# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_2 _database_code_depnum_ccdc_archive 'CCDC 909092' #TrackingRef 'web_deposit_cif_file_0_LaureGuenee_1351875343.Compounds_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H25 Eu F18 N4 O7' _chemical_formula_sum 'C34 H25 Eu F18 N4 O7' _chemical_formula_weight 1095.54 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.48340(10) _cell_length_b 18.5861(2) _cell_length_c 20.5491(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.5470(10) _cell_angle_gamma 90.00 _cell_volume 4227.24(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 34581 _cell_measurement_theta_max 29.5212 _cell_measurement_theta_min 1.9792 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3305 _exptl_crystal_size_mid 0.2151 _exptl_crystal_size_min 0.1653 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 1.612 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'SuperNova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 70644 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 29.59 _reflns_number_total 10864 _reflns_number_gt 9429 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 1997)' _computing_publication_material SHELX_ACTA _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. Disorder: One CF3 group is disordered around the 3-fold axes and was refined in two components with refined occupancies 0.54:0.56 and with isotropic ADP. ; _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^)+(0.0552P)^2^+10.0075P] 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 10864 _refine_ls_number_parameters 573 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.737136(14) 0.219464(9) 0.492739(9) 0.02673(6) Uani 1 1 d . . . F1 F 1.1404(3) 0.3159(2) 0.5418(4) 0.131(2) Uani 1 1 d . . . F2 F 1.0930(4) 0.4164(3) 0.4905(3) 0.147(2) Uani 1 1 d . . . F3 F 1.0966(4) 0.3994(4) 0.5886(3) 0.157(3) Uani 1 1 d . . . F7 F 0.9673(4) 0.1412(3) 0.3654(2) 0.1136(16) Uani 1 1 d . . . F8 F 0.9103(4) 0.0398(2) 0.3785(2) 0.1042(14) Uani 1 1 d . . . F9 F 1.0922(3) 0.0657(3) 0.4433(2) 0.1206(19) Uani 1 1 d . . . F10 F 1.0668(3) 0.0864(2) 0.71324(18) 0.0884(11) Uani 1 1 d . . . F11 F 1.1177(3) 0.1962(2) 0.71927(18) 0.0798(10) Uani 1 1 d . . . F12 F 1.2110(3) 0.1162(2) 0.69081(17) 0.0907(12) Uani 1 1 d . . . F13 F 0.4893(4) 0.2254(2) 0.22470(18) 0.0809(10) Uani 1 1 d . . . F14 F 0.3109(3) 0.2115(2) 0.21235(17) 0.0937(13) Uani 1 1 d . . . F15 F 0.4318(3) 0.12280(19) 0.24231(17) 0.0789(10) Uani 1 1 d . . . F16 F 0.2597(4) 0.3368(3) 0.3908(2) 0.153(3) Uani 1 1 d . . . F17 F 0.3428(5) 0.2898(3) 0.4971(3) 0.132(2) Uani 1 1 d . . . F18 F 0.4087(4) 0.3808(2) 0.4748(3) 0.1029(14) Uani 1 1 d . . . O1 O 0.7815(2) 0.32120(14) 0.57272(14) 0.0360(5) Uani 1 1 d . . . O2 O 0.9142(3) 0.28295(14) 0.49980(17) 0.0398(6) Uani 1 1 d . . . O3 O 0.6771(2) 0.32229(14) 0.41149(14) 0.0385(6) Uani 1 1 d . . . O4 O 0.8419(2) 0.14547(14) 0.44530(14) 0.0357(5) Uani 1 1 d . . . O5 O 0.9144(2) 0.17329(14) 0.59501(14) 0.0348(5) Uani 1 1 d . . . O6 O 0.5780(2) 0.18538(14) 0.37333(14) 0.0370(6) Uani 1 1 d . . . O7 O 0.5433(2) 0.26166(15) 0.48074(14) 0.0365(6) Uani 1 1 d . . . N1 N 0.7113(3) 0.20087(16) 0.61071(16) 0.0300(6) Uani 1 1 d . . . N2 N 0.6944(3) 0.38932(18) 0.62554(18) 0.0401(7) Uani 1 1 d . . . N3 N 0.6806(3) 0.09370(16) 0.51844(17) 0.0324(6) Uani 1 1 d . . . N4 N 0.6672(3) 0.00650(17) 0.58978(18) 0.0358(7) Uani 1 1 d . . . C1 C 0.7129(3) 0.1351(2) 0.6381(2) 0.0347(7) Uani 1 1 d . . . C2 C 0.7403(5) 0.1268(3) 0.7115(2) 0.0560(12) Uani 1 1 d . . . H2 H 0.7436 0.0801 0.7313 0.067 Uiso 1 1 calc R . . C3 C 0.7625(6) 0.1869(3) 0.7552(3) 0.0643(14) Uani 1 1 d . . . H3 H 0.7836 0.1818 0.8057 0.077 Uiso 1 1 calc R . . C4 C 0.7540(5) 0.2546(3) 0.7254(2) 0.0488(10) Uani 1 1 d . . . H4 H 0.7652 0.2968 0.7540 0.059 Uiso 1 1 calc R . . C5 C 0.7289(3) 0.2590(2) 0.6528(2) 0.0343(7) Uani 1 1 d . . . C6 C 0.7342(3) 0.3269(2) 0.61429(19) 0.0340(7) Uani 1 1 d . . . C7 C 0.7159(6) 0.4530(2) 0.5906(3) 0.0626(14) Uani 1 1 d . . . H7B H 0.6633 0.4928 0.5908 0.075 Uiso 1 1 calc R . . H7A H 0.6939 0.4416 0.5389 0.075 Uiso 1 1 calc R . . C8 C 0.8457(7) 0.4773(3) 0.6293(4) 0.085(2) Uani 1 1 d . . . H8A H 0.8965 0.4423 0.6207 0.128 Uiso 1 1 calc R . . H8C H 0.8721 0.4810 0.6821 0.128 Uiso 1 1 calc R . . H8B H 0.8530 0.5244 0.6104 0.128 Uiso 1 1 calc R . . C9 C 0.6119(4) 0.3983(2) 0.6577(2) 0.0446(9) Uani 1 1 d . . . H9B H 0.5925 0.3504 0.6704 0.054 Uiso 1 1 calc R . . H9A H 0.5356 0.4201 0.6206 0.054 Uiso 1 1 calc R . . C10 C 0.6638(5) 0.4450(3) 0.7255(3) 0.0606(13) Uani 1 1 d . . . H10B H 0.6867 0.4918 0.7138 0.091 Uiso 1 1 calc R . . H10C H 0.7353 0.4216 0.7641 0.091 Uiso 1 1 calc R . . H10A H 0.6032 0.4519 0.7426 0.091 Uiso 1 1 calc R . . C11 C 0.6880(3) 0.07798(19) 0.5833(2) 0.0324(7) Uani 1 1 d . . . C12 C 0.6556(3) 0.02912(19) 0.4803(2) 0.0339(7) Uani 1 1 d . . . C13 C 0.6418(3) 0.0136(2) 0.4103(2) 0.0379(8) Uani 1 1 d . . . H13 H 0.6493 0.0501 0.3803 0.045 Uiso 1 1 calc R . . C14 C 0.6168(4) -0.0565(2) 0.3866(3) 0.0469(10) Uani 1 1 d . . . H14 H 0.6064 -0.0687 0.3392 0.056 Uiso 1 1 calc R . . C15 C 0.6064(4) -0.1103(2) 0.4310(3) 0.0510(11) Uani 1 1 d . . . H15 H 0.5890 -0.1581 0.4126 0.061 Uiso 1 1 calc R . . C16 C 0.6205(4) -0.0964(2) 0.5006(3) 0.0470(10) Uani 1 1 d . . . H16 H 0.6131 -0.1331 0.5304 0.056 Uiso 1 1 calc R . . C17 C 0.6460(3) -0.0255(2) 0.5244(2) 0.0372(8) Uani 1 1 d . . . C18 C 0.6711(4) -0.0341(2) 0.6517(2) 0.0444(9) Uani 1 1 d . . . H18A H 0.6154 -0.0756 0.6329 0.053 Uiso 1 1 calc R . . H18B H 0.6427 -0.0030 0.6797 0.053 Uiso 1 1 calc R . . C19 C 0.7979(5) -0.0612(3) 0.7028(3) 0.0670(15) Uani 1 1 d . . . H19A H 0.8237 -0.0952 0.6763 0.101 Uiso 1 1 calc R . . H19C H 0.7975 -0.0854 0.7450 0.101 Uiso 1 1 calc R . . H19B H 0.8540 -0.0204 0.7199 0.101 Uiso 1 1 calc R . . C20 C 0.7262(4) 0.3807(2) 0.4112(2) 0.0406(9) Uani 1 1 d . A . C21 C 0.8468(4) 0.3977(2) 0.4456(2) 0.0452(9) Uani 1 1 d . . . H21 H 0.8721 0.4448 0.4411 0.054 Uiso 1 1 calc R . . C22 C 0.9329(4) 0.3456(2) 0.4874(2) 0.0396(8) Uani 1 1 d . . . C23 C 1.0666(5) 0.3680(3) 0.5236(4) 0.0630(14) Uani 1 1 d . . . C24 C 0.6355(5) 0.4387(3) 0.3641(3) 0.0607(13) Uani 1 1 d D . . F4A F 0.6912(7) 0.4867(4) 0.3386(4) 0.0792(8) Uiso 0.463(4) 1 d PD A 1 F5A F 0.5925(8) 0.4722(4) 0.3989(4) 0.0792(8) Uiso 0.463(4) 1 d PD A 1 F6A F 0.5507(7) 0.4089(4) 0.3013(4) 0.0792(8) Uiso 0.463(4) 1 d PD A 1 F4B F 0.6707(6) 0.5060(4) 0.3878(4) 0.0792(8) Uiso 0.537(4) 1 d PD A 2 F5B F 0.5369(6) 0.4395(4) 0.3807(4) 0.0792(8) Uiso 0.537(4) 1 d PD A 2 F6B F 0.5892(7) 0.4285(4) 0.2969(4) 0.0792(8) Uiso 0.537(4) 1 d PD A 2 C25 C 0.9488(3) 0.1238(2) 0.4728(2) 0.0395(8) Uani 1 1 d . . . C26 C 1.0353(3) 0.1220(2) 0.5463(2) 0.0422(9) Uani 1 1 d . . . H26 H 1.1139 0.1044 0.5589 0.051 Uiso 1 1 calc R . . C27 C 1.0090(3) 0.14524(19) 0.6014(2) 0.0345(7) Uani 1 1 d . . . C28 C 1.1035(4) 0.1358(3) 0.6817(2) 0.0519(11) Uani 1 1 d . . . C29 C 0.9866(5) 0.0956(4) 0.4163(3) 0.0708(17) Uani 1 1 d . . . C30 C 0.4752(3) 0.2106(2) 0.3340(2) 0.0360(8) Uani 1 1 d . . . C31 C 0.4029(3) 0.2521(2) 0.3547(2) 0.0408(8) Uani 1 1 d . . . H31 H 0.3243 0.2656 0.3187 0.049 Uiso 1 1 calc R . . C33 C 0.3579(4) 0.3185(3) 0.4452(3) 0.0544(12) Uani 1 1 d . . . C32 C 0.4439(3) 0.2739(2) 0.4271(2) 0.0367(8) Uani 1 1 d . . . C34 C 0.4252(4) 0.1928(3) 0.2523(2) 0.0519(11) 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 Eu1 0.02443(10) 0.02713(10) 0.02853(10) 0.00337(6) 0.01217(7) 0.00344(6) F1 0.045(2) 0.086(3) 0.239(6) 0.015(3) 0.048(3) -0.0066(19) F2 0.075(3) 0.175(5) 0.159(5) 0.080(4) 0.028(3) -0.052(3) F3 0.080(3) 0.242(7) 0.130(4) -0.085(5) 0.033(3) -0.059(4) F7 0.136(4) 0.154(4) 0.094(3) 0.032(3) 0.091(3) 0.045(3) F8 0.095(3) 0.116(3) 0.080(2) -0.044(2) 0.022(2) 0.029(2) F9 0.0534(19) 0.225(5) 0.072(2) -0.033(3) 0.0191(17) 0.063(3) F10 0.090(3) 0.103(3) 0.0530(18) 0.0338(18) 0.0165(17) 0.008(2) F11 0.0518(18) 0.094(2) 0.0577(18) -0.0281(17) -0.0050(14) 0.0081(17) F12 0.0407(16) 0.151(4) 0.0559(18) -0.004(2) 0.0016(14) 0.0413(19) F13 0.099(3) 0.103(3) 0.0519(18) 0.0010(16) 0.0451(19) -0.009(2) F14 0.0549(19) 0.156(4) 0.0398(16) -0.0178(18) -0.0039(14) 0.031(2) F15 0.091(2) 0.072(2) 0.0584(18) -0.0275(16) 0.0220(17) -0.0061(18) F16 0.071(3) 0.248(6) 0.086(3) -0.058(3) -0.009(2) 0.098(3) F17 0.165(5) 0.126(4) 0.193(5) 0.056(3) 0.156(5) 0.072(3) F18 0.098(3) 0.082(3) 0.124(3) -0.031(2) 0.047(3) 0.026(2) O1 0.0430(15) 0.0325(13) 0.0362(13) 0.0002(10) 0.0215(12) 0.0008(11) O2 0.0370(14) 0.0329(14) 0.0550(17) 0.0064(11) 0.0260(14) 0.0014(10) O3 0.0402(14) 0.0385(14) 0.0340(13) 0.0081(11) 0.0146(11) 0.0030(11) O4 0.0264(12) 0.0397(14) 0.0381(13) -0.0023(11) 0.0123(11) 0.0052(10) O5 0.0265(12) 0.0400(14) 0.0346(13) 0.0049(10) 0.0114(10) 0.0043(10) O6 0.0306(13) 0.0393(14) 0.0362(13) -0.0010(11) 0.0111(11) 0.0064(11) O7 0.0292(13) 0.0457(15) 0.0331(13) 0.0045(11) 0.0131(11) 0.0091(11) N1 0.0262(14) 0.0337(15) 0.0298(14) 0.0038(11) 0.0125(12) 0.0032(11) N2 0.0496(19) 0.0366(17) 0.0353(16) 0.0004(13) 0.0205(15) 0.0062(14) N3 0.0286(14) 0.0298(14) 0.0377(15) 0.0015(12) 0.0144(13) -0.0013(11) N4 0.0315(15) 0.0318(15) 0.0435(17) 0.0073(13) 0.0168(14) 0.0012(12) C1 0.0331(18) 0.0370(18) 0.0340(18) 0.0067(14) 0.0154(15) 0.0014(14) C2 0.086(4) 0.043(2) 0.041(2) 0.0089(18) 0.031(2) -0.002(2) C3 0.102(4) 0.057(3) 0.035(2) 0.008(2) 0.033(3) 0.000(3) C4 0.066(3) 0.046(2) 0.036(2) -0.0005(17) 0.025(2) 0.001(2) C5 0.0332(18) 0.0362(18) 0.0325(17) 0.0024(14) 0.0143(15) 0.0036(14) C6 0.0338(18) 0.0355(18) 0.0285(16) -0.0014(13) 0.0108(14) -0.0003(14) C7 0.110(5) 0.032(2) 0.065(3) 0.008(2) 0.057(3) 0.015(2) C8 0.136(6) 0.054(3) 0.107(5) -0.028(3) 0.092(5) -0.036(4) C9 0.045(2) 0.049(2) 0.039(2) -0.0046(17) 0.0186(18) 0.0091(18) C10 0.066(3) 0.068(3) 0.046(2) -0.014(2) 0.025(2) 0.008(2) C11 0.0256(16) 0.0330(17) 0.0378(18) 0.0079(14) 0.0140(14) 0.0019(13) C12 0.0225(15) 0.0324(17) 0.0439(19) 0.0001(14) 0.0129(15) 0.0011(13) C13 0.0302(18) 0.0369(19) 0.044(2) -0.0027(15) 0.0151(16) 0.0018(14) C14 0.036(2) 0.047(2) 0.050(2) -0.0099(18) 0.0123(18) 0.0011(17) C15 0.041(2) 0.034(2) 0.068(3) -0.0097(19) 0.017(2) -0.0010(16) C16 0.037(2) 0.0328(19) 0.066(3) 0.0015(18) 0.018(2) -0.0015(16) C17 0.0257(17) 0.0339(18) 0.052(2) 0.0037(16) 0.0174(16) 0.0016(14) C18 0.044(2) 0.039(2) 0.053(2) 0.0151(17) 0.0244(19) 0.0003(17) C19 0.058(3) 0.074(4) 0.066(3) 0.031(3) 0.026(3) 0.020(3) C20 0.054(2) 0.0346(19) 0.0309(18) 0.0064(14) 0.0180(17) 0.0041(17) C21 0.058(3) 0.0332(19) 0.043(2) 0.0053(16) 0.022(2) -0.0053(17) C22 0.044(2) 0.0370(19) 0.045(2) -0.0006(16) 0.0260(18) -0.0049(16) C23 0.047(3) 0.053(3) 0.091(4) 0.005(3) 0.033(3) -0.010(2) C24 0.079(4) 0.047(3) 0.043(2) 0.0151(19) 0.016(2) 0.008(2) C25 0.0292(18) 0.044(2) 0.044(2) -0.0033(16) 0.0158(16) 0.0058(15) C26 0.0281(18) 0.049(2) 0.045(2) -0.0012(17) 0.0127(16) 0.0092(16) C27 0.0263(16) 0.0331(18) 0.0362(18) 0.0034(14) 0.0077(14) -0.0002(13) C28 0.037(2) 0.066(3) 0.040(2) 0.002(2) 0.0063(18) 0.015(2) C29 0.045(3) 0.111(5) 0.050(3) -0.011(3) 0.017(2) 0.031(3) C30 0.0315(18) 0.0386(19) 0.0330(18) 0.0003(14) 0.0108(15) 0.0002(14) C31 0.0278(18) 0.049(2) 0.0366(19) 0.0016(16) 0.0075(15) 0.0078(16) C33 0.042(2) 0.061(3) 0.058(3) -0.002(2) 0.021(2) 0.019(2) C32 0.0287(18) 0.0377(19) 0.041(2) 0.0033(15) 0.0137(16) 0.0053(14) C34 0.045(2) 0.066(3) 0.037(2) -0.003(2) 0.0119(19) 0.004(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 Eu1 O4 2.394(2) . ? Eu1 O1 2.396(3) . ? Eu1 O5 2.397(2) . ? Eu1 O3 2.417(3) . ? Eu1 O6 2.421(3) . ? Eu1 O7 2.445(3) . ? Eu1 O2 2.450(3) . ? Eu1 N3 2.566(3) . ? Eu1 N1 2.612(3) . ? Eu1 C6 3.212(4) . ? F1 C23 1.269(7) . ? F2 C23 1.260(6) . ? F3 C23 1.343(8) . ? F7 C29 1.279(7) . ? F8 C29 1.378(8) . ? F9 C29 1.295(6) . ? F10 C28 1.321(6) . ? F11 C28 1.327(6) . ? F12 C28 1.318(5) . ? F13 C34 1.323(6) . ? F14 C34 1.322(6) . ? F15 C34 1.325(6) . ? F16 C33 1.265(6) . ? F17 C33 1.281(7) . ? F18 C33 1.326(7) . ? O1 C6 1.248(4) . ? O2 C22 1.238(5) . ? O3 C20 1.247(5) . ? O4 C25 1.250(4) . ? O5 C27 1.241(4) . ? O6 C30 1.250(5) . ? O7 C32 1.242(5) . ? N1 C5 1.336(5) . ? N1 C1 1.342(5) . ? N2 C6 1.323(5) . ? N2 C9 1.468(5) . ? N2 C7 1.472(6) . ? N3 C11 1.326(5) . ? N3 C12 1.388(5) . ? N4 C11 1.372(5) . ? N4 C17 1.379(5) . ? N4 C18 1.460(5) . ? C1 C2 1.393(5) . ? C1 C11 1.472(5) . ? C2 C3 1.379(7) . ? C2 H2 0.9500 . ? C3 C4 1.382(7) . ? C3 H3 0.9500 . ? C4 C5 1.377(5) . ? C4 H4 0.9500 . ? C5 C6 1.508(5) . ? C7 C8 1.506(9) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 H8A 0.9800 . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.509(6) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10A 0.9800 . ? C12 C13 1.396(5) . ? C12 C17 1.403(5) . ? C13 C14 1.377(6) . ? C13 H13 0.9500 . ? C14 C15 1.399(7) . ? C14 H14 0.9500 . ? C15 C16 1.382(7) . ? C15 H15 0.9500 . ? C16 C17 1.390(6) . ? C16 H16 0.9500 . ? C18 C19 1.525(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19C 0.9800 . ? C19 H19B 0.9800 . ? C20 C21 1.372(6) . ? C20 C24 1.539(6) . ? C21 C22 1.406(6) . ? C21 H21 0.9500 . ? C22 C23 1.537(6) . ? C24 F6B 1.239(8) . ? C24 F5A 1.242(8) . ? C24 F4B 1.341(8) . ? C24 F6A 1.352(8) . ? C24 F4A 1.375(8) . ? C24 F5B 1.422(8) . ? C25 C26 1.392(5) . ? C25 C29 1.535(6) . ? C26 C27 1.386(6) . ? C26 H26 0.9500 . ? C27 C28 1.532(5) . ? C30 C31 1.394(5) . ? C30 C34 1.531(6) . ? C31 C32 1.392(6) . ? C31 H31 0.9500 . ? C33 C32 1.532(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 O4 Eu1 O1 137.39(9) . . ? O4 Eu1 O5 72.22(9) . . ? O1 Eu1 O5 81.63(9) . . ? O4 Eu1 O3 103.06(9) . . ? O1 Eu1 O3 75.48(10) . . ? O5 Eu1 O3 138.94(9) . . ? O4 Eu1 O6 77.51(9) . . ? O1 Eu1 O6 136.29(9) . . ? O5 Eu1 O6 141.89(9) . . ? O3 Eu1 O6 70.12(9) . . ? O4 Eu1 O7 147.64(9) . . ? O1 Eu1 O7 73.75(9) . . ? O5 Eu1 O7 132.25(9) . . ? O3 Eu1 O7 72.58(9) . . ? O6 Eu1 O7 70.84(9) . . ? O4 Eu1 O2 69.69(9) . . ? O1 Eu1 O2 70.32(9) . . ? O5 Eu1 O2 71.27(9) . . ? O3 Eu1 O2 69.09(9) . . ? O6 Eu1 O2 118.75(10) . . ? O7 Eu1 O2 132.46(9) . . ? O4 Eu1 N3 79.33(9) . . ? O1 Eu1 N3 125.16(9) . . ? O5 Eu1 N3 73.97(9) . . ? O3 Eu1 N3 146.64(9) . . ? O6 Eu1 N3 78.19(9) . . ? O7 Eu1 N3 87.67(9) . . ? O2 Eu1 N3 138.86(9) . . ? O4 Eu1 N1 128.83(9) . . ? O1 Eu1 N1 63.67(9) . . ? O5 Eu1 N1 66.36(9) . . ? O3 Eu1 N1 127.86(9) . . ? O6 Eu1 N1 120.70(9) . . ? O7 Eu1 N1 66.11(9) . . ? O2 Eu1 N1 120.26(10) . . ? N3 Eu1 N1 61.62(10) . . ? O4 Eu1 C6 151.50(9) . . ? O1 Eu1 C6 19.59(9) . . ? O5 Eu1 C6 83.04(9) . . ? O3 Eu1 C6 86.22(9) . . ? O6 Eu1 C6 130.69(9) . . ? O7 Eu1 C6 60.81(9) . . ? O2 Eu1 C6 89.36(10) . . ? N3 Eu1 C6 107.65(10) . . ? N1 Eu1 C6 46.36(9) . . ? C6 O1 Eu1 120.3(2) . . ? C22 O2 Eu1 133.8(3) . . ? C20 O3 Eu1 134.0(3) . . ? C25 O4 Eu1 132.1(2) . . ? C27 O5 Eu1 133.6(2) . . ? C30 O6 Eu1 132.4(2) . . ? C32 O7 Eu1 133.2(3) . . ? C5 N1 C1 119.9(3) . . ? C5 N1 Eu1 116.1(2) . . ? C1 N1 Eu1 121.7(2) . . ? C6 N2 C9 125.2(3) . . ? C6 N2 C7 116.9(3) . . ? C9 N2 C7 116.8(3) . . ? C11 N3 C12 105.7(3) . . ? C11 N3 Eu1 120.7(2) . . ? C12 N3 Eu1 133.0(2) . . ? C11 N4 C17 106.5(3) . . ? C11 N4 C18 130.8(3) . . ? C17 N4 C18 122.7(3) . . ? N1 C1 C2 120.2(4) . . ? N1 C1 C11 112.3(3) . . ? C2 C1 C11 127.4(4) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.8(4) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? N1 C5 C4 122.7(4) . . ? N1 C5 C6 111.8(3) . . ? C4 C5 C6 125.0(4) . . ? O1 C6 N2 122.0(3) . . ? O1 C6 C5 115.9(3) . . ? N2 C6 C5 122.1(3) . . ? O1 C6 Eu1 40.09(17) . . ? N2 C6 Eu1 145.2(3) . . ? C5 C6 Eu1 84.6(2) . . ? N2 C7 C8 112.2(5) . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? H7B C7 H7A 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? N2 C9 C10 112.9(4) . . ? N2 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? N2 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? H9B C9 H9A 107.8 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? N3 C11 N4 112.5(3) . . ? N3 C11 C1 120.1(3) . . ? N4 C11 C1 127.4(3) . . ? N3 C12 C13 130.4(3) . . ? N3 C12 C17 108.9(3) . . ? C13 C12 C17 120.6(3) . . ? C14 C13 C12 117.3(4) . . ? C14 C13 H13 121.3 . . ? C12 C13 H13 121.3 . . ? C13 C14 C15 121.4(4) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 122.3(4) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 116.2(4) . . ? C15 C16 H16 121.9 . . ? C17 C16 H16 121.9 . . ? N4 C17 C16 131.4(4) . . ? N4 C17 C12 106.4(3) . . ? C16 C17 C12 122.2(4) . . ? N4 C18 C19 112.1(4) . . ? N4 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? O3 C20 C21 128.5(4) . . ? O3 C20 C24 113.1(4) . . ? C21 C20 C24 118.3(4) . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? O2 C22 C21 127.6(4) . . ? O2 C22 C23 114.9(4) . . ? C21 C22 C23 117.5(4) . . ? F2 C23 F1 111.6(5) . . ? F2 C23 F3 101.8(6) . . ? F1 C23 F3 102.0(6) . . ? F2 C23 C22 115.3(5) . . ? F1 C23 C22 114.5(4) . . ? F3 C23 C22 109.9(4) . . ? F6B C24 F5A 127.9(7) . . ? F6B C24 F4B 117.0(6) . . ? F5A C24 F4B 58.6(5) . . ? F6B C24 F6A 28.3(4) . . ? F5A C24 F6A 113.5(7) . . ? F4B C24 F6A 135.3(6) . . ? F6B C24 F4A 74.5(5) . . ? F5A C24 F4A 108.9(6) . . ? F4B C24 F4A 52.8(4) . . ? F6A C24 F4A 102.4(6) . . ? F6B C24 F5B 105.0(6) . . ? F5A C24 F5B 37.2(4) . . ? F4B C24 F5B 94.5(5) . . ? F6A C24 F5B 81.4(6) . . ? F4A C24 F5B 137.0(6) . . ? F6B C24 C20 114.9(5) . . ? F5A C24 C20 112.1(5) . . ? F4B C24 C20 113.8(5) . . ? F6A C24 C20 109.6(5) . . ? F4A C24 C20 109.9(5) . . ? F5B C24 C20 108.8(4) . . ? O4 C25 C26 129.0(4) . . ? O4 C25 C29 113.9(4) . . ? C26 C25 C29 117.1(4) . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? O5 C27 C26 128.2(3) . . ? O5 C27 C28 112.5(3) . . ? C26 C27 C28 119.3(3) . . ? F12 C28 F10 107.4(4) . . ? F12 C28 F11 107.3(4) . . ? F10 C28 F11 106.7(4) . . ? F12 C28 C27 114.2(4) . . ? F10 C28 C27 109.8(4) . . ? F11 C28 C27 111.1(4) . . ? F7 C29 F9 113.8(6) . . ? F7 C29 F8 102.6(5) . . ? F9 C29 F8 102.7(5) . . ? F7 C29 C25 112.6(5) . . ? F9 C29 C25 115.5(4) . . ? F8 C29 C25 108.0(5) . . ? O6 C30 C31 128.7(4) . . ? O6 C30 C34 113.9(4) . . ? C31 C30 C34 117.4(4) . . ? C32 C31 C30 121.2(3) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? F16 C33 F17 113.1(6) . . ? F16 C33 F18 103.4(5) . . ? F17 C33 F18 101.8(5) . . ? F16 C33 C32 115.6(4) . . ? F17 C33 C32 111.5(4) . . ? F18 C33 C32 110.1(4) . . ? O7 C32 C31 128.2(4) . . ? O7 C32 C33 114.1(4) . . ? C31 C32 C33 117.8(4) . . ? F14 C34 F13 107.8(4) . . ? F14 C34 F15 106.8(4) . . ? F13 C34 F15 106.8(4) . . ? F14 C34 C30 113.6(4) . . ? F13 C34 C30 110.4(4) . . ? F15 C34 C30 111.1(4) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.827 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.130 data_3 _database_code_depnum_ccdc_archive 'CCDC 909093' #TrackingRef 'web_deposit_cif_file_0_LaureGuenee_1351875343.Compounds_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H50 Eu2 F36 N8 O14' _chemical_formula_sum 'C69 H50 Eu2 F36 N8 O14' _chemical_formula_weight 2203.09 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.9162(8) _cell_length_b 18.3619(8) _cell_length_c 24.8681(9) _cell_angle_alpha 90.00 _cell_angle_beta 122.872(2) _cell_angle_gamma 90.00 _cell_volume 8405.