Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'V. A. Petrov' 'W. J. Marshall' 'V. V. Grushin' _publ_contact_author_name 'Dr Vladimir Grushin' _publ_contact_author_address ; Dupont Central Research & Development Experimental Station E328/306 Wilmington Delaware DE 19880-0328 USA ; _publ_contact_author_email 'VLAD.GRUSHIN-1@USA.DUPONTCOM' _publ_section_title ; The First Perfluoroacetylacetonate Metal Complexes: As Unexpectedly Robust as Tricky to Make ; data_00039 _database_code_CSD 171064 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H10 Cl2 Eu F13 N2 O6' _chemical_formula_weight 868.18 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' 'Cl' 'Cl' 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7765(10) _cell_length_b 12.1403(10) _cell_length_c 12.8391(10) _cell_angle_alpha 61.947(10) _cell_angle_beta 62.929(10) _cell_angle_gamma 64.341(10) _cell_volume 1385.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_size_max .48 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 2.587 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 16996 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6498 _reflns_number_gt 6095 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+4.0390P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6498 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.139 _refine_ls_shift/su_mean 0.004 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 0.669904(16) 0.420193(15) 0.363506(15) 0.02265(7) Uani 1 1 d . . . F1 F 1.0920(3) 0.6351(3) 0.0154(3) 0.0556(8) Uani 1 1 d . . . F2 F 1.0189(4) 0.6244(4) 0.2057(3) 0.0666(10) Uani 1 1 d . . . F3 F 0.9414(3) 0.7950(3) 0.0705(3) 0.0574(8) Uani 1 1 d . . . F4 F 0.8774(4) 0.7284(4) -0.0711(3) 0.0623(9) Uani 1 1 d . . . F5 F 0.6183(5) 0.7866(4) -0.0859(4) 0.0918(15) Uani 1 1 d . . . F6 F 0.7727(5) 0.6379(5) -0.1559(3) 0.0786(12) Uani 1 1 d . . . F7 F 0.5838(5) 0.6044(5) -0.0302(3) 0.0799(13) Uani 1 1 d . . . F8 F 0.4688(4) 0.9675(3) 0.2667(4) 0.0861(14) Uani 1 1 d . . . F9 F 0.6464(5) 0.8353(4) 0.2065(6) 0.141(3) Uani 1 1 d . . . F10 F 0.4799(9) 0.8627(7) 0.1673(5) 0.156(3) Uani 1 1 d . . . F11 F 0.8753(8) 0.4648(8) 0.5898(7) 0.0794(16) Uiso 0.602(5) 1 d P . . F12 F 0.7174(7) 0.5708(7) 0.6985(7) 0.0733(14) Uiso 0.602(5) 1 d P . . F13 F 0.7456(10) 0.3620(10) 0.7617(10) 0.115(2) Uiso 0.602(5) 1 d P . . F11' F 0.6938(12) 0.4995(12) 0.7615(11) 0.0794(16) Uiso 0.398(5) 1 d P . . F12' F 0.8646(11) 0.3888(11) 0.6421(10) 0.0733(14) Uiso 0.398(5) 1 d P . . F13' F 0.7991(16) 0.5831(16) 0.6010(15) 0.115(2) Uiso 0.398(5) 1 d P . . O1 O 0.8378(3) 0.5313(3) 0.2444(3) 0.0306(6) Uani 1 1 d . . . O2 O 0.6629(3) 0.5321(3) 0.1548(3) 0.0318(6) Uani 1 1 d . . . O5 O 0.5420(3) 0.6306(3) 0.3713(3) 0.0382(7) Uani 1 1 d . . . O6 O 0.3796(3) 0.7743(3) 0.4577(3) 0.0334(6) Uani 1 1 d . . . O7 O 0.7129(3) 0.4348(3) 0.5202(3) 0.0311(6) Uani 1 1 d . . . O8 O 0.5443(3) 0.5647(3) 0.6248(3) 0.0307(6) Uani 1 1 d . . . N11 N 0.8955(3) 0.2516(3) 0.3631(3) 0.0302(7) Uani 1 1 d . . . N21 N 0.7317(3) 0.2528(3) 0.2652(3) 0.0304(7) Uani 1 1 d . . . C1 C 0.9833(5) 0.6648(5) 0.1082(5) 0.0407(10) Uani 1 1 d . . . C2 C 0.8744(4) 0.6070(4) 0.1365(4) 0.0295(8) Uani 1 1 d . . . C3 C 0.8252(5) 0.6451(4) 0.0416(4) 0.0380(10) Uani 1 1 d . . . C4 C 0.7216(5) 0.6067(4) 0.0566(4) 0.0333(8) Uani 1 1 d . . . C5 C 0.6732(7) 0.6600(6) -0.0559(5) 0.0554(14) Uani 1 1 d . . . C6 C 0.4766(4) 0.7427(4) 0.3722(4) 0.0306(8) Uani 1 1 d . . . C7 C 0.5197(6) 0.8532(5) 0.2517(5) 0.0585(16) Uani 1 1 d . . . C8 C 0.6596(4) 0.4949(4) 0.5937(4) 0.0337(8) Uani 1 1 d . . . C9 C 0.7512(6) 0.4759(7) 0.6615(7) 0.0624(17) Uani 1 1 d . . . C12 C 0.9776(4) 0.2536(4) 0.4058(4) 0.0377(9) Uani 1 1 d . . . H12A H 0.9537 0.3214 0.4334 0.045 Uiso 1 1 calc R . . C13 C 1.0990(4) 0.1583(5) 0.4117(5) 0.0450(11) Uani 1 1 d . . . H13A H 1.1536 0.1634 0.4426 0.054 Uiso 1 1 calc R . . C14 C 1.1355(4) 0.0591(5) 0.3716(5) 0.0475(12) Uani 1 1 d . . . H14A H 1.2148 -0.0056 0.3766 0.057 Uiso 1 1 calc R . . C15 C 1.0535(4) 0.0540(4) 0.3225(4) 0.0422(11) Uani 1 1 d . . . C16 C 0.9323(4) 0.1532(4) 0.3203(4) 0.0323(8) Uani 1 1 d . . . C17 C 1.0858(5) -0.0460(5) 0.2747(5) 0.0546(14) Uani 1 1 d . . . H17A H 1.1640 -0.1129 0.2780 0.066 Uiso 1 1 calc R . . C18 C 1.0068(6) -0.0450(5) 0.2258(6) 0.0553(14) Uani 1 1 d . . . H18A H 1.0313 -0.1109 0.1956 0.066 Uiso 1 1 calc R . . C19 C 0.8844(5) 0.0560(4) 0.2189(5) 0.0452(11) Uani 1 1 d . . . C20 C 0.8467(4) 0.1538(4) 0.2682(4) 0.0330(8) Uani 1 1 d . . . C21 C 0.8011(6) 0.0649(6) 0.1627(6) 0.0553(14) Uani 1 1 d . . . H21A H 0.8229 0.0025 0.1292 0.066 Uiso 1 1 calc R . . C22 C 0.6879(6) 0.1657(6) 0.1575(6) 0.0516(13) Uani 1 1 d . . . H22A H 0.6323 0.1730 0.1199 0.062 Uiso 1 1 calc R . . C23 C 0.6569(5) 0.2584(5) 0.2099(5) 0.0395(10) Uani 1 1 d . . . H23A H 0.5800 0.3269 0.2056 0.047 Uiso 1 1 calc R . . Cl30 Cl 0.3015(14) 0.1839(14) 0.5712(8) 0.268(8) Uani 0.50 1 d P . . Cl31 Cl 0.4284(10) 0.0279(14) 0.4931(9) 0.204(5) Uani 0.50 1 d P . . C30 C 0.4056(11) 0.1411(12) 0.4724(14) 0.052(3) Uani 0.50 1 d P . . 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 0.02062(10) 0.01937(10) 0.02467(11) -0.00702(7) -0.00771(7) -0.00274(7) F1 0.0355(15) 0.0591(19) 0.0611(19) -0.0270(16) 0.0093(13) -0.0228(14) F2 0.062(2) 0.104(3) 0.0549(19) -0.0192(19) -0.0179(16) -0.050(2) F3 0.0549(18) 0.0465(17) 0.074(2) -0.0294(16) -0.0018(16) -0.0271(15) F4 0.087(3) 0.075(2) 0.0289(14) 0.0032(14) -0.0117(15) -0.057(2) F5 0.135(4) 0.061(2) 0.079(3) 0.007(2) -0.078(3) -0.014(2) F6 0.118(3) 0.109(3) 0.0287(15) -0.0154(17) -0.0177(18) -0.062(3) F7 0.101(3) 0.111(3) 0.0517(19) 0.005(2) -0.045(2) -0.063(3) F8 0.073(2) 0.0255(15) 0.092(3) -0.0060(16) 0.010(2) -0.0101(15) F9 0.064(3) 0.054(2) 0.166(5) -0.016(3) 0.054(3) -0.020(2) F10 0.277(10) 0.132(5) 0.061(3) 0.029(3) -0.080(5) -0.099(6) O1 0.0287(14) 0.0317(14) 0.0309(14) -0.0073(11) -0.0098(12) -0.0113(11) O2 0.0364(15) 0.0317(14) 0.0287(14) -0.0060(11) -0.0123(12) -0.0132(12) O5 0.0374(16) 0.0242(14) 0.0573(19) -0.0175(13) -0.0259(15) 0.0034(12) O6 0.0300(14) 0.0260(14) 0.0325(15) -0.0065(11) -0.0065(12) -0.0054(11) O7 0.0246(13) 0.0363(15) 0.0326(14) -0.0163(12) -0.0108(11) -0.0020(11) O8 0.0238(13) 0.0361(15) 0.0343(14) -0.0156(12) -0.0075(11) -0.0077(11) N11 0.0231(15) 0.0271(16) 0.0300(16) -0.0083(13) -0.0062(13) -0.0023(12) N21 0.0285(16) 0.0273(16) 0.0299(16) -0.0136(13) -0.0021(13) -0.0065(13) C1 0.036(2) 0.042(2) 0.044(2) -0.018(2) -0.0043(19) -0.0162(19) C2 0.0275(18) 0.0286(18) 0.0311(19) -0.0140(15) -0.0025(15) -0.0098(15) C3 0.051(3) 0.035(2) 0.0267(19) -0.0035(17) -0.0089(19) -0.022(2) C4 0.044(2) 0.0302(19) 0.0267(18) -0.0069(15) -0.0132(17) -0.0118(17) C5 0.082(4) 0.054(3) 0.036(2) 0.001(2) -0.029(3) -0.031(3) C6 0.0276(19) 0.0215(17) 0.035(2) -0.0056(15) -0.0107(16) -0.0037(14) C7 0.048(3) 0.032(2) 0.047(3) -0.004(2) 0.004(2) -0.003(2) C8 0.0271(19) 0.040(2) 0.035(2) -0.0162(17) -0.0096(16) -0.0070(16) C9 0.042(3) 0.087(5) 0.078(4) -0.057(4) -0.023(3) 0.002(3) C12 0.0266(19) 0.037(2) 0.039(2) -0.0099(18) -0.0105(17) -0.0040(17) C13 0.026(2) 0.049(3) 0.042(2) -0.005(2) -0.0123(19) -0.0053(19) C14 0.025(2) 0.036(2) 0.045(3) -0.004(2) -0.0050(19) 0.0043(17) C15 0.030(2) 0.028(2) 0.038(2) -0.0056(17) 0.0009(18) -0.0014(17) C16 0.0262(18) 0.0241(18) 0.0283(19) -0.0070(15) 0.0017(15) -0.0050(15) C17 0.043(3) 0.027(2) 0.061(3) -0.018(2) -0.001(2) 0.0057(19) C18 0.052(3) 0.033(2) 0.065(3) -0.029(2) -0.004(3) -0.001(2) C19 0.046(3) 0.029(2) 0.049(3) -0.019(2) 0.000(2) -0.0112(19) C20 0.0306(19) 0.0241(18) 0.032(2) -0.0114(15) 0.0012(16) -0.0072(15) C21 0.058(3) 0.051(3) 0.065(3) -0.039(3) -0.001(3) -0.020(3) C22 0.051(3) 0.056(3) 0.063(3) -0.036(3) -0.010(3) -0.019(2) C23 0.038(2) 0.037(2) 0.048(3) -0.022(2) -0.010(2) -0.0098(18) Cl30 0.360(15) 0.408(17) 0.129(6) 0.091(8) -0.123(8) -0.338(15) Cl31 0.156(8) 0.308(14) 0.140(7) -0.105(9) -0.033(6) -0.040(10) C30 0.036(5) 0.059(7) 0.074(8) -0.035(6) -0.011(5) -0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O5 2.361(3) . ? Eu1 O7 2.382(3) . ? Eu1 O1 2.385(3) . ? Eu1 O8 2.387(3) 2_666 ? Eu1 O2 2.391(3) . ? Eu1 O6 2.462(3) 2_666 ? Eu1 N11 2.557(3) . ? Eu1 N21 2.559(3) . ? Eu1 C6 3.117(4) 2_666 ? Eu1 O5 3.134(4) 2_666 ? Eu1 Eu1 4.3542(7) 2_666 ? F1 C1 1.343(5) . ? F2 C1 1.305(6) . ? F3 C1 1.340(6) . ? F4 C3 1.359(5) . ? F5 C5 1.318(7) . ? F6 C5 1.332(7) . ? F7 C5 1.328(7) . ? F8 C7 1.323(7) . ? F9 C7 1.288(8) . ? F10 C7 1.304(9) . ? F11 F12' 0.871(11) . ? F11 C9 1.312(10) . ? F11 F13' 1.360(17) . ? F12 F11' 0.908(11) . ? F12 F13' 1.169(16) . ? F12 C9 1.288(9) . ? F13 C9 1.378(12) . ? F13 F11' 1.509(15) . ? F13 F12' 1.547(15) . ? F11' C9 1.256(12) . ? F12' C9 1.298(12) . ? F13' C9 1.379(17) . ? O1 C2 1.245(5) . ? O2 C4 1.249(5) . ? O5 C6 1.242(5) . ? O5 Eu1 3.134(4) 2_666 ? O6 C6 1.238(5) . ? O6 Eu1 2.462(3) 2_666 ? O7 C8 1.237(5) . ? O8 C8 1.245(5) . ? O8 Eu1 2.387(3) 2_666 ? N11 C12 1.322(6) . ? N11 C16 1.368(5) . ? N21 C23 1.325(6) . ? N21 C20 1.369(5) . ? C1 C2 1.544(6) . ? C2 C3 1.384(6) . ? C3 C4 1.392(6) . ? C4 C5 1.543(6) . ? C6 C7 1.541(6) . ? C6 Eu1 3.117(4) 2_666 ? C8 C9 1.557(7) . ? C12 C13 1.404(6) . ? C13 C14 1.353(8) . ? C14 C15 1.407(8) . ? C15 C16 1.415(6) . ? C15 C17 1.443(7) . ? C16 C20 1.439(7) . ? C17 C18 1.331(9) . ? C18 C19 1.440(7) . ? C19 C21 1.404(8) . ? C19 C20 1.415(6) . ? C21 C22 1.368(8) . ? C22 C23 1.409(6) . ? Cl30 C30 1.426(19) . ? Cl30 Cl31 2.19(2) . ? Cl31 C30 1.198(17) . ? Cl31 Cl31 1.584(19) 2_656 ? Cl31 C30 2.165(18) 2_656 ? C30 Cl31 2.165(18) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Eu1 O7 75.53(10) . . ? O5 Eu1 O1 79.90(11) . . ? O7 Eu1 O1 77.63(10) . . ? O5 Eu1 O8 76.21(10) . 2_666 ? O7 Eu1 O8 124.04(10) . 2_666 ? O1 Eu1 O8 141.14(10) . 2_666 ? O5 Eu1 O2 79.52(11) . . ? O7 Eu1 O2 142.74(10) . . ? O1 Eu1 O2 71.04(10) . . ? O8 Eu1 O2 74.77(10) 2_666 . ? O5 Eu1 O6 120.88(11) . 2_666 ? O7 Eu1 O6 77.25(10) . 2_666 ? O1 Eu1 O6 141.37(10) . 2_666 ? O8 Eu1 O6 77.49(10) 2_666 2_666 ? O2 Eu1 O6 139.91(10) . 2_666 ? O5 Eu1 N11 144.82(11) . . ? O7 Eu1 N11 78.41(10) . . ? O1 Eu1 N11 71.69(10) . . ? O8 Eu1 N11 138.76(11) 2_666 . ? O2 Eu1 N11 109.25(11) . . ? O6 Eu1 N11 74.84(10) 2_666 . ? O5 Eu1 N21 145.79(11) . . ? O7 Eu1 N21 138.61(11) . . ? O1 Eu1 N21 105.87(10) . . ? O8 Eu1 N21 79.38(10) 2_666 . ? O2 Eu1 N21 71.14(11) . . ? O6 Eu1 N21 75.76(10) 2_666 . ? N11 Eu1 N21 64.60(11) . . ? O5 Eu1 C6 99.01(11) . 2_666 ? O7 Eu1 C6 69.08(11) . 2_666 ? O1 Eu1 C6 145.71(10) . 2_666 ? O8 Eu1 C6 69.03(10) 2_666 2_666 ? O2 Eu1 C6 142.92(10) . 2_666 ? O6 Eu1 C6 21.87(10) 2_666 2_666 ? N11 Eu1 C6 93.27(10) . 2_666 ? N21 Eu1 C6 94.16(11) . 2_666 ? O5 Eu1 O5 76.09(11) . 2_666 ? O7 Eu1 O5 63.34(9) . 2_666 ? O1 Eu1 O5 138.01(9) . 2_666 ? O8 Eu1 O5 63.48(9) 2_666 2_666 ? O2 Eu1 O5 135.39(9) . 2_666 ? O6 Eu1 O5 44.79(9) 2_666 2_666 ? N11 Eu1 O5 112.26(9) . 2_666 ? N21 Eu1 O5 113.40(9) . 2_666 ? C6 Eu1 O5 22.93(9) 2_666 2_666 ? O5 Eu1 Eu1 44.32(9) . 2_666 ? O7 Eu1 Eu1 62.71(7) . 2_666 ? O1 Eu1 Eu1 116.10(7) . 2_666 ? O8 Eu1 Eu1 63.21(7) 2_666 2_666 ? O2 Eu1 Eu1 114.44(8) . 2_666 ? O6 Eu1 Eu1 76.55(7) 2_666 2_666 ? N11 Eu1 Eu1 135.72(8) . 2_666 ? N21 Eu1 Eu1 137.25(8) . 2_666 ? C6 Eu1 Eu1 54.69(7) 2_666 2_666 ? O5 Eu1 Eu1 31.76(5) 2_666 2_666 ? F12' F11 C9 69.6(10) . . ? F12' F11 F13' 127.8(13) . . ? C9 F11 F13' 62.1(8) . . ? F11' F12 F13' 131.9(14) . . ? F11' F12 C9 67.2(9) . . ? F13' F12 C9 68.1(9) . . ? C9 F13 F11' 51.3(6) . . ? C9 F13 F12' 52.3(6) . . ? F11' F13 F12' 94.0(9) . . ? F12 F11' C9 71.0(10) . . ? F12 F11' F13 127.7(13) . . ? C9 F11' F13 59.0(7) . . ? F11 F12' C9 71.4(10) . . ? F11 F12' F13 126.4(13) . . ? C9 F12' F13 57.2(7) . . ? F12 F13' F11 110.2(13) . . ? F12 F13' C9 60.0(9) . . ? F11 F13' C9 57.2(8) . . ? C2 O1 Eu1 136.7(3) . . ? C4 O2 Eu1 136.9(3) . . ? C6 O5 Eu1 178.3(3) . . ? C6 O5 Eu1 77.8(3) . 2_666 ? Eu1 O5 Eu1 103.91(11) . 2_666 ? C6 O6 Eu1 110.4(2) . 2_666 ? C8 O7 Eu1 139.3(3) . . ? C8 O8 Eu1 136.3(3) . 2_666 ? C12 N11 C16 118.2(4) . . ? C12 N11 Eu1 122.6(3) . . ? C16 N11 Eu1 119.2(3) . . ? C23 N21 C20 118.1(4) . . ? C23 N21 Eu1 122.5(3) . . ? C20 N21 Eu1 119.4(3) . . ? F2 C1 F3 107.6(4) . . ? F2 C1 F1 108.3(4) . . ? F3 C1 F1 105.8(4) . . ? F2 C1 C2 111.9(4) . . ? F3 C1 C2 111.2(4) . . ? F1 C1 C2 111.8(4) . . ? O1 C2 C3 126.2(4) . . ? O1 C2 C1 116.2(4) . . ? C3 C2 C1 117.7(4) . . ? F4 C3 C2 118.2(4) . . ? F4 C3 C4 118.2(4) . . ? C2 C3 C4 123.5(4) . . ? O2 C4 C3 125.4(4) . . ? O2 C4 C5 116.4(4) . . ? C3 C4 C5 118.2(4) . . ? F5 C5 F7 108.2(6) . . ? F5 C5 F6 107.5(5) . . ? F7 C5 F6 107.7(5) . . ? F5 C5 C4 110.8(5) . . ? F7 C5 C4 110.7(4) . . ? F6 C5 C4 111.8(5) . . ? O6 C6 O5 127.1(4) . . ? O6 C6 C7 117.2(4) . . ? O5 C6 C7 115.7(4) . . ? O6 C6 Eu1 47.77(19) . 2_666 ? O5 C6 Eu1 79.3(2) . 2_666 ? C7 C6 Eu1 164.9(3) . 2_666 ? F9 C7 F10 107.6(7) . . ? F9 C7 F8 105.8(6) . . ? F10 C7 F8 107.6(6) . . ? F9 C7 C6 113.5(5) . . ? F10 C7 C6 109.2(6) . . ? F8 C7 C6 112.9(5) . . ? O7 C8 O8 130.7(4) . . ? O7 C8 C9 114.2(4) . . ? O8 C8 C9 115.1(4) . . ? F11' C9 F12 41.8(6) . . ? F11' C9 F12' 122.1(9) . . ? F12 C9 F12' 129.3(8) . . ? F11' C9 F11 129.8(8) . . ? F12 C9 F11 106.1(7) . . ? F12' C9 F11 39.0(5) . . ? F11' C9 F13 69.7(8) . . ? F12 C9 F13 110.1(7) . . ? F12' C9 F13 70.6(7) . . ? F11 C9 F13 108.2(7) . . ? F11' C9 F13' 92.1(9) . . ? F12 C9 F13' 51.9(7) . . ? F12' C9 F13' 97.7(9) . . ? F11 C9 F13' 60.7(8) . . ? F13 C9 F13' 145.4(9) . . ? F11' C9 C8 116.2(7) . . ? F12 C9 C8 113.2(6) . . ? F12' C9 C8 114.6(6) . . ? F11 C9 C8 112.2(6) . . ? F13 C9 C8 107.0(7) . . ? F13' C9 C8 107.4(9) . . ? N11 C12 C13 123.3(5) . . ? C14 C13 C12 119.1(5) . . ? C13 C14 C15 120.0(4) . . ? C14 C15 C16 117.5(5) . . ? C14 C15 C17 123.9(4) . . ? C16 C15 C17 118.6(5) . . ? N11 C16 C15 121.9(4) . . ? N11 C16 C20 118.5(4) . . ? C15 C16 C20 119.5(4) . . ? C18 C17 C15 121.8(5) . . ? C17 C18 C19 121.4(5) . . ? C21 C19 C20 117.7(5) . . ? C21 C19 C18 123.5(5) . . ? C20 C19 C18 118.8(5) . . ? N21 C20 C19 122.1(4) . . ? N21 C20 C16 117.9(4) . . ? C19 C20 C16 119.9(4) . . ? C22 C21 C19 119.9(5) . . ? C21 C22 C23 118.8(5) . . ? N21 C23 C22 123.3(5) . . ? C30 Cl30 Cl31 30.2(7) . . ? C30 Cl31 Cl31 101.3(16) . 2_656 ? C30 Cl31 C30 134.2(10) . 2_656 ? Cl31 Cl31 C30 32.8(8) 2_656 2_656 ? C30 Cl31 Cl30 36.8(7) . . ? Cl31 Cl31 Cl30 112.2(11) 2_656 . ? C30 Cl31 Cl30 136.0(6) 2_656 . ? Cl31 C30 Cl30 112.9(12) . . ? Cl31 C30 Cl31 45.8(10) . 2_656 ? Cl30 C30 Cl31 121.3(10) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F13' F12 F11' C9 -23.2(17) . . . . ? F13' F12 F11' F13 -6(3) . . . . ? C9 F12 F11' F13 17.1(12) . . . . ? C9 F13 F11' F12 -18.9(13) . . . . ? F12' F13 F11' F12 13.9(17) . . . . ? F12' F13 F11' C9 32.8(7) . . . . ? F13' F11 F12' C9 22.9(15) . . . . ? C9 F11 F12' F13 -16.4(11) . . . . ? F13' F11 F12' F13 7(2) . . . . ? C9 F13 F12' F11 18.6(13) . . . . ? F11' F13 F12' F11 -13.7(17) . . . . ? F11' F13 F12' C9 -32.3(7) . . . . ? F11' F12 F13' F11 -6(2) . . . . ? C9 F12 F13' F11 -28.6(10) . . . . ? F11' F12 F13' C9 23.0(17) . . . . ? F12' F11 F13' F12 5(2) . . . . ? C9 F11 F13' F12 29.6(10) . . . . ? F12' F11 F13' C9 -24.4(16) . . . . ? O5 Eu1 O1 C2 -78.1(4) . . . . ? O7 Eu1 O1 C2 -155.3(4) . . . . ? O8 Eu1 O1 C2 -25.4(5) 2_666 . . . ? O2 Eu1 O1 C2 4.2(4) . . . . ? O6 Eu1 O1 C2 154.2(3) 2_666 . . . ? N11 Eu1 O1 C2 123.0(4) . . . . ? N21 Eu1 O1 C2 67.3(4) . . . . ? C6 Eu1 O1 C2 -169.3(3) 2_666 . . . ? O5 Eu1 O1 C2 -133.8(4) 2_666 . . . ? Eu1 Eu1 O1 C2 -104.4(4) 2_666 . . . ? O5 Eu1 O2 C4 79.8(4) . . . . ? O7 Eu1 O2 C4 31.3(5) . . . . ? O1 Eu1 O2 C4 -3.0(4) . . . . ? O8 Eu1 O2 C4 158.2(4) 2_666 . . . ? O6 Eu1 O2 C4 -154.0(4) 2_666 . . . ? N11 Eu1 O2 C4 -64.9(4) . . . . ? N21 Eu1 O2 C4 -118.1(4) . . . . ? C6 Eu1 O2 C4 170.9(4) 2_666 . . . ? O5 Eu1 O2 C4 137.4(4) 2_666 . . . ? Eu1 Eu1 O2 C4 107.7(4) 2_666 . . . ? O7 Eu1 O5 C6 118(10) . . . . ? O1 Eu1 O5 C6 38(10) . . . . ? O8 Eu1 O5 C6 -111(10) 2_666 . . . ? O2 Eu1 O5 C6 -34(10) . . . . ? O6 Eu1 O5 C6 -177(100) 2_666 . . . ? N11 Eu1 O5 C6 75(10) . . . . ? N21 Eu1 O5 C6 -65(10) . . . . ? C6 Eu1 O5 C6 -176(100) 2_666 . . . ? O5 Eu1 O5 C6 -176(100) 2_666 . . . ? Eu1 Eu1 O5 C6 -176(100) 2_666 . . . ? O7 Eu1 O5 Eu1 -65.57(10) . . . 2_666 ? O1 Eu1 O5 Eu1 -145.28(11) . . . 2_666 ? O8 Eu1 O5 Eu1 65.62(10) 2_666 . . 2_666 ? O2 Eu1 O5 Eu1 142.34(11) . . . 2_666 ? O6 Eu1 O5 Eu1 -0.39(15) 2_666 . . 2_666 ? N11 Eu1 O5 Eu1 -109.02(18) . . . 2_666 ? N21 Eu1 O5 Eu1 111.30(18) . . . 2_666 ? C6 Eu1 O5 Eu1 -0.04(12) 2_666 . . 2_666 ? O5 Eu1 O5 Eu1 -0.001(2) 2_666 . . 2_666 ? O5 Eu1 O7 C8 24.8(4) . . . . ? O1 Eu1 O7 C8 107.4(5) . . . . ? O8 Eu1 O7 C8 -37.1(5) 2_666 . . . ? O2 Eu1 O7 C8 74.3(5) . . . . ? O6 Eu1 O7 C8 -102.2(4) 2_666 . . . ? N11 Eu1 O7 C8 -179.1(5) . . . . ? N21 Eu1 O7 C8 -152.6(4) . . . . ? C6 Eu1 O7 C8 -81.0(4) 2_666 . . . ? O5 Eu1 O7 C8 -56.7(4) 2_666 . . . ? Eu1 Eu1 O7 C8 -20.9(4) 2_666 . . . ? O5 Eu1 N11 C12 21.0(4) . . . . ? O7 Eu1 N11 C12 -21.9(3) . . . . ? O1 Eu1 N11 C12 58.8(3) . . . . ? O8 Eu1 N11 C12 -151.1(3) 2_666 . . . ? O2 Eu1 N11 C12 120.2(3) . . . . ? O6 Eu1 N11 C12 -101.6(3) 2_666 . . . ? N21 Eu1 N11 C12 177.2(4) . . . . ? C6 Eu1 N11 C12 -89.7(3) 2_666 . . . ? O5 Eu1 N11 C12 -76.5(3) 2_666 . . . ? Eu1 Eu1 N11 C12 -50.1(4) 2_666 . . . ? O5 Eu1 N11 C16 -160.8(3) . . . . ? O7 Eu1 N11 C16 156.4(3) . . . . ? O1 Eu1 N11 C16 -122.9(3) . . . . ? O8 Eu1 N11 C16 27.1(3) 2_666 . . . ? O2 Eu1 N11 C16 -61.5(3) . . . . ? O6 Eu1 N11 C16 76.6(3) 2_666 . . . ? N21 Eu1 N11 C16 -4.5(3) . . . . ? C6 Eu1 N11 C16 88.5(3) 2_666 . . . ? O5 Eu1 N11 C16 101.8(3) 2_666 . . . ? Eu1 Eu1 N11 C16 128.1(2) 2_666 . . . ? O5 Eu1 N21 C23 -19.6(4) . . . . ? O7 Eu1 N21 C23 155.9(3) . . . . ? O1 Eu1 N21 C23 -115.0(3) . . . . ? O8 Eu1 N21 C23 25.4(3) 2_666 . . . ? O2 Eu1 N21 C23 -52.0(3) . . . . ? O6 Eu1 N21 C23 105.1(3) 2_666 . . . ? N11 Eu1 N21 C23 -175.2(4) . . . . ? C6 Eu1 N21 C23 93.2(3) 2_666 . . . ? O5 Eu1 N21 C23 80.2(3) 2_666 . . . ? Eu1 Eu1 N21 C23 54.0(4) 2_666 . . . ? O5 Eu1 N21 C20 159.9(3) . . . . ? O7 Eu1 N21 C20 -24.7(4) . . . . ? O1 Eu1 N21 C20 64.5(3) . . . . ? O8 Eu1 N21 C20 -155.1(3) 2_666 . . . ? O2 Eu1 N21 C20 127.5(3) . . . . ? O6 Eu1 N21 C20 -75.5(3) 2_666 . . . ? N11 Eu1 N21 C20 4.3(3) . . . . ? C6 Eu1 N21 C20 -87.4(3) 2_666 . . . ? O5 Eu1 N21 C20 -100.3(3) 2_666 . . . ? Eu1 Eu1 N21 C20 -126.6(3) 2_666 . . . ? Eu1 O1 C2 C3 -5.3(7) . . . . ? Eu1 O1 C2 C1 173.6(3) . . . . ? F2 C1 C2 O1 -0.7(6) . . . . ? F3 C1 C2 O1 -121.0(4) . . . . ? F1 C1 C2 O1 121.0(4) . . . . ? F2 C1 C2 C3 178.3(4) . . . . ? F3 C1 C2 C3 58.0(5) . . . . ? F1 C1 C2 C3 -60.1(6) . . . . ? O1 C2 C3 F4 -179.7(4) . . . . ? C1 C2 C3 F4 1.4(6) . . . . ? O1 C2 C3 C4 2.9(7) . . . . ? C1 C2 C3 C4 -176.0(4) . . . . ? Eu1 O2 C4 C3 2.9(7) . . . . ? Eu1 O2 C4 C5 -176.8(3) . . . . ? F4 C3 C4 O2 -179.1(4) . . . . ? C2 C3 C4 O2 -1.8(8) . . . . ? F4 C3 C4 C5 0.6(7) . . . . ? C2 C3 C4 C5 178.0(5) . . . . ? O2 C4 C5 F5 113.6(5) . . . . ? C3 C4 C5 F5 -66.2(7) . . . . ? O2 C4 C5 F7 -6.5(7) . . . . ? C3 C4 C5 F7 173.7(5) . . . . ? O2 C4 C5 F6 -126.6(5) . . . . ? C3 C4 C5 F6 53.7(6) . . . . ? Eu1 O6 C6 O5 0.9(6) 2_666 . . . ? Eu1 O6 C6 C7 178.9(4) 2_666 . . . ? Eu1 O5 C6 O6 176(100) . . . . ? Eu1 O5 C6 O6 -0.6(4) 2_666 . . . ? Eu1 O5 C6 C7 -2(11) . . . . ? Eu1 O5 C6 C7 -178.7(4) 2_666 . . . ? Eu1 O5 C6 Eu1 176(100) . . . 2_666 ? O6 C6 C7 F9 136.8(6) . . . . ? O5 C6 C7 F9 -44.9(8) . . . . ? Eu1 C6 C7 F9 140.0(11) 2_666 . . . ? O6 C6 C7 F10 -103.2(6) . . . . ? O5 C6 C7 F10 75.1(7) . . . . ? Eu1 C6 C7 F10 -100.0(15) 2_666 . . . ? O6 C6 C7 F8 16.4(8) . . . . ? O5 C6 C7 F8 -165.3(5) . . . . ? Eu1 C6 C7 F8 19.6(18) 2_666 . . . ? Eu1 O7 C8 O8 11.6(8) . . . . ? Eu1 O7 C8 C9 -170.7(4) . . . . ? Eu1 O8 C8 O7 27.2(8) 2_666 . . . ? Eu1 O8 C8 C9 -150.5(4) 2_666 . . . ? F13 F11' C9 F12 -164.3(11) . . . . ? F12 F11' C9 F12' 114.8(12) . . . . ? F13 F11' C9 F12' -49.4(11) . . . . ? F12 F11' C9 F11 67.0(14) . . . . ? F13 F11' C9 F11 -97.2(11) . . . . ? F12 F11' C9 F13 164.3(11) . . . . ? F12 F11' C9 F13' 14.4(11) . . . . ? F13 F11' C9 F13' -149.9(9) . . . . ? F12 F11' C9 C8 -96.3(10) . . . . ? F13 F11' C9 C8 99.5(8) . . . . ? F13' F12 C9 F11' 161.6(14) . . . . ? F11' F12 C9 F12' -96.6(14) . . . . ? F13' F12 C9 F12' 65.0(14) . . . . ? F11' F12 C9 F11 -132.6(11) . . . . ? F13' F12 C9 F11 29.0(11) . . . . ? F11' F12 C9 F13 -15.7(11) . . . . ? F13' F12 C9 F13 145.9(11) . . . . ? F11' F12 C9 F13' -161.6(14) . . . . ? F11' F12 C9 C8 104.0(10) . . . . ? F13' F12 C9 C8 -94.4(11) . . . . ? F11 F12' C9 F11' -115.2(12) . . . . ? F13 F12' C9 F11' 49.1(11) . . . . ? F11 F12' C9 F12 -63.9(14) . . . . ? F13 F12' C9 F12 100.5(11) . . . . ? F13 F12' C9 F11 164.3(11) . . . . ? F11 F12' C9 F13 -164.3(11) . . . . ? F11 F12' C9 F13' -17.8(12) . . . . ? F13 F12' C9 F13' 146.5(9) . . . . ? F11 F12' C9 C8 95.4(10) . . . . ? F13 F12' C9 C8 -100.3(8) . . . . ? F12' F11 C9 F11' 94.0(14) . . . . ? F13' F11 C9 F11' -65.7(13) . . . . ? F12' F11 C9 F12 133.7(11) . . . . ? F13' F11 C9 F12 -26.0(9) . . . . ? F13' F11 C9 F12' -159.6(13) . . . . ? F12' F11 C9 F13 15.6(11) . . . . ? F13' F11 C9 F13 -144.1(10) . . . . ? F12' F11 C9 F13' 159.6(13) . . . . ? F12' F11 C9 C8 -102.2(10) . . . . ? F13' F11 C9 C8 98.2(10) . . . . ? F12' F13 C9 F11' -136.9(9) . . . . ? F11' F13 C9 F12 11.1(8) . . . . ? F12' F13 C9 F12 -125.8(8) . . . . ? F11' F13 C9 F12' 136.9(9) . . . . ? F11' F13 C9 F11 126.6(8) . . . . ? F12' F13 C9 F11 -10.3(7) . . . . ? F11' F13 C9 F13' 62.2(17) . . . . ? F12' F13 C9 F13' -74.8(17) . . . . ? F11' F13 C9 C8 -112.3(7) . . . . ? F12' F13 C9 C8 110.7(7) . . . . ? F12 F13' C9 F11' -12.2(9) . . . . ? F11 F13' C9 F11' 135.5(9) . . . . ? F11 F13' C9 F12 147.7(11) . . . . ? F12 F13' C9 F12' -134.9(9) . . . . ? F11 F13' C9 F12' 12.8(8) . . . . ? F12 F13' C9 F11 -147.7(11) . . . . ? F12 F13' C9 F13 -68.3(18) . . . . ? F11 F13' C9 F13 79.4(16) . . . . ? F12 F13' C9 C8 106.2(8) . . . . ? F11 F13' C9 C8 -106.1(7) . . . . ? O7 C8 C9 F11' -158.7(8) . . . . ? O8 C8 C9 F11' 19.4(10) . . . . ? O7 C8 C9 F12 155.1(6) . . . . ? O8 C8 C9 F12 -26.7(8) . . . . ? O7 C8 C9 F12' -7.5(10) . . . . ? O8 C8 C9 F12' 170.7(8) . . . . ? O7 C8 C9 F11 35.1(8) . . . . ? O8 C8 C9 F11 -146.8(6) . . . . ? O7 C8 C9 F13 -83.4(7) . . . . ? O8 C8 C9 F13 94.7(7) . . . . ? O7 C8 C9 F13' 99.8(9) . . . . ? O8 C8 C9 F13' -82.0(9) . . . . ? C16 N11 C12 C13 -1.4(6) . . . . ? Eu1 N11 C12 C13 176.9(3) . . . . ? N11 C12 C13 C14 0.2(7) . . . . ? C12 C13 C14 C15 1.4(7) . . . . ? C13 C14 C15 C16 -1.7(7) . . . . ? C13 C14 C15 C17 178.3(5) . . . . ? C12 N11 C16 C15 1.0(6) . . . . ? Eu1 N11 C16 C15 -177.4(3) . . . . ? C12 N11 C16 C20 -177.1(4) . . . . ? Eu1 N11 C16 C20 4.6(5) . . . . ? C14 C15 C16 N11 0.5(6) . . . . ? C17 C15 C16 N11 -179.5(4) . . . . ? C14 C15 C16 C20 178.5(4) . . . . ? C17 C15 C16 C20 -1.5(6) . . . . ? C14 C15 C17 C18 -178.1(5) . . . . ? C16 C15 C17 C18 1.9(8) . . . . ? C15 C17 C18 C19 -0.3(9) . . . . ? C17 C18 C19 C21 176.7(6) . . . . ? C17 C18 C19 C20 -1.6(8) . . . . ? C23 N21 C20 C19 -2.5(6) . . . . ? Eu1 N21 C20 C19 178.0(3) . . . . ? C23 N21 C20 C16 175.7(4) . . . . ? Eu1 N21 C20 C16 -3.8(5) . . . . ? C21 C19 C20 N21 1.7(7) . . . . ? C18 C19 C20 N21 -179.9(4) . . . . ? C21 C19 C20 C16 -176.4(4) . . . . ? C18 C19 C20 C16 2.0(7) . . . . ? N11 C16 C20 N21 -0.5(5) . . . . ? C15 C16 C20 N21 -178.6(4) . . . . ? N11 C16 C20 C19 177.7(4) . . . . ? C15 C16 C20 C19 -0.4(6) . . . . ? C20 C19 C21 C22 -0.1(8) . . . . ? C18 C19 C21 C22 -178.5(6) . . . . ? C19 C21 C22 C23 -0.5(9) . . . . ? C20 N21 C23 C22 1.8(7) . . . . ? Eu1 N21 C23 C22 -178.7(4) . . . . ? C21 C22 C23 N21 -0.4(8) . . . . ? C30 Cl30 Cl31 Cl31 79.0(17) . . . 2_656 ? C30 Cl30 Cl31 C30 106.9(17) . . . 2_656 ? Cl31 Cl31 C30 Cl30 -112.1(11) 2_656 . . . ? C30 Cl31 C30 Cl30 -112.1(11) 2_656 . . . ? C30 Cl31 C30 Cl31 0.000(2) 2_656 . . 2_656 ? Cl30 Cl31 C30 Cl31 112.1(11) . . . 2_656 ? Cl31 Cl30 C30 Cl31 -51.1(13) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.752 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.137 data_00045 _database_code_CSD 171065 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H30 Eu F21 O8 P2' _chemical_formula_weight 1383.65 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 17.1873(10) _cell_length_b 15.7823(10) _cell_length_c 20.5220(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 92.472(10) _cell_angle_gamma 90.000(10) _cell_volume 5561.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'ireg block' _exptl_crystal_colour 'light gold' _exptl_crystal_size_max .36 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .40 _exptl_crystal_density_meas multirun _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114173 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 33.15 _reflns_number_total 20416 _reflns_number_gt 14330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20416 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.004 _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 0.261858(6) 0.262429(6) 0.490999(5) 0.02665(4) Uani 1 1 d . . . P3 P 0.31799(3) 0.06251(3) 0.41267(3) 0.02877(11) Uani 1 1 d . . . P6 P 0.13686(3) 0.37422(4) 0.60454(3) 0.03213(12) Uani 1 1 d . . . F1 F 0.46136(12) 0.24974(10) 0.32684(10) 0.0620(5) Uani 1 1 d . . . F2 F 0.4440(2) 0.37138(15) 0.28973(11) 0.1254(11) Uani 1 1 d . . . F3 F 0.53308(14) 0.3484(2) 0.36264(15) 0.1384(14) Uani 1 1 d . . . F4 F 0.44124(13) 0.49144(11) 0.39153(10) 0.0785(6) Uani 1 1 d . . . F5 F 0.32103(18) 0.59760(11) 0.44367(11) 0.1064(9) Uani 1 1 d . . . F6 F 0.42284(14) 0.57717(14) 0.50407(12) 0.0996(8) Uani 1 1 d . . . F7 F 0.31067(13) 0.56169(10) 0.54285(9) 0.0746(6) Uani 1 1 d . . . F11 F 0.16488(18) 0.44766(17) 0.32063(15) 0.1332(12) Uani 1 1 d . . . F12 F 0.13453(19) 0.35586(19) 0.25308(10) 0.1235(11) Uani 1 1 d . . . F13 F 0.04954(14) 0.41083(17) 0.30865(14) 0.1199(11) Uani 1 1 d . . . F14 F 0.02085(12) 0.24402(12) 0.32744(11) 0.0664(6) Uani 1 1 d . . . F15 F 0.02073(14) 0.07666(15) 0.35756(13) 0.1060(8) Uani 1 1 d . . . F16 F -0.03450(11) 0.13791(13) 0.43394(14) 0.0998(8) Uani 1 1 d . . . F17 F 0.05647(13) 0.04897(13) 0.45346(14) 0.1058(9) Uani 1 1 d . . . F21 F 0.51487(13) 0.2941(2) 0.59857(13) 0.1136(10) Uani 1 1 d . . . F22 F 0.48522(13) 0.27919(19) 0.69732(12) 0.1003(8) Uani 1 1 d . . . F23 F 0.51995(11) 0.17487(16) 0.64238(15) 0.1068(9) Uani 1 1 d . . . F24 F 0.38195(10) 0.14456(11) 0.71040(8) 0.0611(5) Uani 1 1 d . . . F25 F 0.22655(14) 0.11716(13) 0.74063(9) 0.0849(7) Uani 1 1 d . . . F26 F 0.26849(16) 0.01790(12) 0.68514(13) 0.1116(10) Uani 1 1 d . . . F27 F 0.16062(14) 0.07520(18) 0.65893(12) 0.1187(11) Uani 1 1 d . . . O1 O 0.36452(9) 0.28633(10) 0.41545(8) 0.0347(3) Uani 1 1 d . . . O2 O 0.30518(10) 0.40864(9) 0.49959(8) 0.0363(3) Uani 1 1 d . . . O3 O 0.30282(9) 0.12881(9) 0.46289(8) 0.0351(3) Uani 1 1 d . . . O6 O 0.16708(10) 0.33287(10) 0.54482(8) 0.0388(4) Uani 1 1 d . . . O11 O 0.19857(10) 0.32408(10) 0.39778(8) 0.0390(4) Uani 1 1 d . . . O12 O 0.14675(9) 0.17903(10) 0.45851(8) 0.0387(4) Uani 1 1 d . . . O21 O 0.37277(10) 0.26214(9) 0.56363(8) 0.0345(3) Uani 1 1 d . . . O22 O 0.23549(10) 0.17694(10) 0.58664(8) 0.0389(4) Uani 1 1 d . . . C1 C 0.46127(18) 0.32935(19) 0.34345(15) 0.0541(7) Uani 1 1 d . . . C2 C 0.40272(14) 0.34841(16) 0.39665(11) 0.0375(5) Uani 1 1 d . . . C3 C 0.39724(17) 0.43033(16) 0.41985(13) 0.0458(6) Uani 1 1 d . . . C4 C 0.34994(15) 0.45524(14) 0.46973(12) 0.0374(5) Uani 1 1 d . . . C5 C 0.3519(2) 0.54871(17) 0.49017(16) 0.0596(8) Uani 1 1 d . . . C11 C 0.12007(18) 0.3829(2) 0.31199(15) 0.0563(7) Uani 1 1 d . . . C12 C 0.13628(15) 0.31412(16) 0.36396(11) 0.0404(5) Uani 1 1 d . . . C13 C 0.08439(16) 0.24811(17) 0.36974(14) 0.0431(6) Uani 1 1 d . . . C14 C 0.09393(13) 0.18330(15) 0.41580(12) 0.0381(5) Uani 1 1 d . . . C15 C 0.03340(16) 0.11039(18) 0.41575(17) 0.0554(7) Uani 1 1 d . . . C21 C 0.47940(19) 0.2463(2) 0.63922(17) 0.0535(8) Uani 1 1 d . . . C22 C 0.39446(15) 0.22811(14) 0.61570(12) 0.0360(5) Uani 1 1 d . . . C23 C 0.34928(15) 0.17541(15) 0.65345(11) 0.0403(5) Uani 1 1 d . . . C24 C 0.27339(15) 0.15250(14) 0.63621(11) 0.0387(5) Uani 1 1 d . . . C25 C 0.23080(19) 0.09025(18) 0.68063(14) 0.0533(7) Uani 1 1 d . . . C31 C 0.41923(13) 0.06233(13) 0.39558(11) 0.0311(4) Uani 1 1 d . . . C32 C 0.47076(15) 0.09434(17) 0.44366(13) 0.0457(6) Uani 1 1 d . . . H32A H 0.4522 0.1144 0.4827 0.055 Uiso 1 1 calc R . . C33 C 0.55022(16) 0.0961(2) 0.43305(15) 0.0565(7) Uani 1 1 d . . . H33A H 0.5850 0.1176 0.4649 0.068 Uiso 1 1 calc R . . C34 C 0.57696(16) 0.06609(19) 0.37543(16) 0.0564(7) Uani 1 1 d . . . H34A H 0.6300 0.0674 0.3684 0.068 Uiso 1 1 calc R . . C35 C 0.52658(16) 0.03413(18) 0.32806(15) 0.0517(7) Uani 1 1 d . . . H35A H 0.5456 0.0134 0.2894 0.062 Uiso 1 1 calc R . . C36 C 0.44697(14) 0.03267(15) 0.33777(13) 0.0408(5) Uani 1 1 d . . . H36A H 0.4126 0.0118 0.3054 0.049 Uiso 1 1 calc R . . C41 C 0.26304(13) 0.08060(15) 0.33764(11) 0.0350(5) Uani 1 1 d . . . C42 C 0.27417(15) 0.15585(17) 0.30431(12) 0.0417(5) Uani 1 1 d . . . H42A H 0.3118 0.1940 0.3198 0.050 Uiso 1 1 calc R . . C43 C 0.22997(17) 0.1747(2) 0.24841(13) 0.0521(7) Uani 1 1 d . . . H43A H 0.2382 0.2251 0.2263 0.063 Uiso 1 1 calc R . . C44 C 0.17401(18) 0.1192(2) 0.22553(15) 0.0611(8) Uani 1 1 d . . . H44A H 0.1441 0.1323 0.1881 0.073 Uiso 1 1 calc R . . C45 C 0.1619(2) 0.0448(2) 0.25736(18) 0.0772(11) Uani 1 1 d . . . H45A H 0.1240 0.0073 0.2412 0.093 Uiso 1 1 calc R . . C46 C 0.20578(18) 0.0247(2) 0.31391(16) 0.0592(8) Uani 1 1 d . . . H46A H 0.1969 -0.0258 0.3357 0.071 Uiso 1 1 calc R . . C51 C 0.29155(12) -0.04018(14) 0.44235(11) 0.0321(4) Uani 1 1 d . . . C52 C 0.31747(14) -0.11420(14) 0.41407(13) 0.0399(5) Uani 1 1 d . . . H52A H 0.3490 -0.1114 0.3784 0.048 Uiso 1 1 calc R . . C53 C 0.29662(16) -0.19200(16) 0.43866(15) 0.0487(6) Uani 1 1 d . . . H53A H 0.3134 -0.2415 0.4190 0.058 Uiso 1 1 calc R . . C54 C 0.25100(16) -0.19669(19) 0.49220(15) 0.0545(7) Uani 1 1 d . . . H54A H 0.2382 -0.2492 0.5093 0.065 Uiso 1 1 calc R . . C55 C 0.22420(16) -0.12302(19) 0.52051(16) 0.0539(7) Uani 1 1 d . . . H55A H 0.1926 -0.1263 0.5561 0.065 Uiso 1 1 calc R . . C56 C 0.24443(14) -0.04417(18) 0.49599(13) 0.0431(6) Uani 1 1 d . . . H56A H 0.2268 0.0052 0.5151 0.052 Uiso 1 1 calc R . . C61 C 0.04554(14) 0.32690(16) 0.62331(11) 0.0361(5) Uani 1 1 d . . . C62 C 0.03040(19) 0.24422(17) 0.60117(17) 0.0535(7) Uani 1 1 d . . . H62A H 0.0675 0.2147 0.5786 0.064 Uiso 1 1 calc R . . C63 C -0.0403(2) 0.2073(2) 0.61326(17) 0.0641(8) Uani 1 1 d . . . H63A H -0.0510 0.1527 0.5984 0.077 Uiso 1 1 calc R . . C64 C -0.0952(2) 0.2505(2) 0.64712(18) 0.0645(9) Uani 1 1 d . . . H64A H -0.1425 0.2248 0.6553 0.077 Uiso 1 1 calc R . . C65 C -0.08044(18) 0.3316(2) 0.66895(15) 0.0604(8) Uani 1 1 d . . . H65A H -0.1177 0.3604 0.6919 0.072 Uiso 1 1 calc R . . C66 C -0.01071(16) 0.37012(19) 0.65694(13) 0.0474(6) Uani 1 1 d . . . H66A H -0.0012 0.4252 0.6713 0.057 Uiso 1 1 calc R . . C71 C 0.20352(14) 0.36448(15) 0.67431(12) 0.0387(5) Uani 1 1 d . . . C72 C 0.18507(18) 0.32029(17) 0.73033(13) 0.0484(6) Uani 1 1 d . . . H72A H 0.1358 0.2967 0.7337 0.058 Uiso 1 1 calc R . . C73 C 0.2407(2) 0.31164(19) 0.78116(15) 0.0618(9) Uani 1 1 d . . . H73A H 0.2286 0.2823 0.8187 0.074 Uiso 1 1 calc R . . C74 C 0.3132(2) 0.3464(2) 0.77583(16) 0.0621(9) Uani 1 1 d . . . H74A H 0.3503 0.3399 0.8098 0.075 Uiso 1 1 calc R . . C75 C 0.33196(18) 0.3903(2) 0.72122(16) 0.0612(9) Uani 1 1 d . . . H75A H 0.3814 0.4137 0.7184 0.073 Uiso 1 1 calc R . . C76 C 0.27733(15) 0.39996(18) 0.67033(14) 0.0468(6) Uani 1 1 d . . . H76A H 0.2899 0.4302 0.6333 0.056 Uiso 1 1 calc R . . C81 C 0.12254(13) 0.48541(15) 0.59049(11) 0.0342(5) Uani 1 1 d . . . C82 C 0.12815(15) 0.54460(16) 0.64042(12) 0.0416(5) Uani 1 1 d . . . H82A H 0.1401 0.5271 0.6830 0.050 Uiso 1 1 calc R . . C83 C 0.11599(16) 0.62960(17) 0.62707(15) 0.0524(7) Uani 1 1 d . . . H83A H 0.1193 0.6691 0.6607 0.063 Uiso 1 1 calc R . . C84 C 0.09910(17) 0.65593(18) 0.56423(16) 0.0559(7) Uani 1 1 d . . . H84A H 0.0906 0.7131 0.5556 0.067 Uiso 1 1 calc R . . C85 C 0.09463(19) 0.5981(2) 0.51397(16) 0.0612(8) Uani 1 1 d . . . H85A H 0.0840 0.6164 0.4714 0.073 Uiso 1 1 calc R . . C86 C 0.10609(17) 0.51199(18) 0.52686(13) 0.0500(6) Uani 1 1 d . . . H86A H 0.1027 0.4727 0.4931 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.03303(7) 0.02231(6) 0.02474(6) -0.00132(4) 0.00276(4) 0.00114(4) P3 0.0300(3) 0.0228(2) 0.0334(3) -0.0035(2) 0.0012(2) 0.00260(19) P6 0.0359(3) 0.0305(3) 0.0303(3) -0.0030(2) 0.0041(2) 0.0058(2) F1 0.0746(13) 0.0494(10) 0.0645(12) -0.0029(8) 0.0329(10) 0.0041(8) F2 0.237(3) 0.0775(15) 0.0684(14) 0.0326(12) 0.0816(18) 0.0543(18) F3 0.0724(15) 0.192(3) 0.155(3) -0.101(2) 0.0604(16) -0.0549(18) F4 0.1153(16) 0.0454(10) 0.0782(13) -0.0025(9) 0.0445(12) -0.0324(10) F5 0.201(3) 0.0307(9) 0.0878(16) 0.0133(10) 0.0077(17) 0.0203(13) F6 0.1091(18) 0.0678(13) 0.1238(19) -0.0450(13) 0.0274(15) -0.0473(13) F7 0.1132(16) 0.0360(9) 0.0769(12) -0.0201(8) 0.0325(12) -0.0138(9) F11 0.157(3) 0.0976(19) 0.138(2) 0.0772(18) -0.073(2) -0.0376(18) F12 0.184(3) 0.142(2) 0.0462(12) 0.0352(13) 0.0218(14) 0.081(2) F13 0.0833(16) 0.129(2) 0.149(2) 0.0853(19) 0.0321(15) 0.0614(15) F14 0.0475(11) 0.0868(14) 0.0627(13) -0.0017(9) -0.0233(10) 0.0067(8) F15 0.1023(18) 0.0978(18) 0.1174(19) -0.0540(15) -0.0005(15) -0.0412(14) F16 0.0449(10) 0.0694(13) 0.188(3) -0.0284(15) 0.0369(13) -0.0083(9) F17 0.0715(14) 0.0606(13) 0.182(3) 0.0335(15) -0.0356(15) -0.0280(10) F21 0.0660(14) 0.163(2) 0.1084(19) 0.0726(19) -0.0346(13) -0.0517(16) F22 0.0591(14) 0.161(2) 0.0781(16) -0.0377(16) -0.0261(12) 0.0095(14) F23 0.0456(11) 0.0995(18) 0.175(3) 0.0155(17) 0.0051(14) 0.0327(11) F24 0.0654(11) 0.0721(11) 0.0456(9) 0.0287(8) -0.0007(8) 0.0181(9) F25 0.1314(18) 0.0736(13) 0.0537(11) 0.0091(10) 0.0485(12) -0.0051(13) F26 0.159(2) 0.0386(10) 0.145(2) 0.0360(12) 0.0987(19) 0.0256(12) F27 0.0929(17) 0.159(3) 0.1032(18) 0.0747(18) -0.0068(14) -0.0631(17) O1 0.0409(9) 0.0297(7) 0.0339(8) 0.0011(7) 0.0061(7) -0.0009(7) O2 0.0462(9) 0.0247(7) 0.0384(9) -0.0025(6) 0.0045(7) -0.0018(6) O3 0.0424(9) 0.0269(7) 0.0362(8) -0.0035(6) 0.0047(7) 0.0049(6) O6 0.0433(9) 0.0364(9) 0.0374(9) -0.0070(7) 0.0097(7) 0.0024(7) O11 0.0467(10) 0.0387(9) 0.0315(8) 0.0036(7) -0.0011(7) 0.0039(7) O12 0.0362(9) 0.0343(8) 0.0451(9) 0.0000(7) -0.0027(7) -0.0013(7) O21 0.0384(9) 0.0349(8) 0.0299(8) 0.0027(6) -0.0005(7) -0.0017(6) O22 0.0465(10) 0.0370(9) 0.0335(8) 0.0028(7) 0.0068(7) -0.0033(7) C1 0.0640(19) 0.0495(16) 0.0506(16) -0.0008(13) 0.0241(14) -0.0110(13) C2 0.0418(13) 0.0381(12) 0.0330(11) -0.0005(10) 0.0061(10) -0.0038(10) C3 0.0600(17) 0.0349(12) 0.0433(14) 0.0030(11) 0.0129(12) -0.0128(11) C4 0.0492(14) 0.0242(10) 0.0385(12) 0.0015(9) -0.0028(10) -0.0030(9) C5 0.090(2) 0.0314(13) 0.0585(18) -0.0071(13) 0.0145(17) -0.0123(14) C11 0.0544(17) 0.0644(19) 0.0495(17) 0.0183(14) -0.0032(13) 0.0111(14) C12 0.0460(14) 0.0469(14) 0.0282(11) -0.0005(10) 0.0015(10) 0.0163(11) C13 0.0353(13) 0.0547(16) 0.0387(14) -0.0069(11) -0.0056(11) 0.0094(10) C14 0.0326(12) 0.0364(12) 0.0452(13) -0.0127(10) 0.0018(10) 0.0033(9) C15 0.0372(14) 0.0465(15) 0.082(2) -0.0161(15) -0.0040(14) -0.0024(11) C21 0.0446(16) 0.0659(19) 0.0491(18) 0.0127(14) -0.0074(14) 0.0065(13) C22 0.0410(13) 0.0318(12) 