Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Shaowu Wang' _publ_contact_author_address ; School of Chemistry and Materials Science Anhui Normal University Institute of Organic Chemistry Wuhu Anhui 241000 CHINA ; _publ_contact_author_email SWWANG@MAIL.AHNU.EDU.CN _publ_section_title ; Homolysis of the Ln-N (Ln = Yb, Eu) bond. Synthesis, structural characterization and catalytic activity of ytterbium(II) and europium(II) complexes with methoxyethyl functionalized indenyl ligands ; loop_ _publ_author_name 'Shaowu Wang' 'Yan Feng' 'Zi-Xiang Huang' 'Lili Mao' 'Enhong Sheng' ; Meihua Xie ; 'Gaosheng Yang' 'Kehua Zhang' 'Wu Zhang' 'Shuangliu Zhou' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 223636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 O2 Si2 Yb' _chemical_formula_weight 663.86 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.44030(10) _cell_length_b 15.96720(10) _cell_length_c 18.5576(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.2900(10) _cell_angle_gamma 90.00 _cell_volume 3080.42(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12592 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 25.06 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 3.137 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5789 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 15911 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.06 _reflns_number_total 8195 _reflns_number_gt 7436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens SMART & SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0186P)^2^+14.0249P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.055(14) _refine_ls_number_reflns 8195 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb -0.01253(4) 0.42531(3) 0.40195(2) 0.03817(11) Uani 1 1 d . . . Yb2 Yb 0.45647(4) 0.07452(3) 0.13217(2) 0.04098(12) Uani 1 1 d . . . Si1 Si 0.0971(4) 0.5969(2) 0.2519(2) 0.0736(11) Uani 1 1 d . . . Si2 Si -0.3028(3) 0.3200(2) 0.50973(16) 0.0522(8) Uani 1 1 d . . . Si3 Si 0.1656(3) 0.2373(3) 0.06035(18) 0.0610(9) Uani 1 1 d . . . Si4 Si 0.5908(3) -0.1590(2) 0.20418(17) 0.0579(8) Uani 1 1 d . . . O1 O 0.1126(9) 0.3979(5) 0.5188(5) 0.074(3) Uani 1 1 d . . . O2 O 0.1624(7) 0.3509(6) 0.3511(5) 0.071(3) Uani 1 1 d . . . O3 O 0.6408(7) 0.1066(6) 0.2183(5) 0.077(3) Uani 1 1 d . . . O4 O 0.5667(8) 0.1571(5) 0.0419(5) 0.069(2) Uani 1 1 d . . . C1 C 0.005(2) 0.5316(13) 0.1831(8) 0.182(13) Uani 1 1 d . . . H1A H -0.0851 0.5421 0.1842 0.273 Uiso 1 1 calc R . . H1B H 0.0226 0.4735 0.1932 0.273 Uiso 1 1 calc R . . H1C H 0.0305 0.5452 0.1360 0.273 Uiso 1 1 calc R . . C2 C 0.2734(19) 0.576(2) 0.2492(12) 0.225(17) Uani 1 1 d . . . H2A H 0.3215 0.6104 0.2845 0.338 Uiso 1 1 calc R . . H2B H 0.2981 0.5890 0.2019 0.338 Uiso 1 1 calc R . . H2C H 0.2908 0.5181 0.2598 0.338 Uiso 1 1 calc R . . C3 C 0.076(2) 0.7068(11) 0.2250(8) 0.128(7) Uani 1 1 d . . . H3A H -0.0130 0.7220 0.2254 0.192 Uiso 1 1 calc R . . H3B H 0.1020 0.7142 0.1771 0.192 Uiso 1 1 calc R . . H3C H 0.1274 0.7417 0.2583 0.192 Uiso 1 1 calc R . . C4 C 0.0562(9) 0.5789(9) 0.3461(6) 0.049(3) Uani 1 1 d . . . C5 C -0.0649(10) 0.5929(7) 0.3743(6) 0.045(3) Uani 1 1 d . . . C6 C -0.1890(11) 0.6148(8) 0.3445(8) 0.064(3) Uani 1 1 d . . . H6A H -0.2031 0.6211 0.2946 0.077 Uiso 1 1 calc R . . C7 C -0.2884(13) 0.6271(8) 0.3846(10) 0.076(4) Uani 1 1 d . . . H7A H -0.3683 0.6428 0.3625 0.091 Uiso 1 1 calc R . . C8 C -0.2709(17) 0.6162(8) 0.4602(11) 0.096(6) Uani 1 1 d . . . H8A H -0.3398 0.6239 0.4879 0.115 Uiso 1 1 calc R . . C9 C -0.1548(16) 0.5949(8) 0.4923(7) 0.076(4) Uani 1 1 d . . . H9A H -0.1451 0.5873 0.5422 0.091 Uiso 1 1 calc R . . C10 C -0.0489(10) 0.5837(7) 0.4531(6) 0.049(3) Uani 1 1 d . . . C11 C 0.0842(11) 0.5651(8) 0.4699(6) 0.055(3) Uani 1 1 d . . . C12 C 0.1437(11) 0.5630(8) 0.4062(7) 0.062(3) Uani 1 1 d . . . H12A H 0.2372 0.5604 0.4043 0.074 Uiso 1 1 calc R . . C13 C 0.1456(19) 0.5420(9) 0.5448(7) 0.100(6) Uani 1 1 d . . . H13A H 0.2357 0.5573 0.5467 0.120 Uiso 1 1 calc R . . H13B H 0.1069 0.5775 0.5793 0.120 Uiso 1 1 calc R . . C14 C 0.140(3) 0.4626(10) 0.5688(9) 0.180(13) Uani 1 1 d . . . H14A H 0.0753 0.4607 0.6031 0.216 Uiso 1 1 calc R . . H14B H 0.2219 0.4499 0.5955 0.216 Uiso 1 1 calc R . . C15 C 0.1634(17) 0.3180(10) 0.5415(10) 0.098(6) Uani 1 1 d . . . H15A H 0.2082 0.3228 0.5888 0.148 Uiso 1 1 calc R . . H15B H 0.2218 0.2989 0.5079 0.148 Uiso 1 1 calc R . . H15C H 0.0943 0.2786 0.5428 0.148 Uiso 1 1 calc R . . C16 C -0.1818(14) 0.3040(10) 0.5894(6) 0.080(4) Uani 1 1 d . . . H16A H -0.1316 0.2550 0.5818 0.121 Uiso 1 1 calc R . . H16B H -0.2256 0.2969 0.6323 0.121 Uiso 1 1 calc R . . H16C H -0.1263 0.3520 0.5950 0.121 Uiso 1 1 calc R . . C17 C -0.4204(14) 0.2314(10) 0.5067(7) 0.089(5) Uani 1 1 d . . . H17A H -0.4837 0.2388 0.4663 0.133 Uiso 1 1 calc R . . H17B H -0.4619 0.2304 0.5507 0.133 Uiso 1 1 calc R . . H17C H -0.3758 0.1795 0.5015 0.133 Uiso 1 1 calc R . . C18 C -0.4002(11) 0.4160(9) 0.5258(6) 0.069(3) Uani 1 1 d . . . H18A H -0.4632 0.4245 0.4854 0.104 Uiso 1 1 calc R . . H18B H -0.3444 0.4638 0.5311 0.104 Uiso 1 1 calc R . . H18C H -0.4429 0.4087 0.5690 0.104 Uiso 1 1 calc R . . C19 C -0.2176(10) 0.3247(6) 0.4262(5) 0.038(2) Uani 1 1 d . . . C20 C -0.2594(9) 0.3621(7) 0.3570(5) 0.043(3) Uani 1 1 d . . . C21 C -0.3605(9) 0.4161(9) 0.3341(6) 0.052(3) Uani 1 1 d . . . H21A H -0.4133 0.4373 0.3675 0.063 Uiso 1 1 calc R . . C22 C -0.3822(12) 0.4381(9) 0.2617(7) 0.067(3) Uani 1 1 d . . . H22A H -0.4500 0.4737 0.2469 0.080 Uiso 1 1 calc R . . C23 C -0.3035(12) 0.4076(10) 0.2108(6) 0.070(4) Uani 1 1 d . . . H23A H -0.3202 0.4220 0.1623 0.084 Uiso 1 1 calc R . . C24 C -0.2026(12) 0.3567(9) 0.2320(6) 0.060(3) Uani 1 1 d . . . H24A H -0.1494 0.3381 0.1977 0.072 Uiso 1 1 calc R . . C25 C -0.1765(9) 0.3313(7) 0.3052(5) 0.041(2) Uani 1 1 d . . . C26 C -0.0867(10) 0.2763(7) 0.3415(6) 0.046(3) Uani 1 1 d . . . C27 C -0.1139(10) 0.2720(7) 0.4132(5) 0.043(2) Uani 1 1 d . . . H27A H -0.0783 0.2294 0.4473 0.051 Uiso 1 1 calc R . . C28 C 0.0278(10) 0.2363(8) 0.3094(7) 0.065(3) Uani 1 1 d . . . H28A H 0.0635 0.1932 0.3422 0.078 Uiso 1 1 calc R . . H28B H -0.0022 0.2092 0.2642 0.078 Uiso 1 1 calc R . . C29 C 0.1282(15) 0.2943(13) 0.2961(13) 0.148(10) Uani 1 1 d . . . H29A H 0.2041 0.2625 0.2867 0.177 Uiso 1 1 calc R . . H29B H 0.1012 0.3256 0.2525 0.177 Uiso 1 1 calc R . . C30 C 0.2947(13) 0.3640(12) 0.3659(10) 0.118(7) Uani 1 1 d . . . H30A H 0.3408 0.3260 0.3376 0.177 Uiso 1 1 calc R . . H30B H 0.3189 0.3543 0.4164 0.177 Uiso 1 1 calc R . . H30C H 0.3153 0.4206 0.3539 0.177 Uiso 1 1 calc R . . C31 C -0.0064(13) 0.2218(19) 0.0622(11) 0.207(16) Uani 1 1 d . . . H31A H -0.0250 0.1629 0.0620 0.310 Uiso 1 1 calc R . . H31B H -0.0510 0.2475 0.0203 0.310 Uiso 1 1 calc R . . H31C H -0.0342 0.2468 0.1052 0.310 Uiso 1 1 calc R . . C32 C 0.216(2) 0.2023(14) -0.0264(7) 0.138(9) Uani 1 1 d . . . H32A H 0.2015 0.1431 -0.0315 0.207 Uiso 1 1 calc R . . H32B H 0.3056 0.2140 -0.0283 0.207 Uiso 1 1 calc R . . H32C H 0.1668 0.2312 -0.0650 0.207 Uiso 1 1 calc R . . C33 C 0.199(3) 0.3525(13) 0.0645(12) 0.169(10) Uani 1 1 d . . . H33A H 0.1734 0.3748 0.1090 0.253 Uiso 1 1 calc R . . H33B H 0.1514 0.3798 0.0244 0.253 Uiso 1 1 calc R . . H33C H 0.2893 0.3620 0.0621 0.253 Uiso 1 1 calc R . . C34 C 0.2568(9) 0.1869(7) 0.1384(5) 0.043(3) Uani 1 1 d . . . C35 C 0.2239(10) 0.1192(7) 0.1818(6) 0.049(3) Uani 1 1 d . . . C36 C 0.1187(12) 0.0626(9) 0.1770(8) 0.075(4) Uani 1 1 d . . . H36A H 0.0568 0.0644 0.1376 0.090 Uiso 1 1 calc R . . C37 C 0.1093(14) 0.0021(10) 0.2342(10) 0.096(6) Uani 1 1 d . . . H37A H 0.0429 -0.0369 0.2322 0.115 Uiso 1 1 calc R . . C38 C 0.2041(18) 0.0046(10) 0.2926(9) 0.090(5) Uani 1 1 d . . . H38A H 0.1977 -0.0348 0.3291 0.107 Uiso 1 1 calc R . . C39 C 0.3018(16) 0.0573(11) 0.3011(7) 0.084(4) Uani 1 1 d . . . H39A H 0.3588 0.0567 0.3427 0.101 Uiso 1 1 calc R . . C40 C 0.3160(12) 0.1138(8) 0.2455(6) 0.062(4) Uani 1 1 d . . . C41 C 0.4054(12) 0.1811(9) 0.2402(6) 0.060(3) Uani 1 1 d . . . C42 C 0.3676(10) 0.2229(8) 0.1769(6) 0.054(3) Uani 1 1 d . . . H42A H 0.4037 0.2770 0.1641 0.064 Uiso 1 1 calc R . . C43 C 0.5240(15) 0.1962(14) 0.2908(10) 0.138(9) Uani 1 1 