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 58766 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 52.23 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4328 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6376 _exptl_absorpt_correction_T_max 0.8789 _exptl_absorpt_process_details 'XRED; Stoe & Cie, 1999' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'Stoe Ipds' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 74386 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.71 _reflns_number_total 15887 _reflns_number_gt 12085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material Shelxl_ACTA _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. Disorder: Three disordered CF3 units were modelled by refining them in two parts (refined occupancies around 0.5:0.5)with isotropic ADP. One ethyl group (C38 C39) is disordered over 2 sites (refined occupancies 0.65:0.35) and was refined with isotropic ADP. ; _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^)+(0.0909P)^2^+18.1401P] 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 15887 _refine_ls_number_parameters 1132 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.007 _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 1.0229(4) 0.3300(4) -0.0357(4) 0.0457(16) Uani 1 1 d . . . C2 C 1.0381(5) 0.3300(5) -0.0831(4) 0.062(2) Uani 1 1 d . . . H2 H 1.0157 0.3644 -0.1170 0.075 Uiso 1 1 calc R . . C3 C 1.0859(5) 0.2795(5) -0.0800(5) 0.067(2) Uani 1 1 d . . . H3 H 1.0955 0.2775 -0.1129 0.080 Uiso 1 1 calc R . . C4 C 1.1198(5) 0.2316(5) -0.0296(4) 0.056(2) Uani 1 1 d . . . H4 H 1.1545 0.1976 -0.0260 0.067 Uiso 1 1 calc R . . C5 C 1.1020(4) 0.2343(4) 0.0156(4) 0.0464(16) Uani 1 1 d . . . C6 C 1.1244(5) 0.1795(4) 0.0675(4) 0.0515(18) Uani 1 1 d . B . C7 C 1.2027(7) 0.0884(8) 0.1424(6) 0.100(4) Uani 1 1 d . B . H7B H 1.1587 0.0573 0.1229 0.121 Uiso 1 1 calc R . . H7A H 1.2433 0.0583 0.1482 0.121 Uiso 1 1 calc R . . C8 C 1.2195(9) 0.1132(9) 0.2026(7) 0.135(6) Uani 1 1 d . . . H8A H 1.1769 0.1374 0.1978 0.203 Uiso 1 1 calc R . . H8B H 1.2600 0.1477 0.2201 0.203 Uiso 1 1 calc R . . H8C H 1.2332 0.0717 0.2318 0.203 Uiso 1 1 calc R . . C9 C 1.2542(5) 0.1827(6) 0.1026(6) 0.080(3) Uani 1 1 d . B . H9A H 1.2915 0.1932 0.1480 0.096 Uiso 1 1 calc R . . H9B H 1.2402 0.2294 0.0789 0.096 Uiso 1 1 calc R . . C10 C 1.2868(7) 0.1332(7) 0.0757(8) 0.107(5) Uani 1 1 d . . . H10B H 1.2515 0.1258 0.0298 0.161 Uiso 1 1 calc R . . H10C H 1.2991 0.0861 0.0977 0.161 Uiso 1 1 calc R . . H10A H 1.3309 0.1556 0.0821 0.161 Uiso 1 1 calc R . . C11 C 0.9705(4) 0.3777(4) -0.0337(4) 0.0449(16) Uani 1 1 d . . . C12 C 0.8976(4) 0.4155(4) -0.0058(4) 0.0477(17) Uani 1 1 d . . . C13 C 0.8585(4) 0.4268(4) 0.0231(4) 0.0493(17) Uani 1 1 d . . . H13 H 0.8586 0.3912 0.0509 0.059 Uiso 1 1 calc R . . C14 C 0.8201(5) 0.4904(5) 0.0104(4) 0.058(2) Uani 1 1 d . . . C15 C 0.8188(5) 0.5418(5) -0.0334(4) 0.063(2) Uani 1 1 d . . . H15 H 0.7911 0.5851 -0.0425 0.075 Uiso 1 1 calc R . . C16 C 0.8557(5) 0.5312(5) -0.0624(4) 0.061(2) Uani 1 1 d . . . H16 H 0.8540 0.5654 -0.0919 0.074 Uiso 1 1 calc R . . C17 C 0.8962(4) 0.4672(4) -0.0467(4) 0.0507(18) Uani 1 1 d . . . C18 C 0.9043(6) 0.4644(5) -0.1765(4) 0.069(2) Uani 1 1 d . . . H18C H 0.9136 0.4946 -0.2038 0.104 Uiso 1 1 calc R . . H18B H 0.8550 0.4738 -0.1868 0.104 Uiso 1 1 calc R . . H18A H 0.9090 0.4129 -0.1840 0.104 Uiso 1 1 calc R . . C19 C 0.9586(5) 0.4828(4) -0.1072(4) 0.0541(19) Uani 1 1 d . . . H19A H 1.0081 0.4704 -0.0963 0.065 Uiso 1 1 calc R . . H19B H 0.9572 0.5359 -0.1008 0.065 Uiso 1 1 calc R . . C20 C 0.7800(5) 0.5088(5) 0.0429(4) 0.061(2) Uani 1 1 d . . . H20B H 0.8027 0.4809 0.0834 0.074 Uiso 1 1 calc R . . H20A H 0.7879 0.5611 0.0544 0.074 Uiso 1 1 calc R . . C21 C 0.6995(5) 0.4945(4) 0.0056(4) 0.0536(19) Uani 1 1 d . . . C22 C 0.6499(4) 0.5510(4) -0.0219(4) 0.0474(17) Uani 1 1 d . . . H22 H 0.6655 0.5991 -0.0223 0.057 Uiso 1 1 calc R . . C23 C 0.5763(4) 0.5355(4) -0.0492(4) 0.0441(16) Uani 1 1 d . . . C24 C 0.4605(4) 0.5397(4) -0.0898(3) 0.0420(15) Uani 1 1 d . . . C25 C 0.5543(5) 0.4643(4) -0.0490(4) 0.0469(17) Uani 1 1 d . . . C26 C 0.6022(5) 0.4063(4) -0.0239(4) 0.057(2) Uani 1 1 d . . . H26 H 0.5862 0.3579 -0.0252 0.069 Uiso 1 1 calc R . . C27 C 0.6745(5) 0.4227(4) 0.0028(4) 0.058(2) Uani 1 1 d . . . H27 H 0.7090 0.3843 0.0202 0.070 Uiso 1 1 calc R . . C28 C 0.4353(5) 0.4037(4) -0.0829(4) 0.055(2) Uani 1 1 d . . . H28A H 0.3958 0.4182 -0.0770 0.066 Uiso 1 1 calc R . . H28B H 0.4658 0.3671 -0.0498 0.066 Uiso 1 1 calc R . . C29 C 0.4033(6) 0.3709(5) -0.1479(5) 0.069(2) Uani 1 1 d . . . H29B H 0.3712 0.4064 -0.1806 0.104 Uiso 1 1 calc R . . H29C H 0.3755 0.3273 -0.1516 0.104 Uiso 1 1 calc R . . H29A H 0.4424 0.3575 -0.1541 0.104 Uiso 1 1 calc R . . C30 C 0.3885(4) 0.5724(4) -0.1172(4) 0.0450(16) Uani 1 1 d . . . C31 C 0.3231(4) 0.5359(4) -0.1413(4) 0.0539(19) Uani 1 1 d . . . H31 H 0.3222 0.4841 -0.1407 0.065 Uiso 1 1 calc R . . C32 C 0.2603(5) 0.5743(5) -0.1659(4) 0.060(2) Uani 1 1 d . . . H32 H 0.2154 0.5494 -0.1832 0.072 Uiso 1 1 calc R . . C33 C 0.2620(5) 0.6496(5) -0.1655(4) 0.059(2) Uani 1 1 d . . . H33 H 0.2191 0.6774 -0.1808 0.071 Uiso 1 1 calc R . . C34 C 0.3292(4) 0.6832(4) -0.1416(4) 0.0482(17) Uani 1 1 d . . . C35 C 0.3390(5) 0.7639(5) -0.1467(5) 0.063(2) Uani 1 1 d . C . C36 C 0.2623(7) 0.8031(6) -0.1081(7) 0.096(4) Uani 1 1 d . C . H36B H 0.2839 0.8323 -0.0684 0.115 Uiso 1 1 calc R . . H36A H 0.2663 0.7511 -0.0960 0.115 Uiso 1 1 calc R . . C37 C 0.1829(9) 0.8226(8) -0.1513(10) 0.139(7) Uani 1 1 d . . . H37B H 0.1594 0.7890 -0.1878 0.208 Uiso 1 1 calc R . . H37A H 0.1784 0.8725 -0.1670 0.208 Uiso 1 1 calc R . . H37C H 0.1594 0.8189 -0.1273 0.208 Uiso 1 1 calc R . . C40 C 0.8692(8) 0.1946(10) -0.0925(6) 0.127(6) Uani 1 1 d D A . C41 C 0.8045(7) 0.2009(10) -0.0947(5) 0.127(6) Uani 1 1 d . . . H41 H 0.7601 0.1925 -0.1345 0.152 Uiso 1 1 calc R . . C42 C 0.8016(5) 0.2184(6) -0.0433(5) 0.074(3) Uani 1 1 d . . . C43 C 0.7274(6) 0.2098(7) -0.0511(6) 0.087(3) Uani 1 1 d . . . C44 C 0.8620(10) 0.1779(9) -0.1599(8) 0.167(8) Uiso 1 1 d D . . F4A F 0.8160(10) 0.1243(10) -0.1913(9) 0.156(3) Uiso 0.572(10) 1 d PD A 1 F5A F 0.9233(9) 0.1369(11) -0.1432(9) 0.156(3) Uiso 0.572(10) 1 d PD A 1 F6A F 0.8712(11) 0.2399(9) -0.1791(9) 0.156(3) Uiso 0.572(10) 1 d PD A 1 F4B F 0.7943(12) 0.2054(13) -0.2044(11) 0.156(3) Uiso 0.428(10) 1 d PD A 2 F5B F 0.8506(15) 0.1014(10) -0.1646(13) 0.156(3) Uiso 0.428(10) 1 d PD A 2 F6B F 0.9194(12) 0.1828(15) -0.1581(13) 0.156(3) Uiso 0.428(10) 1 d PD A 2 C45 C 0.9430(7) 0.0623(5) 0.0842(6) 0.077(3) Uani 1 1 d . . . C49A C 0.9138(14) -0.0088(14) 0.0467(11) 0.128(2) Uiso 0.462(14) 1 d PD B 1 F7A F 0.8522(12) 0.0010(11) -0.0058(9) 0.128(2) Uiso 0.462(14) 1 d PD B 1 F8A F 0.9487(13) -0.0333(11) 0.0196(9) 0.128(2) Uiso 0.462(14) 1 d PD B 1 F9A F 0.9198(12) -0.0637(11) 0.0800(9) 0.128(2) Uiso 0.462(14) 1 d PD B 1 C49B C 0.8881(15) -0.0006(14) 0.0506(12) 0.128(2) Uiso 0.538(14) 1 d PD B 2 F7B F 0.8243(11) 0.0145(10) 0.0053(8) 0.128(2) Uiso 0.538(14) 1 d PD B 2 F8B F 0.9088(12) -0.0306(10) 0.0137(8) 0.128(2) Uiso 0.538(14) 1 d PD B 2 F9B F 0.8851(11) -0.0506(10) 0.0838(8) 0.128(2) Uiso 0.538(14) 1 d PD B 2 C46 C 0.9883(8) 0.0591(5) 0.1508(5) 0.094(4) Uani 1 1 d . B . H46 H 0.9940 0.0142 0.1721 0.113 Uiso 1 1 calc R . . C47 C 1.0243(6) 0.1188(5) 0.1855(5) 0.066(2) Uani 1 1 d . . . C48A C 1.0831(13) 0.1177(12) 0.2648(13) 0.075(3) Uiso 0.428(16) 1 d PD B 1 F10A F 1.1339(13) 0.0761(12) 0.2826(10) 0.119(3) Uiso 0.428(16) 1 d PD B 1 F11A F 1.0330(11) 0.1281(15) 0.2795(10) 0.119(3) Uiso 0.428(16) 1 d PD B 1 F12A F 1.1213(13) 0.1717(10) 0.2902(11) 0.119(3) Uiso 0.428(16) 1 d PD B 1 C48B C 1.0647(10) 0.1080(10) 0.2569(9) 0.075(3) Uiso 0.572(16) 1 d PD B 2 F10B F 1.1066(10) 0.0521(9) 0.2788(8) 0.119(3) Uiso 0.572(16) 1 d PD B 2 F11B F 1.0268(8) 0.0814(11) 0.2802(7) 0.1195(8) Uiso 0.572(16) 1 d PD B 2 F12B F 1.0915(10) 0.1657(8) 0.2894(8) 0.1195(8) Uiso 0.572(16) 1 d PD B 2 C51 C 1.1168(4) 0.3290(4) 0.1958(4) 0.0483(17) Uani 1 1 d . . . C52 C 1.0758(4) 0.3450(4) 0.2218(4) 0.0477(17) Uani 1 1 d . . . H52 H 1.0995 0.3626 0.2644 0.057 Uiso 1 1 calc R . . C53 C 1.0014(4) 0.3357(4) 0.1867(4) 0.0463(17) Uani 1 1 d . . . C54 C 0.9632(6) 0.3556(7) 0.2220(6) 0.080(3) Uani 1 1 d . . . C55 C 1.1969(5) 0.3449(6) 0.2350(4) 0.064(2) Uani 1 1 d . . . C56 C 0.5621(5) 0.6397(4) -0.1996(4) 0.0509(18) Uani 1 1 d . C . C57 C 0.4996(5) 0.6061(4) -0.2470(4) 0.0537(19) Uani 1 1 d . . . H57 H 0.4991 0.5836 -0.2817 0.064 Uiso 1 1 calc R . . C58 C 0.4374(4) 0.6045(4) -0.2455(4) 0.0477(17) Uani 1 1 d . C . C59 C 0.6276(6) 0.6394(6) -0.2063(5) 0.070(3) Uani 1 1 d . . . C60 C 0.3762(5) 0.5528(5) -0.2930(4) 0.061(2) Uani 1 1 d . . . C61 C 0.4660(6) 0.8465(5) -0.2262(5) 0.068(2) Uani 1 1 d . C . C62 C 0.4877(6) 0.9056(5) -0.1844(5) 0.073(3) Uani 1 1 d . . . H62 H 0.4783 0.9537 -0.2010 0.087 Uiso 1 1 calc R . . C63 C 0.5228(5) 0.8949(4) -0.1189(5) 0.058(2) Uani 1 1 d . C . C64 C 0.5485(7) 0.9616(5) -0.0759(6) 0.073(3) Uani 1 1 d . . . C65 C 0.4355(10) 0.8625(7) -0.2973(6) 0.109(5) Uani 1 1 d . . . C66 C 0.5315(5) 0.7805(4) 0.0245(4) 0.0489(18) Uani 1 1 d . C . C67 C 0.6063(5) 0.7830(4) 0.0564(4) 0.059(2) Uani 1 1 d . . . H67 H 0.6337 0.8093 0.0954 0.071 Uiso 1 1 calc R . . C68 C 0.6423(5) 0.7465(4) 0.0311(4) 0.0529(19) Uani 1 1 d . C . C69 C 0.7231(6) 0.7433(7) 0.0720(5) 0.080(3) Uani 1 1 d . . . C70 C 0.4983(6) 0.8168(5) 0.0581(4) 0.062(2) Uani 1 1 d . . . Eu1 Eu 0.98218(2) 0.23729(2) 0.063660(17) 0.04207(11) Uani 1 1 d . . . Eu2 Eu 0.49516(2) 0.713938(19) -0.117809(18) 0.04272(12) Uani 1 1 d . C . F1 F 0.7160(4) 0.2635(4) -0.0221(4) 0.114(3) Uani 1 1 d . . . F2 F 0.7273(4) 0.1488(4) -0.0222(4) 0.102(2) Uani 1 1 d . . . F3 F 0.6732(4) 0.2043(4) -0.1106(4) 0.121(3) Uani 1 1 d . . . F13 F 1.2188(4) 0.3826(4) 0.2878(3) 0.100(2) Uani 1 1 d . . . F14 F 1.2353(3) 0.2848(4) 0.2531(4) 0.112(2) Uani 1 1 d . . . F15 F 1.2168(3) 0.3845(5) 0.2026(3) 0.103(2) Uani 1 1 d . . . F16 F 0.9505(8) 0.2939(6) 0.2439(6) 0.180(5) Uani 1 1 d . . . F17 F 0.9996(4) 0.3919(6) 0.2727(4) 0.148(4) Uani 1 1 d . . . F18 F 0.8997(5) 0.3806(6) 0.1845(4) 0.147(4) Uani 1 1 d . . . F19 F 0.6895(3) 0.6404(4) -0.1514(3) 0.0922(19) Uani 1 1 d . . . F20 F 0.6245(4) 0.5909(5) -0.2449(4) 0.131(3) Uani 1 1 d . . . F21 F 0.6277(4) 0.7024(5) -0.2349(4) 0.117(3) Uani 1 1 d . . . F22 F 0.3856(4) 0.4877(3) -0.2674(3) 0.113(3) Uani 1 1 d . . . F23 F 0.3712(4) 0.5426(4) -0.3470(3) 0.103(2) Uani 1 1 d . . . F24 F 0.3118(4) 0.5751(4) -0.3080(4) 0.113(3) Uani 1 1 d . . . F25 F 0.4457(6) 0.8168(5) -0.3271(4) 0.123(3) Uani 1 1 d . . . F26 F 0.4422(9) 0.9272(5) -0.3093(4) 0.226(8) Uani 1 1 d . . . F27 F 0.3583(7) 0.8546(8) -0.3285(5) 0.186(5) Uani 1 1 d . . . F28 F 0.5357(6) 1.0234(3) -0.1056(4) 0.135(4) Uani 1 1 d . . . F29 F 0.5206(5) 0.9634(4) -0.0411(4) 0.116(3) Uani 1 1 d . . . F30 F 0.6185(5) 0.9611(4) -0.0361(5) 0.131(3) Uani 1 1 d . . . F31 F 0.4473(4) 0.8624(4) 0.0202(3) 0.096(2) Uani 1 1 d . . . F32 F 0.4669(6) 0.7676(4) 0.0740(5) 0.140(4) Uani 1 1 d . . . F33 F 0.5431(4) 0.8509(5) 0.1103(3) 0.119(3) Uani 1 1 d . . . F34 F 0.7537(4) 0.7166(5) 0.0441(4) 0.120(3) Uani 1 1 d . . . F35 F 0.7450(5) 0.6976(10) 0.1203(5) 0.210(7) Uani 1 1 d . . . F36 F 0.7554(5) 0.8020(6) 0.0981(6) 0.197(6) Uani 1 1 d . . . N1 N 1.0532(3) 0.2827(3) 0.0118(3) 0.0457(14) Uani 1 1 d . B . N2 N 1.1896(4) 0.1506(4) 0.0983(4) 0.067(2) Uani 1 1 d . . . N3 N 0.9441(4) 0.3592(3) 0.0021(3) 0.0474(14) Uani 1 1 d . B . N4 N 0.9436(4) 0.4431(3) -0.0638(3) 0.0488(15) Uani 1 1 d . . . N5 N 0.3892(4) 0.6457(3) -0.1192(3) 0.0467(14) Uani 1 1 d . . . N6 N 0.3038(6) 0.8152(4) -0.1371(5) 0.085(3) Uani 1 1 d D . . C38A C 0.3306(15) 0.8921(10) -0.1305(13) 0.106(4) Uiso 0.65(3) 1 d PD C 1 H38A H 0.3186 0.9214 -0.1040 0.127 Uiso 0.65 1 calc P C 1 H38B H 0.3839 0.8929 -0.1103 0.127 Uiso 0.65 1 calc P C 1 C39A C 0.2950(14) 0.9196(12) -0.1930(13) 0.106(4) Uiso 0.65(3) 1 d PD C 1 H39A H 0.3104 0.9699 -0.1919 0.158 Uiso 0.65 1 calc P C 1 H39B H 0.2423 0.9183 -0.2122 0.158 Uiso 0.65 1 calc P C 1 H39C H 0.3072 0.8897 -0.2185 0.158 Uiso 0.65 1 calc P C 1 C38B C 0.297(3) 0.8876(16) -0.165(2) 0.106(4) Uiso 0.35(3) 1 d PD C 2 H38C H 0.2602 0.9147 -0.1610 0.127 Uiso 0.35 1 calc P C 2 H38D H 0.3439 0.9129 -0.1369 0.127 Uiso 0.35 1 calc P C 2 C39B C 0.278(2) 0.894(2) -0.2272(19) 0.106(4) Uiso 0.35(3) 1 d PD C 2 H39D H 0.2795 0.9459 -0.2370 0.158 Uiso 0.35 1 calc P C 2 H39E H 0.2293 0.8750 -0.2563 0.158 Uiso 0.35 1 calc P C 2 H39F H 0.3130 0.8670 -0.2327 0.158 Uiso 0.35 1 calc P C 2 N7 N 0.5175(3) 0.5824(3) -0.0748(3) 0.0438(14) Uani 1 1 d . . . N8 N 0.4801(4) 0.4683(3) -0.0746(3) 0.0454(14) Uani 1 1 d . . . O1 O 1.0769(3) 0.1596(3) 0.0776(3) 0.0573(14) Uani 1 1 d . B . O2 O 0.3836(4) 0.7790(3) -0.1612(3) 0.0621(15) Uani 1 1 d . . . O3 O 0.9318(4) 0.2034(4) -0.0452(3) 0.075(2) Uani 1 1 d . A . O4 O 0.8524(3) 0.2398(3) 0.0104(3) 0.0584(14) Uani 1 1 d . B . O5 O 0.9348(4) 0.1141(3) 0.0502(3) 0.0618(15) Uani 1 1 d . B . O7 O 1.0270(4) 0.1798(3) 0.1657(3) 0.0651(16) Uani 1 1 d . B . O8 O 1.0940(3) 0.3016(3) 0.1417(3) 0.0527(13) Uani 1 1 d . B . O9 O 0.9599(3) 0.3130(3) 0.1316(3) 0.0495(12) Uani 1 1 d . B . O10 O 0.5738(3) 0.6708(3) -0.1498(3) 0.0517(13) Uani 1 1 d . . . O11 O 0.4251(3) 0.6347(3) -0.2084(3) 0.0493(12) Uani 1 1 d . . . O12 O 0.4696(4) 0.7811(3) -0.2136(3) 0.0609(15) Uani 1 1 d . . . O13 O 0.5372(3) 0.8362(3) -0.0902(3) 0.0522(13) Uani 1 1 d . . . O14 O 0.4880(3) 0.7498(3) -0.0263(3) 0.0501(12) Uani 1 1 d . . . O15 O 0.6138(3) 0.7143(3) -0.0217(3) 0.0519(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 0.042(4) 0.056(4) 0.044(4) 0.005(3) 0.027(3) 0.001(3) C2 0.069(6) 0.080(6) 0.062(5) 0.025(4) 0.051(5) 0.019(5) C3 0.076(6) 0.078(6) 0.076(6) 0.010(5) 0.060(5) 0.013(5) C4 0.058(5) 0.059(5) 0.071(5) 0.001(4) 0.048(5) 0.005(4) C5 0.048(4) 0.045(4) 0.052(4) 0.001(3) 0.031(4) 0.005(3) C6 0.056(5) 0.050(4) 0.050(4) -0.002(3) 0.029(4) 0.015(4) C7 0.090(9) 0.123(10) 0.096(9) 0.035(8) 0.056(8) 0.049(8) C8 0.129(13) 0.135(13) 0.096(11) 0.013(9) 0.031(10) 0.044(11) C9 0.053(6) 0.072(6) 0.093(8) 0.009(5) 0.027(5) 0.007(5) C10 0.080(8) 0.085(8) 0.182(14) 0.028(8) 0.087(9) 0.028(6) C11 0.043(4) 0.052(4) 0.047(4) 0.004(3) 0.029(4) -0.001(3) C12 0.043(4) 0.051(4) 0.054(4) 0.009(3) 0.029(4) 0.010(3) C13 0.046(4) 0.055(4) 0.050(4) 0.009(3) 0.028(4) 0.011(3) C14 0.048(5) 0.062(5) 0.064(5) 0.000(4) 0.032(4) 0.013(4) C15 0.058(5) 0.057(5) 0.068(6) 0.005(4) 0.030(5) 0.017(4) C16 0.071(6) 0.053(5) 0.066(5) 0.011(4) 0.041(5) 0.011(4) C17 0.049(5) 0.053(4) 0.051(4) 0.004(3) 0.028(4) 0.005(3) C18 0.082(7) 0.070(6) 0.061(6) 0.014(4) 0.042(5) 0.009(5) C19 0.065(5) 0.053(4) 0.052(5) 0.010(3) 0.037(4) -0.001(4) C20 0.050(5) 0.075(6) 0.058(5) -0.004(4) 0.028(4) 0.014(4) C21 0.054(5) 0.056(5) 0.056(5) -0.003(4) 0.033(4) 0.010(4) C22 0.053(5) 0.043(4) 0.056(4) -0.003(3) 0.036(4) 0.005(3) C23 0.052(4) 0.044(4) 0.046(4) -0.003(3) 0.033(4) 0.004(3) C24 0.048(4) 0.045(4) 0.045(4) 0.000(3) 0.033(4) 0.001(3) C25 0.064(5) 0.041(4) 0.050(4) -0.001(3) 0.040(4) 0.002(3) C26 0.081(6) 0.042(4) 0.064(5) -0.001(4) 0.049(5) 0.005(4) C27 0.069(6) 0.050(4) 0.061(5) 0.003(4) 0.039(5) 0.015(4) C28 0.074(6) 0.042(4) 0.061(5) 0.002(3) 0.045(5) -0.007(4) C29 0.084(7) 0.053(5) 0.074(6) -0.001(4) 0.045(6) -0.008(5) C30 0.052(4) 0.044(4) 0.049(4) -0.005(3) 0.034(4) 0.001(3) C31 0.052(5) 0.053(4) 0.069(5) -0.009(4) 0.041(4) -0.009(4) C32 0.052(5) 0.072(6) 0.068(6) -0.005(4) 0.041(5) -0.007(4) C33 0.053(5) 0.066(5) 0.067(5) 0.002(4) 0.039(5) 0.009(4) C34 0.048(4) 0.057(4) 0.052(4) 0.004(3) 0.035(4) 0.006(3) C35 0.067(6) 0.060(5) 0.077(6) 0.012(4) 0.050(5) 0.020(4) C36 0.106(9) 0.080(7) 0.149(12) -0.010(7) 0.101(9) 0.009(6) C37 0.132(13) 0.100(10) 0.25(2) 0.026(12) 0.149(15) 0.034(9) C40 0.113(11) 0.225(17) 0.064(7) -0.053(9) 0.061(8) -0.088(12) C41 0.079(8) 0.245(19) 0.044(6) -0.033(8) 0.026(6) -0.074(10) C42 0.060(6) 0.092(7) 0.065(6) 0.003(5) 0.029(5) -0.022(5) C43 0.056(6) 0.093(8) 0.096(8) -0.006(6) 0.031(6) -0.012(6) C45 0.098(8) 0.048(5) 0.096(8) 0.000(5) 0.059(7) -0.006(5) C46 0.166(13) 0.040(5) 0.082(8) 0.010(5) 0.072(8) -0.009(6) C47 0.095(7) 0.053(5) 0.066(6) 0.005(4) 0.054(6) 0.004(5) C51 0.049(4) 0.054(4) 0.046(4) 0.010(3) 0.028(4) -0.001(3) C52 0.049(4) 0.054(4) 0.044(4) -0.005(3) 0.028(4) -0.002(3) C53 0.058(5) 0.041(4) 0.051(4) -0.003(3) 0.037(4) 0.003(3) C54 0.064(6) 0.106(8) 0.085(7) -0.023(6) 0.050(6) 0.000(6) C55 0.054(5) 0.090(6) 0.050(5) 0.013(4) 0.030(4) 0.003(5) C56 0.060(5) 0.049(4) 0.065(5) -0.005(4) 0.049(4) -0.003(4) C57 0.059(5) 0.056(4) 0.064(5) -0.015(4) 0.044(4) -0.008(4) C58 0.057(5) 0.042(4) 0.053(4) 0.001(3) 0.036(4) 0.001(3) C59 0.069(6) 0.089(7) 0.073(6) -0.018(5) 0.053(6) -0.011(5) C60 0.062(6) 0.064(5) 0.067(6) -0.019(4) 0.041(5) -0.015(4) C61 0.088(7) 0.063(6) 0.067(6) 0.008(4) 0.050(6) 0.003(5) C62 0.115(9) 0.045(5) 0.080(7) 0.006(4) 0.067(7) 0.004(5) C63 0.075(6) 0.046(4) 0.088(6) 0.000(4) 0.067(5) 0.001(4) C64 0.121(10) 0.041(5) 0.090(7) -0.006(4) 0.079(8) -0.004(5) C65 0.150(14) 0.084(8) 0.071(8) 0.013(6) 0.046(9) -0.005(9) C66 0.079(6) 0.030(3) 0.058(5) 0.002(3) 0.050(5) 0.006(3) C67 0.084(6) 0.045(4) 0.057(5) -0.005(4) 0.043(5) 0.001(4) C68 0.065(5) 0.049(4) 0.058(5) -0.006(3) 0.041(4) -0.002(4) C69 0.067(6) 0.107(8) 0.066(6) -0.024(6) 0.037(5) -0.007(6) C70 0.083(7) 0.052(5) 0.064(5) -0.002(4) 0.049(5) 0.013(4) Eu1 0.0503(2) 0.04300(19) 0.0436(2) 0.00077(14) 0.03249(17) 0.00217(15) Eu2 0.0540(2) 0.03709(18) 0.0521(2) -0.00335(14) 0.03850(19) -0.00157(15) F1 0.076(4) 0.088(4) 0.171(8) -0.026(5) 0.062(5) -0.011(4) F2 0.095(5) 0.082(4) 0.169(7) 0.003(4) 0.097(5) -0.008(3) F3 0.058(4) 0.127(6) 0.128(6) -0.019(5) 0.017(4) -0.010(4) F13 0.076(4) 0.146(6) 0.075(4) -0.027(4) 0.039(3) -0.039(4) F14 0.056(4) 0.104(5) 0.137(6) 0.015(4) 0.026(4) 0.015(4) F15 0.063(4) 0.173(7) 0.075(4) 0.030(4) 0.039(3) -0.026(4) F16 0.268(14) 0.180(9) 0.237(12) 0.026(9) 0.231(12) 0.018(9) F17 0.096(5) 0.246(10) 0.124(6) -0.113(7) 0.074(5) -0.028(6) F18 0.099(6) 0.257(11) 0.112(6) -0.011(6) 0.074(5) 0.062(7) F19 0.060(4) 0.157(6) 0.072(4) 0.001(4) 0.044(3) 0.012(4) F20 0.099(5) 0.185(8) 0.157(7) -0.092(6) 0.101(5) -0.029(5) F21 0.107(5) 0.155(7) 0.135(6) 0.023(5) 0.095(5) -0.015(5) F22 0.124(6) 0.068(4) 0.107(5) 0.000(3) 0.036(5) -0.042(4) F23 0.111(5) 0.132(5) 0.074(4) -0.048(4) 0.056(4) -0.046(4) F24 0.066(4) 0.133(6) 0.127(6) -0.062(5) 0.043(4) -0.025(4) F25 0.193(9) 0.115(6) 0.086(5) -0.005(4) 0.092(6) -0.016(6) F26 0.46(2) 0.089(5) 0.093(6) 0.011(4) 0.124(10) -0.071(9) F27 0.173(11) 0.248(14) 0.093(7) 0.010(7) 0.044(7) 0.057(10) F28 0.288(12) 0.042(3) 0.151(7) -0.005(4) 0.169(8) -0.005(5) F29 0.200(9) 0.083(4) 0.148(6) -0.039(4) 0.148(7) -0.027(5) F30 0.131(7) 0.091(5) 0.157(8) -0.063(5) 0.069(6) -0.032(5) F31 0.105(5) 0.100(4) 0.084(4) -0.005(3) 0.052(4) 0.046(4) F32 0.248(11) 0.085(4) 0.223(10) 0.002(5) 0.216(10) 0.012(5) F33 0.105(5) 0.159(7) 0.081(4) -0.050(4) 0.043(4) 0.037(5) F34 0.063(4) 0.182(8) 0.124(6) -0.061(6) 0.057(4) -0.025(5) F35 0.087(6) 0.39(2) 0.147(9) 0.140(12) 0.060(6) 0.084(9) F36 0.084(6) 0.183(9) 0.260(13) -0.150(10) 0.051(7) -0.044(6) N1 0.047(3) 0.048(3) 0.049(3) 0.003(3) 0.031(3) 0.005(3) N2 0.060(5) 0.065(4) 0.078(5) 0.015(4) 0.039(4) 0.018(4) N3 0.051(4) 0.049(3) 0.055(4) 0.007(3) 0.037(3) 0.010(3) N4 0.058(4) 0.046(3) 0.056(4) 0.008(3) 0.040(3) 0.003(3) N5 0.056(4) 0.043(3) 0.058(4) 0.000(3) 0.042(3) 0.005(3) N6 0.111(7) 0.053(4) 0.142(8) 0.002(5) 0.100(7) 0.015(4) N7 0.053(4) 0.041(3) 0.050(4) -0.001(3) 0.036(3) 0.000(3) N8 0.061(4) 0.034(3) 0.053(4) 0.005(2) 0.039(3) 0.001(3) O1 0.069(4) 0.056(3) 0.069(4) 0.013(3) 0.052(3) 0.019(3) O2 0.074(4) 0.050(3) 0.076(4) 0.013(3) 0.051(3) 0.013(3) O3 0.083(5) 0.115(5) 0.050(3) -0.028(3) 0.051(4) -0.038(4) O4 0.050(3) 0.058(3) 0.067(4) -0.004(3) 0.032(3) -0.002(3) O5 0.076(4) 0.048(3) 0.067(4) -0.003(3) 0.043(3) -0.010(3) O7 0.098(5) 0.058(3) 0.053(3) 0.006(3) 0.050(3) 0.004(3) O8 0.053(3) 0.067(3) 0.048(3) 0.002(2) 0.034(3) -0.001(3) O9 0.043(3) 0.061(3) 0.054(3) -0.004(2) 0.032(3) 0.004(2) O10 0.054(3) 0.057(3) 0.060(3) -0.016(3) 0.042(3) -0.006(2) O11 0.057(3) 0.053(3) 0.054(3) -0.008(2) 0.040(3) -0.008(2) O12 0.087(4) 0.051(3) 0.062(3) 0.003(3) 0.052(3) -0.001(3) O13 0.068(4) 0.036(3) 0.060(3) 0.000(2) 0.040(3) -0.005(2) O14 0.067(4) 0.045(3) 0.057(3) -0.007(2) 0.046(3) -0.003(2) O15 0.061(3) 0.047(3) 0.062(3) -0.012(2) 0.043(3) -0.003(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 N1 1.320(9) . ? C1 C2 1.387(10) . ? C1 C11 1.466(10) . ? C2 C3 1.371(12) . ? C2 H2 0.9500 . ? C3 C4 1.373(12) . ? C3 H3 0.9500 . ? C4 C5 1.377(10) . ? C4 H4 0.9500 . ? C5 N1 1.353(9) . ? C5 C6 1.493(11) . ? C6 O1 1.251(10) . ? C6 N2 1.312(11) . ? C6 Eu1 3.244(8) . ? C7 C8 1.408(18) . ? C7 N2 1.500(14) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N2 1.484(13) . ? C9 C10 1.518(16) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10A 0.9800 . ? C11 N3 1.343(9) . ? C11 N4 1.367(10) . ? C12 C17 1.377(10) . ? C12 N3 1.389(9) . ? C12 C13 1.402(10) . ? C13 C14 1.372(11) . ? C13 H13 0.9500 . ? C14 C15 1.430(13) . ? C14 C20 1.521(11) . ? C15 C16 1.360(12) . ? C15 H15 0.9500 . ? C16 C17 1.394(11) . ? C16 H16 0.9500 . ? C17 N4 1.392(10) . ? C18 C19 1.509(12) . ? C18 H18C 0.9800 . ? C18 H18B 0.9800 . ? C18 H18A 0.9800 . ? C19 N4 1.481(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.506(12) . ? C20 H20B 0.9900 . ? C20 H20A 0.9900 . ? C21 C22 1.384(11) . ? C21 C27 1.415(12) . ? C22 C23 1.398(11) . ? C22 H22 0.9500 . ? C23 N7 1.385(9) . ? C23 C25 1.393(10) . ? C24 N7 1.345(9) . ? C24 N8 1.366(9) . ? C24 C30 1.465(10) . ? C25 C26 1.384(11) . ? C25 N8 1.390(10) . ? C26 C27 1.377(13) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 N8 1.481(9) . ? C28 C29 1.497(12) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C29 H29A 0.9800 . ? C30 N5 1.348(9) . ? C30 C31 1.390(11) . ? C31 C32 1.361(12) . ? C31 H31 0.9500 . ? C32 C33 1.383(12) . ? C32 H32 0.9500 . ? C33 C34 1.397(12) . ? C33 H33 0.9500 . ? C34 N5 1.310(10) . ? C34 C35 1.514(12) . ? C35 O2 1.242(10) . ? C35 N6 1.320(11) . ? C35 Eu2 3.225(9) . ? C36 N6 1.451(13) . ? C36 C37 1.510(19) . ? C36 H36B 0.9900 . ? C36 H36A 0.9900 . ? C37 H37B 0.9800 . ? C37 H37A 0.9800 . ? C37 H37C 0.9800 . ? C40 O3 1.242(14) . ? C40 C41 1.392(19) . ? C40 C44 1.625(16) . ? C41 C42 1.353(16) . ? C41 H41 0.9500 . ? C42 O4 1.251(11) . ? C42 C43 1.538(15) . ? C43 F3 1.306(13) . ? C43 F1 1.322(14) . ? C43 F2 1.332(14) . ? C44 F6B 1.240(19) . ? C44 F6A 1.293(14) . ? C44 F4A 1.320(15) . ? C44 F4B 1.378(19) . ? C44 F5A 1.393(15) . ? C44 F5B 1.42(2) . ? C45 O5 1.219(11) . ? C45 C46 1.396(16) . ? C45 C49A 1.53(3) . ? C45 C49B 1.55(3) . ? C49A F9A 1.266(16) . ? C49A F7A 1.282(16) . ? C49A F8A 1.342(17) . ? C49B F9B 1.26(2) . ? C49B F7B 1.26(2) . ? C49B F8B 1.34(2) . ? C46 C47 1.353(14) . ? C46 H46 0.9500 . ? C47 O7 1.237(10) . ? C47 C48B 1.51(2) . ? C47 C48A 1.67(3) . ? C48A F10A 1.219(18) . ? C48A F12A 1.228(19) . ? C48A F11A 1.345(19) . ? C48B F12B 1.266(17) . ? C48B F10B 1.286(16) . ? C48B F11B 1.335(18) . ? C51 O8 1.258(9) . ? C51 C52 1.392(10) . ? C51 C55 1.504(12) . ? C52 C53 1.380(11) . ? C52 H52 0.9500 . ? C53 O9 1.237(9) . ? C53 C54 1.551(11) . ? C54 F17 1.256(12) . ? C54 F18 1.268(13) . ? C54 F16 1.349(15) . ? C55 F14 1.311(11) . ? C55 F15 1.322(10) . ? C55 F13 1.324(11) . ? C56 O10 1.256(9) . ? C56 C57 1.378(12) . ? C56 C59 1.533(11) . ? C57 C58 1.383(11) . ? C57 H57 0.9500 . ? C58 O11 1.227(9) . ? C58 C60 1.541(11) . ? C59 F20 1.283(11) . ? C59 F19 1.302(12) . ? C59 F21 1.358(13) . ? C60 F23 1.299(10) . ? C60 F24 1.316(11) . ? C60 F22 1.318(11) . ? C61 O12 1.234(10) . ? C61 C62 1.395(13) . ? C61 C65 1.541(15) . ? C62 C63 1.385(13) . ? C62 H62 0.9500 . ? C63 O13 1.237(9) . ? C63 C64 1.519(12) . ? C64 F30 