0.0351(12) -0.0012(9) -0.0003(10) 0.0078(9) C23 0.0499(14) 0.0384(12) 0.0328(12) 0.0096(10) 0.0038(10) 0.0143(10) C24 0.0559(15) 0.0282(11) 0.0330(12) 0.0049(9) 0.0145(10) 0.0065(10) C25 0.071(2) 0.0413(14) 0.0493(16) 0.0113(12) 0.0218(14) 0.0016(13) C31 0.0317(11) 0.0235(10) 0.0381(11) 0.0010(8) 0.0004(9) 0.0013(8) C32 0.0379(13) 0.0555(16) 0.0433(14) -0.0008(12) -0.0040(11) -0.0023(11) C33 0.0333(14) 0.075(2) 0.0604(18) 0.0047(15) -0.0105(13) -0.0058(13) C34 0.0337(14) 0.0605(18) 0.075(2) 0.0165(16) 0.0064(13) 0.0029(12) C35 0.0438(15) 0.0540(16) 0.0588(17) -0.0021(13) 0.0175(13) 0.0102(12) C36 0.0384(13) 0.0371(12) 0.0473(14) -0.0076(10) 0.0043(11) 0.0025(10) C41 0.0322(11) 0.0362(12) 0.0363(12) -0.0063(9) -0.0006(9) 0.0063(9) C42 0.0407(13) 0.0478(14) 0.0366(12) 0.0005(11) 0.0033(10) 0.0062(11) C43 0.0537(16) 0.0654(18) 0.0374(13) 0.0082(13) 0.0039(12) 0.0158(14) C44 0.0518(17) 0.086(2) 0.0443(16) -0.0015(16) -0.0090(13) 0.0196(16) C45 0.068(2) 0.082(3) 0.078(2) -0.011(2) -0.0356(19) -0.0143(18) C46 0.0609(18) 0.0486(17) 0.0662(19) 0.0002(14) -0.0192(15) -0.0115(14) C51 0.0269(10) 0.0292(10) 0.0401(12) -0.0029(9) -0.0008(9) 0.0008(8) C52 0.0421(13) 0.0290(11) 0.0489(14) -0.0043(10) 0.0051(11) 0.0007(9) C53 0.0525(16) 0.0275(12) 0.0658(18) -0.0032(11) 0.0014(13) 0.0002(10) C54 0.0506(16) 0.0363(15) 0.077(2) 0.0116(13) 0.0052(15) -0.0116(11) C55 0.0463(15) 0.0489(16) 0.0680(19) 0.0064(14) 0.0189(14) -0.0070(12) C56 0.0390(13) 0.0377(14) 0.0531(15) -0.0019(11) 0.0078(11) 0.0010(9) C61 0.0390(12) 0.0397(12) 0.0301(11) 0.0023(9) 0.0066(9) 0.0008(9) C62 0.0532(18) 0.0462(15) 0.062(2) -0.0061(13) 0.0118(15) -0.0023(12) C63 0.068(2) 0.0537(18) 0.072(2) -0.0044(16) 0.0124(17) -0.0184(16) C64 0.0497(19) 0.085(2) 0.060(2) 0.0073(16) 0.0113(15) -0.0204(15) C65 0.0515(17) 0.077(2) 0.0545(17) -0.0046(16) 0.0222(14) -0.0017(15) C66 0.0491(15) 0.0521(16) 0.0418(14) -0.0063(12) 0.0136(12) 0.0006(12) C71 0.0446(13) 0.0347(12) 0.0364(12) -0.0067(10) -0.0014(10) 0.0142(10) C72 0.0618(17) 0.0401(14) 0.0426(14) -0.0029(11) -0.0051(12) 0.0108(12) C73 0.092(3) 0.0511(17) 0.0414(15) 0.0003(13) -0.0106(15) 0.0247(17) C74 0.072(2) 0.0562(18) 0.0556(18) -0.0165(15) -0.0240(16) 0.0293(16) C75 0.0506(17) 0.069(2) 0.063(2) -0.0235(16) -0.0125(15) 0.0203(15) C76 0.0421(14) 0.0521(15) 0.0457(14) -0.0090(12) -0.0019(11) 0.0147(11) C81 0.0331(11) 0.0327(11) 0.0369(12) -0.0009(9) 0.0019(9) 0.0053(9) C82 0.0483(14) 0.0384(12) 0.0387(13) -0.0027(10) 0.0096(11) 0.0044(10) C83 0.0584(17) 0.0341(13) 0.0659(18) -0.0049(12) 0.0162(14) 0.0030(11) C84 0.0521(16) 0.0354(13) 0.081(2) 0.0106(14) 0.0091(15) 0.0077(12) C85 0.071(2) 0.0567(18) 0.0553(18) 0.0218(15) -0.0102(15) 0.0049(15) C86 0.0638(18) 0.0449(15) 0.0406(14) 0.0018(11) -0.0063(12) 0.0038(13) _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 O6 2.2945(16) . ? Eu1 O3 2.3044(15) . ? Eu1 O11 2.3686(16) . ? Eu1 O21 2.3687(17) . ? Eu1 O1 2.4281(16) . ? Eu1 O2 2.4288(15) . ? Eu1 O22 2.4402(16) . ? Eu1 O12 2.4448(16) . ? P3 O3 1.4994(16) . ? P3 C31 1.790(2) . ? P3 C41 1.794(2) . ? P3 C51 1.797(2) . ? P6 O6 1.5009(16) . ? P6 C81 1.794(2) . ? P6 C61 1.795(2) . ? P6 C71 1.801(2) . ? F1 C1 1.302(3) . ? F2 C1 1.309(4) . ? F3 C1 1.314(4) . ? F4 C3 1.370(3) . ? F5 C5 1.320(4) . ? F6 C5 1.320(4) . ? F7 C5 1.333(3) . ? F11 C11 1.287(4) . ? F12 C11 1.316(4) . ? F13 C11 1.289(3) . ? F14 C13 1.367(3) . ? F15 C15 1.317(4) . ? F16 C15 1.314(3) . ? F17 C15 1.292(4) . ? F21 C21 1.297(4) . ? F22 C21 1.300(4) . ? F23 C21 1.325(4) . ? F24 C23 1.364(3) . ? F25 C25 1.308(3) . ? F26 C25 1.314(3) . ? F27 C25 1.290(4) . ? O1 C2 1.250(3) . ? O2 C4 1.245(3) . ? O11 C12 1.260(3) . ? O12 C14 1.236(3) . ? O21 C22 1.239(3) . ? O22 C24 1.245(3) . ? C1 C2 1.546(4) . ? C2 C3 1.382(4) . ? C3 C4 1.391(4) . ? C4 C5 1.534(3) . ? C11 C12 1.539(4) . ? C12 C13 1.380(4) . ? C13 C14 1.398(4) . ? C14 C15 1.551(4) . ? C21 C22 1.545(4) . ? C22 C23 1.395(3) . ? C23 C24 1.385(4) . ? C24 C25 1.546(3) . ? C31 C36 1.379(3) . ? C31 C32 1.392(3) . ? C32 C33 1.392(4) . ? C33 C34 1.372(4) . ? C34 C35 1.370(4) . ? C35 C36 1.391(4) . ? C41 C42 1.388(3) . ? C41 C46 1.394(4) . ? C42 C43 1.381(3) . ? C43 C44 1.369(4) . ? C44 C45 1.364(5) . ? C45 C46 1.393(4) . ? C51 C52 1.387(3) . ? C51 C56 1.396(3) . ? C52 C53 1.381(3) . ? C53 C54 1.379(4) . ? C54 C55 1.387(4) . ? C55 C56 1.392(4) . ? C61 C66 1.391(3) . ? C61 C62 1.402(4) . ? C62 C63 1.380(4) . ? C63 C64 1.377(5) . ? C64 C65 1.376(4) . ? C65 C66 1.376(4) . ? C71 C76 1.392(4) . ? C71 C72 1.393(4) . ? C72 C73 1.391(4) . ? C73 C74 1.371(5) . ? C74 C75 1.368(5) . ? C75 C76 1.382(4) . ? C81 C82 1.387(3) . ? C81 C86 1.389(3) . ? C82 C83 1.383(4) . ? C83 C84 1.374(4) . ? C84 C85 1.376(4) . ? C85 C86 1.397(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 O6 Eu1 O3 142.63(6) . . ? O6 Eu1 O11 83.05(6) . . ? O3 Eu1 O11 107.96(6) . . ? O6 Eu1 O21 105.47(6) . . ? O3 Eu1 O21 84.81(6) . . ? O11 Eu1 O21 146.94(6) . . ? O6 Eu1 O1 141.51(5) . . ? O3 Eu1 O1 75.17(6) . . ? O11 Eu1 O1 75.02(6) . . ? O21 Eu1 O1 79.33(6) . . ? O6 Eu1 O2 74.13(6) . . ? O3 Eu1 O2 142.33(6) . . ? O11 Eu1 O2 78.29(6) . . ? O21 Eu1 O2 73.75(5) . . ? O1 Eu1 O2 70.72(5) . . ? O6 Eu1 O22 73.76(6) . . ? O3 Eu1 O22 76.39(6) . . ? O11 Eu1 O22 141.45(6) . . ? O21 Eu1 O22 70.44(6) . . ? O1 Eu1 O22 139.89(6) . . ? O2 Eu1 O22 122.27(5) . . ? O6 Eu1 O12 79.00(6) . . ? O3 Eu1 O12 72.03(6) . . ? O11 Eu1 O12 70.29(6) . . ? O21 Eu1 O12 142.22(5) . . ? O1 Eu1 O12 120.75(6) . . ? O2 Eu1 O12 140.65(5) . . ? O22 Eu1 O12 75.26(6) . . ? O3 P3 C31 109.58(10) . . ? O3 P3 C41 112.22(10) . . ? C31 P3 C41 108.19(11) . . ? O3 P3 C51 110.02(10) . . ? C31 P3 C51 109.10(10) . . ? C41 P3 C51 107.64(11) . . ? O6 P6 C81 110.12(10) . . ? O6 P6 C61 109.33(11) . . ? C81 P6 C61 109.05(11) . . ? O6 P6 C71 112.42(10) . . ? C81 P6 C71 106.82(11) . . ? C61 P6 C71 109.03(12) . . ? C2 O1 Eu1 136.46(15) . . ? C4 O2 Eu1 136.04(15) . . ? P3 O3 Eu1 151.01(10) . . ? P6 O6 Eu1 151.84(11) . . ? C12 O11 Eu1 138.00(16) . . ? C14 O12 Eu1 136.46(16) . . ? C22 O21 Eu1 138.38(16) . . ? C24 O22 Eu1 136.02(16) . . ? F1 C1 F2 105.7(3) . . ? F1 C1 F3 106.7(3) . . ? F2 C1 F3 108.2(3) . . ? F1 C1 C2 112.4(2) . . ? F2 C1 C2 111.4(3) . . ? F3 C1 C2 112.0(3) . . ? O1 C2 C3 125.6(2) . . ? O1 C2 C1 115.6(2) . . ? C3 C2 C1 118.8(2) . . ? F4 C3 C2 117.7(2) . . ? F4 C3 C4 117.6(2) . . ? C2 C3 C4 124.6(2) . . ? O2 C4 C3 126.1(2) . . ? O2 C4 C5 116.1(2) . . ? C3 C4 C5 117.8(2) . . ? F6 C5 F5 107.2(3) . . ? F6 C5 F7 106.9(3) . . ? F5 C5 F7 106.6(3) . . ? F6 C5 C4 113.3(3) . . ? F5 C5 C4 111.2(2) . . ? F7 C5 C4 111.3(2) . . ? F11 C11 F13 107.0(3) . . ? F11 C11 F12 104.4(3) . . ? F13 C11 F12 106.1(3) . . ? F11 C11 C12 112.0(2) . . ? F13 C11 C12 114.8(3) . . ? F12 C11 C12 111.8(3) . . ? O11 C12 C13 125.7(2) . . ? O11 C12 C11 114.7(2) . . ? C13 C12 C11 119.6(2) . . ? F14 C13 C12 118.9(2) . . ? F14 C13 C14 117.5(2) . . ? C12 C13 C14 123.6(2) . . ? O12 C14 C13 125.5(2) . . ? O12 C14 C15 115.6(2) . . ? C13 C14 C15 118.9(2) . . ? F17 C15 F16 109.3(3) . . ? F17 C15 F15 105.9(3) . . ? F16 C15 F15 106.1(3) . . ? F17 C15 C14 111.6(2) . . ? F16 C15 C14 111.0(2) . . ? F15 C15 C14 112.7(3) . . ? F21 C21 F22 109.7(3) . . ? F21 C21 F23 105.4(3) . . ? F22 C21 F23 106.0(3) . . ? F21 C21 C22 111.8(2) . . ? F22 C21 C22 113.3(3) . . ? F23 C21 C22 110.2(3) . . ? O21 C22 C23 125.7(2) . . ? O21 C22 C21 115.7(2) . . ? C23 C22 C21 118.6(2) . . ? F24 C23 C24 118.3(2) . . ? F24 C23 C22 118.0(2) . . ? C24 C23 C22 123.7(2) . . ? O22 C24 C23 125.6(2) . . ? O22 C24 C25 115.7(2) . . ? C23 C24 C25 118.7(2) . . ? F27 C25 F25 107.2(3) . . ? F27 C25 F26 108.4(3) . . ? F25 C25 F26 105.3(3) . . ? F27 C25 C24 111.9(2) . . ? F25 C25 C24 113.3(2) . . ? F26 C25 C24 110.4(2) . . ? C36 C31 C32 120.0(2) . . ? C36 C31 P3 122.97(18) . . ? C32 C31 P3 117.04(18) . . ? C33 C32 C31 119.7(3) . . ? C34 C33 C32 119.7(3) . . ? C35 C34 C33 120.9(3) . . ? C34 C35 C36 120.0(3) . . ? C31 C36 C35 119.7(2) . . ? C42 C41 C46 118.7(2) . . ? C42 C41 P3 118.72(18) . . ? C46 C41 P3 122.5(2) . . ? C43 C42 C41 120.7(3) . . ? C44 C43 C42 120.1(3) . . ? C45 C44 C43 120.4(3) . . ? C44 C45 C46 120.4(3) . . ? C45 C46 C41 119.7(3) . . ? C52 C51 C56 120.0(2) . . ? C52 C51 P3 121.84(18) . . ? C56 C51 P3 118.16(18) . . ? C53 C52 C51 120.2(2) . . ? C54 C53 C52 120.3(3) . . ? C53 C54 C55 119.9(3) . . ? C54 C55 C56 120.3(3) . . ? C55 C56 C51 119.2(2) . . ? C66 C61 C62 119.6(2) . . ? C66 C61 P6 122.4(2) . . ? C62 C61 P6 118.0(2) . . ? C63 C62 C61 119.2(3) . . ? C64 C63 C62 120.6(3) . . ? C65 C64 C63 120.3(3) . . ? C66 C65 C64 120.2(3) . . ? C65 C66 C61 120.1(3) . . ? C76 C71 C72 119.4(2) . . ? C76 C71 P6 118.0(2) . . ? C72 C71 P6 122.6(2) . . ? C73 C72 C71 119.6(3) . . ? C74 C73 C72 119.9(3) . . ? C75 C74 C73 121.0(3) . . ? C74 C75 C76 119.9(3) . . ? C75 C76 C71 120.2(3) . . ? C82 C81 C86 119.7(2) . . ? C82 C81 P6 122.38(18) . . ? C86 C81 P6 117.87(19) . . ? C83 C82 C81 120.1(2) . . ? C84 C83 C82 120.2(3) . . ? C83 C84 C85 120.4(3) . . ? C84 C85 C86 120.0(3) . . ? C81 C86 C85 119.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Eu1 O1 C2 19.1(3) . . . . ? O3 Eu1 O1 C2 -169.8(2) . . . . ? O11 Eu1 O1 C2 76.5(2) . . . . ? O21 Eu1 O1 C2 -82.4(2) . . . . ? O2 Eu1 O1 C2 -6.1(2) . . . . ? O22 Eu1 O1 C2 -123.6(2) . . . . ? O12 Eu1 O1 C2 132.1(2) . . . . ? O6 Eu1 O2 C4 -156.9(2) . . . . ? O3 Eu1 O2 C4 33.4(3) . . . . ? O11 Eu1 O2 C4 -70.9(2) . . . . ? O21 Eu1 O2 C4 91.3(2) . . . . ? O1 Eu1 O2 C4 7.1(2) . . . . ? O22 Eu1 O2 C4 144.6(2) . . . . ? O12 Eu1 O2 C4 -108.2(2) . . . . ? C31 P3 O3 Eu1 98.5(2) . . . . ? C41 P3 O3 Eu1 -21.7(2) . . . . ? C51 P3 O3 Eu1 -141.56(19) . . . . ? O6 Eu1 O3 P3 114.5(2) . . . . ? O11 Eu1 O3 P3 12.1(2) . . . . ? O21 Eu1 O3 P3 -136.7(2) . . . . ? O1 Eu1 O3 P3 -56.4(2) . . . . ? O2 Eu1 O3 P3 -82.0(2) . . . . ? O22 Eu1 O3 P3 152.2(2) . . . . ? O12 Eu1 O3 P3 73.5(2) . . . . ? C81 P6 O6 Eu1 115.2(2) . . . . ? C61 P6 O6 Eu1 -125.0(2) . . . . ? C71 P6 O6 Eu1 -3.8(3) . . . . ? O3 Eu1 O6 P6 94.4(2) . . . . ? O11 Eu1 O6 P6 -155.0(2) . . . . ? O21 Eu1 O6 P6 -7.6(2) . . . . ? O1 Eu1 O6 P6 -99.9(2) . . . . ? O2 Eu1 O6 P6 -75.3(2) . . . . ? O22 Eu1 O6 P6 56.1(2) . . . . ? O12 Eu1 O6 P6 133.8(2) . . . . ? O6 Eu1 O11 C12 -73.5(2) . . . . ? O3 Eu1 O11 C12 69.8(2) . . . . ? O21 Eu1 O11 C12 178.7(2) . . . . ? O1 Eu1 O11 C12 138.4(2) . . . . ? O2 Eu1 O11 C12 -148.7(2) . . . . ? O22 Eu1 O11 C12 -20.7(3) . . . . ? O12 Eu1 O11 C12 7.3(2) . . . . ? O6 Eu1 O12 C14 84.8(2) . . . . ? O3 Eu1 O12 C14 -119.1(2) . . . . ? O11 Eu1 O12 C14 -1.7(2) . . . . ? O21 Eu1 O12 C14 -174.11(19) . . . . ? O1 Eu1 O12 C14 -59.5(2) . . . . ? O2 Eu1 O12 C14 37.3(3) . . . . ? O22 Eu1 O12 C14 160.7(2) . . . . ? O6 Eu1 O21 C22 70.7(2) . . . . ? O3 Eu1 O21 C22 -72.7(2) . . . . ? O11 Eu1 O21 C22 172.0(2) . . . . ? O1 Eu1 O21 C22 -148.5(2) . . . . ? O2 Eu1 O21 C22 138.6(2) . . . . ? O22 Eu1 O21 C22 4.7(2) . . . . ? O12 Eu1 O21 C22 -21.2(3) . . . . ? O6 Eu1 O22 C24 -118.2(2) . . . . ? O3 Eu1 O22 C24 84.5(2) . . . . ? O11 Eu1 O22 C24 -173.63(19) . . . . ? O21 Eu1 O22 C24 -4.7(2) . . . . ? O1 Eu1 O22 C24 38.6(2) . . . . ? O2 Eu1 O22 C24 -59.6(2) . . . . ? O12 Eu1 O22 C24 159.2(2) . . . . ? Eu1 O1 C2 C3 3.4(4) . . . . ? Eu1 O1 C2 C1 -177.38(17) . . . . ? F1 C1 C2 O1 -0.3(4) . . . . ? F2 C1 C2 O1 118.2(3) . . . . ? F3 C1 C2 O1 -120.5(3) . . . . ? F1 C1 C2 C3 179.0(3) . . . . ? F2 C1 C2 C3 -62.6(4) . . . . ? F3 C1 C2 C3 58.8(4) . . . . ? O1 C2 C3 F4 -177.2(2) . . . . ? C1 C2 C3 F4 3.6(4) . . . . ? O1 C2 C3 C4 2.5(5) . . . . ? C1 C2 C3 C4 -176.7(3) . . . . ? Eu1 O2 C4 C3 -5.6(4) . . . . ? Eu1 O2 C4 C5 173.89(19) . . . . ? F4 C3 C4 O2 178.3(2) . . . . ? C2 C3 C4 O2 -1.4(5) . . . . ? F4 C3 C4 C5 -1.2(4) . . . . ? C2 C3 C4 C5 179.1(3) . . . . ? O2 C4 C5 F6 127.8(3) . . . . ? C3 C4 C5 F6 -52.6(4) . . . . ? O2 C4 C5 F5 -111.4(3) . . . . ? C3 C4 C5 F5 68.2(4) . . . . ? O2 C4 C5 F7 7.3(4) . . . . ? C3 C4 C5 F7 -173.1(3) . . . . ? Eu1 O11 C12 C13 -8.6(4) . . . . ? Eu1 O11 C12 C11 172.12(18) . . . . ? F11 C11 C12 O11 -13.0(4) . . . . ? F13 C11 C12 O11 -135.3(3) . . . . ? F12 C11 C12 O11 103.8(3) . . . . ? F11 C11 C12 C13 167.6(3) . . . . ? F13 C11 C12 C13 45.4(4) . . . . ? F12 C11 C12 C13 -75.5(4) . . . . ? O11 C12 C13 F14 -177.1(2) . . . . ? C11 C12 C13 F14 2.1(4) . . . . ? O11 C12 C13 C14 1.3(4) . . . . ? C11 C12 C13 C14 -179.4(2) . . . . ? Eu1 O12 C14 C13 -2.3(4) . . . . ? Eu1 O12 C14 C15 178.96(16) . . . . ? F14 C13 C14 O12 -177.7(2) . . . . ? C12 C13 C14 O12 3.8(4) . . . . ? F14 C13 C14 C15 0.9(4) . . . . ? C12 C13 C14 C15 -177.5(2) . . . . ? O12 C14 C15 F17 -11.7(4) . . . . ? C13 C14 C15 F17 169.5(3) . . . . ? O12 C14 C15 F16 110.6(3) . . . . ? C13 C14 C15 F16 -68.3(4) . . . . ? O12 C14 C15 F15 -130.6(3) . . . . ? C13 C14 C15 F15 50.5(3) . . . . ? Eu1 O21 C22 C23 -4.6(4) . . . . ? Eu1 O21 C22 C21 174.85(18) . . . . ? F21 C21 C22 O21 -1.3(4) . . . . ? F22 C21 C22 O21 123.3(3) . . . . ? F23 C21 C22 O21 -118.2(3) . . . . ? F21 C21 C22 C23 178.2(3) . . . . ? F22 C21 C22 C23 -57.2(4) . . . . ? F23 C21 C22 C23 61.3(4) . . . . ? O21 C22 C23 F24 -178.6(2) . . . . ? C21 C22 C23 F24 1.9(3) . . . . ? O21 C22 C23 C24 1.6(4) . . . . ? C21 C22 C23 C24 -177.9(2) . . . . ? Eu1 O22 C24 C23 4.8(4) . . . . ? Eu1 O22 C24 C25 -174.18(16) . . . . ? F24 C23 C24 O22 178.4(2) . . . . ? C22 C23 C24 O22 -1.8(4) . . . . ? F24 C23 C24 C25 -2.6(3) . . . . ? C22 C23 C24 C25 177.1(2) . . . . ? O22 C24 C25 F27 -1.4(4) . . . . ? C23 C24 C25 F27 179.5(3) . . . . ? O22 C24 C25 F25 -122.8(3) . . . . ? C23 C24 C25 F25 58.1(3) . . . . ? O22 C24 C25 F26 119.4(3) . . . . ? C23 C24 C25 F26 -59.7(4) . . . . ? O3 P3 C31 C36 -156.05(19) . . . . ? C41 P3 C31 C36 -33.4(2) . . . . ? C51 P3 C31 C36 83.4(2) . . . . ? O3 P3 C31 C32 23.6(2) . . . . ? C41 P3 C31 C32 146.29(19) . . . . ? C51 P3 C31 C32 -96.9(2) . . . . ? C36 C31 C32 C33 -0.1(4) . . . . ? P3 C31 C32 C33 -179.8(2) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? C32 C33 C34 C35 -0.1(5) . . . . ? C33 C34 C35 C36 0.7(5) . . . . ? C32 C31 C36 C35 0.6(4) . . . . ? P3 C31 C36 C35 -179.7(2) . . . . ? C34 C35 C36 C31 -1.0(4) . . . . ? O3 P3 C41 C42 59.8(2) . . . . ? C31 P3 C41 C42 -61.2(2) . . . . ? C51 P3 C41 C42 -179.00(18) . . . . ? O3 P3 C41 C46 -115.6(2) . . . . ? C31 P3 C41 C46 123.4(2) . . . . ? C51 P3 C41 C46 5.6(3) . . . . ? C46 C41 C42 C43 -0.6(4) . . . . ? P3 C41 C42 C43 -176.2(2) . . . . ? C41 C42 C43 C44 0.5(4) . . . . ? C42 C43 C44 C45 -0.5(5) . . . . ? C43 C44 C45 C46 0.6(6) . . . . ? C44 C45 C46 C41 -0.7(6) . . . . ? C42 C41 C46 C45 0.7(5) . . . . ? P3 C41 C46 C45 176.1(3) . . . . ? O3 P3 C51 C52 -163.08(19) . . . . ? C31 P3 C51 C52 -42.8(2) . . . . ? C41 P3 C51 C52 74.4(2) . . . . ? O3 P3 C51 C56 16.0(2) . . . . ? C31 P3 C51 C56 136.27(19) . . . . ? C41 P3 C51 C56 -106.54(19) . . . . ? C56 C51 C52 C53 0.2(4) . . . . ? P3 C51 C52 C53 179.3(2) . . . . ? C51 C52 C53 C54 -1.1(4) . . . . ? C52 C53 C54 C55 1.7(4) . . . . ? C53 C54 C55 C56 -1.3(4) . . . . ? C54 C55 C56 C51 0.4(4) . . . . ? C52 C51 C56 C55 0.1(4) . . . . ? P3 C51 C56 C55 -179.0(2) . . . . ? O6 P6 C61 C66 -153.6(2) . . . . ? C81 P6 C61 C66 -33.1(2) . . . . ? C71 P6 C61 C66 83.1(2) . . . . ? O6 P6 C61 C62 24.4(3) . . . . ? C81 P6 C61 C62 144.9(2) . . . . ? C71 P6 C61 C62 -98.8(2) . . . . ? C66 C61 C62 C63 0.0(5) . . . . ? P6 C61 C62 C63 -178.1(3) . . . . ? C61 C62 C63 C64 -0.6(5) . . . . ? C62 C63 C64 C65 0.5(6) . . . . ? C63 C64 C65 C66 0.2(5) . . . . ? C64 C65 C66 C61 -0.7(5) . . . . ? C62 C61 C66 C65 0.7(4) . . . . ? P6 C61 C66 C65 178.7(2) . . . . ? O6 P6 C71 C76 60.7(2) . . . . ? C81 P6 C71 C76 -60.2(2) . . . . ? C61 P6 C71 C76 -177.95(18) . . . . ? O6 P6 C71 C72 -116.7(2) . . . . ? C81 P6 C71 C72 122.4(2) . . . . ? C61 P6 C71 C72 4.7(2) . . . . ? C76 C71 C72 C73 -0.5(4) . . . . ? P6 C71 C72 C73 176.8(2) . . . . ? C71 C72 C73 C74 -0.2(4) . . . . ? C72 C73 C74 C75 0.6(4) . . . . ? C73 C74 C75 C76 -0.2(4) . . . . ? C74 C75 C76 C71 -0.5(4) . . . . ? C72 C71 C76 C75 0.9(4) . . . . ? P6 C71 C76 C75 -176.6(2) . . . . ? O6 P6 C81 C82 -151.4(2) . . . . ? C61 P6 C81 C82 88.6(2) . . . . ? C71 P6 C81 C82 -29.1(2) . . . . ? O6 P6 C81 C86 27.9(2) . . . . ? C61 P6 C81 C86 -92.1(2) . . . . ? C71 P6 C81 C86 150.2(2) . . . . ? C86 C81 C82 C83 1.2(4) . . . . ? P6 C81 C82 C83 -179.5(2) . . . . ? C81 C82 C83 C84 -0.7(4) . . . . ? C82 C83 C84 C85 -0.4(5) . . . . ? C83 C84 C85 C86 1.0(5) . . . . ? C82 C81 C86 C85 -0.6(4) . . . . ? P6 C81 C86 C85 -180.0(2) . . . . ? C84 C85 C86 C81 -0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 33.15 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.237 _refine_diff_density_min -0.873 _refine_diff_density_rms 0.102 data_00052 _database_code_CSD 171066 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H30 F21 O8 P2 Tb' _chemical_formula_weight 1390.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 17.2022(10) _cell_length_b 15.7548(10) _cell_length_c 20.4466(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 92.641(10) _cell_angle_gamma 90.000(10) _cell_volume 5535.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'ireg bloc!' _exptl_crystal_colour colorless _exptl_crystal_size_max .38 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .42 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 1.457 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35468 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.29 _reflns_number_total 12992 _reflns_number_gt 10382 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00013(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12992 _refine_ls_number_parameters 749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.238543(8) 0.237995(8) 0.508846(6) 0.02574(5) Uani 1 1 d . . . P3 P 0.36283(4) 0.12755(5) 0.39575(4) 0.03085(17) Uani 1 1 d . . . P6 P 0.18269(4) 0.43650(4) 0.58710(4) 0.02760(16) Uani 1 1 d . . . F1 F 0.19136(15) -0.06085(13) 0.45565(11) 0.0720(7) Uani 1 1 d . . . F2 F 0.1817(2) -0.09702(15) 0.55520(13) 0.1062(11) Uani 1 1 d . . . F3 F 0.07959(16) -0.07660(17) 0.49468(15) 0.0979(10) Uani 1 1 d . . . F4 F 0.06059(15) 0.00873(14) 0.60725(12) 0.0751(7) Uani 1 1 d . . . F5 F 0.0580(2) 0.12915(18) 0.70966(13) 0.1263(14) Uani 1 1 d . . . F6 F -0.03106(16) 0.1513(3) 0.63698(18) 0.1367(16) Uani 1 1 d . . . F7 F 0.04007(15) 0.25073(13) 0.67255(12) 0.0602(6) Uani 1 1 d . . . F11 F 0.3331(2) 0.0524(2) 0.67916(18) 0.1365(15) Uani 1 1 d . . . F12 F 0.3667(2) 0.1433(2) 0.74626(13) 0.1258(14) Uani 1 1 d . . . F13 F 0.44861(16) 0.0869(2) 0.68964(17) 0.1232(13) Uani 1 1 d . . . F14 F 0.47869(14) 0.25474(14) 0.67189(13) 0.0622(7) Uani 1 1 d . . . F15 F 0.47955(16) 0.42277(19) 0.64220(15) 0.1015(10) Uani 1 1 d . . . F16 F 0.53392(13) 0.36174(16) 0.56547(16) 0.0932(9) Uani 1 1 d . . . F17 F 0.44301(14) 0.45118(16) 0.54624(16) 0.0992(10) Uani 1 1 d . . . F21 F -0.01335(16) 0.2048(2) 0.40228(16) 0.1152(13) Uani 1 1 d . . . F22 F 0.01478(15) 0.2220(2) 0.30355(15) 0.0977(10) Uani 1 1 d . . . F23 F -0.01993(14) 0.32526(19) 0.36019(18) 0.1050(11) Uani 1 1 d . . . F24 F 0.11743(12) 0.35711(14) 0.29052(10) 0.0586(6) Uani 1 1 d . . . F25 F 0.23155(18) 0.48370(15) 0.31602(15) 0.1058(11) Uani 1 1 d . . . F26 F 0.27245(16) 0.38474(16) 0.25949(11) 0.0806(8) Uani 1 1 d . . . F27 F 0.33922(16) 0.4260(2) 0.34192(14) 0.1135(12) Uani 1 1 d . . . O1 O 0.19686(12) 0.09260(12) 0.49952(10) 0.0345(5) Uani 1 1 d . . . O2 O 0.13680(11) 0.21486(13) 0.58367(10) 0.0330(4) Uani 1 1 d . . . O3 O 0.33282(11) 0.16893(13) 0.45577(10) 0.0357(5) Uani 1 1 d . . . O6 O 0.19751(11) 0.37017(12) 0.53658(10) 0.0331(4) Uani 1 1 d . . . O11 O 0.30069(12) 0.17607(13) 0.60116(10) 0.0370(5) Uani 1 1 d . . . O12 O 0.35248(11) 0.32099(13) 0.54088(10) 0.0363(5) Uani 1 1 d . . . O21 O 0.12826(13) 0.23816(12) 0.43767(10) 0.0316(5) Uani 1 1 d . . . O22 O 0.26475(12) 0.32344(13) 0.41436(10) 0.0362(5) Uani 1 1 d . . . C1 C 0.1504(3) -0.0481(2) 0.5085(2) 0.0569(10) Uani 1 1 d . . . C2 C 0.15209(18) 0.04524(18) 0.52925(15) 0.0353(7) Uani 1 1 d . . . C3 C 0.1049(2) 0.0702(2) 0.57907(17) 0.0442(8) Uani 1 1 d . . . C4 C 0.09884(17) 0.1519(2) 0.60213(14) 0.0343(7) Uani 1 1 d . . . C5 C 0.0404(2) 0.1711(3) 0.65568(19) 0.0550(10) Uani 1 1 d . . . C11 C 0.3793(2) 0.1164(3) 0.68713(19) 0.0550(10) Uani 1 1 d . . . C12 C 0.36324(19) 0.1851(2) 0.63515(14) 0.0381(7) Uani 1 1 d . . . C13 C 0.4152(2) 0.2512(2) 0.62944(18) 0.0411(8) Uani 1 1 d . . . C14 C 0.40587(17) 0.31669(19) 0.58364(15) 0.0356(7) Uani 1 1 d . . . C15 C 0.4662(2) 0.3890(2) 0.5834(2) 0.0536(10) Uani 1 1 d . . . C21 C 0.0209(2) 0.2541(2) 0.3618(2) 0.0506(10) Uani 1 1 d . . . C22 C 0.10606(18) 0.27274(19) 0.38520(15) 0.0342(7) Uani 1 1 d . . . C23 C 0.15041(19) 0.3255(2) 0.34757(15) 0.0373(7) Uani 1 1 d . . . C24 C 0.22659(19) 0.34811(18) 0.36451(15) 0.0363(7) Uani 1 1 d . . . C25 C 0.2689(2) 0.4109(2) 0.32024(18) 0.0498(9) Uani 1 1 d . . . C31 C 0.37721(16) 0.01611(19) 0.40983(15) 0.0324(6) Uani 1 1 d . . . C32 C 0.3937(2) -0.0110(2) 0.47334(16) 0.0482(8) Uani 1 1 d . . . H32A H 0.3970 0.0282 0.5073 0.058 Uiso 1 1 calc R . . C33 C 0.4053(2) -0.0968(3) 0.48650(19) 0.0585(10) Uani 1 1 d . . . H33A H 0.4158 -0.1152 0.5292 0.070 Uiso 1 1 calc R . . C34 C 0.4011(2) -0.1547(2) 0.4354(2) 0.0525(9) Uani 1 1 d . . . H34A H 0.4097 -0.2120 0.4438 0.063 Uiso 1 1 calc R . . C35 C 0.3843(2) -0.1279(2) 0.37257(19) 0.0500(9) Uani 1 1 d . . . H35A H 0.3811 -0.1673 0.3387 0.060 Uiso 1 1 calc R . . C36 C 0.37206(18) -0.0429(2) 0.35922(16) 0.0390(7) Uani 1 1 d . . . H36A H 0.3604 -0.0252 0.3165 0.047 Uiso 1 1 calc R . . C41 C 0.29653(18) 0.13755(19) 0.32546(15) 0.0366(7) Uani 1 1 d . . . C42 C 0.22273(19) 0.1021(2) 0.32939(17) 0.0449(8) Uani 1 1 d . . . H42A H 0.2101 0.0720 0.3666 0.054 Uiso 1 1 calc R . . C43 C 0.1682(2) 0.1115(3) 0.2779(2) 0.0578(11) Uani 1 1 d . . . H43A H 0.1189 0.0878 0.2806 0.069 Uiso 1 1 calc R . . C44 C 0.1866(2) 0.1559(3) 0.22299(19) 0.0593(11) Uani 1 1 d . . . H44A H 0.1496 0.1626 0.1888 0.071 Uiso 1 1 calc R . . C45 C 0.2594(3) 0.1904(2) 0.21833(18) 0.0591(11) Uani 1 1 d . . . H45A H 0.2717 0.2198 0.1808 0.071 Uiso 1 1 calc R . . C46 C 0.3146(2) 0.1816(2) 0.26955(16) 0.0470(8) Uani 1 1 d . . . H46A H 0.3638 0.2053 0.2663 0.056 Uiso 1 1 calc R . . C51 C 0.45402(18) 0.1749(2) 0.37696(14) 0.0352(7) Uani 1 1 d . . . C52 C 0.50997(19) 0.1321(2) 0.34303(16) 0.0450(8) Uani 1 1 d . . . H52A H 0.5004 0.0771 0.3283 0.054 Uiso 1 1 calc R . . C53 C 0.5798(2) 0.1710(3) 0.33106(19) 0.0576(10) Uani 1 1 d . . . H53A H 0.6167 0.1422 0.3077 0.069 Uiso 1 1 calc R . . C54 C 0.5952(2) 0.2515(3) 0.3532(2) 0.0606(11) Uani 1 1 d . . . H54A H 0.6427 0.2770 0.3454 0.073 Uiso 1 1 calc R . . C55 C 0.5399(2) 0.2950(3) 0.3872(2) 0.0620(11) Uani 1 1 d . . . H55A H 0.5505 0.3497 0.4022 0.074 Uiso 1 1 calc R . . C56 C 0.4690(2) 0.2574(2) 0.3991(2) 0.0507(9) Uani 1 1 d . . . H56A H 0.4318 0.2870 0.4216 0.061 Uiso 1 1 calc R . . C61 C 0.08146(16) 0.43661(17) 0.60411(14) 0.0290(6) Uani 1 1 d . . . C62 C 0.05368(18) 0.4666(2) 0.66255(16) 0.0394(7) Uani 1 1 d . . . H62A H 0.0880 0.4874 0.6951 0.047 Uiso 1 1 calc R . . C63 C -0.0255(2) 0.4652(2) 0.67192(18) 0.0501(9) Uani 1 1 d . . . H63A H -0.0444 0.4860 0.7107 0.060 Uiso 1 1 calc R . . C64 C -0.0763(2) 0.4332(2) 0.6243(2) 0.0541(10) Uani 1 1 d . . . H64A H -0.1293 0.4320 0.6313 0.065 Uiso 1 1 calc R . . C65 C -0.04961(19) 0.4032(3) 0.56634(19) 0.0542(10) Uani 1 1 d . . . H65A H -0.0845 0.3819 0.5343 0.065 Uiso 1 1 calc R . . C66 C 0.03014(18) 0.4046(2) 0.55583(16) 0.0434(8) Uani 1 1 d . . . H66A H 0.0487 0.3842 0.5168 0.052 Uiso 1 1 calc R . . C71 C 0.20909(16) 0.53931(18) 0.55742(14) 0.0312(6) Uani 1 1 d . . . C72 C 0.18316(18) 0.61380(19) 0.58590(17) 0.0381(7) Uani 1 1 d . . . H72A H 0.1516 0.6111 0.6216 0.046 Uiso 1 1 calc R . . C73 C 0.2042(2) 0.6916(2) 0.56129(18) 0.0469(8) Uani 1 1 d . . . H73A H 0.1877 0.7412 0.5811 0.056 Uiso 1 1 calc R . . C74 C 0.2493(2) 0.6964(2) 0.50769(19) 0.0532(10) Uani 1 1 d . . . H74A H 0.2618 0.7491 0.4905 0.064 Uiso 1 1 calc R . . C75 C 0.2761(2) 0.6227(2) 0.47919(19) 0.0508(9) Uani 1 1 d . . . H75A H 0.3076 0.6262 0.4435 0.061 Uiso 1 1 calc R . . C76 C 0.25595(17) 0.5436(2) 0.50373(16) 0.0424(8) Uani 1 1 d . . . H76A H 0.2736 0.4941 0.4845 0.051 Uiso 1 1 calc R . . C81 C 0.23794(16) 0.41875(19) 0.66279(14) 0.0330(6) Uani 1 1 d . . . C82 C 0.22624(18) 0.3435(2) 0.69630(15) 0.0402(7) Uani 1 1 d . . . H82A H 0.1883 0.3055 0.6809 0.048 Uiso 1 1 calc R . . C83 C 0.2708(2) 0.3249(3) 0.75259(17) 0.0509(9) Uani 1 1 d . . . H83A H 0.2625 0.2746 0.7750 0.061 Uiso 1 1 calc R . . C84 C 0.3268(2) 0.3800(3) 0.77534(18) 0.0581(10) Uani 1 1 d . . . H84A H 0.3567 0.3670 0.8130 0.070 Uiso 1 1 calc R . . C85 C 0.3391(2) 0.4542(3) 0.7429(2) 0.0713(13) Uani 1 1 d . . . H85A H 0.3771 0.4918 0.7589 0.086 Uiso 1 1 calc R . . C86 C 0.2953(2) 0.4740(2) 0.6864(2) 0.0579(10) Uani 1 1 d . . . H86A H 0.3044 0.5244 0.6643 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03248(9) 0.02118(8) 0.02356(8) -0.00110(5) 0.00147(6) 0.00137(5) P3 0.0357(4) 0.0282(4) 0.0287(4) -0.0022(3) 0.0031(3) 0.0058(3) P6 0.0299(4) 0.0216(3) 0.0312(4) -0.0034(3) 0.0003(3) 0.0020(3) F1 0.1104(19) 0.0343(12) 0.0740(15) -0.0171(11) 0.0328(14) -0.0120(12) F2 0.207(3) 0.0283(13) 0.0835(19) 0.0118(12) 0.006(2) 0.0200(17) F3 0.108(2) 0.0659(17) 0.122(2) -0.0464(16) 0.0299(18) -0.0476(16) F4 0.1112(19) 0.0419(13) 0.0756(16) -0.0020(11) 0.0428(14) -0.0306(13) F5 0.241(4) 0.0771(19) 0.0683(17) 0.0345(15) 0.085(2) 0.063(2) F6 0.0703(19) 0.191(4) 0.154(3) -0.101(3) 0.059(2) -0.056(2) F7 0.0734(16) 0.0476(13) 0.0622(16) -0.0039(10) 0.0312(13) 0.0020(10) F11 0.162(3) 0.104(3) 0.136(3) 0.082(2) -0.079(2) -0.044(2) F12 0.202(4) 0.131(3) 0.0458(16) 0.0346(16) 0.024(2) 0.081(3) F13 0.0829(19) 0.129(3) 0.160(3) 0.094(2) 0.0356(19) 0.0602(19) F14 0.0468(13) 0.0802(17) 0.0574(15) -0.0016(11) -0.0220(12) 0.0077(10) F15 0.099(2) 0.094(2) 0.111(2) -0.0521(18) -0.0033(18) -0.0371(17) F16 0.0435(13) 0.0635(16) 0.175(3) -0.0273(17) 0.0333(15) -0.0083(11) F17 0.0688(16) 0.0531(16) 0.172(3) 0.0314(17) -0.0355(18) -0.0245(12) F21 0.0656(17) 0.168(3) 0.108(2) 0.077(2) -0.0376(16) -0.054(2) F22 0.0576(16) 0.156(3) 0.077(2) -0.0372(19) -0.0246(15) 0.0072(17) F23 0.0449(14) 0.096(2) 0.175(3) 0.005(2) 0.0052(17) 0.0303(14) F24 0.0657(13) 0.0656(14) 0.0439(12) 0.0256(10) -0.0040(10) 0.0156(11) F25 0.153(3) 0.0368(13) 0.135(2) 0.0347(14) 0.092(2) 0.0243(15) F26 0.129(2) 0.0680(16) 0.0489(14) 0.0077(11) 0.0436(15) -0.0065(15) F27 0.087(2) 0.154(3) 0.098(2) 0.073(2) -0.0068(17) -0.059(2) O1 0.0433(12) 0.0246(11) 0.0357(11) -0.0011(8) 0.0029(9) -0.0021(9) O2 0.0362(11) 0.0307(11) 0.0325(11) -0.0009(9) 0.0050(9) -0.0011(9) O3 0.0391(11) 0.0337(11) 0.0352(12) -0.0062(9) 0.0095(9) 0.0015(9) O6 0.0401(11) 0.0250(10) 0.0343(11) -0.0034(8) 0.0047(9) 0.0035(8) O11 0.0442(12) 0.0380(12) 0.0286(11) 0.0044(9) -0.0013(9) 0.0041(10) O12 0.0355(11) 0.0315(11) 0.0415(12) -0.0016(9) -0.0021(9) 0.0001(9) O21 0.0397(12) 0.0308(11) 0.0239(11) 0.0018(8) -0.0033(9) -0.0014(8) O22 0.0443(12) 0.0340(11) 0.0304(11) 0.0024(9) 0.0049(9) -0.0033(9) C1 0.081(3) 0.0323(19) 0.058(2) -0.0076(17) 0.015(2) -0.0100(18) C2 0.0450(17) 0.0237(15) 0.0368(17) 0.0006(12) -0.0026(14) -0.0021(13) C3 0.057(2) 0.0311(17) 0.0457(19) 0.0035(14) 0.0126(16) -0.0131(15) C4 0.0398(16) 0.0348(16) 0.0285(15) -0.0015(12) 0.0030(13) -0.0070(13) C5 0.065(2) 0.052(2) 0.050(2) -0.0030(17) 0.0227(19) -0.0111(19) C11 0.055(2) 0.061(3) 0.048(2) 0.0192(18) -0.0051(18) 0.0099(19) C12 0.0461(18) 0.0451(19) 0.0233(15) 0.0017(13) 0.0017(13) 0.0146(15) C13 0.0338(17) 0.052(2) 0.0370(19) -0.0058(14) -0.0059(14) 0.0082(14) C14 0.0311(15) 0.0358(17) 0.0398(18) -0.0109(13) 0.0001(13) 0.0034(12) C15 0.041(2) 0.043(2) 0.076(3) -0.0130(19) -0.0064(19) -0.0014(16) C21 0.045(2) 0.066(3) 0.040(2) 0.0110(17) -0.0084(17) 0.0055(17) C22 0.0387(17) 0.0311(16) 0.0323(17) -0.0015(12) -0.0036(13) 0.0072(13) C23 0.0471(18) 0.0351(17) 0.0296(16) 0.0077(12) 0.0016(14) 0.0137(14) C24 0.0544(19) 0.0251(15) 0.0306(16) 0.0027(12) 0.0144(14) 0.0057(13) C25 0.067(2) 0.0377(19) 0.046(2) 0.0114(15) 0.0155(19) 0.0025(17) C31 0.0325(15) 0.0285(15) 0.0366(17) 0.0003(12) 0.0040(13) 0.0048(12) C32 0.064(2) 0.043(2) 0.0374(19) 0.0004(15) -0.0055(17) 0.0049(17) C33 0.069(2) 0.053(2) 0.052(2) 0.0200(18) -0.011(2) 0.0054(19) C34 0.051(2) 0.0309(18) 0.076(3) 0.0097(17) 0.0068(19) 0.0087(15) C35 0.057(2) 0.0326(18) 0.061(2) -0.0070(16) 0.0125(18) 0.0049(16) C36 0.0455(18) 0.0360(17) 0.0359(17) -0.0037(13) 0.0070(14) 0.0020(14) C41 0.0413(17) 0.0325(16) 0.0358(17) -0.0041(13) -0.0016(14) 0.0133(13) C42 0.0448(19) 0.049(2) 0.0408(19) -0.0097(15) -0.0035(15) 0.0124(16) C43 0.048(2) 0.065(3) 0.060(3) -0.026(2) -0.0122(19) 0.0177(18) C44 0.073(3) 0.056(2) 0.047(2) -0.0142(18) -0.023(2) 0.030(2) C45 0.090(3) 0.045(2) 0.041(2) 0.0021(16) -0.011(2) 0.020(2) C46 0.059(2) 0.0387(19) 0.0426(19) -0.0005(15) -0.0042(17) 0.0119(16) C51 0.0395(16) 0.0377(17) 0.0286(15) 0.0013(12) 0.0037(13) 0.0008(13) C52 0.050(2) 0.049(2) 0.0370(18) -0.0051(15) 0.0087(15) -0.0010(16) C53 0.050(2) 0.072(3) 0.052(2) -0.002(2) 0.0195(18) 0.000(2) C54 0.049(2) 0.079(3) 0.055(3) 0.005(2) 0.0109(19) -0.019(2) C55 0.067(3) 0.054(2) 0.066(3) -0.006(2) 0.012(2) -0.020(2) C56 0.053(2) 0.045(2) 0.054(2) -0.0069(16) 0.0103(18) -0.0008(16) C61 0.0307(14) 0.0234(14) 0.0328(15) 0.0020(11) 0.0004(12) 0.0023(11) C62 0.0381(17) 0.0350(17) 0.0454(19) -0.0078(14) 0.0042(14) 0.0009(13) C63 0.045(2) 0.051(2) 0.055(2) -0.0022(17) 0.0167(17) 0.0093(16) C64 0.0302(17) 0.058(2) 0.075(3) 0.015(2) 0.0062(17) 0.0035(16) C65 0.0330(18) 0.072(3) 0.056(2) 0.0056(19) -0.0106(17) -0.0042(17) C66 0.0386(17) 0.052(2) 0.0388(18) -0.0016(15) -0.0028(14) -0.0016(15) C71 0.0279(14) 0.0291(15) 0.0362(16) -0.0010(12) -0.0019(12) 0.0016(11) C72 0.0383(17) 0.0286(16) 0.0476(19) -0.0034(13) 0.0046(14) 0.0011(13) C73 0.052(2) 0.0259(17) 0.063(2) -0.0038(15) 0.0009(18) -0.0005(14) C74 0.049(2) 0.033(2) 0.077(3) 0.0122(17) 0.002(2) -0.0102(15) C75 0.047(2) 0.048(2) 0.058(2) 0.0074(17) 0.0152(17) -0.0067(16) C76 0.0386(18) 0.0372(19) 0.052(2) 0.0001(14) 0.0051(15) 0.0008(14) C81 0.0308(15) 0.0332(16) 0.0348(16) -0.0058(12) -0.0002(12) 0.0059(12) C82 0.0392(17) 0.0435(19) 0.0381(18) 0.0012(14) 0.0021(14) 0.0044(14) C83 0.054(2) 0.062(2) 0.0369(19) 0.0075(16) 0.0040(16) 0.0133(18) C84 0.052(2) 0.082(3) 0.039(2) -0.0013(19) -0.0097(17) 0.018(2) C85 0.064(3) 0.077(3) 0.071(3) -0.009(2) -0.032(2) -0.013(2) C86 0.060(2) 0.047(2) 0.064(3) 0.0016(18) -0.023(2) -0.0084(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O3 2.2702(19) . ? Tb1 O6 2.2788(19) . ? Tb1 O21 2.337(2) . ? Tb1 O11 2.3391(19) . ? Tb1 O2 2.405(2) . ? Tb1 O1 2.4053(19) . ? Tb1 O22 2.414(2) . ? Tb1 O12 2.421(2) . ? P3 O3 1.502(2) . ? P3 C31 1.794(3) . ? P3 C51 1.795(3) . ? P3 C41 1.800(3) . ? P6 O6 1.499(2) . ? P6 C61 1.791(3) . ? P6 C71 1.796(3) . ? P6 C81 1.800(3) . ? F1 C1 1.333(4) . ? F2 C1 1.322(5) . ? F3 C1 1.317(5) . ? F4 C3 1.376(4) . ? F5 C5 1.310(5) . ? F6 C5 1.308(5) . ? F7 C5 1.302(4) . ? F11 C11 1.289(5) . ? F12 C11 1.309(5) . ? F13 C11 1.278(4) . ? F14 C13 1.364(4) . ? F15 C15 1.326(4) . ? F16 C15 1.309(4) . ? F17 C15 1.291(4) . ? F21 C21 1.296(5) . ? F22 C21 1.293(5) . ? F23 C21 1.322(4) . ? F24 C23 1.367(3) . ? F25 C25 1.316(4) . ? F26 C25 1.313(4) . ? F27 C25 1.292(4) . ? O1 C2 1.250(4) . ? O2 C4 1.255(3) . ? O11 C12 1.262(3) . ? O12 C14 1.240(3) . ? O21 C22 1.247(4) . ? O22 C24 1.249(4) . ? C1 C2 1.529(4) . ? C2 C3 1.389(4) . ? C3 C4 1.376(4) . ? C4 C5 1.550(5) . ? C11 C12 1.533(5) . ? C12 C13 1.381(5) . ? C13 C14 1.398(5) . ? C14 C15 1.541(5) . ? C21 C22 1.548(5) . ? C22 C23 1.385(4) . ? C23 C24 1.387(4) . ? C24 C25 1.545(4) . ? C31 C32 1.384(4) . ? C31 C36 1.391(4) . ? C32 C33 1.391(5) . ? C33 C34 1.386(5) . ? C34 C35 1.371(5) . ? C35 C36 1.381(4) . ? C41 C46 1.385(5) . ? C41 C42 1.393(5) . ? C42 C43 1.385(5) . ? C43 C44 1.372(6) . ? C44 C45 1.373(6) . ? C45 C46 1.388(5) . ? C51 C52 1.387(4) . ? C51 C56 1.397(4) . ? C52 C53 1.380(5) . ? C53 C54 1.369(5) . ? C54 C55 1.385(6) . ? C55 C56 1.387(5) . ? C61 C66 1.389(4) . ? C61 C62 1.390(4) . ? C62 C63 1.384(4) . ? C63 C64 1.374(5) . ? C64 C65 1.374(5) . ? C65 C66 1.399(5) . ? C71 C72 1.392(4) . ? C71 C76 1.393(4) . ? C72 C73 1.380(4) . ? C73 C74 1.373(5) . ? C74 C75 1.388(5) . ? C75 C76 1.394(5) . ? C81 C86 1.386(4) . ? C81 C82 1.389(4) . ? C82 C83 1.384(4) . ? C83 C84 1.362(5) . ? C84 C85 1.366(6) . ? C85 C86 1.386(5) . ? 