) Uani 1 1 d . . . N4 N 0.0540(4) 0.7518(3) 0.9281(4) 0.0411(14) Uani 1 1 d . . . C1 C 0.0904(4) 0.9483(3) 0.7454(4) 0.0331(15) Uani 1 1 d . . . C2 C 0.1186(5) 1.0100(3) 0.7771(4) 0.0423(18) Uani 1 1 d . . . H2A H 0.0930 1.0286 0.8230 0.051 Uiso 1 1 calc R . . C3 C 0.1835(6) 1.0439(4) 0.7415(6) 0.064(3) Uani 1 1 d . . . H3A H 0.2002 1.0857 0.7628 0.077 Uiso 1 1 calc R . . C4 C 0.2239(6) 1.0177(5) 0.6757(6) 0.074(3) Uani 1 1 d . . . H4A H 0.2689 1.0409 0.6533 0.089 Uiso 1 1 calc R . . C5 C 0.1983(6) 0.9570(5) 0.6424(5) 0.063(2) Uani 1 1 d . . . H5A H 0.2265 0.9387 0.5978 0.076 Uiso 1 1 calc R . . C6 C 0.1299(4) 0.9222(4) 0.6752(4) 0.0394(17) Uani 1 1 d . . . C7 C 0.1036(5) 0.8607(4) 0.6335(4) 0.0399(17) Uani 1 1 d . . . H7A H 0.1421 0.8392 0.5999 0.048 Uiso 1 1 calc R . . C8 C 0.0124(5) 0.7721(3) 0.5954(4) 0.0385(16) Uani 1 1 d . . . C9 C 0.0473(5) 0.7540(4) 0.5214(5) 0.053(2) Uani 1 1 d . . . H9A H 0.0862 0.7828 0.4973 0.064 Uiso 1 1 calc R . . C10 C 0.0255(6) 0.6938(5) 0.4822(6) 0.067(3) Uani 1 1 d . . . H10A H 0.0508 0.6813 0.4332 0.080 Uiso 1 1 calc R . . C11 C -0.0336(6) 0.6530(5) 0.5167(6) 0.070(3) Uani 1 1 d . . . H11A H -0.0497 0.6129 0.4903 0.084 Uiso 1 1 calc R . . C12 C -0.0697(6) 0.6708(4) 0.5904(5) 0.064(3) Uani 1 1 d . . . H12A H -0.1101 0.6427 0.6133 0.076 Uiso 1 1 calc R . . C13 C -0.0463(5) 0.7300(3) 0.6304(4) 0.0378(16) Uani 1 1 d . . . C14 C -0.1091(5) 0.7081(4) 0.7572(5) 0.0468(19) Uani 1 1 d . . . H14A H -0.1056 0.6624 0.7428 0.056 Uiso 1 1 calc R . . C15 C -0.1454(5) 0.7250(3) 0.8356(5) 0.0394(17) Uani 1 1 d . . . C16 C -0.1933(5) 0.6735(4) 0.8713(5) 0.052(2) Uani 1 1 d . . . H16A H -0.1983 0.6318 0.8446 0.063 Uiso 1 1 calc R . . C17 C -0.2336(6) 0.6833(4) 0.9458(6) 0.069(3) Uani 1 1 d . . . H17A H -0.2672 0.6495 0.9679 0.083 Uiso 1 1 calc R . . C18 C -0.2223(5) 0.7444(4) 0.9856(5) 0.056(2) Uani 1 1 d . . . H18A H -0.2479 0.7514 1.0360 0.067 Uiso 1 1 calc R . . C19 C -0.1737(5) 0.7956(4) 0.9527(5) 0.0445(18) Uani 1 1 d . . . H19A H -0.1673 0.8365 0.9811 0.053 Uiso 1 1 calc R . . C20 C -0.1343(4) 0.7864(3) 0.8772(4) 0.0343(15) Uani 1 1 d . . . C21 C 0.2081(5) 0.9641(3) 0.9459(4) 0.0389(16) Uani 1 1 d . . . C22 C 0.2425(6) 1.0236(4) 0.9804(5) 0.059(2) Uani 1 1 d . . . H22A H 0.2110 1.0492 1.0169 0.071 Uiso 1 1 calc R . . C23 C 0.3215(6) 1.0446(5) 0.9615(6) 0.067(3) Uani 1 1 d . . . H23A H 0.3416 1.0851 0.9839 0.081 Uiso 1 1 calc R . . C24 C 0.3716(6) 1.0079(5) 0.9105(6) 0.066(3) Uani 1 1 d . . . H24A H 0.4249 1.0234 0.8984 0.080 Uiso 1 1 calc R . . C25 C 0.3429(5) 0.9484(4) 0.8777(5) 0.056(2) Uani 1 1 d . . . H25A H 0.3773 0.9230 0.8437 0.067 Uiso 1 1 calc R . . C26 C 0.2617(4) 0.9246(4) 0.8944(4) 0.0418(17) Uani 1 1 d . . . C27 C 0.2361(5) 0.8610(4) 0.8563(5) 0.0463(18) Uani 1 1 d . . . H27A H 0.2758 0.8387 0.8248 0.056 Uiso 1 1 calc R . . C28 C 0.1523(5) 0.7685(3) 0.8214(4) 0.0404(17) Uani 1 1 d . . . C29 C 0.1916(5) 0.7491(4) 0.7489(5) 0.056(2) Uani 1 1 d . . . H29A H 0.2297 0.7781 0.7241 0.067 Uiso 1 1 calc R . . C30 C 0.1733(6) 0.6861(5) 0.7140(6) 0.065(3) Uani 1 1 d . . . H30A H 0.1996 0.6726 0.6659 0.077 Uiso 1 1 calc R . . C31 C 0.1168(7) 0.6439(5) 0.7505(6) 0.070(3) Uani 1 1 d . . . H31A H 0.1061 0.6014 0.7273 0.084 Uiso 1 1 calc R . . C32 C 0.0751(5) 0.6629(4) 0.8210(5) 0.055(2) Uani 1 1 d . . . H32A H 0.0355 0.6344 0.8444 0.066 Uiso 1 1 calc R . . C33 C 0.0940(5) 0.7264(4) 0.8563(5) 0.0440(18) Uani 1 1 d . . . C34 C 0.0288(5) 0.7104(4) 0.9850(5) 0.051(2) Uani 1 1 d . . . H34A H 0.0371 0.6642 0.9756 0.061 Uiso 1 1 calc R . . C35 C -0.0103(5) 0.7285(4) 1.0604(5) 0.052(2) Uani 1 1 d . . . C36 C -0.0379(6) 0.6759(5) 1.1112(7) 0.074(3) Uani 1 1 d . . . H36A H -0.0316 0.6311 1.0938 0.088 Uiso 1 1 calc R . . C37 C -0.0739(7) 0.6880(6) 1.1855(7) 0.084(3) Uani 1 1 d . . . H37A H -0.0943 0.6522 1.2168 0.101 Uiso 1 1 calc R . . C38 C -0.0796(6) 0.7538(5) 1.2134(6) 0.072(3) Uani 1 1 d . . . H38A H -0.1032 0.7624 1.2644 0.086 Uiso 1 1 calc R . . C39 C -0.0513(5) 0.8068(5) 1.1674(5) 0.057(2) Uani 1 1 d . . . H39A H -0.0537 0.8507 1.1887 0.069 Uiso 1 1 calc R . . C40 C -0.0182(5) 0.7966(4) 1.0878(4) 0.0425(17) Uani 1 1 d . . . C41 C -0.0108(7) 1.0729(5) 0.5745(6) 0.089(4) Uani 1 1 d . . . H41A H 0.0177 1.0413 0.5396 0.134 Uiso 1 1 calc R . . H41B H 0.0292 1.1022 0.6011 0.134 Uiso 1 1 calc R . . H41C H -0.0488 1.0998 0.5418 0.134 Uiso 1 1 calc R . . C42 C -0.0586(6) 1.0346(4) 0.6385(5) 0.051(2) Uani 1 1 d . . . C43 C -0.1043(6) 1.0700(4) 0.6973(5) 0.056(2) Uani 1 1 d . . . H43A H -0.1099 1.1167 0.6898 0.068 Uiso 1 1 calc R . . C44 C -0.1416(5) 1.0422(4) 0.7649(5) 0.0448(19) Uani 1 1 d . . . C45 C -0.1840(6) 1.0862(4) 0.8280(5) 0.068(3) Uani 1 1 d . . . H45A H -0.2062 1.0579 0.8708 0.102 Uiso 1 1 calc R . . H45B H -0.2286 1.1111 0.8020 0.102 Uiso 1 1 calc R . . H45C H -0.1442 1.1174 0.8515 0.102 Uiso 1 1 calc R . . C46 C -0.2086(7) 0.8004(6) 0.4759(5) 0.089(4) Uani 1 1 d . . . H46A H -0.1616 0.8212 0.4498 0.133 Uiso 1 1 calc R . . H46B H -0.2593 0.8164 0.4504 0.133 Uiso 1 1 calc R . . H46C H -0.2051 0.7518 0.4700 0.133 Uiso 1 1 calc R . . C47 C -0.2082(6) 0.8186(4) 0.5659(6) 0.061(2) Uani 1 1 d . . . C48 C -0.2693(6) 0.7944(4) 0.6171(6) 0.067(3) Uani 1 1 d . . . H48A H -0.3081 0.7641 0.5950 0.080 Uiso 1 1 calc R . . C49 C -0.2771(5) 0.8124(4) 0.7006(6) 0.056(2) Uani 1 1 d . . . C50 C -0.3497(6) 0.7855(5) 0.7496(7) 0.082(3) Uani 1 1 d . . . H50A H -0.3458 0.8021 0.8051 0.123 Uiso 1 1 calc R . . H50B H -0.3483 0.7367 0.7499 0.123 Uiso 1 1 calc R . . H50C H -0.4012 0.8007 0.7248 0.123 Uiso 1 1 calc R . . C51 C 0.3968(13) 1.0277(10) 0.1811(15) 0.249(14) Uani 1 1 d D . . H51A H 0.4353 1.0321 0.1365 0.373 Uiso 1 1 calc R . . H51B H 0.3665 1.0695 0.1873 0.373 Uiso 1 1 calc R . . H51C H 0.3584 0.9914 0.1693 0.373 Uiso 1 1 calc R . . C52 C 0.443(2) 1.0126(11) 0.2579(12) 0.27(2) Uani 1 1 d D . . H52A H 0.4749 0.9708 0.2527 0.319 Uiso 1 1 calc R . . H52B H 0.4813 1.0494 0.2718 0.319 Uiso 1 1 calc R . . C53 C 0.4001(18) 1.0025(10) 0.3985(15) 0.36(3) Uani 1 1 d D . . H53A H 0.4446 1.0352 0.4079 0.436 Uiso 1 1 calc R . . H53B H 0.4240 0.9577 0.4080 0.436 Uiso 1 1 calc R . . C54 C 0.3392(13) 1.0135(8) 0.4624(11) 0.204(11) Uani 1 1 d D . . H54A H 0.3652 1.0068 0.5154 0.305 Uiso 1 1 calc R . . H54B H 0.2940 0.9818 0.4555 0.305 Uiso 1 1 calc R . . H54C H 0.3181 1.0591 0.4586 0.305 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.03346(18) 0.02463(16) 0.03482(17) -0.00331(12) -0.00209(13) 0.00022(12) Er2 0.03327(18) 0.02558(16) 0.03215(17) -0.00292(12) 0.00047(12) -0.00008(12) O1 0.037(3) 0.026(2) 0.034(2) -0.0003(19) 0.004(2) -0.006(2) O2 0.036(3) 0.027(2) 0.038(3) 0.0001(19) 0.004(2) -0.0067(19) O3 0.039(3) 0.037(3) 0.051(3) -0.010(2) 0.004(2) -0.006(2) O4 0.065(4) 0.032(3) 0.044(3) -0.001(2) 0.010(3) -0.004(2) O5 0.064(4) 0.025(2) 0.044(3) 0.002(2) -0.001(3) 0.004(2) O6 0.053(3) 0.027(2) 0.046(3) -0.004(2) 0.003(2) 0.006(2) O7 0.051(3) 0.048(3) 0.049(3) -0.006(3) -0.013(3) 0.009(3) O8 0.035(3) 0.037(3) 0.067(3) -0.008(3) -0.002(2) -0.005(2) O9 0.053(4) 0.036(3) 0.049(3) -0.009(2) -0.004(2) 0.012(2) O10 0.35(3) 0.28(2) 0.26(2) -0.04(2) 0.05(2) -0.146(19) N1 0.039(4) 0.034(3) 0.035(3) -0.004(2) -0.001(3) 0.001(3) N2 0.041(4) 0.024(3) 0.040(3) -0.005(2) 0.001(3) -0.001(2) N3 0.038(4) 0.034(3) 0.038(3) 0.002(3) -0.004(3) 0.009(3) N4 0.041(4) 0.029(3) 0.053(4) 0.000(3) -0.001(3) 0.002(3) C1 0.034(4) 0.026(3) 0.039(4) 0.003(3) -0.005(3) -0.001(3) C2 0.058(5) 0.028(4) 0.041(4) -0.001(3) 0.003(4) -0.008(3) C3 0.074(7) 0.053(5) 0.066(6) -0.001(4) 0.004(5) -0.033(5) C4 0.066(7) 0.074(7) 0.083(7) 0.000(6) 0.027(5) -0.034(5) C5 0.060(6) 0.074(6) 0.056(5) -0.001(5) 0.020(4) -0.013(5) C6 0.039(4) 0.036(4) 0.044(4) 0.006(3) 0.002(3) -0.002(3) C7 0.040(4) 0.044(4) 0.036(4) 0.000(3) 0.016(3) -0.004(3) C8 0.044(4) 0.029(3) 0.043(4) -0.003(3) -0.008(3) 0.007(3) C9 0.064(6) 0.048(5) 0.048(5) -0.010(4) 0.003(4) 0.009(4) C10 0.071(7) 0.069(6) 0.061(6) -0.035(5) 0.004(5) 0.005(5) C11 0.080(7) 0.052(5) 0.079(7) -0.034(5) -0.004(5) 0.004(5) C12 0.089(7) 0.034(4) 0.068(6) -0.018(4) -0.005(5) -0.015(4) C13 0.046(4) 0.030(3) 0.038(4) -0.005(3) -0.002(3) 0.002(3) C14 0.052(5) 0.028(4) 0.061(5) -0.003(4) 0.001(4) -0.002(3) C15 0.042(4) 0.022(3) 0.054(5) 0.000(3) 0.000(3) -0.007(3) C16 0.061(6) 0.025(4) 0.071(6) 0.004(4) 0.005(4) -0.009(4) C17 0.084(7) 0.046(5) 0.078(6) 0.002(5) 0.026(5) -0.026(5) C18 0.049(5) 0.063(6) 0.057(5) 0.006(4) 0.017(4) -0.014(4) C19 0.039(4) 0.045(4) 0.050(5) -0.002(4) 0.007(3) -0.005(3) C20 0.030(4) 0.031(3) 0.042(4) 0.011(3) -0.004(3) -0.004(3) C21 0.043(4) 0.035(4) 0.039(4) 0.004(3) -0.004(3) -0.007(3) C22 0.063(6) 0.045(5) 0.070(6) -0.012(4) 0.001(5) -0.014(4) C23 0.062(6) 0.048(5) 0.093(7) 0.006(5) 0.004(5) -0.027(5) C24 0.042(5) 0.068(6) 0.089(7) 0.025(5) 0.007(5) -0.015(5) C25 0.050(5) 0.047(5) 0.071(6) 0.014(4) 0.012(4) -0.008(4) C26 0.035(4) 0.045(4) 0.046(4) 0.005(3) 0.008(3) 0.003(3) C27 0.036(4) 0.049(4) 0.054(5) 0.006(4) 0.006(4) 0.012(4) C28 0.047(5) 0.032(4) 0.042(4) -0.002(3) -0.005(3) 0.015(3) C29 0.063(6) 0.059(5) 0.046(5) 0.000(4) 0.003(4) 0.036(4) C30 0.080(7) 0.053(5) 0.060(6) -0.012(5) -0.006(5) 0.030(5) C31 0.083(7) 0.051(5) 0.074(6) -0.032(5) -0.021(5) 0.026(5) C32 0.055(5) 0.030(4) 0.080(6) -0.007(4) -0.014(5) 0.014(4) C33 0.049(5) 0.035(4) 0.048(4) -0.008(3) -0.005(4) 0.015(3) C34 0.055(5) 0.029(4) 0.069(6) 0.010(4) -0.002(4) -0.003(3) C35 0.048(5) 0.046(5) 0.061(5) 0.015(4) 0.006(4) 0.000(4) C36 0.064(7) 0.050(5) 0.106(8) 0.022(5) 0.024(6) 0.003(5) C37 0.088(8) 0.079(8) 0.086(8) 0.036(6) 0.031(6) -0.001(6) C38 0.070(7) 0.074(7) 0.072(6) 0.025(5) 0.030(5) 0.005(5) C39 0.057(6) 0.063(6) 0.051(5) 0.010(4) 0.008(4) 0.012(4) C40 0.036(4) 0.050(5) 0.041(4) 0.007(3) 0.002(3) -0.004(3) C41 