# Copyright The Royal Society of Chemistry, 1998. data_p1bar _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'EU2(calix-5)4DMSO4 x 5THF' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C158 H214 Eu2 O24 S4' _chemical_formula_weight 2929.45 _chemical_melting_point ? _chemical_compound_source ? 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' 'Eu' 'Eu' -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 16.442(3) _cell_length_b 16.496(3) _cell_length_c 32.629(7) _cell_angle_alpha 97.97(3) _cell_angle_beta 97.51(3) _cell_angle_gamma 114.26(3) _cell_volume 7816.0(27) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'verkantet eingesunkene Steinplatten' _exptl_crystal_colour 'egg yolk' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method ? _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type N/A _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44486 _diffrn_reflns_av_R_equivalents 0.2389 _diffrn_reflns_av_sigmaI/netI 0.5093 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 24.05 _reflns_number_total 22971 _reflns_number_observed 6273 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00024(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 22971 _refine_ls_number_parameters 724 _refine_ls_number_restraints 229 _refine_ls_R_factor_all 0.2806 _refine_ls_R_factor_obs 0.1120 _refine_ls_wR_factor_all 0.3174 _refine_ls_wR_factor_obs 0.2475 _refine_ls_goodness_of_fit_all 0.822 _refine_ls_goodness_of_fit_obs 1.231 _refine_ls_restrained_S_all 0.824 _refine_ls_restrained_S_obs 1.221 _refine_ls_shift/esd_max 0.242 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Eu1 Eu 0.07014(7) -0.03585(7) 0.54044(3) 0.0351(3) Uani 1 d . . O101 O 0.1673(8) 0.1077(8) 0.5311(4) 0.033(3) Uiso 1 d . . O102 O 0.2119(9) -0.0042(9) 0.5934(4) 0.048(4) Uani 1 d . . O103 O 0.0791(10) -0.1397(9) 0.5913(4) 0.061(4) Uani 1 d . . O104 O -0.0836(9) -0.1427(8) 0.5290(4) 0.040(3) Uani 1 d . . O105 O -0.0232(8) 0.0481(8) 0.5311(4) 0.044(4) Uani 1 d D . S1 S 0.1579(7) -0.1852(7) 0.4790(2) 0.150(4) Uani 1 d D . O501 O 0.1303(10) -0.1261(9) 0.5079(4) 0.070(5) Uiso 1 d D . C511 C 0.1805(29) -0.2635(23) 0.5058(14) 0.217(22) Uiso 1 d D . C512 C 0.2686(16) -0.1209(18) 0.4709(14) 0.562(76) Uani 1 d D . S2 S 0.1036(4) 0.0165(4) 0.6544(2) 0.054(2) Uani 1 d D . O502 O 0.0652(8) 0.0205(9) 0.6103(3) 0.044(4) Uani 1 d D . C521 C 0.1751(13) 0.1306(12) 0.6800(8) 0.079(8) Uani 1 d D . C522 C 0.0135(15) -0.0048(18) 0.6826(9) 0.125(14) Uani 1 d D . C101 C 0.2233(14) 0.1773(13) 0.5651(6) 0.0540(7) Uiso 1 d D . C102 C 0.1972(14) 0.2372(13) 0.5851(6) 0.0540(7) Uiso 1 d D . C103 C 0.2546(14) 0.3033(13) 0.6202(6) 0.0540(7) Uiso 1 d D . C104 C 0.3416(14) 0.3125(13) 0.6365(6) 0.0540(7) Uiso 1 d D . C105 C 0.3717(14) 0.2501(14) 0.6162(7) 0.0540(7) Uiso 1 d D . C106 C 0.3098(15) 0.1828(14) 0.5794(6) 0.0540(7) Uiso 1 d D . C107 C 0.4050(13) 0.3858(13) 0.6759(6) 0.0540(7) Uiso 1 d D . C108 C 0.4014(22) 0.4731(19) 0.6709(11) 0.142(2) Uiso 1 d D . C109 C 0.3720(21) 0.3603(23) 0.7152(9) 0.142(2) Uiso 1 d D . C110 C 0.5025(17) 0.4002(23) 0.6812(11) 0.142(2) Uiso 1 d D . C111 C 0.1040(13) 0.2358(13) 0.5691(6) 0.040(2) Uiso 1 d . . C112 C 0.0281(13) 0.1820(14) 0.5876(6) 0.0540(7) Uiso 1 d D . C113 C 0.0108(13) 0.2204(14) 0.6240(6) 0.0540(7) Uiso 1 d D . C114 C -0.0626(13) 0.1765(14) 0.6420(6) 0.0540(7) Uiso 1 d D . C115 C -0.1225(14) 0.0887(15) 0.6213(6) 0.0540(7) Uiso 1 d D . C116 C -0.1128(14) 0.0422(15) 0.5861(7) 0.0540(7) Uiso 1 d D . C117 C -0.0337(14) 0.0917(14) 0.5686(5) 0.0540(7) Uiso 1 d D . C118 C -0.0779(13) 0.2283(13) 0.6825(6) 0.0540(7) Uiso 1 d D . C119 C -0.1748(16) 0.1812(21) 0.6897(11) 0.142(2) Uiso 1 d D . C120 C -0.0122(18) 0.2359(23) 0.7190(10) 0.142(2) Uiso 1 d D . C121 C -0.0674(22) 0.3216(18) 0.6766(11) 0.142(2) Uiso 1 d D . C122 C -0.1820(13) -0.0510(13) 0.5652(6) 0.040(2) Uiso 1 d . . C123 