# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Cheng-Yong Su' _publ_contact_author_email cesscy@mail.sysu.edu.cn _publ_author_name 'Cheng-Yong Su' data_1 _database_code_depnum_ccdc_archive 'CCDC 803981' #TrackingRef '- Crystal data and Checkcif.pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H70 Eu F9 N6 O21 S3' _chemical_formula_weight 1630.36 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9443(7) _cell_length_b 17.1237(9) _cell_length_c 17.3069(9) _cell_angle_alpha 118.444(5) _cell_angle_beta 103.191(5) _cell_angle_gamma 96.751(4) _cell_volume 3656.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14227 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7457 _exptl_absorpt_correction_T_max 0.9032 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Germini _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21952 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.1338 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14207 _reflns_number_gt 9860 _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^)+(0.1000P)^2^+28.7978P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14207 _refine_ls_number_parameters 962 _refine_ls_number_restraints 334 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2355 _refine_ls_wR_factor_gt 0.2262 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.11967(3) 0.04191(3) 0.10828(3) 0.01728(15) Uani 1 1 d . . . O1 O 0.2099(5) 0.1778(5) 0.1355(5) 0.0296(16) Uani 1 1 d . . . O2 O 0.9455(5) 0.8570(5) 0.7887(5) 0.0378(19) Uani 1 1 d . . . O3 O 0.8301(6) 0.0672(5) 0.0004(5) 0.0399(19) Uani 1 1 d . . . O4 O 0.0448(4) 0.0513(4) -0.0255(4) 0.0205(14) Uani 1 1 d . . . O5 O 0.0918(5) -0.0481(5) -0.8292(5) 0.0290(16) Uani 1 1 d . . . O6 O 0.7290(5) -0.0588(5) -0.2022(6) 0.045(2) Uani 1 1 d . . . N1 N 0.4402(6) 0.4023(6) 0.2815(6) 0.0290(19) Uani 1 1 d . . . N2 N 0.8672(5) 0.5829(5) 0.5961(5) 0.0235(18) Uani 1 1 d . . . N3 N 0.7984(6) 0.3243(6) 0.1495(5) 0.030(2) Uani 1 1 d . . . N4 N 0.1839(6) 0.1546(6) -0.1490(6) 0.0253(18) Uani 1 1 d . . . N5 N 0.1451(6) -0.0680(6) -0.5994(6) 0.0270(19) Uani 1 1 d . . . N6 N 0.5542(6) 0.0753(6) -0.2814(6) 0.033(2) Uani 1 1 d . . . C1 C 0.4309(9) 0.2182(10) -0.1637(9) 0.057(4) Uani 1 1 d . . . H1A H 0.4943 0.2194 -0.1667 0.086 Uiso 1 1 calc R . . H1B H 0.4238 0.2041 -0.1176 0.086 Uiso 1 1 calc R . . H1C H 0.4196 0.2774 -0.1472 0.086 Uiso 1 1 calc R . . C2 C 0.3608(8) -0.0282(8) -0.4995(8) 0.039(3) Uani 1 1 d . . . H2A H 0.4286 -0.0062 -0.4819 0.058 Uiso 1 1 calc R . . H2B H 0.3300 -0.0203 -0.5495 0.058 Uiso 1 1 calc R . . H2C H 0.3444 -0.0924 -0.5195 0.058 Uiso 1 1 calc R . . C3 C 0.0905(7) 0.0399(8) -0.3736(7) 0.032(2) Uani 1 1 d . . . H3A H 0.0591 0.0417 -0.4275 0.048 Uiso 1 1 calc R . . H3B H 0.0789 0.0865 -0.3204 0.048 Uiso 1 1 calc R . . H3C H 0.0662 -0.0195 -0.3830 0.048 Uiso 1 1 calc R . . C4 C 0.3924(7) 0.0961(7) -0.3312(7) 0.026(2) Uani 1 1 d . . . C5 C 0.3286(7) 0.0251(7) -0.4180(7) 0.026(2) Uani 1 1 d . . . C6 C 0.2305(7) 0.0035(7) -0.4289(7) 0.026(2) Uani 1 1 d . . . C7 C 0.1976(7) 0.0575(7) -0.3576(7) 0.025(2) Uani 1 1 d . . . C8 C 0.2601(7) 0.1294(7) -0.2721(7) 0.026(2) Uani 1 1 d . . . C9 C 0.3589(7) 0.1447(8) -0.2584(7) 0.033(2) Uani 1 1 d . . . C10 C 0.4974(7) 0.1213(8) -0.3188(8) 0.032(2) Uani 1 1 d . . . H10A H 0.5043 0.1058 -0.3784 0.038 Uiso 1 1 calc R . . H10B H 0.5229 0.1874 -0.2773 0.038 Uiso 1 1 calc R . . C11 C 0.6430(7) 0.1226(8) -0.2173(7) 0.034(2) Uani 1 1 d . . . H11A H 0.6636 0.1854 -0.1934 0.041 Uiso 1 1 calc R . . C12 C 0.7023(7) 0.0812(7) -0.1869(7) 0.033(2) Uani 1 1 d . . . H12A H 0.7608 0.1163 -0.1407 0.039 Uiso 1 1 calc R . . C13 C 0.6745(8) -0.0168(8) -0.2263(8) 0.038(3) Uani 1 1 d . . . C14 C 0.5835(9) -0.0618(9) -0.2907(11) 0.067(5) Uani 1 1 d . . . H14A H 0.5604 -0.1248 -0.3168 0.080 Uiso 1 1 calc R . . C15 C 0.5267(9) -0.0149(9) -0.3167(10) 0.059(4) Uani 1 1 d . . . H15A H 0.4666 -0.0477 -0.3607 0.070 Uiso 1 1 calc R . . C16 C 0.1650(7) -0.0796(7) -0.5176(7) 0.029(2) Uani 1 1 d . . . H16A H 0.1928 -0.1311 -0.5311 0.034 Uiso 1 1 calc R . . H16B H 0.1051 -0.0948 -0.5086 0.034 Uiso 1 1 calc R . . C17 C 0.1473(7) 0.0137(7) -0.5921(7) 0.028(2) Uani 1 1 d . . . H17A H 0.1613 0.0659 -0.5336 0.033 Uiso 1 1 calc R . . C18 C 0.1294(7) 0.0224(7) -0.6684(7) 0.029(2) Uani 1 1 d . . . H18A H 0.1332 0.0804 -0.6606 0.034 Uiso 1 1 calc R . . C19 C 0.1055(6) -0.0538(7) -0.7571(7) 0.024(2) Uani 1 1 d . . . C20 C 0.1004(8) -0.1408(8) -0.7633(7) 0.033(2) Uani 1 1 d . . . H20A H 0.0825 -0.1947 -0.8212 0.040 Uiso 1 1 calc R . . C21 C 0.1216(7) -0.1445(7) -0.6852(7) 0.028(2) Uani 1 1 d . . . H21A H 0.1201 -0.2013 -0.6903 0.033 Uiso 1 1 calc R . . C22 C 0.2241(8) 0.1942(7) -0.1971(8) 0.033(2) Uani 1 1 d . . . H22A H 0.2763 0.2480 -0.1513 0.040 Uiso 1 1 calc R . . H22B H 0.1754 0.2145 -0.2249 0.040 Uiso 1 1 calc R . . C23 C 0.1429(7) 0.2070(7) -0.0866(7) 0.029(2) Uani 1 1 d . . . H23A H 0.1445 0.2665 -0.0741 0.035 Uiso 1 1 calc R . . C24 C 0.1006(7) 0.1760(7) -0.0431(7) 0.028(2) Uani 1 1 d . . . H24A H 0.0763 0.2149 0.0015 0.034 Uiso 1 1 calc R . . C25 C 0.0922(7) 0.0847(7) -0.0642(6) 0.021(2) Uani 1 1 d . . . C26 C 0.1391(7) 0.0336(7) -0.1243(6) 0.026(2) Uani 1 1 d . . . H26A H 0.1398 -0.0255 -0.1370 0.032 Uiso 1 1 calc R . . C27 C 0.1836(7) 0.0705(7) -0.1642(7) 0.030(2) Uani 1 1 d . . . H27A H 0.2151 0.0359 -0.2036 0.036 Uiso 1 1 calc R . . C28 C 0.6412(8) 0.5092(9) 0.5088(8) 0.043(3) Uani 1 1 d . . . H28A H 0.6544 0.5751 0.5441 0.065 Uiso 1 1 calc R . . H28B H 0.6737 0.4884 0.5472 0.065 Uiso 1 1 calc R . . H28C H 0.5738 0.4825 0.4880 0.065 Uiso 1 1 calc R . . C29 C 0.5859(8) 0.4224(8) 0.1743(7) 0.037(3) Uani 1 1 d . . . H29A H 0.5243 0.4292 0.1793 0.056 Uiso 1 1 calc R . . H29B H 0.5796 0.3610 0.1255 0.056 Uiso 1 1 calc R . . H29C H 0.6129 0.4659 0.1603 0.056 Uiso 1 1 calc R . . C30 C 0.9048(7) 0.4379(8) 0.3694(8) 0.040(3) Uani 1 1 d . . . H30A H 0.9485 0.4945 0.4208 0.060 Uiso 1 1 calc R . . H30B H 0.9178 0.4251 0.3133 0.060 Uiso 1 1 calc R . . H30C H 0.9122 0.3886 0.3802 0.060 Uiso 1 1 calc R . . C31 C 0.6751(7) 0.4802(7) 0.4261(7) 0.029(2) Uani 1 1 d . . . C32 C 0.6179(7) 0.4657(6) 0.3420(7) 0.027(2) Uani 1 1 d . . . C33 C 0.6509(7) 0.4401(7) 0.2660(7) 0.027(2) Uani 1 1 d . . . C34 C 0.7448(7) 0.4339(6) 0.2756(7) 0.026(2) Uani 1 1 d . . . C35 C 0.8038(7) 0.4465(7) 0.3599(7) 0.029(2) Uani 1 1 d . . . C36 C 0.7680(7) 0.4677(6) 0.4330(7) 0.026(2) Uani 1 1 d . . . C37 C 0.5209(7) 0.4853(7) 0.3352(7) 0.029(2) Uani 1 1 d . . . H37A H 0.5179 0.5215 0.3975 0.035 Uiso 1 1 calc R . . H37B H 0.5143 0.5222 0.3068 0.035 Uiso 1 1 calc R . . C38 C 0.3585(8) 0.4020(8) 0.2262(8) 0.036(3) Uani 1 1 d . . . H38A H 0.3556 0.4539 0.2221 0.043 Uiso 1 1 calc R . . C39 C 0.2817(8) 0.3281(8) 0.1771(8) 0.041(3) Uani 1 1 d . . . H39A H 0.2278 0.3296 0.1388 0.049 Uiso 1 1 calc R . . C40 C 0.2821(7) 0.2494(7) 0.1831(7) 0.027(2) Uani 1 1 d . . . C41 C 0.3645(8) 0.2537(8) 0.2439(10) 0.048(3) Uani 1 1 d . . . H41A H 0.3672 0.2046 0.2530 0.058 Uiso 1 1 calc R . . C42 C 0.4415(8) 0.3290(8) 0.2904(9) 0.046(3) Uani 1 1 d . . . H42A H 0.4962 0.3292 0.3292 0.056 Uiso 1 1 calc R . . C43 C 0.7850(8) 0.4189(7) 0.1996(7) 0.035(3) Uani 1 1 d . . . H43A H 0.7425 0.4288 0.1555 0.041 Uiso 1 1 calc R . . H43B H 0.8460 0.4638 0.2258 0.041 Uiso 1 1 calc R . . C44 C 0.7462(9) 0.2520(8) 0.1450(8) 