d . . . H43A H 0.5577 0.2511 0.2803 0.165 Uiso 1 1 calc R . . H43B H 0.4991 0.1978 0.3399 0.165 Uiso 1 1 calc R . . C44 C 0.6208(13) 0.1392(12) 0.2882(8) 0.090(5) Uani 1 1 d . . . H44A H 0.6034 0.0925 0.3194 0.108 Uiso 1 1 calc R . . H44B H 0.7003 0.1650 0.3083 0.108 Uiso 1 1 calc R . . C45 C 0.7696(12) 0.1047(11) 0.2029(10) 0.113(7) Uani 1 1 d . . . H45A H 0.8241 0.1202 0.2453 0.170 Uiso 1 1 calc R . . H45B H 0.7818 0.1433 0.1645 0.170 Uiso 1 1 calc R . . H45C H 0.7913 0.0492 0.1883 0.170 Uiso 1 1 calc R . . C46 C 0.7696(14) -0.1438(12) 0.2182(8) 0.102(5) Uani 1 1 d . . . H46A H 0.8074 -0.1586 0.1747 0.153 Uiso 1 1 calc R . . H46B H 0.8046 -0.1788 0.2572 0.153 Uiso 1 1 calc R . . H46C H 0.7882 -0.0862 0.2297 0.153 Uiso 1 1 calc R . . C47 C 0.5573(15) -0.2715(10) 0.1859(8) 0.093(5) Uani 1 1 d . . . H47A H 0.4660 -0.2803 0.1789 0.139 Uiso 1 1 calc R . . H47B H 0.5929 -0.3044 0.2262 0.139 Uiso 1 1 calc R . . H47C H 0.5957 -0.2882 0.1430 0.139 Uiso 1 1 calc R . . C48 C 0.5165(17) -0.1330(11) 0.2894(7) 0.103(6) Uani 1 1 d . . . H48A H 0.4250 -0.1408 0.2820 0.155 Uiso 1 1 calc R . . H48B H 0.5348 -0.0757 0.3023 0.155 Uiso 1 1 calc R . . H48C H 0.5514 -0.1691 0.3277 0.155 Uiso 1 1 calc R . . C49 C 0.5256(11) -0.0921(9) 0.1272(6) 0.056(3) Uani 1 1 d . . . C50 C 0.3933(12) -0.0918(7) 0.0956(6) 0.051(3) Uani 1 1 d . . . C51 C 0.2792(13) -0.1255(9) 0.1162(7) 0.071(4) Uani 1 1 d . . . H51A H 0.2794 -0.1555 0.1592 0.085 Uiso 1 1 calc R . . C52 C 0.1664(16) -0.1144(10) 0.0731(8) 0.086(5) Uani 1 1 d . . . H52A H 0.0918 -0.1390 0.0869 0.103 Uiso 1 1 calc R . . C53 C 0.1594(17) -0.0686(13) 0.0107(8) 0.100(5) Uani 1 1 d . . . H53A H 0.0811 -0.0627 -0.0171 0.120 Uiso 1 1 calc R . . C54 C 0.2667(19) -0.0320(10) -0.0107(8) 0.087(5) Uani 1 1 d . . . H54A H 0.2607 0.0005 -0.0525 0.105 Uiso 1 1 calc R . . C55 C 0.3883(13) -0.0422(8) 0.0297(7) 0.062(3) Uani 1 1 d . . . C56 C 0.5130(15) -0.0165(8) 0.0203(6) 0.063(4) Uani 1 1 d . . . C57 C 0.5947(13) -0.0495(8) 0.0769(7) 0.069(4) Uani 1 1 d . . . H57A H 0.6888 -0.0494 0.0780 0.082 Uiso 1 1 calc R . . C58 C 0.5501(19) 0.0411(10) -0.0412(8) 0.105(6) Uani 1 1 d . . . H58A H 0.6002 0.0093 -0.0732 0.126 Uiso 1 1 calc R . . H58B H 0.4725 0.0601 -0.0692 0.126 Uiso 1 1 calc R . . C59 C 0.6246(15) 0.1139(10) -0.0142(7) 0.082(4) Uani 1 1 d . . . H59A H 0.7101 0.0958 0.0042 0.098 Uiso 1 1 calc R . . H59C H 0.6334 0.1523 -0.0540 0.098 Uiso 1 1 calc R . . C60 C 0.6051(17) 0.2440(9) 0.0510(10) 0.107(6) Uani 1 1 d . . . H60D H 0.6455 0.2622 0.0093 0.160 Uiso 1 1 calc R . . H60A H 0.6647 0.2494 0.0933 0.160 Uiso 1 1 calc R . . H60B H 0.5307 0.2779 0.0564 0.160 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 Yb1 0.0381(2) 0.0286(2) 0.0475(2) -0.0053(2) 0.00256(16) -0.0013(2) Yb2 0.0397(2) 0.0422(3) 0.0423(2) -0.0060(2) 0.01009(16) 0.0004(2) Si1 0.091(3) 0.063(3) 0.071(2) 0.0078(18) 0.0281(19) -0.010(2) Si2 0.0617(19) 0.050(2) 0.0470(17) -0.0002(14) 0.0157(14) -0.0110(16) Si3 0.0573(19) 0.070(2) 0.0577(19) 0.0200(18) 0.0136(15) 0.0138(18) Si4 0.068(2) 0.057(2) 0.0490(17) -0.0019(15) 0.0091(15) 0.0118(17) O1 0.096(7) 0.037(5) 0.084(6) -0.002(4) -0.025(5) 0.003(4) O2 0.046(5) 0.059(6) 0.112(7) -0.036(5) 0.022(4) -0.003(4) O3 0.035(4) 0.099(8) 0.094(6) -0.019(5) -0.005(4) -0.001(4) O4 0.078(6) 0.048(5) 0.089(6) 0.010(5) 0.048(5) -0.004(5) C1 0.32(3) 0.16(2) 0.073(11) -0.050(12) 0.072(15) -0.15(2) C2 0.152(19) 0.33(4) 0.22(2) 0.15(3) 0.131(19) 0.13(3) C3 0.21(2) 0.090(14) 0.085(11) 0.032(10) 0.027(12) -0.014(14) C4 0.049(6) 0.036(6) 0.064(6) 0.009(7) 0.016(5) -0.001(6) C5 0.053(6) 0.029(7) 0.053(6) -0.001(5) 0.001(5) 0.009(5) C6 0.043(7) 0.044(7) 0.106(10) 0.007(7) 0.004(6) 0.002(6) C7 0.046(8) 0.042(8) 0.139(14) 0.008(8) 0.002(8) 0.011(6) C8 0.106(13) 0.036(8) 0.156(16) 0.003(9) 0.066(12) 0.031(8) C9 0.126(13) 0.034(8) 0.072(8) -0.005(6) 0.031(8) 0.005(8) C10 0.066(7) 0.022(6) 0.062(6) -0.004(5) 0.012(5) 0.001(6) C11 0.076(8) 0.025(6) 0.063(7) -0.011(6) -0.006(6) -0.007(6) C12 0.051(6) 0.030(7) 0.100(9) 0.000(7) -0.016(6) -0.025(6) C13 0.179(17) 0.052(10) 0.060(9) -0.012(7) -0.037(10) -0.020(10) C14 0.39(4) 0.043(10) 0.084(12) -0.015(9) -0.114(17) 0.026(15) C15 0.092(12) 0.066(12) 0.129(15) 0.011(10) -0.031(10) 0.015(9) C16 0.112(11) 0.088(11) 0.042(7) -0.001(7) 0.005(7) 0.003(9) C17 0.103(11) 0.094(12) 0.074(9) 0.002(8) 0.032(8) -0.057(10) C18 0.084(8) 0.068(9) 0.059(7) 0.000(7) 0.028(6) 0.013(8) C19 0.047(6) 0.034(6) 0.031(5) 0.000(4) 0.000(4) -0.002(5) C20 0.034(6) 0.048(7) 0.047(6) -0.007(5) 0.010(4) -0.005(5) C21 0.047(6) 0.050(7) 0.060(6) -0.003(6) 0.004(5) -0.006(6) C22 0.063(7) 0.050(9) 0.085(9) 0.000(7) -0.005(6) 0.012(7) C23 0.077(8) 0.087(12) 0.043(6) 0.013(7) -0.004(5) -0.003(8) C24 0.070(8) 0.063(9) 0.048(7) -0.001(6) 0.017(6) -0.014(7) C25 0.047(6) 0.036(6) 0.040(5) -0.005(4) 0.009(4) -0.008(5) C26 0.041(6) 0.037(6) 0.063(7) -0.003(5) 0.013(5) 0.001(5) C27 0.051(6) 0.028(6) 0.049(6) -0.002(5) 0.001(5) -0.002(5) C28 0.038(6) 0.060(9) 0.099(9) -0.025(7) 0.010(6) 0.001(6) C29 0.061(10) 0.119(17) 0.27(3) -0.119(18) 0.074(13) -0.032(11) C30 0.048(9) 0.118(16) 0.184(18) -0.045(13) -0.009(10) 0.007(9) C31 0.034(8) 0.38(4) 0.20(2) 0.20(3) -0.005(10) 0.023(14) C32 0.20(2) 0.16(2) 0.050(9) 0.010(10) 0.017(10) 0.085(17) C33 0.25(3) 0.076(14) 0.18(2) 0.048(14) 0.03(2) 0.041(17) C34 0.042(6) 0.047(7) 0.040(6) 0.008(5) 0.013(4) 0.005(5) C35 0.041(6) 0.050(7) 0.060(7) 0.011(5) 0.020(5) 0.013(5) C36 0.053(7) 0.054(9) 0.122(11) 0.001(9) 0.023(7) 0.002(7) C37 0.054(9) 0.076(11) 0.168(17) 0.000(11) 0.062(10) -0.027(8) C38 0.103(13) 0.064(11) 0.106(13) 0.027(9) 0.033(10) 0.008(10) C39 0.111(11) 0.090(13) 0.054(7) 0.002(8) 0.027(7) 0.022(11) C40 0.075(8) 0.077(9) 0.037(6) 0.013(6) 0.019(5) 0.039(7) C41 0.065(8) 0.074(9) 0.041(6) -0.018(6) 0.007(5) 0.014(7) C42 0.045(6) 0.047(7) 0.070(8) -0.021(6) 0.011(5) -0.003(6) C43 0.065(10) 0.20(2) 0.133(15) -0.103(15) -0.040(9) 0.045(13) C44 0.049(8) 0.144(16) 0.073(10) -0.010(10) -0.018(7) -0.029(9) C45 0.054(8) 0.118(17) 0.172(16) -0.060(12) 0.033(9) -0.037(9) C46 0.092(11) 0.129(16) 0.083(10) 0.010(10) 0.001(8) 0.020(10) C47 0.115(12) 0.078(11) 0.086(10) 0.031(9) 0.011(8) 0.005(10) C48 0.141(15) 0.116(14) 0.054(8) 0.009(8) 0.019(8) 0.027(12) C49 0.067(7) 0.062(10) 0.039(6) -0.008(6) 0.009(5) 0.009(7) C50 0.073(8) 0.031(8) 0.046(6) -0.014(5) 0.000(5) 0.007(6) C51 0.076(9) 0.070(10) 0.064(8) -0.005(7) -0.005(7) -0.023(8) C52 0.098(12) 0.069(10) 0.087(11) -0.020(8) -0.012(9) -0.026(8) C53 0.107(12) 0.105(14) 0.083(10) -0.009(11) -0.029(9) -0.029(13) C54 0.130(15) 0.059(10) 0.065(9) -0.020(7) -0.033(9) 0.014(10) C55 0.082(9) 0.045(8) 0.058(7) -0.017(6) -0.002(7) 0.010(7) C56 0.104(11) 0.057(8) 0.032(6) 0.001(5) 0.020(6) 0.019(7) C57 0.075(9) 0.070(11) 0.066(8) -0.010(7) 0.030(7) 0.008(7) C58 0.173(17) 0.080(12) 0.073(10) 0.001(8) 0.065(10) 0.001(12) C59 0.102(11) 0.070(10) 0.079(9) 0.028(8) 0.043(8) -0.005(9) C60 0.121(14) 0.047(10) 0.164(16) -0.007(10) 0.076(12) -0.022(9) _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 Yb1 O2 2.440(8) . ? Yb1 O1 2.466(8) . ? Yb1 C27 2.682(11) . ? Yb1 C11 2.711(11) . ? Yb1 C26 2.713(11) . ? Yb1 C12 2.734(11) . ? Yb1 C10 2.740(11) . ? Yb1 C19 2.746(10) . ? Yb1 C5 2.769(11) . ? Yb1 C4 2.782(13) . ? Yb1 C25 2.800(10) . ? Yb1 C20 2.821(10) . ? Yb2 O3 2.440(8) . ? Yb2 O4 2.495(7) . ? Yb2 C56 2.645(11) . ? Yb2 C42 2.703(11) . ? Yb2 C57 2.707(12) . ? Yb2 C55 2.711(11) . ? Yb2 C41 2.720(11) . ? Yb2 C40 2.745(10) . ? Yb2 C49 2.761(14) . ? Yb2 C34 2.762(10) . ? Yb2 C35 2.769(10) . ? Yb2 C50 2.805(12) . ? Si1 C3 1.832(17) . ? Si1 C1 1.848(17) . ? Si1 C4 1.859(10) . ? Si1 C2 1.876(18) . ? Si2 C19 1.859(10) . ? Si2 C17 1.870(13) . ? Si2 C16 1.871(12) . ? Si2 C18 1.879(13) . ? Si3 C31 1.817(15) . ? Si3 C32 1.826(15) . ? Si3 C34 1.843(10) . ? Si3 C33 1.87(2) . ? Si4 C47 1.856(16) . ? Si4 C49 1.861(12) . ? Si4 C48 1.872(13) . ? Si4 C46 1.876(15) . ? O1 C14 1.399(16) . ? O1 C15 1.431(16) . ? O2 C29 1.385(18) . ? O2 C30 1.400(15) . ? O3 C45 1.401(14) . ? O3 C44 1.431(16) . ? O4 C59 1.428(16) . ? O4 C60 1.450(16) . ? C4 C12 1.399(14) . ? C4 C5 1.429(14) . ? C5 C6 1.405(15) . ? C5 C10 1.464(14) . ? C6 C7 1.346(19) . ? C7 