# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Cheng Li' _publ_contact_author_email CHLI@NJU.EDU.CN _publ_section_title ; Single Ion Magnets Based on Chiral Schiffbase Mononuclear Lanthanide Complex [Ln(FTA)3L] (Ln= Sm, Eu, Gd, Tb and Dy) ; loop_ _publ_author_name 'Cheng Li.' 'Dong-Ping Li.' 'Dong-Sheng Liu.' 'Tian-Wei Wang.' ; Xiao-Zeng You ; # Attachment 'Dy.cif' data_p32Dy _database_code_depnum_ccdc_archive 'CCDC 752491' #TrackingRef 'Dy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 Dy F9 N2 O11' _chemical_formula_sum 'C44 H32 Dy F9 N2 O11' _chemical_formula_weight 1098.22 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' F F 0.0171 0.0103 '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 Trigonal _symmetry_space_group_name_H-M 'P3(2) ' _symmetry_space_group_name_Hall 'P 32 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 10.4545(8) _cell_length_b 10.4545(8) _cell_length_c 34.431(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3259.0(5) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4795 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1635 _exptl_absorpt_coefficient_mu 1.821 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17610 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.99 _reflns_number_total 8415 _reflns_number_gt 6284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.027(11) _chemical_absolute_configuration unk _refine_ls_number_reflns 8415 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 0.845 _refine_ls_restrained_S_all 0.844 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3907(9) 0.3414(8) 0.2829(2) 0.0426(18) Uani 1 1 d . . . C2 C 0.4035(9) 0.3132(8) 0.2409(2) 0.0417(18) Uani 1 1 d . . . C3 C 0.3409(9) 0.3684(10) 0.2139(2) 0.0451(19) Uani 1 1 d . . . H3 H 0.2998 0.4235 0.2232 0.054 Uiso 1 1 calc R . . C4 C 0.3380(11) 0.3435(10) 0.1737(2) 0.052(2) Uani 1 1 d . . . C5 C 0.2342(8) 0.3613(8) 0.1500(2) 0.0413(18) Uani 1 1 d . . . C7 C 0.0503(9) 0.4006(9) 0.1339(2) 0.043(2) Uani 1 1 d . . . H7 H -0.0332 0.4102 0.1357 0.051 Uiso 1 1 calc R . . C8 C 0.1067(9) 0.3825(9) 0.1029(2) 0.0463(19) Uani 1 1 d . . . H8 H 0.0780 0.3929 0.0781 0.056 Uiso 1 1 calc R . . C9 C 0.2167(9) 0.3451(9) 0.1100(2) 0.050(2) Uani 1 1 d . . . H9 H 0.2653 0.3167 0.0924 0.060 Uiso 1 1 calc R . . C10 C 0.9524(8) 0.3351(9) 0.2604(2) 0.0418(18) Uani 1 1 d . . . C11 C 0.8741(8) 0.3732(9) 0.2323(2) 0.0425(18) Uani 1 1 d . . . C12 C 0.9115(9) 0.5182(9) 0.2304(2) 0.0441(18) Uani 1 1 d . . . H12 H 0.9872 0.5874 0.2460 0.053 Uiso 1 1 calc R . . C13 C 0.8336(9) 0.5651(9) 0.2042(2) 0.0464(19) Uani 1 1 d . . . C14 C 0.8892(9) 0.7272(9) 0.2041(2) 0.047(2) Uani 1 1 d . . . C15 C 1.0201(8) 0.8313(9) 0.2191(2) 0.0408(17) Uani 1 1 d . . . H15 H 1.0829 0.8139 0.2344 0.049 Uiso 1 1 calc R . . C16 C 1.0417(10) 0.9555(9) 0.2086(2) 0.048(2) Uani 1 1 d . . . H16 H 1.1287 1.0445 0.2124 0.058 Uiso 1 1 calc R . . C17 C 0.9230(10) 0.9408(9) 0.1915(3) 0.051(2) Uani 1 1 d . . . H17 H 0.9101 1.0191 0.1841 0.062 Uiso 1 1 calc R . . C19 C 0.7549(9) 0.4036(10) 0.0557(2) 0.0473(19) Uani 1 1 d . . . C20 C 0.7101(8) 0.2930(9) 0.0866(2) 0.0402(16) Uani 1 1 d . . . C21 C 0.7081(8) 0.1660(8) 0.07960(19) 0.0389(17) Uani 1 1 d . . . H21 H 0.7338 0.1494 0.0550 0.047 Uiso 1 1 calc R . . C22 C 0.6677(8) 0.0554(8) 0.1087(2) 0.0383(16) Uani 1 1 d . . . C23 C 0.6517(8) -0.0908(8) 0.0995(2) 0.0409(18) Uani 1 1 d . . . C25 C 0.6759(12) -0.2619(10) 0.0657(3) 0.063(3) Uani 1 1 d . . . H25 H 0.6988 -0.3115 0.0471 0.076 Uiso 1 1 calc R . . C26 C 0.6111(10) -0.3121(11) 0.0994(3) 0.061(2) Uani 1 1 d . . . H26 H 0.5788 -0.4071 0.1086 0.074 Uiso 1 1 calc R . . C27 C 0.5976(10) -0.2091(10) 0.1187(3) 0.053(2) Uani 1 1 d . . . H27 H 0.5541 -0.2227 0.1430 0.063 Uiso 1 1 calc R . . C28 C 0.0869(10) -0.0394(10) 0.0445(3) 0.057(2) Uani 1 1 d . . . H28 H 0.0340 -0.0565 0.0675 0.069 Uiso 1 1 calc R . . C29 C 0.0150(11) -0.0655(10) 0.0090(3) 0.059(3) Uani 1 1 d . . . H29 H -0.0860 -0.1000 0.0082 0.071 Uiso 1 1 calc R . . C30 C 0.0941(10) -0.0399(9) -0.0254(2) 0.056(2) Uani 1 1 d . . . H30 H 0.0460 -0.0574 -0.0492 0.068 Uiso 1 1 calc R . . C31 C 0.2451(11) 0.0117(10) -0.0242(3) 0.058(2) Uani 1 1 d . . . H31 H 0.2980 0.0288 -0.0472 0.069 Uiso 1 1 calc R . . C32 C 0.3170(11) 0.0378(11) 0.0114(2) 0.053(2) Uani 1 1 d . . . H32 H 0.4180 0.0723 0.0122 0.063 Uiso 1 1 calc R . . C33 C 0.2379(10) 0.0122(9) 0.0457(3) 0.047(2) Uani 1 1 d . . . C34 C 0.3190(9) 0.0402(9) 0.0848(2) 0.0428(18) Uani 1 1 d . . . H34A H 0.3916 0.0089 0.0821 0.051 Uiso 1 1 calc R . . H34B H 0.3728 0.1460 0.0891 0.051 Uiso 1 1 calc R . . C35 C 0.2313(9) -0.0306(9) 0.1203(2) 0.0459(19) Uani 1 1 d . . . H35 H 0.1666 0.0089 0.1270 0.055 Uiso 1 1 calc R . . C36 C 0.1445(11) -0.2037(10) 0.1191(3) 0.064(3) Uani 1 1 d . . . H36A H 0.0390 -0.2414 0.1210 0.076 Uiso 1 1 calc R . . H36B H 0.1645 -0.2391 0.0951 0.076 Uiso 1 1 calc R . . C37 C 0.3038(8) -0.1241(9) 0.16752(19) 0.0396(17) Uani 1 1 d . . . C38 C 0.4011(9) -0.1345(8) 0.1984(2) 0.050(2) Uani 1 1 d . . . C39 C 0.4885(10) -0.2320(10) 0.2375(2) 0.053(2) Uani 1 1 d . . . H39A H 0.5596 -0.2581 0.2278 0.063 Uiso 1 1 calc R . . H39B H 0.4482 -0.2823 0.2619 0.063 Uiso 1 1 calc R . . C40 C 0.5593(11) -0.0588(10) 0.2418(2) 0.051(2) Uani 1 1 d . . . H40 H 0.6639 -0.0126 0.2347 0.061 Uiso 1 1 calc R . . C41 C 0.5501(9) -0.0186(10) 0.2845(2) 0.0459(19) Uani 1 1 d . . . H41A H 0.6280 -0.0218 0.2991 0.055 Uiso 1 1 calc R . . H41B H 0.5697 0.0824 0.2853 0.055 Uiso 1 1 calc R . . C42 C 0.4099(9) -0.1127(10) 0.3042(2) 0.052(2) Uani 1 1 d . . . C43 C 0.4080(8) -0.2117(8) 0.33147(19) 0.0359(16) Uani 1 1 d . . . H43 H 0.4938 -0.2147 0.3367 0.043 Uiso 1 1 calc R . . C44 C 0.2779(9) -0.3063(9) 0.3509(3) 0.047(2) Uani 1 1 d . . . H44 H 0.2766 -0.3725 0.3692 0.056 Uiso 1 1 calc R . . C45 C 0.1497(10) -0.3018(11) 0.3432(2) 0.059(3) Uani 1 1 d . . . H45 H 0.0627 -0.3651 0.3562 0.071 Uiso 1 1 calc R . . C46 C 0.1517(9) -0.2027(9) 0.3159(2) 0.0446(19) Uani 1 1 d . . . H46 H 0.0659 -0.1997 0.3107 0.054 Uiso 1 1 calc R . . C47 C 0.2818(9) -0.1082(10) 0.2964(2) 0.051(2) Uani 1 1 d . . . H47 H 0.2830 -0.0419 0.2782 0.061 Uiso 1 1 calc R . . Dy1 Dy 0.57578(4) 0.22420(4) 0.177085(10) 0.04411(11) Uani 1 1 d . . . F1 F 0.2787(5) 0.2235(5) 0.29714(13) 0.0566(13) Uani 1 1 d . . . F2 F 0.3677(5) 0.4488(5) 0.29217(14) 0.0514(11) Uani 1 1 d . . . F3 F 0.4921(6) 0.3529(6) 0.30355(15) 0.0612(14) Uani 1 1 d . . . F4 F 0.8858(6) 0.2917(6) 0.29499(14) 0.0547(13) Uani 1 1 d . . . F5 F 1.0894(5) 0.4415(5) 0.26878(13) 0.0496(11) Uani 1 1 d . . . F6 F 0.9763(5) 0.2270(5) 0.24976(15) 0.0520(12) Uani 1 1 d . . . F7 F 0.8108(5) 0.3757(5) 0.02444(13) 0.0552(13) Uani 1 1 d . . . F8 F 0.6285(5) 0.4118(6) 0.04252(15) 0.0602(13) Uani 1 1 d . . . F9 F 0.8479(5) 0.5395(5) 0.06587(13) 0.0470(11) Uani 1 1 d . . . N1 N 0.4911(7) -0.0180(7) 0.21524(18) 0.0423(15) Uani 1 1 d . . . N2 N 0.3395(8) -0.0044(8) 0.1520(2) 0.0495(17) Uani 1 1 d . . . O1 O 0.4721(6) 0.2520(6) 0.23259(14) 0.0424(12) Uani 1 1 d . . . O2 O 0.4140(6) 0.2962(6) 0.15714(14) 0.0416(12) Uani 1 1 d . . . O3 O 0.7662(6) 0.2642(6) 0.21545(17) 0.0448(13) Uani 1 1 d . . . O4 O 0.7243(5) 0.4856(6) 0.18761(16) 0.0421(12) Uani 1 1 d . . . O5 O 0.6726(6) 0.3261(6) 0.11683(17) 0.0468(13) Uani 1 1 d . . . O6 O 0.6391(7) 0.0648(6) 0.14175(15) 0.0420(13) Uani 1 1 d . . . O7 O 0.3715(6) -0.2654(6) 0.20895(16) 0.0463(13) Uani 1 1 d . . . O8 O 0.1945(6) -0.2491(6) 0.15101(16) 0.0516(14) Uani 1 1 d . . . O9 O 0.1410(6) 0.4032(6) 0.16499(16) 0.0480(13) Uani 1 1 d . . . O10 O 0.8127(7) 0.7839(7) 0.18570(17) 0.0551(15) Uani 1 1 d . . . O11 O 0.7025(6) -0.1172(6) 0.06430(16) 0.0504(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(5) 0.031(4) 0.042(4) -0.005(3) -0.007(4) 0.017(4) C2 0.053(5) 0.032(4) 0.033(4) 0.006(3) 0.000(3) 0.016(4) C3 0.045(4) 0.054(5) 0.036(4) 0.003(4) 0.002(3) 0.025(4) C4 0.073(6) 0.062(6) 0.026(4) 0.006(3) -0.001(4) 0.038(5) C5 0.034(4) 0.038(4) 0.033(4) 0.015(3) 0.002(3) 0.004(3) C7 0.028(4) 0.037(4) 0.041(4) 0.010(3) 0.002(3) 0.000(3) C8 0.047(5) 0.046(5) 0.038(4) 0.001(3) -0.009(3) 0.018(4) C9 0.040(4) 0.053(5) 0.054(5) 0.002(4) -0.002(4) 0.021(4) C10 0.038(4) 0.032(4) 0.045(4) -0.016(3) -0.011(3) 0.009(3) C11 0.036(4) 0.048(5) 0.037(4) 0.003(3) 0.010(3) 0.015(4) C12 0.048(5) 0.043(4) 0.040(4) -0.005(3) -0.003(3) 0.021(4) C13 0.054(5) 0.037(4) 0.030(4) -0.004(3) -0.006(3) 0.009(4) C14 0.032(4) 0.036(4) 0.051(5) 0.015(4) -0.003(3) 0.002(3) C15 0.041(4) 0.047(5) 0.030(4) -0.014(3) -0.007(3) 0.019(4) C16 0.050(5) 0.032(4) 0.035(4) -0.017(3) 0.007(3) 0.000(4) C17 0.058(5) 0.041(4) 0.052(5) 0.014(4) 0.020(4) 0.021(4) C19 0.038(4) 0.050(5) 0.041(4) 0.012(4) 0.010(3) 0.013(4) C20 0.034(4) 0.045(4) 0.038(4) 0.002(3) -0.006(3) 0.017(3) C21 0.040(4) 0.045(4) 0.025(4) -0.004(3) -0.004(3) 0.016(4) C22 0.027(4) 0.038(4) 0.039(4) 0.000(3) -0.004(3) 0.008(3) C23 0.020(3) 0.033(4) 0.044(4) -0.009(3) -0.001(3) -0.005(3) C25 0.077(6) 0.040(5) 0.060(5) -0.007(4) 0.012(5) 0.019(5) C26 0.060(5) 0.058(5) 0.065(6) 0.004(4) 0.030(5) 0.028(5) C27 0.057(5) 0.049(5) 0.054(5) 0.000(4) 0.012(4) 0.029(4) C28 0.041(5) 0.048(5) 0.069(6) 0.018(4) -0.012(4) 0.012(4) C29 0.046(5) 0.037(5) 0.062(6) -0.009(4) -0.014(4) -0.004(4) C30 0.050(5) 0.044(5) 0.043(5) -0.007(4) -0.025(4) -0.001(4) C31 0.075(6) 0.066(6) 0.052(5) -0.030(4) -0.026(4) 0.050(5) C32 0.065(6) 0.078(6) 0.033(4) -0.020(4) -0.022(4) 0.049(5) C33 0.043(5) 0.043(5) 0.047(5) -0.014(4) -0.015(4) 0.015(4) C34 0.038(4) 0.040(4) 0.039(4) -0.013(3) -0.007(3) 0.011(3) C35 0.032(4) 0.042(4) 0.051(5) -0.005(4) -0.004(3) 0.008(4) C36 0.049(5) 0.050(5) 0.050(5) -0.013(4) -0.013(4) -0.007(4) C37 0.031(4) 0.044(4) 0.021(3) -0.001(3) 0.002(3) 0.002(3) C38 0.036(4) 0.029(4) 0.053(5) 0.003(3) -0.007(3) -0.009(3) C39 0.055(5) 0.044(5) 0.047(5) 0.009(4) 0.004(4) 0.015(4) C40 0.062(5) 0.046(5) 0.037(4) -0.006(3) -0.010(4) 0.022(4) C41 0.034(4) 0.061(5) 0.034(4) 0.005(4) 0.000(3) 0.017(4) C42 0.034(4) 0.044(5) 0.042(4) -0.005(4) -0.012(3) -0.009(4) C43 0.037(4) 0.043(4) 0.026(3) -0.005(3) 0.002(3) 0.019(3) C44 0.040(4) 0.028(4) 0.054(5) 0.003(3) 0.013(3) 0.003(3) C45 0.046(5) 0.079(7) 0.043(5) -0.006(5) 0.014(4) 0.024(5) C46 0.038(4) 0.046(4) 0.045(4) -0.019(4) 0.000(3) 0.017(4) C47 0.040(4) 0.052(5) 0.044(4) -0.020(4) -0.012(3) 0.011(4) Dy1 0.0429(2) 0.0395(2) 0.03645(16) -0.00446(17) -0.00503(18) 0.01044(18) F1 0.058(3) 0.053(3) 0.044(2) -0.014(2) 0.011(2) 0.016(2) F2 0.052(3) 0.047(3) 0.050(3) -0.022(2) -0.011(2) 0.021(2) F3 0.054(3) 0.061(3) 0.057(3) 0.009(2) -0.022(2) 0.020(3) F4 0.054(3) 0.057(3) 0.051(3) 0.021(2) 0.000(2) 0.026(3) F5 0.045(3) 0.048(3) 0.047(3) -0.015(2) -0.016(2) 0.016(2) F6 0.042(3) 0.035(2) 0.076(3) -0.015(2) -0.017(2) 0.017(2) F7 0.061(3) 0.051(3) 0.038(2) -0.009(2) -0.002(2) 0.016(2) F8 0.053(3) 0.062(3) 0.056(3) 0.022(2) -0.007(2) 0.021(3) F9 0.053(3) 0.039(3) 0.040(2) -0.0006(19) -0.001(2) 0.016(2) N1 0.041(4) 0.045(4) 0.036(3) -0.004(3) 0.003(3) 0.018(3) N2 0.049(4) 0.044(4) 0.047(4) -0.015(3) -0.014(3) 0.017(3) O1 0.040(3) 0.044(3) 0.038(3) -0.003(2) -0.001(2) 0.017(3) O2 0.034(3) 0.038(3) 0.034(3) -0.001(2) -0.004(2) 0.004(2) O3 0.038(3) 0.036(3) 0.049(3) 0.000(2) -0.006(2) 0.011(2) O4 0.027(3) 0.041(3) 0.051(3) 0.002(2) -0.006(2) 0.012(2) O5 0.044(3) 0.041(3) 0.051(3) -0.005(3) -0.005(2) 0.018(3) O6 0.052(4) 0.041(3) 0.030(3) 0.013(2) 0.005(2) 0.021(3) O7 0.043(3) 0.038(3) 0.049(3) -0.007(2) 0.002(2) 0.014(2) O8 0.029(3) 0.047(3) 0.053(3) -0.009(3) -0.013(2) 0.000(2) O9 0.040(3) 0.049(3) 0.046(3) -0.014(3) -0.011(3) 0.016(3) O10 0.068(4) 0.050(3) 0.051(3) -0.017(3) -0.021(3) 0.032(3) O11 0.048(3) 0.046(3) 0.048(3) -0.010(3) 0.008(3) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F3 1.233(9) . ? C1 F1 1.300(9) . ? C1 F2 1.301(9) . ? C1 C2 1.495(11) . ? C2 O1 1.209(10) . ? C2 C3 1.415(11) . ? C3 C4 1.406(11) . ? C3 H3 0.9300 . ? C4 O2 1.262(10) . ? C4 C5 1.441(11) . ? C5 O9 1.354(10) . ? C5 C9 1.389(11) . ? C7 C8 1.279(12) . ? C7 O9 1.421(9) . ? C7 H7 0.9300 . ? C8 C9 1.409(12) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 F6 1.325(9) . ? C10 F5 1.334(8) . ? C10 F4 1.339(10) . ? C10 C11 1.447(11) . ? C11 O3 1.274(9) . ? C11 C12 1.364(11) . ? C12 C13 1.455(12) . ? C12 H12 0.9300 . ? C13 O4 1.172(9) . ? C13 C14 1.492(11) . ? C14 C15 1.354(11) . ? C14 O10 1.366(10) . ? C15 C16 1.254(12) . ? C15 H15 0.9300 . ? C16 C17 1.311(13) . ? C16 H16 0.9300 . ? C17 O10 1.472(10) . ? C17 H17 0.9300 . ? C19 F9 1.305(10) . ? C19 F7 1.325(10) . ? C19 F8 1.440(10) . ? C19 C20 1.464(11) . ? C20 O5 1.223(9) . ? C20 C21 1.340(11) . ? C21 C22 1.424(10) . ? C21 H21 0.9300 . ? C22 O6 1.194(9) . ? C22 C23 1.486(11) . ? C23 C27 1.259(12) . ? C23 O11 1.405(9) . ? C25 C26 1.312(13) . ? C25 O11 1.395(11) . ? C25 H25 0.9300 . ? C26 C27 1.330(12) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.390(13) . ? C28 C33 1.390(12) . ? C28 H28 0.9300 . ? C29 C30 1.390(13) . ? C29 H29 0.9300 . ? C30 C31 1.390(13) . ? C30 H30 0.9300 . ? C31 C32 1.390(11) . ? C31 H31 0.9300 . ? C32 C33 1.390(13) . ? C32 H32 0.9300 . ? C33 C34 1.538(11) . ? C34 C35 1.485(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N2 1.496(10) . ? C35 C36 1.568(12) . ? C35 H35 0.9800 . ? C36 O8 1.398(11) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 N2 1.235(10) . ? C37 O8 1.358(9) . ? C37 C38 1.514(11) . ? C38 N1 1.248(10) . ? C38 O7 1.294(10) . ? C39 O7 1.469(10) . ? C39 C40 1.583(12) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 N1 1.354(11) . ? C40 C41 1.547(11) . ? C40 H40 0.9800 . ? C41 C42 1.461(11) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.390(12) . ? C42 C47 1.390(13) . ? C43 C44 1.390(10) . ? C43 H43 0.9300 . ? C44 C45 1.390(13) . ? C44 H44 0.9300 . ? C45 C46 1.390(13) . ? C45 H45 0.9300 . ? C46 C47 1.390(12) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? Dy1 O3 2.248(5) . ? Dy1 O2 2.274(6) . ? Dy1 O1 2.286(5) . ? Dy1 O5 2.320(6) . ? Dy1 O4 2.401(5) . ? Dy1 O6 2.408(6) . ? Dy1 N2 2.580(6) . ? Dy1 N1 2.584(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 C1 F1 101.4(6) . . ? F3 C1 F2 107.2(6) . . ? F1 C1 F2 104.9(7) . . ? F3 C1 C2 114.8(8) . . ? F1 C1 C2 107.8(6) . . ? F2 C1 C2 118.8(7) . . ? O1 C2 C3 125.3(7) . . ? O1 C2 C1 117.9(7) . . ? C3 C2 C1 116.6(7) . . ? C4 C3 C2 122.8(8) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? O2 C4 C3 123.9(8) . . ? O2 C4 C5 117.2(7) . . ? C3 C4 C5 118.7(8) . . ? O9 C5 C9 110.1(7) . . ? O9 C5 C4 122.5(7) . . ? C9 C5 C4 127.4(8) . . ? C8 C7 O9 106.2(8) . . ? C8 C7 H7 126.9 . . ? O9 C7 H7 126.9 . . ? C7 C8 C9 113.3(8) . . ? C7 C8 H8 123.3 . . ? C9 C8 H8 123.3 . . ? C5 C9 C8 102.4(8) . . ? C5 C9 H9 128.8 . . ? C8 C9 H9 128.8 . . ? F6 C10 F5 100.9(6) . . ? F6 C10 F4 104.2(7) . . ? F5 C10 F4 104.5(6) . . ? F6 C10 C11 115.0(6) . . ? F5 C10 C11 115.7(7) . . ? F4 C10 C11 114.8(7) . . ? O3 C11 C12 127.4(8) . . ? O3 C11 C10 115.3(7) . . ? C12 C11 C10 116.7(7) . . ? C11 C12 C13 120.4(7) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? O4 C13 C12 125.1(7) . . ? O4 C13 C14 119.5(8) . . ? C12 C13 C14 114.8(7) . . ? C15 C14 O10 113.8(7) . . ? C15 C14 C13 125.1(8) . . ? O10 C14 C13 120.9(7) . . ? C16 C15 C14 108.0(8) . . ? C16 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? C15 C16 C17 109.7(7) . . ? C15 C16 H16 125.1 . . ? C17 C16 H16 125.1 . . ? C16 C17 O10 111.1(7) . . ? C16 C17 H17 124.5 . . ? O10 C17 H17 124.5 . . ? F9 C19 F7 106.7(6) . . ? F9 C19 F8 103.1(7) . . ? F7 C19 F8 106.0(6) . . ? F9 C19 C20 115.7(7) . . ? F7 C19 C20 114.7(8) . . ? F8 C19 C20 109.6(6) . . ? O5 C20 C21 125.8(7) . . ? O5 C20 C19 114.6(7) . . ? C21 C20 C19 119.6(7) . . ? C20 C21 C22 122.0(7) . . ? C20 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? O6 C22 C21 126.1(7) . . ? O6 C22 C23 112.5(7) . . ? C21 C22 C23 121.4(7) . . ? C27 C23 O11 