0.042(3) Uani 1 1 d . . . H44A H 0.7006 0.2609 0.1749 0.051 Uiso 1 1 calc R . . C45 C 0.7580(9) 0.1671(8) 0.0985(8) 0.041(3) Uani 1 1 d . . . H45A H 0.7235 0.1198 0.1007 0.050 Uiso 1 1 calc R . . C46 C 0.8211(8) 0.1477(8) 0.0463(7) 0.034(3) Uani 1 1 d . . . C47 C 0.8728(8) 0.2248(8) 0.0506(8) 0.040(3) Uani 1 1 d . . . H47A H 0.9155 0.2172 0.0176 0.048 Uiso 1 1 calc R . . C48 C 0.8613(8) 0.3095(9) 0.1019(8) 0.041(3) Uani 1 1 d . . . H48A H 0.8976 0.3593 0.1047 0.049 Uiso 1 1 calc R . . C49 C 0.8310(8) 0.4827(7) 0.5235(7) 0.031(2) Uani 1 1 d . . . H49A H 0.7950 0.4510 0.5451 0.038 Uiso 1 1 calc R . . H49B H 0.8845 0.4568 0.5132 0.038 Uiso 1 1 calc R . . C50 C 0.8915(7) 0.6461(7) 0.5736(7) 0.027(2) Uani 1 1 d . . . H50A H 0.8870 0.6263 0.5122 0.033 Uiso 1 1 calc R . . C51 C 0.9222(7) 0.7374(7) 0.6378(7) 0.028(2) Uani 1 1 d . . . H51A H 0.9407 0.7787 0.6203 0.033 Uiso 1 1 calc R . . C52 C 0.9267(7) 0.7708(7) 0.7306(7) 0.029(2) Uani 1 1 d . . . C53 C 0.9092(8) 0.7022(7) 0.7540(7) 0.033(3) Uani 1 1 d . . . H53A H 0.9165 0.7194 0.8152 0.040 Uiso 1 1 calc R . . C54 C 0.8816(7) 0.6110(7) 0.6858(7) 0.028(2) Uani 1 1 d . . . H54A H 0.8725 0.5670 0.7023 0.034 Uiso 1 1 calc R . . C55 C 0.2073(10) 0.3083(9) 0.6445(9) 0.051(3) Uani 1 1 d . . . O16 O 0.5393(15) 0.1935(15) 0.1306(15) 0.166(7) Uani 1 1 d DU . . C58 C 0.470(2) 0.124(2) 0.071(2) 0.183(9) Uani 1 1 d DU . . C59 C 0.431(3) 0.049(2) 0.088(2) 0.210(11) Uani 1 1 d DU . . H59A H 0.4829 0.0377 0.1219 0.315 Uiso 1 1 calc R . . H59B H 0.3966 -0.0060 0.0299 0.315 Uiso 1 1 calc R . . H59C H 0.3891 0.0699 0.1240 0.315 Uiso 1 1 calc R . . C60 C 0.390(2) 0.133(2) 0.010(2) 0.183(10) Uani 1 1 d DU . . H60A H 0.4134 0.1774 -0.0041 0.275 Uiso 1 1 calc R . . H60B H 0.3439 0.1521 0.0409 0.275 Uiso 1 1 calc R . . H60C H 0.3602 0.0742 -0.0469 0.275 Uiso 1 1 calc R . . S1 S 0.0783(3) 0.2720(2) 0.6041(2) 0.0519(9) Uani 1 1 d . . . O7 O 0.0564(8) 0.2541(7) 0.6718(7) 0.069(3) Uani 1 1 d . . . O8 O 0.0545(8) 0.3512(7) 0.6068(7) 0.068(3) Uani 1 1 d . . . O9 O 0.0566(7) 0.1930(7) 0.5150(7) 0.066(3) Uani 1 1 d . . . F1 F 0.2423(7) 0.2389(6) 0.6363(7) 0.082(3) Uani 1 1 d . . . F2 F 0.2409(7) 0.3752(6) 0.7329(6) 0.089(3) Uani 1 1 d . . . F3 F 0.2374(6) 0.3400(6) 0.5966(6) 0.068(2) Uani 1 1 d . . . S2 S 0.5592(5) 0.2921(4) 0.5369(4) 0.0407(14) Uani 0.50 1 d PDU A 1 O10 O 0.6129(11) 0.3832(9) 0.6163(9) 0.041(4) Uani 0.50 1 d PDU A 1 O11 O 0.5230(11) 0.2934(10) 0.4574(9) 0.040(4) Uani 0.50 1 d PDU A 1 O12 O 0.6013(14) 0.2222(13) 0.5321(14) 0.070(5) Uiso 0.50 1 d PDU A 1 C56 C 0.462(2) 0.2665(16) 0.5688(18) 0.067(6) Uani 0.50 1 d PDU A 1 F4 F 0.4136(14) 0.1804(10) 0.5134(12) 0.081(5) Uani 0.50 1 d PDU A 1 F5 F 0.3957(12) 0.3105(11) 0.5513(13) 0.082(5) Uani 0.50 1 d PDU A 1 F6 F 0.4718(16) 0.2895(13) 0.6472(13) 0.094(6) Uani 0.50 1 d PDU A 1 S2' S 0.6990(9) 0.1588(8) 0.3099(7) 0.113(4) Uani 0.50 1 d PDU B 2 O10' O 0.664(2) 0.166(2) 0.3857(19) 0.159(10) Uani 0.50 1 d PDU B 2 O11' O 0.6620(16) 0.2238(15) 0.2998(18) 0.094(7) Uani 0.50 1 d PDU B 2 O12' O 0.6907(11) 0.0705(9) 0.2423(10) 0.039(4) Uani 0.50 1 d PDU B 2 C56' C 0.820(2) 0.198(2) 0.362(2) 0.115(9) Uani 0.50 1 d PDU B 2 F4' F 0.846(2) 0.2815(19) 0.4332(19) 0.172(10) Uani 0.50 1 d PDU B 2 F5' F 0.857(2) 0.210(2) 0.3019(19) 0.160(10) Uani 0.50 1 d PDU B 2 F6' F 0.858(2) 0.150(2) 0.375(2) 0.161(10) Uani 0.50 1 d PDU B 2 S3 S 0.2893(4) 0.6011(3) 0.0481(3) 0.0779(12) Uani 1 1 d U . . O13 O 0.3432(9) 0.6515(9) 0.0223(9) 0.093(4) Uani 1 1 d U . . O14 O 0.1923(10) 0.5500(9) -0.0156(10) 0.112(4) Uani 1 1 d U . . O15 O 0.3016(13) 0.6543(11) 0.1464(10) 0.128(5) Uani 1 1 d U . . C57 C 0.339(3) 0.508(2) 0.037(2) 0.144(7) Uani 1 1 d U . . F7 F 0.4309(14) 0.5425(13) 0.0965(14) 0.194(7) Uani 1 1 d U . . F8 F 0.2960(12) 0.4511(10) 0.0535(11) 0.159(5) Uani 1 1 d U . . F9 F 0.3388(13) 0.4549(11) -0.0501(13) 0.165(6) Uani 1 1 d U . . O1W O 0.0801(10) 0.3728(9) 0.8638(9) 0.111(5) Uani 1 1 d U . . O2W O 0.0387(10) 0.6402(9) 0.0432(9) 0.108(5) Uani 1 1 d U . . O4W O 0.0941(9) 0.4094(11) 0.1176(10) 0.109(4) Uani 1 1 d U . . O5W O 0.0746(16) 0.5650(16) 0.2995(15) 0.186(8) Uiso 1 1 d . . . O3W O 0.228(2) 0.697(2) 0.303(2) 0.128(11) Uiso 0.50 1 d P C 1 O6W O 0.229(3) 0.578(3) 0.240(3) 0.171(15) Uiso 0.50 1 d P D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.0133(2) 0.0193(2) 0.0125(2) 0.00514(17) 0.00163(16) 0.00082(16) O1 0.021(3) 0.029(4) 0.031(4) 0.013(3) 0.004(3) 0.000(3) O2 0.043(5) 0.023(4) 0.032(4) 0.002(3) 0.020(4) 0.002(3) O3 0.049(5) 0.039(5) 0.038(4) 0.017(4) 0.024(4) 0.023(4) O4 0.016(3) 0.022(3) 0.014(3) 0.006(3) 0.000(3) -0.005(3) O5 0.023(4) 0.042(4) 0.028(4) 0.024(3) 0.007(3) 0.003(3) O6 0.023(4) 0.042(5) 0.057(5) 0.031(4) -0.015(4) -0.003(4) N1 0.022(4) 0.021(4) 0.033(5) 0.006(4) 0.011(4) 0.000(3) N2 0.022(4) 0.021(4) 0.013(4) -0.001(3) 0.004(3) 0.005(3) N3 0.030(5) 0.032(5) 0.018(4) 0.005(4) 0.015(4) 0.001(4) N4 0.022(4) 0.030(5) 0.027(4) 0.016(4) 0.011(4) 0.004(4) N5 0.024(4) 0.038(5) 0.026(4) 0.022(4) 0.007(4) 0.007(4) N6 0.018(4) 0.042(6) 0.044(5) 0.027(5) 0.007(4) 0.006(4) C1 0.036(7) 0.077(10) 0.041(7) 0.020(7) 0.014(6) 0.005(7) C2 0.037(6) 0.051(8) 0.043(7) 0.029(6) 0.023(6) 0.022(6) C3 0.020(5) 0.044(7) 0.031(6) 0.017(5) 0.014(4) 0.007(5) C4 0.018(5) 0.042(6) 0.032(5) 0.026(5) 0.014(4) 0.011(4) C5 0.025(5) 0.034(6) 0.030(5) 0.022(5) 0.014(4) 0.011(4) C6 0.022(5) 0.039(6) 0.025(5) 0.023(5) 0.005(4) 0.010(4) C7 0.017(5) 0.039(6) 0.027(5) 0.023(5) 0.010(4) 0.006(4) C8 0.021(5) 0.041(6) 0.029(5) 0.025(5) 0.014(4) 0.006(4) C9 0.023(5) 0.045(7) 0.030(6) 0.025(5) 0.002(4) -0.002(5) C10 0.019(5) 0.048(7) 0.043(6) 0.032(6) 0.015(5) 0.011(5) C11 0.022(5) 0.034(6) 0.036(6) 0.012(5) 0.006(5) 0.007(5) C12 0.024(5) 0.038(6) 0.019(5) 0.005(5) -0.001(4) 0.002(5) C13 0.026(6) 0.038(7) 0.044(6) 0.022(6) 0.006(5) 0.003(5) C14 0.034(7) 0.042(8) 0.096(11) 0.041(8) -0.028(7) -0.009(6) C15 0.032(7) 0.051(8) 0.077(10) 0.040(8) -0.015(7) -0.005(6) C16 0.031(6) 0.036(6) 0.027(5) 0.023(5) 0.010(4) 0.006(5) C17 0.027(5) 0.033(6) 0.018(5) 0.013(4) 0.003(4) 0.003(4) C18 0.030(6) 0.027(6) 0.036(6) 0.018(5) 0.018(5) 0.011(4) C19 0.008(4) 0.034(6) 0.029(5) 0.021(5) -0.004(4) -0.003(4) C20 0.033(6) 0.037(6) 0.022(5) 0.014(5) 0.002(5) -0.001(5) C21 0.030(6) 0.027(6) 0.027(5) 0.017(5) 0.009(4) 0.006(4) C22 0.042(6) 0.032(6) 0.039(6) 0.024(5) 0.023(5) 0.012(5) C23 0.022(5) 0.032(6) 0.037(6) 0.020(5) 0.010(5) 0.010(4) C24 0.031(6) 0.027(6) 0.024(5) 0.012(4) 0.009(4) 0.003(4) C25 0.020(5) 0.027(5) 0.015(4) 0.010(4) 0.004(4) 0.004(4) C26 0.034(6) 0.030(6) 0.020(5) 0.014(4) 0.012(4) 0.010(5) C27 0.033(6) 0.034(6) 0.030(5) 0.017(5) 0.018(5) 0.010(5) C28 0.027(6) 0.058(8) 0.040(7) 0.016(6) 0.027(5) 0.010(5) C29 0.027(6) 0.044(7) 0.027(6) 0.013(5) 0.002(5) 0.000(5) C30 0.024(6) 0.045(7) 0.038(6) 0.010(5) 0.015(5) 0.009(5) C31 0.026(5) 0.021(5) 0.028(5) 0.005(4) 0.012(4) -0.003(4) C32 0.022(5) 0.016(5) 0.026(5) -0.002(4) 0.011(4) 0.002(4) C33 0.022(5) 0.020(5) 0.031(5) 0.010(4) 0.006(4) -0.001(4) C34 0.023(5) 0.019(5) 0.024(5) 0.001(4) 0.011(4) 0.001(4) C35 0.025(5) 0.017(5) 0.024(5) -0.003(4) 0.008(4) 0.000(4) C36 0.021(5) 0.018(5) 0.024(5) 0.003(4) 0.005(4) -0.002(4) C37 0.020(5) 0.021(5) 0.033(5) 0.004(4) 0.011(4) 0.000(4) C38 0.030(6) 0.032(6) 0.042(6) 0.020(5) 0.005(5) 0.002(5) C39 0.025(6) 0.035(7) 0.047(7) 