C -0.1753(11) -0.1336(12) 0.5784(6) 0.0540(7) Uiso 1 d D . C124 C -0.2159(11) -0.1634(13) 0.6123(6) 0.0540(7) Uiso 1 d D . C125 C -0.2099(11) -0.2360(13) 0.6269(5) 0.0540(7) Uiso 1 d D . C126 C -0.1612(14) -0.2840(14) 0.6075(6) 0.0540(7) Uiso 1 d D . C127 C -0.1197(14) -0.2509(14) 0.5739(6) 0.0540(7) Uiso 1 d D . C128 C -0.1267(14) -0.1741(15) 0.5593(7) 0.0540(7) Uiso 1 d D . C129 C -0.2582(12) -0.2712(13) 0.6624(6) 0.0540(7) Uiso 1 d D . C130 C -0.2350(22) -0.1967(18) 0.6987(9) 0.142(2) Uiso 1 d D . C131 C -0.3603(17) -0.3095(22) 0.6428(10) 0.142(2) Uiso 1 d D . C132 C -0.2471(22) -0.3510(19) 0.6747(11) 0.142(2) Uiso 1 d D . C133 C -0.0831(13) -0.3049(13) 0.5487(6) 0.040(2) Uiso 1 d . . C134 C 0.0050(14) -0.3013(15) 0.5729(6) 0.0540(7) Uiso 1 d D . C135 C 0.0126(14) -0.3846(15) 0.5718(5) 0.0540(7) Uiso 1 d D . C136 C 0.0965(14) -0.3844(13) 0.5914(5) 0.0540(7) Uiso 1 d D . C137 C 0.1673(14) -0.3025(15) 0.6118(6) 0.0540(7) Uiso 1 d D . C138 C 0.1682(15) -0.2147(15) 0.6138(6) 0.0540(7) Uiso 1 d D . C139 C 0.0802(15) -0.2193(15) 0.5918(6) 0.0540(7) Uiso 1 d D . C140 C 0.1067(13) -0.4728(13) 0.5909(6) 0.0540(7) Uiso 1 d D . C141 C 0.0378(18) -0.5273(24) 0.6117(9) 0.142(2) Uiso 1 d D . C142 C 0.1974(17) -0.4581(25) 0.6186(9) 0.142(2) Uiso 1 d D . C143 C 0.1035(22) -0.5087(25) 0.5473(7) 0.142(2) Uiso 1 d D . C144 C 0.2447(13) -0.1271(13) 0.6396(6) 0.040(2) Uiso 1 d . . C145 C 0.3080(14) -0.0748(14) 0.6149(6) 0.0540(7) Uiso 1 d D . C146 C 0.3927(14) -0.0828(13) 0.6130(5) 0.0540(7) Uiso 1 d D . C147 C 0.4566(12) -0.0285(13) 0.5939(5) 0.0540(7) Uiso 1 d D . C148 C 0.4388(14) 0.0397(14) 0.5746(6) 0.0540(7) Uiso 1 d D . C149 C 0.3611(15) 0.0513(15) 0.5763(6) 0.0540(7) Uiso 1 d D . C150 C 0.2924(15) -0.0071(15) 0.5939(6) 0.0540(7) Uiso 1 d D . C151 C 0.5476(12) -0.0340(13) 0.5918(6) 0.0540(7) Uiso 1 d D . C152 C 0.5738(24) -0.0733(20) 0.6256(9) 0.142(2) Uiso 1 d D . C153 C 0.5429(24) -0.0744(21) 0.5483(7) 0.142(2) Uiso 1 d D . C154 C 0.6272(23) 0.0631(16) 0.6023(10) 0.142(2) Uiso 1 d D . C155 C 0.3438(13) 0.1214(13) 0.5542(6) 0.040(2) Uiso 1 d . . Eu3 Eu -0.03588(7) 0.07014(7) 1.04043(3) 0.0341(3) Uani 1 d . . O301 O -0.1419(8) -0.0814(8) 1.0284(4) 0.039(3) Uiso 1 d . . O302 O -0.1381(9) 0.0818(9) 1.0914(4) 0.052(4) Uani 1 d . . O303 O -0.0037(9) 0.2137(8) 1.0935(4) 0.047(4) Uani 1 d . . O304 O 0.1091(8) 0.1672(8) 1.0323(4) 0.036(3) Uani 1 d . . O305 O 0.0499(8) -0.0233(8) 1.0318(4) 0.034(3) Uani 1 d . . S5 S -0.1869(8) 0.1563(8) 0.9792(2) 0.157(4) Uani 1 d D . O505 O -0.1266(10) 0.1297(11) 1.0082(4) 0.078(5) Uani 1 d D . C551 C -0.1279(20) 0.2655(20) 0.9748(14) 0.307(43) Uani 1 d D . C552 C -0.2697(22) 0.1746(26) 1.0083(12) 0.160(15) Uiso 1 d D . S6 S 0.0158(4) 0.1039(4) 1.1545(2) 0.054(2) Uani 1 d D . O506 O 0.0194(9) 0.0651(9) 1.1101(3) 0.043(4) Uani 1 d D . C561 C 0.1316(12) 0.1729(17) 1.1790(7) 0.096(10) Uani 1 d D . C562 C -0.0030(20) 0.0131(14) 1.1831(7) 0.099(11) Uani 1 d D . C301 C -0.1729(14) -0.1240(13) 1.0602(6) 0.0540(7) Uiso 1 d D . C302 C -0.2485(13) -0.1206(12) 1.0739(6) 0.0540(7) Uiso 1 d D . C303 C -0.2818(13) -0.1616(12) 1.1062(6) 0.0540(7) Uiso 1 d D . C304 C -0.2363(14) -0.2074(13) 1.1272(6) 0.0540(7) Uiso 1 d D . C305 C -0.1618(14) -0.2122(14) 1.1129(6) 0.0540(7) Uiso 1 d D . C306 C -0.1270(14) -0.1714(14) 1.0792(6) 0.0540(7) Uiso 1 d D . C307 C -0.2717(13) -0.2607(13) 1.1617(6) 0.0540(7) Uiso 1 d D . C308 C -0.1985(18) -0.2353(22) 1.1987(9) 0.142(2) Uiso 1 d D . C309 C -0.3097(21) -0.3618(17) 1.1414(10) 0.142(2) Uiso 1 d D . C310 C -0.3534(18) -0.2484(22) 1.1735(11) 0.142(2) Uiso 1 d D . C311 C -0.0476(13) -0.1823(13) 1.0655(6) 0.040(2) Uiso 1 d . . C312 C 0.0428(14) -0.1115(14) 1.0859(6) 0.0540(7) Uiso 1 d D . C313 C 0.0896(14) -0.1185(13) 1.1214(6) 0.0540(7) Uiso 1 d D . C314 C 0.1799(14) -0.0580(13) 1.1431(6) 0.0540(7) Uiso 1 d D . C315 C 0.2227(14) 0.0162(14) 1.1239(7) 