# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'licun. Li' _publ_contact_author_address ;School of Nankai University Tianjin China ; _publ_contact_author_email llicun@nankai.edu.cn loop_ _publ_author_name _publ_author_address 'Xuelan Mei.' ;School of Nankai University Tianjin China ; 'Ruina Liu.' ;School of Nankai University Tianjin China ; 'Chao Wang.' ;School of Nankai University Tianjin China ; 'Peipei Yang.' ;School of Nankai University Tianjin China ; 'Daizheng Liao.' ;School of Nankai University Tianjin China ; data_1 _database_code_depnum_ccdc_archive 'CCDC 843544' #TrackingRef 'CIF file for compounds 1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 F18 Gd2 N6 O16' _chemical_formula_weight 2073.94 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' 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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.613(3) _cell_length_b 12.202(3) _cell_length_c 16.414(4) _cell_angle_alpha 105.214(4) _cell_angle_beta 101.262(3) _cell_angle_gamma 104.368(2) _cell_volume 2088.1(9) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6825 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.1 _exptl_crystal_description sheet _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 1.649 _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 1.684 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7293 _exptl_absorpt_correction_T_max 0.7293 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15425 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7288 _reflns_number_gt 6185 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7288 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.27702(2) 0.28021(2) 0.262928(18) 0.01844(8) Uani 1 1 d . . . F1 F 0.3451(3) -0.0062(3) 0.4790(2) 0.0486(10) Uani 1 1 d . . . F2 F 0.3183(6) 0.1545(4) 0.5410(3) 0.115(2) Uani 1 1 d . . . F3 F 0.4741(4) 0.1576(4) 0.4920(4) 0.115(3) Uani 1 1 d . . . F4 F 0.4880(6) 0.5008(4) 0.1118(4) 0.119(2) Uani 1 1 d . . . F5 F 0.4633(4) 0.3575(4) 0.0024(3) 0.0947(19) Uani 1 1 d . . . F6 F 0.6293(3) 0.4293(4) 0.0982(4) 0.0987(19) Uani 1 1 d . . . F7 F 0.3889(3) 0.6988(3) 0.2569(3) 0.0505(10) Uani 1 1 d . . . F8 F 0.2131(3) 0.7250(3) 0.2466(3) 0.0592(12) Uani 1 1 d . . . F9 F 0.3125(3) 0.7097(3) 0.3647(2) 0.0516(10) Uani 1 1 d . . . O1 O 0.3069(3) 0.2137(3) 0.3844(2) 0.0223(8) Uani 1 1 d . . . O2 O 0.1377(3) 0.0846(3) 0.2196(2) 0.0222(8) Uani 1 1 d . . . O3 O 0.3629(3) 0.3224(3) 0.1522(2) 0.0247(8) Uani 1 1 d . . . O4 O 0.4047(3) 0.1589(3) 0.2321(2) 0.0227(8) Uani 1 1 d . . . O5 O 0.2939(3) 0.4813(3) 0.2810(2) 0.0216(8) Uani 1 1 d . . . O6 O 0.1055(3) 0.2785(3) 0.1598(2) 0.0220(8) Uani 1 1 d . . . O7 O 0.1448(3) 0.3493(3) 0.3486(2) 0.0206(8) Uani 1 1 d . . . O8 O 0.0599(3) 0.3186(4) 0.6067(3) 0.0353(10) Uani 1 1 d . . . N1 N 0.0892(3) 0.3200(4) 0.4035(3) 0.0203(10) Uani 1 1 d . . . N2 N 0.0478(3) 0.3043(4) 0.5253(3) 0.0225(10) Uani 1 1 d . . . N3 N 0.4974(3) 0.4196(4) 0.3623(3) 0.0218(10) Uani 1 1 d . . . C14 C 0.4871(4) 0.1564(4) 0.1929(3) 0.0224(12) Uani 1 1 d . . . C13 C 0.5242(5) 0.2381(5) 0.1477(4) 0.0294(13) Uani 1 1 d . . . H13 H 0.5943 0.2400 0.1280 0.035 Uiso 1 1 calc R . . C12 C 0.4603(4) 0.3133(5) 0.1327(3) 0.0232(12) Uani 1 1 d . . . C15 C 0.5472(4) 0.0603(4) 0.1930(4) 0.0212(12) Uani 1 1 d . . . C16 C 0.5481(4) 0.0113(4) 0.2602(4) 0.0246(12) Uani 1 1 d . . . H16 H 0.5134 0.0392 0.3048 0.029 Uiso 1 1 calc R . . C17 C 0.6001(4) -0.0788(5) 0.2614(4) 0.0319(14) Uani 1 1 d . . . H17 H 0.6020 -0.1103 0.3073 0.038 Uiso 1 1 calc R . . C18 C 0.6492(5) -0.1217(5) 0.1945(4) 0.0359(15) Uani 1 1 d . . . H18 H 0.6834 -0.1829 0.1954 0.043 Uiso 1 1 calc R . . C19 C 0.6484(4) -0.0749(5) 0.1255(4) 0.0315(14) Uani 1 1 d . . . H19 H 0.6811 -0.1043 0.0801 0.038 Uiso 1 1 calc R . . C20 C 0.5975(4) 0.0166(5) 0.1263(4) 0.0280(13) Uani 1 1 d . . . H20 H 0.5971 0.0495 0.0812 0.034 Uiso 1 1 calc R . . C11 C 0.5117(5) 0.3996(5) 0.0861(4) 0.0300(14) Uani 1 1 d . . . C4 C 0.1220(4) -0.0026(4) 0.2485(3) 0.0201(11) Uani 1 1 d . . . C3 C 0.1992(4) 0.0044(4) 0.3308(3) 0.0229(12) Uani 1 1 d . . . H3 H 0.1917 -0.0656 0.3450 0.028 Uiso 1 1 calc R . . C2 C 0.2826(4) 0.1081(4) 0.3889(3) 0.0212(12) Uani 1 1 d . . . C5 C 0.0190(4) -0.1150(4) 0.1957(3) 0.0199(11) Uani 1 1 d . . . C6 C -0.0243(4) -0.2045(4) 0.2305(4) 0.0265(13) Uani 1 1 d . . . H6 H 0.0106 -0.1947 0.2890 0.032 Uiso 1 1 calc R . . C7 C -0.1189(4) -0.3078(5) 0.1784(4) 0.0316(14) Uani 1 1 d . . . H7 H -0.1467 -0.3679 0.2016 0.038 Uiso 1 1 calc R . . C8 C -0.1724(5) -0.3219(5) 0.0917(4) 0.0319(14) Uani 1 1 d . . . H8 H -0.2356 -0.3919 0.0567 0.038 Uiso 1 1 calc R . . C9 C -0.1327(4) -0.2330(5) 0.0568(4) 0.0266(12) Uani 1 1 d . . . H9 H -0.1687 -0.2426 -0.0015 0.032 Uiso 1 1 calc R . . C10 C -0.0376(4) -0.1283(4) 0.1100(4) 0.0246(12) Uani 1 1 d . . . H10 H -0.0121 -0.0669 0.0874 0.029 Uiso 1 1 calc R . . C1 C 0.3554(5) 0.1024(5) 0.4744(4) 0.0394(16) Uani 1 1 d . . . C24 C 0.0580(4) 0.3547(5) 0.1401(3) 0.0228(12) Uani 1 1 d . . . C23 C 0.1143(4) 0.4795(4) 0.1800(4) 0.0254(13) Uani 1 1 d . . . H23 H 0.0736 0.5297 0.1624 0.031 Uiso 1 1 calc R . . C22 C 0.2260(4) 0.5308(4) 0.2434(3) 0.0211(12) Uani 1 1 d . . . C25 C -0.0631(4) 0.3053(5) 0.0697(3) 0.0240(12) Uani 1 1 d . . . C26 C -0.1244(4) 0.1818(5) 0.0414(4) 0.0272(13) Uani 1 1 d . . . H26 H -0.0916 0.1331 0.0675 0.033 Uiso 1 1 calc R . . C27 C -0.2340(5) 0.1325(5) -0.0256(4) 0.0338(14) Uani 1 1 d . . . H27 H -0.2749 0.0506 -0.0441 0.041 Uiso 1 1 calc R . . C28 C -0.2831(5) 0.2041(5) -0.0653(4) 0.0383(16) Uani 1 1 d . . . H28 H -0.3557 0.1705 -0.1112 0.046 Uiso 1 1 calc R . . C29 C -0.2230(5) 0.3268(5) -0.0358(4) 0.0404(16) Uani 1 1 d . . . H29 H -0.2568 0.3757 -0.0611 0.048 Uiso 1 1 calc R . . C30 C -0.1144(4) 0.3759(5) 0.0300(4) 0.0335(15) Uani 1 1 d . . . H30 H -0.0744 0.4580 0.0484 0.040 Uiso 1 1 calc R . . C21 C 0.2832(5) 0.6665(5) 0.2779(4) 0.0283(13) Uani 1 1 d . . . C31 C -0.0504(4) 0.2648(4) 0.3763(3) 0.0211(12) Uani 1 1 d . . . C34 C -0.0936(4) 0.1673(5) 0.2875(4) 0.0319(14) Uani 1 1 d . . . H34A H -0.1815 0.1299 0.2727 0.048 Uiso 1 1 calc R . . H34B H -0.0525 0.1086 0.2899 0.048 Uiso 1 1 calc R . . H34C H -0.0743 0.2018 0.2436 0.048 Uiso 1 1 calc R . . C33 C -0.1004(4) 0.3681(5) 0.3702(4) 0.0294(13) Uani 1 1 d . . . H33A H -0.1892 0.3391 0.3520 0.044 Uiso 1 1 calc R . . H33B H -0.0709 0.4009 0.3282 0.044 Uiso 1 1 calc R . . H33C H -0.0724 0.4293 0.4268 0.044 Uiso 1 1 calc R . . C32 C -0.0682(4) 0.2219(5) 0.4553(4) 0.0254(13) Uani 1 1 d . . . C35 C -0.0627(5) 0.0950(4) 0.4433(4) 0.0347(15) Uani 1 1 d . . . H35A H -0.1354 0.0386 0.3992 0.052 Uiso 1 1 calc R . . H35B H -0.0588 0.0793 0.4979 0.052 Uiso 1 1 calc R . . H35C H 0.0095 0.0875 0.4252 0.052 Uiso 1 1 calc R . . C36 C -0.1797(4) 0.2375(5) 0.4856(4) 0.0353(15) Uani 1 1 d . . . H36A H -0.1751 0.3203 0.5008 0.053 Uiso 1 1 calc R . . H36B H -0.1810 0.2121 0.5361 0.053 Uiso 1 1 calc R . . H36C H -0.2538 0.1901 0.4391 0.053 Uiso 1 1 calc R . . C37 C 0.1367(4) 0.3507(4) 0.4901(3) 0.0181(11) Uani 1 1 d . . . C38 C 0.2633(4) 0.4276(4) 0.5395(3) 0.0199(11) Uani 1 1 d . . . C39 C 0.3218(4) 0.4169(4) 0.6184(3) 0.0227(12) Uani 1 1 d . . . H39 H 0.2818 0.3600 0.6404 0.027 Uiso 1 1 calc R . . C41 C 0.5590(4) 0.5067(4) 0.3363(4) 0.0236(12) Uani 1 1 d . . . H41 H 0.5195 0.5166 0.2850 0.028 Uiso 1 1 calc R . . C42 C 0.5562(4) 0.4088(4) 0.4371(3) 0.0223(12) Uani 1 1 d . . . H42 H 0.5162 0.3477 0.4555 0.027 Uiso 1 1 calc R . . C40 C 0.3264(4) 0.5164(4) 0.5111(4) 0.0205(11) Uani 1 1 d . . . H40 H 0.2908 0.5256 0.4584 0.025 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 Gd1 0.01656(13) 0.01690(14) 0.01890(16) 0.00490(11) 0.00376(10) 0.00216(10) F1 0.054(2) 0.0259(19) 0.052(3) 0.0205(19) -0.0125(18) 0.0009(15) F2 0.255(7) 0.091(4) 0.025(3) 0.020(3) 0.018(3) 0.115(4) F3 0.057(3) 0.097(4) 0.145(5) 0.095(4) -0.062(3) -0.045(3) F4 0.226(6) 0.063(3) 0.168(6) 0.082(4) 0.166(5) 0.085(4) F5 0.119(4) 0.085(4) 0.036(3) 0.038(3) -0.007(3) -0.041(3) F6 0.038(2) 0.131(4) 0.157(5) 0.118(4) 0.028(3) 0.003(2) F7 0.041(2) 0.030(2) 0.079(3) 0.021(2) 0.0227(19) 0.0003(16) F8 0.051(2) 0.0223(18) 0.081(3) 0.005(2) -0.019(2) 0.0148(16) F9 0.071(2) 0.028(2) 0.037(2) -0.0054(18) 0.0071(19) 0.0050(17) O1 0.0241(18) 0.0180(19) 0.021(2) 0.0079(17) 0.0033(16) 0.0016(15) O2 0.0187(17) 0.0171(19) 0.025(2) 0.0034(17) 0.0036(15) 0.0015(14) O3 0.0240(18) 0.026(2) 0.023(2) 0.0091(18) 0.0061(16) 0.0060(16) O4 0.0210(18) 0.0194(19) 0.028(2) 0.0050(17) 0.0105(16) 0.0072(15) O5 0.0197(17) 0.0197(19) 0.026(2) 0.0112(17) 0.0039(16) 0.0054(15) O6 0.0192(17) 0.0205(19) 0.023(2) 0.0085(17) 0.0001(15) 0.0042(15) O7 0.0175(17) 0.028(2) 0.015(2) 0.0056(17) 0.0080(15) 0.0032(15) O8 0.030(2) 0.051(3) 0.022(2) 0.016(2) 0.0090(18) 0.0025(18) N1 0.012(2) 0.020(2) 0.023(3) 0.003(2) 0.0006(19) 0.0023(17) N2 0.019(2) 0.027(2) 0.021(3) 0.009(2) 0.0064(19) 0.0028(18) N3 0.019(2) 0.023(2) 0.023(3) 0.006(2) 