106.7(7) . . ? C27 C23 C22 131.6(8) . . ? O11 C23 C22 121.7(7) . . ? C26 C25 O11 104.4(8) . . ? C26 C25 H25 127.8 . . ? O11 C25 H25 127.8 . . ? C25 C26 C27 111.0(9) . . ? C25 C26 H26 124.5 . . ? C27 C26 H26 124.5 . . ? C23 C27 C26 110.9(9) . . ? C23 C27 H27 124.6 . . ? C26 C27 H27 124.6 . . ? C29 C28 C33 120.0(10) . . ? C29 C28 H28 120.0 . . ? C33 C28 H28 120.0 . . ? C28 C29 C30 120.0(9) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.0(8) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.0(9) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.0(9) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.0(8) . . ? C32 C33 C34 119.3(7) . . ? C28 C33 C34 120.7(8) . . ? C35 C34 C33 118.8(7) . . ? C35 C34 H34A 107.6 . . ? C33 C34 H34A 107.6 . . ? C35 C34 H34B 107.6 . . ? C33 C34 H34B 107.6 . . ? H34A C34 H34B 107.1 . . ? C34 C35 N2 106.7(6) . . ? C34 C35 C36 114.2(7) . . ? N2 C35 C36 100.3(7) . . ? C34 C35 H35 111.6 . . ? N2 C35 H35 111.6 . . ? C36 C35 H35 111.6 . . ? O8 C36 C35 105.8(6) . . ? O8 C36 H36A 110.6 . . ? C35 C36 H36A 110.6 . . ? O8 C36 H36B 110.6 . . ? C35 C36 H36B 110.6 . . ? H36A C36 H36B 108.7 . . ? N2 C37 O8 118.5(7) . . ? N2 C37 C38 120.3(6) . . ? O8 C37 C38 119.9(7) . . ? N1 C38 O7 124.6(8) . . ? N1 C38 C37 117.5(8) . . ? O7 C38 C37 117.3(6) . . ? O7 C39 C40 101.1(6) . . ? O7 C39 H39A 111.6 . . ? C40 C39 H39A 111.6 . . ? O7 C39 H39B 111.6 . . ? C40 C39 H39B 111.6 . . ? H39A C39 H39B 109.4 . . ? N1 C40 C41 116.3(8) . . ? N1 C40 C39 106.2(7) . . ? C41 C40 C39 110.0(7) . . ? N1 C40 H40 108.0 . . ? C41 C40 H40 108.0 . . ? C39 C40 H40 108.0 . . ? C42 C41 C40 115.9(7) . . ? C42 C41 H41A 108.3 . . ? C40 C41 H41A 108.3 . . ? C42 C41 H41B 108.3 . . ? C40 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C43 C42 C47 120.0(8) . . ? C43 C42 C41 116.8(8) . . ? C47 C42 C41 123.2(8) . . ? C44 C43 C42 120.0(8) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0(8) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0(8) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0(8) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C42 120.0(9) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? O3 Dy1 O2 148.5(2) . . ? O3 Dy1 O1 85.3(2) . . ? O2 Dy1 O1 74.46(19) . . ? O3 Dy1 O5 107.3(2) . . ? O2 Dy1 O5 78.70(19) . . ? O1 Dy1 O5 144.6(2) . . ? O3 Dy1 O4 72.01(19) . . ? O2 Dy1 O4 80.43(17) . . ? O1 Dy1 O4 78.87(19) . . ? O5 Dy1 O4 74.16(19) . . ? O3 Dy1 O6 84.3(2) . . ? O2 Dy1 O6 125.70(18) . . ? O1 Dy1 O6 145.31(18) . . ? O5 Dy1 O6 70.02(18) . . ? O4 Dy1 O6 128.23(19) . . ? O3 Dy1 N2 135.9(2) . . ? O2 Dy1 N2 71.3(2) . . ? O1 Dy1 N2 95.9(2) . . ? O5 Dy1 N2 97.0(2) . . ? O4 Dy1 N2 151.6(2) . . ? O6 Dy1 N2 69.9(2) . . ? O3 Dy1 N1 73.8(2) . . ? O2 Dy1 N1 122.04(19) . . ? O1 Dy1 N1 75.39(19) . . ? O5 Dy1 N1 139.58(19) . . ? O4 Dy1 N1 138.42(19) . . ? O6 Dy1 N1 69.93(18) . . ? N2 Dy1 N1 64.0(2) . . ? C38 N1 C40 105.3(7) . . ? C38 N1 Dy1 116.3(5) . . ? C40 N1 Dy1 132.5(5) . . ? C37 N2 C35 108.2(6) . . ? C37 N2 Dy1 117.3(5) . . ? C35 N2 Dy1 134.4(5) . . ? C2 O1 Dy1 135.1(5) . . ? C4 O2 Dy1 135.3(5) . . ? C11 O3 Dy1 137.7(5) . . ? C13 O4 Dy1 136.6(5) . . ? C20 O5 Dy1 139.5(5) . . ? C22 O6 Dy1 134.9(5) . . ? C38 O7 C39 101.8(6) . . ? C37 O8 C36 106.3(6) . . ? C5 O9 C7 106.8(6) . . ? C14 O10 C17 96.8(6) . . ? C25 O11 C23 107.0(6) . . ? 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 F3 C1 C2 O1 26.5(10) . . . . ? F1 C1 C2 O1 -85.6(9) . . . . ? F2 C1 C2 O1 155.3(7) . . . . ? F3 C1 C2 C3 -150.0(7) . . . . ? F1 C1 C2 C3 97.9(8) . . . . ? F2 C1 C2 C3 -21.2(11) . . . . ? O1 C2 C3 C4 7.1(14) . . . . ? C1 C2 C3 C4 -176.6(8) . . . . ? C2 C3 C4 O2 -14.2(14) . . . . ? C2 C3 C4 C5 160.6(8) . . . . ? O2 C4 C5 O9 176.2(7) . . . . ? C3 C4 C5 O9 1.0(12) . . . . ? O2 C4 C5 C9 -6.4(13) . . . . ? C3 C4 C5 C9 178.5(8) . . . . ? O9 C7 C8 C9 10.8(10) . . . . ? O9 C5 C9 C8 0.6(9) . . . . ? C4 C5 C9 C8 -177.1(8) . . . . ? C7 C8 C9 C5 -7.4(10) . . . . ? F6 C10 C11 O3 41.9(10) . . . . ? F5 C10 C11 O3 159.0(7) . . . . ? F4 C10 C11 O3 -79.1(9) . . . . ? F6 C10 C11 C12 -146.2(7) . . . . ? F5 C10 C11 C12 -29.0(10) . . . . ? F4 C10 C11 C12 92.9(9) . . . . ? O3 C11 C12 C13 -6.4(13) . . . . ? C10 C11 C12 C13 -177.2(7) . . . . ? C11 C12 C13 O4 11.5(13) . . . . ? C11 C12 C13 C14 -177.9(8) . . . . ? O4 C13 C14 C15 -173.7(8) . . . . ? C12 C13 C14 C15 15.2(13) . . . . ? O4 C13 C14 O10 1.5(13) . . . . ? C12 C13 C14 O10 -169.6(7) . . . . ? O10 C14 C15 C16 -5.9(10) . . . . ? C13 C14 C15 C16 169.6(8) . . . . ? C14 C15 C16 C17 8.1(10) . . . . ? C15 C16 C17 O10 -7.6(10) . . . . ? F9 C19 C20 O5 48.0(10) . . . . ? F7 C19 C20 O5 173.0(7) . . . . ? F8 C19 C20 O5 -68.0(9) . . . . ? F9 C19 C20 C21 -134.2(8) . . . . ? F7 C19 C20 C21 -9.3(11) . . . . ? F8 C19 C20 C21 109.8(8) . . . . ? O5 C20 C21 C22 -3.5(12) . . . . ? C19 C20 C21 C22 179.0(7) . . . . ? C20 C21 C22 O6 -3.7(12) . . . . ? C20 C21 C22 C23 173.9(7) . . . . ? O6 C22 C23 C27 9.7(13) . . . . ? C21 C22 C23 C27 -168.2(9) . . . . ? O6 C22 C23 O11 -169.5(7) . . . . ? C21 C22 C23 O11 12.6(11) . . . . ? O11 C25 C26 C27 -0.7(12) . . . . ? O11 C23 C27 C26 1.3(11) . . . . ? C22 C23 C27 C26 -177.9(8) . . . . ? C25 C26 C27 C23 -0.4(13) . . . . ? C33 C28 C29 C30 0.0(14) . . . . ? C28 C29 C30 C31 0.0(14) . . . . ? C29 C30 C31 C32 0.0(14) . . . . ? C30 C31 C32 C33 0.0(14) . . . . ? C31 C32 C33 C28 0.0(14) . . . . ? C31 C32 C33 C34 179.4(8) . . . . ? C29 C28 C33 C32 0.0(14) . . . . ? C29 C28 C33 C34 -179.4(8) . . . . ? C32 C33 C34 C35 -160.5(8) . . . . ? C28 C33 C34 C35 18.9(13) . . . . ? C33 C34 C35 N2 171.0(7) . . . . ? C33 C34 C35 C36 61.1(11) . . . . ? C34 C35 C36 O8 121.8(8) . . . . ? N2 C35 C36 O8 8.0(9) . . . . ? N2 C37 C38 N1 20.0(12) . . . . ? O8 C37 C38 N1 -173.6(7) . . . . ? N2 C37 C38 O7 -168.9(8) . . . . ? O8 C37 C38 O7 -2.5(11) . . . . ? O7 C39 C40 N1 -5.4(9) . . . . ? O7 C39 C40 C41 121.2(7) . . . . ? N1 C40 C41 C42 77.3(11) . . . . ? C39 C40 C41 C42 -43.4(11) . . . . ? C40 C41 C42 C43 106.1(9) . . . . ? C40 C41 C42 C47 -72.9(12) . . . . ? C47 C42 C43 C44 0.0(12) . . . . ? C41 C42 C43 C44 -179.1(7) . . . . ? C42 C43 C44 C45 0.0(12) . . . . ? C43 C44 C45 C46 0.0(12) . . . . ? C44 C45 C46 C47 0.0(12) . . . . ? C45 C46 C47 C42 0.0(12) . . . . ? C43 C42 C47 C46 0.0(12) . . . . ? C41 C42 C47 C46 179.0(8) . . . . ? O7 C38 N1 C40 7.7(12) . . . . ? C37 C38 N1 C40 178.2(7) . . . . ? O7 C38 N1 Dy1 164.2(7) . . . . ? C37 C38 N1 Dy1 -25.4(10) . . . . ? C41 C40 N1 C38 -123.0(8) . . . . ? C39 C40 N1 C38 -0.2(9) . . . . ? C41 C40 N1 Dy1 86.1(9) . . . . ? C39 C40 N1 Dy1 -151.1(6) . . . . ? O3 Dy1 N1 C38 -149.6(7) . . . . ? O2 Dy1 N1 C38 60.5(7) . . . . ? O1 Dy1 N1 C38 121.2(7) . . . . ? O5 Dy1 N1 C38 -51.7(8) . . . . ? O4 Dy1 N1 C38 174.7(6) . . . . ? O6 Dy1 N1 C38 -59.8(6) . . . . ? N2 Dy1 N1 C38 17.1(6) . . . . ? O3 Dy1 N1 C40 -1.1(7) . . . . ? O2 Dy1 N1 C40 -151.0(7) . . . . ? O1 Dy1 N1 C40 -90.3(7) . . . . ? O5 Dy1 N1 C40 96.8(7) . . . . ? O4 Dy1 N1 C40 -36.8(8) . . . . ? O6 Dy1 N1 C40 88.7(7) . . . . ? N2 Dy1 N1 C40 165.5(8) . . . . ? O8 C37 N2 C35 8.0(10) . . . . ? C38 C37 N2 C35 174.6(7) . . . . ? O8 C37 N2 Dy1 -169.6(5) . . . . ? C38 C37 N2 Dy1 -3.1(10) . . . . ? C34 C35 N2 C37 -128.7(8) . . . . ? C36 C35 N2 C37 -9.4(9) . . . . ? C34 C35 N2 Dy1 48.3(10) . . . . ? C36 C35 N2 Dy1 167.7(6) . . . . ? O3 Dy1 N2 C37 12.4(8) . . . . ? O2 Dy1 N2 C37 -148.2(7) . . . . ? O1 Dy1 N2 C37 -76.9(6) . . . . ? O5 Dy1 N2 C37 136.2(6) . . . . ? O4 Dy1 N2 C37 -154.3(5) . . . . ? O6 Dy1 N2 C37 70.5(6) . . . . ? N1 Dy1 N2 C37 -6.3(6) . . . . ? O3 Dy1 N2 C35 -164.5(7) . . . . ? O2 Dy1 N2 C35 34.9(7) . . . . ? O1 Dy1 N2 C35 106.3(7) . . . . ? O5 Dy1 N2 C35 -40.6(8) . . . . ? O4 Dy1 N2 C35 28.8(10) . . . . ? O6 Dy1 N2 C35 -106.3(8) . . . . ? N1 Dy1 N2 C35 176.9(8) . . . . ? C3 C2 O1 Dy1 13.0(13) . . . . ? C1 C2 O1 Dy1 -163.2(5) . . . . ? O3 Dy1 O1 C2 138.4(7) . . . . ? O2 Dy1 O1 C2 -17.2(7) . . . . ? O5 Dy1 O1 C2 24.9(9) . . . . ? O4 Dy1 O1 C2 65.8(7) . . . . ? O6 Dy1 O1 C2 -148.7(7) . . . . ? N2 Dy1 O1 C2 -85.9(7) . . . . ? N1 Dy1 O1 C2 -147.1(8) . . . . ? C3 C4 O2 Dy1 1.8(14) . . . . ? C5 C4 O2 Dy1 -173.1(5) . . . . ? O3 Dy1 O2 C4 -42.3(9) . . . . ? O1 Dy1 O2 C4 9.6(8) . . . . ? O5 Dy1 O2 C4 -147.1(8) . . . . ? O4 Dy1 O2 C4 -71.4(8) . . . . ? O6 Dy1 O2 C4 157.9(7) . . . . ? N2 Dy1 O2 C4 111.5(8) . . . . ? N1 Dy1 O2 C4 70.7(8) . . . . ? C12 C11 O3 Dy1 -2.3(13) . . . . ? C10 C11 O3 Dy1 168.6(6) . . . . ? O2 Dy1 O3 C11 -25.9(9) . . . . ? O1 Dy1 O3 C11 -75.4(7) . . . . ? O5 Dy1 O3 C11 70.7(8) . . . . ? O4 Dy1 O3 C11 4.4(7) . . . . ? O6 Dy1 O3 C11 137.7(7) . . . . ? N2 Dy1 O3 C11 -169.0(7) . . . . ? N1 Dy1 O3 C11 -151.6(8) . . . . ? C12 C13 O4 Dy1 -8.6(13) . . . . ? C14 C13 O4 Dy1 -178.8(5) . . . . ? O3 Dy1 O4 C13 1.3(8) . . . . ? O2 Dy1 O4 C13 165.8(8) . . . . ? O1 Dy1 O4 C13 89.9(8) . . . . ? O5 Dy1 O4 C13 -113.4(8) . . . . ? O6 Dy1 O4 C13 -65.9(8) . . . . ? N2 Dy1 O4 C13 171.6(7) . . . . ? N1 Dy1 O4 C13 37.4(9) . . . . ? C21 C20 O5 Dy1 -2.4(13) . . . . ? C19 C20 O5 Dy1 175.2(5) . . . . ? O3 Dy1 O5 C20 85.2(8) . . . . ? O2 Dy1 O5 C20 -126.8(8) . . . . ? O1 Dy1 O5 C20 -168.1(7) . . . . ? O4 Dy1 O5 C20 150.0(8) . . . . ? O6 Dy1 O5 C20 8.1(7) . . . . ? N2 Dy1 O5 C20 -57.6(8) . . . . ? N1 Dy1 O5 C20 0.0(9) . . . . ? C21 C22 O6 Dy1 16.4(12) . . . . ? C23 C22 O6 Dy1 -161.4(5) . . . . ? O3 Dy1 O6 C22 -125.6(8) . . . . ? O2 Dy1 O6 C22 44.0(8) . . . . ? O1 Dy1 O6 C22 161.2(6) . . . . ? O5 Dy1 O6 C22 -14.8(7) . . . . ? O4 Dy1 O6 C22 -63.8(8) . . . . ? N2 Dy1 O6 C22 90.9(8) . . . . ? N1 Dy1 O6 C22 159.6(8) . . . . ? N1 C38 O7 C39 -11.3(11) . . . . ? C37 C38 O7 C39 178.2(7) . . . . ? C40 C39 O7 C38 8.5(8) . . . . ? N2 C37 O8 C36 -2.3(10) . . . . ? C38 C37 O8 C36 -168.9(8) . . . . ? C35 C36 O8 C37 -4.3(9) . . . . ? C9 C5 O9 C7 5.5(8) . . . . ? C4 C5 O9 C7 -176.7(7) . . . . ? C8 C7 O9 C5 -9.9(8) . . . . ? C15 C14 O10 C17 1.3(9) . . . . ? C13 C14 O10 C17 -174.5(8) . . . . ? C16 C17 O10 C14 3.6(9) . . . . ? C26 C25 O11 C23 1.4(10) . . . . ? C27 C23 O11 C25 -1.7(10) . . . . ? C22 C23 O11 C25 177.6(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.958 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.092 # Attachment 'Gd.cif' data_90630c _database_code_depnum_ccdc_archive 'CCDC 752492' #TrackingRef 'Gd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 F9 Gd N2 O11' _chemical_formula_sum 'C44 H32 F9 Gd N2 O11' _chemical_formula_weight 1092.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P3(2) ' _symmetry_space_group_name_Hall 'P 32 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 10.4887(10) _cell_length_b 10.4887(10) _cell_length_c 34.490(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3286.0(6) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5932 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 25.14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1629 _exptl_absorpt_coefficient_mu 1.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16945 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.34 _reflns_number_total 7504 _reflns_number_gt 6064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(11) _chemical_absolute_configuration unk _refine_ls_number_reflns 7504 _refine_ls_number_parameters 580 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.2835(10) 1.2853(9) 0.3486(3) 0.051(2) Uani 1 1 d . . . C2 C 1.1639(8) 1.2030(9) 0.3187(2) 0.0460(19) Uani 1 1 d . . . C3 C 1.0580(8) 1.2412(8) 0.3167(2) 0.0432(18) Uani 1 1 d . . . H3 H 1.0670 1.3168 0.3326 0.052 Uiso 1 1 calc R . . C4 C 0.9352(8) 1.1723(9) 0.29173(19) 0.0423(18) Uani 1 1 d . . . C5 C 0.8235(9) 1.2215(8) 0.2890(2) 0.0433(18) Uani 1 1 d . . . C6 C 0.6990(9) 1.1519(9) 0.2714(2) 0.0443(17) Uani 1 1 d . . . H6 H 0.6554 1.0611 0.2590 0.053 Uiso 1 1 calc R . . C7 C 0.6466(9) 1.2513(9) 0.2761(3) 0.053(2) Uani 1 1 d . . . H7 H 0.5559 1.2328 0.2667 0.063 Uiso 1 1 calc R . . C8 C 0.7339(9) 1.3686(10) 0.2944(2) 0.0493(19) Uani 1 1 d . . . H8 H 0.7194 1.4474 0.2998 0.059 Uiso 1 1 calc R . . C9 C 1.0190(9) 1.0862(9) 0.1401(2) 0.0460(18) Uani 1 1 d . . . C10 C 1.0822(8) 1.0437(8) 0.1709(2) 0.0439(17) Uani 1 1 d . . . C11 C 1.2088(9) 1.0389(9) 0.1653(2) 0.0481(19) Uani 1 1 d . . . H11 H 1.2504 1.0622 0.1407 0.058 Uiso 1 1 calc R . . C12 C 1.2836(8) 1.0010(8) 0.1941(2) 0.0456(19) Uani 1 1 d . . . C13 C 1.4066(9) 0.9892(10) 0.1837(2) 0.049(2) Uani 1 1 d . . . C14 C 1.4734(8) 0.9417(9) 0.2042(3) 0.056(2) Uani 1 1 d . . . H14 H 1.4481 0.9094 0.2296 0.067 Uiso 1 1 calc R . . C15 C 1.5838(8) 0.9432(9) 0.1853(2) 0.050(2) Uani 1 1 d . . . H15 H 1.6428 0.9079 0.1952 0.060 Uiso 1 1 calc R . . C16 C 1.5993(9) 1.0005(9) 0.1508(2) 0.052(2) Uani 1 1 d . . . H16 H 1.6707 1.0201 0.1321 0.062 Uiso 1 1 calc R . . C17 C 0.7116(10) 0.7288(10) 0.3676(3) 0.052(2) Uani 1 1 d . . . C18 C 0.7481(9) 0.7325(8) 0.3250(2) 0.0416(17) Uani 1 1 d . . . C19 C 0.6335(9) 0.6689(9) 0.3002(2) 0.046(2) Uani 1 1 d . . . H19 H 0.5379 0.6272 0.3097 0.055 Uiso 1 1 calc R . . C20 C 0.6570(8) 0.6647(9) 0.2596(2) 0.048(2) Uani 1 1 d . . . C21 C 0.5332(8) 0.5685(8) 0.2343(2) 0.0428(17) Uani 1 1 d . . . C22 C 0.5283(10) 0.5476(8) 0.1974(3) 0.057(2) Uani 1 1 d . . . H22 H 0.6051 0.5985 0.1800 0.069 Uiso 1 1 calc R . . C23 C 0.3848(9) 0.4330(9) 0.1882(2) 0.052(2) Uani 1 1 d . . . H23 H 0.3487 0.3986 0.1635 0.062 Uiso 1 1 calc R . . C24 C 0.3154(10) 0.3864(10) 0.2191(2) 0.048(2) Uani 1 1 d . . . H24 H 0.2194 0.3082 0.2208 0.057 Uiso 1 1 calc R . . C25 C 1.2853(4) 0.7405(5) 0.41669(15) 0.053(2) Uani 1 1 d G . . H25 H 1.3749 0.8246 0.4219 0.064 Uiso 1 1 calc R . . C26 C 1.2474(5) 0.6094(6) 0.43567(14) 0.0464(19) Uani 1 1 d G . . H26 H 1.3117 0.6057 0.4536 0.056 Uiso 1 1 calc R . . C27 C 1.1134(6) 0.4837(4) 0.42785(15) 0.062(3) Uani 1 1 d G . . H27 H 1.0881 0.3960 0.4405 0.074 Uiso 1 1 calc R . . C28 C 1.0173(5) 0.4893(4) 0.40105(15) 0.054(2) Uani 1 1 d G . . H28 H 0.9277 0.4052 0.3958 0.065 Uiso 1 1 calc R . . C29 C 1.0552(5) 0.6204(5) 0.38207(14) 0.051(2) Uani 1 1 d G . . H29 H 0.9909 0.6241 0.3641 0.062 Uiso 1 1 calc R . . C30 C 1.1892(5) 0.7460(4) 0.38989(15) 0.047(2) Uani 1 1 d G . . C31 C 1.2342(9) 0.8857(9) 0.3696(2) 0.0452(18) Uani 1 1 d . . . H31A H 1.3110 0.9649 0.3847 0.054 Uiso 1 1 calc R . . H31B H 1.1507 0.9015 0.3690 0.054 Uiso 1 1 calc R . . C32 C 1.2896(8) 0.8965(9) 0.3289(2) 0.0474(19) Uani 1 1 d . . . H32 H 1.3485 1.0006 0.3217 0.057 Uiso 1 1 calc R . . C33 C 1.3850(8) 0.8224(8) 0.3236(2) 0.0402(16) Uani 1 1 d . . . H33A H 1.4828 0.8930 0.3144 0.048 Uiso 1 1 calc R . . H33B H 1.3938 0.7804 0.3478 0.048 Uiso 1 1 calc R . . C34 C 1.1941(9) 0.7310(9) 0.2845(2) 0.0486(19) Uani 1 1 d . . . C35 C 1.0926(10) 0.6427(9) 0.2525(2) 0.0452(18) Uani 1 1 d . . . C36 C 1.0150(10) 0.4780(9) 0.2049(2) 0.051(2) Uani 1 1 d . . . H36A H 0.9468 0.3734 0.2080 0.061 Uiso 1 1 calc R . . H36B H 1.0671 0.4931 0.1806 0.061 Uiso 1 1 calc R . . C37 C 0.9319(10) 0.5620(9) 0.2048(2) 0.0468(19) Uani 1 1 d . . . H37 H 0.8280 0.4946 0.2108 0.056 Uiso 1 1 calc R . . C38 C 0.9435(8) 0.6457(9) 0.1695(2) 0.0454(19) Uani 1 1 d . . . H38A H 1.0467 0.7169 0.1655 0.054 Uiso 1 1 calc R . . H38B H 0.8935 0.7009 0.1743 0.054 Uiso 1 1 calc R . . C39 C 0.8845(5) 0.5632(5) 0.13226(11) 0.0435(19) Uani 1 1 d G . . C40 C 0.9378(5) 0.6414(4) 0.09789(14) 0.0487(19) Uani 1 1 d G . . H40 H 1.0037 0.7422 0.0986 0.058 Uiso 1 1 calc R . . C41 C 0.8924(6) 0.5690(5) 0.06249(11) 0.055(2) Uani 1 1 d G . . H41 H 0.9281 0.6214 0.0395 0.067 Uiso 1 1 calc R . . C42 C 0.7939(6) 0.4184(5) 0.06147(12) 0.053(2) Uani 1 1 d G . . H42 H 0.7636 0.3700 0.0378 0.064 Uiso 1 1 calc R . . C43 C 0.7407(6) 0.3402(4) 0.09584(15) 0.050(2) Uani 1 1 d G . . H43 H 0.6748 0.2395 0.0952 0.060 Uiso 1 1 calc R . . C44 C 0.7860(5) 0.4126(5) 0.13124(12) 0.051(2) Uani 1 1 d G . . H44 H 0.7504 0.3603 0.1542 0.061 Uiso 1 1 calc R . . F1 F 1.4102(5) 1.3058(5) 0.33656(13) 