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 Tb1 O6 142.49(7) . . ? O3 Tb1 O21 106.27(7) . . ? O6 Tb1 O21 84.38(7) . . ? O3 Tb1 O11 82.87(7) . . ? O6 Tb1 O11 108.40(7) . . ? O21 Tb1 O11 146.16(7) . . ? O3 Tb1 O2 142.03(7) . . ? O6 Tb1 O2 74.77(7) . . ? O21 Tb1 O2 78.61(7) . . ? O11 Tb1 O2 75.08(7) . . ? O3 Tb1 O1 73.89(7) . . ? O6 Tb1 O1 142.69(7) . . ? O21 Tb1 O1 73.81(7) . . ? O11 Tb1 O1 77.89(7) . . ? O2 Tb1 O1 71.52(7) . . ? O3 Tb1 O22 73.79(7) . . ? O6 Tb1 O22 76.17(7) . . ? O21 Tb1 O22 71.17(7) . . ? O11 Tb1 O22 141.54(7) . . ? O2 Tb1 O22 139.62(7) . . ? O1 Tb1 O22 122.25(7) . . ? O3 Tb1 O12 78.52(7) . . ? O6 Tb1 O12 72.26(7) . . ? O21 Tb1 O12 142.33(7) . . ? O11 Tb1 O12 70.90(7) . . ? O2 Tb1 O12 120.90(7) . . ? O1 Tb1 O12 140.39(7) . . ? O22 Tb1 O12 74.73(7) . . ? O3 P3 C31 110.09(13) . . ? O3 P3 C51 109.34(13) . . ? C31 P3 C51 109.01(14) . . ? O3 P3 C41 112.67(13) . . ? C31 P3 C41 106.94(14) . . ? C51 P3 C41 108.70(15) . . ? O6 P6 C61 109.40(13) . . ? O6 P6 C71 110.01(13) . . ? C61 P6 C71 109.14(13) . . ? O6 P6 C81 112.59(12) . . ? C61 P6 C81 108.22(13) . . ? C71 P6 C81 107.39(14) . . ? C2 O1 Tb1 135.89(19) . . ? C4 O2 Tb1 135.6(2) . . ? P3 O3 Tb1 151.48(13) . . ? P6 O6 Tb1 150.78(12) . . ? C12 O11 Tb1 138.1(2) . . ? C14 O12 Tb1 136.5(2) . . ? C22 O21 Tb1 138.0(2) . . ? C24 O22 Tb1 135.7(2) . . ? F3 C1 F2 107.3(4) . . ? F3 C1 F1 107.0(3) . . ? F2 C1 F1 106.5(3) . . ? F3 C1 C2 113.2(3) . . ? F2 C1 C2 111.0(3) . . ? F1 C1 C2 111.5(3) . . ? O1 C2 C3 125.6(3) . . ? O1 C2 C1 116.3(3) . . ? C3 C2 C1 118.1(3) . . ? C4 C3 F4 117.6(3) . . ? C4 C3 C2 124.9(3) . . ? F4 C3 C2 117.5(3) . . ? O2 C4 C3 126.0(3) . . ? O2 C4 C5 114.9(3) . . ? C3 C4 C5 119.1(3) . . ? F7 C5 F6 106.9(4) . . ? F7 C5 F5 105.5(3) . . ? F6 C5 F5 107.7(4) . . ? F7 C5 C4 112.7(3) . . ? F6 C5 C4 112.3(3) . . ? F5 C5 C4 111.4(3) . . ? F13 C11 F11 106.9(4) . . ? F13 C11 F12 105.9(4) . . ? F11 C11 F12 104.1(4) . . ? F13 C11 C12 115.0(3) . . ? F11 C11 C12 112.0(3) . . ? F12 C11 C12 112.3(3) . . ? O11 C12 C13 125.3(3) . . ? O11 C12 C11 115.1(3) . . ? C13 C12 C11 119.6(3) . . ? F14 C13 C12 118.7(3) . . ? F14 C13 C14 117.3(3) . . ? C12 C13 C14 124.0(3) . . ? O12 C14 C13 124.8(3) . . ? O12 C14 C15 115.7(3) . . ? C13 C14 C15 119.4(3) . . ? F17 C15 F16 109.8(4) . . ? F17 C15 F15 105.3(3) . . ? F16 C15 F15 105.4(3) . . ? F17 C15 C14 111.9(3) . . ? F16 C15 C14 111.5(3) . . ? F15 C15 C14 112.5(3) . . ? F22 C21 F21 109.5(4) . . ? F22 C21 F23 106.7(3) . . ? F21 C21 F23 105.5(4) . . ? F22 C21 C22 113.2(3) . . ? F21 C21 C22 111.5(3) . . ? F23 C21 C22 109.9(3) . . ? O21 C22 C23 125.8(3) . . ? O21 C22 C21 115.5(3) . . ? C23 C22 C21 118.6(3) . . ? F24 C23 C22 118.4(3) . . ? F24 C23 C24 118.0(3) . . ? C22 C23 C24 123.6(3) . . ? O22 C24 C23 125.4(3) . . ? O22 C24 C25 115.7(3) . . ? C23 C24 C25 118.9(3) . . ? F27 C25 F26 107.4(3) . . ? F27 C25 F25 108.0(4) . . ? F26 C25 F25 104.8(3) . . ? F27 C25 C24 112.1(3) . . ? F26 C25 C24 113.4(3) . . ? F25 C25 C24 110.8(3) . . ? C32 C31 C36 119.7(3) . . ? C32 C31 P3 118.3(2) . . ? C36 C31 P3 122.1(2) . . ? C31 C32 C33 120.2(3) . . ? C34 C33 C32 119.4(3) . . ? C35 C34 C33 120.4(3) . . ? C34 C35 C36 120.5(3) . . ? C35 C36 C31 119.8(3) . . ? C46 C41 C42 119.3(3) . . ? C46 C41 P3 123.0(3) . . ? C42 C41 P3 117.7(2) . . ? C43 C42 C41 120.0(4) . . ? C44 C43 C42 120.2(4) . . ? C43 C44 C45 120.3(3) . . ? C44 C45 C46 120.2(4) . . ? C41 C46 C45 120.1(4) . . ? C52 C51 C56 119.5(3) . . ? C52 C51 P3 122.6(3) . . ? C56 C51 P3 117.9(3) . . ? C53 C52 C51 120.2(3) . . ? C54 C53 C52 120.7(4) . . ? C53 C54 C55 119.8(4) . . ? C54 C55 C56 120.5(4) . . ? C55 C56 C51 119.4(4) . . ? C66 C61 C62 120.1(3) . . ? C66 C61 P6 117.0(2) . . ? C62 C61 P6 122.9(2) . . ? C63 C62 C61 119.5(3) . . ? C64 C63 C62 120.3(3) . . ? C65 C64 C63 120.7(3) . . ? C64 C65 C66 119.7(3) . . ? C61 C66 C65 119.5(3) . . ? C72 C71 C76 119.8(3) . . ? C72 C71 P6 121.9(2) . . ? C76 C71 P6 118.3(2) . . ? C73 C72 C71 120.1(3) . . ? C74 C73 C72 120.5(3) . . ? C73 C74 C75 120.0(3) . . ? C74 C75 C76 120.3(3) . . ? C71 C76 C75 119.3(3) . . ? C86 C81 C82 118.8(3) . . ? C86 C81 P6 122.7(3) . . ? C82 C81 P6 118.3(2) . . ? C83 C82 C81 120.2(3) . . ? C84 C83 C82 120.3(4) . . ? C83 C84 C85 120.2(3) . . ? C84 C85 C86 120.5(4) . . ? C85 C86 C81 120.0(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Tb1 O1 C2 157.0(3) . . . . ? O6 Tb1 O1 C2 -33.6(3) . . . . ? O21 Tb1 O1 C2 -90.3(3) . . . . ? O11 Tb1 O1 C2 71.0(3) . . . . ? O2 Tb1 O1 C2 -7.1(3) . . . . ? O22 Tb1 O1 C2 -144.8(3) . . . . ? O12 Tb1 O1 C2 109.3(3) . . . . ? O3 Tb1 O2 C4 -19.4(3) . . . . ? O6 Tb1 O2 C4 169.7(3) . . . . ? O21 Tb1 O2 C4 82.5(3) . . . . ? O11 Tb1 O2 C4 -76.0(3) . . . . ? O1 Tb1 O2 C4 6.0(3) . . . . ? O22 Tb1 O2 C4 124.4(3) . . . . ? O12 Tb1 O2 C4 -132.3(3) . . . . ? C31 P3 O3 Tb1 -114.6(3) . . . . ? C51 P3 O3 Tb1 125.7(3) . . . . ? C41 P3 O3 Tb1 4.7(3) . . . . ? O6 Tb1 O3 P3 -94.9(3) . . . . ? O21 Tb1 O3 P3 7.3(3) . . . . ? O11 Tb1 O3 P3 154.0(3) . . . . ? O2 Tb1 O3 P3 99.6(3) . . . . ? O1 Tb1 O3 P3 74.6(3) . . . . ? O22 Tb1 O3 P3 -56.9(3) . . . . ? O12 Tb1 O3 P3 -134.1(3) . . . . ? C61 P6 O6 Tb1 -99.3(3) . . . . ? C71 P6 O6 Tb1 140.8(2) . . . . ? C81 P6 O6 Tb1 21.1(3) . . . . ? O3 Tb1 O6 P6 -113.6(2) . . . . ? O21 Tb1 O6 P6 136.9(3) . . . . ? O11 Tb1 O6 P6 -11.0(3) . . . . ? O2 Tb1 O6 P6 57.2(2) . . . . ? O1 Tb1 O6 P6 83.1(3) . . . . ? O22 Tb1 O6 P6 -151.2(3) . . . . ? O12 Tb1 O6 P6 -73.0(3) . . . . ? O3 Tb1 O11 C12 72.4(3) . . . . ? O6 Tb1 O11 C12 -70.8(3) . . . . ? O21 Tb1 O11 C12 -178.9(3) . . . . ? O2 Tb1 O11 C12 -138.8(3) . . . . ? O1 Tb1 O11 C12 147.4(3) . . . . ? O22 Tb1 O11 C12 20.0(3) . . . . ? O12 Tb1 O11 C12 -7.9(3) . . . . ? O3 Tb1 O12 C14 -84.3(3) . . . . ? O6 Tb1 O12 C14 119.5(3) . . . . ? O21 Tb1 O12 C14 173.9(2) . . . . ? O11 Tb1 O12 C14 2.0(3) . . . . ? O2 Tb1 O12 C14 60.4(3) . . . . ? O1 Tb1 O12 C14 -37.9(3) . . . . ? O22 Tb1 O12 C14 -160.4(3) . . . . ? O3 Tb1 O21 C22 -70.6(3) . . . . ? O6 Tb1 O21 C22 72.7(3) . . . . ? O11 Tb1 O21 C22 -172.3(3) . . . . ? O2 Tb1 O21 C22 148.2(3) . . . . ? O1 Tb1 O21 C22 -137.9(3) . . . . ? O22 Tb1 O21 C22 -4.6(3) . . . . ? O12 Tb1 O21 C22 21.6(3) . . . . ? O3 Tb1 O22 C24 118.4(3) . . . . ? O6 Tb1 O22 C24 -84.3(3) . . . . ? O21 Tb1 O22 C24 4.4(3) . . . . ? O11 Tb1 O22 C24 173.4(2) . . . . ? O2 Tb1 O22 C24 -39.3(3) . . . . ? O1 Tb1 O22 C24 60.1(3) . . . . ? O12 Tb1 O22 C24 -159.3(3) . . . . ? Tb1 O1 C2 C3 5.4(5) . . . . ? Tb1 O1 C2 C1 -174.2(2) . . . . ? F3 C1 C2 O1 -128.2(3) . . . . ? F2 C1 C2 O1 111.1(4) . . . . ? F1 C1 C2 O1 -7.5(5) . . . . ? F3 C1 C2 C3 52.2(5) . . . . ? F2 C1 C2 C3 -68.6(5) . . . . ? F1 C1 C2 C3 172.8(3) . . . . ? O1 C2 C3 C4 1.8(6) . . . . ? C1 C2 C3 C4 -178.6(3) . . . . ? O1 C2 C3 F4 -178.5(3) . . . . ? C1 C2 C3 F4 1.1(5) . . . . ? Tb1 O2 C4 C3 -3.1(5) . . . . ? Tb1 O2 C4 C5 177.1(2) . . . . ? F4 C3 C4 O2 177.4(3) . . . . ? C2 C3 C4 O2 -2.9(6) . . . . ? F4 C3 C4 C5 -2.8(5) . . . . ? C2 C3 C4 C5 176.9(3) . . . . ? O2 C4 C5 F7 0.4(5) . . . . ? C3 C4 C5 F7 -179.4(3) . . . . ? O2 C4 C5 F6 121.2(4) . . . . ? C3 C4 C5 F6 -58.6(5) . . . . ? O2 C4 C5 F5 -117.9(4) . . . . ? C3 C4 C5 F5 62.3(5) . . . . ? Tb1 O11 C12 C13 9.2(5) . . . . ? Tb1 O11 C12 C11 -172.1(2) . . . . ? F13 C11 C12 O11 134.2(4) . . . . ? F11 C11 C12 O11 12.0(5) . . . . ? F12 C11 C12 O11 -104.6(4) . . . . ? F13 C11 C12 C13 -46.9(5) . . . . ? F11 C11 C12 C13 -169.1(4) . . . . ? F12 C11 C12 C13 74.2(5) . . . . ? O11 C12 C13 F14 176.8(3) . . . . ? C11 C12 C13 F14 -2.0(5) . . . . ? O11 C12 C13 C14 -1.4(5) . . . . ? C11 C12 C13 C14 179.9(3) . . . . ? Tb1 O12 C14 C13 2.2(5) . . . . ? Tb1 O12 C14 C15 -179.5(2) . . . . ? F14 C13 C14 O12 177.9(3) . . . . ? C12 C13 C14 O12 -3.9(5) . . . . ? F14 C13 C14 C15 -0.4(5) . . . . ? C12 C13 C14 C15 177.8(3) . . . . ? O12 C14 C15 F17 12.4(5) . . . . ? C13 C14 C15 F17 -169.1(3) . . . . ? O12 C14 C15 F16 -111.1(4) . . . . ? C13 C14 C15 F16 67.4(5) . . . . ? O12 C14 C15 F15 130.7(3) . . . . ? C13 C14 C15 F15 -50.8(4) . . . . ? Tb1 O21 C22 C23 4.4(5) . . . . ? Tb1 O21 C22 C21 -175.2(2) . . . . ? F22 C21 C22 O21 -123.7(4) . . . . ? F21 C21 C22 O21 0.4(5) . . . . ? F23 C21 C22 O21 117.1(4) . . . . ? F22 C21 C22 C23 56.7(4) . . . . ? F21 C21 C22 C23 -179.2(4) . . . . ? F23 C21 C22 C23 -62.5(4) . . . . ? O21 C22 C23 F24 178.9(3) . . . . ? C21 C22 C23 F24 -1.6(5) . . . . ? O21 C22 C23 C24 -1.1(5) . . . . ? C21 C22 C23 C24 178.5(3) . . . . ? Tb1 O22 C24 C23 -4.0(5) . . . . ? Tb1 O22 C24 C25 174.2(2) . . . . ? F24 C23 C24 O22 -178.9(3) . . . . ? C22 C23 C24 O22 1.1(5) . . . . ? F24 C23 C24 C25 2.9(4) . . . . ? C22 C23 C24 C25 -177.1(3) . . . . ? O22 C24 C25 F27 1.7(4) . . . . ? C23 C24 C25 F27 -180.0(3) . . . . ? O22 C24 C25 F26 123.5(3) . . . . ? C23 C24 C25 F26 -58.2(4) . . . . ? O22 C24 C25 F25 -118.9(4) . . . . ? C23 C24 C25 F25 59.4(4) . . . . ? O3 P3 C31 C32 -27.7(3) . . . . ? C51 P3 C31 C32 92.2(3) . . . . ? C41 P3 C31 C32 -150.4(3) . . . . ? O3 P3 C31 C36 152.1(2) . . . . ? C51 P3 C31 C36 -88.0(3) . . . . ? C41 P3 C31 C36 29.3(3) . . . . ? C36 C31 C32 C33 0.2(5) . . . . ? P3 C31 C32 C33 -180.0(3) . . . . ? C31 C32 C33 C34 0.7(6) . . . . ? C32 C33 C34 C35 -1.1(6) . . . . ? C33 C34 C35 C36 0.6(6) . . . . ? C34 C35 C36 C31 0.3(5) . . . . ? C32 C31 C36 C35 -0.8(5) . . . . ? P3 C31 C36 C35 179.5(2) . . . . ? O3 P3 C41 C46 116.5(3) . . . . ? C31 P3 C41 C46 -122.4(3) . . . . ? C51 P3 C41 C46 -4.8(3) . . . . ? O3 P3 C41 C42 -60.7(3) . . . . ? C31 P3 C41 C42 60.4(3) . . . . ? C51 P3 C41 C42 178.0(2) . . . . ? C46 C41 C42 C43 -0.5(5) . . . . ? P3 C41 C42 C43 176.8(3) . . . . ? C41 C42 C43 C44 0.0(5) . . . . ? C42 C43 C44 C45 0.7(6) . . . . ? C43 C44 C45 C46 -0.8(6) . . . . ? C42 C41 C46 C45 0.3(5) . . . . ? P3 C41 C46 C45 -176.8(3) . . . . ? C44 C45 C46 C41 0.3(5) . . . . ? O3 P3 C51 C52 153.9(3) . . . . ? C31 P3 C51 C52 33.5(3) . . . . ? C41 P3 C51 C52 -82.8(3) . . . . ? O3 P3 C51 C56 -24.6(3) . . . . ? C31 P3 C51 C56 -145.0(3) . . . . ? C41 P3 C51 C56 98.8(3) . . . . ? C56 C51 C52 C53 -0.3(5) . . . . ? P3 C51 C52 C53 -178.7(3) . . . . ? C51 C52 C53 C54 0.9(6) . . . . ? C52 C53 C54 C55 -0.8(6) . . . . ? C53 C54 C55 C56 0.0(7) . . . . ? C54 C55 C56 C51 0.6(6) . . . . ? C52 C51 C56 C55 -0.5(5) . . . . ? P3 C51 C56 C55 178.0(3) . . . . ? O6 P6 C61 C66 -23.5(3) . . . . ? C71 P6 C61 C66 96.9(3) . . . . ? C81 P6 C61 C66 -146.5(2) . . . . ? O6 P6 C61 C62 156.2(2) . . . . ? C71 P6 C61 C62 -83.4(3) . . . . ? C81 P6 C61 C62 33.2(3) . . . . ? C66 C61 C62 C63 -0.8(5) . . . . ? P6 C61 C62 C63 179.5(2) . . . . ? C61 C62 C63 C64 1.0(5) . . . . ? C62 C63 C64 C65 -0.8(6) . . . . ? C63 C64 C65 C66 0.4(6) . . . . ? C62 C61 C66 C65 0.4(5) . . . . ? P6 C61 C66 C65 -179.9(3) . . . . ? C64 C65 C66 C61 -0.1(6) . . . . ? O6 P6 C71 C72 162.9(2) . . . . ? C61 P6 C71 C72 42.9(3) . . . . ? C81 P6 C71 C72 -74.3(3) . . . . ? O6 P6 C71 C76 -16.2(3) . . . . ? C61 P6 C71 C76 -136.2(2) . . . . ? C81 P6 C71 C76 106.7(2) . . . . ? C76 C71 C72 C73 -0.4(5) . . . . ? P6 C71 C72 C73 -179.4(2) . . . . ? C71 C72 C73 C74 1.5(5) . . . . ? C72 C73 C74 C75 -2.1(5) . . . . ? C73 C74 C75 C76 1.5(5) . . . . ? C72 C71 C76 C75 -0.2(4) . . . . ? P6 C71 C76 C75 178.9(2) . . . . ? C74 C75 C76 C71 -0.4(5) . . . . ? O6 P6 C81 C86 115.1(3) . . . . ? C61 P6 C81 C86 -123.9(3) . . . . ? C71 P6 C81 C86 -6.2(3) . . . . ? O6 P6 C81 C82 -60.2(3) . . . . ? C61 P6 C81 C82 60.8(3) . . . . ? C71 P6 C81 C82 178.5(2) . . . . ? C86 C81 C82 C83 0.6(5) . . . . ? P6 C81 C82 C83 176.1(2) . . . . ? C81 C82 C83 C84 -0.4(5) . . . . ? C82 C83 C84 C85 0.3(6) . . . . ? C83 C84 C85 C86 -0.6(7) . . . . ? C84 C85 C86 C81 0.8(7) . . . . ? C82 C81 C86 C85 -0.8(6) . . . . ? P6 C81 C86 C85 -176.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.988 _refine_diff_density_min -1.227 _refine_diff_density_rms 0.102 data_00063 _database_code_CSD 171067 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H20 Eu2 F20 N4 O8' _chemical_formula_weight 1344.50 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 Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y, -z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 22.2956(10) _cell_length_b 18.0122(8) _cell_length_c 21.9719(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 90.000(10) _cell_angle_gamma 90.000(10) _cell_volume 8823.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max .20 _exptl_crystal_size_mid .04 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5168 _exptl_absorpt_coefficient_mu 2.957 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55115 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 28.33 _reflns_number_total 10706 _reflns_number_gt 6749 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10706 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu -0.042522(9) 0.161498(13) 0.327466(9) 0.02293(6) Uani 1 1 d . . . Eu2 Eu 0.059696(9) 0.011724(13) 0.313474(10) 0.02726(6) Uani 1 1 d . . . F1 F 0.05001(9) 0.14027(13) 0.27983(9) 0.0238(5) Uani 1 1 d . . . F2 F 0.01731(10) 0.08637(14) 0.38687(11) 0.0324(6) Uani 1 1 d . . . F3 F -0.04136(9) 0.03261(13) 0.29179(10) 0.0244(5) Uani 1 1 d . . . F7 F 0.031(2) 0.4191(6) 0.2978(9) 0.123(10) Uani 0.50 1 d P . . F8 F 0.0508(5) 0.4254(7) 0.248(3) 0.142(9) Uani 0.50 1 d P . . F9 F 0.0286(15) 0.4264(6) 0.2060(11) 0.078(4) Uani 0.50 1 d P . . F11 F -0.17951(13) 0.32316(18) 0.43666(14) 0.0611(9) Uani 1 1 d . . . F12 F -0.13088(14) 0.42126(18) 0.41303(14) 0.0641(9) Uani 1 1 d . . . F13 F -0.12160(13) 0.37418(18) 0.50209(13) 0.0608(9) Uani 1 1 d . . . F14 F -0.01175(12) 0.40518(16) 0.45277(13) 0.0497(8) Uani 1 1 d . . . F15 F 0.09695(15) 0.4094(2) 0.39946(19) 0.0896(12) Uani 1 1 d . . . F16 F 0.13835(13) 0.3056(2) 0.38883(17) 0.0809(12) Uani 1 1 d . . . F17 F 0.10749(14) 0.3402(2) 0.47530(14) 0.0878(13) Uani 1 1 d . . . F31 F 0.21935(14) -0.1398(2) 0.39375(17) 0.0830(12) Uani 1 1 d . . . F32 F 0.16980(16) -0.2386(2) 0.37448(15) 0.0794(11) Uani 1 1 d . . . F33 F 0.17806(15) -0.19985(19) 0.46638(14) 0.0727(10) Uani 1 1 d . . . F34 F 0.06074(14) -0.23089(17) 0.44491(13) 0.0619(9) Uani 1 1 d . . . F35 F -0.04747(16) -0.1765(3) 0.49398(16) 0.1061(15) Uani 1 1 d . . . F36 F -0.10083(15) -0.1317(2) 0.42321(17) 0.0857(12) Uani 1 1 d . . . F37 F -0.05919(17) -0.2347(2) 0.4109(2) 0.1000(14) Uani 1 1 d . . . F41 F -0.024(3) -0.2454(9) 0.3017(10) 0.184(11) Uani 0.50 1 d P . . F42 F 0.0277(13) -0.2540(6) 0.2927(11) 0.094(4) Uani 0.50 1 d P . . F43 F 0.0555(8) -0.2522(8) 0.247(2) 0.139(6) Uani 0.50 1 d P . . O1 O -0.08891(13) 0.24708(17) 0.39744(13) 0.0321(8) Uani 1 1 d . . . O2 O 0.03494(12) 0.24187(18) 0.37699(13) 0.0319(8) Uani 1 1 d . . . O6 O -0.04142(12) 0.28230(16) 0.27951(12) 0.0286(7) Uani 1 1 d . . . O31 O 0.12029(14) -0.07003(19) 0.37419(14) 0.0408(9) Uani 1 1 d . . . O32 O -0.00434(14) -0.06885(18) 0.38233(14) 0.0402(9) Uani 1 1 d . . . O36 O 0.04693(15) -0.10926(19) 0.26998(15) 0.0438(9) Uani 1 1 d . . . N11 N -0.12093(17) 0.0937(2) 0.39306(16) 0.0352(10) Uani 1 1 d . . . N12 N -0.15231(15) 0.1772(2) 0.29549(16) 0.0324(10) Uani 1 1 d . . . N41 N 0.15206(16) 0.0792(2) 0.35450(18) 0.0369(10) Uani 1 1 d . . . N42 N 0.15846(17) -0.0101(2) 0.25533(18) 0.0423(11) Uani 1 1 d . . . C1 C -0.1278(2) 0.3566(3) 0.4433(2) 0.0448(14) Uani 1 1 d . . . C2 C -0.0755(2) 0.3083(3) 0.41949(18) 0.0328(11) Uani 1 1 d . . . C3 C -0.0177(2) 0.3379(3) 0.42493(19) 0.0326(11) Uani 1 1 d . . . C4 C 0.0341(2) 0.3026(3) 0.40464(19) 0.0304(11) Uani 1 1 d . . . C5 C 0.0945(2) 0.3402(3) 0.4171(2) 0.0419(13) Uani 1 1 d . . . C6 C 0.0000 0.3120(4) 0.2500 0.0275(15) Uani 1 2 d S . . C7 C 0.0000 0.3966(4) 0.2500 0.045(2) Uani 1 2 d S . . C12 C -0.1062(3) 0.0512(3) 0.4401(2) 0.0459(14) Uani 1 1 d . . . H12A H -0.0658 0.0414 0.4469 0.055 Uiso 1 1 calc R . . C13 C -0.1484(3) 0.0205(3) 0.4799(2) 0.0672(19) Uani 1 1 d . . . H13A H -0.1364 -0.0092 0.5123 0.081 Uiso 1 1 calc R . . C14 C -0.2074(3) 0.0355(4) 0.4699(3) 0.069(2) Uani 1 1 d . . . H14A H -0.2361 0.0158 0.4961 0.083 Uiso 1 1 calc R . . C15 C -0.2255(3) 0.0791(4) 0.4220(3) 0.0591(17) Uani 1 1 d . . . C16 C -0.1804(2) 0.1075(3) 0.3837(2) 0.0417(13) Uani 1 1 d . . . C17 C -0.2862(3) 0.0961(4) 0.4085(3) 0.079(2) Uani 1 1 d . . . H17A H -0.3160 0.0778 0.4340 0.095 Uiso 1 1 calc R . . C18 C -0.3023(3) 0.1367(4) 0.3612(3) 0.077(2) Uani 1 1 d . . . H18A H -0.3428 0.1456 0.3541 0.092 Uiso 1 1 calc R . . C19 C -0.2582(2) 0.1675(4) 0.3203(3) 0.0572(17) Uani 1 1 d . . . C20 C -0.19735(19) 0.1517(3) 0.3320(2) 0.0386(13) Uani 1 1 d . . . C21 C -0.2709(2) 0.2100(4) 0.2696(3) 0.066(2) Uani 1 1 d . . . H21A H -0.3107 0.2208 0.2602 0.079 Uiso 1 1 calc R . . C22 C -0.2263(2) 0.2367(3) 0.2329(2) 0.0562(17) Uani 1 1 d . . . H22A H -0.2351 0.2663 0.1993 0.067 Uiso 1 1 calc R . . C23 C -0.1674(2) 0.2183(3) 0.2472(2) 0.0392(13) Uani 1 1 d . . . H23A H -0.1369 0.2355 0.2220 0.047 Uiso 1 1 calc R . . C31 C 0.1712(3) -0.1770(4) 0.4092(3) 0.0573(16) Uani 1 1 d . . . C32 C 0.1136(2) -0.1316(3) 0.3997(2) 0.0395(13) Uani 1 1 d . . . C33 C 0.0601(2) -0.1623(3) 0.4175(2) 0.0429(13) Uani 1 1 d . . . C34 C 0.0043(2) -0.1294(3) 0.4089(2) 0.0398(13) Uani 1 1 d . . . C35 C -0.0512(3) -0.1682(3) 0.4350(3) 0.0515(15) Uani 1 1 d . . . C36 C 0.0000 -0.1392(4) 0.2500 0.045(2) Uani 1 2 d S . . C37 C 0.0000 -0.2237(5) 0.2500 0.067(3) Uani 1 2 d S . . C42 C 0.1493(2) 0.1254(3) 0.4017(2) 0.0455(14) Uani 1 1 d . . . H42A H 0.1116 0.1412 0.4144 0.055 Uiso 1 1 calc R . . C43 C 0.1996(2) 0.1518(3) 0.4335(3) 0.0570(17) Uani 1 1 d . . . H43A H 0.1953 0.1838 0.4664 0.068 Uiso 1 1 calc R . . C44 C 0.2541(3) 0.1292(4) 0.4148(3) 0.0603(17) Uani 1 1 d . . . H44A H 0.2879 0.1455 0.4357 0.072 Uiso 1 1 calc R . . C45 C 0.2612(2) 0.0821(3) 0.3650(3) 0.0527(16) Uani 1 1 d . . . C46 C 0.2072(2) 0.0574(3) 0.3355(2) 0.0440(14) Uani 1 1 d . . . C47 C 0.3163(3) 0.0565(5) 0.3406(3) 0.084(2) Uani 1 1 d . . . H47A H 0.3516 0.0703 0.3601 0.101 Uiso 1 1 calc R . . C48 C 0.3203(2) 0.0141(4) 0.2916(3) 0.079(2) Uani 1 1 d . . . H48A H 0.3579 -0.0001 0.2775 0.095 Uiso 1 1 calc R . . C49 C 0.2674(3) -0.0102(4) 0.2600(3) 0.067(2) Uani 1 1 d . . . C50 C 0.2108(2) 0.0117(3) 0.2832(2) 0.0443(14) Uani 1 1 d . . . C51 C 0.2682(3) -0.0553(4) 0.2084(3) 0.081(2) Uani 1 1 d . . . H51A H 0.3047 -0.0720 0.1930 0.097 Uiso 1 1 calc R . . C52 C 0.2165(3) -0.0749(4) 0.1804(3) 0.072(2) Uani 1 1 d . . . H52A H 0.2172 -0.1038 0.1454 0.086 Uiso 1 1 calc R . . C53 C 0.1611(2) -0.0505(3) 0.2055(2) 0.0512(15) Uani 1 1 d . . . H53A H 0.1255 -0.0636 0.1860 0.061 Uiso 1 1 calc R . . O60 O 0.05712(16) 0.5900(2) 0.1932(2) 0.0507(10) Uani 1 1 d . . . O61 O -0.04284(15) 0.5861(2) 0.18696(16) 0.0501(10) Uani 1 1 d . . . C60 C 0.0077(3) 0.5866(3) 0.1633(3) 0.0459(14) Uani 1 1 d . . . C61 C 0.0138(2) 0.5847(3) 0.0956(3) 0.0641(17) Uani 1 1 d . . . H61A H -0.0253 0.5822 0.0774 0.096 Uiso 1 1 calc R . . H61B H 0.0367 0.5418 0.0840 0.096 Uiso 1 1 calc R . . H61C H 0.0340 0.6288 0.0820 0.096 Uiso 1 1 calc R . . H60D H 0.051(3) 0.586(4) 0.230(3) 0.12(3) Uiso 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 0.02377(11) 0.02026(12) 0.02476(11) -0.00060(10) 0.00052(9) -0.00004(10) Eu2 0.02508(11) 0.02399(13) 0.03270(13) 0.00660(10) 0.00042(9) 0.00384(10) F1 0.0199(12) 0.0219(14) 0.0294(13) -0.0018(10) -0.0019(10) -0.0016(11) F2 0.0272(13) 0.0220(15) 0.0482(16) -0.0021(12) -0.0004(11) -0.0015(12) F3 0.0239(12) 0.0209(14) 0.0285(13) 0.0016(10) 0.0009(10) -0.0017(11) F7 0.26(3) 0.036(5) 0.069(7) 0.014(6) -0.066(10) -0.055(13) F8 0.062(6) 0.032(6) 0.33(3) -0.001(18) -0.004(16) -0.020(5) F9 0.127(13) 0.026(5) 0.082(7) 0.013(6) 0.055(7) 0.000(9) F11 0.0436(18) 0.061(2) 0.078(2) -0.0190(18) 0.0093(16) 0.0059(17) F12 0.077(2) 0.040(2) 0.075(2) 0.0071(18) 0.0016(18) 0.0218(18) F13 0.067(2) 0.070(3) 0.0455(19) -0.0219(17) 0.0142(15) 0.0093(18) F14 0.0615(19) 0.0325(19) 0.0552(19) -0.0170(15) 0.0025(15) -0.0033(16) F15 0.070(2) 0.046(3) 0.152(4) 0.018(2) -0.002(2) -0.025(2) F16 0.0427(19) 0.087(3) 0.113(3) -0.050(2) 0.0110(19) -0.0193(19) F17 0.074(2) 0.135(4) 0.054(2) -0.006(2) -0.0225(17) -0.048(2) F31 0.053(2) 0.085(3) 0.112(3) 0.043(2) 0.011(2) 0.034(2) F32 0.101(3) 0.062(3) 0.076(2) -0.003(2) 0.009(2) 0.050(2) F33 0.093(3) 0.066(3) 0.059(2) 0.0218(18) -0.0146(18) 0.034(2) F34 0.085(2) 0.036(2) 0.065(2) 0.0262(16) 0.0068(17) 0.0141(18) F35 0.092(3) 0.168(5) 0.059(2) 0.042(3) 0.030(2) -0.014(3) F36 0.067(2) 0.062(3) 0.128(3) 0.041(2) 0.037(2) 0.001(2) F37 0.099(3) 0.049(3) 0.153(4) -0.024(3) 0.043(3) -0.023(2) F41 0.41(4) 0.057(9) 0.081(12) 0.005(8) 0.07(2) -0.08(2) F42 0.188(13) 0.015(5) 0.079(11) 0.021(7) -0.022(9) 0.007(8) F43 0.162(12) 0.038(7) 0.218(19) -0.026(12) -0.019(15) 0.042(7) O1 0.0399(19) 0.027(2) 0.0293(17) -0.0070(15) 0.0037(14) -0.0017(16) O2 0.0340(18) 0.029(2) 0.0330(18) -0.0063(15) -0.0052(13) -0.0015(15) O6 0.0345(18) 0.0210(18) 0.0302(17) 0.0003(14) -0.0014(14) 0.0004(15) O31 0.045(2) 0.033(2) 0.044(2) 0.0160(17) -0.0021(16) 0.0101(17) O32 0.049(2) 0.029(2) 0.042(2) 0.0154(16) 0.0096(16) 0.0055(17) O36 0.061(2) 0.026(2) 0.045(2) 0.0020(16) 0.0091(18) 0.0072(19) N11 0.045(3) 0.026(3) 0.035(2) -0.0054(19) 0.0083(18) -0.005(2) N12 0.026(2) 0.036(3) 0.035(2) -0.0100(19) 0.0018(16) 0.0003(19) N41 0.024(2) 0.039(3) 0.047(3) 0.017(2) -0.0051(18) -0.0010(19) N42 0.039(2) 0.043(3) 0.045(3) 0.017(2) 0.0105(19) 0.011(2) C1 0.046(3) 0.040(4) 0.049(3) -0.007(3) 0.005(3) 0.009(3) C2 0.048(3) 0.029(3) 0.021(2) 0.002(2) -0.002(2) 0.005(2) C3 0.050(3) 0.020(3) 0.027(2) -0.005(2) -0.002(2) -0.003(3) C4 0.040(3) 0.029(3) 0.023(2) 0.000(2) -0.005(2) -0.007(2) C5 0.048(3) 0.036(3) 0.042(3) -0.007(3) 0.001(2) -0.014(3) C6 0.039(4) 0.020(4) 0.024(3) 0.000 -0.008(3) 0.000 C7 0.070(6) 0.026(5) 0.038(5) 0.000 0.005(4) 0.000 C12 0.067(4) 0.032(3) 0.039(3) -0.001(3) 0.016(3) 0.002(3) C13 0.103(5) 0.054(5) 0.045(4) 0.009(3) 0.029(3) -0.009(4) C14 0.088(5) 0.055(5) 0.064(4) -0.006(4) 0.045(4) -0.026(4) C15 0.062(4) 0.059(5) 0.056(4) -0.018(3) 0.027(3) -0.017(3) C16 0.038(3) 0.037(3) 0.051(3) -0.015(3) 0.019(2) -0.016(3) C17 0.050(4) 0.095(7) 0.092(6) -0.024(5) 0.036(4) -0.029(4) C18 0.035(4) 0.096(6) 0.100(6) -0.032(5) 0.016(4) -0.014(4) C19 0.026(3) 0.079(5) 0.066(4) -0.029(4) 0.000(3) -0.005(3) C20 0.027(3) 0.041(3) 0.047(3) -0.015(3) 0.009(2) -0.006(2) C21 0.027(3) 0.087(6) 0.083(5) -0.035(4) -0.012(3) 0.015(3) C22 0.047(3) 0.072(5) 0.050(4) -0.014(3) -0.013(3) 0.018(3) C23 0.036(3) 0.043(3) 0.040(3) -0.009(3) -0.011(2) 0.007(2) C31 0.078(4) 0.048(4) 0.046(4) 0.009(3) 0.006(3) 0.024(4) C32 0.054(3) 0.033(3) 0.032(3) 0.008(2) -0.001(2) 0.018(3) C33 0.060(3) 0.030(3) 0.039(3) 0.016(2) 0.001(2) 0.016(3) C34 0.060(4) 0.028(3) 0.031(3) 0.000(2) 0.010(2) 0.000(3) C35 0.066(4) 0.036(4) 0.052(3) 0.009(3) 0.019(3) 0.004(3) C36 0.087(7) 0.024(5) 0.024(4) 0.000 0.013(4) 0.000 C37 0.125(10) 0.029(6) 0.046(7) 0.000 0.005(6) 0.000 C42 0.047(3) 0.042(4) 0.048(3) 0.015(3) -0.016(3) -0.004(3) C43 0.049(4) 0.058(5) 0.064(4) 0.019(3) -0.024(3) -0.012(3) C44 0.050(4) 0.063(5) 0.068(4) 0.035(4) -0.025(3) -0.015(3) C45 0.025(3) 0.059(4) 0.074(4) 0.042(3) -0.010(3) -0.007(3) C46 0.038(3) 0.045(4) 0.050(3) 0.027(3) -0.003(2) -0.002(3) C47 0.029(3) 0.119(7) 0.102(6) 0.054(5) 0.003(4) 0.006(4) C48 0.020(3) 0.114(7) 0.102(5) 0.049(5) 0.008(3) 0.021(4) C49 0.044(4) 0.085(6) 0.073(4) 0.035(4) 0.023(3) 0.024(4) C50 0.026(3) 0.047(4) 0.059(3) 0.031(3) 0.008(2) 0.011(3) C51 0.046(4) 0.095(6) 0.100(6) 0.048(5) 0.036(4) 0.041(4) C52 0.072(5) 0.074(5) 0.070(4) 0.021(4) 0.038(4) 0.037(4) C53 0.052(3) 0.051(4) 0.051(4) 0.015(3) 0.010(3) 0.022(3) O60 0.037(2) 0.046(3) 0.069(3) 0.005(2) 0.000(2) -0.0026(18) O61 0.039(2) 0.045(3) 0.066(3) -0.0024(19) -0.0006(19) -0.0052(18) C60 0.057(4) 0.022(3) 0.059(4) 0.001(3) -0.003(3) 0.004(3) C61 0.075(4) 0.052(4) 0.065(4) -0.003(3) -0.001(3) -0.007(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 Eu1 F2 2.305(2) . ? Eu1 F1 2.345(2) . ? Eu1 F1 2.394(2) 7_556 ? Eu1 O1 2.410(3) . ? Eu1 O6 2.418(3) . ? Eu1 F3 2.450(2) . ? Eu1 O2 2.503(3) . ? Eu1 N12 2.562(3) . ? Eu1 N11 2.574(4) . ? Eu1 Eu2 3.5449(5) . ? Eu1 Eu1 3.8967(5) 7_556 ? Eu1 Eu2 4.1248(5) 7_556 ? Eu2 F2 2.302(2) . ? Eu2 F3 2.333(2) . ? Eu2 F3 2.379(2) 7_556 ? Eu2 O36 2.396(3) . ? Eu2 O31 2.403(3) . ? Eu2 F1 2.440(2) . ? Eu2 O32 2.536(3) . ? Eu2 N41 2.555(4) . ? Eu2 N42 2.576(4) . ? Eu2 Eu2 3.8556(6) 7_556 ? Eu2 Eu1 4.1249(5) 7_556 ? F1 Eu1 2.394(2) 7_556 ? F3 Eu2 2.379(2) 7_556 ? F7 F8 1.19(3) . ? F7 C7 1.322(13) . ? F7 F9 1.340(19) 7_556 ? F8 F9 1.04(2) . ? F8 C7 1.246(11) . ? F9 C7 1.276(10) . ? F9 F7 1.340(19) 7_556 ? F11 C1 1.309(6) . ? F12 C1 1.343(6) . ? F13 C1 1.338(5) . ? F14 C3 1.365(5) . ? F15 C5 1.308(6) . ? F16 C5 1.315(6) . ? F17 C5 1.311(5) . ? F31 C31 1.310(7) . ? F32 C31 1.347(6) . ? F33 C31 1.331(6) . ? F34 C33 1.375(5) . ? F35 C35 1.308(6) . ? F36 C35 1.312(6) . ? F37 C35 1.322(6) . ? F41 F42 1.18(3) . ? F41 F43 1.28(2) 7_556 ? F41 C37 1.313(17) . ? F42 F43 1.18(2) . ? F42 C37 1.249(13) . ? F43 F41 1.28(2) 7_556 ? F43 C37 1.341(17) . ? O1 C2 1.242(5) . ? O2 C4 1.252(5) . ? O6 C6 1.248(4) . ? O31 C32 1.251(5) . ? O32 C34 1.253(5) . ? O36 C36 1.257(4) . ? N11 C12 1.327(6) . ? N11 C16 1.365(6) . ? N12 C23 1.336(6) . ? N12 C20 1.365(5) . ? N41 C42 1.330(6) . ? N41 C46 1.356(6) . ? N42 C53 1.317(6) . ? N42 C50 1.375(6) . ? C1 C2 1.545(6) . ? C2 C3 1.399(6) . ? C3 C4 1.392(6) . ? C4 C5 1.531(6) . ? C6 O6 1.248(4) 7_556 ? C6 C7 1.525(9) . ? C7 F8 1.246(11) 7_556 ? C7 F9 1.276(10) 7_556 ? C7 F7 1.322(13) 7_556 ? C12 C13 1.399(7) . ? C13 C14 1.361(8) . ? C14 C15 1.374(8) . ? C15 C16 1.408(7) . ? C15 C17 1.419(8) . ? C16 C20 1.437(7) . ? C17 C18 1.320(9) . ? C18 C19 1.442(8) . ? C19 C21 1.381(8) . ? C19 C20 1.411(6) . ? C21 C22 1.368(7) . ? C22 C23 1.391(6) . ? C31 C32 1.536(7) . ? C32 C33 1.372(7) . ? C33 C34 1.389(6) . ? C34 C35 1.533(7) . ? C36 O36 1.257(4) 7_556 ? C36 C37 1.521(11) . ? C37 F42 1.249(13) 7_556 ? C37 F41 1.313(17) 7_556 ? C37 F43 1.341(17) 7_556 ? C42 C43 1.405(6) . ? C43 C44 1.346(7) . ? C44 C45 1.393(8) . ? C45 C47 1.417(8) . ? C45 C46 1.437(7) . ? C46 C50 1.417(7) . ? C47 C48 1.322(9) . ? C48 C49 1.438(9) . ? C49 C51 1.396(9) . ? C49 C50 1.415(7) . ? C51 C52 1.353(9) . ? C52 C53 1.422(7) . ? O60 C60 1.285(6) . ? O61 C60 1.240(6) . ? C60 C61 1.494(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 Eu1 F1 69.38(8) . . ? F2 Eu1 F1 120.27(8) . 7_556 ? F1 Eu1 F1 66.16(8) . 7_556 ? F2 Eu1 O1 105.22(9) . . ? F1 Eu1 O1 140.04(9) . . ? F1 Eu1 O1 134.45(9) 7_556 . ? F2 Eu1 O6 140.28(9) . . ? F1 Eu1 O6 86.75(9) . . ? F1 Eu1 O6 73.46(8) 7_556 . ? O1 Eu1 O6 72.95(10) . . ? F2 Eu1 F3 67.60(8) . . ? F1 Eu1 F3 72.15(7) . . ? F1 Eu1 F3 62.26(7) 7_556 . ? O1 Eu1 F3 144.54(9) . . ? O6 Eu1 F3 135.49(8) . . ? F2 Eu1 O2 72.18(9) . . ? F1 Eu1 O2 71.41(9) . . ? F1 Eu1 O2 124.66(8) 7_556 . ? O1 Eu1 O2 69.44(10) . . ? O6 Eu1 O2 70.24(10) . . ? F3 Eu1 O2 132.83(8) . . ? F2 Eu1 N12 140.61(11) . . ? F1 Eu1 N12 137.40(9) . . ? F1 Eu1 N12 71.40(9) 7_556 . ? O1 Eu1 N12 72.21(11) . . ? O6 Eu1 N12 77.93(11) . . ? F3 Eu1 N12 91.54(10) . . ? O2 Eu1 N12 135.62(11) . . ? F2 Eu1 N11 78.32(11) . . ? F1 Eu1 N11 140.38(11) . . ? F1 Eu1 N11 115.36(10) 7_556 . ? O1 Eu1 N11 69.80(11) . . ? O6 Eu1 N11 132.67(11) . . ? F3 Eu1 N11 74.75(10) . . ? O2 Eu1 N11 119.98(10) . . ? N12 Eu1 N11 63.70(12) . . ? F2 Eu1 Eu2 39.68(6) . . ? F1 Eu1 Eu2 43.24(6) . . ? F1 Eu1 Eu2 80.67(5) 7_556 . ? O1 Eu1 Eu2 144.87(7) . . ? O6 Eu1 Eu2 129.84(7) . . ? F3 Eu1 Eu2 40.93(5) . . ? O2 Eu1 Eu2 91.96(7) . . ? N12 Eu1 Eu2 132.41(8) . . ? N11 Eu1 Eu2 97.14(9) . . ? F2 Eu1 Eu1 102.30(6) . 7_556 ? F1 Eu1 Eu1 35.11(5) . 7_556 ? F1 Eu1 Eu1 34.27(5) 7_556 7_556 ? O1 Eu1 Eu1 140.00(7) . 7_556 ? O6 Eu1 Eu1 67.31(7) . 7_556 ? F3 Eu1 Eu1 73.47(5) . 7_556 ? O2 Eu1 Eu1 92.53(7) . 7_556 ? N12 Eu1 Eu1 103.02(8) . 7_556 ? N11 Eu1 Eu1 145.06(8) . 7_556 ? Eu2 Eu1 Eu1 67.134(10) . 7_556 ? F2 Eu1 Eu2 95.44(6) . 7_556 ? F1 Eu1 Eu2 68.89(5) . 7_556 ? F1 Eu1 Eu2 31.77(5) 7_556 7_556 ? O1 Eu1 Eu2 149.02(7) . 7_556 ? O6 Eu1 Eu2 105.21(7) . 7_556 ? F3 Eu1 Eu2 30.82(5) . 7_556 ? O2 Eu1 Eu2 140.25(7) . 7_556 ? N12 Eu1 Eu2 77.15(8) . 7_556 ? N11 Eu1 Eu2 92.71(8) . 7_556 ? Eu2 Eu1 Eu2 59.790(10) . 7_556 ? Eu1 Eu1 Eu2 52.357(8) 7_556 7_556 ? F2 Eu2 F3 69.67(8) . . ? F2 Eu2 F3 121.21(8) . 7_556 ? F3 Eu2 F3 67.05(9) . 7_556 ? F2 Eu2 O36 139.60(10) . . ? F3 Eu2 O36 87.16(10) . . ? F3 Eu2 O36 74.67(9) 7_556 . ? F2 Eu2 O31 101.53(10) . . ? F3 Eu2 O31 139.03(9) . . ? F3 Eu2 O31 137.17(9) 7_556 . ? O36 Eu2 O31 74.39(11) . . ? F2 Eu2 F1 67.77(8) . . ? F3 Eu2 F1 72.53(7) . . ? F3 Eu2 F1 62.62(7) 7_556 . ? O36 Eu2 F1 137.02(9) . . ? O31 Eu2 F1 143.08(10) . . ? F2 Eu2 O32 71.66(10) . . ? F3 Eu2 O32 70.76(9) . . ? F3 Eu2 O32 125.01(9) 7_556 . ? O36 Eu2 O32 69.56(11) . . ? O31 Eu2 O32 68.57(10) . . ? F1 Eu2 O32 132.36(9) . . ? F2 Eu2 N41 78.82(11) . . ? F3 Eu2 N41 140.67(11) . . ? F3 Eu2 N41 113.97(10) 7_556 . ? O36 Eu2 N41 131.97(12) . . ? O31 Eu2 N41 69.05(12) . . ? F1 Eu2 N41 74.15(10) . . ? O32 Eu2 N41 121.02(11) . . ? F2 Eu2 N42 141.95(12) . . ? F3 Eu2 N42 138.48(10) . . ? F3 Eu2 N42 71.87(10) 7_556 . ? O36 Eu2 N42 76.39(13) . . ? O31 Eu2 N42 72.60(11) . . ? F1 Eu2 N42 94.04(10) . . ? O32 Eu2 N42 133.59(12) . . ? N41 Eu2 N42 63.82(14) . . ? F2 Eu2 Eu1 39.73(6) . . ? F3 Eu2 Eu1 43.47(6) . . ? F3 Eu2 Eu1 81.57(5) 7_556 . ? O36 Eu2 Eu1 130.56(8) . . ? O31 Eu2 Eu1 141.23(8) . . ? F1 Eu2 Eu1 41.17(5) . . ? O32 Eu2 Eu1 91.25(7) . . ? N41 Eu2 Eu1 97.22(9) . . ? N42 Eu2 Eu1 135.15(9) . . ? F2 Eu2 Eu2 102.90(6) . 7_556 ? F3 Eu2 Eu2 35.48(5) . 7_556 ? F3 Eu2 Eu2 34.70(5) 7_556 7_556 ? O36 Eu2 Eu2 68.26(8) . 7_556 ? O31 Eu2 Eu2 142.17(8) . 7_556 ? F1 Eu2 Eu2 73.72(5) . 7_556 ? O32 Eu2 Eu2 92.46(7) . 7_556 ? N41 Eu2 Eu2 144.25(8) . 7_556 ? N42 Eu2 Eu2 103.38(9) . 7_556 ? Eu1 Eu2 Eu2 67.597(10) . 7_556 ? F2 Eu2 Eu1 96.07(6) . 7_556 ? F3 Eu2 Eu1 69.61(5) . 7_556 ? F3 Eu2 Eu1 31.86(6) 7_556 7_556 ? O36 Eu2 Eu1 106.52(8) . 7_556 ? O31 Eu2 Eu1 150.44(8) . 7_556 ? F1 Eu2 Eu1 31.10(5) . 7_556 ? O32 Eu2 Eu1 140.33(7) . 7_556 ? N41 Eu2 Eu1 91.64(8) . 7_556 ? N42 Eu2 Eu1 78.88(9) . 7_556 ? Eu1 Eu2 Eu1 60.508(10) . 7_556 ? Eu2 Eu2 Eu1 52.609(9) 7_556 7_556 ? Eu1 F1 Eu1 110.62(8) . 7_556 ? Eu1 F1 Eu2 95.59(8) . . ? Eu1 F1 Eu2 117.13(9) 7_556 . ? Eu2 F2 Eu1 100.59(9) . . ? Eu2 F3 Eu2 109.81(8) . 7_556 ? Eu2 F3 Eu1 95.60(8) . . ? Eu2 F3 Eu1 117.32(9) 7_556 . ? F8 F7 C7 59.2(10) . . ? F8 F7 F9 107.4(16) . 7_556 ? C7 F7 F9 57.3(7) . 7_556 ? F9 F8 F7 129.8(18) . . ? F9 F8 C7 67.2(11) . . ? F7 F8 C7 65.7(10) . . ? F8 F9 C7 64.1(11) . . ? F8 F9 F7 121.7(14) . 7_556 ? C7 F9 F7 60.7(6) . 7_556 ? F42 F41 F43 113(3) . 7_556 ? F42 F41 C37 59.9(13) . . ? F43 F41 C37 62.2(12) 7_556 . ? F41 F42 F43 130.6(19) . . ? F41 F42 C37 65.5(12) . . ? F43 F42 C37 66.9(9) . . ? F42 F43 F41 115(3) . 7_556 ? F42 F43 C37 58.9(12) . . ? F41 F43 C37 60.0(14) 7_556 . ? C2 O1 Eu1 135.5(3) . . ? C4 O2 Eu1 135.0(3) . . ? C6 O6 Eu1 128.2(3) . . ? C32 O31 Eu2 136.4(3) . . ? C34 O32 Eu2 133.6(3) . . ? C36 O36 Eu2 129.0(4) . . ? C12 N11 C16 117.6(4) . . ? C12 N11 Eu1 122.8(3) . . ? C16 N11 Eu1 119.3(3) . . ? C23 N12 C20 117.9(4) . . ? C23 N12 Eu1 121.3(3) . . ? C20 N12 Eu1 120.3(3) . . ? C42 N41 C46 117.5(4) . . ? C42 N41 Eu2 122.3(3) . . ? C46 N41 Eu2 119.0(4) . . ? C53 N42 C50 119.4(4) . . ? C53 N42 Eu2 122.3(4) . . ? C50 N42 Eu2 117.5(3) . . ? F11 C1 F13 107.8(4) . . ? F11 C1 F12 107.4(4) . . ? F13 C1 F12 106.1(4) . . ? F11 C1 C2 111.7(4) . . ? F13 C1 C2 112.5(4) . . ? F12 C1 C2 111.1(4) . . ? O1 C2 C3 126.4(4) . . ? O1 C2 C1 116.7(4) . . ? C3 C2 C1 116.9(4) . . ? F14 C3 C4 117.9(4) . . ? F14 C3 C2 117.7(4) . . ? C4 C3 C2 124.3(4) . . ? O2 C4 C3 124.5(4) . . ? O2 C4 C5 117.4(4) . . ? C3 C4 C5 118.1(4) . . ? F15 C5 F17 106.2(5) . . ? F15 C5 F16 106.3(4) . . ? F17 C5 F16 107.3(5) . . ? F15 C5 C4 113.9(5) . . ? F17 C5 C4 111.6(4) . . ? F16 C5 C4 111.1(4) . . ? O6 C6 O6 129.3(6) . 7_556 ? O6 C6 C7 115.3(3) . . ? O6 C6 C7 115.3(3) 7_556 . ? F8 C7 F8 130.9(14) 7_556 . ? F8 C7 F9 48.7(12) 7_556 7_556 ? F8 C7 F9 108.1(10) . 7_556 ? F8 C7 F9 108.1(10) 7_556 . ? F8 C7 F9 48.7(12) . . ? F9 C7 F9 130.3(12) 7_556 . ? F8 C7 F7 108.4(10) 7_556 . ? F8 C7 F7 55.1(11) . . ? F9 C7 F7 62.1(7) 7_556 . ? F9 C7 F7 102.1(7) . . ? F8 C7 F7 55.1(11) 7_556 7_556 ? F8 C7 F7 108.4(10) . 7_556 ? F9 C7 F7 102.1(7) 7_556 7_556 ? F9 C7 F7 62.1(7) . 7_556 ? F7 C7 F7 144.2(12) . 7_556 ? F8 C7 C6 114.6(7) 7_556 . ? F8 C7 C6 114.6(7) . . ? F9 C7 C6 114.9(6) 7_556 . ? F9 C7 C6 114.8(6) . . ? F7 C7 C6 107.9(6) . . ? F7 C7 C6 107.9(6) 7_556 . ? N11 C12 C13 123.3(5) . . ? C14 C13 C12 118.1(6) . . ? C13 C14 C15 121.4(5) . . ? C14 C15 C16 117.2(6) . . ? C14 C15 C17 124.3(6) . . ? C16 C15 C17 118.5(6) . . ? N11 C16 C15 122.5(5) . . ? N11 C16 C20 118.4(4) . . ? C15 C16 C20 119.1(5) . . ? C18 C17 C15 122.9(6) . . ? C17 C18 C19 121.3(6) . . ? C21 C19 C20 117.2(5) . . ? C21 C19 C18 125.2(5) . . ? C20 C19 C18 117.6(6) . . ? N12 C20 C19 122.2(5) . . ? N12 C20 C16 117.2(4) . . ? C19 C20 C16 120.6(5) . . ? C22 C21 C19 121.4(5) . . ? C21 C22 C23 118.0(5) . . ? N12 C23 C22 123.3(5) . . ? F31 C31 F33 108.0(5) . . ? F31 C31 F32 107.0(5) . . ? F33 C31 F32 106.4(5) . . ? F31 C31 C32 112.2(5) . . ? F33 C31 C32 112.9(5) . . ? F32 C31 C32 110.0(5) . . ? O31 C32 C33 126.0(5) . . ? O31 C32 C31 115.6(5) . . ? C33 C32 C31 118.3(5) . . ? C32 C33 F34 118.5(4) . . ? C32 C33 C34 124.6(5) . . ? F34 C33 C34 116.8(5) . . ? O32 C34 C33 124.9(5) . . ? O32 C34 C35 116.5(5) . . ? C33 C34 C35 118.6(5) . . ? F35 C35 F36 107.9(5) . . ? F35 C35 F37 107.6(5) . . ? F36 C35 F37 105.1(5) . . ? F35 C35 C34 111.8(5) . . ? F36 C35 C34 112.3(5) . . ? F37 C35 C34 111.8(5) . . ? O36 C36 O36 129.1(7) . 7_556 ? O36 C36 C37 115.4(4) . . ? O36 C36 C37 115.4(4) 7_556 . ? F42 C37 F42 128.1(14) . 7_556 ? F42 C37 F41 54.6(14) . . ? F42 C37 F41 108.6(10) 7_556 . ? F42 C37 F41 108.6(10) . 7_556 ? F42 C37 F41 54.6(14) 7_556 7_556 ? F41 C37 F41 145.4(19) . 7_556 ? F42 C37 F43 104.4(8) . 7_556 ? F42 C37 F43 54.2(10) 7_556 7_556 ? F41 C37 F43 57.8(10) . 7_556 ? F41 C37 F43 107.7(11) 7_556 7_556 ? F42 C37 F43 54.2(10) . . ? F42 C37 F43 104.4(8) 7_556 . ? F41 C37 F43 107.7(11) . . ? F41 C37 F43 57.8(10) 7_556 . ? F43 C37 F43 134.9(18) 7_556 . ? F42 C37 C36 116.0(7) . . ? F42 C37 C36 116.0(7) 7_556 . ? F41 C37 C36 107.3(10) . . ? F41 C37 C36 107.3(10) 7_556 . ? F43 C37 C36 112.5(9) 7_556 . ? F43 C37 C36 112.5(9) . . ? N41 C42 C43 124.2(5) . . ? C44 C43 C42 117.8(6) . . ? C43 C44 C45 121.8(5) . . ? C44 C45 C47 126.4(6) . . ? C44 C45 C46 116.5(5) . . ? C47 C45 C46 117.0(6) . . ? N41 C46 C50 118.0(4) . . ? N41 C46 C45 122.1(5) . . ? C50 C46 C45 119.9(5) . . ? C48 C47 C45 123.7(6) . . ? C47 C48 C49 120.8(6) . . ? C51 C49 C50 117.8(6) . . ? C51 C49 C48 123.9(6) . . ? C50 C49 C48 118.2(6) . . ? N42 C50 C49 121.1(6) . . ? N42 C50 C46 118.6(4) . . ? C49 C50 C46 120.3(5) . . ? C52 C51 C49 120.5(6) . . ? C51 C52 C53 119.1(6) . . ? N42 C53 C52 122.0(6) . . ? O61 C60 O60 124.5(5) . . ? O61 C60 C61 120.0(5) . . ? O60 C60 C61 115.5(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Eu1 Eu2 F2 118.47(12) . . . . ? F1 Eu1 Eu2 F2 -176.57(10) 7_556 . . . ? O1 Eu1 Eu2 F2 2.81(15) . . . . ? O6 Eu1 Eu2 F2 124.28(12) . . . . ? F3 Eu1 Eu2 F2 -118.62(12) . . . . ? O2 Eu1 Eu2 F2 58.61(11) . . . . ? N12 Eu1 Eu2 F2 -122.57(14) . . . . ? N11 Eu1 Eu2 F2 -61.93(12) . . . . ? Eu1 Eu1 Eu2 F2 150.53(9) 7_556 . . . ? Eu2 Eu1 Eu2 F2 -150.90(9) 7_556 . . . ? F2 Eu1 Eu2 F3 118.62(12) . . . . ? F1 Eu1 Eu2 F3 -122.91(11) . . . . ? F1 Eu1 Eu2 F3 -57.95(9) 7_556 . . . ? O1 Eu1 Eu2 F3 121.43(15) . . . . ? O6 Eu1 Eu2 F3 -117.10(11) . . . . ? O2 Eu1 Eu2 F3 177.23(10) . . . . ? N12 Eu1 Eu2 F3 -3.95(13) . . . . ? N11 Eu1 Eu2 F3 56.69(11) . . . . ? Eu1 Eu1 Eu2 F3 -90.85(8) 7_556 . . . ? Eu2 Eu1 Eu2 F3 -32.28(8) 7_556 . . . ? F2 Eu1 Eu2 F3 -176.01(10) . . . 7_556 ? F1 Eu1 Eu2 F3 -57.54(9) . . . 7_556 ? F1 Eu1 Eu2 F3 7.42(7) 7_556 . . 7_556 ? O1 Eu1 Eu2 F3 -173.20(14) . . . 7_556 ? O6 Eu1 Eu2 F3 -51.73(10) . . . 7_556 ? F3 Eu1 Eu2 F3 65.37(9) . . . 7_556 ? O2 Eu1 Eu2 F3 -117.40(9) . . . 7_556 ? N12 Eu1 Eu2 F3 61.42(12) . . . 7_556 ? N11 Eu1 Eu2 F3 122.06(10) . . . 7_556 ? Eu1 Eu1 Eu2 F3 -25.48(5) 7_556 . . 7_556 ? Eu2 Eu1 Eu2 F3 33.09(5) 7_556 . . 7_556 ? F2 Eu1 Eu2 O36 122.58(14) . . . . ? F1 Eu1 Eu2 O36 -118.95(13) . . . . ? F1 Eu1 Eu2 O36 -53.99(11) 7_556 . . . ? O1 Eu1 Eu2 O36 125.39(16) . . . . ? O6 Eu1 Eu2 O36 -113.14(13) . . . . ? F3 Eu1 Eu2 O36 3.96(13) . . . . ? O2 Eu1 Eu2 O36 -178.81(12) . . . . ? N12 Eu1 Eu2 O36 0.01(15) . . . . ? N11 Eu1 Eu2 O36 60.65(13) . . . . ? Eu1 Eu1 Eu2 O36 -86.90(10) 7_556 . . . ? Eu2 Eu1 Eu2 O36 -28.32(10) 7_556 . . . ? F2 Eu1 Eu2 O31 2.57(15) . . . . ? F1 Eu1 Eu2 O31 121.04(15) . . . . ? F1 Eu1 Eu2 O31 -174.00(14) 7_556 . . . ? O1 Eu1 Eu2 O31 5.37(18) . . . . ? O6 Eu1 Eu2 O31 126.85(15) . . . . ? F3 Eu1 Eu2 O31 -116.05(15) . . . . ? O2 Eu1 Eu2 O31 61.18(14) . . . . ? N12 Eu1 Eu2 O31 -120.00(17) . . . . ? N11 Eu1 Eu2 O31 -59.36(15) . . . . ? Eu1 Eu1 Eu2 O31 153.09(13) 7_556 . . . ? Eu2 Eu1 Eu2 O31 -148.34(13) 7_556 . . . ? F2 Eu1 Eu2 F1 -118.47(12) . . . . ? F1 Eu1 Eu2 F1 64.96(9) 7_556 . . . ? O1 Eu1 Eu2 F1 -115.67(14) . . . . ? O6 Eu1 Eu2 F1 5.81(11) . . . . ? F3 Eu1 Eu2 F1 122.91(11) . . . . ? O2 Eu1 Eu2 F1 -59.86(10) . . . . ? N12 Eu1 Eu2 F1 118.95(14) . . . . ? N11 Eu1 Eu2 F1 179.60(11) . . . . ? Eu1 Eu1 Eu2 F1 32.05(7) 7_556 . . . ? Eu2 Eu1 Eu2 F1 90.62(7) 7_556 . . . ? F2 Eu1 Eu2 O32 58.76(12) . . . . ? F1 Eu1 Eu2 O32 177.23(10) . . . . ? F1 Eu1 Eu2 O32 -117.81(9) 7_556 . . . ? O1 Eu1 Eu2 O32 61.56(15) . . . . ? O6 Eu1 Eu2 O32 -176.96(11) . . . . ? F3 Eu1 Eu2 O32 -59.86(10) . . . . ? O2 Eu1 Eu2 O32 117.37(10) . . . . ? N12 Eu1 Eu2 O32 -63.81(13) . . . . ? N11 Eu1 Eu2 O32 -3.17(11) . . . . ? Eu1 Eu1 Eu2 O32 -150.72(7) 7_556 . . . ? Eu2 Eu1 Eu2 O32 -92.15(7) 7_556 . . . ? F2 Eu1 Eu2 N41 -62.73(12) . . . . ? F1 Eu1 Eu2 N41 55.75(11) . . . . ? F1 Eu1 Eu2 N41 120.70(10) 7_556 . . . ? O1 Eu1 Eu2 N41 -59.92(15) . . . . ? O6 Eu1 Eu2 N41 61.56(12) . . . . ? F3 Eu1 Eu2 N41 178.65(11) . . . . ? O2 Eu1 Eu2 N41 -4.12(11) . . . . ? N12 Eu1 Eu2 N41 174.70(14) . . . . ? N11 Eu1 Eu2 N41 -124.66(12) . . . . ? Eu1 Eu1 Eu2 N41 87.80(9) 7_556 . . . ? Eu2 Eu1 Eu2 N41 146.37(9) 7_556 . . . ? F2 Eu1 Eu2 N42 -122.51(17) . . . . ? F1 Eu1 Eu2 N42 -4.04(16) . . . . ? F1 Eu1 Eu2 N42 60.92(15) 7_556 . . . ? O1 Eu1 Eu2 N42 -119.70(19) . . . . ? O6 Eu1 Eu2 N42 1.77(16) . . . . ? F3 Eu1 Eu2 N42 118.87(16) . . . . ? O2 Eu1 Eu2 N42 -63.90(16) . . . . ? N12 Eu1 Eu2 N42 114.92(18) . . . . ? N11 Eu1 Eu2 N42 175.56(16) . . . . ? Eu1 Eu1 Eu2 N42 28.02(14) 7_556 . . . ? Eu2 Eu1 Eu2 N42 86.59(14) 7_556 . . . ? F2 Eu1 Eu2 Eu2 150.90(9) . . . 