0.0069(19) 0.0057(18) C14 0.019(3) 0.024(3) 0.018(3) 0.000(2) 0.004(2) 0.003(2) C13 0.024(3) 0.030(3) 0.036(4) 0.012(3) 0.015(3) 0.005(2) C12 0.024(3) 0.026(3) 0.017(3) 0.006(3) 0.010(2) 0.002(2) C15 0.016(2) 0.020(3) 0.024(3) 0.002(2) 0.005(2) 0.004(2) C16 0.016(2) 0.024(3) 0.027(3) 0.004(3) 0.002(2) 0.002(2) C17 0.024(3) 0.028(3) 0.038(4) 0.012(3) 0.002(3) 0.003(2) C18 0.027(3) 0.024(3) 0.046(4) 0.002(3) 0.000(3) 0.009(2) C19 0.024(3) 0.035(3) 0.027(4) -0.003(3) 0.005(3) 0.010(2) C20 0.022(3) 0.028(3) 0.031(4) 0.008(3) 0.005(2) 0.007(2) C11 0.023(3) 0.028(3) 0.037(4) 0.012(3) 0.009(3) 0.002(2) C4 0.023(3) 0.015(3) 0.025(3) 0.007(2) 0.012(2) 0.007(2) C3 0.022(3) 0.017(3) 0.029(3) 0.010(3) 0.004(2) 0.005(2) C2 0.018(2) 0.025(3) 0.020(3) 0.009(2) 0.004(2) 0.006(2) C5 0.019(2) 0.015(3) 0.025(3) 0.004(2) 0.008(2) 0.004(2) C6 0.024(3) 0.022(3) 0.031(4) 0.010(3) 0.003(2) 0.003(2) C7 0.027(3) 0.021(3) 0.043(4) 0.009(3) 0.013(3) -0.001(2) C8 0.027(3) 0.021(3) 0.036(4) -0.002(3) 0.007(3) 0.003(2) C9 0.027(3) 0.028(3) 0.022(3) 0.006(3) 0.010(2) 0.006(2) C10 0.023(3) 0.021(3) 0.028(3) 0.007(3) 0.010(2) 0.004(2) C1 0.048(4) 0.019(3) 0.031(4) 0.006(3) -0.011(3) -0.004(3) C24 0.020(3) 0.028(3) 0.017(3) 0.007(3) 0.006(2) 0.004(2) C23 0.024(3) 0.022(3) 0.029(3) 0.010(3) 0.002(2) 0.009(2) C22 0.021(3) 0.018(3) 0.021(3) 0.002(2) 0.007(2) 0.005(2) C25 0.018(3) 0.026(3) 0.020(3) 0.003(3) 0.000(2) 0.004(2) C26 0.023(3) 0.030(3) 0.022(3) 0.008(3) -0.001(2) 0.002(2) C27 0.027(3) 0.027(3) 0.035(4) 0.006(3) 0.005(3) -0.004(2) C28 0.026(3) 0.041(4) 0.033(4) 0.011(3) -0.005(3) -0.003(3) C29 0.036(3) 0.039(4) 0.039(4) 0.014(3) -0.006(3) 0.009(3) C30 0.024(3) 0.032(3) 0.039(4) 0.013(3) -0.003(3) 0.005(2) C21 0.024(3) 0.025(3) 0.028(4) 0.005(3) -0.003(3) 0.007(2) C31 0.013(2) 0.024(3) 0.023(3) 0.005(2) 0.004(2) 0.004(2) C34 0.019(3) 0.032(3) 0.030(4) -0.002(3) 0.005(2) -0.002(2) C33 0.020(3) 0.032(3) 0.036(4) 0.011(3) 0.006(2) 0.010(2) C32 0.013(2) 0.027(3) 0.031(4) 0.008(3) 0.003(2) 0.001(2) C35 0.028(3) 0.021(3) 0.049(4) 0.010(3) 0.009(3) 0.001(2) C36 0.023(3) 0.044(4) 0.041(4) 0.017(3) 0.012(3) 0.010(3) C37 0.016(2) 0.022(3) 0.016(3) 0.007(2) 0.003(2) 0.006(2) C38 0.017(2) 0.020(3) 0.020(3) 0.007(2) 0.004(2) 0.003(2) C39 0.019(3) 0.025(3) 0.025(3) 0.008(3) 0.009(2) 0.005(2) C41 0.021(3) 0.025(3) 0.023(3) 0.010(3) 0.004(2) 0.004(2) C42 0.019(3) 0.018(3) 0.030(3) 0.009(3) 0.009(2) 0.003(2) C40 0.017(2) 0.017(3) 0.026(3) 0.005(2) 0.006(2) 0.005(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 Gd1 O1 2.340(3) . ? Gd1 O6 2.340(3) . ? Gd1 O5 2.346(3) . ? Gd1 O3 2.347(4) . ? Gd1 O2 2.359(3) . ? Gd1 O4 2.374(3) . ? Gd1 O7 2.431(3) . ? Gd1 N3 2.619(4) . ? F1 C1 1.325(6) . ? F2 C1 1.319(8) . ? F3 C1 1.311(7) . ? F4 C11 1.312(7) . ? F5 C11 1.285(7) . ? F6 C11 1.283(6) . ? F7 C21 1.333(6) . ? F8 C21 1.324(5) . ? F9 C21 1.324(6) . ? O1 C2 1.274(5) . ? O2 C4 1.261(5) . ? O3 C12 1.257(6) . ? O4 C14 1.254(6) . ? O5 C22 1.269(5) . ? O6 C24 1.272(5) . ? O7 N1 1.281(5) . ? O8 N2 1.276(5) . ? N1 C37 1.332(6) . ? N1 C31 1.516(6) . ? N2 C37 1.355(6) . ? N2 C32 1.504(6) . ? N3 C42 1.339(6) . ? N3 C41 1.343(6) . ? C14 C13 1.425(7) . ? C14 C15 1.506(6) . ? C13 C12 1.355(7) . ? C13 H13 0.9300 . ? C12 C11 1.530(7) . ? C15 C16 1.386(7) . ? C15 C20 1.386(7) . ? C16 C17 1.382(7) . ? C16 H16 0.9300 . ? C17 C18 1.377(8) . ? C17 H17 0.9300 . ? C18 C19 1.397(8) . ? C18 H18 0.9300 . ? C19 C20 1.385(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C4 C3 1.437(7) . ? C4 C5 1.490(6) . ? C3 C2 1.359(7) . ? C3 H3 0.9300 . ? C2 C1 1.519(7) . ? C5 C10 1.379(7) . ? C5 C6 1.393(7) . ? C6 C7 1.381(7) . ? C6 H6 0.9300 . ? C7 C8 1.383(7) . ? C7 H7 0.9300 . ? C8 C9 1.378(7) . ? C8 H8 0.9300 . ? C9 C10 1.397(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C24 C23 1.411(7) . ? C24 C25 1.502(6) . ? C23 C22 1.373(6) . ? C23 H23 0.9300 . ? C22 C21 1.522(7) . ? C25 C30 1.386(7) . ? C25 C26 1.402(7) . ? C26 C27 1.385(7) . ? C26 H26 0.9300 . ? C27 C28 1.383(7) . ? C27 H27 0.9300 . ? C28 C29 1.389(7) . ? C28 H28 0.9300 . ? C29 C30 1.367(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C34 1.517(7) . ? C31 C33 1.530(6) . ? C31 C32 1.551(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C32 C36 1.512(7) . ? C32 C35 1.527(7) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.466(6) . ? C38 C40 1.390(6) . ? C38 C39 1.395(7) . ? C39 C41 1.389(6) 2_666 ? C39 H39 0.9300 . ? C41 C39 1.389(6) 2_666 ? C41 H41 0.9300 . ? C42 C40 1.392(6) 2_666 ? C42 H42 0.9300 . ? C40 C42 1.392(6) 2_666 ? C40 H40 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 O1 Gd1 O6 135.53(11) . . ? O1 Gd1 O5 120.90(12) . . ? O6 Gd1 O5 73.71(11) . . ? O1 Gd1 O3 144.34(11) . . ? O6 Gd1 O3 77.60(12) . . ? O5 Gd1 O3 74.95(12) . . ? O1 Gd1 O2 73.00(11) . . ? O6 Gd1 O2 75.19(11) . . ? O5 Gd1 O2 144.78(10) . . ? O3 Gd1 O2 113.78(12) . . ? O1 Gd1 O4 76.94(12) . . ? O6 Gd1 O4 124.62(12) . . ? O5 Gd1 O4 135.14(11) . . ? O3 Gd1 O4 71.14(12) . . ? O2 Gd1 O4 77.29(11) . . ? O1 Gd1 O7 74.02(11) . . ? O6 Gd1 O7 74.79(12) . . ? O5 Gd1 O7 67.94(11) . . ? O3 Gd1 O7 138.49(11) . . ? O2 Gd1 O7 88.29(11) . . ? O4 Gd1 O7 150.29(12) . . ? O1 Gd1 N3 76.02(12) . . ? O6 Gd1 N3 141.50(12) . . ? O5 Gd1 N3 69.75(11) . . ? O3 Gd1 N3 81.60(12) . . ? O2 Gd1 N3 143.28(12) . . ? O4 Gd1 N3 76.93(12) . . ? O7 Gd1 N3 101.72(12) . . ? C2 O1 Gd1 130.7(3) . . ? C4 O2 Gd1 137.3(3) . . ? C12 O3 Gd1 132.4(3) . . ? C14 O4 Gd1 137.1(3) . . ? C22 O5 Gd1 132.6(3) . . ? C24 O6 Gd1 137.3(3) . . ? N1 O7 Gd1 138.7(3) . . ? O7 N1 C37 127.0(4) . . ? O7 N1 C31 120.3(4) . . ? C37 N1 C31 111.7(4) . . ? O8 N2 C37 126.1(4) . . ? O8 N2 C32 122.1(4) . . ? C37 N2 C32 111.6(4) . . ? C42 N3 C41 116.6(4) . . ? C42 N3 Gd1 124.8(3) . . ? C41 N3 Gd1 118.7(3) . . ? O4 C14 C13 123.2(5) . . ? O4 C14 C15 117.6(5) . . ? C13 C14 C15 119.1(5) . . ? C12 C13 C14 121.9(5) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? O3 C12 C13 128.6(5) . . ? O3 C12 C11 114.4(4) . . ? C13 C12 C11 117.0(5) . . ? C16 C15 C20 119.2(5) . . ? C16 C15 C14 118.8(5) . . ? C20 C15 C14 122.0(5) . . ? C17 C16 C15 120.4(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.8(6) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 121.0(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 118.2(6) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C15 121.4(5) . . ? C19 C20 H20 119.3 . . ? C15 C20 H20 119.3 . . ? F6 C11 F5 106.1(6) . . ? F6 C11 F4 105.3(5) . . ? F5 C11 F4 105.4(5) . . ? F6 C11 C12 115.1(5) . . ? F5 C11 C12 112.4(5) . . ? F4 C11 C12 111.8(5) . . ? O2 C4 C3 121.9(4) . . ? O2 C4 C5 118.5(4) . . ? C3 C4 C5 119.6(4) . . ? C2 C3 C4 123.2(5) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? O1 C2 C3 129.4(5) . . ? O1 C2 C1 113.1(4) . . ? C3 C2 C1 117.4(5) . . ? C10 C5 C6 119.2(5) . . ? C10 C5 C4 118.3(4) . . ? C6 C5 C4 122.5(5) . . ? C7 C6 C5 120.2(5) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.1(5) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.5(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C5 C10 C9 120.8(5) . . ? C5 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? F3 C1 F2 107.1(6) . . ? F3 C1 F1 106.3(5) . . ? F2 C1 F1 104.3(5) . . ? F3 C1 C2 111.8(5) . . ? F2 C1 C2 110.7(5) . . ? F1 C1 C2 116.0(5) . . ? O6 C24 C23 123.2(4) . . ? O6 C24 C25 116.4(4) . . ? C23 C24 C25 120.4(4) . . ? C22 C23 C24 123.5(4) . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? O5 C22 C23 129.4(5) . . ? O5 C22 C21 111.2(4) . . ? C23 C22 C21 119.4(4) . . ? C30 C25 C26 119.0(4) . . ? C30 C25 C24 122.8(5) . . ? C26 C25 C24 118.2(4) . . ? C27 C26 C25 119.8(5) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.5(5) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.4(5) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 120.4(5) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C25 120.9(5) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? F8 C21 F9 107.3(5) . . ? F8 C21 F7 106.2(5) . . ? F9 C21 F7 105.7(4) . . ? F8 C21 C22 114.7(4) . . ? F9 C21 C22 112.1(5) . . ? F7 C21 C22 110.3(4) . . ? N1 C31 C34 110.4(4) . . ? N1 C31 C33 104.9(4) . . ? C34 C31 C33 110.2(4) . . ? N1 C31 C32 100.3(4) . . ? C34 C31 C32 115.6(4) . . ? C33 C31 C32 114.4(4) . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N2 C32 C36 109.2(4) . . ? N2 C32 C35 106.2(4) . . ? C36 C32 C35 110.8(4) . . ? N2 C32 C31 100.7(4) . . ? C36 C32 C31 115.4(4) . . ? C35 C32 C31 113.6(5) . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 N2 109.1(4) . . ? N1 C37 C38 125.2(5) . . ? N2 C37 C38 125.6(5) . . ? C40 C38 C39 118.1(4) . . ? C40 C38 C37 121.1(4) . . ? C39 C38 C37 120.7(4) . . ? C41 C39 C38 118.6(5) 2_666 . ? C41 C39 H39 120.7 2_666 . ? C38 C39 H39 120.7 . . ? N3 C41 C39 123.9(5) . 2_666 ? N3 C41 H41 118.0 . . ? C39 C41 H41 118.0 2_666 . ? N3 C42 C40 123.9(5) . 2_666 ? N3 C42 H42 118.0 . . ? C40 C42 H42 118.0 2_666 . ? C38 C40 C42 118.8(5) . 2_666 ? C38 C40 H40 120.6 . . ? C42 C40 H40 120.6 2_666 . ? 