1.297(14) . ? C64 F28 1.299(11) . ? C64 F29 1.304(11) . ? C65 F25 1.217(16) . ? C65 F26 1.253(14) . ? C65 F27 1.44(2) . ? C66 O14 1.231(10) . ? C66 C67 1.381(13) . ? C66 C70 1.528(10) . ? C67 C68 1.415(11) . ? C67 H67 0.9500 . ? C68 O15 1.255(9) . ? C68 C69 1.489(14) . ? C69 F36 1.259(14) . ? C69 F34 1.295(12) . ? C69 F35 1.323(15) . ? C70 F33 1.287(11) . ? C70 F31 1.302(11) . ? C70 F32 1.319(11) . ? Eu1 O1 2.384(5) . ? Eu1 O3 2.384(5) . ? Eu1 O4 2.399(6) . ? Eu1 O7 2.412(5) . ? Eu1 O9 2.433(5) . ? Eu1 O5 2.436(5) . ? Eu1 O8 2.450(6) . ? Eu1 N3 2.581(6) . ? Eu1 N1 2.637(6) . ? Eu2 O13 2.381(5) . ? Eu2 O2 2.389(6) . ? Eu2 O10 2.392(5) . ? Eu2 O15 2.393(6) . ? Eu2 O11 2.406(5) . ? Eu2 O14 2.453(5) . ? Eu2 O12 2.461(5) . ? Eu2 N7 2.579(6) . ? Eu2 N5 2.622(6) . ? N6 C38B 1.46(2) . ? N6 C38A 1.505(19) . ? C38A C39A 1.40(3) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? C38B C39B 1.39(3) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B H39D 0.9800 . ? C39B H39E 0.9800 . ? C39B H39F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.6(7) . . ? N1 C1 C11 112.7(6) . . ? C2 C1 C11 125.6(7) . . ? C3 C2 C1 118.8(8) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.2(8) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 117.9(7) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N1 C5 C4 122.1(7) . . ? N1 C5 C6 112.3(6) . . ? C4 C5 C6 125.1(7) . . ? O1 C6 N2 121.7(8) . . ? O1 C6 C5 116.9(7) . . ? N2 C6 C5 121.4(8) . . ? O1 C6 Eu1 37.9(3) . . ? N2 C6 Eu1 150.9(6) . . ? C5 C6 Eu1 83.9(4) . . ? C8 C7 N2 111.6(12) . . ? C8 C7 H7B 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7A 109.3 . . ? H7B C7 H7A 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 112.9(9) . . ? N2 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N2 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? N3 C11 N4 111.9(6) . . ? N3 C11 C1 119.9(6) . . ? N4 C11 C1 128.2(6) . . ? C17 C12 N3 109.9(6) . . ? C17 C12 C13 120.1(7) . . ? N3 C12 C13 129.9(7) . . ? C14 C13 C12 118.5(7) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 119.6(7) . . ? C13 C14 C20 121.8(8) . . ? C15 C14 C20 118.6(7) . . ? C16 C15 C14 122.5(8) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C17 116.3(8) . . ? C15 C16 H16 121.9 . . ? C17 C16 H16 121.9 . . ? C12 C17 N4 106.5(6) . . ? C12 C17 C16 123.0(7) . . ? N4 C17 C16 130.4(7) . . ? C19 C18 H18C 109.5 . . ? C19 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? C19 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? N4 C19 C18 111.9(7) . . ? N4 C19 H19A 109.2 . . ? C18 C19 H19A 109.2 . . ? N4 C19 H19B 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C21 C20 C14 117.1(7) . . ? C21 C20 H20B 108.0 . . ? C14 C20 H20B 108.0 . . ? C21 C20 H20A 108.0 . . ? C14 C20 H20A 108.0 . . ? H20B C20 H20A 107.3 . . ? C22 C21 C27 119.6(8) . . ? C22 C21 C20 121.2(8) . . ? C27 C21 C20 119.1(8) . . ? C21 C22 C23 118.5(7) . . ? C21 C22 H22 120.8 . . ? C23 C22 H22 120.8 . . ? N7 C23 C25 110.3(7) . . ? N7 C23 C22 129.6(7) . . ? C25 C23 C22 120.0(7) . . ? N7 C24 N8 112.1(6) . . ? N7 C24 C30 119.6(6) . . ? N8 C24 C30 128.3(7) . . ? C26 C25 N8 131.4(7) . . ? C26 C25 C23 123.0(8) . . ? N8 C25 C23 105.6(6) . . ? C27 C26 C25 116.2(8) . . ? C27 C26 H26 121.9 . . ? C25 C26 H26 121.9 . . ? C26 C27 C21 122.8(8) . . ? C26 C27 H27 118.6 . . ? C21 C27 H27 118.6 . . ? N8 C28 C29 111.1(6) . . ? N8 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? N8 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? N5 C30 C31 119.7(7) . . ? N5 C30 C24 113.3(7) . . ? C31 C30 C24 126.9(7) . . ? C32 C31 C30 119.9(8) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 119.9(8) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 117.5(8) . . ? C32 C33 H33 121.2 . . ? C34 C33 H33 121.2 . . ? N5 C34 C33 122.2(7) . . ? N5 C34 C35 113.2(7) . . ? C33 C34 C35 124.2(7) . . ? O2 C35 N6 121.6(8) . . ? O2 C35 C34 114.4(7) . . ? N6 C35 C34 124.0(8) . . ? O2 C35 Eu2 38.9(4) . . ? N6 C35 Eu2 144.9(8) . . ? C34 C35 Eu2 83.4(4) . . ? N6 C36 C37 113.6(12) . . ? N6 C36 H36B 108.9 . . ? C37 C36 H36B 108.9 . . ? N6 C36 H36A 108.9 . . ? C37 C36 H36A 108.9 . . ? H36B C36 H36A 107.7 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37A 109.5 . . ? H37B C37 H37A 109.5 . . ? C36 C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? O3 C40 C41 127.2(10) . . ? O3 C40 C44 116.1(12) . . ? C41 C40 C44 116.6(12) . . ? C42 C41 C40 123.4(10) . . ? C42 C41 H41 118.3 . . ? C40 C41 H41 118.3 . . ? O4 C42 C41 127.7(10) . . ? O4 C42 C43 115.8(9) . . ? C41 C42 C43 116.5(10) . . ? F3 C43 F1 110.6(10) . . ? F3 C43 F2 106.2(10) . . ? F1 C43 F2 106.2(11) . . ? F3 C43 C42 113.6(11) . . ? F1 C43 C42 110.8(9) . . ? F2 C43 C42 109.1(10) . . ? F6B C44 F6A 65.7(15) . . ? F6B C44 F4A 121(2) . . ? F6A C44 F4A 131.3(19) . . ? F6B C44 F4B 129(2) . . ? F6A C44 F4B 72.3(16) . . ? F4A C44 F4B 69.8(14) . . ? F6B C44 F5A 39.8(13) . . ? F6A C44 F5A 105.5(16) . . ? F4A C44 F5A 94.3(14) . . ? F4B C44 F5A 151.8(19) . . ? F6B C44 F5B 101.7(18) . . ? F6A C44 F5B 154(2) . . ? F4A C44 F5B 33.9(13) . . ? F4B C44 F5B 103.4(18) . . ? F5A C44 F5B 65.6(13) . . ? F6B C44 C40 115.0(18) . . ? F6A C44 C40 105.6(15) . . ? F4A C44 C40 111.5(15) . . ? F4B C44 C40 102.6(16) . . ? F5A C44 C40 105.0(15) . . ? F5B C44 C40 100.8(17) . . ? O5 C45 C46 126.8(9) . . ? O5 C45 C49A 112.8(12) . . ? C46 C45 C49A 118.7(11) . . ? O5 C45 C49B 115.5(13) . . ? C46 C45 C49B 116.9(12) . . ? C49A C45 C49B 24.0(11) . . ? F9A C49A F7A 117(2) . . ? F9A C49A F8A 100.1(18) . . ? F7A C49A F8A 96.3(18) . . ? F9A C49A C45 114.9(19) . . ? F7A C49A C45 111.2(19) . . ? F8A C49A C45 115(2) . . ? F9B C49B F7B 109(2) . . ? F9B C49B F8B 108(2) . . ? F7B C49B F8B 95.8(19) . . ? F9B C49B C45 120(2) . . ? F7B C49B C45 119(2) . . ? F8B C49B C45 103.0(19) . . ? C47 C46 C45 121.0(8) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? O7 C47 C46 128.1(9) . . ? O7 C47 C48B 117.6(10) . . ? C46 C47 C48B 114.2(10) . . ? O7 C47 C48A 107.9(11) . . ? C46 C47 C48A 123.5(11) . . ? C48B C47 C48A 12.6(10) . . ? F10A C48A F12A 95(2) . . ? F10A C48A F11A 135(3) . . ? F12A C48A F11A 100.1(18) . . ? F10A C48A C47 113.8(18) . . ? F12A C48A C47 118(2) . . ? F11A C48A C47 95.7(17) . . ? F12B C48B F10B 114.8(18) . . ? F12B C48B F11B 102.3(15) . . ? F10B C48B F11B 89.6(15) . . ? F12B C48B C47 114.4(15) . . ? F10B C48B C47 115.6(15) . . ? F11B C48B C47 117.0(15) . . ? O8 C51 C52 126.8(7) . . ? O8 C51 C55 114.6(7) . . ? C52 C51 C55 118.6(7) . . ? C53 C52 C51 121.3(7) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? O9 C53 C52 130.4(7) . . ? O9 C53 C54 114.1(8) . . ? C52 C53 C54 115.5(7) . . ? F17 C54 F18 113.2(10) . . ? F17 C54 F16 101.5(11) . . ? F18 C54 F16 102.5(11) . . ? F17 C54 C53 116.7(9) . . ? F18 C54 C53 112.5(9) . . ? F16 C54 C53 108.8(9) . . ? F14 C55 F15 108.2(8) . . ? F14 C55 F13 106.3(8) . . ? F15 C55 F13 104.8(8) . . ? F14 C55 C51 111.4(8) . . ? F15 C55 C51 111.5(7) . . ? F13 C55 C51 114.3(7) . . ? O10 C56 C57 128.5(7) . . ? O10 C56 C59 114.1(7) . . ? C57 C56 C59 117.4(7) . . ? C56 C57 C58 121.6(7) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? O11 C58 C57 129.2(8) . . ? O11 C58 C60 113.6(7) . . ? C57 C58 C60 116.9(7) . . ? F20 C59 F19 113.4(9) . . ? F20 C59 F21 102.5(9) . . ? F19 C59 F21 103.9(9) . . ? F20 C59 C56 114.3(8) . . ? F19 C59 C56 112.8(8) . . ? F21 C59 C56 108.7(8) . . ? F23 C60 F24 106.0(9) . . ? F23 C60 F22 105.8(8) . . ? F24 C60 F22 106.3(8) . . ? F23 C60 C58 115.6(7) . . ? F24 C60 C58 112.3(7) . . ? F22 C60 C58 110.2(8) . . ? O12 C61 C62 128.1(9) . . ? O12 C61 C65 113.9(9) . . ? C62 C61 C65 117.9(9) . . ? C63 C62 C61 120.9(8) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? O13 C63 C62 127.4(8) . . ? O13 C63 C64 114.5(8) . . ? C62 C63 C64 118.1(8) . . ? F30 C64 F28 104.0(10) . . ? F30 C64 F29 106.3(10) . . ? F28 C64 F29 108.7(8) . . ? F30 C64 C63 111.4(8) . . ? F28 C64 C63 114.9(9) . . ? F29 C64 C63 111.0(8) . . ? F25 C65 F26 115.1(14) . . ? F25 C65 F27 98.9(12) . . ? F26 C65 F27 102.9(15) . . ? F25 C65 C61 117.3(12) . . ? F26 C65 C61 114.8(12) . . ? F27 C65 C61 104.5(12) . . ? O14 C66 C67 128.3(7) . . ? O14 C66 C70 115.4(8) . . ? C67 C66 C70 116.2(7) . . ? C66 C67 C68 120.2(8) . . ? C66 C67 H67 119.9 . . ? C68 C67 H67 119.9 . . ? O15 C68 C67 127.4(8) . . ? O15 C68 C69 115.3(7) . . ? C67 C68 C69 117.3(8) . . ? F36 C69 F34 106.9(11) . . ? F36 C69 F35 104.3(12) . . ? F34 C69 F35 102.0(11) . . ? F36 C69 C68 116.4(10) . . ? F34 C69 C68 114.8(9) . . ? F35 C69 C68 110.9(10) . . ? F33 C70 F31 107.6(7) . . ? F33 C70 F32 105.5(9) . . ? F31 C70 F32 106.0(9) . . ? F33 C70 C66 115.8(8) . . ? F31 C70 C66 111.2(7) . . ? F32 C70 C66 110.1(7) . . ? O1 Eu1 O3 80.8(2) . . ? O1 Eu1 O4 140.3(2) . . ? O3 Eu1 O4 72.4(2) . . ? O1 Eu1 O7 76.1(2) . . ? O3 Eu1 O7 138.9(2) . . ? O4 Eu1 O7 105.9(2) . . ? O1 Eu1 O9 136.72(19) . . ? O3 Eu1 O9 142.5(2) . . ? O4 Eu1 O9 75.37(19) . . ? O7 Eu1 O9 68.92(19) . . ? O1 Eu1 O5 74.8(2) . . ? O3 Eu1 O5 72.6(2) . . ? O4 Eu1 O5 69.7(2) . . ? O7 Eu1 O5 68.8(2) . . ? O9 Eu1 O5 113.24(19) . . ? O1 Eu1 O8 75.9(2) . . ? O3 Eu1 O8 132.30(18) . . ? O4 Eu1 O8 143.52(19) . . ? O7 Eu1 O8 73.5(2) . . ? O9 Eu1 O8 70.50(17) . . ? O5 Eu1 O8 136.5(2) . . ? O1 Eu1 N3 125.52(18) . . ? O3 Eu1 N3 75.6(2) . . ? O4 Eu1 N3 75.6(2) . . ? O7 Eu1 N3 145.1(2) . . ? O9 Eu1 N3 78.12(18) . . ? O5 Eu1 N3 138.4(2) . . ? O8 Eu1 N3 85.1(2) . . ? O1 Eu1 N1 64.01(18) . . ? O3 Eu1 N1 63.9(2) . . ? O4 Eu1 N1 124.1(2) . . ? O7 Eu1 N1 129.9(2) . . ? O9 Eu1 N1 123.58(18) . . ? O5 Eu1 N1 123.16(19) . . ? O8 Eu1 N1 68.49(18) . . ? N3 Eu1 N1 61.52(18) . . ? O1 Eu1 C6 18.79(19) . . ? O3 Eu1 C6 78.1(2) . . ? O4 Eu1 C6 148.7(2) . . ? O7 Eu1 C6 89.4(2) . . ? O9 Eu1 C6 135.91(19) . . ? O5 Eu1 C6 91.8(2) . . ? O8 Eu1 C6 66.59(19) . . ? N3 Eu1 C6 107.29(19) . . ? N1 Eu1 C6 45.99(19) . . ? O13 Eu2 O2 78.5(2) . . ? O13 Eu2 O10 99.90(18) . . ? O2 Eu2 O10 139.5(2) . . ? O13 Eu2 O15 70.66(18) . . ? O2 Eu2 O15 137.79(19) . . ? O10 Eu2 O15 75.25(18) . . ? O13 Eu2 O11 142.19(18) . . ? O2 Eu2 O11 84.4(2) . . ? O10 Eu2 O11 72.36(17) . . ? O15 Eu2 O11 137.03(18) . . ? O13 Eu2 O14 71.88(17) . . ? O2 Eu2 O14 73.7(2) . . ? O10 Eu2 O14 144.85(19) . . ? O15 Eu2 O14 69.77(18) . . ? O11 Eu2 O14 134.49(17) . . ? O13 Eu2 O12 69.89(19) . . ? O2 Eu2 O12 70.9(2) . . ? O10 Eu2 O12 70.8(2) . . ? O15 Eu2 O12 121.3(2) . . ? O11 Eu2 O12 72.71(18) . . ? O14 Eu2 O12 131.84(18) . . ? O13 Eu2 N7 143.76(19) . . ? O2 Eu2 N7 124.94(19) . . ? O10 Eu2 N7 79.59(18) . . ? O15 Eu2 N7 74.30(19) . . ? O11 Eu2 N7 72.71(19) . . ? O14 Eu2 N7 87.72(17) . . ? O12 Eu2 N7 139.72(18) . . ? O13 Eu2 N5 130.95(18) . . ? O2 Eu2 N5 63.28(19) . . ? O10 Eu2 N5 129.08(17) . . ? O15 Eu2 N5 119.24(19) . . ? O11 Eu2 N5 65.69(17) . . ? O14 Eu2 N5 68.84(18) . . ? O12 Eu2 N5 119.4(2) . . ? N7 Eu2 N5 61.67(19) . . ? O13 Eu2 C35 89.7(2) . . ? O2 Eu2 C35 19.0(2) . . ? O10 Eu2 C35 152.8(2) . . ? O15 Eu2 C35 131.9(2) . . ? O11 Eu2 C35 84.4(2) . . ? O14 Eu2 C35 62.4(2) . . ? O12 Eu2 C35 89.1(2) . . ? N7 Eu2 C35 107.4(2) . . ? N5 Eu2 C35 46.2(2) . . ? C1 N1 C5 119.3(6) . . ? C1 N1 Eu1 120.1(5) . . ? C5 N1 Eu1 114.4(5) . . ? C6 N2 C9 125.2(8) . . ? C6 N2 C7 116.8(8) . . ? C9 N2 C7 117.0(8) . . ? C11 N3 C12 105.2(6) . . ? C11 N3 Eu1 119.8(5) . . ? C12 N3 Eu1 135.0(5) . . ? C11 N4 C17 106.4(6) . . ? C11 N4 C19 129.2(6) . . ? C17 N4 C19 124.4(6) . . ? C34 N5 C30 120.7(7) . . ? C34 N5 Eu2 115.6(5) . . ? C30 N5 Eu2 120.3(5) . . ? C35 N6 C36 124.5(9) . . ? C35 N6 C38B 119.0(17) . . ? C36 N6 C38B 116.0(18) . . ? C35 N6 C38A 117.1(12) . . ? C36 N6 C38A 113.8(11) . . ? C38B N6 C38A 30.0(17) . . ? C39A C38A N6 105.5(18) . . ? C39A C38A H38A 110.6 . . ? N6 C38A H38A 110.6 . . ? C39A C38A H38B 110.6 . . ? N6 C38A H38B 110.6 . . ? H38A C38A H38B 108.8 . . ? C38A C39A H39A 109.5 . . ? C38A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C38A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? C39B C38B N6 120(3) . . ? C39B C38B H38C 107.3 . . ? N6 C38B H38C 107.3 . . ? C39B C38B H38D 107.3 . . ? N6 C38B H38D 107.3 . . ? H38C C38B H38D 106.9 . . ? C38B C39B H39D 109.5 . . ? C38B C39B H39E 109.5 . . ? H39D C39B H39E 109.5 . . ? C38B C39B H39F 109.5 . . ? H39D C39B H39F 109.5 . . ? H39E C39B H39F 109.5 . . ? C24 N7 C23 104.9(6) . . ? C24 N7 Eu2 119.5(5) . . ? C23 N7 Eu2 133.9(5) . . ? C24 N8 C25 107.0(6) . . ? C24 N8 C28 130.1(7) . . ? C25 N8 C28 122.9(6) . . ? C6 O1 Eu1 123.3(5) . . ? C35 O2 Eu2 122.1(5) . . ? C40 O3 Eu1 134.6(7) . . ? C42 O4 Eu1 133.3(6) . . ? C45 O5 Eu1 137.5(7) . . ? C47 O7 Eu1 137.3(6) . . ? C51 O8 Eu1 133.3(5) . . ? C53 O9 Eu1 131.2(5) . . ? C56 O10 Eu2 132.9(5) . . ? C58 O11 Eu2 133.6(5) . . ? C61 O12 Eu2 133.2(6) . . ? C63 O13 Eu2 135.9(6) . . ? C66 O14 Eu2 132.2(5) . . ? C68 O15 Eu2 134.5(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.391 _refine_diff_density_min -1.385 _refine_diff_density_rms 0.120 data_4 _database_code_depnum_ccdc_archive 'CCDC 909094' #TrackingRef 'web_deposit_cif_file_0_LaureGuenee_1351875343.Compounds_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C108 H74 Eu3 F54 N13 O20), 5.5(C2 H3 N)' _chemical_formula_sum 'C119 H90.50 Eu3 F54 N18.50 O20' _chemical_formula_weight 3581.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.6614(4) _cell_length_b 19.7308(4) _cell_length_c 23.4654(5) _cell_angle_alpha 95.2886(19) _cell_angle_beta 96.6780(19) _cell_angle_gamma 114.691(2) _cell_volume 7288.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23637 _cell_measurement_theta_min 2.7926 _cell_measurement_theta_max 73.2983 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3420 _exptl_crystal_size_mid 0.2203 _exptl_crystal_size_min 0.1365 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3538 _exptl_absorpt_coefficient_mu 10.343 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.204 _exptl_absorpt_correction_T_max 0.506 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4679 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53489 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 73.46 _reflns_number_total 28544 _reflns_number_gt 23163 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep 3' _computing_publication_material ShelX_ACTA _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. Solvate molecules: CH3CN solvate molecules whith large anisotropic displacement parameters were refined isotropically. One CH3CN was disordered over two positions (pop refined 0.73/0.27). Another CH3CN was refined with occupancy fixed to 0.5 and restrains on bond lengths, leading to 5.5(CH3CN) in the asymetric unit. Disorderd CF3 groups: Many of CF3 groups showed high anisotropic displacement parameters due to disorder along 3-fold axes. Two of them were refined in two parts with isotropic displacement parameters and refined occupancies around 0.5. ; _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^)+(0.0876P)^2^+6.2643P] 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 28544 _refine_ls_number_parameters 1894 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1585 _refine_ls_wR_factor_gt 0.1455 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.040250(18) 0.565756(15) 0.784601(11) 0.03212(7) Uani 1 1 d . . . Eu2 Eu 0.639675(18) 0.867993(16) 0.884127(12) 0.03361(8) Uani 1 1 d . . . Eu3 Eu -0.349656(19) 0.775485(17) 0.395670(13) 0.03709(8) Uani 1 1 d . . . F1 F 0.0990(5) 0.6060(5) 0.5863(2) 0.137(3) Uani 1 1 d . . . F2 F 0.2255(6) 0.6830(4) 0.6015(2) 0.161(4) Uani 1 1 d . . . F3 F 0.1904(5) 0.5703(4) 0.6100(3) 0.120(2) Uani 1 1 d . . . F4 F 0.3040(7) 0.8537(3) 0.7740(3) 0.196(5) Uani 1 1 d . . . F5 F 0.2490(4) 0.8276(3) 0.8487(3) 0.113(2) Uani 1 1 d . . . F6 F 0.3484(4) 0.8051(4) 0.8327(3) 0.145(3) Uani 1 1 d . . . F7 F -0.2603(4) 0.5363(6) 0.7412(4) 0.158(4) Uani 1 1 d . . . F8 F -0.3121(4) 0.4777(6) 0.8080(5) 0.169(4) Uani 1 1 d . . . F9 F -0.2279(6) 0.5902(6) 0.8254(5) 0.185(4) Uani 1 1 d . . . F10 F -0.1461(6) 0.2933(3) 0.8099(3) 0.142(3) Uani 1 1 d . . . F11 F -0.1926(4) 0.3205(3) 0.8830(3) 0.117(2) Uani 1 1 d . . . F12 F -0.0633(5) 0.3466(5) 0.8877(4) 0.161(4) Uani 1 1 d . . . F14A F -0.0017(10) 0.8385(8) 0.7993(6) 0.1170(17) Uiso 0.493(6) 1 d P A 3 F15A F 0.0977(10) 0.8380(9) 0.7529(6) 0.1170(17) Uiso 0.493(6) 1 d P A 3 F13A F -0.0314(10) 0.7707(8) 0.7173(7) 0.1170(17) Uiso 0.493(6) 1 d P A 3 F13B F -0.0612(10) 0.7700(8) 0.7439(6) 0.1170(17) Uiso 0.507(6) 1 d P A 4 F14B F 0.0579(10) 0.8592(8) 0.7852(6) 0.1170(17) Uiso 0.507(6) 1 d P A 4 F15B F 0.0434(9) 0.7899(8) 0.7053(6) 0.1170(17) Uiso 0.507(6) 1 d P A 4 F16 F -0.0132(4) 0.6887(6) 0.9741(3) 0.159(4) Uani 1 1 d . . . F17 F 0.0820(9) 0.7892(6) 0.9718(3) 0.217(5) Uani 1 1 d . . . F18 F 0.1067(5) 0.6981(6) 0.9860(2) 0.154(4) Uani 1 1 d . . . F19 F 0.3354(4) 0.6375(3) 0.8186(3) 0.115(2) Uani 1 1 d . . . F20 F 0.3759(4) 0.6049(3) 0.7450(2) 0.1032(18) Uani 1 1 d . . . F21 F 0.4327(4) 0.6033(3) 0.8277(3) 0.118(2) Uani 1 1 d . . . F22 F 0.4275(4) 0.8340(4) 0.6684(3) 0.134(3) Uani 1 1 d . . . F23 F 0.5449(6) 0.8385(4) 0.6558(2) 0.131(3) Uani 1 1 d . . . F24 F 0.5411(4) 0.9331(3) 0.6975(2) 0.0989(17) Uani 1 1 d . . . F25 F 0.6388(7) 0.6762(7) 0.7190(4) 0.263(8) Uani 1 1 d . . . F26 F 0.7038(11) 0.7728(7) 0.6996(3) 0.250(8) Uani 1 1 d . . . F27 F 0.7604(7) 0.7129(8) 0.7242(3) 0.211(6) Uani 1 1 d . . . F28B F 0.8196(11) 0.7303(10) 0.9622(8) 0.1231(19) Uiso 0.462(8) 1 d P B 6 F29B F 0.9009(10) 0.8402(10) 0.9611(7) 0.1231(19) Uiso 0.538(8) 1 d P B 5 F30B F 0.8644(9) 0.7261(8) 0.9230(6) 0.1231(19) Uiso 0.538(8) 1 d P B 5 F31 F 0.8319(5) 1.0677(4) 1.0640(5) 0.191(5) Uani 1 1 d . . . F32 F 0.9026(4) 1.0208(4) 1.0267(3) 0.121(2) Uani 1 1 d . . . F33 F 0.8665(4) 0.9909(5) 1.1041(3) 0.134(3) Uani 1 1 d . . . F34 F 0.5640(6) 0.6875(4) 1.0175(3) 0.139(3) Uani 1 1 d . . . F35 F 0.5326(4) 0.7585(4) 1.0697(3) 0.1074(19) Uani 1 1 d . . . F36 F 0.6470(4) 0.7512(5) 1.0957(4) 0.164(4) Uani 1 1 d . . . F37 F -0.0849(5) 0.9238(8) 0.5351(4) 0.211(6) Uani 1 1 d . . . F38 F -0.1392(7) 0.8427(5) 0.5821(6) 0.254(8) Uani 1 1 d . . . F39 F -0.1241(4) 0.9517(4) 0.6060(3) 0.137(3) Uani 1 1 d . . . F40 F -0.4234(7) 0.9748(6) 0.4869(3) 0.177(5) Uani 1 1 d . . . F41 F -0.4741(6) 0.8982(6) 0.5371(5) 0.193(5) Uani 1 1 d . . . F42 F -0.3695(6) 0.9872(6) 0.5727(3) 0.194(5) Uani 1 1 d . . . F43 F -0.1445(3) 0.6682(4) 0.4386(3) 0.1073(19) Uani 1 1 d . . . F44 F -0.1455(6) 0.6511(8) 0.3507(3) 0.240(7) Uani 1 1 d . . . F45 F -0.2092(5) 0.5634(4) 0.3932(5) 0.171(4) Uani 1 1 d . . . F46 F -0.4879(4) 0.5338(3) 0.2297(2) 0.1068(19) Uani 1 1 d . . . F47 F -0.5604(3) 0.5251(3) 0.2982(3) 0.0982(17) Uani 1 1 d . . . F48 F -0.4867(3) 0.4642(2) 0.2937(2) 0.0805(12) Uani 1 1 d . . . F49 F -0.1954(5) 1.0611(4) 0.3975(8) 0.280(9) Uani 1 1 d . . . F50 F -0.1140(8) 1.0372(5) 0.4454(4) 0.212(6) Uani 1 1 d . . . F51 F -0.0880(6) 1.0648(4) 0.3696(5) 0.189(4) Uani 1 1 d . . . F52 F -0.2591(6) 0.7625(6) 0.2036(3) 0.177(4) Uani 1 1 d . . . F53 F -0.1759(8) 0.8684(5) 0.2031(4) 0.203(5) Uani 1 1 d . . . F54 F -0.1442(7) 0.7949(7) 0.2476(3) 0.201(5) Uani 1 1 d . . . O1 O 0.7688(2) 0.9452(2) 0.85166(17) 0.0454(8) Uani 1 1 d . . . O1H O 0.1089(2) 0.5867(2) 0.70064(16) 0.0445(8) Uani 1 1 d . . . O2 O -0.4329(3) 0.8136(2) 0.32780(16) 0.0463(8) Uani 1 1 d . . . O2H O 0.1761(2) 0.6805(2) 0.80632(15) 0.0452(8) Uani 1 1 d . . . O3H O -0.0384(3) 0.4585(2) 0.82886(17) 0.0482(9) Uani 1 1 d . . . O4H O -0.1029(3) 0.5561(2) 0.79197(17) 0.0491(9) Uani 1 1 d . . . O5H O 0.0462(3) 0.6312(3) 0.87627(16) 0.0526(10) Uani 1 1 d . . . O6H O 0.0259(3) 0.6769(2) 0.76290(18) 0.0516(10) Uani 1 1 d . . . O7H O 0.5135(3) 0.7542(2) 0.85168(16) 0.0454(8) Uani 1 1 d . . . O8H O 0.5711(2) 0.8805(2) 0.79156(15) 0.0423(8) Uani 1 1 d . . . O9H O 0.6619(3) 0.7946(2) 0.80408(17) 0.0488(9) Uani 1 1 d . . . O10H O 0.7356(3) 0.8179(2) 0.91890(18) 0.0512(10) Uani 1 1 d . . . O11H O 0.7361(3) 0.9543(2) 0.97112(16) 0.0483(9) Uani 1 1 d . . . O12H O 0.6022(3) 0.8127(2) 0.97003(16) 0.0494(9) Uani 1 1 d . . . O13H O -0.2485(3) 0.8244(2) 0.48407(18) 0.0550(10) Uani 1 1 d . . . O14H O -0.3902(3) 0.8536(2) 0.45949(18) 0.0540(10) Uani 1 1 d . . . O15H O -0.2595(2) 0.7115(2) 0.39560(17) 0.0455(8) Uani 1 1 d . . . O16H O -0.4250(2) 0.6560(2) 0.33105(16) 0.0443(8) Uani 1 1 d . . . O17H O -0.2537(3) 0.9074(2) 0.3972(2) 0.0587(11) Uani 1 1 d . . . O18H O -0.2829(3) 0.7914(2) 0.30961(17) 0.0502(9) Uani 1 1 d . . . N1 N 0.0464(3) 0.4395(2) 0.74274(17) 0.0352(8) Uani 1 1 d . . . N2 N 0.1448(3) 0.5311(2) 0.84256(17) 0.0363(8) Uani 1 1 d . . . N3 N 0.2151(3) 0.4604(3) 0.8582(2) 0.0463(10) Uani 1 1 d . . . N4 N 0.5311(3) 0.9132(2) 0.91391(17) 0.0363(8) Uani 1 1 d . . . N5 N 0.4707(3) 0.9932(2) 0.91851(17) 0.0357(8) Uani 1 1 d . . . N6 N 0.6691(3) 1.0073(2) 0.87903(16) 0.0350(8) Uani 1 1 d . . . N7 N 0.8855(3) 1.0550(3) 0.8828(2) 0.0451(10) Uani 1 1 d . . . N8 N -0.0623(3) 0.4909(2) 0.69150(17) 0.0373(8) Uani 1 1 d . . . N9 N -0.0916(3) 0.4118(3) 0.60849(18) 0.0411(9) Uani 1 1 d . . . N10 N -0.4092(3) 0.6739(3) 0.46212(19) 0.0410(9) Uani 1 1 d . . . N11 N -0.5110(3) 0.5974(3) 0.5058(2) 0.0440(10) Uani 1 1 d . . . N12 N -0.5119(3) 0.7163(3) 0.39747(18) 0.0411(9) Uani 1 1 d . . . N13 N -0.5303(4) 0.8604(3) 0.3299(2) 0.0532(12) Uani 1 1 d . . . C1 C 0.0871(3) 0.4107(3) 0.7776(2) 0.0377(10) Uani 1 1 d . . . C1H C 0.1639(4) 0.6418(3) 0.6847(2) 0.0494(13) Uani 1 1 d . . . C2 C 0.0669(4) 0.3337(3) 0.7716(2) 0.0467(12) Uani 1 1 d . . . H2 H 0.0969 0.3146 0.7967 0.056 Uiso 1 1 calc R . . C2H C 0.2167(4) 0.7110(3) 0.7162(2) 0.0495(13) Uani 1 1 d . . . H2H H 0.2526 