0.0540(7) Uiso 1 d D . C316 C 0.1818(15) 0.0271(14) 1.0884(7) 0.0540(7) Uiso 1 d D . C317 C 0.0919(15) -0.0355(15) 1.0683(7) 0.0540(7) Uiso 1 d D . C318 C 0.2262(13) -0.0781(13) 1.1826(6) 0.0540(7) Uiso 1 d D . C319 C 0.1807(21) -0.1735(16) 1.1901(11) 0.142(2) Uiso 1 d D . C320 C 0.2391(22) -0.0113(18) 1.2208(10) 0.142(2) Uiso 1 d D . C321 C 0.3211(18) -0.0699(22) 1.1758(11) 0.142(2) Uiso 1 d D . C322 C 0.2378(13) 0.1060(13) 1.0698(6) 0.040(2) Uiso 1 d . . C323 C 0.2383(13) 0.1991(14) 1.0857(6) 0.0540(7) Uiso 1 d D . C324 C 0.3071(13) 0.2559(14) 1.1220(6) 0.0540(7) Uiso 1 d D . C325 C 0.3102(12) 0.3439(14) 1.1361(5) 0.0540(7) Uiso 1 d D . C326 C 0.2530(14) 0.3726(15) 1.1164(6) 0.0540(7) Uiso 1 d D . C327 C 0.1813(14) 0.3107(15) 1.0793(6) 0.0540(7) Uiso 1 d D . C328 C 0.1761(15) 0.2258(15) 1.0657(7) 0.0540(7) Uiso 1 d D . C329 C 0.3854(12) 0.4054(13) 1.1760(6) 0.0540(7) Uiso 1 d D . C330 C 0.3579(22) 0.3717(21) 1.2146(9) 0.142(2) Uiso 1 d D . C331 C 0.4018(23) 0.5027(17) 1.1816(11) 0.142(2) Uiso 1 d D . C332 C 0.4755(19) 0.4023(22) 1.1725(11) 0.142(2) Uiso 1 d D . C333 C 0.1234(13) 0.3449(13) 1.0548(6) 0.040(2) Uiso 1 d . . C334 C 0.0518(13) 0.3611(14) 1.0771(5) 0.0540(7) Uiso 1 d D . C335 C 0.0406(13) 0.4383(14) 1.0745(5) 0.0540(7) Uiso 1 d D . C336 C -0.0309(13) 0.4523(13) 1.0928(5) 0.0540(7) Uiso 1 d D . C337 C -0.0831(14) 0.3874(15) 1.1119(6) 0.0540(7) Uiso 1 d D . C338 C -0.0725(14) 0.3097(15) 1.1145(6) 0.0540(7) Uiso 1 d D . C339 C -0.0057(14) 0.2954(15) 1.0940(6) 0.0540(7) Uiso 1 d D . C340 C -0.0453(13) 0.5368(13) 1.0869(6) 0.0540(7) Uiso 1 d D . C341 C -0.0634(22) 0.5469(25) 1.0421(7) 0.142(2) Uiso 1 d D . C342 C 0.0425(16) 0.6135(23) 1.1095(9) 0.142(2) Uiso 1 d D . C343 C -0.1184(18) 0.5488(25) 1.1070(9) 0.142(2) Uiso 1 d D . C344 C -0.1290(13) 0.2415(13) 1.1393(6) 0.040(2) Uiso 1 d . . C345 C -0.2136(15) 0.1675(14) 1.1146(6) 0.0540(7) Uiso 1 d D . C346 C -0.3011(15) 0.1686(14) 1.1127(5) 0.0540(7) Uiso 1 d D . C347 C -0.3856(13) 0.0952(14) 1.0924(5) 0.0540(7) Uiso 1 d D . C348 C -0.3852(14) 0.0116(14) 1.0713(6) 0.0540(7) Uiso 1 d D . C349 C -0.3020(15) 0.0053(15) 1.0732(6) 0.0540(7) Uiso 1 d D . C350 C -0.2188(15) 0.0795(15) 1.0918(6) 0.0540(7) Uiso 1 d D . C351 C -0.4774(13) 0.0990(13) 1.0902(6) 0.0540(7) Uiso 1 d D . C352 C -0.5133(24) 0.0974(22) 1.0479(7) 0.142(2) Uiso 1 d D . C353 C -0.5344(24) 0.0206(17) 1.1078(10) 0.142(2) Uiso 1 d D . C354 C -0.4695(25) 0.1806(17) 1.1218(9) 0.142(2) Uiso 1 d D . C355 C -0.3034(13) -0.0838(13) 1.0499(6) 0.040(2) Uiso 1 d . . O610 O -0.3070(15) -0.2427(15) 0.5299(10) 0.311(5) Uiso 1 d D . C611 C -0.2610(19) -0.2983(17) 0.5364(17) 0.311(5) Uiso 1 d D . C612 C -0.3224(24) -0.3843(24) 0.4946(18) 0.311(5) Uiso 1 d D . C613 C -0.4228(37) -0.3852(43) 0.4795(19) 0.311(5) Uiso 1 d D . C614 C -0.4175(23) -0.3021(32) 0.5142(19) 0.311(5) Uiso 1 d D . O620 O 0.2064(12) -0.0473(24) 0.7928(12) 0.311(5) Uiso 1 d D . C621 C 0.2922(24) -0.0604(31) 0.8030(16) 0.311(5) Uiso 1 d D . C622 C 0.3515(16) -0.0018(40) 0.7762(17) 0.311(5) Uiso 1 d D . C623 C 0.2866(38) 0.0228(41) 0.7432(16) 0.311(5) Uiso 1 d D . C624 C 0.1976(31) 0.0031(45) 0.7618(20) 0.311(5) Uiso 1 d D . O630 O 0.0096(14) -0.2005(17) 0.7367(14) 0.311(5) Uiso 1 d D . C631 C -0.0221(29) -0.2833(31) 0.7555(14) 0.311(5) Uiso 1 d D . C632 C 0.0179(39) -0.3405(22) 0.7293(20) 0.311(5) Uiso 1 d D . C633 C 0.0594(41) -0.2913(39) 0.6948(18) 0.311(5) Uiso 1 d D . C634 C 0.0468(48) -0.1984(36) 0.6997(18) 0.311(5) Uiso 1 d D . O640 O -0.3817(12) 0.2490(27) 1.3068(10) 0.311(5) Uiso 1 d D . C641 C -0.4385(31) 0.2946(31) 1.3129(14) 0.311(5) Uiso 1 d D . C642 C -0.5135(20) 0.2507(36) 1.2699(18) 0.311(5) Uiso 1 d D . C643 C -0.4837(37) 0.1885(42) 1.2409(11) 0.311(5) Uiso 1 d D . C644 C -0.4077(40) 0.1733(38) 1.2696(18) 0.311(5) Uiso 1 d D . O650 O -0.3764(13) -0.4579(18) 0.9774(14) 0.311(5) Uiso 1 d D . C651 C -0.3280(23) -0.3678(31) 1.0062(14) 0.311(5) Uiso 1 d D . C652 C -0.3919(37) -0.3221(22) 0.9927(20) 0.311(5) Uiso 1 d D . C653 C -0.4671(33) -0.3881(37) 0.9534(19) 0.311(5) Uiso 1 d D . C654 C -0.4558(37) -0.4794(30) 0.9449(16) 0.311(5) Uiso 1 d D . O660 O 0.4989(22) 0.1286(21) 0.6953(10) 0.311(5) Uiso 1 d D . C661 C 0.4393(18) 0.1662(33) 0.7116(16) 0.311(5) Uiso 1 d D . C662 C 0.4999(27) 0.2232(33) 0.7564(14) 0.311(5) Uiso 1 d D . C663 C 0.5880(30) 0.2083(42) 0.7630(12) 0.311(5) Uiso 1 d D . C664 C 0.5720(33) 0.1247(40) 0.7260(18) 0.311(5) Uiso 1 d D . O670 O -0.2777(16) -0.5645(29) 1.1879(8) 0.311(5) Uiso 1 d D . C671 C -0.2631(23) -0.4915(27) 1.2252(17) 0.311(5) Uiso 1 d D . C672 C -0.2035(40) -0.5100(37) 1.2595(9) 0.311(5) Uiso 1 d D . C673 C -0.1760(36) -0.5854(42) 1.2382(17) 0.311(5) Uiso 1 d D . C674 C -0.2337(47) -0.6230(36) 1.1913(16) 0.311(5) Uiso 1 d D . O680 O 0.2407(15) -0.4106(27) 0.4287(11) 0.311(5) Uiso 1 d D . C681 C 0.2406(35) -0.4407(28) 0.3840(14) 0.311(5) Uiso 1 d D . C682 C 0.3271(35) -0.3633(42) 0.3772(13) 0.311(5) Uiso 1 d D . C683 C 0.3712(32) -0.2872(30) 0.4207(18) 0.311(5) Uiso 1 d D . C684 C 0.3110(43) -0.3202(35) 0.4526(13) 0.311(5) Uiso 1 d D . O690 O 0.1233(23) 0.4863(20) 1.1959(12) 0.384(30) Uiso 1 d D . C691 C 0.1422(37) 0.5820(28) 1.2018(20) 0.759(132) Uiso 1 d D . C692 C 0.2268(52) 0.6238(19) 1.2421(21) 0.472(64) Uiso 1 d D . C693 C 0.2183(33) 0.5418(34) 1.2636(12) 0.228(24) Uiso 1 d D . C694 C 0.1609(45) 0.4507(21) 1.2280(20) 0.332(39) Uiso 1 d D . O700 O -0.4045(22) 0.2371(16) 0.9271(14) 0.348(26) Uiso 1 d D . C701 C -0.3107(27) 0.2975(36) 0.9503(16) 0.346(41) Uiso 1 d D . C702 C -0.2845(27) 0.3778(27) 0.9272(21) 0.312(35) Uiso 1 d D . C703 C -0.3617(51) 0.3445(43) 0.8842(20) 0.428(55) Uiso 1 d D . C704 C -0.4382(36) 0.2532(44) 0.8861(19) 0.374(46) Uiso 1 d 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 0.0378(7) 0.0367(7) 0.0397(7) 0.0037(5) 0.0063(5) 0.0267(6) O102 0.054(9) 0.064(9) 0.042(8) 0.012(7) 0.012(7) 0.039(8) O103 0.079(10) 0.050(9) 0.057(9) -0.018(7) -0.012(8) 0.047(9) O104 0.067(9) 0.035(7) 0.039(8) 0.013(6) 0.023(7) 0.038(7) O105 0.027(7) 0.018(7) 0.077(10) -0.003(7) 0.038(7) -0.004(6) S1 0.260(10) 0.255(11) 0.068(5) 0.019(6) 0.025(6) 0.249(10) C512 0.079(27) 0.368(60) 0.932(149) -0.543(85) 0.056(52) 0.027(36) S2 0.069(4) 0.050(4) 0.041(3) 0.006(3) 0.005(3) 0.028(3) O502 0.044(8) 0.062(9) 0.044(8) 0.015(7) 0.002(6) 0.041(8) C521 0.063(16) 0.039(14) 0.091(19) -0.018(13) -0.019(14) -0.002(13) C522 0.071(19) 0.125(26) 0.133(26) 0.047(21) 0.077(19) -0.023(19) Eu3 0.0373(7) 0.0367(7) 0.0382(7) 0.0032(5) 0.0088(5) 0.0269(6) O302 0.045(8) 0.069(10) 0.057(9) -0.009(7) 0.005(7) 0.048(8) O303 0.076(10) 0.036(8) 0.040(8) 0.001(6) 0.017(7) 0.036(8) O304 0.041(7) 0.038(7) 0.039(8) 0.004(6) -0.010(6) 0.035(7) O305 0.021(7) 0.017(7) 0.053(9) 0.013(6) 0.003(6) -0.004(6) S5 0.275(10) 0.271(11) 0.069(5) 0.018(6) 0.021(6) 0.269(10) O505 0.108(12) 0.115(13) 0.066(10) 0.002(9) 0.018(9) 0.106(12) C551 0.169(39) 0.095(28) 0.500(87) 0.140(43) -0.227(49) -0.031(29) S6 0.047(3) 0.063(4) 0.047(3) -0.002(3) 0.011(3) 0.021(3) O506 0.047(8) 0.050(9) 0.040(8) -0.001(7) 0.012(7) 0.032(7) C561 0.045(15) 0.150(27) 0.065(17) -0.030(17) -0.014(13) 0.037(17) C562 0.140(26) 0.079(20) 0.056(17) 0.014(14) 0.041(17) 0.022(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O105 2.314(14) 2_556 ? Eu1 O501 2.317(11) . ? Eu1 O101 2.340(11) . ? Eu1 O104 2.355(13) . ? Eu1 O502 2.363(11) . ? Eu1 O105 2.471(14) . ? Eu1 O102 2.527(13) . ? Eu1 O103 2.58(2) . ? Eu1 Eu1 3.899(2) 2_556 ? O101 C101 1.38(2) . ? O102 C150 1.34(2) . ? O103 C139 1.32(3) . ? O104 C128 1.33(2) . ? O105 C117 1.399(5) . ? O105 Eu1 2.315(14) 2_556 ? S1 O501 1.506(9) . ? S1 C512 1.767(9) . ? S1 C511 1.79(3) . ? S2 O502 1.516(8) . ? S2 C521 1.76(2) . ? S2 C522 1.78(2) . ? C101 C102 1.35(3) . ? C101 C106 