# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 1145/181 data_shelxs1323 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H101 O11 Y3' _chemical_formula_weight 1072.98 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' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.431(13) _cell_length_b 10.867(6) _cell_length_c 27.55(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.15(6) _cell_angle_gamma 90.00 _cell_volume 5744(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 3.052 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6308 _exptl_absorpt_correction_T_max 0.9986 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe AED2' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 7522 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1543 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 22.53 _reflns_number_total 7522 _reflns_number_gt 3877 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+19.7193P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7522 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2186 _refine_ls_R_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1400 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _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 Y1 Y 0.35532(6) 0.77388(11) 0.35989(5) 0.0406(4) Uani 1 1 d . . . Y2 Y 0.23743(6) 0.69122(12) 0.25727(5) 0.0521(4) Uani 1 1 d . . . Y3 Y 0.18962(6) 0.68136(12) 0.37550(5) 0.0528(4) Uani 1 1 d . . . O1 O 0.3533(4) 0.7527(6) 0.2777(3) 0.040(2) Uani 1 1 d . . . O2 O 0.2935(4) 0.7424(6) 0.4225(3) 0.039(2) Uani 1 1 d . . . O3 O 0.1424(4) 0.6497(7) 0.2948(3) 0.046(2) Uani 1 1 d . . . O4 O 0.2426(3) 0.8328(6) 0.3270(2) 0.0312(19) Uani 1 1 d . . . O5 O 0.2828(4) 0.6002(6) 0.3366(3) 0.038(2) Uani 1 1 d . . . O6 O 0.1156(4) 0.7855(9) 0.4117(3) 0.076(3) Uani 1 1 d . . . O7 O 0.1536(5) 0.5250(8) 0.4132(3) 0.071(3) Uani 1 1 d . . . O8 O 0.2021(4) 0.8054(9) 0.1939(3) 0.066(3) Uani 1 1 d . . . O9 O 0.2350(4) 0.5404(8) 0.2051(4) 0.073(3) Uani 1 1 d . . . O10 O 0.4162(4) 0.9264(7) 0.3802(3) 0.049(2) Uani 1 1 d . . . O11 O 0.4767(4) 0.6931(8) 0.3925(3) 0.055(2) Uani 1 1 d . . . C1 C 0.4051(7) 0.7761(12) 0.2467(5) 0.050(4) Uani 1 1 d . . . C2 C 0.4738(7) 0.740(2) 0.2706(6) 0.169(12) Uani 1 1 d . . . H2A H 0.4850 0.7840 0.3011 0.253 Uiso 1 1 calc R . . H2B H 0.5074 0.7602 0.2497 0.253 Uiso 1 1 calc R . . H2C H 0.4746 0.6535 0.2768 0.253 Uiso 1 1 calc R . . C3 C 0.3843(8) 0.7148(17) 0.1993(6) 0.119(7) Uani 1 1 d . . . H3A H 0.3387 0.7425 0.1848 0.178 Uiso 1 1 calc R . . H3B H 0.3834 0.6274 0.2042 0.178 Uiso 1 1 calc R . . H3C H 0.4170 0.7343 0.1778 0.178 Uiso 1 1 calc R . . C4 C 0.4069(9) 0.9146(15) 0.2362(6) 0.125(7) Uani 1 1 d . . . H4A H 0.3619 0.9408 0.2200 0.187 Uiso 1 1 calc R . . H4B H 0.4412 0.9311 0.2155 0.187 Uiso 1 1 calc R . . H4C H 0.4188 0.9585 0.2666 0.187 Uiso 1 1 calc R . . C5 C 0.3122(6) 0.7587(13) 0.4746(4) 0.045(4) Uani 1 1 d . . . C6 C 0.3906(6) 0.7401(14) 0.4888(5) 0.076(5) Uani 1 1 d . . . H6A H 0.4026 0.6579 0.4807 0.115 Uiso 1 1 calc R . . H6B H 0.4037 0.7529 0.5236 0.115 Uiso 1 1 calc R . . H6C H 0.4148 0.7979 0.4713 0.115 Uiso 1 1 calc R . . C7 C 0.2733(7) 0.6658(14) 0.5010(5) 0.091(5) Uani 1 1 d . . . H7A H 0.2855 0.5841 0.4923 0.136 Uiso 1 1 calc R . . H7B H 0.2240 0.6777 0.4916 0.136 Uiso 1 1 calc R . . H7C H 0.2856 0.6768 0.5359 0.136 Uiso 1 1 calc R . . C8 C 0.2934(7) 0.8878(13) 0.4883(5) 0.076(5) Uani 1 1 d . . . H8A H 0.3183 0.9463 0.4716 0.114 Uiso 1 1 calc R . . H8B H 0.3057 0.8989 0.5232 0.114 Uiso 1 1 calc R . . H8C H 0.2441 