0.157(11) 0.042(5) 0.069(6) 0.020(5) 0.038(7) -0.004(6) C42 0.071(6) 0.034(4) 0.048(5) 0.009(3) 0.002(4) 0.002(4) C43 0.085(7) 0.025(4) 0.060(5) 0.005(4) 0.010(5) 0.006(4) C44 0.055(5) 0.029(4) 0.050(5) -0.004(3) -0.011(4) 0.009(3) C45 0.104(8) 0.032(4) 0.069(6) -0.007(4) 0.012(5) 0.021(5) C46 0.092(9) 0.110(9) 0.063(6) -0.028(6) -0.028(6) -0.004(7) C47 0.064(6) 0.050(5) 0.067(6) -0.017(4) -0.026(5) 0.001(4) C48 0.060(6) 0.041(5) 0.098(8) -0.013(5) -0.030(6) -0.006(4) C49 0.044(5) 0.039(4) 0.086(7) 0.004(4) -0.019(5) 0.003(4) C50 0.048(6) 0.064(6) 0.134(10) 0.014(6) 0.005(6) -0.023(5) C51 0.22(3) 0.18(2) 0.35(4) -0.16(2) 0.08(2) -0.071(18) C52 0.55(6) 0.144(18) 0.104(15) 0.007(14) 0.01(2) -0.13(3) C53 0.78(8) 0.130(19) 0.18(3) -0.05(2) 0.12(4) -0.23(3) C54 0.34(3) 0.120(14) 0.156(16) 0.014(12) 0.130(18) -0.031(16) _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 Er1 O7 2.271(5) . ? Er1 O8 2.275(5) . ? Er1 O5 2.279(5) . ? Er1 O1 2.307(4) . ? Er1 O2 2.326(4) . ? Er1 O6 2.332(4) . ? Er1 N1 2.519(6) . ? Er1 N2 2.528(5) . ? Er1 Er2 3.8283(5) . ? Er2 O4 2.161(5) . ? Er2 O3 2.199(5) . ? Er2 O2 2.315(4) . ? Er2 O1 2.317(4) . ? Er2 O9 2.336(5) . ? Er2 N3 2.433(6) . ? Er2 N4 2.440(6) . ? O1 C1 1.340(8) . ? O2 C20 1.355(7) . ? O3 C21 1.311(8) . ? O4 C40 1.302(8) . ? O5 C42 1.254(8) . ? O6 C44 1.289(8) . ? O7 C47 1.271(9) . ? O8 C49 1.261(9) . ? O9 H9 0.845(10) . ? O10 C53 1.32(3) . ? O10 C52 1.44(3) . ? N1 C7 1.287(8) . ? N1 C8 1.427(8) . ? N2 C14 1.297(9) . ? N2 C13 1.420(8) . ? N3 C27 1.277(9) . ? N3 C28 1.426(8) . ? N4 C34 1.298(9) . ? N4 C33 1.426(9) . ? C1 C2 1.390(9) . ? C1 C6 1.408(9) . ? C2 C3 1.367(11) . ? C2 H2A 0.9300 . ? C3 C4 1.357(12) . ? C3 H3A 0.9300 . ? C4 C5 1.370(12) . ? C4 H4A 0.9300 . ? C5 C6 1.401(10) . ? C5 H5A 0.9300 . ? C6 C7 1.444(10) . ? C7 H7A 0.9300 . ? C8 C9 1.377(10) . ? C8 C13 1.379(10) . ? C9 C10 1.387(11) . ? C9 H9A 0.9300 . ? C10 C11 1.366(13) . ? C10 H10A 0.9300 . ? C11 C12 1.380(12) . ? C11 H11A 0.9300 . ? C12 C13 1.381(10) . ? C12 H12A 0.9300 . ? C14 C15 1.446(10) . ? C14 H14A 0.9300 . ? C15 C20 1.393(9) . ? C15 C16 1.399(9) . ? C16 C17 1.390(11) . ? C16 H16A 0.9300 . ? C17 C18 1.373(12) . ? C17 H17A 0.9300 . ? C18 C19 1.384(10) . ? C18 H18A 0.9300 . ? C19 C20 1.398(10) . ? C19 H19A 0.9300 . ? C21 C22 1.407(10) . ? C21 C26 1.433(10) . ? C22 C23 1.371(12) . ? C22 H22A 0.9300 . ? C23 C24 1.365(13) . ? C23 H23A 0.9300 . ? C24 C25 1.363(12) . ? C24 H24A 0.9300 . ? C25 C26 1.411(10) . ? C25 H25A 0.9300 . ? C26 C27 1.452(10) . ? C27 H27A 0.9300 . ? C28 C33 1.375(11) . ? C28 C29 1.394(10) . ? C29 C30 1.391(12) . ? C29 H29A 0.9300 . ? C30 C31 1.368(14) . ? C30 H30A 0.9300 . ? C31 C32 1.385(13) . ? C31 H31A 0.9300 . ? C32 C33 1.403(10) . ? C32 H32A 0.9300 . ? C34 C35 1.427(11) . ? C34 H34A 0.9300 . ? C35 C36 1.398(11) . ? C35 C40 1.416(11) . ? C36 C37 1.363(13) . ? C36 H36A 0.9300 . ? C37 C38 1.373(14) . ? C37 H37A 0.9300 . ? C38 C39 1.362(12) . ? C38 H38A 0.9300 . ? C39 C40 1.416(10) . ? C39 H39A 0.9300 . ? C41 C42 1.501(11) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.395(11) . ? C43 C44 1.370(10) . ? C43 H43A 0.9300 . ? C44 C45 1.508(10) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.504(11) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.377(13) . ? C48 C49 1.407(12) . ? C48 H48A 0.9300 . ? C49 C50 1.513(12) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 C52 1.474(18) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.449(17) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Er1 O8 74.35(19) . . ? O7 Er1 O5 75.57(18) . . ? O8 Er1 O5 123.47(19) . . ? O7 Er1 O1 143.52(18) . . ? O8 Er1 O1 142.10(17) . . ? O5 Er1 O1 80.23(17) . . ? O7 Er1 O2 140.16(17) . . ? O8 Er1 O2 77.89(17) . . ? O5 Er1 O2 144.26(16) . . ? O1 Er1 O2 68.42(15) . . ? O7 Er1 O6 117.08(17) . . ? O8 Er1 O6 79.07(18) . . ? O5 Er1 O6 73.81(17) . . ? O1 Er1 O6 80.80(16) . . ? O2 Er1 O6 84.34(16) . . ? O7 Er1 N1 77.51(18) . . ? O8 Er1 N1 137.33(18) . . ? O5 Er1 N1 78.22(18) . . ? O1 Er1 N1 71.08(16) . . ? O2 Er1 N1 106.01(17) . . ? O6 Er1 N1 143.12(18) . . ? O7 Er1 N2 76.16(18) . . ? O8 Er1 N2 79.54(18) . . ? O5 Er1 N2 135.77(17) . . ? O1 Er1 N2 104.42(16) . . ? O2 Er1 N2 71.11(16) . . ? O6 Er1 N2 150.25(18) . . ? N1 Er1 N2 62.88(18) . . ? O7 Er1 Er2 163.90(13) . . ? O8 Er1 Er2 109.91(13) . . ? O5 Er1 Er2 112.12(13) . . ? O1 Er1 Er2 34.21(10) . . ? O2 Er1 Er2 34.32(11) . . ? O6 Er1 Er2 78.99(12) . . ? N1 Er1 Er2 90.00(12) . . ? N2 Er1 Er2 89.18(12) . . ? O4 Er2 O3 90.52(19) . . ? O4 Er2 O2 100.84(18) . . ? O3 Er2 O2 159.37(17) . . ? O4 Er2 O1 164.39(18) . . ? O3 Er2 O1 96.63(16) . . ? O2 Er2 O1 68.45(15) . . ? O4 Er2 O9 87.16(19) . . ? O3 Er2 O9 83.96(18) . . ? O2 Er2 O9 79.52(17) . . ? O1 Er2 O9 79.85(17) . . ? O4 Er2 N3 117.97(19) . . ? O3 Er2 N3 74.41(18) . . ? O2 Er2 N3 113.96(17) . . ? O1 Er2 N3 77.43(16) . . ? O9 Er2 N3 146.33(19) . . ? O4 Er2 N4 73.79(19) . . ? O3 Er2 N4 120.76(19) . . ? O2 Er2 N4 79.24(18) . . ? O1 Er2 N4 113.58(17) . . ? O9 Er2 N4 148.1(2) . . ? N3 Er2 N4 65.1(2) . . ? O4 Er2 Er1 133.74(14) . . ? O3 Er2 Er1 128.57(13) . . ? O2 Er2 Er1 34.51(11) . . ? O1 Er2 Er1 34.04(11) . . ? O9 Er2 Er1 75.48(12) . . ? N3 Er2 Er1 98.08(13) . . ? N4 Er2 Er1 99.25(14) . . ? C1 O1 Er1 123.1(4) . . ? C1 O1 Er2 125.0(4) . . ? Er1 O1 Er2 111.75(17) . . ? C20 O2 Er2 123.6(4) . . ? C20 O2 Er1 124.6(4) . . ? Er2 O2 Er1 111.16(17) . . ? C21 O3 Er2 140.6(4) . . ? C40 O4 Er2 141.8(5) . . ? C42 O5 Er1 137.4(5) . . ? C44 O6 Er1 134.6(5) . . ? C47 O7 Er1 133.2(6) . . ? C49 O8 Er1 132.4(6) . . ? Er2 O9 H9 108(6) . . ? C53 O10 C52 121(3) . . ? C7 N1 C8 119.9(6) . . ? C7 N1 Er1 126.5(5) . . ? C8 N1 Er1 113.5(4) . . ? C14 N2 C13 119.0(6) . . ? C14 N2 Er1 127.3(5) . . ? C13 N2 Er1 113.4(4) . . ? C27 N3 C28 118.5(6) . . ? C27 N3 Er2 130.4(5) . . ? C28 N3 Er2 110.7(4) . . ? C34 N4 C33 120.5(6) . . ? C34 N4 Er2 129.1(5) . . ? C33 N4 Er2 110.2(4) . . ? O1 C1 C2 120.8(6) . . ? O1 C1 C6 121.1(6) . . ? C2 C1 C6 118.0(7) . . ? C3 C2 C1 120.9(7) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C4 C3 C2 121.4(8) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 119.8(8) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 120.5(8) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 119.4(7) . . ? C5 C6 C7 117.1(7) . . ? C1 C6 C7 123.5(6) . . ? N1 C7 C6 125.1(7) . . ? N1 C7 H7A 117.5 . . ? C6 C7 H7A 117.5 . . ? C9 C8 C13 119.4(7) . . ? C9 C8 N1 124.5(7) . . ? C13 C8 N1 116.1(6) . . ? C8 C9 C10 121.1(8) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.5 . . ? C11 C10 C9 119.0(8) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 120.4(8) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C11 C12 C13 120.4(9) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C8 C13 C12 119.6(7) . . ? C8 C13 N2 116.2(6) . . ? C12 C13 N2 124.2(7) . . ? N2 C14 C15 124.1(7) . . ? N2 C14 H14A 117.9 . . ? C15 C14 H14A 117.9 . . ? C20 C15 C16 119.6(7) . . ? C20 C15 C14 125.1(6) . . ? C16 C15 C14 115.3(6) . . ? C17 C16 C15 121.5(7) . . ? C17 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? C18 C17 C16 118.1(8) . . ? C18 C17 H17A 120.9 . . ? C16 C17 H17A 120.9 . . ? C17 C18 C19 121.6(8) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C18 C19 C20 120.5(7) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? O2 C20 C15 121.6(6) . . ? O2 C20 C19 119.7(6) . . ? C15 C20 C19 118.7(6) . . ? O3 C21 C22 121.2(7) . . ? O3 C21 C26 122.2(6) . . ? C22 C21 C26 116.5(7) . . ? C23 C22 C21 121.3(9) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C24 C23 C22 121.9(8) . . ? C24 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C25 C24 C23 119.5(8) . . ? C25 C24 H24A 120.3 . . ? C23 C24 H24A 120.3 . . ? C24 C25 C26 121.1(9) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C21 119.6(7) . . ? C25 C26 C27 117.3(7) . . ? C21 C26 C27 123.0(7) . . ? N3 C27 C26 126.8(7) . . ? N3 C27 H27A 116.6 . . ? C26 C27 H27A 116.6 . . ? C33 C28 C29 120.0(7) . . ? C33 C28 N3 115.7(6) . . ? C29 C28 N3 124.2(7) . . ? C30 C29 C28 119.4(9) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C31 C30 C29 120.0(9) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 121.5(8) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C31 C32 C33 118.3(9) . . ? C31 C32 H32A 120.9 . . ? C33 C32 H32A 120.9 . . ? C28 C33 C32 120.7(7) . . ? C28 C33 N4 116.2(6) . . ? C32 C33 N4 123.2(8) . . ? N4 C34 C35 126.7(7) . . ? N4 C34 H34A 116.7 . . ? C35 C34 H34A 116.7 . . ? C36 C35 C40 118.9(8) . . ? C36 C35 C34 117.9(8) . . ? C40 C35 C34 123.2(7) . . ? C37 C36 C35 122.2(10) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C36 C37 C38 119.1(9) . . ? C36 C37 H37A 120.5 . . ? C38 C37 H37A 120.5 . . ? C39 C38 C37 121.0(9) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C38 C39 C40 121.5(9) . . ? C38 C39 H39A 119.3 . . ? C40 C39 H39A 119.3 . . ? O4 C40 C35 121.8(7) . . ? O4 C40 C39 121.0(7) . . ? C35 C40 C39 117.2(7) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O5 C42 C43 123.5(7) . . ? O5 C42 C41 116.6(7) . . ? C43 C42 C41 120.0(7) . . ? C44 C43 C42 125.9(7) . . ? C44 C43 H43A 117.0 . . ? C42 C43 H43A 117.0 . . ? O6 C44 C43 123.9(7) . . ? O6 C44 C45 114.6(7) . . ? C43 C44 C45 121.4(7) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O7 C47 C48 124.0(8) . . ? O7 C47 C46 115.4(9) . . ? C48 C47 C46 120.6(8) . . ? C47 C48 C49 124.5(8) . . ? C47 C48 H48A 117.8 . . ? C49 C48 H48A 117.8 . . ? O8 C49 C48 124.2(8) . . ? O8 C49 C50 116.0(9) . . ? C48 C49 C50 119.8(8) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O10 C52 C51 105(3) . . ? O10 C52 H52A 110.8 . . ? C51 C52 H52A 110.8 . . ? O10 C52 H52B 110.8 . . ? C51 C52 H52B 110.8 . . ? H52A C52 H52B 108.9 . . ? O10 C53 C54 122(3) . . ? O10 C53 H53A 106.8 . . ? C54 C53 H53A 106.8 . . ? O10 C53 H53B 106.8 . . ? C54 C53 H53B 106.8 . . ? H53A C53 H53B 106.