0.022(6) -0.007(5) -0.004(5) C40 0.018(5) 0.031(6) 0.026(5) 0.014(5) 0.003(4) -0.003(4) C41 0.034(7) 0.033(7) 0.074(9) 0.034(7) 0.003(6) -0.004(5) C42 0.027(6) 0.045(7) 0.066(8) 0.038(7) -0.003(6) -0.001(5) C43 0.039(6) 0.028(6) 0.031(6) 0.008(5) 0.020(5) 0.004(5) C44 0.045(7) 0.040(7) 0.041(6) 0.014(6) 0.031(6) 0.007(5) C45 0.048(7) 0.032(6) 0.044(7) 0.013(5) 0.029(6) 0.009(5) C46 0.030(6) 0.043(7) 0.025(5) 0.010(5) 0.015(5) 0.021(5) C47 0.032(6) 0.043(7) 0.038(6) 0.014(6) 0.017(5) 0.011(5) C48 0.030(6) 0.048(7) 0.048(7) 0.022(6) 0.026(6) 0.009(5) C49 0.035(6) 0.026(6) 0.025(5) 0.007(4) 0.011(5) 0.009(5) C50 0.031(5) 0.026(5) 0.021(5) 0.009(4) 0.010(4) 0.005(4) C51 0.029(5) 0.023(5) 0.028(5) 0.010(4) 0.013(4) 0.003(4) C52 0.015(5) 0.032(6) 0.020(5) 0.003(5) -0.001(4) -0.001(4) C53 0.032(6) 0.036(6) 0.016(5) 0.004(5) 0.004(4) 0.008(5) C54 0.031(6) 0.032(6) 0.021(5) 0.012(5) 0.014(4) 0.010(5) C55 0.066(9) 0.044(8) 0.043(7) 0.029(6) 0.010(7) -0.001(7) O16 0.137(11) 0.161(12) 0.181(12) 0.067(10) 0.083(10) 0.010(9) C58 0.176(13) 0.180(13) 0.174(12) 0.076(10) 0.066(11) 0.036(11) C59 0.196(16) 0.197(17) 0.197(16) 0.070(12) 0.088(13) 0.019(13) C60 0.174(16) 0.210(16) 0.128(14) 0.064(12) 0.034(12) 0.057(13) S1 0.066(2) 0.0420(19) 0.0445(18) 0.0229(16) 0.0196(17) -0.0021(16) O7 0.102(8) 0.055(6) 0.059(6) 0.034(5) 0.038(6) 0.013(6) O8 0.082(7) 0.073(7) 0.074(7) 0.050(6) 0.039(6) 0.022(6) O9 0.075(7) 0.050(6) 0.054(6) 0.018(5) 0.021(5) -0.008(5) F1 0.087(7) 0.072(6) 0.119(8) 0.073(6) 0.037(6) 0.024(5) F2 0.105(8) 0.071(6) 0.048(5) 0.023(5) -0.004(5) -0.025(5) F3 0.071(6) 0.065(5) 0.089(6) 0.054(5) 0.037(5) 0.007(4) S2 0.063(4) 0.022(3) 0.026(3) 0.007(2) 0.000(3) 0.026(3) O10 0.055(8) 0.025(7) 0.029(7) 0.005(6) 0.003(6) 0.027(6) O11 0.044(8) 0.039(8) 0.030(7) 0.021(6) 0.001(6) -0.009(6) C56 0.107(11) 0.050(9) 0.070(9) 0.048(8) 0.039(9) 0.004(8) F4 0.132(12) 0.034(7) 0.077(9) 0.030(7) 0.044(9) 0.003(8) F5 0.078(10) 0.053(9) 0.103(10) 0.028(8) 0.051(9) -0.009(7) F6 0.131(12) 0.075(10) 0.078(10) 0.036(8) 0.055(9) 0.014(9) S2' 0.142(8) 0.107(7) 0.086(6) 0.064(5) 0.023(6) -0.018(6) O10' 0.140(14) 0.154(15) 0.132(14) 0.040(11) 0.049(12) 0.014(12) O11' 0.086(11) 0.069(11) 0.122(12) 0.039(9) 0.040(10) 0.041(9) O12' 0.057(8) 0.014(6) 0.042(7) 0.003(6) 0.033(7) 0.019(6) C56' 0.145(13) 0.119(13) 0.124(13) 0.096(10) 0.036(11) 0.044(11) F4' 0.166(15) 0.168(15) 0.159(15) 0.081(12) 0.027(12) 0.045(13) F5' 0.153(15) 0.156(14) 0.155(15) 0.077(12) 0.024(12) 0.052(12) F6' 0.168(15) 0.150(15) 0.142(14) 0.068(12) 0.040(12) 0.017(12) S3 0.088(3) 0.072(3) 0.059(2) 0.027(2) 0.022(2) 0.008(2) O13 0.094(8) 0.094(8) 0.089(7) 0.053(6) 0.029(6) -0.002(6) O14 0.094(8) 0.086(8) 0.116(9) 0.039(7) 0.013(7) -0.006(7) O15 0.167(10) 0.110(8) 0.086(7) 0.045(7) 0.039(7) 0.004(7) C57 0.174(11) 0.134(10) 0.146(11) 0.100(9) 0.027(9) 0.042(9) F7 0.180(12) 0.166(11) 0.210(12) 0.105(9) -0.005(10) 0.058(10) F8 0.190(11) 0.130(9) 0.159(10) 0.105(8) 0.007(8) 0.011(8) F9 0.173(11) 0.136(10) 0.173(11) 0.070(9) 0.048(9) 0.065(9) O1W 0.109(10) 0.093(9) 0.094(9) 0.017(7) 0.056(8) 0.006(7) O2W 0.120(10) 0.091(9) 0.103(9) 0.032(7) 0.067(8) 0.014(7) O4W 0.081(8) 0.136(11) 0.107(9) 0.067(8) 0.014(7) 0.035(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.284(7) 2_655 ? Eu1 O5 2.316(6) 1_556 ? Eu1 O2 2.318(7) 2_666 ? Eu1 O1 2.320(7) . ? Eu1 O6 2.358(7) 2_655 ? Eu1 O4 2.420(6) . ? Eu1 O4 2.436(6) 2 ? Eu1 Eu1 4.0560(10) 2 ? O1 C40 1.290(11) . ? O2 C52 1.276(12) . ? O2 Eu1 2.318(7) 2_666 ? O3 C46 1.265(13) . ? O3 Eu1 2.284(7) 2_655 ? O4 C25 1.328(11) . ? O4 Eu1 2.436(6) 2 ? O5 C19 1.270(11) . ? O5 Eu1 2.316(6) 1_554 ? O6 C13 1.275(13) . ? O6 Eu1 2.358(7) 2_655 ? N1 C42 1.338(14) . ? N1 C38 1.366(14) . ? N1 C37 1.472(12) . ? N2 C54 1.341(12) . ? N2 C50 1.353(13) . ? N2 C49 1.495(12) . ? N3 C44 1.342(14) . ? N3 C48 1.355(13) . ? N3 C43 1.494(13) . ? N4 C27 1.334(13) . ? N4 C23 1.362(13) . ? N4 C22 1.478(12) . ? N5 C17 1.340(13) . ? N5 C21 1.358(13) . ? N5 C16 1.490(12) . ? N6 C15 1.328(16) . ? N6 C11 1.366(13) . ? N6 C10 1.467(13) . ? C1 C9 1.530(16) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C5 1.498(14) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C7 1.528(13) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C9 1.385(15) . ? C4 C5 1.406(14) . ? C4 C10 1.515(13) . ? C5 C6 1.413(13) . ? C6 C7 1.385(14) . ? C6 C16 1.498(14) . ? C7 C8 1.393(14) . ? C8 C9 1.412(14) . ? C8 C22 1.514(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.362(15) . ? C11 H11A 0.9300 . ? C12 C13 1.440(16) . ? C12 H12A 0.9300 . ? C13 C14 1.389(16) . ? C14 C15 1.377(17) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.369(14) . ? C17 H17A 0.9300 . ? C18 C19 1.385(14) . ? C18 H18A 0.9300 . ? C19 C20 1.432(15) . ? C20 C21 1.351(14) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.330(14) . ? C23 H23A 0.9300 . ? C24 C25 1.408(14) . ? C24 H24A 0.9300 . ? C25 C26 1.396(13) . ? C26 C27 1.358(14) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C31 1.506(14) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C33 1.524(14) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C35 1.513(14) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.397(15) . ? C31 C36 1.417(14) . ? C32 C33 1.401(14) . ? C32 C37 1.517(13) . ? C33 C34 1.398(14) . ? C34 C35 1.422(14) . ? C34 C43 1.495(14) . ? C35 C36 1.390(14) . ? C36 C49 1.513(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.352(15) . ? C38 H38A 0.9300 . ? C39 C40 1.402(15) . ? C39 H39A 0.9300 . ? C40 C41 1.394(15) . ? C41 C42 1.370(15) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.342(16) . ? C44 H44A 0.9300 . ? C45 C46 1.411(15) . ? C45 H45A 0.9300 . ? C46 C47 1.409(17) . ? C47 C48 1.351(16) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.354(14) . ? C50 H50A 0.9300 . ? C51 C52 1.407(14) . ? C51 H51A 0.9300 . ? C52 C53 1.428(16) . ? C53 C54 1.367(14) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C55 F3 1.313(14) . ? C55 F1 1.314(16) . ? C55 F2 1.323(15) . ? C55 S1 1.811(15) . ? O16 C58 1.271(18) . ? C58 C60 1.481(18) . ? C58 C59 1.522(19) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? S1 O9 1.412(10) . ? S1 O8 1.424(11) . ? S1 O7 1.438(10) . ? S2 O11 1.370(13) . ? S2 O12 1.393(16) . ? S2 O10 1.457(15) . ? S2 C56 1.75(3) . ? C56 F6 1.18(3) . ? C56 F4 1.30(3) . ? C56 F5 1.37(3) . ? S2' O11' 1.364(17) . ? S2' O12' 1.368(15) . ? S2' O10' 1.48(2) . ? S2' C56' 1.71(3) . ? C56' F6' 1.14(3) . ? C56' F4' 1.30(3) . ? C56' F5' 1.36(3) . ? S3 O13 1.401(12) . ? S3 O15 1.449(14) . ? S3 O14 1.462(14) . ? S3 C57 1.78(3) . ? C57 F8 1.28(3) . ? C57 F9 1.34(3) . ? C57 F7 1.37(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O5 92.2(3) 2_655 1_556 ? O3 Eu1 O2 174.6(3) 2_655 2_666 ? O5 Eu1 O2 85.7(3) 1_556 2_666 ? O3 Eu1 O1 102.3(3) 2_655 . ? O5 Eu1 O1 145.4(2) 1_556 . ? O2 Eu1 O1 82.1(2) 2_666 . ? O3 Eu1 O6 79.6(3) 2_655 2_655 ? O5 Eu1 O6 74.8(2) 1_556 2_655 ? O2 Eu1 O6 104.6(3) 2_666 2_655 ? O1 Eu1 O6 77.1(2) . 2_655 ? O3 Eu1 O4 80.0(2) 2_655 . ? O5 Eu1 O4 138.7(2) 1_556 . ? O2 Eu1 O4 98.2(3) 2_666 . ? O1 Eu1 O4 75.4(2) . . ? O6 Eu1 O4 141.2(3) 2_655 . ? O3 Eu1 O4 90.8(3) 2_655 2 ? O5 Eu1 O4 73.0(2) 1_556 2 ? O2 Eu1 O4 83.8(2) 2_666 2 ? O1 Eu1 O4 136.9(2) . 2 ? O6 Eu1 O4 145.9(2) 2_655 2 ? O4 Eu1 O4 66.7(2) . 2 ? O3 Eu1 Eu1 84.6(2) 2_655 2 ? O5 Eu1 Eu1 105.79(16) 1_556 2 ? O2 Eu1 Eu1 91.1(2) 2_666 2 ? O1 Eu1 Eu1 106.74(17) . 