7_556 ? F1 Eu1 Eu2 Eu2 -90.62(7) . . . 7_556 ? F1 Eu1 Eu2 Eu2 -25.67(5) 7_556 . . 7_556 ? O1 Eu1 Eu2 Eu2 153.71(13) . . . 7_556 ? O6 Eu1 Eu2 Eu2 -84.81(9) . . . 7_556 ? F3 Eu1 Eu2 Eu2 32.28(8) . . . 7_556 ? O2 Eu1 Eu2 Eu2 -150.48(7) . . . 7_556 ? N12 Eu1 Eu2 Eu2 28.33(11) . . . 7_556 ? N11 Eu1 Eu2 Eu2 88.98(8) . . . 7_556 ? Eu1 Eu1 Eu2 Eu2 -58.571(8) 7_556 . . 7_556 ? F2 Eu1 Eu2 Eu1 -150.53(9) . . . 7_556 ? F1 Eu1 Eu2 Eu1 -32.05(7) . . . 7_556 ? F1 Eu1 Eu2 Eu1 32.91(5) 7_556 . . 7_556 ? O1 Eu1 Eu2 Eu1 -147.72(13) . . . 7_556 ? O6 Eu1 Eu2 Eu1 -26.24(9) . . . 7_556 ? F3 Eu1 Eu2 Eu1 90.85(8) . . . 7_556 ? O2 Eu1 Eu2 Eu1 -91.91(7) . . . 7_556 ? N12 Eu1 Eu2 Eu1 86.90(11) . . . 7_556 ? N11 Eu1 Eu2 Eu1 147.55(8) . . . 7_556 ? Eu2 Eu1 Eu2 Eu1 58.571(8) 7_556 . . 7_556 ? F2 Eu1 F1 Eu1 158.60(12) . . . 7_556 ? F1 Eu1 F1 Eu1 19.56(11) 7_556 . . 7_556 ? O1 Eu1 F1 Eu1 -112.10(13) . . . 7_556 ? O6 Eu1 F1 Eu1 -53.77(10) . . . 7_556 ? F3 Eu1 F1 Eu1 86.46(9) . . . 7_556 ? O2 Eu1 F1 Eu1 -124.01(12) . . . 7_556 ? N12 Eu1 F1 Eu1 14.43(19) . . . 7_556 ? N11 Eu1 F1 Eu1 121.13(15) . . . 7_556 ? Eu2 Eu1 F1 Eu1 121.76(12) . . . 7_556 ? Eu2 Eu1 F1 Eu1 53.90(7) 7_556 . . 7_556 ? F2 Eu1 F1 Eu2 36.84(7) . . . . ? F1 Eu1 F1 Eu2 -102.20(5) 7_556 . . . ? O1 Eu1 F1 Eu2 126.14(13) . . . . ? O6 Eu1 F1 Eu2 -175.53(8) . . . . ? F3 Eu1 F1 Eu2 -35.30(7) . . . . ? O2 Eu1 F1 Eu2 114.23(10) . . . . ? N12 Eu1 F1 Eu2 -107.33(15) . . . . ? N11 Eu1 F1 Eu2 -0.63(17) . . . . ? Eu1 Eu1 F1 Eu2 -121.76(12) 7_556 . . . ? Eu2 Eu1 F1 Eu2 -67.86(5) 7_556 . . . ? F2 Eu2 F1 Eu1 -37.37(7) . . . . ? F3 Eu2 F1 Eu1 37.27(7) . . . . ? F3 Eu2 F1 Eu1 109.97(9) 7_556 . . . ? O36 Eu2 F1 Eu1 102.82(13) . . . . ? O31 Eu2 F1 Eu1 -116.74(14) . . . . ? O32 Eu2 F1 Eu1 -3.75(14) . . . . ? N41 Eu2 F1 Eu1 -121.53(12) . . . . ? N42 Eu2 F1 Eu1 177.15(11) . . . . ? Eu2 Eu2 F1 Eu1 74.38(5) 7_556 . . . ? Eu1 Eu2 F1 Eu1 116.59(11) 7_556 . . . ? F2 Eu2 F1 Eu1 -153.97(11) . . . 7_556 ? F3 Eu2 F1 Eu1 -79.33(9) . . . 7_556 ? F3 Eu2 F1 Eu1 -6.63(8) 7_556 . . 7_556 ? O36 Eu2 F1 Eu1 -13.77(17) . . . 7_556 ? O31 Eu2 F1 Eu1 126.67(14) . . . 7_556 ? O32 Eu2 F1 Eu1 -120.34(12) . . . 7_556 ? N41 Eu2 F1 Eu1 121.88(13) . . . 7_556 ? N42 Eu2 F1 Eu1 60.55(13) . . . 7_556 ? Eu1 Eu2 F1 Eu1 -116.59(11) . . . 7_556 ? Eu2 Eu2 F1 Eu1 -42.21(7) 7_556 . . 7_556 ? F3 Eu2 F2 Eu1 -40.09(8) . . . . ? F3 Eu2 F2 Eu1 4.61(12) 7_556 . . . ? O36 Eu2 F2 Eu1 -98.97(16) . . . . ? O31 Eu2 F2 Eu1 -178.36(10) . . . . ? F1 Eu2 F2 Eu1 38.69(8) . . . . ? O32 Eu2 F2 Eu1 -115.78(11) . . . . ? N41 Eu2 F2 Eu1 115.99(11) . . . . ? N42 Eu2 F2 Eu1 105.21(16) . . . . ? Eu2 Eu2 F2 Eu1 -27.47(8) 7_556 . . . ? Eu1 Eu2 F2 Eu1 25.51(7) 7_556 . . . ? F1 Eu1 F2 Eu2 -40.05(8) . . . . ? F1 Eu1 F2 Eu2 3.92(12) 7_556 . . . ? O1 Eu1 F2 Eu2 -178.33(9) . . . . ? O6 Eu1 F2 Eu2 -96.84(14) . . . . ? F3 Eu1 F2 Eu2 38.46(8) . . . . ? O2 Eu1 F2 Eu2 -116.34(10) . . . . ? N12 Eu1 F2 Eu2 101.32(15) . . . . ? N11 Eu1 F2 Eu2 116.62(11) . . . . ? Eu1 Eu1 F2 Eu2 -27.65(8) 7_556 . . . ? Eu2 Eu1 F2 Eu2 24.97(7) 7_556 . . . ? F2 Eu2 F3 Eu2 158.46(12) . . . 7_556 ? F3 Eu2 F3 Eu2 19.26(11) 7_556 . . 7_556 ? O36 Eu2 F3 Eu2 -55.28(11) . . . 7_556 ? O31 Eu2 F3 Eu2 -117.38(14) . . . 7_556 ? F1 Eu2 F3 Eu2 86.30(9) . . . 7_556 ? O32 Eu2 F3 Eu2 -124.61(12) . . . 7_556 ? N41 Eu2 F3 Eu2 119.60(15) . . . 7_556 ? N42 Eu2 F3 Eu2 10.4(2) . . . 7_556 ? Eu1 Eu2 F3 Eu2 121.71(12) . . . 7_556 ? Eu1 Eu2 F3 Eu2 53.51(7) 7_556 . . 7_556 ? F2 Eu2 F3 Eu1 36.75(8) . . . . ? F3 Eu2 F3 Eu1 -102.44(5) 7_556 . . . ? O36 Eu2 F3 Eu1 -176.99(10) . . . . ? O31 Eu2 F3 Eu1 120.91(14) . . . . ? F1 Eu2 F3 Eu1 -35.41(7) . . . . ? O32 Eu2 F3 Eu1 113.69(10) . . . . ? N41 Eu2 F3 Eu1 -2.11(18) . . . . ? N42 Eu2 F3 Eu1 -111.28(16) . . . . ? Eu2 Eu2 F3 Eu1 -121.71(12) 7_556 . . . ? Eu1 Eu2 F3 Eu1 -68.20(5) 7_556 . . . ? F2 Eu1 F3 Eu2 -37.32(8) . . . . ? F1 Eu1 F3 Eu2 37.18(7) . . . . ? F1 Eu1 F3 Eu2 109.09(9) 7_556 . . . ? O1 Eu1 F3 Eu2 -122.20(14) . . . . ? O6 Eu1 F3 Eu2 102.81(12) . . . . ? O2 Eu1 F3 Eu2 -3.77(14) . . . . ? N12 Eu1 F3 Eu2 177.08(10) . . . . ? N11 Eu1 F3 Eu2 -120.74(11) . . . . ? Eu1 Eu1 F3 Eu2 73.96(6) 7_556 . . . ? Eu2 Eu1 F3 Eu2 115.72(12) 7_556 . . . ? F2 Eu1 F3 Eu2 -153.04(12) . . . 7_556 ? F1 Eu1 F3 Eu2 -78.55(9) . . . 7_556 ? F1 Eu1 F3 Eu2 -6.63(8) 7_556 . . 7_556 ? O1 Eu1 F3 Eu2 122.08(14) . . . 7_556 ? O6 Eu1 F3 Eu2 -12.91(16) . . . 7_556 ? O2 Eu1 F3 Eu2 -119.49(12) . . . 7_556 ? N12 Eu1 F3 Eu2 61.36(12) . . . 7_556 ? N11 Eu1 F3 Eu2 123.54(13) . . . 7_556 ? Eu2 Eu1 F3 Eu2 -115.72(12) . . . 7_556 ? Eu1 Eu1 F3 Eu2 -41.77(7) 7_556 . . 7_556 ? C7 F7 F8 F9 21.3(18) . . . . ? F9 F7 F8 F9 -11(2) 7_556 . . . ? F9 F7 F8 C7 -32.1(9) 7_556 . . . ? F7 F8 F9 C7 -21.1(18) . . . . ? F7 F8 F9 F7 -1(3) . . . 7_556 ? C7 F8 F9 F7 20.1(14) . . . 7_556 ? F43 F41 F42 F43 18(3) 7_556 . . . ? C37 F41 F42 F43 -16.4(18) . . . . ? F43 F41 F42 C37 34.4(14) 7_556 . . . ? F41 F42 F43 F41 -6(3) . . . 7_556 ? C37 F42 F43 F41 -22.3(16) . . . 7_556 ? F41 F42 F43 C37 16.2(17) . . . . ? F2 Eu1 O1 C2 87.8(4) . . . . ? F1 Eu1 O1 C2 11.9(5) . . . . ? F1 Eu1 O1 C2 -94.9(4) 7_556 . . . ? O6 Eu1 O1 C2 -50.9(4) . . . . ? F3 Eu1 O1 C2 160.4(4) . . . . ? O2 Eu1 O1 C2 23.9(4) . . . . ? N12 Eu1 O1 C2 -133.3(4) . . . . ? N11 Eu1 O1 C2 158.9(4) . . . . ? Eu2 Eu1 O1 C2 85.9(4) . . . . ? Eu1 Eu1 O1 C2 -44.1(5) 7_556 . . . ? Eu2 Eu1 O1 C2 -142.1(4) 7_556 . . . ? F2 Eu1 O2 C4 -133.4(4) . . . . ? F1 Eu1 O2 C4 152.9(4) . . . . ? F1 Eu1 O2 C4 111.6(4) 7_556 . . . ? O1 Eu1 O2 C4 -18.9(4) . . . . ? O6 Eu1 O2 C4 59.7(4) . . . . ? F3 Eu1 O2 C4 -165.9(4) . . . . ? N12 Eu1 O2 C4 12.9(5) . . . . ? N11 Eu1 O2 C4 -69.0(4) . . . . ? Eu2 Eu1 O2 C4 -168.4(4) . . . . ? Eu1 Eu1 O2 C4 124.4(4) 7_556 . . . ? Eu2 Eu1 O2 C4 149.9(3) 7_556 . . . ? F2 Eu1 O6 C6 44.4(3) . . . . ? F1 Eu1 O6 C6 -7.3(3) . . . . ? F1 Eu1 O6 C6 -73.4(3) 7_556 . . . ? O1 Eu1 O6 C6 137.8(3) . . . . ? F3 Eu1 O6 C6 -67.6(3) . . . . ? O2 Eu1 O6 C6 64.1(3) . . . . ? N12 Eu1 O6 C6 -147.3(3) . . . . ? N11 Eu1 O6 C6 177.1(2) . . . . ? Eu2 Eu1 O6 C6 -11.3(3) . . . . ? Eu1 Eu1 O6 C6 -37.5(3) 7_556 . . . ? Eu2 Eu1 O6 C6 -74.4(3) 7_556 . . . ? F2 Eu2 O31 C32 90.9(5) . . . . ? F3 Eu2 O31 C32 18.7(5) . . . . ? F3 Eu2 O31 C32 -92.9(5) 7_556 . . . ? O36 Eu2 O31 C32 -47.7(5) . . . . ? F1 Eu2 O31 C32 159.1(4) . . . . ? O32 Eu2 O31 C32 26.0(4) . . . . ? N41 Eu2 O31 C32 164.0(5) . . . . ? N42 Eu2 O31 C32 -128.0(5) . . . . ? Eu1 Eu2 O31 C32 89.2(5) . . . . ? Eu2 Eu2 O31 C32 -38.5(5) 7_556 . . . ? Eu1 Eu2 O31 C32 -143.8(4) 7_556 . . . ? F2 Eu2 O32 C34 -132.3(5) . . . . ? F3 Eu2 O32 C34 153.5(5) . . . . ? F3 Eu2 O32 C34 112.0(4) 7_556 . . . ? O36 Eu2 O32 C34 59.3(4) . . . . ? O31 Eu2 O32 C34 -21.4(4) . . . . ? F1 Eu2 O32 C34 -165.0(4) . . . . ? N41 Eu2 O32 C34 -68.2(5) . . . . ? N42 Eu2 O32 C34 13.8(5) . . . . ? Eu1 Eu2 O32 C34 -167.4(4) . . . . ? Eu2 Eu2 O32 C34 124.9(4) 7_556 . . . ? Eu1 Eu2 O32 C34 150.7(4) 7_556 . . . ? F2 Eu2 O36 C36 49.8(4) . . . . ? F3 Eu2 O36 C36 -3.7(3) . . . . ? F3 Eu2 O36 C36 -70.6(3) 7_556 . . . ? O31 Eu2 O36 C36 139.3(3) . . . . ? F1 Eu2 O36 C36 -64.1(3) . . . . ? O32 Eu2 O36 C36 66.8(3) . . . . ? N41 Eu2 O36 C36 -179.3(3) . . . . ? N42 Eu2 O36 C36 -145.2(3) . . . . ? Eu1 Eu2 O36 C36 -6.4(4) . . . . ? Eu2 Eu2 O36 C36 -34.6(3) 7_556 . . . ? Eu1 Eu2 O36 C36 -71.4(3) 7_556 . . . ? F2 Eu1 N11 C12 9.1(4) . . . . ? F1 Eu1 N11 C12 44.6(4) . . . . ? F1 Eu1 N11 C12 127.2(3) 7_556 . . . ? O1 Eu1 N11 C12 -102.1(4) . . . . ? O6 Eu1 N11 C12 -142.3(3) . . . . ? F3 Eu1 N11 C12 78.8(4) . . . . ? O2 Eu1 N11 C12 -52.2(4) . . . . ? N12 Eu1 N11 C12 178.3(4) . . . . ? Eu2 Eu1 N11 C12 44.2(4) . . . . ? Eu1 Eu1 N11 C12 103.9(4) 7_556 . . . ? Eu2 Eu1 N11 C12 104.1(4) 7_556 . . . ? F2 Eu1 N11 C16 -177.9(3) . . . . ? F1 Eu1 N11 C16 -142.3(3) . . . . ? F1 Eu1 N11 C16 -59.7(3) 7_556 . . . ? O1 Eu1 N11 C16 70.9(3) . . . . ? O6 Eu1 N11 C16 30.7(4) . . . . ? F3 Eu1 N11 C16 -108.2(3) . . . . ? O2 Eu1 N11 C16 120.8(3) . . . . ? N12 Eu1 N11 C16 -8.6(3) . . . . ? Eu2 Eu1 N11 C16 -142.8(3) . . . . ? Eu1 Eu1 N11 C16 -83.1(4) 7_556 . . . ? Eu2 Eu1 N11 C16 -82.9(3) 7_556 . . . ? F2 Eu1 N12 C23 -163.1(3) . . . . ? F1 Eu1 N12 C23 -42.8(4) . . . . ? F1 Eu1 N12 C23 -47.7(3) 7_556 . . . ? O1 Eu1 N12 C23 104.4(4) . . . . ? O6 Eu1 N12 C23 28.7(3) . . . . ? F3 Eu1 N12 C23 -107.7(3) . . . . ? O2 Eu1 N12 C23 73.2(4) . . . . ? N11 Eu1 N12 C23 -179.8(4) . . . . ? Eu2 Eu1 N12 C23 -105.1(3) . . . . ? Eu1 Eu1 N12 C23 -34.3(4) 7_556 . . . ? Eu2 Eu1 N12 C23 -80.2(3) 7_556 . . . ? F2 Eu1 N12 C20 25.5(4) . . . . ? F1 Eu1 N12 C20 145.9(3) . . . . ? F1 Eu1 N12 C20 140.9(4) 7_556 . . . ? O1 Eu1 N12 C20 -67.0(3) . . . . ? O6 Eu1 N12 C20 -142.7(4) . . . . ? F3 Eu1 N12 C20 80.9(3) . . . . ? O2 Eu1 N12 C20 -98.2(4) . . . . ? N11 Eu1 N12 C20 8.8(3) . . . . ? Eu2 Eu1 N12 C20 83.5(3) . . . . ? Eu1 Eu1 N12 C20 154.3(3) 7_556 . . . ? Eu2 Eu1 N12 C20 108.4(3) 7_556 . . . ? F2 Eu2 N41 C42 4.8(3) . . . . ? F3 Eu2 N41 C42 41.6(4) . . . . ? F3 Eu2 N41 C42 124.1(3) 7_556 . . . ? O36 Eu2 N41 C42 -145.3(3) . . . . ? O31 Eu2 N41 C42 -102.3(4) . . . . ? F1 Eu2 N41 C42 74.6(4) . . . . ? O32 Eu2 N41 C42 -55.7(4) . . . . ? N42 Eu2 N41 C42 177.4(4) . . . . ? Eu1 Eu2 N41 C42 40.2(4) . . . . ? Eu2 Eu2 N41 C42 101.4(4) 7_556 . . . ? Eu1 Eu2 N41 C42 100.6(4) 7_556 . . . ? F2 Eu2 N41 C46 172.2(3) . . . . ? F3 Eu2 N41 C46 -150.9(3) . . . . ? F3 Eu2 N41 C46 -68.4(3) 7_556 . . . ? O36 Eu2 N41 C46 22.2(4) . . . . ? O31 Eu2 N41 C46 65.2(3) . . . . ? F1 Eu2 N41 C46 -117.9(3) . . . . ? O32 Eu2 N41 C46 111.8(3) . . . . ? N42 Eu2 N41 C46 -15.1(3) . . . . ? Eu1 Eu2 N41 C46 -152.4(3) . . . . ? Eu2 Eu2 N41 C46 -91.2(3) 7_556 . . . ? Eu1 Eu2 N41 C46 -91.9(3) 7_556 . . . ? F2 Eu2 N42 C53 -164.8(3) . . . . ? F3 Eu2 N42 C53 -38.4(5) . . . . ? F3 Eu2 N42 C53 -47.0(4) 7_556 . . . ? O36 Eu2 N42 C53 31.1(4) . . . . ? O31 Eu2 N42 C53 108.7(4) . . . . ? F1 Eu2 N42 C53 -106.4(4) . . . . ? O32 Eu2 N42 C53 74.5(4) . . . . ? N41 Eu2 N42 C53 -176.6(4) . . . . ? Eu1 Eu2 N42 C53 -103.8(4) . . . . ? Eu2 Eu2 N42 C53 -32.2(4) 7_556 . . . ? Eu1 Eu2 N42 C53 -79.1(4) 7_556 . . . ? F2 Eu2 N42 C50 25.5(4) . . . . ? F3 Eu2 N42 C50 151.9(3) . . . . ? F3 Eu2 N42 C50 143.3(4) 7_556 . . . ? O36 Eu2 N42 C50 -138.6(4) . . . . ? O31 Eu2 N42 C50 -61.0(3) . . . . ? F1 Eu2 N42 C50 83.9(3) . . . . ? O32 Eu2 N42 C50 -95.2(4) . . . . ? N41 Eu2 N42 C50 13.7(3) . . . . ? Eu1 Eu2 N42 C50 86.5(3) . . . . ? Eu2 Eu2 N42 C50 158.1(3) 7_556 . . . ? Eu1 Eu2 N42 C50 111.2(3) 7_556 . . . ? Eu1 O1 C2 C3 -22.5(7) . . . . ? Eu1 O1 C2 C1 157.5(3) . . . . ? F11 C1 C2 O1 0.9(6) . . . . ? F13 C1 C2 O1 122.3(5) . . . . ? F12 C1 C2 O1 -119.0(5) . . . . ? F11 C1 C2 C3 -179.1(4) . . . . ? F13 C1 C2 C3 -57.7(6) . . . . ? F12 C1 C2 C3 61.1(6) . . . . ? O1 C2 C3 F14 -177.4(4) . . . . ? C1 C2 C3 F14 2.5(6) . . . . ? O1 C2 C3 C4 1.6(7) . . . . ? C1 C2 C3 C4 -178.5(4) . . . . ? Eu1 O2 C4 C3 12.2(7) . . . . ? Eu1 O2 C4 C5 -168.2(3) . . . . ? F14 C3 C4 O2 -178.0(4) . . . . ? C2 C3 C4 O2 3.0(7) . . . . ? F14 C3 C4 C5 2.4(6) . . . . ? C2 C3 C4 C5 -176.6(4) . . . . ? O2 C4 C5 F15 128.3(5) . . . . ? C3 C4 C5 F15 -52.0(6) . . . . ? O2 C4 C5 F17 -111.4(5) . . . . ? C3 C4 C5 F17 68.3(6) . . . . ? O2 C4 C5 F16 8.3(6) . . . . ? C3 C4 C5 F16 -172.0(4) . . . . ? Eu1 O6 C6 O6 26.54(17) . . . 7_556 ? Eu1 O6 C6 C7 -153.47(17) . . . . ? F9 F8 C7 F8 -77.7(11) . . . 7_556 ? F7 F8 C7 F8 84.7(8) . . . 7_556 ? F9 F8 C7 F9 -128.2(14) . . . 7_556 ? F7 F8 C7 F9 34.1(13) . . . 7_556 ? F7 F8 C7 F9 162.3(16) . . . . ? F9 F8 C7 F7 -162.3(16) . . . . ? F9 F8 C7 F7 -18.2(13) . . . 7_556 ? F7 F8 C7 F7 144.1(13) . . . 7_556 ? F9 F8 C7 C6 102.3(11) . . . . ? F7 F8 C7 C6 -95.3(8) . . . . ? F8 F9 C7 F8 129.0(17) . . . 7_556 ? F7 F9 C7 F8 -31.4(13) 7_556 . . 7_556 ? F7 F9 C7 F8 -160.4(14) 7_556 . . . ? F8 F9 C7 F9 78.3(10) . . . 7_556 ? F7 F9 C7 F9 -82.1(7) 7_556 . . 7_556 ? F8 F9 C7 F7 14.7(13) . . . . ? F7 F9 C7 F7 -145.6(12) 7_556 . . . ? F8 F9 C7 F7 160.4(14) . . . 7_556 ? F8 F9 C7 C6 -101.7(10) . . . . ? F7 F9 C7 C6 97.9(7) 7_556 . . . ? F8 F7 C7 F8 -127.5(15) . . . 7_556 ? F9 F7 C7 F8 15.4(11) 7_556 . . 7_556 ? F9 F7 C7 F8 142.9(13) 7_556 . . . ? F8 F7 C7 F9 -142.9(13) . . . 7_556 ? F8 F7 C7 F9 -13.5(13) . . . . ? F9 F7 C7 F9 129.4(12) 7_556 . . . ? F8 F7 C7 F7 -72.1(10) . . . 7_556 ? F9 F7 C7 F7 70.8(7) 7_556 . . 7_556 ? F8 F7 C7 C6 107.9(10) . . . . ? F9 F7 C7 C6 -109.2(7) 7_556 . . . ? O6 C6 C7 F8 -32(3) . . . 7_556 ? O6 C6 C7 F8 148(3) 7_556 . . 7_556 ? O6 C6 C7 F8 148(3) . . . . ? O6 C6 C7 F8 -32(3) 7_556 . . . ? O6 C6 C7 F9 22(2) . . . 7_556 ? O6 C6 C7 F9 -159(2) 7_556 . . 7_556 ? O6 C6 C7 F9 -158(2) . . . . ? O6 C6 C7 F9 22(2) 7_556 . . . ? O6 C6 C7 F7 88(2) . . . . ? O6 C6 C7 F7 -92(2) 7_556 . . . ? O6 C6 C7 F7 -92(2) . . . 7_556 ? O6 C6 C7 F7 88(2) 7_556 . . 7_556 ? C16 N11 C12 C13 -0.2(7) . . . . ? Eu1 N11 C12 C13 173.0(4) . . . . ? N11 C12 C13 C14 -0.3(9) . . . . ? C12 C13 C14 C15 0.3(10) . . . . ? C13 C14 C15 C16 0.1(9) . . . . ? C13 C14 C15 C17 179.1(6) . . . . ? C12 N11 C16 C15 0.6(7) . . . . ? Eu1 N11 C16 C15 -172.7(4) . . . . ? C12 N11 C16 C20 -178.3(4) . . . . ? Eu1 N11 C16 C20 8.3(6) . . . . ? C14 C15 C16 N11 -0.6(8) . . . . ? C17 C15 C16 N11 -179.7(5) . . . . ? C14 C15 C16 C20 178.4(5) . . . . ? C17 C15 C16 C20 -0.7(8) . . . . ? C14 C15 C17 C18 -178.3(7) . . . . ? C16 C15 C17 C18 0.7(10) . . . . ? C15 C17 C18 C19 -0.8(12) . . . . ? C17 C18 C19 C21 179.5(7) . . . . ? C17 C18 C19 C20 1.0(10) . . . . ? C23 N12 C20 C19 0.0(7) . . . . ? Eu1 N12 C20 C19 171.6(4) . . . . ? C23 N12 C20 C16 179.9(4) . . . . ? Eu1 N12 C20 C16 -8.5(6) . . . . ? C21 C19 C20 N12 0.2(8) . . . . ? C18 C19 C20 N12 178.9(5) . . . . ? C21 C19 C20 C16 -179.7(5) . . . . ? C18 C19 C20 C16 -1.0(8) . . . . ? N11 C16 C20 N12 0.0(7) . . . . ? C15 C16 C20 N12 -179.0(4) . . . . ? N11 C16 C20 C19 179.9(5) . . . . ? C15 C16 C20 C19 0.9(8) . . . . ? C20 C19 C21 C22 -1.0(9) . . . . ? C18 C19 C21 C22 -179.5(6) . . . . ? C19 C21 C22 C23 1.4(9) . . . . ? C20 N12 C23 C22 0.5(7) . . . . ? Eu1 N12 C23 C22 -171.0(4) . . . . ? C21 C22 C23 N12 -1.2(8) . . . . ? Eu2 O31 C32 C33 -23.7(8) . . . . ? Eu2 O31 C32 C31 153.9(4) . . . . ? F31 C31 C32 O31 6.0(7) . . . . ? F33 C31 C32 O31 128.3(5) . . . . ? F32 C31 C32 O31 -113.0(6) . . . . ? F31 C31 C32 C33 -176.2(5) . . . . ? F33 C31 C32 C33 -53.8(7) . . . . ? F32 C31 C32 C33 64.8(6) . . . . ? O31 C32 C33 F34 179.8(4) . . . . ? C31 C32 C33 F34 2.2(7) . . . . ? O31 C32 C33 C34 1.0(9) . . . . ? C31 C32 C33 C34 -176.5(5) . . . . ? Eu2 O32 C34 C33 15.0(8) . . . . ? Eu2 O32 C34 C35 -166.7(3) . . . . ? C32 C33 C34 O32 2.2(8) . . . . ? F34 C33 C34 O32 -176.6(4) . . . . ? C32 C33 C34 C35 -176.1(5) . . . . ? F34 C33 C34 C35 5.1(7) . . . . ? O32 C34 C35 F35 -119.3(5) . . . . ? C33 C34 C35 F35 59.1(7) . . . . ? O32 C34 C35 F36 2.1(7) . . . . ? C33 C34 C35 F36 -179.5(5) . . . . ? O32 C34 C35 F37 120.0(5) . . . . ? C33 C34 C35 F37 -61.5(7) . . . . ? Eu2 O36 C36 O36 24.45(19) . . . 7_556 ? Eu2 O36 C36 C37 -155.55(19) . . . . ? F41 F42 C37 F42 -86.6(12) . . . 7_556 ? F43 F42 C37 F42 80.0(10) . . . 7_556 ? F43 F42 C37 F41 166.5(16) . . . . ? F41 F42 C37 F41 -146(2) . . . 7_556 ? F43 F42 C37 F41 21(2) . . . 7_556 ? F41 F42 C37 F43 -31.0(17) . . . 7_556 ? F43 F42 C37 F43 135.5(19) . . . 7_556 ? F41 F42 C37 F43 -166.5(16) . . . . ? F41 F42 C37 C36 93.4(12) . . . . ? F43 F42 C37 C36 -100.0(10) . . . . ? F43 F41 C37 F42 -144(2) 7_556 . . . ? F42 F41 C37 F42 124.0(18) . . . 7_556 ? F43 F41 C37 F42 -20(2) 7_556 . . 7_556 ? F42 F41 C37 F41 70.1(11) . . . 7_556 ? F43 F41 C37 F41 -73.9(13) 7_556 . . 7_556 ? F42 F41 C37 F43 144(2) . . . 7_556 ? F42 F41 C37 F43 11.5(13) . . . . ? F43 F41 C37 F43 -132(2) 7_556 . . . ? F42 F41 C37 C36 -109.9(11) . . . . ? F43 F41 C37 C36 106.2(13) 7_556 . . . ? F41 F43 C37 F42 157(2) 7_556 . . . ? F42 F43 C37 F42 -126.8(14) . . . 7_556 ? F41 F43 C37 F42 30(2) 7_556 . . 7_556 ? F42 F43 C37 F41 -11.5(15) . . . . ? F41 F43 C37 F41 145(2) 7_556 . . . ? F42 F43 C37 F41 -157(2) . . . 7_556 ? F42 F43 C37 F43 -73.4(11) . . . 7_556 ? F41 F43 C37 F43 83.1(15) 7_556 . . 7_556 ? F42 F43 C37 C36 106.6(11) . . . . ? F41 F43 C37 C36 -96.9(15) 7_556 . . . ? O36 C36 C37 F42 33.9(18) . . . . ? O36 C36 C37 F42 -146.1(18) 7_556 . . . ? O36 C36 C37 F42 -146.1(18) . . . 7_556 ? O36 C36 C37 F42 33.9(18) 7_556 . . 7_556 ? O36 C36 C37 F41 92(3) . . . . ? O36 C36 C37 F41 -88(3) 7_556 . . . ? O36 C36 C37 F41 -88(3) . . . 7_556 ? O36 C36 C37 F41 92(3) 7_556 . . 7_556 ? O36 C36 C37 F43 154(2) . . . 7_556 ? O36 C36 C37 F43 -26(2) 7_556 . . 7_556 ? O36 C36 C37 F43 -26(2) . . . . ? O36 C36 C37 F43 154(2) 7_556 . . . ? C46 N41 C42 C43 -1.2(7) . . . . ? Eu2 N41 C42 C43 166.5(4) . . . . ? N41 C42 C43 C44 0.4(8) . . . . ? C42 C43 C44 C45 1.0(8) . . . . ? C43 C44 C45 C47 178.3(6) . . . . ? C43 C44 C45 C46 -1.4(8) . . . . ? C42 N41 C46 C50 -176.4(4) . . . . ? Eu2 N41 C46 C50 15.6(6) . . . . ? C42 N41 C46 C45 0.6(7) . . . . ? Eu2 N41 C46 C45 -167.5(4) . . . . ? C44 C45 C46 N41 0.7(7) . . . . ? C47 C45 C46 N41 -179.1(5) . . . . ? C44 C45 C46 C50 177.5(5) . . . . ? C47 C45 C46 C50 -2.2(7) . . . . ? C44 C45 C47 C48 -177.1(7) . . . . ? C46 C45 C47 C48 2.6(10) . . . . ? C45 C47 C48 C49 -1.1(11) . . . . ? C47 C48 C49 C51 -179.6(7) . . . . ? C47 C48 C49 C50 -0.7(10) . . . . ? C53 N42 C50 C49 -1.8(7) . . . . ? Eu2 N42 C50 C49 168.2(4) . . . . ? C53 N42 C50 C46 177.8(5) . . . . ? Eu2 N42 C50 C46 -12.2(6) . . . . ? C51 C49 C50 N42 -0.6(8) . . . . ? C48 C49 C50 N42 -179.5(5) . . . . ? C51 C49 C50 C46 179.9(5) . . . . ? C48 C49 C50 C46 1.0(8) . . . . ? N41 C46 C50 N42 -2.0(7) . . . . ? C45 C46 C50 N42 -179.0(4) . . . . ? N41 C46 C50 C49 177.5(5) . . . . ? C45 C46 C50 C49 0.5(8) . . . . ? C50 C49 C51 C52 2.3(10) . . . . ? C48 C49 C51 C52 -178.9(6) . . . . ? C49 C51 C52 C53 -1.7(10) . . . . ? C50 N42 C53 C52 2.4(8) . . . . ? Eu2 N42 C53 C52 -167.1(4) . . . . ? C51 C52 C53 N42 -0.7(9) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.282 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.132 data_00071 _database_code_CSD 171068 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H30 F21 O8 P2 Tm' _chemical_formula_weight 1400.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tm' 'Tm' -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 17.2223(10) _cell_length_b 15.6980(10) _cell_length_c 20.3127(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 92.883(10) _cell_angle_gamma 90.000(10) _cell_volume 5484.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'ireg block' _exptl_crystal_colour colorless _exptl_crystal_size_max .15 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .18 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34874 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.1245 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28.28 _reflns_number_total 12978 _reflns_number_gt 7611 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12978 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _refine_ls_shift/su_max 0.513 _refine_ls_shift/su_mean 0.037 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 Tm1 Tm 0.239222(10) 0.238721(10) 0.508533(9) 0.02611(6) Uani 1 1 d . . . P3 P 0.36257(7) 0.13082(7) 0.39625(6) 0.0311(3) Uani 1 1 d . . . P6 P 0.18392(6) 0.43495(6) 0.58675(6) 0.0275(3) Uani 1 1 d . . . F1 F 0.19444(18) -0.05847(15) 0.45290(16) 0.0697(9) Uani 1 1 d . . . F2 F 0.1862(2) -0.09569(17) 0.55284(17) 0.1038(14) Uani 1 1 d . . . F3 F 0.0837(2) -0.07575(19) 0.49253(19) 0.0981(13) Uani 1 1 d . . . F4 F 0.06382(17) 0.00958(16) 0.60484(15) 0.0711(10) Uani 1 1 d . . . F5 F 0.0612(3) 0.1296(2) 0.70827(18) 0.1278(18) Uani 1 1 d . . . F6 F -0.0266(2) 0.1508(3) 0.6364(2) 0.143(2) Uani 1 1 d . . . F7 F 0.04259(15) 0.25173(16) 0.67132(13) 0.0593(8) Uani 1 1 d . . . F11 F 0.3286(2) 0.0531(2) 0.6804(2) 0.1338(18) Uani 1 1 d . . . F12 F 0.4446(2) 0.0814(2) 0.6855(2) 0.1263(17) Uani 1 1 d . . . F13 F 0.3692(3) 0.1425(2) 0.74542(18) 0.1279(17) Uani 1 1 d . . . F14 F 0.47812(14) 0.25286(17) 0.67109(13) 0.0602(8) Uani 1 1 d . . . F15 F 0.47998(19) 0.4219(2) 0.64165(18) 0.0925(12) Uani 1 1 d . . . F16 F 0.44250(17) 0.45042(18) 0.54442(19) 0.0945(13) Uani 1 1 d . . . F17 F 0.53254(16) 0.36070(17) 0.56295(18) 0.0852(12) Uani 1 1 d . . . F21 F 0.01412(16) 0.2246(2) 0.30490(17) 0.0929(12) Uani 1 1 d . . . F22 F -0.01103(17) 0.2029(3) 0.40346(19) 0.1173(16) Uani 1 1 d . . . F23 F -0.01974(16) 0.3248(2) 0.36417(19) 0.0999(13) Uani 1 1 d . . . F24 F 0.11717(15) 0.36024(16) 0.29186(13) 0.0577(8) Uani 1 1 d . . . F25 F 0.2325(2) 0.48640(18) 0.31925(18) 0.0984(13) Uani 1 1 d . . . F26 F 0.3393(2) 0.4272(2) 0.34363(18) 0.1062(14) Uani 1 1 d . . . F27 F 0.27187(19) 0.38746(18) 0.26059(15) 0.0788(10) Uani 1 1 d . . . O1 O 0.19954(16) 0.09518(16) 0.49797(14) 0.0334(7) Uani 1 1 d . . . O2 O 0.13971(15) 0.21613(16) 0.58205(13) 0.0322(7) Uani 1 1 d . . . O3 O 0.33246(15) 0.17203(16) 0.45654(14) 0.0334(7) Uani 1 1 d . . . O6 O 0.19840(15) 0.36854(15) 0.53519(13) 0.0294(7) Uani 1 1 d . . . O11 O 0.29881(16) 0.17584(17) 0.59973(14) 0.0352(7) Uani 1 1 d . . . O12 O 0.35062(16) 0.32130(16) 0.53996(14) 0.0339(7) Uani 1 1 d . . . O21 O 0.13031(14) 0.23784(16) 0.43932(13) 0.0310(6) Uani 1 1 d . . . O22 O 0.26561(16) 0.32395(16) 0.41603(14) 0.0333(7) Uani 1 1 d . . . C1 C 0.1537(4) -0.0468(3) 0.5050(3) 0.0564(15) Uani 1 1 d . . . C2 C 0.1556(3) 0.0471(3) 0.5274(2) 0.0350(11) Uani 1 1 d . . . C3 C 0.1076(3) 0.0707(3) 0.5780(2) 0.0393(12) Uani 1 1 d . . . C4 C 0.1016(2) 0.1531(3) 0.6009(2) 0.0331(11) Uani 1 1 d . . . C5 C 0.0433(3) 0.1721(3) 0.6537(3) 0.0540(15) Uani 1 1 d . . . C11 C 0.3776(3) 0.1160(4) 0.6861(3) 0.0544(15) Uani 1 1 d . . . C12 C 0.3605(3) 0.1846(3) 0.6338(2) 0.0350(11) Uani 1 1 d . . . C13 C 0.4139(2) 0.2502(3) 0.6287(2) 0.0386(11) Uani 1 1 d . . . C14 C 0.4048(2) 0.3160(3) 0.5828(2) 0.0343(11) Uani 1 1 d . . . C15 C 0.4657(3) 0.3873(3) 0.5820(3) 0.0505(14) Uani 1 1 d . . . C21 C 0.0217(3) 0.2555(3) 0.3647(3) 0.0501(13) Uani 1 1 d . . . C22 C 0.1070(2) 0.2733(2) 0.3868(2) 0.0307(10) Uani 1 1 d . . . C23 C 0.1500(3) 0.3263(3) 0.3495(2) 0.0357(11) Uani 1 1 d . . . C24 C 0.2271(3) 0.3496(2) 0.3661(2) 0.0316(11) Uani 1 1 d . . . C25 C 0.2681(3) 0.4132(3) 0.3226(3) 0.0449(13) Uani 1 1 d . . . C31 C 0.3768(2) 0.0187(2) 0.4103(2) 0.0304(10) Uani 1 1 d . . . C32 C 0.3725(2) -0.0399(3) 0.3590(2) 0.0380(11) Uani 1 1 d . . . H32A H 0.3615 -0.0217 0.3160 0.046 Uiso 1 1 calc R . . C33 C 0.3847(3) -0.1252(3) 0.3721(3) 0.0492(14) Uani 1 1 d . . . H33A H 0.3811 -0.1646 0.3379 0.059 Uiso 1 1 calc R . . C34 C 0.4022(3) -0.1525(3) 0.4357(3) 0.0517(14) Uani 1 1 d . . . H34A H 0.4111 -0.2099 0.4443 0.062 Uiso 1 1 calc R . . C35 C 0.4062(3) -0.0947(3) 0.4859(3) 0.0545(14) Uani 1 1 d . . . H35A H 0.4177 -0.1131 0.5288 0.065 Uiso 1 1 calc R . . C36 C 0.3934(3) -0.0088(3) 0.4737(2) 0.0457(13) Uani 1 1 d . . . H36A H 0.3960 0.0300 0.5083 0.055 Uiso 1 1 calc R . . C41 C 0.4531(2) 0.1783(3) 0.3779(2) 0.0314(11) Uani 1 1 d . . . C42 C 0.5086(3) 0.1363(3) 0.3433(2) 0.0407(12) Uani 1 1 d . . . H42A H 0.4985 0.0815 0.3278 0.049 Uiso 1 1 calc R . . C43 C 0.5791(3) 0.1744(3) 0.3314(2) 0.0540(14) Uani 1 1 d . . . H43A H 0.6162 0.1453 0.3084 0.065 Uiso 1 1 calc R . . C44 C 0.5937(3) 0.2551(4) 0.3539(2) 0.0586(14) Uani 1 1 d . . . H44A H 0.6411 0.2807 0.3461 0.070 Uiso 1 1 calc R . . C45 C 0.5396(3) 0.2989(3) 0.3877(3) 0.0618(16) Uani 1 1 d . . . H45A H 0.5499 0.3542 0.4020 0.074 Uiso 1 1 calc R . . C46 C 0.4694(3) 0.2607(3) 0.4006(2) 0.0457(12) Uani 1 1 d . . . H46A H 0.4331 0.2899 0.4243 0.055 Uiso 1 1 calc R . . C51 C 0.2964(3) 0.1409(3) 0.3246(2) 0.0358(11) Uani 1 1 d . . . C52 C 0.2229(3) 0.1049(3) 0.3287(2) 0.0439(13) Uani 1 1 d . . . H52A H 0.2103 0.0748 0.3661 0.053 Uiso 1 1 calc R . . C53 C 0.1685(3) 0.1143(3) 0.2761(3) 0.0511(14) Uani 1 1 d . . . H53A H 0.1195 0.0899 0.2783 0.061 Uiso 1 1 calc R . . C54 C 0.1865(3) 0.1591(3) 0.2213(3) 0.0598(16) Uani 1 1 d . . . H54A H 0.1494 0.1658 0.1868 0.072 Uiso 1 1 calc R . . C55 C 0.2589(3) 0.1941(3) 0.2170(3) 0.0566(15) Uani 1 1 d . . . H55A H 0.2712 0.2236 0.1792 0.068 Uiso 1 1 calc R . . C56 C 0.3144(3) 0.1857(3) 0.2693(2) 0.0443(13) Uani 1 1 d . . . H56A H 0.3632 0.2104 0.2666 0.053 Uiso 1 1 calc R . . C61 C 0.2398(2) 0.4171(3) 0.6629(2) 0.0279(10) Uani 1 1 d . . . C62 C 0.2269(3) 0.3425(3) 0.6971(2) 0.0398(12) Uani 1 1 d . . . H62A H 0.1885 0.3049 0.6818 0.048 Uiso 1 1 calc R . . C63 C 0.2716(3) 0.3236(3) 0.7546(2) 0.0463(13) Uani 1 1 d . . . H63A H 0.2628 0.2736 0.7776 0.056 Uiso 1 1 calc R . . C64 C 0.3285(3) 0.3794(3) 0.7768(3) 0.0560(15) Uani 1 1 d . . . H64A H 0.3584 0.3672 0.8151 0.067 Uiso 1 1 calc R . . C65 C 0.3410(3) 0.4520(4) 0.7433(3) 0.0673(17) Uani 1 1 d . . . H65A H 0.3798 0.4892 0.7587 0.081 Uiso 1 1 calc R . . C66 C 0.2971(3) 0.4722(3) 0.6862(3) 0.0528(14) Uani 1 1 d . . . H66A H 0.3064 0.5226 0.6638 0.063 Uiso 1 1 calc R . . C71 C 0.2104(2) 0.5382(2) 0.5571(2) 0.0296(10) Uani 1 1 d . . . C72 C 0.1848(2) 0.6126(3) 0.5854(2) 0.0362(11) Uani 1 1 d . . . H72A H 0.1537 0.6097 0.6215 0.043 Uiso 1 1 calc R . . C73 C 0.2048(3) 0.6909(3) 0.5607(3) 0.0456(13) Uani 1 1 d . . . H73A H 0.1874 0.7405 0.5803 0.055 Uiso 1 1 calc R . . C74 C 0.2502(3) 0.6959(3) 0.5076(3) 0.0484(14) Uani 1 1 d . . . H74A H 0.2632 0.7488 0.4909 0.058 Uiso 1 1 calc R . . C75 C 0.2767(3) 0.6230(3) 0.4787(2) 0.0480(13) Uani 1 1 d . . . H75A H 0.3076 0.6268 0.4426 0.058 Uiso 1 1 calc R . . C76 C 0.2573(2) 0.5434(3) 0.5036(2) 0.0400(12) Uani 1 1 d . . . H76A H 0.2757 0.4940 0.4844 0.048 Uiso 1 1 calc R . . C81 C 0.0827(2) 0.4357(2) 0.6039(2) 0.0297(10) Uani 1 1 d . . . C82 C 0.0556(2) 0.4650(2) 0.6622(2) 0.0368(11) Uani 1 1 d . . . H82A H 0.0903 0.4855 0.6950 0.044 Uiso 1 1 calc R . . C83 C -0.0237(3) 0.4639(3) 0.6723(3) 0.0488(14) Uani 1 1 d . . . H83A H -0.0422 0.4842 0.7115 0.059 Uiso 1 1 calc R . . C84 C -0.0747(3) 0.4325(3) 0.6238(3) 0.0509(14) Uani 1 1 d . . . H84A H -0.1277 0.4315 0.6305 0.061 Uiso 1 1 calc R . . C85 C -0.0482(3) 0.4027(3) 0.5660(3) 0.0573(15) Uani 1 1 d . . . H85A H -0.0830 0.3813 0.5337 0.069 Uiso 1 1 calc R . . C86 C 0.0311(3) 0.4044(3) 0.5554(2) 0.0407(12) Uani 1 1 d . . . H86A H 0.0493 0.3845 0.5159 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tm1 0.03166(10) 0.02297(10) 0.02360(10) -0.00086(9) 0.00053(7) 0.00140(9) P3 0.0354(7) 0.0285(6) 0.0294(7) -0.0016(5) 0.0023(6) 0.0052(5) P6 0.0299(6) 0.0233(6) 0.0292(7) -0.0019(5) 0.0010(5) 0.0025(5) F1 0.105(2) 0.0362(16) 0.071(2) -0.0200(15) 0.034(2) -0.0134(16) F2 0.205(4) 0.0297(18) 0.078(3) 0.0092(17) 0.017(3) 0.027(2) F3 0.097(3) 0.069(2) 0.131(4) -0.050(2) 0.030(2) -0.047(2) F4 0.102(2) 0.0414(17) 0.074(2) -0.0053(15) 0.040(2) -0.0289(16) F5 0.243(5) 0.083(3) 0.065(3) 0.033(2) 0.084(3) 0.068(3) F6 0.074(3) 0.204(4) 0.156(5) -0.116(4) 0.063(3) -0.064(3) F7 0.0679(18) 0.0486(18) 0.064(2) -0.0050(15) 0.0312(15) 0.0023(15) F11 0.154(4) 0.105(3) 0.134(4) 0.088(3) -0.075(3) -0.049(3) F12 0.099(3) 0.124(3) 0.160(4) 0.097(3) 0.049(3) 0.071(3) F13 0.232(5) 0.111(3) 0.041(3) 0.030(2) 0.019(3) 0.075(3) F14 0.0452(15) 0.077(2) 0.0555(19) -0.0018(16) -0.0210(14) 0.0052(16) F15 0.090(3) 0.088(2) 0.099(3) -0.047(2) -0.003(2) -0.032(2) F16 0.068(2) 0.054(2) 0.158(4) 0.036(2) -0.036(2) -0.0245(17) F17 0.0435(19) 0.061(2) 0.154(4) -0.022(2) 0.030(2) -0.0067(16) F21 0.0578(19) 0.152(3) 0.066(3) -0.036(2) -0.0218(18) 0.005(2) F22 0.061(2) 0.174(4) 0.112(3) 0.077(3) -0.042(2) -0.062(2) F23 0.044(2) 0.099(3) 0.155(4) -0.005(2) -0.001(2) 0.0280(19) F24 0.0651(19) 0.0647(19) 0.043(2) 0.0236(14) -0.0057(16) 0.0164(15) F25 0.141(3) 0.0402(19) 0.122(3) 0.0296(19) 0.082(3) 0.026(2) F26 0.084(3) 0.140(3) 0.094(3) 0.067(2) -0.006(2) -0.049(2) F27 0.125(3) 0.069(2) 0.046(2) 0.0064(17) 0.043(2) -0.0067(19) O1 0.0451(19) 0.0243(16) 0.0309(19) 0.0015(13) 0.0026(15) -0.0010(14) O2 0.0350(16) 0.0315(17) 0.0303(19) 0.0031(13) 0.0047(14) -0.0016(13) O3 0.0367(17) 0.0326(17) 0.0314(19) -0.0078(13) 0.0063(15) 0.0055(13) O6 0.0388(17) 0.0242(15) 0.0252(18) -0.0028(12) 0.0024(14) 0.0029(13) O11 0.0380(18) 0.0394(18) 0.0277(19) 0.0032(14) -0.0035(15) 0.0046(14) O12 0.0356(17) 0.0261(16) 0.039(2) 0.0003(14) -0.0036(16) 0.0013(13) O21 0.0362(16) 0.0336(16) 0.0230(16) 0.0040(14) -0.0008(13) -0.0030(14) O22 0.0422(18) 0.0302(17) 0.0279(19) 0.0015(13) 0.0063(15) -0.0004(14) C1 0.086(5) 0.033(3) 0.051(4) -0.007(3) 0.016(4) -0.010(3) C2 0.046(3) 0.021(2) 0.038(3) 0.002(2) -0.007(2) -0.002(2) C3 0.052(3) 0.026(3) 0.040(3) 0.002(2) 0.009(3) -0.011(2) C4 0.034(3) 0.034(3) 0.031(3) -0.001(2) 0.003(2) -0.003(2) C5 0.068(4) 0.047(4) 0.049(4) -0.005(3) 0.020(3) -0.018(3) C11 0.057(4) 0.061(4) 0.045(4) 0.019(3) -0.005(3) 0.008(3) C12 0.047(3) 0.038(3) 0.020(3) 0.002(2) 0.006(2) 0.016(2) C13 0.035(2) 0.044(3) 0.035(3) -0.005(2) -0.005(2) 0.005(2) C14 0.029(3) 0.033(3) 0.041(3) -0.013(2) 0.001(2) 0.007(2) C15 0.034(3) 0.040(3) 0.077(5) -0.013(3) -0.008(3) -0.003(2) C21 0.046(3) 0.060(4) 0.043(3) 0.009(3) -0.007(3) 0.007(3) C22 0.034(2) 0.028(2) 0.030(3) -0.002(2) -0.002(2) 0.006(2) C23 0.046(3) 0.035(3) 0.025(3) 0.006(2) -0.003(2) 0.011(2) C24 0.048(3) 0.024(2) 0.024(3) 0.0035(19) 0.008(2) 0.006(2) C25 0.056(4) 0.039(3) 0.041(4) 0.007(2) 0.014(3) 0.005(3) C31 0.031(2) 0.031(3) 0.029(3) 0.001(2) 0.000(2) 0.005(2) C32 0.045(3) 0.035(3) 0.034(3) -0.001(2) 0.006(2) 0.003(2) C33 0.053(3) 0.033(3) 0.062(4) -0.010(3) 0.007(3) 0.003(2) C34 0.058(3) 0.026(3) 0.072(4) 0.010(3) 0.009(3) 0.005(2) C35 0.067(4) 0.050(3) 0.045(4) 0.018(3) -0.012(3) 0.009(3) C36 0.056(3) 0.043(3) 0.036(3) 0.000(2) -0.010(3) 0.010(2) C41 0.035(3) 0.037(3) 0.023(3) 0.003(2) 0.003(2) 0.003(2) C42 0.048(3) 0.045(3) 0.030(3) -0.003(2) 0.008(2) -0.001(2) C43 0.046(3) 0.066(4) 0.050(4) -0.001(3) 0.011(3) -0.001(3) C44 0.045(3) 0.082(4) 0.049(4) 0.009(3) 0.009(3) -0.020(3) C45 0.065(4) 0.059(4) 0.063(4) -0.009(3) 0.015(3) -0.022(3) C46 0.048(3) 0.038(3) 0.052(3) -0.005(2) 0.011(2) -0.003(2) C51 0.044(3) 0.030(3) 0.033(3) -0.004(2) -0.002(2) 0.013(2) C52 0.046(3) 0.050(3) 0.036(3) -0.010(2) 0.001(3) 0.016(3) C53 0.050(3) 0.053(3) 0.049(4) -0.016(3) -0.016(3) 0.010(3) C54 0.072(4) 0.056(4) 0.048(4) -0.015(3) -0.033(3) 0.030(3) C55 0.087(4) 0.042(3) 0.039(4) 0.003(2) -0.010(3) 0.017(3) C56 0.056(3) 0.039(3) 0.037(3) -0.001(2) -0.005(3) 0.012(2) C61 0.028(2) 0.032(3) 0.023(3) -0.0034(19) -0.001(2) 0.009(2) C62 0.041(3) 0.046(3) 0.032(3) -0.002(2) -0.002(2) 0.004(2) C63 0.051(3) 0.054(3) 0.035(3) 0.008(2) 0.005(3) 0.014(3) C64 0.053(4) 0.073(4) 0.040(4) 0.001(3) -0.012(3) 0.014(3) C65 0.064(4) 0.070(4) 0.064(5) -0.012(3) -0.029(3) -0.010(3) C66 0.055(3) 0.049(3) 0.053(4) 0.003(3) -0.016(3) -0.003(3) C71 0.023(2) 0.030(2) 0.036(3) -0.003(2) -0.001(2) 0.0000(19) C72 0.037(3) 0.030(3) 0.042(3) -0.002(2) -0.002(2) -0.001(2) C73 0.047(3) 0.030(3) 0.060(4) 0.000(2) -0.001(3) -0.002(2) C74 0.047(3) 0.029(3) 0.069(4) 0.004(3) -0.004(3) -0.006(2) C75 0.042(3) 0.051(3) 0.052(4) 0.009(3) 0.009(3) -0.007(3) C76 0.035(3) 0.033(3) 0.052(4) -0.003(2) 0.002(3) 0.002(2) C81 0.035(3) 0.022(2) 0.032(3) 0.0046(19) 0.001(2) 0.0045(19) C82 0.039(3) 0.033(3) 0.038(3) -0.002(2) 0.002(2) 0.004(2) C83 0.045(3) 0.046(3) 0.058(4) -0.001(3) 0.020(3) 0.005(3) C84 0.032(3) 0.059(3) 0.062(4) 0.015(3) 0.008(3) 0.008(3) C85 0.041(3) 0.073(4) 0.056(4) 0.008(3) -0.010(3) -0.005(3) C86 0.037(3) 0.053(3) 0.032(3) -0.001(2) -0.001(2) 0.001(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 Tm1 O3 2.227(2) . ? Tm1 O6 2.231(2) . ? Tm1 O21 2.287(3) . ? Tm1 O11 2.295(3) . ? Tm1 O2 2.356(3) . ? Tm1 O1 2.361(3) . ? Tm1 O22 2.369(3) . ? Tm1 O12 2.376(3) . ? P3 O3 1.500(3) . ? P3 C41 1.784(4) . ? P3 C31 1.797(4) . ? P3 C51 1.809(5) . ? P6 O6 1.507(3) . ? P6 C81 1.794(4) . ? P6 C71 1.796(4) . ? P6 C61 1.802(4) . ? F1 C1 1.311(5) . ? F2 C1 1.339(6) . ? F3 C1 1.301(6) . ? F4 C3 1.352(5) . ? F5 C5 1.317(6) . ? F6 C5 1.282(6) . ? F7 C5 1.301(5) . ? F11 C11 1.301(6) . ? F12 C11 1.276(5) . ? F13 C11 1.290(6) . ? F14 C13 1.368(4) . ? F15 C15 1.339(6) . ? F16 C15 1.302(5) . ? F17 C15 1.302(5) . ? F21 C21 1.308(5) . ? F22 C21 1.290(5) . ? F23 C21 1.301(5) . ? F24 C23 1.381(5) . ? F25 C25 1.304(5) . ? F26 C25 1.296(5) . ? F27 C25 1.327(5) . ? O1 C2 1.243(5) . ? O2 C4 1.258(4) . ? O11 C12 1.247(5) . ? O12 C14 1.246(5) . ? O21 C22 1.251(4) . ? O22 C24 1.250(5) . ? C1 C2 1.541(6) . ? C2 C3 1.401(6) . ? C3 C4 1.380(5) . ? C4 C5 1.533(6) . ? C11 C12 1.530(6) . ? C12 C13 1.388(6) . ? C13 C14 1.395(6) . ? C14 C15 1.534(6) . ? C21 C22 1.541(6) . ? C22 C23 1.367(5) . ? C23 C24 1.402(6) . ? C24 C25 1.530(6) . ? C31 C36 1.375(6) . ? C31 C32 1.389(5) . ? C32 C33 1.379(5) . ? C33 C34 1.380(7) . ? C34 C35 1.364(6) . ? C35 C36 1.386(6) . ? C41 C42 1.382(5) . ? C41 C46 1.396(5) . ? C42 C43 1.386(6) . ? C43 C44 1.364(6) . ? C44 C45 1.372(6) . ? C45 C46 1.386(6) . ? C51 C56 1.375(6) . ? C51 C52 1.392(6) . ? C52 C53 1.394(6) . ? C53 C54 1.365(7) . ? C54 C55 1.370(7) . ? C55 C56 1.398(6) . ? C61 C66 1.378(5) . ? C61 C62 1.385(5) . ? C62 C63 1.397(6) . ? C63 C64 1.374(6) . ? C64 C65 1.351(7) . ? C65 C66 1.389(6) . ? C71 C72 1.384(5) . ? C71 C76 1.389(6) . ? C72 C73 1.379(5) . ? C73 C74 1.366(6) . ? C74 C75 1.374(6) . ? C75 C76 1.395(5) . ? C81 C82 1.375(5) . ? C81 C86 1.382(5) . ? C82 C83 1.391(5) . ? C83 C84 1.377(6) . ? C84 C85 1.363(6) . ? C85 C86 1.394(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 O3 Tm1 O6 141.99(10) . . ? O3 Tm1 O21 107.11(10) . . ? O6 Tm1 O21 84.03(9) . . ? O3 Tm1 O11 82.92(10) . . ? O6 Tm1 O11 109.30(10) . . ? O21 Tm1 O11 144.41(9) . . ? O3 Tm1 O2 142.62(9) . . ? O6 Tm1 O2 74.66(9) . . ? O21 Tm1 O2 77.79(9) . . ? O11 Tm1 O2 74.55(9) . . ? O3 Tm1 O1 73.78(9) . . ? O6 Tm1 O1 143.16(9) . . ? O21 Tm1 O1 73.36(9) . . ? O11 Tm1 O1 77.20(10) . . ? O2 Tm1 O1 72.39(9) . . ? O3 Tm1 O22 73.60(10) . . ? O6 Tm1 O22 75.65(9) . . ? O21 Tm1 O22 72.54(9) . . ? O11 Tm1 O22 141.92(10) . . ? O2 Tm1 O22 139.68(9) . . ? O1 Tm1 O22 122.21(9) . . ? O3 Tm1 O12 78.01(9) . . ? O6 Tm1 O12 72.33(9) . . ? O21 Tm1 O12 142.63(9) . . ? O11 Tm1 O12 72.28(10) . . ? O2 Tm1 O12 121.01(10) . . ? O1 Tm1 O12 140.46(9) . . ? O22 Tm1 O12 73.77(10) . . ? O3 P3 C41 109.38(18) . . ? O3 P3 C31 110.05(18) . . ? C41 P3 C31 109.20(19) . . ? O3 P3 C51 112.90(18) . . ? C41 P3 C51 108.5(2) . . ? C31 P3 C51 106.7(2) . . ? O6 P6 C81 109.59(18) . . ? O6 P6 C71 109.71(18) . . ? C81 P6 C71 108.96(18) . . ? O6 P6 C61 112.88(17) . . ? C81 P6 C61 108.5(2) . . ? C71 P6 C61 107.1(2) . . ? C2 O1 Tm1 135.8(3) . . ? C4 O2 Tm1 136.0(3) . . ? P3 O3 Tm1 151.25(17) . . ? P6 O6 Tm1 149.94(17) . . ? C12 O11 Tm1 137.3(3) . . ? C14 O12 Tm1 135.8(3) . . ? C22 O21 Tm1 137.7(3) . . ? C24 O22 Tm1 135.2(3) . . ? F3 C1 F1 108.8(5) . . ? F3 C1 F2 106.8(4) . . ? F1 C1 F2 106.5(5) . . ? F3 C1 C2 113.4(5) . . ? F1 C1 C2 111.6(4) . . ? F2 C1 C2 109.4(4) . . ? O1 C2 C3 126.0(4) . . ? O1 C2 C1 116.3(4) . . ? C3 C2 C1 117.7(4) . . ? F4 C3 C4 118.4(4) . . ? F4 C3 C2 118.0(4) . . ? C4 C3 C2 123.6(4) . . ? O2 C4 C3 125.8(4) . . ? O2 C4 C5 115.5(4) . . ? C3 C4 C5 118.7(4) . . ? F6 C5 F7 107.7(5) . . ? F6 C5 F5 105.9(5) . . ? F7 C5 F5 105.1(5) . . ? F6 C5 C4 113.4(5) . . ? F7 C5 C4 113.3(4) . . ? F5 C5 C4 110.9(5) . . ? F12 C11 F13 106.9(5) . . ? F12 C11 F11 105.0(5) . . ? F13 C11 F11 103.0(5) . . ? F12 C11 C12 115.8(5) . . ? F13 C11 C12 113.2(5) . . ? F11 C11 C12 111.8(5) . . ? O11 C12 C13 126.1(4) . . ? O11 C12 C11 115.9(4) . . ? C13 C12 C11 118.0(4) . . ? F14 C13 C12 119.5(4) . . ? F14 C13 C14 117.3(4) . . ? C12 C13 C14 123.2(4) . . ? O12 C14 C13 124.8(4) . . ? O12 C14 C15 115.7(4) . . ? C13 C14 C15 119.5(4) . . ? F17 C15 F16 108.6(5) . . ? F17 C15 F15 105.9(4) . . ? F16 C15 F15 105.0(4) . . ? F17 C15 C14 112.6(4) . . ? F16 C15 C14 111.8(4) . . ? F15 C15 C14 112.5(5) . . ? F22 C21 F23 106.5(4) . . ? F22 C21 F21 107.7(5) . . ? F23 C21 F21 105.9(4) . . ? F22 C21 C22 112.1(4) . . ? F23 C21 C22 111.4(4) . . ? F21 C21 C22 112.7(4) . . ? O21 C22 C23 125.7(4) . . ? O21 C22 C21 115.3(4) . . ? C23 C22 C21 118.9(4) . . ? C22 C23 F24 119.7(4) . . ? C22 C23 C24 123.9(4) . . ? F24 C23 C24 116.5(4) . . ? O22 C24 C23 124.7(4) . . ? O22 C24 C25 115.9(4) . . ? C23 C24 C25 119.4(4) . . ? F26 C25 F25 107.6(5) . . ? F26 C25 F27 106.0(4) . . ? F25 C25 F27 105.3(4) . . ? F26 C25 C24 112.1(4) . . ? F25 C25 C24 112.0(4) . . ? F27 C25 C24 113.3(4) . . ? C36 C31 C32 119.6(4) . . ? C36 C31 P3 118.5(3) . . ? C32 C31 P3 121.9(3) . . ? C33 C32 C31 119.9(4) . . ? C34 C33 C32 120.3(5) . . ? C35 C34 C33 119.6(4) . . ? C34 C35 C36 120.7(5) . . ? C31 C36 C35 119.9(4) . . ? C42 C41 C46 118.4(4) . . ? C42 C41 P3 122.8(3) . . ? C46 C41 P3 118.8(3) . . ? C41 C42 C43 121.2(4) . . ? C44 C43 C42 119.4(5) . . ? C43 C44 C45 121.0(5) . . ? C44 C45 C46 119.9(5) . . ? C45 C46 C41 120.1(4) . . ? C56 C51 C52 119.9(4) . . ? C56 C51 P3 123.0(4) . . ? C52 C51 P3 117.0(4) . . ? C53 C52 C51 119.3(5) . . ? C54 C53 C52 120.6(5) . . ? C53 C54 C55 120.2(5) . . ? C54 C55 C56 120.2(5) . . ? C51 C56 C55 119.7(5) . . ? C66 C61 C62 119.3(4) . . ? C66 C61 P6 122.6(4) . . ? C62 C61 P6 118.0(3) . . ? C61 C62 C63 120.2(4) . . ? C64 C63 C62 119.5(5) . . ? C65 C64 C63 120.1(5) . . ? C64 C65 C66 121.3(5) . . ? C61 C66 C65 119.6(5) . . ? C72 C71 C76 119.1(4) . . ? C72 C71 P6 122.0(3) . . ? C76 C71 P6 118.9(3) . . ? C73 C72 C71 120.7(5) . . ? C74 C73 C72 120.1(4) . . ? C73 C74 C75 120.4(4) . . ? C74 C75 C76 120.0(5) . . ? C71 C76 C75 119.7(4) . . ? C82 C81 C86 119.9(4) . . ? C82 C81 P6 123.0(3) . . ? C86 C81 P6 117.1(3) . . ? C81 C82 C83 120.1(4) . . ? C84 C83 C82 119.6(5) . . ? C85 C84 C83 120.6(5) . . ? C84 C85 C86 120.0(5) . . ? C81 C86 C85 119.