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Er1 Er2 O4 -101.8(6) . . . . ? O8 Er1 Er2 O4 1.0(2) . . . . ? O5 Er1 Er2 O4 142.3(2) . . . . ? O1 Er1 Er2 O4 164.7(3) . . . . ? O2 Er1 Er2 O4 -21.2(3) . . . . ? O6 Er1 Er2 O4 75.0(2) . . . . ? N1 Er1 Er2 O4 -140.5(2) . . . . ? N2 Er1 Er2 O4 -77.6(2) . . . . ? O7 Er1 Er2 O3 117.1(5) . . . . ? O8 Er1 Er2 O3 -140.2(2) . . . . ? O5 Er1 Er2 O3 1.1(2) . . . . ? O1 Er1 Er2 O3 23.6(2) . . . . ? O2 Er1 Er2 O3 -162.4(3) . . . . ? O6 Er1 Er2 O3 -66.2(2) . . . . ? N1 Er1 Er2 O3 78.3(2) . . . . ? N2 Er1 Er2 O3 141.2(2) . . . . ? O7 Er1 Er2 O2 -80.6(6) . . . . ? O8 Er1 Er2 O2 22.1(2) . . . . ? O5 Er1 Er2 O2 163.4(2) . . . . ? O1 Er1 Er2 O2 -174.1(3) . . . . ? O6 Er1 Er2 O2 96.1(2) . . . . ? N1 Er1 Er2 O2 -119.3(2) . . . . ? N2 Er1 Er2 O2 -56.4(2) . . . . ? O7 Er1 Er2 O1 93.5(6) . . . . ? O8 Er1 Er2 O1 -163.8(2) . . . . ? O5 Er1 Er2 O1 -22.5(2) . . . . ? O2 Er1 Er2 O1 174.1(3) . . . . ? O6 Er1 Er2 O1 -89.8(2) . . . . ? N1 Er1 Er2 O1 54.8(2) . . . . ? N2 Er1 Er2 O1 117.7(2) . . . . ? O7 Er1 Er2 O9 -173.2(5) . . . . ? O8 Er1 Er2 O9 -70.4(2) . . . . ? O5 Er1 Er2 O9 70.9(2) . . . . ? O1 Er1 Er2 O9 93.3(2) . . . . ? O2 Er1 Er2 O9 -92.6(2) . . . . ? O6 Er1 Er2 O9 3.54(19) . . . . ? N1 Er1 Er2 O9 148.12(19) . . . . ? N2 Er1 Er2 O9 -149.00(19) . . . . ? O7 Er1 Er2 N3 40.6(5) . . . . ? O8 Er1 Er2 N3 143.3(2) . . . . ? O5 Er1 Er2 N3 -75.40(19) . . . . ? O1 Er1 Er2 N3 -52.9(2) . . . . ? O2 Er1 Er2 N3 121.2(2) . . . . ? O6 Er1 Er2 N3 -142.71(18) . . . . ? N1 Er1 Er2 N3 1.87(18) . . . . ? N2 Er1 Er2 N3 64.75(19) . . . . ? O7 Er1 Er2 N4 -25.4(5) . . . . ? O8 Er1 Er2 N4 77.3(2) . . . . ? O5 Er1 Er2 N4 -141.4(2) . . . . ? O1 Er1 Er2 N4 -118.9(2) . . . . ? O2 Er1 Er2 N4 55.2(2) . . . . ? O6 Er1 Er2 N4 151.33(19) . . . . ? N1 Er1 Er2 N4 -64.09(19) . . . . ? N2 Er1 Er2 N4 -1.21(19) . . . . ? O7 Er1 O1 C1 24.6(6) . . . . ? O8 Er1 O1 C1 -157.8(4) . . . . ? O5 Er1 O1 C1 -24.2(5) . . . . ? O2 Er1 O1 C1 173.3(5) . . . . ? O6 Er1 O1 C1 -99.2(5) . . . . ? N1 Er1 O1 C1 56.6(5) . . . . ? N2 Er1 O1 C1 110.8(5) . . . . ? Er2 Er1 O1 C1 176.9(6) . . . . ? O7 Er1 O1 Er2 -152.2(2) . . . . ? O8 Er1 O1 Er2 25.3(3) . . . . ? O5 Er1 O1 Er2 158.9(2) . . . . ? O2 Er1 O1 Er2 -3.59(16) . . . . ? O6 Er1 O1 Er2 83.9(2) . . . . ? N1 Er1 O1 Er2 -120.3(2) . . . . ? N2 Er1 O1 Er2 -66.1(2) . . . . ? O4 Er2 O1 C1 138.3(6) . . . . ? O3 Er2 O1 C1 21.5(5) . . . . ? O2 Er2 O1 C1 -173.2(5) . . . . ? O9 Er2 O1 C1 104.1(5) . . . . ? N3 Er2 O1 C1 -50.8(5) . . . . ? N4 Er2 O1 C1 -106.2(5) . . . . ? Er1 Er2 O1 C1 -176.8(6) . . . . ? O4 Er2 O1 Er1 -44.9(7) . . . . ? O3 Er2 O1 Er1 -161.66(19) . . . . ? O2 Er2 O1 Er1 3.60(16) . . . . ? O9 Er2 O1 Er1 -79.0(2) . . . . ? N3 Er2 O1 Er1 126.0(2) . . . . ? N4 Er2 O1 Er1 70.6(2) . . . . ? O4 Er2 O2 C20 -23.5(5) . . . . ? O3 Er2 O2 C20 -145.8(5) . . . . ? O1 Er2 O2 C20 168.4(5) . . . . ? O9 Er2 O2 C20 -108.5(5) . . . . ? N3 Er2 O2 C20 103.9(5) . . . . ? N4 Er2 O2 C20 47.5(5) . . . . ? Er1 Er2 O2 C20 171.9(6) . . . . ? O4 Er2 O2 Er1 164.59(19) . . . . ? O3 Er2 O2 Er1 42.3(6) . . . . ? O1 Er2 O2 Er1 -3.56(16) . . . . ? O9 Er2 O2 Er1 79.6(2) . . . . ? N3 Er2 O2 Er1 -68.0(2) . . . . ? N4 Er2 O2 Er1 -124.4(2) . . . . ? O7 Er1 O2 C20 -17.1(6) . . . . ? O8 Er1 O2 C20 29.4(5) . . . . ? O5 Er1 O2 C20 161.3(5) . . . . ? O1 Er1 O2 C20 -168.3(5) . . . . ? O6 Er1 O2 C20 109.4(5) . . . . ? N1 Er1 O2 C20 -106.7(5) . . . . ? N2 Er1 O2 C20 -53.5(5) . . . . ? Er2 Er1 O2 C20 -171.8(6) . . . . ? O7 Er1 O2 Er2 154.7(2) . . . . ? O8 Er1 O2 Er2 -158.7(2) . . . . ? O5 Er1 O2 Er2 -26.9(4) . . . . ? O1 Er1 O2 Er2 3.58(16) . . . . ? O6 Er1 O2 Er2 -78.7(2) . . . . ? N1 Er1 O2 Er2 65.1(2) . . . . ? N2 Er1 O2 Er2 118.3(2) . . . . ? O4 Er2 O3 C21 136.9(7) . . . . ? O2 Er2 O3 C21 -99.2(8) . . . . ? O1 Er2 O3 C21 -57.1(7) . . . . ? O9 Er2 O3 C21 -136.1(7) . . . . ? N3 Er2 O3 C21 17.9(7) . . . . ? N4 Er2 O3 C21 65.5(7) . . . . ? Er1 Er2 O3 C21 -70.1(7) . . . . ? O3 Er2 O4 C40 -143.7(8) . . . . ? O2 Er2 O4 C40 53.6(8) . . . . ? O1 Er2 O4 C40 98.8(9) . . . . ? O9 Er2 O4 C40 132.3(8) . . . . ? N3 Er2 O4 C40 -71.2(8) . . . . ? N4 Er2 O4 C40 -21.7(8) . . . . ? Er1 Er2 O4 C40 65.6(8) . . . . ? O7 Er1 O5 C42 129.6(8) . . . . ? O8 Er1 O5 C42 69.9(8) . . . . ? O1 Er1 O5 C42 -77.9(8) . . . . ? O2 Er1 O5 C42 -49.4(9) . . . . ? O6 Er1 O5 C42 5.2(8) . . . . ? N1 Er1 O5 C42 -150.5(8) . . . . ? N2 Er1 O5 C42 -178.6(7) . . . . ? Er2 Er1 O5 C42 -65.3(8) . . . . ? O7 Er1 O6 C44 -61.1(7) . . . . ? O8 Er1 O6 C44 -127.0(7) . . . . ? O5 Er1 O6 C44 2.8(6) . . . . ? O1 Er1 O6 C44 85.3(7) . . . . ? O2 Er1 O6 C44 154.3(7) . . . . ? N1 Er1 O6 C44 45.0(8) . . . . ? N2 Er1 O6 C44 -171.7(6) . . . . ? Er2 Er1 O6 C44 120.0(7) . . . . ? O8 Er1 O7 C47 -25.8(7) . . . . ? O5 Er1 O7 C47 -157.4(7) . . . . ? O1 Er1 O7 C47 152.6(7) . . . . ? O2 Er1 O7 C47 21.6(8) . . . . ? O6 Er1 O7 C47 -94.5(7) . . . . ? N1 Er1 O7 C47 121.7(7) . . . . ? N2 Er1 O7 C47 57.0(7) . . . . ? Er2 Er1 O7 C47 81.9(9) . . . . ? O7 Er1 O8 C49 27.4(6) . . . . ? O5 Er1 O8 C49 87.7(7) . . . . ? O1 Er1 O8 C49 -151.1(6) . . . . ? O2 Er1 O8 C49 -123.7(7) . . . . ? O6 Er1 O8 C49 149.8(7) . . . . ? N1 Er1 O8 C49 -23.1(8) . . . . ? N2 Er1 O8 C49 -51.0(7) . . . . ? Er2 Er1 O8 C49 -136.3(6) . . . . ? O7 Er1 N1 C7 129.7(6) . . . . ? O8 Er1 N1 C7 179.3(5) . . . . ? O5 Er1 N1 C7 52.1(6) . . . . ? O1 Er1 N1 C7 -31.5(5) . . . . ? O2 Er1 N1 C7 -91.3(6) . . . . ? O6 Er1 N1 C7 10.9(7) . . . . ? N2 Er1 N1 C7 -149.6(6) . . . . ? Er2 Er1 N1 C7 -60.5(6) . . . . ? O7 Er1 N1 C8 -46.6(4) . . . . ? O8 Er1 N1 C8 3.1(6) . . . . ? O5 Er1 N1 C8 -124.2(4) . . . . ? O1 Er1 N1 C8 152.3(5) . . . . ? O2 Er1 N1 C8 92.4(4) . . . . ? O6 Er1 N1 C8 -165.3(4) . . . . ? N2 Er1 N1 C8 34.1(4) . . . . ? Er2 Er1 N1 C8 123.2(4) . . . . ? O7 Er1 N2 C14 -125.4(6) . . . . ? O8 Er1 N2 C14 -49.1(6) . . . . ? O5 Er1 N2 C14 -177.0(6) . . . . ? O1 Er1 N2 C14 92.3(6) . . . . ? O2 Er1 N2 C14 31.6(6) . . . . ? O6 Er1 N2 C14 -4.4(8) . . . . ? N1 Er1 N2 C14 151.8(7) . . . . ? Er2 Er1 N2 C14 61.4(6) . . . . ? O7 Er1 N2 C13 48.7(5) . . . . ? O8 Er1 N2 C13 125.0(5) . . . . ? O5 Er1 N2 C13 -2.9(6) . . . . ? O1 Er1 N2 C13 -93.7(5) . . . . ? O2 Er1 N2 C13 -154.4(5) . . . . ? O6 Er1 N2 C13 169.6(4) . . . . ? N1 Er1 N2 C13 -34.2(4) . . . . ? Er2 Er1 N2 C13 -124.6(4) . . . . ? O4 Er2 N3 C27 -96.3(6) . . . . ? O3 Er2 N3 C27 -14.2(6) . . . . ? O2 Er2 N3 C27 145.8(6) . . . . ? O1 Er2 N3 C27 86.5(6) . . . . ? O9 Er2 N3 C27 37.8(8) . . . . ? N4 Er2 N3 C27 -149.8(7) . . . . ? Er1 Er2 N3 C27 113.7(6) . . . . ? O4 Er2 N3 C28 91.2(4) . . . . ? O3 Er2 N3 C28 173.3(5) . . . . ? O2 Er2 N3 C28 -26.8(5) . . . . ? O1 Er2 N3 C28 -86.1(4) . . . . ? O9 Er2 N3 C28 -134.7(4) . . . . ? N4 Er2 N3 C28 37.7(4) . . . . ? Er1 Er2 N3 C28 -58.8(4) . . . . ? O4 Er2 N4 C34 14.9(6) . . . . ? O3 Er2 N4 C34 95.6(7) . . . . ? O2 Er2 N4 C34 -89.8(7) . . . . ? O1 Er2 N4 C34 -150.4(6) . . . . ? O9 Er2 N4 C34 -40.7(8) . . . . ? N3 Er2 N4 C34 147.2(7) . . . . ? Er1 Er2 N4 C34 -118.1(7) . . . . ? O4 Er2 N4 C33 -169.9(5) . . . . ? O3 Er2 N4 C33 -89.3(5) . . . . ? O2 Er2 N4 C33 85.3(5) . . . . ? O1 Er2 N4 C33 24.7(5) . . . . ? O9 Er2 N4 C33 134.4(5) . . . . ? N3 Er2 N4 C33 -37.6(4) . . . . ? Er1 Er2 N4 C33 57.0(5) . . . . ? Er1 O1 C1 C2 124.4(6) . . . . ? Er2 O1 C1 C2 -59.2(8) . . . . ? Er1 O1 C1 C6 -57.9(8) . . . . ? Er2 O1 C1 C6 118.6(6) . . . . ? O1 C1 C2 C3 177.1(7) . . . . ? C6 C1 C2 C3 -0.7(11) . . . . ? C1 C2 C3 C4 -1.8(14) . . . . ? C2 C3 C4 C5 1.7(16) . . . . ? C3 C4 C5 C6 0.9(16) . . . . ? C4 C5 C6 C1 -3.3(13) . . . . ? C4 C5 C6 C7 176.2(8) . . . . ? O1 C1 C6 C5 -174.6(7) . . . . ? C2 C1 C6 C5 3.2(11) . . . . ? O1 C1 C6 C7 5.9(11) . . . . ? C2 C1 C6 C7 -176.3(7) . . . . ? C8 N1 C7 C6 -179.5(6) . . . . ? Er1 N1 C7 C6 4.5(10) . . . . ? C5 C6 C7 N1 -159.2(7) . . . . ? C1 C6 C7 N1 20.3(12) . . . . ? C7 N1 C8 C9 -30.4(10) . . . . ? Er1 N1 C8 C9 146.1(6) . . . . ? C7 N1 C8 C13 151.2(7) . . . . ? Er1 N1 C8 C13 -32.3(7) . . . . ? C13 C8 C9 C10 -1.1(12) . . . . ? N1 C8 C9 C10 -179.4(7) . . . . ? C8 C9 C10 C11 2.2(14) . . . . ? C9 C10 C11 C12 -1.5(15) . . . . ? C10 C11 C12 C13 -0.2(15) . . . . ? C9 C8 C13 C12 -0.7(11) . . . . ? N1 C8 C13 C12 177.8(7) . . . . ? C9 C8 C13 N2 -178.5(6) . . . . ? N1 C8 C13 N2 0.0(9) . . . . ? C11 C12 C13 C8 1.3(13) . . . . ? C11 C12 C13 N2 178.9(8) . . . . ? C14 N2 C13 C8 -153.2(7) . . . . ? Er1 N2 C13 C8 32.2(7) . . . . ? C14 N2 C13 C12 29.0(11) . . . . ? Er1 N2 C13 C12 -145.5(7) . . . . ? C13 N2 C14 C15 179.7(7) . . . . ? Er1 N2 C14 C15 -6.5(11) . . . . ? N2 C14 C15 C20 -19.5(12) . . . . ? N2 C14 C15 C16 162.2(8) . . . . ? C20 C15 C16 C17 3.2(12) . . . . ? C14 C15 C16 C17 -178.4(8) . . . . ? C15 C16 C17 C18 -2.8(14) . . . . ? C16 C17 C18 C19 1.2(14) . . . . ? C17 C18 C19 C20 -0.1(13) . . . . ? Er2 O2 C20 C15 -117.7(6) . . . . ? Er1 O2 C20 C15 53.1(8) . . . . ? Er2 O2 C20 C19 59.4(8) . . . . ? Er1 O2 C20 C19 -129.8(6) . . . . ? C16 C15 C20 O2 175.2(7) . . . . ? C14 C15 C20 O2 -3.1(11) . . . . ? C16 C15 C20 C19 -2.0(11) . . . . ? C14 C15 C20 C19 179.8(7) . . . . ? C18 C19 C20 O2 -176.7(7) . . . . ? C18 C19 C20 C15 0.5(11) . . . . ? Er2 O3 C21 C22 166.4(6) . . . . ? Er2 O3 C21 C26 -14.8(11) . . . . ? O3 C21 C22 C23 -177.3(8) . . . . ? C26 C21 C22 C23 3.9(12) . . . . ? C21 C22 C23 C24 -2.2(15) . . . . ? C22 C23 C24 C25 -0.3(15) . . . . ? C23 C24 C25 C26 1.0(14) . . . . ? C24 C25 C26 C21 0.9(12) . . . . ? C24 C25 C26 C27 179.5(8) . . . . ? O3 C21 C26 C25 178.0(7) . . . . ? C22 C21 C26 C25 -3.2(11) . . . . ? O3 C21 C26 C27 -0.6(11) . . . . ? C22 C21 C26 C27 178.2(7) . . . . ? C28 N3 C27 C26 -178.0(7) . . . . ? Er2 N3 C27 C26 9.9(11) . . . . ? C25 C26 C27 N3 -177.4(7) . . . . ? C21 C26 C27 N3 1.2(12) . . . . ? C27 N3 C28 