2 ? O6 Eu1 Eu1 164.2(2) 2_655 2 ? O4 Eu1 Eu1 33.49(14) . 2 ? O4 Eu1 Eu1 33.23(14) 2 2 ? C40 O1 Eu1 152.1(6) . . ? C52 O2 Eu1 138.4(7) . 2_666 ? C46 O3 Eu1 153.0(7) . 2_655 ? C25 O4 Eu1 124.0(5) . . ? C25 O4 Eu1 120.9(5) . 2 ? Eu1 O4 Eu1 113.3(2) . 2 ? C19 O5 Eu1 147.6(6) . 1_554 ? C13 O6 Eu1 144.9(7) . 2_655 ? C42 N1 C38 118.4(9) . . ? C42 N1 C37 121.8(9) . . ? C38 N1 C37 119.6(9) . . ? C54 N2 C50 118.8(8) . . ? C54 N2 C49 120.3(8) . . ? C50 N2 C49 120.8(8) . . ? C44 N3 C48 118.5(10) . . ? C44 N3 C43 122.4(8) . . ? C48 N3 C43 118.9(9) . . ? C27 N4 C23 118.2(8) . . ? C27 N4 C22 124.2(8) . . ? C23 N4 C22 117.5(8) . . ? C17 N5 C21 118.9(8) . . ? C17 N5 C16 123.0(8) . . ? C21 N5 C16 118.1(8) . . ? C15 N6 C11 118.1(10) . . ? C15 N6 C10 121.4(9) . . ? C11 N6 C10 120.0(9) . . ? C9 C1 H1A 109.5 . . ? C9 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C9 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C5 C2 H2A 109.5 . . ? C5 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C5 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C7 C3 H3A 109.5 . . ? C7 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C7 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 120.1(9) . . ? C9 C4 C10 120.2(9) . . ? C5 C4 C10 119.7(9) . . ? C4 C5 C6 119.0(9) . . ? C4 C5 C2 122.3(9) . . ? C6 C5 C2 118.7(9) . . ? C7 C6 C5 119.9(9) . . ? C7 C6 C16 121.6(9) . . ? C5 C6 C16 118.5(9) . . ? C6 C7 C8 121.3(9) . . ? C6 C7 C3 119.5(9) . . ? C8 C7 C3 119.2(9) . . ? C7 C8 C9 118.5(9) . . ? C7 C8 C22 121.5(9) . . ? C9 C8 C22 119.9(9) . . ? C4 C9 C8 120.7(9) . . ? C4 C9 C1 118.7(9) . . ? C8 C9 C1 120.6(10) . . ? N6 C10 C4 114.2(8) . . ? N6 C10 H10A 108.7 . . ? C4 C10 H10A 108.7 . . ? N6 C10 H10B 108.7 . . ? C4 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 N6 122.5(10) . . ? C12 C11 H11A 118.8 . . ? N6 C11 H11A 118.8 . . ? C11 C12 C13 120.0(10) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? O6 C13 C14 122.6(11) . . ? O6 C13 C12 122.1(10) . . ? C14 C13 C12 115.3(11) . . ? C15 C14 C13 121.3(12) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? N6 C15 C14 122.7(11) . . ? N6 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? N5 C16 C6 114.3(8) . . ? N5 C16 H16A 108.7 . . ? C6 C16 H16A 108.7 . . ? N5 C16 H16B 108.7 . . ? C6 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N5 C17 C18 121.7(9) . . ? N5 C17 H17A 119.1 . . ? C18 C17 H17A 119.1 . . ? C17 C18 C19 121.2(10) . . ? C17 C18 H18A 119.4 . . ? C19 C18 H18A 119.4 . . ? O5 C19 C18 122.9(9) . . ? O5 C19 C20 121.0(9) . . ? C18 C19 C20 116.0(9) . . ? C21 C20 C19 120.0(10) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 N5 122.2(10) . . ? C20 C21 H21A 118.9 . . ? N5 C21 H21A 118.9 . . ? N4 C22 C8 115.1(8) . . ? N4 C22 H22A 108.5 . . ? C8 C22 H22A 108.5 . . ? N4 C22 H22B 108.5 . . ? C8 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C24 C23 N4 122.2(10) . . ? C24 C23 H23A 118.9 . . ? N4 C23 H23A 118.9 . . ? C23 C24 C25 120.4(10) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? O4 C25 C26 122.5(9) . . ? O4 C25 C24 120.8(8) . . ? C26 C25 C24 116.6(9) . . ? C27 C26 C25 119.7(10) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? N4 C27 C26 122.5(9) . . ? N4 C27 H27A 118.7 . . ? C26 C27 H27A 118.7 . . ? C31 C28 H28A 109.5 . . ? C31 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C31 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C33 C29 H29A 109.5 . . ? C33 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C33 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 H30A 109.5 . . ? C35 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C35 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 118.4(9) . . ? C32 C31 C28 122.0(9) . . ? C36 C31 C28 119.6(10) . . ? C31 C32 C33 121.4(9) . . ? C31 C32 C37 119.2(9) . . ? C33 C32 C37 119.3(9) . . ? C34 C33 C32 119.7(9) . . ? C34 C33 C29 120.1(9) . . ? C32 C33 C29 120.2(9) . . ? C33 C34 C35 119.8(9) . . ? C33 C34 C43 120.3(10) . . ? C35 C34 C43 119.8(9) . . ? C36 C35 C34 119.4(9) . . ? C36 C35 C30 120.9(10) . . ? C34 C35 C30 119.7(9) . . ? C35 C36 C31 121.1(9) . . ? C35 C36 C49 119.7(9) . . ? C31 C36 C49 119.1(9) . . ? N1 C37 C32 114.2(8) . . ? N1 C37 H37A 108.7 . . ? C32 C37 H37A 108.7 . . ? N1 C37 H37B 108.7 . . ? C32 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C39 C38 N1 121.7(10) . . ? C39 C38 H38A 119.1 . . ? N1 C38 H38A 119.1 . . ? C38 C39 C40 121.0(10) . . ? C38 C39 H39A 119.5 . . ? C40 C39 H39A 119.5 . . ? O1 C40 C41 122.5(10) . . ? O1 C40 C39 121.7(9) . . ? C41 C40 C39 115.9(9) . . ? C42 C41 C40 121.1(11) . . ? C42 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? N1 C42 C41 121.7(11) . . ? N1 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? N3 C43 C34 112.5(9) . . ? N3 C43 H43A 109.1 . . ? C34 C43 H43A 109.1 . . ? N3 C43 H43B 109.1 . . ? C34 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C45 C44 N3 121.7(10) . . ? C45 C44 H44A 119.1 . . ? N3 C44 H44A 119.1 . . ? C44 C45 C46 121.9(11) . . ? C44 C45 H45A 119.0 . . ? C46 C45 H45A 119.0 . . ? O3 C46 C47 123.5(10) . . ? O3 C46 C45 121.8(11) . . ? C47 C46 C45 114.7(10) . . ? C48 C47 C46 120.9(10) . . ? C48 C47 H47A 119.5 . . ? C46 C47 H47A 119.5 . . ? C47 C48 N3 122.1(11) . . ? C47 C48 H48A 118.9 . . ? N3 C48 H48A 118.9 . . ? N2 C49 C36 111.1(8) . . ? N2 C49 H49A 109.4 . . ? C36 C49 H49A 109.4 . . ? N2 C49 H49B 109.4 . . ? C36 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? N2 C50 C51 121.8(9) . . ? N2 C50 H50A 119.1 . . ? C51 C50 H50A 119.1 . . ? C50 C51 C52 121.0(10) . . ? C50 C51 H51A 119.5 . . ? C52 C51 H51A 119.5 . . ? O2 C52 C51 121.0(10) . . ? O2 C52 C53 123.5(9) . . ? C51 C52 C53 115.5(9) . . ? C54 C53 C52 119.7(9) . . ? C54 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? N2 C54 C53 122.3(10) . . ? N2 C54 H54A 118.8 . . ? C53 C54 H54A 118.8 . . ? F3 C55 F1 109.7(12) . . ? F3 C55 F2 107.3(11) . . ? F1 C55 F2 108.1(11) . . ? F3 C55 S1 110.3(9) . . ? F1 C55 S1 110.1(9) . . ? F2 C55 S1 111.2(11) . . ? O16 C58 C60 120(3) . . ? O16 C58 C59 123(3) . . ? C60 C58 C59 108(3) . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O9 S1 O8 116.3(7) . . ? O9 S1 O7 114.7(6) . . ? O8 S1 O7 114.7(6) . . ? O9 S1 C55 103.0(7) . . ? O8 S1 C55 101.7(6) . . ? O7 S1 C55 103.7(6) . . ? O11 S2 O12 119.0(11) . . ? O11 S2 O10 112.5(9) . . ? O12 S2 O10 113.7(11) . . ? O11 S2 C56 106.6(12) . . ? O12 S2 C56 99.9(12) . . ? O10 S2 C56 102.5(11) . . ? F6 C56 F4 110(2) . . ? F6 C56 F5 102(2) . . ? F4 C56 F5 101(2) . . ? F6 C56 S2 120(2) . . ? F4 C56 S2 111.5(19) . . ? F5 C56 S2 109.0(14) . . ? O11' S2' O12' 128.0(14) . . ? O11' S2' O10' 97.6(17) . . ? O12' S2' O10' 114.3(15) . . ? O11' S2' C56' 110.9(15) . . ? O12' S2' C56' 100.7(14) . . ? O10' S2' C56' 103.3(16) . . ? F6' C56' F4' 113(3) . . ? F6' C56' F5' 104(3) . . ? F4' C56' F5' 102(3) . . ? F6' C56' S2' 117(3) . . ? F4' C56' S2' 112(2) . . ? F5' C56' S2' 107(2) . . ? O13 S3 O15 111.1(9) . . ? O13 S3 O14 115.4(9) . . ? O15 S3 O14 117.2(10) . . ? O13 S3 C57 107.9(13) . . ? O15 S3 C57 103.0(13) . . ? O14 S3 C57 100.2(13) . . ? F8 C57 F9 104(3) . . ? F8 C57 F7 107(2) . . ? F9 C57 F7 109(3) . . ? F8 C57 S3 117(3) . . ? F9 C57 S3 110.3(18) . . ? F7 C57 S3 109(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.819 _refine_diff_density_min -2.028 _refine_diff_density_rms 0.216 #==============================# data_2 _database_code_depnum_ccdc_archive 'CCDC 803982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H76 F9 Gd N6 O22 S3' _chemical_formula_weight 1693.73 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.9365(8) _cell_length_b 17.1361(10) _cell_length_c 17.3016(8) _cell_angle_alpha 118.509(5) _cell_angle_beta 103.354(4) _cell_angle_gamma 96.640(5) _cell_volume 3651.