1.40(3) . ? C102 C103 1.38(3) . ? C102 C111 1.54(3) . ? C103 C104 1.40(3) . ? C104 C105 1.43(3) . ? C104 C107 1.55(2) . ? C105 C106 1.45(3) . ? C106 C155 1.54(3) . ? C107 C108 1.50(2) . ? C107 C109 1.50(2) . ? C107 C110 1.50(2) . ? C111 C112 1.47(3) . ? C112 C113 1.38(3) . ? C112 C117 1.40(3) . ? C113 C114 1.38(3) . ? C114 C115 1.38(3) . ? C114 C118 1.58(2) . ? C115 C116 1.35(3) . ? C116 C117 1.46(3) . ? C116 C122 1.48(3) . ? C118 C120 1.45(2) . ? C118 C121 1.52(2) . ? C118 C119 1.52(2) . ? C122 C123 1.53(3) . ? C123 C128 1.39(3) . ? C123 C124 1.41(3) . ? C124 C125 1.38(3) . ? C125 C126 1.48(3) . ? C125 C129 1.54(2) . ? C126 C127 1.42(3) . ? C127 C128 1.45(3) . ? C127 C133 1.48(3) . ? C129 C130 1.47(2) . ? C129 C132 1.50(2) . ? C129 C131 1.54(2) . ? C133 C134 1.53(3) . ? C134 C139 1.39(3) . ? C134 C135 1.43(3) . ? C135 C136 1.44(3) . ? C136 C137 1.37(3) . ? C136 C140 1.53(2) . ? C137 C138 1.44(3) . ? C138 C139 1.49(3) . ? C138 C144 1.51(3) . ? C140 C141 1.44(2) . ? C140 C143 1.45(2) . ? C140 C142 1.55(2) . ? C144 C145 1.46(3) . ? C145 C146 1.46(3) . ? C145 C150 1.48(3) . ? C146 C147 1.36(3) . ? C147 C148 1.47(3) . ? C147 C151 1.55(2) . ? C148 C149 1.37(3) . ? C149 C150 1.40(3) . ? C149 C155 1.54(3) . ? C151 C153 1.46(2) . ? C151 C152 1.46(2) . ? C151 C154 1.55(2) . ? Eu3 O505 2.318(11) . ? Eu3 O301 2.326(12) . ? Eu3 O305 2.328(13) 2_557 ? Eu3 O304 2.337(13) . ? Eu3 O506 2.360(11) . ? Eu3 O305 2.492(13) . ? Eu3 O303 2.547(12) . ? Eu3 O302 2.556(12) . ? Eu3 Eu3 3.883(2) 2_557 ? O301 C301 1.37(2) . ? O302 C350 1.31(2) . ? O303 C339 1.36(2) . ? O304 C328 1.36(2) . ? O305 C317 1.38(2) . ? O305 Eu3 2.328(13) 2_557 ? S5 O505 1.517(9) . ? S5 C551 1.70(2) . ? S5 C552 1.86(2) . ? S6 O506 1.521(8) . ? S6 C561 1.77(2) . ? S6 C562 1.81(2) . ? C301 C302 1.39(3) . ? C301 C306 1.43(3) . ? C302 C303 1.38(3) . ? C302 C355 1.48(3) . ? C303 C304 1.44(3) . ? C304 C305 1.39(3) . ? C304 C307 1.55(2) . ? C305 C306 1.43(3) . ? C306 C311 1.50(3) . ? C307 C308 1.47(2) . ? C307 C310 1.53(2) . ? C307 C309 1.53(2) . ? C311 C312 1.45(3) . ? C312 C313 1.35(3) . ? C312 C317 1.43(3) . ? C313 C314 1.42(3) . ? C314 C315 1.42(3) . ? C314 C318 1.55(2) . ? C315 C316 1.33(3) . ? C316 C317 1.41(3) . ? C316 C322 1.52(3) . ? C318 C320 1.47(2) . ? C318 C319 1.51(2) . ? C318 C321 1.56(2) . ? C322 C323 1.55(3) . ? C323 C328 1.39(3) . ? C323 C324 1.42(3) . ? C324 C325 1.44(3) . ? C325 C326 1.35(3) . ? C325 C329 1.56(2) . ? C326 C327 1.48(3) . ? C327 C328 1.37(3) . ? C327 C333 1.49(3) . ? C329 C331 1.49(2) . ? C329 C330 1.49(2) . ? C329 C332 1.52(2) . ? C333 C334 1.55(3) . ? C334 C339 1.35(3) . ? C334 C335 1.37(3) . ? C335 C336 1.47(3) . ? C336 C337 1.36(3) . ? C336 C340 1.54(2) . ? C337 C338 1.38(3) . ? C338 C339 1.44(3) . ? C338 C344 1.54(3) . ? C340 C342 1.48(2) . ? C340 C341 1.50(2) . ? C340 C343 1.51(2) . ? C344 C345 1.45(3) . ? C345 C346 1.44(3) . ? C345 C350 1.50(3) . ? C346 C347 1.41(3) . ? C347 C348 1.46(3) . ? C347 C351 1.53(2) . ? C348 C349 1.41(3) . ? C349 C350 1.39(3) . ? C349 C355 1.55(3) . ? C351 C352 1.42(2) . ? C351 C353 1.49(2) . ? C351 C354 1.53(2) . ? O610 C611 1.43(3) . ? O610 C614 1.64(3) . ? C611 C612 1.68(4) . ? C612 C613 1.65(4) . ? C613 C614 1.62(4) . ? O620 C624 1.42(3) . ? O620 C621 1.51(3) . ? C621 C622 1.53(3) . ? C622 C623 1.62(3) . ? C623 C624 1.59(3) . ? O630 C634 1.42(3) . ? O630 C631 1.50(3) . ? C631 C632 1.58(3) . ? C632 C633 1.54(3) . ? C633 C634 1.62(3) . ? O640 C641 1.44(3) . ? O640 C644 1.49(3) . ? C641 C642 1.60(3) . ? C642 C643 1.57(3) . ? C643 C644 1.59(3) . ? O650 C654 1.45(3) . ? O650 C651 1.47(3) . ? C651 C652 1.58(3) . ? C652 C653 1.56(3) . ? C653 C654 1.58(3) . ? O660 C661 1.47(3) . ? O660 C664 1.49(3) . ? C661 C662 1.58(3) . ? C662 C663 1.56(3) . ? C663 C664 1.61(3) . ? O670 C674 1.43(3) . ? O670 C671 1.51(3) . ? C671 C672 1.54(3) . ? C672 C673 1.59(3) . ? C673 C674 1.58(3) . ? O680 