C8 1.41(2) . ? C8 C9 1.34(2) . ? C9 C10 1.390(17) . ? C10 C11 1.427(15) . ? C11 C12 1.384(16) . ? C11 C13 1.522(16) . ? C13 C14 1.35(2) . ? C19 C27 1.410(14) . ? C19 C20 1.446(14) . ? C20 C21 1.399(15) . ? C20 C25 1.438(13) . ? C21 C22 1.388(15) . ? C22 C23 1.396(17) . ? C23 C24 1.360(18) . ? C24 C25 1.421(15) . ? C25 C26 1.409(15) . ? C26 C27 1.388(14) . ? C26 C28 1.525(14) . ? C28 C29 1.44(2) . ? C34 C35 1.409(15) . ? C34 C42 1.423(14) . ? C35 C36 1.419(17) . ? C35 C40 1.456(15) . ? C36 C37 1.44(2) . ? C37 C38 1.40(2) . ? C38 C39 1.32(2) . ? C39 C40 1.388(18) . ? C40 C41 1.432(18) . ? C41 C42 1.378(16) . ? C41 C43 1.503(17) . ? C43 C44 1.36(2) . ? C49 C57 1.407(17) . ? C49 C50 1.451(16) . ? C50 C51 1.392(17) . ? C50 C55 1.454(17) . ? C51 C52 1.373(19) . ? C52 C53 1.36(2) . ? C53 C54 1.36(2) . ? C54 C55 1.42(2) . ? C55 C56 1.391(18) . ? C56 C57 1.394(17) . ? C56 C58 1.543(18) . ? C58 C59 1.46(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 O2 Yb1 O1 84.2(3) . . ? O2 Yb1 C27 84.3(3) . . ? O1 Yb1 C27 87.2(3) . . ? O2 Yb1 C11 108.7(3) . . ? O1 Yb1 C11 66.0(3) . . ? C27 Yb1 C11 147.9(3) . . ? O2 Yb1 C26 66.9(3) . . ? O1 Yb1 C26 108.5(3) . . ? C27 Yb1 C26 29.8(3) . . ? C11 Yb1 C26 173.7(3) . . ? O2 Yb1 C12 86.4(4) . . ? O1 Yb1 C12 81.4(3) . . ? C27 Yb1 C12 165.9(3) . . ? C11 Yb1 C12 29.4(3) . . ? C26 Yb1 C12 149.8(4) . . ? O2 Yb1 C10 135.7(3) . . ? O1 Yb1 C10 86.4(3) . . ? C27 Yb1 C10 138.3(3) . . ? C11 Yb1 C10 30.3(3) . . ? C26 Yb1 C10 155.4(3) . . ? C12 Yb1 C10 49.4(4) . . ? O2 Yb1 C19 113.6(3) . . ? O1 Yb1 C19 96.3(3) . . ? C27 Yb1 C19 30.1(3) . . ? C11 Yb1 C19 131.9(3) . . ? C26 Yb1 C19 50.0(3) . . ? C12 Yb1 C19 159.6(4) . . ? C10 Yb1 C19 110.4(3) . . ? O2 Yb1 C5 122.8(3) . . ? O1 Yb1 C5 114.4(3) . . ? C27 Yb1 C5 145.4(3) . . ? C11 Yb1 C5 49.4(3) . . ? C26 Yb1 C5 136.6(3) . . ? C12 Yb1 C5 48.4(3) . . ? C10 Yb1 C5 30.8(3) . . ? C19 Yb1 C5 116.9(3) . . ? O2 Yb1 C4 93.3(3) . . ? O1 Yb1 C4 110.5(3) . . ? C27 Yb1 C4 161.9(3) . . ? C11 Yb1 C4 49.4(3) . . ? C26 Yb1 C4 133.8(3) . . ? C12 Yb1 C4 29.4(3) . . ? C10 Yb1 C4 50.5(3) . . ? C19 Yb1 C4 143.9(3) . . ? C5 Yb1 C4 29.8(3) . . ? O2 Yb1 C25 85.8(3) . . ? O1 Yb1 C25 135.4(3) . . ? C27 Yb1 C25 48.6(3) . . ? C11 Yb1 C25 156.7(3) . . ? C26 Yb1 C25 29.6(3) . . ? C12 Yb1 C25 141.0(3) . . ? C10 Yb1 C25 128.4(3) . . ? C19 Yb1 C25 49.6(3) . . ? C5 Yb1 C25 107.5(3) . . ? C4 Yb1 C25 113.4(3) . . ? O2 Yb1 C20 114.0(3) . . ? O1 Yb1 C20 126.3(3) . . ? C27 Yb1 C20 48.7(3) . . ? C11 Yb1 C20 136.3(3) . . ? C26 Yb1 C20 49.1(3) . . ? C12 Yb1 C20 145.3(3) . . ? C10 Yb1 C20 106.3(3) . . ? C19 Yb1 C20 30.1(3) . . ? C5 Yb1 C20 97.6(3) . . ? C4 Yb1 C20 117.7(3) . . ? C25 Yb1 C20 29.6(3) . . ? O3 Yb2 O4 86.8(3) . . ? O3 Yb2 C56 114.2(4) . . ? O4 Yb2 C56 67.2(3) . . ? O3 Yb2 C42 83.5(3) . . ? O4 Yb2 C42 86.3(3) . . ? C56 Yb2 C42 146.1(4) . . ? O3 Yb2 C57 89.2(4) . . ? O4 Yb2 C57 80.6(3) . . ? C56 Yb2 C57 30.2(4) . . ? C42 Yb2 C57 165.4(4) . . ? O3 Yb2 C55 138.1(4) . . ? O4 Yb2 C55 90.0(4) . . ? C56 Yb2 C55 30.1(4) . . ? C42 Yb2 C55 138.0(4) . . ? C57 Yb2 C55 49.1(4) . . ? O3 Yb2 C41 65.3(3) . . ? O4 Yb2 C41 107.4(4) . . ? C56 Yb2 C41 174.6(4) . . ? C42 Yb2 C41 29.4(3) . . ? C57 Yb2 C41 152.2(4) . . ? C55 Yb2 C41 153.0(4) . . ? O3 Yb2 C40 84.0(3) . . ? O4 Yb2 C40 134.9(3) . . ? C56 Yb2 C40 154.2(4) . . ? C42 Yb2 C40 48.8(4) . . ? C57 Yb2 C40 143.0(4) . . ? C55 Yb2 C40 124.8(4) . . ? C41 Yb2 C40 30.4(4) . . ? O3 Yb2 C49 91.8(3) . . ? O4 Yb2 C49 110.4(3) . . ? C56 Yb2 C49 50.7(3) . . ? C42 Yb2 C49 162.4(3) . . ? C57 Yb2 C49 29.8(3) . . ? C55 Yb2 C49 50.7(4) . . ? C41 Yb2 C49 134.2(4) . . ? C40 Yb2 C49 113.9(3) . . ? O3 Yb2 C34 112.9(3) . . ? O4 Yb2 C34 94.7(3) . . ? C56 Yb2 C34 127.9(4) . . ? C42 Yb2 C34 30.2(3) . . ? C57 Yb2 C34 157.2(4) . . ? C55 Yb2 C34 109.0(4) . . ? C41 Yb2 C34 50.4(3) . . ? C40 Yb2 C34 50.3(3) . . ? C49 Yb2 C34 146.0(3) . . ? O3 Yb2 C35 113.0(3) . . ? O4 Yb2 C35 124.1(3) . . ? C56 Yb2 C35 132.0(4) . . ? C42 Yb2 C35 48.3(3) . . ? C57 Yb2 C35 146.0(4) . . ? C55 Yb2 C35 103.2(4) . . ? C41 Yb2 C35 49.9(4) . . ? C40 Yb2 C35 30.6(3) . . ? C49 Yb2 C35 120.0(3) . . ? C34 Yb2 C35 29.5(3) . . ? O3 Yb2 C50 120.7(3) . . ? O4 Yb2 C50 116.8(3) . . ? C56 Yb2 C50 49.8(4) . . ? C42 Yb2 C50 145.5(3) . . ? C57 Yb2 C50 48.5(4) . . ? C55 Yb2 C50 30.5(3) . . ? C41 Yb2 C50 135.5(4) . . ? C40 Yb2 C50 105.7(4) . . ? C49 Yb2 C50 30.2(3) . . ? C34 Yb2 C50 117.6(3) . . ? C35 Yb2 C50 97.5(4) . . ? C3 Si1 C1 108.0(10) . . ? C3 Si1 C4 111.9(7) . . ? C1 Si1 C4 114.4(7) . . ? C3 Si1 C2 104.9(12) . . ? C1 Si1 C2 109.2(13) . . ? C4 Si1 C2 108.0(7) . . ? C19 Si2 C17 111.7(5) . . ? C19 Si2 C16 108.9(6) . . ? C17 Si2 C16 108.3(7) . . ? C19 Si2 C18 114.0(5) . . ? C17 Si2 C18 105.0(7) . . ? C16 Si2 C18 108.7(6) . . ? C31 Si3 C32 109.8(11) . . ? C31 Si3 C34 111.4(6) . . ? C32 Si3 C34 112.9(7) . . ? C31 Si3 C33 108.3(12) . . ? C32 Si3 C33 105.7(10) . . ? C34 Si3 C33 108.4(8) . . ? C47 Si4 C49 111.4(6) . . ? C47 Si4 C48 106.5(8) . . ? C49 Si4 C48 111.8(6) . . ? C47 Si4 C46 108.6(8) . . ? C49 Si4 C46 108.7(7) . . ? C48 Si4 C46 109.8(7) . . ? C14 O1 C15 114.6(11) . . ? C14 O1 Yb1 120.8(8) . . ? C15 O1 Yb1 124.6(9) . . ? C29 O2 C30 115.1(11) . . ? C29 O2 Yb1 116.8(8) . . ? C30 O2 Yb1 127.7(9) . . ? C45 O3 C44 114.6(10) . . ? C45 O3 Yb2 125.1(9) . . ? C44 O3 Yb2 119.9(7) . . ? C59 O4 C60 114.5(10) . . ? C59 O4 Yb2 119.1(7) . . ? C60 O4 Yb2 124.6(8) . . ? C12 C4 C5 105.8(10) . . ? C12 C4 Si1 126.0(8) . . ? C5 C4 Si1 127.4(8) . . ? C12 C4 Yb1 73.4(7) . . ? C5 C4 Yb1 74.6(6) . . ? Si1 C4 Yb1 125.2(6) . . ? C6 C5 C4 135.2(11) . . ? C6 C5 C10 115.7(10) . . ? C4 C5 C10 109.1(9) . . ? C6 C5 Yb1 118.2(8) . . ? C4 C5 Yb1 75.6(7) . . ? C10 C5 Yb1 73.5(6) . . ? C7 C6 C5 123.3(14) . . ? C6 C7 C8 119.8(13) . . ? C9 C8 C7 120.1(13) . . ? C8 C9 C10 121.9(14) . . ? C9 C10 C11 136.0(12) . . ? C9 C10 C5 119.1(11) . . ? C11 C10 C5 104.9(9) . . ? C9 C10 Yb1 116.2(8) . . ? C11 C10 Yb1 73.7(6) . . ? C5 C10 Yb1 75.7(6) . . ? C12 C11 C10 108.9(10) . . ? C12 C11 C13 126.1(13) . . ? C10 C11 C13 124.7(12) . . ? C12 C11 Yb1 76.2(7) . . ? C10 C11 Yb1 75.9(6) . . ? C13 C11 Yb1 109.5(8) . . ? C11 C12 C4 111.3(11) . . ? C11 C12 Yb1 74.4(7) . . ? C4 C12 Yb1 77.2(7) . . ? C14 C13 C11 120.1(12) . . ? C13 C14 O1 119.2(13) . . ? C27 C19 C20 105.5(8) . . ? C27 C19 Si2 123.5(8) . . ? C20 C19 Si2 129.0(8) . . ? C27 C19 Yb1 72.5(6) . . ? C20 C19 Yb1 77.8(6) . . ? Si2 C19 Yb1 126.9(5) . . ? C21 C20 C25 119.5(9) . . ? C21 C20 C19 133.0(9) . . ? C25 C20 C19 107.5(9) . . ? C21 C20 Yb1 120.8(8) . . ? C25 C20 Yb1 74.4(6) . . ? C19 C20 Yb1 72.1(5) . . ? C22 C21 C20 120.1(10) . . ? C21 C22 C23 120.9(11) . . ? C24 C23 C22 120.1(11) . . ? C23 C24 C25 121.5(11) . . ? C26 C25 C24 134.1(10) . . ? C26 C25 C20 108.0(9) . . ? C24 C25 C20 117.9(10) . . ? C26 C25 Yb1 71.8(6) . . ? C24 C25 Yb1 120.8(7) . . ? C20 C25 Yb1 76.0(6) . . ? C27 C26 C25 107.7(9) . . ? C27 C26 C28 126.2(10) . . ? C25 C26 C28 125.9(10) . . ? C27 C26 Yb1 73.9(6) . . ? C25 C26 Yb1 78.6(6) . . ? C28 C26 Yb1 109.0(7) . . ? C26 C27 C19 111.3(9) . . ? C26 C27 Yb1 76.3(6) . . ? C19 C27 Yb1 77.5(6) . . ? C29 C28 C26 114.0(11) . . ? O2 C29 C28 115.9(16) . . ? C35 C34 C42 104.6(10) . . ? C35 C34 Si3 130.4(9) . . ? C42 C34 Si3 123.7(9) . . ? C35 C34 Yb2 75.5(6) . . ? C42 C34 Yb2 72.6(6) . . ? Si3 C34 Yb2 126.0(5) . . ? C34 C35 C36 132.9(11) . . ? C34 C35 C40 109.4(10) . . ? C36 C35 C40 117.5(11) . . ? C34 C35 Yb2 75.0(6) . . ? C36 C35 Yb2 120.8(8) . . ? C40 C35 Yb2 73.8(6) . . ? C35 C36 C37 119.0(13) . . ? C38 C37 C36 117.3(13) . . ? C39 C38 C37 126.4(15) . . ? C38 C39 C40 117.4(15) . . ? C39 C40 C41 130.7(13) . . ? C39 C40 C35 122.3(14) . . ? C41 C40 C35 106.6(10) . . ? C39 C40 Yb2 121.5(8) . . ? C41 C40 Yb2 73.9(6) . . ? C35 C40 Yb2 75.6(5) . . ? C42 C41 C40 106.5(10) . . ? C42 C41 C43 127.5(15) . . ? C40 C41 C43 125.7(14) . . ? C42 C41 Yb2 74.6(6) . . ? C40 C41 Yb2 75.8(6) . . ? C43 C41 Yb2 110.8(8) . . ? C41 C42 C34 112.8(11) . . ? C41 C42 Yb2 75.9(7) . . ? C34 C42 Yb2 77.2(6) . . ? C44 C43 C41 116.2(13) . . ? C43 C44 O3 116.4(13) . . ? C57 C49 C50 104.9(10) . . ? C57 C49 Si4 127.8(10) . . ? C50 C49 Si4 125.4(10) . . ? C57 C49 Yb2 73.0(8) . . ? C50 C49 Yb2 76.6(7) . . ? Si4 C49 Yb2 127.3(5) . . ? C51 C50 C49 134.0(12) . . ? C51 C50 C55 118.5(12) . . ? C49 C50 C55 107.5(11) . . ? C51 C50 Yb2 119.2(9) . . ? C49 C50 Yb2 73.2(7) . . ? C55 C50 Yb2 71.1(7) . . ? C52 C51 C50 119.9(14) . . ? C53 C52 C51 122.7(16) . . ? C54 C53 C52 119.9(15) . . ? C53 C54 C55 121.2(16) . . ? C56 C55 C54 134.4(14) . . ? C56 C55 C50 107.8(11) . . ? C54 C55 C50 117.8(14) . . ? C56 C55 Yb2 72.4(7) . . ? C54 C55 Yb2 117.0(9) . . ? C50 C55 Yb2 78.3(6) . . ? C55 C56 C57 108.0(11) . . ? C55 C56 C58 124.8(13) . . ? C57 C56 C58 127.2(14) . . ? C55 C56 Yb2 77.6(7) . . ? C57 C56 Yb2 77.4(7) . . ? C58 C56 Yb2 110.0(9) . . ? C56 C57 C49 111.5(12) . . ? C56 C57 Yb2 72.5(7) . . ? C49 C57 Yb2 77.2(7) . . ? C59 C58 C56 112.5(12) . . ? O4 C59 C58 112.7(11) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.886 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.103 #====# data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 223637' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 Eu N2 O2 Si2' _chemical_formula_weight 756.