Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'William J. Evans' 'Dimitrios G. Giarikos' 'Matthew A. Johnston' 'Michael A. Greci' 'Joseph W. Ziller' _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof William Evans' _publ_contact_author_email 'wevans@uci.edu' _publ_section_title ; Reactivity of the Europium Hexafluroacetylacetonate (hfac) Complex, Eu(hfac)3(diglyme), and related Analogs with Potassium: Formation of the Fluoride hfac "Ate" Complexes, [LnF(hfac)3K(diglyme)]2 ; data_dg24 _database_code_CSD 171876 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 F18 O9 Sm' _chemical_formula_weight 905.70 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' 'Sm' 'Sm' -0.1638 3.4418 '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 10.1210(6) _cell_length_b 15.6745(10) _cell_length_c 19.3010(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.2480(10) _cell_angle_gamma 90.00 _cell_volume 3037.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4531 _exptl_absorpt_correction_T_max 0.6922 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% '< 1.0' _diffrn_reflns_number 31472 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7313 _reflns_number_gt 6668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0253P)^2^+1.4734P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXTL _refine_ls_extinction_coef 0.00017(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7313 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm 0.738977(8) 0.888830(6) 0.238884(4) 0.02031(4) Uani 1 1 d . . . O1 O 0.74804(13) 0.92665(8) 0.11904(6) 0.0259(3) Uani 1 1 d . . . O2 O 0.89748(13) 0.79662(8) 0.18996(7) 0.0277(3) Uani 1 1 d . . . O3 O 0.95279(13) 0.95487(8) 0.25911(7) 0.0297(3) Uani 1 1 d . . . O4 O 0.86739(13) 0.81311(8) 0.33374(7) 0.0272(3) Uani 1 1 d . . . O5 O 0.72328(14) 0.96516(8) 0.34753(7) 0.0305(3) Uani 1 1 d . . . O6 O 0.58309(12) 0.81696(8) 0.30308(6) 0.0263(3) Uani 1 1 d . . . O7 O 0.60552(12) 0.77578(8) 0.16214(7) 0.0266(3) Uani 1 1 d . . . O8 O 0.50629(12) 0.93451(8) 0.18472(7) 0.0261(3) Uani 1 1 d . . . O9 O 0.70927(13) 1.04907(8) 0.22221(7) 0.0272(3) Uani 1 1 d . . . C1 C 0.7868(2) 0.96005(13) 0.00544(10) 0.0351(4) Uani 1 1 d . . . C2 C 0.81994(19) 0.90857(12) 0.07334(9) 0.0255(4) Uani 1 1 d . A . C3 C 0.9250(2) 0.85070(12) 0.07738(10) 0.0302(4) Uani 1 1 d . . . H3A H 0.9762 0.8457 0.0396 0.036 Uiso 1 1 calc R A . C4 C 0.95535(17) 0.80008(11) 0.13647(10) 0.0253(4) Uani 1 1 d . A . C5 C 1.0745(2) 0.73926(15) 0.13824(12) 0.0376(5) Uani 1 1 d . . . C6 C 1.1719(2) 1.00127(17) 0.28854(14) 0.0495(6) Uani 1 1 d . . . C7 C 1.05515(18) 0.94277(12) 0.30104(10) 0.0287(4) Uani 1 1 d . B . C8 C 1.0751(2) 0.88523(12) 0.35626(11) 0.0318(4) Uani 1 1 d . . . H8A H 1.1573 0.8860 0.3861 0.038 Uiso 1 1 calc R B . C9 C 0.97755(18) 0.82655(11) 0.36874(9) 0.0256(4) Uani 1 1 d . B . C10 C 1.0066(2) 0.76882(14) 0.43295(11) 0.0406(5) Uani 1 1 d . . . C11 C 0.7246(3) 1.00731(17) 0.46389(12) 0.0482(6) Uani 1 1 d . . . C12 C 0.6766(2) 0.94769(12) 0.40277(10) 0.0308(4) Uani 1 1 d . C . C13 C 0.5897(2) 0.88231(13) 0.41465(11) 0.0341(4) Uani 1 1 d . . . H13A H 0.5579 0.8779 0.4588 0.041 Uiso 1 1 calc R C . C14 C 0.54878(19) 0.82327(12) 0.36276(10) 0.0280(4) Uani 1 1 d . C . C15 C 0.4521(2) 0.75340(14) 0.38067(12) 0.0404(5) Uani 1 1 d . . . C16 C 0.6346(2) 0.68626(12) 0.16381(13) 0.0400(5) Uani 1 1 d . . . H16A H 0.5703 0.6565 0.1300 0.060 Uiso 1 1 calc R . . H16B H 0.6288 0.6640 0.2108 0.060 Uiso 1 1 calc R . . H16C H 0.7248 0.6771 0.1518 0.060 Uiso 1 1 calc R . . C17 C 0.46426(18) 0.78965(12) 0.15101(10) 0.0303(4) Uani 1 1 d . . . H17A H 0.4249 0.7775 0.1944 0.036 Uiso 1 1 calc R . . H17B H 0.4224 0.7514 0.1137 0.036 Uiso 1 1 calc R . . C18 C 0.4406(2) 0.88125(12) 0.13005(11) 0.0316(4) Uani 1 1 d . . . H18A H 0.4767 0.8927 0.0856 0.038 Uiso 1 1 calc R . . H18B H 0.3439 0.8935 0.1232 0.038 Uiso 1 1 calc R . . C19 C 0.48625(19) 1.02381(12) 0.16833(11) 0.0307(4) Uani 1 1 d . . . H19A H 0.3915 1.0395 0.1686 0.037 Uiso 1 1 calc R . . H19B H 0.5119 1.0365 0.1216 0.037 Uiso 1 1 calc R . . C20 C 0.5726(2) 1.07249(12) 0.22352(11) 0.0316(4) Uani 1 1 d . . . H20A H 0.5615 1.1345 0.2150 0.038 Uiso 1 1 calc R . . H20B H 0.5459 1.0596 0.2700 0.038 Uiso 1 1 calc R . . C21 C 0.7731(2) 1.09933(12) 0.17311(12) 0.0359(5) Uani 1 1 d . . . H21A H 0.7464 1.1592 0.1761 0.054 Uiso 1 1 calc R . . H21B H 0.7461 1.0782 0.1257 0.054 Uiso 1 1 calc R . . H21C H 0.8700 1.0947 0.1843 0.054 Uiso 1 1 calc R . . F1 F 0.6552(14) 0.9684(12) -0.0094(9) 0.060(3) Uani 0.50 1 d P A 1 F2 F 0.8362(13) 1.0376(6) 0.0142(6) 0.070(3) Uani 0.50 1 d P A 1 F3 F 0.8316(17) 0.9268(13) -0.0490(6) 0.076(4) Uani 0.50 1 d P A 1 F1B F 0.6609(13) 0.9823(11) -0.0042(8) 0.058(3) Uani 0.50 1 d P A 2 F2B F 0.8520(11) 1.0324(7) 0.0074(6) 0.075(3) Uani 0.50 1 d P A 2 F3B F 0.8139(16) 0.9196(12) -0.0507(6) 0.062(3) Uani 0.50 1 d P A 2 F4 F 1.1486(12) 0.7392(9) 0.1972(7) 0.078(4) Uani 0.50 1 d P A 1 F5 F 1.0244(11) 0.6588(7) 0.1296(6) 0.068(3) Uani 0.50 1 d P A 1 F6 F 1.1472(13) 0.7529(12) 0.0882(10) 0.049(3) Uani 0.50 1 d P A 1 F4B F 1.1697(13) 0.7674(10) 0.1893(9) 0.078(4) Uani 0.50 1 d P A 2 F5B F 1.0498(10) 0.6616(7) 0.1524(6) 0.070(3) Uani 0.50 1 d P A 2 F6B F 1.1342(15) 0.7381(12) 0.0805(9) 0.059(3) Uani 0.50 1 d P A 2 F7 F 1.1676(8) 1.0329(6) 0.2290(4) 0.104(4) Uani 0.50 1 d P B 1 F8 F 1.2859(11) 0.9680(10) 0.3101(7) 0.076(4) Uani 0.50 1 d P B 1 F9 F 1.1635(13) 1.0732(7) 0.3314(6) 0.091(3) Uani 0.50 1 d P B 1 F7B F 1.1878(10) 0.9876(5) 0.2178(4) 0.095(3) Uani 0.50 1 d P B 2 F8B F 1.2906(12) 0.9792(9) 0.3207(6) 0.0514(19) Uani 0.50 1 d P B 2 F9B F 1.1515(12) 1.0780(7) 0.2950(6) 0.100(4) Uani 0.50 1 d P B 2 F10 F 1.0994(12) 0.7947(8) 0.4804(8) 0.056(3) Uani 0.50 1 d P B 1 F11 F 1.0677(6) 0.6946(3) 0.4082(3) 0.0693(15) Uani 0.50 1 d P B 1 F12 F 0.9068(5) 0.7396(4) 0.4563(3) 0.0758(17) Uani 0.50 1 d P B 1 F10B F 1.1161(11) 0.7855(9) 0.4728(8) 0.053(3) Uani 0.50 1 d P B 2 F11B F 0.9910(7) 0.6908(3) 0.4218(3) 0.089(3) Uani 0.50 1 d P B 2 F12B F 0.9121(5) 0.7909(4) 0.4779(3) 0.0825(18) Uani 0.50 1 d P B 2 F13 F 0.8540(12) 1.0198(6) 0.4713(5) 0.0584(16) Uani 0.50 1 d P C 1 F14 F 0.6797(7) 1.0920(6) 0.4483(6) 0.0594(17) Uani 0.50 1 d P C 1 F15 F 0.6927(16) 0.9821(9) 0.5238(7) 0.103(4) Uani 0.50 1 d P C 1 F13B F 0.8513(12) 0.9985(8) 0.4801(6) 0.122(4) Uani 0.50 1 d P C 2 F14B F 0.6938(13) 1.0804(8) 0.4504(8) 0.120(4) Uani 0.50 1 d P C 2 F15B F 0.6638(15) 0.9939(9) 0.5196(7) 0.075(3) Uani 0.50 1 d P C 2 F16 F 0.5310(15) 0.6880(10) 0.4136(5) 0.0506(16) Uani 0.50 1 d P C 1 F17 F 0.3907(9) 0.7148(5) 0.3270(5) 0.066(2) Uani 0.50 1 d P C 1 F18 F 0.372(2) 0.7718(13) 0.4249(12) 0.046(4) Uani 0.50 1 d P C 1 F16B F 0.5064(15) 0.6828(10) 0.3939(6) 0.089(4) Uani 0.50 1 d P C 2 F17B F 0.3511(9) 0.7463(5) 0.3263(6) 0.070(2) Uani 0.50 1 d P C 2 F18B F 0.386(2) 0.7799(14) 0.4343(12) 0.044(3) Uani 0.50 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02108(5) 0.02333(5) 0.01663(5) 0.00195(3) 0.00276(3) -0.00001(3) O1 0.0289(7) 0.0291(6) 0.0204(6) 0.0025(5) 0.0060(5) 0.0034(5) O2 0.0274(7) 0.0317(7) 0.0248(6) 0.0042(5) 0.0061(5) 0.0052(5) O3 0.0261(7) 0.0324(7) 0.0304(7) 0.0060(6) 0.0030(5) -0.0028(5) O4 0.0277(6) 0.0287(6) 0.0240(6) 0.0041(5) -0.0010(5) -0.0024(5) O5 0.0405(8) 0.0291(7) 0.0228(6) -0.0015(5) 0.0070(6) -0.0041(5) O6 0.0270(6) 0.0301(6) 0.0222(6) 0.0018(5) 0.0051(5) -0.0019(5) O7 0.0272(6) 0.0249(6) 0.0273(7) -0.0016(5) 0.0015(5) 0.0001(5) O8 0.0249(6) 0.0270(6) 0.0258(6) 0.0021(5) 0.0007(5) 0.0018(5) O9 0.0322(7) 0.0231(6) 0.0265(6) 0.0028(5) 0.0039(5) -0.0004(5) C1 0.0461(12) 0.0376(11) 0.0223(9) 0.0038(8) 0.0073(8) 0.0079(9) C2 0.0293(9) 0.0273(8) 0.0198(9) 0.0000(7) 0.0028(7) -0.0010(7) C3 0.0337(10) 0.0349(10) 0.0234(9) 0.0022(8) 0.0093(7) 0.0059(8) C4 0.0223(8) 0.0276(8) 0.0263(9) -0.0017(7) 0.0036(7) 0.0023(7) C5 0.0313(11) 0.0450(12) 0.0384(12) 0.0073(9) 0.0121(9) 0.0114(9) C6 0.0287(11) 0.0598(15) 0.0588(16) 0.0216(13) 0.0010(10) -0.0104(10) C7 0.0245(9) 0.0309(9) 0.0309(10) -0.0014(8) 0.0049(7) -0.0036(7) C8 0.0273(10) 0.0360(10) 0.0307(10) 0.0007(8) -0.0021(8) -0.0022(7) C9 0.0293(9) 0.0254(8) 0.0216(8) -0.0015(7) 0.0012(7) 0.0016(7) C10 0.0437(12) 0.0409(11) 0.0331(11) 0.0103(9) -0.0117(9) -0.0075(9) C11 0.0616(16) 0.0534(15) 0.0317(12) -0.0131(10) 0.0136(11) -0.0114(12) C12 0.0394(11) 0.0315(9) 0.0220(9) -0.0021(7) 0.0055(8) 0.0032(8) C13 0.0427(12) 0.0385(11) 0.0229(9) 0.0010(8) 0.0114(8) -0.0021(8) C14 0.0293(9) 0.0305(9) 0.0255(9) 0.0058(7) 0.0080(7) 0.0017(7) C15 0.0462(13) 0.0409(12) 0.0380(12) 0.0013(9) 0.0200(10) -0.0087(10) C16 0.0432(12) 0.0258(9) 0.0489(13) 0.0001(9) -0.0025(10) 0.0017(8) C17 0.0269(9) 0.0338(10) 0.0286(10) -0.0029(8) -0.0030(7) -0.0033(7) C18 0.0277(10) 0.0369(10) 0.0283(10) 0.0014(8) -0.0040(8) 0.0005(8) C19 0.0299(10) 0.0298(9) 0.0326(10) 0.0064(8) 0.0044(8) 0.0082(7) C20 0.0370(11) 0.0277(9) 0.0308(10) -0.0004(8) 0.0069(8) 0.0083(8) C21 0.0461(12) 0.0260(9) 0.0371(11) 0.0060(8) 0.0108(9) -0.0033(8) F1 0.046(5) 0.092(6) 0.038(4) 0.019(3) -0.013(3) 0.001(4) F2 0.151(8) 0.031(3) 0.032(3) 0.005(2) 0.025(4) -0.006(3) F3 0.126(8) 0.079(6) 0.032(5) 0.020(5) 0.046(5) 0.048(5) F1B 0.063(7) 0.084(5) 0.029(3) 0.020(3) 0.013(4) 0.045(5) F2B 0.082(4) 0.078(6) 0.061(5) 0.040(4) -0.004(3) -0.039(4) F3B 0.097(5) 0.070(5) 0.016(4) -0.004(4) -0.004(3) 0.045(4) F4 0.052(6) 0.135(9) 0.044(2) -0.003(5) -0.006(4) 0.057(6) F5 0.069(5) 0.030(2) 0.108(7) 0.002(3) 0.025(4) 0.016(2) F6 0.031(2) 0.054(5) 0.066(6) 0.011(3) 0.029(2) 0.012(2) F4B 0.026(2) 0.126(8) 0.079(7) -0.023(5) -0.010(3) 0.015(4) F5B 0.048(4) 0.048(4) 0.124(8) 0.045(5) 0.047(5) 0.025(3) F6B 0.075(7) 0.065(7) 0.046(3) 0.015(4) 0.035(4) 0.039(5) F7 0.061(4) 0.162(8) 0.080(6) 0.076(6) -0.019(4) -0.064(5) F8 0.021(3) 0.078(5) 0.133(9) 0.013(5) 0.017(4) -0.008(3) F9 0.059(4) 0.040(4) 0.174(9) -0.014(5) 0.023(6) -0.026(3) F7B 0.067(3) 0.168(8) 0.054(3) 0.001(4) 0.030(2) -0.058(5) F8B 0.031(3) 0.058(3) 0.060(3) 0.016(3) -0.014(2) -0.014(2) F9B 0.051(3) 0.040(3) 0.213(13) 0.035(7) 0.028(8) -0.010(2) F10 0.094(7) 0.040(2) 0.025(2) -0.0002(18) -0.023(4) -0.016(4) F11 0.114(4) 0.0247(19) 0.061(3) 0.0032(16) -0.022(3) 0.013(2) F12 0.052(2) 0.112(4) 0.059(3) 0.057(3) -0.008(2) -0.023(3) F10B 0.034(2) 0.077(6) 0.042(5) 0.020(4) -0.017(2) -0.007(3) F11B 0.164(7) 0.0329(19) 0.052(3) 0.016(2) -0.052(4) -0.031(4) F12B 0.071(3) 0.138(5) 0.044(3) 0.046(3) 0.029(2) 0.039(3) F13 0.062(4) 0.068(2) 0.043(3) -0.015(2) -0.002(2) -0.021(2) F14 0.069(3) 0.037(3) 0.074(4) -0.024(2) 0.015(3) 0.004(2) F15 0.181(11) 0.109(7) 0.021(3) -0.019(4) 0.024(5) -0.087(7) F13B 0.059(5) 0.201(11) 0.096(7) -0.099(7) -0.028(4) 0.020(6) F14B 0.229(11) 0.043(4) 0.083(6) -0.037(4) 0.004(6) -0.008(5) F15B 0.097(4) 0.089(4) 0.045(5) -0.034(3) 0.038(3) -0.018(3) F16 0.066(3) 0.033(3) 0.059(2) 0.0172(19) 0.034(2) 0.008(2) F17 0.080(6) 0.076(4) 0.044(2) -0.006(3) 0.017(4) -0.050(3) F18 0.038(3) 0.042(4) 0.061(8) 0.005(5) 0.021(3) 0.000(4) F16B 0.094(8) 0.033(3) 0.160(11) 0.020(7) 0.094(8) 0.009(4) F17B 0.060(4) 0.103(6) 0.050(2) -0.005(4) 0.013(3) -0.048(4) F18B 0.045(5) 0.051(5) 0.043(4) -0.003(3) 0.032(5) -0.010(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 Sm1 O3 2.3862(13) . ? Sm1 O1 2.4007(12) . ? Sm1 O6 2.4056(12) . ? Sm1 O4 2.4186(12) . ? Sm1 O2 2.4366(13) . ? Sm1 O5 2.4368(13) . ? Sm1 O9 2.5453(12) . ? Sm1 O8 2.5554(13) . ? Sm1 O7 2.5794(12) . ? O1 C2 1.245(2) . ? O2 C4 1.251(2) . ? O3 C7 1.246(2) . ? O4 C9 1.246(2) . ? O5 C12 1.250(2) . ? O6 C14 1.248(2) . ? O7 C16 1.433(2) . ? O7 C17 1.435(2) . ? O8 C18 1.441(2) . ? O8 C19 1.444(2) . ? O9 C20 1.434(2) . ? O9 C21 1.446(2) . ? C1 F3 1.304(15) . ? C1 F2B 1.310(9) . ? C1 F1B 1.311(13) . ? C1 F3B 1.313(14) . ? C1 F2 1.317(9) . ? C1 F1 1.332(14) . ? C1 C2 1.540(3) . ? C2 C3 1.392(3) . ? C3 C4 1.392(3) . ? C4 C5 1.534(3) . ? C5 F5B 1.278(11) . ? C5 F4 1.281(14) . ? C5 F6 1.304(15) . ? C5 F6B 1.333(17) . ? C5 F4B 1.361(15) . ? C5 F5 1.361(12) . ? C6 F9B 1.230(12) . ? C6 F7 1.248(8) . ? C6 F8 1.287(12) . ? C6 F8B 1.327(11) . ? C6 F9 1.407(13) . ? C6 F7B 1.411(8) . ? C6 C7 1.539(3) . ? C7 C8 1.391(3) . ? C8 C9 1.393(3) . ? C9 C10 1.533(3) . ? C10 F12 1.244(5) . ? C10 F11B 1.248(5) . ? C10 F10 1.291(12) . ? C10 F10B 1.294(11) . ? C10 F12B 1.413(5) . ? C10 F11 1.428(6) . ? C11 F14B 1.208(13) . ? C11 F13B 1.288(13) . ? C11 F15 1.301(12) . ? C11 F13 1.314(12) . ? C11 F15B 1.322(12) . ? C11 F14 1.424(11) . ? C11 C12 1.535(3) . ? C12 C13 1.388(3) . ? C13 C14 1.388(3) . ? C14 C15 1.537(3) . ? C15 F16B 1.247(15) . ? C15 F18 1.280(17) . ? C15 F17 1.290(11) . ? C15 F18B 1.365(17) . ? C15 F17B 1.375(11) . ? C15 F16 1.402(14) . ? C17 C18 1.503(3) . ? C19 C20 1.499(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Sm1 O1 84.63(4) . . ? O3 Sm1 O6 139.38(4) . . ? O1 Sm1 O6 135.99(4) . . ? O3 Sm1 O4 72.51(4) . . ? O1 Sm1 O4 140.20(4) . . ? O6 Sm1 O4 72.84(4) . . ? O3 Sm1 O2 72.12(5) . . ? O1 Sm1 O2 70.49(4) . . ? O6 Sm1 O2 115.37(4) . . ? O4 Sm1 O2 71.64(4) . . ? O3 Sm1 O5 78.61(5) . . ? O1 Sm1 O5 136.25(4) . . ? O6 Sm1 O5 70.64(4) . . ? O4 Sm1 O5 71.14(5) . . ? O2 Sm1 O5 137.93(5) . . ? O3 Sm1 O9 71.51(4) . . ? O1 Sm1 O9 69.68(4) . . ? O6 Sm1 O9 116.91(4) . . ? O4 Sm1 O9 128.58(4) . . ? O2 Sm1 O9 127.55(4) . . ? O5 Sm1 O9 66.72(4) . . ? O3 Sm1 O8 135.67(4) . . ? O1 Sm1 O8 71.45(4) . . ? O6 Sm1 O8 73.23(4) . . ? O4 Sm1 O8 145.76(4) . . ? O2 Sm1 O8 128.72(4) . . ? O5 Sm1 O8 93.31(4) . . ? O9 Sm1 O8 65.40(4) . . ? O3 Sm1 O7 142.22(4) . . ? O1 Sm1 O7 72.38(4) . . ? O6 Sm1 O7 69.15(4) . . ? O4 Sm1 O7 106.86(4) . . ? O2 Sm1 O7 72.10(4) . . ? O5 Sm1 O7 138.17(4) . . ? O9 Sm1 O7 124.08(4) . . ? O8 Sm1 O7 64.45(4) . . ? C2 O1 Sm1 136.32(12) . . ? C4 O2 Sm1 133.94(12) . . ? C7 O3 Sm1 134.64(12) . . ? C9 O4 Sm1 133.30(12) . . ? C12 O5 Sm1 134.36(12) . . ? C14 O6 Sm1 135.65(12) . . ? C16 O7 C17 110.47(15) . . ? C16 O7 Sm1 124.64(12) . . ? C17 O7 Sm1 114.93(10) . . ? C18 O8 C19 111.24(14) . . ? C18 O8 Sm1 116.97(11) . . ? C19 O8 Sm1 117.26(10) . . ? C20 O9 C21 112.56(15) . . ? C20 O9 Sm1 110.44(10) . . ? C21 O9 Sm1 124.41(11) . . ? F3 C1 F2B 98.2(10) . . ? F3 C1 F1B 114.9(10) . . ? F2B C1 F1B 104.6(10) . . ? F3 C1 F3B 9.2(16) . . ? F2B C1 F3B 106.5(10) . . ? F1B C1 F3B 108.1(9) . . ? F3 C1 F2 107.9(10) . . ? F2B C1 F2 10.2(9) . . ? F1B C1 F2 96.9(10) . . ? F3B C1 F2 115.8(9) . . ? F3 C1 F1 107.8(10) . . ? F2B C1 F1 114.1(10) . . ? F1B C1 F1 10.5(14) . . ? F3B C1 F1 100.2(9) . . ? F2 C1 F1 106.9(10) . . ? F3 C1 C2 114.6(7) . . ? F2B C1 C2 112.0(5) . . ? F1B C1 C2 111.3(7) . . ? F3B C1 C2 113.8(7) . . ? F2 C1 C2 109.6(5) . . ? F1 C1 C2 109.8(8) . . ? O1 C2 C3 128.25(17) . . ? O1 C2 C1 113.56(16) . . ? C3 C2 C1 118.17(16) . . ? C4 C3 C2 120.38(17) . . ? O2 C4 C3 128.54(17) . . ? O2 C4 C5 113.78(16) . . ? C3 C4 C5 117.68(16) . . ? F5B C5 F4 85.3(8) . . ? F5B C5 F6 117.3(10) . . ? F4 C5 F6 109.7(9) . . ? F5B C5 F6B 106.7(10) . . ? F4 C5 F6B 117.8(9) . . ? F6 C5 F6B 12.8(16) . . ? F5B C5 F4B 107.0(8) . . ? F4 C5 F4B 22.5(10) . . ? F6 C5 F4B 94.0(10) . . ? F6B C5 F4B 104.8(10) . . ? F5B C5 F5 20.8(10) . . ? F4 C5 F5 106.0(8) . . ? F6 C5 F5 107.3(10) . . ? F6B C5 F5 95.0(10) . . ? F4B C5 F5 127.4(7) . . ? F5B C5 C4 114.9(5) . . ? F4 C5 C4 113.0(7) . . ? F6 C5 C4 113.4(8) . . ? F6B C5 C4 115.3(8) . . ? F4B C5 C4 107.3(7) . . ? F5 C5 C4 107.0(5) . . ? F9B C6 F7 73.6(7) . . ? F9B C6 F8 121.3(9) . . ? F7 C6 F8 112.6(8) . . ? F9B C6 F8B 111.2(9) . . ? F7 C6 F8B 117.3(7) . . ? F8 C6 F8B 11.7(14) . . ? F9B C6 F9 29.9(7) . . ? F7 C6 F9 103.1(6) . . ? F8 C6 F9 104.7(9) . . ? F8B C6 F9 93.0(9) . . ? F9B C6 F7B 106.7(6) . . ? F7 C6 F7B 33.3(6) . . ? F8 C6 F7B 92.5(8) . . ? F8B C6 F7B 101.9(8) . . ? F9 C6 F7B 135.5(5) . . ? F9B C6 C7 115.2(6) . . ? F7 C6 C7 116.3(4) . . ? F8 C6 C7 112.5(6) . . ? F8B C6 C7 116.1(5) . . ? F9 C6 C7 106.3(5) . . ? F7B C6 C7 104.2(4) . . ? O3 C7 C8 128.68(18) . . ? O3 C7 C6 113.53(17) . . ? C8 C7 C6 117.79(18) . . ? C7 C8 C9 121.52(18) . . ? O4 C9 C8 128.55(18) . . ? O4 C9 C10 113.94(16) . . ? C8 C9 C10 117.51(17) . . ? F12 C10 F11B 67.1(4) . . ? F12 C10 F10 114.2(8) . . ? F11B C10 F10 119.7(7) . . ? F12 C10 F10B 122.2(8) . . ? F11B C10 F10B 112.4(7) . . ? F10 C10 F10B 12.3(12) . . ? F12 C10 F12B 39.2(3) . . ? F11B C10 F12B 105.3(4) . . ? F10 C10 F12B 88.6(7) . . ? F10B C10 F12B 100.4(7) . . ? F12 C10 F11 103.1(4) . . ? F11B C10 F11 36.4(3) . . ? F10 C10 F11 100.7(7) . . ? F10B C10 F11 89.4(7) . . ? F12B C10 F11 139.5(3) . . ? F12 C10 C9 115.4(3) . . ? F11B C10 C9 115.6(3) . . ? F10 C10 C9 115.8(7) . . ? F10B C10 C9 115.1(7) . . ? F12B C10 C9 106.0(3) . . ? F11 C10 C9 105.0(3) . . ? F14B C11 F13B 112.1(8) . . ? F14B C11 F15 113.2(9) . . ? F13B C11 F15 95.9(9) . . ? F14B C11 F13 96.3(8) . . ? F13B C11 F13 16.6(8) . . ? F15 C11 F13 107.7(9) . . ? F14B C11 F15B 101.1(9) . . ? F13B C11 F15B 109.7(9) . . ? F15 C11 F15B 15.2(13) . . ? F13 C11 F15B 119.7(9) . . ? F14B C11 F14 3.6(9) . . ? F13B C11 F14 115.6(7) . . ? F15 C11 F14 111.2(8) . . ? F13 C11 F14 99.9(5) . . ? F15B C11 F14 98.7(7) . . ? F14B C11 C12 111.3(7) . . ? F13B C11 C12 109.3(6) . . ? F15 C11 C12 114.1(6) . . ? F13 C11 C12 112.9(5) . . ? F15B C11 C12 113.2(7) . . ? F14 C11 C12 110.1(5) . . ? O5 C12 C13 128.19(18) . . ? O5 C12 C11 113.88(18) . . ? C13 C12 C11 117.92(18) . . ? C14 C13 C12 120.70(18) . . ? O6 C14 C13 128.78(18) . . ? O6 C14 C15 114.22(17) . . ? C13 C14 C15 116.96(17) . . ? F16B C15 F18 111.3(10) . . ? F16B C15 F17 84.4(7) . . ? F18 C15 F17 111.2(14) . . ? F16B C15 F18B 111.1(10) . . ? F18 C15 F18B 10(2) . . ? F17 C15 F18B 121.4(13) . . ? F16B C15 F17B 110.5(7) . . ? F18 C15 F17B 93.2(13) . . ? F17 C15 F17B 27.4(4) . . ? F18B C15 F17B 102.5(12) . . ? F16B C15 F16 17.7(10) . . ? F18 C15 F16 103.5(10) . . ? F17 C15 F16 102.1(7) . . ? F18B C15 F16 100.6(10) . . ? F17B C15 F16 127.9(6) . . ? F16B C15 C14 113.6(7) . . ? F18 C15 C14 117.6(11) . . ? F17 C15 C14 114.2(5) . . ? F18B C15 C14 109.8(10) . . ? F17B C15 C14 108.6(5) . . ? F16 C15 C14 106.3(7) . . ? O7 C17 C18 107.87(15) . . ? O8 C18 C17 108.26(15) . . ? O8 C19 C20 106.54(15) . . ? O9 C20 C19 109.55(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Sm1 O1 C2 62.57(17) . . . . ? O6 Sm1 O1 C2 -117.04(17) . . . . ? O4 Sm1 O1 C2 8.3(2) . . . . ? O2 Sm1 O1 C2 -10.34(17) . . . . ? O5 Sm1 O1 C2 129.92(17) . . . . ? O9 Sm1 O1 C2 134.82(18) . . . . ? O8 Sm1 O1 C2 -155.30(18) . . . . ? O7 Sm1 O1 C2 -87.06(17) . . . . ? O3 Sm1 O2 C4 -74.75(16) . . . . ? O1 Sm1 O2 C4 15.82(16) . . . . ? O6 Sm1 O2 C4 148.38(16) . . . . ? O4 Sm1 O2 C4 -151.71(17) . . . . ? O5 Sm1 O2 C4 -122.89(16) . . . . ? O9 Sm1 O2 C4 -26.70(18) . . . . ? O8 Sm1 O2 C4 60.05(18) . . . . ? O7 Sm1 O2 C4 92.93(17) . . . . ? O1 Sm1 O3 C7 -147.81(18) . . . . ? O6 Sm1 O3 C7 31.8(2) . . . . ? O4 Sm1 O3 C7 -0.80(17) . . . . ? O2 Sm1 O3 C7 -76.60(18) . . . . ? O5 