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 O6 Gd1 O1 C2 68.6(4) . . . . ? O5 Gd1 O1 C2 166.8(4) . . . . ? O3 Gd1 O1 C2 -84.8(4) . . . . ? O2 Gd1 O1 C2 22.5(4) . . . . ? O4 Gd1 O1 C2 -58.0(4) . . . . ? O7 Gd1 O1 C2 115.7(4) . . . . ? N3 Gd1 O1 C2 -137.5(4) . . . . ? O1 Gd1 O2 C4 -13.5(4) . . . . ? O6 Gd1 O2 C4 -162.0(5) . . . . ? O5 Gd1 O2 C4 -133.4(4) . . . . ? O3 Gd1 O2 C4 129.0(4) . . . . ? O4 Gd1 O2 C4 66.5(4) . . . . ? O7 Gd1 O2 C4 -87.3(5) . . . . ? N3 Gd1 O2 C4 20.1(6) . . . . ? O1 Gd1 O3 C12 1.8(5) . . . . ? O6 Gd1 O3 C12 -159.5(4) . . . . ? O5 Gd1 O3 C12 124.3(4) . . . . ? O2 Gd1 O3 C12 -92.0(4) . . . . ? O4 Gd1 O3 C12 -25.8(4) . . . . ? O7 Gd1 O3 C12 151.4(4) . . . . ? N3 Gd1 O3 C12 53.1(4) . . . . ? O1 Gd1 O4 C14 -148.7(5) . . . . ? O6 Gd1 O4 C14 74.4(5) . . . . ? O5 Gd1 O4 C14 -27.7(5) . . . . ? O3 Gd1 O4 C14 15.2(4) . . . . ? O2 Gd1 O4 C14 136.1(5) . . . . ? O7 Gd1 O4 C14 -161.1(4) . . . . ? N3 Gd1 O4 C14 -70.3(5) . . . . ? O1 Gd1 O5 C22 -132.7(4) . . . . ? O6 Gd1 O5 C22 1.0(4) . . . . ? O3 Gd1 O5 C22 82.2(4) . . . . ? O2 Gd1 O5 C22 -27.8(5) . . . . ? O4 Gd1 O5 C22 124.1(4) . . . . ? O7 Gd1 O5 C22 -78.8(4) . . . . ? N3 Gd1 O5 C22 168.7(5) . . . . ? O1 Gd1 O6 C24 112.5(5) . . . . ? O5 Gd1 O6 C24 -5.3(5) . . . . ? O3 Gd1 O6 C24 -83.0(5) . . . . ? O2 Gd1 O6 C24 158.0(5) . . . . ? O4 Gd1 O6 C24 -139.3(5) . . . . ? O7 Gd1 O6 C24 65.7(5) . . . . ? N3 Gd1 O6 C24 -24.1(6) . . . . ? O1 Gd1 O7 N1 -25.7(4) . . . . ? O6 Gd1 O7 N1 122.3(4) . . . . ? O5 Gd1 O7 N1 -159.5(4) . . . . ? O3 Gd1 O7 N1 172.2(4) . . . . ? O2 Gd1 O7 N1 47.1(4) . . . . ? O4 Gd1 O7 N1 -13.1(5) . . . . ? N3 Gd1 O7 N1 -97.2(4) . . . . ? Gd1 O7 N1 C37 85.0(6) . . . . ? Gd1 O7 N1 C31 -107.7(4) . . . . ? O1 Gd1 N3 C42 4.3(4) . . . . ? O6 Gd1 N3 C42 154.6(3) . . . . ? O5 Gd1 N3 C42 135.3(4) . . . . ? O3 Gd1 N3 C42 -147.7(4) . . . . ? O2 Gd1 N3 C42 -28.8(5) . . . . ? O4 Gd1 N3 C42 -75.3(4) . . . . ? O7 Gd1 N3 C42 74.3(4) . . . . ? O1 Gd1 N3 C41 -177.7(4) . . . . ? O6 Gd1 N3 C41 -27.4(5) . . . . ? O5 Gd1 N3 C41 -46.7(3) . . . . ? O3 Gd1 N3 C41 30.3(4) . . . . ? O2 Gd1 N3 C41 149.2(3) . . . . ? O4 Gd1 N3 C41 102.8(4) . . . . ? O7 Gd1 N3 C41 -107.7(4) . . . . ? Gd1 O4 C14 C13 -3.1(8) . . . . ? Gd1 O4 C14 C15 178.0(3) . . . . ? O4 C14 C13 C12 -10.1(8) . . . . ? C15 C14 C13 C12 168.8(5) . . . . ? Gd1 O3 C12 C13 26.5(8) . . . . ? Gd1 O3 C12 C11 -153.3(4) . . . . ? C14 C13 C12 O3 -1.7(9) . . . . ? C14 C13 C12 C11 178.1(5) . . . . ? O4 C14 C15 C16 -24.9(7) . . . . ? C13 C14 C15 C16 156.1(5) . . . . ? O4 C14 C15 C20 152.8(5) . . . . ? C13 C14 C15 C20 -26.2(7) . . . . ? C20 C15 C16 C17 1.0(7) . . . . ? C14 C15 C16 C17 178.6(4) . . . . ? C15 C16 C17 C18 -1.3(8) . . . . ? C16 C17 C18 C19 0.6(8) . . . . ? C17 C18 C19 C20 0.4(8) . . . . ? C18 C19 C20 C15 -0.7(8) . . . . ? C16 C15 C20 C19 0.1(8) . . . . ? C14 C15 C20 C19 -177.5(4) . . . . ? O3 C12 C11 F6 151.8(5) . . . . ? C13 C12 C11 F6 -28.1(8) . . . . ? O3 C12 C11 F5 -86.6(6) . . . . ? C13 C12 C11 F5 93.5(6) . . . . ? O3 C12 C11 F4 31.7(7) . . . . ? C13 C12 C11 F4 -148.1(6) . . . . ? Gd1 O2 C4 C3 2.4(7) . . . . ? Gd1 O2 C4 C5 -178.3(3) . . . . ? O2 C4 C3 C2 9.3(8) . . . . ? C5 C4 C3 C2 -169.9(5) . . . . ? Gd1 O1 C2 C3 -23.2(8) . . . . ? Gd1 O1 C2 C1 159.8(4) . . . . ? C4 C3 C2 O1 1.5(9) . . . . ? C4 C3 C2 C1 178.4(5) . . . . ? O2 C4 C5 C10 13.5(7) . . . . ? C3 C4 C5 C10 -167.3(5) . . . . ? O2 C4 C5 C6 -164.4(5) . . . . ? C3 C4 C5 C6 14.8(7) . . . . ? C10 C5 C6 C7 3.0(7) . . . . ? C4 C5 C6 C7 -179.1(4) . . . . ? C5 C6 C7 C8 -1.0(8) . . . . ? C6 C7 C8 C9 -0.5(8) . . . . ? C7 C8 C9 C10 0.0(8) . . . . ? C6 C5 C10 C9 -3.5(7) . . . . ? C4 C5 C10 C9 178.5(4) . . . . ? C8 C9 C10 C5 2.0(7) . . . . ? O1 C2 C1 F3 -50.3(7) . . . . ? C3 C2 C1 F3 132.2(6) . . . . ? O1 C2 C1 F2 68.9(7) . . . . ? C3 C2 C1 F2 -108.5(6) . . . . ? O1 C2 C1 F1 -172.5(5) . . . . ? C3 C2 C1 F1 10.1(8) . . . . ? Gd1 O6 C24 C23 5.4(8) . . . . ? Gd1 O6 C24 C25 -175.4(3) . . . . ? O6 C24 C23 C22 0.5(9) . . . . ? C25 C24 C23 C22 -178.7(5) . . . . ? Gd1 O5 C22 C23 2.9(9) . . . . ? Gd1 O5 C22 C21 -177.5(3) . . . . ? C24 C23 C22 O5 -4.6(10) . . . . ? C24 C23 C22 C21 175.8(5) . . . . ? O6 C24 C25 C30 -167.8(5) . . . . ? C23 C24 C25 C30 11.4(8) . . . . ? O6 C24 C25 C26 10.2(7) . . . . ? C23 C24 C25 C26 -170.6(5) . . . . ? C30 C25 C26 C27 0.4(8) . . . . ? C24 C25 C26 C27 -177.7(5) . . . . ? C25 C26 C27 C28 0.4(9) . . . . ? C26 C27 C28 C29 -1.5(9) . . . . ? C27 C28 C29 C30 1.9(10) . . . . ? C28 C29 C30 C25 -1.1(10) . . . . ? C26 C25 C30 C29 0.0(9) . . . . ? C24 C25 C30 C29 177.9(6) . . . . ? O5 C22 C21 F8 -175.1(5) . . . . ? C23 C22 C21 F8 4.6(8) . . . . ? O5 C22 C21 F9 -52.4(6) . . . . ? C23 C22 C21 F9 127.3(5) . . . . ? O5 C22 C21 F7 65.1(6) . . . . ? C23 C22 C21 F7 -115.2(5) . . . . ? O7 N1 C31 C34 46.0(6) . . . . ? C37 N1 C31 C34 -144.9(4) . . . . ? O7 N1 C31 C33 -72.7(5) . . . . ? C37 N1 C31 C33 96.3(5) . . . . ? O7 N1 C31 C32 168.4(4) . . . . ? C37 N1 C31 C32 -22.5(5) . . . . ? O8 N2 C32 C36 42.5(6) . . . . ? C37 N2 C32 C36 -142.5(4) . . . . ? O8 N2 C32 C35 -77.1(6) . . . . ? C37 N2 C32 C35 98.0(5) . . . . ? O8 N2 C32 C31 164.3(4) . . . . ? C37 N2 C32 C31 -20.6(5) . . . . ? N1 C31 C32 N2 23.7(4) . . . . ? C34 C31 C32 N2 142.4(4) . . . . ? C33 C31 C32 N2 -87.9(4) . . . . ? N1 C31 C32 C36 141.2(4) . . . . ? C34 C31 C32 C36 -100.1(5) . . . . ? C33 C31 C32 C36 29.5(6) . . . . ? N1 C31 C32 C35 -89.3(5) . . . . ? C34 C31 C32 C35 29.4(6) . . . . ? C33 C31 C32 C35 159.0(4) . . . . ? O7 N1 C37 N2 178.7(4) . . . . ? C31 N1 C37 N2 10.5(6) . . . . ? O7 N1 C37 C38 1.6(8) . . . . ? C31 N1 C37 C38 -166.6(4) . . . . ? O8 N2 C37 N1 -177.9(4) . . . . ? C32 N2 C37 N1 7.3(6) . . . . ? O8 N2 C37 C38 -0.9(8) . . . . ? C32 N2 C37 C38 -175.7(4) . . . . ? N1 C37 C38 C40 29.4(8) . . . . ? N2 C37 C38 C40 -147.3(5) . . . . ? N1 C37 C38 C39 -153.4(5) . . . . ? N2 C37 C38 C39 30.0(8) . . . . ? C40 C38 C39 C41 -1.6(7) . . . 2_666 ? C37 C38 C39 C41 -178.9(5) . . . 2_666 ? C42 N3 C41 C39 0.9(8) . . . 2_666 ? Gd1 N3 C41 C39 -177.3(4) . . . 2_666 ? C41 N3 C42 C40 1.7(7) . . . 2_666 ? Gd1 N3 C42 C40 179.8(4) . . . 2_666 ? C39 C38 C40 C42 -0.8(7) . . . 2_666 ? C37 C38 C40 C42 176.5(5) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.971 _refine_diff_density_min -1.105 _refine_diff_density_rms 0.122 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 843545' #TrackingRef 'CIF file for compounds 1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 F18 N6 O16 Tb2' _chemical_formula_weight 2077.30 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.612(4) _cell_length_b 12.193(4) _cell_length_c 16.427(5) _cell_angle_alpha 105.204(5) _cell_angle_beta 101.292(4) _cell_angle_gamma 104.357(4) _cell_volume 2088.0(12) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6236 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 26.0 _exptl_crystal_description sheet _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 1.652 _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1034 _exptl_absorpt_coefficient_mu 1.790 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7160 _exptl_absorpt_correction_T_max 0.7160 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16493 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0887 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7321 _reflns_number_gt 6628 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0322P)^2^+1.5483P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7321 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.77694(3) 0.28027(3) 0.263272(17) 0.02393(10) Uani 1 1 d . . . F1 F 0.9743(5) 0.1572(5) 0.4913(4) 0.124(3) Uani 1 1 d . . . F2 F 0.8186(8) 0.1562(5) 0.5405(3) 0.120(3) Uani 1 1 d . . . F3 F 0.8447(4) -0.0053(3) 0.4797(2) 0.0537(12) Uani 1 1 d . . . F4 F 0.9839(8) 0.4998(5) 0.1097(4) 0.132(3) Uani 1 1 d . . . F5 F 1.1282(5) 0.4334(6) 0.1015(4) 0.112(2) Uani 1 1 d . . . F6 F 0.9659(6) 0.3554(5) 0.0021(3) 0.105(2) Uani 1 1 d . . . F7 F 0.8892(4) 0.6971(3) 0.2566(3) 0.0576(12) Uani 1 1 d . . . F8 F 0.8134(4) 0.7081(3) 0.3647(2) 0.0587(13) Uani 1 1 d . . . F9 F 0.7142(5) 0.7248(3) 0.2469(3) 0.0718(16) Uani 1 1 d . . . O1 O 0.8073(4) 0.2140(3) 0.3841(2) 0.0270(10) Uani 1 1 d . . . O2 O 0.6383(4) 0.0855(3) 0.2196(2) 0.0268(10) Uani 1 1 d . . . O3 O 0.8609(4) 0.3230(4) 0.1527(2) 0.0320(10) Uani 1 1 d . . . O4 O 0.9039(4) 0.1592(3) 0.2326(2) 0.0281(10) Uani 1 1 d . . . O5 O 0.7945(4) 0.4792(3) 0.2808(2) 0.0253(9) Uani 1 1 d . . . O6 O 0.6063(4) 0.2779(3) 0.1603(2) 0.0264(10) Uani 1 1 d . . . O7 O 0.6453(4) 0.3492(3) 0.3490(2) 0.0275(10) Uani 1 1 d . . . O8 O 0.5602(4) 0.3193(4) 0.6074(3) 0.0398(12) Uani 1 1 d . . . N1 N 0.5883(5) 0.3198(4) 0.4037(3) 0.0240(11) Uani 1 1 d . . . N2 N 0.5490(5) 0.3054(4) 0.5256(3) 0.0287(12) Uani 1 1 d . . . N3 N 0.9973(5) 0.4186(4) 0.3613(3) 0.0243(11) Uani 1 1 d . . . C1 C 0.8553(8) 0.1029(6) 0.4746(4) 0.046(2) Uani 1 1 d . . . C2 C 0.7834(6) 0.1089(5) 0.3888(4) 