0.0473(11) Uani 1 1 d . . . F2 F 1.2575(5) 1.2217(5) 0.38120(14) 0.0528(12) Uani 1 1 d . . . F3 F 1.3083(5) 1.4223(4) 0.35575(12) 0.0451(10) Uani 1 1 d . . . F4 F 0.9775(5) 1.1807(5) 0.14978(14) 0.0529(12) Uani 1 1 d . . . F5 F 0.8803(5) 0.9641(5) 0.12776(14) 0.0533(12) Uani 1 1 d . . . F6 F 1.0960(5) 1.1393(5) 0.10908(14) 0.0561(12) Uani 1 1 d . . . F7 F 0.5826(5) 0.6974(5) 0.37793(14) 0.0536(12) Uani 1 1 d . . . F8 F 0.7967(5) 0.8254(5) 0.38784(14) 0.0564(13) Uani 1 1 d . . . F9 F 0.7155(5) 0.6099(5) 0.38340(13) 0.0545(12) Uani 1 1 d . . . Gd1 Gd 1.01581(4) 0.90954(4) 0.262560(11) 0.04574(11) Uani 1 1 d . . . N1 N 1.1730(7) 0.8224(8) 0.30084(18) 0.0466(16) Uani 1 1 d . . . N2 N 1.0034(8) 0.6666(7) 0.23802(19) 0.0471(16) Uani 1 1 d . . . O1 O 1.1681(7) 1.1040(6) 0.30192(16) 0.0520(14) Uani 1 1 d . . . O2 O 0.9036(5) 1.0556(5) 0.27315(15) 0.0399(11) Uani 1 1 d . . . O3 O 0.8575(6) 1.3553(6) 0.30489(16) 0.0467(12) Uani 1 1 d . . . O4 O 1.2368(6) 0.9734(7) 0.22778(17) 0.0497(14) Uani 1 1 d . . . O5 O 1.0070(6) 1.0068(6) 0.20160(16) 0.0441(12) Uani 1 1 d . . . O6 O 1.4771(6) 1.0251(6) 0.14952(16) 0.0497(13) Uani 1 1 d . . . O7 O 0.7757(6) 0.7432(6) 0.24225(15) 0.0437(12) Uani 1 1 d . . . O8 O 0.8811(6) 0.8036(5) 0.31871(14) 0.0426(12) Uani 1 1 d . . . O9 O 0.4018(6) 0.4679(6) 0.25115(15) 0.0443(12) Uani 1 1 d . . . O10 O 1.1167(6) 0.5313(6) 0.23637(15) 0.0486(14) Uani 1 1 d . . . O11 O 1.3045(6) 0.7062(6) 0.29441(16) 0.0483(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.062(6) 0.032(4) 0.050(5) -0.012(4) 0.015(4) 0.016(4) C2 0.035(4) 0.039(4) 0.053(5) -0.003(4) 0.004(3) 0.011(3) C3 0.030(4) 0.036(4) 0.053(5) -0.005(3) -0.009(3) 0.008(3) C4 0.048(4) 0.053(4) 0.019(3) -0.017(3) 0.005(3) 0.019(4) C5 0.045(4) 0.032(4) 0.043(4) -0.012(3) -0.010(3) 0.011(3) C6 0.048(4) 0.044(4) 0.040(4) -0.008(3) -0.013(3) 0.022(4) C7 0.037(4) 0.052(5) 0.065(6) 0.018(4) 0.000(4) 0.019(4) C8 0.057(5) 0.051(5) 0.045(5) 0.014(4) 0.016(4) 0.030(4) C9 0.048(4) 0.048(4) 0.036(4) 0.013(3) 0.019(3) 0.019(4) C10 0.044(4) 0.035(4) 0.044(5) -0.002(3) 0.005(3) 0.013(3) C11 0.046(4) 0.041(4) 0.050(5) 0.001(3) 0.008(3) 0.016(4) C12 0.037(4) 0.036(4) 0.049(5) 0.001(3) 0.008(3) 0.007(3) C13 0.047(5) 0.052(5) 0.043(5) -0.013(4) 0.003(4) 0.021(4) C14 0.027(4) 0.046(5) 0.078(7) 0.002(4) 0.006(4) 0.005(3) C15 0.034(4) 0.065(5) 0.045(5) 0.023(4) -0.004(3) 0.020(4) C16 0.047(4) 0.051(5) 0.045(5) 0.006(4) 0.006(4) 0.014(4) C17 0.054(5) 0.054(5) 0.044(5) -0.007(4) 0.009(4) 0.025(4) C18 0.043(4) 0.023(3) 0.050(5) -0.003(3) -0.013(3) 0.010(3) C19 0.040(4) 0.047(4) 0.034(4) -0.015(3) 0.013(3) 0.007(3) C20 0.039(4) 0.055(5) 0.033(4) -0.006(3) -0.020(3) 0.011(4) C21 0.045(4) 0.033(4) 0.052(5) -0.009(3) -0.007(3) 0.020(3) C22 0.055(5) 0.032(4) 0.059(6) -0.015(4) 0.011(4) 0.002(4) C23 0.055(5) 0.048(5) 0.037(5) -0.020(4) -0.016(4) 0.014(4) C24 0.053(5) 0.053(5) 0.040(5) -0.009(4) -0.018(4) 0.029(4) C25 0.043(4) 0.063(5) 0.049(5) 0.016(4) 0.008(4) 0.023(4) C26 0.048(4) 0.055(5) 0.045(5) 0.011(4) 0.019(3) 0.032(4) C27 0.045(5) 0.065(6) 0.050(6) 0.022(4) 0.017(4) 0.008(4) C28 0.065(5) 0.053(5) 0.033(4) 0.009(4) 0.015(4) 0.021(4) C29 0.049(5) 0.034(4) 0.055(5) -0.004(3) -0.003(4) 0.008(4) C30 0.046(4) 0.051(5) 0.036(4) 0.009(3) 0.011(3) 0.018(4) C31 0.052(5) 0.041(4) 0.036(4) -0.013(3) -0.007(3) 0.018(4) C32 0.042(4) 0.041(4) 0.045(5) -0.014(3) -0.001(3) 0.010(3) C33 0.045(4) 0.030(4) 0.038(4) 0.003(3) -0.001(3) 0.013(3) C34 0.045(4) 0.044(4) 0.048(5) 0.004(4) 0.015(4) 0.016(4) C35 0.064(5) 0.050(5) 0.024(4) 0.004(3) 0.009(3) 0.030(4) C36 0.057(5) 0.050(5) 0.047(5) -0.018(4) -0.007(4) 0.028(4) C37 0.059(5) 0.041(4) 0.029(4) 0.001(3) 0.022(4) 0.017(4) C38 0.034(4) 0.056(5) 0.037(4) 0.001(4) 0.000(3) 0.015(4) C39 0.043(4) 0.039(4) 0.034(4) -0.018(3) 0.013(3) 0.010(3) C40 0.038(4) 0.050(5) 0.047(5) -0.008(4) -0.008(4) 0.013(4) C41 0.047(5) 0.074(6) 0.032(4) -0.003(4) 0.003(3) 0.020(4) C42 0.064(5) 0.060(5) 0.050(5) -0.019(4) -0.016(4) 0.041(5) C43 0.042(4) 0.044(4) 0.052(5) -0.007(4) -0.010(4) 0.013(4) C44 0.036(4) 0.046(5) 0.056(5) -0.002(4) -0.023(4) 0.009(4) F1 0.038(2) 0.039(2) 0.056(3) -0.017(2) -0.008(2) 0.013(2) F2 0.049(3) 0.040(2) 0.058(3) 0.012(2) -0.015(2) 0.014(2) F3 0.046(2) 0.041(2) 0.040(2) -0.0196(18) -0.0128(19) 0.0158(19) F4 0.050(3) 0.045(3) 0.052(3) 0.007(2) 0.008(2) 0.016(2) F5 0.058(3) 0.053(3) 0.048(3) -0.013(2) -0.020(2) 0.026(2) F6 0.053(3) 0.056(3) 0.055(3) 0.024(2) 0.021(2) 0.024(2) F7 0.039(2) 0.056(3) 0.053(3) -0.008(2) 0.014(2) 0.015(2) F8 0.040(2) 0.059(3) 0.051(3) -0.024(2) 0.010(2) 0.011(2) F9 0.060(3) 0.049(3) 0.039(3) 0.0135(19) 0.016(2) 0.016(2) Gd1 0.0431(2) 0.0448(2) 0.03797(18) -0.00443(19) 0.00099(19) 0.01341(19) N1 0.035(3) 0.058(4) 0.032(3) -0.004(3) 0.012(3) 0.012(3) N2 0.056(4) 0.050(4) 0.033(3) -0.007(3) 0.008(3) 0.024(3) O1 0.061(4) 0.046(3) 0.041(3) -0.004(3) -0.007(3) 0.021(3) O2 0.032(2) 0.024(2) 0.051(3) -0.009(2) -0.014(2) 0.004(2) O3 0.045(3) 0.037(3) 0.055(3) 0.000(2) 0.001(2) 0.019(2) O4 0.037(3) 0.052(3) 0.053(4) -0.001(3) -0.016(3) 0.017(3) O5 0.040(3) 0.047(3) 0.045(3) 0.011(2) 0.012(2) 0.021(2) O6 0.042(3) 0.053(3) 0.051(3) 0.001(3) 0.011(2) 0.022(3) O7 0.037(3) 0.041(3) 0.042(3) 0.001(2) 0.004(2) 0.011(2) O8 0.041(3) 0.038(3) 0.032(3) -0.013(2) -0.007(2) 0.008(2) O9 0.045(3) 0.041(3) 0.042(3) -0.016(2) -0.010(2) 0.018(2) O10 0.052(3) 0.045(3) 0.041(3) -0.019(2) -0.004(2) 0.018(3) O11 0.046(3) 0.045(3) 0.052(3) -0.005(2) 0.003(3) 0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F2 1.265(10) . ? C1 F1 1.304(10) . ? C1 F3 1.350(9) . ? C1 C2 1.516(12) . ? C2 O1 1.210(9) . ? C2 C3 1.357(11) . ? C3 C4 1.411(10) . ? C3 H3 0.9300 . ? C4 O2 1.270(8) . ? C4 C5 1.501(12) . ? C5 C6 1.286(11) . ? C5 O3 1.377(9) . ? C6 C7 1.410(12) . ? C6 H6 0.9300 . ? C7 C8 1.274(13) . ? C7 H7 0.9300 . ? C8 O3 1.419(10) . ? C8 H8 0.9300 . ? C9 F6 1.288(8) . ? C9 F4 1.309(10) . ? C9 C10 1.436(12) . ? C9 F5 1.440(9) . ? C10 O5 1.261(9) . ? C10 C11 1.368(11) . ? C11 C12 1.439(12) . ? C11 H11 0.9300 . ? C12 O4 1.237(10) . ? C12 C13 1.402(12) . ? C13 C14 1.260(13) . ? C13 O6 1.343(10) . ? C14 C15 1.323(12) . ? C14 H14 0.9300 . ? C15 C16 1.304(11) . ? C15 H15 0.9300 . ? C16 O6 1.429(10) . ? C16 H16 0.9300 . ? C17 F8 1.186(10) . ? C17 F7 1.273(9) . ? C17 F9 1.380(10) . ? C17 C18 1.514(12) . ? C18 O8 1.228(9) . ? C18 C19 1.349(11) . ? C19 C20 1.425(11) . ? C19 H19 0.9300 . ? C20 O7 1.249(10) . ? C20 C21 1.469(10) . ? C21 C22 1.289(12) . ? C21 O9 1.377(9) . ? C22 C23 1.415(11) . ? C22 H22 0.9300 . ? C23 C24 1.243(12) . ? C23 H23 0.9300 . ? C24 O9 1.415(9) . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 H25 0.9300 . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.472(9) . ? C31 C32 1.502(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N1 1.444(10) . ? C32 C33 1.554(11) . ? C32 H32 0.9800 . ? C33 O11 1.477(9) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N1 1.224(10) . ? C34 O11 1.353(10) . ? C34 C35 1.491(12) . ? C35 N2 1.192(11) . ? C35 O10 1.427(9) . ? C36 O10 1.426(9) . ? C36 C37 1.518(12) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.472(11) . ? C37 N2 1.501(10) . ? C37 H37 0.9800 . ? C38 C39 1.497(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? Gd1 O1 2.301(6) . ? Gd1 O8 2.326(5) . ? Gd1 O7 2.342(5) . ? Gd1 O5 2.359(5) . ? Gd1 O2 2.381(5) . ? Gd1 O4 2.389(6) . ? Gd1 N1 2.608(7) . ? Gd1 N2 2.625(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 C1 F1 107.7(8) . . ? F2 C1 F3 106.0(6) . . ? F1 C1 F3 104.2(6) . . ? F2 C1 C2 113.9(7) . . ? F1 C1 C2 111.2(6) . . ? F3 C1 C2 113.2(8) . . ? O1 C2 C3 127.9(8) . . ? O1 C2 C1 116.1(8) . . ? C3 C2 C1 115.8(7) . . ? C2 C3 C4 123.6(7) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? O2 C4 C3 122.1(7) . . ? O2 C4 C5 115.3(6) . . ? C3 C4 C5 122.1(6) . . ? C6 C5 O3 116.0(7) . . ? C6 C5 C4 125.5(7) . . ? O3 C5 C4 118.5(6) . . ? C5 C6 C7 100.7(7) . . ? C5 C6 H6 129.6 . . ? C7 C6 H6 129.6 . . ? C8 C7 C6 114.5(8) . . ? C8 C7 H7 122.8 . . ? C6 C7 H7 122.8 . . ? C7 C8 O3 106.4(7) . . ? C7 C8 H8 126.8 . . ? O3 C8 H8 126.8 . . ? F6 C9 F4 105.0(6) . . ? F6 C9 C10 117.4(7) . . ? F4 C9 C10 115.2(7) . . ? F6 C9 F5 106.0(6) . . ? F4 C9 F5 100.3(6) . . ? C10 C9 F5 111.1(6) . . ? O5 C10 C11 125.2(8) . . ? O5 C10 C9 113.7(7) . . ? C11 C10 C9 121.1(7) . . ? C10 C11 C12 126.0(8) . . ? C10 C11 H11 117.0 . . ? C12 C11 H11 117.0 . . ? O4 C12 C13 119.6(8) . . ? O4 C12 C11 120.3(8) . . ? C13 C12 C11 120.1(8) . . ? C14 C13 O6 105.4(8) . . ? C14 C13 C12 127.6(9) . . ? O6 C13 C12 127.0(8) . . ? C13 C14 C15 112.1(9) . . ? C13 C14 H14 123.9 . . ? C15 C14 H14 123.9 . . ? C16 C15 C14 111.2(8) . . ? C16 C15 H15 124.4 . . ? C14 C15 H15 124.4 . . ? C15 C16 O6 101.3(7) . . ? C15 C16 H16 129.3 . . ? O6 C16 H16 129.3 . . ? F8 C17 F7 107.7(7) . . ? F8 C17 F9 100.9(7) . . ? F7 C17 F9 99.4(7) . . ? F8 C17 C18 118.5(8) . . ? F7 C17 C18 120.0(8) . . ? F9 C17 C18 106.6(6) . . ? O8 C18 C19 130.5(8) . . ? O8 C18 C17 112.5(7) . . ? C19 C18 C17 116.8(7) . . ? C18 C19 C20 120.9(7) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? O7 C20 C19 125.6(7) . . ? O7 C20 C21 114.5(7) . . ? C19 C20 C21 119.8(7) . . ? C22 C21 O9 110.3(7) . . ? C22 C21 C20 130.6(8) . . ? O9 C21 C20 118.6(7) . . ? C21 C22 C23 107.5(8) . . ? C21 C22 H22 126.3 . . ? C23 C22 H22 126.3 . . ? C24 C23 C22 107.9(7) . . ? C24 C23 H23 126.0 . . ? C22 C23 H23 126.0 . . ? C23 C24 O9 111.1(8) . . ? C23 C24 H24 124.5 . . ? O9 C24 H24 124.5 . . ? C26 C25 C30 120.0 . . ? C26 C25 H25 120.0 . . ? C30 C25 H25 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 C31 121.4(4) . . ? C25 C30 C31 118.6(4) . . ? C30 C31 C32 116.0(6) . . ? C30 C31 H31A 108.3 . . ? C32 C31 H31A 108.3 . . ? C30 C31 H31B 108.3 . . ? C32 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? N1 C32 C31 113.2(6) . . ? N1 C32 C33 103.7(6) . . ? C31 C32 C33 113.2(7) . . ? N1 C32 H32 108.9 . . ? C31 C32 H32 108.9 . . ? C33 C32 H32 108.9 . . ? O11 C33 C32 104.3(6) . . ? O11 C33 H33A 110.9 . . ? C32 C33 H33A 110.9 . . ? O11 C33 H33B 110.9 . . ? C32 C33 H33B 110.9 . . ? H33A C33 H33B 108.9 . . ? N1 C34 O11 122.8(8) . . ? N1 C34 C35 118.4(8) . . ? O11 C34 C35 118.8(7) . . ? N2 C35 O10 119.3(7) . . ? N2 C35 C34 124.8(8) . . ? O10 C35 C34 115.7(7) . . ? O10 C36 C37 107.9(6) . . ? O10 C36 H36A 110.1 . . ? C37 C36 H36A 110.1 . . ? O10 C36 H36B 110.1 . . ? C37 C36 H36B 110.1 . . ? H36A C36 H36B 108.4 . . ? C38 C37 N2 109.5(7) . . ? C38 C37 C36 116.5(7) . . ? N2 C37 C36 101.6(7) . . ? C38 C37 H37 109.6 . . ? N2 C37 H37 109.6 . . ? C36 C37 H37 109.6 . . ? C37 C38 C39 118.6(7) . . ? C37 C38 H38A 107.7 . . ? C39 C38 H38A 107.7 . . ? C37 C38 H38B 107.7 . . ? C39 C38 H38B 107.7 . . ? H38A C38 H38B 107.1 . . ? C40 C39 C44 120.0 . . ? C40 C39 C38 117.5(4) . . ? C44 C39 C38 122.4(4) . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? O1 Gd1 O8 85.35(19) . . ? O1 Gd1 O7 148.0(2) . . ? O8 Gd1 O7 73.91(18) . . ? O1 Gd1 O5 107.6(2) . . ? O8 Gd1 O5 143.39(19) . . ? O7 Gd1 O5 78.19(19) . . ? O1 Gd1 O2 71.74(19) . . ? O8 Gd1 O2 78.58(19) . . ? O7 Gd1 O2 80.32(17) . . ? O5 Gd1 O2 73.72(18) . . ? O1 Gd1 O4 84.3(2) . . ? O8 Gd1 O4 145.53(19) . . ? O7 Gd1 O4 126.16(18) . . ? O5 Gd1 O4 70.95(18) . . ? O2 Gd1 O4 128.2(2) . . ? O1 Gd1 N1 74.4(2) . . ? O8 Gd1 N1 75.56(18) . . ? O7 Gd1 N1 121.5(2) . . ? O5 Gd1 N1 140.45(18) . . ? O2 Gd1 N1 138.60(19) . . ? O4 Gd1 N1 69.99(18) . . ? O1 Gd1 N2 136.5(2) . . ? O8 Gd1 N2 94.67(19) . . ? O7 Gd1 N2 70.6(2) . . ? O5 Gd1 N2 98.0(2) . . ? O2 Gd1 N2 150.85(19) . . ? O4 Gd1 N2 71.4(2) . . ? N1 Gd1 N2 63.7(2) . . ? C34 N1 C32 107.1(7) . . ? C34 N1 Gd1 115.8(6) . . ? C32 N1 Gd1 131.7(5) . . ? C35 N2 C37 108.8(7) . . ? C35 N2 Gd1 114.0(6) . . ? C37 N2 Gd1 136.0(5) . . ? C2 O1 Gd1 137.5(6) . . ? C4 O2 Gd1 136.3(5) . . ? C5 O3 C8 102.4(6) . . ? C12 O4 Gd1 138.8(5) . . ? C10 O5 Gd1 136.7(5) . . ? C13 O6 C16 109.9(7) . . ? C20 O7 Gd1 133.9(5) . . ? C18 O8 Gd1 132.2(5) . . ? C21 O9 C24 103.1(6) . . ? C36 O10 C35 102.3(6) . . ? C34 O11 C33 101.8(6) . . ? 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 F2 C1 C2 O1 -82.0(10) . . . . ? F1 C1 C2 O1 39.9(10) . . . . ? F3 C1 C2 O1 156.8(7) . . . . ? F2 C1 C2 C3 92.4(9) . . . . ? F1 C1 C2 C3 -145.7(8) . . . . ? F3 C1 C2 C3 -28.8(10) . . . . ? O1 C2 C3 C4 -3.7(14) . . . . ? C1 C2 C3 C4 -177.3(7) . . . . ? C2 C3 C4 O2 10.0(12) . . . . ? C2 C3 C4 C5 -177.4(8) . . . . ? O2 C4 C5 C6 3.7(13) . . . . ? C3 C4 C5 C6 -169.4(8) . . . . ? O2 C4 C5 O3 -173.1(6) . . . . ? C3 C4 C5 O3 13.8(12) . . . . ? O3 C5 C6 C7 0.4(10) . . . . ? C4 C5 C6 C7 -176.5(8) . . . . ? C5 C6 C7 C8 0.7(10) . . . . ? C6 C7 C8 O3 -1.5(10) . . . . ? F6 C9 C10 O5 173.3(7) . . . . ? F4 C9 C10 O5 48.7(9) . . . . ? F5 C9 C10 O5 -64.5(9) . . . . ? F6 C9 C10 C11 -9.6(12) . . . . ? F4 C9 C10 C11 -134.2(8) . . . . ? F5 C9 C10 C11 112.6(8) . . . . ? O5 C10 C11 C12 -4.6(13) . . . . ? C9 C10 C11 C12 178.7(8) . . . . ? C10 C11 C12 O4 -2.3(13) . . . . ? C10 C11 C12 C13 175.1(8) . . . . ? O4 C12 C13 C14 6.0(14) . . . . ? C11 C12 C13 C14 -171.5(9) . . . . ? O4 C12 C13 O6 -174.8(7) . . . . ? C11 C12 C13 O6 7.7(13) . . . . ? O6 C13 C14 C15 -0.4(10) . . . . ? C12 C13 C14 C15 178.9(8) . . . . ? C13 C14 C15 C16 3.1(12) . . . . ? C14 C15 C16 O6 -4.0(10) . . . . ? F8 C17 C18 O8 24.6(11) . . . . ? F7 C17 C18 O8 160.1(7) . . . . ? F9 C17 C18 O8 -88.2(8) . . . . ? F8 C17 C18 C19 -150.8(8) . . . . ? F7 C17 C18 C19 -15.2(12) . . . . ? F9 C17 C18 C19 96.5(9) . . . . ? O8 C18 C19 C20 6.7(14) . . . . ? C17 C18 C19 C20 -178.9(8) . . . . ? C18 C19 C20 O7 -17.2(14) . . . . ? C18 C19 C20 C21 166.7(8) . . . . ? O7 C20 C21 C22 3.1(14) . . . . ? C19 C20 C21 C22 179.6(9) . . . . ? O7 C20 C21 O9 173.8(7) . . . . ? C19 C20 C21 O9 -9.7(12) . . . . ? O9 C21 C22 C23 3.2(10) . . . . ? C20 C21 C22 C23 174.5(8) . . . . ? C21 C22 C23 C24 -3.7(11) . . . . ? C22 C23 C24 O9 2.6(11) . . . . ? C30 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C28 C29 C30 C31 178.5(6) . . . . ? C26 C25 C30 C29 0.0 . . . . ? C26 C25 C30 C31 -178.5(6) . . . . ? C29 C30 C31 C32 -77.3(8) . . . . ? C25 C30 C31 C32 101.2(7) . . . . ? C30 C31 C32 N1 79.3(9) . . . . ? C30 C31 C32 C33 -38.4(9) . . . . ? N1 C32 C33 O11 -3.7(7) . . . . ? C31 C32 C33 O11 119.4(7) . . . . ? N1 C34 C35 N2 10.2(12) . . . . ? O11 C34 C35 N2 -170.3(8) . . . . ? N1 C34 C35 O10 -175.9(7) . . . . ? O11 C34 C35 O10 3.6(10) . . . . ? O10 C36 C37 C38 120.9(8) . . . . ? O10 C36 C37 N2 2.0(8) . . . . ? N2 C37 C38 C39 177.5(6) . . . . ? C36 C37 C38 C39 62.9(10) . . . . ? C37 C38 C39 C40 -158.9(6) . . . . ? C37 C38 C39 C44 17.8(9) . . . . ? C44 C39 C40 C41 0.0 . . . . ? C38 C39 C40 C41 176.8(6) . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C39 0.0 . . . . ? C40 C39 C44 C43 0.0 . . . . ? C38 C39 C44 C43 -176.7(6) . . . . ? O11 C34 N1 C32 3.3(10) . . . . ? C35 C34 N1 C32 -177.2(7) . . . . ? O11 C34 N1 Gd1 160.3(6) . . . . ? C35 C34 N1 Gd1 -20.2(9) . . . . ? C31 C32 N1 C34 -122.4(8) . . . . ? C33 C32 N1 C34 0.7(8) . . . . ? C31 C32 N1 Gd1 85.8(8) . . . . ? C33 C32 N1 Gd1 -151.2(5) . . . . ? O1 Gd1 N1 C34 -151.9(6) . . . . ? O8 Gd1 N1 C34 119.0(6) . . . . ? O7 Gd1 N1 C34 58.5(6) . . . . ? O5 Gd1 N1 C34 -52.9(7) . . . . ? O2 Gd1 N1 C34 172.0(5) . . . . ? O4 Gd1 N1 C34 -62.3(6) . . . . ? N2 Gd1 N1 C34 16.2(5) . . . . ? O1 Gd1 N1 C32 -2.0(6) . . . . ? O8 Gd1 N1 C32 -91.1(6) . . . . ? O7 Gd1 N1 C32 -151.5(6) . . . . ? O5 Gd1 N1 C32 97.0(7) . . . . ? O2 Gd1 N1 C32 -38.0(7) . . . . ? O4 Gd1 N1 C32 87.6(6) . . . . ? N2 Gd1 N1 C32 166.1(7) . . . . ? O10 C35 N2 C37 1.7(10) . . . . ? C34 C35 N2 C37 175.4(7) . . . . ? O10 C35 N2 Gd1 -167.8(5) . . . . ? C34 C35 N2 Gd1 5.9(10) . . . . ? C38 C37 N2 C35 -126.0(8) . . . . ? C36 C37 N2 C35 -2.2(8) . . . . ? C38 C37 N2 Gd1 40.1(10) . . . . ? C36 C37 N2 Gd1 164.0(6) . . . . ? O1 Gd1 N2 C35 6.3(7) . . . . ? O8 Gd1 N2 C35 -81.9(6) . . . . ? O7 Gd1 N2 C35 -153.0(6) . . . . ? O5 Gd1 N2 C35 132.6(6) . . . . ? O2 Gd1 N2 C35 -156.7(5) . . . . ? O4 Gd1 N2 C35 65.8(6) . . . . ? N1 Gd1 N2 C35 -10.5(6) . . . . ? O1 Gd1 N2 C37 -159.4(6) . . . . ? O8 Gd1 N2 C37 112.5(7) . . . . ? O7 Gd1 N2 C37 41.4(7) . . . . ? O5 Gd1 N2 C37 -33.1(7) . . . . ? O2 Gd1 N2 C37 37.6(9) . . . . ? O4 Gd1 N2 C37 -99.8(7) . . . . ? N1 Gd1 N2 C37 -176.2(7) . . . . ? C3 C2 O1 Gd1 -6.6(15) . . . . ? C1 C2 O1 Gd1 167.0(5) . . . . ? O8 Gd1 O1 C2 -72.4(8) . . . . ? O7 Gd1 O1 C2 -23.3(10) . . . . ? O5 Gd1 O1 C2 72.6(9) . . . . ? O2 Gd1 O1 C2 7.1(8) . . . . ? O4 Gd1 O1 C2 140.5(8) . . . . ? N1 Gd1 O1 C2 -148.7(9) . . . . ? N2 Gd1 O1 C2 -164.3(8) . . . . ? C3 C4 O2 Gd1 -7.0(12) . . . . ? C5 C4 O2 Gd1 179.9(5) . . . . ? O1 Gd1 O2 C4 0.0(7) . . . . ? O8 Gd1 O2 C4 88.9(7) . . . . ? O7 Gd1 O2 C4 164.3(7) . . . . ? O5 Gd1 O2 C4 -115.3(7) . . . . ? O4 Gd1 O2 C4 -66.9(8) . . . . ? N1 Gd1 O2 C4 36.7(8) . . . . ? N2 Gd1 O2 C4 167.8(6) . . . . ? C6 C5 O3 C8 -1.2(9) . . . . ? C4 C5 O3 C8 175.9(7) . . . . ? C7 C8 O3 C5 1.5(8) . . . . ? C13 C12 O4 Gd1 -160.0(6) . . . . ? C11 C12 O4 Gd1 17.4(12) . . . . ? O1 Gd1 O4 C12 -127.9(8) . . . . ? O8 Gd1 O4 C12 158.9(7) . . . . ? O7 Gd1 O4 C12 41.6(9) . . . . ? O5 Gd1 O4 C12 -17.0(8) . . . . ? O2 Gd1 O4 C12 -66.5(9) . . . . ? N1 Gd1 O4 C12 156.7(8) . . . . ? N2 Gd1 O4 C12 88.7(8) . . . . ? C11 C10 O5 Gd1 -2.2(12) . . . . ? C9 C10 O5 Gd1 174.7(5) . . . . ? O1 Gd1 O5 C10 85.8(7) . . . . ? O8 Gd1 O5 C10 -167.6(6) . . . . ? O7 Gd1 O5 C10 -126.7(7) . . . . ? O2 Gd1 O5 C10 150.0(7) . . . . ? O4 Gd1 O5 C10 8.5(7) . . . . ? N1 Gd1 O5 C10 -0.9(9) . . . . ? N2 Gd1 O5 C10 -58.6(7) . . . . ? C14 C13 O6 C16 -2.1(9) . . . . ? C12 C13 O6 C16 178.5(8) . . . . ? C15 C16 O6 C13 3.8(9) . . . . ? C19 C20 O7 Gd1 7.5(14) . . . . ? C21 C20 O7 Gd1 -176.3(5) . . . . ? O1 Gd1 O7 C20 -45.9(9) . . . . ? O8 Gd1 O7 C20 5.7(7) . . . . ? O5 Gd1 O7 C20 -150.3(8) . . . . ? O2 Gd1 O7 C20 -75.1(8) . . . . ? O4 Gd1 O7 C20 154.1(7) . . . . ? N1 Gd1 O7 C20 66.9(8) . . . . ? N2 Gd1 O7 C20 106.8(8) . . . . ? C19 C18 O8 Gd1 13.3(13) . . . . ? C17 C18 O8 Gd1 -161.3(5) . . . . ? O1 Gd1 O8 C18 139.6(7) . . . . ? O7 Gd1 O8 C18 -15.8(6) . . . . ? O5 Gd1 O8 C18 26.1(8) . . . . ? O2 Gd1 O8 C18 67.3(6) . . . . ? O4 Gd1 O8 C18 -147.4(6) . . . . ? N1 Gd1 O8 C18 -145.3(7) . . . . ? N2 Gd1 O8 C18 -84.0(7) . . . . ? C22 C21 O9 C24 -1.7(9) . . . . ? C20 C21 O9 C24 -174.2(7) . . . . ? C23 C24 O9 C21 -0.7(9) . . . . ? C37 C36 O10 C35 -1.1(8) . . . . ? N2 C35 O10 C36 -0.4(10) . . . . ? C34 C35 O10 C36 -174.6(7) . . . . ? N1 C34 O11 C33 -5.7(10) . . . . ? C35 C34 O11 C33 174.8(7) . . . . ? C32 C33 O11 C34 5.0(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.910 _refine_diff_density_min -0.870 _refine_diff_density_rms 0.087 # Attachment 'Eu.cif' data_p32Eu _database_code_depnum_ccdc_archive 'CCDC 752493' #TrackingRef 'Eu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 Eu F9 N2 O11' _chemical_formula_sum 'C44 H32 Eu F9 N2 O11' _chemical_formula_weight 1087.68 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P3(2) ' _symmetry_space_group_name_Hall 'P 32 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 10.4826(10) _cell_length_b 10.4826(10) _cell_length_c 34.508(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3283.8(8) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5932 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.91 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1626 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24232 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7985 _reflns_number_gt 6626 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(11) _chemical_absolute_configuration unk _refine_ls_number_reflns 7985 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2810(8) -0.0076(8) 0.1453(2) 0.0437(17) Uani 1 1 d . . . C2 C 0.2689(8) 0.0131(8) 0.1033(2) 0.0411(17) Uani 1 1 d . . . C3 C 0.3332(8) -0.0378(8) 0.07645(19) 0.0355(15) Uani 1 1 d . . . H3 H 0.3771 -0.0902 0.0856 0.043 Uiso 1 1 calc R . . C4 C 0.3347(8) -0.0126(8) 0.0347(2) 0.0418(17) Uani 1 1 d . . . C5 C 0.4379(7) -0.0355(8) 0.0125(2) 0.0398(16) Uani 1 1 d . . . C6 C 0.4593(8) -0.0120(9) -0.0240(2) 0.0471(18) Uani 1 1 d . . . H6 H 0.4110 0.0203 -0.0405 0.057 Uiso 1 1 calc R . . C7 C 0.5703(8) -0.0446(8) -0.0347(2) 0.0474(19) Uani 1 1 d . . . H7 H 0.6002 -0.0488 -0.0598 0.057 Uiso 1 1 calc R . . C8 C 0.6237(12) -0.0680(10) -0.0025(3) 0.063(3) Uani 1 1 d . . . H8 H 0.7050 -0.0805 0.0001 0.075 Uiso 1 1 calc R . . C9 C -0.0837(8) -0.0708(9) -0.0844(2) 0.0457(18) Uani 1 1 d . . . C10 C -0.0407(8) 0.0402(8) -0.0529(2) 0.0447(17) Uani 1 1 d . . . C11 C -0.0365(8) 0.1705(8) -0.0577(2) 0.0446(18) Uani 1 1 d . . . H11 H -0.0615 0.1887 -0.0821 0.053 Uiso 1 1 calc R . . C12 C 0.0013(8) 0.2809(9) -0.0298(2) 0.0453(18) Uani 1 1 d . . . C13 C 0.0183(10) 0.4194(10) -0.0417(2) 0.054(2) Uani 1 1 d . . . C14 C 0.0632(9) 0.5346(9) -0.0182(3) 0.054(2) Uani 1 1 d . . . H14 H 0.0940 0.5404 0.0073 0.065 Uiso 1 1 calc R . . C15 C 0.0555(8) 0.6439(8) -0.0386(2) 0.0413(16) Uani 1 1 d . . . H15 H 0.0847 0.7377 -0.0293 0.050 Uiso 1 1 calc R . . C16 C 0.0032(9) 0.5975(9) -0.0717(3) 0.053(2) Uani 1 1 d . . . H16 H -0.0139 0.6500 -0.0908 0.064 Uiso 1 1 calc R . . C17 C -0.2877(8) -0.0056(9) 0.1244(2) 0.0439(18) Uani 1 1 d . . . C18 C -0.2097(7) -0.0442(8) 0.0965(2) 0.0374(16) Uani 1 1 d . . . C19 C -0.2478(8) -0.1901(8) 0.09454(19) 0.0405(16) Uani 1 1 d . . . H19 H -0.3231 -0.2597 0.1100 0.049 Uiso 1 1 calc R . . C20 C -0.1675(8) -0.2353(7) 0.06749(17) 0.0348(15) Uani 1 1 d . . . C21 C -0.2191(8) -0.3979(8) 0.0657(2) 0.0402(17) Uani 1 1 d . . . C22 C -0.1528(10) -0.4588(9) 0.0484(2) 0.056(2) Uani 1 1 d . . . H22 H -0.0627 -0.4155 0.0356 0.067 Uiso 1 1 calc R . . C23 C -0.2623(10) -0.6181(9) 0.0549(2) 0.051(2) Uani 1 1 d . . . H23 H -0.2484 -0.6956 0.0475 0.061 Uiso 1 1 calc R . . C24 C -0.3774(11) -0.6334(8) 0.0720(3) 0.061(2) Uani 1 1 d . . . H24 H -0.4629 -0.7224 0.0768 0.073 Uiso 1 1 calc R . . C25 C 0.3582(11) 0.2986(10) -0.1247(2) 0.052(2) Uani 1 1 d . . . H25 H 0.2575 0.2640 -0.1231 0.063 Uiso 1 1 calc R . . C26 C 0.4262(10) 0.3224(9) -0.1608(2) 0.054(2) Uani 1 1 d . . . H26 H 0.3713 0.3022 -0.1834 0.064 Uiso 1 1 calc R . . C27 C 0.5749(8) 0.3759(7) -0.1623(2) 0.0471(18) Uani 1 1 d . . . H27 H 0.6200 0.3938 -0.1865 0.057 Uiso 1 1 calc R . . C28 C 0.6611(10) 0.4044(10) -0.1295(2) 0.058(2) Uani 1 1 d . . . H28 H 0.7618 0.4395 -0.1313 0.070 Uiso 1 1 calc R . . C29 C 0.5912(10) 0.3786(11) -0.0936(3) 0.062(2) Uani 1 1 d . . . H29 H 0.6462 0.3966 -0.0710 0.074 Uiso 1 1 calc R . . C30 C 0.4415(8) 0.3267(8) -0.0909(2) 0.0442(19) Uani 1 1 d . . . C31 C 0.3541(8) 0.2934(9) -0.0528(2) 0.0444(18) Uani 1 1 d . . . H31A H 0.2782 0.3195 -0.0563 0.053 Uiso 1 1 calc R . . H31B H 0.3051 0.1880 -0.0483 0.053 Uiso 1 1 calc R . . C32 C 0.4401(8) 0.3692(9) -0.0175(2) 0.0459(18) Uani 1 1 d . . . H32 H 0.5085 0.3344 -0.0110 0.055 Uiso 1 1 calc R . . C33 C 0.5202(10) 0.5391(10) -0.0170(2) 0.063(3) Uani 1 1 d . . . H33A H 0.6254 0.5783 -0.0144 0.076 Uiso 1 1 calc R . . H33B H 0.5025 0.5748 -0.0412 0.076 Uiso 1 1 calc R . . C34 C 0.3613(8) 0.4530(8) 0.0279(2) 0.0421(17) Uani 1 1 d . . . C35 C 0.2727(8) 0.4668(8) 0.0603(2) 0.0407(16) Uani 1 1 d . . . C36 C 0.1725(9) 0.5610(9) 0.0992(2) 0.053(2) Uani 1 1 d . . . H36A H 0.1018 0.5874 0.0896 0.064 Uiso 1 1 calc R . . H36B H 0.2137 0.6122 0.1234 0.064 Uiso 1 1 calc R . . C37 C 0.0999(8) 0.3908(8) 0.1044(2) 0.0418(17) Uani 1 1 d . . . H37 H -0.0037 0.3432 0.0966 0.050 Uiso 1 1 calc R . . C38 C 0.1099(9) 0.3468(9) 0.14493(19) 0.050(2) Uani 1 1 d . . . H38A H 0.0910 0.2463 0.1442 0.060 Uiso 1 1 calc R . . H38B H 0.0310 0.3461 0.1598 0.060 Uiso 1 1 calc R . . C39 C 0.2548(8) 0.4404(8) 0.1674(2) 0.0445(18) Uani 1 1 d . . . C40 C 0.2619(10) 0.5428(8) 0.1936(2) 0.0480(19) Uani 1 1 d . . . H40 H 0.1780 0.5484 0.1991 0.058 Uiso 1 1 calc R . . C41 C 0.3941(8) 0.6377(8) 0.2118(2) 0.0421(17) Uani 1 1 d . . . H41 H 0.3987 0.7069 0.2294 0.050 Uiso 1 1 calc R . . C42 C 0.5184(8) 0.6297(7) 0.20368(18) 0.0380(17) Uani 1 1 d . . . H42 H 0.6065 0.6933 0.2161 0.046 Uiso 1 1 calc R . . C43 C 0.5138(10) 0.5282(10) 0.1773(2) 0.057(2) Uani 1 1 d . . . H43 H 0.5984 0.5240 0.1717 0.068 Uiso 1 1 calc R . . C44 C 0.3804(9) 0.4320(11) 0.1590(2) 0.057(2) Uani 1 1 d . . . H44 H 0.3756 0.3628 0.1413 0.069 Uiso 1 1 calc R . . Eu1 Eu 0.09087(4) 0.10452(4) 0.039094(9) 0.04416(11) Uani 1 1 d . . . F1 F 0.1759(6) -0.0298(6) 0.16639(14) 0.0583(12) Uani 1 1 d . . . F2 F 0.3886(6) 0.1070(6) 0.16114(13) 0.0592(12) Uani 1 1 d . . . F3 F 0.3013(5) -0.1195(5) 0.15421(12) 0.0478(10) Uani 1 1 d . . . F4 F 0.0392(5) -0.0815(5) -0.09470(12) 0.0505(11) Uani 1 1 d . . . F5 F -0.1812(5) -0.2039(5) -0.07320(13) 0.0506(11) Uani 1 1 d . . . F6 F -0.1335(5) -0.0381(5) -0.11585(13) 0.0537(11) Uani 1 1 d . . . F7 F -0.4233(5) -0.1150(4) 0.13337(12) 0.0458(10) Uani 1 1 d . . . F8 F -0.3099(5) 0.1021(5) 0.11337(13) 0.0522(11) Uani 1 1 d . . . F9 F -0.2215(5) 0.0357(5) 0.15887(12) 0.0473(10) Uani 1 1 d . . . N1 N 0.1799(6) 0.3544(6) 0.07729(16) 0.0393(14) Uani 1 1 d . . . N2 N 0.3364(7) 0.3394(7) 0.01430(18) 0.0473(15) Uani 1 1 d . . . O1 O 0.1999(5) 0.0769(5) 0.09578(13) 0.0405(11) Uani 1 1 d . . . O2 O 0.2532(6) 0.0310(6) 0.01792(13) 0.0440(12) Uani 1 1 d . . . O3 O 0.5349(5) -0.0695(6) 0.02515(15) 0.0497(13) Uani 1 1 d . . . O4 O 0.0266(6) 0.2647(6) 0.00491(16) 0.0461(13) Uani 1 1 d . . . O5 O -0.0029(6) 0.0045(6) -0.02133(15) 0.0463(12) Uani 1 1 d . . . O6 O -0.0249(6) 0.4525(6) -0.07473(16) 0.0534(14) Uani 1 1 d . . . O7 O -0.1055(6) 0.0622(5) 0.07793(16) 0.0441(12) Uani 1 1 d . . . O8 O -0.0599(5) -0.1590(5) 0.04945(14) 0.0383(11) Uani 1 1 d . . . O9 O -0.3540(6) -0.4986(5) 0.08195(15) 0.0460(12) Uani 1 1 d . . . O10 O 0.2917(6) 0.5959(6) 0.06975(16) 0.0519(13) Uani 1 1 d . . . O11 O 0.4697(6) 0.5862(6) 0.01348(15) 0.0539(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.044(4) 0.039(4) 0.014(3) 0.006(3) 0.016(3) C2 0.039(4) 0.031(4) 0.032(4) 0.002(3) 0.001(3) 0.001(3) C3 0.040(4) 0.040(4) 0.025(3) 0.007(3) -0.003(3) 0.019(3) C4 0.029(4) 0.035(4) 0.040(4) -0.005(3) 0.008(3) 0.001(3) C5 0.027(3) 0.045(4) 0.038(4) 0.000(3) -0.006(3) 0.011(3) C6 0.045(4) 0.051(4) 0.043(4) 0.009(3) 0.013(3) 0.022(4) C7 0.033(4) 0.035(4) 0.056(5) -0.017(3) 0.009(3) 0.003(3) C8 0.082(7) 0.047(5) 0.064(6) -0.029(4) -0.010(5) 0.035(5) C9 0.037(4) 0.043(4) 0.046(4) -0.012(3) -0.008(3) 0.012(3) C10 0.040(4) 0.044(4) 0.040(4) 0.005(3) 0.006(3) 0.013(3) C11 0.041(4) 0.041(4) 0.041(4) 0.019(3) 0.005(3) 0.012(3) C12 0.035(4) 0.052(5) 0.045(4) 0.010(3) 0.015(3) 0.019(4) C13 0.056(5) 0.058(5) 0.046(5) 0.004(4) 0.008(4) 0.029(4) C14 0.037(4) 0.046(5) 0.072(6) -0.001(4) -0.009(4) 0.015(4) C15 0.035(4) 0.032(4) 0.047(4) 0.002(3) -0.015(3) 0.009(3) C16 0.046(4) 0.039(4) 0.071(6) -0.008(4) -0.019(4) 0.020(4) C17 0.029(4) 0.044(4) 0.043(4) 0.012(3) 0.014(3) 0.006(3) C18 0.028(3) 0.040(4) 0.039(4) 0.003(3) -0.010(3) 0.013(3) C19 0.047(4) 0.044(4) 0.031(3) 0.015(3) 0.011(3) 0.023(3) C20 0.047(4) 0.034(3) 0.016(3) 0.009(3) 0.003(3) 0.014(3) C21 0.031(4) 0.044(4) 0.041(4) 0.002(3) -0.001(3) 0.015(3) C22 0.053(5) 0.047(5) 0.052(5) 0.004(4) 0.014(4) 0.013(4) C23 0.062(5) 0.043(4) 0.036(4) -0.010(3) -0.025(4) 0.017(4) C24 0.072(6) 0.025(4) 0.053(5) 0.011(3) -0.004(5) 0.000(4) C25 0.068(5) 0.063(5) 0.038(4) 0.007(4) 0.009(4) 0.041(5) C26 0.060(5) 0.047(4) 0.045(4) 0.016(3) 0.013(4) 0.020(4) C27 0.046(4) 0.028(3) 0.058(5) 0.017(3) 0.015(4) 0.011(3) C28 0.052(5) 0.053(5) 0.049(5) 0.010(4) 0.018(4) 0.011(4) C29 0.050(5) 0.074(6) 0.050(5) -0.013(4) 0.014(4) 0.022(5) C30 0.032(4) 0.035(4) 0.044(4) -0.006(3) 0.002(3) 0.000(3) C31 0.037(4) 0.046(4) 0.034(4) 0.012(3) 0.010(3) 0.009(3) C32 0.031(4) 0.047(4) 0.048(4) 0.016(4) 0.005(3) 0.011(3) C33 0.048(5) 0.060(5) 0.040(4) 0.008(4) 0.018(4) -0.004(4) C34 0.038(4) 0.043(4) 0.034(4) 0.010(3) -0.002(3) 0.012(3) C35 0.032(3) 0.035(4) 0.046(4) 0.012(3) -0.001(3) 0.010(3) C36 0.049(5) 0.042(4) 0.055(5) 0.005(4) -0.004(4) 0.013(4) C37 0.042(4) 0.034(4) 0.036(4) 0.003(3) -0.004(3) 0.009(3) C38 0.052(5) 0.043(4) 0.025(3) -0.004(3) 0.005(3) 0.000(4) C39 0.040(4) 0.027(4) 0.052(5) 0.006(3) 0.003(3) 0.006(3) C40 0.062(5) 0.041(4) 0.033(4) -0.008(3) -0.027(4) 0.020(4) C41 0.034(4) 0.025(3) 0.049(4) 0.001(3) 0.000(3) 0.001(3) C42 0.044(4) 0.038(4) 0.030(3) 0.014(3) -0.008(3) 0.018(3) C43 0.051(5) 0.065(6) 0.050(5) -0.003(4) 0.004(4) 0.026(4) C44 0.045(5) 0.075(6) 0.038(4) 0.007(4) 0.004(3) 0.020(4) Eu1 0.0415(2) 0.0408(2) 0.03794(16) 0.00564(17) 0.00515(18) 0.01136(19) F1 0.061(3) 0.065(3) 0.054(3) 0.021(2) 0.019(2) 0.035(3) F2 0.071(3) 0.066(3) 0.041(2) -0.008(2) -0.015(2) 0.034(3) F3 0.052(3) 0.052(3) 0.042(2) 0.0121(19) 0.0001(19) 0.027(2) F4 0.048(3) 0.049(2) 0.038(2) -0.0176(19) 0.0022(19) 0.012(2) F5 0.047(3) 0.045(3) 0.043(2) -0.0080(19) -0.007(2) 0.011(2) F6 0.061(3) 0.039(2) 0.047(2) -0.0113(19) -0.019(2) 0.014(2) F7 0.043(2) 0.036(2) 0.045(2) 0.0088(18) 0.0095(18) 0.0102(19) F8 0.054(3) 0.045(3) 0.056(3) 0.015(2) 0.015(2) 0.023(2) F9 0.043(2) 0.046(2) 0.045(2) -0.0095(19) -0.0032(19) 0.016(2) N1 0.033(3) 0.041(3) 0.033(3) 0.013(2) 0.006(2) 0.011(3) N2 0.042(4) 0.041(4) 0.040(3) 0.012(3) 0.011(3) 0.007(3) O1 0.041(3) 0.044(3) 0.029(2) -0.002(2) -0.003(2) 0.015(2) O2 0.039(3) 0.054(3) 0.031(3) 0.001(2) 0.001(2) 0.017(2) O3 0.028(3) 0.052(3) 0.047(3) -0.005(2) -0.007(2) 0.003(2) O4 0.048(3) 0.036(3) 0.053(3) -0.003(2) -0.005(3) 0.020(2) O5 0.051(3) 0.046(3) 0.042(3) -0.003(2) -0.009(2) 0.024(3) O6 0.050(3) 0.039(3) 0.054(3) 0.009(2) 0.002(3) 0.009(3) O7 0.039(3) 0.029(3) 0.053(3) 0.001(2) 0.002(2) 0.008(2) O8 0.030(2) 0.030(2) 0.044(3) 0.004(2) 0.006(2) 0.006(2) O9 0.043(3) 0.033(3) 0.043(3) 0.004(2) -0.008(2) 0.005(2) O10 0.058(3) 0.040(3) 0.054(3) 0.014(2) 0.014(3) 0.022(3) O11 0.053(3) 0.050(3) 0.041(3) 0.017(2) 0.019(2) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F1 1.242(9) . ? C1 F2 1.289(9) . ? C1 F3 1.328(9) . ? C1 C2 1.481(10) . ? C2 O1 1.234(9) . ? C2 C3 1.397(11) . ? C3 C4 1.464(9) . ? C3 H3 0.9300 . ? C4 O2 1.289(10) . ? C4 C5 1.439(10) . ? C5 C6 1.283(10) . ? C5 O3 1.309(9) . ? C6 C7 1.415(11) . ? C6 H6 0.9300 . ? C7 C8 1.319(13) . ? C7 H7 0.9300 . ? C8 O3 1.328(11) . ? C8 H8 0.9300 . ? C9 F5 1.309(9) . ? C9 F6 1.323(9) . ? C9 F4 1.394(9) . ? C9 C10 1.487(10) . ? C10 O5 1.279(9) . ? C10 C11 1.355(11) . ? C11 C12 1.400(11) . ? C11 H11 0.9300 . ? C12 O4 1.258(9) . ? C12 C13 1.432(12) . ? C13 C14 1.330(12) . ? C13 O6 1.334(10) . ? C14 C15 1.381(11) . ? C14 H14 0.9300 . ? C15 C16 1.254(11) . ? C15 H15 0.9300 . ? C16 O6 1.400(9) . ? C16 H16 0.9300 . ? C17 F8 1.318(9) . ? C17 F9 1.336(9) . ? C17 F7 1.342(8) . ? C17 C18 1.447(11) . ? C18 O7 1.276(8) . ? C18 C19 1.375(10) . ? C19 C20 1.484(10) . ? C19 H19 0.9300 . ? C20 O8 1.182(8) . ? C20 C21 1.510(10) . ? C21 C22 1.299(11) . ? C21 O9 1.392(9) . ? C22 C23 1.497(11) . ? C22 H22 0.9300 . ? C23 C24 1.279(13) . ? C23 H23 0.9300 . ? C24 O9 1.352(10) . ? C24 H24 0.9300 . ? C25 C26 1.394(11) . ? C25 C30 1.396(11) . ? C25 H25 0.9300 . ? C26 C27 1.369(12) . ? C26 H26 0.9300 . ? C27 C28 1.386(12) . ? C27 H27 0.9300 . ? C28 C29 1.396(11) . ? C28 H28 0.9300 . ? C29 C30 1.383(11) . ? C29 H29 0.9300 . ? C30 C31 1.539(10) . ? C31 C32 1.487(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N2 1.465(9) . ? C32 C33 1.543(12) . ? C32 H32 0.9800 . ? C33 O11 1.377(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N2 1.182(10) . ? C34 O11 1.379(9) . ? C34 C35 1.505(11) . ? C35 N1 1.238(9) . ? C35 O10 1.307(9) . ? C36 O10 1.506(10) . ? C36 C37 1.561(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 N1 1.430(10) . ? C37 C38 1.492(10) . ? C37 H37 0.9800 . ? C38 C39 