Sm1 O3 C7 72.80(18) . . . . ? O9 Sm1 O3 C7 141.84(19) . . . . ? O8 Sm1 O3 C7 155.79(16) . . . . ? O7 Sm1 O3 C7 -95.95(18) . . . . ? O3 Sm1 O4 C9 8.48(16) . . . . ? O1 Sm1 O4 C9 66.37(18) . . . . ? O6 Sm1 O4 C9 -149.99(17) . . . . ? O2 Sm1 O4 C9 84.91(16) . . . . ? O5 Sm1 O4 C9 -75.13(16) . . . . ? O9 Sm1 O4 C9 -38.91(18) . . . . ? O8 Sm1 O4 C9 -141.96(15) . . . . ? O7 Sm1 O4 C9 148.87(16) . . . . ? O3 Sm1 O5 C12 -138.69(19) . . . . ? O1 Sm1 O5 C12 151.72(17) . . . . ? O6 Sm1 O5 C12 14.38(18) . . . . ? O4 Sm1 O5 C12 -63.47(18) . . . . ? O2 Sm1 O5 C12 -92.39(19) . . . . ? O9 Sm1 O5 C12 146.71(19) . . . . ? O8 Sm1 O5 C12 85.32(18) . . . . ? O7 Sm1 O5 C12 31.0(2) . . . . ? O3 Sm1 O6 C14 34.3(2) . . . . ? O1 Sm1 O6 C14 -146.30(16) . . . . ? O4 Sm1 O6 C14 66.80(17) . . . . ? O2 Sm1 O6 C14 126.06(17) . . . . ? O5 Sm1 O6 C14 -8.71(17) . . . . ? O9 Sm1 O6 C14 -58.31(18) . . . . ? O8 Sm1 O6 C14 -108.49(17) . . . . ? O7 Sm1 O6 C14 -176.94(18) . . . . ? O3 Sm1 O7 C16 65.65(17) . . . . ? O1 Sm1 O7 C16 120.89(15) . . . . ? O6 Sm1 O7 C16 -80.92(15) . . . . ? O4 Sm1 O7 C16 -17.36(15) . . . . ? O2 Sm1 O7 C16 46.30(14) . . . . ? O5 Sm1 O7 C16 -97.69(15) . . . . ? O9 Sm1 O7 C16 169.99(14) . . . . ? O8 Sm1 O7 C16 -161.70(16) . . . . ? O3 Sm1 O7 C17 -152.18(11) . . . . ? O1 Sm1 O7 C17 -96.94(12) . . . . ? O6 Sm1 O7 C17 61.25(11) . . . . ? O4 Sm1 O7 C17 124.81(11) . . . . ? O2 Sm1 O7 C17 -171.53(12) . . . . ? O5 Sm1 O7 C17 44.48(14) . . . . ? O9 Sm1 O7 C17 -47.84(13) . . . . ? O8 Sm1 O7 C17 -19.53(11) . . . . ? O3 Sm1 O8 C18 126.67(12) . . . . ? O1 Sm1 O8 C18 65.67(12) . . . . ? O6 Sm1 O8 C18 -87.63(12) . . . . ? O4 Sm1 O8 C18 -95.65(14) . . . . ? O2 Sm1 O8 C18 21.76(14) . . . . ? O5 Sm1 O8 C18 -156.27(12) . . . . ? O9 Sm1 O8 C18 141.23(13) . . . . ? O7 Sm1 O8 C18 -13.18(12) . . . . ? O3 Sm1 O8 C19 -9.34(14) . . . . ? O1 Sm1 O8 C19 -70.35(12) . . . . ? O6 Sm1 O8 C19 136.35(12) . . . . ? O4 Sm1 O8 C19 128.33(12) . . . . ? O2 Sm1 O8 C19 -114.26(12) . . . . ? O5 Sm1 O8 C19 67.71(12) . . . . ? O9 Sm1 O8 C19 5.22(11) . . . . ? O7 Sm1 O8 C19 -149.19(13) . . . . ? O3 Sm1 O9 C20 -163.82(12) . . . . ? O1 Sm1 O9 C20 105.12(12) . . . . ? O6 Sm1 O9 C20 -27.11(12) . . . . ? O4 Sm1 O9 C20 -116.06(11) . . . . ? O2 Sm1 O9 C20 147.91(11) . . . . ? O5 Sm1 O9 C20 -78.57(11) . . . . ? O8 Sm1 O9 C20 26.86(11) . . . . ? O7 Sm1 O9 C20 54.93(12) . . . . ? O3 Sm1 O9 C21 57.46(15) . . . . ? O1 Sm1 O9 C21 -33.61(14) . . . . ? O6 Sm1 O9 C21 -165.83(14) . . . . ? O4 Sm1 O9 C21 105.21(15) . . . . ? O2 Sm1 O9 C21 9.18(17) . . . . ? O5 Sm1 O9 C21 142.71(16) . . . . ? O8 Sm1 O9 C21 -111.86(15) . . . . ? O7 Sm1 O9 C21 -83.79(15) . . . . ? Sm1 O1 C2 C3 4.2(3) . . . . ? Sm1 O1 C2 C1 -174.18(13) . . . . ? F3 C1 C2 O1 -161.2(9) . . . . ? F2B C1 C2 O1 88.0(6) . . . . ? F1B C1 C2 O1 -28.6(8) . . . . ? F3B C1 C2 O1 -151.1(8) . . . . ? F2 C1 C2 O1 77.4(6) . . . . ? F1 C1 C2 O1 -39.7(8) . . . . ? F3 C1 C2 C3 20.3(9) . . . . ? F2B C1 C2 C3 -90.5(6) . . . . ? F1B C1 C2 C3 152.8(8) . . . . ? F3B C1 C2 C3 30.3(9) . . . . ? F2 C1 C2 C3 -101.2(6) . . . . ? F1 C1 C2 C3 141.7(8) . . . . ? O1 C2 C3 C4 4.4(3) . . . . ? C1 C2 C3 C4 -177.31(18) . . . . ? Sm1 O2 C4 C3 -16.0(3) . . . . ? Sm1 O2 C4 C5 164.27(13) . . . . ? C2 C3 C4 O2 1.8(3) . . . . ? C2 C3 C4 C5 -178.51(18) . . . . ? O2 C4 C5 F5B 51.8(6) . . . . ? C3 C4 C5 F5B -127.9(6) . . . . ? O2 C4 C5 F4 -43.8(6) . . . . ? C3 C4 C5 F4 136.4(6) . . . . ? O2 C4 C5 F6 -169.4(9) . . . . ? C3 C4 C5 F6 10.9(9) . . . . ? O2 C4 C5 F6B 176.7(9) . . . . ? C3 C4 C5 F6B -3.1(9) . . . . ? O2 C4 C5 F4B -67.1(6) . . . . ? C3 C4 C5 F4B 113.2(6) . . . . ? O2 C4 C5 F5 72.5(6) . . . . ? C3 C4 C5 F5 -107.3(6) . . . . ? Sm1 O3 C7 C8 -4.5(3) . . . . ? Sm1 O3 C7 C6 176.19(15) . . . . ? F9B C6 C7 O3 62.0(6) . . . . ? F7 C6 C7 O3 -21.3(7) . . . . ? F8 C6 C7 O3 -153.3(8) . . . . ? F8B C6 C7 O3 -165.6(8) . . . . ? F9 C6 C7 O3 92.7(5) . . . . ? F7B C6 C7 O3 -54.5(5) . . . . ? F9B C6 C7 C8 -117.4(6) . . . . ? F7 C6 C7 C8 159.3(6) . . . . ? F8 C6 C7 C8 27.3(8) . . . . ? F8B C6 C7 C8 15.0(8) . . . . ? F9 C6 C7 C8 -86.7(5) . . . . ? F7B C6 C7 C8 126.1(5) . . . . ? O3 C7 C8 C9 4.5(3) . . . . ? C6 C7 C8 C9 -176.2(2) . . . . ? Sm1 O4 C9 C8 -11.7(3) . . . . ? Sm1 O4 C9 C10 169.25(13) . . . . ? C7 C8 C9 O4 3.8(3) . . . . ? C7 C8 C9 C10 -177.13(19) . . . . ? O4 C9 C10 F12 -24.5(5) . . . . ? C8 C9 C10 F12 156.3(4) . . . . ? O4 C9 C10 F11B 50.9(5) . . . . ? C8 C9 C10 F11B -128.2(5) . . . . ? O4 C9 C10 F10 -161.8(7) . . . . ? C8 C9 C10 F10 19.1(7) . . . . ? O4 C9 C10 F10B -175.4(7) . . . . ? C8 C9 C10 F10B 5.5(7) . . . . ? O4 C9 C10 F12B -65.4(3) . . . . ? C8 C9 C10 F12B 115.4(3) . . . . ? O4 C9 C10 F11 88.2(3) . . . . ? C8 C9 C10 F11 -91.0(3) . . . . ? Sm1 O5 C12 C13 -15.6(3) . . . . ? Sm1 O5 C12 C11 163.99(15) . . . . ? F14B C11 C12 O5 60.2(7) . . . . ? F13B C11 C12 O5 -64.2(6) . . . . ? F15 C11 C12 O5 -170.2(8) . . . . ? F13 C11 C12 O5 -46.8(5) . . . . ? F15B C11 C12 O5 173.2(7) . . . . ? F14 C11 C12 O5 63.8(4) . . . . ? F14B C11 C12 C13 -120.2(7) . . . . ? F13B C11 C12 C13 115.4(6) . . . . ? F15 C11 C12 C13 9.4(8) . . . . ? F13 C11 C12 C13 132.8(5) . . . . ? F15B C11 C12 C13 -7.2(8) . . . . ? F14 C11 C12 C13 -116.5(4) . . . . ? O5 C12 C13 C14 3.4(4) . . . . ? C11 C12 C13 C14 -176.2(2) . . . . ? Sm1 O6 C14 C13 3.7(3) . . . . ? Sm1 O6 C14 C15 -173.84(13) . . . . ? C12 C13 C14 O6 2.8(3) . . . . ? C12 C13 C14 C15 -179.8(2) . . . . ? O6 C14 C15 F16B 75.2(6) . . . . ? C13 C14 C15 F16B -102.6(6) . . . . ? O6 C14 C15 F18 -152.3(12) . . . . ? C13 C14 C15 F18 29.9(12) . . . . ? O6 C14 C15 F17 -19.4(4) . . . . ? C13 C14 C15 F17 162.8(4) . . . . ? O6 C14 C15 F18B -159.7(10) . . . . ? C13 C14 C15 F18B 22.5(11) . . . . ? O6 C14 C15 F17B -48.3(4) . . . . ? C13 C14 C15 F17B 133.9(4) . . . . ? O6 C14 C15 F16 92.4(6) . . . . ? C13 C14 C15 F16 -85.5(6) . . . . ? C16 O7 C17 C18 -164.55(16) . . . . ? Sm1 O7 C17 C18 48.04(17) . . . . ? C19 O8 C18 C17 -179.30(15) . . . . ? Sm1 O8 C18 C17 42.17(19) . . . . ? O7 C17 C18 O8 -58.1(2) . . . . ? C18 O8 C19 C20 -172.76(16) . . . . ? Sm1 O8 C19 C20 -34.37(18) . . . . ? C21 O9 C20 C19 86.85(19) . . . . ? Sm1 O9 C20 C19 -57.04(16) . . . . ? O8 C19 C20 O9 60.21(19) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.519 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.062 #===end data_dg19 _database_code_CSD 171877 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 F38 K2 O18 Sm2' _chemical_formula_weight 1927.59 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0241(6) _cell_length_b 12.4246(6) _cell_length_c 13.5664(7) _cell_angle_alpha 92.2920(10) _cell_angle_beta 114.6330(10) _cell_angle_gamma 113.6860(10) _cell_volume 1633.89(14) _cell_formula_units_Z 1 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description multi-faceted-polyhedra _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 934 _exptl_absorpt_coefficient_mu 2.078 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6247 _exptl_absorpt_correction_T_max 0.7322 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% '< 1.0' _diffrn_reflns_number 17419 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.28 _reflns_number_total 7666 _reflns_number_gt 7216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0299P)^2^+1.5301P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7666 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm1 Sm -0.160670(11) -0.140414(10) -0.093501(9) 0.01973(4) Uani 1 1 d . . . K1 K -0.03938(5) 0.17516(5) -0.21720(4) 0.02500(10) Uani 1 1 d . . . F1 F -0.06026(16) 0.06890(13) -0.04800(12) 0.0312(3) Uani 1 1 d . . . O1 O -0.36803(18) -0.12266(18) -0.13695(14) 0.0303(4) Uani 1 1 d . . . O2 O -0.17142(17) -0.09335(16) 0.08330(14) 0.0265(3) Uani 1 1 d . . . O3 O -0.08028(19) -0.26076(16) -0.16472(14) 0.0281(4) Uani 1 1 d . . . O4 O -0.16616(18) -0.09390(15) -0.26749(13) 0.0242(3) Uani 1 1 d . . . O5 O -0.19982(19) -0.30926(16) -0.00527(15) 0.0303(4) Uani 1 1 d . . . O6 O -0.36114(19) -0.32364(17) -0.23211(15) 0.0357(4) Uani 1 1 d . . . O7 O -0.2036(2) 0.22193(19) -0.14415(18) 0.0393(4) Uani 1 1 d . . . O8 O -0.3059(2) 0.11998(17) -0.37131(16) 0.0344(4) Uani 1 1 d . . . O9 O -0.0864(2) 0.2915(2) -0.39197(17) 0.0393(5) Uani 1 1 d . . . C1 C -0.5903(3) -0.1652(3) -0.1689(2) 0.0335(6) Uani 1 1 d . . . C2 C -0.4408(2) -0.1369(2) -0.0894(2) 0.0247(5) Uani 1 1 d . . . C3 C -0.4034(3) -0.1324(2) 0.0227(2) 0.0281(5) Uani 1 1 d . . . H3 H -0.4698 -0.1452 0.0475 0.034 Uiso 1 1 calc R . . C4 C -0.2700(2) -0.1094(2) 0.10027(19) 0.0240(5) Uani 1 1 d . . . C5 C -0.2384(3) -0.1038(3) 0.2228(2) 0.0326(6) Uani 1 1 d . . . C6 C -0.0764(3) -0.4070(2) -0.2773(2) 0.0312(5) Uani 1 1 d . . . C7 C -0.1048(2) -0.2988(2) -0.26158(19) 0.0235(4) Uani 1 1 d . . . C8 C -0.1497(3) -0.2533(2) -0.35492(19) 0.0253(5) Uani 1 1 d . . . H8 H -0.1664 -0.2928 -0.4247 0.030 Uiso 1 1 calc R . . C9 C -0.1703(2) -0.1520(2) -0.34833(18) 0.0223(4) Uani 1 1 d . . . C10 C -0.2032(3) -0.1012(2) -0.4530(2) 0.0290(5) Uani 1 1 d . . . C11 C -0.2738(3) -0.4793(3) 0.0614(3) 0.0399(7) Uani 1 1 d . . . C12 C -0.2895(3) -0.4175(2) -0.0357(2) 0.0273(5) Uani 1 1 d . . . C13 C -0.3983(3) -0.4836(2) -0.1414(2) 0.0361(6) Uani 1 1 d . . . H13 H -0.4567 -0.5670 -0.1527 0.043 Uiso 1 1 calc R . . C14 C -0.4239(3) -0.4299(2) -0.2318(2) 0.0315(5) Uani 1 1 d . A . C15 C -0.5441(4) -0.5128(3) -0.3458(3) 0.0554(9) Uani 1 1 d . . . C16 C -0.1505(4) 0.3183(3) -0.0512(3) 0.0517(8) Uani 1 1 d . . . H16A H -0.0531 0.3420 -0.0018 0.078 Uiso 1 1 calc R . . H16B H -0.2025 0.2914 -0.0097 0.078 Uiso 1 1 calc R . . H16C H -0.1593 0.3880 -0.0780 0.078 Uiso 1 1 calc R . . C17 C -0.3445(3) 0.1824(3) -0.2195(3) 0.0441(7) Uani 1 1 d . . . H17A H -0.3577 0.2513 -0.2469 0.053 Uiso 1 1 calc R . . H17B H -0.4006 0.1510 -0.1810 0.053 Uiso 1 1 calc R . . C18 C -0.3892(3) 0.0847(3) -0.3158(3) 0.0429(7) Uani 1 1 d . . . H18A H -0.3861 0.0128 -0.2883 0.051 Uiso 1 1 calc R . . H18B H -0.4860 0.0606 -0.3708 0.051 Uiso 1 1 calc R . . C19 C -0.3189(3) 0.2101(3) -0.4307(3) 0.0400(6) Uani 1 1 d . . . H19A H -0.2951 0.2837 -0.3791 0.048 Uiso 1 1 calc R . . H19B H -0.4151 0.1791 -0.4906 0.048 Uiso 1 1 calc R . . C20 C -0.2246(3) 0.2401(3) -0.4801(2) 0.0410(7) Uani 1 1 d . . . H20A H -0.2459 0.1658 -0.5292 0.049 Uiso 1 1 calc R . . H20B H -0.2363 0.2986 -0.5259 0.049 Uiso 1 1 calc R . . C21 C 0.0107(5) 0.3324(5) -0.4325(4) 0.0739(13) Uani 1 1 d . . . H21A H 0.1042 0.3671 -0.3694 0.111 Uiso 1 1 calc R . . H21B H -0.0001 0.3945 -0.4724 0.111 Uiso 1 1 calc R . . H21C H -0.0046 0.2639 -0.4837 0.111 Uiso 1 1 calc R . . F2 F -0.65738(18) -0.27391(19) -0.23873(16) 0.0551(5) Uani 1 1 d . . . F3 F -0.59455(19) -0.0848(2) -0.23019(18) 0.0589(6) Uani 1 1 d . . . F4 F -0.66207(17) -0.16470(19) -0.11604(15) 0.0477(4) Uani 1 1 d . . . F5 F -0.34896(19) -0.1457(2) 0.23760(14) 0.0520(5) Uani 1 1 d . . . F6 F -0.1724(2) -0.1688(2) 0.26509(14) 0.0489(5) Uani 1 1 d . . . F7 F -0.1567(2) 0.00948(19) 0.28516(15) 0.0557(5) Uani 1 1 d . . . F8 F -0.1340(2) -0.46435(17) -0.38318(14) 0.0541(5) Uani 1 1 d . . . F9 F -0.1195(3) -0.48657(17) -0.22415(19) 0.0633(6) Uani 1 1 d . . . F10 F 0.0577(2) -0.3699(2) -0.2347(2) 0.0699(7) Uani 1 1 d . . . F11 F -0.1320(2) 0.01995(14) -0.42469(13) 0.0406(4) Uani 1 1 d . . . F12 F -0.1709(2) -0.14123(17) -0.52444(14) 0.0470(5) Uani 1 1 d . . . F13 F -0.33516(19) -0.12997(19) -0.50706(15) 0.0518(5) Uani 1 1 d . . . F14 F -0.3041(3) -0.4328(2) 0.1301(2) 0.0751(7) Uani 1 1 d . . . F15 F -0.3512(3) -0.59824(18) 0.0301(2) 0.0734(7) Uani 1 1 d . . . F16 F -0.1451(2) -0.4598(2) 0.12062(19) 0.0654(6) Uani 1 1 d . . . F17 F -0.6536(10) -0.5847(10) -0.3424(9) 0.122(5) Uani 0.60 1 d P A 1 F18 F -0.5765(8) -0.4551(8) -0.4220(5) 0.080(2) Uani 0.60 1 d P A 1 F19 F -0.5049(12) -0.5812(9) -0.3893(9) 0.107(4) Uani 0.60 1 d P A 1 F17B F -0.6289(15) -0.6134(9) -0.3374(14) 0.087(5) Uani 0.40 1 d P A 2 F18B F -0.6261(15) -0.4612(12) -0.3863(13) 0.152(7) Uani 0.40 1 d P A 2 F19B F -0.5092(16) -0.544(2) -0.4075(13) 0.165(11) Uani 0.40 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02095(7) 0.02005(6) 0.01376(6) 0.00438(4) 0.00707(5) 0.00668(5) K1 0.0270(2) 0.0289(2) 0.0193(2) 0.00907(19) 0.0095(2) 0.0144(2) F1 0.0333(8) 0.0303(8) 0.0268(7) 0.0084(6) 0.0124(6) 0.0136(6) O1 0.0245(9) 0.0454(11) 0.0202(8) 0.0117(7) 0.0103(7) 0.0154(8) O2 0.0249(8) 0.0375(9) 0.0181(8) 0.0069(7) 0.0108(7) 0.0145(7) O3 0.0371(10) 0.0304(9) 0.0176(8) 0.0071(7) 0.0100(7) 0.0193(8) O4 0.0315(9) 0.0260(8) 0.0173(8) 0.0063(6) 0.0116(7) 0.0150(7) O5 0.0328(9) 0.0242(8) 0.0250(9) 0.0080(7) 0.0121(8) 0.0067(7) O6 0.0287(9) 0.0313(10) 0.0251(9) 0.0013(7) 0.0032(8) 0.0048(8) O7 0.0397(11) 0.0462(12) 0.0428(11) 0.0120(9) 0.0226(10) 0.0262(10) O8 0.0326(10) 0.0317(9) 0.0355(10) 0.0115(8) 0.0113(8) 0.0165(8) O9 0.0434(11) 0.0493(12) 0.0363(11) 0.0245(9) 0.0237(9) 0.0248(10) C1 0.0241(12) 0.0434(15) 0.0274(13) 0.0125(11) 0.0094(10) 0.0133(11) C2 0.0218(11) 0.0256(11) 0.0222(11) 0.0074(9) 0.0076(9) 0.0098(9) C3 0.0257(12) 0.0357(13) 0.0240(12) 0.0089(10) 0.0132(10) 0.0136(10) C4 0.0279(12) 0.0272(11) 0.0196(11) 0.0076(9) 0.0125(9) 0.0136(10) C5 0.0324(14) 0.0522(16) 0.0215(12) 0.0102(11) 0.0150(11) 0.0246(12) C6 0.0424(15) 0.0303(13) 0.0254(12) 0.0088(10) 0.0152(11) 0.0214(12) C7 0.0252(11) 0.0215(11) 0.0217(11) 0.0042(8) 0.0099(9) 0.0102(9) C8 0.0308(12) 0.0265(11) 0.0164(10) 0.0037(9) 0.0093(9) 0.0135(10) C9 0.0229(11) 0.0249(11) 0.0154(10) 0.0045(8) 0.0075(9) 0.0093(9) C10 0.0409(14) 0.0317(13) 0.0177(11) 0.0080(9) 0.0123(10) 0.0212(11) C11 0.0501(18) 0.0290(13) 0.0427(16) 0.0162(12) 0.0269(14) 0.0142(13) C12 0.0306(12) 0.0231(11) 0.0325(13) 0.0083(9) 0.0202(11) 0.0106(10) C13 0.0330(14) 0.0228(12) 0.0408(15) 0.0025(11) 0.0178(12) 0.0027(10) C14 0.0210(11) 0.0296(13) 0.0273(13) -0.0040(10) 0.0069(10) 0.0026(10) C15 0.0416(18) 0.0477(19) 0.0357(17) -0.0058(14) 0.0088(15) -0.0047(15) C16 0.072(2) 0.064(2) 0.0376(17) 0.0165(15) 0.0299(17) 0.044(2) C17 0.0375(16) 0.0541(18) 0.060(2) 0.0257(16) 0.0303(15) 0.0291(14) C18 0.0275(14) 0.0426(16) 0.0532(19) 0.0188(14) 0.0164(13) 0.0136(12) C19 0.0392(16) 0.0396(15) 0.0369(15) 0.0142(12) 0.0094(13) 0.0229(13) C20 0.0553(18) 0.0434(16) 0.0244(13) 0.0143(12) 0.0126(13) 0.0288(14) C21 0.082(3) 0.102(3) 0.088(3) 0.066(3) 0.067(3) 0.055(3) F2 0.0309(9) 0.0604(12) 0.0398(10) -0.0085(9) 0.0011(8) 0.0088(8) F3 0.0357(10) 0.0816(15) 0.0631(13) 0.0495(12) 0.0193(9) 0.0317(10) F4 0.0264(8) 0.0759(13) 0.0414(10) 0.0161(9) 0.0156(8) 0.0243(9) F5 0.0401(10) 0.0992(16) 0.0320(9) 0.0273(10) 0.0253(8) 0.0363(10) F6 0.0632(12) 0.0871(14) 0.0320(9) 0.0319(9) 0.0298(9) 0.0572(12) F7 0.0643(13) 0.0589(12) 0.0262(9) -0.0063(8) 0.0155(9) 0.0204(10) F8 0.0933(16) 0.0486(11) 0.0301(9) 0.0063(8) 0.0211(10) 0.0501(11) F9 0.1190(19) 0.0398(10) 0.0702(14) 0.0316(10) 0.0670(14) 0.0466(12) F10 0.0455(12) 0.0580(13) 0.1004(18) 0.0059(12) 0.0201(12) 0.0352(10) F11 0.0673(12) 0.0307(8) 0.0280(8) 0.0145(6) 0.0242(8) 0.0238(8) F12 0.0906(15) 0.0550(11) 0.0271(8) 0.0217(8) 0.0372(9) 0.0508(11) F13 0.0411(10) 0.0685(13) 0.0357(9) 0.0228(9) 0.0050(8) 0.0292(9) F14 0.128(2) 0.0892(17) 0.0707(15) 0.0489(13) 0.0791(17) 0.0689(17) F15 0.0877(17) 0.0307(10) 0.0713(15) 0.0256(10) 0.0312(13) 0.0057(10) F16 0.0587(13) 0.0658(14) 0.0692(14) 0.0437(12) 0.0231(11) 0.0316(11) F17 0.033(3) 0.177(11) 0.052(4) -0.027(6) 0.019(3) -0.038(5) F18 0.062(4) 0.070(3) 0.034(2) -0.003(2) -0.012(2) 0.004(3) F19 0.119(7) 0.105(5) 0.061(5) -0.042(3) 0.007(4) 0.063(5) F17B 0.076(9) 0.031(3) 0.053(5) -0.005(3) -0.001(5) -0.031(4) F18B 0.095(10) 0.071(7) 0.121(11) -0.020(8) -0.079(7) 0.026(7) F19B 0.076(8) 0.25(2) 0.053(7) -0.068(10) 0.042(7) -0.028(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 F1 2.2907(15) 2 ? Sm1 F1 2.3086(15) . ? Sm1 O1 2.4166(18) . ? Sm1 O4 2.4331(16) . ? Sm1 O3 2.4347(17) . ? Sm1 O5 2.4357(17) . ? Sm1 O6 2.4493(18) . ? Sm1 O2 2.5137(16) . ? Sm1 Sm1 3.7187(3) 2 ? Sm1 K1 4.0333(5) 2 ? Sm1 K1 4.2765(5) . ? K1 F1 2.7444(15) . ? K1 O8 2.765(2) . ? K1 O7 2.780(2) . ? K1 O9 2.8004(19) . ? K1 F11 2.8476(17) . ? K1 F6 2.9064(18) 2 ? K1 O5 2.9443(18) 2 ? K1 O4 2.9699(17) . ? K1 O2 3.0228(18) 2 ? K1 F16 3.170(2) 2 ? K1 C18 3.484(3) . ? K1 Sm1 4.0333(5) 2 ? F1 Sm1 2.2907(15) 2 ? O1 C2 1.252(3) . ? O2 C4 1.241(3) . ? O2 K1 3.0228(18) 2 ? O3 C7 1.246(3) . ? O4 C9 1.260(3) . ? O5 C12 1.249(3) . ? O5 K1 2.9443(18) 2 ? O6 C14 1.231(3) . ? O7 C17 1.416(4) . ? O7 C16 1.424(4) . ? O8 C19 1.427(3) . ? O8 C18 1.437(4) . ? O9 C21 1.417(4) . ? O9 C20 1.424(4) . ? C1 F2 1.326(3) . ? C1 F3 1.328(3) . ? C1 F4 1.334(3) . ? C1 C2 1.537(3) . ? C2 C3 1.386(3) . ? C3 C4 1.401(3) . ? C4 C5 1.535(3) . ? C5 F5 1.324(3) . ? C5 F7 1.328(3) . ? C5 F6 1.335(3) . ? C6 F9 1.313(3) . ? C6 F8 1.320(3) . ? C6 F10 1.324(3) . ? C6 C7 1.541(3) . ? C7 C8 1.395(3) . ? C8 C9 1.383(3) . ? C9 C10 1.542(3) . ? C10 F13 1.318(3) . ? C10 F12 1.329(3) . ? C10 F11 1.338(3) . ? C11 F14 1.319(4) . ? C11 F16 1.321(4) . ? C11 F15 1.322(3) . ? C11 C12 1.534(4) . ? C12 C13 1.386(4) . ? C13 C14 1.400(4) . ? C14 C15 1.534(4) . ? C15 F19B 1.193(14) . ? C15 F17 1.282(9) . ? C15 F18 1.297(9) . ? C15 F17B 1.304(11) . ? C15 F18B 1.330(15) . ? C15 F19 1.344(9) . ? C17 C18 1.495(5) . ? C19 C20 1.479(4) . ? F6 K1 2.9065(18) 2 ? F16 K1 3.170(2) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Sm1 F1 72.10(6) 2 . ? F1 Sm1 O1 140.20(6) 2 . ? F1 Sm1 O1 82.88(6) . . ? F1 Sm1 O4 111.92(5) 2 . ? F1 Sm1 O4 77.76(5) . . ? O1 Sm1 O4 91.62(6) . . ? F1 Sm1 O3 78.83(6) 2 . ? F1 Sm1 O3 125.05(6) . . ? O1 Sm1 O3 140.61(6) . . ? O4 Sm1 O3 71.35(5) . . ? F1 Sm1 O5 82.17(6) 2 . ? F1 Sm1 O5 140.35(5) . . ? O1 Sm1 O5 99.64(6) . . ? O4 Sm1 O5 141.06(6) . . ? O3 Sm1 O5 76.59(6) . . ? F1 Sm1 O6 143.22(6) 2 . ? F1 Sm1 O6 143.59(6) . . ? O1 Sm1 O6 70.60(7) . . ? O4 Sm1 O6 78.51(6) . . ? O3 Sm1 O6 71.28(7) . . ? O5 Sm1 O6 70.59(6) . . ? F1 Sm1 O2 74.69(5) 2 . ? F1 Sm1 O2 77.47(5) . . ? O1 Sm1 O2 69.89(6) . . ? O4 Sm1 O2 150.65(6) . . ? O3 Sm1 O2 136.97(5) . . ? O5 Sm1 O2 66.77(6) . . ? O6 Sm1 O2 114.07(6) . . ? F1 Sm1 Sm1 36.21(4) 2 2 ? F1 Sm1 Sm1 35.89(4) . 2 ? O1 Sm1 Sm1 113.35(5) . 2 ? O4 Sm1 Sm1 95.64(4) . 2 ? O3 Sm1 Sm1 103.72(4) . 2 ? O5 Sm1 Sm1 113.21(4) . 2 ? O6 Sm1 Sm1 173.22(5) . 2 ? O2 Sm1 Sm1 72.70(4) . 2 ? F1 Sm1 K1 40.82(4) 2 2 ? F1 Sm1 K1 96.71(4) . 2 ? O1 Sm1 K1 116.17(4) . 2 ? O4 Sm1 K1 151.01(4) . 2 ? O3 Sm1 K1 89.91(4) . 2 ? O5 Sm1 K1 46.47(4) . 2 ? O6 Sm1 K1 117.02(5) . 2 ? O2 Sm1 K1 48.45(4) . 2 ? Sm1 Sm1 K1 66.820(8) 2 2 ? F1 Sm1 K1 90.69(4) 2 . ? F1 Sm1 K1 35.44(4) . . ? O1 Sm1 K1 85.91(4) . . ? O4 Sm1 K1 42.32(4) . . ? O3 Sm1 K1 101.99(4) . . ? O5 Sm1 K1 172.86(4) . . ? O6 Sm1 K1 115.78(5) . . ? O2 Sm1 K1 111.53(4) . . ? Sm1 Sm1 K1 60.111(8) 2 . ? K1 Sm1 K1 126.931(7) 2 . ? F1 K1 O8 105.74(5) . . ? F1 K1 O7 66.79(5) . . ? O8 K1 O7 60.87(6) . . ? F1 K1 O9 162.44(6) . . ? O8 K1 O9 59.93(6) . . ? O7 K1 O9 96.15(6) . . ? F1 K1 F11 117.61(5) . . ? O8 K1 F11 67.45(6) . . ? O7 K1 F11 126.38(6) . . ? O9 K1 F11 68.35(6) . . ? F1 K1 F6 113.77(5) . 