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 31.1608(3) _cell_length_b 34.5218(7) _cell_length_c 14.85250(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15977.2(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10722 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.02 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6288 _exptl_absorpt_coefficient_mu 1.660 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7709 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12431 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4886 _reflns_number_gt 4473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens SMART & SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0197P)^2^+63.3827P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(18) _refine_ls_number_reflns 4886 _refine_ls_number_parameters 389 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu Eu 0.135424(9) 0.091331(8) 0.23657(3) 0.05068(9) Uani 1 1 d . . . Si1 Si 0.15763(8) 0.06856(6) 0.51552(14) 0.0693(6) Uani 1 1 d . . . Si2 Si 0.15113(8) 0.07992(6) -0.04686(14) 0.0674(5) Uani 1 1 d . . . N1 N 0.1239(2) 0.03204(17) 0.4837(6) 0.0860(18) Uani 1 1 d . . . H1A H 0.1201 0.0305 0.4265 0.103 Uiso 1 1 calc R . . N2 N 0.2014(2) 0.0944(2) -0.0194(5) 0.098(2) Uani 1 1 d . . . H2A H 0.2068 0.0926 0.0372 0.118 Uiso 1 1 calc R . . O1 O 0.1314(2) 0.16214(13) 0.1863(4) 0.0890(18) Uani 1 1 d . . . O2 O 0.05974(16) 0.09829(16) 0.3021(4) 0.0849(16) Uani 1 1 d . . . C1 C 0.0576(5) -0.0002(7) 0.4995(17) 0.302(16) Uani 1 1 d . . . H1B H 0.0416 0.0227 0.5140 0.453 Uiso 1 1 calc R . . H1C H 0.0440 -0.0223 0.5260 0.453 Uiso 1 1 calc R . . H1D H 0.0588 -0.0033 0.4354 0.453 Uiso 1 1 calc R . . C2 C 0.1013(10) 0.0067(7) 0.6256(10) 0.36(2) Uani 1 1 d . . . H2B H 0.1304 0.0094 0.6457 0.545 Uiso 1 1 calc R . . H2C H 0.0889 -0.0160 0.6521 0.545 Uiso 1 1 calc R . . H2D H 0.0851 0.0291 0.6434 0.545 Uiso 1 1 calc R . . C3 C 0.1181(10) -0.0339(4) 0.5049(18) 0.314(17) Uani 1 1 d . . . H3A H 0.1474 -0.0361 0.5241 0.471 Uiso 1 1 calc R . . H3B H 0.1167 -0.0354 0.4404 0.471 Uiso 1 1 calc R . . H3C H 0.1015 -0.0545 0.5307 0.471 Uiso 1 1 calc R . . C4 C 0.1006(4) 0.0034(3) 0.5345(7) 0.105(3) Uani 1 1 d . . . C5 C 0.1315(5) 0.1061(3) 0.5872(8) 0.136(5) Uani 1 1 d . . . H5A H 0.1073 0.1167 0.5560 0.204 Uiso 1 1 calc R . . H5B H 0.1517 0.1264 0.5999 0.204 Uiso 1 1 calc R . . H5C H 0.1222 0.0945 0.6426 0.204 Uiso 1 1 calc R . . C6 C 0.2039(3) 0.0494(3) 0.5828(8) 0.129(4) Uani 1 1 d . . . H6A H 0.2187 0.0300 0.5485 0.193 Uiso 1 1 calc R . . H6B H 0.1934 0.0382 0.6377 0.193 Uiso 1 1 calc R . . H6C H 0.2233 0.0702 0.5967 0.193 Uiso 1 1 calc R . . C7 C 0.1777(2) 0.09229(17) 0.4120(4) 0.0527(15) Uani 1 1 d . . . C8 C 0.2084(2) 0.07801(17) 0.3509(5) 0.0547(15) Uani 1 1 d . . . C9 C 0.2289(2) 0.04140(19) 0.3392(5) 0.0651(18) Uani 1 1 d . . . H9A H 0.2221 0.0210 0.3776 0.078 Uiso 1 1 calc R . . C10 C 0.2580(2) 0.0360(2) 0.2736(6) 0.083(2) Uani 1 1 d . . . H10A H 0.2714 0.0120 0.2682 0.100 Uiso 1 1 calc R . . C11 C 0.2683(3) 0.0651(3) 0.2140(6) 0.093(3) Uani 1 1 d . . . H11A H 0.2881 0.0602 0.1685 0.111 Uiso 1 1 calc R . . C12 C 0.2500(2) 0.1014(2) 0.2202(6) 0.075(2) Uani 1 1 d . . . H12A H 0.2572 0.1208 0.1795 0.090 Uiso 1 1 calc R . . C13 C 0.2200(2) 0.10841(18) 0.2895(5) 0.0581(16) Uani 1 1 d . . . C14 C 0.1961(2) 0.14166(17) 0.3140(5) 0.0605(18) Uani 1 1 d . . . C15 C 0.1717(2) 0.13168(17) 0.3881(5) 0.0560(16) Uani 1 1 d . . . H15A H 0.1558 0.1504 0.4250 0.067 Uiso 1 1 calc R . . C16 C 0.1947(3) 0.1801(2) 0.2641(6) 0.088(3) Uani 1 1 d . . . H16A H 0.2054 0.2000 0.3044 0.106 Uiso 1 1 calc R . . H16B H 0.2145 0.1785 0.2138 0.106 Uiso 1 1 calc R . . C17 C 0.1551(4) 0.1921(2) 0.2312(9) 0.122(4) Uani 1 1 d . . . H17A H 0.1596 0.2133 0.1894 0.146 Uiso 1 1 calc R . . H17B H 0.1381 0.2018 0.2809 0.146 Uiso 1 1 calc R . . C18 C 0.0939(4) 0.1775(3) 0.1447(10) 0.160(6) Uani 1 1 d . . . H18A H 0.0985 0.2043 0.1303 0.239 Uiso 1 1 calc R . . H18B H 0.0700 0.1752 0.1852 0.239 Uiso 1 1 calc R . . H18C H 0.0879 0.1633 0.0905 0.239 Uiso 1 1 calc R . . C21 C 0.2740(5) 0.0842(5) -0.0647(17) 0.291(16) Uani 1 1 d . . . H21A H 0.2972 0.0942 -0.1002 0.437 Uiso 1 1 calc R . . H21B H 0.2664 0.0588 -0.0858 0.437 Uiso 1 1 calc R . . H21C H 0.2827 0.0827 -0.0028 0.437 Uiso 1 1 calc R . . C22 C 0.2504(7) 0.1462(5) -0.0361(12) 0.265(13) Uani 1 1 d . . . H22A H 0.2739 0.1564 -0.0707 0.397 Uiso 1 1 calc R . . H22B H 0.2593 0.1430 0.0253 0.397 Uiso 1 1 calc R . . H22C H 0.2267 0.1638 -0.0388 0.397 Uiso 1 1 calc R . . C23 C 0.2256(6) 0.1166(8) -0.1670(10) 0.298(15) Uani 1 1 d . . . H23A H 0.2500 0.1261 -0.1995 0.448 Uiso 1 1 calc R . . H23B H 0.2030 0.1356 -0.1690 0.448 Uiso 1 1 calc R . . H23C H 0.2157 0.0930 -0.1940 0.448 Uiso 1 1 calc R . . C24 C 0.2377(4) 0.1093(4) -0.0725(7) 0.114(4) Uani 1 1 d . . . C25 C 0.1521(5) 0.0407(3) -0.1342(7) 0.146(6) Uani 1 1 d . . . H25A H 0.1691 0.0194 -0.1129 0.219 Uiso 1 1 calc R . . H25B H 0.1643 0.0507 -0.1889 0.219 Uiso 1 1 calc R . . H25C H 0.1233 0.0320 -0.1456 0.219 Uiso 1 1 calc R . . C26 C 0.1173(4) 0.1188(4) -0.0947(10) 0.164(6) Uani 1 1 d . . . H26A H 0.1157 0.1400 -0.0528 0.245 Uiso 1 1 calc R . . H26B H 0.0890 0.1090 -0.1061 0.245 Uiso 1 1 calc R . . H26C H 0.1298 0.1278 -0.1501 0.245 Uiso 1 1 calc R . . C27 C 0.1253(2) 0.06124(18) 0.0555(5) 0.0557(16) Uani 1 1 d . . . C28 C 0.1391(3) 0.02897(16) 0.1105(5) 0.0532(16) Uani 1 1 d . . . C29 C 0.1771(2) 0.00720(17) 0.1139(5) 0.0630(18) Uani 1 1 d . . . H29A H 0.1994 0.0125 0.0742 0.076 Uiso 1 1 calc R . . C30 C 0.1811(3) -0.02183(19) 0.1758(6) 0.076(2) Uani 1 1 d . . . H30A H 0.2063 -0.0361 0.1776 0.091 Uiso 1 1 calc R . . C31 C 0.1483(3) -0.03065(17) 0.2363(8) 0.082(2) Uani 1 1 d . . . H31A H 0.1522 -0.0503 0.2783 0.098 Uiso 1 1 calc R . . C32 C 0.1101(3) -0.01022(18) 0.2340(6) 0.075(2) Uani 1 1 d . . . H32A H 0.0882 -0.0164 0.2740 0.090 Uiso 1 1 calc R . . C33 C 0.1045(2) 0.01999(16) 0.1710(5) 0.0565(16) Uani 1 1 d . . . C34 C 0.0700(2) 0.04610(19) 0.1550(5) 0.0619(18) Uani 1 1 d . . . C35 C 0.0830(2) 0.07039(19) 0.0853(5) 0.0589(17) Uani 1 1 d . . . H35A H 0.0639 0.0884 0.0541 0.071 Uiso 1 1 calc R . . C36 C 0.0291(2) 0.0496(2) 0.2085(6) 0.081(2) Uani 1 1 d . . . H36A H 0.0051 0.0455 0.1681 0.097 Uiso 1 1 calc R . . H36B H 0.0285 0.0289 0.2528 0.097 Uiso 1 1 calc R . . C37 C 0.0228(3) 0.0860(3) 0.2548(11) 0.115(4) Uani 1 1 d . . . H37A H 0.0150 0.1057 0.2112 0.138 Uiso 1 1 calc R . . H37B H -0.0009 0.0834 0.2969 0.138 Uiso 1 1 calc R . . C38 C 0.0516(4) 0.1274(5) 0.3656(13) 0.214(10) Uani 1 1 d . . . H38A H 0.0220 0.1265 0.3833 0.322 Uiso 1 1 calc R . . H38B H 0.0578 0.1522 0.3397 0.322 Uiso 1 1 calc R . . H38C H 0.0695 0.1234 0.4175 0.322 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 Eu 0.04651(13) 0.05184(13) 0.05368(16) -0.00735(16) -0.00609(17) 0.00278(13) Si1 0.0741(13) 0.0821(13) 0.0517(14) 0.0095(10) 0.0018(10) 0.0067(11) Si2 0.0811(14) 0.0682(11) 0.0529(12) 0.0063(9) 0.0050(11) 0.0070(10) N1 0.090(4) 0.107(4) 0.061(4) 0.024(5) -0.004(5) -0.023(3) N2 0.081(4) 0.160(6) 0.055(4) 0.014(5) 0.009(4) -0.021(4) O1 0.108(4) 0.059(3) 0.100(4) 