0.7497 0.6974 0.059 Uiso 1 1 calc R . . C3 C 0.0012(4) 0.2860(3) 0.7273(3) 0.0497(13) Uani 1 1 d . . . H3 H -0.0150 0.2332 0.7223 0.060 Uiso 1 1 calc R . . C3H C 0.2179(3) 0.7247(3) 0.7755(2) 0.0439(11) Uani 1 1 d . . . C4 C -0.0407(4) 0.3150(3) 0.6908(3) 0.0467(12) Uani 1 1 d . . . H4 H -0.0854 0.2827 0.6604 0.056 Uiso 1 1 calc R . . C4H C 0.1703(5) 0.6274(4) 0.6207(3) 0.072(2) Uani 1 1 d . . . C5 C -0.0160(4) 0.3925(3) 0.6994(2) 0.0418(11) Uani 1 1 d . . . C5H C 0.2783(5) 0.8041(4) 0.8075(3) 0.0631(17) Uani 1 1 d . . . C6 C 0.1510(3) 0.4673(3) 0.8257(2) 0.0402(11) Uani 1 1 d . . . C6H C -0.1127(4) 0.4216(4) 0.8351(3) 0.0559(15) Uani 1 1 d . . . C7 C 0.2085(3) 0.5673(3) 0.8911(2) 0.0409(11) Uani 1 1 d . . . C7H C -0.1797(5) 0.4412(5) 0.8233(4) 0.073(2) Uani 1 1 d . . . H7H H -0.2347 0.4076 0.8285 0.088 Uiso 1 1 calc R . . C8 C 0.2301(3) 0.6346(3) 0.9275(2) 0.0411(11) Uani 1 1 d . . . H8 H 0.2011 0.6649 0.9202 0.049 Uiso 1 1 calc R . . C8H C -0.1672(4) 0.5088(4) 0.8041(3) 0.0606(16) Uani 1 1 d . . . C9 C 0.2952(3) 0.6566(3) 0.9747(2) 0.0464(12) Uani 1 1 d . . . C9H C -0.2437(6) 0.5278(8) 0.7951(5) 0.103(3) Uani 1 1 d . . . C10 C 0.3392(4) 0.6119(4) 0.9833(3) 0.0597(16) Uani 1 1 d . . . H10 H 0.3841 0.6281 1.0154 0.072 Uiso 1 1 calc R . . C10H C -0.1314(6) 0.3450(5) 0.8541(4) 0.083(2) Uani 1 1 d . . . C11 C 0.3198(4) 0.5453(4) 0.9468(3) 0.0587(15) Uani 1 1 d . . . H11 H 0.3507 0.5163 0.9524 0.070 Uiso 1 1 calc R . . C11H C 0.0455(4) 0.6942(5) 0.8906(3) 0.066(2) Uani 1 1 d . . . C12 C 0.2522(4) 0.5238(3) 0.9015(2) 0.0472(12) Uani 1 1 d . . . C12H C 0.0375(5) 0.7446(4) 0.8551(4) 0.075(2) Uani 1 1 d . . . H12 H 0.0382 0.7902 0.8730 0.091 Uiso 1 1 calc R . . C13 C 0.3192(4) 0.7282(4) 1.0164(2) 0.0509(13) Uani 1 1 d . . . H13A H 0.2683 0.7257 1.0316 0.061 Uiso 1 1 calc R . . H13B H 0.3608 0.7309 1.0497 0.061 Uiso 1 1 calc R . . C13H C 0.0285(5) 0.7315(4) 0.7949(3) 0.0659(19) Uani 1 1 d . A . C14 C 0.3563(3) 0.7995(3) 0.9900(2) 0.0423(11) Uani 1 1 d . . . C14H C 0.0239(8) 0.7952(5) 0.7626(5) 0.108(4) Uani 1 1 d . . . C15 C 0.4263(3) 0.8145(3) 0.9627(2) 0.0385(10) Uani 1 1 d . . . H15 H 0.4501 0.7794 0.9589 0.046 Uiso 1 1 calc R . . C15H C 0.0540(6) 0.7139(7) 0.9562(4) 0.097(4) Uani 1 1 d . . . C16 C 0.4605(3) 0.8822(3) 0.94099(19) 0.0360(10) Uani 1 1 d . . . C16H C 0.4674(4) 0.7246(3) 0.8028(2) 0.0444(11) Uani 1 1 d . . . C17 C 0.4233(3) 0.9328(3) 0.9448(2) 0.0380(10) Uani 1 1 d . . . C17H C 0.4655(4) 0.7576(3) 0.7532(3) 0.0497(13) Uani 1 1 d . . . H17 H 0.4281 0.7274 0.7188 0.060 Uiso 1 1 calc R . . C18 C 0.3532(4) 0.9188(3) 0.9712(2) 0.0460(12) Uani 1 1 d . . . H18 H 0.3283 0.9531 0.9735 0.055 Uiso 1 1 calc R . . C18H C 0.5162(4) 0.8325(3) 0.7525(2) 0.0454(12) Uani 1 1 d . . . C19 C 0.3216(4) 0.8525(4) 0.9938(2) 0.0475(13) Uani 1 1 d . . . H19 H 0.2742 0.8417 1.0129 0.057 Uiso 1 1 calc R . . C19H C 0.5047(5) 0.8615(4) 0.6951(3) 0.0703(19) Uani 1 1 d . . . C20 C 0.5348(3) 0.9784(3) 0.90141(19) 0.0330(9) Uani 1 1 d . . . C20H C 0.4033(4) 0.6414(4) 0.7990(3) 0.0575(15) Uani 1 1 d . . . C21 C 0.6061(3) 1.0297(3) 0.8767(2) 0.0355(10) Uani 1 1 d . . . C21H C 0.7133(4) 0.7680(3) 0.7973(3) 0.0538(14) Uani 1 1 d . . . C22 C 0.6136(4) 1.0937(3) 0.8543(2) 0.0438(11) Uani 1 1 d . . . H22 H 0.5678 1.1073 0.8510 0.053 Uiso 1 1 calc R . . C22H C 0.7741(5) 0.7664(5) 0.8389(3) 0.078(2) Uani 1 1 d . . . H22A H 0.8131 0.7484 0.8276 0.094 Uiso 1 1 calc R . . C23 C 0.6887(4) 1.1385(3) 0.8366(3) 0.0491(13) Uani 1 1 d . . . H23 H 0.6945 1.1827 0.8207 0.059 Uiso 1 1 calc R . . C23H C 0.7791(5) 0.7906(4) 0.8965(3) 0.0629(17) Uani 1 1 d . B . C24 C 0.7549(4) 1.1181(3) 0.8423(2) 0.0452(12) Uani 1 1 d . . . H24 H 0.8077 1.1488 0.8319 0.054 Uiso 1 1 calc R . . C24H C 0.8474(9) 0.7851(8) 0.9429(6) 0.116(4) Uani 1 1 d . . . C25 C 0.7420(3) 1.0519(3) 0.8636(2) 0.0379(10) Uani 1 1 d . . . C25H C 0.7056(6) 0.7335(5) 0.7347(4) 0.075(2) Uani 1 1 d . . . C26 C 0.8019(4) 1.0151(3) 0.8665(2) 0.0420(11) Uani 1 1 d . . . C26H C 0.7575(4) 0.9405(4) 1.0202(2) 0.0508(14) Uani 1 1 d . . . C27 C 0.9287(4) 1.1353(4) 0.9102(3) 0.0571(15) Uani 1 1 d . . . H27A H 0.9607 1.1392 0.9489 0.069 Uiso 1 1 calc R . . H27B H 0.8856 1.1539 0.9161 0.069 Uiso 1 1 calc R . . C27H C 0.7184(4) 0.8792(4) 1.0467(2) 0.0568(16) Uani 1 1 d . . . H27 H 0.7429 0.8771 1.0844 0.068 Uiso 1 1 calc R . . C28 C 0.9883(5) 1.1846(5) 0.8743(4) 0.080(2) Uani 1 1 d . . . H28A H 1.0148 1.2371 0.8940 0.119 Uiso 1 1 calc R . . H28B H 0.9568 1.1815 0.8361 0.119 Uiso 1 1 calc R . . H28C H 1.0321 1.1674 0.8693 0.119 Uiso 1 1 calc R . . C28H C 0.6427(4) 0.8196(4) 1.0185(3) 0.0532(14) Uani 1 1 d . . . C29 C 0.9373(4) 1.0125(4) 0.8826(3) 0.0592(16) Uani 1 1 d . . . H29A H 0.9097 0.9667 0.9005 0.071 Uiso 1 1 calc R . . H29B H 0.9933 1.0441 0.9069 0.071 Uiso 1 1 calc R . . C29H C 0.6001(6) 0.7547(5) 1.0516(3) 0.073(2) Uani 1 1 d . . . C30 C 0.9499(5) 0.9893(5) 0.8233(4) 0.076(2) Uani 1 1 d . . . H30A H 0.9887 0.9655 0.8265 0.114 Uiso 1 1 calc R . . H30B H 0.9738 1.0339 0.8041 0.114 Uiso 1 1 calc R . . H30C H 0.8953 0.9533 0.8003 0.114 Uiso 1 1 calc R . . C30H C 0.8396(5) 1.0061(5) 1.0543(3) 0.072(2) Uani 1 1 d . . . C31 C -0.0577(3) 0.4301(3) 0.6659(2) 0.0359(10) Uani 1 1 d . . . C31H C -0.2305(5) 0.8763(4) 0.5249(3) 0.0597(16) Uani 1 1 d . . . C32 C -0.1011(3) 0.5151(3) 0.6471(2) 0.0369(10) Uani 1 1 d . . . C32H C -0.2761(5) 0.9167(4) 0.5378(3) 0.0648(18) Uani 1 1 d . . . H32 H -0.2540 0.9565 0.5699 0.078 Uiso 1 1 calc R . . C33 C -0.1207(3) 0.5760(3) 0.6497(2) 0.0406(11) Uani 1 1 d . . . H33 H -0.1093 0.6086 0.6852 0.049 Uiso 1 1 calc R . . C33H C -0.3527(5) 0.8999(4) 0.5048(3) 0.0587(16) Uani 1 1 d . . . C34 C -0.1577(4) 0.5880(3) 0.5984(2) 0.0440(11) Uani 1 1 d . . . C34H C -0.4026(6) 0.9439(5) 0.5250(3) 0.073(2) Uani 1 1 d . . . C35 C -0.1759(4) 0.5380(3) 0.5465(2) 0.0460(12) Uani 1 1 d . . . H35 H -0.2016 0.5471 0.5120 0.055 Uiso 1 1 calc R . . C35H C -0.1455(6) 0.8977(6) 0.5650(4) 0.085(3) Uani 1 1 d . . . C36 C -0.1581(4) 0.4766(3) 0.5438(2) 0.0462(12) Uani 1 1 d . . . H36 H -0.1716 0.4427 0.5086 0.055 Uiso 1 1 calc R . . C36H C -0.4129(4) 0.5982(3) 0.3226(2) 0.0441(11) Uani 1 1 d . . . C37 C -0.1187(3) 0.4665(3) 0.5957(2) 0.0386(10) Uani 1 1 d . . . C37H C -0.3409(4) 0.5890(4) 0.3423(3) 0.0587(16) Uani 1 1 d . . . H37 H -0.3408 0.5411 0.3331 0.070 Uiso 1 1 calc R . . C38 C -0.1763(4) 0.6567(3) 0.5966(3) 0.0504(13) Uani 1 1 d . . . H38A H -0.1618 0.6849 0.6365 0.060 Uiso 1 1 calc R . . H38B H -0.1393 0.6904 0.5725 0.060 Uiso 1 1 calc R . . C38H C -0.2696(4) 0.6476(4) 0.3747(3) 0.0499(13) Uani 1 1 d . . . C39 C -0.2676(4) 0.6374(3) 0.5725(2) 0.0445(12) Uani 1 1 d . . . C39H C -0.1903(5) 0.6336(5) 0.3873(3) 0.0668(19) Uani 1 1 d . . . C40 C -0.2876(4) 0.6679(3) 0.5253(2) 0.0427(11) Uani 1 1 d . . . H40 H -0.2447 0.6996 0.5062 0.051 Uiso 1 1 calc R . . C40H C -0.4873(5) 0.5295(4) 0.2847(3) 0.0588(15) Uani 1 1 d . . . C41 C -0.3723(3) 0.6507(3) 0.5067(2) 0.0392(11) Uani 1 1 d . . . C41H C -0.2029(5) 0.9440(4) 0.3674(3) 0.0656(17) Uani 1 1 d . . . C42 C -0.4350(4) 0.6029(3) 0.5346(2) 0.0426(11) Uani 1 1 d . . . C42H C -0.1853(6) 0.9179(5) 0.3163(4) 0.079(2) Uani 1 1 d . . . H42 H -0.1438 0.9523 0.2977 0.095 Uiso 1 1 calc R . . C43 C -0.4164(4) 0.5722(4) 0.5822(2) 0.0502(13) Uani 1 1 d . . . H43 H -0.4595 0.5405 0.6012 0.060 Uiso 1 1 calc R . . C43H C -0.2271(5) 0.8423(4) 0.2916(3) 0.0621(17) Uani 1 1 d . . . C44 C -0.3321(4) 0.5902(4) 0.6005(2) 0.0505(13) Uani 1 1 d . . . H44 H -0.3171 0.5702 0.6329 0.061 Uiso 1 1 calc R . . C44H C -0.1995(7) 0.8175(6) 0.2367(4) 0.085(2) Uani 1 1 d . . . C45 C -0.4921(3) 0.6405(3) 0.4629(2) 0.0399(10) Uani 1 1 d . . . C45H C -0.1518(8) 1.0289(5) 0.3929(5) 0.101(3) Uani 1 1 d . . . C46 C -0.5509(3) 0.6540(3) 0.4206(2) 0.0421(11) Uani 1 1 d . . . C47 C -0.6364(4) 0.6061(4) 0.4013(3) 0.0538(14) Uani 1 1 d . . . H47 H -0.6629 0.5606 0.4167 0.065 Uiso 1 1 calc R . . C48 C -0.6817(4) 0.6257(4) 0.3595(3) 0.0627(16) Uani 1 1 d . . . H48 H -0.7395 0.5930 0.3447 0.075 Uiso 1 1 calc R . . C49 C -0.6428(4) 0.6929(4) 0.3393(3) 0.0554(15) Uani 1 1 d . . . H49 H -0.6736 0.7087 0.3118 0.066 Uiso 1 1 calc R . . C50 C -0.5577(4) 0.7372(3) 0.3599(2) 0.0438(12) Uani 1 1 d . . . C51 C -0.5037(4) 0.8079(3) 0.3383(2) 0.0468(12) Uani 1 1 d . . . C52 C -0.4785(5) 0.9241(4) 0.3031(3) 0.0681(19) Uani 1 1 d . . . H52A H -0.5152 0.9445 0.2832 0.082 Uiso 1 1 calc R . . H52B H -0.4530 0.9060 0.2733 0.082 Uiso 1 1 calc R . . C53 C -0.4083(6) 0.9873(5) 0.3467(4) 0.084(2) Uani 1 1 d . . . H53A H -0.4330 1.0123 0.3716 0.126 Uiso 1 1 calc R . . H53B H -0.3697 1.0242 0.3259 0.126 Uiso 1 1 calc R . . H53C H -0.3770 0.9661 0.3707 0.126 Uiso 1 1 calc R . . C54 C -0.5981(5) 0.8676(4) 0.3581(3) 0.0647(18) Uani 1 1 d . . . H54A H -0.5743 0.9174 0.3832 0.078 Uiso 1 1 calc R . . H54B H -0.6177 0.8283 0.3833 0.078 Uiso 1 1 calc R . . C55 C -0.6735(6) 0.8602(6) 0.3153(4) 0.087(3) Uani 1 1 d . . . H55A H -0.7148 0.8675 0.3365 0.130 Uiso 1 1 calc R . . H55B H -0.6999 0.8098 0.2919 0.130 Uiso 1 1 calc R . . H55C H -0.6547 0.8984 0.2897 0.130 Uiso 1 1 calc R . . C56 C 0.2501(5) 0.4051(4) 0.8507(3) 0.0635(17) Uani 1 1 d . . . H56A H 0.3124 0.4317 0.8551 0.076 Uiso 1 1 calc R . . H56B H 0.2278 0.3753 0.8112 0.076 Uiso 1 1 calc R . . C57 C 0.2264(8) 0.3536(6) 0.8949(5) 0.109(4) Uani 1 1 d . . . H57A H 0.2475 0.3834 0.9339 0.163 Uiso 1 1 calc R . . H57B H 0.2514 0.3179 0.8905 0.163 Uiso 1 1 calc R . . H57C H 0.1647 0.3257 0.8894 0.163 Uiso 1 1 calc R . . C58 C 0.4494(3) 1.0565(3) 0.9116(2) 0.0407(11) Uani 1 1 d . . . H58A H 0.5019 1.1033 0.9139 0.049 Uiso 1 1 calc R . . H58B H 0.4204 1.0639 0.9437 0.049 Uiso 1 1 calc R . . C59 C 0.3923(4) 1.0424(4) 0.8539(3) 0.0548(15) Uani 1 1 d . . . H59A H 0.3390 0.9977 0.8525 0.082 Uiso 1 1 calc R . . H59B H 0.4204 1.0341 0.8221 0.082 Uiso 1 1 calc R . . H59C H 0.3808 1.0864 0.8499 0.082 Uiso 1 1 calc R . . C60 C -0.0827(4) 0.3603(4) 0.5627(3) 0.0553(15) Uani 1 1 d . . . H60A H -0.1304 0.3441 0.5300 0.066 Uiso 1 1 calc R . . H60B H -0.0851 0.3147 0.5784 0.066 Uiso 1 1 calc R . . C61 C -0.0013(5) 0.3976(6) 0.5409(3) 0.080(3) Uani 1 1 d . . . H61A H 0.0461 0.4105 0.5727 0.121 Uiso 1 1 calc R . . H61B H 0.0021 0.4437 0.5266 0.121 Uiso 1 1 calc R . . H61C H 0.0015 0.3631 0.5093 0.121 Uiso 1 1 calc R . . C62 C -0.5911(4) 0.5627(4) 0.5285(3) 0.0587(16) Uani 1 1 d . . . H62A H -0.5931 0.5185 0.5464 0.070 Uiso 1 1 calc R . . H62B H -0.6393 0.5446 0.4960 0.070 Uiso 1 1 calc R . . C63 C -0.5993(7) 0.6175(6) 0.5725(5) 0.115(4) Uani 1 1 d . . . H63A H -0.5457 0.6447 0.5996 0.172 Uiso 1 1 calc R . . H63B H -0.6442 0.5903 0.5940 0.172 Uiso 1 1 calc R . . H63C H -0.6133 0.6536 0.5529 0.172 Uiso 1 1 calc R . . N1S N 0.1363(7) -0.0923(6) 0.2769(5) 0.125(3) Uani 1 1 d . . . C2S C 0.1869(6) -0.0339(7) 0.2839(4) 0.085(2) Uani 1 1 d . . . C3S C 0.2498(7) 0.0431(7) 0.2922(4) 0.121(5) Uani 1 1 d . . . H3SA H 0.2768 0.0590 0.3331 0.181 Uiso 1 1 calc R . . H3SB H 0.2230 0.0756 0.2812 0.181 Uiso 1 1 calc R . . H3SC H 0.2926 0.0471 0.2679 0.181 Uiso 1 1 calc R . . N4SA N 0.3240(10) 0.7416(9) 0.4774(7) 0.127(3) Uiso 0.727(14) 1 d P C 1 C5SA C 0.3109(15) 0.7827(14) 0.5025(10) 0.127(3) Uiso 0.727(14) 1 d P C 1 C6SA C 0.2902(14) 0.8366(12) 0.5349(9) 0.127(3) Uiso 0.727(14) 1 d P C 1 H6SA H 0.2660 0.8602 0.5079 0.191 Uiso 0.727(14) 1 calc PR C 1 H6SB H 0.3417 0.8755 0.5595 0.191 Uiso 0.727(14) 1 calc PR C 1 H6SC H 0.2491 0.8107 0.5594 0.191 Uiso 0.727(14) 1 calc PR C 1 C5SB C 0.285(4) 0.797(3) 0.490(3) 0.127(3) Uiso 0.273(14) 1 d P C 2 N4SB N 0.265(3) 0.767(2) 0.4359(19) 0.127(3) Uiso 0.273(14) 1 d P C 2 C6SB C 0.242(4) 0.831(3) 0.532(2) 0.127(3) Uiso 0.273(14) 1 d P C 2 H6SD H 0.1809 0.7990 0.5254 0.191 Uiso 0.273(14) 1 calc PR C 2 H6SE H 0.2520 0.8823 0.5246 0.191 Uiso 0.273(14) 1 calc PR C 2 H6SF H 0.2658 0.8340 0.5726 0.191 Uiso 0.273(14) 1 calc PR C 2 N7S N 1.1077(11) 0.8332(9) 0.4250(7) 0.181(6) Uiso 1 1 d . . . C8S C 1.0429(11) 0.8413(9) 0.4237(7) 0.140(5) Uiso 1 1 d . . . C9S C 0.9782(12) 0.8646(11) 0.4112(8) 0.190(8) Uiso 1 1 d . . . H9SA H 0.9297 0.8238 0.3854 0.285 Uiso 1 1 calc R . . H9SB H 0.9993 0.9095 0.3921 0.285 Uiso 1 1 calc R . . H9SC H 0.9605 0.8767 0.4473 0.285 Uiso 1 1 calc R . . N10S N 0.4193(8) 0.7627(7) 0.1892(4) 0.138(5) Uani 1 1 d . . . C11S C 0.4569(6) 0.7302(5) 0.1926(3) 0.0706(19) Uani 1 1 d . . . C12S C 0.5063(7) 0.6886(6) 0.1991(4) 0.096(3) Uani 1 1 d . . . H12A H 0.5016 0.6599 0.1614 0.144 Uiso 1 1 calc R . . H12B H 0.4855 0.6536 0.2268 0.144 Uiso 1 1 calc R . . H12C H 0.5657 0.7237 0.2134 0.144 Uiso 1 1 calc R . . N13S N 0.5210(11) 0.5396(10) 0.0872(7) 0.184(6) Uiso 1 1 d . . . C14S C 0.4648(12) 0.4847(11) 0.0851(7) 0.148(5) Uiso 1 1 d . . . C15S C 0.4008(12) 0.4108(11) 0.0896(8) 0.184(7) Uiso 1 1 d . . . H15A H 0.4186 0.3722 0.0758 0.276 Uiso 1 1 calc R . . H15B H 0.3472 0.4019 0.0658 0.276 Uiso 1 1 calc R . . H15C H 0.3934 0.4083 0.1302 0.276 Uiso 1 1 calc R . . C191 C 0.862(2) 0.525(2) 0.9777(15) 0.152(11) Uiso 0.50 1 d PD . . N15 N 0.911(2) 0.508(2) 0.9924(17) 0.226(16) Uiso 0.50 1 d PD . . C192 C 0.7973(19) 0.5416(18) 0.9558(14) 0.151(11) Uiso 0.50 1 d PD . . H19A H 0.8113 0.5666 0.9217 0.227 Uiso 0.50 1 calc PR . . H19B H 0.7893 0.5752 0.9855 0.227 Uiso 0.50 1 calc PR . . H19C H 0.7451 0.4948 0.9445 0.227 Uiso 0.50 1 calc PR . . F30A F 0.9192(10) 0.7974(9) 0.9205(7) 0.1231(19) Uiso 0.462(8) 1 d P B 6 F29A F 0.8828(11) 0.8511(10) 0.9858(8) 0.1231(19) Uiso 0.462(8) 1 d P B 6 F28A F 0.8071(9) 0.7532(8) 0.9898(6) 0.1231(19) Uiso 0.538(8) 1 d P B 5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.03491(15) 0.03399(13) 0.02873(13) 0.00218(10) 0.00096(10) 0.01784(11) Eu2 0.03560(15) 0.03902(14) 0.03337(14) 0.00453(10) 0.00489(10) 0.02355(12) Eu3 0.03801(16) 0.04030(15) 0.03881(15) 0.00698(11) 0.00619(11) 0.02253(12) F1 0.132(5) 0.232(9) 0.039(2) 0.003(3) 0.001(3) 0.078(6) F2 0.232(8) 0.097(4) 0.076(3) 0.003(3) 0.084(5) -0.017(5) F3 0.160(6) 0.122(5) 0.093(4) -0.008(3) 0.054(4) 0.072(5) F4 0.311(12) 0.059(3) 0.078(4) 0.001(3) -0.008(5) -0.042(5) F5 0.088(4) 0.072(3) 0.141(5) -0.049(3) 0.027(3) 0.009(3) F6 0.065(3) 0.164(6) 0.156(6) -0.092(5) -0.048(4) 0.041(4) F7 0.098(5) 0.286(11) 0.143(6) 0.085(7) 0.023(4) 0.124(7) F8 0.070(4) 0.227(10) 0.261(10) 0.125(8) 0.071(5) 0.085(5) F9 0.147(7) 0.196(9) 0.260(11) -0.026(8) 0.025(7) 0.136(8) F10 0.229(9) 0.062(3) 0.142(5) 0.029(3) 0.115(6) 0.047(4) F11 0.137(5) 0.089(4) 0.140(5) 0.051(3) 0.093(4) 0.039(4) F12 0.141(6) 0.138(6) 0.239(10) 0.132(7) 0.059(6) 0.066(5) F16 0.090(4) 0.324(13) 0.083(4) 0.031(5) 0.037(3) 0.101(6) F17 0.358(16) 0.169(9) 0.096(5) -0.060(6) 0.024(7) 0.108(10) F18 0.148(6) 0.325(11) 0.045(2) -0.034(4) -0.020(3) 0.177(7) F19 0.084(4) 0.077(3) 0.181(6) 0.030(4) 0.075(4) 0.017(3) F20 0.133(5) 0.059(3) 0.073(3) -0.006(2) 0.009(3) 0.005(3) F21 0.130(5) 0.053(3) 0.148(5) 0.031(3) -0.032(4) 0.027(3) F22 0.083(4) 0.158(6) 0.115(4) 0.075(4) -0.041(3) 0.011(4) F23 0.211(8) 0.141(6) 0.070(3) 0.040(3) 0.055(4) 0.092(6) F24 0.139(5) 0.069(3) 0.076(3) 0.028(2) -0.017(3) 0.038(3) F25 0.197(10) 0.239(12) 0.167(8) -0.140(9) 0.088(7) -0.066(9) F26 0.58(3) 0.231(11) 0.071(4) 0.041(6) 0.107(8) 0.285(16) F27 0.230(10) 0.376(16) 0.105(5) -0.072(7) 0.003(6) 0.235(12) F31 0.120(5) 0.121(5) 0.290(11) -0.110(7) -0.114(7) 0.077(5) F32 0.068(3) 0.151(6) 0.098(4) 0.004(4) 0.008(3) 0.007(3) F33 0.082(4) 0.182(7) 0.082(4) 0.019(4) -0.038(3) 0.018(4) F34 0.225(9) 0.087(4) 0.118(5) 0.048(4) 0.059(5) 0.068(5) F35 0.091(4) 0.136(5) 0.117(4) 0.066(4) 0.046(3) 0.054(4) F36 0.089(4) 0.211(8) 0.174(7) 0.144(6) -0.014(4) 0.033(5) F37 0.081(5) 0.384(18) 0.135(7) -0.044(9) -0.021(5) 0.097(8) F38 0.243(11) 0.102(5) 0.328(14) -0.006(7) -0.218(11) 0.065(6) F39 0.112(5) 0.149(6) 0.118(5) -0.068(5) -0.055(4) 0.062(5) F40 0.339(12) 0.256(10) 0.105(4) 0.076(5) 0.092(6) 0.270(11) F41 0.171(8) 0.172(8) 0.307(13) 0.045(9) 0.145(9) 0.114(7) F42 0.223(10) 0.267(11) 0.136(6) -0.110(7) -0.053(6) 0.199(10) F43 0.078(3) 0.154(5) 0.114(4) 0.008(4) -0.010(3) 0.082(4) F44 0.189(8) 0.59(2) 0.140(6) 0.189(10) 0.114(6) 0.307(12) F45 0.107(5) 0.104(5) 0.303(12) -0.002(6) -0.061(6) 0.076(4) F46 0.146(5) 0.081(3) 0.052(2) 0.000(2) -0.015(3) 0.021(3) F47 0.047(2) 0.082(3) 0.147(5) -0.020(3) -0.009(3) 0.024(2) F48 0.085(3) 0.048(2) 0.102(3) 0.004(2) 0.005(3) 0.027(2) F49 0.107(6) 0.065(4) 0.61(3) -0.097(8) -0.053(10) 0.039(4) F50 0.258(13) 0.097(5) 0.149(8) -0.024(5) -0.025(8) -0.028(6) F51 0.186(9) 0.080(4) 0.228(10) 0.002(5) 0.084(8) -0.021(5) F52 0.151(7) 0.259(11) 0.086(4) -0.039(6) 0.046(5) 0.063(7) F53 0.365(15) 0.164(8) 0.150(7) 0.080(6) 0.179(9) 0.136(9) F54 0.227(10) 0.379(16) 0.112(5) 0.002(7) 0.042(6) 0.245(12) O1 0.043(2) 0.049(2) 0.052(2) 0.0042(16) 0.0129(16) 0.0270(17) O1H 0.047(2) 0.0388(18) 0.0428(19) 0.0025(15) 0.0113(16) 0.0134(16) O2 0.047(2) 0.056(2) 0.045(2) 0.0164(17) 0.0070(16) 0.0303(19) O2H 0.046(2) 0.046(2) 0.0340(17) 0.0012(15) -0.0052(15) 0.0149(17) O3H 0.047(2) 0.045(2) 0.051(2) 0.0066(16) 0.0121(17) 0.0178(17) O4H 0.043(2) 0.059(2) 0.048(2) 0.0019(17) 0.0027(17) 0.0275(19) O5H 0.052(2) 0.068(3) 0.0375(19) -0.0103(18) 0.0011(16) 0.031(2) O6H 0.058(2) 0.0399(19) 0.057(2) 0.0000(17) -0.0070(19) 0.0264(18) O7H 0.049(2) 0.0448(19) 0.0401(19) 0.0033(15) 0.0039(16) 0.0195(17) O8H 0.045(2) 0.0442(19) 0.0374(18) 0.0043(15) -0.0022(15) 0.0214(16) O9H 0.047(2) 0.052(2) 0.053(2) -0.0023(17) 0.0085(17) 0.0301(19) O10H 0.054(2) 0.067(3) 0.054(2) 0.0125(19) 0.0083(18) 0.047(2) O11H 0.053(2) 0.054(2) 0.043(2) 0.0014(16) -0.0026(17) 0.0335(19) O12H 0.051(2) 0.066(2) 0.0391(19) 0.0161(17) 0.0055(16) 0.032(2) O13H 0.061(3) 0.058(2) 0.051(2) 0.0028(19) 0.0006(19) 0.035(2) O14H 0.056(3) 0.060(2) 0.053(2) 0.0034(19) 0.0102(19) 0.033(2) O15H 0.040(2) 0.053(2) 0.051(2) 0.0080(17) 0.0075(16) 0.0277(17) O16H 0.046(2) 0.050(2) 0.0434(19) 0.0048(16) 0.0040(16) 0.0282(17) O17H 0.068(3) 0.046(2) 0.061(3) 0.0093(19) 0.015(2) 0.022(2) O18H 0.058(2) 0.055(2) 0.046(2) 0.0111(17) 0.0136(18) 0.031(2) N1 0.035(2) 0.037(2) 0.0354(19) 0.0064(16) 0.0039(16) 0.0183(17) N2 0.035(2) 0.042(2) 0.0332(19) 0.0084(16) 0.0002(16) 0.0183(18) N3 0.046(3) 0.051(3) 0.047(2) 0.011(2) 0.002(2) 0.027(2) N4 0.038(2) 0.040(2) 0.0340(19) 0.0022(16) 0.0027(16) 0.0213(18) N5 0.035(2) 0.043(2) 0.0345(19) -0.0010(16) 0.0016(16) 0.0244(18) N6 0.035(2) 0.042(2) 0.0304(18) 0.0025(16) 0.0026(15) 0.0215(18) N7 0.033(2) 0.053(3) 0.051(2) 0.006(2) 0.0071(19) 0.020(2) N8 0.038(2) 0.043(2) 0.0308(19) 0.0058(16) 0.0022(16) 0.0189(18) N9 0.043(2) 0.044(2) 0.035(2) -0.0009(17) 0.0011(17) 0.0209(19) N10 0.041(2) 0.048(2) 0.043(2) 0.0115(18) 0.0061(18) 0.027(2) N11 0.044(2) 0.055(3) 0.046(2) 0.016(2) 0.0144(19) 0.030(2) N12 0.046(2) 0.050(2) 0.039(2) 0.0076(18) 0.0061(18) 0.033(2) N13 0.071(3) 0.060(3) 0.047(3) 0.012(2) 0.007(2) 0.046(3) C1 0.038(3) 0.041(2) 0.037(2) 0.0071(19) 0.006(2) 0.019(2) C1H 0.053(3) 0.050(3) 0.040(3) 0.004(2) 0.007(2) 0.018(3) C2 0.057(3) 0.043(3) 0.049(3) 0.009(2) 0.010(2) 0.029(3) C2H 0.050(3) 0.046(3) 0.042(3) 0.004(2) 0.008(2) 0.012(2) C3 0.061(4) 0.036(3) 0.055(3) 0.006(2) 0.011(3) 0.025(3) C3H 0.040(3) 0.045(3) 0.041(3) 0.006(2) 0.000(2) 0.015(2) C4 0.051(3) 0.039(3) 0.050(3) 0.000(2) 0.008(2) 0.021(2) C4H 0.075(5) 0.063(4) 0.058(4) -0.002(3) 0.025(4) 0.009(4) C5 0.044(3) 0.042(3) 0.043(3) 0.004(2) 0.007(2) 0.023(2) C5H 0.065(4) 0.053(3) 0.047(3) 0.001(3) -0.004(3) 0.008(3) C6 0.039(3) 0.044(3) 0.040(3) 0.013(2) 0.005(2) 0.020(2) C6H 0.051(4) 0.055(3) 0.062(4) 0.007(3) 0.023(3) 0.020(3) C7 0.040(3) 0.045(3) 0.036(2) 0.013(2) 0.002(2) 0.016(2) C7H 0.047(4) 0.076(5) 0.090(5) 0.019(4) 0.024(4) 0.016(3) C8 0.038(3) 0.046(3) 0.037(2) 0.010(2) 0.003(2) 0.016(2) C8H 0.042(3) 0.078(4) 0.064(4) -0.002(3) 0.006(3) 0.031(3) C9 0.039(3) 0.054(3) 0.033(2) 0.010(2) -0.001(2) 0.009(2) C9H 0.066(6) 0.161(11) 0.109(8) 0.031(7) 0.029(5) 0.069(7) C10 0.048(3) 0.073(4) 0.048(3) 0.016(3) -0.013(3) 0.021(3) C10H 0.090(6) 0.074(5) 0.087(6) 0.032(4) 0.044(5) 0.025(5) C11 0.047(3) 0.068(4) 0.062(4) 0.016(3) -0.006(3) 0.030(3) C11H 0.044(3) 0.087(5) 0.061(4) -0.025(4) -0.003(3) 0.033(3) C12 0.042(3) 0.055(3) 0.046(3) 0.016(2) 0.001(2) 0.023(3) C12H 0.074(5) 0.069(4) 0.087(5) -0.026(4) -0.016(4) 0.050(4) C13 0.048(3) 0.063(3) 0.034(2) 0.009(2) 0.003(2) 0.017(3) C13H 0.058(4) 0.056(4) 0.082(5) -0.008(3) -0.016(3) 0.034(3) C14 0.036(3) 0.052(3) 0.029(2) 0.001(2) 0.0012(19) 0.012(2) C14H 0.129(9) 0.053(4) 0.138(9) -0.022(5) -0.059(7) 0.065(5) C15 0.036(3) 0.047(3) 0.031(2) -0.0010(19) -0.0014(18) 0.020(2) C15H 0.073(5) 0.150(9) 0.073(5) -0.046(6) -0.002(4) 0.070(6) C16 0.034(2) 0.047(3) 0.027(2) -0.0008(19) 0.0000(18) 0.021(2) C16H 0.042(3) 0.046(3) 0.049(3) 0.006(2) 0.011(2) 0.022(2) C17 0.035(3) 0.049(3) 0.031(2) -0.0044(19) -0.0005(18) 0.023(2) C17H 0.046(3) 0.051(3) 0.044(3) 0.003(2) 0.000(2) 0.016(3) C18 0.041(3) 0.061(3) 0.040(3) -0.002(2) 0.005(2) 0.029(3) C18H 0.044(3) 0.050(3) 0.045(3) 0.007(2) 0.003(2) 0.023(2) C19 0.038(3) 0.065(3) 0.037(3) -0.001(2) 0.006(2) 0.021(3) C19H 0.085(5) 0.062(4) 0.052(4) 0.015(3) -0.006(3) 0.024(4) C20 0.030(2) 0.040(2) 0.032(2) 0.0013(18) 0.0004(17) 0.0194(19) C20H 0.057(4) 0.049(3) 0.061(4) 0.005(3) 0.007(3) 0.019(3) C21 0.035(2) 0.041(2) 0.033(2) -0.0010(18) -0.0004(18) 0.021(2) C21H 0.059(4) 0.049(3) 0.060(4) -0.002(3) 0.019(3) 0.030(3) C22 0.045(3) 0.050(3) 0.045(3) 0.009(2) 0.005(2) 0.031(2) C22H 0.082(5) 0.110(6) 0.075(5) -0.003(4) 0.014(4) 0.077(5) C23 0.051(3) 0.047(3) 0.052(3) 