2 ? O8 K1 F6 126.86(6) . 2 ? O7 K1 F6 169.47(7) . 2 ? O9 K1 F6 83.78(5) . 2 ? F11 K1 F6 63.38(6) . 2 ? F1 K1 O5 66.13(5) . 2 ? O8 K1 O5 148.92(6) . 2 ? O7 K1 O5 89.37(6) . 2 ? O9 K1 O5 120.05(6) . 2 ? F11 K1 O5 143.54(6) . 2 ? F6 K1 O5 81.63(5) 2 2 ? F1 K1 O4 62.67(4) . . ? O8 K1 O4 80.59(5) . . ? O7 K1 O4 101.80(6) . . ? O9 K1 O4 120.09(6) . . ? F11 K1 O4 54.98(4) . . ? F6 K1 O4 87.21(6) 2 . ? O5 K1 O4 116.83(5) 2 . ? F1 K1 O2 60.61(5) . 2 ? O8 K1 O2 149.94(6) . 2 ? O7 K1 O2 124.40(5) . 2 ? O9 K1 O2 136.90(5) . 2 ? F11 K1 O2 94.17(5) . 2 ? F6 K1 O2 53.61(4) 2 2 ? O5 K1 O2 54.31(5) 2 2 ? O4 K1 O2 69.35(5) . 2 ? F1 K1 F16 109.66(5) . 2 ? O8 K1 F16 110.68(6) . 2 ? O7 K1 F16 81.84(6) . 2 ? O9 K1 F16 70.07(6) . 2 ? F11 K1 F16 131.38(6) . 2 ? F6 K1 F16 88.27(6) 2 2 ? O5 K1 F16 51.73(5) 2 2 ? O4 K1 F16 168.28(5) . 2 ? O2 K1 F16 99.33(5) 2 2 ? F1 K1 C18 83.74(6) . . ? O8 K1 C18 23.13(7) . . ? O7 K1 C18 42.59(7) . . ? O9 K1 C18 80.49(7) . . ? F11 K1 C18 83.79(7) . . ? F6 K1 C18 146.96(7) 2 . ? O5 K1 C18 131.34(7) 2 . ? O4 K1 C18 76.07(6) . . ? O2 K1 C18 138.58(6) 2 . ? F16 K1 C18 112.92(7) 2 . ? F1 K1 Sm1 33.07(3) . 2 ? O8 K1 Sm1 138.19(4) . 2 ? O7 K1 Sm1 86.59(4) . 2 ? O9 K1 Sm1 156.86(5) . 2 ? F11 K1 Sm1 127.47(4) . 2 ? F6 K1 Sm1 89.42(3) 2 2 ? O5 K1 Sm1 36.86(3) 2 2 ? O4 K1 Sm1 81.45(3) . 2 ? O2 K1 Sm1 38.49(3) 2 2 ? F16 K1 Sm1 87.69(4) 2 2 ? C18 K1 Sm1 115.35(6) . 2 ? Sm1 F1 Sm1 107.90(6) 2 . ? Sm1 F1 K1 106.11(6) 2 . ? Sm1 F1 K1 115.36(6) . . ? C2 O1 Sm1 134.18(15) . . ? C4 O2 Sm1 131.54(15) . . ? C4 O2 K1 121.97(14) . 2 ? Sm1 O2 K1 93.06(5) . 2 ? C7 O3 Sm1 131.51(15) . . ? C9 O4 Sm1 131.81(15) . . ? C9 O4 K1 119.66(14) . . ? Sm1 O4 K1 104.21(5) . . ? C12 O5 Sm1 135.15(17) . . ? C12 O5 K1 128.15(16) . 2 ? Sm1 O5 K1 96.67(6) . 2 ? C14 O6 Sm1 135.82(17) . . ? C17 O7 C16 112.8(2) . . ? C17 O7 K1 119.77(18) . . ? C16 O7 K1 123.48(19) . . ? C19 O8 C18 114.6(2) . . ? C19 O8 K1 115.14(16) . . ? C18 O8 K1 107.77(16) . . ? C21 O9 C20 112.0(3) . . ? C21 O9 K1 118.9(2) . . ? C20 O9 K1 116.14(16) . . ? F2 C1 F3 107.6(2) . . ? F2 C1 F4 107.0(2) . . ? F3 C1 F4 106.8(2) . . ? F2 C1 C2 110.5(2) . . ? F3 C1 C2 111.2(2) . . ? F4 C1 C2 113.5(2) . . ? O1 C2 C3 128.1(2) . . ? O1 C2 C1 113.9(2) . . ? C3 C2 C1 118.0(2) . . ? C2 C3 C4 121.6(2) . . ? O2 C4 C3 128.4(2) . . ? O2 C4 C5 114.1(2) . . ? C3 C4 C5 117.5(2) . . ? F5 C5 F7 107.2(2) . . ? F5 C5 F6 106.9(2) . . ? F7 C5 F6 107.1(2) . . ? F5 C5 C4 114.1(2) . . ? F7 C5 C4 110.8(2) . . ? F6 C5 C4 110.3(2) . . ? F9 C6 F8 107.9(2) . . ? F9 C6 F10 106.3(2) . . ? F8 C6 F10 107.0(2) . . ? F9 C6 C7 111.3(2) . . ? F8 C6 C7 113.5(2) . . ? F10 C6 C7 110.4(2) . . ? O3 C7 C8 128.2(2) . . ? O3 C7 C6 114.8(2) . . ? C8 C7 C6 116.9(2) . . ? C9 C8 C7 121.6(2) . . ? O4 C9 C8 128.9(2) . . ? O4 C9 C10 114.2(2) . . ? C8 C9 C10 116.9(2) . . ? F13 C10 F12 107.9(2) . . ? F13 C10 F11 107.5(2) . . ? F12 C10 F11 106.4(2) . . ? F13 C10 C9 111.0(2) . . ? F12 C10 C9 112.9(2) . . ? F11 C10 C9 110.8(2) . . ? F14 C11 F16 106.8(3) . . ? F14 C11 F15 108.3(3) . . ? F16 C11 F15 106.4(3) . . ? F14 C11 C12 109.8(2) . . ? F16 C11 C12 110.9(2) . . ? F15 C11 C12 114.3(3) . . ? O5 C12 C13 128.8(2) . . ? O5 C12 C11 112.6(2) . . ? C13 C12 C11 118.6(2) . . ? C12 C13 C14 121.3(2) . . ? O6 C14 C13 128.2(2) . . ? O6 C14 C15 115.0(3) . . ? C13 C14 C15 116.8(3) . . ? F19B C15 F17 121.4(10) . . ? F19B C15 F18 79.0(13) . . ? F17 C15 F18 108.7(7) . . ? F19B C15 F17B 105.0(13) . . ? F17 C15 F17B 24.1(11) . . ? F18 C15 F17B 126.0(8) . . ? F19B C15 F18B 116.1(13) . . ? F17 C15 F18B 77.0(10) . . ? F18 C15 F18B 39.9(9) . . ? F17B C15 F18B 100.3(11) . . ? F19B C15 F19 23.8(15) . . ? F17 C15 F19 107.6(8) . . ? F18 C15 F19 102.0(7) . . ? F17B C15 F19 86.5(9) . . ? F18B C15 F19 135.8(9) . . ? F19B C15 C14 114.0(8) . . ? F17 C15 C14 114.4(6) . . ? F18 C15 C14 113.9(4) . . ? F17B C15 C14 112.8(8) . . ? F18B C15 C14 108.0(6) . . ? F19 C15 C14 109.2(6) . . ? O7 C17 C18 108.8(2) . . ? O8 C18 C17 113.5(2) . . ? O8 C18 K1 49.10(12) . . ? C17 C18 K1 85.97(16) . . ? O8 C19 C20 108.5(2) . . ? O9 C20 C19 108.8(2) . . ? C5 F6 K1 123.64(15) . 2 ? C10 F11 K1 125.63(13) . . ? C11 F16 K1 106.84(17) . 2 ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.900 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.084 #===end data_dg21 _database_code_CSD 171878 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 F18 O9 Tb' _chemical_formula_weight 914.27 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' 'Tb' 'Tb' -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.3778(12) _cell_length_b 11.1908(6) _cell_length_c 12.3993(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3105.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.956 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 2.431 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5391 _exptl_absorpt_correction_T_max 0.6552 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% '< 1.0' _diffrn_reflns_number 31687 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7544 _reflns_number_gt 6852 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0236P)^2^+0.7949P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'Automated Patterson' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.045(6) _refine_ls_number_reflns 7544 _refine_ls_number_parameters 510 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 1.124366(4) 0.090873(8) 0.50028(2) 0.01866(4) Uani 1 1 d . . . O1 O 1.12559(8) 0.2594(2) 0.3765(3) 0.0259(7) Uani 1 1 d . . . O2 O 1.14533(9) 0.02577(17) 0.32258(17) 0.0255(4) Uani 1 1 d . . . O3 O 1.02683(8) 0.16755(17) 0.47727(15) 0.0244(5) Uani 1 1 d . . . O4 O 1.11830(9) 0.2680(2) 0.6022(2) 0.0256(6) Uani 1 1 d . . . O5 O 1.17900(8) -0.08839(15) 0.5140(2) 0.0239(4) Uani 1 1 d . . . O6 O 1.05913(9) -0.07047(17) 0.45161(17) 0.0251(4) Uani 1 1 d . . . O7 O 1.07006(9) 0.02581(18) 0.66829(16) 0.0275(4) Uani 1 1 d . . . O8 O 1.18638(9) 0.07921(17) 0.67097(16) 0.0258(4) Uani 1 1 d . . . O9 O 1.23127(8) 0.15707(19) 0.48093(16) 0.0275(5) Uani 1 1 d . . . C1 C 1.1113(2) 0.4012(3) 0.2408(4) 0.0393(11) Uani 1 1 d . . . C2 C 1.12116(11) 0.2705(3) 0.2773(3) 0.0251(6) Uani 1 1 d . . . C3 C 1.12628(12) 0.1829(3) 0.1985(3) 0.0254(6) Uani 1 1 d . . . C4 C 1.13991(16) 0.0659(3) 0.2282(3) 0.0222(7) Uani 1 1 d . . . C5 C 1.15288(15) -0.0261(3) 0.1407(2) 0.0315(7) Uani 1 1 d . . . C6 C 0.94624(13) 0.2904(3) 0.4324(2) 0.0281(6) Uani 1 1 d . . . C7 C 1.00511(11) 0.2700(2) 0.4926(3) 0.0244(5) Uani 1 1 d . . . C8 C 1.02840(14) 0.3633(3) 0.5524(3) 0.0281(6) Uani 1 1 d . . . C9 C 1.08319(13) 0.3536(3) 0.6037(2) 0.0262(6) Uani 1 1 d . . . C10 C 1.10468(16) 0.4584(3) 0.6748(3) 0.0352(7) Uani 1 1 d . . . C11 C 1.22633(12) -0.2728(3) 0.5010(4) 0.0352(6) Uani 1 1 d . . . C12 C 1.17051(12) -0.1945(2) 0.4852(2) 0.0236(6) Uani 1 1 d . . . C13 C 1.11838(13) -0.2472(3) 0.4477(3) 0.0286(7) Uani 1 1 d . . . C14 C 1.06651(12) -0.1811(2) 0.4364(2) 0.0236(6) Uani 1 1 d . . . C15 C 1.01011(15) -0.2469(3) 0.4008(3) 0.0356(8) Uani 1 1 d . . . C16 C 1.26239(16) 0.1595(5) 0.3800(3) 0.0479(11) Uani 1 1 d . . . C17 C 1.27106(14) 0.1314(3) 0.5684(3) 0.0310(7) Uani 1 1 d . . . C18 C 1.23856(13) 0.1539(3) 0.6719(3) 0.0293(7) Uani 1 1 d . . . C19 C 1.15482(19) 0.0813(4) 0.7699(4) 0.0310(10) Uani 1 1 d . . . C20 C 1.10470(16) -0.0078(3) 0.7611(3) 0.0320(7) Uani 1 1 d . . . C21 C 1.01167(14) -0.0297(3) 0.6697(3) 0.0347(7) Uani 1 1 d . . . F1 F 1.1050(2) 0.4144(2) 0.1367(2) 0.1031(13) Uani 1 1 d . . . F2 F 1.15615(17) 0.4670(3) 0.2649(3) 0.1038(13) Uani 1 1 d . . . F3 F 1.06510(16) 0.4485(3) 0.2862(3) 0.1132(15) Uani 1 1 d . . . F4 F 1.12267(9) -0.12691(19) 0.16014(17) 0.0468(6) Uani 1 1 d . . . F5 F 1.13900(11) 0.01067(19) 0.04285(15) 0.0500(5) Uani 1 1 d . . . F6 F 1.21086(10) -0.0536(2) 0.14038(19) 0.0537(6) Uani 1 1 d . . . F7 F 0.90653(7) 0.20520(17) 0.45382(15) 0.0375(4) Uani 1 1 d . . . F8 F 0.95533(9) 0.28449(19) 0.32502(15) 0.0459(5) Uani 1 1 d . . . F9 F 0.92048(10) 0.39375(17) 0.4535(2) 0.0523(6) Uani 1 1 d . . . F10 F 1.15832(12) 0.4911(3) 0.6478(3) 0.0943(12) Uani 1 1 d . . . F11 F 1.07210(14) 0.5561(2) 0.6627(3) 0.0928(11) Uani 1 1 d . . . F12 F 1.1060(2) 0.4285(3) 0.7752(3) 0.0961(14) Uani 1 1 d . . . F13 F 1.27341(9) -0.2239(2) 0.4526(2) 0.0637(7) Uani 1 1 d . . . F14 F 1.23879(10) -0.2854(2) 0.60498(18) 0.0556(6) Uani 1 1 d . . . F15 F 1.22078(9) -0.38235(18) 0.45965(17) 0.0445(5) Uani 1 1 d . . . F16 F 1.01066(11) -0.36122(19) 0.4182(3) 0.0740(8) Uani 1 1 d . . . F17 F 0.96142(10) -0.2031(3) 0.4469(3) 0.0817(9) Uani 1 1 d . . . F18 F 1.00045(12) -0.2329(3) 0.29690(19) 0.0857(10) Uani 1 1 d . . . H3 H 1.1235(14) 0.200(4) 0.137(4) 0.034(10) Uiso 1 1 d . . . H8 H 1.0090(15) 0.422(3) 0.554(3) 0.024(8) Uiso 1 1 d . . . H13 H 1.1158(13) -0.333(3) 0.437(3) 0.026(8) Uiso 1 1 d . . . H16A H 1.2371(14) 0.187(3) 0.319(3) 0.023(8) Uiso 1 1 d . . . H16B H 1.291(2) 0.203(4) 0.393(3) 0.048(12) Uiso 1 1 d . . . H16C H 1.271(2) 0.071(5) 0.356(6) 0.10(2) Uiso 1 1 d . . . H17A H 1.3069(17) 0.185(3) 0.558(3) 0.041(10) Uiso 1 1 d . . . H17B H 1.2832(16) 0.056(3) 0.570(3) 0.035(10) Uiso 1 1 d . . . H18A H 1.2260(13) 0.234(3) 0.679(3) 0.027(8) Uiso 1 1 d . . . H18B H 1.2620(16) 0.133(3) 0.736(3) 0.038(9) Uiso 1 1 d . . . H19A H 1.1773(14) 0.072(3) 0.821(3) 0.023(8) Uiso 1 1 d . . . H19B H 1.1378(17) 0.164(4) 0.777(3) 0.046(12) Uiso 1 1 d . . . H20A H 1.1203(14) -0.088(3) 0.745(3) 0.032(10) Uiso 1 1 d . . . H20B H 1.0805(14) -0.005(3) 0.817(3) 0.030(9) Uiso 1 1 d . . . H21A H 0.9887(14) -0.002(3) 0.734(3) 0.028(8) Uiso 1 1 d . . . H21B H 1.0159(14) -0.111(3) 0.668(3) 0.023(8) Uiso 1 1 d . . . H21C H 0.9908(16) 0.005(3) 0.614(3) 0.034(9) 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 Tb1 0.01871(5) 0.01793(6) 0.01934(6) -0.00242(8) -0.00071(6) 0.00047(4) O1 0.0322(14) 0.0202(12) 0.0254(14) -0.0009(9) 0.0051(8) -0.0006(9) O2 0.0317(10) 0.0217(10) 0.0231(10) -0.0032(8) 0.0004(9) 0.0017(8) O3 0.0230(8) 0.0214(9) 0.0287(14) -0.0007(7) -0.0002(7) 0.0009(7) O4 0.0273(12) 0.0281(13) 0.0213(13) -0.0072(10) -0.0001(9) 0.0000(9) O5 0.0255(8) 0.0249(9) 0.0213(12) -0.0010(8) -0.0023(9) 0.0029(6) O6 0.0259(10) 0.0185(9) 0.0307(10) -0.0025(8) -0.0030(8) -0.0009(8) O7 0.0251(10) 0.0340(12) 0.0235(10) 0.0023(9) 0.0009(8) -0.0066(8) O8 0.0269(10) 0.0305(11) 0.0200(10) -0.0020(8) -0.0027(8) -0.0019(8) O9 0.0209(8) 0.0399(11) 0.0218(14) 0.0014(9) -0.0011(8) -0.0044(8) C1 0.049(2) 0.028(2) 0.041(3) 0.0067(16) 0.0091(18) -0.0005(15) C2 0.0234(14) 0.0223(14) 0.0295(16) 0.0025(12) 0.0054(11) -0.0006(11) C3 0.0263(15) 0.0294(16) 0.0205(15) 0.0018(12) 0.0007(11) -0.0046(11) C4 0.0216(15) 0.0281(15) 0.0170(15) -0.0060(13) -0.0034(12) -0.0024(13) C5 0.0424(18) 0.0289(16) 0.0232(15) -0.0048(12) 0.0036(13) -0.0032(13) C6 0.0295(14) 0.0268(15) 0.0280(15) 0.0060(12) 0.0026(12) 0.0053(12) C7 0.0227(11) 0.0232(11) 0.0273(13) 0.0059(15) 0.0063(14) 0.0041(9) C8 0.0302(15) 0.0219(15) 0.0323(16) -0.0050(12) 0.0024(13) 0.0059(12) C9 0.0337(15) 0.0221(14) 0.0228(14) -0.0049(11) 0.0067(12) -0.0016(12) C10 0.0373(17) 0.0262(16) 0.042(2) -0.0093(15) 0.0033(15) -0.0005(14) C11 0.0318(13) 0.0305(12) 0.0432(16) -0.005(2) -0.0075(19) 0.0107(11) C12 0.0310(12) 0.0267(13) 0.0131(15) -0.0003(10) 0.0005(11) 0.0066(10) C13 0.0337(16) 0.0204(15) 0.0318(16) 0.0018(12) -0.0068(12) 0.0032(11) C14 0.0271(14) 0.0207(14) 0.0229(14) -0.0009(11) -0.0021(11) -0.0011(11) C15 0.0337(16) 0.0266(17) 0.046(2) -0.0023(14) -0.0054(15) -0.0051(12) C16 0.0246(17) 0.091(4) 0.0282(19) 0.002(2) 0.0068(15) -0.014(2) C17 0.0208(15) 0.042(2) 0.0301(17) -0.0029(15) -0.0054(12) -0.0008(14) C18 0.0233(14) 0.0375(18) 0.0270(16) -0.0038(13) -0.0046(13) -0.0012(13) C19 0.030(2) 0.042(2) 0.0209(18) 0.0039(14) -0.0007(15) -0.0061(15) C20 0.0367(16) 0.0339(18) 0.0254(16) 0.0030(13) -0.0002(14) -0.0041(15) C21 0.0278(16) 0.042(2) 0.0343(18) -0.0001(15) 0.0029(14) -0.0107(14) F1 0.222(4) 0.0429(16) 0.0447(17) 0.0149(12) -0.009(2) 0.0348(18) F2 0.122(3) 0.0477(17) 0.141(3) 0.0368(19) -0.035(3) -0.0396(18) F3 0.124(3) 0.0576(18) 0.158(3) 0.059(2) 0.086(3) 0.0530(18) F4 0.0759(16) 0.0308(10) 0.0337(11) -0.0097(9) 0.0053(10) -0.0162(9) F5 0.0859(16) 0.0422(12) 0.0219(9) -0.0043(8) 0.0029(10) -0.0012(11) F6 0.0492(12) 0.0538(13) 0.0580(14) -0.0189(11) 0.0164(11) 0.0136(11) F7 0.0259(8) 0.0412(11) 0.0455(10) 0.0119(8) -0.0037(8) -0.0023(7) F8 0.0482(11) 0.0607(14) 0.0288(10) 0.0171(10) -0.0040(9) 0.0002(10) F9 0.0447(12) 0.0342(11) 0.0779(16) -0.0081(10) -0.0194(11) 0.0205(9) F10 0.0698(18) 0.0651(18) 0.148(3) -0.061(2) 0.0308(19) -0.0387(15) F11 0.101(2) 0.0484(14) 0.129(3) -0.0548(17) -0.044(2) 0.0305(15) F12 0.180(4) 0.074(2) 0.0347(17) -0.0188(16) -0.010(2) -0.051(2) F13 0.0311(10) 0.0470(13) 0.113(2) 0.0080(13) 0.0201(11) 0.0113(9) F14 0.0631(14) 0.0559(14) 0.0479(13) -0.0056(11) -0.0285(11) 0.0261(12) F15 0.0479(11) 0.0293(9) 0.0564(13) -0.0090(8) -0.0069(9) 0.0159(9) F16 0.0574(14) 0.0273(11) 0.137(2) 0.0077(14) -0.0395(16) -0.0122(10) F17 0.0337(11) 0.0770(18) 0.134(3) -0.0524(17) 0.0112(13) -0.0148(11) F18 0.0905(19) 0.116(2) 0.0501(15) 0.0190(15) -0.0404(14) -0.0607(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 O4 2.354(3) . ? Tb1 O5 2.3554(17) . ? Tb1 O3 2.3624(18) . ? Tb1 O2 2.368(2) . ? Tb1 O6 2.3990(19) . ? Tb1 O1 2.432(3) . ? Tb1 O9 2.5159(18) . ? Tb1 O7 2.519(2) . ? Tb1 O8 2.534(2) . ? O1 C2 1.240(5) . ? O2 C4 1.259(4) . ? O3 C7 1.260(3) . ? O4 C9 1.239(4) . ? O5 C12 1.254(3) . ? O6 C14 1.264(3) . ? O7 C20 1.438(4) . ? O7 C21 1.447(3) . ? O8 C19 1.415(5) . ? O8 C18 1.436(4) . ? O9 C17 1.432(4) . ? O9 C16 1.432(4) . ? C1 F2 1.280(5) . ? C1 F3 1.291(5) . ? C1 F1 1.307(6) . ? C1 C2 1.547(5) . ? C2 C3 1.389(5) . ? C3 C4 1.394(5) . ? C4 C5 1.524(4) . ? C5 F5 1.318(4) . ? C5 F6 1.333(4) . ? C5 F4 1.337(4) . ? C6 F9 1.318(3) . ? C6 F7 1.331(3) . ? C6 F8 1.349(4) . ? C6 C7 1.531(4) . ? C7 C8 1.382(4) . ? C8 C9 1.385(4) . ? C9 C10 1.545(4) . ? C10 F12 1.289(6) . ? C10 F10 1.299(4) . ? C10 F11 1.323(4) . ? C11 F14 1.327(5) . ? C11 F13 1.330(4) . ? C11 F15 1.334(4) . ? C11 C12 1.539(4) . ? C12 C13 1.387(4) . ? C13 C14 1.383(4) . ? C14 C15 1.526(4) . ? C15 F16 1.298(4) . ? C15 F18 1.315(4) . ? C15 F17 1.325(4) . ? C17 C18 1.497(5) . ? C19 C20 1.505(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 O4 Tb1 O5 135.09(9) . . ? O4 Tb1 O3 72.89(7) . . ? O5 Tb1 O3 142.90(6) . . ? O4 Tb1 O2 140.34(8) . . ? O5 Tb1 O2 72.67(8) . . ? O3 Tb1 O2 100.51(7) . . ? O4 Tb1 O6 137.18(7) . . ? O5 Tb1 O6 72.12(7) . . ? O3 Tb1 O6 71.39(7) . . ? O2 Tb1 O6 69.81(7) . . ? O4 Tb1 O1 71.74(9) . . ? O5 Tb1 O1 134.44(8) . . ? O3 Tb1 O1 69.67(6) . . ? O2 Tb1 O1 69.45(8) . . ? O6 Tb1 O1 115.58(8) . . ? O4 Tb1 O9 81.84(7) . . ? O5 Tb1 O9 76.36(7) . . ? O3 Tb1 O9 139.47(7) . . ? O2 Tb1 O9 79.25(7) . . ? O6 Tb1 O9 140.92(7) . . ? O1 Tb1 O9 72.59(6) . . ? O4 Tb1 O7 76.81(8) . . ? O5 Tb1 O7 86.82(7) . . ? O3 Tb1 O7 76.07(6) . . ? O2 Tb1 O7 140.91(7) . . ? O6 Tb1 O7 72.36(7) . . ? O1 Tb1 O7 138.73(7) . . ? O9 Tb1 O7 128.51(6) . . ? O4 Tb1 O8 68.08(8) . . ? O5 Tb1 O8 67.15(7) . . ? O3 Tb1 O8 128.71(7) . . ? O2 Tb1 O8 130.76(7) . . ? O6 Tb1 O8 120.30(7) . . ? O1 Tb1 O8 124.12(7) . . ? O9 Tb1 O8 64.79(7) . . ? O7 Tb1 O8 63.81(7) . . ? C2 O1 Tb1 134.6(2) . . ? C4 O2 Tb1 137.4(2) . . ? C7 O3 Tb1 131.99(17) . . ? C9 O4 Tb1 134.0(2) . . ? C12 O5 Tb1 135.00(18) . . ? C14 O6 Tb1 134.09(17) . . ? C20 O7 C21 111.4(2) . . ? C20 O7 Tb1 118.52(18) . . ? C21 O7 Tb1 124.70(19) . . ? C19 O8 C18 112.9(3) . . ? C19 O8 Tb1 116.7(2) . . ? C18 O8 Tb1 114.98(17) . . ? C17 O9 C16 111.3(3) . . ? C17 O9 Tb1 117.38(17) . . ? C16 O9 Tb1 123.4(2) . . ? F2 C1 F3 106.9(4) . . ? F2 C1 F1 104.6(4) . . ? F3 C1 F1 107.3(4) . . ? F2 C1 C2 111.4(4) . . ? F3 C1 C2 111.9(4) . . ? F1 C1 C2 114.2(4) . . ? O1 C2 C3 128.4(3) . . ? O1 C2 C1 113.3(3) . . ? C3 C2 C1 118.2(3) . . ? C2 C3 C4 119.6(3) . . ? O2 C4 C3 127.0(3) . . ? O2 C4 C5 113.7(3) . . ? C3 C4 C5 119.2(3) . . ? F5 C5 F6 107.4(3) . . ? F5 C5 F4 108.1(3) . . ? F6 C5 F4 107.3(3) . . ? F5 C5 C4 113.6(3) . . ? F6 C5 C4 110.1(3) . . ? F4 C5 C4 110.2(3) . . ? F9 C6 F7 107.3(2) . . ? F9 C6 F8 107.8(2) . . ? F7 C6 F8 105.2(3) . . ? F9 C6 C7 114.3(3) . . ? F7 C6 C7 111.7(2) . . ? F8 C6 C7 110.1(2) . . ? O3 C7 C8 128.5(3) . . ? O3 C7 C6 113.3(3) . . ? C8 C7 C6 118.2(2) . . ? C7 C8 C9 121.4(3) . . ? O4 C9 C8 128.0(3) . . ? O4 C9 C10 113.5(3) . . ? C8 C9 C10 118.6(3) . . ? F12 C10 F10 107.5(4) . . ? F12 C10 F11 109.7(4) . . ? F10 C10 F11 104.3(3) . . ? F12 C10 C9 111.2(3) . . ? F10 C10 C9 110.8(3) . . ? F11 C10 C9 113.0(3) . . ? F14 C11 F13 108.4(3) . . ? F14 C11 F15 107.2(3) . . ? F13 C11 F15 106.2(3) . . ? F14 C11 C12 110.7(3) . . ? F13 C11 C12 110.6(3) . . ? F15 C11 C12 113.5(2) . . ? O5 C12 C13 128.7(2) . . ? O5 C12 C11 112.4(2) . . ? C13 C12 C11 118.9(2) . . ? C14 C13 C12 120.8(3) . . ? O6 C14 C13 128.2(3) . . ? O6 C14 C15 114.1(2) . . ? C13 C14 C15 117.8(3) . . ? F16 C15 F18 106.4(3) . . ? F16 C15 F17 107.5(3) . . ? F18 C15 F17 104.1(3) . . ? F16 C15 C14 114.8(3) . . ? F18 C15 C14 111.2(3) . . ? F17 C15 C14 112.1(3) . . ? O9 C17 C18 108.3(2) . . ? O8 C18 C17 106.9(3) . . ? O8 C19 C20 107.4(3) . . ? O7 C20 C19 106.6(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 O4 Tb1 O1 C2 -169.2(3) . . . . ? O5 Tb1 O1 C2 54.7(3) . . . . ? O3 Tb1 O1 C2 -91.2(2) . . . . ? O2 Tb1 O1 C2 19.1(2) . . . . ? O6 Tb1 O1 C2 -34.9(3) . . . . ? O9 Tb1 O1 C2 103.8(3) . . . . ? O7 Tb1 O1 C2 -127.0(2) . . . . ? O8 Tb1 O1 C2 145.1(2) . . . . ? O4 Tb1 O2 C4 -30.1(4) . . . . ? O5 Tb1 O2 C4 -171.9(3) . . . . ? O3 Tb1 O2 C4 45.7(3) . . . . ? O6 Tb1 O2 C4 111.2(3) . . . . ? O1 Tb1 O2 C4 -17.8(3) . . . . ? O9 Tb1 O2 C4 -93.0(3) . . . . ? O7 Tb1 O2 C4 126.5(3) . . . . ? O8 Tb1 O2 C4 -135.6(3) . . . . ? O4 Tb1 O3 C7 18.8(3) . . . . ? O5 Tb1 O3 C7 164.0(3) . . . . ? O2 Tb1 O3 C7 -120.8(3) . . . . ? O6 Tb1 O3 C7 174.8(3) . . . . ? O1 Tb1 O3 C7 -57.6(3) . . . . ? O9 Tb1 O3 C7 -35.1(3) . . . . ? O7 Tb1 O3 C7 99.0(3) . . . . ? O8 Tb1 O3 C7 60.5(3) . . . . ? O5 Tb1 O4 C9 -166.8(3) . . . . ? O3 Tb1 O4 C9 -16.0(3) . . . . ? O2 Tb1 O4 C9 69.9(3) . . . . ? O6 Tb1 O4 C9 -50.6(4) . . . . ? O1 Tb1 O4 C9 57.7(3) . . . . ? O9 Tb1 O4 C9 131.9(3) . . . . ? O7 Tb1 O4 C9 -95.2(3) . . . . ? O8 Tb1 O4 C9 -162.0(3) . . . . ? O4 Tb1 O5 C12 151.8(3) . . . . ? O3 Tb1 O5 C12 22.4(3) . . . . ? O2 Tb1 O5 C12 -62.2(3) . . . . ? O6 Tb1 O5 C12 11.6(3) . . . . ? O1 Tb1 O5 C12 -97.0(3) . . . . ? O9 Tb1 O5 C12 -145.0(3) . . . . ? O7 Tb1 O5 C12 84.1(3) . . . . ? O8 Tb1 O5 C12 147.0(3) . . . . ? O4 Tb1 O6 C14 -145.5(3) . . . . ? O5 Tb1 O6 C14 -7.2(2) . . . . ? O3 Tb1 O6 C14 179.6(3) . . . . ? O2 Tb1 O6 C14 70.4(3) . . . . ? O1 Tb1 O6 C14 124.2(3) . . . . ? O9 Tb1 O6 C14 