C33 151.7(7) . . . . ? Er2 N3 C28 C33 -34.7(7) . . . . ? C27 N3 C28 C29 -31.9(10) . . . . ? Er2 N3 C28 C29 141.7(6) . . . . ? C33 C28 C29 C30 -2.1(11) . . . . ? N3 C28 C29 C30 -178.4(7) . . . . ? C28 C29 C30 C31 0.5(12) . . . . ? C29 C30 C31 C32 1.6(14) . . . . ? C30 C31 C32 C33 -1.9(13) . . . . ? C29 C28 C33 C32 1.8(11) . . . . ? N3 C28 C33 C32 178.4(6) . . . . ? C29 C28 C33 N4 -177.0(6) . . . . ? N3 C28 C33 N4 -0.4(9) . . . . ? C31 C32 C33 C28 0.2(11) . . . . ? C31 C32 C33 N4 178.9(7) . . . . ? C34 N4 C33 C28 -149.3(7) . . . . ? Er2 N4 C33 C28 35.1(8) . . . . ? C34 N4 C33 C32 32.0(11) . . . . ? Er2 N4 C33 C32 -143.7(6) . . . . ? C33 N4 C34 C35 178.5(7) . . . . ? Er2 N4 C34 C35 -6.8(12) . . . . ? N4 C34 C35 C36 175.8(8) . . . . ? N4 C34 C35 C40 -7.6(14) . . . . ? C40 C35 C36 C37 1.4(15) . . . . ? C34 C35 C36 C37 178.2(9) . . . . ? C35 C36 C37 C38 -3.2(17) . . . . ? C36 C37 C38 C39 1.1(17) . . . . ? C37 C38 C39 C40 2.8(15) . . . . ? Er2 O4 C40 C35 16.7(13) . . . . ? Er2 O4 C40 C39 -164.0(6) . . . . ? C36 C35 C40 O4 -178.2(8) . . . . ? C34 C35 C40 O4 5.1(12) . . . . ? C36 C35 C40 C39 2.4(12) . . . . ? C34 C35 C40 C39 -174.2(8) . . . . ? C38 C39 C40 O4 176.2(8) . . . . ? C38 C39 C40 C35 -4.5(12) . . . . ? Er1 O5 C42 C43 -11.5(14) . . . . ? Er1 O5 C42 C41 169.1(6) . . . . ? O5 C42 C43 C44 9.6(15) . . . . ? C41 C42 C43 C44 -171.1(9) . . . . ? Er1 O6 C44 C43 -4.1(12) . . . . ? Er1 O6 C44 C45 178.3(5) . . . . ? C42 C43 C44 O6 -2.1(14) . . . . ? C42 C43 C44 C45 175.3(9) . . . . ? Er1 O7 C47 C48 17.4(13) . . . . ? Er1 O7 C47 C46 -162.1(6) . . . . ? O7 C47 C48 C49 4.9(14) . . . . ? C46 C47 C48 C49 -175.6(8) . . . . ? Er1 O8 C49 C48 -20.9(11) . . . . ? Er1 O8 C49 C50 159.3(6) . . . . ? C47 C48 C49 O8 -3.1(14) . . . . ? C47 C48 C49 C50 176.6(9) . . . . ? C53 O10 C52 C51 -169(2) . . . . ? C52 O10 C53 C54 164(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.890 _refine_diff_density_min -2.360 _refine_diff_density_rms 0.175 _database_code_depnum_ccdc_archive 'CCDC 830605' ####################################################################### # # 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_42 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H76 N4 O19 Tb4' _chemical_formula_weight 1828.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.4209(13) _cell_length_b 14.9879(8) _cell_length_c 21.0093(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.9440(10) _cell_angle_gamma 90.00 _cell_volume 7198.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4320 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 3.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4384 _exptl_absorpt_correction_T_max 0.5367 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25792 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.26 _reflns_number_total 8903 _reflns_number_gt 5378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction SAINT-plus _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0366P)^2^+74.4291P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8903 _refine_ls_number_parameters 416 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.676211(14) 0.18815(2) -0.047298(19) 0.04117(11) Uani 1 1 d . . . Tb2 Tb 0.673615(16) 0.43021(3) -0.05473(2) 0.04815(12) Uani 1 1 d . . . N2 N 0.6251(3) 0.4243(4) 0.0289(4) 0.0501(16) Uani 1 1 d . . . N1 N 0.7100(3) 0.5471(5) 0.0406(4) 0.0559(18) Uani 1 1 d . . . C1 C 0.6752(4) 0.5603(6) 0.0797(5) 0.065(2) Uani 1 1 d . . . H1A H 0.6412 0.5965 0.0520 0.078 Uiso 1 1 calc R . . H1B H 0.6983 0.5915 0.1237 0.078 Uiso 1 1 calc R . . C2 C 0.6561(4) 0.4714(6) 0.0955(5) 0.061(2) Uani 1 1 d . . . H2A H 0.6898 0.4371 0.1269 0.073 Uiso 1 1 calc R . . H2B H 0.6306 0.4799 0.1184 0.073 Uiso 1 1 calc R . . C3 C 0.7512(4) 0.6013(6) 0.0514(5) 0.061(2) Uani 1 1 d . . . H3A H 0.7569 0.6460 0.0845 0.073 Uiso 1 1 calc R . . C4 C 0.7908(3) 0.6016(5) 0.0177(5) 0.055(2) Uani 1 1 d . . . C5 C 0.8006(3) 0.5256(5) -0.0143(4) 0.0457(18) Uani 1 1 d . . . C6 C 0.8388(4) 0.5336(6) -0.0467(5) 0.062(2) Uani 1 1 d . . . H6A H 0.8459 0.4843 -0.0686 0.074 Uiso 1 1 calc R . . C7 C 0.8656(4) 0.6141(7) -0.0462(6) 0.073(3) Uani 1 1 d . . . H7A H 0.8902 0.6184 -0.0683 0.088 Uiso 1 1 calc R . . C8 C 0.8562(4) 0.6875(7) -0.0136(6) 0.081(3) Uani 1 1 d . . . H8A H 0.8745 0.7412 -0.0135 0.097 Uiso 1 1 calc R . . C9 C 0.8195(4) 0.6820(6) 0.0194(6) 0.073(3) Uani 1 1 d . . . H9A H 0.8140 0.7314 0.0425 0.088 Uiso 1 1 calc R . . C10 C 0.5719(3) 0.4023(6) 0.0118(5) 0.057(2) Uani 1 1 d . . . H10A H 0.5569 0.4173 0.0435 0.069 Uiso 1 1 calc R . . C11 C 0.5328(3) 0.3560(6) -0.0525(5) 0.061(2) Uani 1 1 d . . . C12 C 0.5514(3) 0.3125(6) -0.0978(4) 0.053(2) Uani 1 1 d . . . C13 C 0.5103(4) 0.2692(8) -0.1574(5) 0.074(3) Uani 1 1 d . . . H13A H 0.5220 0.2419 -0.1888 0.089 Uiso 1 1 calc R . . C14 C 0.4512(4) 0.2665(10) -0.1704(6) 0.103(4) Uani 1 1 d . . . H14A H 0.4243 0.2347 -0.2089 0.124 Uiso 1 1 calc R . . C15 C 0.4333(4) 0.3107(9) -0.1265(6) 0.103(4) Uani 1 1 d . . . H15A H 0.3938 0.3117 -0.1370 0.124 Uiso 1 1 calc R . . C16 C 0.4727(4) 0.3535(8) -0.0674(6) 0.081(3) Uani 1 1 d . . . H16A H 0.4601 0.3811 -0.0369 0.097 Uiso 1 1 calc R . . C17 C 0.5243(5) 0.6462(8) -0.1327(6) 0.104(4) Uani 1 1 d . . . H17A H 0.5068 0.6098 -0.1095 0.156 Uiso 1 1 calc R . . H17B H 0.4974 0.6531 -0.1817 0.156 Uiso 1 1 calc R . . H17C H 0.5335 0.7038 -0.1105 0.156 Uiso 1 1 calc R . . C18 C 0.5802(4) 0.6018(7) -0.1270(5) 0.069(3) Uani 1 1 d . . . C19 C 0.6125(4) 0.6410(7) -0.1571(6) 0.083(3) Uani 1 1 d . . . H19A H 0.6003 0.6966 -0.1782 0.099 Uiso 1 1 calc R . . C20 C 0.6615(4) 0.6049(7) -0.1587(5) 0.072(3) Uani 1 1 d . . . C21 C 0.6938(5) 0.6543(9) -0.1940(7) 0.119(5) Uani 1 1 d . . . H21A H 0.7270 0.6199 -0.1897 0.178 Uiso 1 1 calc R . . H21B H 0.7067 0.7111 -0.1715 0.178 Uiso 1 1 calc R . . H21C H 0.6680 0.6631 -0.2432 0.178 Uiso 1 1 calc R . . C22 C 0.6024(5) 0.2110(8) 0.1203(6) 0.098(4) Uani 1 1 d . . . H22A H 0.6381 0.2422 0.1484 0.147 Uiso 1 1 calc R . . H22B H 0.5987 0.1608 0.1464 0.147 Uiso 1 1 calc R . . H22C H 0.5698 0.2504 0.1090 0.147 Uiso 1 1 calc R . . C23 C 0.6035(4) 0.1790(6) 0.0530(6) 0.068(3) Uani 1 1 d . . . C24 C 0.5564(4) 0.1312(7) 0.0041(6) 0.075(3) Uani 1 1 d . . . H24A H 0.5247 0.1222 0.0143 0.090 Uiso 1 1 calc R . . C25 C 0.5527(4) 0.0965(7) -0.0575(6) 0.078(3) Uani 1 1 d . . . C26 C 0.5002(5) 0.0405(9) -0.1030(7) 0.123(5) Uani 1 1 d . . . H26A H 0.5039 0.0210 -0.1443 0.184 Uiso 1 1 calc R . . H26B H 0.4653 0.0755 -0.1170 0.184 Uiso 1 1 calc R . . H26C H 0.4981 -0.0104 -0.0765 0.184 Uiso 1 1 calc R . . C27 C 0.7320(4) 0.3802(7) -0.1940(5) 0.074(3) Uani 1 1 d . . . H27A H 0.7311 0.4302 -0.1659 0.111 Uiso 1 1 calc R . . H27B H 0.7068 0.3918 -0.2429 0.111 Uiso 1 1 calc R . . H27C H 0.7713 0.3711 -0.1880 0.111 Uiso 1 1 calc R . . C28 C 0.7111(3) 0.2971(6) -0.1703(4) 0.050(2) Uani 1 1 d . . . C29 C 0.7095(4) 0.2169(6) -0.2043(5) 0.062(2) Uani 1 1 d . . . H29A H 0.7270 0.2162 -0.2350 0.074 Uiso 1 1 calc R . . C30 C 0.6845(3) 0.1390(6) -0.1971(5) 0.057(2) Uani 1 1 d . . . C31 C 0.6796(5) 0.0614(7) -0.2471(5) 0.080(3) Uani 1 1 d . . . H31A H 0.6613 0.0115 -0.2364 0.120 Uiso 1 1 calc R . . H31B H 0.7180 0.0446 -0.2409 0.120 Uiso 1 1 calc R . . H31C H 0.6565 0.0797 -0.2952 0.120 Uiso 1 1 calc R . . O1 O 0.7763(2) 0.4462(3) -0.0139(3) 0.0492(13) Uani 1 1 d . . . O2 O 0.6076(2) 0.3106(4) -0.0863(3) 0.0501(13) Uani 1 1 d . . . O3 O 0.72310(19) 0.3147(3) 0.0227(3) 0.0413(11) Uani 1 1 d D . . H3 H 0.7143 0.3073 0.0567 0.05(2) Uiso 1 1 d RD . . O4 O 0.6828(2) 0.5316(4) -0.1313(3) 0.0685(17) Uani 1 1 d . . . O5 O 0.5935(2) 0.5292(4) -0.0935(3) 0.0674(17) Uani 1 1 d . . . O6 O 0.6497(2) 0.1980(4) 0.0465(3) 0.0547(14) Uani 1 1 d . . . O7 O 0.5911(2) 0.1054(4) -0.0808(3) 0.0679(17) Uani 1 1 d . . . O8 O 0.6954(2) 0.3064(3) -0.1203(3) 0.0478(12) Uani 1 1 d . . . O9 O 0.6649(2) 0.1242(4) -0.1522(3) 0.0598(15) Uani 1 1 d . . . O10 O 0.5692(7) -0.0289(16) -0.2045(12) 0.151(9) Uani 0.50 1 d PU . . H10C H 0.5989 -0.1294 -0.2280 0.226 Uiso 0.50 1 d PR . . H10B H 0.5714 -0.1456 -0.1751 0.226 Uiso 0.50 1 d PR . . H10D H 0.6325 -0.0988 -0.1489 0.226 Uiso 0.50 1 d PR . . C32 C 0.5964(15) -0.1032(15) -0.1979(13) 0.167(17) Uani 0.50 1 d PU . . H32A H 0.5941 0.0145 -0.1858 0.250 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03099(17) 0.0513(2) 0.0498(2) 0.00302(17) 0.02562(15) 0.00370(17) Tb2 0.0404(2) 0.0510(2) 0.0656(3) 0.01016(19) 0.03479(19) 0.01069(17) N2 0.042(3) 0.058(4) 0.061(4) 0.008(3) 0.033(3) 0.014(3) N1 0.043(4) 0.060(4) 0.075(5) 0.000(4) 0.036(4) 0.005(3) C1 0.062(5) 0.067(6) 0.085(7) -0.015(5) 0.049(5) 0.004(4) C2 0.059(5) 0.069(6) 0.065(6) 0.003(5) 0.038(5) 0.009(4) C3 0.054(5) 0.055(5) 0.078(6) -0.005(4) 0.033(5) 0.006(4) C4 0.043(4) 0.049(5) 0.076(6) 0.012(4) 0.028(4) 0.013(4) C5 0.040(4) 0.051(5) 0.050(5) 0.005(4) 0.024(4) 0.005(3) C6 0.058(5) 0.055(5) 0.089(7) 0.005(5) 0.049(5) 0.000(4) C7 0.073(6) 0.066(6) 0.102(8) 0.007(6) 0.058(6) -0.006(5) C8 0.073(6) 0.055(6) 0.127(10) 0.008(6) 0.054(7) -0.011(5) C9 0.066(6) 0.054(6) 0.106(8) -0.005(5) 0.043(6) -0.009(5) C10 0.050(5) 0.069(6) 0.070(6) 0.012(5) 0.042(5) 0.018(4) C11 0.040(4) 0.081(6) 0.073(6) 0.014(5) 0.035(4) 0.014(4) C12 0.034(4) 0.075(6) 0.053(5) 0.016(4) 0.020(4) 0.011(4) C13 0.042(5) 0.126(9) 0.060(6) 0.002(6) 0.027(4) 0.019(5) C14 0.033(5) 0.185(13) 0.089(8) -0.017(8) 0.023(5) -0.001(6) C15 0.032(5) 0.179(13) 0.103(9) -0.014(9) 0.033(5) 0.010(6) C16 0.043(5) 0.114(9) 0.095(8) 0.002(7) 0.040(5) 0.008(5) C17 0.088(8) 0.131(10) 0.114(10) 0.045(8) 0.063(7) 0.064(8) C18 0.052(5) 0.092(7) 0.064(6) 0.024(5) 0.025(5) 0.030(5) C19 0.079(7) 0.089(8) 0.092(8) 0.047(6) 0.048(6) 0.036(6) C20 0.064(6) 0.084(7) 0.080(7) 0.033(6) 0.043(5) 0.023(5) C21 0.110(10) 0.126(11) 