C681 1.47(3) . ? O680 C684 1.48(3) . ? C681 C682 1.54(3) . ? C682 C683 1.62(3) . ? C683 C684 1.53(3) . ? O690 C694 1.46(3) . ? O690 C691 1.46(3) . ? C691 C692 1.62(3) . ? C692 C693 1.58(3) . ? C693 C694 1.60(3) . ? O700 C701 1.47(3) . ? O700 C704 1.48(3) . ? C701 C702 1.55(3) . ? C702 C703 1.62(3) . ? C703 C704 1.53(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 O105 Eu1 O501 75.9(5) 2_556 . ? O105 Eu1 O101 78.3(4) 2_556 . ? O501 Eu1 O101 101.3(5) . . ? O105 Eu1 O104 79.2(4) 2_556 . ? O501 Eu1 O104 100.0(5) . . ? O101 Eu1 O104 144.0(4) . . ? O105 Eu1 O502 147.0(4) 2_556 . ? O501 Eu1 O502 137.1(5) . . ? O101 Eu1 O502 93.6(4) . . ? O104 Eu1 O502 90.3(4) . . ? O105 Eu1 O105 70.9(4) 2_556 . ? O501 Eu1 O105 146.8(5) . . ? O101 Eu1 O105 73.3(4) . . ? O104 Eu1 O105 73.0(4) . . ? O502 Eu1 O105 76.1(4) . . ? O105 Eu1 O102 139.9(4) 2_556 . ? O501 Eu1 O102 75.8(5) . . ? O101 Eu1 O102 80.2(4) . . ? O104 Eu1 O102 133.5(4) . . ? O502 Eu1 O102 67.4(4) . . ? O105 Eu1 O102 132.9(4) . . ? O105 Eu1 O103 138.5(4) 2_556 . ? O501 Eu1 O103 74.3(5) . . ? O101 Eu1 O103 135.6(4) . . ? O104 Eu1 O103 78.3(4) . . ? O502 Eu1 O103 67.1(4) . . ? O105 Eu1 O103 132.7(4) . . ? O102 Eu1 O103 55.6(4) . . ? O105 Eu1 Eu1 36.8(3) 2_556 2_556 ? O501 Eu1 Eu1 112.7(4) . 2_556 ? O101 Eu1 Eu1 72.3(3) . 2_556 ? O104 Eu1 Eu1 72.7(3) . 2_556 ? O502 Eu1 Eu1 110.2(3) . 2_556 ? O105 Eu1 Eu1 34.1(3) . 2_556 ? O102 Eu1 Eu1 152.3(3) . 2_556 ? O103 Eu1 Eu1 151.0(3) . 2_556 ? C101 O101 Eu1 121.5(10) . . ? C150 O102 Eu1 139.0(11) . . ? C139 O103 Eu1 141.5(12) . . ? C128 O104 Eu1 124.8(11) . . ? C117 O105 Eu1 135.7(12) . 2_556 ? C117 O105 Eu1 115.3(12) . . ? Eu1 O105 Eu1 109.1(4) 2_556 . ? O501 S1 C512 110.1(13) . . ? O501 S1 C511 110.3(18) . . ? C512 S1 C511 98.9(11) . . ? S1 O501 Eu1 168.8(11) . . ? O502 S2 C521 105.3(11) . . ? O502 S2 C522 106.0(13) . . ? C521 S2 C522 99.1(9) . . ? S2 O502 Eu1 136.2(8) . . ? C102 C101 O101 123.1(20) . . ? C102 C101 C106 119.9(20) . . ? O101 C101 C106 117.0(19) . . ? C101 C102 C103 120.8(21) . . ? C101 C102 C111 121.4(19) . . ? C103 C102 C111 117.9(19) . . ? C102 C103 C104 122.5(20) . . ? C103 C104 C105 118.4(18) . . ? C103 C104 C107 122.2(19) . . ? C105 C104 C107 119.3(19) . . ? C104 C105 C106 117.1(20) . . ? C101 C106 C105 121.2(20) . . ? C101 C106 C155 120.3(19) . . ? C105 C106 C155 118.4(19) . . ? C108 C107 C109 109.2(18) . . ? C108 C107 C110 108.6(18) . . ? C109 C107 C110 108.3(18) . . ? C108 C107 C104 107.3(20) . . ? C109 C107 C104 110.3(19) . . ? C110 C107 C104 113.2(20) . . ? C112 C111 C102 116.8(15) . . ? C113 C112 C117 116.5(18) . . ? C113 C112 C111 120.9(18) . . ? C117 C112 C111 122.6(18) . . ? C114 C113 C112 124.7(19) . . ? C115 C114 C113 116.3(18) . . ? C115 C114 C118 123.3(18) . . ? C113 C114 C118 120.4(18) . . ? C116 C115 C114 125.3(20) . . ? C115 C116 C117 116.0(18) . . ? C115 C116 C122 121.6(19) . . ? C117 C116 C122 122.2(17) . . ? O105 C117 C112 120.5(17) . . ? O105 C117 C116 118.2(16) . . ? C112 C117 C116 121.2(15) . . ? C120 C118 C121 111.0(18) . . ? C120 C118 C119 110.5(18) . . ? C121 C118 C119 104.2(18) . . ? C120 C118 C114 108.6(20) . . ? C121 C118 C114 110.0(19) . . ? C119 C118 C114 112.5(20) . . ? C116 C122 C123 120.4(16) . . ? C128 C123 C124 121.5(20) . . ? C128 C123 C122 121.2(19) . . ? C124 C123 C122 117.2(18) . . ? C125 C124 C123 120.4(19) . . ? C124 C125 C126 121.2(18) . . ? C124 C125 C129 120.2(19) . . ? C126 C125 C129 118.5(19) . . ? C127 C126 C125 116.8(20) . . ? C126 C127 C128 120.7(20) . . ? C126 C127 C133 119.2(20) . . ? C128 C127 C133 119.2(19) . . ? O104 C128 C123 121.8(20) . . ? O104 C128 C127 118.9(19) . . ? C123 C128 C127 119.3(20) . . ? C130 C129 C132 112.9(19) . . ? C130 C129 C125 111.1(19) . . ? C132 C129 C125 114.6(21) . . ? C130 C129 C131 108.7(18) . . ? C132 C129 C131 104.3(17) . . ? C125 C129 C131 104.5(18) . . ? C127 C133 C134 112.9(16) . . ? C139 C134 