30.5(3) . . . . ? O7 Tb1 O6 C14 -99.6(3) . . . . ? O8 Tb1 O6 C14 -55.8(3) . . . . ? O4 Tb1 O7 C20 -85.3(2) . . . . ? O5 Tb1 O7 C20 52.5(2) . . . . ? O3 Tb1 O7 C20 -160.7(2) . . . . ? O2 Tb1 O7 C20 109.7(2) . . . . ? O6 Tb1 O7 C20 124.8(2) . . . . ? O1 Tb1 O7 C20 -126.3(2) . . . . ? O9 Tb1 O7 C20 -17.2(2) . . . . ? O8 Tb1 O7 C20 -13.5(2) . . . . ? O4 Tb1 O7 C21 122.8(2) . . . . ? O5 Tb1 O7 C21 -99.4(2) . . . . ? O3 Tb1 O7 C21 47.4(2) . . . . ? O2 Tb1 O7 C21 -42.2(3) . . . . ? O6 Tb1 O7 C21 -27.1(2) . . . . ? O1 Tb1 O7 C21 81.8(3) . . . . ? O9 Tb1 O7 C21 -169.1(2) . . . . ? O8 Tb1 O7 C21 -165.4(3) . . . . ? O4 Tb1 O8 C19 65.8(2) . . . . ? O5 Tb1 O8 C19 -117.9(2) . . . . ? O3 Tb1 O8 C19 22.6(2) . . . . ? O2 Tb1 O8 C19 -155.7(2) . . . . ? O6 Tb1 O8 C19 -67.1(2) . . . . ? O1 Tb1 O8 C19 112.9(2) . . . . ? O9 Tb1 O8 C19 156.9(2) . . . . ? O7 Tb1 O8 C19 -19.8(2) . . . . ? O4 Tb1 O8 C18 -69.84(19) . . . . ? O5 Tb1 O8 C18 106.5(2) . . . . ? O3 Tb1 O8 C18 -113.04(19) . . . . ? O2 Tb1 O8 C18 68.6(2) . . . . ? O6 Tb1 O8 C18 157.27(19) . . . . ? O1 Tb1 O8 C18 -22.7(2) . . . . ? O9 Tb1 O8 C18 21.33(19) . . . . ? O7 Tb1 O8 C18 -155.5(2) . . . . ? O4 Tb1 O9 C17 81.1(2) . . . . ? O5 Tb1 O9 C17 -59.4(2) . . . . ? O3 Tb1 O9 C17 132.4(2) . . . . ? O2 Tb1 O9 C17 -134.0(2) . . . . ? O6 Tb1 O9 C17 -96.3(2) . . . . ? O1 Tb1 O9 C17 154.4(2) . . . . ? O7 Tb1 O9 C17 15.2(2) . . . . ? O8 Tb1 O9 C17 11.50(19) . . . . ? O4 Tb1 O9 C16 -132.6(3) . . . . ? O5 Tb1 O9 C16 86.9(3) . . . . ? O3 Tb1 O9 C16 -81.3(3) . . . . ? O2 Tb1 O9 C16 12.4(3) . . . . ? O6 Tb1 O9 C16 50.1(3) . . . . ? O1 Tb1 O9 C16 -59.3(3) . . . . ? O7 Tb1 O9 C16 161.5(3) . . . . ? O8 Tb1 O9 C16 157.8(3) . . . . ? Tb1 O1 C2 C3 -15.2(4) . . . . ? Tb1 O1 C2 C1 167.6(2) . . . . ? F2 C1 C2 O1 63.6(5) . . . . ? F3 C1 C2 O1 -56.0(5) . . . . ? F1 C1 C2 O1 -178.3(4) . . . . ? F2 C1 C2 C3 -114.0(4) . . . . ? F3 C1 C2 C3 126.4(4) . . . . ? F1 C1 C2 C3 4.2(5) . . . . ? O1 C2 C3 C4 -2.2(5) . . . . ? C1 C2 C3 C4 174.9(3) . . . . ? Tb1 O2 C4 C3 11.9(6) . . . . ? Tb1 O2 C4 C5 -171.0(2) . . . . ? C2 C3 C4 O2 4.3(5) . . . . ? C2 C3 C4 C5 -172.6(3) . . . . ? O2 C4 C5 F5 170.8(3) . . . . ? C3 C4 C5 F5 -11.8(4) . . . . ? O2 C4 C5 F6 -68.8(4) . . . . ? C3 C4 C5 F6 108.6(3) . . . . ? O2 C4 C5 F4 49.4(4) . . . . ? C3 C4 C5 F4 -133.2(3) . . . . ? Tb1 O3 C7 C8 -17.3(5) . . . . ? Tb1 O3 C7 C6 160.53(17) . . . . ? F9 C6 C7 O3 175.3(3) . . . . ? F7 C6 C7 O3 53.2(3) . . . . ? F8 C6 C7 O3 -63.3(3) . . . . ? F9 C6 C7 C8 -6.6(4) . . . . ? F7 C6 C7 C8 -128.6(3) . . . . ? F8 C6 C7 C8 114.8(3) . . . . ? O3 C7 C8 C9 1.7(5) . . . . ? C6 C7 C8 C9 -176.1(3) . . . . ? Tb1 O4 C9 C8 10.7(5) . . . . ? Tb1 O4 C9 C10 -171.0(2) . . . . ? C7 C8 C9 O4 2.0(5) . . . . ? C7 C8 C9 C10 -176.3(3) . . . . ? O4 C9 C10 F12 -66.3(4) . . . . ? C8 C9 C10 F12 112.3(4) . . . . ? O4 C9 C10 F10 53.2(4) . . . . ? C8 C9 C10 F10 -128.2(4) . . . . ? O4 C9 C10 F11 169.9(3) . . . . ? C8 C9 C10 F11 -11.6(5) . . . . ? Tb1 O5 C12 C13 -11.6(5) . . . . ? Tb1 O5 C12 C11 171.6(2) . . . . ? F14 C11 C12 O5 66.7(3) . . . . ? F13 C11 C12 O5 -53.5(4) . . . . ? F15 C11 C12 O5 -172.7(3) . . . . ? F14 C11 C12 C13 -110.5(3) . . . . ? F13 C11 C12 C13 129.4(3) . . . . ? F15 C11 C12 C13 10.2(5) . . . . ? O5 C12 C13 C14 0.9(5) . . . . ? C11 C12 C13 C14 177.5(3) . . . . ? Tb1 O6 C14 C13 2.5(5) . . . . ? Tb1 O6 C14 C15 -177.34(19) . . . . ? C12 C13 C14 O6 3.6(5) . . . . ? C12 C13 C14 C15 -176.6(3) . . . . ? O6 C14 C15 F16 -158.6(3) . . . . ? C13 C14 C15 F16 21.6(5) . . . . ? O6 C14 C15 F18 80.6(4) . . . . ? C13 C14 C15 F18 -99.3(4) . . . . ? O6 C14 C15 F17 -35.5(4) . . . . ? C13 C14 C15 F17 144.6(3) . . . . ? C16 O9 C17 C18 169.0(3) . . . . ? Tb1 O9 C17 C18 -40.8(3) . . . . ? C19 O8 C18 C17 173.3(3) . . . . ? Tb1 O8 C18 C17 -49.4(3) . . . . ? O9 C17 C18 O8 57.6(3) . . . . ? C18 O8 C19 C20 -175.3(3) . . . . ? Tb1 O8 C19 C20 48.2(4) . . . . ? C21 O7 C20 C19 -162.8(3) . . . . ? Tb1 O7 C20 C19 41.7(4) . . . . ? O8 C19 C20 O7 -56.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.665 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.063 #===end data_dg34 _database_code_CSD 171879 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H42 F38 K2 Nd2 O18' _chemical_formula_weight 2007.51 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 '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 13.1362(9) _cell_length_b 13.3292(9) _cell_length_c 22.1816(14) _cell_angle_alpha 90.7270(10) _cell_angle_beta 91.9570(10) _cell_angle_gamma 110.7140(10) _cell_volume 3629.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour lt_purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.688 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6680 _exptl_absorpt_correction_T_max 0.8104 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% '< 1.0' _diffrn_reflns_number 39261 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 28.29 _reflns_number_total 17150 _reflns_number_gt 13659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0431P)^2^+17.7849P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXTL _refine_ls_extinction_coef 0.00011(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 17150 _refine_ls_number_parameters 977 _refine_ls_number_restraints 396 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.377 _refine_ls_shift/su_mean 0.007 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 Nd1 Nd 0.88201(2) 0.87890(2) 0.467940(11) 0.02324(8) Uani 1 1 d . . . K1 K 0.86965(11) 1.17107(13) 0.42241(9) 0.0638(5) Uani 1 1 d . . . O1 O 0.8966(3) 0.7531(3) 0.54513(17) 0.0316(8) Uani 1 1 d . . . O2 O 0.7440(3) 0.8551(3) 0.54261(18) 0.0356(8) Uani 1 1 d . . . O3 O 0.7264(3) 0.7258(3) 0.4306(2) 0.0402(9) Uani 1 1 d . . . O4 O 0.7437(3) 0.9423(3) 0.42016(16) 0.0307(8) Uani 1 1 d . . . O5 O 0.9584(3) 0.9789(3) 0.37699(16) 0.0350(8) Uani 1 1 d . . . O6 O 0.9504(3) 0.7694(3) 0.4040(2) 0.0403(9) Uani 1 1 d . . . O7 O 0.8331(5) 1.2820(6) 0.3217(4) 0.095(2) Uani 1 1 d . . . O8 O 0.7475(5) 1.3045(4) 0.4346(3) 0.0812(19) Uani 1 1 d . . . O9 O 0.7818(4) 1.1906(4) 0.5320(2) 0.0547(12) Uani 1 1 d . . . C32 C 0.6544(5) 0.8504(4) -0.0607(2) 0.0356(12) Uani 1 1 d D . . F32 F 0.6779(3) 0.9503(3) -0.0397(2) 0.0549(10) Uani 1 1 d D . . F33 F 0.6451(3) 0.8515(3) -0.12057(15) 0.0520(9) Uani 1 1 d D . . F34 F 0.7408(3) 0.8226(3) -0.04694(16) 0.0433(8) Uani 1 1 d D . . C1 C 0.8608(5) 0.6017(5) 0.6052(3) 0.0452(15) Uani 1 1 d D . . F1 F 0.9350(5) 0.5807(5) 0.5748(3) 0.114(3) Uani 1 1 d D . . F2 F 0.7814(3) 0.5093(3) 0.6096(2) 0.0676(12) Uani 1 1 d D . . F3 F 0.9036(7) 0.6314(4) 0.6595(3) 0.133(3) Uani 1 1 d D . . C2 C 0.8261(4) 0.6894(4) 0.5768(2) 0.0310(11) Uani 1 1 d . . . C3 C 0.7238(4) 0.6912(4) 0.5901(2) 0.0341(12) Uani 1 1 d . . . H3A H 0.6746 0.6332 0.6108 0.041 Uiso 1 1 calc R . . C4 C 0.6929(4) 0.7763(4) 0.5734(2) 0.0310(11) Uani 1 1 d . . . C5 C 0.5835(5) 0.7791(5) 0.5938(3) 0.0430(14) Uani 1 1 d D . . F4 F 0.6000(4) 0.8624(4) 0.6318(2) 0.0759(14) Uani 1 1 d D . . F5 F 0.5249(4) 0.7932(5) 0.5478(2) 0.0892(19) Uani 1 1 d D . . F6 F 0.5243(3) 0.6931(3) 0.62285(19) 0.0566(10) Uani 1 1 d D . . C6 C 0.5635(5) 0.5932(5) 0.3987(3) 0.0580(19) Uani 1 1 d D . . F7 F 0.6047(5) 0.5511(4) 0.3554(3) 0.0981(19) Uani 1 1 d D . . F8 F 0.5672(5) 0.5341(4) 0.4450(3) 0.106(2) Uani 1 1 d D . . F9 F 0.4633(4) 0.5749(4) 0.3800(3) 0.104(2) Uani 1 1 d D . . C7 C 0.6323(4) 0.7111(5) 0.4107(3) 0.0369(12) Uani 1 1 d . . . C8 C 0.5864(4) 0.7877(5) 0.3973(2) 0.0335(12) Uani 1 1 d . . . H8A H 0.5119 0.7648 0.3841 0.040 Uiso 1 1 calc R . . C9 C 0.6468(4) 0.8977(4) 0.4026(2) 0.0301(11) Uani 1 1 d . . . C10 C 0.5882(5) 0.9753(5) 0.3882(3) 0.0473(15) Uani 1 1 d D . . F10 F 0.5636(4) 1.0149(4) 0.4392(2) 0.0807(15) Uani 1 1 d D . . F11 F 0.6515(3) 1.0585(4) 0.3587(2) 0.0784(16) Uani 1 1 d D . . F12 F 0.4955(3) 0.9323(3) 0.3557(2) 0.0598(11) Uani 1 1 d D . . C11 C 1.0361(7) 1.0517(6) 0.2871(3) 0.064(2) Uani 1 1 d D . . F13 F 1.1277(10) 1.0566(11) 0.2592(6) 0.100(4) Uiso 0.50 1 d PD A 1 F14 F 1.0399(7) 1.1461(6) 0.3096(4) 0.0521(19) Uiso 0.50 1 d PD A 1 F15 F 0.9654(10) 1.0327(10) 0.2414(5) 0.091(4) Uiso 0.50 1 d PD A 1 F13B F 1.0781(10) 1.0353(9) 0.2383(5) 0.078(3) Uiso 0.50 1 d P A 2 F14B F 1.0908(9) 1.1399(9) 0.3121(5) 0.074(3) Uiso 0.50 1 d P A 2 F15B F 0.9345(12) 1.0549(12) 0.2574(7) 0.104(4) Uiso 0.50 1 d P A 2 C12 C 1.0026(5) 0.9588(5) 0.3322(3) 0.0408(13) Uani 1 1 d . A . C13 C 1.0222(6) 0.8666(6) 0.3169(3) 0.0519(17) Uani 1 1 d . . . H13A H 1.0560 0.8628 0.2802 0.062 Uiso 1 1 calc R A . C14 C 0.9926(5) 0.7790(5) 0.3547(3) 0.0473(16) Uani 1 1 d . A . C15 C 1.0099(6) 0.6738(7) 0.3343(4) 0.081(3) Uani 1 1 d D . . F16 F 1.1102(8) 0.6959(10) 0.3171(6) 0.098(3) Uiso 0.50 1 d PD A 1 F17 F 1.0243(7) 0.6141(7) 0.3848(4) 0.059(2) Uiso 0.50 1 d PD A 1 F18 F 0.9112(7) 0.6024(7) 0.3155(4) 0.047(2) Uiso 0.50 1 d PD A 1 F16B F 1.0508(7) 0.6894(7) 0.2732(4) 0.064(2) Uiso 0.50 1 d P A 2 F17B F 1.0716(12) 0.6514(11) 0.3614(7) 0.100(4) Uiso 0.50 1 d P A 2 F18B F 0.9451(16) 0.6119(16) 0.3081(9) 0.126(7) Uiso 0.50 1 d P A 2 C16 C 0.8529(13) 1.2631(11) 0.2640(6) 0.131(5) Uani 1 1 d . . . H16A H 0.8323 1.3115 0.2374 0.197 Uiso 1 1 calc R . . H16B H 0.8102 1.1885 0.2522 0.197 Uiso 1 1 calc R . . H16C H 0.9306 1.2756 0.2607 0.197 Uiso 1 1 calc R . . C17 C 0.7611(9) 1.3393(8) 0.3322(6) 0.093(4) Uani 1 1 d . . . H17A H 0.7760 1.3979 0.3030 0.111 Uiso 1 1 calc R . . H17B H 0.6853 1.2899 0.3241 0.111 Uiso 1 1 calc R . . C18 C 0.7699(8) 1.3840(8) 0.3913(6) 0.094(3) Uani 1 1 d . . . H18A H 0.8445 1.4364 0.3992 0.112 Uiso 1 1 calc R . . H18B H 0.7183 1.4226 0.3946 0.112 Uiso 1 1 calc R . . C19 C 0.7514(8) 1.3436(7) 0.4936(5) 0.084(3) Uani 1 1 d . . . H19A H 0.7070 1.3899 0.4955 0.100 Uiso 1 1 calc R . . H19B H 0.8275 1.3877 0.5058 0.100 Uiso 1 1 calc R . . C20 C 0.7085(7) 1.2518(8) 0.5370(4) 0.072(2) Uani 1 1 d . . . H20A H 0.7108 1.2797 0.5788 0.086 Uiso 1 1 calc R . . H20B H 0.6325 1.2063 0.5254 0.086 Uiso 1 1 calc R . . C21 C 0.7402(7) 1.1029(7) 0.5711(4) 0.069(2) Uani 1 1 d . . . H21A H 0.7128 1.1267 0.6071 0.103 Uiso 1 1 calc R . . H21B H 0.7983 1.0763 0.5831 0.103 Uiso 1 1 calc R . . H21C H 0.6807 1.0453 0.5500 0.103 Uiso 1 1 calc R . . F19 F 1.0649(2) 0.9443(2) 0.49947(13) 0.0279(6) Uani 1 1 d . . . Nd2 Nd 0.44363(2) 0.56199(2) 0.062979(11) 0.02264(8) Uani 1 1 d . . . K2 K 0.76766(9) 0.68705(10) 0.05660(5) 0.0339(3) Uani 1 1 d . . . O11 O 0.2642(3) 0.4206(3) 0.06473(16) 0.0303(8) Uani 1 1 d . . . O12 O 0.4404(3) 0.4313(3) 0.14055(17) 0.0350(8) Uani 1 1 d . . . O13 O 0.3659(3) 0.6179(3) 0.14906(16) 0.0329(8) Uani 1 1 d . . . O14 O 0.5918(3) 0.6710(3) 0.13476(15) 0.0294(7) Uani 1 1 d . . . O15 O 0.5670(3) 0.7163(3) 0.00803(16) 0.0285(7) Uani 1 1 d . . . O16 O 0.3415(3) 0.6631(3) 0.01760(17) 0.0339(8) Uani 1 1 d . . . O17 O 0.7915(4) 0.5203(4) 0.1239(2) 0.0534(12) Uani 1 1 d . . . O18 O 0.9655(4) 0.7136(5) 0.1154(2) 0.0602(13) Uani 1 1 d . . . O19 O 0.9342(4) 0.8937(4) 0.0658(2) 0.0540(12) Uani 1 1 d . . . C22 C 0.0898(5) 0.3294(5) 0.0969(3) 0.0505(16) Uani 1 1 d D . . F20 F 0.0338(4) 0.2658(6) 0.1386(2) 0.116(3) Uani 1 1 d D . . F21 F 0.0543(4) 0.4092(4) 0.0917(3) 0.110(2) Uani 1 1 d D . . F22 F 0.0618(3) 0.2725(4) 0.0457(2) 0.0704(13) Uani 1 1 d D . . C23 C 0.2132(4) 0.3707(4) 0.1085(2) 0.0339(12) Uani 1 1 d . . . C24 C 0.2541(5) 0.3471(5) 0.1622(2) 0.0383(13) Uani 1 1 d . . . H24A H 0.2054 0.3100 0.1919 0.046 Uiso 1 1 calc R . . C25 C 0.3659(5) 0.3768(4) 0.1736(2) 0.0367(12) Uani 1 1 d . . . C26 C 0.4066(6) 0.3420(5) 0.2325(3) 0.0531(18) Uani 1 1 d D . . F23 F 0.3314(4) 0.2618(4) 0.2581(2) 0.0891(17) Uani 1 1 d D . . F24 F 0.4859(5) 0.3060(6) 0.2241(2) 0.106(2) Uani 1 1 d D . . F25 F 0.4401(7) 0.4215(4) 0.2706(2) 0.141(3) Uani 1 1 d D . . C27 C 0.3085(5) 0.6620(5) 0.2410(3) 0.0457(15) Uani 1 1 d D . . F26 F 0.3428(3) 0.7222(4) 0.29029(18) 0.0737(15) Uani 1 1 d D . . F27 F 0.2542(5) 0.5636(4) 0.2573(2) 0.096(2) Uani 1 1 d D . . F28 F 0.2368(4) 0.6951(5) 0.2125(2) 0.0804(16) Uani 1 1 d D . . C28 C 0.4001(4) 0.6620(4) 0.1995(2) 0.0322(11) Uani 1 1 d . . . C29 C 0.5073(5) 0.7083(5) 0.2214(2) 0.0354(12) Uani 1 1 d . . . H29A H 0.5215 0.7394 0.2610 0.043 Uiso 1 1 calc R . . C30 C 0.5941(4) 0.7101(4) 0.1867(2) 0.0302(11) Uani 1 1 d . . . C31 C 0.7099(5) 0.7644(5) 0.2153(2) 0.0422(14) Uani 1 1 d D . . F29 F 0.7466(5) 0.6927(4) 0.2367(3) 0.114(2) Uani 1 1 d D . . F30 F 0.7787(3) 0.8150(5) 0.1748(2) 0.0908(19) Uani 1 1 d D . . F31 F 0.7169(3) 0.8338(4) 0.2589(2) 0.0799(16) Uani 1 1 d D . . C33 C 0.5505(4) 0.7738(4) -0.0326(2) 0.0276(10) Uani 1 1 d . . . C34 C 0.4528(4) 0.7813(4) -0.0534(2) 0.0329(11) Uani 1 1 d . . . H34A H 0.4518 0.8234 -0.0875 0.039 Uiso 1 1 calc R . . C35 C 0.3555(4) 0.7274(4) -0.0248(2) 0.0314(11) Uani 1 1 d . . . C36 C 0.2539(5) 0.7524(5) -0.0445(3) 0.0436(14) Uani 1 1 d D . . F35 F 0.1632(3) 0.6719(3) -0.0341(2) 0.0678(13) Uani 1 1 d D . . F36 F 0.2499(4) 0.7717(4) -0.10299(19) 0.0733(13) Uani 1 1 d D . . F37 F 0.2515(4) 0.8377(4) -0.0146(2) 0.0722(13) Uani 1 1 d D . . C37 C 0.7096(7) 0.4573(7) 0.1607(4) 0.067(2) Uani 1 1 d . . . H37A H 0.7335 0.4035 0.1803 0.101 Uiso 1 1 calc R . . H37B H 0.6430 0.4211 0.1359 0.101 Uiso 1 1 calc R . . H37C H 0.6949 0.5031 0.1915 0.101 Uiso 1 1 calc R . . C38 C 0.8969(6) 0.5360(7) 0.1494(4) 0.063(2) Uani 1 1 d . . . H38A H 0.9083 0.4665 0.1505 0.076 Uiso 1 1 calc R . . H38B H 0.9031 0.5647 0.1912 0.076 Uiso 1 1 calc R . . C39 C 0.9809(7) 0.6121(8) 0.1128(4) 0.071(2) Uani 1 1 d . . . H39A H 1.0546 0.6202 0.1292 0.085 Uiso 1 1 calc R . . H39B H 0.9736 0.5851 0.0705 0.085 Uiso 1 1 calc R . . C40 C 1.0515(6) 0.7985(8) 0.0929(4) 0.071(2) Uani 1 1 d . . . H40A H 1.0599 0.7840 0.0499 0.085 Uiso 1 1 calc R . . H40B H 1.1201 0.8052 0.1154 0.085 Uiso 1 1 calc R . . C41 C 1.0304(6) 0.8995(7) 0.0992(4) 0.071(3) Uani 1 1 d . . . H41A H 1.0226 0.9141 0.1423 0.085 Uiso 1 1 calc R . . H41B H 1.0931 0.9594 0.0846 0.085 Uiso 1 1 calc R . . C42 C 0.9128(8) 0.9907(6) 0.0691(4) 0.071(2) Uani 1 1 d . . . H42A H 0.9819 1.0517 0.0718 0.107 Uiso 1 1 calc R . . H42B H 0.8714 0.9910 0.1050 0.107 Uiso 1 1 calc R . . H42C H 0.8705 0.9964 0.0329 0.107 Uiso 1 1 calc R . . C43 C 0.4235(8) 0.9686(7) 0.1936(3) 0.064(2) Uani 1 1 d . . . C44 C 0.4078(7) 0.9095(6) 0.1407(3) 0.0565(18) Uani 1 1 d . . . H44A H 0.3356 0.8709 0.1259 0.068 Uiso 1 1 calc R . . C45 C 0.4932(7) 0.9045(6) 0.1088(4) 0.0611(19) Uani 1 1 d . . . H45A H 0.4791 0.8633 0.0721 0.073 Uiso 1 1 calc R . . C46 C 0.5968(8) 0.9570(8) 0.1282(5) 0.082(3) Uani 1 1 d . . . H46A H 0.6556 0.9523 0.1061 0.098 Uiso 1 1 calc R . . C47 C 0.6159(10) 1.0172(9) 0.1805(6) 0.107(4) Uani 1 1 d . . . H47A H 0.6887 1.0555 0.1945 0.129 Uiso 1 1 calc R . . C48 C 0.5292(11) 1.0229(8) 0.2133(4) 0.095(4) Uani 1 1 d . . . H48A H 0.5435 1.0647 0.2497 0.114 Uiso 1 1 calc R . . C49 C 0.3279(11) 0.9737(10) 0.2286(5) 0.107(4) Uani 1 1 d . . . H49A H 0.2596 0.9313 0.2069 0.160 Uiso 1 1 calc R . . H49B H 0.3324 1.0484 0.2326 0.160 Uiso 1 1 calc R . . H49C H 0.3301 0.9446 0.2688 0.160 Uiso 1 1 calc R . . F38 F 0.5870(2) 0.5108(2) 0.03532(12) 0.0291(6) 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 Nd1 0.02088(13) 0.02040(13) 0.02680(14) 0.00264(10) -0.00087(10) 0.00540(10) K1 0.0341(7) 0.0474(8) 0.1014(13) 0.0409(9) -0.0150(8) 0.0043(6) O1 0.0259(17) 0.0300(19) 0.037(2) 0.0100(15) 0.0022(15) 0.0076(15) O2 0.034(2) 0.034(2) 0.039(2) 0.0114(16) 0.0077(16) 0.0116(16) O3 0.034(2) 0.0283(19) 0.053(3) -0.0047(17) -0.0092(18) 0.0064(16) O4 0.0250(17) 0.0297(18) 0.0355(19) 0.0038(15) -0.0050(15) 0.0078(14) O5 0.041(2) 0.035(2) 0.0291(19) 0.0025(16) 0.0076(16) 0.0133(17) O6 0.041(2) 0.030(2) 0.053(3) -0.0056(18) 0.0042(19) 0.0155(17) O7 0.065(4) 0.116(6) 0.115(6) 0.074(5) 0.018(4) 0.043(4) O8 0.096(5) 0.041(3) 0.104(5) 0.013(3) -0.033(4) 0.024(3) O9 0.042(2) 0.046(3) 0.076(3) 0.009(2) -0.009(2) 0.017(2) C32 0.039(3) 0.030(3) 0.040(3) 0.007(2) 0.010(2) 0.015(2) F32 0.049(2) 0.0271(17) 0.083(3) 0.0015(17) 0.016(2) 0.0050(15) F33 0.056(2) 0.065(2) 0.0362(18) 0.0213(17) 0.0158(17) 0.0218(19) F34 0.0321(17) 0.046(2) 0.053(2) 0.0170(16) 0.0134(15) 0.0138(15) C1 0.039(3) 0.034(3) 0.059(4) 0.020(3) 0.002(3) 0.009(3) F1 0.097(4) 0.109(4) 0.181(6) 0.099(4) 0.080(4) 0.082(4) F2 0.055(2) 0.036(2) 0.110(4) 0.028(2) 0.010(2) 0.0122(18) F3 0.206(7) 0.070(3) 0.125(5) -0.010(3) -0.113(5) 0.063(4) C2 0.029(2) 0.026(2) 0.035(3) 0.008(2) -0.004(2) 0.005(2) C3 0.027(2) 0.035(3) 0.034(3) 0.013(2) 0.002(2) 0.003(2) C4 0.025(2) 0.036(3) 0.031(3) 0.005(2) 0.002(2) 0.009(2) C5 0.039(3) 0.055(4) 0.037(3) 0.016(3) 0.011(3) 0.019(3) F4 0.078(3) 0.062(3) 0.093(4) 0.002(3) 0.044(3) 0.028(2) F5 0.048(2) 0.178(6) 0.059(3) 0.052(3) 0.016(2) 0.060(3) F6 0.0352(18) 0.059(2) 0.074(3) 0.025(2) 0.0236(18) 0.0125(17) C6 0.051(4) 0.035(3) 0.071(5) -0.006(3) -0.015(4) -0.003(3) F7 0.096(4) 0.055(3) 0.129(5) -0.045(3) -0.014(4) 0.013(3) F8 0.122(5) 0.046(3) 0.104(4) 0.015(3) -0.020(4) -0.026(3) F9 0.043(2) 0.050(3) 0.199(7) -0.027(3) -0.034(3) -0.005(2) C7 0.031(3) 0.034(3) 0.036(3) -0.007(2) -0.005(2) 0.001(2) C8 0.024(2) 0.040(3) 0.032(3) -0.007(2) -0.004(2) 0.006(2) C9 0.026(2) 0.039(3) 0.025(2) 0.001(2) -0.0016(19) 0.012(2) C10 0.034(3) 0.051(4) 0.056(4) 0.010(3) -0.012(3) 0.016(3) F10 0.092(4) 0.099(4) 0.079(3) -0.022(3) -0.013(3) 0.071(3) F11 0.048(2) 0.060(3) 0.119(4) 0.046(3) -0.019(2) 0.009(2) F12 0.0332(18) 0.068(3) 0.075(3) 0.015(2) -0.0181(18) 0.0158(18) C11 0.083(6) 0.062(5) 0.031(3) -0.002(3) 0.026(4) 0.004(4) C12 0.034(3) 0.046(3) 0.034(3) -0.004(3) 0.005(2) 0.004(3) C13 0.050(4) 0.050(4) 0.051(4) -0.014(3) 0.023(3) 0.009(3) C14 0.030(3) 0.042(3) 0.067(4) -0.020(3) 0.006(3) 0.010(3) C15 0.047(4) 0.083(6) 0.107(8) -0.052(6) 0.011(5) 0.016(4) C16 0.171(14) 0.127(11) 0.113(10) -0.022(9) -0.072(10) 0.082(10) C17 0.097(7) 0.059(5) 0.125(9) 0.012(5) -0.055(7) 0.035(5) C18 0.071(6) 0.075(6) 0.142(10) 0.047(7) 0.016(6) 0.033(5) C19 0.075(6) 0.054(5) 0.121(9) -0.001(5) -0.025(6) 0.025(4) C20 0.071(5) 0.082(6) 0.073(5) -0.010(5) -0.002(4) 0.042(5) C21 0.071(5) 0.067(5) 0.067(5) 0.001(4) 0.025(4) 0.020(4) F19 0.0232(13) 0.0275(14) 0.0315(15) 0.0010(12) -0.0009(11) 0.0076(11) Nd2 0.02205(13) 0.02494(14) 0.01964(13) 0.00008(9) 0.00298(9) 0.00656(10) K2 0.0237(5) 0.0432(7) 0.0307(6) -0.0023(5) -0.0004(4) 0.0069(5) O11 0.0268(17) 0.0333(19) 0.0268(18) -0.0007(15) 0.0026(14) 0.0058(15) O12 0.034(2) 0.038(2) 0.0320(19) 0.0083(16) 0.0011(16) 0.0102(16) O13 0.0285(18) 0.040(2) 0.0273(18) -0.0064(16) 0.0036(15) 0.0090(16) O14 0.0275(17) 0.0346(19) 0.0244(17) -0.0041(14) 0.0022(14) 0.0089(15) O15 0.0255(17) 0.0294(18) 0.0291(18) 0.0058(14) 0.0010(14) 0.0075(14) O16 0.0297(19) 0.037(2) 0.037(2) 0.0021(16) 0.0040(16) 0.0147(16) O17 0.052(3) 0.065(3) 0.051(3) 0.004(2) -0.011(2) 0.031(2) O18 0.037(2) 0.080(4) 0.063(3) -0.003(3) 0.000(2) 0.021(2) O19 0.044(2) 0.048(3) 0.056(3) -0.007(2) 