0.152(13) 0.077(10) 0.086(10) 0.035(8) C22 0.116(9) 0.116(9) 0.112(9) 0.017(7) 0.097(8) 0.024(7) C23 0.070(6) 0.075(7) 0.088(7) 0.029(5) 0.062(6) 0.025(5) C24 0.058(6) 0.084(7) 0.114(9) 0.022(6) 0.067(6) 0.008(5) C25 0.042(5) 0.091(8) 0.107(9) 0.013(6) 0.039(5) -0.006(5) C26 0.068(7) 0.164(13) 0.139(12) -0.014(10) 0.048(8) -0.048(8) C27 0.084(7) 0.089(7) 0.075(7) 0.018(5) 0.059(6) 0.017(6) C28 0.042(4) 0.072(6) 0.048(4) 0.014(4) 0.030(4) 0.018(4) C29 0.056(5) 0.084(7) 0.066(6) 0.005(5) 0.045(5) 0.012(5) C30 0.039(4) 0.077(6) 0.054(5) 0.001(4) 0.021(4) 0.006(4) C31 0.091(7) 0.088(7) 0.080(7) -0.021(6) 0.055(6) -0.012(6) O1 0.039(3) 0.042(3) 0.078(4) 0.008(3) 0.036(3) 0.006(2) O2 0.030(2) 0.071(4) 0.056(3) 0.011(3) 0.026(2) 0.009(2) O3 0.034(2) 0.049(3) 0.050(3) 0.007(2) 0.027(2) 0.007(2) O4 0.061(4) 0.082(4) 0.078(4) 0.030(4) 0.046(3) 0.026(3) O5 0.050(3) 0.083(4) 0.079(4) 0.033(4) 0.036(3) 0.021(3) O6 0.055(3) 0.060(4) 0.066(4) 0.010(3) 0.043(3) 0.010(3) O7 0.039(3) 0.092(5) 0.080(4) 0.001(4) 0.033(3) -0.012(3) O8 0.043(3) 0.063(3) 0.048(3) 0.006(3) 0.029(2) 0.011(3) O9 0.057(3) 0.072(4) 0.061(4) -0.009(3) 0.036(3) -0.003(3) O10 0.082(11) 0.21(2) 0.170(18) -0.121(17) 0.067(12) -0.084(13) C32 0.22(3) 0.065(15) 0.079(16) 0.059(13) -0.066(17) -0.079(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O9 2.304(6) . ? Tb1 O7 2.320(5) . ? Tb1 O6 2.349(5) . ? Tb1 O3 2.377(5) . ? Tb1 O3 2.380(4) 7_655 ? Tb1 O1 2.410(5) 7_655 ? Tb1 O2 2.416(5) . ? Tb1 O8 2.527(5) . ? Tb1 Tb2 3.6307(6) . ? Tb1 Tb1 3.8649(7) 7_655 ? Tb1 Tb2 3.8930(5) 7_655 ? Tb2 O4 2.297(6) . ? Tb2 O3 2.331(5) . ? Tb2 O2 2.344(5) . ? Tb2 O5 2.358(5) . ? Tb2 O1 2.376(5) . ? Tb2 N1 2.514(7) . ? Tb2 O8 2.513(5) . ? Tb2 N2 2.553(6) . ? Tb2 Tb1 3.8930(5) 7_655 ? N2 C10 1.280(9) . ? N2 C2 1.453(11) . ? N1 C3 1.265(10) . ? N1 C1 1.459(9) . ? C1 C2 1.504(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.461(11) . ? C3 H3A 0.9300 . ? C4 C5 1.401(11) . ? C4 C9 1.401(11) . ? C5 O1 1.343(9) . ? C5 C6 1.413(10) . ? C6 C7 1.383(12) . ? C6 H6A 0.9300 . ? C7 C8 1.372(13) . ? C7 H7A 0.9300 . ? C8 C9 1.385(14) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C11 1.456(12) . ? C10 H10A 0.9300 . ? C11 C12 1.395(11) . ? C11 C16 1.418(11) . ? C12 O2 1.341(8) . ? C12 C13 1.392(12) . ? C13 C14 1.405(11) . ? C13 H13A 0.9300 . ? C14 C15 1.364(15) . ? C14 H14A 0.9300 . ? C15 C16 1.367(14) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.525(12) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O5 1.259(10) . ? C18 C19 1.371(13) . ? C19 C20 1.372(12) . ? C19 H19A 0.9300 . ? C20 O4 1.249(10) . ? C20 C21 1.517(13) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.505(13) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O6 1.272(10) . ? C23 C24 1.388(14) . ? C24 C25 1.360(14) . ? C24 H24A 0.9300 . ? C25 O7 1.276(10) . ? C25 C26 1.510(14) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.522(12) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O8 1.283(8) . ? C28 C29 1.390(12) . ? C29 C30 1.368(12) . ? C29 H29A 0.9300 . ? C30 O9 1.263(9) . ? C30 C31 1.535(12) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O1 Tb1 2.410(5) 7_655 ? O3 Tb1 2.380(4) 7_655 ? O3 H3 0.8453 . ? O10 C32 1.29(4) . ? O10 H32A 0.8728 . ? C32 H10C 0.7694 . ? C32 H10B 1.1408 . ? C32 H10D 1.0387 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Tb1 O7 77.2(2) . . ? O9 Tb1 O6 150.2(2) . . ? O7 Tb1 O6 73.6(2) . . ? O9 Tb1 O3 137.98(18) . . ? O7 Tb1 O3 139.75(19) . . ? O6 Tb1 O3 71.38(18) . . ? O9 Tb1 O3 82.64(18) . 7_655 ? O7 Tb1 O3 145.88(19) . 7_655 ? O6 Tb1 O3 119.65(18) . 7_655 ? O3 Tb1 O3 71.31(18) . 7_655 ? O9 Tb1 O1 89.2(2) . 7_655 ? O7 Tb1 O1 84.19(19) . 7_655 ? O6 Tb1 O1 82.31(18) . 7_655 ? O3 Tb1 O1 109.77(17) . 7_655 ? O3 Tb1 O1 68.19(16) 7_655 7_655 ? O9 Tb1 O2 102.86(19) . . ? O7 Tb1 O2 82.2(2) . . ? O6 Tb1 O2 78.88(17) . . ? O3 Tb1 O2 72.28(17) . . ? O3 Tb1 O2 129.50(16) 7_655 . ? O1 Tb1 O2 159.25(16) 7_655 . ? O9 Tb1 O8 71.76(19) . . ? O7 Tb1 O8 126.33(19) . . ? O6 Tb1 O8 131.85(17) . . ? O3 Tb1 O8 68.79(16) . . ? O3 Tb1 O8 70.71(15) 7_655 . ? O1 Tb1 O8 136.46(15) 7_655 . ? O2 Tb1 O8 64.13(15) . . ? O9 Tb1 Tb2 112.47(15) . . ? O7 Tb1 Tb2 121.61(16) . . ? O6 Tb1 Tb2 88.09(13) . . ? O3 Tb1 Tb2 39.09(11) . . ? O3 Tb1 Tb2 91.43(11) 7_655 . ? O1 Tb1 Tb2 148.58(13) 7_655 . ? O2 Tb1 Tb2 39.57(12) . . ? O8 Tb1 Tb2 43.77(11) . . ? O9 Tb1 Tb1 112.20(13) . 7_655 ? O7 Tb1 Tb1 168.27(16) . 7_655 ? O6 Tb1 Tb1 96.22(14) . 7_655 ? O3 Tb1 Tb1 35.68(10) . 7_655 ? O3 Tb1 Tb1 35.63(12) 7_655 7_655 ? O1 Tb1 Tb1 88.81(12) 7_655 7_655 ? O2 Tb1 Tb1 101.80(12) . 7_655 ? O8 Tb1 Tb1 64.80(12) . 7_655 ? Tb2 Tb1 Tb1 62.488(11) . 7_655 ? O9 Tb1 Tb2 91.07(14) . 7_655 ? O7 Tb1 Tb2 118.90(16) . 7_655 ? O6 Tb1 Tb2 97.97(13) . 7_655 ? O3 Tb1 Tb2 85.27(10) . 7_655 ? O3 Tb1 Tb2 33.88(11) 7_655 7_655 ? O1 Tb1 Tb2 35.26(11) 7_655 7_655 ? O2 Tb1 Tb2 157.20(13) . 7_655 ? O8 Tb1 Tb2 104.52(11) . 7_655 ? Tb2 Tb1 Tb2 118.295(11) . 7_655 ? Tb1 Tb1 Tb2 55.808(10) 7_655 7_655 ? O4 Tb2 O3 142.21(17) . . ? O4 Tb2 O2 126.0(2) . . ? O3 Tb2 O2 74.38(17) . . ? O4 Tb2 O5 71.29(19) . . ? O3 Tb2 O5 146.00(18) . . ? O2 Tb2 O5 88.84(19) . . ? O4 Tb2 O1 75.76(19) . . ? O3 Tb2 O1 69.55(16) . . ? O2 Tb2 O1 135.79(17) . . ? O5 Tb2 O1 135.04(19) . . ? O4 Tb2 N1 89.0(2) . . ? O3 Tb2 N1 93.6(2) . . ? O2 Tb2 N1 136.59(19) . . ? O5 Tb2 N1 78.3(2) . . ? O1 Tb2 N1 71.27(19) . . ? O4 Tb2 O8 89.45(19) . . ? O3 Tb2 O8 69.71(16) . . ? O2 Tb2 O8 65.32(16) . . ? O5 Tb2 O8 129.7(2) . . ? O1 Tb2 O8 78.59(17) . . ? N1 Tb2 O8 149.25(18) . . ? O4 Tb2 N2 137.1(2) . . ? O3 Tb2 N2 76.69(18) . . ? O2 Tb2 N2 70.5(2) . . ? O5 Tb2 N2 69.8(2) . . ? O1 Tb2 N2 122.7(2) . . ? N1 Tb2 N2 66.1(2) . . ? O8 Tb2 N2 129.83(19) . . ? O4 Tb2 Tb1 133.27(16) . . ? O3 Tb2 Tb1 40.00(12) . . ? O2 Tb2 Tb1 41.02(12) . . ? O5 Tb2 Tb1 129.80(16) . . ? O1 Tb2 Tb1 95.09(12) . . ? N1 Tb2 Tb1 131.98(16) . . ? O8 Tb2 Tb1 44.06(11) . . ? N2 Tb2 Tb1 86.62(15) . . ? O4 Tb2 Tb1 108.11(14) . 7_655 ? O3 Tb2 Tb1 34.68(11) . 7_655 ? O2 Tb2 Tb1 102.46(12) . 7_655 ? O5 Tb2 Tb1 165.38(17) . 7_655 ? O1 Tb2 Tb1 35.85(12) . 7_655 ? N1 Tb2 Tb1 87.06(14) . 7_655 ? O8 Tb2 Tb1 64.36(11) . 7_655 ? N2 Tb2 Tb1 104.97(14) . 7_655 ? Tb1 Tb2 Tb1 61.705(11) . 7_655 ? C10 N2 C2 117.3(7) . . ? C10 N2 Tb2 125.7(6) . . ? C2 N2 Tb2 115.1(5) . . ? C3 N1 C1 118.1(8) . . ? C3 N1 Tb2 125.2(6) . . ? C1 N1 Tb2 116.2(5) . . ? N1 C1 C2 109.7(7) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 108.1(7) . . ? N2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N1 C3 C4 127.5(8) . . ? N1 C3 H3A 116.3 . . ? C4 C3 H3A 116.3 . . ? C5 C4 C9 120.7(8) . . ? C5 C4 C3 122.3(8) . . ? C9 C4 C3 117.0(8) . . ? O1 C5 C4 122.6(7) . . ? O1 C5 C6 119.6(7) . . ? C4 C5 C6 117.8(7) . . ? C7 C6 C5 120.7(8) . . ? C7 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C8 C7 C6 120.6(9) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 120.3(9) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C8 C9 C4 119.7(9) . . ? C8 C9 H9A 120.1 . . ? C4 C9 H9A 120.1 . . ? N2 C10 C11 126.4(7) . . ? N2 C10 H10A 116.8 . . ? C11 C10 H10A 116.8 . . ? C12 C11 C16 119.4(9) . . ? C12 C11 C10 123.8(7) . . ? C16 C11 C10 116.8(8) . . ? O2 C12 C13 118.3(7) . . ? O2 C12 C11 122.6(8) . . ? C13 C12 C11 119.1(7) . . ? C12 C13 C14 120.4(9) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 119.9(11) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.9(9) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C11 120.2(10) . . ? C15 C16 H16A 119.9 . . ? C11 C16 H16A 119.9 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O5 C18 C19 124.0(8) . . ? O5 C18 C17 115.8(9) . . ? C19 C18 C17 120.2(9) . . ? C18 C19 C20 125.2(9) . . ? C18 C19 H19A 117.4 . . ? C20 C19 H19A 117.4 . . ? O4 C20 C19 123.5(9) . . ? O4 C20 C21 115.9(8) . . ? C19 C20 C21 120.6(9) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O6 C23 C24 125.1(9) . . ? O6 C23 C22 115.3(10) . . ? C24 C23 C22 119.6(8) . . ? C25 C24 C23 125.4(8) . . ? C25 C24 H24A 117.3 . . ? C23 C24 H24A 117.3 . . ? O7 C25 C24 125.4(9) . . ? O7 C25 C26 115.3(11) . . ? C24 C25 C26 119.2(9) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O8 C28 C29 124.4(8) . . ? O8 C28 C27 117.2(8) . . ? C29 C28 C27 118.4(7) . . ? C30 C29 C28 126.2(8) . . ? C30 C29 H29A 116.9 . . ? C28 C29 H29A 116.9 . . ? O9 C30 C29 125.9(8) . . ? O9 C30 C31 115.9(8) . . ? C29 C30 C31 118.2(8) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C5 O1 Tb2 121.6(4) . . ? C5 O1 Tb1 128.2(4) . 7_655 ? Tb2 O1 Tb1 108.89(19) . 7_655 ? C12 O2 Tb2 127.6(5) . . ? C12 O2 Tb1 129.1(5) . . ? Tb2 O2 Tb1 99.41(17) . . ? Tb2 O3 Tb1 100.92(18) . . ? Tb2 O3 Tb1 111.45(18) . 7_655 ? Tb1 O3 Tb1 108.69(18) . 7_655 ? Tb2 O3 H3 115.2 . . ? Tb1 O3 H3 99.8 . . ? Tb1 O3 H3 118.2 7_655 . ? C20 O4 Tb2 138.5(6) . . ? C18 O5 Tb2 135.9(5) . . ? C23 O6 Tb1 133.8(6) . . ? C25 O7 Tb1 135.1(7) . . ? C28 O8 Tb2 138.6(5) . . ? C28 O8 Tb1 129.2(5) . . ? Tb2 O8 Tb1 92.17(15) . . ? C30 O9 Tb1 135.7(6) . . ? C32 O10 H32A 110.2 . . ? O10 C32 H10C 125.9 . . ? O10 C32 H10B 98.9 . . ? H10C C32 H10B 108.7 . . ? O10 C32 H10D 104.6 . . ? H10C C32 H10D 119.5 . . ? H10B C32 H10D 91.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O6 0.85 2.26 2.757(7) 117.8 . O10 H32A O9 0.87 2.31 3.172(17) 169.9 . O10 H32A O7 0.87 2.62 3.137(18) 118.8 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.420 _refine_diff_density_min -1.586 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 839728' ####################################################################### # # 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_36 #TrackingRef '6Dy.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H78 Dy4 N6 O18' _chemical_formula_sum 'C66 H78 Dy4 N6 O18' _chemical_formula_weight 1893.