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Tm1 O1 C2 156.3(4) . . . . ? O6 Tm1 O1 C2 -35.1(5) . . . . ? O21 Tm1 O1 C2 -89.7(4) . . . . ? O11 Tm1 O1 C2 70.1(4) . . . . ? O2 Tm1 O1 C2 -7.5(4) . . . . ? O22 Tm1 O1 C2 -145.7(4) . . . . ? O12 Tm1 O1 C2 110.1(4) . . . . ? O3 Tm1 O2 C4 -19.9(5) . . . . ? O6 Tm1 O2 C4 169.5(4) . . . . ? O21 Tm1 O2 C4 82.4(4) . . . . ? O11 Tm1 O2 C4 -75.0(4) . . . . ? O1 Tm1 O2 C4 6.2(4) . . . . ? O22 Tm1 O2 C4 125.6(4) . . . . ? O12 Tm1 O2 C4 -132.6(4) . . . . ? C41 P3 O3 Tm1 126.5(3) . . . . ? C31 P3 O3 Tm1 -113.5(3) . . . . ? C51 P3 O3 Tm1 5.6(4) . . . . ? O6 Tm1 O3 P3 -95.3(4) . . . . ? O21 Tm1 O3 P3 7.3(4) . . . . ? O11 Tm1 O3 P3 152.3(4) . . . . ? O2 Tm1 O3 P3 99.5(4) . . . . ? O1 Tm1 O3 P3 73.6(3) . . . . ? O22 Tm1 O3 P3 -58.0(3) . . . . ? O12 Tm1 O3 P3 -134.4(4) . . . . ? C81 P6 O6 Tm1 -100.2(3) . . . . ? C71 P6 O6 Tm1 140.2(3) . . . . ? C61 P6 O6 Tm1 20.8(4) . . . . ? O3 Tm1 O6 P6 -113.1(3) . . . . ? O21 Tm1 O6 P6 136.6(3) . . . . ? O11 Tm1 O6 P6 -9.5(4) . . . . ? O2 Tm1 O6 P6 57.7(3) . . . . ? O1 Tm1 O6 P6 84.9(4) . . . . ? O22 Tm1 O6 P6 -149.9(3) . . . . ? O12 Tm1 O6 P6 -72.7(3) . . . . ? O3 Tm1 O11 C12 71.9(4) . . . . ? O6 Tm1 O11 C12 -71.0(4) . . . . ? O21 Tm1 O11 C12 -178.4(3) . . . . ? O2 Tm1 O11 C12 -138.2(4) . . . . ? O1 Tm1 O11 C12 146.8(4) . . . . ? O22 Tm1 O11 C12 20.2(5) . . . . ? O12 Tm1 O11 C12 -7.7(4) . . . . ? O3 Tm1 O12 C14 -83.0(4) . . . . ? O6 Tm1 O12 C14 121.1(4) . . . . ? O21 Tm1 O12 C14 174.5(3) . . . . ? O11 Tm1 O12 C14 3.4(4) . . . . ? O2 Tm1 O12 C14 62.1(4) . . . . ? O1 Tm1 O12 C14 -37.9(5) . . . . ? O22 Tm1 O12 C14 -159.1(4) . . . . ? O3 Tm1 O21 C22 -71.4(4) . . . . ? O6 Tm1 O21 C22 71.4(4) . . . . ? O11 Tm1 O21 C22 -173.4(3) . . . . ? O2 Tm1 O21 C22 147.0(4) . . . . ? O1 Tm1 O21 C22 -138.0(4) . . . . ? O22 Tm1 O21 C22 -5.4(4) . . . . ? O12 Tm1 O21 C22 21.2(5) . . . . ? O3 Tm1 O22 C24 119.6(4) . . . . ? O6 Tm1 O22 C24 -83.1(4) . . . . ? O21 Tm1 O22 C24 5.1(4) . . . . ? O11 Tm1 O22 C24 173.8(3) . . . . ? O2 Tm1 O22 C24 -39.4(4) . . . . ? O1 Tm1 O22 C24 61.5(4) . . . . ? O12 Tm1 O22 C24 -158.5(4) . . . . ? Tm1 O1 C2 C3 5.7(7) . . . . ? Tm1 O1 C2 C1 -174.9(3) . . . . ? F3 C1 C2 O1 -129.5(5) . . . . ? F1 C1 C2 O1 -6.3(7) . . . . ? F2 C1 C2 O1 111.4(5) . . . . ? F3 C1 C2 C3 49.8(6) . . . . ? F1 C1 C2 C3 173.1(4) . . . . ? F2 C1 C2 C3 -69.3(6) . . . . ? O1 C2 C3 F4 -179.5(4) . . . . ? C1 C2 C3 F4 1.2(7) . . . . ? O1 C2 C3 C4 1.8(8) . . . . ? C1 C2 C3 C4 -177.5(5) . . . . ? Tm1 O2 C4 C3 -3.1(7) . . . . ? Tm1 O2 C4 C5 177.5(3) . . . . ? F4 C3 C4 O2 178.2(4) . . . . ? C2 C3 C4 O2 -3.1(8) . . . . ? F4 C3 C4 C5 -2.4(7) . . . . ? C2 C3 C4 C5 176.3(5) . . . . ? O2 C4 C5 F6 122.8(5) . . . . ? C3 C4 C5 F6 -56.7(7) . . . . ? O2 C4 C5 F7 -0.4(7) . . . . ? C3 C4 C5 F7 -179.8(4) . . . . ? O2 C4 C5 F5 -118.2(5) . . . . ? C3 C4 C5 F5 62.4(6) . . . . ? Tm1 O11 C12 C13 8.1(7) . . . . ? Tm1 O11 C12 C11 -172.1(3) . . . . ? F12 C11 C12 O11 128.5(5) . . . . ? F13 C11 C12 O11 -107.6(6) . . . . ? F11 C11 C12 O11 8.2(7) . . . . ? F12 C11 C12 C13 -51.8(7) . . . . ? F13 C11 C12 C13 72.2(6) . . . . ? F11 C11 C12 C13 -172.0(5) . . . . ? O11 C12 C13 F14 178.0(4) . . . . ? C11 C12 C13 F14 -1.8(6) . . . . ? O11 C12 C13 C14 -0.6(7) . . . . ? C11 C12 C13 C14 179.7(4) . . . . ? Tm1 O12 C14 C13 0.4(7) . . . . ? Tm1 O12 C14 C15 178.8(3) . . . . ? F14 C13 C14 O12 178.0(4) . . . . ? C12 C13 C14 O12 -3.4(7) . . . . ? F14 C13 C14 C15 -0.3(6) . . . . ? C12 C13 C14 C15 178.3(4) . . . . ? O12 C14 C15 F17 -110.3(5) . . . . ? C13 C14 C15 F17 68.2(6) . . . . ? O12 C14 C15 F16 12.2(6) . . . . ? C13 C14 C15 F16 -169.3(4) . . . . ? O12 C14 C15 F15 130.1(4) . . . . ? C13 C14 C15 F15 -51.4(6) . . . . ? Tm1 O21 C22 C23 4.9(7) . . . . ? Tm1 O21 C22 C21 -173.6(3) . . . . ? F22 C21 C22 O21 -2.9(6) . . . . ? F23 C21 C22 O21 116.4(5) . . . . ? F21 C21 C22 O21 -124.6(5) . . . . ? F22 C21 C22 C23 178.5(4) . . . . ? F23 C21 C22 C23 -62.3(6) . . . . ? F21 C21 C22 C23 56.7(6) . . . . ? O21 C22 C23 F24 179.1(4) . . . . ? C21 C22 C23 F24 -2.5(6) . . . . ? O21 C22 C23 C24 -1.0(7) . . . . ? C21 C22 C23 C24 177.5(4) . . . . ? Tm1 O22 C24 C23 -4.5(7) . . . . ? Tm1 O22 C24 C25 173.4(3) . . . . ? C22 C23 C24 O22 0.9(7) . . . . ? F24 C23 C24 O22 -179.1(4) . . . . ? C22 C23 C24 C25 -176.8(4) . . . . ? F24 C23 C24 C25 3.1(6) . . . . ? O22 C24 C25 F26 3.0(6) . . . . ? C23 C24 C25 F26 -179.0(4) . . . . ? O22 C24 C25 F25 -118.0(5) . . . . ? C23 C24 C25 F25 59.9(6) . . . . ? O22 C24 C25 F27 122.9(5) . . . . ? C23 C24 C25 F27 -59.1(6) . . . . ? O3 P3 C31 C36 -28.1(4) . . . . ? C41 P3 C31 C36 91.9(4) . . . . ? C51 P3 C31 C36 -151.0(4) . . . . ? O3 P3 C31 C32 152.7(3) . . . . ? C41 P3 C31 C32 -87.2(4) . . . . ? C51 P3 C31 C32 29.9(4) . . . . ? C36 C31 C32 C33 0.2(7) . . . . ? P3 C31 C32 C33 179.3(3) . . . . ? C31 C32 C33 C34 -0.9(7) . . . . ? C32 C33 C34 C35 1.0(8) . . . . ? C33 C34 C35 C36 -0.4(8) . . . . ? C32 C31 C36 C35 0.4(7) . . . . ? P3 C31 C36 C35 -178.7(4) . . . . ? C34 C35 C36 C31 -0.4(7) . . . . ? O3 P3 C41 C42 154.7(4) . . . . ? C31 P3 C41 C42 34.2(4) . . . . ? C51 P3 C41 C42 -81.8(4) . . . . ? O3 P3 C41 C46 -23.8(4) . . . . ? C31 P3 C41 C46 -144.3(4) . . . . ? C51 P3 C41 C46 99.7(4) . . . . ? C46 C41 C42 C43 0.2(7) . . . . ? P3 C41 C42 C43 -178.3(4) . . . . ? C41 C42 C43 C44 -0.4(7) . . . . ? C42 C43 C44 C45 -0.3(8) . . . . ? C43 C44 C45 C46 1.2(8) . . . . ? C44 C45 C46 C41 -1.4(8) . . . . ? C42 C41 C46 C45 0.7(7) . . . . ? P3 C41 C46 C45 179.3(4) . . . . ? O3 P3 C51 C56 115.8(4) . . . . ? C41 P3 C51 C56 -5.6(4) . . . . ? C31 P3 C51 C56 -123.2(4) . . . . ? O3 P3 C51 C52 -60.6(4) . . . . ? C41 P3 C51 C52 178.0(3) . . . . ? C31 P3 C51 C52 60.4(4) . . . . ? C56 C51 C52 C53 0.5(6) . . . . ? P3 C51 C52 C53 177.0(3) . . . . ? C51 C52 C53 C54 -0.7(7) . . . . ? C52 C53 C54 C55 1.0(8) . . . . ? C53 C54 C55 C56 -1.2(7) . . . . ? C52 C51 C56 C55 -0.7(7) . . . . ? P3 C51 C56 C55 -177.0(3) . . . . ? C54 C55 C56 C51 1.1(7) . . . . ? O6 P6 C61 C66 114.5(4) . . . . ? C81 P6 C61 C66 -123.8(4) . . . . ? C71 P6 C61 C66 -6.3(4) . . . . ? O6 P6 C61 C62 -61.9(4) . . . . ? C81 P6 C61 C62 59.7(4) . . . . ? C71 P6 C61 C62 177.2(3) . . . . ? C66 C61 C62 C63 0.1(7) . . . . ? P6 C61 C62 C63 176.7(3) . . . . ? C61 C62 C63 C64 -0.2(7) . . . . ? C62 C63 C64 C65 0.0(8) . . . . ? C63 C64 C65 C66 0.2(9) . . . . ? C62 C61 C66 C65 0.2(7) . . . . ? P6 C61 C66 C65 -176.3(4) . . . . ? C64 C65 C66 C61 -0.3(9) . . . . ? O6 P6 C71 C72 162.5(3) . . . . ? C81 P6 C71 C72 42.5(4) . . . . ? C61 P6 C71 C72 -74.7(4) . . . . ? O6 P6 C71 C76 -16.8(4) . . . . ? C81 P6 C71 C76 -136.8(4) . . . . ? C61 P6 C71 C76 106.1(4) . . . . ? C76 C71 C72 C73 0.6(7) . . . . ? P6 C71 C72 C73 -178.7(3) . . . . ? C71 C72 C73 C74 0.2(7) . . . . ? C72 C73 C74 C75 -0.5(7) . . . . ? C73 C74 C75 C76 0.1(8) . . . . ? C72 C71 C76 C75 -1.1(7) . . . . ? P6 C71 C76 C75 178.2(3) . . . . ? C74 C75 C76 C71 0.7(7) . . . . ? O6 P6 C81 C82 156.2(3) . . . . ? C71 P6 C81 C82 -83.7(4) . . . . ? C61 P6 C81 C82 32.6(4) . . . . ? O6 P6 C81 C86 -23.3(4) . . . . ? C71 P6 C81 C86 96.7(3) . . . . ? C61 P6 C81 C86 -147.0(3) . . . . ? C86 C81 C82 C83 -0.6(6) . . . . ? P6 C81 C82 C83 179.9(3) . . . . ? C81 C82 C83 C84 0.7(7) . . . . ? C82 C83 C84 C85 -0.2(7) . . . . ? C83 C84 C85 C86 -0.4(8) . . . . ? C82 C81 C86 C85 0.0(6) . . . . ? P6 C81 C86 C85 179.5(3) . . . . ? C84 C85 C86 C81 0.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.872 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.109 data_00077 _database_code_CSD 171069 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H33 Eu F18 O8 P2' _chemical_formula_weight 1329.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 12.8980(10) _cell_length_b 13.5177(10) _cell_length_c 30.432(2) _cell_angle_alpha 90.000(10) _cell_angle_beta 91.342(10) _cell_angle_gamma 90.000(10) _cell_volume 5304.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max .37 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2632 _exptl_absorpt_coefficient_mu 1.358 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 33514 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.29 _reflns_number_total 12504 _reflns_number_gt 8358 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12504 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0741 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.004 _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 0.260588(13) 0.178234(11) 0.103481(5) 0.02620(5) Uani 1 1 d . . . F1 F 0.2709(3) -0.18131(17) 0.05944(10) 0.0952(10) Uani 1 1 d . . . O1 O 0.29905(18) 0.01506(15) 0.07637(7) 0.0347(6) Uani 1 1 d . . . C1 C 0.3495(4) -0.1327(3) 0.04374(13) 0.0519(11) Uani 1 1 d . . . F2 F 0.4300(3) -0.1480(2) 0.07004(10) 0.1036(12) Uani 1 1 d . . . O2 O 0.29938(17) 0.18723(16) 0.02611(7) 0.0332(5) Uani 1 1 d . . . C2 C 0.3251(3) -0.0218(2) 0.04073(11) 0.0344(8) Uani 1 1 d . . . P3 P 0.24596(7) -0.00175(6) 0.19461(3) 0.0292(2) Uani 1 1 d . . . F3 F 0.3703(2) -0.17485(17) 0.00589(8) 0.0800(9) Uani 1 1 d . . . O3 O 0.28760(17) 0.07493(15) 0.16397(7) 0.0301(5) Uani 1 1 d . . . C3 C 0.3335(3) 0.0248(3) 0.00037(11) 0.0388(9) Uani 1 1 d . . . H3A H 0.3525 -0.0124 -0.0247 0.047 Uiso 1 1 calc R . . F4 F 0.3518(2) 0.25639(18) -0.05248(7) 0.0775(8) Uani 1 1 d . . . C4 C 0.3144(3) 0.1259(3) -0.00370(11) 0.0350(8) Uani 1 1 d . . . F5 F 0.3416(2) 0.11322(19) -0.08119(7) 0.0836(9) Uani 1 1 d . . . C5 C 0.3048(4) 0.1704(3) -0.05005(12) 0.0521(11) Uani 1 1 d . . . P6 P 0.22843(7) 0.44245(6) 0.07081(3) 0.0284(2) Uani 1 1 d . . . F6 F 0.2044(2) 0.1859(2) -0.06065(7) 0.0804(8) Uani 1 1 d . . . O6 O 0.20928(17) 0.33540(15) 0.08099(7) 0.0324(5) Uani 1 1 d . . . F11 F 0.6545(7) 0.2050(11) 0.0860(4) 0.136(4) Uani 0.598(5) 1 d P . . F11' F 0.6587(14) 0.1313(17) 0.1560(6) 0.136(4) Uani 0.402(5) 1 d P . . F12 F 0.6259(5) 0.0794(7) 0.1234(7) 0.150(4) Uani 0.598(5) 1 d P . . F12' F 0.6862(10) 0.2588(10) 0.1233(9) 0.150(4) Uani 0.402(5) 1 d P . . F13 F 0.6951(5) 0.2024(14) 0.1509(4) 0.157(6) Uani 0.598(5) 1 d P . . F13' F 0.6370(9) 0.129(2) 0.0905(7) 0.157(6) Uani 0.402(5) 1 d P . . O11 O 0.44568(18) 0.18071(17) 0.10607(7) 0.0356(5) Uani 1 1 d . . . C11 C 0.6235(4) 0.1757(5) 0.12351(18) 0.0796(17) Uani 1 1 d . . . O12 O 0.31864(18) 0.29414(15) 0.15952(7) 0.0344(6) Uani 1 1 d . . . C12 C 0.5136(3) 0.2150(3) 0.13187(12) 0.0442(10) Uani 1 1 d . . . C13 C 0.5010(3) 0.2823(3) 0.16589(12) 0.0491(10) Uani 1 1 d . . . H13A H 0.5599 0.3035 0.1826 0.059 Uiso 1 1 calc R . . F14 F 0.3542(3) 0.47844(17) 0.19472(8) 0.0927(10) Uani 1 1 d . . . C14 C 0.4046(3) 0.3185(2) 0.17573(10) 0.0340(8) Uani 1 1 d . . . F15 F 0.3400(2) 0.37063(19) 0.24390(8) 0.0804(9) Uani 1 1 d . . . C15 C 0.3972(3) 0.3986(3) 0.21128(12) 0.0446(10) Uani 1 1 d . . . F16 F 0.4875(2) 0.4259(2) 0.22861(8) 0.0829(9) Uani 1 1 d . . . F21 F -0.1556(2) 0.1770(3) 0.03276(10) 0.1284(15) Uani 1 1 d . . . O21 O 0.10089(18) 0.13855(17) 0.06436(7) 0.0357(6) Uani 1 1 d . . . C21 C -0.0636(4) 0.1383(4) 0.02927(16) 0.0604(13) Uani 1 1 d . . . F22 F -0.0223(2) 0.1683(2) -0.00699(9) 0.0968(10) Uani 1 1 d . . . O22 O 0.11479(18) 0.20585(16) 0.15106(7) 0.0330(5) Uani 1 1 d . . . C22 C 0.0073(3) 0.1584(2) 0.06992(12) 0.0373(9) Uani 1 1 d . . . F23 F -0.0799(2) 0.0421(2) 0.02483(9) 0.0950(10) Uani 1 1 d . . . C23 C -0.0379(3) 0.1944(3) 0.10702(12) 0.0414(9) Uani 1 1 d . . . H23A H -0.1104 0.2072 0.1065 0.050 Uiso 1 1 calc R . . C24 C 0.0200(3) 0.2128(2) 0.14542(11) 0.0336(8) Uani 1 1 d . . . F24 F 0.0199(3) 0.2769(6) 0.21777(14) 0.0922(19) Uani 0.836(7) 1 d P . . F24' F -0.1329(17) 0.230(3) 0.1896(8) 0.0922(19) Uani 0.164(7) 1 d P . . F25 F -0.1016(6) 0.1777(4) 0.19983(15) 0.0969(16) Uani 0.836(7) 1 d P . . F25' F -0.038(3) 0.3394(18) 0.1922(10) 0.0969(16) Uani 0.164(7) 1 d P . . F26 F -0.1015(5) 0.3224(4) 0.17592(12) 0.0918(16) Uani 0.836(7) 1 d P . . F26' F -0.004(3) 0.202(2) 0.2228(7) 0.0918(16) Uani 0.164(7) 1 d P . . C25 C -0.0401(3) 0.2466(3) 0.18589(13) 0.0477(10) Uani 1 1 d . . . C31 C 0.3217(3) -0.1126(2) 0.19281(10) 0.0329(8) Uani 1 1 d . . . C32 C 0.2853(3) -0.2013(3) 0.21105(12) 0.0478(10) Uani 1 1 d . . . H32A H 0.2181 -0.2038 0.2231 0.057 Uiso 1 1 calc R . . C33 C 0.3473(4) -0.2848(3) 0.21144(14) 0.0579(12) Uani 1 1 d . . . H33A H 0.3232 -0.3446 0.2240 0.069 Uiso 1 1 calc R . . C34 C 0.4449(4) -0.2804(3) 0.19325(14) 0.0614(13) Uani 1 1 d . . . H34A H 0.4879 -0.3375 0.1937 0.074 Uiso 1 1 calc R . . C35 C 0.4800(4) -0.1948(3) 0.17465(14) 0.0567(11) Uani 1 1 d . . . H35A H 0.5464 -0.1927 0.1619 0.068 Uiso 1 1 calc R . . C36 C 0.4174(3) -0.1107(3) 0.17458(12) 0.0439(9) Uani 1 1 d . . . H36A H 0.4416 -0.0513 0.1617 0.053 Uiso 1 1 calc R . . C41 C 0.2475(3) 0.0440(2) 0.25029(10) 0.0307(8) Uani 1 1 d . . . C42 C 0.2320(3) 0.1441(3) 0.25617(12) 0.0440(10) Uani 1 1 d . . . H42A H 0.2228 0.1861 0.2314 0.053 Uiso 1 1 calc R . . C43 C 0.2300(3) 0.1836(3) 0.29846(12) 0.0534(11) Uani 1 1 d . . . H43A H 0.2188 0.2524 0.3025 0.064 Uiso 1 1 calc R . . C44 C 0.2441(3) 0.1230(3) 0.33427(12) 0.0520(11) Uani 1 1 d . . . H44A H 0.2425 0.1499 0.3631 0.062 Uiso 1 1 calc R . . C45 C 0.2607(3) 0.0239(3) 0.32851(12) 0.0516(11) Uani 1 1 d . . . H45A H 0.2708 -0.0178 0.3534 0.062 Uiso 1 1 calc R . . C46 C 0.2628(3) -0.0161(3) 0.28652(11) 0.0405(9) Uani 1 1 d . . . H46A H 0.2748 -0.0849 0.2827 0.049 Uiso 1 1 calc R . . C51 C 0.1141(3) -0.0343(2) 0.18038(10) 0.0321(8) Uani 1 1 d . . . C52 C 0.0879(3) -0.0503(2) 0.13635(11) 0.0359(8) Uani 1 1 d . . . H52A H 0.1399 -0.0462 0.1148 0.043 Uiso 1 1 calc R . . C53 C -0.0131(3) -0.0720(3) 0.12375(12) 0.0448(10) Uani 1 1 d . . . H53A H -0.0303 -0.0825 0.0936 0.054 Uiso 1 1 calc R . . C54 C -0.0887(3) -0.0785(3) 0.15467(13) 0.0529(11) Uani 1 1 d . . . H54A H -0.1584 -0.0919 0.1458 0.064 Uiso 1 1 calc R . . C55 C -0.0633(3) -0.0655(4) 0.19835(14) 0.0676(14) Uani 1 1 d . . . H55A H -0.1149 -0.0721 0.2199 0.081 Uiso 1 1 calc R . . C56 C 0.0381(3) -0.0428(3) 0.21097(13) 0.0560(11) Uani 1 1 d . . . H56A H 0.0551 -0.0330 0.2412 0.067 Uiso 1 1 calc R . . C61 C 0.1656(3) 0.5204(2) 0.10974(11) 0.0322(8) Uani 1 1 d . . . C62 C 0.1309(3) 0.4771(3) 0.14773(12) 0.0520(11) Uani 1 1 d . . . H62A H 0.1409 0.4082 0.1524 0.062 Uiso 1 1 calc R . . C63 C 0.0815(4) 0.5330(4) 0.17915(15) 0.0746(14) Uani 1 1 d . . . H63A H 0.0584 0.5026 0.2053 0.089 Uiso 1 1 calc R . . C64 C 0.0660(3) 0.6322(4) 0.17251(17) 0.0716(15) Uani 1 1 d . . . H64A H 0.0315 0.6703 0.1940 0.086 Uiso 1 1 calc R . . C65 C 0.0998(4) 0.6764(3) 0.13523(17) 0.0649(13) Uani 1 1 d . . . H65A H 0.0891 0.7453 0.1308 0.078 Uiso 1 1 calc R . . C66 C 0.1499(3) 0.6208(3) 0.10368(14) 0.0510(11) Uani 1 1 d . . . H66A H 0.1735 0.6520 0.0778 0.061 Uiso 1 1 calc R . . C71 C 0.3640(3) 0.4717(2) 0.07171(10) 0.0304(8) Uani 1 1 d . . . C72 C 0.4294(3) 0.4091(3) 0.04913(11) 0.0366(8) Uani 1 1 d . . . H72A H 0.4019 0.3521 0.0347 0.044 Uiso 1 1 calc R . . C73 C 0.5343(3) 0.4294(3) 0.04760(12) 0.0463(10) Uani 1 1 d . . . H73A H 0.5786 0.3859 0.0322 0.056 Uiso 1 1 calc R . . C74 C 0.5750(3) 0.5110(3) 0.06788(11) 0.0461(10) Uani 1 1 d . . . H74A H 0.6471 0.5247 0.0665 0.055 Uiso 1 1 calc R . . C75 C 0.5107(3) 0.5736(3) 0.09047(13) 0.0534(11) Uani 1 1 d . . . H75A H 0.5387 0.6306 0.1046 0.064 Uiso 1 1 calc R . . C76 C 0.4062(3) 0.5538(3) 0.09255(11) 0.0427(9) Uani 1 1 d . . . H76A H 0.3627 0.5969 0.1085 0.051 Uiso 1 1 calc R . . C81 C 0.1802(3) 0.4699(3) 0.01628(11) 0.0364(8) Uani 1 1 d . . . C82 C 0.1986(3) 0.5588(3) -0.00453(12) 0.0527(11) Uani 1 1 d . . . H82A H 0.2374 0.6093 0.0100 0.063 Uiso 1 1 calc R . . C83 C 0.1595(4) 0.5737(4) -0.04735(16) 0.0779(17) Uani 1 1 d . . . H83A H 0.1714 0.6348 -0.0618 0.093 Uiso 1 1 calc R . . C84 C 0.1039(4) 0.5004(5) -0.06854(15) 0.090(2) Uani 1 1 d . . . H84A H 0.0766 0.5113 -0.0974 0.108 Uiso 1 1 calc R . . C85 C 0.0881(4) 0.4127(5) -0.04825(15) 0.0810(17) Uani 1 1 d . . . H85A H 0.0512 0.3617 -0.0634 0.097 Uiso 1 1 calc R . . C86 C 0.1252(3) 0.3962(3) -0.00560(12) 0.0545(11) Uani 1 1 d . . . H86A H 0.1128 0.3347 0.0084 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02698(9) 0.02630(9) 0.02533(9) -0.00072(8) 0.00068(6) -0.00032(8) F1 0.134(3) 0.0342(14) 0.120(2) 0.0022(15) 0.041(2) -0.0092(16) O1 0.0393(15) 0.0307(13) 0.0342(13) -0.0043(10) 0.0028(11) 0.0004(11) C1 0.071(3) 0.040(2) 0.044(2) -0.0088(19) -0.003(2) 0.011(2) F2 0.130(3) 0.0759(19) 0.102(2) -0.0318(16) -0.065(2) 0.0573(19) O2 0.0358(14) 0.0379(13) 0.0259(12) -0.0008(10) 0.0020(10) -0.0035(11) C2 0.028(2) 0.0329(19) 0.042(2) -0.0115(16) -0.0014(17) -0.0001(15) P3 0.0322(5) 0.0295(5) 0.0260(4) 0.0010(4) 0.0007(4) -0.0013(4) F3 0.124(3) 0.0522(15) 0.0641(16) -0.0259(13) 0.0028(16) 0.0267(15) O3 0.0329(13) 0.0300(12) 0.0273(12) 0.0031(9) 0.0002(10) -0.0007(10) C3 0.045(2) 0.039(2) 0.0328(19) -0.0123(16) 0.0064(17) -0.0021(17) F4 0.129(3) 0.0613(16) 0.0429(14) 0.0079(12) 0.0125(15) -0.0303(16) C4 0.031(2) 0.045(2) 0.0286(18) -0.0042(16) 0.0030(16) -0.0064(17) F5 0.135(3) 0.0809(19) 0.0355(13) -0.0092(13) 0.0265(16) 0.0013(18) C5 0.068(3) 0.056(3) 0.032(2) -0.006(2) 0.005(2) -0.010(2) P6 0.0300(5) 0.0281(5) 0.0271(5) 0.0036(4) 0.0027(4) 0.0021(4) F6 0.078(2) 0.116(2) 0.0466(15) 0.0112(14) -0.0185(14) 0.0046(17) O6 0.0345(14) 0.0302(13) 0.0325(12) -0.0008(10) 0.0006(11) 0.0007(10) F11 0.096(6) 0.187(9) 0.129(6) 0.022(6) 0.074(5) 0.052(6) F11' 0.096(6) 0.187(9) 0.129(6) 0.022(6) 0.074(5) 0.052(6) F12 0.062(4) 0.111(5) 0.279(13) -0.004(7) 0.027(6) 0.046(3) F12' 0.062(4) 0.111(5) 0.279(13) -0.004(7) 0.027(6) 0.046(3) F13 0.037(3) 0.274(14) 0.159(8) -0.148(9) -0.039(4) 0.044(6) F13' 0.037(3) 0.274(14) 0.159(8) -0.148(9) -0.039(4) 0.044(6) O11 0.0312(14) 0.0433(14) 0.0323(13) -0.0049(11) 0.0001(11) -0.0019(12) C11 0.053(3) 0.133(6) 0.053(3) -0.042(4) -0.003(3) -0.018(3) O12 0.0341(14) 0.0332(13) 0.0358(13) -0.0047(10) -0.0054(11) -0.0010(10) C12 0.031(2) 0.068(3) 0.034(2) -0.0056(18) 0.0039(18) -0.0030(19) C13 0.031(2) 0.072(3) 0.044(2) -0.018(2) -0.0077(19) -0.001(2) F14 0.164(3) 0.0382(14) 0.0731(17) -0.0147(13) -0.0437(19) 0.0204(17) C14 0.041(2) 0.0341(19) 0.0266(17) 0.0031(15) -0.0045(16) -0.0044(18) F15 0.105(2) 0.0777(18) 0.0598(16) -0.0306(14) 0.0348(16) -0.0298(16) C15 0.051(3) 0.041(2) 0.041(2) -0.0036(18) -0.010(2) -0.009(2) F16 0.0619(18) 0.110(2) 0.0760(18) -0.0533(16) -0.0100(15) -0.0182(16) F21 0.065(2) 0.213(4) 0.105(2) -0.086(2) -0.0524(19) 0.069(2) O21 0.0308(14) 0.0367(13) 0.0395(14) -0.0072(11) -0.0050(12) 0.0014(11) C21 0.046(3) 0.067(3) 0.067(3) -0.030(3) -0.017(2) 0.020(2) F22 0.089(2) 0.147(3) 0.0527(17) 0.0104(17) -0.0309(16) -0.034(2) O22 0.0257(13) 0.0419(14) 0.0315(13) -0.0006(10) -0.0003(11) -0.0004(11) C22 0.033(2) 0.034(2) 0.044(2) -0.0042(16) -0.0082(18) 0.0021(16) F23 0.093(2) 0.099(2) 0.092(2) -0.0379(18) -0.0216(18) -0.0277(18) C23 0.026(2) 0.046(2) 0.051(2) -0.0075(18) -0.0015(18) 0.0073(17) C24 0.035(2) 0.0256(17) 0.040(2) 0.0002(15) 0.0058(18) 0.0006(15) F24 0.048(2) 0.166(5) 0.062(2) -0.066(3) -0.0026(17) 0.015(2) F24' 0.048(2) 0.166(5) 0.062(2) -0.066(3) -0.0026(17) 0.015(2) F25 0.119(4) 0.083(3) 0.092(3) -0.007(2) 0.068(3) -0.033(3) F25' 0.119(4) 0.083(3) 0.092(3) -0.007(2) 0.068(3) -0.033(3) F26 0.107(4) 0.094(3) 0.076(2) -0.003(2) 0.027(2) 0.067(3) F26' 0.107(4) 0.094(3) 0.076(2) -0.003(2) 0.027(2) 0.067(3) C25 0.036(2) 0.057(3) 0.051(3) 0.002(2) 0.009(2) 0.006(2) C31 0.039(2) 0.0324(19) 0.0273(18) -0.0036(14) -0.0032(16) 0.0031(16) C32 0.053(3) 0.040(2) 0.050(2) 0.0008(18) 0.001(2) -0.0017(19) C33 0.080(4) 0.032(2) 0.062(3) 0.003(2) -0.003(3) 0.006(2) C34 0.075(4) 0.046(3) 0.062(3) -0.012(2) -0.008(3) 0.023(2) C35 0.054(3) 0.057(3) 0.059(3) -0.010(2) 0.003(2) 0.017(2) C36 0.047(3) 0.041(2) 0.043(2) -0.0037(17) -0.002(2) 0.0073(19) C41 0.0277(19) 0.0336(19) 0.0308(18) -0.0006(15) 0.0011(15) -0.0029(15) C42 0.055(3) 0.042(2) 0.035(2) 0.0030(16) 0.0033(19) 0.0037(19) C43 0.075(3) 0.042(2) 0.044(2) -0.011(2) 0.006(2) 0.000(2) C44 0.056(3) 0.068(3) 0.031(2) -0.012(2) 0.004(2) -0.007(2) C45 0.060(3) 0.063(3) 0.032(2) 0.0048(19) -0.003(2) -0.003(2) C46 0.049(2) 0.038(2) 0.035(2) 0.0010(16) -0.0007(18) -0.0027(18) C51 0.037(2) 0.0314(19) 0.0277(18) 0.0045(14) -0.0010(16) -0.0034(16) C52 0.036(2) 0.035(2) 0.037(2) 0.0007(15) 0.0016(17) -0.0048(16) C53 0.052(3) 0.040(2) 0.042(2) -0.0002(17) -0.008(2) -0.0108(19) C54 0.042(3) 0.062(3) 0.055(3) 0.005(2) -0.012(2) -0.016(2) C55 0.037(3) 0.112(4) 0.054(3) 0.003(3) 0.013(2) -0.020(3) C56 0.041(3) 0.091(3) 0.036(2) 0.002(2) -0.002(2) -0.017(2) C61 0.031(2) 0.0306(19) 0.0351(19) -0.0035(15) 0.0001(16) 0.0001(15) C62 0.055(3) 0.056(3) 0.046(2) -0.008(2) 0.017(2) -0.005(2) C63 0.081(4) 0.086(4) 0.059(3) -0.017(3) 0.031(3) -0.003(3) C64 0.045(3) 0.089(4) 0.082(4) -0.046(3) 0.017(3) 0.003(3) C65 0.054(3) 0.042(2) 0.098(4) -0.024(3) -0.007(3) 0.012(2) C66 0.050(3) 0.037(2) 0.066(3) -0.004(2) 0.003(2) 0.0012(19) C71 0.032(2) 0.0298(18) 0.0297(18) 0.0065(14) -0.0001(15) -0.0012(15) C72 0.033(2) 0.035(2) 0.043(2) 0.0002(16) 0.0060(17) -0.0047(16) C73 0.038(2) 0.051(2) 0.051(2) -0.0004(19) 0.011(2) 0.0060(19) C74 0.029(2) 0.068(3) 0.041(2) 0.005(2) 0.0032(18) -0.007(2) C75 0.042(3) 0.063(3) 0.055(3) -0.018(2) 0.005(2) -0.019(2) C76 0.039(2) 0.045(2) 0.045(2) -0.0104(18) 0.0084(19) -0.0033(18) C81 0.027(2) 0.053(2) 0.0287(18) 0.0072(17) 0.0046(16) 0.0119(17) C82 0.047(3) 0.066(3) 0.046(2) 0.023(2) 0.015(2) 0.018(2) C83 0.060(3) 0.117(5) 0.058(3) 0.054(3) 0.029(3) 0.048(3) C84 0.057(4) 0.176(7) 0.037(3) 0.025(4) 0.002(3) 0.051(4) C85 0.053(3) 0.145(5) 0.044(3) -0.002(3) -0.013(2) 0.006(3) C86 0.049(3) 0.080(3) 0.035(2) 0.003(2) -0.006(2) 0.000(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 O6 2.324(2) . ? Eu1 O3 2.330(2) . ? Eu1 O11 2.387(2) . ? Eu1 O1 2.411(2) . ? Eu1 O21 2.415(2) . ? Eu1 O12 2.422(2) . ? Eu1 O2 2.422(2) . ? Eu1 O22 2.429(2) . ? F1 C1 1.307(5) . ? O1 C2 1.247(4) . ? C1 F2 1.313(5) . ? C1 F3 1.318(4) . ? C1 C2 1.535(5) . ? O2 C4 1.248(4) . ? C2 C3 1.387(5) . ? P3 O3 1.502(2) . ? P3 C31 1.790(3) . ? P3 C51 1.800(3) . ? P3 C41 1.803(3) . ? C3 C4 1.393(5) . ? F4 C5 1.313(4) . ? C4 C5 1.536(5) . ? F5 C5 1.320(4) . ? C5 F6 1.343(5) . ? P6 O6 1.502(2) . ? P6 C71 1.793(3) . ? P6 C61 1.793(3) . ? P6 C81 1.797(3) . ? F11 F13' 1.07(2) . ? F11 C11 1.281(9) . ? F11 F12' 1.400(17) . ? F11' F13 1.083(15) . ? F11' C11 1.234(16) . ? F11' F12 1.279(18) . ? F12 F13' 1.21(2) . ? F12 C11 1.302(10) . ? F12' F13 1.138(15) . ? F12' C11 1.383(15) . ? F13 C11 1.282(7) . ? F13' C11 1.207(12) . ? O11 C12 1.252(4) . ? C11 C12 1.541(6) . ? O12 C14 1.247(4) . ? C12 C13 1.390(5) . ? C13 C14 1.375(5) . ? F14 C15 1.309(4) . ? C14 C15 1.535(5) . ? F15 C15 1.306(4) . ? C15 F16 1.320(4) . ? F21 C21 1.303(5) . ? O21 C22 1.252(4) . ? C21 F22 1.301(5) . ? C21 F23 1.324(5) . ? C21 C22 1.545(5) . ? O22 C24 1.235(4) . ? C22 C23 1.372(5) . ? C23 C24 1.394(5) . ? C24 C25 1.540(5) . ? F24 F26' 1.08(3) . ? F24 C25 1.293(5) . ? F24 F25' 1.36(4) . ? F24' F25 0.87(4) . ? F24' C25 1.23(2) . ? F24' F26 1.38(4) . ? F25 C25 1.301(5) . ? F25 F26' 1.46(3) . ? F25' F26 0.98(3) . ? F25' C25 1.27(2) . ? F26 C25 1.325(5) . ? F26' C25 1.35(2) . ? C31 C36 1.365(5) . ? C31 C32 1.406(5) . ? C32 C33 1.383(5) . ? C33 C34 1.389(6) . ? C34 C35 1.370(6) . ? C35 C36 1.394(5) . ? C41 C46 1.380(4) . ? C41 C42 1.380(5) . ? C42 C43 1.394(5) . ? C43 C44 1.372(5) . ? C44 C45 1.369(5) . ? C45 C46 1.389(5) . ? C51 C56 1.372(5) . ? C51 C52 1.391(4) . ? C52 C53 1.381(5) . ? C53 C54 1.374(5) . ? C54 C55 1.373(5) . ? C55 C56 1.388(5) . ? C61 C62 1.380(5) . ? C61 C66 1.385(5) . ? C62 C63 1.386(5) . ? C63 C64 1.370(6) . ? C64 C65 1.363(6) . ? C65 C66 1.391(6) . ? C71 C76 1.383(4) . ? C71 C72 1.388(4) . ? C72 C73 1.383(5) . ? C73 C74 1.364(5) . ? C74 C75 1.379(5) . ? C75 C76 1.377(5) . ? C81 C82 1.382(5) . ? C81 C86 1.385(5) . ? C82 C83 1.401(6) . ? C83 C84 1.375(7) . ? C84 C85 1.355(7) . ? C85 C86 1.391(5) . ? 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 O6 Eu1 O3 144.78(7) . . ? O6 Eu1 O11 105.94(8) . . ? O3 Eu1 O11 81.46(8) . . ? O6 Eu1 O1 142.68(7) . . ? O3 Eu1 O1 72.17(7) . . ? O11 Eu1 O1 79.07(8) . . ? O6 Eu1 O21 79.87(8) . . ? O3 Eu1 O21 111.49(8) . . ? O11 Eu1 O21 149.33(8) . . ? O1 Eu1 O21 78.93(8) . . ? O6 Eu1 O12 72.37(7) . . ? O3 Eu1 O12 78.08(7) . . ? O11 Eu1 O12 71.05(8) . . ? O1 Eu1 O12 140.38(7) . . ? O21 Eu1 O12 137.47(8) . . ? O6 Eu1 O2 74.43(7) . . ? O3 Eu1 O2 140.15(7) . . ? O11 Eu1 O2 78.58(7) . . ? O1 Eu1 O2 70.39(7) . . ? O21 Eu1 O2 74.05(8) . . ? O12 Eu1 O2 125.78(7) . . ? O6 Eu1 O22 79.39(7) . . ? O3 Eu1 O22 74.02(7) . . ? O11 Eu1 O22 139.99(7) . . ? O1 Eu1 O22 120.87(8) . . ? O21 Eu1 O22 70.41(7) . . ? O12 Eu1 O22 73.24(8) . . ? O2 Eu1 O22 138.80(7) . . ? C2 O1 Eu1 136.5(2) . . ? F1 C1 F2 107.9(4) . . ? F1 C1 F3 106.1(4) . . ? F2 C1 F3 106.9(4) . . ? F1 C1 C2 110.7(4) . . ? F2 C1 C2 110.4(3) . . ? F3 C1 C2 114.5(3) . . ? C4 O2 Eu1 135.4(2) . . ? O1 C2 C3 128.1(3) . . ? O1 C2 C1 113.4(3) . . ? C3 C2 C1 118.5(3) . . ? O3 P3 C31 110.82(15) . . ? O3 P3 C51 111.64(14) . . ? C31 P3 C51 107.54(16) . . ? O3 P3 C41 110.54(14) . . ? C31 P3 C41 108.78(15) . . ? C51 P3 C41 107.40(15) . . ? P3 O3 Eu1 148.77(14) . . ? C2 C3 C4 120.5(3) . . ? O2 C4 C3 128.1(3) . . ? O2 C4 C5 113.3(3) . . ? C3 C4 C5 118.5(3) . . ? F4 C5 F5 107.7(3) . . ? F4 C5 F6 107.0(4) . . ? F5 C5 F6 106.2(3) . . ? F4 C5 C4 111.8(3) . . ? F5 C5 C4 114.0(3) . . ? F6 C5 C4 109.8(3) . . ? O6 P6 C71 112.02(14) . . ? O6 P6 C61 110.54(14) . . ? C71 P6 C61 108.42(15) . . ? O6 P6 C81 109.52(15) . . ? C71 P6 C81 106.54(16) . . ? C61 P6 C81 109.70(16) . . ? P6 O6 Eu1 153.49(14) . . ? F13' F11 C11 61.1(10) . . ? F13' F11 F12' 117.3(13) . . ? C11 F11 F12' 61.9(7) . . ? F13 F11' C11 66.8(10) . . ? F13 F11' F12 120.8(16) . . ? C11 F11' F12 62.4(11) . . ? F13' F12 F11' 107.3(12) . . ? F13' F12 C11 57.2(8) . . ? F11' F12 C11 57.1(8) . . ? F13 F12' C11 60.2(9) . . ? F13 F12' F11 105.9(13) . . ? C11 F12' F11 54.8(7) . . ? F11' F13 F12' 131.5(14) . . ? F11' F13 C11 62.3(9) . . ? F12' F13 C11 69.4(9) . . ? F11 F13' C11 68.2(9) . . ? F11 F13' F12 131.6(13) . . ? C11 F13' F12 65.1(9) . . ? C12 O11 Eu1 135.3(2) . . ? F13' C11 F11' 110.7(12) . . ? F13' C11 F13 125.1(7) . . ? F11' C11 F13 50.9(7) . . ? F13' C11 F11 50.7(11) . . ? F11' C11 F11 138.4(8) . . ? F13 C11 F11 105.0(8) . . ? F13' C11 F12 57.7(11) . . ? F11' C11 F12 60.5(9) . . ? F13 C11 F12 105.4(9) . . ? F11 C11 F12 107.4(7) . . ? F13' C11 F12' 109.3(11) . . ? F11' C11 F12' 101.2(10) . . ? F13 C11 F12' 50.4(7) . . ? F11 C11 F12' 63.3(8) . . ? F12 C11 F12' 142.9(7) . . ? F13' C11 C12 118.1(6) . . ? F11' C11 C12 111.0(7) . . ? F13 C11 C12 116.6(5) . . ? F11 C11 C12 110.4(6) . . ? F12 C11 C12 111.5(5) . . ? F12' C11 C12 105.1(6) . . ? C14 O12 Eu1 135.0(2) . . ? O11 C12 C13 128.1(4) . . ? O11 C12 C11 113.7(3) . . ? C13 C12 C11 118.2(4) . . ? C14 C13 C12 121.2(3) . . ? O12 C14 C13 128.2(3) . . ? O12 C14 C15 113.3(3) . . ? C13 C14 C15 118.5(3) . . ? F15 C15 F14 106.8(4) . . ? F15 C15 F16 106.6(3) . . ? F14 C15 F16 106.5(3) . . ? F15 C15 C14 112.2(3) . . ? F14 C15 C14 110.1(3) . . ? F16 C15 C14 114.2(4) . . ? C22 O21 Eu1 134.4(2) . . ? F22 C21 F21 109.5(4) . . ? F22 C21 F23 106.7(4) . . ? F21 C21 F23 105.1(4) . . ? F22 C21 C22 112.2(4) . . ? F21 C21 C22 112.7(3) . . ? F23 C21 C22 110.2(4) . . ? C24 O22 Eu1 135.0(2) . . ? O21 C22 C23 128.1(3) . . ? O21 C22 C21 114.1(3) . . ? C23 C22 C21 117.8(3) . . ? C22 C23 C24 121.5(3) . . ? O22 C24 C23 127.7(3) . . ? O22 C24 C25 115.3(3) . . ? C23 C24 C25 117.0(3) . . ? F26' F24 C25 68.9(14) . . ? F26' F24 F25' 121.2(17) . . ? C25 F24 F25' 57.2(10) . . ? F25 F24' C25 74.7(16) . . ? F25 F24' F26 135(2) . . ? C25 F24' F26 60.8(17) . . ? F24' F25 C25 65(2) . . ? F24' F25 F26' 112.3(19) . . ? C25 F25 F26' 58.2(10) . . ? F26 F25' C25 70.9(14) . . ? F26 F25' F24 126(2) . . ? C25 F25' F24 58.9(14) . . ? F25' F26 C25 64.7(17) . . ? F25' F26 F24' 107.9(18) . . ? C25 F26 F24' 53.8(9) . . ? F24 F26' C25 63.2(11) . . ? F24 F26' F25 112.7(16) . . ? C25 F26' F25 54.9(11) . . ? F24' C25 F25' 100.9(17) . . ? F24' C25 F24 123.8(10) . . ? F25' C25 F24 63.9(17) . . ? F24' C25 F25 40.1(18) . . ? F25' C25 F25 132.2(10) . . ? F24 C25 F25 109.9(4) . . ? F24' C25 F26 65.3(19) . . ? F25' C25 F26 44.4(17) . . ? F24 C25 F26 105.8(4) . . ? F25 C25 F26 105.2(4) . . ? F24' C25 F26' 99.2(16) . . ? F25' C25 F26' 108.1(16) . . ? F24 C25 F26' 47.9(14) . . ? F25 C25 F26' 66.9(15) . . ? F26 C25 F26' 137.0(8) . . ? F24' C25 C24 122.1(10) . . ? F25' C25 C24 113.8(9) . . ? F24 C25 C24 113.0(3) . . ? F25 C25 C24 111.7(4) . . ? F26 C25 C24 110.8(3) . . ? F26' C25 C24 111.1(8) . . ? C36 C31 C32 119.3(3) . . ? C36 C31 P3 119.7(3) . . ? C32 C31 P3 121.0(3) . . ? C33 C32 C31 120.1(4) . . ? C32 C33 C34 119.4(4) . . ? C35 C34 C33 120.8(4) . . ? C34 C35 C36 119.5(4) . . ? C31 C36 C35 120.9(4) . . ? C46 C41 C42 119.5(3) . . ? C46 C41 P3 123.2(3) . . ? C42 C41 P3 117.4(3) . . ? C41 C42 C43 120.1(3) . . ? C44 C43 C42 120.0(4) . . ? C45 C44 C43 120.1(3) . . ? C44 C45 C46 120.4(4) . . ? C41 C46 C45 120.0(3) . . ? C56 C51 C52 118.6(3) . . ? C56 C51 P3 122.9(3) . . ? C52 C51 P3 118.4(3) . . ? C53 C52 C51 120.4(4) . . ? C54 C53 C52 120.3(4) . . ? C55 C54 C53 119.8(4) . . ? C54 C55 C56 119.9(4) . . ? C51 C56 C55 120.9(4) . . ? C62 C61 C66 118.6(3) . . ? C62 C61 P6 117.7(3) . . ? C66 C61 P6 123.7(3) . . ? C61 C62 C63 120.7(4) . . ? C64 C63 C62 120.0(4) . . ? C65 C64 C63 120.3(4) . . ? C64 C65 C66 120.0(4) . . ? C61 C66 C65 120.5(4) . . ? C76 C71 C72 118.7(3) . . ? C76 C71 P6 123.9(3) . . ? C72 C71 P6 117.5(3) . . ? C73 C72 C71 120.1(3) . . ? C74 C73 C72 120.8(4) . . ? C73 C74 C75 119.5(4) . . ? C76 C75 C74 120.3(4) . . ? C75 C76 C71 120.6(3) . . ? C82 C81 C86 119.8(3) . . ? C82 C81 P6 122.9(3) . . ? C86 C81 P6 117.3(3) . . ? C81 C82 C83 119.3(5) . . ? C84 C83 C82 120.3(5) . . ? C85 C84 C83 120.0(5) . . ? C84 C85 C86 120.9(5) . . ? C81 C86 C85 119.