0.003(2) 0.000(2) C22 0.031(3) 0.057(4) 0.053(4) -0.007(3) 0.008(3) 0.002(3) F20 0.042(3) 0.180(6) 0.077(3) 0.030(4) 0.021(2) -0.023(3) F21 0.036(2) 0.088(4) 0.212(7) -0.042(4) -0.003(3) 0.031(3) F22 0.039(2) 0.083(3) 0.072(3) -0.024(2) -0.009(2) 0.003(2) C23 0.030(3) 0.032(3) 0.035(3) -0.007(2) 0.008(2) 0.005(2) C24 0.043(3) 0.034(3) 0.030(3) 0.001(2) 0.010(2) 0.002(2) C25 0.047(3) 0.032(3) 0.027(3) 0.005(2) 0.004(2) 0.008(2) C26 0.062(4) 0.047(4) 0.040(3) 0.015(3) -0.010(3) 0.007(3) F23 0.094(4) 0.090(4) 0.061(3) 0.052(3) 0.000(3) 0.003(3) F24 0.091(4) 0.171(6) 0.074(3) 0.064(4) 0.004(3) 0.068(4) F25 0.270(9) 0.057(3) 0.055(3) -0.005(2) -0.075(4) 0.013(4) C27 0.038(3) 0.062(4) 0.035(3) -0.007(3) 0.011(3) 0.015(3) F26 0.051(2) 0.119(4) 0.046(2) -0.039(2) 0.0083(18) 0.025(2) F27 0.104(4) 0.075(3) 0.096(4) 0.007(3) 0.075(3) 0.006(3) F28 0.050(2) 0.149(5) 0.058(3) -0.016(3) 0.007(2) 0.057(3) C28 0.036(3) 0.030(3) 0.031(3) 0.001(2) 0.008(2) 0.011(2) C29 0.038(3) 0.039(3) 0.025(2) -0.003(2) 0.004(2) 0.009(2) C30 0.034(3) 0.029(3) 0.026(2) -0.001(2) 0.000(2) 0.008(2) C31 0.033(3) 0.061(4) 0.030(3) -0.007(3) 0.000(2) 0.014(3) F29 0.078(4) 0.083(4) 0.176(6) -0.007(4) -0.077(4) 0.031(3) F30 0.041(2) 0.137(5) 0.052(3) -0.019(3) 0.0072(19) -0.020(3) F31 0.045(2) 0.108(4) 0.067(3) -0.053(3) -0.007(2) 0.005(2) C33 0.030(2) 0.025(2) 0.030(2) 0.0026(19) 0.005(2) 0.011(2) C34 0.037(3) 0.035(3) 0.030(3) 0.004(2) 0.001(2) 0.017(2) C35 0.034(3) 0.031(3) 0.032(3) -0.001(2) -0.002(2) 0.015(2) C36 0.037(3) 0.051(4) 0.050(4) 0.003(3) -0.002(3) 0.024(3) F35 0.0310(19) 0.062(3) 0.108(4) 0.016(2) -0.010(2) 0.0148(18) F36 0.062(3) 0.116(4) 0.060(3) 0.019(3) -0.009(2) 0.053(3) F37 0.058(3) 0.068(3) 0.106(4) -0.022(3) -0.012(2) 0.044(2) C37 0.066(5) 0.063(5) 0.084(6) 0.024(4) 0.000(4) 0.036(4) C38 0.056(4) 0.089(6) 0.058(4) 0.008(4) -0.003(4) 0.043(4) C39 0.053(4) 0.091(6) 0.082(6) -0.001(5) -0.002(4) 0.044(5) C40 0.031(3) 0.103(7) 0.068(5) -0.006(5) -0.002(3) 0.011(4) C41 0.043(4) 0.081(6) 0.056(4) -0.008(4) -0.003(3) -0.018(4) C42 0.091(6) 0.043(4) 0.064(5) -0.004(4) 0.016(4) 0.005(4) C43 0.105(7) 0.059(5) 0.042(4) 0.013(3) 0.011(4) 0.045(5) C44 0.069(5) 0.064(5) 0.044(4) -0.005(3) -0.006(3) 0.033(4) C45 0.079(5) 0.057(4) 0.052(4) 0.001(3) 0.009(4) 0.029(4) C46 0.074(6) 0.084(7) 0.089(7) 0.029(6) 0.009(5) 0.028(5) C47 0.088(8) 0.095(8) 0.098(8) 0.038(7) -0.032(7) -0.017(6) C48 0.134(10) 0.061(6) 0.055(5) 0.000(4) -0.019(6) -0.006(6) C49 0.168(12) 0.122(9) 0.076(6) 0.035(6) 0.057(7) 0.102(9) F38 0.0291(14) 0.0344(16) 0.0238(14) -0.0024(12) 0.0014(11) 0.0112(12) _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 Nd1 F19 2.307(3) 2_776 ? Nd1 F19 2.326(3) . ? Nd1 O6 2.431(4) . ? Nd1 O3 2.433(4) . ? Nd1 O2 2.438(4) . ? Nd1 O1 2.461(4) . ? Nd1 O5 2.473(4) . ? Nd1 O4 2.474(3) . ? K1 F19 2.647(3) 2_776 ? K1 O9 2.774(6) . ? K1 O8 2.801(7) . ? K1 O7 2.814(6) . ? K1 O4 2.908(4) . ? K1 O1 2.933(4) 2_776 ? K1 F11 3.015(4) . ? O1 C2 1.255(6) . ? O1 K1 2.933(4) 2_776 ? O2 C4 1.253(6) . ? O3 C7 1.246(7) . ? O4 C9 1.245(6) . ? O5 C12 1.241(7) . ? O6 C14 1.231(8) . ? O7 C16 1.352(14) . ? O7 C17 1.433(12) . ? O8 C19 1.396(12) . ? O8 C18 1.397(11) . ? O9 C21 1.422(9) . ? O9 C20 1.472(9) . ? C32 F32 1.330(6) . ? C32 F33 1.330(6) . ? C32 F34 1.340(6) . ? C32 C33 1.544(7) . ? F34 K2 3.027(4) . ? C1 F3 1.306(7) . ? C1 F2 1.310(6) . ? C1 F1 1.311(7) . ? C1 C2 1.532(8) . ? F1 K1 3.394(7) 2_776 ? C2 C3 1.394(8) . ? C3 C4 1.385(8) . ? C4 C5 1.533(8) . ? C5 F5 1.312(7) . ? C5 F6 1.325(6) . ? C5 F4 1.335(7) . ? C6 F9 1.303(7) . ? C6 F8 1.311(8) . ? C6 F7 1.330(8) . ? C6 C7 1.525(8) . ? C7 C8 1.388(8) . ? C8 C9 1.400(8) . ? C9 C10 1.522(8) . ? C10 F11 1.324(7) . ? C10 F12 1.329(6) . ? C10 F10 1.338(7) . ? C11 F14B 1.250(12) . ? C11 F13B 1.283(12) . ? C11 F15 1.310(11) . ? C11 F14 1.330(9) . ? C11 F13 1.354(11) . ? C11 F15B 1.482(17) . ? C11 C12 1.550(9) . ? C12 C13 1.383(9) . ? C13 C14 1.395(10) . ? C14 C15 1.562(10) . ? C15 F18B 1.095(19) . ? C15 F17B 1.118(15) . ? C15 F16 1.316(10) . ? C15 F18 1.356(10) . ? C15 F17 1.429(11) . ? C15 F16B 1.464(13) . ? C17 C18 1.418(15) . ? C19 C20 1.524(13) . ? F19 Nd1 2.307(3) 2_776 ? F19 K1 2.647(3) 2_776 ? Nd2 F38 2.316(3) . ? Nd2 F38 2.338(3) 2_665 ? Nd2 O16 2.419(4) . ? Nd2 O13 2.425(3) . ? Nd2 O11 2.444(3) . ? Nd2 O12 2.455(4) . ? Nd2 O14 2.482(3) . ? Nd2 O15 2.486(3) . ? K2 F38 2.707(3) . ? K2 O18 2.772(5) . ? K2 O17 2.795(5) . ? K2 O19 2.847(5) . ? K2 O14 2.885(4) . ? K2 O15 2.967(4) . ? K2 O11 2.979(4) 2_665 ? O11 C23 1.257(6) . ? O11 K2 2.979(4) 2_665 ? O12 C25 1.257(7) . ? O13 C28 1.248(6) . ? O14 C30 1.254(6) . ? O15 C33 1.252(6) . ? O16 C35 1.255(7) . ? O17 C37 1.402(9) . ? O17 C38 1.420(8) . ? O18 C40 1.398(10) . ? O18 C39 1.437(10) . ? O19 C42 1.418(10) . ? O19 C41 1.421(9) . ? C22 F21 1.309(8) . ? C22 F20 1.320(7) . ? C22 F22 1.324(7) . ? C22 C23 1.527(8) . ? F22 K2 3.159(5) 2_665 ? C23 C24 1.376(8) . ? C24 C25 1.392(8) . ? C25 C26 1.532(8) . ? C26 F25 1.285(7) . ? C26 F24 1.309(8) . ? C26 F23 1.322(7) . ? C27 F27 1.315(7) . ? C27 F26 1.316(6) . ? C27 F28 1.320(7) . ? C27 C28 1.540(8) . ? C28 C29 1.389(8) . ? C29 C30 1.390(8) . ? C30 C31 1.544(8) . ? C31 F29 1.301(7) . ? C31 F31 1.306(6) . ? C31 F30 1.312(7) . ? C33 C34 1.386(7) . ? C34 C35 1.403(8) . ? C35 C36 1.536(8) . ? C36 F37 1.319(7) . ? C36 F35 1.321(7) . ? C36 F36 1.330(7) . ? C38 C39 1.481(12) . ? C40 C41 1.472(13) . ? C43 C48 1.372(14) . ? C43 C44 1.373(10) . ? C43 C49 1.519(13) . ? C44 C45 1.368(11) . ? C45 C46 1.344(13) . ? C46 C47 1.364(16) . ? C47 C48 1.397(17) . ? F38 Nd2 2.338(3) 2_665 ? 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 F19 Nd1 F19 69.12(12) 2_776 . ? F19 Nd1 O6 137.90(12) 2_776 . ? F19 Nd1 O6 80.02(12) . . ? F19 Nd1 O3 143.52(12) 2_776 . ? F19 Nd1 O3 147.26(12) . . ? O6 Nd1 O3 72.42(14) . . ? F19 Nd1 O2 82.49(12) 2_776 . ? F19 Nd1 O2 119.06(12) . . ? O6 Nd1 O2 138.85(13) . . ? O3 Nd1 O2 74.87(14) . . ? F19 Nd1 O1 115.08(11) 2_776 . ? F19 Nd1 O1 75.71(11) . . ? O6 Nd1 O1 82.49(14) . . ? O3 Nd1 O1 83.37(13) . . ? O2 Nd1 O1 69.48(12) . . ? F19 Nd1 O5 76.93(11) 2_776 . ? F19 Nd1 O5 81.29(12) . . ? O6 Nd1 O5 70.51(14) . . ? O3 Nd1 O5 105.08(14) . . ? O2 Nd1 O5 143.29(13) . . ? O1 Nd1 O5 147.11(13) . . ? F19 Nd1 O4 76.21(11) 2_776 . ? F19 Nd1 O4 139.79(11) . . ? O6 Nd1 O4 115.94(13) . . ? O3 Nd1 O4 70.38(13) . . ? O2 Nd1 O4 74.36(13) . . ? O1 Nd1 O4 139.71(12) . . ? O5 Nd1 O4 71.40(13) . . ? F19 K1 O9 72.95(12) 2_776 . ? F19 K1 O8 132.48(18) 2_776 . ? O9 K1 O8 59.62(18) . . ? F19 K1 O7 166.70(19) 2_776 . ? O9 K1 O7 120.2(2) . . ? O8 K1 O7 60.6(2) . . ? F19 K1 O4 64.01(9) 2_776 . ? O9 K1 O4 89.05(13) . . ? O8 K1 O4 115.02(15) . . ? O7 K1 O4 115.1(2) . . ? F19 K1 O1 63.33(10) 2_776 2_776 ? O9 K1 O1 101.77(13) . 2_776 ? O8 K1 O1 121.59(16) . 2_776 ? O7 K1 O1 109.54(16) . 2_776 ? O4 K1 O1 119.65(11) . 2_776 ? F19 K1 F11 115.92(11) 2_776 . ? O9 K1 F11 94.35(15) . . ? O8 K1 F11 72.88(16) . . ? O7 K1 F11 67.12(17) . . ? O4 K1 F11 52.98(11) . . ? O1 K1 F11 162.40(16) 2_776 . ? C2 O1 Nd1 131.3(3) . . ? C2 O1 K1 122.8(3) . 2_776 ? Nd1 O1 K1 103.54(12) . 2_776 ? C4 O2 Nd1 131.8(4) . . ? C7 O3 Nd1 136.0(4) . . ? C9 O4 Nd1 134.2(3) . . ? C9 O4 K1 127.0(3) . . ? Nd1 O4 K1 98.68(11) . . ? C12 O5 Nd1 134.1(4) . . ? C12 O5 K1 137.2(4) . . ? Nd1 O5 K1 88.53(11) . . ? C14 O6 Nd1 135.9(4) . . ? C16 O7 C17 118.4(8) . . ? C16 O7 K1 125.3(7) . . ? C17 O7 K1 113.9(6) . . ? C19 O8 C18 113.7(8) . . ? C19 O8 K1 112.6(5) . . ? C18 O8 K1 113.0(6) . . ? C21 O9 C20 105.2(6) . . ? C21 O9 K1 122.5(4) . . ? C20 O9 K1 120.5(5) . . ? F32 C32 F33 107.9(5) . . ? F32 C32 F34 106.9(5) . . ? F33 C32 F34 107.1(4) . . ? F32 C32 C33 110.7(4) . . ? F33 C32 C33 112.6(4) . . ? F34 C32 C33 111.4(4) . . ? C32 F34 K2 127.4(3) . . ? F3 C1 F2 107.2(6) . . ? F3 C1 F1 106.1(7) . . ? F2 C1 F1 105.3(6) . . ? F3 C1 C2 110.7(5) . . ? F2 C1 C2 114.3(5) . . ? F1 C1 C2 112.7(5) . . ? C1 F1 K1 99.5(4) . 2_776 ? O1 C2 C3 128.1(5) . . ? O1 C2 C1 114.4(5) . . ? C3 C2 C1 117.4(5) . . ? C4 C3 C2 120.9(5) . . ? O2 C4 C3 127.9(5) . . ? O2 C4 C5 113.3(5) . . ? C3 C4 C5 118.8(5) . . ? F5 C5 F6 108.8(5) . . ? F5 C5 F4 106.1(6) . . ? F6 C5 F4 105.9(5) . . ? F5 C5 C4 110.9(5) . . ? F6 C5 C4 114.6(5) . . ? F4 C5 C4 110.1(5) . . ? F9 C6 F8 111.1(7) . . ? F9 C6 F7 104.5(6) . . ? F8 C6 F7 102.5(7) . . ? F9 C6 C7 115.0(6) . . ? F8 C6 C7 111.9(5) . . ? F7 C6 C7 110.9(6) . . ? O3 C7 C8 128.1(5) . . ? O3 C7 C6 113.5(5) . . ? C8 C7 C6 118.4(5) . . ? C7 C8 C9 121.8(5) . . ? O4 C9 C8 128.2(5) . . ? O4 C9 C10 114.0(5) . . ? C8 C9 C10 117.8(5) . . ? F11 C10 F12 107.6(5) . . ? F11 C10 F10 106.4(6) . . ? F12 C10 F10 106.7(5) . . ? F11 C10 C9 110.9(5) . . ? F12 C10 C9 114.5(5) . . ? F10 C10 C9 110.3(5) . . ? C10 F11 K1 113.2(3) . . ? F14B C11 F13B 112.0(9) . . ? F14B C11 F15 128.4(10) . . ? F13B C11 F15 69.2(8) . . ? F14B C11 F14 31.4(5) . . ? F13B C11 F14 126.6(8) . . ? F15 C11 F14 103.9(9) . . ? F14B C11 F13 87.2(9) . . ? F13B C11 F13 33.0(6) . . ? F15 C11 F13 101.5(9) . . ? F14 C11 F13 113.3(9) . . ? F14B C11 F15B 111.5(10) . . ? F13B C11 F15B 95.5(9) . . ? F15 C11 F15B 27.6(7) . . ? F14 C11 F15B 81.7(8) . . ? F13 C11 F15B 126.1(10) . . ? F14B C11 C12 112.6(7) . . ? F13B C11 C12 116.7(8) . . ? F15 C11 C12 111.2(8) . . ? F14 C11 C12 114.9(6) . . ? F13 C11 C12 111.0(9) . . ? F15B C11 C12 107.2(8) . . ? O5 C12 C13 129.6(6) . . ? O5 C12 C11 112.9(6) . . ? C13 C12 C11 117.5(6) . . ? C12 C13 C14 120.7(6) . . ? O6 C14 C13 129.2(6) . . ? O6 C14 C15 111.5(7) . . ? C13 C14 C15 119.3(6) . . ? F18B C15 F17B 119.8(16) . . ? F18B C15 F16 117.1(13) . . ? F17B C15 F16 57.8(9) . . ? F18B C15 F18 17.6(12) . . ? F17B C15 F18 123.5(12) . . ? F16 C15 F18 134.6(9) . . ? F18B C15 F17 101.0(14) . . ? F17B C15 F17 36.2(8) . . ? F16 C15 F17 93.6(9) . . ? F18 C15 F17 95.8(8) . . ? F18B C15 F16B 77.9(12) . . ? F17B C15 F16B 105.0(10) . . ? F16 C15 F16B 51.2(7) . . ? F18 C15 F16B 93.5(8) . . ? F17 C15 F16B 134.8(8) . . ? F18B C15 C14 119.7(13) . . ? F17B C15 C14 116.2(10) . . ? F16 C15 C14 110.1(8) . . ? F18 C15 C14 107.4(7) . . ? F17 C15 C14 111.4(7) . . ? F16B C15 C14 107.6(8) . . ? C18 C17 O7 114.6(8) . . ? O8 C18 C17 111.3(9) . . ? O8 C19 C20 110.9(7) . . ? O9 C20 C19 104.9(7) . . ? Nd1 F19 Nd1 110.88(12) 2_776 . ? Nd1 F19 K1 111.22(11) 2_776 2_776 ? Nd1 F19 K1 117.14(11) . 2_776 ? F38 Nd2 F38 69.51(11) . 2_665 ? F38 Nd2 O16 135.72(11) . . ? F38 Nd2 O16 79.10(12) 2_665 . ? F38 Nd2 O13 142.70(11) . . ? F38 Nd2 O13 146.46(11) 2_665 . ? O16 Nd2 O13 76.96(13) . . ? F38 Nd2 O11 116.83(11) . . ? F38 Nd2 O11 75.94(11) 2_665 . ? O16 Nd2 O11 83.13(13) . . ? O13 Nd2 O11 78.16(12) . . ? F38 Nd2 O12 78.92(12) . . ? F38 Nd2 O12 113.77(12) 2_665 . ? O16 Nd2 O12 144.00(13) . . ? O13 Nd2 O12 75.40(13) . . ? O11 Nd2 O12 68.99(12) . . ? F38 Nd2 O14 78.35(11) . . ? F38 Nd2 O14 141.82(11) 2_665 . ? O16 Nd2 O14 113.15(13) . . ? O13 Nd2 O14 70.32(12) . . ? O11 Nd2 O14 139.18(11) . . ? O12 Nd2 O14 78.29(12) . . ? F38 Nd2 O15 74.54(11) . . ? F38 Nd2 O15 80.04(11) 2_665 . ? O16 Nd2 O15 69.82(12) . . ? O13 Nd2 O15 112.62(12) . . ? O11 Nd2 O15 146.69(12) . . ? O12 Nd2 O15 143.21(12) . . ? O14 Nd2 O15 71.81(11) . . ? F38 K2 O18 131.46(14) . . ? F38 K2 O17 72.10(12) . . ? O18 K2 O17 60.10(16) . . ? F38 K2 O19 168.61(13) . . ? O18 K2 O19 59.92(16) . . ? O17 K2 O19 119.16(15) . . ? F38 K2 O14 65.63(9) . . ? O18 K2 O14 115.09(13) . . ? O17 K2 O14 85.02(13) . . ? O19 K2 O14 111.77(13) . . ? F38 K2 O15 61.55(9) . . ? O18 K2 O15 164.71(14) . . ? O17 K2 O15 129.79(13) . . ? O19 K2 O15 107.29(13) . . ? O14 K2 O15 59.70(10) . . ? F38 K2 O11 62.14(9) . 2_665 ? O18 K2 O11 114.61(13) . 2_665 ? O17 K2 O11 97.81(13) . 2_665 ? O19 K2 O11 115.09(12) . 2_665 ? O14 K2 O11 123.61(10) . 2_665 ? O15 K2 O11 77.58(10) . 2_665 ? C23 O11 Nd2 130.0(3) . . ? C23 O11 K2 119.9(3) . 2_665 ? Nd2 O11 K2 104.57(12) . 2_665 ? C25 O12 Nd2 131.5(4) . . ? C28 O13 Nd2 136.4(3) . . ? C30 O14 Nd2 134.1(3) . . ? C30 O14 K2 130.0(3) . . ? Nd2 O14 K2 95.85(11) . . ? C33 O15 Nd2 132.8(3) . . ? C33 O15 K2 132.5(3) . . ? Nd2 O15 K2 93.73(11) . . ? C35 O16 Nd2 135.5(3) . . ? C37 O17 C38 111.5(6) . . ? C37 O17 K2 122.0(4) . . ? C38 O17 K2 117.1(5) . . ? C40 O18 C39 114.0(6) . . ? C40 O18 K2 112.5(5) . . ? C39 O18 K2 107.7(4) . . ? C42 O19 C41 112.8(6) . . ? C42 O19 K2 123.5(5) . . ? C41 O19 K2 115.6(5) . . ? F21 C22 F20 107.8(6) . . ? F21 C22 F22 106.7(6) . . ? F20 C22 F22 105.4(6) . . ? F21 C22 C23 110.9(5) . . ? F20 C22 C23 114.7(6) . . ? F22 C22 C23 111.0(5) . . ? C22 F22 K2 119.5(3) . 2_665 ? O11 C23 C24 128.6(5) . . ? O11 C23 C22 112.8(5) . . ? C24 C23 C22 118.5(5) . . ? C23 C24 C25 121.0(5) . . ? O12 C25 C24 127.0(5) . . ? O12 C25 C26 114.4(5) . . ? C24 C25 C26 118.6(5) . . ? F25 C26 F24 108.8(7) . . ? F25 C26 F23 108.1(6) . . ? F24 C26 F23 104.0(6) . . ? F25 C26 C25 110.0(6) . . ? F24 C26 C25 112.3(6) . . ? F23 C26 C25 113.4(5) . . ? F27 C27 F26 107.9(5) . . ? F27 C27 F28 105.9(6) . . ? F26 C27 F28 107.4(5) . . ? F27 C27 C28 109.8(5) . . ? F26 C27 C28 114.2(5) . . ? F28 C27 C28 111.3(5) . . ? O13 C28 C29 128.3(5) . . ? O13 C28 C27 113.4(5) . . ? C29 C28 C27 118.3(5) . . ? C28 C29 C30 121.5(5) . . ? O14 C30 C29 128.6(5) . . ? O14 C30 C31 114.1(5) . . ? C29 C30 C31 117.2(5) . . ? F29 C31 F31 107.8(6) . . ? F29 C31 F30 105.7(6) . . ? F31 C31 F30 107.2(5) . . ? F29 C31 C30 110.4(5) . . ? F31 C31 C30 114.3(5) . . ? F30 C31 C30 111.0(5) . . ? C31 F30 K2 115.5(4) . . ? O15 C33 C34 128.9(5) . . ? O15 C33 C32 114.8(4) . . ? C34 C33 C32 116.2(5) . . ? C33 C34 C35 120.8(5) . . ? O16 C35 C34 127.6(5) . . ? O16 C35 C36 114.5(5) . . ? C34 C35 C36 117.8(5) . . ? F37 C36 F35 107.7(5) . . ? F37 C36 F36 107.4(5) . . ? F35 C36 F36 106.3(5) . . ? F37 C36 C35 110.4(5) . . ? F35 C36 C35 111.8(5) . . ? F36 C36 C35 112.9(5) . . ? O17 C38 C39 110.0(6) . . ? O18 C39 C38 107.9(6) . . ? O18 C39 K2 49.2(3) . . ? C38 C39 K2 84.9(4) . . ? O18 C40 C41 110.2(7) . . ? O19 C41 C40 111.0(6) . . ? C48 C43 C44 117.0(9) . . ? C48 C43 C49 121.6(9) . . ? C44 C43 C49 121.4(9) . . ? C45 C44 C43 121.9(8) . . ? C46 C45 C44 121.2(8) . . ? C45 C46 C47 118.8(10) . . ? C46 C47 C48 120.5(10) . . ? C43 C48 C47 120.7(9) . . ? Nd2 F38 Nd2 110.49(11) . 2_665 ? Nd2 F38 K2 105.03(11) . . ? Nd2 F38 K2 116.87(11) 2_665 . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 3.642 _refine_diff_density_min -2.764 _refine_diff_density_rms 0.133 #===end data_maj33 _database_code_CSD 171880 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H73 Eu F12 O13 Zr2' _chemical_formula_weight 1372.42 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' 'Zr' 'Zr' -2.9673 0.5597 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.6625(9) _cell_length_b 21.3117(11) _cell_length_c 16.4412(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.9110(10) _cell_angle_gamma 90.00 _cell_volume 5732.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 1.530 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6088 _exptl_absorpt_correction_T_max 0.6917 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% '< 1.0' _diffrn_reflns_number 18523 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6764 _reflns_number_gt 6083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0624P)^2^+38.1827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6764 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.0000 0.324876(12) 0.2500 0.02857(10) Uani 1 2 d S . . Zr1 Zr 0.00503(2) 0.181057(18) 0.35228(2) 0.02812(11) Uani 1 1 d . . . O1 O 0.1228(2) 0.36703(16) 0.2168(2) 0.0410(7) Uani 1 1 d . . . O2 O 0.0436(2) 0.41330(16) 0.3377(2) 0.0455(8) Uani 1 1 d . . . O3 O 0.07701(16) 0.22428(13) 0.26193(17) 0.0282(5) Uani 1 1 d . . . O4 O 0.00912(19) 0.27640(14) 0.38311(17) 0.0344(6) Uani 1 1 d . . . O5 O 0.0966(2) 0.15012(16) 0.43157(19) 0.0410(7) Uani 1 1 d . . . O6 O -0.0848(2) 0.15429(17) 0.4018(2) 0.0423(7) Uani 1 1 d . . . O7 O 0.0000 0.11494(19) 0.2500 0.0317(8) Uani 1 2 d S . . C1 C 0.0833(4) 0.5105(3) 0.3992(5) 0.0706(19) Uani 1 1 d . . . C2 C 0.0917(3) 0.4577(2) 0.3361(3) 0.0497(12) Uani 1 1 d . A . C3 C 0.1497(3) 0.4644(3) 0.2870(3) 0.0508(12) Uani 1 1 d . . . H3A H 0.1824 0.5012 0.2912 0.061 Uiso 1 1 calc R A . C4 C 0.1604(3) 0.4173(3) 0.2310(3) 0.0465(11) Uani 1 1 d . A . C5 C 0.2285(4) 0.4269(3) 0.1795(4) 0.0655(17) Uani 1 1 d . . . C6 C 0.1659(2) 0.2250(2) 0.2704(3) 0.0365(9) Uani 1 1 d . . . H6A H 0.1798 0.2453 0.2200 0.044 Uiso 1 1 calc R . . C7 C 0.2047(3) 0.2631(3) 0.3457(3) 0.0478(11) Uani 1 1 d . . . H7A H 0.1821 0.3057 0.3411 0.072 Uiso 1 1 calc R . . H7B H 0.2640 0.2650 0.3488 0.072 Uiso 1 1 calc R . . H7C H 0.1931 0.2431 0.3959 0.072 Uiso 1 1 calc R . . C8 C 0.2008(3) 0.1590(3) 0.2771(4) 0.0502(12) Uani 1 1 d . . . H8A H 0.1759 0.1347 0.2282 0.075 Uiso 1 1 calc R . . H8B H 0.1890 0.1388 0.3270 0.075 Uiso 1 1 calc R . . H8C H 0.2601 0.1610 0.2804 0.075 Uiso 1 1 calc R . . C9 C 0.0072(4) 0.2955(4) 0.4666(4) 0.074(2) Uani 1 1 d . . . H9A H -0.0011 0.2548 0.4943 0.089 Uiso 1 1 calc R . . C10 C 0.0896(4) 0.3159(3) 0.5116(4) 0.0623(16) Uani 1 1 d . . . H10A H 0.0862 0.3280 0.5683 0.093 Uiso 1 1 calc R . . H10B H 0.1082 0.3518 0.4829 0.093 Uiso 1 1 calc R . . H10C H 0.1285 0.2812 0.5130 0.093 Uiso 1 1 calc R . . C11 C -0.0600(5) 0.3302(4) 0.4779(5) 0.086(3) Uani 1 1 d . . . H11A H -0.1097 0.3116 0.4456 0.129 Uiso 1 1 calc R . . H11B H -0.0543 0.3734 0.4593 0.129 Uiso 1 1 calc R . . H11C H -0.0634 0.3303 0.5367 0.129 Uiso 1 1 calc R . . C12 C 0.1562(4) 0.1328(3) 0.5019(3) 0.0565(14) Uani 1 1 d . . . H12A H 0.1978 0.1671 0.5117 0.068 Uiso 1 1 calc R . . C13 C 0.1173(5) 0.1293(4) 0.5770(4) 0.080(2) Uani 1 1 d . . . H13A H 0.0906 0.1693 0.5842 0.120 Uiso 1 1 calc R . . H13B H 0.1593 0.1207 0.6260 0.120 Uiso 1 1 calc R . . H13C H 0.0765 0.0956 0.5698 0.120 Uiso 1 1 calc R . . C14 C 0.1994(6) 0.0745(4) 0.4855(5) 0.110(4) Uani 1 1 d . . . H14A H 0.2236 0.0803 0.4362 0.165 Uiso 1 1 calc R . . H14B H 0.1604 0.0395 0.4764 0.165 Uiso 1 1 calc R . . H14C H 0.2426 0.0651 0.5333 0.165 Uiso 1 1 calc R . . C15 C -0.1454(4) 0.1289(3) 0.4428(4) 0.0673(17) Uani 1 1 d . . . H15A H -0.1757 0.0975 0.4032 0.081 Uiso 1 1 calc R . . C16 C -0.2072(5) 0.1775(3) 0.4528(6) 0.080(2) Uani 1 1 d . . . H16A H -0.2278 0.1973 0.3991 0.120 Uiso 1 1 calc R . . H16B H -0.1817 0.2093 0.4924 0.120 Uiso 1 1 calc R . . H16C H -0.2526 0.1577 0.4733 0.120 Uiso 1 1 calc R . . C17 C -0.1114(6) 0.0937(4) 0.5148(7) 0.118(4) Uani 1 1 d . . . H17A H -0.0726 0.0629 0.5008 0.178 Uiso 1 1 calc R . . H17B H -0.1552 0.0720 0.5357 0.178 Uiso 1 1 calc R . . H17C H -0.0829 0.1222 0.5576 0.178 Uiso 1 1 calc R . . C18 C 0.0254(6) 0.0499(4) 0.2621(7) 0.045(2) Uani 0.50 1 d P . . C19 C 0.0111(6) 0.0177(3) 0.1782(4) 0.073(2) Uani 1 1 d . . . F1 F 0.1008(7) 0.4827(5) 0.4792(6) 0.080(3) Uiso 0.62(2) 1 d P A 1 F2 F 0.0076(5) 0.5305(4) 0.3902(7) 0.078(3) Uiso 0.62(2) 1 d P A 1 