0.0267(14) Uani 1 1 d . . . C3 C 0.6991(6) 0.0044(5) 0.3304(4) 0.0314(15) Uani 1 1 d . . . H3 H 0.6908 -0.0657 0.3444 0.038 Uiso 1 1 calc R . . C4 C 0.6236(6) -0.0011(5) 0.2488(4) 0.0258(14) Uani 1 1 d . . . C5 C 0.5183(6) -0.1140(5) 0.1960(4) 0.0253(13) Uani 1 1 d . . . C6 C 0.4762(6) -0.2044(5) 0.2296(4) 0.0321(15) Uani 1 1 d . . . H6 H 0.5125 -0.1952 0.2877 0.039 Uiso 1 1 calc R . . C7 C 0.3818(6) -0.3074(5) 0.1786(4) 0.0372(17) Uani 1 1 d . . . H7 H 0.3543 -0.3673 0.2021 0.045 Uiso 1 1 calc R . . C8 C 0.3279(6) -0.3212(6) 0.0923(4) 0.0398(17) Uani 1 1 d . . . H8 H 0.2642 -0.3910 0.0576 0.048 Uiso 1 1 calc R . . C9 C 0.3677(6) -0.2324(6) 0.0569(4) 0.0365(16) Uani 1 1 d . . . H9 H 0.3313 -0.2427 -0.0014 0.044 Uiso 1 1 calc R . . C10 C 0.4629(6) -0.1268(5) 0.1092(4) 0.0295(15) Uani 1 1 d . . . H10 H 0.4890 -0.0658 0.0863 0.035 Uiso 1 1 calc R . . C11 C 1.0073(7) 0.3992(6) 0.0852(4) 0.0407(18) Uani 1 1 d . . . C12 C 0.9598(6) 0.3131(5) 0.1330(4) 0.0297(15) Uani 1 1 d . . . C13 C 1.0238(6) 0.2382(6) 0.1484(4) 0.0348(16) Uani 1 1 d . . . H13 H 1.0946 0.2409 0.1295 0.042 Uiso 1 1 calc R . . C14 C 0.9863(6) 0.1556(5) 0.1927(4) 0.0302(15) Uani 1 1 d . . . C15 C 1.0468(6) 0.0610(5) 0.1937(4) 0.0302(15) Uani 1 1 d . . . C16 C 1.0970(6) 0.0171(6) 0.1270(4) 0.0353(16) Uani 1 1 d . . . H16 H 1.0961 0.0494 0.0816 0.042 Uiso 1 1 calc R . . C17 C 1.1482(7) -0.0737(6) 0.1269(4) 0.0394(17) Uani 1 1 d . . . H17 H 1.1821 -0.1021 0.0821 0.047 Uiso 1 1 calc R . . C18 C 1.1485(7) -0.1222(6) 0.1949(5) 0.048(2) Uani 1 1 d . . . H18 H 1.1817 -0.1842 0.1948 0.058 Uiso 1 1 calc R . . C19 C 1.1001(6) -0.0791(6) 0.2625(4) 0.0375(17) Uani 1 1 d . . . H19 H 1.1032 -0.1102 0.3085 0.045 Uiso 1 1 calc R . . C20 C 1.0465(6) 0.0111(5) 0.2615(4) 0.0302(15) Uani 1 1 d . . . H20 H 1.0107 0.0380 0.3056 0.036 Uiso 1 1 calc R . . C21 C 0.7846(7) 0.6658(6) 0.2773(4) 0.0351(16) Uani 1 1 d . . . C22 C 0.7269(6) 0.5292(5) 0.2438(4) 0.0260(14) Uani 1 1 d . . . C23 C 0.6156(6) 0.4786(5) 0.1796(4) 0.0335(16) Uani 1 1 d . . . H23 H 0.5762 0.5289 0.1608 0.040 Uiso 1 1 calc R . . C24 C 0.5587(6) 0.3535(6) 0.1410(4) 0.0283(14) Uani 1 1 d . . . C25 C 0.4376(6) 0.3048(6) 0.0706(4) 0.0295(15) Uani 1 1 d . . . C26 C 0.3768(6) 0.1816(6) 0.0423(4) 0.0329(15) Uani 1 1 d . . . H26 H 0.4101 0.1331 0.0685 0.039 Uiso 1 1 calc R . . C27 C 0.2662(6) 0.1310(6) -0.0249(4) 0.0385(17) Uani 1 1 d . . . H27 H 0.2257 0.0490 -0.0435 0.046 Uiso 1 1 calc R . . C28 C 0.2170(7) 0.2032(6) -0.0638(4) 0.0459(19) Uani 1 1 d . . . H28 H 0.1435 0.1696 -0.1089 0.055 Uiso 1 1 calc R . . C29 C 0.2770(7) 0.3254(7) -0.0358(4) 0.049(2) Uani 1 1 d . . . H29 H 0.2432 0.3735 -0.0621 0.059 Uiso 1 1 calc R . . C30 C 0.3868(6) 0.3767(6) 0.0311(4) 0.0369(16) Uani 1 1 d . . . H30 H 0.4265 0.4589 0.0495 0.044 Uiso 1 1 calc R . . C31 C 0.4499(6) 0.2645(5) 0.3761(4) 0.0261(14) Uani 1 1 d . . . C32 C 0.4317(6) 0.2216(5) 0.4553(4) 0.0297(15) Uani 1 1 d . . . C33 C 0.4070(6) 0.1668(6) 0.2874(4) 0.0375(17) Uani 1 1 d . . . H33A H 0.4275 0.2011 0.2437 0.056 Uiso 1 1 calc R . . H33B H 0.3190 0.1301 0.2721 0.056 Uiso 1 1 calc R . . H33C H 0.4473 0.1075 0.2902 0.056 Uiso 1 1 calc R . . C34 C 0.3991(6) 0.3668(5) 0.3697(4) 0.0309(15) Uani 1 1 d . . . H34A H 0.4267 0.4281 0.4261 0.046 Uiso 1 1 calc R . . H34B H 0.3103 0.3371 0.3512 0.046 Uiso 1 1 calc R . . H34C H 0.4285 0.3995 0.3276 0.046 Uiso 1 1 calc R . . C35 C 0.4382(7) 0.0955(5) 0.4445(4) 0.0427(18) Uani 1 1 d . . . H35A H 0.5071 0.0861 0.4225 0.064 Uiso 1 1 calc R . . H35B H 0.3630 0.0380 0.4039 0.064 Uiso 1 1 calc R . . H35C H 0.4485 0.0828 0.5004 0.064 Uiso 1 1 calc R . . C36 C 0.3206(6) 0.2380(6) 0.4861(4) 0.0367(16) Uani 1 1 d . . . H36A H 0.3207 0.2146 0.5375 0.055 Uiso 1 1 calc R . . H36B H 0.2461 0.1893 0.4404 0.055 Uiso 1 1 calc R . . H36C H 0.3245 0.3206 0.4999 0.055 Uiso 1 1 calc R . . C37 C 0.6382(6) 0.3520(5) 0.4905(4) 0.0236(13) Uani 1 1 d . . . C38 C 0.7638(6) 0.4285(5) 0.5399(4) 0.0254(14) Uani 1 1 d . . . C39 C 0.8269(6) 0.5159(5) 0.5112(4) 0.0262(14) Uani 1 1 d . . . H39 H 0.7914 0.5242 0.4582 0.031 Uiso 1 1 calc R . . C40 C 0.8219(6) 0.4178(5) 0.6191(3) 0.0259(14) Uani 1 1 d . . . H40 H 0.7816 0.3610 0.6411 0.031 Uiso 1 1 calc R . . C41 C 1.0560(6) 0.4086(5) 0.4374(3) 0.0254(14) Uani 1 1 d . . . H41 H 1.0158 0.3482 0.4564 0.031 Uiso 1 1 calc R . . C42 C 1.0595(6) 0.5063(5) 0.3359(4) 0.0296(15) Uani 1 1 d . . . H42 H 1.0201 0.5165 0.2847 0.036 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 Tb1 0.02050(18) 0.02197(17) 0.02473(16) 0.00645(12) 0.00379(12) 0.00205(12) F1 0.061(4) 0.113(5) 0.153(5) 0.104(4) -0.064(4) -0.043(4) F2 0.261(9) 0.100(4) 0.027(2) 0.022(3) 0.021(4) 0.120(5) F3 0.063(3) 0.029(2) 0.056(2) 0.023(2) -0.011(2) 0.004(2) F4 0.244(9) 0.068(4) 0.187(6) 0.089(4) 0.174(6) 0.088(5) F5 0.045(4) 0.146(6) 0.165(6) 0.127(5) 0.015(4) -0.007(4) F6 0.147(6) 0.081(4) 0.040(3) 0.032(3) 0.000(3) -0.034(4) F7 0.055(3) 0.033(2) 0.083(3) 0.023(2) 0.026(3) -0.001(2) F8 0.080(4) 0.033(2) 0.038(2) -0.0081(19) 0.008(2) 0.002(2) F9 0.063(4) 0.031(2) 0.094(3) 0.008(2) -0.026(3) 0.018(2) O1 0.031(3) 0.021(2) 0.023(2) 0.0074(18) 0.0041(19) 0.0013(19) O2 0.023(3) 0.021(2) 0.029(2) 0.0041(18) 0.0040(19) 0.0019(18) O3 0.029(3) 0.042(3) 0.028(2) 0.018(2) 0.009(2) 0.010(2) O4 0.020(3) 0.032(2) 0.036(2) 0.0139(19) 0.0136(19) 0.0089(19) O5 0.028(3) 0.022(2) 0.027(2) 0.0100(18) 0.0052(19) 0.0071(19) O6 0.018(2) 0.031(2) 0.022(2) 0.0074(18) -0.0026(18) 0.0027(19) O7 0.025(3) 0.034(2) 0.026(2) 0.0127(19) 0.0118(19) 0.007(2) O8 0.028(3) 0.052(3) 0.031(2) 0.015(2) 0.008(2) -0.002(2) N1 0.017(3) 0.019(3) 0.029(3) 0.003(2) 0.004(2) 0.000(2) N2 0.021(3) 0.030(3) 0.030(3) 0.010(2) 0.001(2) 0.002(2) N3 0.020(3) 0.021(3) 0.027(3) 0.007(2) 0.005(2) 0.001(2) C1 0.052(6) 0.023(4) 0.039(4) 0.010(3) -0.014(4) -0.006(3) C2 0.020(4) 0.026(3) 0.035(3) 0.014(3) 0.009(3) 0.005(3) C3 0.030(4) 0.020(3) 0.041(4) 0.011(3) 0.004(3) 0.006(3) C4 0.019(4) 0.027(3) 0.029(3) 0.006(3) 0.006(3) 0.008(3) C5 0.020(4) 0.024(3) 0.033(3) 0.010(3) 0.009(3) 0.006(3) C6 0.029(4) 0.028(4) 0.034(3) 0.010(3) 0.006(3) 0.004(3) C7 0.031(4) 0.024(3) 0.050(4) 0.011(3) 0.006(3) 0.003(3) C8 0.029(4) 0.024(4) 0.050(4) -0.002(3) 0.009(3) -0.003(3) C9 0.035(4) 0.035(4) 0.029(3) 0.000(3) 0.007(3) 0.006(3) C10 0.031(4) 0.029(3) 0.027(3) 0.006(3) 0.011(3) 0.008(3) C11 0.042(5) 0.039(4) 0.044(4) 0.018(3) 0.020(4) 0.006(4) C12 0.030(4) 0.031(4) 0.021(3) 0.005(3) 0.006(3) 0.002(3) C13 0.034(4) 0.036(4) 0.038(4) 0.014(3) 0.018(3) 0.009(3) C14 0.025(4) 0.029(3) 0.030(3) 0.003(3) 0.003(3) 0.007(3) C15 0.021(4) 0.031(4) 0.032(3) 0.006(3) 0.004(3) 0.003(3) C16 0.032(4) 0.037(4) 0.032(3) 0.008(3) 0.006(3) 0.010(3) C17 0.033(5) 0.039(4) 0.045(4) 0.010(3) 0.009(3) 0.014(3) C18 0.038(5) 0.032(4) 0.066(5) 0.006(4) 0.007(4) 0.012(3) C19 0.027(4) 0.037(4) 0.039(4) 0.013(3) -0.002(3) 0.001(3) C20 0.020(4) 0.025(3) 0.036(3) 0.006(3) 0.000(3) 0.002(3) C21 0.031(4) 0.029(4) 0.038(4) 0.008(3) -0.002(3) 0.009(3) C22 0.028(4) 0.022(3) 0.025(3) 0.005(3) 0.007(3) 0.005(3) C23 0.032(4) 0.027(3) 0.035(3) 0.008(3) 0.000(3) 0.007(3) C24 0.025(4) 0.037(4) 0.022(3) 0.012(3) 0.003(3) 0.007(3) C25 0.024(4) 0.034(4) 0.023(3) 0.005(3) 0.000(3) 0.005(3) C26 0.028(4) 0.033(4) 0.031(3) 0.007(3) 0.008(3) 0.002(3) C27 0.027(4) 0.041(4) 0.033(3) 0.010(3) 0.000(3) -0.005(3) C28 0.037(5) 0.046(5) 0.037(4) 0.010(3) -0.007(3) 0.000(4) C29 0.047(5) 0.047(5) 0.048(4) 0.020(4) -0.001(4) 0.013(4) C30 0.028(4) 0.041(4) 0.036(4) 0.013(3) -0.001(3) 0.008(3) C31 0.013(3) 0.029(3) 0.030(3) 0.008(3) 0.002(3) -0.001(3) C32 0.020(4) 0.026(3) 0.038(3) 0.010(3) 0.009(3) -0.001(3) C33 0.019(4) 0.040(4) 0.036(4) -0.001(3) 0.001(3) -0.001(3) C34 0.025(4) 0.032(4) 0.033(3) 0.011(3) 0.005(3) 0.006(3) C35 0.036(5) 0.029(4) 0.057(4) 0.015(3) 0.009(4) 0.002(3) C36 0.023(4) 0.045(4) 0.043(4) 0.015(3) 0.013(3) 0.008(3) C37 0.022(4) 0.021(3) 0.029(3) 0.009(3) 0.009(3) 0.005(3) C38 0.020(4) 0.025(3) 0.028(3) 0.006(3) 0.007(3) 0.004(3) C39 0.022(4) 0.028(3) 0.029(3) 0.008(3) 0.009(3) 0.008(3) C40 0.023(4) 0.026(3) 0.024(3) 0.007(3) 0.007(3) 0.002(3) C41 0.029(4) 0.018(3) 0.026(3) 0.003(3) 0.008(3) 0.005(3) C42 0.031(4) 0.027(3) 0.026(3) 0.009(3) 0.008(3) 0.002(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 Tb1 O5 2.318(4) . ? Tb1 O6 2.328(4) . ? Tb1 O1 2.329(4) . ? Tb1 O3 2.336(4) . ? Tb1 O2 2.346(4) . ? Tb1 O4 2.364(4) . ? Tb1 O7 2.426(4) . ? Tb1 N3 2.609(5) . ? F1 C1 1.314(9) . ? F2 C1 1.313(9) . ? F3 C1 1.319(7) . ? F4 C11 1.300(8) . ? F5 C11 1.312(9) . ? F6 C11 1.271(7) . ? F7 C21 1.318(8) . ? F8 C21 1.334(7) . ? F9 C21 1.325(7) . ? O1 C2 1.268(6) . ? O2 C4 1.258(7) . ? O3 C12 1.277(7) . ? O4 C14 1.264(7) . ? O5 C22 1.266(7) . ? O6 C24 1.262(7) . ? O7 N1 1.288(6) . ? O8 N2 1.286(6) . ? N1 C37 1.338(7) . ? N1 C31 1.503(7) . ? N2 C37 1.357(7) . ? N2 C32 1.519(7) . ? N3 C42 1.345(7) . ? N3 C41 1.352(7) . ? C1 C2 1.522(8) . ? C2 C3 1.370(8) . ? C3 C4 1.425(8) . ? C3 H3 