C135 119.6(21) . . ? C139 C134 C133 121.9(20) . . ? C135 C134 C133 118.2(18) . . ? C134 C135 C136 120.5(19) . . ? C137 C136 C135 118.1(19) . . ? C137 C136 C140 120.1(19) . . ? C135 C136 C140 121.7(18) . . ? C136 C137 C138 126.0(21) . . ? C137 C138 C139 113.2(19) . . ? C137 C138 C144 124.1(20) . . ? C139 C138 C144 122.3(20) . . ? O103 C139 C134 122.3(21) . . ? O103 C139 C138 115.3(19) . . ? C134 C139 C138 122.5(21) . . ? C141 C140 C143 118.4(19) . . ? C141 C140 C136 106.0(20) . . ? C143 C140 C136 106.6(20) . . ? C141 C140 C142 104.0(17) . . ? C143 C140 C142 109.1(18) . . ? C136 C140 C142 113.0(21) . . ? C145 C144 C138 113.9(15) . . ? C146 C145 C144 120.8(20) . . ? C146 C145 C150 117.4(19) . . ? C144 C145 C150 121.6(19) . . ? C147 C146 C145 121.8(20) . . ? C146 C147 C148 118.5(19) . . ? C146 C147 C151 123.3(20) . . ? C148 C147 C151 118.2(18) . . ? C149 C148 C147 122.0(19) . . ? C148 C149 C150 120.2(22) . . ? C148 C149 C155 120.2(19) . . ? C150 C149 C155 119.2(20) . . ? O102 C150 C149 123.1(21) . . ? O102 C150 C145 117.1(19) . . ? C149 C150 C145 119.7(21) . . ? C153 C151 C152 118.2(20) . . ? C153 C151 C147 108.1(19) . . ? C152 C151 C147 111.8(21) . . ? C153 C151 C154 106.7(17) . . ? C152 C151 C154 101.6(17) . . ? C147 C151 C154 110.0(20) . . ? C106 C155 C149 116.7(16) . . ? O505 Eu3 O301 99.6(5) . . ? O505 Eu3 O305 75.0(5) . 2_557 ? O301 Eu3 O305 78.7(4) . 2_557 ? O505 Eu3 O304 102.1(5) . . ? O301 Eu3 O304 144.1(4) . . ? O305 Eu3 O304 79.8(4) 2_557 . ? O505 Eu3 O506 136.9(4) . . ? O301 Eu3 O506 90.5(4) . . ? O305 Eu3 O506 148.0(4) 2_557 . ? O304 Eu3 O506 92.8(4) . . ? O505 Eu3 O305 147.7(4) . . ? O301 Eu3 O305 73.2(4) . . ? O305 Eu3 O305 72.7(5) 2_557 . ? O304 Eu3 O305 73.1(4) . . ? O506 Eu3 O305 75.3(4) . . ? O505 Eu3 O303 75.5(5) . . ? O301 Eu3 O303 134.3(4) . . ? O305 Eu3 O303 139.0(4) 2_557 . ? O304 Eu3 O303 79.3(4) . . ? O506 Eu3 O303 67.9(4) . . ? O305 Eu3 O303 132.2(4) . . ? O505 Eu3 O302 73.9(5) . . ? O301 Eu3 O302 79.5(4) . . ? O305 Eu3 O302 138.0(4) 2_557 . ? O304 Eu3 O302 134.1(4) . . ? O506 Eu3 O302 66.9(4) . . ? O305 Eu3 O302 132.6(4) . . ? O303 Eu3 O302 55.2(4) . . ? O505 Eu3 Eu3 112.8(3) . 2_557 ? O301 Eu3 Eu3 72.3(3) . 2_557 ? O305 Eu3 Eu3 37.8(3) 2_557 2_557 ? O304 Eu3 Eu3 73.0(3) . 2_557 ? O506 Eu3 Eu3 110.2(3) . 2_557 ? O305 Eu3 Eu3 34.9(3) . 2_557 ? O303 Eu3 Eu3 152.1(3) . 2_557 ? O302 Eu3 Eu3 151.7(3) . 2_557 ? C301 O301 Eu3 123.1(10) . . ? C350 O302 Eu3 141.4(12) . . ? C339 O303 Eu3 139.2(11) . . ? C328 O304 Eu3 122.5(11) . . ? C317 O305 Eu3 135.8(13) . 2_557 ? C317 O305 Eu3 116.9(12) . . ? Eu3 O305 Eu3 107.3(5) 2_557 . ? O505 S5 C551 109.7(15) . . ? O505 S5 C552 108.4(15) . . ? C551 S5 C552 97.4(16) . . ? S5 O505 Eu3 168.6(9) . . ? O506 S6 C561 103.9(10) . . ? O506 S6 C562 105.6(10) . . ? C561 S6 C562 97.3(12) . . ? S6 O506 Eu3 136.6(8) . . ? O301 C301 C302 119.6(21) . . ? O301 C301 C306 119.7(19) . . ? C302 C301 C306 120.7(20) . . ? C303 C302 C301 121.9(22) . . ? C303 C302 C355 117.6(19) . . ? C301 C302 C355 120.0(19) . . ? C302 C303 C304 119.5(20) . . ? C305 C304 C303 118.4(19) . . ? C305 C304 C307 117.8(20) . . ? C303 C304 C307 123.5(19) . . ? C304 C305 C306 123.0(21) . . ? C305 C306 C301 116.5(20) . . ? C305 C306 C311 118.7(20) . . ? C301 C306 C311 124.8(19) . . ? C308 C307 C310 112.1(18) . . ? C308 C307 C309 110.9(19) . . ? C310 C307 C309 104.9(17) . . ? C308 C307 C304 111.2(20) . . ? C310 C307 C304 110.8(21) . . ? C309 C307 C304 106.7(19) . . ? C312 C311 C306 116.6(16) . . ? C313 C312 C317 115.2(19) . . ? C313 C312 C311 120.9(19) . . ? C317 C312 C311 123.6(20) . . ? C312 C313 C314 127.1(20) . . ? C315 C314 C313 113.8(19) . . ? C315 C314 C318 125.2(18) . . ? C313 C314 C318 121.0(18) . . ? C316 C315 C314 122.8(20) . . ? C315 C316 C317 120.8(21) . . ? C315 C316 C322 117.1(19) . . ? C317 C316 C322 122.0(20) . . ? O305 C317 C316 120.3(19) . . ? O305 C317 C312 