0.000(3) -0.046(4) 0.019(3) O2 0.053(3) 0.121(4) 0.080(4) -0.034(3) 0.000(3) 0.007(3) C1 0.126(11) 0.45(3) 0.33(3) 0.25(3) -0.016(18) -0.121(17) C2 0.61(5) 0.42(3) 0.068(9) 0.030(14) 0.045(18) -0.36(3) C3 0.55(5) 0.141(12) 0.25(3) 0.044(16) 0.21(3) 0.00(2) C4 0.112(8) 0.103(6) 0.099(8) 0.031(6) 0.018(6) -0.020(6) C5 0.192(14) 0.135(8) 0.081(7) -0.008(7) 0.060(9) 0.019(8) C6 0.105(8) 0.175(10) 0.106(9) 0.063(8) -0.038(7) -0.028(8) C7 0.051(3) 0.062(3) 0.045(4) 0.004(3) 0.001(3) 0.002(3) C8 0.043(3) 0.062(3) 0.058(4) -0.002(3) -0.010(3) 0.007(3) C9 0.059(4) 0.065(4) 0.072(5) -0.008(3) -0.012(4) 0.006(3) C10 0.058(5) 0.093(5) 0.098(7) -0.026(5) -0.002(5) 0.020(4) C11 0.055(4) 0.140(8) 0.083(7) -0.029(6) 0.008(4) 0.002(5) C12 0.051(4) 0.115(6) 0.059(6) 0.000(4) 0.002(4) -0.018(4) C13 0.051(4) 0.068(4) 0.056(4) -0.002(3) -0.008(3) -0.011(3) C14 0.072(5) 0.053(3) 0.057(4) 0.002(3) -0.019(4) -0.013(3) C15 0.063(4) 0.056(3) 0.049(4) -0.008(3) -0.009(3) 0.003(3) C16 0.100(6) 0.068(4) 0.097(7) 0.017(4) -0.032(6) -0.008(4) C17 0.155(9) 0.071(4) 0.139(9) 0.046(7) -0.068(10) -0.025(5) C18 0.176(12) 0.082(6) 0.221(15) 0.018(7) -0.125(12) 0.015(7) C21 0.142(13) 0.30(2) 0.43(4) 0.17(2) 0.18(2) 0.090(14) C22 0.36(3) 0.27(2) 0.162(18) -0.005(15) 0.101(18) -0.21(2) C23 0.176(17) 0.62(4) 0.097(11) 0.101(19) 0.032(11) -0.14(2) C24 0.102(8) 0.161(9) 0.080(7) 0.029(7) 0.031(6) -0.031(7) C25 0.238(17) 0.129(8) 0.071(7) -0.027(6) 0.036(9) -0.038(10) C26 0.118(9) 0.221(14) 0.151(12) 0.117(11) 0.036(9) 0.067(10) C27 0.061(4) 0.058(3) 0.048(4) 0.001(3) 0.001(3) 0.001(3) C28 0.061(4) 0.048(3) 0.050(4) -0.008(3) -0.006(3) 0.000(3) C29 0.071(5) 0.051(3) 0.067(5) -0.010(3) 0.003(4) 0.005(3) C30 0.088(5) 0.055(4) 0.083(6) -0.009(4) -0.012(5) 0.015(4) C31 0.112(6) 0.050(3) 0.082(5) 0.013(5) -0.020(7) 0.002(4) C32 0.100(6) 0.061(4) 0.064(4) -0.006(4) -0.002(6) -0.025(4) C33 0.071(4) 0.048(3) 0.051(4) -0.008(3) -0.007(3) -0.011(3) C34 0.053(4) 0.066(4) 0.066(5) -0.010(4) -0.007(4) -0.010(3) C35 0.060(4) 0.063(4) 0.053(4) 0.000(3) -0.011(3) -0.005(3) C36 0.054(4) 0.104(5) 0.084(7) 0.000(5) -0.001(4) -0.013(4) C37 0.057(4) 0.159(8) 0.130(12) -0.038(8) 0.023(7) 0.001(5) C38 0.098(9) 0.272(18) 0.27(2) -0.187(17) 0.022(11) 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 Eu O1 2.559(5) . ? Eu O2 2.563(5) . ? Eu C14 2.813(6) . ? Eu C13 2.813(6) . ? Eu C33 2.819(6) . ? Eu C34 2.839(6) . ? Eu C28 2.856(6) . ? Eu C35 2.869(7) . ? Eu C8 2.876(6) . ? Eu C15 2.877(6) . ? Eu C27 2.901(7) . ? Eu C7 2.921(7) . ? Si1 N1 1.708(7) . ? Si1 C7 1.851(7) . ? Si1 C5 1.863(11) . ? Si1 C6 1.876(10) . ? Si2 N2 1.694(7) . ? Si2 C27 1.837(7) . ? Si2 C26 1.849(11) . ? Si2 C25 1.875(10) . ? N1 C4 1.438(10) . ? N2 C24 1.472(11) . ? O1 C18 1.423(11) . ? O1 C17 1.435(10) . ? O2 C38 1.401(12) . ? O2 C37 1.414(12) . ? C1 C4 1.442(18) . ? C2 C4 1.358(17) . ? C3 C4 1.46(2) . ? C7 C8 1.408(9) . ? C7 C15 1.418(8) . ? C8 C9 1.427(8) . ? C8 C13 1.436(9) . ? C9 C10 1.344(11) . ? C10 C11 1.378(12) . ? C11 C12 1.379(11) . ? C12 C13 1.411(10) . ? C13 C14 1.417(9) . ? C14 C15 1.381(9) . ? C14 C16 1.521(9) . ? C16 C17 1.391(11) . ? C21 C24 1.429(18) . ? C22 C24 1.440(17) . ? C23 C24 1.476(19) . ? C27 C35 1.424(10) . ? C27 C28 1.447(9) . ? C28 C29 1.402(10) . ? C28 C33 1.438(10) . ? C29 C30 1.366(10) . ? C30 C31 1.393(12) . ? C31 C32 1.385(10) . ? C32 C33 1.413(10) . ? C33 C34 1.422(9) . ? C34 C35 1.392(10) . ? C34 C36 1.507(10) . ? C36 C37 1.447(13) . ? 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 Eu O2 88.6(2) . . ? O1 Eu C14 64.06(18) . . ? O2 Eu C14 113.9(2) . . ? O1 Eu C13 85.84(19) . . ? O2 Eu C13 137.43(19) . . ? C14 Eu C13 29.17(19) . . ? O1 Eu C33 135.80(19) . . ? O2 Eu C33 84.18(19) . . ? C14 Eu C33 155.6(2) . . ? C13 Eu C33 126.88(19) . . ? O1 Eu C34 111.43(19) . . ? O2 Eu C34 63.45(19) . . ? C14 Eu C34 175.2(2) . . ? C13 Eu C34 155.1(2) . . ? C33 Eu C34 29.12(19) . . ? O1 Eu C28 122.04(19) . . ? O2 Eu C28 110.9(2) . . ? C14 Eu C28 135.0(2) . . ? C13 Eu C28 107.7(2) . . ? C33 Eu C28 29.3(2) . . ? C34 Eu C28 48.3(2) . . ? O1 Eu C35 89.09(18) . . ? O2 Eu C35 78.32(19) . . ? C14 Eu C35 149.09(19) . . ? C13 Eu C35 143.6(2) . . ? C33 Eu C35 46.74(19) . . ? C34 Eu C35 28.2(2) . . ? C28 Eu C35 47.1(2) . . ? O1 Eu C8 111.34(18) . . ? O2 Eu C8 121.2(2) . . ? C14 Eu C8 47.60(18) . . ? C13 Eu C8 29.21(19) . . ? C33 Eu C8 109.57(18) . . ? C34 Eu C8 137.06(19) . . ? C28 Eu C8 103.6(2) . . ? C35 Eu C8 150.69(18) . . ? O1 Eu C15 77.60(17) . . ? O2 Eu C15 91.06(19) . . ? C14 Eu C15 28.06(19) . . ? C13 Eu C15 46.6(2) . . ? C33 Eu C15 145.85(19) . . ? C34 Eu C15 151.8(2) . . ? C28 Eu C15 149.6(2) . . ? C35 Eu C15 163.23(18) . . ? C8 Eu C15 45.99(18) . . ? O1 Eu C27 93.78(18) . . ? O2 Eu C27 106.59(18) . . ? C14 Eu C27 132.4(2) . . ? C13 Eu C27 115.9(2) . . ? C33 Eu C27 47.87(19) . . ? C34 Eu C27 47.9(2) . . ? C28 Eu C27 29.10(18) . . ? C35 Eu C27 28.57(19) . . ? C8 Eu C27 125.20(19) . . ? C15 Eu C27 160.3(2) . . ? O1 Eu C7 105.77(17) . . ? O2 Eu C7 94.32(18) . . ? C14 Eu C7 47.53(18) . . ? C13 Eu C7 47.57(19) . . ? C33 Eu C7 118.21(18) . . ? C34 Eu C7 135.32(19) . . ? C28 Eu C7 125.15(18) . . ? C35 Eu C7 163.37(18) . . ? C8 Eu C7 28.11(18) . . ? C15 Eu C7 28.30(17) . . ? C27 Eu C7 151.73(18) . . ? N1 Si1 C7 107.8(4) . . ? N1 Si1 C5 113.7(5) . . ? C7 Si1 C5 108.3(4) . . ? N1 Si1 C6 111.1(4) . . ? C7 Si1 C6 109.8(4) . . ? C5 Si1 C6 106.1(6) . . ? N2 Si2 C27 108.0(4) . . ? N2 Si2 C26 113.9(6) . . ? C27 Si2 C26 108.9(5) . . ? N2 Si2 C25 111.4(6) . . ? C27 Si2 C25 109.0(4) . . ? C26 Si2 C25 105.5(7) . . ? C4 N1 Si1 132.2(8) . . ? C24 N2 Si2 133.2(7) . . ? C18 O1 C17 110.9(6) . . ? C18 O1 Eu 121.5(6) . . ? C17 O1 Eu 121.8(5) . . ? C38 O2 C37 113.7(8) . . ? C38 O2 Eu 119.3(6) . . ? C37 O2 Eu 122.2(6) . . ? C2 C4 N1 117.2(11) . . ? C2 C4 C1 112.4(18) . . ? N1 C4 C1 109.8(10) . . ? C2 C4 C3 111.5(18) . . ? N1 C4 C3 105.1(11) . . ? C1 C4 C3 99.3(17) . . ? C8 C7 C15 105.3(6) . . ? C8 C7 Si1 127.6(5) . . ? C15 C7 Si1 126.0(5) . . ? C8 C7 Eu 74.2(4) . . ? C15 C7 Eu 74.2(4) . . ? Si1 C7 Eu 125.7(3) . . ? C7 C8 C9 133.8(7) . . ? C7 C8 C13 108.9(5) . . ? C9 C8 C13 117.2(6) . . ? C7 C8 Eu 77.7(4) . . ? C9 C8 Eu 115.1(4) . . ? C13 C8 Eu 73.0(4) . . ? C10 C9 C8 120.9(8) . . ? C9 C10 C11 121.4(7) . . ? C10 C11 C12 121.6(8) . . ? C11 C12 C13 118.5(7) . . ? C12 C13 C14 132.5(7) . . ? C12 C13 C8 120.3(6) . . ? C14 C13 C8 107.2(6) . . ? C12 C13 Eu 112.3(5) . . ? C14 C13 Eu 75.4(4) . . ? C8 C13 Eu 77.8(4) . . ? C15 C14 C13 107.0(6) . . ? C15 C14 C16 126.2(7) . . ? C13 C14 C16 126.6(7) . . ? C15 C14 Eu 78.6(4) . . ? C13 C14 Eu 75.4(3) . . ? C16 C14 Eu 108.7(4) . . ? C14 C15 C7 111.4(6) . . ? C14 C15 Eu 73.4(4) . . ? C7 C15 Eu 77.5(4) . . ? C17 C16 C14 117.1(7) . . ? C16 C17 O1 114.0(8) . . ? C21 C24 C22 106.8(16) . . ? C21 C24 N2 110.6(10) . . ? C22 C24 N2 108.7(11) . . ? C21 C24 C23 112.6(15) . . ? C22 C24 C23 106.0(15) . . ? N2 C24 C23 111.9(11) . . ? C35 C27 C28 105.7(6) . . ? C35 C27 Si2 125.8(5) . . ? C28 C27 Si2 127.3(5) . . ? C35 C27 Eu 74.5(4) . . ? C28 C27 Eu 73.7(4) . . ? Si2 C27 Eu 126.4(3) . . ? C29 C28 C33 119.6(6) . . ? C29 C28 C27 133.2(7) . . ? C33 C28 C27 107.2(6) . . ? C29 C28 Eu 114.5(5) . . ? C33 C28 Eu 73.9(3) . . ? C27 C28 Eu 77.2(3) . . ? C30 C29 C28 119.6(7) . . ? C29 C30 C31 121.9(7) . . ? C32 C31 C30 120.2(8) . . ? C31 C32 C33 119.9(8) . . ? C32 C33 C34 132.2(7) . . ? C32 C33 C28 118.7(6) . . ? C34 C33 C28 109.0(6) . . ? C32 C33 Eu 111.9(4) . . ? C34 C33 Eu 76.2(3) . . ? C28 C33 Eu 76.8(3) . . ? C35 C34 C33 106.6(6) . . ? C35 C34 C36 126.2(7) . . ? C33 C34 C36 127.0(7) . . ? C35 C34 Eu 77.1(4) . . ? C33 C34 Eu 74.6(4) . . ? C36 C34 Eu 109.8(5) . . ? C34 C35 C27 111.5(6) . . ? C34 C35 Eu 74.7(4) . . ? C27 C35 Eu 76.9(4) . . ? C37 C36 C34 115.8(7) . . ? O2 C37 C36 112.6(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.570 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.058 #=====# data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 223638' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H42 Eu O2 Si2' _chemical_formula_weight 642.78 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' Si Si 0.0817 0.0704 