0.9300 . ? C4 C5 1.506(8) . ? C5 C6 1.384(8) . ? C5 C10 1.394(8) . ? C6 C7 1.374(8) . ? C6 H6 0.9300 . ? C7 C8 1.380(8) . ? C7 H7 0.9300 . ? C8 C9 1.382(9) . ? C8 H8 0.9300 . ? C9 C10 1.400(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.529(8) . ? C12 C13 1.354(9) . ? C13 C14 1.424(8) . ? C13 H13 0.9300 . ? C14 C15 1.494(8) . ? C15 C16 1.387(8) . ? C15 C20 1.402(8) . ? C16 C17 1.380(9) . ? C16 H16 0.9300 . ? C17 C18 1.394(9) . ? C17 H17 0.9300 . ? C18 C19 1.382(9) . ? C18 H18 0.9300 . ? C19 C20 1.393(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.532(8) . ? C22 C23 1.376(8) . ? C23 C24 1.412(8) . ? C23 H23 0.9300 . ? C24 C25 1.502(8) . ? C25 C30 1.395(8) . ? C25 C26 1.397(8) . ? C26 C27 1.395(8) . ? C26 H26 0.9300 . ? C27 C28 1.382(9) . ? C27 H27 0.9300 . ? C28 C29 1.385(9) . ? C28 H28 0.9300 . ? C29 C30 1.385(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C33 1.517(7) . ? C31 C34 1.524(8) . ? C31 C32 1.555(8) . ? C32 C36 1.514(8) . ? C32 C35 1.524(8) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.456(8) . ? C38 C39 1.380(8) . ? C38 C40 1.398(8) . ? C39 C41 1.390(8) 2_766 ? C39 H39 0.9300 . ? C40 C42 1.382(8) 2_766 ? C40 H40 0.9300 . ? C41 C39 1.390(8) 2_766 ? C41 H41 0.9300 . ? C42 C40 1.382(8) 2_766 ? C42 H42 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 O5 Tb1 O6 73.97(14) . . ? O5 Tb1 O1 121.10(13) . . ? O6 Tb1 O1 135.74(15) . . ? O5 Tb1 O3 74.36(14) . . ? O6 Tb1 O3 77.01(15) . . ? O1 Tb1 O3 144.70(15) . . ? O5 Tb1 O2 144.95(15) . . ? O6 Tb1 O2 74.91(14) . . ? O1 Tb1 O2 73.28(13) . . ? O3 Tb1 O2 113.56(14) . . ? O5 Tb1 O4 134.90(14) . . ? O6 Tb1 O4 124.39(13) . . ? O1 Tb1 O4 76.75(14) . . ? O3 Tb1 O4 71.68(14) . . ? O2 Tb1 O4 77.20(14) . . ? O5 Tb1 O7 68.30(14) . . ? O6 Tb1 O7 75.15(13) . . ? O1 Tb1 O7 74.02(14) . . ? O3 Tb1 O7 138.14(14) . . ? O2 Tb1 O7 88.44(14) . . ? O4 Tb1 O7 150.10(13) . . ? O5 Tb1 N3 69.78(14) . . ? O6 Tb1 N3 141.64(14) . . ? O1 Tb1 N3 76.10(14) . . ? O3 Tb1 N3 81.54(15) . . ? O2 Tb1 N3 143.36(14) . . ? O4 Tb1 N3 76.61(14) . . ? O7 Tb1 N3 102.05(14) . . ? C2 O1 Tb1 130.9(4) . . ? C4 O2 Tb1 136.6(4) . . ? C12 O3 Tb1 131.7(4) . . ? C14 O4 Tb1 137.3(4) . . ? C22 O5 Tb1 132.8(4) . . ? C24 O6 Tb1 137.2(4) . . ? N1 O7 Tb1 139.2(3) . . ? O7 N1 C37 125.3(5) . . ? O7 N1 C31 120.6(4) . . ? C37 N1 C31 113.2(5) . . ? O8 N2 C37 126.5(5) . . ? O8 N2 C32 121.3(5) . . ? C37 N2 C32 112.0(5) . . ? C42 N3 C41 116.3(5) . . ? C42 N3 Tb1 119.2(4) . . ? C41 N3 Tb1 124.6(4) . . ? F2 C1 F1 107.5(7) . . ? F2 C1 F3 104.7(6) . . ? F1 C1 F3 106.3(7) . . ? F2 C1 C2 110.5(7) . . ? F1 C1 C2 110.9(6) . . ? F3 C1 C2 116.4(5) . . ? O1 C2 C3 129.2(6) . . ? O1 C2 C1 113.6(5) . . ? C3 C2 C1 117.1(5) . . ? C2 C3 C4 122.5(6) . . ? C2 C3 H3 118.8 . . ? C4 C3 H3 118.8 . . ? O2 C4 C3 123.2(6) . . ? O2 C4 C5 117.9(5) . . ? C3 C4 C5 118.9(5) . . ? C6 C5 C10 119.6(6) . . ? C6 C5 C4 122.9(5) . . ? C10 C5 C4 117.5(5) . . ? C7 C6 C5 121.2(6) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 119.5(6) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 120.7(6) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 119.8(6) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C5 C10 C9 119.3(6) . . ? C5 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? F6 C11 F4 107.7(7) . . ? F6 C11 F5 105.3(7) . . ? F4 C11 F5 103.1(7) . . ? F6 C11 C12 113.8(6) . . ? F4 C11 C12 113.2(6) . . ? F5 C11 C12 112.9(6) . . ? O3 C12 C13 128.8(6) . . ? O3 C12 C11 112.7(6) . . ? C13 C12 C11 118.5(6) . . ? C12 C13 C14 122.1(6) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? O4 C14 C13 122.7(6) . . ? O4 C14 C15 117.9(6) . . ? C13 C14 C15 119.4(6) . . ? C16 C15 C20 119.4(6) . . ? C16 C15 C14 121.7(6) . . ? C20 C15 C14 118.8(6) . . ? C17 C16 C15 121.1(6) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 119.1(7) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.7(7) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 119.9(6) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C15 119.6(6) . . ? C19 C20 H20 120.2 . . ? C15 C20 H20 120.2 . . ? F7 C21 F9 107.0(6) . . ? F7 C21 F8 106.2(6) . . ? F9 C21 F8 106.9(5) . . ? F7 C21 C22 110.5(5) . . ? F9 C21 C22 115.1(5) . . ? F8 C21 C22 110.7(5) . . ? O5 C22 C23 129.6(6) . . ? O5 C22 C21 111.8(5) . . ? C23 C22 C21 118.6(6) . . ? C22 C23 C24 122.8(6) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? O6 C24 C23 123.3(6) . . ? O6 C24 C25 116.8(5) . . ? C23 C24 C25 119.8(6) . . ? C30 C25 C26 119.5(6) . . ? C30 C25 C24 122.7(6) . . ? C26 C25 C24 117.8(6) . . ? C27 C26 C25 120.2(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 119.8(6) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C29 120.1(6) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.7(7) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 119.8(6) . . ? C29 C30 H30 120.1 . . ? C25 C30 H30 120.1 . . ? N1 C31 C33 110.7(5) . . ? N1 C31 C34 105.1(5) . . ? C33 C31 C34 110.0(5) . . ? N1 C31 C32 100.2(4) . . ? C33 C31 C32 115.7(5) . . ? C34 C31 C32 114.2(5) . . ? C36 C32 N2 109.0(5) . . ? C36 C32 C35 111.0(5) . . ? N2 C32 C35 105.8(5) . . ? C36 C32 C31 115.7(5) . . ? N2 C32 C31 100.3(5) . . ? C35 C32 C31 114.0(5) . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 N2 107.8(5) . . ? N1 C37 C38 126.6(5) . . ? N2 C37 C38 125.5(5) . . ? C39 C38 C40 118.4(6) . . ? C39 C38 C37 120.9(5) . . ? C40 C38 C37 120.7(5) . . ? C38 C39 C41 119.2(6) . 2_766 ? C38 C39 H39 120.4 . . ? C41 C39 H39 120.4 2_766 . ? C42 C40 C38 118.4(6) 2_766 . ? C42 C40 H40 120.8 2_766 . ? C38 C40 H40 120.8 . . ? N3 C41 C39 123.4(6) . 2_766 ? N3 C41 H41 118.3 . . ? C39 C41 H41 118.3 2_766 . ? N3 C42 C40 124.3(6) . 2_766 ? N3 C42 H42 117.9 . . ? C40 C42 H42 117.9 2_766 . ? 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 O5 Tb1 O1 C2 167.3(5) . . . . ? O6 Tb1 O1 C2 68.2(6) . . . . ? O3 Tb1 O1 C2 -84.9(6) . . . . ? O2 Tb1 O1 C2 22.5(5) . . . . ? O4 Tb1 O1 C2 -57.9(5) . . . . ? O7 Tb1 O1 C2 115.7(5) . . . . ? N3 Tb1 O1 C2 -137.2(5) . . . . ? O5 Tb1 O2 C4 -134.3(5) . . . . ? O6 Tb1 O2 C4 -162.3(6) . . . . ? O1 Tb1 O2 C4 -13.5(5) . . . . ? O3 Tb1 O2 C4 129.5(5) . . . . ? O4 Tb1 O2 C4 66.3(5) . . . . ? O7 Tb1 O2 C4 -87.3(5) . . . . ? N3 Tb1 O2 C4 21.0(6) . . . . ? O5 Tb1 O3 C12 124.4(5) . . . . ? O6 Tb1 O3 C12 -158.9(5) . . . . ? O1 Tb1 O3 C12 2.2(6) . . . . ? O2 Tb1 O3 C12 -92.0(5) . . . . ? O4 Tb1 O3 C12 -25.5(5) . . . . ? O7 Tb1 O3 C12 151.8(5) . . . . ? N3 Tb1 O3 C12 53.1(5) . . . . ? O5 Tb1 O4 C14 -28.3(6) . . . . ? O6 Tb1 O4 C14 73.8(6) . . . . ? O1 Tb1 O4 C14 -149.3(6) . . . . ? O3 Tb1 O4 C14 14.7(6) . . . . ? O2 Tb1 O4 C14 135.2(6) . . . . ? O7 Tb1 O4 C14 -161.6(5) . . . . ? N3 Tb1 O4 C14 -70.7(6) . . . . ? O6 Tb1 O5 C22 1.8(5) . . . . ? O1 Tb1 O5 C22 -132.4(5) . . . . ? O3 Tb1 O5 C22 82.4(5) . . . . ? O2 Tb1 O5 C22 -26.4(6) . . . . ? O4 Tb1 O5 C22 124.7(5) . . . . ? O7 Tb1 O5 C22 -78.3(5) . . . . ? N3 Tb1 O5 C22 169.0(5) . . . . ? O5 Tb1 O6 C24 -6.2(6) . . . . ? O1 Tb1 O6 C24 112.2(6) . . . . ? O3 Tb1 O6 C24 -83.4(6) . . . . ? O2 Tb1 O6 C24 157.5(6) . . . . ? O4 Tb1 O6 C24 -140.1(5) . . . . ? O7 Tb1 O6 C24 65.1(6) . . . . ? N3 Tb1 O6 C24 -25.7(7) . . . . ? O5 Tb1 O7 N1 -160.4(5) . . . . ? O6 Tb1 O7 N1 121.3(5) . . . . ? O1 Tb1 O7 N1 -26.6(5) . . . . ? O3 Tb1 O7 N1 171.1(5) . . . . ? O2 Tb1 O7 N1 46.5(5) . . . . ? O4 Tb1 O7 N1 -14.1(7) . . . . ? N3 Tb1 O7 N1 -98.1(5) . . . . ? Tb1 O7 N1 C37 85.5(7) . . . . ? Tb1 O7 N1 C31 -106.4(6) . . . . ? O5 Tb1 N3 C42 -46.2(4) . . . . ? O6 Tb1 N3 C42 -26.2(5) . . . . ? O1 Tb1 N3 C42 -177.3(5) . . . . ? O3 Tb1 N3 C42 30.2(4) . . . . ? O2 Tb1 N3 C42 148.7(4) . . . . ? O4 Tb1 N3 C42 103.3(4) . . . . ? O7 Tb1 N3 C42 -107.4(4) . . . . ? O5 Tb1 N3 C41 134.2(5) . . . . ? O6 Tb1 N3 C41 154.2(4) . . . . ? O1 Tb1 N3 C41 3.0(4) . . . . ? O3 Tb1 N3 C41 -149.5(4) . . . . ? O2 Tb1 N3 C41 -31.0(5) . . . . ? O4 Tb1 N3 C41 -76.4(4) . . . . ? O7 Tb1 N3 C41 72.9(4) . . . . ? Tb1 O1 C2 C3 -23.3(10) . . . . ? Tb1 O1 C2 C1 160.4(5) . . . . ? F2 C1 C2 O1 67.8(8) . . . . ? F1 C1 C2 O1 -51.3(9) . . . . ? F3 C1 C2 O1 -172.9(6) . . . . ? F2 C1 C2 C3 -108.9(7) . . . . ? F1 C1 C2 C3 131.9(7) . . . . ? F3 C1 C2 C3 10.3(10) . . . . ? O1 C2 C3 C4 2.1(11) . . . . ? C1 C2 C3 C4 178.2(6) . . . . ? Tb1 O2 C4 C3 2.8(9) . . . . ? Tb1 O2 C4 C5 -179.3(4) . . . . ? C2 C3 C4 O2 8.6(10) . . . . ? C2 C3 C4 C5 -169.3(6) . . . . ? O2 C4 C5 C6 -165.4(6) . . . . ? C3 C4 C5 C6 12.6(9) . . . . ? O2 C4 C5 C10 15.2(8) . . . . ? C3 C4 C5 C10 -166.8(6) . . . . ? C10 C5 C6 C7 0.9(10) . . . . ? C4 C5 C6 C7 -178.5(6) . . . . ? C5 C6 C7 C8 0.1(10) . . . . ? C6 C7 C8 C9 -0.3(10) . . . . ? C7 C8 C9 C10 -0.5(10) . . . . ? C6 C5 C10 C9 -1.7(9) . . . . ? C4 C5 C10 C9 177.7(5) . . . . ? C8 C9 C10 C5 1.5(10) . . . . ? Tb1 O3 C12 C13 25.9(9) . . . . ? Tb1 O3 C12 C11 -154.5(4) . . . . ? F6 C11 C12 O3 -91.2(8) . . . . ? F4 C11 C12 O3 32.3(9) . . . . ? F5 C11 C12 O3 148.9(6) . . . . ? F6 C11 C12 C13 88.5(9) . . . . ? F4 C11 C12 C13 -148.1(7) . . . . ? F5 