119.3(19) . . ? C316 C317 C312 120.4(21) . . ? C320 C318 C319 110.1(18) . . ? C320 C318 C314 110.2(20) . . ? C319 C318 C314 116.6(20) . . ? C320 C318 C321 109.1(18) . . ? C319 C318 C321 102.4(18) . . ? C314 C318 C321 108.0(19) . . ? C316 C322 C323 117.4(16) . . ? C328 C323 C324 122.3(21) . . ? C328 C323 C322 122.2(19) . . ? C324 C323 C322 115.6(19) . . ? C323 C324 C325 116.0(20) . . ? C326 C325 C324 122.9(19) . . ? C326 C325 C329 121.5(20) . . ? C324 C325 C329 115.6(19) . . ? C325 C326 C327 119.4(20) . . ? C328 C327 C326 118.6(21) . . ? C328 C327 C333 121.4(20) . . ? C326 C327 C333 119.7(19) . . ? O304 C328 C327 119.3(21) . . ? O304 C328 C323 119.9(20) . . ? C327 C328 C323 120.8(21) . . ? C331 C329 C330 109.0(18) . . ? C331 C329 C332 107.4(18) . . ? C330 C329 C332 108.1(18) . . ? C331 C329 C325 112.2(21) . . ? C330 C329 C325 109.6(18) . . ? C332 C329 C325 110.4(19) . . ? C327 C333 C334 115.7(16) . . ? C339 C334 C335 120.6(21) . . ? C339 C334 C333 120.6(21) . . ? C335 C334 C333 118.3(19) . . ? C334 C335 C336 119.5(19) . . ? C337 C336 C335 117.8(20) . . ? C337 C336 C340 124.1(19) . . ? C335 C336 C340 118.0(18) . . ? C336 C337 C338 123.0(21) . . ? C337 C338 C339 117.7(20) . . ? C337 C338 C344 120.9(19) . . ? C339 C338 C344 121.4(21) . . ? C334 C339 O303 123.2(20) . . ? C334 C339 C338 120.9(22) . . ? O303 C339 C338 115.9(19) . . ? C342 C340 C341 108.3(18) . . ? C342 C340 C343 106.6(18) . . ? C341 C340 C343 106.5(19) . . ? C342 C340 C336 103.4(20) . . ? C341 C340 C336 115.8(20) . . ? C343 C340 C336 115.7(21) . . ? C345 C344 C338 115.4(16) . . ? C346 C345 C344 123.2(19) . . ? C346 C345 C350 113.6(19) . . ? C344 C345 C350 122.9(20) . . ? C347 C346 C345 125.1(20) . . ? C346 C347 C348 118.0(19) . . ? C346 C347 C351 124.0(19) . . ? C348 C347 C351 118.0(18) . . ? C349 C348 C347 119.6(19) . . ? C350 C349 C348 121.6(21) . . ? C350 C349 C355 119.7(20) . . ? C348 C349 C355 118.4(19) . . ? O302 C350 C349 125.3(20) . . ? O302 C350 C345 112.8(18) . . ? C349 C350 C345 121.8(21) . . ? C352 C351 C353 115.1(19) . . ? C352 C351 C354 112.9(20) . . ? C353 C351 C354 102.3(17) . . ? C352 C351 C347 109.4(20) . . ? C353 C351 C347 105.3(20) . . ? C354 C351 C347 111.5(21) . . ? C302 C355 C349 115.9(16) . . ? C611 O610 C614 112.6(21) . . ? O610 C611 C612 98.1(21) . . ? C613 C612 C611 109.7(17) . . ? C614 C613 C612 101.9(25) . . ? C613 C614 O610 100.9(23) . . ? C624 O620 C621 120.4(11) . . ? O620 C621 C622 101.2(11) . . ? C621 C622 C623 107.9(13) . . ? C624 C623 C622 105.1(13) . . ? O620 C624 C623 102.5(12) . . ? C634 O630 C631 121.7(13) . . ? O630 C631 C632 99.6(10) . . ? C633 C632 C631 109.6(10) . . ? C632 C633 C634 107.1(10) . . ? O630 C634 C633 101.0(11) . . ? C641 O640 C644 121.1(13) . . ? O640 C641 C642 101.5(10) . . ? C643 C642 C641 107.2(11) . . ? C642 C643 C644 107.6(14) . . ? O640 C644 C643 99.6(13) . . ? C654 O650 C651 121.3(12) . . ? O650 C651 C652 100.8(10) . . ? C653 C652 C651 108.4(11) . . ? C652 C653 C654 107.8(10) . . ? O650 C654 C653 101.3(10) . . ? C661 O660 C664 118.7(18) . . ? O660 C661 C662 100.7(10) . . ? C663 C662 C661 108.6(10) . . ? C662 C663 C664 107.0(14) . . ? O660 C664 C663 98.6(16) . . ? C674 O670 C671 120.5(11) . . ? O670 C671 C672 101.2(10) . . ? C671 C672 C673 108.8(11) . . ? C674 C673 C672 106.6(11) . . ? O670 C674 C673 102.3(10) . . ? C681 O680 C684 119.3(12) . . ? O680 C681 C682 102.5(10) . . ? C681 C682 C683 107.6(10) . . ? C684 C683 C682 107.9(10) . . ? O680 C684 C683 102.6(10) . . ? C694 O690 C691 122.2(14) . . ? O690 C691 C692 99.4(15) . . ? C693 C692 C691 105.6(19) . . ? C692 C693 C694 106.7(16) . . ? O690 C694 C693 100.4(12) . . ? C701 O700 C704 119.1(15) . . ? O700 C701 C702 102.0(13) . . ? C701 C702 C703 106.8(13) . . ? C704 C703 C702 107.8(11) . . ? O700 C704 C703 102.4(11) . . ? _refine_diff_density_max 1.106 _refine_diff_density_min -1.179 _refine_diff_density_rms 0.164