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Eu1 O1 C2 22.0(4) . . . . ? O3 Eu1 O1 C2 -164.4(3) . . . . ? O11 Eu1 O1 C2 -80.0(3) . . . . ? O21 Eu1 O1 C2 78.5(3) . . . . ? O12 Eu1 O1 C2 -121.2(3) . . . . ? O2 Eu1 O1 C2 1.7(3) . . . . ? O22 Eu1 O1 C2 137.5(3) . . . . ? O6 Eu1 O2 C4 -159.5(3) . . . . ? O3 Eu1 O2 C4 28.7(4) . . . . ? O11 Eu1 O2 C4 90.1(3) . . . . ? O1 Eu1 O2 C4 7.8(3) . . . . ? O21 Eu1 O2 C4 -75.9(3) . . . . ? O12 Eu1 O2 C4 146.5(3) . . . . ? O22 Eu1 O2 C4 -107.0(3) . . . . ? Eu1 O1 C2 C3 -5.7(6) . . . . ? Eu1 O1 C2 C1 174.6(2) . . . . ? F1 C1 C2 O1 55.6(4) . . . . ? F2 C1 C2 O1 -63.8(5) . . . . ? F3 C1 C2 O1 175.6(4) . . . . ? F1 C1 C2 C3 -124.1(4) . . . . ? F2 C1 C2 C3 116.5(4) . . . . ? F3 C1 C2 C3 -4.2(6) . . . . ? C31 P3 O3 Eu1 120.4(2) . . . . ? C51 P3 O3 Eu1 0.5(3) . . . . ? C41 P3 O3 Eu1 -118.9(2) . . . . ? O6 Eu1 O3 P3 92.3(3) . . . . ? O11 Eu1 O3 P3 -162.1(3) . . . . ? O1 Eu1 O3 P3 -80.9(2) . . . . ? O21 Eu1 O3 P3 -11.0(3) . . . . ? O12 Eu1 O3 P3 125.6(3) . . . . ? O2 Eu1 O3 P3 -101.6(3) . . . . ? O22 Eu1 O3 P3 49.8(2) . . . . ? O1 C2 C3 C4 1.7(6) . . . . ? C1 C2 C3 C4 -178.5(3) . . . . ? Eu1 O2 C4 C3 -13.9(6) . . . . ? Eu1 O2 C4 C5 163.0(2) . . . . ? C2 C3 C4 O2 8.0(6) . . . . ? C2 C3 C4 C5 -168.8(3) . . . . ? O2 C4 C5 F4 43.9(5) . . . . ? C3 C4 C5 F4 -138.9(4) . . . . ? O2 C4 C5 F5 166.3(3) . . . . ? C3 C4 C5 F5 -16.5(5) . . . . ? O2 C4 C5 F6 -74.7(4) . . . . ? C3 C4 C5 F6 102.6(4) . . . . ? C71 P6 O6 Eu1 8.7(3) . . . . ? C61 P6 O6 Eu1 -112.3(3) . . . . ? C81 P6 O6 Eu1 126.7(3) . . . . ? O3 Eu1 O6 P6 87.1(3) . . . . ? O11 Eu1 O6 P6 -10.7(3) . . . . ? O1 Eu1 O6 P6 -103.6(3) . . . . ? O21 Eu1 O6 P6 -159.8(3) . . . . ? O12 Eu1 O6 P6 52.8(3) . . . . ? O2 Eu1 O6 P6 -83.7(3) . . . . ? O22 Eu1 O6 P6 128.5(3) . . . . ? F13 F11' F12 F13' -5(2) . . . . ? C11 F11' F12 F13' 28.7(10) . . . . ? F13 F11' F12 C11 -33.9(13) . . . . ? F13' F11 F12' F13 6.6(16) . . . . ? C11 F11 F12' F13 33.5(9) . . . . ? F13' F11 F12' C11 -26.9(10) . . . . ? C11 F11' F13 F12' -5.3(16) . . . . ? F12 F11' F13 F12' 27(2) . . . . ? F12 F11' F13 C11 32.5(13) . . . . ? C11 F12' F13 F11' 5.0(15) . . . . ? F11 F12' F13 F11' -26(2) . . . . ? F11 F12' F13 C11 -31.3(8) . . . . ? F12' F11 F13' C11 27.1(9) . . . . ? C11 F11 F13' F12 -16.0(13) . . . . ? F12' F11 F13' F12 11(2) . . . . ? F11' F12 F13' F11 -12(2) . . . . ? C11 F12 F13' F11 16.4(13) . . . . ? F11' F12 F13' C11 -28.7(9) . . . . ? O6 Eu1 O11 C12 76.4(3) . . . . ? O3 Eu1 O11 C12 -68.3(3) . . . . ? O1 Eu1 O11 C12 -141.7(3) . . . . ? O21 Eu1 O11 C12 173.5(3) . . . . ? O12 Eu1 O11 C12 12.0(3) . . . . ? O2 Eu1 O11 C12 146.4(3) . . . . ? O22 Eu1 O11 C12 -16.0(4) . . . . ? F11 F13' C11 F11' -136.4(11) . . . . ? F12 F13' C11 F11' 30.5(11) . . . . ? F11 F13' C11 F13 -80.3(14) . . . . ? F12 F13' C11 F13 86.6(14) . . . . ? F12 F13' C11 F11 166.9(11) . . . . ? F11 F13' C11 F12 -166.9(11) . . . . ? F11 F13' C11 F12' -25.8(10) . . . . ? F12 F13' C11 F12' 141.1(9) . . . . ? F11 F13' C11 C12 94.2(10) . . . . ? F12 F13' C11 C12 -98.9(10) . . . . ? F13 F11' C11 F13' 119.1(11) . . . . ? F12 F11' C11 F13' -29.5(10) . . . . ? F12 F11' C11 F13 -148.6(10) . . . . ? F13 F11' C11 F11 65.5(17) . . . . ? F12 F11' C11 F11 -83.1(16) . . . . ? F13 F11' C11 F12 148.6(10) . . . . ? F13 F11' C11 F12' 3.3(10) . . . . ? F12 F11' C11 F12' -145.3(8) . . . . ? F13 F11' C11 C12 -107.8(8) . . . . ? F12 F11' C11 C12 103.6(7) . . . . ? F11' F13 C11 F13' -89.1(17) . . . . ? F12' F13 C11 F13' 86.6(16) . . . . ? F12' F13 C11 F11' 175.8(12) . . . . ? F11' F13 C11 F11 -141.3(10) . . . . ? F12' F13 C11 F11 34.5(9) . . . . ? F11' F13 C11 F12 -28.1(9) . . . . ? F12' F13 C11 F12 147.7(9) . . . . ? F11' F13 C11 F12' -175.8(12) . . . . ? F11' F13 C11 C12 96.3(10) . . . . ? F12' F13 C11 C12 -88.0(10) . . . . ? F12' F11 C11 F13' -152.7(10) . . . . ? F13' F11 C11 F11' 76.4(18) . . . . ? F12' F11 C11 F11' -76.2(16) . . . . ? F13' F11 C11 F13 123.4(10) . . . . ? F12' F11 C11 F13 -29.2(6) . . . . ? F13' F11 C11 F12 11.6(10) . . . . ? F12' F11 C11 F12 -141.1(7) . . . . ? F13' F11 C11 F12' 152.7(10) . . . . ? F13' F11 C11 C12 -110.2(8) . . . . ? F12' F11 C11 C12 97.2(7) . . . . ? F11' F12 C11 F13' 146.9(10) . . . . ? F13' F12 C11 F11' -146.9(10) . . . . ? F13' F12 C11 F13 -122.1(8) . . . . ? F11' F12 C11 F13 24.8(8) . . . . ? F13' F12 C11 F11 -10.6(9) . . . . ? F11' F12 C11 F11 136.3(9) . . . . ? F13' F12 C11 F12' -79.1(17) . . . . ? F11' F12 C11 F12' 67.8(16) . . . . ? F13' F12 C11 C12 110.4(7) . . . . ? F11' F12 C11 C12 -102.6(8) . . . . ? F13 F12' C11 F13' -120.1(11) . . . . ? F11 F12' C11 F13' 22.1(10) . . . . ? F13 F12' C11 F11' -3.4(10) . . . . ? F11 F12' C11 F11' 138.9(8) . . . . ? F11 F12' C11 F13 142.3(9) . . . . ? F13 F12' C11 F11 -142.3(9) . . . . ? F13 F12' C11 F12 -58.6(18) . . . . ? F11 F12' C11 F12 83.7(15) . . . . ? F13 F12' C11 C12 112.2(6) . . . . ? F11 F12' C11 C12 -105.5(6) . . . . ? O6 Eu1 O12 C14 -119.6(3) . . . . ? O3 Eu1 O12 C14 79.8(3) . . . . ? O11 Eu1 O12 C14 -5.2(3) . . . . ? O1 Eu1 O12 C14 38.0(3) . . . . ? O21 Eu1 O12 C14 -171.4(3) . . . . ? O2 Eu1 O12 C14 -64.8(3) . . . . ? O22 Eu1 O12 C14 156.4(3) . . . . ? Eu1 O11 C12 C13 -13.1(6) . . . . ? Eu1 O11 C12 C11 166.9(3) . . . . ? F13' C11 C12 O11 10(2) . . . . ? F11' C11 C12 O11 -119.2(15) . . . . ? F13 C11 C12 O11 -174.9(13) . . . . ? F11 C11 C12 O11 65.5(10) . . . . ? F12 C11 C12 O11 -53.8(11) . . . . ? F12' C11 C12 O11 132.2(13) . . . . ? F13' C11 C12 C13 -169.9(19) . . . . ? F11' C11 C12 C13 60.9(16) . . . . ? F13 C11 C12 C13 5.1(15) . . . . ? F11 C11 C12 C13 -114.4(9) . . . . ? F12 C11 C12 C13 126.3(11) . . . . ? F12' C11 C12 C13 -47.8(14) . . . . ? O11 C12 C13 C14 1.5(7) . . . . ? C11 C12 C13 C14 -178.5(4) . . . . ? Eu1 O12 C14 C13 -0.9(6) . . . . ? Eu1 O12 C14 C15 179.7(2) . . . . ? C12 C13 C14 O12 5.4(6) . . . . ? C12 C13 C14 C15 -175.3(3) . . . . ? O12 C14 C15 F15 59.0(4) . . . . ? C13 C14 C15 F15 -120.4(4) . . . . ? O12 C14 C15 F14 -59.8(4) . . . . ? C13 C14 C15 F14 120.8(4) . . . . ? O12 C14 C15 F16 -179.5(3) . . . . ? C13 C14 C15 F16 1.1(5) . . . . ? O6 Eu1 O21 C22 -64.6(3) . . . . ? O3 Eu1 O21 C22 80.7(3) . . . . ? O11 Eu1 O21 C22 -168.8(3) . . . . ? O1 Eu1 O21 C22 146.3(3) . . . . ? O12 Eu1 O21 C22 -15.1(4) . . . . ? O2 Eu1 O21 C22 -141.1(3) . . . . ? O22 Eu1 O21 C22 17.7(3) . . . . ? O6 Eu1 O22 C24 68.5(3) . . . . ? O3 Eu1 O22 C24 -134.9(3) . . . . ? O11 Eu1 O22 C24 170.7(3) . . . . ? O1 Eu1 O22 C24 -77.7(3) . . . . ? O21 Eu1 O22 C24 -14.4(3) . . . . ? O12 Eu1 O22 C24 143.1(3) . . . . ? O2 Eu1 O22 C24 17.4(3) . . . . ? Eu1 O21 C22 C23 -15.4(6) . . . . ? Eu1 O21 C22 C21 165.0(3) . . . . ? F22 C21 C22 O21 -43.2(5) . . . . ? F21 C21 C22 O21 -167.4(4) . . . . ? F23 C21 C22 O21 75.5(5) . . . . ? F22 C21 C22 C23 137.2(4) . . . . ? F21 C21 C22 C23 12.9(6) . . . . ? F23 C21 C22 C23 -104.1(4) . . . . ? O21 C22 C23 C24 -0.9(6) . . . . ? C21 C22 C23 C24 178.7(4) . . . . ? Eu1 O22 C24 C23 8.4(5) . . . . ? Eu1 O22 C24 C25 -171.1(2) . . . . ? C22 C23 C24 O22 4.4(6) . . . . ? C22 C23 C24 C25 -176.1(3) . . . . ? F26 F24' F25 C25 -8(2) . . . . ? C25 F24' F25 F26' 35.4(14) . . . . ? F26 F24' F25 F26' 28(3) . . . . ? F26' F24 F25' F26 -2(3) . . . . ? C25 F24 F25' F26 24.8(17) . . . . ? F26' F24 F25' C25 -27.0(16) . . . . ? F24 F25' F26 C25 -22.3(16) . . . . ? C25 F25' F26 F24' 33.0(13) . . . . ? F24 F25' F26 F24' 11(3) . . . . ? F25 F24' F26 F25' -29(3) . . . . ? C25 F24' F26 F25' -37.6(16) . . . . ? F25 F24' F26 C25 8(2) . . . . ? F25' F24 F26' C25 24.1(14) . . . . ? C25 F24 F26' F25 -24.5(10) . . . . ? F25' F24 F26' F25 0(2) . . . . ? F24' F25 F26' F24 -11(2) . . . . ? C25 F25 F26' F24 26.9(11) . . . . ? F24' F25 F26' C25 -38.2(19) . . . . ? F25 F24' C25 F25' -146.6(18) . . . . ? F26 F24' C25 F25' 27.2(15) . . . . ? F25 F24' C25 F24 -80.8(18) . . . . ? F26 F24' C25 F24 93.0(15) . . . . ? F26 F24' C25 F25 173.8(16) . . . . ? F25 F24' C25 F26 -173.8(16) . . . . ? F25 F24' C25 F26' -36.0(17) . . . . ? F26 F24' C25 F26' 137.8(11) . . . . ? F25 F24' C25 C24 86.2(18) . . . . ? F26 F24' C25 C24 -100.0(13) . . . . ? F26 F25' C25 F24' -36.5(16) . . . . ? F24 F25' C25 F24' 122.5(13) . . . . ? F26 F25' C25 F24 -158.9(14) . . . . ? F26 F25' C25 F25 -65(2) . . . . ? F24 F25' C25 F25 93.9(19) . . . . ? F24 F25' C25 F26 158.9(14) . . . . ? F26 F25' C25 F26' -140.0(14) . . . . ? F24 F25' C25 F26' 19.0(14) . . . . ? F26 F25' C25 C24 96.0(11) . . . . ? F24 F25' C25 C24 -105.0(8) . . . . ? F26' F24 C25 F24' 70(2) . . . . ? F25' F24 C25 F24' -86(2) . . . . ? F26' F24 C25 F25' 155.4(15) . . . . ? F26' F24 C25 F25 27.2(12) . . . . ? F25' F24 C25 F25 -128.2(11) . . . . ? F26' F24 C25 F26 140.3(12) . . . . ? F25' F24 C25 F26 -15.1(11) . . . . ? F25' F24 C25 F26' -155.4(15) . . . . ? F26' F24 C25 C24 -98.3(12) . . . . ? F25' F24 C25 C24 106.3(11) . . . . ? F26' F25 C25 F24' -140.9(17) . . . . ? F24' F25 C25 F25' 47(3) . . . . ? F26' F25 C25 F25' -94(2) . . . . ? F24' F25 C25 F24 119.3(15) . . . . ? F26' F25 C25 F24 -21.6(9) . . . . ? F24' F25 C25 F26 5.8(15) . . . . ? F26' F25 C25 F26 -135.1(9) . . . . ? F24' F25 C25 F26' 140.9(17) . . . . ? F24' F25 C25 C24 -114.5(15) . . . . ? F26' F25 C25 C24 104.6(9) . . . . ? F25' F26 C25 F24' 140.0(17) . . . . ? F24' F26 C25 F25' -140.0(17) . . . . ? F25' F26 C25 F24 19.6(14) . . . . ? F24' F26 C25 F24 -120.4(11) . . . . ? F25' F26 C25 F25 135.9(14) . . . . ? F24' F26 C25 F25 -4.1(11) . . . . ? F25' F26 C25 F26' 64(3) . . . . ? F24' F26 C25 F26' -76(2) . . . . ? F25' F26 C25 C24 -103.2(14) . . . . ? F24' F26 C25 C24 116.8(11) . . . . ? F24 F26' C25 F24' -127.9(14) . . . . ? F25 F26' C25 F24' 24.3(13) . . . . ? F24 F26' C25 F25' -23.2(16) . . . . ? F25 F26' C25 F25' 129.0(12) . . . . ? F25 F26' C25 F24 152.2(11) . . . . ? F24 F26' C25 F25 -152.2(11) . . . . ? F24 F26' C25 F26 -64(2) . . . . ? F25 F26' C25 F26 88(2) . . . . ? F24 F26' C25 C24 102.4(8) . . . . ? F25 F26' C25 C24 -105.4(7) . . . . ? O22 C24 C25 F24' -158(3) . . . . ? C23 C24 C25 F24' 22(3) . . . . ? O22 C24 C25 F25' 80(2) . . . . ? C23 C24 C25 F25' -99(2) . . . . ? O22 C24 C25 F24 9.8(6) . . . . ? C23 C24 C25 F24 -169.8(5) . . . . ? O22 C24 C25 F25 -114.7(5) . . . . ? C23 C24 C25 F25 65.7(6) . . . . ? O22 C24 C25 F26 128.3(5) . . . . ? C23 C24 C25 F26 -51.3(6) . . . . ? O22 C24 C25 F26' -42.1(19) . . . . ? C23 C24 C25 F26' 138.3(19) . . . . ? O3 P3 C31 C36 15.8(3) . . . . ? C51 P3 C31 C36 138.0(3) . . . . ? C41 P3 C31 C36 -105.9(3) . . . . ? O3 P3 C31 C32 -166.1(3) . . . . ? C51 P3 C31 C32 -43.8(3) . . . . ? C41 P3 C31 C32 72.2(3) . . . . ? C36 C31 C32 C33 1.7(5) . . . . ? P3 C31 C32 C33 -176.5(3) . . . . ? C31 C32 C33 C34 -0.7(6) . . . . ? C32 C33 C34 C35 -0.6(6) . . . . ? C33 C34 C35 C36 0.9(6) . . . . ? C32 C31 C36 C35 -1.3(5) . . . . ? P3 C31 C36 C35 176.9(3) . . . . ? C34 C35 C36 C31 0.0(6) . . . . ? O3 P3 C41 C46 -147.8(3) . . . . ? C31 P3 C41 C46 -26.0(4) . . . . ? C51 P3 C41 C46 90.2(3) . . . . ? O3 P3 C41 C42 32.4(3) . . . . ? C31 P3 C41 C42 154.2(3) . . . . ? C51 P3 C41 C42 -89.7(3) . . . . ? C46 C41 C42 C43 -1.3(6) . . . . ? P3 C41 C42 C43 178.5(3) . . . . ? C41 C42 C43 C44 0.5(6) . . . . ? C42 C43 C44 C45 0.3(7) . . . . ? C43 C44 C45 C46 -0.3(7) . . . . ? C42 C41 C46 C45 1.2(6) . . . . ? P3 C41 C46 C45 -178.6(3) . . . . ? C44 C45 C46 C41 -0.5(6) . . . . ? O3 P3 C51 C56 -134.8(3) . . . . ? C31 P3 C51 C56 103.4(3) . . . . ? C41 P3 C51 C56 -13.5(4) . . . . ? O3 P3 C51 C52 44.4(3) . . . . ? C31 P3 C51 C52 -77.4(3) . . . . ? C41 P3 C51 C52 165.7(3) . . . . ? C56 C51 C52 C53 1.5(5) . . . . ? P3 C51 C52 C53 -177.7(3) . . . . ? C51 C52 C53 C54 -0.3(5) . . . . ? C52 C53 C54 C55 -1.5(6) . . . . ? C53 C54 C55 C56 2.1(7) . . . . ? C52 C51 C56 C55 -0.9(6) . . . . ? P3 C51 C56 C55 178.3(3) . . . . ? C54 C55 C56 C51 -0.9(7) . . . . ? O6 P6 C61 C62 14.4(3) . . . . ? C71 P6 C61 C62 -108.7(3) . . . . ? C81 P6 C61 C62 135.3(3) . . . . ? O6 P6 C61 C66 -165.3(3) . . . . ? C71 P6 C61 C66 71.5(3) . . . . ? C81 P6 C61 C66 -44.4(4) . . . . ? C66 C61 C62 C63 -0.1(6) . . . . ? P6 C61 C62 C63 -179.9(3) . . . . ? C61 C62 C63 C64 0.5(7) . . . . ? C62 C63 C64 C65 -0.6(7) . . . . ? C63 C64 C65 C66 0.3(7) . . . . ? C62 C61 C66 C65 -0.2(6) . . . . ? P6 C61 C66 C65 179.5(3) . . . . ? C64 C65 C66 C61 0.1(6) . . . . ? O6 P6 C71 C76 -134.0(3) . . . . ? C61 P6 C71 C76 -11.7(3) . . . . ? C81 P6 C71 C76 106.3(3) . . . . ? O6 P6 C71 C72 47.6(3) . . . . ? C61 P6 C71 C72 169.9(2) . . . . ? C81 P6 C71 C72 -72.1(3) . . . . ? C76 C71 C72 C73 -0.3(5) . . . . ? P6 C71 C72 C73 178.2(3) . . . . ? C71 C72 C73 C74 -0.4(6) . . . . ? C72 C73 C74 C75 0.5(6) . . . . ? C73 C74 C75 C76 0.0(6) . . . . ? C74 C75 C76 C71 -0.7(6) . . . . ? C72 C71 C76 C75 0.8(5) . . . . ? P6 C71 C76 C75 -177.5(3) . . . . ? O6 P6 C81 C82 -171.3(3) . . . . ? C71 P6 C81 C82 -50.0(3) . . . . ? C61 P6 C81 C82 67.2(3) . . . . ? O6 P6 C81 C86 6.7(3) . . . . ? C71 P6 C81 C86 128.0(3) . . . . ? C61 P6 C81 C86 -114.8(3) . . . . ? C86 C81 C82 C83 1.1(6) . . . . ? P6 C81 C82 C83 179.1(3) . . . . ? C81 C82 C83 C84 -0.4(6) . . . . ? C82 C83 C84 C85 -1.0(7) . . . . ? C83 C84 C85 C86 1.6(8) . . . . ? C82 C81 C86 C85 -0.5(6) . . . . ? P6 C81 C86 C85 -178.6(3) . . . . ? C84 C85 C86 C81 -0.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.158 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.096 data_00079 _database_code_CSD 171070 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H33 F18 O8 P2 Tb' _chemical_formula_weight 1336.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 17.1654(10) _cell_length_b 15.4783(10) _cell_length_c 20.6482(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 93.837(10) _cell_angle_gamma 90.000(10) _cell_volume 5473.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_size_max .23 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 34667 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.31 _reflns_number_total 12899 _reflns_number_gt 9198 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12899 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.235914(9) 0.228532(10) 0.011242(7) 0.02537(6) Uani 1 1 d . . . P3 P 0.17770(5) 0.42751(6) 0.09327(4) 0.0283(2) Uani 1 1 d . . . P6 P 0.36276(5) 0.12442(6) -0.10260(4) 0.0288(2) Uani 1 1 d . . . F1 F -0.0111(2) 0.2089(2) 0.1329(2) 0.1401(19) Uani 1 1 d . . . F2 F 0.0773(3) 0.1688(3) 0.20303(17) 0.1412(19) Uani 1 1 d . . . F3 F -0.00242(19) 0.0790(2) 0.16307(16) 0.0943(10) Uani 1 1 d . . . F4 F 0.09666(19) -0.11229(18) 0.01304(18) 0.1027(12) Uani 1 1 d . . . F5 F 0.2171(2) -0.1019(2) 0.0298(2) 0.1255(15) Uani 1 1 d . . . F6 F 0.1667(3) -0.0697(2) -0.06122(18) 0.151(2) Uani 1 1 d . . . F11 F 0.01309(16) 0.1474(2) -0.13667(14) 0.0796(9) Uani 1 1 d . . . F12 F -0.02972(17) 0.2702(2) -0.1150(2) 0.1115(14) Uani 1 1 d . . . F13 F 0.01342(19) 0.2444(3) -0.20785(15) 0.1102(13) Uani 1 1 d . . . F14 F 0.2238(2) 0.4369(3) -0.22069(16) 0.1377(18) Uani 1 1 d . . . F15 F 0.3297(2) 0.37938(19) -0.18814(17) 0.1044(13) Uani 1 1 d . . . F16 F 0.2833(2) 0.47942(17) -0.13589(13) 0.0885(10) Uani 1 1 d . . . F21 F 0.44816(19) 0.1083(2) 0.21669(17) 0.1227(15) Uani 1 1 d . . . F22 F 0.3698(2) 0.0297(2) 0.16514(16) 0.1099(13) Uani 1 1 d . . . F23 F 0.3293(2) 0.1093(2) 0.23490(16) 0.1191(15) Uani 1 1 d . . . F24 F 0.5058(2) 0.3883(2) 0.14490(18) 0.1334(17) Uani 1 1 d . . . F25 F 0.5057(2) 0.3802(2) 0.04607(19) 0.1203(15) Uani 1 1 d . . . F26 F 0.42633(16) 0.46033(16) 0.08829(18) 0.0925(11) Uani 1 1 d . . . O1 O 0.13485(14) 0.19693(16) 0.08239(11) 0.0372(6) Uani 1 1 d . . . O2 O 0.19918(15) 0.07967(15) -0.00159(12) 0.0371(6) Uani 1 1 d . . . O3 O 0.19115(14) 0.35935(14) 0.04368(11) 0.0332(6) Uani 1 1 d . . . O6 O 0.33116(14) 0.16390(15) -0.04347(11) 0.0344(6) Uani 1 1 d . . . O11 O 0.12565(14) 0.22550(15) -0.06295(11) 0.0334(6) Uani 1 1 d . . . O12 O 0.25931(13) 0.32247(15) -0.07809(11) 0.0331(6) Uani 1 1 d . . . O21 O 0.29995(14) 0.16394(15) 0.10275(11) 0.0361(6) Uani 1 1 d . . . O22 O 0.34917(14) 0.31543(15) 0.04542(11) 0.0338(6) Uani 1 1 d . . . C1 C 0.0383(3) 0.1475(3) 0.1487(3) 0.0714(15) Uani 1 1 d . . . C2 C 0.0960(2) 0.1322(3) 0.09557(19) 0.0422(9) Uani 1 1 d . . . C3 C 0.0993(2) 0.0506(3) 0.0687(2) 0.0468(10) Uani 1 1 d . . . H3A H 0.0656 0.0080 0.0818 0.056 Uiso 1 1 calc R . . C4 C 0.1517(2) 0.0308(2) 0.02279(19) 0.0397(9) Uani 1 1 d . . . C5 C 0.1553(3) -0.0627(3) -0.0015(3) 0.0675(14) Uani 1 1 d . . . C11 C 0.0250(3) 0.2307(3) -0.1440(2) 0.0581(12) Uani 1 1 d . . . C12 C 0.1062(2) 0.2592(2) -0.11633(19) 0.0383(9) Uani 1 1 d . . . C13 C 0.1477(2) 0.3175(2) -0.15157(17) 0.0393(9) Uani 1 1 d . . . H13A H 0.1258 0.3388 -0.1908 0.047 Uiso 1 1 calc R . . C14 C 0.2215(2) 0.3444(2) -0.12884(17) 0.0343(8) Uani 1 1 d . . . C15 C 0.2644(3) 0.4096(3) -0.16963(19) 0.0451(10) Uani 1 1 d . . . C21 C 0.3763(3) 0.1062(3) 0.1894(2) 0.0578(12) Uani 1 1 d . . . C22 C 0.3602(2) 0.1774(2) 0.13806(17) 0.0366(9) Uani 1 1 d . . . C23 C 0.4114(2) 0.2457(3) 0.13753(18) 0.0417(10) Uani 1 1 d . . . H23A H 0.4533 0.2487 0.1685 0.050 Uiso 1 1 calc R . . C24 C 0.4009(2) 0.3109(2) 0.09058(17) 0.0326(8) Uani 1 1 d . . . C25 C 0.4592(2) 0.3858(3) 0.0927(2) 0.0455(10) Uani 1 1 d . . . C31 C 0.07615(19) 0.4316(2) 0.10816(16) 0.0288(7) Uani 1 1 d . . . C32 C 0.0496(2) 0.4609(3) 0.16554(18) 0.0434(10) Uani 1 1 d . . . H32A H 0.0850 0.4790 0.1989 0.052 Uiso 1 1 calc R . . C33 C -0.0298(3) 0.4636(3) 0.1737(2) 0.0559(12) Uani 1 1 d . . . H33A H -0.0474 0.4841 0.2125 0.067 Uiso 1 1 calc R . . C34 C -0.0824(2) 0.4365(3) 0.1257(2) 0.0520(11) Uani 1 1 d . . . H34A H -0.1356 0.4385 0.1316 0.062 Uiso 1 1 calc R . . C35 C -0.0562(2) 0.4064(3) 0.0687(2) 0.0596(13) Uani 1 1 d . . . H35A H -0.0919 0.3874 0.0359 0.071 Uiso 1 1 calc R . . C36 C 0.0228(2) 0.4038(3) 0.05957(19) 0.0476(10) Uani 1 1 d . . . H36A H 0.0400 0.3833 0.0207 0.057 Uiso 1 1 calc R . . C41 C 0.2328(2) 0.4086(2) 0.16907(16) 0.0328(8) Uani 1 1 d . . . C42 C 0.2220(2) 0.3297(3) 0.20060(17) 0.0393(9) Uani 1 1 d . . . H42A H 0.1863 0.2896 0.1827 0.047 Uiso 1 1 calc R . . C43 C 0.2644(2) 0.3117(3) 0.25825(19) 0.0502(11) Uani 1 1 d . . . H43A H 0.2567 0.2596 0.2794 0.060 Uiso 1 1 calc R . . C44 C 0.3175(3) 0.3696(3) 0.2845(2) 0.0581(13) Uani 1 1 d . . . H44A H 0.3462 0.3566 0.3231 0.070 Uiso 1 1 calc R . . C45 C 0.3288(3) 0.4473(4) 0.2540(2) 0.0678(14) Uani 1 1 d . . . H45A H 0.3649 0.4867 0.2722 0.081 Uiso 1 1 calc R . . C46 C 0.2867(2) 0.4670(3) 0.1962(2) 0.0524(11) Uani 1 1 d . . . H46A H 0.2946 0.5195 0.1757 0.063 Uiso 1 1 calc R . . C51 C 0.20707(19) 0.5309(2) 0.06354(16) 0.0288(7) Uani 1 1 d . . . C52 C 0.2589(2) 0.5327(2) 0.01513(18) 0.0368(9) Uani 1 1 d . . . H52A H 0.2777 0.4813 -0.0011 0.044 Uiso 1 1 calc R . . C53 C 0.2830(2) 0.6114(3) -0.0093(2) 0.0472(10) Uani 1 1 d . . . H53A H 0.3177 0.6126 -0.0420 0.057 Uiso 1 1 calc R . . C54 C 0.2555(2) 0.6874(3) 0.0149(2) 0.0453(10) Uani 1 1 d . . . H54A H 0.2711 0.7399 -0.0018 0.054 Uiso 1 1 calc R . . C55 C 0.2045(2) 0.6856(2) 0.06413(19) 0.0416(9) Uani 1 1 d . . . H55A H 0.1866 0.7372 0.0809 0.050 Uiso 1 1 calc R . . C56 C 0.1803(2) 0.6082(2) 0.08838(17) 0.0355(8) Uani 1 1 d . . . H56A H 0.1459 0.6075 0.1214 0.043 Uiso 1 1 calc R . . C61 C 0.38020(19) 0.0105(2) -0.09052(17) 0.0305(8) Uani 1 1 d . . . C62 C 0.3932(2) -0.0197(3) -0.02735(19) 0.0449(10) Uani 1 1 d . . . H62A H 0.3932 0.0185 0.0074 0.054 Uiso 1 1 calc R . . C63 C 0.4062(3) -0.1068(3) -0.0164(2) 0.0542(12) Uani 1 1 d . . . H63A H 0.4151 -0.1270 0.0259 0.065 Uiso 1 1 calc R . . C64 C 0.4059(2) -0.1634(3) -0.0674(2) 0.0551(12) Uani 1 1 d . . . H64A H 0.4151 -0.2218 -0.0597 0.066 Uiso 1 1 calc R . . C65 C 0.3922(3) -0.1341(3) -0.1299(2) 0.0542(12) Uani 1 1 d . . . H65A H 0.3918 -0.1727 -0.1644 0.065 Uiso 1 1 calc R . . C66 C 0.3788(2) -0.0469(2) -0.14168(19) 0.0423(9) Uani 1 1 d . . . H66A H 0.3689 -0.0272 -0.1840 0.051 Uiso 1 1 calc R . . C71 C 0.4528(2) 0.1767(2) -0.11905(16) 0.0318(8) Uani 1 1 d . . . C72 C 0.4662(2) 0.2595(2) -0.09530(19) 0.0421(9) Uani 1 1 d . . . H72A H 0.4292 0.2864 -0.0712 0.051 Uiso 1 1 calc R . . C73 C 0.5346(2) 0.3023(3) -0.1075(2) 0.0516(11) Uani 1 1 d . . . H73A H 0.5435 0.3579 -0.0917 0.062 Uiso 1 1 calc R . . C74 C 0.5893(3) 0.2625(3) -0.1428(2) 0.0527(11) Uani 1 1 d . . . H74A H 0.6352 0.2912 -0.1509 0.063 Uiso 1 1 calc R . . C75 C 0.5765(2) 0.1808(3) -0.1663(2) 0.0551(12) Uani 1 1 d . . . H75A H 0.6138 0.1546 -0.1904 0.066 Uiso 1 1 calc R . . C76 C 0.5087(2) 0.1366(3) -0.15471(18) 0.0448(10) Uani 1 1 d . . . H76A H 0.5005 0.0808 -0.1705 0.054 Uiso 1 1 calc R . . C81 C 0.2969(2) 0.1344(2) -0.17438(17) 0.0339(8) Uani 1 1 d . . . C82 C 0.2237(2) 0.0955(3) -0.17390(19) 0.0420(9) Uani 1 1 d . . . H82A H 0.2105 0.0645 -0.1377 0.050 Uiso 1 1 calc R . . C83 C 0.1708(3) 0.1028(3) -0.2268(2) 0.0522(11) Uani 1 1 d . . . H83A H 0.1219 0.0771 -0.2263 0.063 Uiso 1 1 calc R . . C84 C 0.1909(3) 0.1482(3) -0.2803(2) 0.0564(13) Uani 1 1 d . . . H84A H 0.1555 0.1522 -0.3163 0.068 Uiso 1 1 calc R . . C85 C 0.2621(3) 0.1878(3) -0.2817(2) 0.0561(12) Uani 1 1 d . . . H85A H 0.2742 0.2193 -0.3181 0.067 Uiso 1 1 calc R . . C86 C 0.3169(2) 0.1811(3) -0.22841(18) 0.0430(9) Uani 1 1 d . . . H86A H 0.3656 0.2074 -0.2291 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.03034(9) 0.02113(9) 0.02470(9) -0.00080(7) 0.00222(6) 0.00139(7) P3 0.0299(5) 0.0246(4) 0.0301(5) -0.0026(4) 0.0008(4) 0.0048(4) P6 0.0288(5) 0.0268(5) 0.0309(5) -0.0033(4) 0.0034(4) 0.0029(4) F1 0.150(4) 0.092(3) 0.194(4) 0.057(3) 0.127(3) 0.062(3) F2 0.163(4) 0.196(5) 0.072(2) -0.060(3) 0.068(2) -0.086(3) F3 0.097(2) 0.080(2) 0.114(3) 0.0108(19) 0.068(2) -0.0171(19) F4 0.105(3) 0.0444(17) 0.165(3) -0.0206(19) 0.054(2) -0.0350(17) F5 0.108(3) 0.0381(18) 0.231(5) -0.008(2) 0.016(3) 0.0162(19) F6 0.304(6) 0.058(2) 0.101(3) -0.041(2) 0.092(3) -0.075(3) F11 0.0589(18) 0.076(2) 0.100(2) -0.0028(17) -0.0210(16) -0.0244(16) F12 0.0339(17) 0.126(3) 0.173(4) -0.047(3) -0.0053(19) 0.0184(18) F13 0.076(2) 0.176(4) 0.072(2) 0.036(2) -0.0428(18) -0.038(2) F14 0.126(3) 0.185(4) 0.095(2) 0.109(3) -0.050(2) -0.081(3) F15 0.122(3) 0.0597(19) 0.143(3) 0.0284(19) 0.094(2) 0.0145(18) F16 0.155(3) 0.0467(16) 0.0666(19) 0.0002(14) 0.0308(19) -0.0358(18) F21 0.085(2) 0.145(3) 0.132(3) 0.099(3) -0.046(2) -0.019(2) F22 0.172(4) 0.053(2) 0.101(3) 0.0243(18) -0.026(2) 0.028(2) F23 0.151(3) 0.124(3) 0.090(2) 0.073(2) 0.067(2) 0.065(3) F24 0.122(3) 0.119(3) 0.145(3) 0.046(2) -0.090(3) -0.073(2) F25 0.117(3) 0.090(2) 0.164(4) -0.048(2) 0.087(3) -0.060(2) F26 0.0512(17) 0.0353(15) 0.189(3) -0.0152(18) -0.0090(19) -0.0044(13) O1 0.0403(15) 0.0330(14) 0.0394(15) 0.0011(12) 0.0104(12) -0.0046(12) O2 0.0393(15) 0.0260(13) 0.0464(15) 0.0008(11) 0.0066(12) -0.0023(12) O3 0.0420(15) 0.0233(12) 0.0349(14) -0.0045(10) 0.0068(11) 0.0046(11) O6 0.0353(14) 0.0317(14) 0.0371(14) -0.0083(11) 0.0086(11) -0.0002(11) O11 0.0342(14) 0.0360(14) 0.0295(13) -0.0006(11) 0.0000(10) -0.0016(11) O12 0.0373(14) 0.0344(14) 0.0270(13) 0.0042(11) -0.0026(10) -0.0012(11) O21 0.0404(15) 0.0340(14) 0.0336(14) 0.0041(11) 0.0000(11) 0.0014(12) O22 0.0373(14) 0.0306(13) 0.0325(13) 0.0016(11) -0.0055(11) -0.0022(11) C1 0.083(4) 0.058(3) 0.079(4) -0.005(3) 0.045(3) -0.011(3) C2 0.042(2) 0.041(2) 0.044(2) 0.0078(19) 0.0078(18) 0.0042(19) C3 0.047(3) 0.038(2) 0.057(3) 0.008(2) 0.016(2) -0.0092(19) C4 0.043(2) 0.0263(19) 0.049(2) 0.0006(17) -0.0035(19) -0.0015(17) C5 0.089(4) 0.029(2) 0.087(4) -0.001(3) 0.025(3) -0.010(3) C11 0.037(2) 0.071(3) 0.065(3) 0.016(3) -0.013(2) -0.003(2) C12 0.035(2) 0.040(2) 0.039(2) -0.0044(18) -0.0028(16) 0.0090(17) C13 0.044(2) 0.039(2) 0.033(2) 0.0060(17) -0.0084(17) 0.0010(18) C14 0.044(2) 0.0298(19) 0.0292(19) -0.0011(15) 0.0037(16) 0.0040(17) C15 0.059(3) 0.044(2) 0.033(2) 0.0039(18) 0.0008(19) -0.001(2) C21 0.058(3) 0.060(3) 0.054(3) 0.020(2) -0.009(2) 0.012(2) C22 0.040(2) 0.040(2) 0.0300(19) 0.0040(17) 0.0042(16) 0.0129(18) C23 0.036(2) 0.053(3) 0.035(2) 0.0064(18) -0.0069(16) 0.0050(18) C24 0.0284(19) 0.0330(19) 0.037(2) -0.0084(16) 0.0033(15) 0.0054(16) C25 0.035(2) 0.043(2) 0.056(3) -0.003(2) -0.010(2) 0.0016(19) C31 0.0275(18) 0.0255(18) 0.0331(19) -0.0007(15) -0.0007(14) 0.0013(14) C32 0.034(2) 0.057(3) 0.040(2) -0.0145(19) 0.0017(17) 0.0017(19) C33 0.047(3) 0.072(3) 0.051(3) -0.005(2) 0.015(2) 0.008(2) C34 0.030(2) 0.063(3) 0.063(3) 0.009(2) 0.001(2) 0.005(2) C35 0.042(3) 0.080(4) 0.054(3) -0.001(2) -0.017(2) -0.005(2) C36 0.041(2) 0.066(3) 0.035(2) -0.004(2) -0.0024(17) 0.001(2) C41 0.0296(19) 0.036(2) 0.0323(19) -0.0032(16) 0.0004(15) 0.0076(16) C42 0.037(2) 0.048(2) 0.033(2) 0.0034(17) 0.0039(16) 0.0069(18) C43 0.044(3) 0.064(3) 0.044(2) 0.016(2) 0.0084(19) 0.014(2) C44 0.046(3) 0.092(4) 0.035(2) 0.010(2) -0.0056(19) 0.018(3) C45 0.060(3) 0.086(4) 0.054(3) -0.010(3) -0.022(2) -0.008(3) C46 0.056(3) 0.048(3) 0.051(3) 0.000(2) -0.016(2) -0.003(2) C51 0.0275(18) 0.0238(17) 0.0344(19) -0.0031(15) -0.0029(14) 0.0028(14) C52 0.035(2) 0.032(2) 0.045(2) -0.0057(17) 0.0065(17) 0.0023(16) C53 0.044(2) 0.043(2) 0.056(3) -0.001(2) 0.013(2) -0.0060(19) C54 0.049(3) 0.031(2) 0.055(3) 0.0028(19) 0.001(2) -0.0098(19) C55 0.048(2) 0.026(2) 0.051(2) -0.0045(18) -0.0005(19) 0.0027(18) C56 0.039(2) 0.032(2) 0.036(2) -0.0021(16) 0.0028(16) 0.0041(17) C61 0.0268(18) 0.0283(18) 0.036(2) 0.0010(15) 0.0028(15) 0.0019(15) C62 0.051(3) 0.044(2) 0.039(2) -0.0020(19) -0.0031(18) 0.002(2) C63 0.058(3) 0.049(3) 0.056(3) 0.022(2) -0.003(2) 0.005(2) C64 0.053(3) 0.030(2) 0.083(4) 0.013(2) 0.014(2) 0.009(2) C65 0.063(3) 0.031(2) 0.071(3) -0.009(2) 0.017(2) -0.001(2) C66 0.049(2) 0.035(2) 0.043(2) -0.0048(18) 0.0065(18) 0.0027(18) C71 0.0325(19) 0.034(2) 0.0291(18) 0.0030(15) 0.0018(15) 0.0048(16) C72 0.047(2) 0.034(2) 0.047(2) -0.0021(18) 0.0095(18) -0.0028(18) C73 0.054(3) 0.042(2) 0.060(3) 0.000(2) 0.008(2) -0.012(2) C74 0.042(2) 0.064(3) 0.053(3) 0.004(2) 0.010(2) -0.017(2) C75 0.043(3) 0.065(3) 0.060(3) -0.002(2) 0.023(2) -0.004(2) C76 0.046(2) 0.045(2) 0.045(2) -0.0079(19) 0.0136(19) -0.0039(19) C81 0.039(2) 0.0272(19) 0.034(2) -0.0053(15) -0.0024(16) 0.0094(16) C82 0.042(2) 0.042(2) 0.042(2) -0.0082(18) 0.0010(18) 0.0050(19) C83 0.045(3) 0.051(3) 0.060(3) -0.017(2) -0.008(2) 0.009(2) C84 0.061(3) 0.058(3) 0.048(3) -0.023(2) -0.019(2) 0.024(2) C85 0.075(3) 0.054(3) 0.037(2) 0.004(2) -0.007(2) 0.017(3) C86 0.047(2) 0.041(2) 0.041(2) 0.0005(18) -0.0037(18) 0.0087(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O6 2.280(2) . ? Tb1 O3 2.282(2) . ? Tb1 O21 2.345(2) . ? Tb1 O11 2.354(2) . ? Tb1 O1 2.398(2) . ? Tb1 O2 2.399(2) . ? Tb1 O12 2.403(2) . ? Tb1 O22 2.430(2) . ? P3 O3 1.499(2) . ? P3 C31 1.791(3) . ? P3 C41 1.798(3) . ? P3 C51 1.798(4) . ? P6 O6 1.499(2) . ? P6 C71 1.798(4) . ? P6 C61 1.803(3) . ? P6 C81 1.810(4) . ? F1 C1 1.303(6) . ? F2 C1 1.308(6) . ? F3 C1 1.315(5) . ? F4 C5 1.316(5) . ? F5 C5 1.349(6) . ? F6 C5 1.267(6) . ? F11 C11 1.315(5) . ? F12 C11 1.301(6) . ? F13 C11 1.336(5) . ? F14 C15 1.294(5) . ? F15 C15 1.296(5) . ? F16 C15 1.314(5) . ? F21 C21 1.322(5) . ? F22 C21 1.287(6) . ? F23 C21 1.280(5) . ? F24 C25 1.299(5) . ? F25 C25 1.294(5) . ? F26 C25 1.286(4) . ? O1 C2 1.244(4) . ? O2 C4 1.243(4) . ? O11 C12 1.244(4) . ? O12 C14 1.243(4) . ? O21 C22 1.242(4) . ? O22 C24 1.245(4) . ? C1 C2 1.544(6) . ? C2 C3 1.382(5) . ? C3 C4 1.384(5) . ? C4 C5 1.533(6) . ? C11 C12 1.537(6) . ? C12 C13 1.386(5) . ? C13 C14 1.385(5) . ? C14 C15 1.534(5) . ? C21 C22 1.541(5) . ? C22 C23 1.376(5) . ? C23 C24 1.403(5) . ? C24 C25 1.530(5) . ? C31 C32 1.375(5) . ? C31 C36 1.381(5) . ? C32 C33 1.385(5) . ? C33 C34 1.361(6) . ? C34 C35 1.369(6) . ? C35 C36 1.382(6) . ? C41 C46 1.384(5) . ? C41 C42 1.403(5) . ? C42 C43 1.382(5) . ? C43 C44 1.365(6) . ? C44 C45 1.378(7) . ? C45 C46 1.387(6) . ? C51 C52 1.382(5) . ? C51 C56 1.393(5) . ? C52 C53 1.392(5) . ? C53 C54 1.373(6) . ? C54 C55 1.385(5) . ? C55 C56 1.374(5) . ? C61 C66 1.379(5) . ? C61 C62 1.390(5) . ? C62 C63 1.382(6) . ? C63 C64 1.371(6) . ? C64 C65 1.373(6) . ? C65 C66 1.387(5) . ? C71 C72 1.386(5) . ? C71 C76 1.393(5) . ? C72 C73 1.386(5) . ? C73 C74 1.373(6) . ? C74 C75 1.366(6) . ? C75 C76 1.385(5) . ? C81 C86 1.392(5) . ? C81 C82 1.393(5) . ? C82 C83 1.378(5) . ? C83 C84 1.373(6) . ? C84 C85 1.370(6) . ? C85 C86 1.402(5) . ? 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 O6 Tb1 O3 143.27(8) . . ? O6 Tb1 O21 84.21(8) . . ? O3 Tb1 O21 106.90(8) . . ? O6 Tb1 O11 103.93(8) . . ? O3 Tb1 O11 86.38(8) . . ? O21 Tb1 O11 145.97(8) . . ? O6 Tb1 O1 141.85(9) . . ? O3 Tb1 O1 74.31(8) . . ? O21 Tb1 O1 74.85(8) . . ? O11 Tb1 O1 79.14(8) . . ? O6 Tb1 O2 73.49(8) . . ? O3 Tb1 O2 142.51(8) . . ? O21 Tb1 O2 77.59(8) . . ? O11 Tb1 O2 73.44(8) . . ? O1 Tb1 O2 71.10(8) . . ? O6 Tb1 O12 73.92(8) . . ? O3 Tb1 O12 76.43(8) . . ? O21 Tb1 O12 141.52(8) . . ? O11 Tb1 O12 71.40(8) . . ? O1 Tb1 O12 139.34(8) . . ? O2 Tb1 O12 123.54(8) . . ? O6 Tb1 O22 78.48(8) . . ? O3 Tb1 O22 72.67(8) . . ? O21 Tb1 O22 71.29(8) . . ? O11 Tb1 O22 142.45(8) . . ? O1 Tb1 O22 122.19(8) . . ? O2 Tb1 O22 139.74(8) . . ? O12 Tb1 O22 73.53(8) . . ? O3 P3 C31 109.78(15) . . ? O3 P3 C41 112.59(15) . . ? C31 P3 C41 108.53(16) . . ? O3 P3 C51 109.50(15) . . ? C31 P3 C51 108.99(16) . . ? C41 P3 C51 107.37(16) . . ? O6 P6 C71 109.44(15) . . ? O6 P6 C61 110.59(15) . . ? C71 P6 C61 109.24(16) . . ? O6 P6 C81 113.08(15) . . ? C71 P6 C81 107.78(17) . . ? C61 P6 C81 106.59(16) . . ? C2 O1 Tb1 136.0(2) . . ? C4 O2 Tb1 135.6(2) . . ? P3 O3 Tb1 153.56(15) . . ? P6 O6 Tb1 153.26(15) . . ? C12 O11 Tb1 136.4(2) . . ? C14 O12 Tb1 135.1(2) . . ? C22 O21 Tb1 136.7(2) . . ? C24 O22 Tb1 134.6(2) . . ? F1 C1 F2 108.6(5) . . ? F1 C1 F3 107.3(5) . . ? F2 C1 F3 105.1(5) . . ? F1 C1 C2 111.7(4) . . ? F2 C1 C2 109.5(4) . . ? F3 C1 C2 114.3(4) . . ? O1 C2 C3 127.6(4) . . ? O1 C2 C1 114.3(4) . . ? C3 C2 C1 118.1(4) . . ? C2 C3 C4 121.7(4) . . ? O2 C4 C3 128.0(4) . . ? O2 C4 C5 113.6(4) . . ? C3 C4 C5 118.4(4) . . ? F6 C5 F4 110.0(5) . . ? F6 C5 F5 105.0(5) . . ? F4 C5 F5 102.6(4) . . ? F6 C5 C4 114.3(4) . . ? F4 C5 C4 115.4(4) . . ? F5 C5 C4 108.4(4) . . ? F12 C11 F11 106.6(4) . . ? F12 C11 F13 108.4(4) . . ? F11 C11 F13 104.8(4) . . ? F12 C11 C12 111.0(4) . . ? F11 C11 C12 112.5(4) . . ? F13 C11 C12 113.1(4) . . ? O11 C12 C13 128.4(4) . . ? O11 C12 C11 113.1(4) . . ? C13 C12 C11 118.5(4) . . ? C14 C13 C12 120.5(3) . . ? O12 C14 C13 128.2(3) . . ? O12 C14 C15 113.6(3) . . ? C13 C14 C15 118.2(3) . . ? F14 C15 F15 107.8(4) . . ? F14 C15 F16 105.4(4) . . ? F15 C15 F16 105.4(4) . . ? F14 C15 C14 114.2(4) . . ? F15 C15 C14 112.4(3) . . ? F16 C15 C14 111.1(3) . . ? F23 C21 F22 106.1(5) . . ? F23 C21 F21 107.6(4) . . ? F22 C21 F21 104.1(4) . . ? F23 C21 C22 112.6(4) . . ? F22 C21 C22 112.6(4) . . ? F21 C21 C22 113.3(4) . . ? O21 C22 C23 129.2(3) . . ? O21 C22 C21 112.8(4) . . ? C23 C22 C21 118.0(4) . . ? C22 C23 C24 120.4(3) . . ? O22 C24 C23 127.6(4) . . ? O22 C24 C25 114.3(3) . . ? C23 C24 C25 118.1(3) . . ? F26 C25 F25 107.2(4) . . ? F26 C25 F24 106.0(4) . . ? F25 C25 F24 104.1(4) . . ? F26 C25 C24 113.2(3) . . ? F25 C25 C24 111.3(3) . . ? F24 C25 C24 114.3(4) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 P3 122.8(3) . . ? C36 C31 P3 118.0(3) . . ? C31 C32 C33 120.0(4) . . ? C34 C33 C32 120.8(4) . . ? C33 C34 C35 119.4(4) . . ? C34 C35 C36 120.5(4) . . ? C31 C36 C35 120.1(4) . . ? C46 C41 C42 119.1(3) . . ? C46 C41 P3 123.0(3) . . ? C42 C41 P3 117.9(3) . . ? C43 C42 C41 119.8(4) . . ? C44 C43 C42 120.6(4) . . ? C43 C44 C45 120.2(4) . . ? C44 C45 C46 120.3(4) . . ? C41 C46 C45 120.1(4) . . ? C52 C51 C56 119.6(3) . . ? C52 C51 P3 118.3(3) . . ? C56 C51 P3 122.2(3) . . ? C51 C52 C53 120.0(3) . . ? C54 C53 C52 120.0(4) . . ? C53 C54 C55 120.0(4) . . ? C56 C55 C54 120.4(4) . . ? C55 C56 C51 120.0(4) . . ? C66 C61 C62 119.7(3) . . ? C66 C61 P6 122.0(3) . . ? C62 C61 P6 118.3(3) . . ? C63 C62 C61 119.8(4) . . ? C64 C63 C62 120.3(4) . . ? C63 C64 C65 120.2(4) . . ? C64 C65 C66 120.2(4) . . ? C61 C66 C65 119.9(4) . . ? C72 C71 C76 119.8(3) . . ? C72 C71 P6 118.3(3) . . ? C76 C71 P6 122.0(3) . . ? C73 C72 C71 120.0(4) . . ? C74 C73 C72 120.0(4) . . ? C75 C74 C73 120.3(4) . . ? C74 C75 C76 120.9(4) . . ? C75 C76 C71 119.1(4) . . ? C86 C81 C82 120.1(3) . . ? C86 C81 P6 121.7(3) . . ? C82 C81 P6 118.1(3) . . ? C83 C82 C81 120.4(4) . . ? C84 C83 C82 119.4(4) . . ? C85 C84 C83 121.3(4) . . ? C84 C85 C86 120.2(4) . . ? C81 C86 C85 118.6(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Tb1 O1 C2 -22.2(4) . . . . ? O3 Tb1 O1 C2 165.9(4) . . . . ? O21 Tb1 O1 C2 -81.2(4) . . . . ? O11 Tb1 O1 C2 76.6(4) . . . . ? O2 Tb1 O1 C2 0.6(3) . . . . ? O12 Tb1 O1 C2 120.4(3) . . . . ? O22 Tb1 O1 C2 -137.0(3) . . . . ? O6 Tb1 O2 C4 165.1(4) . . . . ? O3 Tb1 O2 C4 -24.1(4) . . . . ? O21 Tb1 O2 C4 77.5(3) . . . . ? O11 Tb1 O2 C4 -84.4(3) . . . . ? O1 Tb1 O2 C4 -0.5(3) . . . . ? O12 Tb1 O2 C4 -137.8(3) . . . . ? O22 Tb1 O2 C4 117.3(3) . . . . ? C31 P3 O3 Tb1 -108.0(3) . . . . ? C41 P3 O3 Tb1 13.0(4) . . . . ? C51 P3 O3 Tb1 132.4(3) . . . . ? O6 Tb1 O3 P3 -107.1(3) . . . . ? O21 Tb1 O3 P3 -3.7(4) . . . . ? O11 Tb1 O3 P3 144.4(3) . . . . ? O1 Tb1 O3 P3 64.6(3) . . . . ? O2 Tb1 O3 P3 87.8(4) . . . . ? O12 Tb1 O3 P3 -143.9(4) . . . . ? O22 Tb1 O3 P3 -67.2(3) . . . . ? C71 P6 O6 Tb1 126.6(3) . . . . ? C61 P6 O6 Tb1 -113.0(3) . . . . ? C81 P6 O6 Tb1 6.5(4) . . . . ? O3 Tb1 O6 P6 -96.9(3) . . . . ? O21 Tb1 O6 P6 152.5(3) . . . . ? O11 Tb1 O6 P6 6.0(3) . . . . ? O1 Tb1 O6 P6 96.1(3) . . . . ? O2 Tb1 O6 P6 73.7(3) . . . . ? O12 Tb1 O6 P6 -59.5(3) . . . . ? O22 Tb1 O6 P6 -135.5(3) . . . . ? O6 Tb1 O11 C12 -66.2(3) . . . . ? O3 Tb1 O11 C12 78.1(3) . . . . ? O21 Tb1 O11 C12 -166.6(3) . . . . ? O1 Tb1 O11 C12 152.8(4) . . . . ? O2 Tb1 O11 C12 -133.9(4) . . . . ? O12 Tb1 O11 C12 1.2(3) . . . . ? O22 Tb1 O11 C12 23.0(4) . . . . ? O6 Tb1 O12 C14 111.6(3) . . . . ? O3 Tb1 O12 C14 -90.3(3) . . . . ? O21 Tb1 O12 C14 169.5(3) . . . . ? O11 Tb1 O12 C14 0.4(3) . . . . ? O1 Tb1 O12 C14 -45.4(4) . . . . ? O2 Tb1 O12 C14 54.7(3) . . . . ? O22 Tb1 O12 C14 -165.9(3) . . . . ? O6 Tb1 O21 C22 76.5(3) . . . . ? O3 Tb1 O21 C22 -67.7(3) . . . . ? O11 Tb1 O21 C22 -177.0(3) . . . . ? O1 Tb1 O21 C22 -135.6(3) . . . . ? O2 Tb1 O21 C22 150.9(3) . . . . ? O12 Tb1 O21 C22 21.6(4) . . . . ? O22 Tb1 O21 C22 -3.2(3) . . . . ? O6 Tb1 O22 C24 -89.0(3) . . . . ? O3 Tb1 O22 C24 114.0(3) . . . . ? O21 Tb1 O22 C24 -1.3(3) . . . . ? O11 Tb1 O22 C24 173.0(3) . . . . ? O1 Tb1 O22 C24 56.1(3) . . . . ? O2 Tb1 O22 C24 -42.6(4) . . . . ? O12 Tb1 O22 C24 -165.4(3) . . . . ? Tb1 O1 C2 C3 -1.6(7) . . . . ? Tb1 O1 C2 C1 177.9(3) . . . . ? F1 C1 C2 O1 58.3(6) . . . . ? F2 C1 C2 O1 -62.0(6) . . . . ? F3 C1 C2 O1 -179.5(4) . . . . ? F1 C1 C2 C3 -122.1(5) . . . . ? F2 C1 C2 C3 117.6(5) . . . . ? F3 C1 C2 C3 0.0(7) . . . . ? O1 C2 C3 C4 2.2(7) . . . . ? C1 C2 C3 C4 -177.3(4) . . . . ? Tb1 O2 C4 C3 1.5(6) . . . . ? Tb1 O2 C4 C5 -177.0(3) . . . . ? C2 C3 C4 O2 -2.2(7) . . . . ? C2 C3 C4 C5 176.2(4) . . . . ? O2 C4 C5 F6 -38.3(7) . . . . ? C3 C4 C5 F6 143.0(5) . . . . ? O2 C4 C5 F4 -167.3(4) . . . . ? C3 C4 C5 F4 14.1(7) . . . . ? O2 C4 C5 F5 78.4(5) . . . . ? C3 C4 C5 F5 -100.2(5) . . . . ? Tb1 O11 C12 C13 -2.2(6) . . . . ? Tb1 O11 C12 C11 178.3(3) . . . . ? F12 C11 C12 O11 77.1(5) . . . . ? F11 C11 C12 O11 -42.3(5) . . . . ? F13 C11 C12 O11 -160.9(4) . . . . ? F12 C11 C12 C13 -102.4(5) . . . . ? F11 C11 C12 C13 138.2(4) . . . . ? F13 C11 C12 C13 19.7(6) . . . . ? O11 C12 C13 C14 1.3(7) . . . . ? C11 C12 C13 C14 -179.4(4) . . . . ? Tb1 O12 C14 C13 -1.2(6) . . . . ? Tb1 O12 C14 C15 178.8(2) . . . . ? C12 C13 C14 O12 0.4(6) . . . . ? C12 C13 C14 C15 -179.5(4) . . . . ? O12 C14 C15 F14 -176.2(4) . . . . ? C13 C14 C15 F14 3.7(6) . . . . ? O12 C14 C15 F15 60.6(5) . . . . ? C13 C14 C15 F15 -119.4(4) . . . . ? O12 C14 C15 F16 -57.2(5) . . . . ? C13 C14 C15 F16 122.8(4) . . . . ? Tb1 O21 C22 C23 5.9(6) . . . . ? Tb1 O21 C22 C21 -175.1(3) . . . . ? F23 C21 C22 O21 -72.7(5) . . . . ? F22 C21 C22 O21 47.2(5) . . . . ? F21 C21 C22 O21 164.9(4) . . . . ? F23 C21 C22 C23 106.4(5) . . . . ? F22 C21 C22 C23 -133.7(4) . . . . ? F21 C21 C22 C23 -15.9(6) . . . . ? O21 C22 C23 C24 -3.0(6) . . . . ? C21 C22 C23 C24 178.0(4) . . . . ? Tb1 O22 C24 C23 3.5(6) . . . . ? Tb1 O22 C24 C25 -177.6(2) . . . . ? C22 C23 C24 O22 -1.6(6) . . . . ? C22 C23 C24 C25 179.5(4) . . . . ? O22 C24 C25 F26 48.7(5) . . . . ? C23 C24 C25 F26 -132.3(4) . . . . ? O22 C24 C25 F25 -72.2(5) . . . . ? C23 C24 C25 F25 106.9(4) . . . . ? O22 C24 C25 F24 170.2(4) . . . . ? C23 C24 C25 F24 -10.8(6) . . . . ? O3 P3 C31 C32 154.4(3) . . . . ? C41 P3 C31 C32 30.9(4) . . . . ? C51 P3 C31 C32 -85.7(3) . . . . ? O3 P3 C31 C36 -25.5(3) . . . . ? C41 P3 C31 C36 -149.0(3) . . . . ? C51 P3 C31 C36 94.4(3) . . . . ? C36 C31 C32 C33 -1.0(6) . . . . ? P3 C31 C32 C33 179.1(3) . . . . ? C31 C32 C33 C34 0.7(7) . . . . ? C32 C33 C34 C35 0.0(7) . . . . ? C33 C34 C35 C36 -0.4(7) . . . . ? C32 C31 C36 C35 0.6(6) . . . . ? P3 C31 C36 C35 -179.6(3) . . . . ? C34 C35 C36 C31 0.1(7) . . . . ? O3 P3 C41 C46 120.9(3) . . . . ? C31 P3 C41 C46 -117.4(3) . . . . ? C51 P3 C41 C46 0.3(4) . . . . ? O3 P3 C41 C42 -57.0(3) . . . . ? C31 P3 C41 C42 64.7(3) . . . . ? C51 P3 C41 C42 -177.6(3) . . . . ? C46 C41 C42 C43 0.6(6) . . . . ? P3 C41 C42 C43 178.6(3) . . . . ? C41 C42 C43 C44 -0.8(6) . . . . ? C42 C43 C44 C45 0.6(7) . . . . ? C43 C44 C45 C46 -0.4(7) . . . . ? C42 C41 C46 C45 -0.3(6) . . . . ? P3 C41 C46 C45 -178.2(3) . . . . ? C44 C45 C46 C41 0.2(7) . . . . ? O3 P3 C51 C52 -21.2(3) . . . . ? C31 P3 C51 C52 -141.3(3) . . . . ? C41 P3 C51 C52 101.3(3) . . . . ? O3 P3 C51 C56 159.8(3) . . . . ? C31 P3 C51 C56 39.7(3) . . . . ? C41 P3 C51 C56 -77.7(3) . . . . ? C56 C51 C52 C53 -1.1(5) . . . . ? P3 C51 C52 C53 179.9(3) . . . . ? C51 C52 C53 C54 0.2(6) . . . . ? C52 C53 C54 C55 0.8(6) . . . . ? C53 C54 C55 C56 -1.0(6) . . . . ? C54 C55 C56 C51 0.1(6) . . . . ? C52 C51 C56 C55 0.9(5) . . . . ? P3 C51 C56 C55 179.9(3) . . . . ? O6 P6 C61 C66 153.6(3) . . . . ? C71 P6 C61 C66 -85.8(3) . . . . ? C81 P6 C61 C66 30.3(4) . . . . ? O6 P6 C61 C62 -24.5(3) . . . . ? C71 P6 C61 C62 96.0(3) . . . . ? C81 P6 C61 C62 -147.8(3) . . . . ? C66 C61 C62 C63 1.3(6) . . . . ? P6 C61 C62 C63 179.5(3) . . . . ? C61 C62 C63 C64 -0.3(6) . . . . ? C62 C63 C64 C65 -0.5(7) . . . . ? C63 C64 C65 C66 0.3(7) . . . . ? C62 C61 C66 C65 -1.5(6) . . . . ? P6 C61 C66 C65 -179.6(3) . . . . ? C64 C65 C66 C61 0.7(6) . . . . ? O6 P6 C71 C72 -23.3(3) . . . . ? C61 P6 C71 C72 -144.6(3) . . . . ? C81 P6 C71 C72 100.0(3) . . . . ? O6 P6 C71 C76 156.8(3) . . . . ? C61 P6 C71 C76 35.6(4) . . . . ? C81 P6 C71 C76 -79.8(3) . . . . ? C76 C71 C72 C73 0.4(6) . . . . ? P6 C71 C72 C73 -179.4(3) . . . . ? C71 C72 C73 C74 -0.2(6) . . . . ? C72 C73 C74 C75 0.2(7) . . . . ? C73 C74 C75 C76 -0.3(7) . . . . ? C74 C75 C76 C71 0.6(7) . . . . ? C72 C71 C76 C75 -0.6(6) . . . . ? P6 C71 C76 C75 179.2(3) . . . . ? O6 P6 C81 C86 117.1(3) . . . . ? C71 P6 C81 C86 -4.0(4) . . . . ? C61 P6 C81 C86 -121.1(3) . . . . ? O6 P6 C81 C82 -61.3(3) . . . . ? C71 P6 C81 C82 177.6(3) . . . . ? C61 P6 C81 C82 60.5(3) . . . . ? C86 C81 C82 C83 0.2(6) . . . . ? P6 C81 C82 C83 178.6(3) . . . . ? C81 C82 C83 C84 0.4(6) . . . . ? C82 C83 C84 C85 -1.1(6) . . . . ? C83 C84 C85 C86 1.3(7) . . . . ? C82 C81 C86 C85 -0.1(6) . . . . ? P6 C81 C86 C85 -178.4(3) . . . . ? C84 C85 C86 C81 -0.