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _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 11.9873(5) _cell_length_b 12.6398(5) _cell_length_c 14.0357(9) _cell_angle_alpha 112.4560(10) _cell_angle_beta 101.5560(10) _cell_angle_gamma 105.7770(10) _cell_volume 1777.28(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.769 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 4.226 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4303 _exptl_absorpt_correction_T_max 0.5167 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13167 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8774 _reflns_number_gt 7028 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+0.5183P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8774 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.008 _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 0.447250(13) 0.547908(13) 0.388909(12) 0.02955(5) Uani 1 1 d . . . Dy2 Dy 0.687331(14) 0.783831(14) 0.642472(12) 0.03363(5) Uani 1 1 d . . . C28 C 0.3688(3) 0.6907(3) 0.6190(3) 0.0385(8) Uani 1 1 d . . . O6 O 0.6001(2) 0.5200(2) 0.31290(19) 0.0393(5) Uani 1 1 d . . . O3 O 0.6202(2) 0.5743(2) 0.52520(17) 0.0307(5) Uani 1 1 d D . . O1 O 0.6668(2) 0.6689(2) 0.74218(17) 0.0364(5) Uani 1 1 d . . . O8 O 0.4575(2) 0.6862(2) 0.58249(18) 0.0365(5) Uani 1 1 d . . . O2 O 0.5836(2) 0.7618(2) 0.47269(19) 0.0387(5) Uani 1 1 d . . . O7 O 0.4063(2) 0.5826(2) 0.23791(19) 0.0417(6) Uani 1 1 d . . . O9 O 0.2609(2) 0.5655(3) 0.3760(2) 0.0469(6) Uani 1 1 d . . . O4 O 0.6741(3) 0.9187(2) 0.7993(2) 0.0529(7) Uani 1 1 d . . . O5 O 0.7883(3) 0.9836(2) 0.6719(2) 0.0596(8) Uani 1 1 d . . . N2 N 0.8305(3) 0.7796(3) 0.5296(2) 0.0406(7) Uani 1 1 d . . . C30 C 0.1977(3) 0.5821(3) 0.4385(3) 0.0425(8) Uani 1 1 d . . . N1 N 0.8974(3) 0.8049(3) 0.7393(3) 0.0471(8) Uani 1 1 d . . . C5 C 0.7244(3) 0.7255(3) 0.8498(3) 0.0397(8) Uani 1 1 d . . . C23 C 0.6376(3) 0.5471(3) 0.2430(3) 0.0423(8) Uani 1 1 d . . . C25 C 0.4655(4) 0.6001(3) 0.1759(3) 0.0447(9) Uani 1 1 d . . . C4 C 0.8538(3) 0.7948(3) 0.8973(3) 0.0457(9) Uani 1 1 d . . . C27 C 0.3993(4) 0.7605(4) 0.7410(3) 0.0517(10) Uani 1 1 d . . . H27A H 0.4611 0.7410 0.7779 0.078 Uiso 1 1 calc R . . H27B H 0.3263 0.7370 0.7590 0.078 Uiso 1 1 calc R . . H27C H 0.4298 0.8480 0.7639 0.078 Uiso 1 1 calc R . . C2 C 0.9355(3) 0.7510(4) 0.5674(3) 0.0499(10) Uani 1 1 d . . . H2A H 0.9956 0.7704 0.5333 0.060 Uiso 1 1 calc R . . H2B H 0.9084 0.6633 0.5470 0.060 Uiso 1 1 calc R . . C10 C 0.8326(3) 0.8254(3) 0.4636(3) 0.0460(9) Uani 1 1 d . . . H10A H 0.8998 0.8332 0.4394 0.055 Uiso 1 1 calc R . . C24 C 0.5748(4) 0.5843(4) 0.1759(3) 0.0480(9) Uani 1 1 d . . . H24A H 0.6094 0.5999 0.1266 0.058 Uiso 1 1 calc R . . C12 C 0.6231(4) 0.8364(3) 0.4300(3) 0.0430(9) Uani 1 1 d . . . C29 C 0.2449(3) 0.6366(4) 0.5527(3) 0.0448(9) Uani 1 1 d . . . H29A H 0.1875 0.6369 0.5886 0.054 Uiso 1 1 calc R . . C11 C 0.7423(4) 0.8669(3) 0.4219(3) 0.0462(9) Uani 1 1 d . . . C6 C 0.6599(4) 0.7165(4) 0.9212(3) 0.0515(10) Uani 1 1 d . . . H6A H 0.5751 0.6716 0.8924 0.062 Uiso 1 1 calc R . . C3 C 0.9317(4) 0.8122(4) 0.8343(3) 0.0539(10) Uani 1 1 d . . . H3A H 1.0149 0.8304 0.8659 0.065 Uiso 1 1 calc R . . C19 C 0.7677(4) 1.1211(4) 0.8279(3) 0.0600(11) Uani 1 1 d . . . H19A H 0.7865 1.2043 0.8733 0.072 Uiso 1 1 calc R . . C18 C 0.8025(4) 1.0909(3) 0.7364(4) 0.0559(11) Uani 1 1 d . . . C31 C 0.0618(3) 0.5409(4) 0.3831(3) 0.0598(11) Uani 1 1 d . . . H31A H 0.0482 0.5895 0.3468 0.090 Uiso 1 1 calc R . . H31B H 0.0217 0.5520 0.4368 0.090 Uiso 1 1 calc R . . H31C H 0.0285 0.4549 0.3301 0.090 Uiso 1 1 calc R . . C22 C 0.7565(4) 0.5342(4) 0.2340(4) 0.0623(12) Uani 1 1 d . . . H22A H 0.8092 0.5528 0.3043 0.093 Uiso 1 1 calc R . . H22B H 0.7967 0.5908 0.2098 0.093 Uiso 1 1 calc R . . H22C H 0.7395 0.4508 0.1820 0.093 Uiso 1 1 calc R . . C1 C 0.9928(3) 0.8262(4) 0.6899(3) 0.0593(11) Uani 1 1 d . . . H1A H 1.0577 0.8022 0.7169 0.071 Uiso 1 1 calc R . . H1B H 1.0289 0.9136 0.7098 0.071 Uiso 1 1 calc R . . C9 C 0.9112(4) 0.8465(4) 1.0113(3) 0.0660(13) Uani 1 1 d . . . H9A H 0.9965 0.8883 1.0416 0.079 Uiso 1 1 calc R . . C16 C 0.7752(4) 0.9426(4) 0.3721(4) 0.0660(13) Uani 1 1 d . . . H16A H 0.8521 0.9602 0.3638 0.079 Uiso 1 1 calc R . . C13 C 0.5464(4) 0.8865(4) 0.3917(4) 0.0637(12) Uani 1 1 d . . . H13A H 0.4681 0.8681 0.3971 0.076 Uiso 1 1 calc R . . C20 C 0.7060(4) 1.0338(4) 0.8557(3) 0.0498(9) Uani 1 1 d . . . C8 C 0.8459(5) 0.8374(4) 1.0790(3) 0.0723(14) Uani 1 1 d . . . H8A H 0.8859 0.8740 1.1544 0.087 Uiso 1 1 calc R . . C26 C 0.4089(5) 0.6424(5) 0.0975(4) 0.0716(14) Uani 1 1 d . . . H26A H 0.3315 0.5779 0.0453 0.107 Uiso 1 1 calc R . . H26B H 0.4637 0.6604 0.0594 0.107 Uiso 1 1 calc R . . H26C H 0.3956 0.7157 0.1381 0.107 Uiso 1 1 calc R . . C7 C 0.7195(5) 0.7730(4) 1.0340(3) 0.0646(13) Uani 1 1 d . . . H7A H 0.6740 0.7675 1.0795 0.077 Uiso 1 1 calc R . . C14 C 0.5836(5) 0.9640(5) 0.3452(4) 0.0790(16) Uani 1 1 d . . . H14A H 0.5307 0.9972 0.3207 0.095 Uiso 1 1 calc R . . C15 C 0.6982(5) 0.9907(5) 0.3358(5) 0.0870(18) Uani 1 1 d . . . H15A H 0.7232 1.0419 0.3046 0.104 Uiso 1 1 calc R . . C21 C 0.6737(5) 1.0740(5) 0.9584(4) 0.0912(18) Uani 1 1 d . . . H21A H 0.5858 1.0483 0.9391 0.137 Uiso 1 1 calc R . . H21B H 0.7121 1.1626 1.0006 0.137 Uiso 1 1 calc R . . H21C H 0.7025 1.0366 1.0009 0.137 Uiso 1 1 calc R . . C33 C 0.0035(7) 0.4183(6) 0.0939(5) 0.0923(18) Uani 1 1 d . . . C17 C 0.8657(6) 1.1936(4) 0.7107(5) 0.109(2) Uani 1 1 d . . . H17A H 0.8518 1.1597 0.6334 0.164 Uiso 1 1 calc R . . H17B H 0.9527 1.2292 0.7505 0.164 Uiso 1 1 calc R . . H17C H 0.8325 1.2566 0.7320 0.164 Uiso 1 1 calc R . . N3 N -0.0952(6) 0.3744(7) 0.0944(5) 0.143(3) Uani 1 1 d . . . C32 C 0.1216(5) 0.4730(6) 0.0957(5) 0.103(2) Uani 1 1 d . . . H32A H 0.1241 0.5350 0.0718 0.155 Uiso 1 1 calc R . . H32B H 0.1437 0.4109 0.0476 0.155 Uiso 1 1 calc R . . H32C H 0.1789 0.5108 0.1691 0.155 Uiso 1 1 calc R . . H3O H 0.668(5) 0.561(6) 0.490(5) 0.155 Uiso 1 1 d 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 Dy1 0.03205(8) 0.02972(8) 0.03153(8) 0.01734(7) 0.01545(7) 0.01054(6) Dy2 0.03906(9) 0.02664(8) 0.03491(9) 0.01487(7) 0.01689(7) 0.00827(6) C28 0.053(2) 0.0304(17) 0.044(2) 0.0210(15) 0.0282(18) 0.0193(15) O6 0.0415(13) 0.0478(14) 0.0396(13) 0.0243(12) 0.0224(11) 0.0205(11) O3 0.0345(12) 0.0296(11) 0.0324(12) 0.0175(10) 0.0171(10) 0.0098(9) O1 0.0407(13) 0.0338(12) 0.0290(12) 0.0146(10) 0.0113(10) 0.0066(10) O8 0.0387(13) 0.0341(12) 0.0425(13) 0.0183(11) 0.0230(11) 0.0148(10) O2 0.0460(14) 0.0346(13) 0.0421(13) 0.0236(11) 0.0206(11) 0.0122(10) O7 0.0486(15) 0.0509(15) 0.0399(13) 0.0286(12) 0.0217(12) 0.0235(12) O9 0.0428(14) 0.0662(18) 0.0485(15) 0.0332(14) 0.0245(12) 0.0287(13) O4 0.0671(18) 0.0360(14) 0.0491(15) 0.0145(12) 0.0276(14) 0.0128(13) O5 0.087(2) 0.0304(14) 0.0553(16) 0.0171(13) 0.0348(16) 0.0103(14) N2 0.0442(17) 0.0332(15) 0.0439(17) 0.0169(13) 0.0223(14) 0.0102(13) C30 0.041(2) 0.049(2) 0.057(2) 0.0328(19) 0.0264(18) 0.0242(17) N1 0.0397(17) 0.0514(19) 0.0458(18) 0.0228(15) 0.0179(15) 0.0085(14) C5 0.050(2) 0.0314(18) 0.0372(19) 0.0172(15) 0.0145(17) 0.0129(15) C23 0.047(2) 0.0394(19) 0.0410(19) 0.0170(16) 0.0244(17) 0.0120(16) C25 0.059(2) 0.046(2) 0.0359(19) 0.0233(17) 0.0191(18) 0.0211(18) C4 0.046(2) 0.043(2) 0.040(2) 0.0210(17) 0.0089(17) 0.0073(17) C27 0.057(2) 0.051(2) 0.049(2) 0.0198(19) 0.028(2) 0.0218(19) C2 0.045(2) 0.048(2) 0.063(3) 0.028(2) 0.026(2) 0.0175(18) C10 0.050(2) 0.040(2) 0.046(2) 0.0195(17) 0.0284(18) 0.0075(17) C24 0.060(2) 0.055(2) 0.051(2) 0.037(2) 0.034(2) 0.024(2) C12 0.057(2) 0.0300(18) 0.043(2) 0.0216(16) 0.0173(18) 0.0112(16) C29 0.042(2) 0.054(2) 0.053(2) 0.0279(19) 0.0316(18) 0.0220(17) C11 0.057(2) 0.038(2) 0.045(2) 0.0239(17) 0.0224(19) 0.0095(17) C6 0.066(3) 0.042(2) 0.043(2) 0.0202(18) 0.025(2) 0.0100(19) C3 0.040(2) 0.055(2) 0.054(2) 0.023(2) 0.0092(19) 0.0085(18) C19 0.075(3) 0.034(2) 0.062(3) 0.0111(19) 0.029(2) 0.020(2) C18 0.068(3) 0.031(2) 0.063(3) 0.0209(19) 0.024(2) 0.0100(18) C31 0.042(2) 0.087(3) 0.064(3) 0.040(3) 0.025(2) 0.031(2) C22 0.056(3) 0.081(3) 0.070(3) 0.040(3) 0.041(2) 0.033(2) C1 0.035(2) 0.072(3) 0.065(3) 0.032(2) 0.019(2) 0.0102(19) C9 0.062(3) 0.064(3) 0.047(2) 0.026(2) 0.001(2) 0.002(2) C16 0.072(3) 0.063(3) 0.071(3) 0.047(3) 0.031(3) 0.009(2) C13 0.074(3) 0.051(3) 0.073(3) 0.038(2) 0.032(3) 0.016(2) C20 0.049(2) 0.044(2) 0.042(2) 0.0093(18) 0.0138(18) 0.0159(18) C8 0.093(4) 0.065(3) 0.034(2) 0.018(2) 0.010(2) 0.010(3) C26 0.096(4) 0.101(4) 0.065(3) 0.062(3) 0.043(3) 0.059(3) C7 0.094(4) 0.050(3) 0.043(2) 0.020(2) 0.031(2) 0.014(2) C14 0.084(4) 0.077(3) 0.097(4) 0.069(3) 0.023(3) 0.026(3) C15 0.089(4) 0.093(4) 0.110(4) 0.086(4) 0.037(3) 0.019(3) C21 0.115(4) 0.061(3) 0.072(3) 0.006(3) 0.056(3) 0.018(3) C33 0.093(5) 0.084(4) 0.075(4) 0.017(3) 0.012(4) 0.039(4) C17 0.171(6) 0.040(3) 0.118(5) 0.039(3) 0.081(5) 0.017(3) N3 0.095(4) 0.145(6) 0.113(5) -0.002(4) 0.031(4) 0.033(4) C32 0.079(4) 0.113(5) 0.126(5) 0.069(5) 0.028(4) 0.037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O9 2.283(2) . ? Dy1 O7 2.310(2) . ? Dy1 O6 2.338(2) . ? Dy1 O3 2.370(2) . ? Dy1 O3 2.372(2) 2_666 ? Dy1 O2 2.400(2) . ? Dy1 O1 2.422(2) 2_666 ? Dy1 O8 2.564(2) . ? Dy1 Dy2 3.6004(3) . ? Dy1 Dy1 3.8638(3) 2_666 ? Dy1 Dy2 3.8736(3) 2_666 ? Dy2 O4 2.279(3) . ? Dy2 O3 2.313(2) . ? Dy2 O5 2.313(2) . ? Dy2 O2 2.328(2) . ? Dy2 O1 2.372(2) . ? Dy2 N1 2.499(3) . ? Dy2 O8 2.500(2) . ? Dy2 N2 2.556(3) . ? Dy2 Dy1 3.8736(3) 2_666 ? C28 O8 1.275(4) . ? C28 C29 1.396(5) . ? C28 C27 1.504(5) . ? O6 C23 1.277(4) . ? O3 Dy1 2.372(2) 2_666 ? O3 H3O 0.838(10) . ? O1 C5 1.326(4) . ? O1 Dy1 2.422(2) 2_666 ? O2 C12 1.333(4) . ? O7 C25 1.273(4) . ? O9 C30 1.265(4) . ? O4 C20 1.260(4) . ? O5 C18 1.250(5) . ? N2 C10 1.268(4) . ? N2 C2 1.457(5) . ? C30 C29 1.395(5) . ? C30 C31 1.501(5) . ? N1 C3 1.273(5) . ? N1 C1 1.468(5) . ? C5 C6 1.401(5) . ? C5 C4 1.421(5) . ? C23 C24 1.387(5) . ? C23 C22 1.502(5) . ? C25 C24 1.378(5) . ? C25 C26 1.519(5) . ? C4 C9 1.407(5) . ? C4 C3 1.438(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C2 C1 1.502(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C10 C11 1.441(6) . ? C10 H10A 0.9300 . ? C24 H24A 0.9300 . ? C12 C13 1.383(6) . ? C12 C11 1.415(5) . ? C29 H29A 0.9300 . ? C11 C16 1.405(5) . ? C6 C7 1.390(5) . ? C6 H6A 0.9300 . ? C3 H3A 0.9300 . ? C19 C18 1.377(6) . ? C19 C20 1.384(6) . ? C19 H19A 0.9300 . ? C18 C17 1.524(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C9 C8 1.364(6) . ? C9 H9A 0.9300 . ? C16 C15 1.354(7) . ? C16 H16A 0.9300 . ? C13 C14 1.397(6) . ? C13 H13A 0.9300 . ? C20 C21 1.502(6) . ? C8 C7 1.382(6) . ? C8 H8A 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C7 H7A 0.9300 . ? C14 C15 1.369(7) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C33 N3 1.165(8) . ? C33 C32 1.387(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 Dy1 O7 77.76(8) . . ? O9 Dy1 O6 150.55(8) . . ? O7 Dy1 O6 73.79(8) . . ? O9 Dy1 O3 138.23(8) . . ? O7 Dy1 O3 138.66(7) . . ? O6 Dy1 O3 70.96(8) . . ? O9 Dy1 O3 83.04(8) . 