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5365(3) _cell_length_b 16.2922(5) _cell_length_c 18.6379(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.4450(10) _cell_angle_gamma 90.00 _cell_volume 3185.00(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7549 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 24.92 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.98 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 2.067 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5639 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 10892 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.92 _reflns_number_total 8612 _reflns_number_gt 7922 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens SMART & SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+9.8667P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(14) _refine_ls_number_reflns 8612 _refine_ls_number_parameters 632 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 0.05607(4) 0.43102(2) 0.36741(2) 0.04555(12) Uani 1 1 d . . . Eu2 Eu 0.52453(4) 0.06989(2) 0.09760(2) 0.04269(11) Uani 1 1 d . . . Si1 Si 0.3418(3) 0.26100(19) 0.43525(16) 0.0686(8) Uani 1 1 d . . . Si2 Si -0.0899(3) 0.66352(18) 0.30027(14) 0.0635(8) Uani 1 1 d . . . Si3 Si 0.8122(3) 0.17942(16) -0.01103(13) 0.0562(7) Uani 1 1 d . . . Si4 Si 0.4024(4) -0.10054(19) 0.24559(18) 0.0804(9) Uani 1 1 d . . . O1 O -0.1303(7) 0.3965(5) 0.2739(4) 0.085(2) Uani 1 1 d . . . O2 O -0.0603(7) 0.3486(4) 0.4617(4) 0.074(2) Uani 1 1 d . . . O3 O 0.3477(6) 0.1517(4) 0.1511(4) 0.073(2) Uani 1 1 d . . . O4 O 0.3858(7) 0.0966(4) -0.0238(4) 0.075(2) Uani 1 1 d . . . C1 C -0.2596(11) 0.4021(9) 0.2894(8) 0.118(6) Uani 1 1 d . . . H1A H -0.3145 0.3866 0.2476 0.177 Uiso 1 1 calc R . . H1B H -0.2781 0.4574 0.3026 0.177 Uiso 1 1 calc R . . H1C H -0.2734 0.3659 0.3286 0.177 Uiso 1 1 calc R . . C2 C -0.1103(13) 0.3576(11) 0.2097(8) 0.116(6) Uani 1 1 d . . . H2A H -0.1833 0.3223 0.1975 0.140 Uiso 1 1 calc R . . H2B H -0.1125 0.3997 0.1728 0.140 Uiso 1 1 calc R . . C3 C -0.0072(16) 0.3128(12) 0.2034(9) 0.175(10) Uani 1 1 d . . . H3A H 0.0184 0.3223 0.1555 0.209 Uiso 1 1 calc R . . H3B H -0.0323 0.2557 0.2055 0.209 Uiso 1 1 calc R . . C4 C 0.1082(11) 0.3238(8) 0.2552(6) 0.076(3) Uani 1 1 d . . . C5 C 0.1455(9) 0.2793(6) 0.3165(6) 0.065(3) Uani 1 1 d . . . H5A H 0.1084 0.2261 0.3274 0.078 Uiso 1 1 calc R . . C6 C 0.2544(8) 0.3122(6) 0.3560(5) 0.049(2) Uani 1 1 d . . . C7 C 0.2931(9) 0.3813(6) 0.3147(5) 0.053(2) Uani 1 1 d . . . C8 C 0.1981(11) 0.3866(7) 0.2512(5) 0.073(4) Uani 1 1 d . . . C9 C 0.2193(17) 0.4498(12) 0.2020(8) 0.128(7) Uani 1 1 d . . . H9A H 0.1637 0.4556 0.1605 0.154 Uiso 1 1 calc R . . C10 C 0.318(2) 0.5015(12) 0.2137(12) 0.158(12) Uani 1 1 d . . . H10A H 0.3257 0.5430 0.1802 0.190 Uiso 1 1 calc R . . C11 C 0.4077(16) 0.4970(10) 0.2724(12) 0.131(7) Uani 1 1 d . . . H11A H 0.4759 0.5335 0.2769 0.157 Uiso 1 1 calc R . . C12 C 0.3951(10) 0.4361(8) 0.3261(7) 0.082(3) Uani 1 1 d . . . H12A H 0.4525 0.4329 0.3671 0.098 Uiso 1 1 calc R . . C13 C 0.2949(17) 0.2995(11) 0.5216(6) 0.145(7) Uani 1 1 d . . . H13A H 0.3126 0.3572 0.5255 0.217 Uiso 1 1 calc R . . H13B H 0.3422 0.2710 0.5606 0.217 Uiso 1 1 calc R . . H13C H 0.2053 0.2904 0.5239 0.217 Uiso 1 1 calc R . . C14 C 0.3065(18) 0.1480(9) 0.4305(9) 0.156(7) Uani 1 1 d . . . H14A H 0.2167 0.1394 0.4319 0.234 Uiso 1 1 calc R . . H14B H 0.3522 0.1208 0.4707 0.234 Uiso 1 1 calc R . . H14C H 0.3327 0.1261 0.3864 0.234 Uiso 1 1 calc R . . C15 C 0.5165(12) 0.2725(14) 0.4329(9) 0.192(11) Uani 1 1 d . . . H15A H 0.5387 0.3296 0.4356 0.288 Uiso 1 1 calc R . . H15B H 0.5414 0.2497 0.3889 0.288 Uiso 1 1 calc R . . H15C H 0.5599 0.2440 0.4732 0.288 Uiso 1 1 calc R . . C16 C -0.1001(14) 0.2649(8) 0.4514(8) 0.111(5) Uani 1 1 d . . . H16A H -0.1409 0.2467 0.4925 0.167 Uiso 1 1 calc R . . H16B H -0.0270 0.2311 0.4459 0.167 Uiso 1 1 calc R . . H16C H -0.1588 0.2608 0.4090 0.167 Uiso 1 1 calc R . . C17 C -0.1254(13) 0.3909(9) 0.5152(7) 0.098(4) Uani 1 1 d . . . H17A H -0.1365 0.3537 0.5548 0.117 Uiso 1 1 calc R . . H17B H -0.2094 0.4071 0.4942 0.117 Uiso 1 1 calc R . . C18 C -0.0549(16) 0.4653(8) 0.5439(6) 0.106(5) Uani 1 1 d . . . H18A H 0.0214 0.4482 0.5733 0.128 Uiso 1 1 calc R . . H18B H -0.1080 0.4954 0.5746 0.128 Uiso 1 1 calc R . . C19 C -0.0170(13) 0.5225(6) 0.4842(5) 0.070(3) Uani 1 1 d . . . C20 C -0.0964(10) 0.5564(7) 0.4273(5) 0.064(3) Uani 1 1 d . . . H20A H -0.1898 0.5555 0.4244 0.077 Uiso 1 1 calc R . . C21 C -0.0255(10) 0.6003(5) 0.3793(5) 0.053(2) Uani 1 1 d . . . C22 C 0.1070(11) 0.5969(6) 0.4115(5) 0.059(3) Uani 1 1 d . . . C23 C 0.1098(12) 0.5480(6) 0.4766(5) 0.068(3) Uani 1 1 d . . . C24 C 0.2280(15) 0.5307(8) 0.5167(6) 0.090(4) Uani 1 1 d . . . H24A H 0.2322 0.4975 0.5574 0.108 Uiso 1 1 calc R . . C25 C 0.3342(15) 0.5642(10) 0.4936(7) 0.105(4) Uani 1 1 d . . . H25A H 0.4120 0.5536 0.5199 0.126 Uiso 1 1 calc R . . C26 C 0.3333(13) 0.6146(8) 0.4314(8) 0.099(4) Uani 1 1 d . . . H26A H 0.4088 0.6372 0.4183 0.119 Uiso 1 1 calc R . . C27 C 0.2192(12) 0.6300(7) 0.3906(7) 0.080(4) Uani 1 1 d . . . H27A H 0.2177 0.6623 0.3494 0.096 Uiso 1 1 calc R . . C28 C -0.0167(14) 0.6336(9) 0.2161(6) 0.111(5) Uani 1 1 d . . . H28A H -0.0325 0.5764 0.2064 0.167 Uiso 1 1 calc R . . H28B H 0.0735 0.6432 0.2226 0.167 Uiso 1 1 calc R . . H28C H -0.0538 0.6658 0.1764 0.167 Uiso 1 1 calc R . . C29 C -0.2645(12) 0.6481(10) 0.2848(7) 0.115(5) Uani 1 1 d . . . H29A H -0.3037 0.6645 0.3270 0.173 Uiso 1 1 calc R . . H29B H -0.2822 0.5912 0.2750 0.173 Uiso 1 1 calc R . . H29C H -0.2980 0.6806 0.2444 0.173 Uiso 1 1 calc R . . C30 C -0.0576(15) 0.7752(7) 0.3175(7) 0.114(5) Uani 1 1 d . . . H30A H -0.0953 0.7919 0.3601 0.170 Uiso 1 1 calc R . . H30B H -0.0939 0.8067 0.2771 0.170 Uiso 1 1 calc R . . H30C H 0.0327 0.7843 0.3240 0.170 Uiso 1 1 calc R . . C31 C 0.2178(11) 0.1397(10) 0.1374(9) 0.129(6) Uani 1 1 d . . . H31A H 0.1734 0.1784 0.1647 0.193 Uiso 1 1 calc R . . H31B H 0.1966 0.0849 0.1511 0.193 Uiso 1 1 calc R . . H31C H 0.1931 0.1473 0.0870 0.193 Uiso 1 1 calc R . . C32 C 0.3816(16) 0.2181(13) 0.1935(15) 0.253(17) Uani 1 1 d . . . H32A H 0.3103 0.2559 0.1871 0.304 Uiso 1 1 calc R . . H32B H 0.3850 0.1988 0.2429 0.304 Uiso 1 1 calc R . . C33 C 0.4861(10) 0.2635(6) 0.1896(6) 0.069(3) Uani 1 1 d . . . H33A H 0.5151 0.2818 0.2379 0.083 Uiso 1 1 calc R . . H33B H 0.4622 0.3120 0.1613 0.083 Uiso 1 1 calc R . . C34 C 0.5969(8) 0.2240(5) 0.1579(5) 0.048(2) Uani 1 1 d . . . C35 C 0.6283(8) 0.2289(5) 0.0869(5) 0.045(2) Uani 1 1 d . . . H35A H 0.5925 0.2703 0.0525 0.054 Uiso 1 1 calc R . . C36 C 0.7335(8) 0.1784(5) 0.0743(4) 0.046(2) Uani 1 1 d . . . C37 C 0.7730(9) 0.1404(5) 0.1422(4) 0.047(2) Uani 1 1 d . . . C38 C 0.6897(9) 0.1707(5) 0.1942(4) 0.050(2) Uani 1 1 d . . . C39 C 0.7137(10) 0.1443(7) 0.2679(5) 0.066(3) Uani 1 1 d . . . H39A H 0.6589 0.1610 0.3013 0.079 Uiso 1 1 calc R . . C40 C 0.8155(11) 0.0951(7) 0.2899(5) 0.077(4) Uani 1 1 d . . . H40A H 0.8337 0.0821 0.3384 0.093 Uiso 1 1 calc R . . C41 C 0.8924(10) 0.0646(8) 0.2379(5) 0.081(3) Uani 1 1 d . . . H41A H 0.9577 0.0281 0.2526 0.097 Uiso 1 1 calc R . . C42 C 0.8745(9) 0.0866(6) 0.1663(5) 0.064(3) Uani 1 1 d . . . H42A H 0.9285 0.0663 0.1338 0.077 Uiso 1 1 calc R . . C43 C 0.6863(12) 0.1928(7) -0.0897(5) 0.087(4) Uani 1 1 d . . . H43A H 0.6390 0.2422 -0.0833 0.130 Uiso 1 1 calc R . . H43B H 0.6295 0.1466 -0.0921 0.130 Uiso 1 1 calc R . . H43C H 0.7267 0.1964 -0.1337 0.130 Uiso 1 1 calc R . . C44 C 0.9258(12) 0.2676(7) -0.0125(6) 0.092(4) Uani 1 1 d . . . H44A H 0.9912 0.2623 0.0267 0.138 Uiso 1 1 calc R . . H44B H 0.8805 0.3181 -0.0077 0.138 Uiso 1 1 calc R . . H44C H 0.9638 0.2676 -0.0573 0.138 Uiso 1 1 calc R . . C45 C 0.9040(11) 0.0820(7) -0.0252(5) 0.087(3) Uani 1 1 d . . . H45A H 0.9683 0.0744 0.0144 0.131 Uiso 1 1 calc R . . H45B H 0.9438 0.0859 -0.0693 0.131 Uiso 1 1 calc R . . H45C H 0.8467 0.0360 -0.0278 0.131 Uiso 1 1 calc R . . C46 C 0.3411(15) 0.1757(7) -0.0476(7) 0.099(5) Uani 1 1 d . . . H46A H 0.2927 0.1707 -0.0937 0.149 Uiso 1 1 calc R . . H46B H 0.4126 0.2113 -0.0518 0.149 Uiso 1 1 calc R . . H46C H 0.2881 0.1982 -0.0134 0.149 Uiso 1 1 calc R . . C47 C 0.341(2) 0.0332(8) -0.0670(8) 