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.398 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.102 data_00109 _database_code_CSD 171071 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H21 Eu2 F36 N3 O15' _chemical_formula_weight 1831.57 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 P2(1)/c 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 19.580(4) _cell_length_b 14.668(3) _cell_length_c 21.290(5) _cell_angle_alpha 90.000(10) _cell_angle_beta 93.527(10) _cell_angle_gamma 90.000(10) _cell_volume 6103(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'ireg block' _exptl_crystal_colour colorless _exptl_crystal_size_max .14 _exptl_crystal_size_mid .24 _exptl_crystal_size_min .24 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 2.211 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38886 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 28.30 _reflns_number_total 14504 _reflns_number_gt 9645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14504 _refine_ls_number_parameters 910 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.215534(13) -0.182759(16) 0.424210(12) 0.02486(8) Uani 1 1 d . . . O1 O 0.20622(18) -0.2886(2) 0.33745(18) 0.0371(9) Uani 1 1 d . . . F1 F 0.2455(3) -0.4134(4) 0.2520(3) 0.124(2) Uani 1 1 d . . . C1 C 0.1798(4) -0.4129(4) 0.2731(3) 0.0576(19) Uani 1 1 d . . . Eu2 Eu 0.297027(12) 0.036236(16) 0.355309(12) 0.02357(8) Uani 1 1 d . . . O2 O 0.1642(2) -0.3152(3) 0.4656(2) 0.0449(10) Uani 1 1 d . . . C2 C 0.1875(4) -0.3692(4) 0.3347(3) 0.069(2) Uani 1 1 d . . . F2 F 0.1445(3) -0.3649(3) 0.2319(2) 0.1096(19) Uani 1 1 d . . . F3 F 0.1645(4) -0.4964(3) 0.2682(3) 0.130(2) Uani 1 1 d . . . C3 C 0.1550(5) -0.4226(5) 0.3827(4) 0.085(3) Uani 1 1 d . . . H3A H 0.1370 -0.4811 0.3720 0.102 Uiso 1 1 calc R . . F4 F 0.1143(8) -0.4356(6) 0.5447(4) 0.262(8) Uani 1 1 d . . . C4 C 0.1495(4) -0.3880(6) 0.4481(5) 0.081(3) Uani 1 1 d . . . F5 F 0.1191(6) -0.5305(4) 0.4837(4) 0.204(5) Uani 1 1 d . . . C5 C 0.1142(7) -0.4508(7) 0.4942(6) 0.103(4) Uani 1 1 d . . . F6 F 0.0488(5) -0.4353(8) 0.4750(7) 0.281(7) Uani 1 1 d . . . O11 O 0.3072(2) -0.2967(2) 0.43229(18) 0.0393(9) Uani 1 1 d . . . C11 C 0.3739(7) -0.4262(8) 0.4547(5) 0.106(4) Uani 1 1 d . . . F11 F 0.3589(6) -0.4689(7) 0.4093(4) 0.230(6) Uani 1 1 d . . . O12 O 0.2592(2) -0.2010(3) 0.53028(17) 0.0383(9) Uani 1 1 d . . . C12 C 0.3311(4) -0.3471(5) 0.4762(4) 0.068(2) Uani 1 1 d . . . F12 F 0.3908(4) -0.4807(4) 0.4991(3) 0.155(3) Uani 1 1 d . . . C13 C 0.3184(4) -0.3412(5) 0.5418(4) 0.070(2) Uani 1 1 d . . . H13A H 0.3352 -0.3865 0.5707 0.084 Uiso 1 1 calc R . . F13 F 0.4334(4) -0.3889(5) 0.4437(5) 0.195(5) Uani 1 1 d . . . C14 C 0.2800(4) -0.2658(5) 0.5621(3) 0.063(2) Uani 1 1 d . . . F14 F 0.2097(3) -0.2428(5) 0.6428(2) 0.117(2) Uani 1 1 d . . . F15 F 0.2894(3) -0.3297(3) 0.6664(2) 0.0940(16) Uani 1 1 d . . . C15 C 0.2786(4) -0.2607(5) 0.6311(3) 0.0603(19) Uani 1 1 d . . . F16 F 0.3079(3) -0.1871(3) 0.6548(2) 0.0829(14) Uani 1 1 d . . . O21 O 0.09775(18) -0.1940(2) 0.37897(18) 0.0362(9) Uani 1 1 d . . . C21 C -0.0157(3) -0.2440(6) 0.3593(4) 0.063(2) Uani 1 1 d . . . F21 F 0.0057(2) -0.2987(5) 0.3199(3) 0.165(4) Uani 1 1 d . . . O22 O 0.13561(18) -0.1179(2) 0.49425(18) 0.0362(9) Uani 1 1 d . . . C22 C 0.0427(3) -0.2045(4) 0.4047(3) 0.0483(16) Uani 1 1 d . . . F22 F -0.0496(3) -0.1782(4) 0.3307(3) 0.118(2) Uani 1 1 d . . . F23 F -0.0618(2) -0.2830(4) 0.3928(3) 0.1108(19) Uani 1 1 d . . . C23 C 0.0273(3) -0.1802(4) 0.4649(3) 0.0542(18) Uani 1 1 d . . . H23A H -0.0167 -0.1938 0.4789 0.065 Uiso 1 1 calc R . . C24 C 0.0756(3) -0.1354(4) 0.5057(3) 0.0439(15) Uani 1 1 d . . . F24 F 0.0543(3) -0.1710(4) 0.6094(2) 0.0988(17) Uani 1 1 d . . . C25 C 0.0520(3) -0.1042(5) 0.5677(4) 0.0570(19) Uani 1 1 d . . . F25 F 0.0865(3) -0.0379(4) 0.5917(3) 0.143(3) Uani 1 1 d . . . F26 F -0.0133(2) -0.0800(4) 0.5657(2) 0.0943(16) Uani 1 1 d . . . O31 O 0.31500(17) 0.1470(2) 0.44231(18) 0.0322(8) Uani 1 1 d . . . F31 F 0.3357(2) 0.2379(3) 0.5635(2) 0.0778(13) Uani 1 1 d . . . C31 C 0.3475(3) 0.2719(4) 0.5067(4) 0.0503(17) Uani 1 1 d . . . O32 O 0.41455(18) 0.0407(2) 0.39520(18) 0.0344(9) Uani 1 1 d . . . F32 F 0.2936(2) 0.3154(3) 0.4861(2) 0.0863(16) Uani 1 1 d . . . C32 C 0.3649(3) 0.1936(4) 0.4628(3) 0.0393(14) Uani 1 1 d . . . F33 F 0.3986(2) 0.3286(3) 0.5192(2) 0.0863(15) Uani 1 1 d . . . C33 C 0.4344(3) 0.1781(4) 0.4518(3) 0.0391(14) Uani 1 1 d . . . H33A H 0.4683 0.2207 0.4663 0.047 Uiso 1 1 calc R . . C34 C 0.4525(3) 0.1015(4) 0.4202(3) 0.0405(14) Uani 1 1 d . . . F34 F 0.5452(2) -0.0006(3) 0.4348(3) 0.1060(19) Uani 1 1 d . . . F35 F 0.56955(19) 0.1391(3) 0.4470(2) 0.0918(16) Uani 1 1 d . . . C35 C 0.5293(3) 0.0828(5) 0.4145(4) 0.0556(18) Uani 1 1 d . . . F36 F 0.5460(2) 0.0844(5) 0.3573(3) 0.114(2) Uani 1 1 d . . . O41 O 0.20254(17) 0.1414(2) 0.36058(18) 0.0317(8) Uani 1 1 d . . . F41 F 0.07706(18) 0.2219(3) 0.3281(2) 0.0745(13) Uani 1 1 d . . . C41 C 0.1263(3) 0.2637(4) 0.3625(4) 0.0491(17) Uani 1 1 d . . . O42 O 0.33475(17) 0.1768(2) 0.31280(18) 0.0320(8) Uani 1 1 d . . . C42 C 0.1967(3) 0.2245(3) 0.3480(3) 0.0315(12) Uani 1 1 d . . . F42 F 0.1142(2) 0.2482(3) 0.4224(2) 0.0801(14) Uani 1 1 d . . . F43 F 0.12031(19) 0.3511(2) 0.3522(3) 0.0844(16) Uani 1 1 d . . . C43 C 0.2436(3) 0.2832(3) 0.3230(3) 0.0373(14) Uani 1 1 d . . . H43A H 0.2312 0.3452 0.3162 0.045 Uiso 1 1 calc R . . F44 F 0.3636(3) 0.3015(3) 0.2178(3) 0.1038(18) Uani 1 1 d . . . C44 C 0.3083(3) 0.2543(4) 0.3076(3) 0.0347(13) Uani 1 1 d . . . C45 C 0.3549(3) 0.3244(4) 0.2781(4) 0.0526(18) Uani 1 1 d . . . F45 F 0.4143(2) 0.3261(4) 0.3054(3) 0.132(3) Uani 1 1 d . . . F46 F 0.3294(2) 0.4075(2) 0.2739(2) 0.0806(14) Uani 1 1 d . . . O51 O 0.24261(18) 0.0532(2) 0.25151(18) 0.0351(9) Uani 1 1 d . . . F51 F 0.15307(18) 0.0679(3) 0.15175(18) 0.0602(11) Uani 1 1 d . . . C51 C 0.2111(3) 0.1096(5) 0.1520(3) 0.0545(19) Uani 1 1 d . . . O52 O 0.37072(18) -0.0154(2) 0.27639(17) 0.0315(8) Uani 1 1 d . . . C52 C 0.2640(3) 0.0682(4) 0.1985(3) 0.0389(14) Uani 1 1 d . . . F52 F 0.2300(2) 0.1125(5) 0.0939(2) 0.122(2) Uani 1 1 d . . . C53 C 0.3300(3) 0.0500(4) 0.1793(3) 0.0366(13) Uani 1 1 d . . . H53A H 0.3421 0.0679 0.1386 0.044 Uiso 1 1 calc R . . F53 F 0.1997(3) 0.1954(3) 0.1687(3) 0.125(2) Uani 1 1 d . . . F54 F 0.4472(2) -0.1142(3) 0.1898(2) 0.0822(14) Uani 1 1 d . . . C54 C 0.3776(3) 0.0057(3) 0.2197(3) 0.0333(13) Uani 1 1 d . . . F55 F 0.49753(19) 0.0001(4) 0.2313(2) 0.0811(14) Uani 1 1 d . . . C55 C 0.4449(3) -0.0247(4) 0.1941(3) 0.0455(15) Uani 1 1 d . . . F56 F 0.4552(2) 0.0089(4) 0.1385(2) 0.0856(15) Uani 1 1 d . . . O60 O 0.19598(18) -0.0673(3) 0.34140(18) 0.0399(10) Uani 1 1 d . . . N61 N 0.1425(2) -0.0625(3) 0.2983(2) 0.0320(10) Uani 1 1 d . . . C62 C 0.0942(3) -0.0004(4) 0.3061(3) 0.0386(14) Uani 1 1 d . . . H62A H 0.0980 0.0399 0.3411 0.046 Uiso 1 1 calc R . . C63 C 0.0387(3) 0.0054(4) 0.2632(3) 0.0520(18) Uani 1 1 d . . . H63A H 0.0037 0.0492 0.2683 0.062 Uiso 1 1 calc R . . C64 C 0.0352(4) -0.0537(5) 0.2128(4) 0.062(2) Uani 1 1 d . . . H64A H -0.0020 -0.0498 0.1820 0.074 Uiso 1 1 calc R . . C65 C 0.0853(3) -0.1180(5) 0.2069(3) 0.0546(18) Uani 1 1 d . . . H65A H 0.0824 -0.1601 0.1729 0.065 Uiso 1 1 calc R . . C66 C 0.1395(3) -0.1207(4) 0.2507(3) 0.0431(15) Uani 1 1 d . . . H66A H 0.1749 -0.1643 0.2468 0.052 Uiso 1 1 calc R . . O70 O 0.2561(2) -0.0280(2) 0.45329(17) 0.0370(9) Uani 1 1 d . . . N71 N 0.2443(2) 0.0150(3) 0.5075(2) 0.0294(10) Uani 1 1 d . . . C72 C 0.1954(3) 0.0777(4) 0.5085(3) 0.0373(13) Uani 1 1 d . . . H72A H 0.1682 0.0916 0.4712 0.045 Uiso 1 1 calc R . . C73 C 0.1844(3) 0.1220(4) 0.5634(3) 0.0470(16) Uani 1 1 d . . . H73A H 0.1503 0.1680 0.5640 0.056 Uiso 1 1 calc R . . C74 C 0.2219(4) 0.1007(4) 0.6169(3) 0.0530(17) Uani 1 1 d . . . H74A H 0.2133 0.1302 0.6553 0.064 Uiso 1 1 calc R . . C75 C 0.2724(4) 0.0363(4) 0.6152(3) 0.0487(16) Uani 1 1 d . . . H75A H 0.2992 0.0209 0.6524 0.058 Uiso 1 1 calc R . . C76 C 0.2840(3) -0.0060(4) 0.5591(3) 0.0388(14) Uani 1 1 d . . . H76A H 0.3196 -0.0496 0.5569 0.047 Uiso 1 1 calc R . . O80 O 0.31919(18) -0.1268(2) 0.37396(19) 0.0381(9) Uani 1 1 d . . . N81 N 0.3726(2) -0.1758(3) 0.3544(2) 0.0290(10) Uani 1 1 d . . . C82 C 0.4346(3) -0.1620(4) 0.3828(3) 0.0437(15) Uani 1 1 d . . . H82A H 0.4408 -0.1196 0.4164 0.052 Uiso 1 1 calc R . . C83 C 0.4896(3) -0.2106(4) 0.3622(4) 0.0572(19) Uani 1 1 d . . . H83A H 0.5342 -0.2023 0.3817 0.069 Uiso 1 1 calc R . . C84 C 0.4790(3) -0.2709(4) 0.3135(4) 0.0550(19) Uani 1 1 d . . . H84A H 0.5165 -0.3036 0.2984 0.066 Uiso 1 1 calc R . . C85 C 0.4155(3) -0.2838(4) 0.2869(3) 0.0509(17) Uani 1 1 d . . . H85A H 0.4080 -0.3266 0.2537 0.061 Uiso 1 1 calc R . . C86 C 0.3619(3) -0.2350(4) 0.3078(3) 0.0404(14) Uani 1 1 d . . . H86A H 0.3171 -0.2435 0.2890 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02576(14) 0.02155(12) 0.02795(15) 0.00087(11) 0.00721(11) -0.00185(10) O1 0.039(2) 0.0302(19) 0.043(2) -0.0121(18) 0.0055(19) -0.0035(17) F1 0.163(6) 0.109(4) 0.106(5) -0.034(4) 0.060(4) 0.011(4) C1 0.091(6) 0.041(4) 0.041(4) -0.015(3) 0.009(4) -0.011(4) Eu2 0.01989(13) 0.02101(12) 0.03022(15) 0.00273(11) 0.00496(10) 0.00115(10) O2 0.052(3) 0.028(2) 0.057(3) -0.004(2) 0.018(2) -0.0113(19) C2 0.119(7) 0.036(4) 0.050(5) -0.008(3) -0.006(5) -0.008(4) F2 0.175(6) 0.084(3) 0.063(3) -0.009(3) -0.045(4) 0.013(4) F3 0.234(7) 0.054(3) 0.099(4) -0.027(3) -0.006(4) -0.044(4) C3 0.130(8) 0.052(4) 0.076(6) -0.009(4) 0.026(6) -0.020(5) F4 0.59(2) 0.126(6) 0.079(5) -0.011(5) 0.103(9) -0.093(9) C4 0.073(5) 0.062(5) 0.110(8) 0.024(5) 0.030(5) -0.007(4) F5 0.409(14) 0.058(4) 0.162(7) 0.014(4) 0.155(8) -0.039(6) C5 0.124(9) 0.076(7) 0.111(9) 0.025(6) 0.017(7) -0.077(7) F6 0.178(9) 0.281(14) 0.388(19) 0.200(13) 0.041(10) -0.079(9) O11 0.049(2) 0.034(2) 0.036(2) 0.0145(18) 0.0107(19) 0.0132(18) C11 0.141(10) 0.087(7) 0.095(8) 0.056(6) 0.055(7) 0.092(7) F11 0.292(13) 0.267(12) 0.123(7) -0.112(8) -0.055(7) 0.116(10) O12 0.051(2) 0.035(2) 0.029(2) 0.0061(17) 0.0008(19) 0.0075(18) C12 0.070(5) 0.050(4) 0.086(6) 0.007(4) 0.024(5) 0.007(4) F12 0.279(9) 0.082(4) 0.108(5) 0.033(4) 0.044(5) 0.060(5) C13 0.089(6) 0.064(5) 0.059(5) 0.018(4) 0.014(4) 0.014(4) F13 0.191(8) 0.144(6) 0.265(11) 0.092(7) 0.142(8) 0.116(6) C14 0.102(6) 0.042(4) 0.044(4) -0.002(3) 0.006(4) 0.008(4) F14 0.119(5) 0.158(6) 0.079(4) 0.015(4) 0.034(3) 0.008(4) F15 0.158(5) 0.076(3) 0.046(3) 0.025(2) -0.002(3) 0.017(3) C15 0.076(5) 0.060(5) 0.044(4) 0.006(4) -0.007(4) -0.002(4) F16 0.113(4) 0.075(3) 0.059(3) -0.008(2) -0.006(3) -0.017(3) O21 0.027(2) 0.042(2) 0.040(2) -0.0009(18) 0.0052(17) -0.0088(17) C21 0.030(3) 0.068(5) 0.091(6) -0.024(5) 0.001(4) -0.013(3) F21 0.055(3) 0.233(7) 0.206(7) -0.180(6) 0.000(4) -0.014(4) O22 0.031(2) 0.036(2) 0.043(2) -0.0046(18) 0.0138(18) -0.0056(17) C22 0.038(3) 0.042(3) 0.064(5) -0.003(3) 0.001(3) -0.009(3) F22 0.094(4) 0.121(5) 0.130(5) -0.002(4) -0.055(4) -0.008(3) F23 0.069(3) 0.143(5) 0.121(5) -0.024(4) 0.009(3) -0.064(3) C23 0.039(4) 0.059(4) 0.067(5) -0.019(4) 0.024(3) -0.014(3) C24 0.041(3) 0.043(3) 0.051(4) -0.007(3) 0.022(3) -0.005(3) F24 0.110(4) 0.131(5) 0.057(3) 0.010(3) 0.020(3) 0.006(3) C25 0.044(4) 0.067(5) 0.063(5) -0.013(4) 0.025(4) -0.018(4) F25 0.136(5) 0.172(6) 0.133(5) -0.113(5) 0.098(4) -0.100(4) F26 0.070(3) 0.124(4) 0.093(4) -0.022(3) 0.041(3) 0.020(3) O31 0.0276(19) 0.0290(18) 0.041(2) -0.0047(17) 0.0078(17) -0.0048(16) F31 0.110(4) 0.072(3) 0.054(3) -0.018(2) 0.021(3) -0.004(3) C31 0.053(4) 0.033(3) 0.067(5) -0.009(3) 0.011(4) -0.009(3) O32 0.0277(19) 0.035(2) 0.040(2) 0.0005(18) -0.0014(17) 0.0038(16) F32 0.096(3) 0.070(3) 0.090(4) -0.035(2) -0.023(3) 0.045(3) C32 0.045(3) 0.031(3) 0.043(4) 0.002(3) 0.011(3) -0.002(3) F33 0.082(3) 0.055(3) 0.122(4) -0.036(3) 0.012(3) -0.019(2) C33 0.032(3) 0.037(3) 0.049(4) -0.009(3) 0.004(3) -0.013(2) C34 0.028(3) 0.049(3) 0.045(4) 0.005(3) 0.002(3) -0.003(3) F34 0.036(2) 0.086(3) 0.194(6) 0.011(4) -0.002(3) 0.017(2) F35 0.033(2) 0.111(4) 0.130(4) -0.053(3) -0.006(2) -0.012(2) C35 0.027(3) 0.069(5) 0.070(5) -0.010(4) -0.008(3) -0.002(3) F36 0.042(3) 0.220(7) 0.083(4) -0.032(4) 0.024(3) -0.006(3) O41 0.0256(18) 0.0274(18) 0.043(2) 0.0045(17) 0.0088(17) 0.0023(15) F41 0.031(2) 0.071(3) 0.121(4) -0.009(3) -0.003(2) 0.0060(19) C41 0.036(3) 0.029(3) 0.084(5) 0.009(3) 0.014(4) 0.006(3) O42 0.0235(18) 0.0260(18) 0.047(2) 0.0075(17) 0.0073(17) 0.0002(15) C42 0.025(3) 0.029(3) 0.041(3) 0.001(2) 0.004(2) 0.007(2) F42 0.071(3) 0.094(3) 0.079(3) 0.013(3) 0.039(2) 0.036(2) F43 0.055(2) 0.035(2) 0.168(5) 0.022(3) 0.044(3) 0.0216(18) C43 0.034(3) 0.023(2) 0.056(4) 0.007(3) 0.010(3) 0.001(2) F44 0.128(4) 0.082(3) 0.111(4) 0.022(3) 0.079(4) -0.006(3) C44 0.026(3) 0.030(3) 0.048(4) 0.005(3) 0.005(3) -0.006(2) C45 0.042(4) 0.030(3) 0.087(6) 0.013(3) 0.016(4) -0.002(3) F45 0.046(3) 0.122(4) 0.222(7) 0.111(5) -0.040(3) -0.049(3) F46 0.082(3) 0.036(2) 0.129(4) 0.026(2) 0.048(3) 0.004(2) O51 0.0270(19) 0.042(2) 0.036(2) 0.0129(18) -0.0013(17) -0.0022(16) F51 0.040(2) 0.079(3) 0.059(3) 0.021(2) -0.0144(19) -0.0122(19) C51 0.051(4) 0.056(4) 0.054(5) 0.027(4) -0.020(3) -0.010(3) O52 0.033(2) 0.0328(19) 0.029(2) 0.0057(17) 0.0078(17) 0.0066(16) C52 0.041(3) 0.032(3) 0.043(4) 0.010(3) -0.003(3) -0.006(3) F52 0.065(3) 0.233(7) 0.065(3) 0.088(4) -0.012(3) -0.014(4) C53 0.044(3) 0.036(3) 0.030(3) 0.008(3) 0.005(3) -0.009(3) F53 0.139(5) 0.051(3) 0.172(6) 0.026(3) -0.097(4) 0.009(3) F54 0.064(3) 0.051(2) 0.136(4) -0.015(3) 0.052(3) 0.008(2) C54 0.037(3) 0.026(3) 0.038(3) -0.002(2) 0.011(3) -0.001(2) F55 0.034(2) 0.133(4) 0.077(3) -0.032(3) 0.009(2) -0.004(2) C55 0.048(4) 0.044(3) 0.047(4) 0.000(3) 0.022(3) 0.000(3) F56 0.073(3) 0.128(4) 0.060(3) 0.024(3) 0.041(2) 0.025(3) O60 0.034(2) 0.041(2) 0.044(3) 0.0146(19) -0.0119(19) -0.0110(17) N61 0.027(2) 0.033(2) 0.035(3) 0.009(2) -0.005(2) -0.0073(19) C62 0.035(3) 0.036(3) 0.045(4) 0.001(3) -0.004(3) 0.000(3) C63 0.034(3) 0.050(4) 0.070(5) 0.004(4) -0.014(3) 0.003(3) C64 0.053(4) 0.066(5) 0.062(5) 0.013(4) -0.033(4) -0.016(4) C65 0.063(4) 0.053(4) 0.045(4) -0.012(3) -0.016(3) -0.006(3) C66 0.044(3) 0.042(3) 0.043(4) -0.003(3) 0.005(3) 0.001(3) O70 0.056(3) 0.0298(19) 0.027(2) -0.0063(16) 0.0173(19) -0.0076(18) N71 0.031(2) 0.030(2) 0.029(2) -0.0073(19) 0.010(2) -0.0074(19) C72 0.036(3) 0.034(3) 0.042(4) -0.006(3) 0.004(3) 0.001(2) C73 0.045(4) 0.043(3) 0.054(4) -0.005(3) 0.013(3) 0.006(3) C74 0.075(5) 0.041(3) 0.045(4) -0.012(3) 0.025(4) -0.007(3) C75 0.067(4) 0.048(4) 0.032(3) -0.011(3) 0.001(3) -0.006(3) C76 0.039(3) 0.037(3) 0.040(4) -0.005(3) -0.005(3) -0.002(3) O80 0.033(2) 0.0226(18) 0.062(3) 0.0073(18) 0.0239(19) 0.0089(15) N81 0.024(2) 0.024(2) 0.040(3) 0.006(2) 0.011(2) 0.0056(17) C82 0.037(3) 0.036(3) 0.057(4) -0.005(3) -0.007(3) 0.002(3) C83 0.027(3) 0.050(4) 0.093(6) -0.001(4) -0.006(4) 0.013(3) C84 0.041(4) 0.039(3) 0.089(6) 0.003(4) 0.035(4) 0.014(3) C85 0.051(4) 0.051(4) 0.052(4) -0.008(3) 0.012(3) 0.012(3) C86 0.034(3) 0.052(4) 0.035(3) -0.004(3) 0.000(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O12 2.380(4) . ? Eu1 O2 2.380(4) . ? Eu1 O1 2.411(4) . ? Eu1 O22 2.422(4) . ? Eu1 O21 2.450(4) . ? Eu1 O11 2.450(4) . ? Eu1 O60 2.457(4) . ? Eu1 O70 2.471(3) . ? Eu1 O80 2.491(3) . ? Eu1 Eu2 3.9120(8) . ? O1 C2 1.239(7) . ? F1 C1 1.389(9) . ? C1 F3 1.263(8) . ? C1 F2 1.292(8) . ? C1 C2 1.459(9) . ? Eu2 O42 2.387(3) . ? Eu2 O52 2.403(4) . ? Eu2 O32 2.404(4) . ? Eu2 O51 2.407(4) . ? Eu2 O41 2.417(3) . ? Eu2 O80 2.459(3) . ? Eu2 O70 2.467(4) . ? Eu2 O31 2.473(4) . ? Eu2 O60 2.498(3) . ? O2 C4 1.162(9) . ? C2 C3 1.464(11) . ? C3 C4 1.491(12) . ? F4 C5 1.098(13) . ? C4 C5 1.541(11) . ? F5 C5 1.195(12) . ? C5 F6 1.338(14) . ? O11 C12 1.259(8) . ? C11 F11 1.174(14) . ? C11 F12 1.266(9) . ? C11 F13 1.323(14) . ? C11 C12 1.519(11) . ? O12 C14 1.222(7) . ? C12 C13 1.436(10) . ? C13 C14 1.420(10) . ? C14 C15 1.473(10) . ? F14 C15 1.413(9) . ? F15 C15 1.271(8) . ? C15 F16 1.309(8) . ? O21 C22 1.249(7) . ? C21 F21 1.251(8) . ? C21 F22 1.302(9) . ? C21 F23 1.316(9) . ? C21 C22 1.562(9) . ? O22 C24 1.242(6) . ? C22 C23 1.380(9) . ? C23 C24 1.407(8) . ? C24 C25 1.497(9) . ? F24 C25 1.322(8) . ? C25 F25 1.272(7) . ? C25 F26 1.324(7) . ? O31 C32 1.250(6) . ? F31 C31 1.342(8) . ? C31 F32 1.286(7) . ? C31 F33 1.315(7) . ? C31 C32 1.532(8) . ? O32 C34 1.259(6) . ? C32 C33 1.412(8) . ? C33 C34 1.368(8) . ? C34 C35 1.541(8) . ? F34 C35 1.329(8) . ? F35 C35 1.309(7) . ? C35 F36 1.281(8) . ? O41 C42 1.252(6) . ? F41 C41 1.324(7) . ? C41 F43 1.306(6) . ? C41 F42 1.330(8) . ? C41 C42 1.542(7) . ? O42 C44 1.250(6) . ? C42 C43 1.388(7) . ? C43 C44 1.395(7) . ? F44 C45 1.349(9) . ? C44 C45 1.535(8) . ? C45 F45 1.269(8) . ? C45 F46 1.318(7) . ? O51 C52 1.247(7) . ? F51 C51 1.291(7) . ? C51 F52 1.313(8) . ? C51 F53 1.332(9) . ? C51 C52 1.514(8) . ? O52 C54 1.260(6) . ? C52 C53 1.405(8) . ? C53 C54 1.391(8) . ? F54 C55 1.317(7) . ? C54 C55 1.524(8) . ? F55 C55 1.313(7) . ? C55 F56 1.309(7) . ? O60 N61 1.350(5) . ? N61 C66 1.324(7) . ? N61 C62 1.332(7) . ? C62 C63 1.378(8) . ? C63 C64 1.378(10) . ? C64 C65 1.372(10) . ? C65 C66 1.370(8) . ? O70 N71 1.349(5) . ? N71 C72 1.328(7) . ? N71 C76 1.341(7) . ? C72 C73 1.365(8) . ? C73 C74 1.353(9) . ? C74 C75 1.370(9) . ? C75 C76 1.376(8) . ? O80 N81 1.356(5) . ? N81 C86 1.324(7) . ? N81 C82 1.338(7) . ? C82 C83 1.385(8) . ? C83 C84 1.368(9) . ? C84 C85 1.349(9) . ? C85 C86 1.367(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 Eu1 O2 72.10(14) . . ? O12 Eu1 O1 131.34(13) . . ? O2 Eu1 O1 75.18(14) . . ? O12 Eu1 O22 70.60(13) . . ? O2 Eu1 O22 77.85(13) . . ? O1 Eu1 O22 134.70(12) . . ? O12 Eu1 O21 129.80(13) . . ? O2 Eu1 O21 71.44(14) . . ? O1 Eu1 O21 68.30(12) . . ? O22 Eu1 O21 68.91(12) . . ? O12 Eu1 O11 68.78(13) . . ? O2 Eu1 O11 75.01(13) . . ? O1 Eu1 O11 68.61(13) . . ? O22 Eu1 O11 136.29(13) . . ? O21 Eu1 O11 130.47(13) . . ? O12 Eu1 O60 142.11(13) . . ? O2 Eu1 O60 140.97(13) . . ? O1 Eu1 O60 83.84(13) . . ? O22 Eu1 O60 95.34(13) . . ? O21 Eu1 O60 70.31(12) . . ? O11 Eu1 O60 126.98(13) . . ? O12 Eu1 O70 76.96(12) . . ? O2 Eu1 O70 142.50(13) . . ? O1 Eu1 O70 142.31(12) . . ? O22 Eu1 O70 72.21(12) . . ? O21 Eu1 O70 116.15(13) . . ? O11 Eu1 O70 112.74(13) . . ? O60 Eu1 O70 65.18(12) . . ? O12 Eu1 O80 100.94(13) . . ? O2 Eu1 O80 143.25(12) . . ? O1 Eu1 O80 84.73(13) . . ? O22 Eu1 O80 135.20(12) . . ? O21 Eu1 O80 128.73(13) . . ? O11 Eu1 O80 69.05(12) . . ? O60 Eu1 O80 63.90(12) . . ? O70 Eu1 O80 63.09(12) . . ? O12 Eu1 Eu2 108.48(9) . . ? O2 Eu1 Eu2 179.10(11) . . ? O1 Eu1 Eu2 104.75(9) . . ? O22 Eu1 Eu2 101.66(9) . . ? O21 Eu1 Eu2 107.69(9) . . ? O11 Eu1 Eu2 105.83(9) . . ? O60 Eu1 Eu2 38.22(8) . . ? O70 Eu1 Eu2 37.58(8) . . ? O80 Eu1 Eu2 37.49(7) . . ? C2 O1 Eu1 131.2(4) . . ? F3 C1 F2 111.0(7) . . ? F3 C1 F1 100.8(7) . . ? F2 C1 F1 104.4(6) . . ? F3 C1 C2 120.8(7) . . ? F2 C1 C2 113.1(6) . . ? F1 C1 C2 104.3(6) . . ? O42 Eu2 O52 78.10(12) . . ? O42 Eu2 O32 78.38(12) . . ? O52 Eu2 O32 69.69(12) . . ? O42 Eu2 O51 72.09(12) . . ? O52 Eu2 O51 68.99(12) . . ? O32 Eu2 O51 132.97(13) . . ? O42 Eu2 O41 73.85(11) . . ? O52 Eu2 O41 136.69(12) . . ? O32 Eu2 O41 133.23(12) . . ? O51 Eu2 O41 71.32(13) . . ? O42 Eu2 O80 147.76(11) . . ? O52 Eu2 O80 72.48(12) . . ? O32 Eu2 O80 79.27(12) . . ? O51 Eu2 O80 108.21(13) . . ? O41 Eu2 O80 137.86(11) . . ? O42 Eu2 O70 140.76(12) . . ? O52 Eu2 O70 135.33(12) . . ? O32 Eu2 O70 93.76(13) . . ? O51 Eu2 O70 131.86(12) . . ? O41 Eu2 O70 85.12(12) . . ? O80 Eu2 O70 63.60(12) . . ? O42 Eu2 O31 71.54(12) . . ? O52 Eu2 O31 131.81(12) . . ? O32 Eu2 O31 68.19(12) . . ? O51 Eu2 O31 130.89(12) . . ? O41 Eu2 O31 67.66(12) . . ? O80 Eu2 O31 120.17(13) . . ? O70 Eu2 O31 69.89(12) . . ? O42 Eu2 O60 137.88(12) . . ? O52 Eu2 O60 103.35(13) . . ? O32 Eu2 O60 142.42(12) . . ? O51 Eu2 O60 69.59(12) . . ? O41 Eu2 O60 77.92(12) . . ? O80 Eu2 O60 63.78(12) . . ? O70 Eu2 O60 64.65(12) . . ? O31 Eu2 O60 124.31(12) . . ? O42 Eu2 Eu1 173.86(8) . . ? O52 Eu2 Eu1 106.25(8) . . ? O32 Eu2 Eu1 107.07(9) . . ? O51 Eu2 Eu1 105.15(9) . . ? O41 Eu2 Eu1 100.12(8) . . ? O80 Eu2 Eu1 38.07(8) . . ? O70 Eu2 Eu1 37.65(8) . . ? O31 Eu2 Eu1 107.53(8) . . ? O60 Eu2 Eu1 37.50(8) . . ? C4 O2 Eu1 137.2(5) . . ? O1 C2 C1 118.5(7) . . ? O1 C2 C3 128.1(7) . . ? C1 C2 C3 111.6(6) . . ? C2 C3 C4 122.0(7) . . ? O2 C4 C3 125.5(7) . . ? O2 C4 C5 117.2(9) . . ? C3 C4 C5 116.9(8) . . ? F4 C5 F5 112.7(12) . . ? F4 C5 F6 102.1(15) . . ? F5 C5 F6 101.2(10) . . ? F4 C5 C4 121.9(10) . . ? F5 C5 C4 114.9(11) . . ? F6 C5 C4 99.3(10) . . ? C12 O11 Eu1 133.6(4) . . ? F11 C11 F12 108.6(11) . . ? F11 C11 F13 104.6(11) . . ? F12 C11 F13 101.6(11) . . ? F11 C11 C12 122.8(12) . . ? F12 C11 C12 112.4(8) . . ? F13 C11 C12 104.2(10) . . ? C14 O12 Eu1 134.5(4) . . ? O11 C12 C13 127.5(7) . . ? O11 C12 C11 114.3(7) . . ? C13 C12 C11 118.0(7) . . ? C14 C13 C12 117.9(7) . . ? O12 C14 C13 127.0(7) . . ? O12 C14 C15 119.2(6) . . ? C13 C14 C15 112.6(7) . . ? F15 C15 F16 112.1(6) . . ? F15 C15 F14 99.7(7) . . ? F16 C15 F14 100.3(6) . . ? F15 C15 C14 122.5(7) . . ? F16 C15 C14 113.0(7) . . ? F14 C15 C14 105.2(6) . . ? C22 O21 Eu1 130.8(4) . . ? F21 C21 F22 110.1(9) . . ? F21 C21 F23 110.7(7) . . ? F22 C21 F23 103.2(6) . . ? F21 C21 C22 113.0(6) . . ? F22 C21 C22 110.3(6) . . ? F23 C21 C22 109.1(7) . . ? C24 O22 Eu1 134.0(4) . . ? O21 C22 C23 128.3(6) . . ? O21 C22 C21 113.1(6) . . ? C23 C22 C21 118.5(6) . . ? C22 C23 C24 121.2(6) . . ? O22 C24 C23 125.6(6) . . ? O22 C24 C25 117.2(6) . . ? C23 C24 C25 117.1(5) . . ? F25 C25 F24 107.6(7) . . ? F25 C25 F26 107.2(7) . . ? F24 C25 F26 102.4(6) . . ? F25 C25 C24 113.7(6) . . ? F24 C25 C24 111.4(6) . . ? F26 C25 C24 113.7(6) . . ? C32 O31 Eu2 133.9(4) . . ? F32 C31 F33 110.7(5) . . ? F32 C31 F31 108.1(6) . . ? F33 C31 F31 102.9(6) . . ? F32 C31 C32 111.9(6) . . ? F33 C31 C32 113.6(6) . . ? F31 C31 C32 109.1(5) . . ? C34 O32 Eu2 134.1(3) . . ? O31 C32 C33 126.5(5) . . ? O31 C32 C31 115.1(5) . . ? C33 C32 C31 118.4(5) . . ? C34 C33 C32 119.7(5) . . ? O32 C34 C33 128.8(5) . . ? O32 C34 C35 113.2(5) . . ? C33 C34 C35 118.1(5) . . ? F36 C35 F35 108.1(6) . . ? F36 C35 F34 105.0(7) . . ? F35 C35 F34 106.7(6) . . ? F36 C35 C34 112.3(6) . . ? F35 C35 C34 113.8(6) . . ? F34 C35 C34 110.4(6) . . ? C42 O41 Eu2 132.2(3) . . ? F43 C41 F41 107.8(5) . . ? F43 C41 F42 108.1(6) . . ? F41 C41 F42 106.5(5) . . ? F43 C41 C42 113.9(5) . . ? F41 C41 C42 110.3(5) . . ? F42 C41 C42 110.0(5) . . ? C44 O42 Eu2 133.0(3) . . ? O41 C42 C43 129.2(5) . . ? O41 C42 C41 113.0(4) . . ? C43 C42 C41 117.8(5) . . ? C42 C43 C44 122.3(5) . . ? O42 C44 C43 129.2(5) . . ? O42 C44 C45 113.1(5) . . ? C43 C44 C45 117.6(5) . . ? F45 C45 F46 110.2(6) . . ? F45 C45 F44 106.0(6) . . ? F46 C45 F44 103.6(6) . . ? F45 C45 C44 112.2(6) . . ? F46 C45 C44 114.6(5) . . ? F44 C45 C44 109.5(5) . . ? C52 O51 Eu2 134.0(4) . . ? F51 C51 F52 108.1(6) . . ? F51 C51 F53 106.7(6) . . ? F52 C51 F53 106.4(6) . . ? F51 C51 C52 112.3(5) . . ? F52 C51 C52 114.1(6) . . ? F53 C51 C52 108.8(6) . . ? C54 O52 Eu2 134.1(3) . . ? O51 C52 C53 126.6(5) . . ? O51 C52 C51 114.2(5) . . ? C53 C52 C51 119.3(6) . . ? C54 C53 C52 120.1(5) . . ? O52 C54 C53 126.9(5) . . ? O52 C54 C55 114.7(5) . . ? C53 C54 C55 118.4(5) . . ? F56 C55 F55 106.5(5) . . ? F56 C55 F54 107.8(6) . . ? F55 C55 F54 106.8(6) . . ? F56 C55 C54 113.5(5) . . ? F55 C55 C54 111.5(5) . . ? F54 C55 C54 110.5(5) . . ? N61 O60 Eu1 127.1(3) . . ? N61 O60 Eu2 128.6(3) . . ? Eu1 O60 Eu2 104.28(13) . . ? C66 N61 C62 122.5(5) . . ? C66 N61 O60 118.9(5) . . ? C62 N61 O60 118.6(5) . . ? N61 C62 C63 119.8(6) . . ? C62 C63 C64 118.5(6) . . ? C65 C64 C63 120.1(6) . . ? C66 C65 C64 119.1(6) . . ? N61 C66 C65 119.9(6) . . ? N71 O70 Eu2 128.8(3) . . ? N71 O70 Eu1 125.1(3) . . ? Eu2 O70 Eu1 104.77(13) . . ? C72 N71 C76 121.9(5) . . ? C72 N71 O70 119.9(5) . . ? C76 N71 O70 118.2(4) . . ? N71 C72 C73 119.6(6) . . ? C74 C73 C72 120.3(6) . . ? C73 C74 C75 119.4(6) . . ? C74 C75 C76 119.5(6) . . ? N71 C76 C75 119.2(6) . . ? N81 O80 Eu2 126.7(3) . . ? N81 O80 Eu1 128.5(3) . . ? Eu2 O80 Eu1 104.44(12) . . ? C86 N81 C82 122.4(5) . . ? C86 N81 O80 119.2(4) . . ? C82 N81 O80 118.5(5) . . ? N81 C82 C83 118.7(6) . . ? C84 C83 C82 119.2(6) . . ? C85 C84 C83 120.1(6) . . ? C84 C85 C86 119.8(6) . . ? N81 C86 C85 119.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O12 Eu1 O1 C2 43.5(7) . . . . ? O2 Eu1 O1 C2 -5.5(6) . . . . ? O22 Eu1 O1 C2 -60.9(7) . . . . ? O21 Eu1 O1 C2 -81.1(6) . . . . ? O11 Eu1 O1 C2 73.9(6) . . . . ? O60 Eu1 O1 C2 -152.3(6) . . . . ? O70 Eu1 O1 C2 173.8(6) . . . . ? O80 Eu1 O1 C2 143.4(6) . . . . ? Eu2 Eu1 O1 C2 175.4(6) . . . . ? O12 Eu1 Eu2 O42 -113.3(9) . . . . ? O2 Eu1 Eu2 O42 17(7) . . . . ? O1 Eu1 Eu2 O42 102.8(9) . . . . ? O22 Eu1 Eu2 O42 -40.1(9) . . . . ? O21 Eu1 Eu2 O42 31.3(9) . . . . ? O11 Eu1 Eu2 O42 174.3(9) . . . . ? O60 Eu1 Eu2 O42 43.7(9) . . . . ? O70 Eu1 Eu2 O42 -78.8(9) . . . . ? O80 Eu1 Eu2 O42 162.8(9) . . . . ? O12 Eu1 Eu2 O52 112.14(13) . . . . ? O2 Eu1 Eu2 O52 -118(7) . . . . ? O1 Eu1 Eu2 O52 -31.77(13) . . . . ? O22 Eu1 Eu2 O52 -174.63(13) . . . . ? O21 Eu1 Eu2 O52 -103.27(13) . . . . ? O11 Eu1 Eu2 O52 39.72(13) . . . . ? O60 Eu1 Eu2 O52 -90.86(18) . . . . ? O70 Eu1 Eu2 O52 146.61(18) . . . . ? O80 Eu1 Eu2 O52 28.27(18) . . . . ? O12 Eu1 Eu2 O32 38.93(14) . . . . ? O2 Eu1 Eu2 O32 169(7) . . . . ? O1 Eu1 Eu2 O32 -104.99(13) . . . . ? O22 Eu1 Eu2 O32 112.16(13) . . . . ? O21 Eu1 Eu2 O32 -176.49(13) . . . . ? O11 Eu1 Eu2 O32 -33.50(14) . . . . ? O60 Eu1 Eu2 O32 -164.08(19) . . . . ? O70 Eu1 Eu2 O32 73.39(18) . . . . ? O80 Eu1 Eu2 O32 -44.94(18) . . . . ? O12 Eu1 Eu2 O51 -175.79(13) . . . . ? O2 Eu1 Eu2 O51 -46(7) . . . . ? O1 Eu1 Eu2 O51 40.29(13) . . . . ? O22 Eu1 Eu2 O51 -102.57(13) . . . . ? O21 Eu1 Eu2 O51 -31.21(13) . . . . ? O11 Eu1 Eu2 O51 111.78(13) . . . . ? O60 Eu1 Eu2 O51 -18.80(18) . . . . ? O70 Eu1 Eu2 O51 -141.33(18) . . . . ? O80 Eu1 Eu2 O51 100.33(18) . . . . ? O12 Eu1 Eu2 O41 -102.57(13) . . . . ? O2 Eu1 Eu2 O41 28(7) . . . . ? O1 Eu1 Eu2 O41 113.51(13) . . . . ? O22 Eu1 Eu2 O41 -29.34(13) . . . . ? O21 Eu1 Eu2 O41 42.01(13) . . . . ? O11 Eu1 Eu2 O41 -175.00(13) . . . . ? O60 Eu1 Eu2 O41 54.42(18) . . . . ? O70 Eu1 Eu2 O41 -68.11(18) . . . . ? O80 Eu1 Eu2 O41 173.56(18) . . . . ? O12 Eu1 Eu2 O80 83.87(19) . . . . ? O2 Eu1 Eu2 O80 -146(7) . . . . ? O1 Eu1 Eu2 O80 -60.05(18) . . . . ? O22 Eu1 Eu2 O80 157.10(18) . . . . ? O21 Eu1 Eu2 O80 -131.55(18) . . . . ? O11 Eu1 Eu2 O80 11.45(19) . . . . ? O60 Eu1 Eu2 O80 -119.1(2) . . . . ? O70 Eu1 Eu2 O80 118.3(2) . . . . ? O12 Eu1 Eu2 O70 -34.47(18) . . . . ? O2 Eu1 Eu2 O70 96(7) . . . . ? O1 Eu1 Eu2 O70 -178.38(18) . . . . ? O22 Eu1 Eu2 O70 38.76(18) . . . . ? O21 Eu1 Eu2 O70 110.12(18) . . . . ? O11 Eu1 Eu2 O70 -106.89(18) . . . . ? O60 Eu1 Eu2 O70 122.5(2) . . . . ? O80 Eu1 Eu2 O70 -118.3(2) . . . . ? O12 Eu1 Eu2 O31 -32.97(13) . . . . ? O2 Eu1 Eu2 O31 97(7) . . . . ? O1 Eu1 Eu2 O31 -176.89(12) . . . . ? O22 Eu1 Eu2 O31 40.25(12) . . . . ? O21 Eu1 Eu2 O31 111.61(13) . . . . ? O11 Eu1 Eu2 O31 -105.40(13) . . . . ? O60 Eu1 Eu2 O31 124.02(18) . . . . ? O70 Eu1 Eu2 O31 1.49(17) . . . . ? O80 Eu1 Eu2 O31 -116.85(18) . . . . ? O12 Eu1 Eu2 O60 -156.99(19) . . . . ? O2 Eu1 Eu2 O60 -27(7) . . . . ? O1 Eu1 Eu2 O60 59.09(18) . . . . ? O22 Eu1 Eu2 O60 -83.77(18) . . . . ? O21 Eu1 Eu2 O60 -12.41(19) . . . . ? O11 Eu1 Eu2 O60 130.58(19) . . . . ? O70 Eu1 Eu2 O60 -122.5(2) . . . . ? O80 Eu1 Eu2 O60 119.1(2) . . . . ? O12 Eu1 O2 C4 -139.9(8) . . . . ? O1 Eu1 O2 C4 3.6(8) . . . . ? O22 Eu1 O2 C4 146.8(8) . . . . ? O21 Eu1 O2 C4 75.3(8) . . . . ? O11 Eu1 O2 C4 -67.8(8) . . . . ? O60 Eu1 O2 C4 63.4(8) . . . . ? O70 Eu1 O2 C4 -175.7(7) . . . . ? O80 Eu1 O2 C4 -55.5(9) . . . . ? Eu2 Eu1 O2 C4 90(7) . . . . ? Eu1 O1 C2 C1 173.0(5) . . . . ? Eu1 O1 C2 C3 9.9(13) . . . . ? F3 C1 C2 O1 176.0(8) . . . . ? F2 C1 C2 O1 -48.9(11) . . . . ? F1 C1 C2 O1 63.9(9) . . . . ? F3 C1 C2 C3 -18.2(12) . . . . ? F2 C1 C2 C3 116.8(8) . . . . ? F1 C1 C2 C3 -130.4(7) . . . . ? O1 C2 C3 C4 -9.5(15) . . . . ? C1 C2 C3 C4 -173.6(8) . . . . ? Eu1 O2 C4 C3 -5.3(14) . . . . ? Eu1 O2 C4 C5 -178.5(7) . . . . ? C2 C3 C4 O2 6.8(15) . . . . ? C2 C3 C4 C5 -180.0(9) . . . . ? O2 C4 C5 F4 -15(2) . . . . ? C3 C4 C5 F4 171.0(16) . . . . ? O2 C4 C5 F5 -157.6(11) . . . . ? C3 C4 C5 F5 28.7(17) . . . . ? O2 C4 C5 F6 95.4(12) . . . . ? C3 C4 C5 F6 -78.4(13) . . . . ? O12 Eu1 O11 C12 24.0(6) . . . . ? O2 Eu1 O11 C12 -52.2(6) . . . . ? O1 Eu1 O11 C12 -131.9(6) . . . . ? O22 Eu1 O11 C12 1.2(7) . . . . ? O21 Eu1 O11 C12 -100.8(6) . . . . ? O60 Eu1 O11 C12 164.2(6) . . . . ? O70 Eu1 O11 C12 88.9(6) . . . . ? O80 Eu1 O11 C12 135.6(6) . . . . ? Eu2 Eu1 O11 C12 128.1(6) . . . . ? O2 Eu1 O12 C14 43.8(7) . . . . ? O1 Eu1 O12 C14 -6.2(7) . . . . ? O22 Eu1 O12 C14 126.9(7) . . . . ? O21 Eu1 O12 C14 89.0(7) . . . . ? O11 Eu1 O12 C14 -36.6(6) . . . . ? O60 Eu1 O12 C14 -160.1(6) . . . . ? O70 Eu1 O12 C14 -157.7(7) . . . . ? O80 Eu1 O12 C14 -98.9(7) . . . . ? Eu2 Eu1 O12 C14 -136.9(6) . . . . ? Eu1 O11 C12 C13 -12.1(12) . . . . ? Eu1 O11 C12 C11 163.1(7) . . . . ? F11 C11 C12 O11 -40.3(18) . . . . ? F12 C11 C12 O11 -172.8(10) . . . . ? F13 C11 C12 O11 78.0(12) . . . . ? F11 C11 C12 C13 135.5(13) . . . . ? F12 C11 C12 C13 2.9(17) . . . . ? F13 C11 C12 C13 -106.2(9) . . . . ? O11 C12 C13 C14 -6.6(13) . . . . ? C11 C12 C13 C14 178.3(9) . . . . ? Eu1 O12 C14 C13 36.5(12) . . . . ? Eu1 O12 C14 C15 -156.6(5) . . . . ? C12 C13 C14 O12 -4.5(13) . . . . ? C12 C13 C14 C15 -172.1(7) . . . . ? O12 C14 C15 F15 168.9(7) . . . . ? C13 C14 C15 F15 -22.4(12) . . . . ? O12 C14 C15 F16 -51.9(11) . . . . ? C13 C14 C15 F16 116.8(8) . . . . ? O12 C14 C15 F14 56.5(9) . . . . ? C13 C14 C15 F14 -134.8(7) . . . . ? O12 Eu1 O21 C22 5.7(5) . . . . ? O2 Eu1 O21 C22 51.2(5) . . . . ? O1 Eu1 O21 C22 132.2(5) . . . . ? O22 Eu1 O21 C22 -32.6(5) . . . . ? O11 Eu1 O21 C22 101.0(5) . . . . ? O60 Eu1 O21 C22 -136.7(5) . . . . ? O70 Eu1 O21 C22 -89.0(5) . . . . ? O80 Eu1 O21 C22 -164.3(4) . . . . ? Eu2 Eu1 O21 C22 -128.6(5) . . . . ? O12 Eu1 O22 C24 -117.2(6) . . . . ? O2 Eu1 O22 C24 -42.1(5) . . . . ? O1 Eu1 O22 C24 12.4(6) . . . . ? O21 Eu1 O22 C24 32.5(5) . . . . ? O11 Eu1 O22 C24 -94.6(6) . . . . ? O60 Eu1 O22 C24 99.0(5) . . . . ? O70 Eu1 O22 C24 160.8(6) . . . . ? O80 Eu1 O22 C24 156.8(5) . . . . ? Eu2 Eu1 O22 C24 137.1(5) . . . . ? Eu1 O21 C22 C23 26.4(10) . . . . ? Eu1 O21 C22 C21 -158.3(4) . . . . ? F21 C21 C22 O21 34.0(10) . . . . ? F22 C21 C22 O21 -89.8(8) . . . . ? F23 C21 C22 O21 157.6(6) . . . . ? F21 C21 C22 C23 -150.2(8) . . . . ? F22 C21 C22 C23 86.0(9) . . . . ? F23 C21 C22 C23 -26.7(9) . . . . ? O21 C22 C23 C24 1.8(11) . . . . ? C21 C22 C23 C24 -173.3(6) . . . . ? Eu1 O22 C24 C23 -24.0(10) . . . . ? Eu1 O22 C24 C25 157.7(4) . . . . ? C22 C23 C24 O22 -3.8(11) . . . . ? C22 C23 C24 C25 174.5(6) . . . . ? O22 C24 C25 F25 23.1(10) . . . . ? C23 C24 C25 F25 -155.3(7) . . . . ? O22 C24 C25 F24 -98.7(7) . . . . ? C23 C24 C25 F24 82.9(8) . . . . ? O22 C24 C25 F26 146.2(6) . . . . ? C23 C24 C25 F26 -32.2(9) . . . . ? O42 Eu2 O31 C32 -56.8(5) . . . . ? O52 Eu2 O31 C32 -3.0(5) . . . . ? O32 Eu2 O31 C32 27.7(5) . . . . ? O51 Eu2 O31 C32 -100.9(5) . . . . ? O41 Eu2 O31 C32 -136.4(5) . . . . ? O80 Eu2 O31 C32 90.1(5) . . . . ? O70 Eu2 O31 C32 130.6(5) . . . . ? O60 Eu2 O31 C32 167.2(5) . . . . ? Eu1 Eu2 O31 C32 129.6(5) . . . . ? O42 Eu2 O32 C34 44.7(5) . . . . ? O52 Eu2 O32 C34 126.1(5) . . . . ? O51 Eu2 O32 C34 96.3(5) . . . . ? O41 Eu2 O32 C34 -9.7(6) . . . . ? O80 Eu2 O32 C34 -158.7(5) . . . . ? O70 Eu2 O32 C34 -96.5(5) . . . . ? O31 Eu2 O32 C34 -29.9(5) . . . . ? O60 Eu2 O32 C34 -148.3(5) . . . . ? Eu1 Eu2 O32 C34 -132.4(5) . . . . ? Eu2 O31 C32 C33 -18.9(9) . . . . ? Eu2 O31 C32 C31 164.3(4) . . . . ? F32 C31 C32 O31 -43.2(8) . . . . ? F33 C31 C32 O31 -169.4(6) . . . . ? F31 C31 C32 O31 76.4(7) . . . . ? F32 C31 C32 C33 139.8(6) . . . . ? F33 C31 C32 C33 13.5(9) . . . . ? F31 C31 C32 C33 -100.7(6) . . . . ? O31 C32 C33 C34 -5.8(10) . . . . ? C31 C32 C33 C34 170.9(6) . . . . ? Eu2 O32 C34 C33 23.8(10) . . . . ? Eu2 O32 C34 C35 -157.7(4) . . . . ? C32 C33 C34 O32 3.8(10) . . . . ? C32 C33 C34 C35 -174.5(6) . . . . ? O32 C34 C35 F36 65.0(8) . . . . ? C33 C34 C35 F36 -116.4(7) . . . . ? O32 C34 C35 F35 -171.8(6) . . . . ? C33 C34 C35 F35 6.8(10) . . . . ? O32 C34 C35 F34 -51.9(8) . . . . ? C33 C34 C35 F34 126.7(7) . . . . ? O42 Eu2 O41 C42 -4.8(5) . . . . ? O52 Eu2 O41 C42 -56.5(5) . . . . ? O32 Eu2 O41 C42 51.1(5) . . . . ? O51 Eu2 O41 C42 -80.9(5) . . . . ? O80 Eu2 O41 C42 -177.7(4) . . . . ? O70 Eu2 O41 C42 141.7(5) . . . . ? O31 Eu2 O41 C42 71.5(5) . . . . ? O60 Eu2 O41 C42 -153.2(5) . . . . ? Eu1 Eu2 O41 C42 176.4(5) . . . . ? O52 Eu2 O42 C44 151.3(5) . . . . ? O32 Eu2 O42 C44 -137.3(5) . . . . ? O51 Eu2 O42 C44 79.8(5) . . . . ? O41 Eu2 O42 C44 4.7(5) . . . . ? O80 Eu2 O42 C44 175.7(5) . . . . ? O70 Eu2 O42 C44 -55.7(6) . . . . ? O31 Eu2 O42 C44 -66.6(5) . . . . ? O60 Eu2 O42 C44 54.5(6) . . . . ? Eu1 Eu2 O42 C44 15.7(13) . . . . ? Eu2 O41 C42 C43 4.0(9) . . . . ? Eu2 O41 C42 C41 -176.9(4) . . . . ? F43 C41 C42 O41 177.3(6) . . . . ? F41 C41 C42 O41 -61.3(7) . . . . ? F42 C41 C42 O41 55.9(7) . . . . ? F43 C41 C42 C43 -3.4(9) . . . . ? F41 C41 C42 C43 117.9(6) . . . . ? F42 C41 C42 C43 -124.8(6) . . . . ? O41 C42 C43 C44 -0.1(10) . . . . ? C41 C42 C43 C44 -179.2(6) . . . . ? Eu2 O42 C44 C43 -3.7(10) . . . . ? Eu2 O42 C44 C45 178.1(4) . . . . ? C42 C43 C44 O42 -0.2(10) . . . . ? C42 C43 C44 C45 177.9(6) . . . . ? O42 C44 C45 F45 -51.2(9) . . . . ? C43 C44 C45 F45 130.4(7) . . . . ? O42 C44 C45 F46 -177.8(6) . . . . ? C43 C44 C45 F46 3.8(9) . . . . ? O42 C44 C45 F44 66.3(7) . . . . ? C43 C44 C45 F44 -112.1(6) . . . . ? O42 Eu2 O51 C52 53.1(5) . . . . ? O52 Eu2 O51 C52 -30.7(5) . . . . ? O32 Eu2 O51 C52 -0.7(6) . . . . ? O41 Eu2 O51 C52 131.6(5) . . . . ? O80 Eu2 O51 C52 -92.9(5) . . . . ? O70 Eu2 O51 C52 -163.5(5) . . . . ? O31 Eu2 O51 C52 97.0(5) . . . . ? O60 Eu2 O51 C52 -144.7(5) . . . . ? Eu1 Eu2 O51 C52 -132.6(5) . . . . ? O42 Eu2 