1.544(11) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.377(11) . ? C39 C44 1.393(12) . ? C40 C41 1.387(10) . ? C40 H40 0.9300 . ? C41 C42 1.375(10) . ? C41 H41 0.9300 . ? C42 C43 1.383(11) . ? C42 H42 0.9300 . ? C43 C44 1.400(12) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? Eu1 O7 2.306(5) . ? Eu1 O2 2.310(5) . ? Eu1 O5 2.320(5) . ? Eu1 O1 2.355(5) . ? Eu1 O4 2.408(5) . ? Eu1 O8 2.427(4) . ? Eu1 N1 2.651(6) . ? Eu1 N2 2.662(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 C1 F2 101.9(7) . . ? F1 C1 F3 102.6(6) . . ? F2 C1 F3 105.8(6) . . ? F1 C1 C2 118.0(7) . . ? F2 C1 C2 112.2(6) . . ? F3 C1 C2 114.8(7) . . ? O1 C2 C3 126.4(7) . . ? O1 C2 C1 113.6(7) . . ? C3 C2 C1 120.0(7) . . ? C2 C3 C4 123.1(7) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? O2 C4 C5 120.4(6) . . ? O2 C4 C3 123.8(6) . . ? C5 C4 C3 115.8(7) . . ? C6 C5 O3 107.1(7) . . ? C6 C5 C4 124.4(7) . . ? O3 C5 C4 128.2(7) . . ? C5 C6 C7 107.2(8) . . ? C5 C6 H6 126.4 . . ? C7 C6 H6 126.4 . . ? C8 C7 C6 107.6(7) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 O3 104.3(8) . . ? C7 C8 H8 127.8 . . ? O3 C8 H8 127.8 . . ? F5 C9 F6 108.6(6) . . ? F5 C9 F4 104.5(6) . . ? F6 C9 F4 108.1(6) . . ? F5 C9 C10 112.9(6) . . ? F6 C9 C10 113.6(7) . . ? F4 C9 C10 108.6(6) . . ? O5 C10 C11 122.7(7) . . ? O5 C10 C9 114.2(7) . . ? C11 C10 C9 123.1(7) . . ? C10 C11 C12 127.1(7) . . ? C10 C11 H11 116.5 . . ? C12 C11 H11 116.5 . . ? O4 C12 C11 122.3(7) . . ? O4 C12 C13 118.8(7) . . ? C11 C12 C13 118.8(7) . . ? C14 C13 O6 107.2(8) . . ? C14 C13 C12 123.6(8) . . ? O6 C13 C12 128.5(8) . . ? C13 C14 C15 107.5(8) . . ? C13 C14 H14 126.2 . . ? C15 C14 H14 126.2 . . ? C16 C15 C14 109.8(8) . . ? C16 C15 H15 125.1 . . ? C14 C15 H15 125.1 . . ? C15 C16 O6 107.6(7) . . ? C15 C16 H16 126.2 . . ? O6 C16 H16 126.2 . . ? F8 C17 F9 105.4(7) . . ? F8 C17 F7 103.5(6) . . ? F9 C17 F7 103.2(5) . . ? F8 C17 C18 114.5(6) . . ? F9 C17 C18 114.2(6) . . ? F7 C17 C18 114.8(7) . . ? O7 C18 C19 126.4(7) . . ? O7 C18 C17 116.5(7) . . ? C19 C18 C17 116.9(6) . . ? C18 C19 C20 119.3(6) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? O8 C20 C19 128.1(6) . . ? O8 C20 C21 115.1(6) . . ? C19 C20 C21 116.5(6) . . ? C22 C21 O9 113.7(7) . . ? C22 C21 C20 126.6(7) . . ? O9 C21 C20 119.6(6) . . ? C21 C22 C23 100.3(7) . . ? C21 C22 H22 129.8 . . ? C23 C22 H22 129.8 . . ? C24 C23 C22 111.0(8) . . ? C24 C23 H23 124.5 . . ? C22 C23 H23 124.5 . . ? C23 C24 O9 108.6(7) . . ? C23 C24 H24 125.7 . . ? O9 C24 H24 125.7 . . ? C26 C25 C30 119.8(8) . . ? C26 C25 H25 120.1 . . ? C30 C25 H25 120.1 . . ? C27 C26 C25 118.9(8) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 122.9(8) . . ? C26 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C27 C28 C29 117.5(9) . . ? C27 C28 H28 121.3 . . ? C29 C28 H28 121.3 . . ? C30 C29 C28 121.1(9) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C25 119.7(8) . . ? C29 C30 C31 125.1(7) . . ? C25 C30 C31 115.2(7) . . ? C32 C31 C30 116.4(6) . . ? C32 C31 H31A 108.2 . . ? C30 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? C30 C31 H31B 108.2 . . ? H31A C31 H31B 107.3 . . ? N2 C32 C31 108.3(6) . . ? N2 C32 C33 98.9(6) . . ? C31 C32 C33 117.4(7) . . ? N2 C32 H32 110.5 . . ? C31 C32 H32 110.5 . . ? C33 C32 H32 110.5 . . ? O11 C33 C32 109.7(6) . . ? O11 C33 H33A 109.7 . . ? C32 C33 H33A 109.7 . . ? O11 C33 H33B 109.7 . . ? C32 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? N2 C34 O11 122.1(7) . . ? N2 C34 C35 123.8(6) . . ? O11 C34 C35 114.0(6) . . ? N1 C35 O10 120.5(7) . . ? N1 C35 C34 119.3(7) . . ? O10 C35 C34 120.2(6) . . ? O10 C36 C37 103.2(6) . . ? O10 C36 H36A 111.1 . . ? C37 C36 H36A 111.1 . . ? O10 C36 H36B 111.1 . . ? C37 C36 H36B 111.1 . . ? H36A C36 H36B 109.1 . . ? N1 C37 C38 112.9(7) . . ? N1 C37 C36 102.3(6) . . ? C38 C37 C36 113.1(6) . . ? N1 C37 H37 109.4 . . ? C38 C37 H37 109.4 . . ? C36 C37 H37 109.4 . . ? C37 C38 C39 118.3(6) . . ? C37 C38 H38A 107.7 . . ? C39 C38 H38A 107.7 . . ? C37 C38 H38B 107.7 . . ? C39 C38 H38B 107.7 . . ? H38A C38 H38B 107.1 . . ? C40 C39 C44 120.1(8) . . ? C40 C39 C38 118.5(7) . . ? C44 C39 C38 121.0(7) . . ? C39 C40 C41 120.0(8) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.2(8) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.7(7) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.3(8) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C39 C44 C43 119.7(9) . . ? C39 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? O7 Eu1 O2 148.79(19) . . ? O7 Eu1 O5 107.43(19) . . ? O2 Eu1 O5 77.38(19) . . ? O7 Eu1 O1 86.28(18) . . ? O2 Eu1 O1 74.79(17) . . ? O5 Eu1 O1 144.38(18) . . ? O7 Eu1 O4 83.4(2) . . ? O2 Eu1 O4 125.99(18) . . ? O5 Eu1 O4 70.84(18) . . ? O1 Eu1 O4 144.57(17) . . ? O7 Eu1 O8 71.61(17) . . ? O2 Eu1 O8 80.57(17) . . ? O5 Eu1 O8 74.35(18) . . ? O1 Eu1 O8 79.51(17) . . ? O4 Eu1 O8 128.01(18) . . ? O7 Eu1 N1 74.95(18) . . ? O2 Eu1 N1 122.21(18) . . ? O5 Eu1 N1 138.92(18) . . ? O1 Eu1 N1 75.87(17) . . ? O4 Eu1 N1 68.73(17) . . ? O8 Eu1 N1 139.35(16) . . ? O7 Eu1 N2 136.2(2) . . ? O2 Eu1 N2 71.0(2) . . ? O5 Eu1 N2 97.15(19) . . ? O1 Eu1 N2 94.37(19) . . ? O4 Eu1 N2 71.1(2) . . ? O8 Eu1 N2 151.48(19) . . ? N1 Eu1 N2 62.99(19) . . ? C35 N1 C37 110.1(6) . . ? C35 N1 Eu1 115.2(5) . . ? C37 N1 Eu1 128.7(4) . . ? C34 N2 C32 108.5(6) . . ? C34 N2 Eu1 115.3(5) . . ? C32 N2 Eu1 135.2(5) . . ? C2 O1 Eu1 133.8(5) . . ? C4 O2 Eu1 134.9(4) . . ? C5 O3 C8 113.1(7) . . ? C12 O4 Eu1 135.4(5) . . ? C10 O5 Eu1 139.3(5) . . ? C13 O6 C16 107.7(6) . . ? C18 O7 Eu1 138.7(5) . . ? C20 O8 Eu1 134.9(5) . . ? C24 O9 C21 105.9(7) . . ? C35 O10 C36 103.8(6) . . ? C33 O11 C34 100.6(6) . . ? 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 F1 C1 C2 O1 34.2(9) . . . . ? F2 C1 C2 O1 -83.8(8) . . . . ? F3 C1 C2 O1 155.3(6) . . . . ? F1 C1 C2 C3 -146.0(7) . . . . ? F2 C1 C2 C3 96.0(8) . . . . ? F3 C1 C2 C3 -24.9(10) . . . . ? O1 C2 C3 C4 4.1(11) . . . . ? C1 C2 C3 C4 -175.7(6) . . . . ? C2 C3 C4 O2 -14.7(11) . . . . ? C2 C3 C4 C5 163.6(7) . . . . ? O2 C4 C5 C6 1.7(11) . . . . ? C3 C4 C5 C6 -176.6(7) . . . . ? O2 C4 C5 O3 175.0(7) . . . . ? C3 C4 C5 O3 -3.3(11) . . . . ? O3 C5 C6 C7 4.4(8) . . . . ? C4 C5 C6 C7 178.9(7) . . . . ? C5 C6 C7 C8 -8.1(9) . . . . ? C6 C7 C8 O3 8.1(9) . . . . ? F5 C9 C10 O5 50.8(9) . . . . ? F6 C9 C10 O5 175.0(6) . . . . ? F4 C9 C10 O5 -64.6(8) . . . . ? F5 C9 C10 C11 -131.6(8) . . . . ? F6 C9 C10 C11 -7.4(11) . . . . ? F4 C9 C10 C11 113.0(8) . . . . ? O5 C10 C11 C12 -3.1(12) . . . . ? C9 C10 C11 C12 179.5(7) . . . . ? C10 C11 C12 O4 -5.3(12) . . . . ? C10 C11 C12 C13 171.8(8) . . . . ? O4 C12 C13 C14 1.7(13) . . . . ? C11 C12 C13 C14 -175.5(8) . . . . ? O4 C12 C13 O6 -167.9(8) . . . . ? C11 C12 C13 O6 14.9(13) . . . . ? O6 C13 C14 C15 -3.9(10) . . . . ? C12 C13 C14 C15 -175.4(8) . . . . ? C13 C14 C15 C16 2.9(10) . . . . ? C14 C15 C16 O6 -0.7(10) . . . . ? F8 C17 C18 O7 38.5(9) . . . . ? F9 C17 C18 O7 -83.0(8) . . . . ? F7 C17 C18 O7 158.1(6) . . . . ? F8 C17 C18 C19 -146.1(7) . . . . ? F9 C17 C18 C19 92.3(8) . . . . ? F7 C17 C18 C19 -26.5(10) . . . . ? O7 C18 C19 C20 -2.8(11) . . . . ? C17 C18 C19 C20 -177.7(6) . . . . ? C18 C19 C20 O8 9.4(11) . . . . ? C18 C19 C20 C21 -177.6(6) . . . . ? O8 C20 C21 C22 4.2(11) . . . . ? C19 C20 C21 C22 -169.7(8) . . . . ? O8 C20 C21 O9 -172.2(6) . . . . ? C19 C20 C21 O9 13.8(9) . . . . ? O9 C21 C22 C23 0.2(9) . . . . ? C20 C21 C22 C23 -176.5(7) . . . . ? C21 C22 C23 C24 3.8(10) . . . . ? C22 C23 C24 O9 -6.3(10) . . . . ? C30 C25 C26 C27 -1.2(12) . . . . ? C25 C26 C27 C28 1.6(12) . . . . ? C26 C27 C28 C29 -0.9(13) . . . . ? C27 C28 C29 C30 -0.1(14) . . . . ? C28 C29 C30 C25 0.4(14) . . . . ? C28 C29 C30 C31 179.4(8) . . . . ? C26 C25 C30 C29 0.3(13) . . . . ? C26 C25 C30 C31 -178.8(8) . . . . ? C29 C30 C31 C32 22.3(13) . . . . ? C25 C30 C31 C32 -158.7(7) . . . . ? C30 C31 C32 N2 172.6(7) . . . . ? C30 C31 C32 C33 61.7(10) . . . . ? N2 C32 C33 O11 4.4(9) . . . . ? C31 C32 C33 O11 120.5(8) . . . . ? N2 C34 C35 N1 9.4(11) . . . . ? O11 C34 C35 N1 -174.7(7) . . . . ? N2 C34 C35 O10 -169.2(7) . . . . ? O11 C34 C35 O10 6.7(10) . . . . ? O10 C36 C37 N1 -2.4(7) . . . . ? O10 C36 C37 C38 119.4(7) . . . . ? N1 C37 C38 C39 75.1(9) . . . . ? C36 C37 C38 C39 -40.4(11) . . . . ? C37 C38 C39 C40 99.8(9) . . . . ? C37 C38 C39 C44 -74.2(11) . . . . ? C44 C39 C40 C41 -0.2(12) . . . . ? C38 C39 C40 C41 -174.2(7) . . . . ? C39 C40 C41 C42 -0.1(11) . . . . ? C40 C41 C42 C43 0.5(11) . . . . ? C41 C42 C43 C44 -0.6(11) . . . . ? C40 C39 C44 C43 0.0(12) . . . . ? C38 C39 C44 C43 173.9(7) . . . . ? C42 C43 C44 C39 0.4(12) . . . . ? O10 C35 N1 C37 3.7(9) . . . . ? C34 C35 N1 C37 -174.9(6) . . . . ? O10 C35 N1 Eu1 158.9(5) . . . . ? C34 C35 N1 Eu1 -19.6(8) . . . . ? C38 C37 N1 C35 -122.2(7) . . . . ? C36 C37 N1 C35 -0.3(8) . . . . ? C38 C37 N1 Eu1 86.9(7) . . . . ? C36 C37 N1 Eu1 -151.2(5) . . . . ? O7 Eu1 N1 C35 -151.8(6) . . . . ? O2 Eu1 N1 C35 56.8(6) . . . . ? O5 Eu1 N1 C35 -52.4(6) . . . . ? O1 Eu1 N1 C35 118.2(5) . . . . ? O4 Eu1 N1 C35 -63.2(5) . . . . ? O8 Eu1 N1 C35 172.7(5) . . . . ? N2 Eu1 N1 C35 15.7(5) . . . . ? O7 Eu1 N1 C37 -2.1(5) . . . . ? O2 Eu1 N1 C37 -153.5(5) . . . . ? O5 Eu1 N1 C37 97.3(6) . . . . ? O1 Eu1 N1 C37 -92.0(6) . . . . ? O4 Eu1 N1 C37 86.5(6) . . . . ? O8 Eu1 N1 C37 -37.6(7) . . . . ? N2 Eu1 N1 C37 165.4(6) . . . . ? O11 C34 N2 C32 1.7(10) . . . . ? C35 C34 N2 C32 177.3(7) . . . . ? O11 C34 N2 Eu1 -168.9(5) . . . . ? C35 C34 N2 Eu1 6.7(10) . . . . ? C31 C32 N2 C34 -126.4(7) . . . . ? C33 C32 N2 C34 -3.5(8) . . . . ? C31 C32 N2 Eu1 41.5(10) . . . . ? C33 C32 N2 Eu1 164.4(6) . . . . ? O7 Eu1 N2 C34 6.5(7) . . . . ? O2 Eu1 N2 C34 -154.9(6) . . . . ? O5 Eu1 N2 C34 131.1(6) . . . . ? O1 Eu1 N2 C34 -82.6(6) . . . . ? O4 Eu1 N2 C34 64.2(6) . . . . ? O8 Eu1 N2 C34 -158.7(5) . . . . ? N1 Eu1 N2 C34 -10.9(5) . . . . ? O7 Eu1 N2 C32 -160.8(6) . . . . ? O2 Eu1 N2 C32 37.8(7) . . . . ? O5 Eu1 N2 C32 -36.2(7) . . . . ? O1 Eu1 N2 C32 110.1(7) . . . . ? O4 Eu1 N2 C32 -103.0(7) . . . . ? O8 Eu1 N2 C32 34.0(9) . . . . ? N1 Eu1 N2 C32 -178.2(8) . . . . ? C3 C2 O1 Eu1 16.0(11) . . . . ? C1 C2 O1 Eu1 -164.2(5) . . . . ? O7 Eu1 O1 C2 137.2(6) . . . . ? O2 Eu1 O1 C2 -17.8(6) . . . . ? O5 Eu1 O1 C2 22.0(8) . . . . ? O4 Eu1 O1 C2 -149.7(6) . . . . ? O8 Eu1 O1 C2 65.2(6) . . . . ? N1 Eu1 O1 C2 -147.4(6) . . . . ? N2 Eu1 O1 C2 -86.7(6) . . . . ? C5 C4 O2 Eu1 -173.0(5) . . . . ? C3 C4 O2 Eu1 5.1(11) . . . . ? O7 Eu1 O2 C4 -47.8(8) . . . . ? O5 Eu1 O2 C4 -150.7(7) . . . . ? O1 Eu1 O2 C4 6.8(6) . . . . ? O4 Eu1 O2 C4 154.6(6) . . . . ? O8 Eu1 O2 C4 -74.8(6) . . . . ? N1 Eu1 O2 C4 68.8(7) . . . . ? N2 Eu1 O2 C4 107.0(7) . . . . ? C6 C5 O3 C8 0.7(9) . . . . ? C4 C5 O3 C8 -173.5(7) . . . . ? C7 C8 O3 C5 -5.8(9) . . . . ? C11 C12 O4 Eu1 19.6(11) . . . . ? C13 C12 O4 Eu1 -157.5(6) . . . . ? O7 Eu1 O4 C12 -128.5(7) . . . . ? O2 Eu1 O4 C12 40.0(8) . . . . ? O5 Eu1 O4 C12 -17.4(7) . . . . ? O1 Eu1 O4 C12 157.5(6) . . . . ? O8 Eu1 O4 C12 -68.1(7) . . . . ? N1 Eu1 O4 C12 155.1(7) . . . . ? N2 Eu1 O4 C12 87.5(7) . . . . ? C11 C10 O5 Eu1 -2.8(12) . . . . ? C9 C10 O5 Eu1 174.9(5) . . . . ? O7 Eu1 O5 C10 85.2(7) . . . . ? O2 Eu1 O5 C10 -126.8(8) . . . . ? O1 Eu1 O5 C10 -166.0(6) . . . . ? O4 Eu1 O5 C10 8.9(7) . . . . ? O8 Eu1 O5 C10 149.6(8) . . . . ? N1 Eu1 O5 C10 -1.7(9) . . . . ? N2 Eu1 O5 C10 -58.2(8) . . . . ? C14 C13 O6 C16 3.5(9) . . . . ? C12 C13 O6 C16 174.5(8) . . . . ? C15 C16 O6 C13 -1.7(10) . . . . ? C19 C18 O7 Eu1 -8.7(12) . . . . ? C17 C18 O7 Eu1 166.1(5) . . . . ? O2 Eu1 O7 C18 -18.5(9) . . . . ? O5 Eu1 O7 C18 75.8(7) . . . . ? O1 Eu1 O7 C18 -70.6(7) . . . . ? O4 Eu1 O7 C18 143.3(7) . . . . ? O8 Eu1 O7 C18 9.6(7) . . . . ? N1 Eu1 O7 C18 -147.0(7) . . . . ? N2 Eu1 O7 C18 -163.1(6) . . . . ? C19 C20 O8 Eu1 -5.1(11) . . . . ? C21 C20 O8 Eu1 -178.2(4) . . . . ? O7 Eu1 O8 C20 -2.4(6) . . . . ? O2 Eu1 O8 C20 163.3(7) . . . . ? O5 Eu1 O8 C20 -117.3(7) . . . . ? O1 Eu1 O8 C20 87.2(6) . . . . ? O4 Eu1 O8 C20 -67.9(7) . . . . ? N1 Eu1 O8 C20 33.8(8) . . . . ? N2 Eu1 O8 C20 166.9(6) . . . . ? C23 C24 O9 C21 6.1(9) . . . . ? C22 C21 O9 C24 -3.8(9) . . . . ? C20 C21 O9 C24 173.1(7) . . . . ? N1 C35 O10 C36 -5.2(9) . . . . ? C34 C35 O10 C36 173.3(6) . . . . ? C37 C36 O10 C35 4.2(7) . . . . ? C32 C33 O11 C34 -3.6(9) . . . . ? N2 C34 O11 C33 1.4(10) . . . . ? C35 C34 O11 C33 -174.7(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.032 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.087 # Attachment 'Sm.cif' data_p32Sm _database_code_depnum_ccdc_archive 'CCDC 752495' #TrackingRef 'Sm.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 F9 N2 O11 Sm' _chemical_formula_sum 'C44 H32 F9 N2 O11 Sm' _chemical_formula_weight 1086.07 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P3(2) ' _symmetry_space_group_name_Hall 'P 32 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 10.4701(10) _cell_length_b 10.4701(10) _cell_length_c 34.531(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3278.3(7) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5932 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.91 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1623 _exptl_absorpt_coefficient_mu 1.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.83 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17683 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7818 _reflns_number_gt 6204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.05P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(13) _chemical_absolute_configuration unk _refine_ls_number_reflns 7818 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.57549(4) 0.22996(4) 0.177002(11) 0.04611(12) Uani 1 1 d . . . F1 F 0.2784(5) 0.2287(5) 0.29881(12) 0.0482(11) Uani 1 1 d . . . F2 F 0.3620(5) 0.4545(5) 0.29229(13) 0.0467(10) Uani 1 1 d . . . F3 F 0.4970(5) 0.3670(5) 0.30234(13) 0.0452(11) Uani 1 1 d . . . F4 F 0.8870(5) 0.3014(5) 0.29686(13) 0.0475(11) Uani 1 1 d . . . F5 F 1.0905(5) 0.4524(5) 0.27110(13) 0.0485(11) Uani 1 1 d . . . F6 F 0.9743(5) 0.2322(5) 0.25207(13) 0.0520(12) Uani 1 1 d . . . F7 F 0.7972(5) 0.3693(5) 0.02145(13) 0.0537(12) Uani 1 1 d . . . F8 F 0.6299(5) 0.4154(5) 0.04186(13) 0.0537(12) Uani 1 1 d . . . F9 F 0.8456(5) 0.5338(5) 0.06347(13) 0.0454(11) Uani 1 1 d . . . O1 O 0.4670(6) 0.2586(6) 0.23312(15) 0.0466(13) Uani 1 1 d . . . O2 O 0.4085(6) 0.3055(6) 0.15787(15) 0.0466(13) Uani 1 1 d . . . O3 O 0.7723(6) 0.2725(6) 0.21657(16) 0.0478(14) Uani 1 1 d . . . O4 O 0.7258(6) 0.4931(6) 0.18691(15) 0.0441(12) Uani 1 1 d . . . O5 O 0.6680(6) 0.3299(6) 0.11535(17) 0.0513(14) Uani 1 1 d . . . O6 O 0.6391(7) 0.0696(7) 0.14120(17) 0.0487(14) Uani 1 1 d . . . O7 O 0.3773(7) -0.2619(6) 0.20826(15) 0.0523(14) Uani 1 1 d . . . O8 O 0.1986(6) -0.2511(6) 0.15174(16) 0.0553(16) Uani 1 1 d . . . O9 O 0.1291(6) 0.4010(6) 0.16591(16) 0.0453(13) Uani 1 1 d . . . O10 O 1.0211(6) 0.8342(6) 0.22037(16) 0.0487(13) Uani 1 1 d . . . O11 O 0.6914(6) -0.1165(6) 0.06310(16) 0.0535(15) Uani 1 1 d . . . N1 N 0.4879(7) -0.0173(7) 0.21550(18) 0.0426(15) Uani 1 1 d . . . N2 N 0.3282(8) -0.0035(7) 0.1529(2) 0.0526(17) Uani 1 1 d . . . C1 C 0.3833(10) 0.3450(9) 0.2832(2) 0.049(2) Uani 1 1 d . . . C2 C 0.3997(10) 0.3260(8) 0.2410(2) 0.048(2) Uani 1 1 d . . . C3 C 0.3308(9) 0.3719(9) 0.2155(2) 0.0440(19) Uani 1 1 d . . . H3 H 0.2836 0.4208 0.2249 0.053 Uiso 1 1 calc R . . C4 C 0.3298(9) 0.3463(9) 0.1746(2) 0.048(2) Uani 1 1 d . . . C5 C 0.2277(9) 0.3691(9) 0.1501(2) 0.049(2) Uani 1 1 d . . . C7 C 0.0468(10) 0.4019(11) 0.1354(3) 0.054(2) Uani 1 1 d . . . H7 H -0.0324 0.4183 0.1374 0.064 Uiso 1 1 calc R . . C8 C 0.0933(9) 0.3773(9) 0.1038(2) 0.0450(19) Uani 1 1 d . . . H8 H 0.0574 0.3770 0.0791 0.054 Uiso 1 1 calc R . . C9 C 0.2084(9) 0.3509(9) 0.1129(2) 0.050(2) Uani 1 1 d . . . H9 H 0.2606 0.3254 0.0958 0.060 Uiso 1 1 calc R . . C10 C 0.9539(9) 0.3417(9) 0.2636(2) 0.049(2) Uani 1 1 d . . . C11 C 0.8754(8) 0.3796(9) 0.2346(2) 0.0443(19) Uani 1 1 d . . . C12 C 0.9128(10) 0.5252(10) 0.2310(2) 0.055(2) Uani 1 1 d . . . H12 H 0.9931 0.5958 0.2449 0.066 Uiso 1 1 calc R . . C13 C 0.8351(9) 0.5728(9) 0.2069(2) 0.0471(19) Uani 1 1 d . . . C14 C 0.8905(9) 0.7320(10) 0.2035(2) 0.048(2) Uani 1 1 d . . . C15 C 0.8221(9) 0.7924(9) 0.1853(2) 0.0484(19) Uani 1 1 d . . . H15 H 0.7323 0.7456 0.1723 0.058 Uiso 1 1 calc R . . C16 C 1.0291(10) 0.9679(9) 0.2102(2) 0.050(2) Uani 1 1 d . . . H16 H 1.1062 1.0599 0.2174 0.060 Uiso 1 1 calc R . . C17 C 0.9227(9) 0.9505(9) 0.1905(2) 0.048(2) Uani 1 1 d . . . H17 H 0.9090 1.0255 0.1807 0.057 Uiso 1 1 calc R . . C19 C 0.7477(9) 0.4000(9) 0.0528(2) 0.0478(19) Uani 1 1 d . . . C20 C 0.7055(8) 0.2902(9) 0.0846(2) 0.0415(17) Uani 1 1 d . . . C21 C 0.7070(8) 0.1644(9) 0.0790(2) 0.0455(19) Uani 1 1 d . . . H21 H 0.7349 0.1472 0.0549 0.055 Uiso 1 1 calc R . . C22 C 0.6690(10) 0.0592(10) 0.1075(3) 0.054(2) Uani 1 1 d . . . C23 C 0.6510(9) -0.0867(10) 0.0973(2) 0.048(2) Uani 1 1 d . . . C25 C 0.6591(9) -0.2640(9) 0.0659(2) 0.049(2) Uani 1 1 d . . . H25 H 0.6728 -0.3174 0.0465 0.059 Uiso 1 1 calc R . . C26 C 0.6079(10) -0.3122(10) 0.0997(3) 0.058(2) Uani 1 1 d . . . H26 H 0.5777 -0.4063 0.1092 0.069 Uiso 1 1 calc R . . C27 C 0.6054(8) -0.1991(10) 0.1198(3) 0.048(2) Uani 1 1 d . . . H27 H 0.5756 -0.2036 0.1454 0.057 Uiso 1 1 calc R . . C28 C 0.0767(8) -0.0442(10) 0.0455(3) 0.052(2) Uani 1 1 d . . . H28 H 0.0239 -0.0613 0.0684 0.062 Uiso 1 1 calc R . . C29 C 0.0041(10) -0.0747(9) 0.0101(2) 0.049(2) Uani 1 1 d . . . H29 H -0.0973 -0.1122 0.0093 0.058 Uiso 1 1 calc R . . C30 C 0.0830(10) -0.0492(10) -0.0241(3) 0.058(2) Uani 1 1 d . . . H30 H 0.0344 -0.0695 -0.0478 0.070 Uiso 1 1 calc R . . C31 C 0.2345(10) 0.0068(10) -0.0230(3) 0.056(2) Uani 1 1 d . . . H31 H 0.2873 0.0239 -0.0459 0.067 Uiso 1 1 calc R . . C32 C 0.3071(10) 0.0373(11) 0.0124(3) 0.055(2) Uani 1 1 d . . . H32 H 0.4085 0.0748 0.0132 0.066 Uiso 1 1 calc R . . C33 C 0.2282(10) 0.0118(10) 0.0467(3) 0.050(2) Uani 1 1 d . . . C34 C 0.3116(9) 0.0402(9) 0.0839(2) 0.048(2) Uani 1 1 d . . . H34A H 0.3615 0.1455 0.0887 0.058 Uiso 1 1 calc R . . H34B H 0.3875 0.0141 0.0799 0.058 Uiso 1 1 calc R . . C35 C 0.2289(10) -0.0362(9) 0.1201(2) 0.0450(19) Uani 1 1 d . . . H35 H 0.1586 -0.0032 0.1261 0.054 Uiso 1 1 calc R . . C36 C 0.1472(10) -0.2047(10) 0.1195(3) 0.057(2) Uani 1 1 d . . . H36A H 0.0417 -0.2436 0.1215 0.069 Uiso 1 1 calc R . . H36B H 0.1673 -0.2399 0.0955 0.069 Uiso 1 1 calc R . . C37 C 0.3032(9) -0.1259(9) 0.1671(2) 0.0448(18) Uani 1 1 d . . . C38 C 0.3912(9) -0.1331(9) 0.1981(2) 0.0469(19) Uani 1 1 d . . . C39 C 0.4933(10) -0.2290(9) 0.2375(2) 0.050(2) Uani 1 1 d . . . H39A H 0.5642 -0.2556 0.2280 0.060 Uiso 1 1 calc R . . H39B H 0.4509 -0.2812 0.2615 0.060 Uiso 1 1 calc R . . C40 C 0.5659(10) -0.0604(10) 0.2432(2) 0.053(2) Uani 1 1 d . . . H40 H 0.6700 -0.0138 0.2356 0.063 Uiso 1 1 calc R . . C41 C 0.5557(9) -0.0128(10) 0.2842(2) 0.049(2) Uani 1 1 d . . . H41A H 0.6350 -0.0102 0.2994 0.059 Uiso 1 1 calc R . . H41B H 0.5726 0.0870 0.2832 0.059 Uiso 1 1 calc R . . C42 C 0.4127(9) -0.1074(9) 0.3053(2) 0.049(2) Uani 1 1 d . . . C43 C 0.4042(10) -0.2105(9) 0.3321(2) 0.053(2) Uani 1 1 d . . . H43 H 0.4874 -0.2177 0.3376 0.064 Uiso 1 1 calc R . . C44 C 0.2715(9) -0.3029(9) 0.3507(2) 0.050(2) Uani 1 1 d . . . H44 H 0.2659 -0.3719 0.3686 0.060 Uiso 1 1 calc R . . C45 C 0.1473(9) -0.2922(9) 0.3424(2) 0.049(2) Uani 1 1 d . . . H45 H 0.0585 -0.3540 0.3548 0.059 Uiso 1 1 calc R . . C46 C 0.1557(9) -0.1890(10) 0.3157(2) 0.052(2) Uani 1 1 d . . . H46 H 0.0726 -0.1818 0.3102 0.063 Uiso 1 1 calc R . . C47 C 0.2884(9) -0.0967(10) 0.2971(2) 0.050(2) Uani 1 1 d . . . H47 H 0.2941 -0.0277 0.2792 0.060 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 Sm1 0.0465(3) 0.0436(2) 0.03433(17) -0.0046(2) -0.0035(2) 0.0120(2) F1 0.042(2) 0.050(3) 0.044(2) 0.009(2) 0.0200(19) 0.016(2) F2 0.050(3) 0.043(3) 0.046(2) -0.0205(19) -0.001(2) 0.023(2) F3 0.041(2) 0.049(3) 0.045(2) -0.023(2) -0.018(2) 0.022(2) F4 0.056(3) 0.043(3) 0.044(3) 0.010(2) 0.006(2) 0.024(2) F5 0.042(3) 0.039(2) 0.053(3) -0.012(2) -0.018(2) 0.011(2) F6 0.051(3) 0.041(3) 0.056(3) -0.013(2) -0.012(2) 0.017(2) F7 0.051(3) 0.052(3) 0.048(3) 0.013(2) 0.017(2) 0.018(2) F8 0.054(3) 0.043(3) 0.050(3) 0.016(2) -0.011(2) 0.014(2) F9 0.041(3) 0.041(3) 0.044(3) 0.0090(19) 0.0149(19) 0.012(2) O1 0.047(3) 0.049(3) 0.037(3) 0.010(2) 0.003(2) 0.019(3) O2 0.047(3) 0.044(3) 0.037(3) 0.003(2) -0.001(2) 0.014(3) O3 0.045(3) 0.040(3) 0.046(3) -0.010(3) -0.006(2) 0.012(3) O4 0.039(3) 0.040(3) 0.042(3) -0.009(2) -0.011(2) 0.012(2) O5 0.044(3) 0.045(3) 0.054(3) 0.004(3) 0.011(3) 0.015(3) O6 0.047(4) 0.047(3) 0.045(3) 0.003(3) 0.001(3) 0.019(3) O7 0.056(4) 0.042(3) 0.047(3) -0.007(2) -0.014(3) 0.016(3) O8 0.039(3) 0.047(3) 0.047(3) -0.004(2) -0.015(2) -0.004(3) O9 0.038(3) 0.039(3) 0.053(3) -0.011(2) -0.018(3) 0.014(2) O10 0.045(3) 0.044(3) 0.045(3) -0.010(2) -0.009(2) 0.014(3) O11 0.052(3) 0.047(3) 0.048(3) -0.005(3) 0.015(3) 0.015(3) N1 0.038(4) 0.039(4) 0.042(4) 0.002(3) 0.004(3) 0.012(3) N2 0.053(4) 0.039(4) 0.052(4) -0.004(3) -0.005(3) 0.013(3) C1 0.050(5) 0.050(5) 0.041(5) -0.010(4) -0.004(4) 0.019(4) C2 0.058(5) 0.027(4) 0.049(5) -0.009(3) -0.003(4) 0.015(4) C3 0.042(4) 0.041(4) 0.038(4) -0.014(3) -0.005(3) 0.012(4) C4 0.041(4) 0.043(5) 0.048(5) -0.004(4) -0.003(4) 0.013(4) C5 0.038(4) 0.045(5) 0.050(5) -0.010(4) -0.013(4) 0.009(4) C7 0.046(5) 0.062(6) 0.052(6) 0.022(4) 0.001(4) 0.026(4) C8 0.045(4) 0.048(5) 0.034(4) 0.011(3) -0.014(3) 0.018(4) C9 0.048(5) 0.049(5) 0.050(5) -0.011(4) -0.019(4) 0.023(4) C10 0.048(5) 0.050(5) 0.039(4) -0.024(4) -0.005(4) 0.015(4) C11 0.035(4) 0.046(5) 0.036(4) -0.006(3) 0.001(3) 0.009(4) C12 0.055(5) 0.051(5) 0.045(5) -0.004(4) -0.007(4) 0.016(4) C13 0.045(5) 0.040(4) 0.048(5) -0.001(3) -0.004(4) 0.015(4) C14 0.036(4) 0.051(5) 0.047(5) -0.002(4) -0.008(4) 0.015(4) C15 0.041(4) 0.048(5) 0.042(4) -0.017(4) -0.014(3) 0.011(4) C16 0.047(5) 0.044(5) 0.043(4) -0.013(4) 0.011(4) 0.012(4) C17 0.052(5) 0.053(5) 0.037(4) 0.020(3) 0.015(4) 0.025(4) C19 0.045(5) 0.040(4) 0.048(5) 0.008(3) 0.013(4) 0.013(4) C20 0.039(4) 0.044(4) 0.038(4) -0.001(3) -0.001(3) 0.018(3) C21 0.036(4) 0.047(5) 0.042(5) -0.009(3) -0.002(3) 0.012(4) C22 0.052(5) 0.047(5) 0.050(5) -0.015(4) -0.006(4) 0.014(4) C23 0.040(5) 0.057(5) 0.035(4) -0.014(4) -0.008(3) 0.015(4) C25 0.051(5) 0.047(5) 0.051(5) -0.015(4) 0.017(4) 0.025(4) C26 0.063(6) 0.050(5) 0.052(5) 0.013(4) 0.014(4) 0.022(5) C27 0.036(4) 0.057(5) 0.054(5) 0.014(4) 0.013(4) 0.027(4) C28 0.025(4) 0.057(5) 0.061(6) 0.022(4) 0.004(4) 0.012(4) C29 0.046(5) 0.039(4) 0.051(5) 0.009(4) -0.017(4) 0.014(4) C30 0.055(5) 0.050(5) 0.052(5) -0.012(4) -0.019(4) 0.012(4) C31 0.049(5) 0.051(5) 0.062(5) -0.017(4) -0.013(4) 0.020(4) C32 0.039(5) 0.061(6) 0.055(5) -0.008(4) 0.004(4) 0.018(4) C33 0.040(5) 0.054(5) 0.048(5) -0.007(4) -0.017(4) 0.017(4) C34 0.047(5) 0.043(5) 0.047(5) -0.017(4) -0.007(4) 0.017(4) C35 0.052(5) 0.037(4) 0.040(4) -0.013(3) -0.002(4) 0.018(4) C36 0.052(5) 0.049(5) 0.050(5) -0.010(4) -0.018(4) 0.010(4) C37 0.042(4) 0.044(5) 0.041(4) 0.001(3) 0.001(3) 0.016(4) C38 0.040(4) 0.046(5) 0.042(4) 0.001(4) 0.003(3) 0.012(4) C39 0.061(5) 0.045(5) 0.042(5) 0.006(4) 0.005(4) 0.025(4) C40 0.051(5) 0.049(5) 0.043(5) 0.012(4) -0.001(4) 0.014(4) C41 0.044(5) 0.054(5) 0.036(4) -0.001(4) -0.011(3) 0.014(4) C42 0.044(5) 0.038(5) 0.046(5) -0.006(4) -0.006(4) 0.007(4) C43 0.050(5) 0.051(5) 0.041(5) 0.006(4) 0.009(4) 0.013(4) C44 0.055(5) 0.038(4) 0.052(5) 0.016(4) 0.022(4) 0.020(4) C45 0.040(5) 0.048(5) 0.035(4) -0.016(4) 0.012(3) 0.003(4) C46 0.045(5) 0.052(5) 0.038(4) -0.011(4) -0.010(3) 0.008(4) C47 0.043(5) 0.055(5) 0.044(4) -0.022(4) -0.012(4) 0.019(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 Sm1 O3 2.322(6) . ? Sm1 O1 2.340(6) . ? Sm1 O2 2.345(6) . ? Sm1 O5 2.356(6) . ? Sm1 O4 2.418(5) . ? Sm1 O6 2.431(6) . ? Sm1 N1 2.634(6) . ? Sm1 N2 2.654(7) . ? F1 C1 1.281(9) . ? F2 C1 1.311(10) . ? F3 C1 1.278(10) . ? F4 C10 1.303(9) . ? F5 C10 1.341(9) . ? F6 C10 1.328(9) . ? F7 C19 1.308(9) . ? F8 C19 1.374(10) . ? F9 C19 1.309(9) . ? O1 C2 1.250(10) . ? O2 C4 1.244(10) . ? O3 C11 1.265(9) . ? O4 C13 1.237(9) . ? O5 C20 1.272(9) . ? O6 C22 1.223(10) . ? O7 C38 1.330(10) . ? O7 C39 1.481(10) . ? O8 C37 1.328(9) . ? O8 C36 1.424(10) . ? O9 C5 1.350(10) . ? O9 C7 1.364(10) . ? O10 C14 1.375(10) . ? O10 C16 1.405(10) . ? O11 C23 1.343(9) . ? O11 C25 1.410(10) . ? N1 C38 1.277(10) . ? N1 C40 1.467(11) . ? N2 C37 1.272(10) . ? N2 C35 1.458(11) . ? C1 C2 1.495(11) . ? C2 C3 1.368(12) . ? C3 C4 1.436(11) . ? C3 H3 0.9300 . ? C4 C5 1.473(12) . ? C5 C9 1.300(11) . ? C7 C8 1.272(12) . ? C7 H7 0.9300 . ? C8 C9 1.401(11) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.469(12) . ? C11 C12 1.377(12) . ? C12 C13 1.415(12) . ? C12 H12 0.9300 . ? C13 C14 1.471(12) . ? C14 C15 1.328(12) . ? C15 C17 1.463(12) . ? C15 H15 0.9300 . ? C16 C17 1.237(12) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.488(11) . ? C20 C21 1.339(11) . ? C21 C22 1.380(12) . ? C21 H21 0.9300 . ? C22 C23 1.485(12) . ? C23 C27 1.286(12) . ? C25 C26 1.278(12) . ? C25 H25 0.9300 . ? C26 C27 1.383(12) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.390(12) . ? C28 C33 1.390(11) . ? C28 H28 0.9300 . ? C29 C30 1.390(13) . ? C29 H29 0.9300 . ? C30 C31 1.390(13) . ? C30 H30 0.9300 . ? C31 C32 1.390(12) . ? C31 H31 0.9300 . ? C32 C33 1.390(12) . ? C32 H32 0.9300 . ? C33 C34 1.497(11) . ? C34 C35 1.503(11) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.528(12) . ? C35 H35 0.9800 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.436(11) . ? C39 C40 1.546(12) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.525(12) . ? C40 H40 0.9800 . ? C41 C42 1.508(12) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.390(12) . ? C42 C47 1.390(12) . ? C43 C44 1.390(11) . ? C43 H43 0.9300 . ? C44 C45 1.390(12) . ? C44 H44 0.9300 . ? C45 C46 1.390(13) . ? C45 H45 0.9300 . ? C46 C47 1.390(12) . ? C46 H46 0.9300 . ? C47 H47 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 O3 Sm1 O1 85.9(2) . . ? O3 Sm1 O2 147.20(19) . . ? O1 Sm1 O2 72.45(19) . . ? O3 Sm1 O5 108.5(2) . . ? O1 Sm1 O5 144.1(2) . . ? O2 Sm1 O5 78.8(2) . . ? O3 Sm1 O4 71.87(19) . . ? O1 Sm1 O4 79.51(19) . . ? O2 Sm1 O4 79.97(18) . . ? O5 Sm1 O4 74.53(19) . . ? O3 Sm1 O6 84.8(2) . . ? O1 Sm1 O6 145.88(19) . . ? O2 Sm1 O6 126.69(19) . . ? O5 Sm1 O6 69.7(2) . . ? O4 Sm1 O6 127.7(2) . . ? O3 Sm1 N1 74.4(2) . . ? O1 Sm1 N1 75.83(19) . . ? O2 Sm1 N1 121.45(19) . . ? O5 Sm1 N1 139.1(2) . . ? O4 Sm1 N1 139.19(19) . . ? O6 Sm1 N1 70.05(19) . . ? O3 Sm1 N2 136.5(2) . . ? O1 Sm1 N2 93.7(2) . . ? O2 Sm1 N2 70.9(2) . . ? O5 Sm1 N2 96.9(2) . . ? O4 Sm1 N2 150.8(2) . . ? O6 Sm1 N2 71.5(2) . . ? N1 Sm1 N2 63.5(2) . . ? C2 O1 Sm1 134.3(5) . . ? C4 O2 Sm1 135.9(5) . . ? C11 O3 Sm1 137.9(6) . . ? C13 O4 Sm1 134.7(5) . . ? C20 O5 Sm1 137.3(5) . . ? C22 O6 Sm1 135.7(6) . . ? C38 O7 C39 106.5(6) . . ? C37 O8 C36 104.0(6) . . ? C5 O9 C7 104.7(7) . . ? C14 O10 C16 102.1(7) . . ? C23 O11 C25 105.2(6) . . ? C38 N1 C40 108.3(7) . . ? C38 N1 Sm1 114.6(5) . . ? C40 N1 Sm1 131.1(5) . . ? C37 N2 C35 107.4(7) . . ? C37 N2 Sm1 114.9(6) . . ? C35 N2 Sm1 135.5(5) . . ? F3 C1 F1 103.5(7) . . ? F3 C1 F2 105.7(6) . . ? F1 C1 F2 107.0(7) . . ? F3 C1 C2 111.7(8) . . ? F1 C1 C2 112.6(7) . . ? F2 C1 C2 115.6(7) . . ? O1 C2 C3 127.2(8) . . ? O1 C2 C1 115.0(8) . . ? C3 C2 C1 117.7(8) . . ? C2 C3 C4 121.5(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? O2 C4 C3 125.2(8) . . ? O2 C4 C5 116.5(7) . . ? C3 C4 C5 118.2(8) . . ? C9 C5 O9 110.7(8) . . ? C9 C5 C4 128.1(9) . . ? O9 C5 C4 121.0(7) . . ? C8 C7 O9 110.8(8) . . ? C8 C7 H7 124.6 . . ? O9 C7 H7 124.6 . . ? C7 C8 C9 107.6(7) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? C5 C9 C8 106.2(8) . . ? C5 C9 H9 126.9 . . ? C8 C9 H9 126.9 . . ? F4 C10 F6 106.1(7) . . ? F4 C10 F5 106.1(6) . . ? F6 C10 F5 104.0(7) . . ? F4 C10 C11 113.8(7) . . ? F6 C10 C11 112.6(6) . . ? F5 C10 C11 113.4(7) . . ? O3 C11 C12 125.5(8) . . ? O3 C11 C10 116.1(8) . . ? C12 C11 C10 118.3(7) . . ? C11 C12 C13 123.2(8) . . ? C11 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? O4 C13 C12 126.3(8) . . ? O4 C13 C14 115.3(7) . . ? C12 C13 C14 118.4(7) . . ? C15 C14 O10 113.2(8) . . ? C15 C14 C13 125.2(8) . . ? O10 C14 C13 121.5(7) . . ? C14 C15 C17 103.0(7) . . ? C14 C15 H15 128.5 . . ? C17 C15 H15 128.5 . . ? C17 C16 O10 113.0(7) . . ? C17 C16 H16 123.5 . . ? O10 C16 H16 123.5 . . ? C16 C17 C15 108.7(8) . . ? C16 C17 H17 125.7 . . ? C15 C17 H17 125.7 . . ? F7 C19 F9 107.6(6) . . ? F7 C19 F8 106.9(7) . . ? F9 C19 F8 102.7(7) . . ? F7 C19 C20 115.0(7) . . ? F9 C19 C20 113.0(7) . . ? F8 C19 C20 110.9(6) . . ? O5 C20 C21 126.8(7) . . ? O5 C20 C19 112.6(7) . . ? C21 C20 C19 120.5(7) . . ? C20 C21 C22 122.8(8) . . ? C20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? O6 C22 C21 126.3(8) . . ? O6 C22 C23 114.3(8) . . ? C21 C22 C23 119.3(8) . . ? C27 C23 O11 109.6(8) . . ? C27 C23 C22 126.5(8) . . ? O11 C23 C22 123.7(8) . . ? C26 C25 O11 108.6(7) . . ? C26 C25 H25 125.7 . . ? O11 C25 H25 125.7 . . ? C25 C26 C27 107.6(8) . . ? C25 C26 H26 126.2 . . ? C27 C26 H26 126.2 . . ? C23 C27 C26 108.9(8) . . ? C23 C27 H27 125.5 . . ? C26 C27 H27 125.5 . . ? C29 C28 C33 120.0(8) . . ? C29 C28 H28 120.0 . . ? C33 C28 H28 120.0 . . ? C30 C29 C28 120.0(8) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0(8) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0(9) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.0(8) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.0(8) . . ? C32 C33 C34 117.4(8) . . ? C28 C33 C34 122.5(8) . . ? C33 C34 C35 119.0(7) . . ? C33 C34 H34A 107.6 . . ? C35 C34 H34A 107.6 . . ? C33 C34 H34B 107.6 . . ? C35 C34 H34B 107.6 . . ? H34A C34 H34B 107.0 . . ? N2 C35 C34 111.6(7) . . ? N2 C35 C36 101.8(7) . . ? C34 C35 C36 116.4(7) . . ? N2 C35 H35 108.9 . . ? C34 C35 H35 108.9 . . ? C36 C35 H35 108.9 . . ? O8 C36 C35 107.1(6) . . ? O8 C36 H36A 110.3 . . ? C35 C36 H36A 110.3 . . ? O8 C36 H36B 110.3 . . ? C35 C36 H36B 110.3 . . ? H36A C36 H36B 108.5 . . ? N2 C37 O8 119.5(7) . . ? N2 C37 C38 121.7(7) . . ? O8 C37 C38 118.7(7) . . ? N1 C38 O7 118.0(7) . . ? N1 C38 C37 121.8(8) . . ? O7 C38 C37 120.1(7) . . ? O7 C39 C40 103.3(6) . . ? O7 C39 H39A 111.1 . . ? C40 C39 H39A 111.1 . . ? O7 C39 H39B 111.1 . . ? C40 C39 H39B 111.1 . . ? H39A C39 H39B 109.1 . . ? N1 C40 C41 111.4(8) . . ? N1 C40 C39 103.7(7) . . ? C41 C40 C39 114.6(7) . . ? N1 C40 H40 109.0 . . ? C41 C40 H40 109.0 . . ? C39 C40 H40 109.0 . . ? C42 C41 C40 116.4(7) . . ? C42 C41 H41A 108.2 . . ? C40 C41 H41A 108.2 . . ? C42 C41 H41B 108.2 . . ? C40 C41 H41B 108.2 . . ? H41A C41 H41B 107.3 . . ? C43 C42 C47 120.0(8) . . ? C43 C42 C41 119.2(8) . . ? C47 C42 C41 120.7(8) . . ? C44 C43 C42 120.0(9) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0(8) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0(7) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0(9) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C42 120.0(9) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? 