F3 F 0.1469(5) 0.5496(4) 0.4121(6) 0.073(3) Uiso 0.62(2) 1 d P A 1 F1A F 0.0748(11) 0.4947(7) 0.4669(9) 0.074(4) Uiso 0.38(2) 1 d P A 2 F2A F 0.0138(8) 0.5460(7) 0.3615(10) 0.075(4) Uiso 0.38(2) 1 d P A 2 F3A F 0.1219(9) 0.5642(7) 0.3802(10) 0.075(4) Uiso 0.38(2) 1 d P A 2 F4 F 0.1987(6) 0.4552(6) 0.1111(6) 0.096(3) Uiso 0.577(15) 1 d P A 1 F5 F 0.2920(5) 0.4578(4) 0.2186(5) 0.068(2) Uiso 0.577(15) 1 d P A 1 F6 F 0.2629(5) 0.3686(4) 0.1644(6) 0.080(3) Uiso 0.577(15) 1 d P A 1 F4A F 0.2012(5) 0.4245(5) 0.0999(6) 0.060(3) Uiso 0.423(15) 1 d P A 2 F5A F 0.2627(10) 0.4855(8) 0.1918(10) 0.112(5) Uiso 0.423(15) 1 d P A 2 F6A F 0.2828(9) 0.3855(7) 0.1991(11) 0.102(4) Uiso 0.423(15) 1 d P A 2 C20 C -0.0390(7) 0.8202(5) 0.2352(8) 0.117(4) Uiso 1 1 d . . . C21 C -0.0863(10) 0.7617(9) 0.2161(10) 0.157(5) Uiso 1 1 d . . . C22 C -0.0683(14) 0.7148(12) 0.2193(14) 0.101(6) Uiso 0.50 1 d P . . C23 C -0.0206(11) 0.7057(8) 0.2455(15) 0.086(5) Uiso 0.50 1 d P . . C24 C -0.0627(19) 0.6538(15) 0.233(2) 0.152(10) Uiso 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 0.02998(16) 0.02719(16) 0.02936(17) 0.000 0.00772(11) 0.000 Zr1 0.0295(2) 0.0325(2) 0.0224(2) 0.00291(13) 0.00514(15) 0.00065(13) O1 0.0398(17) 0.0428(17) 0.0433(18) -0.0050(14) 0.0153(14) -0.0060(14) O2 0.0491(19) 0.0416(18) 0.0481(19) -0.0112(14) 0.0153(15) -0.0098(15) O3 0.0262(13) 0.0319(14) 0.0267(13) -0.0005(10) 0.0054(10) -0.0013(10) O4 0.0414(16) 0.0370(15) 0.0255(14) -0.0044(11) 0.0082(12) 0.0007(12) O5 0.0428(17) 0.0472(18) 0.0299(15) 0.0068(13) -0.0013(13) 0.0064(14) O6 0.0447(18) 0.0465(18) 0.0402(17) 0.0049(14) 0.0194(14) -0.0020(15) O7 0.034(2) 0.0289(19) 0.032(2) 0.000 0.0074(16) 0.000 C1 0.072(4) 0.049(3) 0.092(5) -0.025(3) 0.018(4) -0.013(3) C2 0.055(3) 0.041(2) 0.050(3) -0.008(2) 0.003(2) -0.003(2) C3 0.054(3) 0.044(3) 0.053(3) 0.001(2) 0.006(2) -0.013(2) C4 0.042(2) 0.051(3) 0.046(3) 0.004(2) 0.007(2) -0.006(2) C5 0.056(3) 0.080(4) 0.059(4) 0.019(3) 0.006(3) -0.026(3) C6 0.0254(19) 0.048(2) 0.036(2) 0.0003(18) 0.0065(16) 0.0006(17) C7 0.038(2) 0.063(3) 0.040(2) -0.003(2) -0.0006(19) -0.007(2) C8 0.037(2) 0.061(3) 0.054(3) 0.001(2) 0.010(2) 0.011(2) C9 0.049(3) 0.137(6) 0.037(3) -0.044(4) 0.008(2) -0.002(4) C10 0.072(4) 0.073(4) 0.039(3) -0.015(3) 0.002(3) 0.001(3) C11 0.086(5) 0.118(7) 0.058(4) -0.037(4) 0.023(4) 0.011(4) C12 0.059(3) 0.061(3) 0.042(3) 0.010(2) -0.007(2) 0.003(3) C13 0.084(5) 0.112(6) 0.042(3) 0.029(4) 0.004(3) -0.003(4) C14 0.133(8) 0.109(7) 0.073(5) 0.017(5) -0.017(5) 0.070(6) C15 0.065(4) 0.073(4) 0.076(4) 0.020(3) 0.044(3) 0.004(3) C16 0.077(5) 0.085(5) 0.095(6) 0.022(4) 0.058(5) 0.024(4) C17 0.127(7) 0.109(7) 0.151(9) 0.085(7) 0.106(7) 0.054(6) C18 0.058(7) 0.029(4) 0.052(7) 0.003(4) 0.018(6) 0.006(3) C19 0.140(7) 0.030(2) 0.052(3) -0.009(2) 0.027(4) 0.000(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 O1 2.390(3) 2 ? Eu1 O1 2.390(3) . ? Eu1 O4 2.399(3) 2 ? Eu1 O4 2.399(3) . ? Eu1 O2 2.400(3) . ? Eu1 O2 2.400(3) 2 ? Eu1 O3 2.487(3) 2 ? Eu1 O3 2.487(3) . ? Eu1 Zr1 3.4894(5) 2 ? Eu1 Zr1 3.4894(5) . ? Zr1 O6 1.921(3) . ? Zr1 O5 1.926(3) . ? Zr1 O4 2.092(3) . ? Zr1 O7 2.183(3) . ? Zr1 O3 2.273(3) . ? Zr1 O3 2.296(3) 2 ? Zr1 Zr1 3.3355(8) 2 ? O1 C4 1.241(6) . ? O2 C2 1.243(6) . ? O3 C6 1.462(5) . ? O3 Zr1 2.296(3) 2 ? O4 C9 1.439(6) . ? O5 C12 1.423(6) . ? O6 C15 1.423(6) . ? O7 C18 1.451(9) 2 ? O7 C18 1.451(9) . ? O7 Zr1 2.183(3) 2 ? C1 F1A 1.196(15) . ? C1 F2 1.313(10) . ? C1 F3 1.334(9) . ? C1 F3A 1.377(14) . ? C1 F1 1.422(13) . ? C1 F2A 1.424(15) . ? C1 C2 1.556(8) . ? C2 C3 1.380(8) . ? C3 C4 1.396(8) . ? C4 C5 1.552(8) . ? C5 F6A 1.262(15) . ? C5 F4 1.290(11) . ? C5 F4A 1.303(11) . ? C5 F5 1.307(9) . ? C5 F5A 1.371(16) . ? C5 F6 1.411(12) . ? C6 C8 1.517(7) . ? C6 C7 1.519(6) . ? C9 C11 1.382(10) . ? C9 C10 1.496(9) . ? C12 C14 1.486(10) . ? C12 C13 1.501(9) . ? C15 C17 1.425(11) . ? C15 C16 1.490(9) . ? C18 C18 0.86(2) 2 ? C18 C19 1.425(13) 2 ? C18 C19 1.518(13) . ? C19 C18 1.425(13) 2 ? C20 C20 1.30(2) 2 ? C20 C21 1.476(18) . ? C21 C22 1.04(2) . ? C21 C23 1.63(2) . ? C22 C23 0.85(2) . ? C22 C24 1.32(4) . ? C22 C23 1.50(3) 2 ? C23 C23 0.67(4) 2 ? C23 C24 1.31(3) . ? C23 C22 1.50(3) 2 ? C23 C24 1.76(3) 2 ? C24 C23 1.76(3) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Eu1 O1 135.83(16) 2 . ? O1 Eu1 O4 117.45(11) 2 2 ? O1 Eu1 O4 82.12(11) . 2 ? O1 Eu1 O4 82.12(11) 2 . ? O1 Eu1 O4 117.45(11) . . ? O4 Eu1 O4 128.97(14) 2 . ? O1 Eu1 O2 75.08(12) 2 . ? O1 Eu1 O2 70.56(11) . . ? O4 Eu1 O2 147.77(11) 2 . ? O4 Eu1 O2 80.24(11) . . ? O1 Eu1 O2 70.56(11) 2 2 ? O1 Eu1 O2 75.08(12) . 2 ? O4 Eu1 O2 80.24(11) 2 2 ? O4 Eu1 O2 147.77(11) . 2 ? O2 Eu1 O2 76.54(18) . 2 ? O1 Eu1 O3 83.74(10) 2 2 ? O1 Eu1 O3 139.22(10) . 2 ? O4 Eu1 O3 67.30(9) 2 2 ? O4 Eu1 O3 69.10(9) . 2 ? O2 Eu1 O3 144.79(10) . 2 ? O2 Eu1 O3 122.44(11) 2 2 ? O1 Eu1 O3 139.22(10) 2 . ? O1 Eu1 O3 83.74(10) . . ? O4 Eu1 O3 69.10(9) 2 . ? O4 Eu1 O3 67.30(9) . . ? O2 Eu1 O3 122.44(11) . . ? O2 Eu1 O3 144.79(10) 2 . ? O3 Eu1 O3 60.92(12) 2 . ? O1 Eu1 Zr1 119.78(8) 2 2 ? O1 Eu1 Zr1 99.43(8) . 2 ? O4 Eu1 Zr1 35.94(7) 2 2 ? O4 Eu1 Zr1 93.03(7) . 2 ? O2 Eu1 Zr1 162.95(9) . 2 ? O2 Eu1 Zr1 115.04(9) 2 2 ? O3 Eu1 Zr1 40.52(6) 2 2 ? O3 Eu1 Zr1 41.05(6) . 2 ? O1 Eu1 Zr1 99.43(8) 2 . ? O1 Eu1 Zr1 119.78(8) . . ? O4 Eu1 Zr1 93.03(7) 2 . ? O4 Eu1 Zr1 35.94(7) . . ? O2 Eu1 Zr1 115.04(9) . . ? O2 Eu1 Zr1 162.95(9) 2 . ? O3 Eu1 Zr1 41.05(6) 2 . ? O3 Eu1 Zr1 40.52(6) . . ? Zr1 Eu1 Zr1 57.103(14) 2 . ? O6 Zr1 O5 101.10(15) . . ? O6 Zr1 O4 100.25(14) . . ? O5 Zr1 O4 100.56(13) . . ? O6 Zr1 O7 102.44(12) . . ? O5 Zr1 O7 102.14(12) . . ? O4 Zr1 O7 143.91(11) . . ? O6 Zr1 O3 161.28(13) . . ? O5 Zr1 O3 97.62(12) . . ? O4 Zr1 O3 76.58(11) . . ? O7 Zr1 O3 72.92(9) . . ? O6 Zr1 O3 94.29(13) . 2 ? O5 Zr1 O3 164.51(12) . 2 ? O4 Zr1 O3 78.20(11) . 2 ? O7 Zr1 O3 72.47(9) . 2 ? O3 Zr1 O3 66.99(12) . 2 ? O6 Zr1 Zr1 122.21(11) . 2 ? O5 Zr1 Zr1 124.38(10) . 2 ? O4 Zr1 Zr1 103.73(8) . 2 ? O7 Zr1 Zr1 40.19(8) . 2 ? O3 Zr1 Zr1 43.38(7) . 2 ? O3 Zr1 Zr1 42.85(7) 2 2 ? O6 Zr1 Eu1 121.03(11) . . ? O5 Zr1 Eu1 124.79(11) . . ? O4 Zr1 Eu1 42.30(8) . . ? O7 Zr1 Eu1 101.64(8) . . ? O3 Zr1 Eu1 45.31(7) . . ? O3 Zr1 Eu1 45.35(7) 2 . ? Zr1 Zr1 Eu1 61.449(7) 2 . ? C4 O1 Eu1 134.9(3) . . ? C2 O2 Eu1 135.0(3) . . ? C6 O3 Zr1 126.4(2) . . ? C6 O3 Zr1 121.2(2) . 2 ? Zr1 O3 Zr1 93.77(10) . 2 ? C6 O3 Eu1 119.8(2) . . ? Zr1 O3 Eu1 94.16(9) . . ? Zr1 O3 Eu1 93.60(9) 2 . ? C9 O4 Zr1 120.0(4) . . ? C9 O4 Eu1 137.7(4) . . ? Zr1 O4 Eu1 101.75(11) . . ? C12 O5 Zr1 168.7(4) . . ? C15 O6 Zr1 173.5(4) . . ? C18 O7 C18 34.6(8) 2 . ? C18 O7 Zr1 133.6(5) 2 . ? C18 O7 Zr1 122.9(5) . . ? C18 O7 Zr1 122.9(5) 2 2 ? C18 O7 Zr1 133.6(5) . 2 ? Zr1 O7 Zr1 99.61(16) . 2 ? F1A C1 F2 85.2(10) . . ? F1A C1 F3 105.0(11) . . ? F2 C1 F3 122.1(8) . . ? F1A C1 F3A 125.9(11) . . ? F2 C1 F3A 100.6(11) . . ? F3 C1 F3A 28.9(6) . . ? F1A C1 F1 20.3(8) . . ? F2 C1 F1 105.4(8) . . ? F3 C1 F1 95.5(8) . . ? F3A C1 F1 122.2(10) . . ? F1A C1 F2A 109.0(11) . . ? F2 C1 F2A 25.0(6) . . ? F3 C1 F2A 107.0(10) . . ? F3A C1 F2A 80.5(13) . . ? F1 C1 F2A 129.3(9) . . ? F1A C1 C2 117.3(9) . . ? F2 C1 C2 111.5(6) . . ? F3 C1 C2 112.9(6) . . ? F3A C1 C2 110.2(8) . . ? F1 C1 C2 106.6(6) . . ? F2A C1 C2 105.2(7) . . ? O2 C2 C3 128.2(5) . . ? O2 C2 C1 113.3(5) . . ? C3 C2 C1 118.5(5) . . ? C2 C3 C4 120.1(5) . . ? O1 C4 C3 128.5(5) . . ? O1 C4 C5 114.0(5) . . ? C3 C4 C5 117.5(5) . . ? F6A C5 F4 133.6(10) . . ? F6A C5 F4A 109.0(10) . . ? F4 C5 F4A 30.5(5) . . ? F6A C5 F5 75.6(9) . . ? F4 C5 F5 109.6(7) . . ? F4A C5 F5 127.5(7) . . ? F6A C5 F5A 109.9(11) . . ? F4 C5 F5A 77.5(8) . . ? F4A C5 F5A 103.8(9) . . ? F5 C5 F5A 36.3(7) . . ? F6A C5 F6 29.8(7) . . ? F4 C5 F6 111.2(8) . . ? F4A C5 F6 82.2(7) . . ? F5 C5 F6 102.2(7) . . ? F5A C5 F6 131.0(9) . . ? F6A C5 C4 109.4(8) . . ? F4 C5 C4 109.7(7) . . ? F4A C5 C4 113.0(6) . . ? F5 C5 C4 113.9(6) . . ? F5A C5 C4 111.5(9) . . ? F6 C5 C4 110.1(6) . . ? O3 C6 C8 111.4(4) . . ? O3 C6 C7 110.5(4) . . ? C8 C6 C7 109.7(4) . . ? C11 C9 O4 116.4(6) . . ? C11 C9 C10 118.0(6) . . ? O4 C9 C10 111.7(5) . . ? O5 C12 C14 111.0(5) . . ? O5 C12 C13 109.7(5) . . ? C14 C12 C13 114.0(7) . . ? O6 C15 C17 112.8(6) . . ? O6 C15 C16 110.8(5) . . ? C17 C15 C16 116.6(6) . . ? C18 C18 C19 79.0(14) 2 2 ? C18 C18 O7 72.7(4) 2 . ? C19 C18 O7 113.8(8) 2 . ? C18 C18 C19 67.1(13) 2 . ? C19 C18 C19 113.2(8) 2 . ? O7 C18 C19 108.5(7) . . ? C18 C19 C18 33.9(8) 2 . ? C20 C20 C21 122.4(8) 2 . ? C22 C21 C20 131(2) . . ? C22 C21 C23 27.4(15) . . ? C20 C21 C23 104.6(12) . . ? C23 C22 C21 118(3) . . ? C23 C22 C24 70(2) . . ? C21 C22 C24 165(3) . . ? C23 C22 C23 10(2) . 2 ? C21 C22 C23 113(2) . 2 ? C24 C22 C23 77.0(19) . 2 ? C23 C23 C22 158(5) 2 . ? C23 C23 C24 122.0(16) 2 . ? C22 C23 C24 72(2) . . ? C23 C23 C22 13(3) 2 2 ? C22 C23 C22 158(3) . 2 ? C24 C23 C22 129(2) . 2 ? C23 C23 C21 131.6(13) 2 . ? C22 C23 C21 34.3(19) . . ? C24 C23 C21 105.2(19) . . ? C22 C23 C21 125.5(17) 2 . ? C23 C23 C24 39.1(12) 2 2 ? C22 C23 C24 150(3) . 2 ? C24 C23 C24 83(3) . 2 ? C22 C23 C24 47.0(13) 2 2 ? C21 C23 C24 168.8(18) . 2 ? C23 C24 C22 37.8(14) . . ? C23 C24 C23 18.9(12) . 2 ? C22 C24 C23 56.0(17) . 2 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.458 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.131 #===end data_mg43 _database_code_CSD 171881 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 Eu F18 O9' _chemical_formula_weight 907.31 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 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 9.7264(5) _cell_length_b 15.5649(7) _cell_length_c 20.5469(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.5190(10) _cell_angle_gamma 90.00 _cell_volume 3024.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.993 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 2.231 _exptl_absorpt_correction_type 'Semi-empirical via SADABS' _exptl_absorpt_correction_T_min 0.4105 _exptl_absorpt_correction_T_max 0.4920 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 19148 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7178 _reflns_number_gt 6794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _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^)+(0.0134P)^2^+2.8989P] 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 7178 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0211 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0454 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.689340(9) 0.688178(5) 0.124983(4) 0.01699(3) Uani 1 1 d . . . O1 O 0.94714(14) 0.73623(9) 0.14078(7) 0.0257(3) Uani 1 1 d . . . O2 O 0.86674(14) 0.56713(9) 0.13486(7) 0.0246(3) Uani 1 1 d . . . O3 O 0.58449(14) 0.54198(8) 0.08427(7) 0.0252(3) Uani 1 1 d . . . O4 O 0.74046(14) 0.66248(8) 0.01664(6) 0.0213(3) Uani 1 1 d . . . O5 O 0.70253(15) 0.82360(8) 0.06904(7) 0.0235(3) Uani 1 1 d . . . O6 O 0.45697(14) 0.71389(9) 0.06160(7) 0.0227(3) Uani 1 1 d . . . O7 O 0.59726(15) 0.80412(9) 0.17882(7) 0.0249(3) Uani 1 1 d . . . O8 O 0.54890(14) 0.62701(9) 0.19758(7) 0.0262(3) Uani 1 1 d . . . O9 O 0.82132(14) 0.68674(9) 0.23927(7) 0.0236(3) Uani 1 1 d . . . C1 C 0.9902(3) 0.81638(16) 0.17415(13) 0.0372(5) Uani 1 1 d . . . C2 C 1.0503(2) 0.67089(15) 0.16539(11) 0.0292(4) Uani 1 1 d . . . C3 C 1.0057(2) 0.58991(15) 0.12740(11) 0.0292(4) Uani 1 1 d . . . C4 C 0.8186(2) 0.48937(13) 0.09898(11) 0.0303(4) Uani 1 1 d . . . C5 C 0.6743(3) 0.46984(13) 0.10863(12) 0.0328(5) Uani 1 1 d . . . C6 C 0.4382(2) 0.51875(15) 0.07794(13) 0.0339(5) Uani 1 1 d . . . C7 C 0.8273(2) 0.65813(13) -0.08142(10) 0.0261(4) Uani 1 1 d . . . C8 C 0.78283(19) 0.70839(12) -0.02501(9) 0.0201(3) Uani 1 1 d . . . C9 C 0.7911(2) 0.79701(12) -0.02748(10) 0.0230(4) Uani 1 1 d . . . C10 C 0.74735(19) 0.84779(12) 0.01979(9) 0.0216(4) Uani 1 1 d . A . C11 C 0.7569(3) 0.94565(14) 0.01288(11) 0.0336(5) Uani 1 1 d . . . C12 C 0.2286(2) 0.76033(14) 0.00887(10) 0.0269(4) Uani 1 1 d . . . C13 C 0.36726(19) 0.77129(12) 0.06243(9) 0.0217(4) Uani 1 1 d . B . C14 C 0.3745(2) 0.83964(13) 0.10674(10) 0.0262(4) Uani 1 1 d . . . C15 C 0.4890(2) 0.84924(12) 0.16177(10) 0.0235(4) Uani 1 1 d . B . C16 C 0.4835(3) 0.92386(15) 0.21029(12) 0.0372(5) Uani 1 1 d . . . C17 C 0.4297(3) 0.5831(2) 0.27885(12) 0.0444(6) Uani 1 1 d . . . C18 C 0.5624(2) 0.61791(13) 0.25916(10) 0.0248(4) Uani 1 1 d . C . C19 C 0.6805(2) 0.63489(14) 0.31057(10) 0.0272(4) Uani 1 1 d . . . C20 C 0.80230(19) 0.66753(12) 0.29547(9) 0.0213(3) Uani 1 1 d . C . C21 C 0.9318(2) 0.68486(14) 0.35329(10) 0.0280(4) Uani 1 1 d . . . F1 F 0.87969(18) 0.58146(9) -0.06014(8) 0.0497(4) Uani 1 1 d . . . F2 F 0.71763(15) 0.64415(10) -0.13258(7) 0.0429(3) Uani 1 1 d . . . F3 F 0.92563(15) 0.69875(9) -0.10543(7) 0.0403(3) Uani 1 1 d . . . F4 F 0.8035(8) 0.9713(5) -0.0387(3) 0.076(3) Uani 0.56 1 d P A 1 F4' F 0.7465(13) 0.9700(6) -0.0463(4) 0.108(5) Uani 0.44 1 d P A 2 F5 F 0.8347(8) 0.9809(4) 0.0646(3) 0.082(3) Uani 0.56 1 d P A 1 F5' F 0.8850(10) 0.9691(6) 0.0449(6) 0.108(4) Uani 0.44 1 d P A 2 F6 F 0.6295(6) 0.9802(4) 0.0042(4) 0.081(2) Uani 0.56 1 d P A 1 F6' F 0.6782(11) 0.9878(5) 0.0404(6) 0.111(4) Uani 0.44 1 d P A 2 F7 F 0.2462(8) 0.7196(4) -0.0462(4) 0.0355(14) Uani 0.58 1 d P B 1 F7' F 0.2488(13) 0.7368(7) -0.0471(5) 0.063(3) Uani 0.42 1 d P B 2 F8 F 0.1680(8) 0.8352(4) -0.0135(3) 0.0397(10) Uani 0.58 1 d P B 1 F8' F 0.1444(13) 0.8256(8) 0.0026(6) 0.104(4) Uani 0.42 1 d P B 2 F9 F 0.1356(13) 0.7151(11) 0.0318(6) 0.052(2) Uani 0.58 1 d P B 1 F9' F 0.1576(17) 0.6957(15) 0.0288(9) 0.067(5) Uani 0.42 1 d P B 2 F10 F 0.3739(2) 0.97564(12) 0.19022(10) 0.0696(6) Uani 1 1 d . B . F11 F 0.5992(2) 0.97046(11) 0.22108(11) 0.0679(5) Uani 1 1 d . B . F12 F 0.4741(3) 0.89362(13) 0.26933(9) 0.0781(6) Uani 1 1 d . B . F13 F 0.3442(5) 0.5415(4) 0.2345(2) 0.0644(12) Uani 0.50 1 d P C 1 F13' F 0.4183(6) 0.4952(3) 0.2572(3) 0.0778(14) Uani 0.50 1 d P C 2 F14 F 0.4479(13) 0.5531(10) 0.3383(5) 0.091(4) Uani 0.50 1 d P C 1 F14' F 0.4413(13) 0.5765(9) 0.3424(4) 0.066(3) Uani 0.50 1 d P C 2 F15 F 0.3416(5) 0.6603(4) 0.2810(3) 0.0823(18) Uani 0.50 1 d P C 1 F15' F 0.3213(4) 0.6169(5) 0.2516(3) 0.083(2) Uani 0.50 1 d P C 2 F16 F 0.92584(15) 0.64545(10) 0.41003(6) 0.0430(3) Uani 1 1 d . C . F17 F 1.05036(14) 0.65984(12) 0.33703(7) 0.0473(4) Uani 1 1 d . C . F18 F 0.94392(15) 0.76872(9) 0.36610(7) 0.0413(3) Uani 1 1 d . C . H1A H 0.918(3) 0.857(2) 0.1606(15) 0.054(9) Uiso 1 1 d . . . H1B H 1.073(3) 0.8346(19) 0.1601(15) 0.052(8) Uiso 1 1 d . . . H1C H 1.012(4) 0.810(2) 0.2217(18) 0.064(10) Uiso 1 1 d . . . H2A H 1.062(2) 0.6639(15) 0.2125(12) 0.026(6) Uiso 1 1 d . . . H2B H 1.139(3) 0.6865(16) 0.1582(13) 0.035(7) Uiso 1 1 d . . . H3A H 1.004(2) 0.5965(15) 0.0823(12) 0.026(6) Uiso 1 1 d . . . H3B H 1.069(3) 0.5473(17) 0.1462(13) 0.034(6) Uiso 1 1 d . . . H4A H 0.819(2) 0.4958(15) 0.0520(12) 0.025(6) Uiso 1 1 d . . . H4B H 0.880(3) 0.4416(17) 0.1170(13) 0.038(7) Uiso 1 1 d . . . H5A H 0.637(3) 0.4194(17) 0.0822(13) 0.033(6) Uiso 1 1 d . . . H5B H 0.678(3) 0.4584(17) 0.1550(14) 0.040(7) Uiso 1 1 d . . . H6A H 0.428(3) 0.5003(17) 0.1212(14) 0.035(7) Uiso 1 1 d . . . H6B H 0.416(2) 0.4705(16) 0.0470(12) 0.028(6) Uiso 1 1 d . . . H6C H 0.387(3) 0.567(2) 0.0603(15) 0.054(9) Uiso 1 1 d . . . H9A H 0.822(3) 0.8211(15) -0.0596(13) 0.029(6) Uiso 1 1 d . . . H14A H 0.304(3) 0.8775(17) 0.1002(12) 0.034(6) Uiso 1 1 d . . . H19A H 0.680(3) 0.6195(17) 0.3537(14) 0.038(7) 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 0.01636(5) 0.01873(5) 0.01513(5) -0.00051(3) 0.00219(3) 0.00068(3) O1 0.0221(7) 0.0301(7) 0.0231(7) 0.0014(5) 0.0015(5) -0.0035(5) O2 0.0235(7) 0.0253(7) 0.0248(7) 0.0020(5) 0.0051(5) 0.0047(5) O3 0.0257(7) 0.0198(6) 0.0308(7) -0.0021(5) 0.0081(6) -0.0024(5) O4 0.0251(7) 0.0197(6) 0.0191(6) -0.0004(5) 0.0052(5) 0.0003(5) O5 0.0288(7) 0.0209(6) 0.0218(6) -0.0001(5) 0.0075(5) 0.0018(5) O6 0.0210(6) 0.0236(6) 0.0221(6) -0.0017(5) 0.0019(5) 0.0031(5) O7 0.0269(7) 0.0260(7) 0.0213(6) -0.0027(5) 0.0049(5) 0.0025(5) O8 0.0248(7) 0.0337(7) 0.0192(6) -0.0007(5) 0.0036(5) -0.0067(6) O9 0.0211(6) 0.0299(7) 0.0189(6) 0.0009(5) 0.0028(5) -0.0008(5) C1 0.0352(12) 0.0361(12) 0.0368(13) -0.0026(10) 0.0012(10) -0.0130(10) C2 0.0156(9) 0.0469(12) 0.0240(10) 0.0052(9) 0.0027(7) 0.0030(8) C3 0.0225(9) 0.0389(11) 0.0269(10) 0.0053(8) 0.0071(8) 0.0102(8) C4 0.0378(11) 0.0210(9) 0.0319(11) -0.0001(8) 0.0075(9) 0.0082(8) C5 0.0422(12) 0.0193(9) 0.0360(12) 0.0026(8) 0.0075(9) -0.0001(8) C6 0.0310(11) 0.0312(11) 0.0404(13) -0.0096(10) 0.0099(9) -0.0125(9) C7 0.0277(10) 0.0279(10) 0.0243(9) -0.0024(8) 0.0091(8) 0.0009(8) C8 0.0175(8) 0.0242(9) 0.0174(8) -0.0013(7) 0.0019(6) 0.0010(6) C9 0.0249(9) 0.0243(9) 0.0202(9) 0.0035(7) 0.0059(7) 0.0003(7) C10 0.0196(8) 0.0205(8) 0.0222(9) 0.0016(7) -0.0001(7) 0.0008(7) C11 0.0445(12) 0.0228(10) 0.0336(11) 0.0001(8) 0.0092(9) -0.0017(9) C12 0.0194(9) 0.0319(10) 0.0281(10) 0.0041(8) 0.0029(7) 0.0008(7) C13 0.0194(8) 0.0231(9) 0.0225(9) 0.0040(7) 0.0049(7) -0.0016(7) C14 0.0263(10) 0.0229(9) 0.0300(10) 0.0024(8) 0.0077(8) 0.0076(8) C15 0.0295(10) 0.0210(9) 0.0230(9) -0.0005(7) 0.0118(7) -0.0009(7) C16 0.0457(13) 0.0324(11) 0.0349(12) -0.0088(9) 0.0122(10) 0.0057(10) C17 0.0312(12) 0.0766(19) 0.0250(11) 0.0069(11) 0.0059(9) -0.0158(12) C18 0.0247(9) 0.0282(10) 0.0224(9) -0.0006(7) 0.0071(7) -0.0022(7) C19 0.0257(10) 0.0374(11) 0.0181(9) 0.0027(8) 0.0042(7) -0.0006(8) C20 0.0210(9) 0.0225(8) 0.0188(8) -0.0023(7) 0.0013(7) 0.0038(7) C21 0.0230(9) 0.0387(11) 0.0205(9) -0.0022(8) 0.0014(7) 0.0010(8) F1 0.0754(11) 0.0376(8) 0.0455(8) 0.0042(6) 0.0330(8) 0.0263(7) F2 0.0384(7) 0.0575(9) 0.0307(7) -0.0208(6) 0.0039(6) -0.0058(6) F3 0.0411(8) 0.0487(8) 0.0389(7) -0.0105(6) 0.0249(6) -0.0101(6) F4 0.138(5) 0.027(2) 0.094(6) 0.009(3) 0.092(5) -0.002(3) F4' 0.254(13) 0.022(3) 0.026(3) 0.012(2) -0.010(5) -0.007(5) F5 0.150(8) 0.027(2) 0.043(2) 0.0000(15) -0.029(3) -0.022(3) F5' 0.071(4) 0.033(3) 0.189(11) 0.003(5) -0.032(5) -0.030(3) F6 0.049(2) 0.025(2) 0.165(7) 0.015(3) 0.016(3) 0.0175(15) F6' 0.162(10) 0.024(2) 0.201(10) 0.002(5) 0.151(9) 0.015(5) F7 0.028(2) 0.0384(15) 0.035(3) -0.0191(15) -0.0036(17) 0.0081(14) F7' 0.032(4) 0.135(8) 0.018(3) 0.015(4) 0.002(2) -0.020(5) F8 0.046(3) 0.0304(16) 0.0329(14) 0.0045(12) -0.0108(14) 0.0150(15) F8' 0.040(4) 0.082(7) 0.157(11) -0.046(6) -0.044(6) 0.034(4) F9 0.022(2) 0.101(7) 0.032(2) 0.024(3) 0.0021(15) -0.017(3) F9' 0.041(7) 0.094(9) 0.057(5) 0.028(5) -0.010(4) -0.043(7) F10 0.0718(12) 0.0586(11) 0.0729(12) -0.0292(9) 0.0057(9) 0.0331(9) F11 0.0670(11) 0.0458(9) 0.0924(14) -0.0391(9) 0.0217(10) -0.0166(8) F12 0.144(2) 0.0639(12) 0.0381(9) -0.0144(8) 0.0437(11) 0.0031(12) F13 0.050(2) 0.097(4) 0.053(2) -0.022(2) 0.0260(19) -0.047(2) F13' 0.089(3) 0.051(2) 0.112(4) -0.012(2) 0.059(3) -0.039(2) F14 0.031(3) 0.169(9) 0.067(6) 0.083(6) 0.001(4) -0.019(4) F14' 