0.195(11) Uani 1 1 d . . . H47A H 0.2503 0.0434 -0.0784 0.234 Uiso 1 1 calc R . . H47B H 0.3797 0.0390 -0.1118 0.234 Uiso 1 1 calc R . . C48 C 0.3519(15) -0.0467(7) -0.0483(6) 0.101(5) Uani 1 1 d . . . H48A H 0.4001 -0.0736 -0.0833 0.122 Uiso 1 1 calc R . . H48B H 0.2670 -0.0704 -0.0533 0.122 Uiso 1 1 calc R . . C49 C 0.4131(10) -0.0693(6) 0.0259(5) 0.061(2) Uani 1 1 d . . . C50 C 0.3534(9) -0.0671(7) 0.0894(6) 0.067(3) Uani 1 1 d . . . H50A H 0.2610 -0.0625 0.0912 0.081 Uiso 1 1 calc R . . C51 C 0.4420(10) -0.0862(6) 0.1508(5) 0.057(3) Uani 1 1 d . . . C52 C 0.5610(10) -0.1022(5) 0.1214(5) 0.052(2) Uani 1 1 d . . . C53 C 0.5427(10) -0.0918(5) 0.0446(5) 0.050(2) Uani 1 1 d . . . C54 C 0.6501(15) -0.0988(6) 0.0032(7) 0.087(4) Uani 1 1 d . . . H54A H 0.6403 -0.0895 -0.0462 0.104 Uiso 1 1 calc R . . C55 C 0.7687(14) -0.1194(7) 0.0372(9) 0.099(4) Uani 1 1 d . . . H55A H 0.8385 -0.1257 0.0107 0.119 Uiso 1 1 calc R . . C56 C 0.7813(13) -0.1305(7) 0.1116(9) 0.091(4) Uani 1 1 d . . . H56A H 0.8611 -0.1448 0.1337 0.109 Uiso 1 1 calc R . . C57 C 0.6845(11) -0.1217(6) 0.1535(7) 0.071(3) Uani 1 1 d . . . H57A H 0.6989 -0.1284 0.2032 0.086 Uiso 1 1 calc R . . C58 C 0.4267(18) -0.2059(9) 0.2775(7) 0.142(7) Uani 1 1 d . . . H58A H 0.5143 -0.2211 0.2754 0.212 Uiso 1 1 calc R . . H58B H 0.3730 -0.2423 0.2476 0.212 Uiso 1 1 calc R . . H58C H 0.4056 -0.2099 0.3264 0.212 Uiso 1 1 calc R . . C59 C 0.494(2) -0.0320(11) 0.3108(8) 0.200(11) Uani 1 1 d . . . H59A H 0.5839 -0.0428 0.3102 0.300 Uiso 1 1 calc R . . H59B H 0.4698 -0.0419 0.3584 0.300 Uiso 1 1 calc R . . H59C H 0.4773 0.0242 0.2978 0.300 Uiso 1 1 calc R . . C60 C 0.2274(17) -0.0778(18) 0.2482(10) 0.235(13) Uani 1 1 d . . . H60A H 0.1783 -0.1130 0.2149 0.353 Uiso 1 1 calc R . . H60B H 0.2111 -0.0215 0.2350 0.353 Uiso 1 1 calc R . . H60C H 0.2037 -0.0871 0.2960 0.353 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 0.0458(2) 0.0458(2) 0.0455(2) -0.0092(2) 0.00688(18) 0.0016(2) Eu2 0.0442(2) 0.0317(2) 0.0514(2) -0.0059(2) 0.00073(18) -0.0020(2) Si1 0.0656(19) 0.074(2) 0.0678(18) 0.0260(15) 0.0153(15) 0.0196(16) Si2 0.081(2) 0.0579(17) 0.0518(14) 0.0006(13) 0.0051(14) 0.0110(15) Si3 0.0673(18) 0.0538(16) 0.0493(14) -0.0035(12) 0.0144(12) -0.0122(14) Si4 0.101(3) 0.063(2) 0.081(2) 0.0067(15) 0.0295(19) -0.0056(18) O1 0.060(5) 0.096(6) 0.096(6) -0.035(5) -0.014(4) 0.010(4) O2 0.080(5) 0.053(4) 0.093(5) 0.004(4) 0.030(4) -0.004(4) O3 0.050(4) 0.060(4) 0.110(6) -0.029(4) 0.012(4) -0.001(4) O4 0.093(5) 0.042(4) 0.082(5) 0.002(3) -0.028(4) 0.010(4) C1 0.059(8) 0.133(14) 0.163(13) -0.042(11) 0.013(8) -0.016(8) C2 0.065(9) 0.170(16) 0.107(11) -0.011(11) -0.035(8) -0.013(10) C3 0.113(13) 0.25(2) 0.148(14) -0.130(15) -0.071(11) 0.086(14) C4 0.057(7) 0.107(9) 0.065(7) -0.039(7) 0.003(5) 0.007(7) C5 0.054(6) 0.055(6) 0.084(7) -0.025(6) -0.006(5) 0.004(5) C6 0.035(5) 0.056(6) 0.057(5) -0.006(5) 0.011(4) 0.013(4) C7 0.047(6) 0.056(6) 0.059(6) 0.008(5) 0.018(5) 0.013(5) C8 0.087(8) 0.101(9) 0.036(5) 0.010(5) 0.025(5) 0.061(7) C9 0.142(14) 0.177(19) 0.074(8) 0.050(11) 0.053(9) 0.079(14) C10 0.19(2) 0.119(14) 0.19(2) 0.107(15) 0.140(19) 0.097(15) C11 0.105(13) 0.088(11) 0.22(2) 0.035(13) 0.095(14) 0.010(10) C12 0.068(7) 0.068(7) 0.117(9) 0.006(8) 0.047(6) 0.008(7) C13 0.184(17) 0.195(17) 0.054(7) 0.019(9) 0.008(9) 0.083(15) C14 0.20(2) 0.090(11) 0.175(16) 0.066(11) 0.015(14) 0.014(12) C15 0.064(9) 0.33(3) 0.181(16) 0.152(19) -0.007(10) 0.033(14) C16 0.106(11) 0.081(9) 0.156(13) 0.009(9) 0.060(10) -0.021(8) C17 0.112(11) 0.107(10) 0.081(8) 0.029(8) 0.050(8) 0.019(9) C18 0.187(16) 0.078(8) 0.063(7) 0.007(6) 0.051(8) 0.017(10) C19 0.112(10) 0.055(6) 0.047(6) -0.007(5) 0.027(6) 0.017(7) C20 0.074(6) 0.062(7) 0.060(6) -0.008(5) 0.024(5) 0.022(6) C21 0.078(7) 0.042(5) 0.040(5) 0.000(4) 0.012(5) 0.012(5) C22 0.081(8) 0.042(6) 0.050(5) -0.007(4) -0.012(5) 0.007(5) C23 0.107(9) 0.053(7) 0.043(5) -0.016(4) 0.005(5) 0.009(6) C24 0.141(13) 0.071(8) 0.052(7) -0.015(6) -0.022(8) 0.006(9) C25 0.130(12) 0.083(9) 0.092(9) -0.008(9) -0.039(8) -0.012(11) C26 0.087(10) 0.092(10) 0.116(11) -0.024(9) -0.003(9) -0.022(8) C27 0.085(9) 0.062(7) 0.089(8) -0.009(6) -0.015(7) -0.029(7) C28 0.139(13) 0.141(12) 0.054(7) 0.007(7) 0.016(7) 0.029(10) C29 0.093(10) 0.142(13) 0.106(10) 0.010(9) -0.014(8) 0.030(10) C30 0.160(14) 0.069(9) 0.110(10) 0.018(7) 0.001(10) 0.001(9) C31 0.054(8) 0.155(14) 0.175(15) -0.051(12) -0.007(9) 0.010(9) C32 0.099(13) 0.22(2) 0.46(4) -0.27(3) 0.124(19) -0.078(14) C33 0.071(7) 0.055(6) 0.084(7) -0.021(5) 0.015(6) 0.002(5) C34 0.042(5) 0.042(5) 0.061(5) -0.019(4) 0.007(4) -0.008(4) C35 0.050(5) 0.026(4) 0.060(5) -0.001(4) 0.007(4) -0.001(4) C36 0.048(5) 0.041(5) 0.048(5) -0.003(4) 0.004(4) -0.003(4) C37 0.055(6) 0.044(5) 0.042(5) 0.002(4) 0.001(4) -0.011(5) C38 0.053(6) 0.054(5) 0.044(5) -0.012(4) 0.003(4) -0.012(5) C39 0.064(7) 0.088(8) 0.047(5) -0.013(5) 0.015(5) -0.023(6) C40 0.073(7) 0.115(11) 0.042(5) 0.019(6) -0.002(5) -0.007(7) C41 0.087(8) 0.077(7) 0.073(7) 0.015(7) -0.017(6) 0.010(8) C42 0.057(6) 0.062(7) 0.072(6) 0.001(5) 0.005(5) -0.004(5) C43 0.108(10) 0.097(9) 0.055(6) -0.007(6) 0.012(6) 0.003(8) C44 0.101(9) 0.085(8) 0.094(8) -0.014(7) 0.029(7) -0.039(7) C45 0.120(9) 0.085(8) 0.061(6) -0.010(6) 0.029(6) 0.014(8) C46 0.130(12) 0.049(7) 0.108(10) 0.012(7) -0.045(9) 0.027(7) C47 0.39(3) 0.054(8) 0.112(11) 0.011(8) -0.141(16) -0.018(12) C48 0.157(13) 0.062(9) 0.075(8) 0.002(6) -0.043(8) -0.006(8) C49 0.090(7) 0.029(4) 0.059(5) -0.007(5) -0.015(5) -0.005(6) C50 0.054(6) 0.042(5) 0.102(8) -0.006(7) -0.014(5) -0.020(6) C51 0.067(6) 0.038(6) 0.067(6) 0.003(5) 0.014(5) 0.000(5) C52 0.064(6) 0.036(5) 0.055(5) -0.003(4) -0.004(5) 0.001(5) C53 0.072(6) 0.022(5) 0.057(5) -0.015(4) 0.005(5) 0.002(4) C54 0.159(13) 0.031(5) 0.077(7) -0.012(5) 0.049(8) -0.001(7) C55 0.102(11) 0.064(8) 0.139(13) 0.012(8) 0.054(10) 0.030(8) C56 0.079(9) 0.060(7) 0.135(12) 0.016(8) 0.014(9) 0.015(7) C57 0.070(8) 0.051(6) 0.091(8) -0.002(6) -0.006(6) 0.003(6) C58 0.22(2) 0.100(11) 0.098(10) 0.032(9) 0.005(11) -0.032(12) C59 0.35(3) 0.175(18) 0.086(10) -0.043(11) 0.077(14) -0.146(19) C60 0.169(17) 0.36(3) 0.20(2) 0.15(2) 0.118(16) 0.11(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O1 2.561(7) . ? Eu1 O2 2.609(7) . ? Eu1 C19 2.806(9) . ? Eu1 C23 2.806(9) . ? Eu1 C4 2.819(10) . ? Eu1 C8 2.840(8) . ? Eu1 C5 2.841(9) . ? Eu1 C22 2.861(9) . ? Eu1 C6 2.871(8) . ? Eu1 C7 2.886(9) . ? Eu1 C20 2.888(9) . ? Eu1 C21 2.904(9) . ? Eu2 O3 2.567(7) . ? Eu2 O4 2.611(6) . ? Eu2 C53 2.826(7) . ? Eu2 C35 2.827(8) . ? Eu2 C34 2.827(8) . ? Eu2 C49 2.829(9) . ? Eu2 C52 2.860(9) . ? Eu2 C50 2.865(9) . ? Eu2 C36 2.889(9) . ? Eu2 C38 2.893(8) . ? Eu2 C51 2.894(9) . ? Eu2 C37 2.908(8) . ? Si1 C13 1.839(13) . ? Si1 C15 1.855(14) . ? Si1 C6 1.862(9) . ? Si1 C14 1.878(15) . ? Si2 C29 1.852(13) . ? Si2 C21 1.870(9) . ? Si2 C30 1.873(12) . ? Si2 C28 1.877(11) . ? Si3 C36 1.863(9) . ? Si3 C44 1.871(11) . ? Si3 C45 1.891(11) . ? Si3 C43 1.895(11) . ? Si4 C58 1.828(14) . ? Si4 C59 1.855(15) . ? Si4 C51 1.868(10) . ? Si4 C60 1.886(17) . ? O1 C2 1.387(16) . ? O1 C1 1.423(13) . ? O2 C16 1.435(13) . ? O2 C17 1.438(13) . ? O3 C32 1.368(15) . ? O3 C31 1.382(13) . ? O4 C47 1.366(13) . ? O4 C46 1.428(11) . ? C2 C3 1.322(18) . ? C3 C4 1.490(16) . ? C4 C5 1.377(15) . ? C4 C8 1.402(15) . ? C5 C6 1.409(12) . ? C6 C7 1.444(13) . ? C7 C12 1.398(14) . ? C7 C8 1.478(13) . ? C8 C9 1.411(18) . ? C9 C10 1.34(3) . ? C10 C11 1.38(3) . ? C11 C12 1.425(19) . ? C17 C18 1.495(17) . ? C18 C19 1.533(15) . ? C19 C20 1.400(14) . ? C19 C23 1.419(15) . ? C20 C21 1.414(13) . ? C21 C22 1.468(14) . ? C22 C27 1.388(15) . ? C22 C23 1.448(13) . ? C23 C24 1.419(16) . ? C24 C25 1.351(18) . ? C25 C26 1.420(18) . ? C26 C27 1.383(16) . ? C32 C33 1.334(18) . ? C33 C34 1.501(12) . ? C34 C35 1.398(12) . ? C34 C38 1.429(12) . ? C35 C36 1.418(11) . ? C36 C37 1.435(11) . ? C37 C42 1.423(13) . ? C37 C38 1.453(12) . ? C38 C39 1.438(13) . ? C39 C40 1.370(15) . ? C40 C41 1.411(15) . ? C41 C42 1.378(13) . ? C47 C48 1.351(15) . ? C48 C49 1.515(13) . ? C49 C50 1.392(13) . ? C49 C53 1.424(13) . ? C50 C51 1.440(13) . ? C51 C52 1.439(13) . ? C52 C57 1.416(14) . ? C52 C53 1.437(12) . ? C53 C54 1.432(15) . ? C54 C55 1.387(18) . ? C55 C56 1.393(18) . ? C56 C57 1.350(17) . ? 