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 O3 Sm1 O1 C2 135.5(7) . . . . ? O2 Sm1 O1 C2 -19.5(7) . . . . ? O5 Sm1 O1 C2 19.1(9) . . . . ? O4 Sm1 O1 C2 63.2(7) . . . . ? O6 Sm1 O1 C2 -150.0(7) . . . . ? N1 Sm1 O1 C2 -149.6(7) . . . . ? N2 Sm1 O1 C2 -88.1(7) . . . . ? O3 Sm1 O2 C4 -45.0(9) . . . . ? O1 Sm1 O2 C4 6.1(7) . . . . ? O5 Sm1 O2 C4 -152.0(8) . . . . ? O4 Sm1 O2 C4 -75.9(8) . . . . ? O6 Sm1 O2 C4 154.0(7) . . . . ? N1 Sm1 O2 C4 66.5(8) . . . . ? N2 Sm1 O2 C4 106.6(8) . . . . ? O1 Sm1 O3 C11 -71.2(8) . . . . ? O2 Sm1 O3 C11 -23.1(10) . . . . ? O5 Sm1 O3 C11 75.1(8) . . . . ? O4 Sm1 O3 C11 9.1(7) . . . . ? O6 Sm1 O3 C11 141.7(8) . . . . ? N1 Sm1 O3 C11 -147.6(8) . . . . ? N2 Sm1 O3 C11 -162.3(7) . . . . ? O3 Sm1 O4 C13 -5.4(7) . . . . ? O1 Sm1 O4 C13 83.7(8) . . . . ? O2 Sm1 O4 C13 157.5(8) . . . . ? O5 Sm1 O4 C13 -121.4(8) . . . . ? O6 Sm1 O4 C13 -73.4(8) . . . . ? N1 Sm1 O4 C13 30.3(9) . . . . ? N2 Sm1 O4 C13 162.4(7) . . . . ? O3 Sm1 O5 C20 83.8(8) . . . . ? O1 Sm1 O5 C20 -166.6(6) . . . . ? O2 Sm1 O5 C20 -129.3(8) . . . . ? O4 Sm1 O5 C20 148.1(8) . . . . ? O6 Sm1 O5 C20 6.9(7) . . . . ? N1 Sm1 O5 C20 -3.5(9) . . . . ? N2 Sm1 O5 C20 -60.4(8) . . . . ? O3 Sm1 O6 C22 -125.1(8) . . . . ? O1 Sm1 O6 C22 160.1(7) . . . . ? O2 Sm1 O6 C22 44.7(9) . . . . ? O5 Sm1 O6 C22 -13.1(8) . . . . ? O4 Sm1 O6 C22 -62.9(9) . . . . ? N1 Sm1 O6 C22 159.6(8) . . . . ? N2 Sm1 O6 C22 92.0(8) . . . . ? O3 Sm1 N1 C38 -152.7(6) . . . . ? O1 Sm1 N1 C38 117.6(6) . . . . ? O2 Sm1 N1 C38 58.8(7) . . . . ? O5 Sm1 N1 C38 -52.2(7) . . . . ? O4 Sm1 N1 C38 172.2(5) . . . . ? O6 Sm1 N1 C38 -62.7(6) . . . . ? N2 Sm1 N1 C38 16.0(6) . . . . ? O3 Sm1 N1 C40 -3.6(7) . . . . ? O1 Sm1 N1 C40 -93.3(7) . . . . ? O2 Sm1 N1 C40 -152.0(6) . . . . ? O5 Sm1 N1 C40 96.9(7) . . . . ? O4 Sm1 N1 C40 -38.7(8) . . . . ? O6 Sm1 N1 C40 86.4(7) . . . . ? N2 Sm1 N1 C40 165.1(7) . . . . ? O3 Sm1 N2 C37 3.5(8) . . . . ? O1 Sm1 N2 C37 -84.6(6) . . . . ? O2 Sm1 N2 C37 -154.6(7) . . . . ? O5 Sm1 N2 C37 129.8(6) . . . . ? O4 Sm1 N2 C37 -159.6(5) . . . . ? O6 Sm1 N2 C37 64.0(6) . . . . ? N1 Sm1 N2 C37 -12.4(6) . . . . ? O3 Sm1 N2 C35 -157.2(7) . . . . ? O1 Sm1 N2 C35 114.8(8) . . . . ? O2 Sm1 N2 C35 44.8(7) . . . . ? O5 Sm1 N2 C35 -30.8(8) . . . . ? O4 Sm1 N2 C35 39.7(10) . . . . ? O6 Sm1 N2 C35 -96.7(8) . . . . ? N1 Sm1 N2 C35 -173.1(8) . . . . ? Sm1 O1 C2 C3 20.8(13) . . . . ? Sm1 O1 C2 C1 -164.9(5) . . . . ? F3 C1 C2 O1 36.3(10) . . . . ? F1 C1 C2 O1 -79.6(10) . . . . ? F2 C1 C2 O1 157.1(7) . . . . ? F3 C1 C2 C3 -148.9(8) . . . . ? F1 C1 C2 C3 95.2(9) . . . . ? F2 C1 C2 C3 -28.1(11) . . . . ? O1 C2 C3 C4 -0.4(13) . . . . ? C1 C2 C3 C4 -174.5(7) . . . . ? Sm1 O2 C4 C3 6.1(13) . . . . ? Sm1 O2 C4 C5 -173.7(5) . . . . ? C2 C3 C4 O2 -12.9(13) . . . . ? C2 C3 C4 C5 166.9(8) . . . . ? C7 O9 C5 C9 -0.3(9) . . . . ? C7 O9 C5 C4 -175.0(8) . . . . ? O2 C4 C5 C9 0.5(13) . . . . ? C3 C4 C5 C9 -179.3(8) . . . . ? O2 C4 C5 O9 174.3(7) . . . . ? C3 C4 C5 O9 -5.5(12) . . . . ? C5 O9 C7 C8 -1.8(10) . . . . ? O9 C7 C8 C9 3.0(10) . . . . ? O9 C5 C9 C8 2.0(9) . . . . ? C4 C5 C9 C8 176.3(8) . . . . ? C7 C8 C9 C5 -3.1(10) . . . . ? Sm1 O3 C11 C12 -9.8(13) . . . . ? Sm1 O3 C11 C10 166.1(5) . . . . ? F4 C10 C11 O3 -82.1(9) . . . . ? F6 C10 C11 O3 38.6(10) . . . . ? F5 C10 C11 O3 156.4(7) . . . . ? F4 C10 C11 C12 94.1(9) . . . . ? F6 C10 C11 C12 -145.1(8) . . . . ? F5 C10 C11 C12 -27.3(10) . . . . ? O3 C11 C12 C13 2.4(14) . . . . ? C10 C11 C12 C13 -173.5(8) . . . . ? Sm1 O4 C13 C12 2.8(14) . . . . ? Sm1 O4 C13 C14 -179.9(5) . . . . ? C11 C12 C13 O4 0.7(15) . . . . ? C11 C12 C13 C14 -176.5(8) . . . . ? C16 O10 C14 C15 -0.7(9) . . . . ? C16 O10 C14 C13 -179.6(8) . . . . ? O4 C13 C14 C15 9.3(14) . . . . ? C12 C13 C14 C15 -173.2(9) . . . . ? O4 C13 C14 O10 -172.0(7) . . . . ? C12 C13 C14 O10 5.5(13) . . . . ? O10 C14 C15 C17 1.2(10) . . . . ? C13 C14 C15 C17 -180.0(8) . . . . ? C14 O10 C16 C17 -0.2(9) . . . . ? O10 C16 C17 C15 1.0(10) . . . . ? C14 C15 C17 C16 -1.3(10) . . . . ? Sm1 O5 C20 C21 -2.9(13) . . . . ? Sm1 O5 C20 C19 175.8(5) . . . . ? F7 C19 C20 O5 175.4(7) . . . . ? F9 C19 C20 O5 51.4(9) . . . . ? F8 C19 C20 O5 -63.3(9) . . . . ? F7 C19 C20 C21 -5.8(11) . . . . ? F9 C19 C20 C21 -129.8(8) . . . . ? F8 C19 C20 C21 115.6(8) . . . . ? O5 C20 C21 C22 -1.4(13) . . . . ? C19 C20 C21 C22 180.0(8) . . . . ? Sm1 O6 C22 C21 15.3(14) . . . . ? Sm1 O6 C22 C23 -160.3(6) . . . . ? C20 C21 C22 O6 -4.8(14) . . . . ? C20 C21 C22 C23 170.5(8) . . . . ? C25 O11 C23 C27 2.8(9) . . . . ? C25 O11 C23 C22 178.4(8) . . . . ? O6 C22 C23 C27 1.6(13) . . . . ? C21 C22 C23 C27 -174.3(9) . . . . ? O6 C22 C23 O11 -173.3(8) . . . . ? C21 C22 C23 O11 10.7(13) . . . . ? C23 O11 C25 C26 -1.6(10) . . . . ? O11 C25 C26 C27 -0.1(11) . . . . ? O11 C23 C27 C26 -2.9(10) . . . . ? C22 C23 C27 C26 -178.4(8) . . . . ? C25 C26 C27 C23 1.9(11) . . . . ? C33 C28 C29 C30 0.0(13) . . . . ? C28 C29 C30 C31 0.0(13) . . . . ? C29 C30 C31 C32 0.0(14) . . . . ? C30 C31 C32 C33 0.0(14) . . . . ? C31 C32 C33 C28 0.0(14) . . . . ? C31 C32 C33 C34 177.2(8) . . . . ? C29 C28 C33 C32 0.0(14) . . . . ? C29 C28 C33 C34 -177.1(8) . . . . ? C32 C33 C34 C35 -157.2(8) . . . . ? C28 C33 C34 C35 20.0(13) . . . . ? C37 N2 C35 C34 -125.9(8) . . . . ? Sm1 N2 C35 C34 35.8(10) . . . . ? C37 N2 C35 C36 -1.1(9) . . . . ? Sm1 N2 C35 C36 160.6(6) . . . . ? C33 C34 C35 N2 176.3(7) . . . . ? C33 C34 C35 C36 60.1(11) . . . . ? C37 O8 C36 C35 -3.8(9) . . . . ? N2 C35 C36 O8 3.0(9) . . . . ? C34 C35 C36 O8 124.6(8) . . . . ? C35 N2 C37 O8 -1.5(11) . . . . ? Sm1 N2 C37 O8 -167.4(6) . . . . ? C35 N2 C37 C38 174.8(7) . . . . ? Sm1 N2 C37 C38 8.9(10) . . . . ? C36 O8 C37 N2 3.5(10) . . . . ? C36 O8 C37 C38 -172.9(7) . . . . ? C40 N1 C38 O7 1.8(10) . . . . ? Sm1 N1 C38 O7 157.8(6) . . . . ? C40 N1 C38 C37 -175.5(7) . . . . ? Sm1 N1 C38 C37 -19.6(10) . . . . ? C39 O7 C38 N1 -3.5(10) . . . . ? C39 O7 C38 C37 173.8(7) . . . . ? N2 C37 C38 N1 7.6(13) . . . . ? O8 C37 C38 N1 -176.1(8) . . . . ? N2 C37 C38 O7 -169.7(8) . . . . ? O8 C37 C38 O7 6.7(12) . . . . ? C38 O7 C39 C40 3.5(9) . . . . ? C38 N1 C40 C41 -123.1(8) . . . . ? Sm1 N1 C40 C41 86.4(8) . . . . ? C38 N1 C40 C39 0.7(9) . . . . ? Sm1 N1 C40 C39 -149.9(6) . . . . ? O7 C39 C40 N1 -2.5(8) . . . . ? O7 C39 C40 C41 119.1(8) . . . . ? N1 C40 C41 C42 78.4(10) . . . . ? C39 C40 C41 C42 -38.9(11) . . . . ? C40 C41 C42 C43 99.9(10) . . . . ? C40 C41 C42 C47 -77.3(11) . . . . ? C47 C42 C43 C44 0.0(13) . . . . ? C41 C42 C43 C44 -177.3(8) . . . . ? C42 C43 C44 C45 0.0(13) . . . . ? C43 C44 C45 C46 0.0(12) . . . . ? C44 C45 C46 C47 0.0(12) . . . . ? C45 C46 C47 C42 0.0(12) . . . . ? C43 C42 C47 C46 0.0(12) . . . . ? C41 C42 C47 C46 177.3(7) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.029 _refine_diff_density_min -1.028 _refine_diff_density_rms 0.091 # Attachment 'Tb.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 752496' #TrackingRef 'Tb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 F9 N2 O11 Tb' _chemical_formula_sum 'C44 H32 F9 N2 O11 Tb' _chemical_formula_weight 1094.64 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'P3(2) ' _symmetry_space_group_name_Hall 'P 32 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 10.4758(16) _cell_length_b 10.4758(16) _cell_length_c 34.546(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3283.2(10) _cell_formula_units_Z 3 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3467 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 19.85 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17671 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5850 _reflns_number_gt 4813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.055P)^2^+1.99P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(14) _chemical_absolute_configuration unk _refine_ls_number_reflns 5850 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3856(10) 0.3282(11) 0.0614(3) 0.045(2) Uani 1 1 d . . . C2 C 0.4176(12) 0.3495(11) 0.1035(3) 0.046(2) Uani 1 1 d . . . C3 C 0.2988(10) 0.2999(11) 0.1283(3) 0.040(2) Uani 1 1 d . . . H3 H 0.2035 0.2547 0.1184 0.048 Uiso 1 1 calc R . . C4 C 0.3233(11) 0.3185(10) 0.1700(3) 0.041(2) Uani 1 1 d . . . C5 C 0.1977(10) 0.2976(11) 0.1941(3) 0.042(2) Uani 1 1 d . . . C6 C 0.1972(11) 0.3165(11) 0.2324(3) 0.047(2) Uani 1 1 d . . . H6 H 0.2746 0.3427 0.2497 0.057 Uiso 1 1 calc R . . C7 C 0.0570(11) 0.2888(11) 0.2408(3) 0.049(3) Uani 1 1 d . . . H7 H 0.0212 0.2896 0.2653 0.059 Uiso 1 1 calc R . . C8 C -0.0188(11) 0.2608(11) 0.2081(3) 0.045(3) Uani 1 1 d . . . H8 H -0.1150 0.2425 0.2060 0.054 Uiso 1 1 calc R . . C9 C 0.9503(11) 0.3268(11) 0.0826(3) 0.045(2) Uani 1 1 d . . . C10 C 0.8324(11) 0.2913(10) 0.1101(4) 0.047(3) Uani 1 1 d . . . C11 C 0.7215(12) 0.1440(12) 0.1128(3) 0.053(3) Uani 1 1 d . . . H11 H 0.7280 0.0738 0.0978 0.063 Uiso 1 1 calc R . . C12 C 0.5987(11) 0.0986(10) 0.1379(3) 0.048(2) Uani 1 1 d . . . C13 C 0.4917(12) -0.0632(11) 0.1407(3) 0.053(3) Uani 1 1 d . . . C14 C 0.3653(12) -0.1185(12) 0.1579(4) 0.060(3) Uani 1 1 d . . . H14 H 0.3239 -0.0680 0.1697 0.072 Uiso 1 1 calc R . . C15 C 0.3042(11) -0.2721(10) 0.1547(3) 0.049(3) Uani 1 1 d . . . H15 H 0.2134 -0.3436 0.1644 0.059 Uiso 1 1 calc R . . C16 C 0.3973(12) -0.2961(11) 0.1358(4) 0.055(3) Uani 1 1 d . . . H16 H 0.3842 -0.3893 0.1309 0.065 Uiso 1 1 calc R . . C17 C 0.6807(11) 0.2644(11) 0.2898(3) 0.044(2) Uani 1 1 d . . . C18 C 0.7508(10) 0.3749(12) 0.2584(3) 0.046(2) Uani 1 1 d . . . C19 C 0.8780(10) 0.5047(11) 0.2625(3) 0.051(3) Uani 1 1 d . . . H19 H 0.9230 0.5235 0.2867 0.061 Uiso 1 1 calc R . . C20 C 0.9468(11) 0.6107(12) 0.2351(4) 0.052(3) Uani 1 1 d . . . C21 C 1.0754(11) 0.7567(12) 0.2453(3) 0.047(3) Uani 1 1 d . . . C22 C 1.1401(11) 0.8713(12) 0.2244(3) 0.051(3) Uani 1 1 d . . . H22 H 1.1097 0.8795 0.1997 0.061 Uiso 1 1 calc R . . C23 C 1.2581(12) 0.9794(12) 0.2426(4) 0.059(3) Uani 1 1 d . . . H23 H 1.3239 1.0718 0.2325 0.070 Uiso 1 1 calc R . . C24 C 1.2632(12) 0.9315(12) 0.2765(4) 0.056(3) Uani 1 1 d . . . H24 H 1.3305 0.9852 0.2959 0.067 Uiso 1 1 calc R . . C25 C 0.6069(10) 0.6311(10) 0.3317(3) 0.042(2) Uani 1 1 d . . . H25 H 0.6726 0.5959 0.3308 0.050 Uiso 1 1 calc R . . C26 C 0.5625(11) 0.6582(12) 0.3672(3) 0.056(3) Uani 1 1 d . . . H26 H 0.5985 0.6411 0.3900 0.067 Uiso 1 1 calc R . . C27 C 0.4643(11) 0.7109(10) 0.3685(3) 0.049(3) Uani 1 1 d . . . H27 H 0.4346 0.7290 0.3923 0.059 Uiso 1 1 calc R . . C28 C 0.4104(12) 0.7364(12) 0.3344(3) 0.052(3) Uani 1 1 d . . . H28 H 0.3447 0.7716 0.3353 0.063 Uiso 1 1 calc R . . C29 C 0.4548(11) 0.7093(13) 0.2989(3) 0.051(3) Uani 1 1 d . . . H29 H 0.4188 0.7264 0.2760 0.062 Uiso 1 1 calc R . . C30 C 0.5531(12) 0.6567(12) 0.2975(4) 0.050(3) Uani 1 1 d . . . C31 C 0.6035(11) 0.6227(12) 0.2594(3) 0.044(2) Uani 1 1 d . . . H31A H 0.7037 0.6428 0.2629 0.053 Uiso 1 1 calc R . . H31B H 0.5427 0.5177 0.2546 0.053 Uiso 1 1 calc R . . C32 C 0.6006(11) 0.7022(10) 0.2232(3) 0.044(2) Uani 1 1 d . . . H32 H 0.4979 0.6692 0.2163 0.053 Uiso 1 1 calc R . . C33 C 0.6839(13) 0.8662(12) 0.2252(4) 0.058(3) Uani 1 1 d . . . H33A H 0.6167 0.9046 0.2243 0.069 Uiso 1 1 calc R . . H33B H 0.7399 0.8988 0.2491 0.069 Uiso 1 1 calc R . . C34 C 0.7594(11) 0.7885(9) 0.1762(3) 0.041(2) Uani 1 1 d . . . C35 C 0.8591(10) 0.7979(10) 0.1463(3) 0.043(2) Uani 1 1 d . . . C36 C 1.0545(12) 0.8998(12) 0.1061(3) 0.052(3) Uani 1 1 d . . . H36A H 1.1517 0.9282 0.1161 0.063 Uiso 1 1 calc R . . H36B H 1.0650 0.9521 0.0821 0.063 Uiso 1 1 calc R . . C37 C 0.9600(13) 0.7265(13) 0.0998(3) 0.055(3) Uani 1 1 d . . . H37 H 1.0201 0.6825 0.1070 0.066 Uiso 1 1 calc R . . C38 C 0.9024(11) 0.6786(11) 0.0614(3) 0.046(2) Uani 1 1 d . . . H38A H 0.8192 0.5792 0.0633 0.055 Uiso 1 1 calc R . . H38B H 0.9776 0.6734 0.0463 0.055 Uiso 1 1 calc R . . C39 C 0.8519(12) 0.7725(12) 0.0387(4) 0.048(3) Uani 1 1 d . . . C40 C 0.9510(12) 0.8744(11) 0.0124(3) 0.052(3) Uani 1 1 d . . . H40 H 1.0402 0.8784 0.0076 0.062 Uiso 1 1 calc R . . C41 C 0.9167(12) 0.9704(11) -0.0066(4) 0.054(3) Uani 1 1 d . . . H41 H 0.9830 1.0386 -0.0241 0.065 Uiso 1 1 calc R . . C42 C 0.7834(11) 0.9645(12) 0.0007(3) 0.051(3) Uani 1 1 d . . . H42 H 0.7604 1.0287 -0.0120 0.062 Uiso 1 1 calc R . . C43 C 0.6843(13) 0.8626(12) 0.0269(3) 0.051(3) Uani 1 1 d . . . H43 H 0.5950 0.8586 0.0318 0.061 Uiso 1 1 calc R . . C44 C 0.7185(11) 0.7666(12) 0.0459(3) 0.049(2) Uani 1 1 d . . . H44 H 0.6522 0.6984 0.0635 0.058 Uiso 1 1 calc R . . F1 F 0.3909(7) 0.4429(7) 0.0460(2) 0.0608(17) Uani 1 1 d . . . F2 F 0.4700(7) 0.3076(7) 0.0421(2) 0.0598(18) Uani 1 1 d . . . F3 F 0.2517(6) 0.2153(7) 0.05143(19) 0.0557(15) Uani 1 1 d . . . F4 F 0.9273(6) 0.3739(7) 0.0488(2) 0.0510(15) Uani 1 1 d . . . F5 F 0.9780(6) 0.2210(6) 0.07475(19) 0.0511(15) Uani 1 1 d . . . F6 F 1.0804(6) 0.4370(6) 0.0933(2) 0.0561(17) Uani 1 1 d . . . F7 F 0.7639(6) 0.2932(6) 0.32046(19) 0.0544(16) Uani 1 1 d . . . F8 F 0.6447(7) 0.1276(6) 0.27817(19) 0.0511(16) Uani 1 1 d . . . F9 F 0.5499(7) 0.2509(6) 0.30041(18) 0.0526(15) Uani 1 1 d . . . N1 N 0.8395(9) 0.6827(10) 0.1296(3) 0.050(2) Uani 1 1 d . . . N2 N 0.6667(9) 0.6678(8) 0.1928(3) 0.046(2) Uani 1 1 d . . . O1 O 0.5518(7) 0.4133(7) 0.1119(2) 0.0457(16) Uani 1 1 d . . . O2 O 0.4460(7) 0.3652(7) 0.1863(2) 0.0474(17) Uani 1 1 d . . . O3 O 0.0654(8) 0.2628(8) 0.1783(2) 0.0483(17) Uani 1 1 d . . . O4 O 0.8362(7) 0.3975(8) 0.1285(2) 0.0461(18) Uani 1 1 d . . . O5 O 0.5695(6) 0.1780(6) 0.15671(19) 0.0349(14) Uani 1 1 d . . . O6 O 0.5205(7) -0.1636(8) 0.1236(2) 0.0511(18) Uani 1 1 d . . . O7 O 0.6745(8) 0.3378(8) 0.2277(3) 0.056(2) Uani 1 1 d . . . O8 O 0.9054(8) 0.6001(8) 0.2021(3) 0.0501(19) Uani 1 1 d . . . O9 O 1.1489(8) 0.7832(8) 0.2793(2) 0.0547(19) Uani 1 1 d . . . O10 O 0.7797(8) 0.9158(7) 0.1928(2) 0.0526(19) Uani 1 1 d . . . O11 O 0.9710(7) 0.9298(7) 0.1339(2) 0.0499(17) Uani 1 1 d . . . Tb1 Tb 0.68225(4) 0.44008(4) 0.166841(13) 0.03699(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(5) 0.050(6) 0.045(7) 0.009(5) 0.001(5) 0.015(4) C2 0.054(6) 0.045(5) 0.036(6) -0.010(5) -0.006(5) 0.023(5) C3 0.033(5) 0.046(5) 0.033(6) -0.011(4) -0.012(4) 0.014(4) C4 0.046(5) 0.030(4) 0.040(6) 0.004(4) 0.008(5) 0.015(4) C5 0.037(5) 0.052(6) 0.029(5) -0.007(4) -0.008(4) 0.016(4) C6 0.039(5) 0.051(6) 0.042(6) 0.002(5) -0.005(5) 0.015(4) C7 0.048(6) 0.045(5) 0.045(7) -0.005(5) 0.010(5) 0.017(5) C8 0.034(5) 0.036(5) 0.052(7) 0.013(5) 0.013(5) 0.008(4) C9 0.047(6) 0.039(5) 0.041(6) -0.011(5) 0.001(5) 0.017(5) C10 0.042(5) 0.032(5) 0.058(7) 0.003(5) 0.006(5) 0.013(4) C11 0.051(6) 0.051(6) 0.045(7) 0.001(5) 0.010(5) 0.017(5) C12 0.050(6) 0.040(5) 0.049(7) -0.001(5) 0.012(5) 0.020(5) C13 0.043(6) 0.040(6) 0.039(6) -0.005(5) -0.003(5) -0.006(5) C14 0.056(7) 0.049(6) 0.080(9) -0.002(6) 0.019(6) 0.030(5) C15 0.039(5) 0.041(5) 0.050(7) 0.024(5) -0.012(5) 0.008(4) C16 0.061(7) 0.032(5) 0.054(7) -0.011(5) -0.025(6) 0.010(5) C17 0.041(5) 0.047(6) 0.037(6) 0.007(4) -0.015(4) 0.016(4) C18 0.030(5) 0.057(6) 0.046(6) 0.008(5) 0.005(4) 0.017(4) C19 0.038(5) 0.046(5) 0.044(6) -0.017(5) -0.020(5) 0.003(4) C20 0.036(5) 0.048(6) 0.076(9) -0.020(6) -0.012(6) 0.024(5) C21 0.039(5) 0.044(6) 0.037(6) -0.015(5) -0.011(5) 0.007(4) C22 0.036(5) 0.052(6) 0.046(7) -0.015(5) -0.011(5) 0.007(5) C23 0.053(6) 0.044(6) 0.068(9) -0.008(6) -0.007(6) 0.016(5) C24 0.054(6) 0.049(6) 0.056(8) -0.012(6) -0.019(6) 0.019(5) C25 0.044(5) 0.038(5) 0.036(6) -0.012(4) -0.010(5) 0.015(4) C26 0.039(5) 0.063(7) 0.047(7) -0.020(5) 0.000(5) 0.011(5) C27 0.051(6) 0.035(5) 0.042(6) 0.001(4) 0.020(5) 0.006(4) C28 0.047(6) 0.047(6) 0.046(7) -0.008(5) 0.012(5) 0.012(5) C29 0.046(6) 0.068(7) 0.038(6) -0.008(5) 0.004(5) 0.026(5) C30 0.048(6) 0.050(6) 0.050(7) 0.008(5) 0.013(5) 0.023(5) C31 0.040(5) 0.051(6) 0.035(6) -0.006(5) -0.008(5) 0.018(5) C32 0.046(5) 0.040(5) 0.031(6) -0.023(4) -0.017(4) 0.010(4) C33 0.052(6) 0.051(6) 0.049(7) -0.016(5) -0.002(5) 0.010(5) C34 0.048(5) 0.028(4) 0.042(6) 0.007(4) 0.002(4) 0.014(4) C35 0.038(5) 0.042(5) 0.037(6) -0.016(4) -0.013(4) 0.010(4) C36 0.047(6) 0.053(6) 0.049(7) 0.005(5) 0.013(5) 0.018(5) C37 0.061(7) 0.066(7) 0.043(7) 0.005(5) 0.003(5) 0.036(6) C38 0.044(5) 0.039(5) 0.043(6) 0.004(4) 0.017(5) 0.012(4) C39 0.046(6) 0.051(6) 0.053(7) 0.004(5) 0.008(5) 0.029(5) C40 0.054(6) 0.040(5) 0.052(7) 0.018(5) 0.008(5) 0.018(5) C41 0.055(6) 0.039(5) 0.052(7) 0.005(5) -0.013(5) 