2_666 ? O7 Dy1 O3 147.51(8) . 2_666 ? O6 Dy1 O3 118.10(8) . 2_666 ? O3 Dy1 O3 70.88(8) . 2_666 ? O9 Dy1 O2 101.02(9) . . ? O7 Dy1 O2 81.10(8) . . ? O6 Dy1 O2 82.08(8) . . ? O3 Dy1 O2 73.37(8) . . ? O3 Dy1 O2 128.63(7) 2_666 . ? O9 Dy1 O1 86.98(9) . 2_666 ? O7 Dy1 O1 84.92(8) . 2_666 ? O6 Dy1 O1 83.12(8) . 2_666 ? O3 Dy1 O1 111.20(8) . 2_666 ? O3 Dy1 O1 68.00(7) 2_666 2_666 ? O2 Dy1 O1 161.97(7) . 2_666 ? O9 Dy1 O8 72.24(8) . . ? O7 Dy1 O8 126.88(8) . . ? O6 Dy1 O8 132.39(8) . . ? O3 Dy1 O8 68.37(7) . . ? O3 Dy1 O8 69.61(7) 2_666 . ? O2 Dy1 O8 63.50(7) . . ? O1 Dy1 O8 134.52(7) 2_666 . ? O9 Dy1 Dy2 112.72(7) . . ? O7 Dy1 Dy2 120.37(6) . . ? O6 Dy1 Dy2 88.52(6) . . ? O3 Dy1 Dy2 39.17(5) . . ? O3 Dy1 Dy2 91.15(5) 2_666 . ? O2 Dy1 Dy2 39.67(5) . . ? O1 Dy1 Dy2 149.91(5) 2_666 . ? O8 Dy1 Dy2 43.97(5) . . ? O9 Dy1 Dy1 112.52(6) . 2_666 ? O7 Dy1 Dy1 168.09(6) . 2_666 ? O6 Dy1 Dy1 95.11(6) . 2_666 ? O3 Dy1 Dy1 35.46(5) . 2_666 ? O3 Dy1 Dy1 35.42(5) 2_666 2_666 ? O2 Dy1 Dy1 101.99(5) . 2_666 ? O1 Dy1 Dy1 89.53(5) 2_666 2_666 ? O8 Dy1 Dy1 63.89(5) . 2_666 ? Dy2 Dy1 Dy1 62.407(6) . 2_666 ? O9 Dy1 Dy2 91.33(7) . 2_666 ? O7 Dy1 Dy2 120.41(6) . 2_666 ? O6 Dy1 Dy2 96.48(6) . 2_666 ? O3 Dy1 Dy2 84.73(5) . 2_666 ? O3 Dy1 Dy2 33.74(5) 2_666 2_666 ? O2 Dy1 Dy2 157.32(5) . 2_666 ? O1 Dy1 Dy2 35.67(5) 2_666 2_666 ? O8 Dy1 Dy2 103.30(5) . 2_666 ? Dy2 Dy1 Dy2 117.869(5) . 2_666 ? Dy1 Dy1 Dy2 55.462(4) 2_666 2_666 ? O4 Dy2 O3 141.91(8) . . ? O4 Dy2 O5 71.69(9) . . ? O3 Dy2 O5 146.18(8) . . ? O4 Dy2 O2 120.58(9) . . ? O3 Dy2 O2 75.76(8) . . ? O5 Dy2 O2 81.72(9) . . ? O4 Dy2 O1 77.63(9) . . ? O3 Dy2 O1 69.81(7) . . ? O5 Dy2 O1 139.63(9) . . ? O2 Dy2 O1 137.57(8) . . ? O4 Dy2 N1 92.88(10) . . ? O3 Dy2 N1 95.01(9) . . ? O5 Dy2 N1 84.30(11) . . ? O2 Dy2 N1 136.71(9) . . ? O1 Dy2 N1 71.52(9) . . ? O4 Dy2 O8 85.18(9) . . ? O3 Dy2 O8 70.35(7) . . ? O5 Dy2 O8 121.95(10) . . ? O2 Dy2 O8 65.51(7) . . ? O1 Dy2 O8 79.85(8) . . ? N1 Dy2 O8 151.01(9) . . ? O4 Dy2 N2 138.74(9) . . ? O3 Dy2 N2 77.62(8) . . ? O5 Dy2 N2 71.21(9) . . ? O2 Dy2 N2 70.61(9) . . ? O1 Dy2 N2 122.95(9) . . ? N1 Dy2 N2 66.10(10) . . ? O8 Dy2 N2 130.40(8) . . ? O4 Dy2 Dy1 129.99(7) . . ? O3 Dy2 Dy1 40.33(6) . . ? O5 Dy2 Dy1 122.87(7) . . ? O2 Dy2 Dy1 41.16(5) . . ? O1 Dy2 Dy1 96.90(5) . . ? N1 Dy2 Dy1 133.01(8) . . ? O8 Dy2 Dy1 45.41(5) . . ? N2 Dy2 Dy1 86.00(7) . . ? O4 Dy2 Dy1 108.38(6) . 2_666 ? O3 Dy2 Dy1 34.73(5) . 2_666 ? O5 Dy2 Dy1 173.75(8) . 2_666 ? O2 Dy2 Dy1 103.20(5) . 2_666 ? O1 Dy2 Dy1 36.54(5) . 2_666 ? N1 Dy2 Dy1 89.46(7) . 2_666 ? O8 Dy2 Dy1 64.06(5) . 2_666 ? N2 Dy2 Dy1 106.54(6) . 2_666 ? Dy1 Dy2 Dy1 62.131(5) . 2_666 ? O8 C28 C29 124.1(3) . . ? O8 C28 C27 118.2(3) . . ? C29 C28 C27 117.7(3) . . ? C23 O6 Dy1 134.3(2) . . ? Dy2 O3 Dy1 100.49(8) . . ? Dy2 O3 Dy1 111.52(8) . 2_666 ? Dy1 O3 Dy1 109.12(8) . 2_666 ? Dy2 O3 H3O 110(5) . . ? Dy1 O3 H3O 102(4) . . ? Dy1 O3 H3O 121(5) 2_666 . ? C5 O1 Dy2 119.78(19) . . ? C5 O1 Dy1 132.1(2) . 2_666 ? Dy2 O1 Dy1 107.79(8) . 2_666 ? C28 O8 Dy2 141.0(2) . . ? C28 O8 Dy1 128.4(2) . . ? Dy2 O8 Dy1 90.62(7) . . ? C12 O2 Dy2 125.5(2) . . ? C12 O2 Dy1 131.8(2) . . ? Dy2 O2 Dy1 99.17(8) . . ? C25 O7 Dy1 135.0(2) . . ? C30 O9 Dy1 135.5(2) . . ? C20 O4 Dy2 139.0(3) . . ? C18 O5 Dy2 137.2(3) . . ? C10 N2 C2 118.4(3) . . ? C10 N2 Dy2 125.2(3) . . ? C2 N2 Dy2 114.3(2) . . ? O9 C30 C29 125.2(3) . . ? O9 C30 C31 116.0(3) . . ? C29 C30 C31 118.8(3) . . ? C3 N1 C1 117.0(3) . . ? C3 N1 Dy2 124.7(3) . . ? C1 N1 Dy2 117.8(2) . . ? O1 C5 C6 121.0(3) . . ? O1 C5 C4 121.6(3) . . ? C6 C5 C4 117.4(3) . . ? O6 C23 C24 124.2(3) . . ? O6 C23 C22 116.1(3) . . ? C24 C23 C22 119.7(3) . . ? O7 C25 C24 125.1(3) . . ? O7 C25 C26 115.8(4) . . ? C24 C25 C26 119.1(3) . . ? C9 C4 C5 119.2(4) . . ? C9 C4 C3 117.3(4) . . ? C5 C4 C3 123.5(3) . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N2 C2 C1 109.1(3) . . ? N2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? N2 C10 C11 127.1(3) . . ? N2 C10 H10A 116.5 . . ? C11 C10 H10A 116.5 . . ? C25 C24 C23 125.6(3) . . ? C25 C24 H24A 117.2 . . ? C23 C24 H24A 117.2 . . ? O2 C12 C13 119.8(4) . . ? O2 C12 C11 122.2(3) . . ? C13 C12 C11 118.0(3) . . ? C30 C29 C28 127.0(3) . . ? C30 C29 H29A 116.5 . . ? C28 C29 H29A 116.5 . . ? C16 C11 C12 118.6(4) . . ? C16 C11 C10 118.2(4) . . ? C12 C11 C10 123.2(3) . . ? C7 C6 C5 121.6(4) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? N1 C3 C4 126.1(4) . . ? N1 C3 H3A 116.9 . . ? C4 C3 H3A 116.9 . . ? C18 C19 C20 123.3(4) . . ? C18 C19 H19A 118.3 . . ? C20 C19 H19A 118.3 . . ? O5 C18 C19 124.7(4) . . ? O5 C18 C17 116.0(4) . . ? C19 C18 C17 119.3(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C1 C2 109.0(3) . . ? N1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? N1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C8 C9 C4 122.1(4) . . ? C8 C9 H9A 118.9 . . ? C4 C9 H9A 118.9 . . ? C15 C16 C11 122.0(4) . . ? C15 C16 H16A 119.0 . . ? C11 C16 H16A 119.0 . . ? C12 C13 C14 121.7(4) . . ? C12 C13 H13A 119.2 . . ? C14 C13 H13A 119.2 . . ? O4 C20 C19 123.7(4) . . ? O4 C20 C21 116.0(4) . . ? C19 C20 C21 120.3(4) . . ? C9 C8 C7 119.1(4) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C15 C14 C13 119.7(5) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 119.9(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C33 C32 178.6(8) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 Dy1 Dy2 O4 13.20(11) . . . . ? O7 Dy1 Dy2 O4 101.99(11) . . . . ? O6 Dy1 Dy2 O4 172.19(10) . . . . ? O3 Dy1 Dy2 O4 -126.82(11) . . . . ? O3 Dy1 Dy2 O4 -69.73(10) 2_666 . . . ? O2 Dy1 Dy2 O4 92.83(12) . . . . ? O1 Dy1 Dy2 O4 -114.28(14) 2_666 . . . ? O8 Dy1 Dy2 O4 -11.25(11) . . . . ? Dy1 Dy1 Dy2 O4 -91.26(9) 2_666 . . . ? Dy2 Dy1 Dy2 O4 -91.26(9) 2_666 . . . ? O9 Dy1 Dy2 O3 140.02(10) . . . . ? O7 Dy1 Dy2 O3 -131.19(10) . . . . ? O6 Dy1 Dy2 O3 -60.99(9) . . . . ? O3 Dy1 Dy2 O3 57.09(11) 2_666 . . . ? O2 Dy1 Dy2 O3 -140.35(12) . . . . ? O1 Dy1 Dy2 O3 12.54(12) 2_666 . . . ? O8 Dy1 Dy2 O3 115.57(10) . . . . ? Dy1 Dy1 Dy2 O3 35.56(7) 2_666 . . . ? Dy2 Dy1 Dy2 O3 35.56(7) 2_666 . . . ? O9 Dy1 Dy2 O5 -79.88(11) . . . . ? O7 Dy1 Dy2 O5 8.90(11) . . . . ? O6 Dy1 Dy2 O5 79.10(11) . . . . ? O3 Dy1 Dy2 O5 140.10(12) . . . . ? O3 Dy1 Dy2 O5 -162.82(10) 2_666 . . . ? O2 Dy1 Dy2 O5 -0.25(12) . . . . ? O1 Dy1 Dy2 O5 152.63(14) 2_666 . . . ? O8 Dy1 Dy2 O5 -104.33(11) . . . . ? Dy1 Dy1 Dy2 O5 175.65(9) 2_666 . . . ? Dy2 Dy1 Dy2 O5 175.65(9) 2_666 . . . ? O9 Dy1 Dy2 O2 -79.63(11) . . . . ? O7 Dy1 Dy2 O2 9.16(11) . . . . ? O6 Dy1 Dy2 O2 79.36(11) . . . . ? O3 Dy1 Dy2 O2 140.35(12) . . . . ? O3 Dy1 Dy2 O2 -162.56(10) 2_666 . . . ? O1 Dy1 Dy2 O2 152.89(14) 2_666 . . . ? O8 Dy1 Dy2 O2 -104.08(11) . . . . ? Dy1 Dy1 Dy2 O2 175.91(9) 2_666 . . . ? Dy2 Dy1 Dy2 O2 175.91(9) 2_666 . . . ? O9 Dy1 Dy2 O1 92.83(9) . . . . ? O7 Dy1 Dy2 O1 -178.38(9) . . . . ? O6 Dy1 Dy2 O1 -108.18(8) . . . . ? O3 Dy1 Dy2 O1 -47.19(10) . . . . ? O3 Dy1 Dy2 O1 9.90(8) 2_666 . . . ? O2 Dy1 Dy2 O1 172.46(11) . . . . ? O1 Dy1 Dy2 O1 -34.66(16) 2_666 . . . ? O8 Dy1 Dy2 O1 68.38(9) . . . . ? Dy1 Dy1 Dy2 O1 -11.63(6) 2_666 . . . ? Dy2 Dy1 Dy2 O1 -11.63(6) 2_666 . . . ? O9 Dy1 Dy2 N1 163.93(11) . . . . ? O7 Dy1 Dy2 N1 -107.28(12) . . . . ? O6 Dy1 Dy2 N1 -37.08(11) . . . . ? O3 Dy1 Dy2 N1 23.91(12) . . . . ? O3 Dy1 Dy2 N1 81.00(11) 2_666 . . . ? O2 Dy1 Dy2 N1 -116.44(13) . . . . ? O1 Dy1 Dy2 N1 36.45(14) 2_666 . . . ? O8 Dy1 Dy2 N1 139.48(12) . . . . ? Dy1 Dy1 Dy2 N1 59.47(9) 2_666 . . . ? Dy2 Dy1 Dy2 N1 59.47(9) 2_666 . . . ? O9 Dy1 Dy2 O8 24.45(10) . . . . ? O7 Dy1 Dy2 O8 113.24(10) . . . . ? O6 Dy1 Dy2 O8 -176.56(9) . . . . ? O3 Dy1 Dy2 O8 -115.57(10) . . . . ? O3 Dy1 Dy2 O8 -58.48(9) 2_666 . . . ? O2 Dy1 Dy2 O8 104.08(11) . . . . ? O1 Dy1 Dy2 O8 -103.03(13) 2_666 . . . ? Dy1 Dy1 Dy2 O8 -80.01(7) 2_666 . . . ? Dy2 Dy1 Dy2 O8 -80.01(7) 2_666 . . . ? O9 Dy1 Dy2 N2 -144.44(10) . . . . ? O7 Dy1 Dy2 N2 -55.65(10) . . . . ? O6 Dy1 Dy2 N2 14.55(9) . . . . ? O3 Dy1 Dy2 N2 75.54(10) . . . . ? O3 Dy1 Dy2 N2 132.63(9) 2_666 . . . ? O2 Dy1 Dy2 N2 -64.81(11) . . . . ? O1 Dy1 Dy2 N2 88.07(12) 2_666 . . . ? O8 Dy1 Dy2 N2 -168.89(10) . . . . ? Dy1 Dy1 Dy2 N2 111.10(7) 2_666 . . . ? Dy2 Dy1 Dy2 N2 111.10(7) 2_666 . . . ? O9 Dy1 Dy2 Dy1 104.46(7) . . . 2_666 ? O7 Dy1 Dy2 Dy1 -166.75(7) . . . 2_666 ? O6 Dy1 Dy2 Dy1 -96.55(6) . . . 2_666 ? O3 Dy1 Dy2 Dy1 -35.56(7) . . . 2_666 ? O3 Dy1 Dy2 Dy1 21.53(5) 2_666 . . 2_666 ? O2 Dy1 Dy2 Dy1 -175.91(9) . . . 2_666 ? O1 Dy1 Dy2 Dy1 -23.02(10) 2_666 . . 