C11 C12 C13 -31.4(9) . . . . ? O3 C12 C13 C14 -0.6(10) . . . . ? C11 C12 C13 C14 179.8(6) . . . . ? Tb1 O4 C14 C13 -1.7(10) . . . . ? Tb1 O4 C14 C15 177.6(4) . . . . ? C12 C13 C14 O4 -11.6(10) . . . . ? C12 C13 C14 C15 169.1(6) . . . . ? O4 C14 C15 C16 153.2(6) . . . . ? C13 C14 C15 C16 -27.5(9) . . . . ? O4 C14 C15 C20 -23.3(9) . . . . ? C13 C14 C15 C20 156.0(6) . . . . ? C20 C15 C16 C17 -0.9(10) . . . . ? C14 C15 C16 C17 -177.4(6) . . . . ? C15 C16 C17 C18 0.4(11) . . . . ? C16 C17 C18 C19 -1.0(11) . . . . ? C17 C18 C19 C20 2.2(11) . . . . ? C18 C19 C20 C15 -2.7(10) . . . . ? C16 C15 C20 C19 2.0(9) . . . . ? C14 C15 C20 C19 178.6(6) . . . . ? Tb1 O5 C22 C23 1.1(10) . . . . ? Tb1 O5 C22 C21 -177.3(4) . . . . ? F7 C21 C22 O5 64.1(7) . . . . ? F9 C21 C22 O5 -174.6(6) . . . . ? F8 C21 C22 O5 -53.2(7) . . . . ? F7 C21 C22 C23 -114.5(7) . . . . ? F9 C21 C22 C23 6.8(9) . . . . ? F8 C21 C22 C23 128.2(6) . . . . ? O5 C22 C23 C24 -2.1(11) . . . . ? C21 C22 C23 C24 176.2(6) . . . . ? Tb1 O6 C24 C23 7.3(10) . . . . ? Tb1 O6 C24 C25 -175.1(4) . . . . ? C22 C23 C24 O6 -1.9(10) . . . . ? C22 C23 C24 C25 -179.4(6) . . . . ? O6 C24 C25 C30 -167.4(6) . . . . ? C23 C24 C25 C30 10.3(9) . . . . ? O6 C24 C25 C26 10.5(8) . . . . ? C23 C24 C25 C26 -171.8(6) . . . . ? C30 C25 C26 C27 0.1(10) . . . . ? C24 C25 C26 C27 -177.8(6) . . . . ? C25 C26 C27 C28 0.2(10) . . . . ? C26 C27 C28 C29 -0.3(11) . . . . ? C27 C28 C29 C30 0.3(12) . . . . ? C28 C29 C30 C25 0.0(11) . . . . ? C26 C25 C30 C29 -0.2(10) . . . . ? C24 C25 C30 C29 177.7(6) . . . . ? O7 N1 C31 C33 45.5(7) . . . . ? C37 N1 C31 C33 -145.0(5) . . . . ? O7 N1 C31 C34 -73.2(6) . . . . ? C37 N1 C31 C34 96.2(5) . . . . ? O7 N1 C31 C32 168.2(4) . . . . ? C37 N1 C31 C32 -22.4(6) . . . . ? O8 N2 C32 C36 42.7(7) . . . . ? C37 N2 C32 C36 -142.5(5) . . . . ? O8 N2 C32 C35 -76.7(7) . . . . ? C37 N2 C32 C35 98.1(6) . . . . ? O8 N2 C32 C31 164.6(5) . . . . ? C37 N2 C32 C31 -20.6(6) . . . . ? N1 C31 C32 C36 140.4(5) . . . . ? C33 C31 C32 C36 -100.6(6) . . . . ? C34 C31 C32 C36 28.6(7) . . . . ? N1 C31 C32 N2 23.4(5) . . . . ? C33 C31 C32 N2 142.4(5) . . . . ? C34 C31 C32 N2 -88.4(6) . . . . ? N1 C31 C32 C35 -89.1(6) . . . . ? C33 C31 C32 C35 29.9(8) . . . . ? C34 C31 C32 C35 159.1(6) . . . . ? O7 N1 C37 N2 179.1(5) . . . . ? C31 N1 C37 N2 10.3(6) . . . . ? O7 N1 C37 C38 2.2(9) . . . . ? C31 N1 C37 C38 -166.7(5) . . . . ? O8 N2 C37 N1 -178.0(5) . . . . ? C32 N2 C37 N1 7.5(7) . . . . ? O8 N2 C37 C38 -1.1(9) . . . . ? C32 N2 C37 C38 -175.5(5) . . . . ? N1 C37 C38 C39 28.5(9) . . . . ? N2 C37 C38 C39 -147.9(6) . . . . ? N1 C37 C38 C40 -153.7(6) . . . . ? N2 C37 C38 C40 29.9(9) . . . . ? C40 C38 C39 C41 -1.3(8) . . . 2_766 ? C37 C38 C39 C41 176.6(5) . . . 2_766 ? C39 C38 C40 C42 -1.2(9) . . . 2_766 ? C37 C38 C40 C42 -179.1(5) . . . 2_766 ? C42 N3 C41 C39 0.8(8) . . . 2_766 ? Tb1 N3 C41 C39 -179.5(4) . . . 2_766 ? C41 N3 C42 C40 2.0(9) . . . 2_766 ? Tb1 N3 C42 C40 -177.7(4) . . . 2_766 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.014 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.123 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 843546' #TrackingRef 'CIF file for compounds 1-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 Dy2 F18 N6 O16' _chemical_formula_weight 2084.44 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' Dy Dy -0.1892 4.4098 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.613(8) _cell_length_b 12.204(7) _cell_length_c 16.441(10) _cell_angle_alpha 105.058(9) _cell_angle_beta 101.383(5) _cell_angle_gamma 104.289(8) _cell_volume 2094(2) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7511 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.9 _exptl_crystal_description sheet _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 1.653 _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 1.881 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7048 _exptl_absorpt_correction_T_max 0.7048 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16796 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.1301 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7365 _reflns_number_gt 6216 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7365 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Dy1 Dy 0.27687(3) 0.28143(3) 0.26399(2) 0.02840(11) Uani 1 1 d . . . F1 F 0.3446(4) -0.0056(4) 0.4788(3) 0.0555(14) Uani 1 1 d . . . F2 F 0.3160(7) 0.1556(6) 0.5401(3) 0.119(3) Uani 1 1 d . . . F3 F 0.4746(5) 0.1572(5) 0.4913(4) 0.120(3) Uani 1 1 d . . . F4 F 0.4762(7) 0.4970(5) 0.1053(5) 0.124(3) Uani 1 1 d . . . F5 F 0.6273(5) 0.4366(6) 0.1029(4) 0.107(2) Uani 1 1 d . . . F6 F 0.4670(6) 0.3529(5) 0.0010(3) 0.102(2) Uani 1 1 d . . . F7 F 0.3142(5) 0.7079(4) 0.3647(3) 0.0606(15) Uani 1 1 d . . . F8 F 0.2139(4) 0.7243(4) 0.2463(3) 0.0707(19) Uani 1 1 d . . . F9 F 0.3895(4) 0.6966(4) 0.2562(3) 0.0593(15) Uani 1 1 d . . . O1 O 0.3080(4) 0.2149(4) 0.3838(3) 0.0290(12) Uani 1 1 d . . . O2 O 0.1389(4) 0.0888(4) 0.2199(3) 0.0294(12) Uani 1 1 d . . . O3 O 0.3617(4) 0.3229(4) 0.1538(3) 0.0343(13) Uani 1 1 d . . . O4 O 0.4031(4) 0.1604(4) 0.2339(3) 0.0320(12) Uani 1 1 d . . . O5 O 0.2948(4) 0.4797(4) 0.2811(3) 0.0289(12) Uani 1 1 d . . . O6 O 0.1068(4) 0.2792(4) 0.1615(3) 0.0297(12) Uani 1 1 d . . . O7 O 0.1456(4) 0.3486(4) 0.3485(3) 0.0296(12) Uani 1 1 d . . . O8 O 0.0601(5) 0.3185(5) 0.6070(3) 0.0425(15) Uani 1 1 d . . . N1 N 0.0894(5) 0.3201(5) 0.4035(4) 0.0288(15) Uani 1 1 d . . . N2 N 0.0480(5) 0.3042(6) 0.5259(4) 0.0328(16) Uani 1 1 d . . . N3 N 0.4961(5) 0.4185(5) 0.3613(3) 0.0275(14) Uani 1 1 d . . . C1 C 0.3547(9) 0.1038(7) 0.4746(6) 0.053(3) Uani 1 1 d . . . C2 C 0.2832(6) 0.1087(6) 0.3873(5) 0.0294(17) Uani 1 1 d . . . C3 C 0.1989(6) 0.0044(7) 0.3294(5) 0.035(2) Uani 1 1 d . . . H3 H 0.1905 -0.0658 0.3433 0.042 Uiso 1 1 calc R . . C4 C 0.1232(6) 0.0008(6) 0.2482(5) 0.0265(17) Uani 1 1 d . . . C5 C 0.0189(6) -0.1125(6) 0.1954(5) 0.0272(17) Uani 1 1 d . . . C6 C -0.0226(6) -0.2027(7) 0.2294(5) 0.036(2) Uani 1 1 d . . . H6 H 0.0139 -0.1943 0.2872 0.044 Uiso 1 1 calc R . . C7 C -0.1178(7) -0.3045(7) 0.1776(5) 0.041(2) Uani 1 1 d . . . H7 H -0.1466 -0.3640 0.2011 0.049 Uiso 1 1 calc R . . C8 C -0.1710(7) -0.3193(7) 0.0907(5) 0.042(2) Uani 1 1 d . . . H8 H -0.2334 -0.3895 0.0556 0.050 Uiso 1 1 calc R . . C9 C -0.1313(7) -0.2293(7) 0.0557(5) 0.039(2) Uani 1 1 d . . . H9 H -0.1679 -0.2387 -0.0024 0.047 Uiso 1 1 calc R . . C10 C -0.0358(6) -0.1242(6) 0.1084(4) 0.0327(19) Uani 1 1 d . . . H10 H -0.0091 -0.0631 0.0859 0.039 Uiso 1 1 calc R . . C11 C 0.5063(8) 0.3988(8) 0.0854(6) 0.045(2) Uani 1 1 d . . . C12 C 0.4594(7) 0.3146(7) 0.1335(5) 0.0336(19) Uani 1 1 d . . . C13 C 0.5227(7) 0.2391(6) 0.1491(5) 0.038(2) Uani 1 1 d . . . H13 H 0.5930 0.2414 0.1296 0.046 Uiso 1 1 calc R . . C14 C 0.4870(6) 0.1570(6) 0.1936(5) 0.0316(19) Uani 1 1 d . . . C15 C 0.5463(6) 0.0620(7) 0.1949(5) 0.0311(18) Uani 1 1 d . . . C16 C 0.5463(6) 0.0115(6) 0.2622(5) 0.0345(19) Uani 1 1 d . . . H16 H 0.5107 0.0384 0.3063 0.041 Uiso 1 1 calc R . . C17 C 0.5995(7) -0.0788(7) 0.2636(5) 0.042(2) Uani 1 1 d . . . H17 H 0.6022 -0.1100 0.3096 0.051 Uiso 1 1 calc R . . C18 C 0.6487(7) -0.1223(7) 0.1957(5) 0.048(2) Uani 1 1 d . . . H18 H 0.6825 -0.1839 0.1958 0.058 Uiso 1 1 calc R . . C19 C 0.6471(7) -0.0732(7) 0.1274(5) 0.048(2) Uani 1 1 d . . . H19 H 0.6798 -0.1020 0.0821 0.058 Uiso 1 1 calc R . . C20 C 0.5966(7) 0.0185(7) 0.1279(5) 0.040(2) Uani 1 1 d . . . H20 H 0.5963 0.0514 0.0829 0.048 Uiso 1 1 calc R . . C21 C 0.2840(7) 0.6659(7) 0.2776(5) 0.0351(19) Uani 1 1 d . . . C22 C 0.2268(7) 0.5308(7) 0.2445(5) 0.0314(18) Uani 1 1 d . . . C23 C 0.1164(7) 0.4796(7) 0.1808(5) 0.0348(19) Uani 1 1 d . . . H23 H 0.0766 0.5298 0.1621 0.042 Uiso 1 1 calc R . . C24 C 0.0587(6) 0.3542(7) 0.1414(4) 0.0301(18) Uani 1 1 d . . . C25 C -0.0625(6) 0.3055(7) 0.0708(4) 0.0332(19) Uani 1 1 d . . . C26 C -0.1142(7) 0.3764(7) 0.0309(5) 0.044(2) Uani 1 1 d . . . H26 H -0.0740 0.4583 0.0488 0.053 Uiso 1 1 calc R . . C27 C -0.2244(7) 0.3267(7) -0.0350(5) 0.051(2) Uani 1 1 d . . . H27 H -0.2587 0.3751 -0.0607 0.061 Uiso 1 1 calc R . . C28 C -0.2838(7) 0.2047(7) -0.0626(5) 0.048(2) Uani 1 1 d . . . H28 H -0.3568 0.1711 -0.1080 0.058 Uiso 1 1 calc R . . C29 C -0.2352(7) 0.1316(7) -0.0230(5) 0.039(2) Uani 1 1 d . . . H29 H -0.2768 0.0501 -0.0404 0.047 Uiso 1 1 calc R . . C30 C -0.1239(7) 0.1820(7) 0.0427(5) 0.0350(19) Uani 1 1 d . . . H30 H -0.0897 0.1336 0.0683 0.042 Uiso 1 1 calc R . . C31 C -0.0489(6) 0.2647(6) 0.3768(5) 0.0276(17) Uani 1 1 d . . . C32 C -0.0683(6) 0.2230(6) 0.4547(5) 0.0300(18) Uani 1 1 d . . . C33 C -0.0933(6) 0.1681(6) 0.2877(4) 0.039(2) Uani 1 1 d . . . H33A H -0.0734 0.2029 0.2442 0.059 Uiso 1 1 calc R . . H33B H -0.1813 0.1318 0.2730 0.059 Uiso 1 1 calc R . . H33C H -0.0533 0.1084 0.2897 0.059 Uiso 1 1 calc R . . C34 C -0.1000(6) 0.3683(6) 0.3702(5) 0.0354(19) Uani 1 1 d . . . H34A H -0.0699 0.4307 