0.011(5) C42 0.046(6) 0.059(7) 0.035(6) -0.011(5) -0.017(5) 0.016(5) C43 0.061(6) 0.058(6) 0.037(6) -0.012(5) -0.012(5) 0.032(5) C44 0.046(5) 0.062(6) 0.044(6) 0.003(5) 0.015(5) 0.032(5) F1 0.056(4) 0.069(4) 0.051(4) 0.018(3) -0.012(3) 0.027(3) F2 0.046(3) 0.056(4) 0.059(4) -0.023(3) 0.015(3) 0.012(3) F3 0.045(3) 0.059(4) 0.049(4) -0.013(3) -0.012(3) 0.015(3) F4 0.042(3) 0.056(3) 0.052(4) 0.012(3) 0.010(3) 0.023(3) F5 0.048(3) 0.036(3) 0.055(4) 0.009(3) 0.010(3) 0.009(2) F6 0.045(3) 0.039(3) 0.068(5) -0.008(3) 0.016(3) 0.008(3) F7 0.044(3) 0.043(3) 0.060(4) 0.013(3) -0.018(3) 0.010(2) F8 0.056(4) 0.046(3) 0.042(4) 0.007(3) -0.008(3) 0.018(3) F9 0.058(4) 0.041(3) 0.048(4) 0.016(3) 0.025(3) 0.017(3) N1 0.040(4) 0.053(5) 0.042(5) -0.009(4) -0.014(4) 0.013(4) N2 0.045(5) 0.034(4) 0.044(5) 0.000(4) 0.023(4) 0.008(3) O1 0.033(3) 0.045(4) 0.047(4) -0.001(3) -0.006(3) 0.010(3) O2 0.041(4) 0.034(3) 0.056(5) 0.004(3) 0.013(3) 0.010(3) O3 0.050(4) 0.060(4) 0.042(4) -0.017(4) -0.008(3) 0.033(4) O4 0.036(4) 0.053(4) 0.043(4) -0.013(3) 0.016(3) 0.017(3) O5 0.042(3) 0.029(3) 0.036(4) -0.001(3) 0.012(3) 0.020(3) O6 0.041(4) 0.049(4) 0.051(5) -0.005(4) 0.003(3) 0.013(3) O7 0.040(4) 0.049(4) 0.060(5) -0.001(4) -0.011(4) 0.008(3) O8 0.043(4) 0.043(4) 0.056(5) 0.011(4) -0.008(4) 0.015(3) O9 0.050(4) 0.053(4) 0.050(5) -0.018(4) -0.021(4) 0.017(3) O10 0.053(4) 0.039(4) 0.056(5) -0.011(3) 0.004(4) 0.016(3) O11 0.040(3) 0.049(4) 0.055(5) 0.000(3) 0.008(3) 0.018(3) Tb1 0.0326(2) 0.0321(2) 0.0406(2) -0.0063(2) -0.0016(2) 0.0118(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F2 1.211(12) . ? C1 F1 1.291(11) . ? C1 F3 1.352(11) . ? C1 C2 1.482(15) . ? C2 O1 1.251(12) . ? C2 C3 1.380(15) . ? C3 C4 1.461(14) . ? C3 H3 0.9300 . ? C4 O2 1.256(12) . ? C4 C5 1.476(14) . ? C5 C6 1.342(15) . ? C5 O3 1.358(11) . ? C6 C7 1.378(14) . ? C6 H6 0.9300 . ? C7 C8 1.326(15) . ? C7 H7 0.9300 . ? C8 O3 1.346(12) . ? C8 H8 0.9300 . ? C9 F5 1.307(11) . ? C9 F6 1.324(11) . ? C9 F4 1.334(13) . ? C9 C10 1.453(15) . ? C10 O4 1.264(11) . ? C10 C11 1.395(13) . ? C11 C12 1.422(14) . ? C11 H11 0.9300 . ? C12 O5 1.208(11) . ? C12 C13 1.496(13) . ? C13 C14 1.293(15) . ? C13 O6 1.365(14) . ? C14 C15 1.407(15) . ? C14 H14 0.9300 . ? C15 C16 1.298(16) . ? C15 H15 0.9300 . ? C16 O6 1.407(12) . ? C16 H16 0.9300 . ? C17 F7 1.308(11) . ? C17 F8 1.349(12) . ? C17 F9 1.355(12) . ? C17 C18 1.484(14) . ? C18 O7 1.266(13) . ? C18 C19 1.354(13) . ? C19 C20 1.361(17) . ? C19 H19 0.9300 . ? C20 O8 1.204(14) . ? C20 C21 1.490(13) . ? C21 C22 1.268(16) . ? C21 O9 1.354(13) . ? C22 C23 1.344(14) . ? C22 H22 0.9300 . ? C23 C24 1.287(17) . ? C23 H23 0.9300 . ? C24 O9 1.413(12) . ? C24 H24 0.9300 . ? C25 C26 1.390(14) . ? C25 C30 1.390(16) . ? C25 H25 0.9300 . ? C26 C27 1.390(16) . ? C26 H26 0.9300 . ? C27 C28 1.390(16) . ? C27 H27 0.9300 . ? C28 C29 1.390(15) . ? C28 H28 0.9300 . ? C29 C30 1.390(15) . ? C29 H29 0.9300 . ? C30 C31 1.528(15) . ? C31 C32 1.511(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 N2 1.401(13) . ? C32 C33 1.490(14) . ? C32 H32 0.9800 . ? C33 O10 1.418(13) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N2 1.281(11) . ? C34 O10 1.366(11) . ? C34 C35 1.438(14) . ? C35 N1 1.259(13) . ? C35 O11 1.360(11) . ? C36 O11 1.434(13) . ? C36 C37 1.590(15) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.440(16) . ? C37 N1 1.510(14) . ? C37 H37 0.9800 . ? C38 C39 1.544(15) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.390(14) . ? C39 C44 1.390(13) . ? C40 C41 1.390(15) . ? C40 H40 0.9300 . ? C41 C42 1.390(15) . ? C41 H41 0.9300 . ? C42 C43 1.390(15) . ? C42 H42 0.9300 . ? C43 C44 1.390(15) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? N1 Tb1 2.578(9) . ? N2 Tb1 2.628(8) . ? O1 Tb1 2.274(7) . ? O2 Tb1 2.291(7) . ? O4 Tb1 2.296(6) . ? O5 Tb1 2.411(6) . ? O7 Tb1 2.344(8) . ? O8 Tb1 2.416(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 F2 C1 F1 104.0(9) . . ? F2 C1 F3 103.5(9) . . ? F1 C1 F3 104.5(8) . . ? F2 C1 C2 115.9(9) . . ? F1 C1 C2 111.4(9) . . ? F3 C1 C2 116.1(9) . . ? O1 C2 C3 128.2(10) . . ? O1 C2 C1 114.6(9) . . ? C3 C2 C1 117.2(9) . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? O2 C4 C3 124.8(9) . . ? O2 C4 C5 118.0(9) . . ? C3 C4 C5 116.9(9) . . ? C6 C5 O3 110.8(9) . . ? C6 C5 C4 127.1(9) . . ? O3 C5 C4 122.0(9) . . ? C5 C6 C7 104.9(9) . . ? C5 C6 H6 127.5 . . ? C7 C6 H6 127.5 . . ? C8 C7 C6 109.0(10) . . ? C8 C7 H7 125.5 . . ? C6 C7 H7 125.5 . . ? C7 C8 O3 109.4(9) . . ? C7 C8 H8 125.3 . . ? O3 C8 H8 125.3 . . ? F5 C9 F6 103.3(8) . . ? F5 C9 F4 106.9(8) . . ? F6 C9 F4 102.7(8) . . ? F5 C9 C10 116.1(9) . . ? F6 C9 C10 114.3(9) . . ? F4 C9 C10 112.2(9) . . ? O4 C10 C11 125.6(10) . . ? O4 C10 C9 117.1(8) . . ? C11 C10 C9 117.3(9) . . ? C10 C11 C12 121.6(10) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? O5 C12 C11 126.5(9) . . ? O5 C12 C13 116.2(9) . . ? C11 C12 C13 117.3(10) . . ? C14 C13 O6 115.1(9) . . ? C14 C13 C12 123.9(11) . . ? O6 C13 C12 121.0(10) . . ? C13 C14 C15 104.8(10) . . ? C13 C14 H14 127.6 . . ? C15 C14 H14 127.6 . . ? C16 C15 C14 107.8(9) . . ? C16 C15 H15 126.1 . . ? C14 C15 H15 126.1 . . ? C15 C16 O6 111.5(9) . . ? C15 C16 H16 124.3 . . ? O6 C16 H16 124.3 . . ? F7 C17 F8 106.6(8) . . ? F7 C17 F9 109.1(9) . . ? F8 C17 F9 103.8(7) . . ? F7 C17 C18 113.5(8) . . ? F8 C17 C18 112.2(9) . . ? F9 C17 C18 111.1(8) . . ? O7 C18 C19 123.4(10) . . ? O7 C18 C17 112.4(9) . . ? C19 C18 C17 124.1(10) . . ? C18 C19 C20 126.8(11) . . ? C18 C19 H19 116.6 . . ? C20 C19 H19 116.6 . . ? O8 C20 C19 124.4(9) . . ? O8 C20 C21 114.8(11) . . ? C19 C20 C21 120.6(11) . . ? C22 C21 O9 108.7(9) . . ? C22 C21 C20 128.1(11) . . ? O9 C21 C20 123.1(10) . . ? C21 C22 C23 111.2(11) . . ? C21 C22 H22 124.4 . . ? C23 C22 H22 124.4 . . ? C24 C23 C22 107.3(11) . . ? C24 C23 H23 126.4 . . ? C22 C23 H23 126.4 . . ? C23 C24 O9 108.2(10) . . ? C23 C24 H24 125.9 . . ? O9 C24 H24 125.9 . . ? C26 C25 C30 120.0(10) . . ? C26 C25 H25 120.0 . . ? C30 C25 H25 120.0 . . ? C25 C26 C27 120.0(11) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0(10) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0(11) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0(12) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 120.0(11) . . ? C29 C30 C31 122.1(11) . . ? C25 C30 C31 117.9(9) . . ? C32 C31 C30 118.8(9) . . ? C32 C31 H31A 107.6 . . ? C30 C31 H31A 107.6 . . ? C32 C31 H31B 107.6 . . ? C30 C31 H31B 107.6 . . ? H31A C31 H31B 107.0 . . ? N2 C32 C33 104.7(9) . . ? N2 C32 C31 109.3(9) . . ? C33 C32 C31 115.8(9) . . ? N2 C32 H32 109.0 . . ? C33 C32 H32 109.0 . . ? C31 C32 H32 109.0 . . ? O10 C33 C32 106.5(9) . . ? O10 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? O10 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? N2 C34 O10 116.6(9) . . ? N2 C34 C35 123.7(9) . . ? O10 C34 C35 118.8(8) . . ? N1 C35 O11 118.3(9) . . ? N1 C35 C34 120.0(9) . . ? O11 C35 C34 121.6(8) . . ? O11 C36 C37 104.0(8) . . ? O11 C36 H36A 111.0 . . ? C37 C36 H36A 111.0 . . ? O11 C36 H36B 111.0 . . ? C37 C36 H36B 111.0 . . ? H36A C36 H36B 109.0 . . ? C38 C37 N1 112.3(9) . . ? C38 C37 C36 115.9(10) . . ? N1 C37 C36 101.7(9) . . ? C38 C37 H37 108.9 . . ? N1 C37 H37 108.9 . . ? C36 C37 H37 108.9 . . ? C37 C38 C39 117.7(9) . . ? C37 C38 H38A 107.9 . . ? C39 C38 H38A 107.9 . . ? C37 C38 H38B 107.9 . . ? C39 C38 H38B 107.9 . . ? H38A C38 H38B 107.2 . . ? C40 C39 C44 120.0(10) . . ? C40 C39 C38 117.3(9) . . ? C44 C39 C38 122.5(10) . . ? C41 C40 C39 120.0(11) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.0(11) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.0(11) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.0(10) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 120.0(10) . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? C35 N1 C37 108.1(9) . . ? C35 N1 Tb1 115.7(7) . . ? C37 N1 Tb1 131.6(7) . . ? C34 N2 C32 107.9(8) . . ? C34 N2 Tb1 112.6(6) . . ? C32 N2 Tb1 138.8(6) . . ? C2 O1 Tb1 134.8(7) . . ? C4 O2 Tb1 136.3(7) . . ? C8 O3 C5 105.8(8) . . ? C10 O4 Tb1 138.1(6) . . ? C12 O5 Tb1 135.5(6) . . ? C13 O6 C16 100.6(8) . . ? C18 O7 Tb1 137.6(7) . . ? C20 O8 Tb1 136.0(7) . . ? C21 O9 C24 104.4(9) . . ? C34 O10 C33 103.8(7) . . ? C35 O11 C36 107.4(8) . . ? O1 Tb1 O2 73.9(3) . . ? O1 Tb1 O4 86.1(3) . . ? O2 Tb1 O4 147.7(2) . . ? O1 Tb1 O7 144.3(2) . . ? O2 Tb1 O7 78.2(3) . . ? O4 Tb1 O7 107.2(3) . . ? O1 Tb1 O5 79.4(2) . . ? O2 Tb1 O5 79.8(2) . . ? O4 Tb1 O5 71.7(2) . . ? O7 Tb1 O5 74.0(2) . . ? O1 Tb1 O8 145.1(2) . . ? O2 Tb1 O8 126.5(3) . . ? O4 Tb1 O8 84.0(3) . . ? O7 Tb1 O8 70.4(2) . . ? O5 Tb1 O8 128.0(2) . . ? O1 Tb1 N1 75.7(2) . . ? O2 Tb1 N1 122.1(3) . . ? O4 Tb1 N1 74.9(3) . . ? O7 Tb1 N1 139.3(2) . . ? O5 Tb1 N1 139.3(3) . . ? O8 Tb1 N1 69.4(2) . . ? O1 Tb1 N2 95.2(3) . . ? O2 Tb1 N2 70.4(2) . . ? O4 Tb1 N2 137.8(3) . . ? O7 Tb1 N2 96.0(3) . . ? O5 Tb1 N2 150.0(2) . . ? O8 Tb1 N2 71.1(3) . . ? N1 Tb1 N2 64.8(3) . . ? 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 F2 C1 C2 O1 33.2(13) . . . . ? F1 C1 C2 O1 -85.4(11) . . . . ? F3 C1 C2 O1 155.1(9) . . . . ? F2 C1 C2 C3 -147.8(10) . . . . ? F1 C1 C2 C3 93.5(11) . . . . ? F3 C1 C2 C3 -26.0(14) . . . . ? O1 C2 C3 C4 -0.8(17) . . . . ? C1 C2 C3 C4 -179.6(9) . . . . ? C2 C3 C4 O2 -7.0(15) . . . . ? C2 C3 C4 C5 165.4(9) . . . . ? O2 C4 C5 C6 -3.3(16) . . . . ? C3 C4 C5 C6 -176.3(10) . . . . ? O2 C4 C5 O3 172.8(8) . . . . ? C3 C4 C5 O3 -0.1(14) . . . . ? O3 C5 C6 C7 1.4(12) . . . . ? C4 C5 C6 C7 177.9(10) . . . . ? C5 C6 C7 C8 -2.5(12) . . . . ? C6 C7 C8 O3 2.6(12) . . . . ? F5 C9 C10 O4 155.4(10) . . . . ? F6 C9 C10 O4 35.3(15) . . . . ? F4 C9 C10 O4 -81.2(12) . . . . ? F5 C9 C10 C11 -27.1(15) . . . . ? F6 C9 C10 C11 -147.2(10) . . . . ? F4 C9 C10 C11 96.3(12) . . . . ? O4 C10 C11 C12 -0.7(19) . . . . ? C9 C10 C11 C12 -177.9(11) . . . . ? C10 C11 C12 O5 6(2) . . . . ? C10 C11 C12 C13 -175.7(11) . . . . ? O5 C12 C13 C14 8.5(19) . . . . ? C11 C12 C13 C14 -169.7(12) . . . . ? O5 C12 C13 O6 -173.9(10) . . . . ? C11 C12 C13 O6 7.9(17) . . . . ? O6 C13 C14 C15 4.1(15) . . . . ? C12 C13 C14 C15 -178.2(11) . . . . ? C13 C14 C15 C16 -0.5(14) . . . . ? C14 C15 C16 O6 -3.0(13) . . . . ? F7 C17 C18 O7 173.8(9) . . . . ? F8 C17 C18 O7 52.9(12) . . . . ? F9 C17 C18 O7 -62.9(12) . . . . ? F7 C17 C18 C19 -9.7(16) . . . . ? F8 C17 C18 C19 -130.6(11) . . . . ? F9 C17 C18 C19 113.6(11) . . . . ? O7 C18 C19 C20 -3.3(19) . . . . ? C17 C18 C19 C20 -179.4(11) . . . . ? C18 C19 C20 O8 -3.1(19) . . . . ? C18 C19 C20 C21 171.7(11) . . . . ? O8 C20 C21 C22 4.1(18) . . . . ? C19 C20 C21 C22 -171.2(12) . . . . ? O8 C20 C21 O9 -171.2(10) . . . . ? C19 C20 C21 O9 13.6(17) . . . . ? O9 C21 C22 C23 -0.1(14) . . . . ? C20 C21 C22 C23 -175.9(11) . . . . ? C21 C22 C23 C24 -2.4(15) . . . . ? C22 C23 C24 O9 3.8(14) . . . . ? C30 C25 C26 C27 0.0(15) . . . . ? C25 C26 C27 C28 0.0(15) . . . . ? C26 C27 C28 C29 0.0(15) . . . . ? C27 C28 C29 C30 0.0(16) . . . . ? C28 C29 C30 C25 0.0(17) . . . . ? C28 C29 C30 C31 179.0(10) . . . . ? C26 C25 C30 C29 0.0(16) . . . . ? C26 C25 C30 C31 -179.0(9) . . . . ? C29 C30 C31 C32 25.5(16) . . . . ? C25 C30 C31 C32 -155.5(9) . . . . ? C30 C31 C32 N2 173.2(9) . . . . ? C30 C31 C32 C33 55.4(13) . . . . ? N2 C32 C33 O10 7.3(12) . . . . ? C31 C32 C33 O10 127.6(10) . . . . ? N2 C34 C35 N1 14.2(16) . . . . ? O10 C34 C35 N1 -177.4(9) . . . . ? N2 C34 C35 O11 -169.3(10) . . . . ? O10 C34 C35 O11 -0.9(15) . . . . ? O11 C36 C37 C38 116.6(11) . . . . ? O11 C36 C37 N1 -5.5(11) . . . . ? N1 C37 C38 C39 80.3(12) . . . . ? C36 C37 C38 C39 -36.0(13) . . . . ? C37 C38 C39 C40 97.2(13) . . . . ? C37 C38 C39 C44 -77.4(14) . . . . ? C44 C39 C40 C41 0.0(18) . . . . ? C38 C39 C40 C41 -174.7(11) . . . . ? C39 C40 C41 C42 0.0(18) . . . . ? C40 C41 C42 C43 0.0(16) . . . . ? C41 C42 C43 C44 0.0(15) . . . . ? C42 C43 C44 C39 0.0(16) . . . . ? C40 C39 C44 C43 0.0(18) . . . . ? C38 C39 C44 C43 174.4(10) . . . . ? O11 C35 N1 C37 3.4(13) . . . . ? C34 C35 N1 C37 -180.0(9) . . . . ? O11 C35 N1 Tb1 162.2(7) . . . . ? C34 C35 N1 Tb1 -21.2(12) . . . . ? C38 C37 N1 C35 -122.9(10) . . . . ? C36 C37 N1 C35 1.6(11) . . . . ? C38 C37 N1 Tb1 82.9(11) . . . . ? C36 C37 N1 Tb1 -152.5(7) . . . . ? O10 C34 N2 C32 4.7(13) . . . . ? C35 C34 N2 C32 173.4(9) . . . . ? O10 C34 N2 Tb1 -167.6(7) . . . . ? C35 C34 N2 Tb1 1.1(13) . . . . ? C33 C32 N2 C34 -7.1(12) . . . . ? C31 C32 N2 C34 -131.7(9) . . . . ? C33 C32 N2 Tb1 162.0(9) . . . . ? C31 C32 N2 Tb1 37.5(13) . . . . ? C3 C2 O1 Tb1 17.1(17) . . . . ? C1 C2 O1 Tb1 -164.1(7) . . . . ? C3 C4 O2 Tb1 -1.0(15) . . . . ? C5 C4 O2 Tb1 -173.3(6) . . . . ? C7 C8 O3 C5 -1.7(11) . . . . ? C6 C5 O3 C8 0.1(12) . . . . ? C4 C5 O3 C8 -176.6(9) . . . . ? C11 C10 O4 Tb1 -10.3(19) . . . . ? C9 C10 O4 Tb1 166.9(8) . . . . ? C11 C12 O5 Tb1 -1.7(19) . . . . ? C13 C12 O5 Tb1 -179.8(7) . . . . ? C14 C13 O6 C16 -5.6(13) . . . . ? C12 C13 O6 C16 176.6(10) . . . . ? C15 C16 O6 C13 5.1(12) . . . . ? C19 C18 O7 Tb1 -1.6(18) . . . . ? C17 C18 O7 Tb1 174.9(7) . . . . ? C19 C20 O8 Tb1 14.3(18) . . . . ? C21 C20 O8 Tb1 -160.7(7) . . . . ? C22 C21 O9 C24 2.3(13) . . . . ? C20 C21 O9 C24 178.4(10) . . . . ? C23 C24 O9 C21 -3.8(13) . . . . ? N2 C34 O10 C33 0.2(12) . . . . ? C35 C34 O10 C33 -169.1(9) . . . . ? C32 C33 O10 C34 -4.7(11) . . . . ? N1 C35 O11 C36 -7.4(13) . . . . ? C34 C35 O11 C36 176.0(10) . . . . ? C37 C36 O11 C35 7.4(11) . . . . ? C2 O1 Tb1 O2 -17.1(9) . . . . ? C2 O1 Tb1 O4 137.4(9) . . . . ? C2 O1 Tb1 O7 23.0(11) . . . . ? C2 O1 Tb1 O5 65.2(9) . . . . ? C2 O1 Tb1 O8 -149.0(9) . . . . ? C2 O1 Tb1 N1 -147.2(9) . . . . ? C2 O1 Tb1 N2 -84.9(9) . . . . ? C4 O2 Tb1 O1 9.2(8) . . . . ? C4 O2 Tb1 O4 -44.6(11) . . . . ? C4 O2 Tb1 O7 -148.3(9) . . . . ? C4 O2 Tb1 O5 -72.7(9) . . . . ? C4 O2 Tb1 O8 157.1(8) . . . . ? C4 O2 Tb1 N1 70.1(9) . . . . ? C4 O2 Tb1 N2 110.9(9) . . . . ? C10 O4 Tb1 O1 -69.7(11) . . . . ? C10 O4 Tb1 O2 -18.7(14) . . . . ? C10 O4 Tb1 O7 76.5(11) . . . . ? C10 O4 Tb1 O5 10.4(11) . . . . ? C10 O4 Tb1 O8 143.9(11) . . . . ? C10 O4 Tb1 N1 -145.9(11) . . . . ? C10 O4 Tb1 N2 -163.1(10) . . . . ? C18 O7 Tb1 O1 -168.6(9) . . . . ? C18 O7 Tb1 O2 -129.5(11) . . . . ? C18 O7 Tb1 O4 83.4(11) . . . . ? C18 O7 Tb1 O5 147.9(11) . . . . ? C18 O7 Tb1 O8 6.5(10) . . . . ? C18 O7 Tb1 N1 -3.3(13) . . . . ? C18 O7 Tb1 N2 -61.0(11) . . . . ? C12 O5 Tb1 O1 85.1(10) . . . . ? C12 O5 Tb1 O2 160.4(10) . . . . ? C12 O5 Tb1 O4 -4.2(10) . . . . ? C12 O5 Tb1 O7 -119.0(10) . . . . ? C12 O5 Tb1 O8 -70.8(11) . . . . ? C12 O5 Tb1 N1 32.2(11) . . . . ? C12 O5 Tb1 N2 167.1(10) . . . . ? C20 O8 Tb1 O1 162.0(9) . . . . ? C20 O8 Tb1 O2 44.8(11) . . . . ? C20 O8 Tb1 O4 -123.7(11) . . . . ? C20 O8 Tb1 O7 -13.0(10) . . . . ? C20 O8 Tb1 O5 -62.5(12) . . . . ? C20 O8 Tb1 N1 160.2(11) . . . . ? C20 O8 Tb1 N2 90.8(11) . . . . ? C35 N1 Tb1 O1 117.9(8) . . . . ? C37 N1 Tb1 O1 -89.5(9) . . . . ? C35 N1 Tb1 O2 57.8(8) . . . . ? C37 N1 Tb1 O2 -149.6(8) . . . . ? C35 N1 Tb1 O4 -152.3(8) . . . . ? C37 N1 Tb1 O4 0.3(8) . . . . ? C35 N1 Tb1 O7 -53.3(9) . . . . ? C37 N1 Tb1 O7 99.3(9) . . . . ? C35 N1 Tb1 O5 171.9(6) . . . . ? C37 N1 Tb1 O5 -35.5(10) . . . . ? C35 N1 Tb1 O8 -63.1(7) . . . . ? C37 N1 Tb1 O8 89.5(8) . . . . ? C35 N1 Tb1 N2 15.0(7) . . . . ? C37 N1 Tb1 N2 167.6(9) . . . . ? C34 N2 Tb1 O1 -79.1(8) . . . . ? C32 N2 Tb1 O1 112.0(10) . . . . ? C34 N2 Tb1 O2 -150.0(8) . . . . ? C32 N2 Tb1 O2 41.2(10) . . . . ? C34 N2 Tb1 O4 10.8(10) . . . . ? C32 N2 Tb1 O4 -158.1(9) . . . . ? C34 N2 Tb1 O7 134.8(7) . . . . ? C32 N2 Tb1 O7 -34.0(11) . . . . ? C34 N2 Tb1 O5 -156.9(6) . . . . ? C32 N2 Tb1 O5 34.2(14) . . . . ? C34 N2 Tb1 O8 67.9(7) . . . . ? C32 N2 Tb1 O8 -101.0(11) . . . . ? C34 N2 Tb1 N1 -7.6(7) . . . . ? C32 N2 Tb1 N1 -176.5(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.092 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.105