0.012(2) 0.007(3) 0.024(3) C23H 0.062(4) 0.072(4) 0.075(4) 0.009(3) 0.011(3) 0.049(4) C24 0.041(3) 0.044(3) 0.049(3) 0.010(2) 0.010(2) 0.016(2) C24H 0.120(9) 0.135(10) 0.157(11) 0.027(8) 0.034(8) 0.113(9) C25 0.033(2) 0.045(3) 0.038(2) 0.004(2) 0.0035(19) 0.020(2) C25H 0.085(6) 0.082(5) 0.064(4) -0.014(4) 0.012(4) 0.049(5) C26 0.044(3) 0.056(3) 0.038(2) 0.010(2) 0.015(2) 0.030(3) C26H 0.048(3) 0.072(4) 0.042(3) -0.005(3) -0.002(2) 0.041(3) C27 0.038(3) 0.065(4) 0.058(3) -0.008(3) 0.000(3) 0.019(3) C27H 0.059(4) 0.090(5) 0.038(3) 0.013(3) 0.001(3) 0.048(4) C28 0.051(4) 0.065(4) 0.109(6) 0.007(4) 0.025(4) 0.010(3) C28H 0.054(4) 0.075(4) 0.050(3) 0.019(3) 0.011(3) 0.045(3) C29 0.044(3) 0.069(4) 0.072(4) 0.006(3) 0.005(3) 0.034(3) C29H 0.086(5) 0.092(6) 0.058(4) 0.035(4) 0.014(4) 0.052(5) C30 0.061(4) 0.094(6) 0.090(5) 0.001(4) 0.017(4) 0.052(4) C30H 0.054(4) 0.097(6) 0.063(4) -0.006(4) -0.011(3) 0.040(4) C31 0.033(2) 0.035(2) 0.037(2) -0.0002(18) 0.0013(19) 0.0149(19) C31H 0.062(4) 0.070(4) 0.048(3) 0.002(3) -0.001(3) 0.034(3) C32 0.027(2) 0.040(2) 0.036(2) -0.0011(19) -0.0012(18) 0.0098(19) C32H 0.082(5) 0.065(4) 0.046(3) -0.009(3) 0.004(3) 0.036(4) C33 0.037(3) 0.047(3) 0.035(2) 0.001(2) -0.0030(19) 0.020(2) C33H 0.077(5) 0.062(4) 0.044(3) 0.006(3) 0.015(3) 0.035(3) C34 0.041(3) 0.053(3) 0.040(3) 0.003(2) -0.003(2) 0.026(2) C34H 0.103(6) 0.092(5) 0.051(4) 0.004(4) 0.023(4) 0.067(5) C35 0.041(3) 0.060(3) 0.037(3) 0.005(2) 0.000(2) 0.024(3) C35H 0.072(6) 0.087(6) 0.086(6) -0.018(5) -0.018(4) 0.039(5) C36 0.048(3) 0.059(3) 0.033(2) -0.001(2) 0.002(2) 0.029(3) C36H 0.047(3) 0.048(3) 0.044(3) 0.008(2) 0.009(2) 0.027(2) C37 0.036(3) 0.046(3) 0.035(2) 0.002(2) 0.0014(19) 0.021(2) C37H 0.060(4) 0.050(3) 0.076(4) 0.000(3) 0.002(3) 0.038(3) C38 0.055(3) 0.052(3) 0.046(3) 0.006(2) -0.009(2) 0.030(3) C38H 0.050(3) 0.063(4) 0.052(3) 0.017(3) 0.014(3) 0.036(3) C39 0.051(3) 0.048(3) 0.038(3) 0.002(2) -0.002(2) 0.029(3) C39H 0.065(4) 0.087(5) 0.068(4) 0.004(4) 0.003(3) 0.057(4) C40 0.046(3) 0.051(3) 0.037(2) 0.006(2) 0.002(2) 0.028(2) C40H 0.065(4) 0.057(4) 0.053(3) 0.002(3) 0.005(3) 0.028(3) C41 0.047(3) 0.049(3) 0.029(2) 0.0069(19) 0.004(2) 0.030(2) C41H 0.070(5) 0.055(4) 0.066(4) 0.014(3) 0.012(3) 0.022(3) C42 0.054(3) 0.049(3) 0.038(2) 0.011(2) 0.011(2) 0.033(3) C42H 0.088(6) 0.068(5) 0.081(5) 0.022(4) 0.039(4) 0.025(4) C43 0.063(4) 0.059(3) 0.042(3) 0.018(2) 0.015(3) 0.036(3) C43H 0.068(4) 0.080(5) 0.053(3) 0.022(3) 0.020(3) 0.041(4) C44 0.068(4) 0.063(3) 0.036(3) 0.014(2) 0.008(2) 0.042(3) C44H 0.084(6) 0.112(7) 0.061(5) 0.017(5) 0.029(4) 0.040(6) C45 0.039(3) 0.044(3) 0.045(3) 0.012(2) 0.009(2) 0.024(2) C45H 0.116(8) 0.055(5) 0.105(8) 0.013(5) 0.025(6) 0.008(5) C46 0.039(3) 0.050(3) 0.048(3) 0.009(2) 0.010(2) 0.028(2) C47 0.044(3) 0.058(3) 0.066(4) 0.018(3) 0.011(3) 0.026(3) C48 0.039(3) 0.075(4) 0.072(4) 0.017(3) 0.006(3) 0.023(3) C49 0.043(3) 0.072(4) 0.063(4) 0.018(3) 0.002(3) 0.036(3) C50 0.047(3) 0.057(3) 0.043(3) 0.010(2) 0.009(2) 0.037(3) C51 0.057(4) 0.051(3) 0.039(3) 0.008(2) 0.000(2) 0.032(3) C52 0.090(5) 0.064(4) 0.063(4) 0.022(3) 0.004(4) 0.046(4) C53 0.086(6) 0.060(4) 0.096(6) 0.011(4) -0.011(5) 0.029(4) C54 0.084(5) 0.077(4) 0.059(4) 0.009(3) 0.008(3) 0.061(4) C55 0.104(7) 0.116(7) 0.075(5) 0.014(5) -0.001(5) 0.086(6) C56 0.054(4) 0.065(4) 0.079(4) 0.011(3) 0.001(3) 0.036(3) C57 0.130(9) 0.085(6) 0.118(8) 0.016(6) -0.023(7) 0.064(7) C58 0.042(3) 0.046(3) 0.040(2) -0.003(2) -0.002(2) 0.029(2) C59 0.054(4) 0.065(4) 0.051(3) 0.005(3) -0.010(3) 0.038(3) C60 0.073(4) 0.058(3) 0.041(3) -0.011(2) -0.002(3) 0.040(3) C61 0.067(5) 0.121(7) 0.065(4) -0.020(4) 0.003(4) 0.062(5) C62 0.050(4) 0.078(4) 0.060(4) 0.027(3) 0.025(3) 0.032(3) C63 0.124(9) 0.112(8) 0.145(9) 0.027(7) 0.092(8) 0.066(7) N1S 0.122(8) 0.098(7) 0.138(9) 0.026(6) 0.006(7) 0.034(6) C2S 0.079(6) 0.109(7) 0.066(5) 0.017(5) 0.013(4) 0.038(6) C3S 0.102(8) 0.148(11) 0.059(5) 0.017(6) 0.014(5) 0.003(7) N10S 0.183(11) 0.157(9) 0.112(7) -0.014(7) -0.041(7) 0.133(9) C11S 0.088(5) 0.076(5) 0.064(4) 0.015(3) 0.002(4) 0.053(4) C12S 0.130(9) 0.136(9) 0.069(5) 0.029(5) 0.017(5) 0.101(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O5H 2.372(4) . ? Eu1 O6H 2.402(4) . ? Eu1 O3H 2.402(4) . ? Eu1 O1H 2.410(4) . ? Eu1 O2H 2.471(4) . ? Eu1 O4H 2.482(4) . ? Eu1 N2 2.525(4) . ? Eu1 N8 2.547(4) . ? Eu1 N1 2.643(4) . ? Eu2 O7H 2.387(4) . ? Eu2 O10H 2.396(4) . ? Eu2 O12H 2.409(4) . ? Eu2 O1 2.412(4) . ? Eu2 O9H 2.434(4) . ? Eu2 O8H 2.446(3) . ? Eu2 O11H 2.469(4) . ? Eu2 N4 2.567(4) . ? Eu2 N6 2.593(4) . ? Eu2 C26 3.218(6) . ? Eu3 O13H 2.399(4) . ? Eu3 O15H 2.409(4) . ? Eu3 O2 2.422(4) . ? Eu3 O16H 2.425(4) . ? Eu3 O14H 2.425(4) . ? Eu3 O18H 2.435(4) . ? Eu3 O17H 2.435(4) . ? Eu3 N10 2.598(4) . ? Eu3 N12 2.611(5) . ? Eu3 C51 3.224(6) . ? F1 C4H 1.294(10) . ? F2 C4H 1.287(9) . ? F3 C4H 1.325(10) . ? F4 C5H 1.278(9) . ? F5 C5H 1.284(9) . ? F6 C5H 1.300(10) . ? F7 C9H 1.308(13) . ? F8 C9H 1.293(14) . ? F9 C9H 1.266(15) . ? F10 C10H 1.305(11) . ? F11 C10H 1.287(9) . ? F12 C10H 1.345(12) . ? F14A C14H 1.396(17) . ? F15A C14H 1.284(18) . ? F13A C14H 1.261(16) . ? F13B C14H 1.372(17) . ? F14B C14H 1.185(16) . ? F15B C14H 1.431(18) . ? F16 C15H 1.223(12) . ? F17 C15H 1.352(14) . ? F18 C15H 1.259(11) . ? F19 C20H 1.309(9) . ? F20 C20H 1.326(8) . ? F21 C20H 1.275(8) . ? F22 C19H 1.292(9) . ? F23 C19H 1.380(10) . ? F24 C19H 1.277(9) . ? F25 C25H 1.230(12) . ? F26 C25H 1.189(12) . ? F27 C25H 1.238(10) . ? F28B C24H 1.15(2) . ? F29B C24H 1.104(18) . ? F30B C24H 1.375(16) . ? F31 C30H 1.281(10) . ? F32 C30H 1.293(10) . ? F33 C30H 1.318(10) . ? F34 C29H 1.336(11) . ? F35 C29H 1.339(10) . ? F36 C29H 1.274(9) . ? F37 C35H 1.296(14) . ? F38 C35H 1.234(12) . ? F39 C35H 1.262(10) . ? F40 C34H 1.233(9) . ? F41 C34H 1.292(13) . ? F42 C34H 1.257(10) . ? F43 C39H 1.315(9) . ? F44 C39H 1.211(10) . ? F45 C39H 1.307(11) . ? F46 C40H 1.300(8) . ? F47 C40H 1.335(9) . ? F48 C40H 1.329(8) . ? F49 C45H 1.194(14) . ? F50 C45H 1.293(14) . ? F51 C45H 1.272(13) . ? F52 C44H 1.261(12) . ? F53 C44H 1.294(12) . ? F54 C44H 1.244(12) . ? O1 C26 1.248(7) . ? O1H C1H 1.243(7) . ? O2 C51 1.264(7) . ? O2H C3H 1.238(7) . ? O3H C6H 1.241(7) . ? O4H C8H 1.217(9) . ? O5H C11H 1.264(9) . ? O6H C13H 1.236(8) . ? O7H C16H 1.256(7) . ? O8H C18H 1.243(7) . ? O9H C21H 1.243(7) . ? O10H C23H 1.242(7) . ? O11H C26H 1.260(7) . ? O12H C28H 1.235(7) . ? O13H C31H 1.243(8) . ? O14H C33H 1.247(8) . ? O15H C38H 1.241(7) . ? O16H C36H 1.249(7) . ? O17H C41H 1.230(9) . ? O18H C43H 1.228(9) . ? N1 C1 1.340(6) . ? N1 C5 1.350(7) . ? N2 C6 1.336(7) . ? N2 C7 1.398(6) . ? N3 C6 1.353(7) . ? N3 C12 1.397(8) . ? N3 C56 1.467(8) . ? N4 C20 1.322(6) . ? N4 C16 1.396(7) . ? N5 C20 1.374(6) . ? N5 C17 1.389(7) . ? N5 C58 1.465(6) . ? N6 C25 1.335(7) . ? N6 C21 1.354(6) . ? N7 C26 1.337(7) . ? N7 C29 1.476(7) . ? N7 C27 1.481(8) . ? N8 C31 1.328(6) . ? N8 C32 1.407(6) . ? N9 C31 1.360(6) . ? N9 C37 1.393(7) . ? N9 C60 1.479(6) . ? N10 C45 1.335(7) . ? N10 C41 1.380(6) . ? N11 C45 1.360(7) . ? N11 C42 1.388(7) . ? N11 C62 1.478(7) . ? N12 C50 1.334(6) . ? N12 C46 1.335(7) . ? N13 C51 1.324(7) . ? N13 C52 1.461(9) . ? N13 C54 1.484(9) . ? C1 C2 1.398(7) . ? C1 C6 1.487(7) . ? C1H C2H 1.366(8) . ? C1H C4H 1.529(9) . ? C2 C3 1.392(9) . ? C2 H2 0.9500 . ? C2H C3H 1.390(8) . ? C2H H2H 0.9500 . ? C3 C4 1.380(8) . ? C3 H3 0.9500 . ? C3H C5H 1.536(8) . ? C4 C5 1.390(7) . ? C4 H4 0.9500 . ? C5 C31 1.463(7) . ? C6H C7H 1.397(10) . ? C6H C10H 1.529(11) . ? C7 C8 1.389(8) . ? C7 C12 1.394(8) . ? C7H C8H 1.385(11) . ? C7H H7H 0.9500 . ? C8 C9 1.392(7) . ? C8 H8 0.9500 . ? C8H C9H 1.544(11) . ? C9 C10 1.412(9) . ? C9 C13 1.510(8) . ? C10 C11 1.388(10) . ? C10 H10 0.9500 . ? C11 C12 1.391(8) . ? C11 H11 0.9500 . ? C11H C12H 1.395(12) . ? C11H C15H 1.527(10) . ? C12H C13H 1.393(11) . ? C12H H12 0.9500 . ? C13 C14 1.509(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13H C14H 1.551(11) . ? C14 C15 1.393(7) . ? C14 C19 1.418(8) . ? C15 C16 1.389(8) . ? C15 H15 0.9500 . ? C16 C17 1.407(7) . ? C16H C17H 1.389(8) . ? C16H C20H 1.543(8) . ? C17 C18 1.384(8) . ? C17H C18H 1.374(8) . ? C17H H17 0.9500 . ? C18 C19 1.376(9) . ? C18 H18 0.9500 . ? C18H C19H 1.536(9) . ? C19 H19 0.9500 . ? C20 C21 1.470(7) . ? C21 C22 1.375(7) . ? C21H C22H 1.376(10) . ? C21H C25H 1.528(9) . ? C22 C23 1.389(8) . ? C22 H22 0.9500 . ? C22H C23H 1.372(10) . ? C22H H22A 0.9500 . ? C23 C24 1.384(8) . ? C23 H23 0.9500 . ? C23H C24H 1.573(13) . ? C24 C25 1.381(7) . ? C24 H24 0.9500 . ? C24H F30A 1.36(2) . ? C24H F29A 1.42(2) . ? C24H F28A 1.43(2) . ? C25 C26 1.512(7) . ? C26H C27H 1.366(10) . ? C26H C30H 1.545(10) . ? C27 C28 1.507(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27H C28H 1.395(10) . ? C27H H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28H C29H 1.524(10) . ? C29 C30 1.496(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31H C32H 1.388(10) . ? C31H C35H 1.544(10) . ? C32 C33 1.381(7) . ? C32 C37 1.386(7) . ? C32H C33H 1.369(10) . ? C32H H32 0.9500 . ? C33 C34 1.389(7) . ? C33 H33 0.9500 . ? C33H C34H 1.554(9) . ? C34 C35 1.408(8) . ? C34 C38 1.526(7) . ? C35 C36 1.372(8) . ? C35 H35 0.9500 . ? C36 C37 1.405(7) . ? C36 H36 0.9500 . ? C36H C37H 1.390(8) . ? C36H C40H 1.540(9) . ? C37H C38H 1.379(9) . ? C37H H37 0.9500 . ? C38 C39 1.517(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38H C39H 1.539(8) . ? C39 C40 1.387(7) . ? C39 C44 1.413(9) . ? C40 C41 1.393(8) . ? C40 H40 0.9500 . ? C41 C42 1.398(8) . ? C41H C42H 1.380(11) . ? C41H C45H 1.551(11) . ? C42 C43 1.388(7) . ? C42H C43H 1.388(11) . ? C42H H42 0.9500 . ? C43 C44 1.381(9) . ? C43 H43 0.9500 . ? C43H C44H 1.538(10) . ? C44 H44 0.9500 . ? C45 C46 1.475(7) . ? C46 C47 1.396(8) . ? C47 C48 1.379(9) . ? C47 H47 0.9500 . ? C48 C49 1.373(10) . ? C48 H48 0.9500 . ? C49 C50 1.383(9) . ? C49 H49 0.9500 . ? C50 C51 1.498(8) . ? C52 C53 1.523(11) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.518(10) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.491(13) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.518(7) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C61 1.491(11) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.488(11) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? N1S C2S 1.106(13) . ? C2S C3S 1.437(15) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? N4SA C5SA 1.07(2) . ? C5SA C6SA 1.44(3) . ? C6SA H6SA 0.9800 . ? C6SA H6SB 0.9800 . ? C6SA H6SC 0.9800 . ? C5SB N4SB 1.29(7) . ? C5SB C6SB 1.58(8) . ? C6SB H6SD 0.9800 . ? C6SB H6SE 0.9800 . ? C6SB H6SF 0.9800 . ? N7S C8S 1.217(19) . ? C8S C9S 1.41(2) . ? C9S H9SA 0.9800 . ? C9S H9SB 0.9800 . ? C9S H9SC 0.9800 . ? N10S C11S 1.101(11) . ? C11S C12S 1.432(10) . ? C12S H12A 0.9800 . ? C12S H12B 0.9800 . ? C12S H12C 0.9800 . ? N13S C14S 1.11(2) . ? C14S C15S 1.45(2) . ? C15S H15A 0.9800 . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? C191 N15 1.094(19) . ? C191 C192 1.364(18) . ? C192 H19A 0.9800 . ? C192 H19B 0.9800 . ? C192 H19C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5H Eu1 O6H 75.31(15) . . ? O5H Eu1 O3H 81.65(15) . . ? O6H Eu1 O3H 135.71(15) . . ? O5H Eu1 O1H 139.94(15) . . ? O6H Eu1 O1H 80.39(14) . . ? O3H Eu1 O1H 136.22(13) . . ? O5H Eu1 O2H 72.50(14) . . ? O6H Eu1 O2H 67.21(14) . . ? O3H Eu1 O2H 139.06(13) . . ? O1H Eu1 O2H 68.86(12) . . ? O5H Eu1 O4H 71.38(14) . . ? O6H Eu1 O4H 67.92(15) . . ? O3H Eu1 O4H 69.05(14) . . ? O1H Eu1 O4H 126.93(14) . . ? O2H Eu1 O4H 127.70(13) . . ? O5H Eu1 N2 82.67(14) . . ? O6H Eu1 N2 139.08(14) . . ? O3H Eu1 N2 72.14(14) . . ? O1H Eu1 N2 96.04(14) . . ? O2H Eu1 N2 73.49(13) . . ? O4H Eu1 N2 135.67(14) . . ? O5H Eu1 N8 141.41(14) . . ? O6H Eu1 N8 89.66(13) . . ? O3H Eu1 N8 85.35(14) . . ? O1H Eu1 N8 68.33(13) . . ? O2H Eu1 N8 133.95(13) . . ? O4H Eu1 N8 70.03(13) . . ? N2 Eu1 N8 127.14(13) . . ? O5H Eu1 N1 138.18(14) . . ? O6H Eu1 N1 146.51(13) . . ? O3H Eu1 N1 65.56(13) . . ? O1H Eu1 N1 71.42(12) . . ? O2H Eu1 N1 116.32(13) . . ? O4H Eu1 N1 115.88(13) . . ? N2 Eu1 N1 63.57(13) . . ? N8 Eu1 N1 63.58(13) . . ? O7H Eu2 O10H 100.52(15) . . ? O7H Eu2 O12H 74.27(14) . . ? O10H Eu2 O12H 69.36(14) . . ? O7H Eu2 O1 140.02(13) . . ? O10H Eu2 O1 76.52(14) . . ? O12H Eu2 O1 136.27(14) . . ? O7H Eu2 O9H 71.04(14) . . ? O10H Eu2 O9H 69.73(14) . . ? O12H Eu2 O9H 118.99(14) . . ? O1 Eu2 O9H 70.67(13) . . ? O7H Eu2 O8H 72.14(13) . . ? O10H Eu2 O8H 138.93(13) . . ? O12H Eu2 O8H 139.44(14) . . ? O1 Eu2 O8H 84.22(13) . . ? O9H Eu2 O8H 69.74(13) . . ? O7H Eu2 O11H 144.02(14) . . ? O10H Eu2 O11H 71.66(14) . . ? O12H Eu2 O11H 70.11(15) . . ? O1 Eu2 O11H 73.81(14) . . ? O9H Eu2 O11H 132.18(13) . . ? O8H Eu2 O11H 136.49(13) . . ? O7H Eu2 N4 80.73(13) . . ? O10H Eu2 N4 143.49(13) . . ? O12H Eu2 N4 76.12(13) . . ? O1 Eu2 N4 125.18(13) . . ? O9H Eu2 N4 141.15(13) . . ? O8H Eu2 N4 76.63(12) . . ? O11H Eu2 N4 85.96(13) . . ? O7H Eu2 N6 130.40(13) . . ? O10H Eu2 N6 129.02(15) . . ? O12H Eu2 N6 121.27(13) . . ? O1 Eu2 N6 63.38(12) . . ? O9H Eu2 N6 119.53(13) . . ? O8H Eu2 N6 68.61(12) . . ? O11H Eu2 N6 68.01(13) . . ? N4 Eu2 N6 61.81(13) . . ? O7H Eu2 C26 154.53(13) . . ? O10H Eu2 C26 87.57(15) . . ? O12H Eu2 C26 130.87(14) . . ? O1 Eu2 C26 19.68(12) . . ? O9H Eu2 C26 89.68(14) . . ? O8H Eu2 C26 85.84(13) . . ? O11H Eu2 C26 61.45(14) . . ? N4 Eu2 C26 106.99(13) . . ? N6 Eu2 C26 45.96(13) . . ? O13H Eu3 O15H 72.05(13) . . ? O13H Eu3 O2 140.61(14) . . ? O15H Eu3 O2 139.76(13) . . ? O13H Eu3 O16H 137.39(13) . . ? O15H Eu3 O16H 71.76(13) . . ? O2 Eu3 O16H 81.96(13) . . ? O13H Eu3 O14H 71.09(14) . . ? O15H Eu3 O14H 141.85(14) . . ? O2 Eu3 O14H 77.74(14) . . ? O16H Eu3 O14H 134.95(14) . . ? O13H Eu3 O18H 112.49(15) . . ? O15H Eu3 O18H 69.69(13) . . ? O2 Eu3 O18H 74.25(13) . . ? O16H Eu3 O18H 74.38(14) . . ? O14H Eu3 O18H 135.08(14) . . ? O13H Eu3 O17H 69.25(16) . . ? O15H Eu3 O17H 104.08(15) . . ? O2 Eu3 O17H 78.48(15) . . ? O16H Eu3 O17H 142.00(14) . . ? O14H Eu3 O17H 71.40(15) . . ? O18H Eu3 O17H 69.11(15) . . ? O13H Eu3 N10 75.92(15) . . ? O15H Eu3 N10 75.90(13) . . ? O2 Eu3 N10 125.77(14) . . ? O16H Eu3 N10 74.11(14) . . ? O14H Eu3 N10 85.97(14) . . ? O18H Eu3 N10 138.95(13) . . ? O17H Eu3 N10 142.97(15) . . ? O13H Eu3 N12 121.06(15) . . ? O15H Eu3 N12 127.44(14) . . ? O2 Eu3 N12 64.20(13) . . ? O16H Eu3 N12 67.91(13) . . ? O14H Eu3 N12 67.06(14) . . ? O18H Eu3 N12 126.43(14) . . ? O17H Eu3 N12 128.45(15) . . ? N10 Eu3 N12 61.79(14) . . ? O13H Eu3 C51 135.19(14) . . ? O15H Eu3 C51 152.76(14) . . ? O2 Eu3 C51 20.14(14) . . ? O16H Eu3 C51 83.09(13) . . ? O14H Eu3 C51 64.80(14) . . ? O18H Eu3 C51 93.96(14) . . ? O17H Eu3 C51 89.19(16) . . ? N10 Eu3 C51 107.60(15) . . ? N12 Eu3 C51 45.98(14) . . ? C26 O1 Eu2 119.7(3) . . ? C1H O1H Eu1 135.4(4) . . ? C51 O2 Eu3 118.6(3) . . ? C3H O2H Eu1 132.7(3) . . ? C6H O3H Eu1 137.9(4) . . ? C8H O4H Eu1 135.3(4) . . ? C11H O5H Eu1 131.7(5) . . ? C13H O6H Eu1 131.5(5) . . ? C16H O7H Eu2 132.9(4) . . ? C18H O8H Eu2 131.4(4) . . ? C21H O9H Eu2 135.2(4) . . ? C23H O10H Eu2 135.6(4) . . ? C26H O11H Eu2 130.3(4) . . ? C28H O12H Eu2 133.4(4) . . ? C31H O13H Eu3 134.6(4) . . ? C33H O14H Eu3 133.2(4) . . ? C38H O15H Eu3 134.3(4) . . ? C36H O16H Eu3 133.5(4) . . ? C41H O17H Eu3 136.9(5) . . ? C43H O18H Eu3 137.3(4) . . ? C1 N1 C5 118.9(4) . . ? C1 N1 Eu1 118.1(3) . . ? C5 N1 Eu1 117.6(3) . . ? C6 N2 C7 104.7(4) . . ? C6 N2 Eu1 120.8(3) . . ? C7 N2 Eu1 134.3(3) . . ? C6 N3 C12 106.1(4) . . ? C6 N3 C56 131.2(5) . . ? C12 N3 C56 122.4(5) . . ? C20 N4 C16 106.0(4) . . ? C20 N4 Eu2 119.9(3) . . ? C16 N4 Eu2 134.1(3) . . ? C20 N5 C17 106.2(4) . . ? C20 N5 C58 131.0(5) . . ? C17 N5 C58 122.8(4) . . ? C25 N6 C21 118.8(4) . . ? C25 N6 Eu2 117.6(3) . . ? C21 N6 Eu2 121.4(3) . . ? C26 N7 C29 117.0(5) . . ? C26 N7 C27 125.2(5) . . ? C29 N7 C27 116.9(5) . . ? C31 N8 C32 105.2(4) . . ? C31 N8 Eu1 119.1(3) . . ? C32 N8 Eu1 130.1(3) . . ? C31 N9 C37 106.1(4) . . ? C31 N9 C60 129.6(5) . . ? C37 N9 C60 122.3(4) . . ? C45 N10 C41 105.5(4) . . ? C45 N10 Eu3 120.1(3) . . ? C41 N10 Eu3 133.7(4) . . ? C45 N11 C42 106.7(5) . . ? C45 N11 C62 129.7(5) . . ? C42 N11 C62 122.5(5) . . ? C50 N12 C46 119.1(5) . . ? C50 N12 Eu3 115.7(4) . . ? C46 N12 Eu3 122.5(3) . . ? C51 N13 C52 118.2(6) . . ? C51 N13 C54 123.2(6) . . ? C52 N13 C54 117.0(5) . . ? N1 C1 C2 122.8(5) . . ? N1 C1 C6 113.8(4) . . ? C2 C1 C6 123.2(5) . . ? O1H C1H C2H 128.9(5) . . ? O1H C1H C4H 113.0(5) . . ? C2H C1H C4H 118.1(6) . . ? C3 C2 C1 117.3(5) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C1H C2H C3H 120.2(5) . . ? C1H C2H H2H 119.9 . . ? C3H C2H H2H 119.9 . . ? C4 C3 C2 120.5(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? O2H C3H C2H 127.9(5) . . ? O2H C3H C5H 115.2(5) . . ? C2H C3H C5H 116.9(5) . . ? C3 C4 C5 118.6(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? F2 C4H F1 107.1(9) . . ? F2 C4H F3 105.5(8) . . ? F1 C4H F3 103.4(7) . . ? F2 C4H C1H 115.7(6) . . ? F1 C4H C1H 112.8(7) . . ? F3 C4H C1H 111.3(7) . . ? N1 C5 C4 121.9(5) . . ? N1 C5 C31 113.7(4) . . ? C4 C5 C31 124.3(5) . . ? F4 C5H F5 110.3(8) . . ? F4 C5H F6 102.7(9) . . ? F5 C5H F6 104.8(6) . . ? F4 C5H C3H 114.0(6) . . ? F5 C5H C3H 113.5(6) . . ? F6 C5H C3H 110.7(6) . . ? N2 C6 N3 113.5(5) . . ? N2 C6 C1 119.5(4) . . ? N3 C6 C1 127.0(5) . . ? O3H C6H C7H 126.8(7) . . ? O3H C6H C10H 114.7(6) . . ? C7H C6H C10H 118.4(7) . . ? C8 C7 C12 120.4(5) . . ? C8 C7 N2 130.3(5) . . ? C12 C7 N2 109.3(5) . . ? C8H C7H C6H 121.0(6) . . ? C8H C7H H7H 119.5 . . ? C6H C7H H7H 119.5 . . ? C7 C8 C9 118.5(5) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? O4H C8H C7H 128.4(6) . . ? O4H C8H C9H 114.0(8) . . ? C7H C8H C9H 117.6(8) . . ? C8 C9 C10 119.6(5) . . ? C8 C9 C13 120.3(5) . . ? C10 C9 C13 120.0(5) . . ? F9 C9H F8 107.1(10) . . ? F9 C9H F7 105.6(12) . . ? F8 C9H F7 107.9(10) . . ? F9 C9H C8H 111.2(9) . . ? F8 C9H C8H 114.2(10) . . ? F7 C9H C8H 110.5(8) . . ? C11 C10 C9 122.8(5) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? F11 C10H F10 108.5(8) . . ? F11 C10H F12 106.4(8) . . ? F10 C10H F12 103.2(9) . . ? F11 C10H C6H 115.2(8) . . ? F10 C10H C6H 111.5(7) . . ? F12 C10H C6H 111.4(8) . . ? C10 C11 C12 115.8(6) . . ? C10 C11 H11 122.1 . . ? C12 C11 H11 122.1 . . ? O5H C11H C12H 128.9(6) . . ? O5H C11H C15H 112.3(8) . . ? C12H C11H C15H 118.8(7) . . ? C11 C12 C7 122.9(6) . . ? C11 C12 N3 130.8(6) . . ? C7 C12 N3 106.3(5) . . ? C13H C12H C11H 123.2(6) . . ? C13H C12H H12 118.4 . . ? C11H C12H H12 118.4 . . ? C14 C13 C9 114.2(4) . . ? C14 C13 H13A 108.7 . . ? C9 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C9 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? O6H C13H C12H 129.3(7) . . ? O6H C13H C14H 114.6(7) . . ? C12H C13H C14H 116.1(7) . . ? C15 C14 C19 119.4(5) . . ? C15 C14 C13 120.2(5) . . ? C19 C14 C13 120.4(5) . . ? F14B C14H F13A 124.3(12) . . ? F14B C14H F15A 60.5(10) . . ? F13A C14H F15A 112.6(15) . . ? F14B C14H F13B 113.4(11) . . ? F13A C14H F13B 37.9(8) . . ? F15A C14H F13B 144.2(13) . . ? F14B C14H F14A 47.8(9) . . ? F13A C14H F14A 105.3(12) . . ? F15A C14H F14A 108.3(11) . . ? F13B C14H F14A 74.2(10) . . ? F14B C14H F15B 109.2(14) . . ? F13A C14H F15B 56.7(10) . . ? F15A C14H F15B 60.0(11) . . ? F13B C14H F15B 94.5(10) . . ? F14A C14H F15B 140.2(11) . . ? F14B C14H C13H 121.1(10) . . ? F13A C14H C13H 113.0(10) . . ? F15A C14H C13H 109.6(9) . . ? F13B C14H C13H 103.1(11) . . ? F14A C14H C13H 107.6(11) . . ? F15B C14H C13H 112.2(8) . . ? C16 C15 C14 118.2(5) . . ? C16 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? F16 C15H F18 109.8(11) . . ? F16 C15H F17 102.1(9) . . ? F18 C15H F17 104.5(9) . . ? F16 C15H C11H 113.9(8) . . ? F18 C15H C11H 114.8(6) . . ? F17 C15H C11H 110.5(10) . . ? C15 C16 N4 130.8(5) . . ? C15 C16 C17 120.6(5) . . ? N4 C16 C17 108.5(5) . . ? O7H C16H C17H 128.5(5) . . ? O7H C16H C20H 114.7(5) . . ? C17H C16H C20H 116.7(5) . . ? C18 C17 N5 131.3(5) . . ? C18 C17 C16 122.3(5) . . ? N5 C17 C16 106.5(4) . . ? C18H C17H C16H 121.9(5) . . ? C18H C17H H17 119.0 . . ? C16H C17H H17 119.0 . . ? C19 C18 C17 116.4(5) . . ? C19 C18 H18 121.8 . . ? C17 C18 H18 121.8 . . ? O8H C18H C17H 129.3(5) . . ? O8H C18H C19H 114.7(5) . . ? C17H C18H C19H 116.0(5) . . ? C18 C19 C14 123.1(5) . . ? C18 C19 H19 118.5 . . ? C14 C19 H19 118.5 . . ? F24 C19H F22 110.9(7) . . ? F24 C19H F23 101.5(7) . . ? F22 C19H F23 103.3(7) . . ? F24 C19H C18H 115.4(6) . . ? F22 C19H C18H 114.6(7) . . ? F23 C19H C18H 109.6(6) . . ? N4 C20 N5 112.8(4) . . ? N4 C20 C21 120.8(4) . . ? N5 C20 C21 126.3(4) . . ? F21 C20H F19 107.9(7) . . ? F21 C20H F20 106.8(6) . . ? F19 C20H F20 105.1(7) . . ? F21 C20H C16H 113.2(6) . . ? F19 C20H C16H 110.3(5) . . ? F20 C20H C16H 113.1(6) . . ? N6 C21 C22 121.2(5) . . ? N6 C21 C20 111.3(4) . . ? C22 C21 C20 127.5(5) . . ? O9H C21H C22H 127.7(6) . . ? O9H C21H C25H 113.8(6) . . ? C22H C21H C25H 118.5(6) . . ? C21 C22 C23 119.5(5) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C23H C22H C21H 120.9(6) . . ? C23H C22H H22A 119.6 . . ? C21H C22H H22A 119.6 . . ? C24 C23 C22 119.3(5) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? O10H C23H C22H 128.4(6) . . ? O10H C23H C24H 112.5(7) . . ? C22H C23H C24H 119.2(6) . . ? C25 C24 C23 117.9(5) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? F29B C24H F28B 130.5(19) . . ? F29B C24H F30A 66.5(13) . . ? F28B C24H F30A 114.8(13) . . ? F29B C24H F30B 118.7(14) . . ? F28B C24H F30B 61.3(11) . . ? F30A C24H F30B 58.8(9) . . ? F29B C24H F29A 31.2(11) . . ? F28B C24H F29A 113.0(16) . . ? F30A C24H F29A 97.2(15) . . ? F30B C24H F29A 139.7(13) . . ? F29B C24H F28A 107.8(15) . . ? F28B C24H F28A 36.8(11) . . ? F30A C24H F28A 139.5(12) . . ? F30B C24H F28A 97.2(12) . . ? F29A C24H F28A 80.8(11) . . ? F29B C24H C23H 113.7(13) . . ? F28B C24H C23H 111.1(15) . . ? F30A C24H C23H 110.6(12) . . ? F30B C24H C23H 109.5(11) . . ? F29A C24H C23H 109.3(9) . . ? F28A C24H C23H 108.1(10) . . ? N6 C25 C24 123.1(5) . . ? N6 C25 C26 110.4(4) . . ? C24 C25 C26 126.1(5) . . ? F26 C25H F25 103.5(12) . . ? F26 C25H F27 105.2(11) . . ? F25 C25H F27 104.0(10) . . ? F26 C25H C21H 114.6(7) . . ? F25 C25H C21H 111.5(8) . . ? F27 C25H C21H 116.6(8) . . ? O1 C26 N7 121.8(5) . . ? O1 C26 C25 115.9(5) . . ? N7 C26 C25 122.3(5) . . ? O1 C26 Eu2 40.6(2) . . ? N7 C26 Eu2 144.3(4) . . ? C25 C26 Eu2 84.5(3) . . ? O11H C26H C27H 130.0(6) . . ? O11H C26H C30H 112.0(6) . . ? C27H C26H C30H 118.0(6) . . ? N7 C27 C28 112.6(5) . . ? N7 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? N7 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C26H C27H C28H 120.1(5) . . ? C26H C27H H27 119.9 . . ? C28H C27H H27 119.