0.4259 0.053 Uiso 1 1 calc R . . H34B H -0.1888 0.3396 0.3539 0.053 Uiso 1 1 calc R . . H34C H -0.0732 0.3990 0.3266 0.053 Uiso 1 1 calc R . . C35 C -0.0626(6) 0.0956(6) 0.4447(5) 0.042(2) Uani 1 1 d . . . H35A H 0.0109 0.0880 0.4285 0.063 Uiso 1 1 calc R . . H35B H -0.1341 0.0388 0.3999 0.063 Uiso 1 1 calc R . . H35C H -0.0609 0.0805 0.4993 0.063 Uiso 1 1 calc R . . C36 C -0.1804(6) 0.2375(6) 0.4858(5) 0.042(2) Uani 1 1 d . . . H36A H -0.1786 0.2153 0.5378 0.064 Uiso 1 1 calc R . . H36B H -0.2547 0.1871 0.4407 0.064 Uiso 1 1 calc R . . H36C H -0.1787 0.3194 0.4985 0.064 Uiso 1 1 calc R . . C37 C 0.1381(6) 0.3515(6) 0.4910(5) 0.0277(17) Uani 1 1 d . . . C38 C 0.2642(6) 0.4286(6) 0.5403(4) 0.0272(17) Uani 1 1 d . . . C39 C 0.3232(6) 0.4173(6) 0.6194(4) 0.0322(18) Uani 1 1 d . . . H39 H 0.2842 0.3599 0.6413 0.039 Uiso 1 1 calc R . . C40 C 0.3271(6) 0.5164(6) 0.5116(4) 0.0285(18) Uani 1 1 d . . . H40 H 0.2915 0.5248 0.4586 0.034 Uiso 1 1 calc R . . C41 C 0.5555(6) 0.4077(6) 0.4371(4) 0.0283(17) Uani 1 1 d . . . H41 H 0.5160 0.3467 0.4557 0.034 Uiso 1 1 calc R . . C42 C 0.5579(6) 0.5052(6) 0.3361(4) 0.0316(19) Uani 1 1 d . . . H42 H 0.5183 0.5146 0.2846 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0247(2) 0.0282(2) 0.02518(19) 0.00638(17) 0.00149(14) 0.00269(15) F1 0.060(3) 0.036(3) 0.057(3) 0.024(3) -0.013(3) 0.005(2) F2 0.252(9) 0.097(5) 0.028(3) 0.018(3) 0.014(4) 0.111(6) F3 0.074(4) 0.106(5) 0.135(6) 0.096(5) -0.060(4) -0.039(4) F4 0.220(8) 0.077(5) 0.177(7) 0.090(5) 0.161(6) 0.090(5) F5 0.043(4) 0.146(6) 0.146(6) 0.112(5) 0.014(4) -0.004(4) F6 0.144(6) 0.080(5) 0.037(3) 0.026(3) -0.002(4) -0.030(4) F7 0.084(4) 0.036(3) 0.039(3) -0.005(3) 0.009(3) 0.004(3) F8 0.060(4) 0.033(3) 0.090(4) 0.002(3) -0.024(3) 0.017(3) F9 0.053(3) 0.041(3) 0.080(4) 0.024(3) 0.024(3) 0.000(3) O1 0.030(3) 0.023(3) 0.029(3) 0.007(2) 0.003(2) 0.004(2) O2 0.025(3) 0.027(3) 0.028(3) 0.000(2) 0.002(2) 0.008(2) O3 0.029(3) 0.044(3) 0.032(3) 0.019(3) 0.007(2) 0.009(3) O4 0.027(3) 0.037(3) 0.030(3) 0.011(3) 0.008(2) 0.007(2) O5 0.030(3) 0.021(3) 0.033(3) 0.010(2) 0.006(2) 0.003(2) O6 0.025(3) 0.037(3) 0.020(3) 0.007(2) -0.002(2) 0.007(2) O7 0.031(3) 0.031(3) 0.023(3) 0.007(2) 0.005(2) 0.008(2) O8 0.039(3) 0.057(4) 0.025(3) 0.015(3) 0.004(2) 0.005(3) N1 0.024(3) 0.030(4) 0.026(3) 0.004(3) 0.001(3) 0.006(3) N2 0.019(3) 0.040(4) 0.030(3) 0.011(3) 0.000(3) -0.001(3) N3 0.026(3) 0.027(4) 0.020(3) 0.007(3) -0.002(2) 0.000(3) C1 0.069(7) 0.024(5) 0.040(5) 0.006(4) -0.020(5) 0.000(4) C2 0.025(4) 0.027(4) 0.036(4) 0.018(4) 0.006(3) 0.004(3) C3 0.030(4) 0.029(5) 0.036(4) 0.007(4) -0.003(3) 0.006(3) C4 0.026(4) 0.023(4) 0.029(4) 0.009(4) 0.008(3) 0.005(3) C5 0.024(4) 0.024(4) 0.027(4) 0.006(3) 0.001(3) 0.003(3) C6 0.026(4) 0.040(5) 0.031(4) 0.008(4) -0.005(3) 0.005(4) C7 0.033(5) 0.035(5) 0.043(5) 0.006(4) 0.004(4) 0.003(4) C8 0.039(5) 0.023(5) 0.043(5) -0.005(4) 0.001(4) 0.000(4) C9 0.038(5) 0.038(5) 0.035(5) 0.006(4) 0.012(4) 0.007(4) C10 0.037(4) 0.025(4) 0.029(4) 0.003(4) 0.008(3) 0.005(3) C11 0.041(5) 0.050(6) 0.044(5) 0.020(5) 0.012(4) 0.008(5) C12 0.031(4) 0.034(5) 0.031(4) 0.012(4) 0.006(3) 0.001(4) C13 0.038(5) 0.033(5) 0.041(5) 0.010(4) 0.007(4) 0.013(4) C14 0.030(4) 0.025(4) 0.030(4) 0.001(4) -0.001(3) 0.008(3) C15 0.025(4) 0.032(5) 0.032(4) 0.010(4) 0.003(3) 0.006(3) C16 0.031(4) 0.035(5) 0.030(4) 0.009(4) 0.002(3) 0.007(4) C17 0.031(5) 0.039(5) 0.044(5) 0.011(4) -0.006(4) 0.005(4) C18 0.032(5) 0.036(5) 0.059(6) 0.001(5) -0.002(4) 0.009(4) C19 0.043(5) 0.052(6) 0.043(5) 0.006(5) 0.007(4) 0.016(5) C20 0.037(5) 0.046(6) 0.039(5) 0.011(4) 0.007(4) 0.019(4) C21 0.032(4) 0.033(5) 0.035(4) 0.010(4) 0.001(3) 0.009(4) C22 0.035(4) 0.025(4) 0.026(4) 0.002(4) 0.007(3) 0.005(3) C23 0.036(5) 0.030(5) 0.034(4) 0.008(4) 0.003(4) 0.010(4) C24 0.020(4) 0.042(5) 0.022(4) 0.007(4) 0.003(3) 0.004(3) C25 0.025(4) 0.044(5) 0.023(4) 0.005(4) 0.002(3) 0.009(4) C26 0.035(5) 0.044(5) 0.043(5) 0.017(4) -0.005(4) 0.004(4) C27 0.043(5) 0.040(5) 0.056(6) 0.020(5) -0.011(4) 0.005(4) C28 0.038(5) 0.049(6) 0.035(5) 0.007(5) -0.006(4) -0.004(4) C29 0.031(4) 0.042(5) 0.031(4) 0.008(4) 0.002(3) -0.001(4) C30 0.035(5) 0.034(5) 0.029(4) 0.009(4) 0.003(3) 0.005(4) C31 0.024(4) 0.023(4) 0.028(4) 0.003(3) 0.001(3) 0.003(3) C32 0.017(4) 0.028(4) 0.037(4) 0.009(4) 0.001(3) 0.001(3) C33 0.021(4) 0.036(5) 0.042(5) -0.002(4) 0.002(3) -0.002(3) C34 0.029(4) 0.035(5) 0.038(4) 0.015(4) 0.001(3) 0.007(4) C35 0.038(5) 0.038(5) 0.042(5) 0.008(4) 0.006(4) 0.007(4) C36 0.027(4) 0.051(6) 0.045(5) 0.016(4) 0.006(4) 0.008(4) C37 0.029(4) 0.022(4) 0.028(4) 0.009(3) 0.004(3) 0.004(3) C38 0.026(4) 0.022(4) 0.029(4) 0.005(3) 0.006(3) 0.007(3) C39 0.030(4) 0.035(5) 0.027(4) 0.009(4) 0.007(3) 0.003(3) C40 0.023(4) 0.032(5) 0.024(4) 0.005(3) -0.002(3) 0.008(3) C41 0.028(4) 0.019(4) 0.035(4) 0.007(4) 0.005(3) 0.006(3) C42 0.036(4) 0.028(5) 0.023(4) 0.000(4) 0.006(3) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O5 2.314(5) . ? Dy1 O1 2.316(5) . ? Dy1 O6 2.320(4) . ? Dy1 O2 2.327(5) . ? Dy1 O3 2.332(5) . ? Dy1 O4 2.356(4) . ? Dy1 O7 2.406(4) . ? Dy1 N3 2.596(5) . ? F1 C1 1.332(9) . ? F2 C1 1.319(11) . ? F3 C1 1.321(11) . ? F4 C11 1.309(9) . ? F5 C11 1.312(9) . ? F6 C11 1.292(9) . ? F7 C21 1.330(8) . ? F8 C21 1.322(8) . ? F9 C21 1.332(8) . ? O1 C2 1.276(8) . ? O2 C4 1.266(8) . ? O3 C12 1.265(8) . ? O4 C14 1.285(8) . ? O5 C22 1.274(8) . ? O6 C24 1.263(8) . ? O7 N1 1.284(7) . ? O8 N2 1.273(7) . ? N1 C37 1.349(8) . ? N1 C31 1.504(8) . ? N2 C37 1.367(9) . ? N2 C32 1.513(8) . ? N3 C42 1.333(9) . ? N3 C41 1.355(8) . ? C1 C2 1.533(10) . ? C2 C3 1.368(9) . ? C3 C4 1.430(9) . ? C3 H3 0.9300 . ? C4 C5 1.505(9) . ? C5 C6 1.385(10) . ? C5 C10 1.400(9) . ? C6 C7 1.376(9) . ? C6 H6 0.9300 . ? C7 C8 1.385(10) . ? C7 H7 0.9300 . ? C8 C9 1.390(10) . ? C8 H8 0.9300 . ? C9 C10 1.402(9) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.514(11) . ? C12 C13 1.355(9) . ? C13 C14 1.417(10) . ? C13 H13 0.9300 . ? C14 C15 1.490(9) . ? C15 C20 1.392(9) . ? C15 C16 1.400(10) . ? C16 C17 1.393(9) . ? C16 H16 0.9300 . ? C17 C18 1.396(10) . ? C17 H17 0.9300 . ? C18 C19 1.403(11) . ? C18 H18 0.9300 . ? C19 C20 1.384(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.518(10) . ? C22 C23 1.366(9) . ? C23 C24 1.420(9) . ? C23 H23 0.9300 . ? C24 C25 1.505(8) . ? C25 C26 1.391(10) . ? C25 C30 1.403(9) . ? C26 C27 1.381(9) . ? C26 H26 0.9300 . ? C27 C28 1.385(10) . ? C27 H27 0.9300 . ? C28 C29 1.393(10) . ? C28 H28 0.9300 . ? C29 C30 1.388(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C33 1.519(8) . ? C31 C32 1.531(10) . ? C31 C34 1.542(8) . ? C32 C36 1.523(8) . ? C32 C35 1.540(9) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.463(9) . ? C38 C40 1.385(9) . ? C38 C39 1.404(9) . ? C39 C42 1.390(9) 2_666 ? C39 H39 0.9300 . ? C40 C41 1.394(8) 2_666 ? C40 H40 0.9300 . ? C41 C40 1.394(8) 2_666 ? C41 H41 0.9300 . ? C42 C39 1.390(9) 2_666 ? C42 H42 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 O5 Dy1 O1 121.37(16) . . ? O5 Dy1 O6 74.09(16) . . ? O1 Dy1 O6 135.91(17) . . ? O5 Dy1 O2 144.84(15) . . ? O1 Dy1 O2 73.68(16) . . ? O6 Dy1 O2 74.48(17) . . ? O5 Dy1 O3 74.68(16) . . ? O1 Dy1 O3 143.90(16) . . ? O6 Dy1 O3 77.44(17) . . ? O2 Dy1 O3 113.04(16) . . ? O5 Dy1 O4 134.93(17) . . ? O1 Dy1 O4 76.26(16) . . ? O6 Dy1 O4 124.41(15) . . ? O2 Dy1 O4 77.14(16) . . ? O3 Dy1 O4 71.32(17) . . ? O5 Dy1 O7 68.73(16) . . ? O1 Dy1 O7 74.29(16) . . ? O6 Dy1 O7 75.04(16) . . ? O2 Dy1 O7 88.23(16) . . ? O3 Dy1 O7 138.84(17) . . ? O4 Dy1 O7 149.78(17) . . ? O5 Dy1 N3 69.67(17) . . ? O1 Dy1 N3 76.04(18) . . ? O6 Dy1 N3 141.68(19) . . ? O2 Dy1 N3 143.74(17) . . ? O3 Dy1 N3 81.38(18) . . ? O4 Dy1 N3 76.69(17) . . ? O7 Dy1 N3 102.34(16) . . ? C2 O1 Dy1 130.1(5) . . ? C4 O2 Dy1 136.9(5) . . ? C12 O3 Dy1 133.3(5) . . ? C14 O4 Dy1 137.0(5) . . ? C22 O5 Dy1 133.1(5) . . ? C24 O6 Dy1 137.6(4) . . ? N1 O7 Dy1 139.6(4) . . ? O7 N1 C37 126.5(6) . . ? O7 N1 C31 120.8(6) . . ? C37 N1 C31 111.8(6) . . ? O8 N2 C37 125.7(6) . . ? O8 N2 C32 122.9(6) . . ? C37 N2 C32 111.2(6) . . ? C42 N3 C41 116.1(6) . . ? C42 N3 Dy1 119.3(5) . . ? C41 N3 Dy1 124.6(5) . . ? F2 C1 F3 108.8(8) . . ? F2 C1 F1 104.9(9) . . ? F3 C1 F1 105.3(8) . . ? F2 C1 C2 111.2(8) . . ? F3 C1 C2 110.8(9) . . ? F1 C1 C2 115.3(7) . . ? O1 C2 C3 130.3(7) . . ? O1 C2 C1 112.2(7) . . ? C3 C2 C1 117.3(7) . . ? C2 C3 C4 121.6(8) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? O2 C4 C3 122.9(7) . . ? O2 C4 C5 119.0(6) . . ? C3 C4 C5 118.0(7) . . ? C6 C5 C10 120.3(7) . . ? C6 C5 C4 122.8(7) . . ? C10 C5 C4 116.8(7) . . ? C7 C6 C5 120.1(7) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.5(8) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 120.2(8) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C8 C9 C10 119.7(8) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C5 C10 C9 119.2(8) . . ? C5 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? F6 C11 F4 105.9(8) . . ? F6 