0.045(4) 0.136(7) 0.022(3) -0.003(4) 0.018(3) -0.023(4) F15 0.030(2) 0.121(4) 0.102(4) -0.035(3) 0.027(2) -0.001(2) F15' 0.0193(17) 0.134(5) 0.093(4) 0.076(4) 0.009(2) 0.012(3) F16 0.0390(7) 0.0620(9) 0.0216(6) 0.0103(6) -0.0059(5) -0.0072(7) F17 0.0224(6) 0.0862(11) 0.0298(7) -0.0124(7) -0.0012(5) 0.0117(7) F18 0.0432(8) 0.0402(8) 0.0366(7) -0.0119(6) 0.0016(6) -0.0120(6) _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 2.3640(13) . ? Eu1 O7 2.3970(13) . ? Eu1 O9 2.3986(13) . ? Eu1 O5 2.4185(13) . ? Eu1 O4 2.4249(13) . ? Eu1 O8 2.4393(13) . ? Eu1 O2 2.5307(13) . ? Eu1 O3 2.5532(13) . ? Eu1 O1 2.5635(14) . ? O1 C2 1.435(2) . ? O1 C1 1.438(3) . ? O2 C4 1.437(2) . ? O2 C3 1.440(2) . ? O3 C5 1.439(3) . ? O3 C6 1.444(2) . ? O4 C8 1.256(2) . ? O5 C10 1.250(2) . ? O6 C13 1.252(2) . ? O7 C15 1.246(2) . ? O8 C18 1.249(2) . ? O9 C20 1.248(2) . ? C2 C3 1.493(3) . ? C4 C5 1.494(3) . ? C7 F2 1.329(2) . ? C7 F1 1.331(2) . ? C7 F3 1.333(2) . ? C7 C8 1.542(3) . ? C8 C9 1.383(3) . ? C9 C10 1.394(3) . ? C10 C11 1.535(3) . ? C11 F6' 1.241(7) . ? C11 F4' 1.255(7) . ? C11 F5 1.275(6) . ? C11 F4 1.309(6) . ? C11 F5' 1.317(9) . ? C11 F6 1.324(6) . ? C12 F7' 1.264(10) . ? C12 F8' 1.292(12) . ? C12 F9 1.318(12) . ? C12 F9' 1.337(19) . ? C12 F8 1.337(6) . ? C12 F7 1.342(6) . ? C12 C13 1.538(3) . ? C13 C14 1.391(3) . ? C14 C15 1.397(3) . ? C15 C16 1.540(3) . ? C16 F11 1.313(3) . ? C16 F10 1.323(3) . ? C16 F12 1.324(3) . ? C17 F15' 1.194(5) . ? C17 F13 1.260(4) . ? C17 F14 1.281(10) . ? C17 F14' 1.287(8) . ? C17 F13' 1.435(5) . ? C17 F15 1.482(6) . ? C17 C18 1.538(3) . ? C18 C19 1.392(3) . ? C19 C20 1.390(3) . ? C20 C21 1.540(3) . ? C21 F16 1.331(2) . ? C21 F17 1.332(2) . ? C21 F18 1.331(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O7 73.41(5) . . ? O6 Eu1 O9 139.89(5) . . ? O7 Eu1 O9 74.18(5) . . ? O6 Eu1 O5 74.97(5) . . ? O7 Eu1 O5 68.30(5) . . ? O9 Eu1 O5 113.43(5) . . ? O6 Eu1 O4 84.09(4) . . ? O7 Eu1 O4 136.62(5) . . ? O9 Eu1 O4 136.02(5) . . ? O5 Eu1 O4 70.27(4) . . ? O6 Eu1 O8 78.64(5) . . ? O7 Eu1 O8 71.85(5) . . ? O9 Eu1 O8 69.25(5) . . ? O5 Eu1 O8 136.91(5) . . ? O4 Eu1 O8 139.58(4) . . ? O6 Eu1 O2 135.76(4) . . ? O7 Eu1 O2 147.65(5) . . ? O9 Eu1 O2 73.48(4) . . ? O5 Eu1 O2 125.17(4) . . ? O4 Eu1 O2 70.64(4) . . ? O8 Eu1 O2 97.42(5) . . ? O6 Eu1 O3 73.33(5) . . ? O7 Eu1 O3 131.18(5) . . ? O9 Eu1 O3 113.19(5) . . ? O5 Eu1 O3 133.04(5) . . ? O4 Eu1 O3 72.79(4) . . ? O8 Eu1 O3 67.33(5) . . ? O2 Eu1 O3 64.87(4) . . ? O6 Eu1 O1 143.25(5) . . ? O7 Eu1 O1 100.48(5) . . ? O9 Eu1 O1 66.11(4) . . ? O5 Eu1 O1 69.32(5) . . ? O4 Eu1 O1 76.11(4) . . ? O8 Eu1 O1 135.03(4) . . ? O2 Eu1 O1 65.08(5) . . ? O3 Eu1 O1 127.26(4) . . ? C2 O1 C1 110.20(17) . . ? C2 O1 Eu1 114.85(11) . . ? C1 O1 Eu1 118.73(13) . . ? C4 O2 C3 110.73(15) . . ? C4 O2 Eu1 116.85(11) . . ? C3 O2 Eu1 116.59(12) . . ? C5 O3 C6 109.97(16) . . ? C5 O3 Eu1 114.70(12) . . ? C6 O3 Eu1 124.21(12) . . ? C8 O4 Eu1 134.58(12) . . ? C10 O5 Eu1 135.62(12) . . ? C13 O6 Eu1 133.87(12) . . ? C15 O7 Eu1 132.61(13) . . ? C18 O8 Eu1 136.25(12) . . ? C20 O9 Eu1 138.33(12) . . ? O1 C2 C3 108.71(16) . . ? O2 C3 C2 108.49(16) . . ? O2 C4 C5 107.86(17) . . ? O3 C5 C4 107.95(17) . . ? F2 C7 F1 106.73(18) . . ? F2 C7 F3 107.32(17) . . ? F1 C7 F3 107.12(17) . . ? F2 C7 C8 111.29(16) . . ? F1 C7 C8 111.17(16) . . ? F3 C7 C8 112.89(16) . . ? O4 C8 C9 128.57(18) . . ? O4 C8 C7 114.70(16) . . ? C9 C8 C7 116.70(17) . . ? C8 C9 C10 120.66(18) . . ? O5 C10 C9 127.92(18) . . ? O5 C10 C11 114.47(17) . . ? C9 C10 C11 117.60(18) . . ? F6' C11 F4' 111.3(7) . . ? F6' C11 F5 72.6(6) . . ? F4' C11 F5 125.1(6) . . ? F6' C11 F4 125.2(5) . . ? F4' C11 F4 24.2(7) . . ? F5 C11 F4 107.1(5) . . ? F6' C11 F5' 103.8(6) . . ? F4' C11 F5' 104.7(7) . . ? F5 C11 F5' 32.5(6) . . ? F4 C11 F5' 81.6(6) . . ? F6' C11 F6 35.8(6) . . ? F4' C11 F6 83.5(6) . . ? F5 C11 F6 107.0(5) . . ? F4 C11 F6 104.9(5) . . ? F5' C11 F6 134.5(5) . . ? F6' C11 C10 115.1(4) . . ? F4' C11 C10 113.4(5) . . ? F5 C11 C10 112.8(3) . . ? F4 C11 C10 114.7(4) . . ? F5' C11 C10 107.4(4) . . ? F6 C11 C10 109.9(3) . . ? F7' C12 F8' 111.5(7) . . ? F7' C12 F9 115.9(9) . . ? F8' C12 F9 89.1(9) . . ? F7' C12 F9' 105.1(11) . . ? F8' C12 F9' 105.2(10) . . ? F9 C12 F9' 16.6(15) . . ? F7' C12 F8 95.1(6) . . ? F8' C12 F8 20.4(7) . . ? F9 C12 F8 107.7(7) . . ? F9' C12 F8 122.9(9) . . ? F7' C12 F7 11.4(8) . . ? F8' C12 F7 119.3(6) . . ? F9 C12 F7 106.4(8) . . ? F9' C12 F7 94.5(10) . . ? F8 C12 F7 104.7(4) . . ? F7' C12 C13 112.7(6) . . ? F8' C12 C13 114.4(6) . . ? F9 C12 C13 111.3(6) . . ? F9' C12 C13 107.1(8) . . ? F8 C12 C13 113.0(4) . . ? F7 C12 C13 113.1(4) . . ? O6 C13 C14 128.76(18) . . ? O6 C13 C12 114.12(17) . . ? C14 C13 C12 117.04(17) . . ? C13 C14 C15 121.32(18) . . ? O7 C15 C14 128.96(18) . . ? O7 C15 C16 113.47(18) . . ? C14 C15 C16 117.55(18) . . ? F11 C16 F10 108.2(2) . . ? F11 C16 F12 106.4(2) . . ? F10 C16 F12 106.2(2) . . ? F11 C16 C15 111.58(19) . . ? F10 C16 C15 113.9(2) . . ? F12 C16 C15 110.21(19) . . ? F15' C17 F13 61.7(4) . . ? F15' C17 F14 121.2(6) . . ? F13 C17 F14 115.0(7) . . ? F15' C17 F14' 111.6(7) . . ? F13 C17 F14' 125.3(6) . . ? F14 C17 F14' 17.2(12) . . ? F15' C17 F13' 106.2(5) . . ? F13 C17 F13' 45.2(3) . . ? F14 C17 F13' 86.0(7) . . ? F14' C17 F13' 102.7(7) . . ? F15' C17 F15 37.3(4) . . ? F13 C17 F15 98.7(4) . . ? F14 C17 F15 102.6(7) . . ? F14' C17 F15 87.0(7) . . ? F13' C17 F15 141.1(3) . . ? F15' C17 C18 115.2(3) . . ? F13 C17 C18 116.3(2) . . ? F14 C17 C18 116.2(6) . . ? F14' C17 C18 114.5(6) . . ? F13' C17 C18 105.3(3) . . ? F15 C17 C18 104.4(3) . . ? O8 C18 C19 128.30(18) . . ? O8 C18 C17 114.23(17) . . ? C19 C18 C17 117.47(18) . . ? C20 C19 C18 119.70(18) . . ? O9 C20 C19 127.81(18) . . ? O9 C20 C21 113.61(17) . . ? C19 C20 C21 118.57(17) . . ? F16 C21 F17 107.62(17) . . ? F16 C21 F18 107.38(17) . . ? F17 C21 F18 107.12(18) . . ? F16 C21 C20 113.58(17) . . ? F17 C21 C20 110.82(16) . . ? F18 C21 C20 110.06(17) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.539 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.063 data_mg44 _database_code_CSD 177170 _journal_coden_Cambridge 186 loop_ _publ_author_name 'William J. Evans' 'Dimitrios G. Giarikos' 'Matthew A. Johnston' 'Michael A. Greci' 'Joseph W. Ziller' _publ_requested_journal 'Dalton Transactions' _publ_contact_author_name 'Prof William Evans' _publ_contact_author_email 'wevans@uci.edu' _publ_section_title ; Reactivity of the Europium Hexafluroacetylacetonate (hfac) Complex, Eu(hfac)3(diglyme), and related Analogs with Potassium: Formation of the Fluoride hfac "Ate" Complexes, [LnF(hfac)3K(diglyme)]2 ; _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H42 Eu2 F38 K2 O18' _chemical_formula_weight 2022.95 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' 'K' 'K' 0.2009 0.2494 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.1218(6) _cell_length_b 13.2706(6) _cell_length_c 22.1257(10) _cell_angle_alpha 91.1710(10) _cell_angle_beta 91.8270(10) _cell_angle_gamma 111.0050(10) _cell_volume 3592.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 2.006 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7805 _exptl_absorpt_correction_T_max 0.8891 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 '50 frames' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 36765 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 28.38 _reflns_number_total 16562 _reflns_number_gt 11396 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0312P)^2^+47.1157P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16562 _refine_ls_number_parameters 855 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.11702(3) 0.11964(3) 0.031012(18) 0.01945(10) Uani 1 1 d . . . Eu2 Eu 0.44537(3) 0.56119(3) -0.437181(18) 0.01836(10) Uani 1 1 d . . . K1 K 0.1217(2) -0.1593(2) 0.08940(18) 0.0859(12) Uani 1 1 d . . . K2 K 0.76657(14) 0.68958(15) -0.44300(9) 0.0294(4) Uani 1 1 d . . . O1 O 0.2548(4) 0.0614(4) 0.0793(3) 0.0261(13) Uani 1 1 d . . . O2 O 0.2700(5) 0.2764(5) 0.0661(3) 0.0341(14) Uani 1 1 d . . . O3 O 0.1040(4) 0.2443(4) -0.0442(3) 0.0272(13) Uani 1 1 d . . . O4 O 0.2528(5) 0.1386(5) -0.0435(3) 0.0295(13) Uani 1 1 d . . . O5 O 0.0451(5) 0.0232(5) 0.1218(3) 0.0294(13) Uani 1 1 d . . . O6 O 0.0518(5) 0.2321(5) 0.0928(3) 0.0385(16) Uani 1 1 d . . . O7 O 0.1694(9) -0.2513(9) 0.1997(5) 0.095(3) Uiso 1 1 d . . . O8 O 0.2085(12) -0.3112(11) 0.0844(7) 0.128(5) Uiso 1 1 d . . . O9 O 0.2109(7) -0.1874(7) -0.0249(4) 0.057(2) Uiso 1 1 d . . . O11 O 0.2677(4) 0.4220(4) -0.4360(2) 0.0243(12) Uani 1 1 d . . . O12 O 0.4422(5) 0.4337(5) -0.3595(3) 0.0302(14) Uani 1 1 d . . . O13 O 0.3414(4) 0.6601(4) -0.4805(3) 0.0266(13) Uani 1 1 d . . . O14 O 0.5679(4) 0.7164(4) -0.4888(2) 0.0224(12) Uani 1 1 d . . . O15 O 0.5906(4) 0.6703(4) -0.3658(3) 0.0257(12) Uani 1 1 d . . . O16 O 0.3653(4) 0.6158(5) -0.3531(3) 0.0272(13) Uani 1 1 d . . . O17 O 0.7873(6) 0.5200(6) -0.3749(3) 0.0453(17) Uiso 1 1 d . . . O18 O 0.9641(6) 0.7118(6) -0.3860(3) 0.0514(19) Uiso 1 1 d . . . O19 O 0.9358(6) 0.8944(6) -0.4326(3) 0.0463(17) Uiso 1 1 d . . . F1 F 0.5022(5) 0.0792(5) 0.1484(3) 0.0567(17) Uani 1 1 d . . . F2 F 0.3461(5) -0.0497(5) 0.1450(4) 0.076(2) Uani 1 1 d . . . F3 F 0.4383(6) -0.0091(6) 0.0653(4) 0.079(2) Uani 1 1 d . . . F4 F 0.5313(5) 0.4355(6) 0.1147(5) 0.102(3) Uani 1 1 d . . . F5 F 0.3886(7) 0.4541(6) 0.1438(4) 0.089(3) Uani 1 1 d . . . F6 F 0.4229(7) 0.4728(6) 0.0521(4) 0.097(3) Uani 1 1 d . . . F7 F 0.4739(5) 0.2990(5) -0.1234(3) 0.0554(17) Uani 1 1 d . . . F8 F 0.4716(5) 0.1961(7) -0.0501(3) 0.070(2) Uani 1 1 d . . . F9 F 0.3941(6) 0.1286(6) -0.1338(3) 0.070(2) Uani 1 1 d . . . F10 F 0.2232(5) 0.4878(5) -0.1099(4) 0.078(2) Uani 1 1 d . . . F11 F 0.0855(11) 0.3671(7) -0.1495(5) 0.157(6) Uani 1 1 d . . . F12 F 0.0814(8) 0.4302(8) -0.0655(5) 0.123(4) Uani 1 1 d . . . F13 F -0.0553(8) -0.1424(6) 0.1870(3) 0.091(3) Uani 1 1 d . . . F14 F 0.0400(13) -0.0352(9) 0.2517(5) 0.162(6) Uani 1 1 d . . . F15 F -0.1156(13) -0.0492(10) 0.2435(7) 0.199(8) Uani 1 1 d . . . F16 F -0.0865(15) 0.3105(8) 0.1968(10) 0.321(15) Uani 1 1 d . . . F17 F -0.0194(11) 0.3883(9) 0.1210(6) 0.148(5) Uani 1 1 d . . . F18 F 0.0771(10) 0.3920(7) 0.1908(5) 0.122(4) Uani 1 1 d . . . F19 F 0.3371(11) 0.2509(12) -0.2477(6) 0.043(4) Uiso 0.53(3) 1 d P A 1 F19' F 0.3201(14) 0.2790(15) -0.2370(8) 0.055(5) Uiso 0.47(3) 1 d P A 2 F20 F 0.4963(15) 0.3290(17) -0.2711(8) 0.068(5) Uiso 0.53(3) 1 d P A 1 F20' F 0.4717(19) 0.4230(13) -0.2349(8) 0.063(6) Uiso 0.47(3) 1 d P A 2 F21 F 0.4167(14) 0.4218(9) -0.2259(6) 0.050(5) Uiso 0.53(3) 1 d P A 1 F21' F 0.4765(14) 0.2873(16) -0.2814(8) 0.050(5) Uiso 0.47(3) 1 d P A 2 F22 F 0.0636(5) 0.2735(5) -0.4569(3) 0.0569(17) Uani 1 1 d . . . F23 F 0.0343(6) 0.2665(8) -0.3640(4) 0.101(3) Uani 1 1 d . . . F24 F 0.0565(5) 0.4110(6) -0.4101(5) 0.100(3) Uani 1 1 d . . . F25 F 0.2529(5) 0.8363(5) -0.5127(3) 0.064(2) Uani 1 1 d . . . F26 F 0.2476(5) 0.7655(6) -0.6003(3) 0.0597(18) Uani 1 1 d . . . F27 F 0.1618(4) 0.6682(5) -0.5295(3) 0.0568(17) Uani 1 1 d . . . F28 F 0.7415(4) 0.8229(4) -0.5457(2) 0.0360(12) Uani 1 1 d . . . F29 F 0.6441(5) 0.8498(5) -0.6193(3) 0.0465(15) Uani 1 1 d . . . F30 F 0.6778(5) 0.9505(4) -0.5381(3) 0.0472(15) Uani 1 1 d . . . F31 F 0.7138(5) 0.8391(6) -0.2419(3) 0.071(2) Uani 1 1 d . . . F32 F 0.7772(5) 0.8162(7) -0.3253(3) 0.081(3) Uani 1 1 d . . . F33 F 0.7436(7) 0.6963(7) -0.2609(5) 0.111(4) Uani 1 1 d . . . F34 F 0.3380(5) 0.7190(6) -0.2112(3) 0.070(2) Uani 1 1 d . . . F35 F 0.2491(7) 0.5601(6) -0.2457(4) 0.089(3) Uani 1 1 d . . . F36 F 0.2337(5) 0.6932(7) -0.2899(3) 0.075(2) Uani 1 1 d . . . F37 F -0.0650(4) 0.0552(4) 0.0025(2) 0.0271(10) Uani 1 1 d . . . F38 F 0.5843(4) 0.5058(4) -0.4640(2) 0.0298(11) Uani 1 1 d . . . C1 C 0.4103(8) 0.0329(8) 0.1146(5) 0.041(2) Uani 1 1 d . . . C2 C 0.3526(7) 0.1093(7) 0.0973(4) 0.0265(18) Uani 1 1 d . . . C3 C 0.4119(7) 0.2200(7) 0.1020(4) 0.0299(19) Uani 1 1 d . . . H3A H 0.4864 0.2450 0.1157 0.036 Uiso 1 1 calc R . . C4 C 0.3636(7) 0.2939(7) 0.0870(4) 0.031(2) Uani 1 1 d . . . C5 C 0.4305(9) 0.4143(9) 0.0988(6) 0.055(3) Uani 1 1 d . . . C6 C 0.4131(8) 0.2121(8) -0.0949(5) 0.040(2) Uani 1 1 d . . . C7 C 0.3056(7) 0.2173(7) -0.0731(4) 0.0283(18) Uani 1 1 d . . . C8 C 0.2760(7) 0.3046(7) -0.0892(4) 0.033(2) Uani 1 1 d . . . H8A H 0.3258 0.3623 -0.1102 0.039 Uiso 1 1 calc R . . C9 C 0.1762(7) 0.3086(7) -0.0753(4) 0.030(2) Uani 1 1 d . . . C10 C 0.1439(8) 0.3994(8) -0.1017(5) 0.045(3) Uani 1 1 d . . . C11 C -0.0387(12) -0.0487(11) 0.2098(6) 0.064(4) Uani 1 1 d . . . C12 C -0.0040(8) 0.0431(8) 0.1658(4) 0.038(2) Uani 1 1 d . . . C13 C -0.0244(9) 0.1360(9) 0.1783(5) 0.051(3) Uani 1 1 d . . . H13A H -0.0625 0.1394 0.2136 0.061 Uiso 1 1 calc R . . C14 C 0.0077(8) 0.2243(8) 0.1420(5) 0.045(3) Uani 1 1 d . . . C15 C -0.0113(13) 0.3255(11) 0.1651(8) 0.076(4) Uani 1 1 d . . . C16 C 0.2818(17) -0.1146(16) -0.0593(9) 0.126(7) Uiso 1 1 d . . . H16A H 0.2703 -0.0458 -0.0560 0.189 Uiso 1 1 calc R . . H16B H 0.2701 -0.1409 -0.1016 0.189 Uiso 1 1 calc R . . H16C H 0.3567 -0.1042 -0.0455 0.189 Uiso 1 1 calc R . . C17 C 0.222(3) -0.297(3) -0.0181(17) 0.249(17) Uiso 1 1 d . . . H17A H 0.1506 -0.3525 -0.0312 0.299 Uiso 1 1 calc R . . H17B H 0.2762 -0.3015 -0.0467 0.299 Uiso 1 1 calc R . . C18 C 0.2505(14) -0.3228(14) 0.0378(8) 0.092(5) Uiso 1 1 d . . . H18A H 0.2416 -0.4001 0.0346 0.111 Uiso 1 1 calc R . . H18B H 0.3298 -0.2819 0.0442 0.111 Uiso 1 1 calc R . . C19 C 0.2476(15) -0.3438(14) 0.1404(8) 0.096(5) Uiso 1 1 d . . . H19A H 0.2405 -0.4204 0.1361 0.116 Uiso 1 1 calc R . . H19B H 0.3260 -0.2999 0.1479 0.116 Uiso 1 1 calc R . . C20 C 0.195(2) -0.332(2) 0.1847(11) 0.149(9) Uiso 1 1 d . . . H20A H 0.2360 -0.3446 0.2206 0.178 Uiso 1 1 calc R . . H20B H 0.1256 -0.3946 0.1814 0.178 Uiso 1 1 calc R . . C21 C 0.1169(18) -0.2580(18) 0.2520(10) 0.137(8) Uiso 1 1 d . . . H21A H 0.1019 -0.1916 0.2591 0.205 Uiso 1 1 calc R . . H21B H 0.1630 -0.2672 0.2856 0.205 Uiso 1 1 calc R . . H21C H 0.0479 -0.3200 0.2491 0.205 Uiso 1 1 calc R . . C22 C 0.0909(8) 0.3318(8) -0.4052(5) 0.043(2) Uani 1 1 d . . . C23 C 0.2145(7) 0.3716(7) -0.3928(4) 0.0299(19) Uani 1 1 d . . . C24 C 0.2553(8) 0.3489(7) -0.3388(4) 0.034(2) Uani 1 1 d . . . H24A H 0.2063 0.3123 -0.3089 0.041 Uiso 1 1 calc R . . C25 C 0.3666(8) 0.3786(7) -0.3276(4) 0.0300(19) Uani 1 1 d . A . C26 C 0.4065(10) 0.3429(8) -0.2675(4) 0.046(3) Uani 1 1 d . . . C27 C 0.2531(7) 0.7478(7) -0.5415(5) 0.034(2) Uani 1 1 d . . . C28 C 0.3550(7) 0.7235(6) -0.5228(4) 0.0249(17) Uani 1 1 d . . . C29 C 0.4515(7) 0.7778(7) -0.5512(4) 0.0267(18) Uani 1 1 d . . . H29A H 0.4497 0.8196 -0.5852 0.032 Uiso 1 1 calc R . . C30 C 0.5504(7) 0.7722(6) -0.5308(4) 0.0234(17) Uani 1 1 d . . . C31 C 0.6532(7) 0.8489(7) -0.5595(4) 0.031(2) Uani 1 1 d . . . C32 C 0.7067(8) 0.7659(8) -0.2848(4) 0.038(2) Uani 1 1 d . . . C33 C 0.5916(7) 0.7105(6) -0.3134(4) 0.0253(17) Uani 1 1 d . . . C34 C 0.5044(7) 0.7078(7) -0.2798(4) 0.032(2) Uani 1 1 d . . . H34A H 0.5178 0.7397 -0.2401 0.038 Uiso 1 1 calc R . . C35 C 0.3979(7) 0.6601(7) -0.3021(4) 0.0272(18) Uani 1 1 d . . . C36 C 0.3050(8) 0.6583(8) -0.2612(4) 0.038(2) Uani 1 1 d . . . C37 C 0.7102(10) 0.4608(10) -0.3330(6) 0.060(3) Uiso 1 1 d . . . H37A H 0.6363 0.4518 -0.3481 0.090 Uiso 1 1 calc R . . H37B H 0.7255 0.5001 -0.2938 0.090 Uiso 1 1 calc R . . H37C H 0.7158 0.3896 -0.3283 0.090 Uiso 1 1 calc R . . C38 C 0.8952(9) 0.5331(9) -0.3525(6) 0.054(3) Uiso 1 1 d . . . H38A H 0.9049 0.4625 -0.3533 0.065 Uiso 1 1 calc R . . H38B H 0.9061 0.5615 -0.3101 0.065 Uiso 1 1 calc R . . C39 C 0.9755(11) 0.6090(10) -0.3906(6) 0.063(3) Uiso 1 1 d . . . H39A H 1.0504 0.6157 -0.3771 0.075 Uiso 1 1 calc R . . H39B H 0.9631 0.5817 -0.4333 0.075 Uiso 1 1 calc R . . C40 C 1.0512(11) 0.7974(10) -0.4058(6) 0.063(3) Uiso 1 1 d . . . H40A H 1.0627 0.7840 -0.4488 0.076 Uiso 1 1 calc R . . H40B H 1.1183 0.8033 -0.3819 0.076 Uiso 1 1 calc R . . C41 C 1.0313(10) 0.8998(9) -0.3995(6) 0.055(3) Uiso 1 1 d . . . H41A H 1.0239 0.9152 -0.3562 0.066 Uiso 1 1 calc R . . H41B H 1.0946 0.9595 -0.4142 0.066 Uiso 1 1 calc R . . C42 C 0.9161(10) 0.9926(10) -0.4296(6) 0.060(3) Uiso 1 1 d . . . H42A H 0.8490 0.9844 -0.4532 0.090 Uiso 1 1 calc R . . H42B H 0.9777 1.0504 -0.4461 0.090 Uiso 1 1 calc R . . H42C H 0.9080 1.0109 -0.3873 0.090 Uiso 1 1 calc R . . C43 C 0.5791(9) 1.0295(9) -0.6932(5) 0.050(3) Uiso 1 1 d . . . C44 C 0.5899(9) 1.0896(8) -0.6405(5) 0.045(2) Uiso 1 1 d . . . H44A H 0.6609 1.1319 -0.6246 0.054 Uiso 1 1 calc R . . C45 C 0.5012(9) 1.0901(9) -0.6106(6) 0.053(3) Uiso 1 1 d . . . H45A H 0.5112 1.1319 -0.5740 0.064 Uiso 1 1 calc R . . C46 C 0.3977(13) 1.0310(12) -0.6324(7) 0.079(4) Uiso 1 1 d . . . H46A H 0.3349 1.0319 -0.6126 0.095 Uiso 1 1 calc R . . C47 C 0.3896(15) 0.9696(14) -0.6852(8) 0.093(5) Uiso 1 1 d . . . H47A H 0.3192 0.9258 -0.7012 0.112 Uiso 1 1 calc R . . C48 C 0.4774(12) 0.9701(12) -0.7140(7) 0.079(4) Uiso 1 1 d . . . H48A H 0.4678 0.9274 -0.7503 0.095 Uiso 1 1 calc R . . C49 C 0.6780(12) 1.0297(12) -0.7265(7) 0.080(4) Uiso 1 1 d . . . H49A H 0.7446 1.0770 -0.7045 0.121 Uiso 1 1 calc R . . H49B H 0.6750 1.0561 -0.7673 0.121 Uiso 1 1 calc R . . H49C H 0.6786 0.9561 -0.7292 0.121 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 0.0167(2) 0.01626(19) 0.0231(2) 0.00063(16) -0.00265(16) 0.00344(15) Eu2 0.0172(2) 0.0202(2) 0.0170(2) -0.00082(15) 0.00185(16) 0.00587(16) K1 0.0351(13) 0.0474(14) 0.157(3) 0.0608(18) -0.0392(17) -0.0072(11) K2 0.0192(9) 0.0387(10) 0.0274(10) -0.0021(8) 0.0003(8) 0.0070(8) O1 0.021(3) 0.026(3) 0.028(3) 0.003(2) -0.006(2) 0.004(2) O2 0.036(4) 0.022(3) 0.039(4) -0.008(3) -0.011(3) 0.007(3) O3 0.020(3) 0.022(3) 0.034(3) 0.009(2) -0.002(3) 0.001(2) O4 0.030(3) 0.030(3) 0.029(3) 0.006(3) 0.009(3) 0.010(3) O5 0.033(3) 0.034(3) 0.024(3) 0.004(3) 0.008(3) 0.015(3) O6 0.039(4) 0.027(3) 0.051(4) -0.013(3) 0.000(3) 0.014(3) O11 0.019(3) 0.026(3) 0.022(3) -0.005(2) -0.002(2) 0.003(2) O12 0.031(3) 0.034(3) 0.025(3) 0.009(3) 0.006(3) 0.010(3) O13 0.024(3) 0.027(3) 0.032(3) -0.001(3) 0.001(3) 0.013(2) O14 0.022(3) 0.026(3) 0.018(3) -0.002(2) -0.002(2) 0.007(2) O15 0.021(3) 0.029(3) 0.026(3) -0.001(2) 0.004(2) 0.006(2) O16 0.021(3) 0.036(3) 0.023(3) -0.005(3) 0.003(2) 0.008(2) F1 0.030(3) 0.064(4) 0.070(5) 0.010(3) -0.024(3) 0.011(3) F2 0.038(4) 0.060(4) 0.121(7) 0.049(4) -0.020(4) 0.005(3) F3 0.077(5) 0.091(6) 0.095(6) -0.023(5) -0.013(4) 0.065(5) F4 0.033(4) 0.044(4) 0.207(11) -0.027(5) -0.031(5) -0.009(3) F5 0.087(6) 0.049(4) 0.116(7) -0.042(4) -0.004(5) 0.009(4) F6 0.109(7) 0.040(4) 0.097(7) 0.014(4) -0.027(5) -0.024(4) F7 0.034(3) 0.058(4) 0.073(5) 0.030(3) 0.024(3) 0.011(3) F8 0.040(4) 0.133(7) 0.052(4) 0.036(4) 0.011(3) 0.046(4) F9 0.069(5) 0.063(4) 0.076(5) -0.011(4) 0.032(4) 0.020(4) F10 0.048(4) 0.036(3) 0.147(8) 0.038(4) 0.009(4) 