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14277 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 26 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1730 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7350 _exptl_absorpt_correction_T_max 0.8985 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Germini _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22845 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14269 _reflns_number_gt 10447 _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^)+(0.0705P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14269 _refine_ls_number_parameters 937 _refine_ls_number_restraints 156 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.068 _refine_ls_shift/su_mean 0.003 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 -0.11921(2) 0.458392(19) 0.39204(2) 0.01742(10) Uani 1 1 d . . . S1 S 0.07891(17) 0.77234(13) 0.10497(15) 0.0530(6) Uani 1 1 d . . . S2 S 0.2894(2) 0.10119(17) 0.54885(19) 0.0763(8) Uani 1 1 d . . . O1 O 0.7302(3) 0.4407(3) 0.2964(4) 0.0431(12) Uani 1 1 d . . . O1W O 0.0792(6) 0.8716(5) 0.3639(6) 0.113(3) Uani 1 1 d . . . O2 O 0.0910(3) 0.4508(3) -0.3310(3) 0.0282(10) Uani 1 1 d . . . O3 O 0.0449(3) 0.5505(2) 0.4746(3) 0.0217(9) Uani 1 1 d . . . O3W O 0.0885(7) 0.9059(7) 0.6205(8) 0.132(3) Uani 1 1 d . . . O4 O -0.7909(3) 0.6766(3) 0.6351(3) 0.0310(10) Uani 1 1 d . . . O12 O 0.3437(6) 0.1506(5) 0.5215(5) 0.094(2) Uani 1 1 d . . . O5 O -0.1679(4) 0.5674(3) 0.5001(3) 0.0421(13) Uani 1 1 d . . . O11 O 0.2974(9) 0.1522(6) 0.6450(6) 0.144(4) Uani 1 1 d U . . O5W O -0.0722(10) 0.9351(8) 0.1983(11) 0.202(6) Uani 1 1 d U . . O6 O -0.0550(3) 1.3578(3) 1.2895(3) 0.0354(12) Uani 1 1 d . . . O10 O 0.1941(6) 0.0520(5) 0.4869(7) 0.123(3) Uani 1 1 d . . . O4W O 0.2254(12) 0.154(3) 0.7822(19) 0.55(3) Uani 1 1 d . . . O7 O 0.0557(5) 0.7538(4) 0.1717(4) 0.0666(18) Uani 1 1 d . . . O8 O 0.0565(5) 0.6926(4) 0.0144(4) 0.0680(18) Uani 1 1 d . . . O9 O 0.0529(5) 0.8508(4) 0.1058(5) 0.0738(19) Uani 1 1 d . . . O16 O -0.4635(9) 0.6873(8) 0.6250(10) 0.171(5) Uani 1 1 d DU . . C62 C 0.3386(9) 0.2824(9) 0.1845(12) 0.208(12) Uani 1 1 d D . . H62A H 0.3720 0.2719 0.1407 0.312 Uiso 1 1 calc R . . H62B H 0.2957 0.2255 0.1655 0.312 Uiso 1 1 calc R . . H62C H 0.3837 0.3060 0.2450 0.312 Uiso 1 1 calc R . . O2W O -0.0394(6) 0.8613(5) 0.4577(6) 0.105(3) Uani 1 1 d . . . F1 F 0.2395(5) 0.8768(4) 0.2352(4) 0.093(2) Uani 1 1 d . . . F2 F 0.2441(4) 0.7406(4) 0.1377(5) 0.0854(18) Uani 1 1 d . . . F3 F 0.2374(4) 0.8408(3) 0.0979(4) 0.0705(15) Uani 1 1 d . . . F4 F 0.4340(8) 0.0438(8) 0.5948(11) 0.261(8) Uani 1 1 d . . . F5 F 0.2995(8) -0.0465(5) 0.5541(7) 0.176(4) Uani 1 1 d . . . F6 F 0.3433(7) -0.0402(6) 0.4528(8) 0.152(3) Uani 1 1 d . . . S3 S 0.4386(3) 0.2075(2) -0.0375(2) 0.1054(12) Uani 1 1 d U . . C57 C 0.5419(14) 0.2374(12) -0.0632(14) 0.138(6) Uani 1 1 d U . . F7 F 0.5290(11) 0.2116(8) -0.1512(9) 0.215(5) Uani 1 1 d U . . F8 F 0.5873(8) 0.3224(5) -0.0113(7) 0.178(4) Uani 1 1 d U . . F9 F 0.6060(8) 0.1907(6) -0.0458(9) 0.183(4) Uani 1 1 d U . . O13 O 0.3983(10) 0.2789(8) -0.0305(9) 0.203(6) Uani 1 1 d U . . O14 O 0.3854(7) 0.1150(5) -0.1174(6) 0.116(3) Uani 1 1 d U . . O15 O 0.4814(7) 0.2058(6) 0.0439(6) 0.120(3) Uani 1 1 d U . . N1 N 0.5552(4) 0.5755(4) 0.2199(4) 0.0350(13) Uani 1 1 d . . . N2 N 0.1449(4) 0.4317(3) -0.1000(3) 0.0244(11) Uani 1 1 d . . . N3 N 0.1838(4) 0.6535(3) 0.3508(4) 0.0257(12) Uani 1 1 d . . . N4 N -0.5608(4) 0.9012(3) 0.7806(4) 0.0284(12) Uani 1 1 d . . . N5 N -0.1315(4) 1.0831(3) 1.0964(3) 0.0259(12) Uani 1 1 d . . . N6 N -0.2020(4) 0.8237(3) 0.6487(4) 0.0299(13) Uani 1 1 d . . . C1 C -0.0960(5) 0.9374(4) 0.8675(5) 0.0396(17) Uani 1 1 d . . . H1A H -0.0958 0.8853 0.8110 0.059 Uiso 1 1 calc R . . H1B H -0.0718 0.9290 0.9187 0.059 Uiso 1 1 calc R . . H1C H -0.0563 0.9922 0.8782 0.059 Uiso 1 1 calc R . . C55 C 0.2062(7) 0.8095(5) 0.1455(6) 0.057(2) Uani 1 1 d . . . C2 C -0.3595(5) 1.0095(5) 1.0085(5) 0.0429(18) Uani 1 1 d . . . H2A H -0.3547 1.0743 1.0381 0.064 Uiso 1 1 calc R . . H2B H -0.3209 0.9972 1.0519 0.064 Uiso 1 1 calc R . . H2C H -0.4248 0.9762 0.9881 0.064 Uiso 1 1 calc R . . C56 C 0.3437(15) 0.0088(9) 0.5379(10) 0.123(6) Uani 1 1 d . . . C3 C -0.4144(5) 0.9215(5) 0.6753(5) 0.0399(17) Uani 1 1 d . . . H3A H -0.4138 0.9788 0.6779 0.060 Uiso 1 1 calc R . . H3B H -0.4781 0.8914 0.6649 0.060 Uiso 1 1 calc R . . H3C H -0.3930 0.8826 0.6252 0.060 Uiso 1 1 calc R . . C4 C -0.2318(4) 0.9683(3) 0.9337(4) 0.0260(14) Uani 1 1 d . . . C5 C -0.3251(5) 0.9793(4) 0.9255(4) 0.0281(15) Uani 1 1 d . . . C6 C -0.3826(4) 0.9656(4) 0.8415(4) 0.0260(14) Uani 1 1 d . . . C7 C -0.3493(4) 0.9395(4) 0.7654(4) 0.0271(14) Uani 1 1 d . . . C8 C -0.2556(5) 0.9332(4) 0.7759(4) 0.0281(14) Uani 1 1 d . . . C9 C -0.1971(5) 0.9464(4) 0.8589(5) 0.0281(15) Uani 1 1 d . . . C10 C -0.1696(5) 0.9835(4) 1.0240(4) 0.0317(15) Uani 1 1 d . . . H10A H -0.2063 0.9528 1.0460 0.038 Uiso 1 1 calc R . . H10B H -0.1168 0.9563 1.0137 0.038 Uiso 1 1 calc R . . C11 C -0.1090(4) 1.1459(4) 1.0728(4) 0.0269(14) Uani 1 1 d . . . H11A H -0.1139 1.1256 1.0112 0.032 Uiso 1 1 calc R . . C12 C -0.0795(5) 1.2375(4) 1.1366(4) 0.0294(15) Uani 1 1 d . . . H12A H -0.0633 1.2788 1.1185 0.035 Uiso 1 1 calc R . . C13 C -0.0731(4) 1.2709(4) 1.2310(4) 0.0275(14) Uani 1 1 d . . . C14 C -0.0898(5) 1.2030(4) 1.2547(5) 0.0325(16) Uani 1 1 d . . . H14A H -0.0805 1.2208 1.3165 0.039 Uiso 1 1 calc R . . C15 C -0.1192(5) 1.1124(4) 1.1876(5) 0.0304(15) Uani 1 1 d . . . H15A H -0.1313 1.0689 1.2041 0.037 Uiso 1 1 calc R . . C16 C -0.4795(4) 0.9855(4) 0.8341(5) 0.0327(16) Uani 1 1 d . . . H16A H -0.4825 1.0228 0.8964 0.039 Uiso 1 1 calc R . . H16B H -0.4863 1.0213 0.8044 0.039 Uiso 1 1 calc R . . C17 C -0.5586(5) 0.8282(5) 0.7897(6) 0.048(2) Uani 1 1 d . . . H17A H -0.5037 0.8286 0.8286 0.058 Uiso 1 1 calc R . . C18 C -0.6355(5) 0.7530(5) 0.7429(6) 0.048(2) Uani 1 1 d . . . H18A H -0.6318 0.7037 0.7516 0.058 Uiso 1 1 calc R . . C19 C -0.7194(5) 0.7478(4) 0.6826(5) 0.0284(14) Uani 1 1 d . . . C20 C -0.7190(5) 0.8271(4) 0.6771(5) 0.0379(17) Uani 1 1 d . . . H20A H -0.7731 0.8292 0.6393 0.045 Uiso 1 1 calc R . . C21 C -0.6413(5) 0.9008(4) 0.7258(5) 0.0344(16) Uani 1 1 d . . . H21A H -0.6438 0.9524 0.7211 0.041 Uiso 1 1 calc R . . C22 C -0.2162(5) 0.9176(4) 0.6990(5) 0.0345(16) Uani 1 1 d . . . H22A H -0.2594 0.9271 0.6549 0.041 Uiso 1 1 calc R . . H22B H -0.1555 0.9628 0.7249 0.041 Uiso 1 1 calc R . . C23 C -0.2520(5) 0.7527(4) 0.6463(5) 0.0400(18) Uani 1 1 d . . . H23A H -0.2953 0.7623 0.6788 0.048 Uiso 1 1 calc R . . C24 C -0.2413(5) 0.6664(4) 0.5975(5) 0.0408(19) Uani 1 1 d . . . H24A H -0.2770 0.6184 0.5977 0.049 Uiso 1 1 calc R . . C25 C -0.1783(5) 0.6488(4) 0.5474(5) 0.0331(16) Uani 1 1 d . . . C26 C -0.1259(5) 0.7247(5) 0.5522(5) 0.0389(18) Uani 1 1 d . . . H26A H -0.0812 0.7173 0.5215 0.047 Uiso 1 1 calc R . . C27 C -0.1396(5) 0.8090(5) 