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O12H C28H C27H 128.8(6) . . ? O12H C28H C29H 113.7(6) . . ? C27H C28H C29H 117.5(6) . . ? N7 C29 C30 113.6(6) . . ? N7 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? N7 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? F36 C29H F34 108.8(8) . . ? F36 C29H F35 107.6(7) . . ? F34 C29H F35 101.0(8) . . ? F36 C29H C28H 115.4(8) . . ? F34 C29H C28H 112.7(6) . . ? F35 C29H C28H 110.2(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? F31 C30H F32 106.3(10) . . ? F31 C30H F33 108.7(8) . . ? F32 C30H F33 103.4(7) . . ? F31 C30H C26H 112.4(6) . . ? F32 C30H C26H 112.3(6) . . ? F33 C30H C26H 113.2(8) . . ? N8 C31 N9 113.1(4) . . ? N8 C31 C5 119.7(4) . . ? N9 C31 C5 127.1(4) . . ? O13H C31H C32H 128.3(6) . . ? O13H C31H C35H 114.1(6) . . ? C32H C31H C35H 117.6(6) . . ? C33 C32 C37 121.7(5) . . ? C33 C32 N8 129.6(4) . . ? C37 C32 N8 108.7(4) . . ? C33H C32H C31H 120.8(6) . . ? C33H C32H H32 119.6 . . ? C31H C32H H32 119.6 . . ? C32 C33 C34 117.6(5) . . ? C32 C33 H33 121.2 . . ? C34 C33 H33 121.2 . . ? O14H C33H C32H 129.7(6) . . ? O14H C33H C34H 113.0(6) . . ? C32H C33H C34H 117.3(6) . . ? C33 C34 C35 120.3(5) . . ? C33 C34 C38 120.9(5) . . ? C35 C34 C38 118.8(5) . . ? F40 C34H F42 112.6(9) . . ? F40 C34H F41 103.3(10) . . ? F42 C34H F41 100.8(9) . . ? F40 C34H C33H 113.3(6) . . ? F42 C34H C33H 114.7(7) . . ? F41 C34H C33H 110.6(7) . . ? C36 C35 C34 122.5(5) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? F38 C35H F39 111.9(10) . . ? F38 C35H F37 104.1(12) . . ? F39 C35H F37 102.2(10) . . ? F38 C35H C31H 112.9(9) . . ? F39 C35H C31H 115.7(8) . . ? F37 C35H C31H 108.7(9) . . ? C35 C36 C37 116.4(5) . . ? C35 C36 H36 121.8 . . ? C37 C36 H36 121.8 . . ? O16H C36H C37H 128.1(6) . . ? O16H C36H C40H 114.9(5) . . ? C37H C36H C40H 117.0(5) . . ? C32 C37 N9 106.9(4) . . ? C32 C37 C36 121.5(5) . . ? N9 C37 C36 131.6(5) . . ? C38H C37H C36H 121.7(5) . . ? C38H C37H H37 119.1 . . ? C36H C37H H37 119.1 . . ? C39 C38 C34 113.9(5) . . ? C39 C38 H38A 108.8 . . ? C34 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? C34 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? O15H C38H C37H 129.0(5) . . ? O15H C38H C39H 114.1(6) . . ? C37H C38H C39H 116.8(6) . . ? C40 C39 C44 120.2(5) . . ? C40 C39 C38 120.8(5) . . ? C44 C39 C38 118.9(5) . . ? F44 C39H F45 109.0(9) . . ? F44 C39H F43 108.9(9) . . ? F45 C39H F43 100.3(7) . . ? F44 C39H C38H 113.1(7) . . ? F45 C39H C38H 112.2(7) . . ? F43 C39H C38H 112.6(6) . . ? C39 C40 C41 118.3(5) . . ? C39 C40 H40 120.9 . . ? C41 C40 H40 120.9 . . ? F46 C40H F48 108.2(6) . . ? F46 C40H F47 108.9(7) . . ? F48 C40H F47 105.0(6) . . ? F46 C40H C36H 111.6(6) . . ? F48 C40H C36H 113.0(6) . . ? F47 C40H C36H 109.9(5) . . ? N10 C41 C40 130.2(5) . . ? N10 C41 C42 109.5(5) . . ? C40 C41 C42 120.3(5) . . ? O17H C41H C42H 127.8(7) . . ? O17H C41H C45H 114.1(7) . . ? C42H C41H C45H 118.0(7) . . ? N11 C42 C43 131.6(6) . . ? N11 C42 C41 105.9(4) . . ? C43 C42 C41 122.5(5) . . ? C41H C42H C43H 121.3(7) . . ? C41H C42H H42 119.4 . . ? C43H C42H H42 119.4 . . ? C44 C43 C42 116.6(6) . . ? C44 C43 H43 121.7 . . ? C42 C43 H43 121.7 . . ? O18H C43H C42H 127.2(6) . . ? O18H C43H C44H 115.2(7) . . ? C42H C43H C44H 117.6(7) . . ? C43 C44 C39 122.2(5) . . ? C43 C44 H44 118.9 . . ? C39 C44 H44 118.9 . . ? F54 C44H F52 104.2(11) . . ? F54 C44H F53 110.1(10) . . ? F52 C44H F53 102.5(10) . . ? F54 C44H C43H 112.9(8) . . ? F52 C44H C43H 112.7(8) . . ? F53 C44H C43H 113.7(9) . . ? N10 C45 N11 112.4(5) . . ? N10 C45 C46 119.7(5) . . ? N11 C45 C46 127.9(5) . . ? F49 C45H F51 112.7(12) . . ? F49 C45H F50 104.0(13) . . ? F51 C45H F50 99.5(12) . . ? F49 C45H C41H 113.0(10) . . ? F51 C45H C41H 115.3(10) . . ? F50 C45H C41H 110.8(9) . . ? N12 C46 C47 121.1(5) . . ? N12 C46 C45 112.3(5) . . ? C47 C46 C45 126.4(5) . . ? C48 C47 C46 119.0(6) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C49 C48 C47 119.5(6) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 118.3(6) . . ? C48 C49 H49 120.8 . . ? C50 C49 H49 120.8 . . ? N12 C50 C49 122.6(6) . . ? N12 C50 C51 111.8(5) . . ? C49 C50 C51 125.2(5) . . ? O2 C51 N13 122.6(6) . . ? O2 C51 C50 116.2(5) . . ? N13 C51 C50 121.2(6) . . ? O2 C51 Eu3 41.3(2) . . ? N13 C51 Eu3 145.4(4) . . ? C50 C51 Eu3 84.0(3) . . ? N13 C52 C53 112.9(6) . . ? N13 C52 H52A 109.0 . . ? C53 C52 H52A 109.0 . . ? N13 C52 H52B 109.0 . . ? C53 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N13 C54 C55 113.6(6) . . ? N13 C54 H54A 108.9 . . ? C55 C54 H54A 108.9 . . ? N13 C54 H54B 108.9 . . ? C55 C54 H54B 108.9 . . ? H54A C54 H54B 107.7 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N3 C56 C57 109.9(7) . . ? N3 C56 H56A 109.7 . . ? C57 C56 H56A 109.7 . . ? N3 C56 H56B 109.7 . . ? C57 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N5 C58 C59 111.3(4) . . ? N5 C58 H58A 109.4 . . ? C59 C58 H58A 109.4 . . ? N5 C58 H58B 109.4 . . ? C59 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N9 C60 C61 111.4(6) . . ? N9 C60 H60A 109.4 . . ? C61 C60 H60A 109.4 . . ? N9 C60 H60B 109.4 . . ? C61 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N11 C62 C63 111.4(7) . . ? N11 C62 H62A 109.4 . . ? C63 C62 H62A 109.4 . . ? N11 C62 H62B 109.4 . . ? C63 C62 H62B 109.4 . . ? H62A C62 H62B 108.0 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N1S C2S C3S 177.5(13) . . ? C2S C3S H3SA 109.5 . . ? C2S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C2S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? N4SA C5SA C6SA 178(3) . . ? N4SB C5SB C6SB 133(6) . . ? C5SB C6SB H6SD 109.5 . . ? C5SB C6SB H6SE 109.5 . . ? H6SD C6SB H6SE 109.5 . . ? C5SB C6SB H6SF 109.5 . . ? H6SD C6SB H6SF 109.5 . . ? H6SE C6SB H6SF 109.5 . . ? N7S C8S C9S 164(2) . . ? C8S C9S H9SA 109.5 . . ? C8S C9S H9SB 109.5 . . ? H9SA C9S H9SB 109.5 . . ? C8S C9S H9SC 109.5 . . ? H9SA C9S H9SC 109.5 . . ? H9SB C9S H9SC 109.5 . . ? N10S C11S C12S 178.2(10) . . ? C11S C12S H12A 109.5 . . ? C11S C12S H12B 109.5 . . ? H12A C12S H12B 109.5 . . ? C11S C12S H12C 109.5 . . ? H12A C12S H12C 109.5 . . ? H12B C12S H12C 109.5 . . ? N13S C14S C15S 170(2) . . ? C14S C15S H15A 109.5 . . ? C14S C15S H15B 109.5 . . ? H15A C15S H15B 109.5 . . ? C14S C15S H15C 109.5 . . ? H15A C15S H15C 109.5 . . ? H15B C15S H15C 109.5 . . ? N15 C191 C192 175(5) . . ? C191 C192 H19A 109.5 . . ? C191 C192 H19B 109.5 . . ? H19A C192 H19B 109.5 . . ? C191 C192 H19C 109.5 . . ? H19A C192 H19C 109.5 . . ? H19B C192 H19C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 66.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.328 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.098 data_5 _database_code_depnum_ccdc_archive 'CCDC 909095' #TrackingRef 'web_deposit_cif_file_0_LaureGuenee_1351875343.Compounds_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H25 F18 Lu N4 O7, 2(C2 H3 N)' _chemical_formula_sum 'C38 H31 F18 Lu N6 O7' _chemical_formula_weight 1200.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -6.6179 4.6937 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2354(2) _cell_length_b 14.4044(2) _cell_length_c 14.8029(3) _cell_angle_alpha 77.3039(16) _cell_angle_beta 72.1925(19) _cell_angle_gamma 68.6551(17) _cell_volume 2296.18(8) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 27244 _cell_measurement_theta_max 73.2353 _cell_measurement_theta_min 3.1567 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2763 _exptl_crystal_size_mid 0.1604 _exptl_crystal_size_min 0.0985 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 5.275 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_max 0.702 _exptl_absorpt_correction_T_min 0.424 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4679 _diffrn_reflns_number 34152 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 73.39 _reflns_number_total 9099 _reflns_number_gt 8704 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SIR97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep 3 (Farrugia, 1997)' _computing_publication_material 'SHELX_Acta (Sheldrick, 2008)' _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^)+(0.0392P)^2^+2.0344P] 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 9099 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.674307(10) 0.292954(8) 0.765264(8) 0.02567(5) Uani 1 1 d . . . F14 F 0.4388(2) 0.06660(16) 0.9267(2) 0.0795(7) Uani 1 1 d . . . F16 F 0.22131(19) 0.47621(18) 1.01578(17) 0.0748(7) Uani 1 1 d . . . F17 F 0.26202(19) 0.16698(18) 0.9420(2) 0.0773(7) Uani 1 1 d . . . F19 F 1.1091(3) 0.2283(3) 0.4651(3) 0.1187(13) Uani 1 1 d . . . F20 F 0.3097(4) 0.56434(19) 0.9049(2) 0.155(2) Uani 1 1 d . . . F21 F 0.3788(3) 0.4936(3) 1.0251(3) 0.1307(15) Uani 1 1 d . . . F22 F 0.3670(3) 0.1290(3) 0.80511(18) 0.1102(12) Uani 1 1 d . . . F23 F 0.8143(3) -0.00931(16) 0.5912(2) 0.0962(10) Uani 1 1 d . . . F24 F 0.8430(3) 0.0623(2) 0.45204(17) 0.0903(9) Uani 1 1 d . . . F25 F 0.6654(2) 0.0917(2) 0.5387(3) 0.1008(11) Uani 1 1 d . . . F26 F 1.0918(2) 0.2697(3) 0.5956(2) 0.1014(10) Uani 1 1 d . . . F27 F 1.0118(2) 0.3783(2) 0.4964(3) 0.1102(12) Uani 1 1 d . . . F28 F 0.9834(3) -0.0465(2) 0.7457(2) 0.1032(10) Uani 1 1 d . . . F29 F 1.0298(3) -0.0644(2) 0.8743(2) 0.1212(13) Uani 1 1 d . . . F30 F 1.0711(2) 0.0440(2) 0.7609(3) 0.1271(14) Uani 1 1 d . . . F31 F 0.7034(3) 0.0619(2) 1.13253(16) 0.0890(8) Uani 1 1 d . . . F32 F 0.6739(4) 0.2164(3) 1.11719(18) 0.1319(16) Uani 1 1 d . . . F33 F 0.5400(2) 0.1611(3) 1.10845(17) 0.0990(10) Uani 1 1 d . . . O1 O 0.79830(16) 0.32484(13) 0.83576(13) 0.0324(4) Uani 1 1 d . . . O2 O 0.50825(17) 0.39940(14) 0.86227(13) 0.0347(4) Uani 1 1 d . . . O3 O 0.52483(16) 0.21998(14) 0.80572(13) 0.0337(4) Uani 1 1 d . . . O4 O 0.70005(16) 0.20053(13) 0.64223(13) 0.0327(4) Uani 1 1 d . . . O5 O 0.84509(16) 0.30924(13) 0.64108(13) 0.0332(4) Uani 1 1 d . . . O6 O 0.64422(17) 0.22156(14) 0.92935(13) 0.0368(4) Uani 1 1 d . . . O7 O 0.82367(17) 0.13984(13) 0.77778(13) 0.0358(4) Uani 1 1 d . . . N1 N 0.68110(18) 0.46929(15) 0.72848(14) 0.0269(4) Uani 1 1 d . . . N1S N 0.8507(6) -0.2454(4) 0.8109(7) 0.165(3) Uani 1 1 d . . . N2 N 0.9546(2) 0.38331(18) 0.80462(17) 0.0371(5) Uani 1 1 d . . . N2S N 0.5119(5) -0.1170(3) 0.6139(4) 0.1163(18) Uani 1 1 d . . . N3 N 0.53930(18) 0.41177(15) 0.66504(14) 0.0279(4) Uani 1 1 d . . . N4 N 0.42326(19) 0.56655(15) 0.62090(15) 0.0293(4) Uani 1 1 d . . . C1 C 0.5957(2) 0.54545(18) 0.69401(17) 0.0301(5) Uani 1 1 d . . . C1S C 0.6957(5) -0.0708(4) 0.8140(4) 0.0962(16) Uani 1 1 d . . . H1SB H 0.7316 -0.0228 0.7686 0.144 Uiso 1 1 calc R . . H1SC H 0.6703 -0.0512 0.8785 0.144 Uiso 1 1 calc R . . H1SA H 0.6252 -0.0713 0.7960 0.144 Uiso 1 1 calc R . . C2 C 0.5878(3) 0.6446(2) 0.6915(2) 0.0431(7) Uani 1 1 d . . . H2 H 0.5258 0.6981 0.6685 0.052 Uiso 1 1 calc R . . C2S C 0.7826(6) -0.1683(4) 0.8126(5) 0.0923(16) Uani 1 1 d . . . C3 C 0.6714(3) 0.6644(2) 0.7229(2) 0.0481(7) Uani 1 1 d . . . H3 H 0.6674 0.7318 0.7213 0.058 Uiso 1 1 calc R . . C3S C 0.3391(5) 0.0494(3) 0.6242(4) 0.0829(13) Uani 1 1 d . . . H3SA H 0.3348 0.0818 0.5592 0.124 Uiso 1 1 calc R . . H3SC H 0.3534 0.0934 0.6581 0.124 Uiso 1 1 calc R . . H3SB H 0.2625 0.0367 0.6583 0.124 Uiso 1 1 calc R . . C4 C 0.7606(3) 0.5862(2) 0.7567(2) 0.0390(6) Uani 1 1 d . . . H4 H 0.8190 0.5985 0.7784 0.047 Uiso 1 1 calc R . . C4S C 0.4361(5) -0.0438(3) 0.6196(3) 0.0699(11) Uani 1 1 d . . . C5 C 0.7627(2) 0.48882(19) 0.75794(17) 0.0298(5) Uani 1 1 d . . . C6 C 0.8436(2) 0.39394(19) 0.80105(17) 0.0299(5) Uani 1 1 d . . . C7 C 1.0276(3) 0.4483(3) 0.7498(2) 0.0490(7) Uani 1 1 d . . . H7A H 0.9819 0.5004 0.7070 0.059 Uiso 1 1 calc R . . H7B H 1.1031 0.4075 0.7092 0.059 Uiso 1 1 calc R . . C8 C 1.0599(4) 0.4988(3) 0.8126(3) 0.0650(10) Uani 1 1 d . . . H8B H 1.1121 0.5379 0.7726 0.098 Uiso 1 1 calc R . . H8C H 1.1028 0.4477 0.8567 0.098 Uiso 1 1 calc R . . H8A H 0.9857 0.5436 0.8493 0.098 Uiso 1 1 calc R . . C9 C 1.0192(3) 0.2876(2) 0.8540(2) 0.0477(7) Uani 1 1 d . . . H9B H 1.1070 0.2785 0.8343 0.057 Uiso 1 1 calc R . . H9A H 1.0072 0.2316 0.8338 0.057 Uiso 1 1 calc R . . C10 C 0.9767(4) 0.2826(3) 0.9617(3) 0.0642(10) Uani 1 1 d . . . H10C H 0.9896 0.3372 0.9823 0.096 Uiso 1 1 calc R . . H10B H 1.0227 0.2179 0.9908 0.096 Uiso 1 1 calc R . . H10A H 0.8903 0.2896 0.9818 0.096 Uiso 1 1 calc R . . C11 C 0.5180(2) 0.50965(18) 0.66047(17) 0.0277(5) Uani 1 1 d . . . C12 C 0.4533(2) 0.40346(18) 0.62719(16) 0.0277(5) Uani 1 1 d . . . C13 C 0.4332(2) 0.3181(2) 0.61340(18) 0.0328(5) Uani 1 1 d . . . H13 H 0.4807 0.2522 0.6328 0.039 Uiso 1 1 calc R . . C14 C 0.3412(2) 0.3343(2) 0.5704(2) 0.0370(6) Uani 1 1 d . . . H14 H 0.3258 0.2780 0.5597 0.044 Uiso 1 1 calc R . . C15 C 0.2698(2) 0.4311(2) 0.5420(2) 0.0382(6) Uani 1 1 d . . . H15 H 0.2075 0.4387 0.5127 0.046 Uiso 1 1 calc R . . C16 C 0.2876(2) 0.5160(2) 0.55565(19) 0.0344(5) Uani 1 1 d . . . H16 H 0.2393 0.5817 0.5366 0.041 Uiso 1 1 calc R . . C17 C 0.3806(2) 0.49938(19) 0.59897(17) 0.0290(5) Uani 1 1 d . . . C18 C 0.3646(2) 0.67583(19) 0.6075(2) 0.0352(6) Uani 1 1 d . . . H18A H 0.3224 0.6932 0.5557 0.042 Uiso 1 1 calc R . . H18B H 0.4273 0.7095 0.5875 0.042 Uiso 1 1 calc R . . C19 C 0.2741(3) 0.7144(3) 0.6980(3) 0.0576(9) Uani 1 1 d . . . H19B H 0.2386 0.7875 0.6865 0.086 Uiso 1 1 calc R . . H19C H 0.3155 0.6972 0.7495 0.086 Uiso 1 1 calc R . . H19A H 0.2100 0.6835 0.7164 0.086 Uiso 1 1 calc R . . C20 C 0.4079(2) 0.3922(2) 0.91076(18) 0.0357(6) Uani 1 1 d . . . C21 C 0.3620(2) 0.3144(2) 0.9201(2) 0.0387(6) Uani 1 1 d . . . H21 H 0.2857 0.3163 0.9630 0.046 Uiso 1 1 calc R . . C22 C 0.4259(2) 0.2342(2) 0.86755(19) 0.0337(5) Uani 1 1 d . . . C23 C 0.3726(3) 0.1488(2) 0.8848(2) 0.0454(7) Uani 1 1 d . . . C24 C 0.3278(3) 0.4828(3) 0.9644(3) 0.0581(9) Uani 1 1 d . . . C25 C 0.7881(2) 0.16216(19) 0.57843(18) 0.0334(5) Uani 1 1 d . . . C26 C 0.8954(2) 0.1858(2) 0.5395(2) 0.0386(6) Uani 1 1 d . . . H26 H 0.9555 0.1521 0.4888 0.046 Uiso 1 1 calc R . . C27 C 0.9137(2) 0.2588(2) 0.57513(18) 0.0340(5) Uani 1 1 d . . . C28 C 1.0317(3) 0.2841(3) 0.5295(3) 0.0506(8) Uani 1 1 d . . . C29 C 0.7767(3) 0.0764(2) 0.5394(2) 0.0438(7) Uani 1 1 d . . . C30 C 0.7078(3) 0.1534(2) 0.97613(19) 0.0370(6) Uani 1 1 d . . . C31 C 0.8186(3) 0.0821(2) 0.9413(2) 0.0459(7) Uani 1 1 d . . . H31 H 0.8606 0.0338 0.9845 0.055 Uiso 1 1 calc R . . C32 C 0.8670(3) 0.0819(2) 0.8440(2) 0.0389(6) Uani 1 1 d . . . C33 C 0.9882(3) 0.0025(3) 0.8089(3) 0.0550(8) Uani 1 1 d . . . C34 C 0.6555(3) 0.1501(3) 1.0851(2) 0.0491(7) 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 Lu1 0.02512(7) 0.02539(7) 0.02443(7) -0.00254(5) -0.00684(5) -0.00542(5) F14 0.0618(13) 0.0432(11) 0.128(2) 0.0219(12) -0.0351(14) -0.0201(10) F16 0.0517(12) 0.0741(14) 0.0736(15) -0.0299(12) 0.0185(10) -0.0076(10) F17 0.0436(11) 0.0736(14) 0.1108(19) -0.0045(13) -0.0008(12) -0.0331(10) F19 0.0730(17) 0.150(3) 0.136(3) -0.095(2) 0.0602(17) -0.0649(19) F20 0.192(4) 0.0394(13) 0.105(2) -0.0010(13) 0.073(2) 0.0165(17) F21 0.087(2) 0.196(4) 0.134(3) -0.132(3) 0.0287(19) -0.055(2) F22 0.190(3) 0.147(3) 0.0601(14) 0.0008(16) -0.0308(18) -0.138(3) F23 0.173(3) 0.0371(11) 0.0925(19) -0.0009(11) -0.063(2) -0.0284(14) F24 0.125(2) 0.1043(19) 0.0561(13) -0.0478(13) 0.0116(14) -0.0600(18) F25 0.0586(14) 0.101(2) 0.171(3) -0.091(2) -0.0287(16) -0.0142(13) F26 0.0540(14) 0.162(3) 0.105(2) -0.013(2) -0.0226(14) -0.0527(17) F27 0.0569(14) 0.0749(17) 0.169(3) 0.0307(18) -0.0035(16) -0.0338(13) F28 0.0781(18) 0.0906(19) 0.122(2) -0.0591(18) -0.0268(17) 0.0235(15) F29 0.100(2) 0.100(2) 0.0815(18) 0.0119(16) -0.0242(16) 0.0509(17) F30 0.0434(13) 0.0792(18) 0.209(4) -0.004(2) 0.0126(18) -0.0059(12) F31 0.105(2) 0.0931(18) 0.0439(12) 0.0245(12) -0.0188(12) -0.0216(15) F32 0.263(5) 0.138(3) 0.0446(13) -0.0206(15) -0.0104(19) -0.139(3) F33 0.0631(15) 0.164(3) 0.0452(12) 0.0039(15) 0.0013(11) -0.0296(17) O1 0.0328(9) 0.0332(9) 0.0319(9) -0.0005(7) -0.0126(7) -0.0098(7) O2 0.0370(10) 0.0349(9) 0.0281(9) -0.0054(7) -0.0023(7) -0.0108(8) O3 0.0329(9) 0.0362(9) 0.0318(9) -0.0040(7) -0.0058(7) -0.0129(7) O4 0.0313(9) 0.0329(9) 0.0316(9) -0.0084(7) -0.0072(7) -0.0056(7) O5 0.0310(9) 0.0327(9) 0.0328(9) -0.0063(7) -0.0049(7) -0.0077(7) O6 0.0356(10) 0.0414(10) 0.0305(9) 0.0021(8) -0.0095(8) -0.0116(8) O7 0.0386(10) 0.0302(9) 0.0336(9) -0.0010(7) -0.0123(8) -0.0039(8) N1 0.0270(10) 0.0295(10) 0.0221(9) -0.0031(8) -0.0055(8) -0.0071(8) N1S 0.160(6) 0.079(3) 0.309(10) -0.050(5) -0.125(7) -0.028(4) N2 0.0288(11) 0.0445(13) 0.0362(12) -0.0039(10) -0.0078(9) -0.0105(9) N2S 0.137(4) 0.054(2) 0.133(4) 0.020(2) -0.043(4) -0.011(3) N3 0.0293(10) 0.0281(10) 0.0255(10) -0.0037(8) -0.0072(8) -0.0077(8) N4 0.0302(10) 0.0275(10) 0.0282(10) -0.0017(8) -0.0109(8) -0.0050(8) C1 0.0344(13) 0.0287(12) 0.0260(12) -0.0016(9) -0.0098(10) -0.0080(10) C1S 0.081(3) 0.107(4) 0.096(4) -0.014(3) -0.011(3) -0.032(3) C2 0.0515(17) 0.0281(13) 0.0546(18) -0.0006(12) -0.0283(14) -0.0084(12) C2S 0.101(4) 0.081(3) 0.124(5) -0.018(3) -0.045(3) -0.045(3) C3 0.063(2) 0.0312(14) 0.060(2) -0.0014(13) -0.0304(16) -0.0163(13) C3S 0.099(4) 0.068(3) 0.076(3) -0.019(2) -0.021(3) -0.013(2) C4 0.0455(15) 0.0373(14) 0.0420(15) -0.0022(11) -0.0186(12) -0.0172(12) C4S 0.097(3) 0.050(2) 0.066(2) 0.0097(18) -0.028(2) -0.031(2) C5 0.0297(12) 0.0336(12) 0.0258(11) -0.0036(9) -0.0063(9) -0.0104(10) C6 0.0293(12) 0.0355(13) 0.0247(11) -0.0059(10) -0.0074(9) -0.0083(10) C7 0.0329(14) 0.0615(19) 0.0513(18) -0.0037(15) -0.0032(13) -0.0214(14) C8 0.053(2) 0.077(3) 0.081(3) -0.003(2) -0.0252(19) -0.0366(19) C9 0.0284(14) 0.0502(17) 0.0594(19) -0.0024(14) -0.0178(13) -0.0036(12) C10 0.053(2) 0.072(2) 0.060(2) 0.0090(18) -0.0258(18) -0.0120(18) C11 0.0283(12) 0.0290(11) 0.0235(11) -0.0026(9) -0.0078(9) -0.0059(9) C12 0.0263(11) 0.0331(12) 0.0222(11) -0.0026(9) -0.0053(9) -0.0089(9) C13 0.0334(13) 0.0336(12) 0.0308(13) -0.0027(10) -0.0064(10) -0.0121(10) C14 0.0363(14) 0.0444(15) 0.0365(14) -0.0047(11) -0.0099(11) -0.0194(12) C15 0.0313(13) 0.0527(16) 0.0346(14) -0.0037(12) -0.0117(11) -0.0160(12) C16 0.0291(13) 0.0398(14) 0.0304(13) 0.0010(10) -0.0101(10) -0.0073(10) C17 0.0284(12) 0.0331(12) 0.0228(11) -0.0017(9) -0.0057(9) -0.0083(10) C18 0.0370(14) 0.0277(12) 0.0370(14) -0.0001(10) -0.0157(11) -0.0027(10) C19 0.056(2) 0.0420(17) 0.057(2) -0.0168(15) 0.0000(16) -0.0016(14) C20 0.0357(14) 0.0379(14) 0.0255(12) -0.0020(10) -0.0050(10) -0.0057(11) C21 0.0282(13) 0.0444(15) 0.0361(14) -0.0003(11) -0.0036(11) -0.0092(11) C22 0.0310(13) 0.0389(13) 0.0315(13) 0.0056(10) -0.0135(10) -0.0124(11) C23 0.0413(16) 0.0492(17) 0.0493(17) 0.0051(13) -0.0146(13) -0.0223(13) C24 0.057(2) 0.0520(19) 0.0495(19) -0.0181(15) 0.0133(16) -0.0140(16) C25 0.0358(13) 0.0302(12) 0.0306(13) -0.0041(10) -0.0135(11) -0.0018(10) C26 0.0338(14) 0.0390(14) 0.0357(14) -0.0134(11) -0.0026(11) -0.0033(11) C27 0.0288(12) 0.0358(13) 0.0296(12) -0.0021(10) -0.0056(10) -0.0040(10) C28 0.0347(15) 0.0560(19) 0.0553(19) -0.0151(15) 0.0023(14) -0.0141(14) C29 0.0500(17) 0.0375(14) 0.0424(16) -0.0134(12) -0.0106(13) -0.0080(13) C30 0.0409(15) 0.0434(15) 0.0316(13) 0.0023(11) -0.0131(11) -0.0197(12) C31 0.0486(17) 0.0464(16) 0.0376(15) 0.0063(12) -0.0205(13) -0.0079(13) C32 0.0404(15) 0.0320(13) 0.0433(15) 0.0010(11) -0.0168(12) -0.0083(11) C33 0.0453(18) 0.0454(17) 0.061(2) -0.0013(15) -0.0167(16) 0.0011(14) C34 0.061(2) 0.0579(19) 0.0322(15) 0.0061(13) -0.0151(14) -0.0267(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Lu1 O3 2.2937(17) . ? Lu1 O1 2.2996(18) . ? Lu1 O7 2.3090(18) . ? Lu1 O2 2.3359(18) . ? Lu1 O4 2.3661(17) . ? Lu1 O5 2.3703(18) . ? Lu1 O6 2.3924(18) . ? Lu1 N3 2.487(2) . ? Lu1 N1 2.505(2) . ? F14 C23 1.314(4) . ? F16 C24 1.318(4) . ? F17 C23 1.325(4) . ? F19 C28 1.297(4) . ? F20 C24 1.296(5) . ? F21 C24 1.302(5) . ? F22 C23 1.299(4) . ? F23 C29 1.307(4) . ? F24 C29 1.314(4) . ? F25 C29 1.302(4) . ? F26 C28 1.335(4) . ? F27 C28 1.297(4) . ? F28 C33 1.315(5) . ? F29 C33 1.288(4) . ? F30 C33 1.305(5) . ? F31 C34 1.330(4) . ? F32 C34 1.269(4) . ? F33 C34 1.306(4) . ? O1 C6 1.251(3) . ? O2 C20 1.246(3) . ? O3 C22 1.253(3) . ? O4 C25 1.238(3) . ? O5 C27 1.246(3) . ? O6 C30 1.234(3) . ? O7 C32 1.255(3) . ? N1 C5 1.338(3) . ? N1 C1 1.342(3) . ? N1S C2S 1.120(8) . ? N2 C6 1.327(3) . ? N2 C7 1.470(4) . ? N2 C9 1.476(4) . ? N2S C4S 1.122(6) . ? N3 C11 1.327(3) . ? N3 C12 1.385(3) . ? N4 C11 1.368(3) . ? N4 C17 1.387(3) . ? N4 C18 1.470(3) . ? C1 C2 1.389(4) . ? C1 C11 1.474(3) . ? C1S C2S 1.419(8) . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C1S H1SA 0.9800 . ? C2 C3 1.380(4) . ? C2 H2 0.9500 . ? C3 C4 1.379(4) . ? C3 H3 0.9500 . ? C3S C4S 1.430(6) . ? C3S H3SA 0.9800 . ? C3S H3SC 0.9800 . ? C3S H3SB 0.9800 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C6 1.508(4) . ? C7 C8 1.511(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C8 H8A 0.9800 . ? C9 C10 1.512(5) . ? C9 H9B 0.9900 . ? C9 H9A 0.9900 . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C12 C17 1.398(3) . ? C12 C13 1.405(4) . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.402(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C17 1.394(4) . ? C16 H16 0.9500 . ? C18 C19 1.517(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19A 0.9800 . ? C20 C21 1.392(4) . ? C20 C24 1.529(4) . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.533(4) . ? C25 C26 1.395(4) . ? C25 C29 1.539(4) . ? C26 C27 1.386(4) . ? C26 H26 0.9500 . ? C27 C28 1.534(4) . ? C30 C31 1.397(4) . ? C30 C34 1.539(4) . ? C31 C32 1.380(4) . ? C31 H31 0.9500 . ? C32 C33 1.528(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Lu1 O1 139.40(6) . . ? O3 Lu1 O7 92.66(7) . . ? O1 Lu1 O7 76.69(7) . . ? O3 Lu1 O2 74.68(6) . . ? O1 Lu1 O2 88.49(6) . . ? O7 Lu1 O2 139.87(6) . . ? O3 Lu1 O4 70.41(6) . . ? O1 Lu1 O4 136.56(6) . . ? O7 Lu1 O4 70.04(6) . . ? O2 Lu1 O4 134.88(6) . . ? O3 Lu1 O5 141.56(6) . . ? O1 Lu1 O5 73.80(6) . . ? O7 Lu1 O5 74.84(6) . . ? O2 Lu1 O5 136.53(6) . . ? O4 Lu1 O5 71.16(6) . . ? O3 Lu1 O6 69.61(6) . . ? O1 Lu1 O6 69.87(6) . . ? O7 Lu1 O6 71.26(7) . . ? O2 Lu1 O6 68.62(6) . . ? O4 Lu1 O6 121.65(6) . . ? O5 Lu1 O6 134.71(6) . . ? O3 Lu1 N3 80.70(7) . . ? O1 Lu1 N3 128.66(6) . . ? O7 Lu1 N3 145.60(7) . . ? O2 Lu1 N3 70.92(6) . . ? O4 Lu1 N3 75.97(6) . . ? O5 Lu1 N3 89.51(6) . . ? O6 Lu1 N3 134.61(7) . . ? O3 Lu1 N1 135.40(7) . . ? O1 Lu1 N1 64.91(6) . . ? O7 Lu1 N1 131.88(7) . . ? O2 Lu1 N1 68.91(6) . . ? O4 Lu1 N1 121.19(6) . . ? O5 Lu1 N1 67.62(6) . . ? O6 Lu1 N1 117.15(7) . . ? N3 Lu1 N1 63.83(7) . . ? C6 O1 Lu1 121.87(16) . . ? C20 O2 Lu1 132.91(18) . . ? C22 O3 Lu1 132.89(17) . . ? C25 O4 Lu1 133.50(18) . . ? C27 O5 Lu1 133.81(17) . . ? C30 O6 Lu1 134.37(18) . . ? C32 O7 Lu1 135.87(18) . . ? C5 N1 C1 119.6(2) . . ? C5 N1 Lu1 117.48(16) . . ? C1 N1 Lu1 122.14(16) . . ? C6 N2 C7 126.3(2) . . ? C6 N2 C9 116.5(2) . . ? C7 N2 C9 116.2(2) . . ? C11 N3 C12 105.5(2) . . ? C11 N3 Lu1 119.01(16) . . ? C12 N3 Lu1 133.50(16) . . ? C11 N4 C17 106.2(2) . . ? C11 N4 C18 131.1(2) . . ? C17 N4 C18 122.6(2) . . ? N1 C1 C2 121.0(2) . . ? N1 C1 C11 112.1(2) . . ? C2 C1 C11 126.9(2) . . ? C2S C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C2S C1S H1SA 109.5 . . ? H1SB C1S H1SA 109.5 . . ? H1SC C1S H1SA 109.5 . . ? C3 C2 C1 119.1(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? N1S C2S C1S 179.4(7) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C4S C3S H3SA 109.5 . . ? C4S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? C4S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? H3SC C3S H3SB 109.5 . . ? C3 C4 C5 118.0(3) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? N2S C4S C3S 178.3(6) . . ? N1 C5 C4 122.3(2) . . ? N1 C5 C6 111.0(2) . . ? C4 C5 C6 126.4(2) . . ? O1 C6 N2 121.2(2) . . ? O1 C6 C5 115.4(2) . . ? N2 C6 C5 123.4(2) . . ? N2 C7 C8 113.0(3) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? N2 C9 C10 112.9(3) . . ? N2 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? N2 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? H9B C9 H9A 107.8 . . ? C9 C10 H10C 109.5 . . ? C9 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C9 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? N3 C11 N4 112.7(2) . . ? N3 C11 C1 119.8(2) . . ? N4 C11 C1 127.5(2) . . ? N3 C12 C17 109.4(2) . . ? N3 C12 C13 130.6(2) . . ? C17 C12 C13 120.0(2) . . ? C14 C13 C12 117.1(2) . . ? C14 C13 H13 121.5 . . ? C12 C13 H13 121.5 . . ? C13 C14 C15 122.0(3) . . ? C13 C14 H14 119.0 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 121.8(2) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 116.1(2) . . ? C15 C16 H16 122.0 . . ? C17 C16 H16 122.0 . . ? N4 C17 C16 130.7(2) . . ? N4 C17 C12 106.2(2) . . ? C16 C17 C12 123.1(2) . . ? N4 C18 C19 112.0(2) . . ? N4 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? O2 C20 C21 128.2(3) . . ? O2 C20 C24 113.7(3) . . ? C21 C20 C24 118.1(3) . . ? C22 C21 C20 120.9(2) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? O3 C22 C21 128.9(3) . . ? O3 C22 C23 113.0(2) . . ? C21 C22 C23 118.1(2) . . ? F22 C23 F14 108.5(3) . . ? F22 C23 F17 106.8(3) . . ? F14 C23 F17 105.1(3) . . ? F22 C23 C22 111.3(3) . . ? F14 C23 C22 110.7(2) . . ? F17 C23 C22 114.1(3) . . ? F20 C24 F21 107.9(4) . . ? F20 C24 F16 108.0(4) . . ? F21 C24 F16 105.0(3) . . ? F20 C24 C20 110.3(3) . . ? F21 C24 C20 111.0(3) . . ? F16 C24 C20 114.3(3) . . ? O4 C25 C26 128.3(3) . . ? O4 C25 C29 114.8(2) . . ? C26 C25 C29 116.9(2) . . ? C27 C26 C25 119.7(2) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? O5 C27 C26 128.3(3) . . ? O5 C27 C28 113.5(2) . . ? C26 C27 C28 118.2(2) . . ? F19 C28 F27 110.3(3) . . ? F19 C28 F26 104.0(3) . . ? F27 C28 F26 104.3(3) . . ? F19 C28 C27 115.2(3) . . ? F27 C28 C27 112.1(3) . . ? F26 C28 C27 110.0(3) . . ? F25 C29 F23 108.4(3) . . ? F25 C29 F24 106.8(3) . . ? F23 C29 F24 104.9(3) . . ? F25 C29 C25 111.7(2) . . ? F23 C29 C25 110.6(3) . . ? F24 C29 C25 113.9(3) . . ? O6 C30 C31 127.5(3) . . ? O6 C30 C34 114.0(3) . . ? C31 C30 C34 118.4(3) . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? O7 C32 C31 128.1(3) . . ? O7 C32 C33 113.7(3) . . ? C31 C32 C33 118.2(3) . . ? F29 C33 F30 108.2(4) . . ? F29 C33 F28 106.5(3) . . ? F30 C33 F28 102.8(4) . . ? F29 C33 C32 115.4(3) . . ? F30 C33 C32 111.1(3) . . ? F28 C33 C32 111.9(3) . . ? F32 C34 F33 110.3(4) . . ? F32 C34 F31 107.2(3) . . ? F33 C34 F31 103.7(3) . . ? F32 C34 C30 111.1(3) . . ? F33 C34 C30 111.3(3) . . ? F31 C34 C30 113.0(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 73.39 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.801 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.068 data_7 _database_code_depnum_ccdc_archive 'CCDC 909096' #TrackingRef 'web_deposit_cif_file_0_LaureGuenee_1351875343.Compounds_all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 F12 La N8 O6, 0.5(C28 H4 F36 La2 O16), 2(C2 H3 N)' _chemical_formula_sum 'C66 H54 F30 La2 N10 O14' _chemical_formula_weight 2059.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 11.6721(2) _cell_length_b 15.7298(4) _cell_length_c 22.3967(5) _cell_angle_alpha 78.307(2) _cell_angle_beta 87.1599(17) _cell_angle_gamma 87.3088(18) _cell_volume 4018.90(16) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 16609 _cell_measurement_theta_min 2.8684 _cell_measurement_theta_max 73.3218 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2727 _exptl_crystal_size_mid 0.2193 _exptl_crystal_size_min 0.1389 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 9.331 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.197 _exptl_absorpt_correction_T_max 0.415 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4679 _diffrn_reflns_number 28390 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 73.48 _reflns_number_total 15744 _reflns_number_gt 14417 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP 3 (Farrugia, 1997)' _computing_publication_material SHELX_ACTA _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. Disorder: Two disordered CF3 units were modeled each with 2 components (refined occupancies around 0.5) and with isotropic displacement parameters. One ethyl group is disordered over two sites (refined occupancies 0.55:0.45)and refined with isotropic displacement parameters). ; _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^)+(0.0943P)^2^+2.9832P] 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 15744 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.581456(16) 0.205833(13) 0.129164(8) 0.02609(8) Uani 1 1 d . . . F1H F 0.5464(5) -0.0167(4) 0.3163(2) 0.131(3) Uani 1 1 d . . . F2H F 0.3776(4) -0.0571(3) 0.3201(2) 0.1004(17) Uani 1 1 d . . . F3H F 0.5059(7) -0.1047(3) 0.2646(2) 0.130(3) Uani 1 1 d . . . F4H F 0.1497(4) 0.2412(3) 0.1515(4) 0.134(3) Uani 1 1 d . . . F5H F 0.1040(4) 0.1200(5) 0.2062(3) 0.143(3) Uani 1 1 d . . . F6H F 0.1423(4) 0.1306(4) 0.1147(3) 0.0979(15) Uani 1 1 d . . . F7H F 1.0398(3) 0.2744(4) 0.0160(2) 0.0955(15) Uani 1 1 d . . . F8H F 0.9116(5) 0.3281(4) -0.0415(2) 0.117(2) Uani 1 1 d . . . F9H F 0.9240(6) 0.1919(4) -0.0114(4) 0.163(4) Uani 1 1 d . . . F10A F 0.9473(7) 0.4391(6) 0.1625(4) 0.0865(10) Uiso 0.570(5) 1 d PD A 1 F11A F 0.7850(7) 0.4346(6) 0.2139(4) 0.0865(10) Uiso 0.570(5) 1 d PD A 1 F12A F 0.9166(7) 0.3339(6) 0.2318(4) 0.0865(10) Uiso 0.570(5) 1 d PD A 1 F10B F 0.9584(9) 0.3859(8) 0.1985(5) 0.0865(10) Uiso 0.430(5) 1 d PD A 2 F11B F 0.8049(10) 0.4674(8) 0.1852(6) 0.0865(10) Uiso 0.430(5) 1 d PD A 2 F12B F 0.8102(9) 0.3530(7) 0.2525(5) 0.0865(10) Uiso 0.430(5) 1 d PD A 2 O1A O 0.7503(2) 0.14342(19) 0.19425(13) 0.0356(6) Uani 1 1 d . . . O1B O 0.5289(3) 0.2207(2) 0.23655(13) 0.0403(7) Uani 1 1 d . . . O1H O 0.5280(3) 0.0608(2) 0.19541(13) 0.0388(6) Uani 1 1 d . . . O2H O 0.3664(2) 0.1818(2) 0.13458(14) 0.0383(6) Uani 1 1 d . . . O3H O 0.7020(3) 0.3259(2) 0.15410(14) 0.0384(6) Uani 1 1 d . . . O4H O 0.7506(3) 0.24425(19) 0.05450(13) 0.0356(6) Uani 1 1 d . . . N1A N 0.7128(3) 0.0670(2) 0.10083(15) 0.0297(6) Uani 1 1 d . . . N1B N 0.4408(3) 0.3460(2) 0.14987(16) 0.0338(7) Uani 1 1 d . B . N2A N 0.8092(3) 0.0148(3) 0.25113(17) 0.0407(8) Uani 1 1 d . . . N2B N 0.5113(4) 0.3101(3) 0.30419(19) 0.0533(10) Uani 1 1 d . . . N3A N 0.5338(3) 0.1323(2) 0.03329(15) 0.0300(6) Uani 1 1 d . . . N3B N 0.5106(3) 0.3363(2) 0.03501(15) 0.0321(7) Uani 1 1 d . . . N4A N 0.5893(3) 0.0743(2) -0.04728(15) 0.0329(7) Uani 1 1 d . . . N4B N 0.3852(3) 0.4394(2) -0.00965(16) 0.0364(7) Uani 1 1 d . . . C1A C 0.7157(3) 0.0489(2) 0.04485(18) 0.0312(8) Uani 1 1 d . . . C1B C 0.3737(4) 0.3905(3) 0.10606(19) 0.0335(8) Uani 1 1 d . . . C1H C 0.4423(4) 0.0391(3) 0.2293(2) 0.0411(9) Uani 1 1 d . . . C2A C 0.8079(4) 0.0002(3) 0.0246(2) 0.0416(9) Uani 1 1 d . . . H2A H 0.8111 -0.0107 -0.0156 0.050 Uiso 1 1 calc R . . C2B C 0.2697(4) 0.4294(4) 0.1201(2) 0.0475(11) Uani 1 1 d . . . H2B H 0.2231 0.4598 0.0885 0.057 Uiso 1 1 calc R . . C2H C 0.3298(4) 0.0724(4) 0.2225(2) 0.0451(10) Uani 1 1 d . . . H2H H 0.2718 0.0496 0.2518 0.054 Uiso 1 1 calc R . . C3A C 0.8943(4) -0.0317(3) 0.0643(2) 0.0444(10) Uani 1 1 d . . . H3A H 0.9570 -0.0653 0.0514 0.053 Uiso 1 1 calc R . . C3B C 0.2346(5) 0.4235(4) 0.1804(3) 0.0544(13) Uani 1 1 d . . . H3B H 0.1625 0.4483 0.1909 0.065 Uiso 1 1 calc R . . C3H C 0.3010(4) 0.1381(3) 0.1739(2) 0.0408(9) Uani 1 1 d . . . C4A C 0.8894(4) -0.0147(3) 0.1224(2) 0.0398(9) Uani 1 1 d . . . H4A H 0.9481 -0.0359 0.1501 0.048 Uiso 1 1 calc R . . C4B C 0.3053(4) 0.3811(4) 0.2255(2) 0.0477(11) Uani 1 1 d . B . H4B H 0.2840 0.3777 0.2674 0.057 Uiso 1 1 calc R . . C4H C 0.1728(5) 0.1597(4) 0.1639(3) 0.0595(14) Uani 1 1 d . . . C5A C 0.7963(3) 0.0343(3) 0.13884(18) 0.0328(8) Uani 1 1 d . . . C5B C 0.4078(4) 0.3438(3) 0.20822(19) 0.0372(9) Uani 1 1 d . . . C5H C 0.4662(5) -0.0362(4) 0.2831(3) 0.0599(14) Uani 1 1 d . . . C6A C 0.7838(4) 0.0666(3) 0.19786(18) 0.0342(8) Uani 1 1 d . . . C6B C 0.4880(4) 0.2875(3) 0.25161(19) 0.0392(9) Uani 1 1 d . B . C6H C 0.8071(4) 0.3363(3) 0.1473(2) 0.0419(10) Uani 1 1 d . A . C7A C 0.8255(6) -0.0806(3) 0.2612(2) 0.0558(13) Uani 1 1 d . . . H7AA H 0.8175 -0.0995 0.2221 0.067 Uiso 1 1 calc R . . H7AB H 0.7647 -0.1077 0.2903 0.067 Uiso 1 1 calc R . . C7B C 0.4823(6) 0.3947(4) 0.3207(3) 0.0601(14) Uani 1 1 d . B . H7BA H 0.4502 0.4346 0.2849 0.072 Uiso 1 1 calc R . . H7BB H 0.5535 0.4197 0.3306 0.072 Uiso 1 1 calc R . . C7H C 0.8849(4) 0.3132(3) 0.1034(2) 0.0429(10) Uani 1 1 d . . . H7H H 0.9637 0.3255 0.1040 0.052 Uiso 1 1 calc R . . C8A C 0.9421(7) -0.1118(5) 0.2860(3) 0.082(2) Uani 1 1 d . . . H8AA H 1.0021 -0.0944 0.2543 0.124 Uiso 1 1 calc R . . H8AB H 0.9443 -0.1753 0.2986 0.124 Uiso 1 1 calc R . . H8AC H 0.9554 -0.0860 0.3213 0.124 Uiso 1 1 calc R . . C8B C 0.3972(8) 0.3896(5) 0.3740(3) 0.079(2) Uani 1 1 d . . . H8BA H 0.3247 0.3681 0.3637 0.118 Uiso 1 1 calc R B . H8BB H 0.3836 0.4475 0.3834 0.118 Uiso 1 1 calc R . . H8BC H 0.4279 0.3499 0.4096 0.118 Uiso 1 1 calc R . . C8H C 0.8471(4) 0.2724(3) 0.0588(2) 0.0364(9) Uani 1 1 d . . . C9A C 0.7977(5) 0.0527(4) 0.3058(2) 0.0510(12) Uani 1 1 d . . . H9AA H 0.7878 0.0054 0.3421 0.061 Uiso 1 1 calc R . . H9AB H 0.7279 0.0913 0.3034 0.061 Uiso 1 1 calc R . . C9H C 0.9316(5) 0.2635(4) 0.0055(3) 0.0567(13) Uani 1 1 d . . . C10A C 0.8999(6) 0.1040(6) 0.3138(3) 0.0734(18) Uani 1 1 d . . . H10A H 0.9098 0.1513 0.2782 0.110 Uiso 1 1 calc R . . H10B H 0.9690 0.0657 0.3177 0.110 Uiso 1 1 calc R . . H10C H 0.8873 0.1283 0.3507 0.110 Uiso 1 1 calc R . . C9E C 0.6072(15) 0.2530(13) 0.3405(8) 0.0655(16) Uiso 0.448(11) 1 d P B 1 H9EA H 0.5799 0.2424 0.3839 0.079 Uiso 0.448(11) 1 calc PR B 1 H9EB H 0.6078 0.1961 0.3280 0.079 Uiso 0.448(11) 1 calc PR B 1 C10E C 0.6960(13) 0.2697(10) 0.3400(7) 0.0655(16) Uiso 0.448(11) 1 d P B 1 H10D H 0.7364 0.2274 0.3709 0.098 Uiso 0.448(11) 1 calc PR B 1 H10E H 0.7002 0.3279 0.3489 0.098 Uiso 0.448(11) 1 calc PR B 1 H10F H 0.7320 0.2688 0.2996 0.098 Uiso 0.448(11) 1 calc PR B 1 C9F C 0.5722(13) 0.2481(10) 0.3487(7) 0.0655(16) Uiso 0.552(11) 1 d P B 2 H9FA H 0.6494 0.2422 0.3292 0.079 Uiso 0.552(11) 1 calc PR B 2 H9FB H 0.5831 0.2794 0.3820 0.079 Uiso 0.552(11) 1 calc PR B 2 C10F C 0.5501(11) 0.1699(8) 0.3767(6) 0.0655(16) Uiso 0.552(11) 1 d P B 2 H10G H 0.6144 0.1456 0.4022 0.098 Uiso 0.552(11) 1 calc PR B 2 H10H H 0.5393 0.1338 0.3467 0.098 Uiso 0.552(11) 1 calc PR B 2 H10I H 0.4800 0.1711 0.4026 0.098 Uiso 0.552(11) 1 calc PR B 2 C10H C 0.8559(5) 0.3856(4) 0.1926(3) 0.0593(14) Uani 1 1 d . . . C11A C 0.6144(3) 0.0852(2) 0.00935(18) 0.0309(8) Uani 1 1 d . . . C11B C 0.4218(3) 0.3885(3) 0.04366(18) 0.0317(8) Uani 1 1 d . . . C12A C 0.4514(3) 0.1532(3) -0.01037(17) 0.0312(8) Uani 1 1 d . . . C12B C 0.5337(4) 0.3529(3) -0.02764(18) 0.0330(8) Uani 1 1 d . . . C13A C 0.3481(4) 0.2019(3) -0.01011(19) 0.0345(8) Uani 1 1 d . . . H13A H 0.3229 0.2252 0.0244 0.041 Uiso 1 1 calc R . . C13B C 0.6158(4) 0.3153(3) -0.06295(19) 0.0392(9) Uani 1 1 d . . . H13B H 0.6697 0.2720 -0.0446 0.047 Uiso 1 1 calc R . . C14A C 0.2837(4) 0.2150(3) -0.0615(2) 0.0422(10) Uani 1 1 d . . . H14A H 0.2129 0.2474 -0.0622 0.051 Uiso 1 1 calc R . . C14B C 0.6155(5) 0.3438(3) -0.1256(2) 0.0466(11) Uani 1 1 d . . . H14B H 0.6706 0.3195 -0.1507 0.056 Uiso 1 1 calc R . . C15A C 0.3215(4) 0.1809(3) -0.1131(2) 0.0469(11) Uani 1 1 d . . . H15A H 0.2759 0.1919 -0.1480 0.056 Uiso 1 1 calc R . . C15B C 0.5363(5) 0.4073(3) -0.1528(2) 0.0512(12) Uani 1 1 d . . . H15B H 0.5387 0.4247 -0.1960 0.061 Uiso 1 1 calc R . . C16A C 0.4229(4) 0.1320(3) -0.1143(2) 0.0411(9) Uani 1 1 d . . . H16A H 0.4484 0.1090 -0.1490 0.049 Uiso 1 1 calc R . . C16B C 0.4549(5) 0.4455(3) -0.1191(2) 0.0467(11) Uani 1 1 d . . . H16B H 0.4014 0.4891 -0.1377 0.056 Uiso 1 1 calc R . . C17A C 0.4859(4) 0.1183(3) -0.06126(19) 0.0342(8) Uani 1 1 d . . . C17B C 0.4556(4) 0.4165(3) -0.05585(19) 0.0366(9) Uani 1 1 d . . . C18A C 0.6550(4) 0.0311(3) -0.09132(19) 0.0397(9) Uani 1 1 d . . . H18A H 0.6017 0.0145 -0.1197 0.048 Uiso 1 1 calc R . . H18B H 0.6935 -0.0227 -0.0692 0.048 Uiso 1 1 calc R . . C18B C 0.2891(4) 0.5034(3) -0.0214(2) 0.0458(11) Uani 1 1 d . . . H18C H 0.3071 0.5469 -0.0589 0.055 Uiso 1 1 calc R . . H18D H 0.2781 0.5340 0.0130 0.055 Uiso 1 1 calc R . . C19A C 0.7446(5) 0.0902(4) -0.1277(3) 0.0571(13) Uani 1 1 d . . . H19A H 0.7870 0.0597 -0.1564 0.086 Uiso 1 1 calc R . . H19B H 0.7980 0.1060 -0.0997 0.086 Uiso 1 1 calc R . . H19C H 0.7064 0.1429 -0.1503 0.086 Uiso 1 1 calc R . . C19B C 0.1794(5) 0.4593(4) -0.0291(3) 0.0575(13) Uani 1 1 d . . . H19D H 0.1896 0.4304 -0.0640 0.086 Uiso 1 1 calc R . . H19E H 0.1162 0.5029 -0.0364 0.086 Uiso 1 1 calc R . . H19F H 0.1616 0.4163 0.0079 0.086 Uiso 1 1 calc R . . La2 La 0.950055(19) 0.631851(14) 0.444119(10) 0.03144(8) Uani 1 1 d . . . F1C F 1.2440(7) 0.9185(5) 0.4400(4) 0.171(4) Uani 1 1 d . . . F2C F 1.0691(8) 0.9439(4) 0.4497(6) 0.187(4) Uani 1 1 d . . . F3C F 1.1432(8) 0.8629(6) 0.5153(3) 0.173(4) Uani 1 1 d . . . F4C F 1.3699(4) 0.7319(4) 0.3102(3) 0.114(2) Uani 1 1 d . . . F5C F 1.2361(5) 0.7383(5) 0.25017(19) 0.119(2) Uani 1 1 d . . . F6C F 1.2823(5) 0.6195(3) 0.3053(3) 0.1073(18) Uani 1 1 d . . . F7C F 0.5902(5) 0.7859(4) 0.5033(2) 0.111(2) Uani 1 1 d . . . F8C F 0.6431(4) 0.8888(3) 0.4330(2) 0.0861(12) Uani 1 1 d . . . F9C F 0.5012(3) 0.8163(3) 0.4197(2) 0.0902(13) Uani 1 1 d . . . F1JA F 0.5745(9) 0.6171(7) 0.2915(5) 0.0983(13) Uiso 0.542(8) 1 d P C 1 F2JA F 0.7275(10) 0.6752(8) 0.2356(5) 0.0983(13) Uiso 0.542(8) 1 d P C 1 F3JA F 0.7287(10) 0.5476(8) 0.2867(5) 0.0983(13) Uiso 0.542(8) 1 d P C 1 F1JB F 0.6010(10) 0.6769(8) 0.2599(5) 0.0983(13) Uiso 0.458(8) 1 d P C 2 F2IB F 0.7693(9) 0.6395(7) 0.2362(5) 0.081(3) Uiso 0.458(8) 1 d P C 2 F3JB F 0.6846(11) 0.5453(9) 0.2971(6) 0.0983(13) Uiso 0.458(8) 1 d P C 2 F13C F 0.6002(4) 0.4705(4) 0.4472(3) 0.122(2) Uani 1 1 d . . . F14C F 0.6671(4) 0.3416(4) 0.4719(3) 0.118(2) Uani 1 1 d . . . F15C F 0.6043(4) 0.4061(5) 0.5396(3) 0.123(2) Uani 1 1 d . . . F16C F 1.1044(8) 0.4582(6) 0.3092(2) 0.174(4) Uani 1 1 d . . . F17C F 0.9302(6) 0.4503(4) 0.3250(3) 0.128(2) Uani 1 1 d . . . F18C F 1.0370(9) 0.3361(4) 0.3351(3) 0.179(4) Uani 1 1 d . . . O1C O 1.0265(3) 0.7772(2) 0.44442(17) 0.0478(8) Uani 1 1 d . . . O2C O 1.0899(3) 0.6771(2) 0.35668(14) 0.0435(7) Uani 1 1 d . . . O3C O 0.7824(3) 0.7361(2) 0.44392(17) 0.0500(8) Uani 1 1 d . . . O4C O 0.8351(3) 0.6428(2) 0.35106(15) 0.0466(7) Uani 1 1 d . . . O5C O 0.7903(3) 0.5307(2) 0.47758(16) 0.0452(7) Uani 1 1 d . . . O6C O 0.8523(3) 0.3939(2) 0.51479(16) 0.0441(7) Uani 1 1 d . . . O7C O 1.0183(3) 0.4892(2) 0.42477(19) 0.0528(9) Uani 1 1 d . . . O8C O 1.0792(3) 0.3519(2) 0.44543(15) 0.0485(8) Uani 1 1 d . . . C1C C 1.1203(5) 0.8084(3) 0.4269(3) 0.0522(12) Uani 1 1 d . . . C2C C 1.2005(5) 0.7844(3) 0.3855(2) 0.0507(11) Uani 1 1 d . . . H2C H 1.2724 0.8115 0.3791 0.061 Uiso 1 1 calc R . . C3C C 1.1781(4) 0.7212(3) 0.3529(2) 0.0449(10) Uani 1 1 d . . . C4C C 1.2685(5) 0.7024(5) 0.3051(3) 0.0607(14) Uani 1 1 d . . . C5C C 1.1508(8) 0.8839(5) 0.4565(5) 0.092(3) Uani 1 1 d . . . C6C C 0.6897(4) 0.7475(3) 0.4184(2) 0.0462(11) Uani 1 1 d . . . C7C C 0.6566(5) 0.7133(4) 0.3697(3) 0.0540(12) Uani 1 1 d . . . H7C H 0.5803 0.7241 0.3564 0.065 Uiso 1 1 calc R . . C8C C 0.7331(4) 0.6635(4) 0.3399(2) 0.0484(11) Uani 1 1 d . C . C9C C 0.6891(6) 0.6300(5) 0.2863(3) 0.0706(17) Uani 1 1 d . . . C10C C 0.6033(5) 0.8089(4) 0.4441(3) 0.0619(15) Uani 1 1 d . . . C11C C 0.7815(4) 0.4516(3) 0.49325(19) 0.0390(9) Uani 1 1 d . . . C12C C 0.6628(5) 0.4172(4) 0.4858(3) 0.0621(15) Uani 1 1 d . . . C13C C 1.0425(4) 0.4180(3) 0.4115(2) 0.0383(9) Uani 1 1 d . . . C14C C 1.0221(7) 0.4107(5) 0.3465(3) 0.079(2) Uani 1 1 d . . . N1S N 0.9848(7) 0.7877(4) 0.1586(3) 0.092(2) Uani 1 1 d . . . C1S C 1.0200(8) 0.6287(5) 0.2143(4) 0.086(2) Uani 1 1 d . . . H1SA H 0.9710 0.5901 0.1985 0.128 Uiso 1 1 calc R . . H1SB H 1.0024 0.6244 0.2580 0.128 Uiso 1 1 calc R . . H1SC H 1.1008 0.6116 0.2080 0.128 Uiso 1 1 calc R . . C2S C 0.9988(6) 0.7182(4) 0.1822(3) 0.0650(15) Uani 1 1 d . . . N2S N 0.2575(11) 0.1965(7) 0.3299(5) 0.144(4) Uani 1 1 d . . . C3S C 0.1566(8) 0.1524(5) 0.4338(4) 0.084(2) Uani 1 1 d . . . H3SA H 0.0883 0.1203 0.4298 0.126 Uiso 1 1 calc R . . H3SB H 0.1335 0.2047 0.4495 0.126 Uiso 1 1 calc R . . H3SC H 0.2083 0.1155 0.4622 0.126 Uiso 1 1 calc R . . C4S C 0.2151(8) 0.1769(5) 0.3749(4) 0.083(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.02734(12) 0.02649(12) 0.02303(12) -0.00194(8) -0.00085(8) 0.00004(8) F1H 0.122(4) 0.152(5) 0.091(3) 0.067(3) -0.055(3) -0.063(4) F2H 0.082(3) 0.109(4) 0.080(3) 0.045(3) 0.030(2) -0.004(2) F3H 0.206(7) 0.065(3) 0.091(3) 0.031(3) 0.034(4) 0.044(4) F4H 0.051(2) 0.076(3) 0.289(9) -0.066(4) -0.040(4) 0.021(2) F5H 0.039(2) 0.235(8) 0.125(4) 0.027(5) 0.022(2) -0.003(3) F6H 0.058(2) 0.118(4) 0.132(4) -0.051(3) -0.035(2) 0.005(2) F7H 0.0431(19) 0.133(4) 0.111(3) -0.029(3) 0.027(2) -0.009(2) F8H 0.111(4) 0.154(5) 0.065(3) 0.013(3) 0.037(3) 0.023(4) F9H 0.167(6) 0.120(4) 0.232(8) -0.129(5) 0.152(6) -0.084(4) O1A 0.0354(14) 0.0352(15) 0.0354(14) -0.0050(11) -0.0067(11) 0.0045(11) O1B 0.0463(17) 0.0428(17) 0.0295(14) -0.0035(12) 0.0011(12) 0.0051(13) O1H 0.0405(16) 0.0364(16) 0.0349(15) 0.0024(12) 0.0036(12) -0.0032(12) O2H 0.0302(14) 0.0440(17) 0.0389(15) -0.0042(12) -0.0012(11) -0.0020(12) O3H 0.0433(16) 0.0350(15) 0.0386(15) -0.0109(12) -0.0074(12) 0.0009(12) O4H 0.0402(15) 0.0349(15) 0.0318(14) -0.0063(11) 0.0000(11) -0.0062(12) N1A 0.0316(16) 0.0253(15) 0.0300(15) 0.0001(12) -0.0025(12) -0.0016(12) N1B 0.0351(17) 0.0308(17) 0.0357(17) -0.0077(13) -0.0013(13) 0.0001(13) N2A 0.0432(19) 0.043(2) 0.0329(18) 0.0004(15) -0.0085(14) 0.0051(16) N2B 0.078(3) 0.048(2) 0.035(2) -0.0095(17) -0.0104(19) -0.006(2) N3A 0.0339(16) 0.0263(16) 0.0292(15) -0.0034(12) -0.0034(12) -0.0021(12) N3B 0.0379(17) 0.0312(16) 0.0267(15) -0.0041(12) -0.0021(13) -0.0020(13) N4A 0.0391(17) 