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 O2 88.1(3) . . ? O1 Eu1 C19 113.3(3) . . ? O2 Eu1 C19 64.5(3) . . ? O1 Eu1 C23 137.0(3) . . ? O2 Eu1 C23 86.4(3) . . ? C19 Eu1 C23 29.3(3) . . ? O1 Eu1 C4 63.2(3) . . ? O2 Eu1 C4 108.5(3) . . ? C19 Eu1 C4 172.8(4) . . ? C23 Eu1 C4 156.8(4) . . ? O1 Eu1 C8 81.4(3) . . ? O2 Eu1 C8 134.3(3) . . ? C19 Eu1 C8 158.4(4) . . ? C23 Eu1 C8 129.9(4) . . ? C4 Eu1 C8 28.7(3) . . ? O1 Eu1 C5 80.7(3) . . ? O2 Eu1 C5 88.3(3) . . ? C19 Eu1 C5 147.8(3) . . ? C23 Eu1 C5 141.5(3) . . ? C4 Eu1 C5 28.2(3) . . ? C8 Eu1 C5 46.2(3) . . ? O1 Eu1 C22 120.9(3) . . ? O2 Eu1 C22 112.3(3) . . ? C19 Eu1 C22 48.2(3) . . ? C23 Eu1 C22 29.6(3) . . ? C4 Eu1 C22 139.0(4) . . ? C8 Eu1 C22 111.2(4) . . ? C5 Eu1 C22 149.2(3) . . ? O1 Eu1 C6 108.5(2) . . ? O2 Eu1 C6 95.4(2) . . ? C19 Eu1 C6 132.1(3) . . ? C23 Eu1 C6 114.4(3) . . ? C4 Eu1 C6 48.1(3) . . ? C8 Eu1 C6 48.1(3) . . ? C5 Eu1 C6 28.6(3) . . ? C22 Eu1 C6 122.7(3) . . ? O1 Eu1 C7 109.8(3) . . ? O2 Eu1 C7 124.2(2) . . ? C19 Eu1 C7 136.3(3) . . ? C23 Eu1 C7 108.4(3) . . ? C4 Eu1 C7 48.5(3) . . ? C8 Eu1 C7 29.9(3) . . ? C5 Eu1 C7 46.9(3) . . ? C22 Eu1 C7 102.6(3) . . ? C6 Eu1 C7 29.1(2) . . ? O1 Eu1 C20 90.0(3) . . ? O2 Eu1 C20 77.8(3) . . ? C19 Eu1 C20 28.4(3) . . ? C23 Eu1 C20 47.2(3) . . ? C4 Eu1 C20 151.6(3) . . ? C8 Eu1 C20 145.9(3) . . ? C5 Eu1 C20 163.5(3) . . ? C22 Eu1 C20 46.9(3) . . ? C6 Eu1 C20 160.2(3) . . ? C7 Eu1 C20 149.5(3) . . ? O1 Eu1 C21 92.7(3) . . ? O2 Eu1 C21 106.0(2) . . ? C19 Eu1 C21 48.0(3) . . ? C23 Eu1 C21 48.7(3) . . ? C4 Eu1 C21 136.5(3) . . ? C8 Eu1 C21 118.8(3) . . ? C5 Eu1 C21 164.2(3) . . ? C22 Eu1 C21 29.5(3) . . ? C6 Eu1 C21 150.3(3) . . ? C7 Eu1 C21 124.4(3) . . ? C20 Eu1 C21 28.3(3) . . ? O3 Eu2 O4 83.3(2) . . ? O3 Eu2 C53 134.0(3) . . ? O4 Eu2 C53 84.4(2) . . ? O3 Eu2 C35 81.5(2) . . ? O4 Eu2 C35 88.5(2) . . ? C53 Eu2 C35 142.2(3) . . ? O3 Eu2 C34 64.1(2) . . ? O4 Eu2 C34 107.7(2) . . ? C53 Eu2 C34 160.5(3) . . ? C35 Eu2 C34 28.6(2) . . ? O3 Eu2 C49 108.4(3) . . ? O4 Eu2 C49 63.3(2) . . ? C53 Eu2 C49 29.2(3) . . ? C35 Eu2 C49 147.9(3) . . ? C34 Eu2 C49 169.7(3) . . ? O3 Eu2 C52 122.7(3) . . ? O4 Eu2 C52 110.7(2) . . ? C53 Eu2 C52 29.3(2) . . ? C35 Eu2 C52 149.6(3) . . ? C34 Eu2 C52 141.5(3) . . ? C49 Eu2 C52 48.0(3) . . ? O3 Eu2 C50 87.1(3) . . ? O4 Eu2 C50 77.6(3) . . ? C53 Eu2 C50 47.0(3) . . ? C35 Eu2 C50 163.0(3) . . ? C34 Eu2 C50 149.1(3) . . ? C49 Eu2 C50 28.3(3) . . ? C52 Eu2 C50 47.0(3) . . ? O3 Eu2 C36 109.4(2) . . ? O4 Eu2 C36 98.0(2) . . ? C53 Eu2 C36 116.1(3) . . ? C35 Eu2 C36 28.7(2) . . ? C34 Eu2 C36 48.3(2) . . ? C49 Eu2 C36 135.0(3) . . ? C52 Eu2 C36 122.1(3) . . ? C50 Eu2 C36 162.5(3) . . ? O3 Eu2 C38 83.1(2) . . ? O4 Eu2 C38 134.3(2) . . ? C53 Eu2 C38 133.6(3) . . ? C35 Eu2 C38 46.4(3) . . ? C34 Eu2 C38 28.9(2) . . ? C49 Eu2 C38 161.2(3) . . ? C52 Eu2 C38 113.3(3) . . ? C50 Eu2 C38 144.5(3) . . ? C36 Eu2 C38 47.5(2) . . ? O3 Eu2 C51 94.0(3) . . ? O4 Eu2 C51 106.4(2) . . ? C53 Eu2 C51 48.2(3) . . ? C35 Eu2 C51 163.9(3) . . ? C34 Eu2 C51 136.3(3) . . ? C49 Eu2 C51 48.1(3) . . ? C52 Eu2 C51 29.0(3) . . ? C50 Eu2 C51 29.0(3) . . ? C36 Eu2 C51 148.0(3) . . ? C38 Eu2 C51 117.9(3) . . ? O3 Eu2 C37 110.5(2) . . ? O4 Eu2 C37 126.6(2) . . ? C53 Eu2 C37 112.3(3) . . ? C35 Eu2 C37 46.7(2) . . ? C34 Eu2 C37 48.2(2) . . ? C49 Eu2 C37 140.7(3) . . ? C52 Eu2 C37 103.8(3) . . ? C50 Eu2 C37 150.3(3) . . ? C36 Eu2 C37 28.7(2) . . ? C38 Eu2 C37 29.0(2) . . ? C51 Eu2 C37 122.8(3) . . ? C13 Si1 C15 109.6(9) . . ? C13 Si1 C6 112.8(5) . . ? C15 Si1 C6 110.7(5) . . ? C13 Si1 C14 107.9(8) . . ? C15 Si1 C14 106.9(9) . . ? C6 Si1 C14 108.7(6) . . ? C29 Si2 C21 109.2(6) . . ? C29 Si2 C30 108.6(7) . . ? C21 Si2 C30 110.7(5) . . ? C29 Si2 C28 108.4(6) . . ? C21 Si2 C28 111.6(5) . . ? C30 Si2 C28 108.3(7) . . ? C36 Si3 C44 110.9(5) . . ? C36 Si3 C45 112.8(4) . . ? C44 Si3 C45 107.8(6) . . ? C36 Si3 C43 109.0(5) . . ? C44 Si3 C43 107.6(6) . . ? C45 Si3 C43 108.6(5) . . ? C58 Si4 C59 107.7(8) . . ? C58 Si4 C51 112.9(6) . . ? C59 Si4 C51 113.3(6) . . ? C58 Si4 C60 106.5(10) . . ? C59 Si4 C60 108.4(11) . . ? C51 Si4 C60 107.8(6) . . ? C2 O1 C1 115.5(10) . . ? C2 O1 Eu1 121.2(7) . . ? C1 O1 Eu1 122.3(7) . . ? C16 O2 C17 113.3(9) . . ? C16 O2 Eu1 123.3(7) . . ? C17 O2 Eu1 120.4(6) . . ? C32 O3 C31 114.7(11) . . ? C32 O3 Eu2 118.4(8) . . ? C31 O3 Eu2 126.7(7) . . ? C47 O4 C46 114.4(8) . . ? C47 O4 Eu2 121.3(6) . . ? C46 O4 Eu2 124.1(6) . . ? C3 C2 O1 121.4(11) . . ? C2 C3 C4 120.2(12) . . ? C5 C4 C8 106.7(9) . . ? C5 C4 C3 128.7(15) . . ? C8 C4 C3 124.5(14) . . ? C5 C4 Eu1 76.8(6) . . ? C8 C4 Eu1 76.5(5) . . ? C3 C4 Eu1 110.5(8) . . ? C4 C5 C6 112.8(10) . . ? C4 C5 Eu1 75.0(6) . . ? C6 C5 Eu1 76.9(5) . . ? C5 C6 C7 106.0(9) . . ? C5 C6 Si1 124.2(8) . . ? C7 C6 Si1 128.9(7) . . ? C5 C6 Eu1 74.5(5) . . ? C7 C6 Eu1 76.0(5) . . ? Si1 C6 Eu1 123.5(4) . . ? C12 C7 C6 132.0(10) . . ? C12 C7 C8 122.4(10) . . ? C6 C7 C8 105.6(9) . . ? C12 C7 Eu1 116.5(6) . . ? C6 C7 Eu1 74.9(5) . . ? C8 C7 Eu1 73.3(5) . . ? C4 C8 C9 135.8(13) . . ? C4 C8 C7 108.9(9) . . ? C9 C8 C7 115.3(13) . . ? C4 C8 Eu1 74.8(5) . . ? C9 C8 Eu1 116.0(8) . . ? C7 C8 Eu1 76.8(5) . . ? C10 C9 C8 121.4(17) . . ? C9 C10 C11 124.0(16) . . ? C10 C11 C12 119.4(16) . . ? C7 C12 C11 117.4(13) . . ? O2 C17 C18 112.5(11) . . ? C17 C18 C19 112.8(10) . . ? C20 C19 C23 108.0(9) . . ? C20 C19 C18 127.7(12) . . ? C23 C19 C18 124.3(11) . . ? C20 C19 Eu1 79.1(5) . . ? C23 C19 Eu1 75.4(5) . . ? C18 C19 Eu1 110.5(7) . . ? C19 C20 C21 111.4(10) . . ? C19 C20 Eu1 72.5(5) . . ? C21 C20 Eu1 76.5(5) . . ? C20 C21 C22 105.1(8) . . ? C20 C21 Si2 127.1(8) . . ? C22 C21 Si2 127.1(7) . . ? C20 C21 Eu1 75.3(5) . . ? C22 C21 Eu1 73.6(5) . . ? Si2 C21 Eu1 123.4(4) . . ? C27 C22 C23 119.9(10) . . ? C27 C22 C21 132.3(10) . . ? C23 C22 C21 107.9(10) . . ? C27 C22 Eu1 115.3(7) . . ? C23 C22 Eu1 73.1(5) . . ? C21 C22 Eu1 76.9(5) . . ? C24 C23 C19 132.6(11) . . ? C24 C23 C22 119.8(12) . . ? C19 C23 C22 107.5(10) . . ? C24 C23 Eu1 110.7(7) . . ? C19 C23 Eu1 75.3(5) . . ? C22 C23 Eu1 77.3(5) . . ? C25 C24 C23 117.7(12) . . ? C24 C25 C26 123.5(13) . . ? C27 C26 C25 119.4(13) . . ? C26 C27 C22 119.6(12) . . ? C33 C32 O3 125.4(14) . . ? C32 C33 C34 117.5(10) . . ? C35 C34 C38 105.7(7) . . ? C35 C34 C33 127.6(9) . . ? C38 C34 C33 126.7(8) . . ? C35 C34 Eu2 75.7(5) . . ? C38 C34 Eu2 78.1(5) . . ? C33 C34 Eu2 110.2(6) . . ? C34 C35 C36 112.5(8) . . ? C34 C35 Eu2 75.7(5) . . ? C36 C35 Eu2 78.1(5) . . ? C35 C36 C37 105.7(8) . . ? C35 C36 Si3 123.7(6) . . ? C37 C36 Si3 129.9(7) . . ? C35 C36 Eu2 73.2(5) . . ? C37 C36 Eu2 76.4(5) . . ? Si3 C36 Eu2 122.7(4) . . ? C42 C37 C36 133.7(9) . . ? C42 C37 C38 118.8(8) . . ? C36 C37 C38 107.4(8) . . ? C42 C37 Eu2 118.4(6) . . ? C36 C37 Eu2 74.9(5) . . ? C38 C37 Eu2 74.9(5) . . ? C34 C38 C39 133.1(9) . . ? C34 C38 C37 108.7(7) . . ? C39 C38 C37 118.2(9) . . ? C34 C38 Eu2 73.0(4) . . ? C39 C38 Eu2 117.7(6) . . ? C37 C38 Eu2 76.0(5) . . ? C40 C39 C38 121.5(9) . . ? C39 C40 C41 119.0(9) . . ? C42 C41 C40 122.6(11) . . ? C41 C42 C37 119.7(10) . . ? C48 C47 O4 124.0(10) . . ? C47 C48 C49 119.3(10) . . ? C50 C49 C53 107.4(8) . . ? C50 C49 C48 125.6(11) . . ? C53 C49 C48 126.9(11) . . ? C50 C49 Eu2 77.3(5) . . ? C53 C49 Eu2 75.3(5) . . ? C48 C49 Eu2 111.0(7) . . ? C49 C50 C51 111.0(9) . . ? C49 C50 Eu2 74.5(6) . . ? C51 C50 Eu2 76.6(5) . . ? C52 C51 C50 105.0(9) . . ? C52 C51 Si4 128.2(7) . . ? C50 C51 Si4 126.3(8) . . ? C52 C51 Eu2 74.2(5) . . ? C50 C51 Eu2 74.4(5) . . ? Si4 C51 Eu2 122.4(4) . . ? C57 C52 C53 118.6(10) . . ? C57 C52 C51 132.8(10) . . ? C53 C52 C51 108.6(8) . . ? C57 C52 Eu2 112.9(6) . . ? C53 C52 Eu2 74.1(4) . . ? C51 C52 Eu2 76.8(5) . . ? C49 C53 C54 132.6(10) . . ? C49 C53 C52 107.9(8) . . ? C54 C53 C52 119.3(10) . . ? C49 C53 Eu2 75.6(5) . . ? C54 C53 Eu2 110.2(6) . . ? C52 C53 Eu2 76.7(4) . . ? C55 C54 C53 119.8(11) . . ? C54 C55 C56 118.9(12) . . ? C57 C56 C55 123.8(13) . . ? C56 C57 C52 119.6(12) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.659 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.089 #===END