C11 F5 104.9(8) . . ? F4 C11 F5 104.2(8) . . ? F6 C11 C12 114.1(8) . . ? F4 C11 C12 113.1(7) . . ? F5 C11 C12 113.7(7) . . ? O3 C12 C13 127.2(8) . . ? O3 C12 C11 114.3(7) . . ? C13 C12 C11 118.5(7) . . ? C12 C13 C14 123.1(7) . . ? C12 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? O4 C14 C13 122.2(7) . . ? O4 C14 C15 117.3(7) . . ? C13 C14 C15 120.5(7) . . ? C20 C15 C16 119.3(7) . . ? C20 C15 C14 121.1(7) . . ? C16 C15 C14 119.6(7) . . ? C17 C16 C15 120.3(7) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 119.8(8) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C19 120.0(8) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.6(8) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C15 121.0(8) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? F8 C21 F7 108.1(6) . . ? F8 C21 F9 106.7(7) . . ? F7 C21 F9 105.8(6) . . ? F8 C21 C22 114.8(6) . . ? F7 C21 C22 110.9(7) . . ? F9 C21 C22 110.0(6) . . ? O5 C22 C23 128.6(7) . . ? O5 C22 C21 112.1(6) . . ? C23 C22 C21 119.3(7) . . ? C22 C23 C24 123.9(7) . . ? C22 C23 H23 118.0 . . ? C24 C23 H23 118.0 . . ? O6 C24 C23 122.5(6) . . ? O6 C24 C25 117.1(7) . . ? C23 C24 C25 120.4(7) . . ? C26 C25 C30 118.9(7) . . ? C26 C25 C24 123.1(7) . . ? C30 C25 C24 118.0(7) . . ? C27 C26 C25 120.8(8) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 119.8(8) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 120.7(7) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 119.2(8) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? C29 C30 C25 120.6(7) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? N1 C31 C33 110.8(5) . . ? N1 C31 C32 101.5(5) . . ? C33 C31 C32 116.1(6) . . ? N1 C31 C34 104.7(6) . . ? C33 C31 C34 109.3(6) . . ? C32 C31 C34 113.6(6) . . ? N2 C32 C36 108.9(6) . . ? N2 C32 C31 101.2(6) . . ? C36 C32 C31 117.1(6) . . ? N2 C32 C35 104.9(6) . . ? C36 C32 C35 109.6(6) . . ? C31 C32 C35 114.0(6) . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 H36A 109.5 . . ? C32 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C32 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 N2 108.4(6) . . ? N1 C37 C38 125.6(7) . . ? N2 C37 C38 125.9(7) . . ? C40 C38 C39 118.2(7) . . ? C40 C38 C37 121.1(7) . . ? C39 C38 C37 120.6(7) . . ? C42 C39 C38 117.8(7) 2_666 . ? C42 C39 H39 121.1 2_666 . ? C38 C39 H39 121.1 . . ? C38 C40 C41 119.4(7) . 2_666 ? C38 C40 H40 120.3 . . ? C41 C40 H40 120.3 2_666 . ? N3 C41 C40 123.3(7) . 2_666 ? N3 C41 H41 118.4 . . ? C40 C41 H41 118.4 2_666 . ? N3 C42 C39 125.2(7) . 2_666 ? N3 C42 H42 117.4 . . ? C39 C42 H42 117.4 2_666 . ? 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 O5 Dy1 O1 C2 167.3(5) . . . . ? O6 Dy1 O1 C2 67.6(6) . . . . ? O2 Dy1 O1 C2 22.3(6) . . . . ? O3 Dy1 O1 C2 -84.6(6) . . . . ? O4 Dy1 O1 C2 -58.1(6) . . . . ? O7 Dy1 O1 C2 115.1(6) . . . . ? N3 Dy1 O1 C2 -137.5(6) . . . . ? O5 Dy1 O2 C4 -135.2(6) . . . . ? O1 Dy1 O2 C4 -13.5(6) . . . . ? O6 Dy1 O2 C4 -162.6(6) . . . . ? O3 Dy1 O2 C4 128.7(6) . . . . ? O4 Dy1 O2 C4 65.7(6) . . . . ? O7 Dy1 O2 C4 -87.6(6) . . . . ? N3 Dy1 O2 C4 21.0(7) . . . . ? O5 Dy1 O3 C12 123.6(7) . . . . ? O1 Dy1 O3 C12 0.9(8) . . . . ? O6 Dy1 O3 C12 -159.7(7) . . . . ? O2 Dy1 O3 C12 -92.8(7) . . . . ? O4 Dy1 O3 C12 -26.4(6) . . . . ? O7 Dy1 O3 C12 151.3(6) . . . . ? N3 Dy1 O3 C12 52.4(6) . . . . ? O5 Dy1 O4 C14 -28.1(7) . . . . ? O1 Dy1 O4 C14 -149.0(6) . . . . ? O6 Dy1 O4 C14 74.2(7) . . . . ? O2 Dy1 O4 C14 135.0(6) . . . . ? O3 Dy1 O4 C14 14.9(6) . . . . ? O7 Dy1 O4 C14 -162.1(6) . . . . ? N3 Dy1 O4 C14 -70.4(6) . . . . ? O1 Dy1 O5 C22 -132.2(6) . . . . ? O6 Dy1 O5 C22 2.3(6) . . . . ? O2 Dy1 O5 C22 -25.1(8) . . . . ? O3 Dy1 O5 C22 83.3(6) . . . . ? O4 Dy1 O5 C22 125.3(6) . . . . ? O7 Dy1 O5 C22 -77.5(6) . . . . ? N3 Dy1 O5 C22 169.6(7) . . . . ? O5 Dy1 O6 C24 -5.9(7) . . . . ? O1 Dy1 O6 C24 113.0(7) . . . . ? O2 Dy1 O6 C24 158.1(7) . . . . ? O3 Dy1 O6 C24 -83.3(7) . . . . ? O4 Dy1 O6 C24 -139.9(6) . . . . ? O7 Dy1 O6 C24 65.7(7) . . . . ? N3 Dy1 O6 C24 -25.3(8) . . . . ? O5 Dy1 O7 N1 -159.3(6) . . . . ? O1 Dy1 O7 N1 -25.7(6) . . . . ? O6 Dy1 O7 N1 122.2(6) . . . . ? O2 Dy1 O7 N1 47.8(6) . . . . ? O3 Dy1 O7 N1 171.9(5) . . . . ? O4 Dy1 O7 N1 -12.5(8) . . . . ? N3 Dy1 O7 N1 -97.2(6) . . . . ? Dy1 O7 N1 C37 84.6(9) . . . . ? Dy1 O7 N1 C31 -107.1(7) . . . . ? O5 Dy1 N3 C42 -46.2(5) . . . . ? O1 Dy1 N3 C42 -177.8(5) . . . . ? O6 Dy1 N3 C42 -26.3(6) . . . . ? O2 Dy1 N3 C42 148.2(4) . . . . ? O3 Dy1 N3 C42 30.6(5) . . . . ? O4 Dy1 N3 C42 103.3(5) . . . . ? O7 Dy1 N3 C42 -107.7(5) . . . . ? O5 Dy1 N3 C41 135.0(5) . . . . ? O1 Dy1 N3 C41 3.4(5) . . . . ? O6 Dy1 N3 C41 154.9(4) . . . . ? O2 Dy1 N3 C41 -30.7(6) . . . . ? O3 Dy1 N3 C41 -148.3(5) . . . . ? O4 Dy1 N3 C41 -75.5(5) . . . . ? O7 Dy1 N3 C41 73.5(5) . . . . ? Dy1 O1 C2 C3 -23.4(12) . . . . ? Dy1 O1 C2 C1 161.9(5) . . . . ? F2 C1 C2 O1 68.3(10) . . . . ? F3 C1 C2 O1 -52.9(10) . . . . ? F1 C1 C2 O1 -172.4(7) . . . . ? F2 C1 C2 C3 -107.2(9) . . . . ? F3 C1 C2 C3 131.7(8) . . . . ? F1 C1 C2 C3 12.1(13) . . . . ? O1 C2 C3 C4 2.4(13) . . . . ? C1 C2 C3 C4 176.9(7) . . . . ? Dy1 O2 C4 C3 2.6(11) . . . . ? Dy1 O2 C4 C5 -178.7(4) . . . . ? C2 C3 C4 O2 8.6(11) . . . . ? C2 C3 C4 C5 -170.2(6) . . . . ? O2 C4 C5 C6 -165.2(6) . . . . ? C3 C4 C5 C6 13.6(10) . . . . ? O2 C4 C5 C10 15.1(9) . . . . ? C3 C4 C5 C10 -166.1(6) . . . . ? C10 C5 C6 C7 0.2(11) . . . . ? C4 C5 C6 C7 -179.6(6) . . . . ? C5 C6 C7 C8 1.5(11) . . . . ? C6 C7 C8 C9 -2.1(11) . . . . ? C7 C8 C9 C10 1.0(11) . . . . ? C6 C5 C10 C9 -1.3(10) . . . . ? C4 C5 C10 C9 178.5(6) . . . . ? C8 C9 C10 C5 0.7(11) . . . . ? Dy1 O3 C12 C13 26.7(12) . . . . ? Dy1 O3 C12 C11 -154.3(5) . . . . ? F6 C11 C12 O3 -92.9(9) . . . . ? F4 C11 C12 O3 28.3(11) . . . . ? F5 C11 C12 O3 146.8(7) . . . . ? F6 C11 C12 C13 86.2(10) . . . . ? F4 C11 C12 C13 -152.6(8) . . . . ? F5 C11 C12 C13 -34.1(11) . . . . ? O3 C12 C13 C14 -1.1(13) . . . . ? C11 C12 C13 C14 179.9(7) . . . . ? Dy1 O4 C14 C13 -2.5(11) . . . . ? Dy1 O4 C14 C15 177.7(4) . . . . ? C12 C13 C14 O4 -10.7(12) . . . . ? C12 C13 C14 C15 169.1(7) . . . . ? O4 C14 C15 C20 153.3(7) . . . . ? C13 C14 C15 C20 -26.5(11) . . . . ? O4 C14 C15 C16 -23.7(10) . . . . ? C13 C14 C15 C16 156.5(7) . . . . ? C20 C15 C16 C17 1.9(11) . . . . ? C14 C15 C16 C17 178.9(6) . . . . ? C15 C16 C17 C18 -2.5(11) . . . . ? C16 C17 C18 C19 1.5(12) . . . . ? C17 C18 C19 C20 0.0(12) . . . . ? C18 C19 C20 C15 -0.6(12) . . . . ? C16 C15 C20 C19 -0.4(11) . . . . ? C14 C15 C20 C19 -177.4(7) . . . . ? Dy1 O5 C22 C23 0.4(12) . . . . ? Dy1 O5 C22 C21 -177.7(4) . . . . ? F8 C21 C22 O5 -175.7(7) . . . . ? F7 C21 C22 O5 -52.8(9) . . . . ? F9 C21 C22 O5 63.9(9) . . . . ? F8 C21 C22 C23 6.0(11) . . . . ? F7 C21 C22 C23 128.9(7) . . . . ? F9 C21 C22 C23 -114.4(8) . . . . ? O5 C22 C23 C24 -2.1(13) . . . . ? C21 C22 C23 C24 175.9(7) . . . . ? Dy1 O6 C24 C23 6.5(11) . . . . ? Dy1 O6 C24 C25 -175.4(4) . . . . ? C22 C23 C24 O6 -1.2(12) . . . . ? C22 C23 C24 C25 -179.3(7) . . . . ? O6 C24 C25 C26 -167.8(7) . . . . ? C23 C24 C25 C26 10.4(11) . . . . ? O6 C24 C25 C30 10.5(10) . . . . ? C23 C24 C25 C30 -171.3(7) . . . . ? C30 C25 C26 C27 0.3(12) . . . . ? C24 C25 C26 C27 178.6(7) . . . . ? C25 C26 C27 C28 -0.8(13) . . . . ? C26 C27 C28 C29 1.7(14) . . . . ? C27 C28 C29 C30 -2.2(13) . . . . ? C28 C29 C30 C25 1.7(11) . . . . ? C26 C25 C30 C29 -0.8(11) . . . . ? C24 C25 C30 C29 -179.2(6) . . . . ? O7 N1 C31 C33 44.3(9) . . . . ? C37 N1 C31 C33 -145.7(6) . . . . ? O7 N1 C31 C32 168.2(6) . . . . ? C37 N1 C31 C32 -21.8(7) . . . . ? O7 N1 C31 C34 -73.4(7) . . . . ? C37 N1 C31 C34 96.6(7) . . . . ? O8 N2 C32 C36 40.9(9) . . . . ? C37 N2 C32 C36 -143.4(6) . . . . ? O8 N2 C32 C31 164.9(6) . . . . ? C37 N2 C32 C31 -19.4(8) . . . . ? O8 N2 C32 C35 -76.3(8) . . . . ? C37 N2 C32 C35 99.4(7) . . . . ? N1 C31 C32 N2 22.8(6) . . . . ? C33 C31 C32 N2 143.1(6) . . . . ? C34 C31 C32 N2 -88.9(6) . . . . ? N1 C31 C32 C36 141.0(6) . . . . ? C33 C31 C32 C36 -98.7(7) . . . . ? C34 C31 C32 C36 29.3(9) . . . . ? N1 C31 C32 C35 -89.2(6) . . . . ? C33 C31 C32 C35 31.1(8) . . . . ? C34 C31 C32 C35 159.0(6) . . . . ? O7 N1 C37 N2 179.5(6) . . . . ? C31 N1 C37 N2 10.2(8) . . . . ? O7 N1 C37 C38 2.6(12) . . . . ? C31 N1 C37 C38 -166.7(6) . . . . ? O8 N2 C37 N1 -177.9(6) . . . . ? C32 N2 C37 N1 6.4(8) . . . . ? O8 N2 C37 C38 -1.0(12) . . . . ? C32 N2 C37 C38 -176.6(6) . . . . ? N1 C37 C38 C40 28.6(11) . . . . ? N2 C37 C38 C40 -147.8(7) . . . . ? N1 C37 C38 C39 -153.0(7) . . . . ? N2 C37 C38 C39 30.6(11) . . . . ? C40 C38 C39 C42 -0.4(10) . . . 2_666 ? C37 C38 C39 C42 -178.8(6) . . . 2_666 ? C39 C38 C40 C41 -1.8(10) . . . 2_666 ? C37 C38 C40 C41 176.5(6) . . . 2_666 ? C42 N3 C41 C40 1.8(10) . . . 2_666 ? Dy1 N3 C41 C40 -179.3(4) . . . 2_666 ? C41 N3 C42 C39 0.7(10) . . . 2_666 ? Dy1 N3 C42 C39 -178.2(5) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.482 _refine_diff_density_min -1.565 _refine_diff_density_rms 0.140 #===END