0.6012(5) 0.0412(18) Uani 1 1 d . . . H27A H -0.1050 0.8584 0.6022 0.049 Uiso 1 1 calc R . . C28 C 0.4307(6) 0.7189(6) 0.3372(5) 0.057(2) Uani 1 1 d . . . H28A H 0.4866 0.6984 0.3491 0.086 Uiso 1 1 calc R . . H28B H 0.4025 0.7305 0.3849 0.086 Uiso 1 1 calc R . . H28C H 0.4480 0.7745 0.3370 0.086 Uiso 1 1 calc R . . C29 C 0.0906(5) 0.5399(5) 0.1266(5) 0.0369(16) Uani 1 1 d . . . H29A H 0.0597 0.5432 0.0735 0.055 Uiso 1 1 calc R . . H29B H 0.0791 0.5857 0.1805 0.055 Uiso 1 1 calc R . . H29C H 0.0657 0.4799 0.1155 0.055 Uiso 1 1 calc R . . C30 C 0.3616(5) 0.4718(5) 0.0000(5) 0.0396(17) Uani 1 1 d . . . H30A H 0.4295 0.4938 0.0180 0.059 Uiso 1 1 calc R . . H30B H 0.3310 0.4803 -0.0497 0.059 Uiso 1 1 calc R . . H30C H 0.3451 0.4075 -0.0208 0.059 Uiso 1 1 calc R . . C31 C 0.3595(5) 0.6452(4) 0.2432(5) 0.0317(15) Uani 1 1 d . . . C32 C 0.2612(5) 0.6283(4) 0.2286(4) 0.0263(14) Uani 1 1 d . . . C33 C 0.1973(4) 0.5571(4) 0.1431(4) 0.0253(13) Uani 1 1 d . . . C34 C 0.2318(4) 0.5040(4) 0.0715(4) 0.0252(14) Uani 1 1 d . . . C35 C 0.3289(5) 0.5248(4) 0.0821(5) 0.0304(15) Uani 1 1 d . . . C36 C 0.3923(4) 0.5958(4) 0.1688(5) 0.0290(14) Uani 1 1 d . . . C37 C 0.4973(5) 0.6221(5) 0.1818(5) 0.0346(16) Uani 1 1 d . . . H37A H 0.5043 0.6069 0.1222 0.041 Uiso 1 1 calc R . . H37B H 0.5222 0.6882 0.2236 0.041 Uiso 1 1 calc R . . C38 C 0.5272(5) 0.4829(5) 0.1823(7) 0.059(2) Uani 1 1 d . . . H38A H 0.4673 0.4494 0.1376 0.071 Uiso 1 1 calc R . . C39 C 0.5852(6) 0.4388(6) 0.2091(7) 0.070(3) Uani 1 1 d . . . H39A H 0.5637 0.3755 0.1827 0.084 Uiso 1 1 calc R . . C40 C 0.6765(5) 0.4852(4) 0.2751(5) 0.0372(17) Uani 1 1 d . . . C41 C 0.7032(5) 0.5801(4) 0.3137(5) 0.0320(15) Uani 1 1 d . . . H41A H 0.7623 0.6149 0.3593 0.038 Uiso 1 1 calc R . . C42 C 0.6425(5) 0.6229(5) 0.2846(5) 0.0328(15) Uani 1 1 d . . . H42A H 0.6623 0.6861 0.3102 0.039 Uiso 1 1 calc R . . C43 C 0.1640(5) 0.4208(4) -0.0179(5) 0.0327(15) Uani 1 1 d . . . H43A H 0.1902 0.3683 -0.0314 0.039 Uiso 1 1 calc R . . H43B H 0.1039 0.4074 -0.0085 0.039 Uiso 1 1 calc R . . C44 C 0.1206(5) 0.3554(4) -0.1859(5) 0.0293(15) Uani 1 1 d . . . H44A H 0.1175 0.2983 -0.1916 0.035 Uiso 1 1 calc R . . C45 C 0.1006(5) 0.3600(4) -0.2640(5) 0.0301(15) Uani 1 1 d . . . H45A H 0.0828 0.3061 -0.3220 0.036 Uiso 1 1 calc R . . C46 C 0.1063(4) 0.4456(4) -0.2587(4) 0.0275(14) Uani 1 1 d . . . C47 C 0.1296(5) 0.5234(4) -0.1680(4) 0.0285(14) Uani 1 1 d . . . H47A H 0.1325 0.5814 -0.1600 0.034 Uiso 1 1 calc R . . C48 C 0.1477(5) 0.5144(4) -0.0921(5) 0.0289(14) Uani 1 1 d . . . H48A H 0.1625 0.5665 -0.0334 0.035 Uiso 1 1 calc R . . C49 C 0.2241(5) 0.6932(4) 0.3024(5) 0.0339(16) Uani 1 1 d . . . H49A H 0.2758 0.7476 0.3485 0.041 Uiso 1 1 calc R . . H49B H 0.1751 0.7126 0.2736 0.041 Uiso 1 1 calc R . . C50 C 0.1430(5) 0.7074(4) 0.4130(4) 0.0275(14) Uani 1 1 d . . . H50A H 0.1450 0.7669 0.4257 0.033 Uiso 1 1 calc R . . C51 C 0.0997(4) 0.6749(4) 0.4565(4) 0.0261(14) Uani 1 1 d . . . H51A H 0.0740 0.7133 0.4999 0.031 Uiso 1 1 calc R . . C52 C 0.0926(4) 0.5848(4) 0.4377(4) 0.0218(13) Uani 1 1 d . . . C53 C 0.1379(5) 0.5330(4) 0.3755(4) 0.0278(14) Uani 1 1 d . . . H53A H 0.1375 0.4734 0.3620 0.033 Uiso 1 1 calc R . . C54 C 0.1828(5) 0.5689(4) 0.3346(5) 0.0301(15) Uani 1 1 d . . . H54A H 0.2134 0.5336 0.2945 0.036 Uiso 1 1 calc R . . C58 C -0.5381(15) 0.6174(13) 0.5713(15) 0.190(7) Uani 1 1 d DU . . C59 C -0.5505(16) 0.5365(14) 0.5880(15) 0.215(8) Uani 1 1 d DU . . H59A H -0.6060 0.4885 0.5404 0.323 Uiso 1 1 calc R . . H59B H -0.5580 0.5576 0.6478 0.323 Uiso 1 1 calc R . . H59C H -0.4952 0.5130 0.5860 0.323 Uiso 1 1 calc R . . C60 C -0.6053(16) 0.6340(14) 0.5065(13) 0.212(8) Uani 1 1 d DU . . H60A H -0.5732 0.6843 0.5042 0.318 Uiso 1 1 calc R . . H60B H -0.6584 0.6487 0.5279 0.318 Uiso 1 1 calc R . . H60C H -0.6280 0.5796 0.4454 0.318 Uiso 1 1 calc R . . C61 C 0.1755(9) 0.3108(9) 0.1408(11) 0.161(7) Uani 1 1 d D . . H61A H 0.1567 0.2482 0.0897 0.242 Uiso 1 1 calc R . . H61B H 0.1555 0.3497 0.1185 0.242 Uiso 1 1 calc R . . H61C H 0.1463 0.3151 0.1862 0.242 Uiso 1 1 calc R . . O17 O 0.3068(6) 0.4269(5) 0.2548(6) 0.105(3) Uani 1 1 d D . . C63 C 0.2893(7) 0.3432(4) 0.1877(5) 0.061(3) Uani 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 0.01342(15) 0.01879(14) 0.01112(14) 0.00482(11) -0.00173(10) -0.00078(10) S1 0.0683(15) 0.0409(11) 0.0426(12) 0.0212(9) 0.0159(11) -0.0033(10) S2 0.086(2) 0.0671(15) 0.0557(17) 0.0261(13) 0.0118(15) 0.0038(14) O1 0.025(3) 0.040(3) 0.051(3) 0.027(3) -0.011(2) -0.003(2) O1W 0.113(7) 0.098(5) 0.095(7) 0.027(5) 0.045(6) 0.000(5) O2 0.026(3) 0.040(2) 0.016(2) 0.016(2) 0.0018(19) 0.0034(19) O3 0.016(2) 0.029(2) 0.016(2) 0.0110(18) 0.0020(18) -0.0020(16) O3W 0.093(7) 0.182(9) 0.191(11) 0.145(9) 0.047(7) 0.049(6) O4 0.019(2) 0.030(2) 0.033(3) 0.016(2) -0.003(2) -0.0049(18) O12 0.091(6) 0.095(5) 0.089(6) 0.056(5) 0.017(5) -0.013(4) O5 0.052(3) 0.043(3) 0.033(3) 0.015(2) 0.021(3) 0.025(2) O11 0.248(12) 0.098(6) 0.058(5) 0.025(4) 0.057(7) 0.015(6) O5W 0.243(13) 0.161(9) 0.274(14) 0.158(9) 0.082(10) 0.106(8) O6 0.039(3) 0.021(2) 0.025(3) -0.0018(19) 0.011(2) -0.0021(19) O10 0.077(6) 0.086(5) 0.154(9) 0.050(6) -0.005(6) -0.019(4) O4W 0.130(15) 1.35(8) 0.45(3) 0.72(5) 0.071(18) 0.13(3) O7 0.098(5) 0.056(3) 0.049(4) 0.029(3) 0.034(4) 0.005(3) O8 0.087(5) 0.049(3) 0.045(4) 0.015(3) 0.018(4) -0.008(3) O9 0.082(5) 0.066(4) 0.095(5) 0.056(4) 0.034(4) 0.019(3) O16 0.119(8) 0.167(9) 0.204(11) 0.076(8) 0.066(8) 0.023(7) C62 0.062(9) 0.104(10) 0.25(2) -0.056(11) 0.064(12) -0.013(7) O2W 0.119(7) 0.088(5) 0.093(6) 0.029(4) 0.060(6) 0.010(5) F1 0.108(5) 0.070(3) 0.055(4) 0.027(3) -0.010(3) -0.029(3) F2 0.084(4) 0.073(3) 0.131(6) 0.079(4) 0.028(4) 0.020(3) F3 0.076(4) 0.064(3) 0.092(4) 0.057(3) 0.032(3) 0.005(3) F4 0.150(10) 0.155(9) 0.366(19) 0.151(11) -0.114(11) -0.010(7) F5 0.235(12) 0.108(6) 0.162(9) 0.098(6) -0.009(8) -0.007(6) F6 0.189(10) 0.116(6) 0.152(9) 0.060(6) 0.066(8) 0.069(6) S3 0.149(3) 0.0670(17) 0.071(2) 0.0247(15) 0.003(2) 0.0496(19) C57 0.164(12) 0.124(10) 0.159(12) 0.110(9) 0.047(9) -0.008(8) F7 0.313(12) 0.201(9) 0.172(9) 0.126(8) 0.084(9) 0.062(8) F8 0.249(10) 0.089(5) 0.177(8) 0.066(5) 0.071(7) -0.010(5) F9 0.165(9) 0.133(6) 0.259(11) 0.115(7) 0.067(8) 0.013(6) O13 0.231(11) 0.163(8) 0.179(10) 0.070(7) 0.012(8) 0.137(8) O14 0.146(7) 0.073(5) 0.080(6) 0.022(4) -0.003(5) 0.032(5) O15 0.140(7) 0.120(6) 0.075(5) 0.068(5) -0.020(5) -0.015(5) N1 0.017(3) 0.047(3) 0.045(4) 0.031(3) 0.001(3) 0.005(2) N2 0.026(3) 0.025(3) 0.020(3) 0.013(2) 0.004(2) 0.004(2) N3 0.024(3) 0.031(3) 0.021(3) 0.013(2) 0.008(2) 0.003(2) N4 0.019(3) 0.024(3) 0.029(3) 0.008(2) 0.003(2) -0.002(2) N5 0.026(3) 0.020(2) 0.018(3) 0.003(2) 0.002(2) 0.005(2) N6 0.021(3) 0.033(3) 0.021(3) 0.004(2) 0.007(2) 0.002(2) C1 0.031(4) 0.036(4) 0.034(4) 0.006(3) 0.008(3) 0.008(3) C55 0.076(7) 0.036(4) 0.050(6) 0.024(4) 0.010(5) -0.002(4) C2 0.026(4) 0.064(5) 0.029(4) 0.019(4) 0.010(3) 0.001(3) C56 0.22(2) 0.070(8) 0.066(9) 0.036(7) 0.035(11) 0.028(10) C3 0.035(4) 0.041(4) 0.031(4) 0.015(3) 0.003(3) -0.001(3) C4 0.023(3) 0.012(3) 0.024(3) 0.001(2) 0.000(3) -0.003(2) C5 0.023(4) 0.019(3) 0.027(4) 0.005(3) 0.004(3) -0.004(2) C6 0.018(3) 0.018(3) 0.028(4) 0.004(3) 0.006(3) -0.004(2) C7 0.022(3) 0.019(3) 0.023(3) 0.003(3) 0.001(3) 0.000(2) C8 0.024(4) 0.021(3) 0.025(4) 0.003(3) 0.007(3) 