2_666 ? O8 Dy1 Dy2 Dy1 80.01(7) . . . 2_666 ? Dy2 Dy1 Dy2 Dy1 0.0 2_666 . . 2_666 ? O9 Dy1 O6 C23 30.1(4) . . . . ? O7 Dy1 O6 C23 14.7(3) . . . . ? O3 Dy1 O6 C23 -143.4(3) . . . . ? O3 Dy1 O6 C23 161.9(3) 2_666 . . . ? O2 Dy1 O6 C23 -68.3(3) . . . . ? O1 Dy1 O6 C23 101.4(3) 2_666 . . . ? O8 Dy1 O6 C23 -110.8(3) . . . . ? Dy2 Dy1 O6 C23 -107.6(3) . . . . ? Dy1 Dy1 O6 C23 -169.7(3) 2_666 . . . ? Dy2 Dy1 O6 C23 134.5(3) 2_666 . . . ? O4 Dy2 O3 Dy1 96.13(15) . . . . ? O5 Dy2 O3 Dy1 -75.45(18) . . . . ? O2 Dy2 O3 Dy1 -25.68(8) . . . . ? O1 Dy2 O3 Dy1 129.10(9) . . . . ? N1 Dy2 O3 Dy1 -162.69(9) . . . . ? O8 Dy2 O3 Dy1 43.01(7) . . . . ? N2 Dy2 O3 Dy1 -98.52(9) . . . . ? Dy1 Dy2 O3 Dy1 115.54(11) 2_666 . . . ? O4 Dy2 O3 Dy1 -19.41(19) . . . 2_666 ? O5 Dy2 O3 Dy1 169.01(14) . . . 2_666 ? O2 Dy2 O3 Dy1 -141.22(10) . . . 2_666 ? O1 Dy2 O3 Dy1 13.56(8) . . . 2_666 ? N1 Dy2 O3 Dy1 81.76(10) . . . 2_666 ? O8 Dy2 O3 Dy1 -72.54(9) . . . 2_666 ? N2 Dy2 O3 Dy1 145.93(11) . . . 2_666 ? Dy1 Dy2 O3 Dy1 -115.54(11) . . . 2_666 ? O9 Dy1 O3 Dy2 -62.84(14) . . . . ? O7 Dy1 O3 Dy2 79.43(13) . . . . ? O6 Dy1 O3 Dy2 112.35(9) . . . . ? O3 Dy1 O3 Dy2 -117.33(11) 2_666 . . . ? O2 Dy1 O3 Dy2 25.16(7) . . . . ? O1 Dy1 O3 Dy2 -173.30(6) 2_666 . . . ? O8 Dy1 O3 Dy2 -42.36(7) . . . . ? Dy1 Dy1 O3 Dy2 -117.33(11) 2_666 . . . ? Dy2 Dy1 O3 Dy2 -148.92(6) 2_666 . . . ? O9 Dy1 O3 Dy1 54.49(16) . . . 2_666 ? O7 Dy1 O3 Dy1 -163.24(10) . . . 2_666 ? O6 Dy1 O3 Dy1 -130.32(11) . . . 2_666 ? O3 Dy1 O3 Dy1 0.0 2_666 . . 2_666 ? O2 Dy1 O3 Dy1 142.49(10) . . . 2_666 ? O1 Dy1 O3 Dy1 -55.97(10) 2_666 . . 2_666 ? O8 Dy1 O3 Dy1 74.97(9) . . . 2_666 ? Dy2 Dy1 O3 Dy1 117.33(11) . . . 2_666 ? Dy2 Dy1 O3 Dy1 -31.59(7) 2_666 . . 2_666 ? O4 Dy2 O1 C5 -39.3(2) . . . . ? O3 Dy2 O1 C5 160.8(3) . . . . ? O5 Dy2 O1 C5 1.7(3) . . . . ? O2 Dy2 O1 C5 -161.5(2) . . . . ? N1 Dy2 O1 C5 58.0(3) . . . . ? O8 Dy2 O1 C5 -126.5(3) . . . . ? N2 Dy2 O1 C5 101.5(3) . . . . ? Dy1 Dy2 O1 C5 -168.8(2) . . . . ? Dy1 Dy2 O1 C5 173.8(3) 2_666 . . . ? O4 Dy2 O1 Dy1 146.93(11) . . . 2_666 ? O3 Dy2 O1 Dy1 -12.97(8) . . . 2_666 ? O5 Dy2 O1 Dy1 -172.04(12) . . . 2_666 ? O2 Dy2 O1 Dy1 24.78(16) . . . 2_666 ? N1 Dy2 O1 Dy1 -115.74(12) . . . 2_666 ? O8 Dy2 O1 Dy1 59.69(9) . . . 2_666 ? N2 Dy2 O1 Dy1 -72.27(12) . . . 2_666 ? Dy1 Dy2 O1 Dy1 17.42(8) . . . 2_666 ? C29 C28 O8 Dy2 166.3(3) . . . . ? C27 C28 O8 Dy2 -12.5(5) . . . . ? C29 C28 O8 Dy1 -13.5(5) . . . . ? C27 C28 O8 Dy1 167.8(2) . . . . ? O4 Dy2 O8 C28 -8.4(3) . . . . ? O3 Dy2 O8 C28 141.9(3) . . . . ? O5 Dy2 O8 C28 -73.3(3) . . . . ? O2 Dy2 O8 C28 -135.3(3) . . . . ? O1 Dy2 O8 C28 69.8(3) . . . . ? N1 Dy2 O8 C28 78.8(4) . . . . ? N2 Dy2 O8 C28 -165.2(3) . . . . ? Dy1 Dy2 O8 C28 -179.8(4) . . . . ? Dy1 Dy2 O8 C28 104.7(3) 2_666 . . . ? O4 Dy2 O8 Dy1 171.37(8) . . . . ? O3 Dy2 O8 Dy1 -38.31(7) . . . . ? O5 Dy2 O8 Dy1 106.47(9) . . . . ? O2 Dy2 O8 Dy1 44.54(7) . . . . ? O1 Dy2 O8 Dy1 -110.35(8) . . . . ? N1 Dy2 O8 Dy1 -101.37(18) . . . . ? N2 Dy2 O8 Dy1 14.62(13) . . . . ? Dy1 Dy2 O8 Dy1 -75.50(5) 2_666 . . . ? O9 Dy1 O8 C28 23.5(3) . . . . ? O7 Dy1 O8 C28 82.2(3) . . . . ? O6 Dy1 O8 C28 -175.5(2) . . . . ? O3 Dy1 O8 C28 -142.3(3) . . . . ? O3 Dy1 O8 C28 -65.6(3) 2_666 . . . ? O2 Dy1 O8 C28 136.1(3) . . . . ? O1 Dy1 O8 C28 -43.4(3) 2_666 . . . ? Dy2 Dy1 O8 C28 179.9(3) . . . . ? Dy1 Dy1 O8 C28 -103.7(3) 2_666 . . . ? Dy2 Dy1 O8 C28 -63.6(3) 2_666 . . . ? O9 Dy1 O8 Dy2 -156.36(10) . . . . ? O7 Dy1 O8 Dy2 -97.61(10) . . . . ? O6 Dy1 O8 Dy2 4.66(12) . . . . ? O3 Dy1 O8 Dy2 37.81(6) . . . . ? O3 Dy1 O8 Dy2 114.59(8) 2_666 . . . ? O2 Dy1 O8 Dy2 -43.78(7) . . . . ? O1 Dy1 O8 Dy2 136.75(9) 2_666 . . . ? Dy1 Dy1 O8 Dy2 76.41(5) 2_666 . . . ? Dy2 Dy1 O8 Dy2 116.54(5) 2_666 . . . ? O4 Dy2 O2 C12 81.9(3) . . . . ? O3 Dy2 O2 C12 -135.6(3) . . . . ? O5 Dy2 O2 C12 18.9(3) . . . . ? O1 Dy2 O2 C12 -172.0(2) . . . . ? N1 Dy2 O2 C12 -53.6(3) . . . . ? O8 Dy2 O2 C12 149.8(3) . . . . ? N2 Dy2 O2 C12 -54.0(3) . . . . ? Dy1 Dy2 O2 C12 -160.9(3) . . . . ? Dy1 Dy2 O2 C12 -157.1(3) 2_666 . . . ? O4 Dy2 O2 Dy1 -117.27(9) . . . . ? O3 Dy2 O2 Dy1 25.22(8) . . . . ? O5 Dy2 O2 Dy1 179.79(10) . . . . ? O1 Dy2 O2 Dy1 -11.13(16) . . . . ? N1 Dy2 O2 Dy1 107.29(13) . . . . ? O8 Dy2 O2 Dy1 -49.38(8) . . . . ? N2 Dy2 O2 Dy1 106.87(10) . . . . ? Dy1 Dy2 O2 Dy1 3.72(8) 2_666 . . . ? O9 Dy1 O2 C12 -88.6(3) . . . . ? O7 Dy1 O2 C12 -13.0(3) . . . . ? O6 Dy1 O2 C12 61.7(3) . . . . ? O3 Dy1 O2 C12 134.1(3) . . . . ? O3 Dy1 O2 C12 -178.4(3) 2_666 . . . ? O1 Dy1 O2 C12 26.6(5) 2_666 . . . ? O8 Dy1 O2 C12 -152.2(3) . . . . ? Dy2 Dy1 O2 C12 159.0(4) . . . . ? Dy1 Dy1 O2 C12 155.3(3) 2_666 . . . ? Dy2 Dy1 O2 C12 149.6(3) 2_666 . . . ? O9 Dy1 O2 Dy2 112.42(9) . . . . ? O7 Dy1 O2 Dy2 -172.01(10) . . . . ? O6 Dy1 O2 Dy2 -97.29(9) . . . . ? O3 Dy1 O2 Dy2 -24.88(8) . . . . ? O3 Dy1 O2 Dy2 22.55(13) 2_666 . . . ? O1 Dy1 O2 Dy2 -132.4(2) 2_666 . . . ? O8 Dy1 O2 Dy2 48.80(8) . . . . ? Dy1 Dy1 O2 Dy2 -3.71(8) 2_666 . . . ? Dy2 Dy1 O2 Dy2 -9.4(2) 2_666 . . . ? O9 Dy1 O7 C25 174.3(3) . . . . ? O6 Dy1 O7 C25 -13.4(3) . . . . ? O3 Dy1 O7 C25 19.0(4) . . . . ? O3 Dy1 O7 C25 -130.5(3) 2_666 . . . ? O2 Dy1 O7 C25 70.9(3) . . . . ? O1 Dy1 O7 C25 -97.7(3) 2_666 . . . ? O8 Dy1 O7 C25 117.9(3) . . . . ? Dy2 Dy1 O7 C25 65.0(3) . . . . ? Dy1 Dy1 O7 C25 -35.2(5) 2_666 . . . ? Dy2 Dy1 O7 C25 -101.4(3) 2_666 . . . ? O7 Dy1 O9 C30 -164.7(4) . . . . ? O6 Dy1 O9 C30 -179.8(3) . . . . ? O3 Dy1 O9 C30 -9.1(4) . . . . ? O3 Dy1 O9 C30 41.7(3) 2_666 . . . ? O2 Dy1 O9 C30 -86.4(3) . . . . ? O1 Dy1 O9 C30 109.9(3) 2_666 . . . ? O8 Dy1 O9 C30 -29.1(3) . . . . ? Dy2 Dy1 O9 C30 -46.6(4) . . . . ? Dy1 Dy1 O9 C30 21.6(4) 2_666 . . . ? Dy2 Dy1 O9 C30 74.5(3) 2_666 . . . ? O3 Dy2 O4 C20 -173.2(4) . . . . ? O5 Dy2 O4 C20 1.9(4) . . . . ? O2 Dy2 O4 C20 -66.3(4) . . . . ? O1 Dy2 O4 C20 155.3(4) . . . . ? N1 Dy2 O4 C20 84.9(4) . . . . ? O8 Dy2 O4 C20 -124.1(4) . . . . ? N2 Dy2 O4 C20 28.8(5) . . . . ? Dy1 Dy2 O4 C20 -116.1(4) . . . . ? Dy1 Dy2 O4 C20 175.3(4) 2_666 . . . ? O4 Dy2 O5 C18 -7.3(4) . . . . ? O3 Dy2 O5 C18 167.3(4) . . . . ? O2 Dy2 O5 C18 118.9(4) . . . . ? O1 Dy2 O5 C18 -49.7(5) . . . . ? N1 Dy2 O5 C18 -102.2(4) . . . . ? O8 Dy2 O5 C18 64.6(4) . . . . ? N2 Dy2 O5 C18 -168.9(5) . . . . ? Dy1 Dy2 O5 C18 119.0(4) . . . . ? Dy1 Dy2 O5 C18 -98.9(7) 2_666 . . . ? O4 Dy2 N2 C10 -79.4(3) . . . . ? O3 Dy2 N2 C10 114.3(3) . . . . ? O5 Dy2 N2 C10 -52.4(3) . . . . ? O2 Dy2 N2 C10 35.2(3) . . . . ? O1 Dy2 N2 C10 170.0(3) . . . . ? N1 Dy2 N2 C10 -144.5(3) . . . . ? O8 Dy2 N2 C10 64.0(3) . . . . ? Dy1 Dy2 N2 C10 74.4(3) . . . . ? Dy1 Dy2 N2 C10 133.7(3) 2_666 . . . ? O4 Dy2 N2 C2 84.2(3) . . . . ? O3 Dy2 N2 C2 -82.1(2) . . . . ? O5 Dy2 N2 C2 111.2(2) . . . . ? O2 Dy2 N2 C2 -161.2(2) . . . . ? O1 Dy2 N2 C2 -26.4(3) . . . . ? N1 Dy2 N2 C2 19.1(2) . . . . ? O8 Dy2 N2 C2 -132.4(2) . . . . ? Dy1 Dy2 N2 C2 -122.0(2) . . . . ? Dy1 Dy2 N2 C2 -62.7(2) 2_666 . . . ? Dy1 O9 C30 C29 23.3(6) . . . . ? Dy1 O9 C30 C31 -157.8(3) . . . . ? O4 Dy2 N1 C3 39.6(3) . . . . ? O3 Dy2 N1 C3 -103.1(3) . . . . ? O5 Dy2 N1 C3 110.8(3) . . . . ? O2 Dy2 N1 C3 -177.7(3) . . . . ? O1 Dy2 N1 C3 -36.4(3) . . . . ? O8 Dy2 N1 C3 -45.7(4) . . . . ? N2 Dy2 N1 C3 -177.2(4) . . . . ? Dy1 Dy2 N1 C3 -118.4(3) . . . . ? Dy1 Dy2 N1 C3 -68.8(3) 2_666 . . . ? O4 Dy2 N1 C1 -132.3(3) . . . . ? O3 Dy2 N1 C1 85.0(3) . . . . ? O5 Dy2 N1 C1 -61.0(3) . . . . ? O2 Dy2 N1 C1 10.5(4) . . . . ? O1 Dy2 N1 C1 151.8(3) . . . . ? O8 Dy2 N1 C1 142.4(3) . . . . ? N2 Dy2 N1 C1 10.9(3) . . . . ? Dy1 Dy2 N1 C1 69.7(3) . . . . ? Dy1 Dy2 N1 C1 119.3(3) 2_666 . . . ? Dy2 O1 C5 C6 126.7(3) . . . . ? Dy1 O1 C5 C6 -61.3(5) 2_666 . . . ? Dy2 O1 C5 C4 -54.9(4) . . . . ? Dy1 O1 C5 C4 117.0(3) 2_666 . . . ? Dy1 O6 C23 C24 -13.0(5) . . . . ? Dy1 O6 C23 C22 168.3(3) . . . . ? Dy1 O7 C25 C24 10.3(6) . . . . ? Dy1 O7 C25 C26 -169.3(3) . . . . ? O1 C5 C4 C9 -176.1(4) . . . . ? C6 C5 C4 C9 2.3(6) . . . . ? O1 C5 C4 C3 1.7(6) . . . . ? C6 C5 C4 C3 -179.9(4) . . . . ? C10 N2 C2 C1 119.0(4) . . . . ? Dy2 N2 C2 C1 -45.7(3) . . . . ? C2 N2 C10 C11 -176.0(4) . . . . ? Dy2 N2 C10 C11 -13.0(5) . . . . ? O7 C25 C24 C23 -0.1(7) . . . . ? C26 C25 C24 C23 179.5(4) . . . . ? O6 C23 C24 C25 1.5(6) . . . . ? C22 C23 C24 C25 -179.8(4) . . . . ? Dy2 O2 C12 C13 -128.2(3) . . . . ? Dy1 O2 C12 C13 77.5(4) . . . . ? Dy2 O2 C12 C11 51.8(4) . . . . ? Dy1 O2 C12 C11 -102.5(4) . . . . ? O9 C30 C29 C28 5.3(6) . . . . ? C31 C30 C29 C28 -173.7(4) . . . . ? O8 C28 C29 C30 -7.6(6) . . . . ? C27 C28 C29 C30 171.1(4) . . . . ? O2 C12 C11 C16 177.7(4) . . . . ? C13 C12 C11 C16 -2.3(6) . . . . ? O2 C12 C11 C10 -3.1(6) . . . . ? C13 C12 C11 C10 177.0(4) . . . . ? N2 C10 C11 C16 164.3(4) . . . . ? N2 C10 C11 C12 -14.9(6) . . . . ? O1 C5 C6 C7 178.5(4) . . . . ? C4 C5 C6 C7 0.1(6) . . . . ? C1 N1 C3 C4 179.9(4) . . . . ? Dy2 N1 C3 C4 8.0(6) . . . . ? C9 C4 C3 N1 -158.8(4) . . . . ? C5 C4 C3 N1 23.4(7) . . . . ? Dy2 O5 C18 C19 9.6(8) . . . . ? Dy2 O5 C18 C17 -171.8(4) . . . . ? C20 C19 C18 O5 -3.7(8) . . . . ? C20 C19 C18 C17 177.7(5) . . . . ? C3 N1 C1 C2 149.4(4) . . . . ? Dy2 N1 C1 C2 -38.1(4) . . . . ? N2 C2 C1 N1 53.9(4) . . . . ? C5 C4 C9 C8 -3.2(7) . . . . ? C3 C4 C9 C8 178.9(5) . . . . ? C12 C11 C16 C15 2.7(7) . . . . ? C10 C11 C16 C15 -176.6(5) . . . . ? O2 C12 C13 C14 -179.3(4) . . . . ? C11 C12 C13 C14 0.7(7) . . . . ? Dy2 O4 C20 C19 1.0(7) . . . . ? Dy2 O4 C20 C21 -178.8(3) . . . . ? C18 C19 C20 O4 -1.3(7) . . . . ? C18 C19 C20 C21 178.5(5) . . . . ? C4 C9 C8 C7 1.4(8) . . . . ? C9 C8 C7 C6 1.1(8) . . . . ? C5 C6 C7 C8 -1.9(7) . . . . ? C12 C13 C14 C15 0.6(8) . . . . ? C11 C16 C15 C14 -1.4(9) . . . . ? C13 C14 C15 C16 -0.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.856 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 837060'