0.0296(16) 0.0308(16) -0.0073(13) 0.0007(13) -0.0055(13) N4B 0.0409(18) 0.0298(17) 0.0365(18) 0.0001(13) -0.0089(14) -0.0009(14) C1A 0.0348(19) 0.0252(18) 0.0319(18) -0.0011(14) 0.0001(15) -0.0045(14) C1B 0.037(2) 0.0283(19) 0.035(2) -0.0064(15) -0.0043(16) 0.0016(15) C1H 0.045(2) 0.043(2) 0.033(2) -0.0018(17) 0.0044(17) -0.0094(19) C2A 0.048(2) 0.038(2) 0.037(2) -0.0071(17) 0.0003(18) 0.0054(19) C2B 0.045(3) 0.050(3) 0.048(3) -0.014(2) -0.010(2) 0.013(2) C2H 0.038(2) 0.058(3) 0.037(2) -0.005(2) 0.0078(17) -0.009(2) C3A 0.042(2) 0.038(2) 0.051(3) -0.0066(19) 0.0004(19) 0.0116(18) C3B 0.047(3) 0.062(3) 0.057(3) -0.021(3) 0.002(2) 0.011(2) C3H 0.032(2) 0.047(2) 0.045(2) -0.0148(19) 0.0026(17) -0.0026(18) C4A 0.040(2) 0.037(2) 0.039(2) -0.0022(17) -0.0047(17) 0.0060(17) C4B 0.046(3) 0.053(3) 0.046(2) -0.017(2) 0.006(2) 0.004(2) C4H 0.038(3) 0.073(4) 0.067(3) -0.011(3) 0.001(2) 0.001(2) C5A 0.0344(19) 0.0271(18) 0.0342(19) 0.0005(15) -0.0018(15) -0.0004(15) C5B 0.041(2) 0.037(2) 0.035(2) -0.0096(16) 0.0010(16) -0.0048(17) C5H 0.060(3) 0.058(3) 0.052(3) 0.013(2) 0.008(2) -0.011(3) C6A 0.0343(19) 0.037(2) 0.0288(18) 0.0000(15) -0.0056(15) 0.0016(16) C6B 0.042(2) 0.043(2) 0.032(2) -0.0060(17) 0.0046(16) -0.0068(18) C6H 0.042(2) 0.032(2) 0.051(3) -0.0049(18) -0.0133(19) 0.0049(17) C7A 0.080(4) 0.039(3) 0.042(3) 0.005(2) -0.010(2) 0.007(2) C7B 0.090(4) 0.050(3) 0.045(3) -0.015(2) -0.014(3) -0.011(3) C7H 0.033(2) 0.041(2) 0.057(3) -0.014(2) -0.0097(18) -0.0008(17) C8A 0.106(6) 0.078(5) 0.061(4) -0.012(3) -0.030(4) 0.044(4) C8B 0.130(7) 0.067(4) 0.045(3) -0.024(3) -0.003(3) -0.002(4) C8H 0.034(2) 0.029(2) 0.044(2) -0.0032(16) 0.0011(17) -0.0012(16) C9A 0.061(3) 0.057(3) 0.034(2) -0.006(2) -0.008(2) 0.009(2) C9H 0.046(3) 0.056(3) 0.067(3) -0.013(3) 0.018(2) -0.009(2) C10A 0.073(4) 0.102(5) 0.056(3) -0.039(3) -0.012(3) -0.003(4) C10H 0.054(3) 0.056(3) 0.074(4) -0.022(3) -0.031(3) 0.003(2) C11A 0.0355(19) 0.0232(17) 0.0321(18) -0.0004(14) 0.0001(15) -0.0049(14) C11B 0.0352(19) 0.0288(19) 0.0305(18) -0.0029(14) -0.0073(15) -0.0018(15) C12A 0.0365(19) 0.0268(18) 0.0298(18) -0.0019(14) -0.0024(15) -0.0109(15) C12B 0.041(2) 0.0287(19) 0.0279(18) 0.0000(14) -0.0054(15) -0.0090(16) C13A 0.035(2) 0.033(2) 0.036(2) -0.0073(16) -0.0064(16) -0.0046(16) C13B 0.049(2) 0.036(2) 0.033(2) -0.0054(16) 0.0025(17) -0.0098(18) C14A 0.036(2) 0.037(2) 0.051(3) -0.0015(19) -0.0093(18) -0.0031(17) C14B 0.062(3) 0.046(3) 0.032(2) -0.0071(18) 0.0071(19) -0.015(2) C15A 0.051(3) 0.050(3) 0.038(2) -0.0018(19) -0.0133(19) -0.009(2) C15B 0.075(3) 0.051(3) 0.026(2) 0.0011(18) -0.007(2) -0.021(2) C16A 0.049(2) 0.044(2) 0.031(2) -0.0057(17) -0.0063(17) -0.0106(19) C16B 0.060(3) 0.041(2) 0.036(2) 0.0057(18) -0.013(2) -0.013(2) C17A 0.041(2) 0.0282(19) 0.0333(19) -0.0034(15) -0.0019(16) -0.0081(16) C17B 0.044(2) 0.031(2) 0.034(2) -0.0012(15) -0.0078(16) -0.0089(16) C18A 0.049(2) 0.041(2) 0.031(2) -0.0129(17) 0.0037(17) -0.0055(19) C18B 0.047(2) 0.029(2) 0.058(3) 0.0038(19) -0.016(2) -0.0028(18) C19A 0.068(3) 0.054(3) 0.046(3) -0.005(2) 0.020(2) -0.010(3) C19B 0.050(3) 0.052(3) 0.071(4) -0.008(3) -0.018(3) -0.005(2) La2 0.03440(13) 0.02822(13) 0.03123(13) -0.00422(9) -0.00397(9) -0.00130(9) F1C 0.167(6) 0.179(7) 0.208(7) -0.139(6) 0.109(5) -0.130(6) F2C 0.180(8) 0.079(4) 0.334(14) -0.112(7) -0.020(8) -0.004(4) F3C 0.220(9) 0.213(9) 0.123(5) -0.108(6) 0.059(5) -0.134(7) F4C 0.068(3) 0.142(5) 0.148(5) -0.073(4) 0.048(3) -0.037(3) F5C 0.122(4) 0.174(6) 0.046(2) 0.003(3) 0.026(2) 0.013(4) F6C 0.101(3) 0.079(3) 0.142(5) -0.038(3) 0.058(3) -0.005(3) F7C 0.129(4) 0.129(4) 0.057(2) 0.004(2) 0.020(2) 0.060(4) F8C 0.097(3) 0.055(2) 0.104(3) -0.018(2) 0.000(2) 0.022(2) F9C 0.054(2) 0.106(3) 0.111(3) -0.028(3) -0.011(2) 0.028(2) F13C 0.075(3) 0.104(4) 0.176(6) 0.013(4) -0.075(3) -0.012(3) F14C 0.087(3) 0.089(3) 0.198(6) -0.067(4) -0.049(4) -0.019(3) F15C 0.069(3) 0.153(5) 0.139(5) -0.017(4) 0.041(3) -0.040(3) F16C 0.206(8) 0.235(9) 0.051(3) 0.011(4) 0.043(4) 0.078(7) F17C 0.154(5) 0.146(5) 0.097(4) -0.056(3) -0.076(4) 0.076(4) F18C 0.341(11) 0.112(4) 0.110(4) -0.081(4) -0.132(6) 0.116(6) O1C 0.0536(19) 0.0321(16) 0.056(2) -0.0080(14) 0.0094(15) -0.0052(14) O2C 0.0471(17) 0.0458(18) 0.0366(15) -0.0043(13) -0.0002(13) -0.0091(14) O3C 0.055(2) 0.0420(18) 0.055(2) -0.0136(15) -0.0118(16) 0.0084(15) O4C 0.0467(18) 0.0502(19) 0.0439(17) -0.0103(14) -0.0100(14) 0.0020(14) O5C 0.0413(16) 0.0370(17) 0.0537(19) 0.0002(14) -0.0032(14) -0.0029(13) O6C 0.0402(16) 0.0378(17) 0.0507(18) 0.0017(14) -0.0083(13) -0.0060(13) O7C 0.053(2) 0.0386(18) 0.072(2) -0.0262(17) 0.0066(17) -0.0044(15) O8C 0.060(2) 0.0464(19) 0.0375(16) -0.0047(14) -0.0042(14) 0.0042(15) C1C 0.062(3) 0.038(2) 0.057(3) -0.007(2) 0.002(2) -0.011(2) C2C 0.052(3) 0.041(3) 0.056(3) -0.003(2) 0.005(2) -0.014(2) C3C 0.049(3) 0.046(3) 0.036(2) 0.0019(18) -0.0015(18) -0.003(2) C4C 0.055(3) 0.072(4) 0.056(3) -0.014(3) 0.013(2) -0.011(3) C5C 0.100(6) 0.066(5) 0.121(7) -0.050(5) 0.038(5) -0.038(4) C6C 0.048(3) 0.038(2) 0.047(2) 0.0030(19) -0.004(2) 0.0046(19) C7C 0.048(3) 0.059(3) 0.053(3) -0.006(2) -0.016(2) 0.006(2) C8C 0.046(3) 0.052(3) 0.046(3) -0.005(2) -0.014(2) -0.002(2) C9C 0.065(4) 0.095(5) 0.055(3) -0.019(3) -0.018(3) 0.005(3) C10C 0.059(3) 0.065(4) 0.053(3) 0.003(3) 0.000(2) 0.019(3) C11C 0.036(2) 0.047(3) 0.033(2) -0.0064(17) -0.0033(16) -0.0035(18) C12C 0.044(3) 0.052(3) 0.090(4) -0.011(3) -0.014(3) -0.005(2) C13C 0.041(2) 0.038(2) 0.036(2) -0.0095(17) 0.0013(16) -0.0003(17) C14C 0.117(6) 0.082(5) 0.038(3) -0.021(3) -0.020(3) 0.060(4) N1S 0.120(6) 0.059(4) 0.089(4) -0.002(3) -0.006(4) 0.021(4) C1S 0.106(6) 0.050(4) 0.100(6) -0.012(4) -0.017(5) 0.000(4) C2S 0.077(4) 0.055(4) 0.061(3) -0.010(3) -0.004(3) 0.009(3) N2S 0.176(10) 0.109(7) 0.146(9) -0.038(6) 0.078(8) -0.016(7) C3S 0.118(6) 0.054(4) 0.084(5) -0.025(3) 0.014(4) -0.007(4) C4S 0.094(5) 0.059(4) 0.100(6) -0.028(4) 0.019(4) -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 La1 O1B 2.507(3) . ? La1 O4H 2.537(3) . ? La1 O1H 2.543(3) . ? La1 O1A 2.549(3) . ? La1 O2H 2.550(3) . ? La1 O3H 2.571(3) . ? La1 N3A 2.728(3) . ? La1 N3B 2.757(3) . ? La1 N1A 2.769(3) . ? La1 N1B 2.788(3) . ? F1H C5H 1.309(8) . ? F2H C5H 1.304(7) . ? F3H C5H 1.289(9) . ? F4H C4H 1.274(8) . ? F5H C4H 1.290(8) . ? F6H C4H 1.346(8) . ? F7H C9H 1.321(7) . ? F8H C9H 1.328(8) . ? F9H C9H 1.266(8) . ? F10A C10H 1.444(11) . ? F11A C10H 1.247(10) . ? F12A C10H 1.285(10) . ? F10B C10H 1.211(12) . ? F11B C10H 1.374(13) . ? F12B C10H 1.421(12) . ? O1A C6A 1.240(5) . ? O1B C6B 1.235(6) . ? O1H C1H 1.243(5) . ? O2H C3H 1.252(6) . ? O3H C6H 1.243(6) . ? O4H C8H 1.244(5) . ? N1A C1A 1.340(5) . ? N1A C5A 1.341(5) . ? N1B C5B 1.338(6) . ? N1B C1B 1.346(5) . ? N2A C6A 1.339(5) . ? N2A C9A 1.464(6) . ? N2A C7A 1.476(7) . ? N2B C6B 1.341(6) . ? N2B C9F 1.436(16) . ? N2B C7B 1.471(7) . ? N2B C9E 1.556(19) . ? N3A C11A 1.330(5) . ? N3A C12A 1.387(5) . ? N3B C11B 1.324(6) . ? N3B C12B 1.389(5) . ? N4A C11A 1.361(5) . ? N4A C17A 1.380(6) . ? N4A C18A 1.473(5) . ? N4B C11B 1.371(5) . ? N4B C17B 1.384(6) . ? N4B C18B 1.468(6) . ? C1A C2A 1.402(6) . ? C1A C11A 1.484(6) . ? C1B C2B 1.384(6) . ? C1B C11B 1.486(6) . ? C1H C2H 1.395(7) . ? C1H C5H 1.536(7) . ? C2A C3A 1.385(7) . ? C2A H2A 0.9500 . ? C2B C3B 1.379(8) . ? C2B H2B 0.9500 . ? C2H C3H 1.383(7) . ? C2H H2H 0.9500 . ? C3A C4A 1.379(7) . ? C3A H3A 0.9500 . ? C3B C4B 1.379(8) . ? C3B H3B 0.9500 . ? C3H C4H 1.536(7) . ? C4A C5A 1.381(6) . ? C4A H4A 0.9500 . ? C4B C5B 1.381(7) . ? C4B H4B 0.9500 . ? C5A C6A 1.508(6) . ? C5B C6B 1.506(6) . ? C6H C7H 1.396(7) . ? C6H C10H 1.541(7) . ? C7A C8A 1.519(9) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C7B C8B 1.507(10) . ? C7B H7BA 0.9900 . ? C7B H7BB 0.9900 . ? C7H C8H 1.391(6) . ? C7H H7H 0.9500 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C8B H8BC 0.9800 . ? C8H C9H 1.535(7) . ? C9A C10A 1.509(9) . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C9E C10E 1.08(2) . ? C9E H9EA 0.9900 . ? C9E H9EB 0.9900 . ? C10E H10D 0.9800 . ? C10E H10E 0.9800 . ? C10E H10F 0.9800 . ? C9F C10F 1.29(2) . ? C9F H9FA 0.9900 . ? C9F H9FB 0.9900 . ? C10F H10G 0.9800 . ? C10F H10H 0.9800 . ? C10F H10I 0.9800 . ? C12A C17A 1.397(6) . ? C12A C13A 1.398(6) . ? C12B C17B 1.395(6) . ? C12B C13B 1.397(6) . ? C13A C14A 1.382(6) . ? C13A H13A 0.9500 . ? C13B C14B 1.384(6) . ? C13B H13B 0.9500 . ? C14A C15A 1.412(7) . ? C14A H14A 0.9500 . ? C14B C15B 1.396(8) . ? C14B H14B 0.9500 . ? C15A C16A 1.383(7) . ? C15A H15A 0.9500 . ? C15B C16B 1.376(8) . ? C15B H15B 0.9500 . ? C16A C17A 1.402(6) . ? C16A H16A 0.9500 . ? C16B C17B 1.398(6) . ? C16B H16B 0.9500 . ? C18A C19A 1.524(7) . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C18B C19B 1.518(7) . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? La2 O7C 2.460(3) . ? La2 O3C 2.493(3) . ? La2 O1C 2.494(3) . ? La2 O5C 2.495(3) . ? La2 O2C 2.497(3) . ? La2 O4C 2.507(3) . ? La2 O6C 2.510(3) 2_766 ? La2 O8C 2.543(3) 2_766 ? F1C C5C 1.246(9) . ? F2C C5C 1.301(13) . ? F3C C5C 1.290(12) . ? F4C C4C 1.309(8) . ? F5C C4C 1.311(8) . ? F6C C4C 1.306(8) . ? F7C C10C 1.304(7) . ? F8C C10C 1.332(8) . ? F9C C10C 1.326(8) . ? F1JA C9C 1.358(12) . ? F2JA C9C 1.282(13) . ? F3JA C9C 1.353(14) . ? F1JB C9C 1.328(14) . ? F2IB C9C 1.412(13) . ? F3JB C9C 1.308(16) . ? F13C C12C 1.301(8) . ? F14C C12C 1.286(8) . ? F15C C12C 1.340(9) . ? F16C C14C 1.383(12) . ? F17C C14C 1.279(8) . ? F18C C14C 1.253(8) . ? O1C C1C 1.235(7) . ? O2C C3C 1.258(6) . ? O3C C6C 1.237(6) . ? O4C C8C 1.243(6) . ? O5C C11C 1.230(6) . ? O6C C11C 1.238(6) . ? O6C La2 2.510(3) 2_766 ? O7C C13C 1.232(6) . ? O8C C13C 1.231(6) . ? O8C La2 2.543(3) 2_766 ? C1C C2C 1.380(8) . ? C1C C5C 1.535(9) . ? C2C C3C 1.386(8) . ? C2C H2C 0.9500 . ? C3C C4C 1.529(7) . ? C6C C7C 1.389(8) . ? C6C C10C 1.535(8) . ? C7C C8C 1.395(8) . ? C7C H7C 0.9500 . ? C8C C9C 1.525(8) . ? C11C C12C 1.540(7) . ? C13C C14C 1.514(7) . ? N1S C2S 1.122(9) . ? C1S C2S 1.461(9) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? N2S C4S 1.092(12) . ? C3S C4S 1.445(11) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1B La1 O4H 136.14(10) . . ? O1B La1 O1H 68.72(11) . . ? O4H La1 O1H 130.26(10) . . ? O1B La1 O1A 72.71(10) . . ? O4H La1 O1A 78.26(9) . . ? O1H La1 O1A 70.89(10) . . ? O1B La1 O2H 78.78(10) . . ? O4H La1 O2H 142.50(9) . . ? O1H La1 O2H 67.01(10) . . ? O1A La1 O2H 135.36(10) . . ? O1B La1 O3H 72.09(11) . . ? O4H La1 O3H 66.84(10) . . ? O1H La1 O3H 129.60(10) . . ? O1A La1 O3H 68.08(10) . . ? O2H La1 O3H 133.16(10) . . ? O1B La1 N3A 146.98(10) . . ? O4H La1 N3A 76.32(9) . . ? O1H La1 N3A 85.34(10) . . ? O1A La1 N3A 118.68(10) . . ? O2H La1 N3A 72.26(10) . . ? O3H La1 N3A 140.45(10) . . ? O1B La1 N3B 118.40(10) . . ? O4H La1 N3B 71.58(10) . . ? O1H La1 N3B 143.98(10) . . ? O1A La1 N3B 144.62(10) . . ? O2H La1 N3B 79.47(10) . . ? O3H La1 N3B 83.10(10) . . ? N3A La1 N3B 71.77(10) . . ? O1B La1 N1A 123.08(10) . . ? O4H La1 N1A 63.98(10) . . ? O1H La1 N1A 66.98(10) . . ? O1A La1 N1A 60.30(10) . . ? O2H La1 N1A 113.23(10) . . ? O3H La1 N1A 113.33(10) . . ? N3A La1 N1A 58.37(10) . . ? N3B La1 N1A 118.49(10) . . ? O1B La1 N1B 60.48(10) . . ? O4H La1 N1B 115.43(10) . . ? O1H La1 N1B 114.09(10) . . ? O1A La1 N1B 123.87(10) . . ? O2H La1 N1B 64.46(10) . . ? O3H La1 N1B 69.37(10) . . ? N3A La1 N1B 117.46(10) . . ? N3B La1 N1B 58.08(10) . . ? N1A La1 N1B 175.80(10) . . ? C6A O1A La1 120.6(3) . . ? C6B O1B La1 125.0(3) . . ? C1H O1H La1 131.5(3) . . ? C3H O2H La1 133.0(3) . . ? C6H O3H La1 130.0(3) . . ? C8H O4H La1 133.7(3) . . ? C1A N1A C5A 119.3(4) . . ? C1A N1A La1 121.6(2) . . ? C5A N1A La1 116.7(3) . . ? C5B N1B C1B 118.4(4) . . ? C5B N1B La1 115.2(3) . . ? C1B N1B La1 120.9(3) . . ? C6A N2A C9A 117.4(4) . . ? C6A N2A C7A 125.0(4) . . ? C9A N2A C7A 116.5(4) . . ? C6B N2B C9F 118.3(7) . . ? C6B N2B C7B 125.9(4) . . ? C9F N2B C7B 115.8(7) . . ? C6B N2B C9E 114.6(8) . . ? C9F N2B C9E 16.4(8) . . ? C7B N2B C9E 116.8(8) . . ? C11A N3A C12A 105.3(3) . . ? C11A N3A La1 120.1(3) . . ? C12A N3A La1 131.6(3) . . ? C11B N3B C12B 105.4(3) . . ? C11B N3B La1 120.1(3) . . ? C12B N3B La1 133.2(3) . . ? C11A N4A C17A 106.9(3) . . ? C11A N4A C18A 131.2(4) . . ? C17A N4A C18A 121.8(3) . . ? C11B N4B C17B 106.1(3) . . ? C11B N4B C18B 131.1(4) . . ? C17B N4B C18B 122.7(4) . . ? N1A C1A C2A 120.8(4) . . ? N1A C1A C11A 113.2(3) . . ? C2A C1A C11A 126.0(4) . . ? N1B C1B C2B 121.6(4) . . ? N1B C1B C11B 112.5(4) . . ? C2B C1B C11B 125.8(4) . . ? O1H C1H C2H 127.9(4) . . ? O1H C1H C5H 114.0(4) . . ? C2H C1H C5H 118.0(4) . . ? C3A C2A C1A 118.9(4) . . ? C3A C2A H2A 120.5 . . ? C1A C2A H2A 120.5 . . ? C3B C2B C1B 119.2(5) . . ? C3B C2B H2B 120.4 . . ? C1B C2B H2B 120.4 . . ? C3H C2H C1H 121.3(4) . . ? C3H C2H H2H 119.4 . . ? C1H C2H H2H 119.4 . . ? C4A C3A C2A 120.1(4) . . ? C4A C3A H3A 120.0 . . ? C2A C3A H3A 120.0 . . ? C2B C3B C4B 119.3(5) . . ? C2B C3B H3B 120.3 . . ? C4B C3B H3B 120.3 . . ? O2H C3H C2H 128.4(4) . . ? O2H C3H C4H 114.0(4) . . ? C2H C3H C4H 117.5(4) . . ? C3A C4A C5A 117.7(4) . . ? C3A C4A H4A 121.2 . . ? C5A C4A H4A 121.2 . . ? C3B C4B C5B 118.3(5) . . ? C3B C4B H4B 120.8 . . ? C5B C4B H4B 120.8 . . ? F4H C4H F5H 111.7(7) . . ? F4H C4H F6H 104.9(6) . . ? F5H C4H F6H 102.1(6) . . ? F4H C4H C3H 112.7(5) . . ? F5H C4H C3H 115.1(5) . . ? F6H C4H C3H 109.2(5) . . ? N1A C5A C4A 123.2(4) . . ? N1A C5A C6A 111.9(4) . . ? C4A C5A C6A 124.4(4) . . ? N1B C5B C4B 123.0(4) . . ? N1B C5B C6B 112.0(4) . . ? C4B C5B C6B 124.6(4) . . ? F3H C5H F2H 108.6(6) . . ? F3H C5H F1H 105.0(7) . . ? F2H C5H F1H 106.3(6) . . ? F3H C5H C1H 111.5(5) . . ? F2H C5H C1H 114.2(5) . . ? F1H C5H C1H 110.6(5) . . ? O1A C6A N2A 122.1(4) . . ? O1A C6A C5A 116.6(3) . . ? N2A C6A C5A 121.3(4) . . ? O1B C6B N2B 122.9(4) . . ? O1B C6B C5B 117.0(4) . . ? N2B C6B C5B 120.1(4) . . ? O3H C6H C7H 129.4(4) . . ? O3H C6H C10H 114.3(4) . . ? C7H C6H C10H 116.2(4) . . ? N2A C7A C8A 112.3(5) . . ? N2A C7A H7AA 109.1 . . ? C8A C7A H7AA 109.1 . . ? N2A C7A H7AB 109.1 . . ? C8A C7A H7AB 109.1 . . ? H7AA C7A H7AB 107.9 . . ? N2B C7B C8B 113.6(5) . . ? N2B C7B H7BA 108.8 . . ? C8B C7B H7BA 108.8 . . ? N2B C7B H7BB 108.8 . . ? C8B C7B H7BB 108.8 . . ? H7BA C7B H7BB 107.7 . . ? C8H C7H C6H 120.1(4) . . ? C8H C7H H7H 120.0 . . ? C6H C7H H7H 120.0 . . ? C7A C8A H8AA 109.5 . . ? C7A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C7A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7B C8B H8BA 109.5 . . ? C7B C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? C7B C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? O4H C8H C7H 128.6(4) . . ? O4H C8H C9H 114.0(4) . . ? C7H C8H C9H 117.3(4) . . ? N2A C9A C10A 113.0(5) . . ? N2A C9A H9AA 109.0 . . ? C10A C9A H9AA 109.0 . . ? N2A C9A H9AB 109.0 . . ? C10A C9A H9AB 109.0 . . ? H9AA C9A H9AB 107.8 . . ? F9H C9H F7H 109.3(6) . . ? F9H C9H F8H 109.0(7) . . ? F7H C9H F8H 102.1(5) . . ? F9H C9H C8H 112.3(5) . . ? F7H C9H C8H 114.2(5) . . ? F8H C9H C8H 109.5(5) . . ? C9A C10A H10A 109.5 . . ? C9A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C9A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C10E C9E N2B 125.3(18) . . ? C10E C9E H9EA 106.0 . . ? N2B C9E H9EA 106.0 . . ? C10E C9E H9EB 106.0 . . ? N2B C9E H9EB 106.0 . . ? H9EA C9E H9EB 106.3 . . ? C10F C9F N2B 132.3(13) . . ? C10F C9F H9FA 104.2 . . ? N2B C9F H9FA 104.2 . . ? C10F C9F H9FB 104.2 . . ? N2B C9F H9FB 104.2 . . ? H9FA C9F H9FB 105.5 . . ? C9F C10F H10G 109.5 . . ? C9F C10F H10H 109.5 . . ? H10G C10F H10H 109.5 . . ? C9F C10F H10I 109.5 . . ? H10G C10F H10I 109.5 . . ? H10H C10F H10I 109.5 . . ? F10B C10H F11A 123.6(8) . . ? F10B C10H F12A 52.3(6) . . ? F11A C10H F12A 115.9(8) . . ? F10B C10H F11B 112.5(9) . . ? F11A C10H F11B 33.8(5) . . ? F12A C10H F11B 138.6(8) . . ? F10B C10H F12B 104.4(8) . . ? F11A C10H F12B 64.0(7) . . ? F12A C10H F12B 59.4(6) . . ? F11B C10H F12B 97.4(8) . . ? F10B C10H F10A 45.4(6) . . ? F11A C10H F10A 106.8(7) . . ? F12A C10H F10A 97.7(6) . . ? F11B C10H F10A 78.1(7) . . ? F12B C10H F10A 139.6(7) . . ? F10B C10H C6H 120.6(7) . . ? F11A C10H C6H 114.8(6) . . ? F12A C10H C6H 110.6(6) . . ? F11B C10H C6H 109.5(6) . . ? F12B C10H C6H 109.8(6) . . ? F10A C10H C6H 109.4(6) . . ? N3A C11A N4A 112.5(3) . . ? N3A C11A C1A 120.2(4) . . ? N4A C11A C1A 127.3(4) . . ? N3B C11B N4B 112.8(4) . . ? N3B C11B C1B 121.0(3) . . ? N4B C11B C1B 126.2(4) . . ? N3A C12A C17A 109.5(4) . . ? N3A C12A C13A 130.5(4) . . ? C17A C12A C13A 120.0(4) . . ? N3B C12B C17B 109.3(4) . . ? N3B C12B C13B 130.7(4) . . ? C17B C12B C13B 119.9(4) . . ? C14A C13A C12A 118.1(4) . . ? C14A C13A H13A 121.0 . . ? C12A C13A H13A 121.0 . . ? C14B C13B C12B 117.5(5) . . ? C14B C13B H13B 121.2 . . ? C12B C13B H13B 121.2 . . ? C13A C14A C15A 121.1(4) . . ? C13A C14A H14A 119.5 . . ? C15A C14A H14A 119.5 . . ? C13B C14B C15B 121.5(5) . . ? C13B C14B H14B 119.2 . . ? C15B C14B H14B 119.2 . . ? C16A C15A C14A 122.0(4) . . ? C16A C15A H15A 119.0 . . ? C14A C15A H15A 119.0 . . ? C16B C15B C14B 122.1(4) . . ? C16B C15B H15B 118.9 . . ? C14B C15B H15B 118.9 . . ? C15A C16A C17A 116.0(4) . . ? C15A C16A H16A 122.0 . . ? C17A C16A H16A 122.0 . . ? C15B C16B C17B 116.0(5) . . ? C15B C16B H16B 122.0 . . ? C17B C16B H16B 122.0 . . ? N4A C17A C12A 105.9(3) . . ? N4A C17A C16A 131.2(4) . . ? C12A C17A C16A 122.9(4) . . ? N4B C17B C12B 106.4(4) . . ? N4B C17B C16B 130.7(4) . . ? C12B C17B C16B 122.9(5) . . ? N4A C18A C19A 111.3(4) . . ? N4A C18A H18A 109.4 . . ? C19A C18A H18A 109.4 . . ? N4A C18A H18B 109.4 . . ? C19A C18A H18B 109.4 . . ? H18A C18A H18B 108.0 . . ? N4B C18B C19B 110.7(4) . . ? N4B C18B H18C 109.5 . . ? C19B C18B H18C 109.5 . . ? N4B C18B H18D 109.5 . . ? C19B C18B H18D 109.5 . . ? H18C C18B H18D 108.1 . . ? C18A C19A H19A 109.5 . . ? C18A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? O7C La2 O3C 145.76(12) . . ? O7C La2 O1C 139.34(12) . . ? O3C La2 O1C 72.58(12) . . ? O7C La2 O5C 73.29(12) . . ? O3C La2 O5C 78.70(12) . . ? O1C La2 O5C 146.41(11) . . ? O7C La2 O2C 79.48(12) . . ? O3C La2 O2C 112.88(12) . . ? O1C La2 O2C 68.49(11) . . ? O5C La2 O2C 141.09(12) . . ? O7C La2 O4C 85.60(13) . . ? O3C La2 O4C 68.32(12) . . ? O1C La2 O4C 108.76(12) . . ? O5C La2 O4C 75.27(12) . . ? O2C La2 O4C 75.43(11) . . ? O7C La2 O6C 74.07(12) . 2_766 ? O3C La2 O6C 139.39(12) . 2_766 ? O1C La2 O6C 72.97(12) . 2_766 ? O5C La2 O6C 123.54(10) . 2_766 ? O2C La2 O6C 72.69(11) . 2_766 ? O4C La2 O6C 144.67(12) . 2_766 ? O7C La2 O8C 117.79(13) . 2_766 ? O3C La2 O8C 75.28(12) . 2_766 ? O1C La2 O8C 76.06(12) . 2_766 ? O5C La2 O8C 80.14(12) . 2_766 ? O2C La2 O8C 138.06(12) . 2_766 ? O4C La2 O8C 139.16(12) . 2_766 ? O6C La2 O8C 76.13(12) 2_766 2_766 ? C1C O1C La2 131.5(3) . . ? C3C O2C La2 130.3(3) . . ? C6C O3C La2 135.0(3) . . ? C8C O4C La2 133.4(3) . . ? C11C O5C La2 136.1(3) . . ? C11C O6C La2 143.3(3) . 2_766 ? C13C O7C La2 173.2(4) . . ? C13C O8C La2 109.6(3) . 2_766 ? O1C C1C C2C 129.1(5) . . ? O1C C1C C5C 114.4(5) . . ? C2C C1C C5C 116.5(5) . . ? C1C C2C C3C 121.1(5) . . ? C1C C2C H2C 119.4 . . ? C3C C2C H2C 119.4 . . ? O2C C3C C2C 128.1(5) . . ? O2C C3C C4C 114.1(5) . . ? C2C C3C C4C 117.8(5) . . ? F6C C4C F4C 107.4(6) . . ? F6C C4C F5C 105.6(6) . . ? F4C C4C F5C 106.3(6) . . ? F6C C4C C3C 112.3(5) . . ? F4C C4C C3C 114.5(5) . . ? F5C C4C C3C 110.2(5) . . ? F1C C5C F3C 109.6(9) . . ? F1C C5C F2C 108.7(9) . . ? F3C C5C F2C 97.5(9) . . ? F1C C5C C1C 117.1(7) . . ? F3C C5C C1C 111.7(7) . . ? F2C C5C C1C 110.4(8) . . ? O3C C6C C7C 128.1(5) . . ? O3C C6C C10C 114.4(5) . . ? C7C C6C C10C 117.4(5) . . ? C6C C7C C8C 121.3(5) . . ? C6C C7C H7C 119.3 . . ? C8C C7C H7C 119.3 . . ? O4C C8C C7C 128.0(5) . . ? O4C C8C C9C 114.6(5) . . ? C7C C8C C9C 117.4(5) . . ? F2JA C9C F3JB 123.5(10) . . ? F2JA C9C F1JB 72.8(8) . . ? F3JB C9C F1JB 118.3(10) . . ? F2JA C9C F3JA 105.5(9) . . ? F3JB C9C F3JA 24.0(7) . . ? F1JB C9C F3JA 132.6(9) . . ? F2JA C9C F1JA 116.8(8) . . ? F3JB C9C F1JA 77.1(8) . . ? F1JB C9C F1JA 48.5(6) . . ? F3JA C9C F1JA 99.6(9) . . ? F2JA C9C F2IB 30.7(6) . . ? F3JB C9C F2IB 98.0(9) . . ? F1JB C9C F2IB 99.8(8) . . ? F3JA C9C F2IB 76.6(7) . . ? F1JA C9C F2IB 132.8(8) . . ? F2JA C9C C8C 110.3(8) . . ? F3JB C9C C8C 112.6(8) . . ? F1JB C9C C8C 113.8(8) . . ? F3JA C9C C8C 111.0(7) . . ? F1JA C9C C8C 112.9(7) . . ? F2IB C9C C8C 112.2(7) . . ? F7C C10C F9C 109.1(6) . . ? F7C C10C F8C 106.2(6) . . ? F9C C10C F8C 105.8(5) . . ? F7C C10C C6C 111.2(5) . . ? F9C C10C C6C 114.4(6) . . ? F8C C10C C6C 109.6(5) . . ? O5C C11C O6C 130.8(4) . . ? O5C C11C C12C 115.7(4) . . ? O6C C11C C12C 113.5(4) . . ? F14C C12C F13C 109.5(6) . . ? F14C C12C F15C 104.4(6) . . ? F13C C12C F15C 106.3(6) . . ? F14C C12C C11C 113.7(5) . . ? F13C C12C C11C 113.5(5) . . ? F15C C12C C11C 108.8(5) . . ? O8C C13C O7C 127.2(5) . . ? O8C C13C C14C 116.5(4) . . ? O7C C13C C14C 116.3(5) . . ? F18C C14C F17C 113.5(8) . . ? F18C C14C F16C 103.4(8) . . ? F17C C14C F16C 100.7(7) . . ? F18C C14C C13C 115.6(5) . . ? F17C C14C C13C 114.1(5) . . ? F16C C14C C13C 107.4(7) . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? N1S C2S C1S 177.9(9) . . ? C4S C3S H3SA 109.5 . . ? C4S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C4S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? N2S C4S C3S 178.6(12) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 66.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.541 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.119 ###==END===##