0.001(2) C9 0.023(3) 0.014(3) 0.033(4) 0.003(3) 0.008(3) 0.003(2) C10 0.034(4) 0.022(3) 0.023(4) 0.003(3) 0.005(3) 0.004(3) C11 0.027(4) 0.025(3) 0.017(3) 0.005(3) 0.003(3) 0.002(3) C12 0.030(4) 0.023(3) 0.026(4) 0.006(3) 0.010(3) 0.003(3) C13 0.016(3) 0.032(3) 0.021(3) 0.005(3) 0.004(3) 0.004(3) C14 0.037(4) 0.033(3) 0.016(3) 0.007(3) 0.002(3) 0.010(3) C15 0.034(4) 0.034(3) 0.026(4) 0.015(3) 0.010(3) 0.015(3) C16 0.017(3) 0.024(3) 0.035(4) 0.005(3) 0.000(3) -0.004(2) C17 0.026(4) 0.047(4) 0.062(6) 0.036(4) -0.014(4) -0.008(3) C18 0.030(4) 0.036(4) 0.064(6) 0.032(4) -0.014(4) -0.009(3) C19 0.023(4) 0.029(3) 0.028(4) 0.015(3) 0.006(3) 0.000(3) C20 0.024(4) 0.036(4) 0.045(5) 0.024(3) -0.006(3) -0.001(3) C21 0.029(4) 0.027(3) 0.036(4) 0.013(3) 0.000(3) 0.004(3) C22 0.035(4) 0.026(3) 0.031(4) 0.006(3) 0.015(3) 0.005(3) C23 0.045(5) 0.033(4) 0.041(4) 0.012(3) 0.028(4) 0.009(3) C24 0.045(5) 0.033(4) 0.041(5) 0.013(3) 0.026(4) 0.008(3) C25 0.034(4) 0.033(4) 0.026(4) 0.011(3) 0.008(3) 0.014(3) C26 0.035(4) 0.052(4) 0.030(4) 0.017(3) 0.019(4) 0.014(3) C27 0.037(4) 0.043(4) 0.039(5) 0.015(3) 0.019(4) 0.004(3) C28 0.044(5) 0.070(5) 0.032(5) 0.016(4) 0.000(4) 0.000(4) C29 0.019(4) 0.048(4) 0.041(4) 0.025(3) 0.004(3) 0.004(3) C30 0.038(5) 0.048(4) 0.038(4) 0.024(4) 0.013(4) 0.019(3) C31 0.022(4) 0.045(4) 0.029(4) 0.025(3) 0.001(3) 0.001(3) C32 0.025(4) 0.033(3) 0.028(4) 0.021(3) 0.009(3) 0.005(3) C33 0.019(3) 0.038(3) 0.025(3) 0.024(3) 0.002(3) 0.004(3) C34 0.024(4) 0.035(3) 0.023(3) 0.022(3) 0.004(3) 0.005(3) C35 0.031(4) 0.038(4) 0.033(4) 0.026(3) 0.010(3) 0.012(3) C36 0.016(3) 0.043(4) 0.035(4) 0.028(3) 0.004(3) 0.007(3) C37 0.020(4) 0.048(4) 0.040(4) 0.028(3) 0.006(3) 0.008(3) C38 0.026(4) 0.053(5) 0.083(7) 0.045(5) -0.022(4) -0.007(3) C39 0.033(5) 0.051(5) 0.106(8) 0.051(5) -0.026(5) -0.009(4) C40 0.022(4) 0.037(4) 0.043(4) 0.022(3) -0.004(3) -0.001(3) C41 0.020(3) 0.036(4) 0.027(4) 0.011(3) -0.001(3) 0.003(3) C42 0.021(4) 0.038(4) 0.033(4) 0.016(3) 0.004(3) 0.005(3) C43 0.037(4) 0.042(4) 0.027(4) 0.025(3) 0.007(3) 0.009(3) C44 0.026(4) 0.029(3) 0.028(4) 0.015(3) 0.002(3) 0.002(3) C45 0.030(4) 0.028(3) 0.020(4) 0.011(3) -0.002(3) -0.001(3) C46 0.013(3) 0.043(4) 0.026(4) 0.021(3) 0.001(3) 0.001(3) C47 0.032(4) 0.030(3) 0.025(4) 0.017(3) 0.005(3) 0.008(3) C48 0.030(4) 0.033(3) 0.024(4) 0.016(3) 0.006(3) 0.008(3) C49 0.040(4) 0.028(3) 0.036(4) 0.017(3) 0.018(4) 0.005(3) C50 0.024(4) 0.028(3) 0.026(4) 0.014(3) 0.004(3) 0.003(3) C51 0.024(4) 0.031(3) 0.017(3) 0.010(3) 0.007(3) 0.001(3) C52 0.012(3) 0.034(3) 0.016(3) 0.015(3) -0.003(2) 0.000(2) C53 0.032(4) 0.026(3) 0.025(4) 0.013(3) 0.009(3) 0.005(3) C54 0.037(4) 0.032(3) 0.028(4) 0.016(3) 0.019(3) 0.013(3) C58 0.177(11) 0.181(11) 0.183(11) 0.075(9) 0.052(9) 0.061(9) C59 0.210(14) 0.196(13) 0.213(14) 0.095(11) 0.074(12) 0.009(11) C60 0.190(14) 0.251(13) 0.121(12) 0.054(10) 0.021(10) 0.071(11) C61 0.111(13) 0.119(11) 0.123(14) 0.006(10) -0.022(10) -0.030(9) O17 0.112(7) 0.072(5) 0.112(7) 0.026(5) 0.046(6) 0.037(4) C63 0.129(9) 0.015(3) 0.016(4) 0.006(3) 0.009(5) -0.021(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 Gd1 O5 2.264(4) . ? Gd1 O6 2.300(4) 1_544 ? Gd1 O4 2.308(4) 2_466 ? Gd1 O2 2.310(4) 2_565 ? Gd1 O1 2.352(5) 1_455 ? Gd1 O3 2.403(4) 2_566 ? Gd1 O3 2.424(4) . ? Gd1 Gd1 4.0333(7) 2_566 ? S1 O8 1.430(6) . ? S1 O7 1.437(5) . ? S1 O9 1.436(6) . ? S1 C55 1.786(10) . ? S2 O12 1.414(7) . ? S2 O11 1.428(8) . ? S2 O10 1.429(9) . ? S2 C56 1.812(15) . ? O1 C40 1.278(8) . ? O1 Gd1 2.352(5) 1_655 ? O2 C46 1.267(7) . ? O2 Gd1 2.310(4) 2_565 ? O3 C52 1.315(6) . ? O3 Gd1 2.403(4) 2_566 ? O4 C19 1.281(7) . ? O4 Gd1 2.308(4) 2_466 ? O5 C25 1.288(7) . ? O6 C13 1.287(7) . ? O6 Gd1 2.300(4) 1_566 ? O16 C58 1.299(16) . ? C62 C63 1.331(14) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? F1 C55 1.337(9) . ? F2 C55 1.331(9) . ? F3 C55 1.315(9) . ? F4 C56 1.336(19) . ? F5 C56 1.266(15) . ? F6 C56 1.300(14) . ? S3 O13 1.392(9) . ? S3 O15 1.420(8) . ? S3 O14 1.471(8) . ? S3 C57 1.788(16) . ? C57 F8 1.276(17) . ? C57 F7 1.324(18) . ? C57 F9 1.386(19) . ? N1 C42 1.351(9) . ? N1 C38 1.361(9) . ? N1 C37 1.490(8) . ? N2 C48 1.353(7) . ? N2 C44 1.355(8) . ? N2 C43 1.486(8) . ? N3 C54 1.336(7) . ? N3 C50 1.366(7) . ? N3 C49 1.486(7) . ? N4 C17 1.337(8) . ? N4 C21 1.345(9) . ? N4 C16 1.489(7) . ? N5 C11 1.354(8) . ? N5 C15 1.366(8) . ? N5 C10 1.488(7) . ? N6 C23 1.329(8) . ? N6 C27 1.347(8) . ? N6 C22 1.489(7) . ? C1 C9 1.517(9) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C5 1.513(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C7 1.498(10) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C9 1.405(9) . ? C4 C5 1.412(9) . ? C4 C10 1.502(9) . ? C5 C6 1.398(9) . ? C6 C7 1.406(9) . ? C6 C16 1.516(9) . ? C7 C8 1.393(9) . ? C8 C9 1.392(9) . ? C8 C22 1.499(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.356(8) . ? C11 H11A 0.9300 . ? C12 C13 1.423(9) . ? C12 H12A 0.9300 . ? C13 C14 1.422(9) . ? C14 C15 1.356(8) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.367(9) . ? C17 H17A 0.9300 . ? C18 C19 1.397(10) . ? C18 H18A 0.9300 . ? C19 C20 1.407(9) . ? C20 C21 1.358(9) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.360(9) . ? C23 H23A 0.9300 . ? C24 C25 1.386(9) . ? C24 H24A 0.9300 . ? C25 C26 1.393(9) . ? C26 C27 1.353(9) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C31 1.517(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C33 1.519(9) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C35 1.508(9) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.400(9) . ? C31 C36 1.400(9) . ? C32 C33 1.395(9) . ? C32 C49 1.514(8) . ? C33 C34 1.398(8) . ? C34 C35 1.401(9) . ? C34 C43 1.512(9) . ? C35 C36 1.401(9) . ? C36 C37 1.513(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.356(10) . ? C38 H38A 0.9300 . ? C39 C40 1.399(10) . ? C39 H39A 0.9300 . ? C40 C41 1.394(9) . ? C41 C42 1.381(9) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.357(9) . ? C44 H44A 0.9300 . ? C45 C46 1.415(8) . ? C45 H45A 0.9300 . ? C46 C47 1.417(9) . ? C47 C48 1.363(9) . ? C47 H47A 0.9300 . ? C48 H48A 0.9300 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.355(8) . ? C50 H50A 0.9300 . ? C51 C52 1.403(8) . ? C51 H51A 0.9300 . ? C52 C53 1.403(8) . ? C53 C54 1.367(8) . ? C53 H53A 0.9300 . ? C54 H54A 0.9300 . ? C58 C60 1.482(16) . ? C58 C59 1.545(16) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C63 1.602(13) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? O17 C63 1.286(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Gd1 O6 174.33(18) . 1_544 ? O5 Gd1 O4 102.62(16) . 2_466 ? O6 Gd1 O4 82.07(15) 1_544 2_466 ? O5 Gd1 O2 91.55(16) . 2_565 ? O6 Gd1 O2 86.14(15) 1_544 2_565 ? O4 Gd1 O2 145.89(16) 2_466 2_565 ? O5 Gd1 O1 80.54(19) . 1_455 ? O6 Gd1 O1 103.78(18) 1_544 1_455 ? O4 Gd1 O1 77.28(15) 2_466 1_455 ? O2 Gd1 O1 74.66(15) 2_565 1_455 ? O5 Gd1 O3 79.86(16) . 2_566 ? O6 Gd1 O3 98.46(16) 1_544 2_566 ? O4 Gd1 O3 75.34(14) 2_466 2_566 ? O2 Gd1 O3 138.30(14) 2_565 2_566 ? O1 Gd1 O3 141.67(15) 1_455 2_566 ? O5 Gd1 O3 90.65(16) . . ? O6 Gd1 O3 83.73(14) 1_544 . ? O4 Gd1 O3 136.72(15) 2_466 . ? O2 Gd1 O3 72.79(14) 2_565 . ? O1 Gd1 O3 145.97(14) 1_455 . ? O3 Gd1 O3 66.66(14) 2_566 . ? O5 Gd1 Gd1 84.37(14) . 2_566 ? O6 Gd1 Gd1 91.26(13) 1_544 2_566 ? O4 Gd1 Gd1 106.66(11) 2_466 2_566 ? O2 Gd1 Gd1 105.48(11) 2_565 2_566 ? O1 Gd1 Gd1 164.90(12) 1_455 2_566 ? O3 Gd1 Gd1 33.50(9) 2_566 2_566 ? O3 Gd1 Gd1 33.16(9) . 