0.011(3) F11 0.236(13) 0.063(5) 0.171(10) -0.025(6) -0.166(10) 0.070(7) F12 0.134(8) 0.108(7) 0.178(10) 0.098(7) 0.092(8) 0.093(7) F13 0.151(8) 0.043(4) 0.049(4) 0.008(3) 0.014(5) -0.001(5) F14 0.242(15) 0.101(8) 0.076(7) 0.034(6) -0.054(9) -0.016(9) F15 0.251(16) 0.143(10) 0.245(16) 0.109(11) 0.218(15) 0.099(11) F16 0.36(2) 0.064(6) 0.57(3) 0.044(11) 0.41(3) 0.080(10) F17 0.219(14) 0.122(9) 0.160(11) -0.052(8) -0.045(10) 0.138(10) F18 0.193(11) 0.052(5) 0.121(8) -0.047(5) -0.036(8) 0.049(6) F22 0.034(3) 0.075(4) 0.047(4) -0.021(3) -0.009(3) 0.004(3) F23 0.040(4) 0.151(8) 0.062(5) 0.019(5) 0.017(4) -0.026(5) F24 0.030(4) 0.071(5) 0.198(10) -0.043(6) -0.009(5) 0.023(4) F25 0.052(4) 0.058(4) 0.098(6) -0.024(4) -0.009(4) 0.041(3) F26 0.047(4) 0.094(5) 0.048(4) 0.014(4) -0.012(3) 0.037(4) F27 0.025(3) 0.059(4) 0.086(5) 0.011(4) -0.008(3) 0.015(3) F28 0.023(3) 0.040(3) 0.044(3) 0.012(2) 0.006(2) 0.010(2) F29 0.047(3) 0.059(4) 0.034(3) 0.019(3) 0.011(3) 0.019(3) F30 0.044(3) 0.023(3) 0.070(4) -0.003(3) 0.012(3) 0.006(2) F31 0.041(4) 0.091(5) 0.064(5) -0.049(4) -0.005(3) 0.006(3) F32 0.037(4) 0.124(6) 0.044(4) -0.024(4) 0.008(3) -0.017(4) F33 0.080(6) 0.072(5) 0.177(10) -0.005(6) -0.081(6) 0.029(5) F34 0.046(4) 0.111(6) 0.047(4) -0.041(4) 0.006(3) 0.022(4) F35 0.098(6) 0.061(5) 0.093(6) 0.003(4) 0.076(5) 0.004(4) F36 0.047(4) 0.135(7) 0.056(4) -0.010(4) 0.012(3) 0.051(5) F37 0.022(2) 0.027(2) 0.032(3) 0.001(2) -0.002(2) 0.010(2) F38 0.031(3) 0.033(3) 0.025(3) -0.003(2) -0.001(2) 0.011(2) C1 0.027(5) 0.046(6) 0.049(6) 0.003(5) -0.010(5) 0.014(4) C2 0.025(4) 0.034(5) 0.018(4) -0.003(3) -0.001(3) 0.008(4) C3 0.021(4) 0.037(5) 0.026(5) -0.004(4) -0.002(4) 0.004(4) C4 0.024(5) 0.032(5) 0.028(5) -0.009(4) -0.010(4) 0.002(4) C5 0.044(7) 0.035(6) 0.073(9) -0.005(6) -0.013(6) -0.002(5) C6 0.036(5) 0.046(6) 0.037(6) 0.016(5) 0.005(4) 0.012(5) C7 0.022(4) 0.033(5) 0.026(5) 0.005(4) -0.003(4) 0.005(4) C8 0.026(5) 0.039(5) 0.028(5) 0.010(4) 0.003(4) 0.003(4) C9 0.027(5) 0.025(4) 0.034(5) 0.003(4) -0.004(4) 0.004(4) C10 0.036(6) 0.038(5) 0.061(7) 0.024(5) 0.003(5) 0.010(5) C11 0.076(9) 0.065(8) 0.039(7) -0.001(6) 0.023(7) 0.009(7) C12 0.031(5) 0.041(5) 0.034(5) -0.009(4) 0.005(4) 0.002(4) C13 0.042(6) 0.050(6) 0.052(7) -0.018(5) 0.025(5) 0.004(5) C14 0.030(5) 0.037(5) 0.062(7) -0.020(5) 0.002(5) 0.008(4) C15 0.083(10) 0.047(7) 0.104(12) -0.027(8) 0.029(9) 0.031(7) C22 0.028(5) 0.048(6) 0.044(6) -0.009(5) 0.007(5) 0.004(4) C23 0.024(4) 0.025(4) 0.036(5) -0.003(4) 0.011(4) 0.003(3) C24 0.038(5) 0.029(5) 0.029(5) 0.004(4) 0.015(4) 0.004(4) C25 0.039(5) 0.025(4) 0.022(4) 0.001(3) 0.004(4) 0.007(4) C26 0.061(7) 0.035(5) 0.027(5) 0.005(4) -0.007(5) 0.000(5) C27 0.024(5) 0.037(5) 0.046(6) 0.002(4) 0.000(4) 0.016(4) C28 0.027(4) 0.025(4) 0.026(4) -0.004(3) -0.004(4) 0.014(3) C29 0.034(5) 0.028(4) 0.021(4) -0.002(3) 0.000(4) 0.015(4) C30 0.026(4) 0.018(4) 0.026(4) -0.001(3) 0.003(3) 0.007(3) C31 0.033(5) 0.024(4) 0.036(5) 0.007(4) 0.009(4) 0.012(4) C32 0.030(5) 0.047(6) 0.033(5) -0.008(4) 0.004(4) 0.009(4) C33 0.025(4) 0.026(4) 0.022(4) -0.002(3) -0.002(3) 0.005(3) C34 0.028(5) 0.039(5) 0.024(5) -0.003(4) 0.004(4) 0.007(4) C35 0.026(4) 0.032(4) 0.023(4) 0.000(4) 0.009(4) 0.009(4) C36 0.036(5) 0.047(6) 0.029(5) -0.007(4) 0.014(4) 0.011(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 F37 2.271(5) 2 ? Eu1 F37 2.292(4) . ? Eu1 O6 2.394(6) . ? Eu1 O2 2.408(6) . ? Eu1 O3 2.414(5) . ? Eu1 O4 2.415(6) . ? Eu1 O1 2.433(5) . ? Eu1 O5 2.434(6) . ? Eu1 Eu1 3.7363(8) 2 ? Eu1 K1 3.966(2) . ? Eu1 K1 4.230(2) 2 ? Eu2 F38 2.286(5) . ? Eu2 F38 2.312(5) 2_664 ? Eu2 O16 2.389(5) . ? Eu2 O13 2.398(5) . ? Eu2 O11 2.401(5) . ? Eu2 O12 2.427(6) . ? Eu2 O15 2.441(6) . ? Eu2 O14 2.443(5) . ? Eu2 Eu2 3.7629(8) 2_664 ? Eu2 K2 3.9469(18) . ? Eu2 K2 4.2863(19) 2_664 ? K1 O8 2.648(15) . ? K1 F37 2.711(5) 2 ? K1 O1 2.839(6) . ? K1 O9 2.893(9) . ? K1 O7 2.900(12) . ? K1 O3 2.901(6) 2 ? K1 F2 2.988(7) . ? K1 O5 3.018(7) . ? K1 F13 3.284(10) . ? K1 C18 3.394(18) . ? K1 C20 3.51(2) . ? K2 F38 2.754(5) . ? K2 O18 2.761(8) . ? K2 O17 2.821(7) . ? K2 O19 2.826(7) . ? K2 O15 2.857(6) . ? K2 O14 2.909(6) . ? K2 O11 2.975(6) 2_664 ? K2 F28 2.989(5) . ? K2 F32 3.042(7) . ? K2 F22 3.112(6) 2_664 ? K2 Eu2 4.2863(19) 2_664 ? O1 C2 1.258(10) . ? O2 C4 1.238(10) . ? O3 C9 1.259(10) . ? O3 K1 2.901(6) 2 ? O4 C7 1.241(10) . ? O5 C12 1.259(10) . ? O6 C14 1.238(12) . ? O7 C20 1.28(2) . ? O7 C21 1.35(2) . ? O8 C18 1.217(19) . ? O8 C19 1.46(2) . ? O9 C16 1.345(19) . ? O9 C17 1.51(3) . ? O11 C23 1.257(10) . ? O11 K2 2.975(6) 2_664 ? O12 C25 1.250(10) . ? O13 C28 1.246(10) . ? O14 C30 1.266(9) . ? O15 C33 1.264(10) . ? O16 C35 1.251(10) . ? O17 C37 1.421(13) . ? O17 C38 1.434(13) . ? O18 C40 1.383(14) . ? O18 C39 1.427(13) . ? O19 C41 1.411(13) . ? O19 C42 1.417(13) . ? F1 C1 1.335(11) . ? F2 C1 1.329(12) . ? F3 C1 1.335(12) . ? F4 C5 1.285(13) . ? F5 C5 1.340(14) . ? F6 C5 1.327(14) . ? F7 C6 1.329(10) . ? F8 C6 1.302(11) . ? F9 C6 1.335(12) . ? F10 C10 1.280(11) . ? F11 C10 1.257(13) . ? F12 C10 1.323(14) . ? F13 C11 1.274(14) . ? F14 C11 1.326(17) . ? F15 C11 1.272(15) . ? F16 C15 1.188(16) . ? F17 C15 1.323(19) . ? F18 C15 1.286(17) . ? F19 C26 1.329(15) . ? F19' C26 1.358(19) . ? F20 C26 1.261(18) . ? F20' C26 1.288(18) . ? F21 C26 1.346(16) . ? F21' C26 1.41(2) . ? F22 C22 1.333(11) . ? F22 K2 3.112(6) 2_664 ? F23 C22 1.322(12) . ? F24 C22 1.290(12) . ? F25 C27 1.326(11) . ? F26 C27 1.331(11) . ? F27 C27 1.322(10) . ? F28 C31 1.351(10) . ? F29 C31 1.325(10) . ? F30 C31 1.340(10) . ? F31 C32 1.322(11) . ? F32 C32 1.317(11) . ? F33 C32 1.301(12) . ? F34 C36 1.321(11) . ? F35 C36 1.304(11) . ? F36 C36 1.334(12) . ? F37 Eu1 2.271(5) 2 ? F37 K1 2.711(5) 2 ? F38 Eu2 2.312(5) 2_664 ? C1 C2 1.516(12) . ? C2 C3 1.394(12) . ? C3 C4 1.385(12) . ? C4 C5 1.535(13) . ? C6 C7 1.529(13) . ? C7 C8 1.396(12) . ? C8 C9 1.374(12) . ? C9 C10 1.534(13) . ? C11 C12 1.523(16) . ? C12 C13 1.377(14) . ? C13 C14 1.380(16) . ? C14 C15 1.533(14) . ? C17 C18 1.37(3) . ? C19 C20 1.25(2) . ? C22 C23 1.529(13) . ? C23 C24 1.375(13) . ? C24 C25 1.382(13) . ? C25 C26 1.558(13) . ? C27 C28 1.531(11) . ? C28 C29 1.391(12) . ? C29 C30 1.388(12) . ? C30 C31 1.534(11) . ? C32 C33 1.531(12) . ? C33 C34 1.375(12) . ? C34 C35 1.380(12) . ? C35 C36 1.534(11) . ? C38 C39 1.473(16) . ? C40 C41 1.476(16) . ? C43 C48 1.345(18) . ? C43 C44 1.374(15) . ? C43 C49 1.512(17) . ? C44 C45 1.359(15) . ? C45 C46 1.368(18) . ? C46 C47 1.39(2) . ? C47 C48 1.33(2) . ? 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 F37 Eu1 F37 70.09(18) 2 . ? F37 Eu1 O6 139.57(19) 2 . ? F37 Eu1 O6 78.96(19) . . ? F37 Eu1 O2 144.61(18) 2 . ? F37 Eu1 O2 145.12(18) . . ? O6 Eu1 O2 71.2(2) . . ? F37 Eu1 O3 115.04(18) 2 . ? F37 Eu1 O3 76.74(17) . . ? O6 Eu1 O3 81.0(2) . . ? O2 Eu1 O3 81.1(2) . . ? F37 Eu1 O4 80.59(18) 2 . ? F37 Eu1 O4 120.18(19) . . ? O6 Eu1 O4 138.9(2) . . ? O2 Eu1 O4 75.7(2) . . ? O3 Eu1 O4 70.36(19) . . ? F37 Eu1 O1 77.60(17) 2 . ? F37 Eu1 O1 140.66(17) . . ? O6 Eu1 O1 115.5(2) . . ? O2 Eu1 O1 70.95(19) . . ? O3 Eu1 O1 139.18(18) . . ? O4 Eu1 O1 74.23(19) . . ? F37 Eu1 O5 78.26(18) 2 . ? F37 Eu1 O5 81.26(19) . . ? O6 Eu1 O5 71.8(2) . . ? O2 Eu1 O5 105.3(2) . . ? O3 Eu1 O5 147.69(19) . . ? O4 Eu1 O5 141.91(19) . . ? O1 Eu1 O5 70.51(19) . . ? F37 Eu1 Eu1 35.23(11) 2 2 ? F37 Eu1 Eu1 34.86(11) . 2 ? O6 Eu1 Eu1 110.20(15) . 2 ? O2 Eu1 Eu1 177.24(16) . 2 ? O3 Eu1 Eu1 96.69(13) . 2 ? O4 Eu1 Eu1 102.07(14) . 2 ? O1 Eu1 Eu1 110.12(13) . 2 ? O5 Eu1 Eu1 77.47(14) . 2 ? F37 Eu1 K1 41.28(13) 2 . ? F37 Eu1 K1 95.51(12) . . ? O6 Eu1 K1 120.95(18) . . ? O2 Eu1 K1 115.00(15) . . ? O3 Eu1 K1 155.39(15) . . ? O4 Eu1 K1 94.74(15) . . ? O1 Eu1 K1 45.25(13) . . ? O5 Eu1 K1 49.48(14) . . ? Eu1 Eu1 K1 66.55(4) 2 . ? F37 Eu1 K1 89.03(12) 2 2 ? F37 Eu1 K1 35.44(12) . 2 ? O6 Eu1 K1 79.80(18) . 2 ? O2 Eu1 K1 119.07(15) . 2 ? O3 Eu1 K1 41.47(13) . 2 ? O4 Eu1 K1 96.15(15) . 2 ? O1 Eu1 K1 164.54(15) . 2 ? O5 Eu1 K1 114.68(15) . 2 ? Eu1 Eu1 K1 59.32(4) 2 2 ? K1 Eu1 K1 125.88(3) . 2 ? F38 Eu2 F38 70.1(2) . 2_664 ? F38 Eu2 O16 143.55(18) . . ? F38 Eu2 O16 144.98(18) 2_664 . ? F38 Eu2 O13 137.92(18) . . ? F38 Eu2 O13 78.12(18) 2_664 . ? O16 Eu2 O13 75.2(2) . . ? F38 Eu2 O11 115.73(18) . . ? F38 Eu2 O11 77.04(18) 2_664 . ? O16 Eu2 O11 77.09(19) . . ? O13 Eu2 O11 81.83(19) . . ? F38 Eu2 O12 78.05(18) . . ? F38 Eu2 O12 116.62(19) 2_664 . ? O16 Eu2 O12 75.1(2) . . ? O13 Eu2 O12 142.59(19) . . ? O11 Eu2 O12 69.7(2) . . ? F38 Eu2 O15 79.53(17) . . ? F38 Eu2 O15 141.70(17) 2_664 . ? O16 Eu2 O15 71.01(18) . . ? O13 Eu2 O15 113.00(19) . . ? O11 Eu2 O15 139.06(18) . . ? O12 Eu2 O15 77.67(19) . . ? F38 Eu2 O14 76.80(17) . . ? F38 Eu2 O14 79.70(17) 2_664 . ? O16 Eu2 O14 111.71(19) . . ? O13 Eu2 O14 70.83(18) . . ? O11 Eu2 O14 147.12(18) . . ? O12 Eu2 O14 142.57(19) . . ? O15 Eu2 O14 70.86(18) . . ? F38 Eu2 Eu2 35.30(12) . 2_664 ? F38 Eu2 Eu2 34.84(12) 2_664 2_664 ? O16 Eu2 Eu2 172.64(14) . 2_664 ? O13 Eu2 Eu2 108.93(14) . 2_664 ? O11 Eu2 Eu2 97.23(13) . 2_664 ? O12 Eu2 Eu2 98.60(14) . 2_664 ? O15 Eu2 Eu2 111.83(13) . 2_664 ? O14 Eu2 Eu2 75.61(12) . 2_664 ? F38 Eu2 K2 42.90(12) . . ? F38 Eu2 K2 95.82(12) 2_664 . ? O16 Eu2 K2 116.48(14) . . ? O13 Eu2 K2 117.56(14) . . ? O11 Eu2 K2 157.90(13) . . ? O12 Eu2 K2 95.94(14) . . ? O15 Eu2 K2 46.05(13) . . ? O14 Eu2 K2 47.27(13) . . ? Eu2 Eu2 K2 67.50(3) 2_664 . ? F38 Eu2 K2 87.59(12) . 2_664 ? F38 Eu2 K2 35.52(12) 2_664 2_664 ? O16 Eu2 K2 117.39(14) . 2_664 ? O13 Eu2 K2 81.88(14) . 2_664 ? O11 Eu2 K2 42.04(13) . 2_664 ? O12 Eu2 K2 92.06(15) . 2_664 ? O15 Eu2 K2 164.90(13) . 2_664 ? O14 Eu2 K2 113.99(13) . 2_664 ? Eu2 Eu2 K2 58.29(3) 2_664 2_664 ? K2 Eu2 K2 125.80(3) . 2_664 ? O8 K1 F37 129.0(4) . 2 ? O8 K1 O1 120.5(3) . . ? F37 K1 O1 64.17(15) 2 . ? O8 K1 O9 64.1(4) . . ? F37 K1 O9 66.3(2) 2 . ? O1 K1 O9 84.3(2) . . ? O8 K1 O7 59.8(4) . . ? F37 K1 O7 171.2(3) 2 . ? O1 K1 O7 112.9(3) . . ? O9 K1 O7 122.2(3) . . ? O8 K1 O3 110.4(3) . 2 ? F37 K1 O3 62.67(15) 2 2 ? O1 K1 O3 121.85(17) . 2 ? O9 K1 O3 94.8(2) . 2 ? O7 K1 O3 115.9(3) . 2 ? O8 K1 F2 76.6(4) . . ? F37 K1 F2 115.68(17) 2 . ? O1 K1 F2 53.82(16) . . ? O9 K1 F2 91.0(3) . . ? O7 K1 F2 64.4(3) . . ? O3 K1 F2 172.4(3) 2 . ? O8 K1 O5 167.8(4) . . ? F37 K1 O5 62.23(16) 2 . ? O1 K1 O5 57.22(17) . . ? O9 K1 O5 125.1(2) . . ? O7 K1 O5 109.1(3) . . ? O3 K1 O5 78.17(18) 2 . ? F2 K1 O5 94.5(2) . . ? O8 K1 F13 125.9(4) . . ? F37 K1 F13 98.3(2) 2 . ? O1 K1 F13 101.4(2) . . ? O9 K1 F13 159.7(2) . . ? O7 K1 F13 73.8(3) . . ? O3 K1 F13 65.5(2) 2 . ? F2 K1 F13 108.2(3) . . ? O5 K1 F13 48.73(17) . . ? O8 K1 C18 18.5(4) . . ? F37 K1 C18 111.2(3) 2 . ? O1 K1 C18 110.9(3) . . ? O9 K1 C18 45.6(3) . . ? O7 K1 C18 77.6(4) . . ? O3 K1 C18 108.7(3) 2 . ? F2 K1 C18 78.9(4) . . ? O5 K1 C18 167.7(3) . . ? F13 K1 C18 143.2(3) . . ? O8 K1 C20 39.8(5) . . ? F37 K1 C20 168.2(5) 2 . ? O1 K1 C20 122.4(4) . . ? O9 K1 C20 103.4(4) . . ? O7 K1 C20 20.3(4) . . ? O3 K1 C20 114.4(4) 2 . ? F2 K1 C20 68.8(4) . . ? O5 K1 C20 129.3(4) . . ? F13 K1 C20 90.1(4) . . ? C18 K1 C20 58.0(5) . . ? O8 K1 Eu1 148.4(3) . . ? F37 K1 Eu1 33.56(10) 2 . ? O1 K1 Eu1 37.48(11) . . ? O9 K1 Eu1 87.61(17) . . ? O7 K1 Eu1 139.6(3) . . ? O3 K1 Eu1 84.38(12) 2 . ? F2 K1 Eu1 90.95(13) . . ? O5 K1 Eu1 37.81(11) . . ? F13 K1 Eu1 85.49(15) . . ? C18 K1 Eu1 131.2(3) . . ? C20 K1 Eu1 156.8(4) . . ? F38 K2 O18 129.0(2) . . ? F38 K2 O17 70.29(18) . . ? O18 K2 O17 59.8(2) . . ? F38 K2 O19 171.00(19) . . ? O18 K2 O19 60.0(2) . . ? O17 K2 O19 118.7(2) . . ? F38 K2 O15 65.24(15) . . ? O18 K2 O15 116.2(2) . . ? O17 K2 O15 83.84(19) . . ? O19 K2 O15 113.15(19) . . ? F38 K2 O14 62.48(15) . . ? O18 K2 O14 166.2(2) . . ? O17 K2 O14 128.39(19) . . ? O19 K2 O14 108.82(19) . . ? O15 K2 O14 58.81(16) . . ? F38 K2 O11 61.51(15) . 2_664 ? O18 K2 O11 113.4(2) . 2_664 ? O17 K2 O11 97.34(19) . 2_664 ? O19 K2 O11 115.90(19) . 2_664 ? O15 K2 O11 122.45(16) . 2_664 ? O14 K2 O11 78.11(15) . 2_664 ? F38 K2 F28 100.63(15) . . ? O18 K2 F28 124.17(19) . . ? O17 K2 F28 162.77(19) . . ? O19 K2 F28 71.00(18) . . ? O15 K2 F28 106.08(16) . . ? O14 K2 F28 52.14(14) . . ? O11 K2 F28 65.48(15) 2_664 . ? F38 K2 F32 116.44(16) . . ? O18 K2 F32 74.2(2) . . ? O17 K2 F32 88.9(2) . . ? O19 K2 F32 64.8(2) . . ? O15 K2 F32 52.93(16) . . ? O14 K2 F32 94.00(19) . . ? O11 K2 F32 171.9(2) 2_664 . ? F28 K2 F32 108.3(2) . . ? F38 K2 F22 113.16(16) . 2_664 ? O18 K2 F22 72.9(2) . 2_664 ? O17 K2 F22 105.1(2) . 2_664 ? O19 K2 F22 66.75(19) . 2_664 ? O15 K2 F22 170.03(18) . 2_664 ? O14 K2 F22 111.40(17) . 2_664 ? O11 K2 F22 52.91(15) 2_664 2_664 ? F28 K2 F22 64.17(16) . 2_664 ? F32 K2 F22 130.30(17) . 2_664 ? F38 K2 Eu2 34.40(10) . . ? O18 K2 Eu2 145.99(17) . . ? O17 K2 Eu2 90.47(15) . . ? O19 K2 Eu2 139.44(16) . . ? O15 K2 Eu2 37.96(12) . . ? O14 K2 Eu2 38.09(11) . . ? O11 K2 Eu2 84.56(11) 2_664 . ? F28 K2 Eu2 89.21(10) . . ? F32 K2 Eu2 90.28(13) . . ? F22 K2 Eu2 135.73(12) 2_664 . ? F38 K2 Eu2 29.18(10) . 2_664 ? O18 K2 Eu2 130.66(17) . 2_664 ? O17 K2 Eu2 85.45(15) . 2_664 ? O19 K2 Eu2 146.49(16) . 2_664 ? O15 K2 Eu2 90.97(12) . 2_664 ? O14 K2 Eu2 63.11(11) . 2_664 ? O11 K2 Eu2 32.72(10) 2_664 2_664 ? F28 K2 Eu2 80.41(11) . 2_664 ? F32 K2 Eu2 143.88(13) . 2_664 ? F22 K2 Eu2 85.45(11) 2_664 2_664 ? Eu2 K2 Eu2 54.20(3) . 2_664 ? C2 O1 Eu1 134.0(5) . . ? C2 O1 K1 128.7(5) . . ? Eu1 O1 K1 97.28(18) . . ? C4 O2 Eu1 135.9(6) . . ? C9 O3 Eu1 130.7(5) . . ? C9 O3 K1 120.0(5) . 2 ? Eu1 O3 K1 105.10(19) . 2 ? C7 O4 Eu1 130.9(6) . . ? C12 O5 Eu1 133.4(6) . . ? C12 O5 K1 133.9(6) . . ? Eu1 O5 K1 92.71(18) . . ? C14 O6 Eu1 136.0(6) . . ? C20 O7 C21 116.5(17) . . ? C20 O7 K1 107.8(14) . . ? C21 O7 K1 125.6(12) . . ? C18 O8 C19 117.7(16) . . ? C18 O8 K1 117.9(13) . . ? C19 O8 K1 119.0(11) . . ? C16 O9 C17 118.6(17) . . ? C16 O9 K1 130.4(10) . . ? C17 O9 K1 101.6(15) . . ? C23 O11 Eu2 130.8(5) . . ? C23 O11 K2 118.5(5) . 2_664 ? Eu2 O11 K2 105.23(19) . 2_664 ? C25 O12 Eu2 130.8(6) . . ? C28 O13 Eu2 134.5(5) . . ? C30 O14 Eu2 131.7(5) . . ? C30 O14 K2 131.9(5) . . ? Eu2 O14 K2 94.64(17) . . ? C33 O15 Eu2 133.8(5) . . ? C33 O15 K2 130.1(5) . . ? Eu2 O15 K2 95.99(18) . . ? C35 O16 Eu2 136.3(5) . . ? C37 O17 C38 109.1(8) . . ? C37 O17 K2 124.3(6) . . ? C38 O17 K2 116.6(6) . . ? C40 O18 C39 115.2(9) . . ? C40 O18 K2 113.7(7) . . ? C39 O18 K2 107.0(7) . . ? C41 O19 C42 112.9(9) . . ? C41 O19 K2 116.3(6) . . ? C42 O19 K2 123.1(6) . . ? C1 F2 K1 114.9(6) . . ? C11 F13 K1 116.2(7) . . ? C22 F22 K2 120.0(5) . 2_664 ? C31 F28 K2 126.5(5) . . ? C32 F32 K2 115.9(6) . . ? Eu1 F37 Eu1 109.91(18) 2 . ? Eu1 F37 K1 105.16(19) 2 2 ? Eu1 F37 K1 115.21(18) . 2 ? Eu2 F38 Eu2 109.9(2) . 2_664 ? Eu2 F38 K2 102.70(17) . . ? Eu2 F38 K2 115.30(19) 2_664 . ? F2 C1 F3 106.7(9) . . ? F2 C1 F1 107.2(8) . . ? F3 C1 F1 106.3(8) . . ? F2 C1 C2 111.5(8) . . ? F3 C1 C2 110.6(8) . . ? F1 C1 C2 114.0(8) . . ? O1 C2 C3 128.5(8) . . ? O1 C2 C1 113.3(7) . . ? C3 C2 C1 118.2(8) . . ? C4 C3 C2 120.9(8) . . ? O2 C4 C3 128.6(8) . . ? O2 C4 C5 113.3(8) . . ? C3 C4 C5 118.1(8) . . ? F4 C5 F6 110.1(11) . . ? F4 C5 F5 105.9(11) . . ? F6 C5 F5 103.4(10) . . ? F4 C5 C4 114.6(10) . . ? F6 C5 C4 111.7(9) . . ? F5 C5 C4 110.3(9) . . ? F8 C6 F7 108.5(8) . . ? F8 C6 F9 105.9(9) . . ? F7 C6 F9 106.1(8) . . ? F8 C6 C7 110.9(8) . . ? F7 C6 C7 114.4(8) . . ? F9 C6 C7 110.6(8) . . ? O4 C7 C8 127.5(8) . . ? O4 C7 C6 113.6(8) . . ? C8 C7 C6 118.8(8) . . ? C9 C8 C7 121.1(8) . . ? O3 C9 C8 128.2(8) . . ? O3 C9 C10 114.0(8) . . ? C8 C9 C10 117.8(8) . . ? F11 C10 F10 110.8(11) . . ? F11 C10 F12 104.0(11) . . ? F10 C10 F12 102.8(10) . . ? F11 C10 C9 110.8(9) . . ? F10 C10 C9 115.4(8) . . ? F12 C10 C9 112.2(9) . . ? F15 C11 F13 111.4(12) . . ? F15 C11 F14 99.6(13) . . ? F13 C11 F14 103.5(13) . . ? F15 C11 C12 114.8(13) . . ? F13 C11 C12 115.5(10) . . ? F14 C11 C12 110.2(11) . . ? O5 C12 C13 128.0(9) . . ? O5 C12 C11 112.6(9) . . ? C13 C12 C11 119.4(9) . . ? C12 C13 C14 123.1(9) . . ? O6 C14 C13 127.5(9) . . ? O6 C14 C15 115.7(11) . . ? C13 C14 C15 116.8(11) . . ? F16 C15 F18 110.9(17) . . ? F16 C15 F17 108.6(17) . . ? F18 C15 F17 97.1(12) . . ? F16 C15 C14 116.1(12) . . ? F18 C15 C14 109.9(12) . . ? F17 C15 C14 112.7(12) . . ? C18 C17 O9 118(3) . . ? O8 C18 C17 124(2) . . ? O8 C18 K1 43.6(10) . . ? C17 C18 K1 84.0(18) . . ? C20 C19 O8 111.9(19) . . ? C19 C20 O7 129(2) . . ? C19 C20 K1 83.5(15) . . ? O7 C20 K1 51.9(11) . . ? F24 C22 F23 108.7(10) . . ? F24 C22 F22 107.3(10) . . ? F23 C22 F22 104.7(8) . . ? F24 C22 C23 111.6(8) . . ? F23 C22 C23 113.8(9) . . ? F22 C22 C23 110.2(8) . . ? O11 C23 C24 127.6(8) . . ? O11 C23 C22 113.0(8) . . ? C24 C23 C22 119.4(8) . . ? C23 C24 C25 120.8(8) . . ? O12 C25 C24 128.1(8) . . ? O12 C25 C26 113.9(8) . . ? C24 C25 C26 117.9(8) . . ? F20 C26 F20' 77.8(13) . . ? F20 C26 F19 105.5(12) . . ? F20' C26 F19 126.7(12) . . ? F20 C26 F21 109.7(13) . . ? F20' C26 F21 33.0(8) . . ? F19 C26 F21 108.2(11) . . ? F20 C26 F19' 124.8(13) . . ? F20' C26 F19' 113.1(13) . . ? F19 C26 F19' 23.7(8) . . ? F21 C26 F19' 87.5(11) . . ? F20 C26 F21' 23.5(10) . . ? F20' C26 F21' 100.8(13) . . ? F19 C26 F21' 87.9(10) . . ? F21 C26 F21' 131.2(13) . . ? F19' C26 F21' 110.5(12) . . ? F20 C26 C25 113.8(11) . . ? F20' C26 C25 112.9(10) . . ? F19 C26 C25 113.6(10) . . ? F21 C26 C25 106.1(9) . . ? F19' C26 C25 110.4(11) . . ? F21' C26 C25 108.7(10) . . ? F27 C27 F25 107.7(8) . . ? F27 C27 F26 107.0(8) . . ? F25 C27 F26 106.1(8) . . ? F27 C27 C28 112.3(7) . . ? F25 C27 C28 110.6(8) . . ? F26 C27 C28 112.7(7) . . ? O13 C28 C29 127.6(8) . . ? O13 C28 C27 114.2(7) . . ? C29 C28 C27 118.1(7) . . ? C30 C29 C28 121.4(8) . . ? O14 C30 C29 128.3(8) . . ? O14 C30 C31 115.2(7) . . ? C29 C30 C31 116.4(7) . . ? F29 C31 F30 107.7(7) . . ? F29 C31 F28 107.0(7) . . ? F30 C31 F28 105.8(7) . . ? F29 C31 C30 113.5(8) . . ? F30 C31 C30 110.8(7) . . ? F28 C31 C30 111.6(7) . . ? F33 C32 F32 106.2(9) . . ? F33 C32 F31 106.8(9) . . ? F32 C32 F31 106.1(8) . . ? F33 C32 C33 111.3(8) . . ? F32 C32 C33 111.7(8) . . ? F31 C32 C33 114.2(8) . . ? O15 C33 C34 128.5(8) . . ? O15 C33 C32 113.5(7) . . ? C34 C33 C32 118.0(8) . . ? C33 C34 C35 121.9(8) . . ? O16 C35 C34 127.8(8) . . ? O16 C35 C36 113.5(8) . . ? C34 C35 C36 118.7(8) . . ? F35 C36 F34 107.9(9) . . ? F35 C36 F36 105.9(9) . . ? F34 C36 F36 106.3(8) . . ? F35 C36 C35 111.1(8) . . ? F34 C36 C35 114.0(8) . . ? F36 C36 C35 111.3(8) . . ? O17 C38 C39 108.9(10) . . ? O18 C39 C38 108.9(10) . . ? O18 C40 C41 111.1(10) . . ? O19 C41 C40 111.2(10) . . ? C48 C43 C44 117.6(12) . . ? C48 C43 C49 121.1(12) . . ? C44 C43 C49 121.3(11) . . ? C45 C44 C43 121.5(11) . . ? C44 C45 C46 120.8(13) . . ? C45 C46 C47 116.3(15) . . ? C48 C47 C46 122.1(17) . . ? C47 C48 C43 121.6(16) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 2.452 _refine_diff_density_min -2.011 _refine_diff_density_rms 0.184 #===end #===end