O52 C54 -46.4(5) . . . . ? O32 Eu2 O52 C54 -128.2(5) . . . . ? O51 Eu2 O52 C54 28.8(5) . . . . ? O41 Eu2 O52 C54 4.0(5) . . . . ? O80 Eu2 O52 C54 147.0(5) . . . . ? O70 Eu2 O52 C54 157.7(4) . . . . ? O31 Eu2 O52 C54 -97.9(5) . . . . ? O60 Eu2 O52 C54 90.4(5) . . . . ? Eu1 Eu2 O52 C54 129.2(5) . . . . ? Eu2 O51 C52 C53 23.5(9) . . . . ? Eu2 O51 C52 C51 -157.0(4) . . . . ? F51 C51 C52 O51 -46.7(8) . . . . ? F52 C51 C52 O51 -170.2(6) . . . . ? F53 C51 C52 O51 71.2(7) . . . . ? F51 C51 C52 C53 132.9(6) . . . . ? F52 C51 C52 C53 9.4(9) . . . . ? F53 C51 C52 C53 -109.3(7) . . . . ? O51 C52 C53 C54 4.4(9) . . . . ? C51 C52 C53 C54 -175.1(5) . . . . ? Eu2 O52 C54 C53 -19.9(8) . . . . ? Eu2 O52 C54 C55 162.4(4) . . . . ? C52 C53 C54 O52 -6.2(9) . . . . ? C52 C53 C54 C55 171.5(5) . . . . ? O52 C54 C55 F56 -170.8(5) . . . . ? C53 C54 C55 F56 11.3(8) . . . . ? O52 C54 C55 F55 -50.6(7) . . . . ? C53 C54 C55 F55 131.5(6) . . . . ? O52 C54 C55 F54 68.0(7) . . . . ? C53 C54 C55 F54 -109.9(6) . . . . ? O12 Eu1 O60 N61 -143.2(4) . . . . ? O2 Eu1 O60 N61 -1.0(5) . . . . ? O1 Eu1 O60 N61 56.2(4) . . . . ? O22 Eu1 O60 N61 -78.2(4) . . . . ? O21 Eu1 O60 N61 -12.9(4) . . . . ? O11 Eu1 O60 N61 113.5(4) . . . . ? O70 Eu1 O60 N61 -145.8(4) . . . . ? O80 Eu1 O60 N61 143.4(4) . . . . ? Eu2 Eu1 O60 N61 179.7(5) . . . . ? O12 Eu1 O60 Eu2 37.1(3) . . . . ? O2 Eu1 O60 Eu2 179.36(16) . . . . ? O1 Eu1 O60 Eu2 -123.44(16) . . . . ? O22 Eu1 O60 Eu2 102.10(15) . . . . ? O21 Eu1 O60 Eu2 167.44(19) . . . . ? O11 Eu1 O60 Eu2 -66.2(2) . . . . ? O70 Eu1 O60 Eu2 34.51(13) . . . . ? O80 Eu1 O60 Eu2 -36.30(13) . . . . ? O42 Eu2 O60 N61 6.7(5) . . . . ? O52 Eu2 O60 N61 -80.3(4) . . . . ? O32 Eu2 O60 N61 -154.2(4) . . . . ? O51 Eu2 O60 N61 -19.0(4) . . . . ? O41 Eu2 O60 N61 55.3(4) . . . . ? O80 Eu2 O60 N61 -142.8(4) . . . . ? O70 Eu2 O60 N61 145.6(4) . . . . ? O31 Eu2 O60 N61 107.2(4) . . . . ? Eu1 Eu2 O60 N61 -179.7(5) . . . . ? O42 Eu2 O60 Eu1 -173.67(13) . . . . ? O52 Eu2 O60 Eu1 99.40(15) . . . . ? O32 Eu2 O60 Eu1 25.5(3) . . . . ? O51 Eu2 O60 Eu1 160.62(19) . . . . ? O41 Eu2 O60 Eu1 -125.03(17) . . . . ? O80 Eu2 O60 Eu1 36.90(14) . . . . ? O70 Eu2 O60 Eu1 -34.74(13) . . . . ? O31 Eu2 O60 Eu1 -73.11(19) . . . . ? Eu1 O60 N61 C66 -74.4(6) . . . . ? Eu2 O60 N61 C66 105.2(5) . . . . ? Eu1 O60 N61 C62 104.5(5) . . . . ? Eu2 O60 N61 C62 -76.0(6) . . . . ? C66 N61 C62 C63 -0.5(9) . . . . ? O60 N61 C62 C63 -179.3(5) . . . . ? N61 C62 C63 C64 -0.5(9) . . . . ? C62 C63 C64 C65 1.7(11) . . . . ? C63 C64 C65 C66 -2.0(11) . . . . ? C62 N61 C66 C65 0.2(9) . . . . ? O60 N61 C66 C65 179.1(5) . . . . ? C64 C65 C66 N61 1.0(10) . . . . ? O42 Eu2 O70 N71 3.0(5) . . . . ? O52 Eu2 O70 N71 143.8(4) . . . . ? O32 Eu2 O70 N71 79.2(4) . . . . ? O51 Eu2 O70 N71 -113.4(4) . . . . ? O41 Eu2 O70 N71 -53.9(4) . . . . ? O80 Eu2 O70 N71 155.2(4) . . . . ? O31 Eu2 O70 N71 14.0(4) . . . . ? O60 Eu2 O70 N71 -132.9(4) . . . . ? Eu1 Eu2 O70 N71 -167.5(5) . . . . ? O42 Eu2 O70 Eu1 170.45(13) . . . . ? O52 Eu2 O70 Eu1 -48.7(2) . . . . ? O32 Eu2 O70 Eu1 -113.36(14) . . . . ? O51 Eu2 O70 Eu1 54.1(2) . . . . ? O41 Eu2 O70 Eu1 113.54(15) . . . . ? O80 Eu2 O70 Eu1 -37.29(13) . . . . ? O31 Eu2 O70 Eu1 -178.49(17) . . . . ? O60 Eu2 O70 Eu1 34.61(13) . . . . ? O12 Eu1 O70 N71 -45.3(4) . . . . ? O2 Eu1 O70 N71 -10.4(5) . . . . ? O1 Eu1 O70 N71 170.6(3) . . . . ? O22 Eu1 O70 N71 28.2(4) . . . . ? O21 Eu1 O70 N71 82.8(4) . . . . ? O11 Eu1 O70 N71 -105.3(4) . . . . ? O60 Eu1 O70 N71 133.0(4) . . . . ? O80 Eu1 O70 N71 -155.0(4) . . . . ? Eu2 Eu1 O70 N71 168.1(5) . . . . ? O12 Eu1 O70 Eu2 146.57(17) . . . . ? O2 Eu1 O70 Eu2 -178.53(17) . . . . ? O1 Eu1 O70 Eu2 2.6(3) . . . . ? O22 Eu1 O70 Eu2 -139.91(17) . . . . ? O21 Eu1 O70 Eu2 -85.25(16) . . . . ? O11 Eu1 O70 Eu2 86.57(16) . . . . ? O60 Eu1 O70 Eu2 -35.08(14) . . . . ? O80 Eu1 O70 Eu2 36.93(13) . . . . ? Eu2 O70 N71 C72 64.4(6) . . . . ? Eu1 O70 N71 C72 -100.7(5) . . . . ? Eu2 O70 N71 C76 -114.2(5) . . . . ? Eu1 O70 N71 C76 80.6(5) . . . . ? C76 N71 C72 C73 -0.4(8) . . . . ? O70 N71 C72 C73 -179.0(5) . . . . ? N71 C72 C73 C74 -1.7(9) . . . . ? C72 C73 C74 C75 2.0(10) . . . . ? C73 C74 C75 C76 -0.3(10) . . . . ? C72 N71 C76 C75 2.1(8) . . . . ? O70 N71 C76 C75 -179.3(5) . . . . ? C74 C75 C76 N71 -1.8(9) . . . . ? O42 Eu2 O80 N81 -3.3(5) . . . . ? O52 Eu2 O80 N81 21.8(4) . . . . ? O32 Eu2 O80 N81 -50.1(4) . . . . ? O51 Eu2 O80 N81 81.8(4) . . . . ? O41 Eu2 O80 N81 163.9(3) . . . . ? O70 Eu2 O80 N81 -149.8(4) . . . . ? O31 Eu2 O80 N81 -106.9(4) . . . . ? O60 Eu2 O80 N81 137.0(4) . . . . ? Eu1 Eu2 O80 N81 173.3(5) . . . . ? O42 Eu2 O80 Eu1 -176.61(17) . . . . ? O52 Eu2 O80 Eu1 -151.52(18) . . . . ? O32 Eu2 O80 Eu1 136.58(17) . . . . ? O51 Eu2 O80 Eu1 -91.50(16) . . . . ? O41 Eu2 O80 Eu1 -9.5(3) . . . . ? O70 Eu2 O80 Eu1 36.89(14) . . . . ? O31 Eu2 O80 Eu1 79.78(17) . . . . ? O60 Eu2 O80 Eu1 -36.35(14) . . . . ? O12 Eu1 O80 N81 80.7(4) . . . . ? O2 Eu1 O80 N81 6.0(5) . . . . ? O1 Eu1 O80 N81 -50.5(4) . . . . ? O22 Eu1 O80 N81 154.1(4) . . . . ? O21 Eu1 O80 N81 -107.1(4) . . . . ? O11 Eu1 O80 N81 18.6(4) . . . . ? O60 Eu1 O80 N81 -136.2(4) . . . . ? O70 Eu1 O80 N81 149.8(4) . . . . ? Eu2 Eu1 O80 N81 -173.2(5) . . . . ? O12 Eu1 O80 Eu2 -106.16(15) . . . . ? O2 Eu1 O80 Eu2 179.16(17) . . . . ? O1 Eu1 O80 Eu2 122.71(16) . . . . ? O22 Eu1 O80 Eu2 -32.7(2) . . . . ? O21 Eu1 O80 Eu2 66.1(2) . . . . ? O11 Eu1 O80 Eu2 -168.20(19) . . . . ? O60 Eu1 O80 Eu2 37.00(14) . . . . ? O70 Eu1 O80 Eu2 -37.01(14) . . . . ? Eu2 O80 N81 C86 -107.2(5) . . . . ? Eu1 O80 N81 C86 64.5(6) . . . . ? Eu2 O80 N81 C82 72.4(6) . . . . ? Eu1 O80 N81 C82 -115.8(5) . . . . ? C86 N81 C82 C83 0.8(9) . . . . ? O80 N81 C82 C83 -178.9(5) . . . . ? N81 C82 C83 C84 0.2(10) . . . . ? C82 C83 C84 C85 -1.4(11) . . . . ? C83 C84 C85 C86 1.5(11) . . . . ? C82 N81 C86 C85 -0.6(9) . . . . ? O80 N81 C86 C85 179.0(5) . . . . ? C84 C85 C86 N81 -0.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.564 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.141 data_99276 _database_code_CSD 171072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H12 Eu F21 O12' _chemical_formula_weight 1007.27 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' '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 Rhombohedral _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 14.6594(4) _cell_length_b 14.6594(4) _cell_length_c 54.863(2) _cell_angle_alpha 90.0000(10) _cell_angle_beta 90.0000(10) _cell_angle_gamma 120.0000(10) _cell_volume 10210.4(5) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description wedge _exptl_crystal_colour clear _exptl_crystal_size_max .01 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .10 _exptl_crystal_density_diffrn 1.966 _exptl_crystal_F_000 5832 _exptl_absorpt_coefficient_mu 2.012 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 39654 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -73 _diffrn_reflns_limit_l_max 70 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.29 _reflns_number_total 2833 _reflns_number_gt 1996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2833 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.3333 0.6667 0.020306(3) 0.02139(8) Uani 1 3 d S . . O1 O 0.18481(13) 0.47826(13) 0.01910(3) 0.0304(4) Uani 1 1 d . . . F1 F 0.07452(14) 0.27818(12) 0.02811(3) 0.0595(5) Uani 1 1 d . . . C1 C 0.0483(2) 0.3062(2) 0.00746(6) 0.0421(7) Uani 1 1 d . . . F2 F -0.05356(12) 0.27809(12) 0.00915(3) 0.0536(5) Uani 1 1 d . . . C2 C 0.11675(19) 0.42492(19) 0.00316(5) 0.0319(6) Uani 1 1 d . . . O2 O 0.21204(13) 0.64399(14) -0.01137(3) 0.0309(4) Uani 1 1 d . . . F3 F 0.05646(13) 0.24939(13) -0.01038(3) 0.0548(5) Uani 1 1 d . . . C3 C 0.0969(2) 0.4645(2) -0.01794(5) 0.0346(6) Uani 1 1 d . . . F4 F 0.02236(13) 0.39424(12) -0.03353(3) 0.0507(4) Uani 1 1 d . . . C4 C 0.1453(2) 0.5703(2) -0.02386(4) 0.0296(5) Uani 1 1 d . . . F5 F 0.01336(12) 0.57019(14) -0.04928(3) 0.0496(4) Uani 1 1 d . . . C5' C 0.1158(2) 0.6006(3) -0.04824(5) 0.0426(7) Uani 1 1 d . . . O6 O 0.42547(14) 0.79299(14) 0.05241(3) 0.0331(4) Uani 1 1 d . . . F6 F 0.13582(17) 0.55480(16) -0.06674(3) 0.0620(5) Uani 1 1 d . . . C7 C 0.4993(2) 0.8222(2) 0.06670(5) 0.0365(6) Uani 1 1 d . . . F7 F 0.16929(13) 0.70352(15) -0.05175(3) 0.0548(5) Uani 1 1 d . . . O7 O 0.57945(18) 0.8087(2) 0.06260(4) 0.0537(6) Uani 1 1 d . . . C8 C 0.5048(3) 0.8751(3) 0.09000(5) 0.0533(8) Uani 1 1 d . . . H8A H 0.4342 0.8612 0.0945 0.080 Uiso 1 1 calc R . . H8B H 0.5520 0.9512 0.0882 0.080 Uiso 1 1 calc R . . H8C H 0.5317 0.8480 0.1028 0.080 Uiso 1 1 calc R . . H7 H 0.571(3) 0.780(3) 0.0511(7) 0.080(16) Uiso 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 0.02031(9) 0.02031(9) 0.02355(12) 0.000 0.000 0.01016(4) O1 0.0269(9) 0.0255(9) 0.0342(10) -0.0027(7) -0.0010(7) 0.0096(7) F1 0.0580(12) 0.0300(9) 0.0747(13) 0.0100(9) -0.0070(10) 0.0101(8) C1 0.0307(15) 0.0316(14) 0.059(2) -0.0089(14) -0.0043(14) 0.0122(12) F2 0.0279(9) 0.0336(9) 0.0863(13) -0.0075(9) 0.0076(9) 0.0057(7) C2 0.0243(13) 0.0257(13) 0.0427(15) -0.0053(11) 0.0032(11) 0.0103(11) O2 0.0282(9) 0.0302(9) 0.0345(10) -0.0027(8) -0.0047(8) 0.0148(8) F3 0.0426(10) 0.0348(9) 0.0828(14) -0.0203(9) -0.0044(9) 0.0162(8) C3 0.0268(13) 0.0347(14) 0.0363(14) -0.0097(12) -0.0071(11) 0.0108(11) F4 0.0445(10) 0.0420(9) 0.0542(11) -0.0168(8) -0.0210(8) 0.0131(8) C4 0.0234(12) 0.0395(15) 0.0287(12) -0.0033(12) -0.0011(10) 0.0178(12) F5 0.0356(9) 0.0633(12) 0.0485(10) -0.0037(8) -0.0139(7) 0.0236(8) C5' 0.0382(16) 0.0538(19) 0.0352(16) 0.0014(14) -0.0015(12) 0.0226(15) O6 0.0324(9) 0.0296(9) 0.0356(10) -0.0052(8) -0.0079(8) 0.0141(8) F6 0.0699(13) 0.0993(15) 0.0290(9) -0.0102(9) -0.0023(9) 0.0515(12) C7 0.0368(15) 0.0323(14) 0.0365(15) -0.0019(12) -0.0049(12) 0.0144(12) F7 0.0484(10) 0.0604(12) 0.0434(10) 0.0145(8) -0.0046(8) 0.0180(9) O7 0.0406(13) 0.0749(16) 0.0498(14) -0.0240(12) -0.0193(11) 0.0319(12) C8 0.057(2) 0.068(2) 0.0388(17) -0.0179(16) -0.0144(15) 0.0339(18) _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 O2 2.3877(16) . ? Eu1 O2 2.3878(16) 2_665 ? Eu1 O2 2.3878(16) 3_565 ? Eu1 O6 2.4195(17) 2_665 ? Eu1 O6 2.4196(17) 3_565 ? Eu1 O6 2.4197(17) . ? Eu1 O1 2.5218(16) . ? Eu1 O1 2.5218(16) 3_565 ? Eu1 O1 2.5219(16) 2_665 ? O1 C2 1.261(3) . ? F1 C1 1.326(3) . ? C1 F3 1.329(3) . ? C1 F2 1.338(3) . ? C1 C2 1.531(4) . ? C2 C3 1.390(4) . ? O2 C4 1.239(3) . ? C3 F4 1.364(3) . ? C3 C4 1.383(4) . ? C4 C5' 1.538(4) . ? F5 C5' 1.337(3) . ? C5' F7 1.321(4) . ? C5' F6 1.329(3) . ? O6 C7 1.227(3) . ? C7 O7 1.305(3) . ? C7 C8 1.476(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 O2 Eu1 O2 72.87(6) . 2_665 ? O2 Eu1 O2 72.87(6) . 3_565 ? O2 Eu1 O2 72.87(6) 2_665 3_565 ? O2 Eu1 O6 93.52(6) . 2_665 ? O2 Eu1 O6 136.74(6) 2_665 2_665 ? O2 Eu1 O6 143.10(6) 3_565 2_665 ? O2 Eu1 O6 143.11(6) . 3_565 ? O2 Eu1 O6 93.52(6) 2_665 3_565 ? O2 Eu1 O6 136.74(6) 3_565 3_565 ? O6 Eu1 O6 72.86(7) 2_665 3_565 ? O2 Eu1 O6 136.74(6) . . ? O2 Eu1 O6 143.11(6) 2_665 . ? O2 Eu1 O6 93.52(6) 3_565 . ? O6 Eu1 O6 72.85(7) 2_665 . ? O6 Eu1 O6 72.85(7) 3_565 . ? O2 Eu1 O1 69.72(6) . . ? O2 Eu1 O1 67.86(6) 2_665 . ? O2 Eu1 O1 131.77(5) 3_565 . ? O6 Eu1 O1 68.90(6) 2_665 . ? O6 Eu1 O1 73.39(6) 3_565 . ? O6 Eu1 O1 134.68(6) . . ? O2 Eu1 O1 67.87(6) . 3_565 ? O2 Eu1 O1 131.78(5) 2_665 3_565 ? O2 Eu1 O1 69.72(6) 3_565 3_565 ? O6 Eu1 O1 73.38(6) 2_665 3_565 ? O6 Eu1 O1 134.68(6) 3_565 3_565 ? O6 Eu1 O1 68.90(6) . 3_565 ? O1 Eu1 O1 119.934(3) . 3_565 ? O2 Eu1 O1 131.78(5) . 2_665 ? O2 Eu1 O1 69.72(6) 2_665 2_665 ? O2 Eu1 O1 67.87(6) 3_565 2_665 ? O6 Eu1 O1 134.68(6) 2_665 2_665 ? O6 Eu1 O1 68.89(6) 3_565 2_665 ? O6 Eu1 O1 73.38(6) . 2_665 ? O1 Eu1 O1 119.931(4) . 2_665 ? O1 Eu1 O1 119.931(4) 3_565 2_665 ? C2 O1 Eu1 132.79(16) . . ? F1 C1 F3 107.7(2) . . ? F1 C1 F2 107.3(2) . . ? F3 C1 F2 107.1(2) . . ? F1 C1 C2 110.9(2) . . ? F3 C1 C2 112.7(2) . . ? F2 C1 C2 110.9(2) . . ? O1 C2 C3 125.8(2) . . ? O1 C2 C1 117.6(2) . . ? C3 C2 C1 116.6(2) . . ? C4 O2 Eu1 137.08(17) . . ? F4 C3 C4 117.9(2) . . ? F4 C3 C2 117.6(2) . . ? C4 C3 C2 124.5(2) . . ? O2 C4 C3 125.9(2) . . ? O2 C4 C5' 116.3(2) . . ? C3 C4 C5' 117.9(2) . . ? F7 C5' F6 108.1(2) . . ? F7 C5' F5 107.5(2) . . ? F6 C5' F5 107.1(2) . . ? F7 C5' C4 111.4(2) . . ? F6 C5' C4 110.7(2) . . ? F5 C5' C4 111.8(2) . . ? C7 O6 Eu1 142.13(17) . . ? O6 C7 O7 122.7(3) . . ? O6 C7 C8 122.9(3) . . ? O7 C7 C8 114.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Eu1 O1 C2 16.9(2) . . . . ? O2 Eu1 O1 C2 -62.2(2) 2_665 . . . ? O2 Eu1 O1 C2 -24.4(2) 3_565 . . . ? O6 Eu1 O1 C2 119.2(2) 2_665 . . . ? O6 Eu1 O1 C2 -163.2(2) 3_565 . . . ? O6 Eu1 O1 C2 153.53(19) . . . . ? O1 Eu1 O1 C2 64.4(2) 3_565 . . . ? O1 Eu1 O1 C2 -110.4(2) 2_665 . . . ? Eu1 O1 C2 C3 -10.2(4) . . . . ? Eu1 O1 C2 C1 170.93(16) . . . . ? F1 C1 C2 O1 -0.8(3) . . . . ? F3 C1 C2 O1 -121.6(3) . . . . ? F2 C1 C2 O1 118.3(2) . . . . ? F1 C1 C2 C3 -179.9(2) . . . . ? F3 C1 C2 C3 59.4(3) . . . . ? F2 C1 C2 C3 -60.8(3) . . . . ? O2 Eu1 O2 C4 49.1(2) 2_665 . . . ? O2 Eu1 O2 C4 126.0(2) 3_565 . . . ? O6 Eu1 O2 C4 -89.0(2) 2_665 . . . ? O6 Eu1 O2 C4 -23.2(3) 3_565 . . . ? O6 Eu1 O2 C4 -157.5(2) . . . . ? O1 Eu1 O2 C4 -23.0(2) . . . . ? O1 Eu1 O2 C4 -159.4(2) 3_565 . . . ? O1 Eu1 O2 C4 89.5(2) 2_665 . . . ? O1 C2 C3 F4 177.8(2) . . . . ? C1 C2 C3 F4 -3.3(3) . . . . ? O1 C2 C3 C4 -4.0(4) . . . . ? C1 C2 C3 C4 174.9(2) . . . . ? Eu1 O2 C4 C3 21.1(4) . . . . ? Eu1 O2 C4 C5' -157.92(17) . . . . ? F4 C3 C4 O2 177.9(2) . . . . ? C2 C3 C4 O2 -0.3(4) . . . . ? F4 C3 C4 C5' -3.1(4) . . . . ? C2 C3 C4 C5' 178.7(2) . . . . ? O2 C4 C5' F7 0.4(3) . . . . ? C3 C4 C5' F7 -178.7(2) . . . . ? O2 C4 C5' F6 120.7(3) . . . . ? C3 C4 C5' F6 -58.4(3) . . . . ? O2 C4 C5' F5 -120.0(3) . . . . ? C3 C4 C5' F5 60.9(3) . . . . ? O2 Eu1 O6 C7 -163.9(3) . . . . ? O2 Eu1 O6 C7 -29.5(3) 2_665 . . . ? O2 Eu1 O6 C7 -95.3(3) 3_565 . . . ? O6 Eu1 O6 C7 119.7(3) 2_665 . . . ? O6 Eu1 O6 C7 42.8(3) 3_565 . . . ? O1 Eu1 O6 C7 86.3(3) . . . . ? O1 Eu1 O6 C7 -162.0(3) 3_565 . . . ? O1 Eu1 O6 C7 -29.7(3) 2_665 . . . ? Eu1 O6 C7 O7 24.9(5) . . . . ? Eu1 O6 C7 C8 -154.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.796 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.094 data_00064 _database_code_CSD 171284 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H13 Eu F21 N2 O8' _chemical_formula_weight 1044.35 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 16.8109(10) _cell_length_b 19.8224(10) _cell_length_c 22.705(2) _cell_angle_alpha 90.000(10) _cell_angle_beta 90.000(10) _cell_angle_gamma 90.000(10) _cell_volume 7566.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ellipse _exptl_crystal_colour colorless _exptl_crystal_size_max .08 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .16 _exptl_crystal_density_meas hemisphere _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4040 _exptl_absorpt_coefficient_mu 1.808 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46635 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.30 _reflns_number_total 9195 _reflns_number_gt 5428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9195 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.089278(11) 0.059926(9) 0.033905(8) 0.02857(6) Uani 1 1 d . . . F1 F 0.37298(17) 0.09774(17) 0.00684(15) 0.0917(11) Uani 1 1 d . . . F2 F 0.38238(19) 0.19606(15) 0.0435(2) 0.1246(16) Uani 1 1 d . . . F3 F 0.40252(17) 0.11082(19) 0.09461(17) 0.1045(12) Uani 1 1 d . . . F4 F 0.30020(15) 0.19367(17) 0.15417(13) 0.0955(11) Uani 1 1 d . . . F5 F 0.1656(2) 0.26731(16) 0.19412(15) 0.1035(12) Uani 1 1 d . . . F6 F 0.18774(17) 0.17632(18) 0.24109(12) 0.0926(11) Uani 1 1 d . . . F7 F 0.07153(15) 0.19850(16) 0.21105(11) 0.0750(9) Uani 1 1 d . . . F11 F 0.29719(17) -0.05843(19) 0.14093(13) 0.1064(13) Uani 1 1 d . . . F12 F 0.26846(18) -0.0158(2) 0.22334(14) 0.1224(15) Uani 1 1 d . . . F13 F 0.2276(2) -0.1122(2) 0.20182(19) 0.1299(16) Uani 1 1 d . . . F14 F 0.10451(15) -0.03989(14) 0.24477(11) 0.0714(9) Uani 1 1 d . . . F15 F -0.03044(16) 0.03496(15) 0.26330(11) 0.0741(8) Uani 1 1 d . . . F16 F -0.05639(17) -0.06374(13) 0.23055(13) 0.0784(9) Uani 1 1 d . . . F17 F -0.11145(13) 0.02241(13) 0.19186(11) 0.0549(7) Uani 1 1 d . . . F21 F 0.26039(17) -0.09111(14) -0.07860(14) 0.0860(10) Uani 1 1 d . . . F22 F 0.26811(16) -0.04047(16) -0.16069(11) 0.0821(9) Uani 1 1 d . . . F23 F 0.34640(15) -0.01398(14) -0.09121(13) 0.0735(8) Uani 1 1 d . . . F24 F 0.26907(16) 0.09760(13) -0.14623(11) 0.0717(8) Uani 1 1 d . . . F25 F 0.1666(3) 0.19724(19) -0.17824(16) 0.1398(18) Uani 1 1 d . . . F26 F 0.2362(3) 0.23331(17) -0.10770(19) 0.1358(17) Uani 1 1 d . . . F27 F 0.1104(2) 0.24512(17) -0.10536(17) 0.1281(16) Uani 1 1 d . . . O1 O 0.22404(16) 0.10500(13) 0.03243(12) 0.0419(7) Uani 1 1 d . . . O2 O 0.10695(14) 0.14158(12) 0.11270(11) 0.0372(7) Uani 1 1 d . . . O6 O 0.17129(14) -0.00003(12) 0.10182(11) 0.0345(6) Uani 1 1 d . . . O7 O 0.00769(14) 0.03051(12) 0.12100(11) 0.0339(6) Uani 1 1 d . . . O11 O 0.16661(15) 0.00088(12) -0.03986(11) 0.0377(6) Uani 1 1 d . . . O12 O 0.04002(14) -0.05338(11) 0.02281(10) 0.0310(6) Uani 1 1 d . . . O16 O 0.10751(17) 0.13222(14) -0.05065(12) 0.0491(8) Uani 1 1 d . . . O17 O 0.02133(15) -0.14111(12) -0.03307(11) 0.0379(6) Uani 1 1 d . . . C1 C 0.3564(3) 0.1364(3) 0.0514(3) 0.0616(14) Uani 1 1 d . . . C2 C 0.2683(2) 0.13356(19) 0.06771(18) 0.0389(10) Uani 1 1 d . . . C3 C 0.2432(2) 0.1638(2) 0.1198(2) 0.0534(12) Uani 1 1 d . . . C4 C 0.1650(3) 0.1668(2) 0.13867(18) 0.0434(10) Uani 1 1 d . . . C5 C 0.1470(3) 0.2030(3) 0.1967(2) 0.0606(14) Uani 1 1 d . . . C6 C 0.2415(3) -0.0519(3) 0.1797(2) 0.0657(14) Uani 1 1 d . . . C7 C 0.1667(2) -0.0205(2) 0.15360(18) 0.0391(10) Uani 1 1 d . . . C8 C 0.0991(2) -0.0167(2) 0.18833(17) 0.0418(10) Uani 1 1 d . . . C9 C 0.0245(2) 0.00626(19) 0.16973(17) 0.0354(9) Uani 1 1 d . . . C10 C -0.0437(3) -0.0004(2) 0.21488(19) 0.0455(11) Uani 1 1 d . . . C11 C 0.2718(3) -0.0325(2) -0.1032(2) 0.0493(11) Uani 1 1 d . . . C12 C 0.2120(2) 0.0208(2) -0.08035(17) 0.0388(10) Uani 1 1 d . . . C13 C 0.2131(3) 0.0845(2) -0.10420(18) 0.0475(11) Uani 1 1 d . . . C14 C 0.1603(3) 0.1355(2) -0.08918(19) 0.0509(12) Uani 1 1 d . . . C15 C 0.1678(5) 0.2033(3) -0.1209(3) 0.095(2) Uani 1 1 d . . . C16 C 0.0627(2) -0.11108(19) 0.00418(17) 0.0345(9) Uani 1 1 d . . . C17 C 0.1367(3) -0.1420(2) 0.02844(19) 0.0498(11) Uani 1 1 d . . . H17A H 0.1565 -0.1752 0.0013 0.075 Uiso 1 1 calc R . . H17B H 0.1252 -0.1631 0.0655 0.075 Uiso 1 1 calc R . . H17C H 0.1762 -0.1076 0.0341 0.075 Uiso 1 1 calc R . . N21 N 0.43998(18) 0.22616(15) 0.37631(14) 0.0367(8) Uani 1 1 d . . . H21A H 0.4642 0.2169 0.4087 0.044 Uiso 1 1 calc R . . N31 N 0.5291(2) 0.31154(18) 0.43615(15) 0.0527(10) Uani 1 1 d . . . H31A H 0.5293 0.2686 0.4415 0.063 Uiso 1 1 calc R . . C22 C 0.4022(2) 0.1762(2) 0.34837(18) 0.0423(10) Uani 1 1 d . . . H22A H 0.4015 0.1331 0.3644 0.051 Uiso 1 1 calc R . . C23 C 0.3644(2) 0.1889(2) 0.29600(19) 0.0477(11) Uani 1 1 d . . . H23A H 0.3392 0.1544 0.2754 0.057 Uiso 1 1 calc R . . C24 C 0.3646(3) 0.2538(2) 0.27452(19) 0.0532(12) Uani 1 1 d . . . H24A H 0.3380 0.2636 0.2396 0.064 Uiso 1 1 calc R . . C25 C 0.4036(2) 0.3044(2) 0.30416(17) 0.0438(10) Uani 1 1 d . . . H25A H 0.4040 0.3480 0.2891 0.053 Uiso 1 1 calc R . . C26 C 0.4422(2) 0.28997(19) 0.35661(17) 0.0344(9) Uani 1 1 d . . . C32 C 0.5706(3) 0.3521(3) 0.4712(2) 0.0630(14) Uani 1 1 d . . . H32A H 0.5994 0.3336 0.5021 0.076 Uiso 1 1 calc R . . C33 C 0.5721(3) 0.4213(3) 0.4627(2) 0.0608(14) Uani 1 1 d . . . H33A H 0.6019 0.4488 0.4875 0.073 Uiso 1 1 calc R . . C34 C 0.5296(3) 0.4484(2) 0.4179(2) 0.0578(13) Uani 1 1 d . . . H34A H 0.5301 0.4947 0.4115 0.069 Uiso 1 1 calc R . . C35 C 0.4858(2) 0.4068(2) 0.38214(19) 0.0436(10) Uani 1 1 d . . . H35A H 0.4558 0.4244 0.3514 0.052 Uiso 1 1 calc R . . C36 C 0.4873(2) 0.33897(19) 0.39269(16) 0.0357(9) 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 0.03320(10) 0.02976(10) 0.02275(9) -0.00098(9) 0.00105(9) -0.00477(9) F1 0.0575(18) 0.116(3) 0.102(3) -0.050(2) 0.0341(18) -0.0143(19) F2 0.067(2) 0.0538(19) 0.253(5) -0.004(2) 0.060(3) -0.0244(16) F3 0.056(2) 0.136(3) 0.121(3) -0.021(3) -0.007(2) 0.028(2) F4 0.0407(17) 0.144(3) 0.102(2) -0.082(2) -0.0063(16) -0.0087(17) F5 0.120(3) 0.084(2) 0.106(3) -0.064(2) 0.024(2) -0.020(2) F6 0.064(2) 0.164(3) 0.0497(18) -0.041(2) -0.0191(15) 0.033(2) F7 0.0463(18) 0.125(3) 0.0534(18) -0.0403(17) -0.0044(13) 0.0158(16) F11 0.0521(18) 0.203(4) 0.064(2) 0.035(2) 0.0135(15) 0.058(2) F12 0.071(2) 0.219(5) 0.076(2) -0.028(3) -0.041(2) 0.028(3) F13 0.097(3) 0.130(3) 0.163(4) 0.084(3) 0.026(3) 0.059(2) F14 0.0630(19) 0.108(2) 0.0426(16) 0.0411(16) 0.0083(13) 0.0240(15) F15 0.0676(19) 0.117(2) 0.0379(16) -0.0097(16) 0.0140(14) 0.0033(17) F16 0.0731(19) 0.0637(18) 0.098(2) 0.0397(17) 0.0378(17) 0.0023(15) F17 0.0391(15) 0.0740(17) 0.0516(16) 0.0112(14) 0.0100(12) 0.0015(13) F21 0.088(2) 0.0548(17) 0.115(3) -0.0010(18) 0.049(2) 0.0083(16) F22 0.0686(19) 0.134(3) 0.0434(17) -0.0317(17) -0.0057(14) 0.0369(18) F23 0.0444(17) 0.093(2) 0.083(2) -0.0079(18) -0.0060(15) -0.0002(15) F24 0.082(2) 0.0778(19) 0.0548(18) 0.0068(15) 0.0358(15) -0.0118(16) F25 0.233(5) 0.115(3) 0.071(3) 0.059(2) 0.052(3) 0.032(3) F26 0.166(4) 0.076(2) 0.166(4) 0.012(2) 0.077(3) -0.049(3) F27 0.181(4) 0.077(2) 0.126(3) 0.059(2) 0.080(3) 0.037(2) O1 0.0434(16) 0.0497(16) 0.0327(15) -0.0109(14) 0.0082(13) -0.0163(14) O2 0.0350(16) 0.0406(15) 0.0358(16) -0.0117(13) -0.0015(12) -0.0034(12) O6 0.0304(14) 0.0425(15) 0.0306(15) 0.0018(13) 0.0002(12) -0.0022(11) O7 0.0354(15) 0.0388(14) 0.0276(15) 0.0024(12) 0.0022(11) -0.0002(12) O11 0.0430(16) 0.0405(15) 0.0295(15) -0.0039(13) 0.0041(13) -0.0091(12) O12 0.0362(15) 0.0260(13) 0.0309(15) -0.0011(11) -0.0008(11) -0.0005(11) O16 0.059(2) 0.0470(17) 0.0414(18) 0.0125(14) 0.0082(14) -0.0021(14) O17 0.0463(17) 0.0351(14) 0.0324(15) -0.0058(13) -0.0023(14) 0.0008(12) C1 0.040(3) 0.061(3) 0.084(4) -0.018(3) 0.007(3) -0.009(2) C2 0.037(2) 0.037(2) 0.043(3) -0.0049(19) 0.002(2) -0.0063(19) C3 0.035(3) 0.064(3) 0.061(3) -0.029(3) -0.008(2) -0.007(2) C4 0.047(3) 0.048(3) 0.036(2) -0.018(2) -0.005(2) 0.002(2) C5 0.048(3) 0.078(4) 0.055(3) -0.035(3) -0.013(2) 0.008(3) C6 0.048(3) 0.104(4) 0.045(3) 0.006(3) -0.006(2) 0.018(3) C7 0.037(2) 0.044(2) 0.036(3) 0.001(2) -0.0024(19) -0.0004(19) C8 0.038(3) 0.055(3) 0.033(2) 0.014(2) 0.0005(19) 0.003(2) C9 0.036(2) 0.037(2) 0.033(2) 0.0013(18) 0.0048(18) -0.0084(18) C10 0.044(3) 0.052(3) 0.040(3) 0.012(2) 0.010(2) -0.004(2) C11 0.044(3) 0.064(3) 0.039(3) -0.006(2) 0.005(2) -0.001(2) C12 0.040(2) 0.052(3) 0.025(2) -0.007(2) 0.0008(18) -0.009(2) C13 0.052(3) 0.060(3) 0.030(2) 0.005(2) 0.014(2) -0.010(2) C14 0.065(3) 0.053(3) 0.035(3) 0.010(2) 0.012(2) -0.009(2) C15 0.144(7) 0.066(4) 0.075(5) 0.026(3) 0.062(5) 0.014(4) C16 0.044(2) 0.031(2) 0.029(2) 0.0071(18) 0.0055(18) -0.0021(18) C17 0.059(3) 0.039(2) 0.052(3) 0.001(2) -0.013(2) 0.011(2) N21 0.0351(19) 0.0426(19) 0.0325(19) 0.0024(16) -0.0062(15) 0.0056(15) N31 0.063(3) 0.046(2) 0.049(2) 0.0026(19) -0.015(2) -0.0084(19) C22 0.041(3) 0.036(2) 0.050(3) 0.000(2) -0.002(2) -0.0039(19) C23 0.047(3) 0.044(3) 0.053(3) -0.006(2) -0.016(2) 0.001(2) C24 0.059(3) 0.053(3) 0.048(3) -0.001(2) -0.019(2) 0.008(2) C25 0.055(3) 0.039(2) 0.038(2) 0.0094(19) -0.006(2) 0.005(2) C26 0.033(2) 0.040(2) 0.030(2) 0.0010(18) 0.0017(17) 0.0069(18) C32 0.067(3) 0.069(3) 0.053(3) 0.001(3) -0.023(3) -0.009(3) C33 0.061(3) 0.065(3) 0.057(3) -0.010(3) -0.003(3) -0.021(2) C34 0.064(3) 0.051(3) 0.059(3) -0.002(2) 0.006(3) -0.018(2) C35 0.040(3) 0.044(2) 0.046(3) 0.001(2) 0.003(2) -0.004(2) C36 0.035(2) 0.045(2) 0.027(2) 0.0007(19) 0.0005(17) -0.0015(18) _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 O6 2.386(2) . ? Eu1 O12 2.407(2) . ? Eu1 O16 2.415(3) . ? Eu1 O11 2.422(3) . ? Eu1 O2 2.431(2) . ? Eu1 O1 2.436(3) . ? Eu1 O17 2.459(2) 5 ? Eu1 O7 2.476(2) . ? Eu1 O12 2.530(2) 5 ? Eu1 C16 2.882(4) 5 ? Eu1 Eu1 4.1261(5) 5 ? F1 C1 1.299(5) . ? F2 C1 1.274(5) . ? F3 C1 1.349(6) . ? F4 C3 1.371(4) . ? F5 C5 1.315(6) . ? F6 C5 1.328(5) . ? F7 C5 1.313(5) . ? F11 C6 1.291(5) . ? F12 C6 1.305(6) . ? F13 C6 1.317(6) . ? F14 C8 1.365(4) . ? F15 C10 1.322(5) . ? F16 C10 1.323(4) . ? F17 C10 1.332(5) . ? F21 C11 1.303(5) . ? F22 C11 1.316(5) . ? F23 C11 1.334(5) . ? F24 C13 1.366(4) . ? F25 C15 1.307(7) . ? F26 C15 1.329(8) . ? F27 C15 1.319(6) . ? O1 C2 1.232(4) . ? O2 C4 1.244(4) . ? O6 C7 1.246(4) . ? O7 C9 1.239(4) . ? O11 C12 1.258(4) . ? O12 C16 1.278(4) . ? O12 Eu1 2.530(2) 5 ? O16 C14 1.248(5) . ? O17 C16 1.246(4) . ? O17 Eu1 2.459(2) 5 ? C1 C2 1.527(6) . ? C2 C3 1.391(6) . ? C3 C4 1.384(6) . ? C4 C5 1.531(6) . ? C6 C7 1.523(6) . ? C7 C8 1.385(5) . ? C8 C9 1.399(5) . ? C9 C10 1.544(5) . ? C11 C12 1.548(6) . ? C12 C13 1.374(5) . ? C13 C14 1.387(6) . ? C14 C15 1.531(7) . ? C16 C17 1.493(5) . ? C16 Eu1 2.882(4) 5 ? N21 C22 1.337(5) . ? N21 C26 1.342(4) . ? N31 C32 1.329(5) . ? N31 C36 1.328(5) . ? C22 C23 1.371(5) . ? C23 C24 1.376(5) . ? C24 C25 1.373(5) . ? C25 C26 1.386(5) . ? C26 C36 1.480(5) . ? C32 C33 1.385(6) . ? C33 C34 1.354(6) . ? C34 C35 1.371(6) . ? C35 C36 1.366(5) . ? 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 O6 Eu1 O12 78.56(8) . . ? O6 Eu1 O16 137.40(9) . . ? O12 Eu1 O16 120.94(9) . . ? O6 Eu1 O11 84.03(9) . . ? O12 Eu1 O11 70.21(8) . . ? O16 Eu1 O11 70.66(9) . . ? O6 Eu1 O2 77.60(8) . . ? O12 Eu1 O2 137.76(8) . . ? O16 Eu1 O2 100.05(9) . . ? O11 Eu1 O2 139.92(8) . . ? O6 Eu1 O1 69.76(9) . . ? O12 Eu1 O1 131.37(9) . . ? O16 Eu1 O1 69.72(9) . . ? O11 Eu1 O1 70.64(8) . . ? O2 Eu1 O1 69.64(8) . . ? O6 Eu1 O17 140.17(9) . 5 ? O12 Eu1 O17 110.47(8) . 5 ? O16 Eu1 O17 72.64(9) . 5 ? O11 Eu1 O17 135.79(9) . 5 ? O2 Eu1 O17 70.27(8) . 5 ? O1 Eu1 O17 117.59(9) . 5 ? O6 Eu1 O7 71.74(8) . . ? O12 Eu1 O7 70.93(8) . . ? O16 Eu1 O7 147.65(9) . . ? O11 Eu1 O7 137.38(8) . . ? O2 Eu1 O7 68.70(8) . . ? O1 Eu1 O7 127.78(8) . . ? O17 Eu1 O7 75.02(8) 5 . ? O6 Eu1 O12 143.13(8) . 5 ? O12 Eu1 O12 66.63(9) . 5 ? O16 Eu1 O12 74.62(8) . 5 ? O11 Eu1 O12 94.84(8) . 5 ? O2 Eu1 O12 120.92(8) . 5 ? O1 Eu1 O12 144.20(8) . 5 ? O17 Eu1 O12 51.68(8) 5 5 ? O7 Eu1 O12 85.33(8) . 5 ? O6 Eu1 C16 151.84(9) . 5 ? O12 Eu1 C16 89.54(10) . 5 ? O16 Eu1 C16 70.44(10) . 5 ? O11 Eu1 C16 116.01(10) . 5 ? O2 Eu1 C16 95.45(10) . 5 ? O1 Eu1 C16 133.75(10) . 5 ? O17 Eu1 C16 25.45(9) 5 5 ? O7 Eu1 C16 80.29(9) . 5 ? O12 Eu1 C16 26.30(9) 5 5 ? O6 Eu1 Eu1 112.01(6) . 5 ? O12 Eu1 Eu1 34.25(6) . 5 ? O16 Eu1 Eu1 97.89(7) . 5 ? O11 Eu1 Eu1 81.62(6) . 5 ? O2 Eu1 Eu1 138.33(6) . 5 ? O1 Eu1 Eu1 151.98(6) . 5 ? O17 Eu1 Eu1 79.86(6) 5 5 ? O7 Eu1 Eu1 76.08(6) . 5 ? O12 Eu1 Eu1 32.38(5) 5 5 ? C16 Eu1 Eu1 56.33(8) 5 5 ? C2 O1 Eu1 136.2(3) . . ? C4 O2 Eu1 135.4(3) . . ? C7 O6 Eu1 137.4(2) . . ? C9 O7 Eu1 132.7(2) . . ? C12 O11 Eu1 132.8(2) . . ? C16 O12 Eu1 140.1(2) . . ? C16 O12 Eu1 92.4(2) . 5 ? Eu1 O12 Eu1 113.38(9) . 5 ? C14 O16 Eu1 132.7(3) . . ? C16 O17 Eu1 96.6(2) . 5 ? F2 C1 F1 111.4(5) . . ? F2 C1 F3 104.7(4) . . ? F1 C1 F3 102.8(4) . . ? F2 C1 C2 113.6(4) . . ? F1 C1 C2 112.1(4) . . ? F3 C1 C2 111.6(4) . . ? O1 C2 C3 124.5(4) . . ? O1 C2 C1 116.4(4) . . ? C3 C2 C1 119.0(4) . . ? F4 C3 C4 118.0(4) . . ? F4 C3 C2 117.2(4) . . ? C4 C3 C2 124.8(4) . . ? O2 C4 C3 125.5(4) . . ? O2 C4 C5 116.2(4) . . ? C3 C4 C5 118.3(4) . . ? F7 C5 F5 107.8(4) . . ? F7 C5 F6 106.5(4) . . ? F5 C5 F6 107.3(4) . . ? F7 C5 C4 111.9(4) . . ? F5 C5 C4 111.7(4) . . ? F6 C5 C4 111.4(4) . . ? F11 C6 F12 108.7(5) . . ? F11 C6 F13 107.3(5) . . ? F12 C6 F13 105.6(4) . . ? F11 C6 C7 112.0(4) . . ? F12 C6 C7 110.9(4) . . ? F13 C6 C7 111.9(4) . . ? O6 C7 C8 124.8(4) . . ? O6 C7 C6 116.7(4) . . ? C8 C7 C6 118.6(4) . . ? F14 C8 C7 117.5(3) . . ? F14 C8 C9 116.9(3) . . ? C7 C8 C9 125.5(4) . . ? O7 C9 C8 126.9(4) . . ? O7 C9 C10 117.2(4) . . ? C8 C9 C10 116.0(4) . . ? F15 C10 F16 107.9(4) . . ? F15 C10 F17 106.9(4) . . ? F16 C10 F17 106.8(4) . . ? F15 C10 C9 112.5(3) . . ? F16 C10 C9 112.3(4) . . ? F17 C10 C9 110.2(3) . . ? F21 C11 F22 108.2(4) . . ? F21 C11 F23 107.3(4) . . ? F22 C11 F23 106.3(4) . . ? F21 C11 C12 111.6(4) . . ? F22 C11 C12 112.5(4) . . ? F23 C11 C12 110.7(4) . . ? O11 C12 C13 125.7(4) . . ? O11 C12 C11 115.1(4) . . ? C13 C12 C11 119.1(4) . . ? F24 C13 C12 117.3(4) . . ? F24 C13 C14 118.3(4) . . ? C12 C13 C14 124.4(4) . . ? O16 C14 C13 126.1(4) . . ? O16 C14 C15 115.7(4) . . ? C13 C14 C15 118.2(4) . . ? F25 C15 F27 108.3(6) . . ? F25 C15 F26 106.2(5) . . ? F27 C15 F26 106.9(6) . . ? F25 C15 C14 112.7(5) . . ? F27 C15 C14 111.5(5) . . ? F26 C15 C14 110.9(6) . . ? O17 C16 O12 119.1(4) . . ? O17 C16 C17 121.3(3) . . ? O12 C16 C17 119.6(4) . . ? O17 C16 Eu1 58.0(2) . 5 ? O12 C16 Eu1 61.29(19) . 5 ? C17 C16 Eu1 174.0(3) . 5 ? C22 N21 C26 123.6(3) . . ? C32 N31 C36 118.3(4) . . ? N21 C22 C23 119.7(4) . . ? C22 C23 C24 118.5(4) . . ? C23 C24 C25 120.6(4) . . ? C24 C25 C26 119.6(4) . . ? N21 C26 C25 117.9(4) . . ? N21 C26 C36 116.6(3) . . ? C25 C26 C36 125.5(4) . . ? N31 C32 C33 121.7(5) . . ? C34 C33 C32 119.2(5) . . ? C33 C34 C35 119.3(4) . . ? C36 C35 C34 118.6(4) . . ? N31 C36 C35 122.9(4) . . ? N31 C36 C26 114.4(3) . . ? C35 C36 C26 122.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Eu1 O1 C2 -63.4(4) . . . . ? O12 Eu1 O1 C2 -116.0(4) . . . . ? O16 Eu1 O1 C2 130.1(4) . . . . ? O11 Eu1 O1 C2 -154.0(4) . . . . ? O2 Eu1 O1 C2 20.5(4) . . . . ? O17 Eu1 O1 C2 73.6(4) 5 . . . ? O7 Eu1 O1 C2 -18.4(4) . . . . ? O12 Eu1 O1 C2 135.5(4) 5 . . . ? C16 Eu1 O1 C2 98.1(4) 5 . . . ? Eu1 Eu1 O1 C2 -162.4(3) 5 . . . ? O6 Eu1 O2 C4 53.6(4) . . . . ? O12 Eu1 O2 C4 110.7(4) . . . . ? O16 Eu1 O2 C4 -82.9(4) . . . . ? O11 Eu1 O2 C4 -11.1(4) . . . . ? O1 Eu1 O2 C4 -19.1(4) . . . . ? O17 Eu1 O2 C4 -150.3(4) 5 . . . ? O7 Eu1 O2 C4 128.6(4) . . . . ? O12 Eu1 O2 C4 -161.0(4) 5 . . . ? C16 Eu1 O2 C4 -154.0(4) 5 . . . ? Eu1 Eu1 O2 C4 162.9(3) 5 . . . ? O12 Eu1 O6 C7 -83.1(4) . . . . ? O16 Eu1 O6 C7 153.2(3) . . . . ? O11 Eu1 O6 C7 -154.0(4) . . . . ? O2 Eu1 O6 C7 61.8(4) . . . . ? O1 Eu1 O6 C7 134.4(4) . . . . ? O17 Eu1 O6 C7 25.2(4) 5 . . . ? O7 Eu1 O6 C7 -9.6(4) . . . . ? O12 Eu1 O6 C7 -63.9(4) 5 . . . ? C16 Eu1 O6 C7 -16.4(5) 5 . . . ? Eu1 Eu1 O6 C7 -75.6(4) 5 . . . ? O6 Eu1 O7 C9 8.7(3) . . . . ? O12 Eu1 O7 C9 92.6(3) . . . . ? O16 Eu1 O7 C9 -149.3(3) . . . . ? O11 Eu1 O7 C9 67.4(4) . . . . ? O2 Eu1 O7 C9 -74.7(3) . . . . ? O1 Eu1 O7 C9 -35.5(4) . . . . ? O17 Eu1 O7 C9 -149.0(3) 5 . . . ? O12 Eu1 O7 C9 159.5(3) 5 . . . ? C16 Eu1 O7 C9 -174.5(3) 5 . . . ? Eu1 Eu1 O7 C9 128.0(3) 5 . . . ? O6 Eu1 O11 C12 -118.5(3) . . . . ? O12 Eu1 O11 C12 161.5(4) . . . . ? O16 Eu1 O11 C12 26.7(3) . . . . ? O2 Eu1 O11 C12 -55.9(4) . . . . ? O1 Eu1 O11 C12 -47.9(3) . . . . ? O17 Eu1 O11 C12 62.1(4) 5 . . . ? O7 Eu1 O11 C12 -173.1(3) . . . . ? O12 Eu1 O11 C12 98.5(3) 5 . . . ? C16 Eu1 O11 C12 82.2(3) 5 . . . ? Eu1 Eu1 O11 C12 128.1(3) 5 . . . ? O6 Eu1 O12 C16 -66.3(4) . . . . ? O16 Eu1 O12 C16 72.6(4) . . . . ? O11 Eu1 O12 C16 21.4(4) . . . . ? O2 Eu1 O12 C16 -123.1(4) . . . . ? O1 Eu1 O12 C16 -16.8(4) . . . . ? O17 Eu1 O12 C16 154.1(4) 5 . . . ? O7 Eu1 O12 C16 -140.8(4) . . . . ? O12 Eu1 O12 C16 126.0(4) 5 . . . ? C16 Eu1 O12 C16 139.3(3) 5 . . . ? Eu1 Eu1 O12 C16 126.0(4) 5 . . . ? O6 Eu1 O12 Eu1 167.62(11) . . . 5 ? O16 Eu1 O12 Eu1 -53.43(13) . . . 5 ? O11 Eu1 O12 Eu1 -104.67(11) . . . 5 ? O2 Eu1 O12 Eu1 110.90(12) . . . 5 ? O1 Eu1 O12 Eu1 -142.82(10) . . . 5 ? O17 Eu1 O12 Eu1 28.08(12) 5 . . 5 ? O7 Eu1 O12 Eu1 93.18(10) . . . 5 ? O12 Eu1 O12 Eu1 0.0 5 . . 5 ? C16 Eu1 O12 Eu1 13.30(11) 5 . . 5 ? O6 Eu1 O16 C14 29.9(4) . . . . ? O12 Eu1 O16 C14 -78.2(4) . . . . ? O11 Eu1 O16 C14 -27.2(4) . . . . ? O2 Eu1 O16 C14 112.4(4) . . . . ? O1 Eu1 O16 C14 48.7(4) . . . . ? O17 Eu1 O16 C14 177.9(4) 5 . . . ? O7 Eu1 O16 C14 178.2(3) . . . . ? O12 Eu1 O16 C14 -128.1(4) 5 . . . ? C16 Eu1 O16 C14 -155.3(4) 5 . . . ? Eu1 Eu1 O16 C14 -105.3(4) 5 . . . ? Eu1 O1 C2 C3 -16.7(7) . . . . ? Eu1 O1 C2 C1 164.5(3) . . . . ? F2 C1 C2 O1 116.4(5) . . . . ? F1 C1 C2 O1 -10.9(6) . . . . ? F3 C1 C2 O1 -125.6(4) . . . . ? F2 C1 C2 C3 -62.4(7) . . . . ? F1 C1 C2 C3 170.3(4) . . . . ? F3 C1 C2 C3 55.6(6) . . . . ? O1 C2 C3 F4 -179.8(4) . . . . ? C1 C2 C3 F4 -1.1(6) . . . . ? O1 C2 C3 C4 -0.9(8) . . . . ? C1 C2 C3 C4 177.8(5) . . . . ? Eu1 O2 C4 C3 14.6(7) . . . . ? Eu1 O2 C4 C5 -164.5(3) . . . . ? F4 C3 C4 O2 -179.2(4) . . . . ? C2 C3 C4 O2 1.8(8) . . . . ? F4 C3 C4 C5 -0.1(7) . . . . ? C2 C3 C4 C5 -179.1(4) . . . . ? O2 C4 C5 F7 3.0(6) . . . . ? C3 C4 C5 F7 -176.2(4) . . . . ? O2 C4 C5 F5 -118.0(5) . . . . ? C3 C4 C5 F5 62.8(6) . . . . ? O2 C4 C5 F6 122.1(4) . . . . ? C3 C4 C5 F6 -57.1(6) . . . . ? Eu1 O6 C7 C8 5.9(7) . . . . ? Eu1 O6 C7 C6 -174.3(3) . . . . ? F11 C6 C7 O6 -6.4(7) . . . . ? F12 C6 C7 O6 115.3(5) . . . . ? F13 C6 C7 O6 -127.0(5) . . . . ? F11 C6 C7 C8 173.5(4) . . . . ? F12 C6 C7 C8 -64.8(6) . . . . ? F13 C6 C7 C8 52.8(6) . . . . ? O6 C7 C8 F14 -178.4(4) . . . . ? C6 C7 C8 F14 1.7(6) . . . . ? O6 C7 C8 C9 4.6(7) . . . . ? C6 C7 C8 C9 -175.2(4) . . . . ? Eu1 O7 C9 C8 -4.8(6) . . . . ? Eu1 O7 C9 C10 175.9(2) . . . . ? F14 C8 C9 O7 178.3(4) . . . . ? C7 C8 C9 O7 -4.8(7) . . . . ? F14 C8 C9 C10 -2.4(5) . . . . ? C7 C8 C9 C10 174.5(4) . . . . ? O7 C9 C10 F15 -119.2(4) . . . . ? C8 C9 C10 F15 61.5(5) . . . . ? O7 C9 C10 F16 119.0(4) . . . . ? C8 C9 C10 F16 -60.4(5) . . . . ? O7 C9 C10 F17 0.0(5) . . . . ? C8 C9 C10 F17 -179.4(4) . . . . ? Eu1 O11 C12 C13 -19.6(6) . . . . ? Eu1 O11 C12 C11 159.4(3) . . . . ? F21 C11 C12 O11 4.5(5) . . . . ? F22 C11 C12 O11 126.3(4) . . . . ? F23 C11 C12 O11 -114.9(4) . . . . ? F21 C11 C12 C13 -176.5(4) . . . . ? F22 C11 C12 C13 -54.6(5) . . . . ? F23 C11 C12 C13 64.1(5) . . . . ? O11 C12 C13 F24 177.2(4) . . . . ? C11 C12 C13 F24 -1.7(6) . . . . ? O11 C12 C13 C14 -4.0(7) . . . . ? C11 C12 C13 C14 177.1(4) . . . . ? Eu1 O16 C14 C13 20.7(7) . . . . ? Eu1 O16 C14 C15 -157.5(4) . . . . ? F24 C13 C14 O16 -177.8(4) . . . . ? C12 C13 C14 O16 3.4(8) . . . . ? F24 C13 C14 C15 0.4(7) . . . . ? C12 C13 C14 C15 -178.4(5) . . . . ? O16 C14 C15 F25 -128.3(6) . . . . ? C13 C14 C15 F25 53.4(8) . . . . ? O16 C14 C15 F27 -6.3(8) . . . . ? C13 C14 C15 F27 175.4(5) . . . . ? O16 C14 C15 F26 112.8(5) . . . . ? C13 C14 C15 F26 -65.6(7) . . . . ? Eu1 O17 C16 O12 -5.4(4) 5 . . . ? Eu1 O17 C16 C17 173.0(3) 5 . . . ? Eu1 O12 C16 O17 -126.8(3) . . . . ? Eu1 O12 C16 O17 5.2(3) 5 . . . ? Eu1 O12 C16 C17 54.8(5) . . . . ? Eu1 O12 C16 C17 -173.2(3) 5 . . . ? Eu1 O12 C16 Eu1 -132.0(3) . . . 5 ? C26 N21 C22 C23 1.4(6) . . . . ? N21 C22 C23 C24 -2.0(6) . . . . ? C22 C23 C24 C25 1.7(7) . . . . ? C23 C24 C25 C26 -0.9(7) . . . . ? C22 N21 C26 C25 -0.5(6) . . . . ? C22 N21 C26 C36 -179.5(3) . . . . ? C24 C25 C26 N21 0.3(6) . . . . ? C24 C25 C26 C36 179.1(4) . . . . ? C36 N31 C32 C33 -1.1(7) . . . . ? N31 C32 C33 C34 0.6(8) . . . . ? C32 C33 C34 C35 0.3(7) . . . . ? C33 C34 C35 C36 -0.6(6) . . . . ? C32 N31 C36 C35 0.7(6) . . . . ? C32 N31 C36 C26 -179.2(4) . . . . ? C34 C35 C36 N31 0.1(6) . . . . ? C34 C35 C36 C26 -180.0(4) . . . . ? N21 C26 C36 N31 8.7(5) . . . . ? C25 C26 C36 N31 -170.2(4) . . . . ? N21 C26 C36 C35 -171.2(4) . . . . ? C25 C26 C36 C35 9.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.100 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.100