2_566 ? O8 S1 O7 114.4(3) . . ? O8 S1 O9 114.9(4) . . ? O7 S1 O9 114.9(4) . . ? O8 S1 C55 103.7(4) . . ? O7 S1 C55 104.7(4) . . ? O9 S1 C55 102.1(4) . . ? O12 S2 O11 113.9(5) . . ? O12 S2 O10 115.0(6) . . ? O11 S2 O10 114.3(7) . . ? O12 S2 C56 105.4(7) . . ? O11 S2 C56 104.1(7) . . ? O10 S2 C56 102.2(7) . . ? C40 O1 Gd1 143.1(4) . 1_655 ? C46 O2 Gd1 146.5(4) . 2_565 ? C52 O3 Gd1 123.5(4) . 2_566 ? C52 O3 Gd1 121.6(4) . . ? Gd1 O3 Gd1 113.34(14) 2_566 . ? C19 O4 Gd1 152.2(4) . 2_466 ? C25 O5 Gd1 154.4(4) . . ? C13 O6 Gd1 139.1(4) . 1_566 ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O13 S3 O15 119.9(7) . . ? O13 S3 O14 116.0(7) . . ? O15 S3 O14 112.1(5) . . ? O13 S3 C57 99.5(9) . . ? O15 S3 C57 100.8(8) . . ? O14 S3 C57 105.0(8) . . ? F8 C57 F7 109.0(11) . . ? F8 C57 F9 104.9(16) . . ? F7 C57 F9 103.5(17) . . ? F8 C57 S3 114.1(15) . . ? F7 C57 S3 116.2(15) . . ? F9 C57 S3 108.0(9) . . ? C42 N1 C38 118.6(6) . . ? C42 N1 C37 120.0(5) . . ? C38 N1 C37 120.9(6) . . ? C48 N2 C44 118.9(5) . . ? C48 N2 C43 122.4(5) . . ? C44 N2 C43 118.7(5) . . ? C54 N3 C50 119.5(5) . . ? C54 N3 C49 124.0(5) . . ? C50 N3 C49 116.5(5) . . ? C17 N4 C21 118.9(5) . . ? C17 N4 C16 122.1(6) . . ? C21 N4 C16 118.9(5) . . ? C11 N5 C15 119.3(5) . . ? C11 N5 C10 120.6(5) . . ? C15 N5 C10 120.1(5) . . ? C23 N6 C27 118.7(5) . . ? C23 N6 C22 121.7(5) . . ? C27 N6 C22 119.5(5) . . ? C9 C1 H1A 109.5 . . ? C9 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C9 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? F3 C55 F2 107.9(7) . . ? F3 C55 F1 107.8(6) . . ? F2 C55 F1 107.5(8) . . ? F3 C55 S1 111.3(7) . . ? F2 C55 S1 111.0(5) . . ? F1 C55 S1 111.1(6) . . ? C5 C2 H2A 109.5 . . ? C5 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C5 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? F5 C56 F6 106.0(12) . . ? F5 C56 F4 109.4(14) . . ? F6 C56 F4 108.6(18) . . ? F5 C56 S2 113.8(14) . . ? F6 C56 S2 109.0(10) . . ? F4 C56 S2 109.8(10) . . ? C7 C3 H3A 109.5 . . ? C7 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C7 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 119.8(6) . . ? C9 C4 C10 120.9(6) . . ? C5 C4 C10 119.3(6) . . ? C6 C5 C4 119.1(6) . . ? C6 C5 C2 121.2(6) . . ? C4 C5 C2 119.6(6) . . ? C5 C6 C7 120.8(6) . . ? C5 C6 C16 119.9(6) . . ? C7 C6 C16 119.1(6) . . ? C8 C7 C6 119.3(6) . . ? C8 C7 C3 121.3(6) . . ? C6 C7 C3 119.4(6) . . ? C9 C8 C7 120.6(6) . . ? C9 C8 C22 120.0(6) . . ? C7 C8 C22 119.3(6) . . ? C8 C9 C4 120.1(6) . . ? C8 C9 C1 119.3(6) . . ? C4 C9 C1 120.6(6) . . ? N5 C10 C4 111.6(5) . . ? N5 C10 H10A 109.3 . . ? C4 C10 H10A 109.3 . . ? N5 C10 H10B 109.3 . . ? C4 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? N5 C11 C12 121.7(6) . . ? N5 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? O6 C13 C14 123.1(6) . . ? O6 C13 C12 120.8(6) . . ? C14 C13 C12 116.1(5) . . ? C15 C14 C13 120.2(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 N5 121.8(6) . . ? C14 C15 H15A 119.1 . . ? N5 C15 H15A 119.1 . . ? N4 C16 C6 113.7(5) . . ? N4 C16 H16A 108.8 . . ? C6 C16 H16A 108.8 . . ? N4 C16 H16B 108.8 . . ? C6 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N4 C17 C18 121.2(7) . . ? N4 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C17 C18 C19 122.1(6) . . ? C17 C18 H18A 119.0 . . ? C19 C18 H18A 119.0 . . ? O4 C19 C18 123.2(6) . . ? O4 C19 C20 122.3(6) . . ? C18 C19 C20 114.5(6) . . ? C21 C20 C19 121.3(7) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? N4 C21 C20 121.9(6) . . ? N4 C21 H21A 119.0 . . ? C20 C21 H21A 119.0 . . ? N6 C22 C8 113.2(5) . . ? N6 C22 H22A 108.9 . . ? C8 C22 H22A 108.9 . . ? N6 C22 H22B 108.9 . . ? C8 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? N6 C23 C24 121.6(6) . . ? N6 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? C23 C24 C25 121.2(6) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? O5 C25 C24 122.0(6) . . ? O5 C25 C26 122.0(6) . . ? C24 C25 C26 115.9(6) . . ? C27 C26 C25 120.6(6) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? N6 C27 C26 122.0(6) . . ? N6 C27 H27A 119.0 . . ? C26 C27 H27A 119.0 . . ? C31 C28 H28A 109.5 . . ? C31 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C31 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C33 C29 H29A 109.5 . . ? C33 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C33 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 H30A 109.5 . . ? C35 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C35 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 119.4(6) . . ? C32 C31 C28 121.1(6) . . ? C36 C31 C28 119.4(6) . . ? C33 C32 C31 120.2(6) . . ? C33 C32 C49 119.8(6) . . ? C31 C32 C49 119.7(6) . . ? C32 C33 C34 119.5(6) . . ? C32 C33 C29 120.2(6) . . ? C34 C33 C29 120.3(6) . . ? C33 C34 C35 121.1(6) . . ? C33 C34 C43 119.7(6) . . ? C35 C34 C43 119.1(6) . . ? C34 C35 C36 118.4(6) . . ? C34 C35 C30 119.3(6) . . ? C36 C35 C30 122.3(6) . . ? C31 C36 C35 120.9(6) . . ? C31 C36 C37 119.2(6) . . ? C35 C36 C37 119.8(6) . . ? N1 C37 C36 113.7(5) . . ? N1 C37 H37A 108.8 . . ? C36 C37 H37A 108.8 . . ? N1 C37 H37B 108.8 . . ? C36 C37 H37B 108.8 . . ? H37A C37 H37B 107.7 . . ? C39 C38 N1 121.0(7) . . ? C39 C38 H38A 119.5 . . ? N1 C38 H38A 119.5 . . ? C38 C39 C40 122.2(7) . . ? C38 C39 H39A 118.9 . . ? C40 C39 H39A 118.9 . . ? O1 C40 C41 123.8(6) . . ? O1 C40 C39 120.3(6) . . ? C41 C40 C39 115.9(7) . . ? C42 C41 C40 120.4(6) . . ? C42 C41 H41A 119.8 . . ? C40 C41 H41A 119.8 . . ? N1 C42 C41 121.9(6) . . ? N1 C42 H42A 119.0 . . ? C41 C42 H42A 119.0 . . ? N2 C43 C34 114.6(5) . . ? N2 C43 H43A 108.6 . . ? C34 C43 H43A 108.6 . . ? N2 C43 H43B 108.6 . . ? C34 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? N2 C44 C45 121.9(6) . . ? N2 C44 H44A 119.1 . . ? C45 C44 H44A 119.1 . . ? C44 C45 C46 121.0(6) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? O2 C46 C45 121.4(6) . . ? O2 C46 C47 123.1(6) . . ? C45 C46 C47 115.5(6) . . ? C48 C47 C46 120.8(6) . . ? C48 C47 H47A 119.6 . . ? C46 C47 H47A 119.6 . . ? N2 C48 C47 121.9(6) . . ? N2 C48 H48A 119.1 . . ? C47 C48 H48A 119.1 . . ? N3 C49 C32 114.6(5) . . ? N3 C49 H49A 108.6 . . ? C32 C49 H49A 108.6 . . ? N3 C49 H49B 108.6 . . ? C32 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C51 C50 N3 120.5(6) . . ? C51 C50 H50A 119.7 . . ? N3 C50 H50A 119.7 . . ? C50 C51 C52 121.7(6) . . ? C50 C51 H51A 119.1 . . ? C52 C51 H51A 119.1 . . ? O3 C52 C53 122.2(5) . . ? O3 C52 C51 122.1(5) . . ? C53 C52 C51 115.7(5) . . ? C54 C53 C52 120.8(5) . . ? C54 C53 H53A 119.6 . . ? C52 C53 H53A 119.6 . . ? N3 C54 C53 121.6(5) . . ? N3 C54 H54A 119.2 . . ? C53 C54 H54A 119.2 . . ? O16 C58 C60 111.3(19) . . ? O16 C58 C59 119.2(19) . . ? C60 C58 C59 129(2) . . ? C58 C59 H59A 109.4 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.6 . . ? C58 C60 H60B 109.4 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.4 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C63 C61 H61A 109.5 . . ? C63 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C63 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O17 C63 C62 127.2(10) . . ? O17 C63 C61 104.5(9) . . ? C62 C63 C61 120.7(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.471 _refine_diff_density_min -1.094 _refine_diff_density_rms 0.132 #=============END