0.9003 0.4788 0.114 Uiso 1 1 calc R . . C9 C 0.0729(7) 0.6128(13) 0.2725(5) 0.060(4) Uani 1 1 d . . . C10 C 0.0211(6) 0.6640(14) 0.3040(5) 0.087(5) Uani 1 1 d . . . H10A H 0.0221 0.7522 0.3033 0.131 Uiso 1 1 calc R . . H10B H 0.0339 0.6360 0.3373 0.131 Uiso 1 1 calc R . . H10C H -0.0250 0.6356 0.2912 0.131 Uiso 1 1 calc R . . C11 C 0.0560(7) 0.6625(15) 0.2216(5) 0.089(5) Uani 1 1 d . . . H11A H 0.0570 0.7508 0.2226 0.134 Uiso 1 1 calc R . . H11B H 0.0104 0.6353 0.2070 0.134 Uiso 1 1 calc R . . H11C H 0.0898 0.6334 0.2023 0.134 Uiso 1 1 calc R . . C12 C 0.0704(7) 0.4738(13) 0.2731(6) 0.103(6) Uani 1 1 d . . . H12A H 0.0813 0.4450 0.3064 0.155 Uiso 1 1 calc R . . H12B H 0.1039 0.4415 0.2543 0.155 Uiso 1 1 calc R . . H12C H 0.0246 0.4465 0.2591 0.155 Uiso 1 1 calc R . . C13 C 0.2194(6) 0.9587(10) 0.3214(5) 0.039(3) Uani 1 1 d . . . C14 C 0.2595(6) 1.0237(10) 0.2853(4) 0.049(4) Uani 1 1 d . . . H14A H 0.2509 0.9827 0.2541 0.074 Uiso 1 1 calc R . . H14B H 0.3085 1.0216 0.2979 0.074 Uiso 1 1 calc R . . H14C H 0.2443 1.1077 0.2814 0.074 Uiso 1 1 calc R . . C15 C 0.1416(6) 0.9593(11) 0.3000(4) 0.054(4) Uani 1 1 d . . . H15A H 0.1347 0.9190 0.2686 0.080 Uiso 1 1 calc R . . H15B H 0.1254 1.0427 0.2961 0.080 Uiso 1 1 calc R . . H15C H 0.1160 0.9166 0.3219 0.080 Uiso 1 1 calc R . . C16 C 0.2314(6) 1.0225(10) 0.3708(4) 0.054(4) Uani 1 1 d . . . H16A H 0.2804 1.0223 0.3836 0.081 Uiso 1 1 calc R . . H16B H 0.2065 0.9798 0.3931 0.081 Uiso 1 1 calc R . . H16C H 0.2150 1.1058 0.3670 0.081 Uiso 1 1 calc R . . C17 C 0.3074(7) 0.4773(11) 0.3424(5) 0.052(4) Uani 1 1 d . . . C18 C 0.2479(7) 0.3888(10) 0.3245(5) 0.068(5) Uani 1 1 d . . . H18A H 0.2310 0.4037 0.2903 0.103 Uiso 1 1 calc R . . H18B H 0.2107 0.4015 0.3432 0.103 Uiso 1 1 calc R . . H18C H 0.2643 0.3056 0.3288 0.103 Uiso 1 1 calc R . . C19 C 0.3660(6) 0.4597(11) 0.3114(5) 0.064(4) Uani 1 1 d . . . H19A H 0.3478 0.4735 0.2774 0.096 Uiso 1 1 calc R . . H19B H 0.3838 0.3774 0.3156 0.096 Uiso 1 1 calc R . . H19C H 0.4028 0.5173 0.3219 0.096 Uiso 1 1 calc R . . C20 C 0.3350(7) 0.4528(12) 0.3962(5) 0.071(4) Uani 1 1 d . . . H20A H 0.2979 0.4620 0.4152 0.107 Uiso 1 1 calc R . . H20B H 0.3715 0.5104 0.4076 0.107 Uiso 1 1 calc R . . H20C H 0.3532 0.3706 0.3999 0.107 Uiso 1 1 calc R . . C21 C 0.0664(8) 0.8529(17) 0.4343(6) 0.079(5) Uani 1 1 d . . . C22 C 0.0005(11) 0.780(2) 0.4304(9) 0.192(11) Uani 1 1 d . . . H22A H 0.0098 0.7033 0.4474 0.288 Uiso 1 1 calc R . . H22B H -0.0173 0.7648 0.3964 0.288 Uiso 1 1 calc R . . H22C H -0.0333 0.8258 0.4450 0.288 Uiso 1 1 calc R . . C23 C 0.0481(12) 0.9678(17) 0.4081(9) 0.201(14) Uani 1 1 d . . . H23A H 0.0322 0.9506 0.3740 0.301 Uiso 1 1 calc R . . H23B H 0.0883 1.0203 0.4112 0.301 Uiso 1 1 calc R . . H23C H 0.0117 1.0081 0.4218 0.301 Uiso 1 1 calc R . . C24 C 0.0904(10) 0.873(3) 0.4871(7) 0.248(18) Uani 1 1 d . . . H24A H 0.1021 0.7960 0.5030 0.372 Uiso 1 1 calc R . . H24B H 0.0539 0.9120 0.5013 0.372 Uiso 1 1 calc R . . H24C H 0.1307 0.9258 0.4913 0.372 Uiso 1 1 calc R . . C25 C 0.1290(10) 0.4276(17) 0.4381(7) 0.087(5) Uani 1 1 d . . . C26 C 0.1827(14) 0.3348(19) 0.4520(10) 0.226(15) Uani 1 1 d . . . H26A H 0.2009 0.3083 0.4233 0.339 Uiso 1 1 calc R . . H26B H 0.1629 0.2657 0.4666 0.339 Uiso 1 1 calc R . . H26C H 0.2197 0.3693 0.4753 0.339 Uiso 1 1 calc R . . C27 C 0.1046(15) 0.4630(19) 0.4818(10) 0.236(17) Uani 1 1 d . . . H27A H 0.1405 0.5072 0.5026 0.354 Uiso 1 1 calc R . . H27B H 0.0922 0.3909 0.4986 0.354 Uiso 1 1 calc R . . H27C H 0.0644 0.5148 0.4737 0.354 Uiso 1 1 calc R . . C28 C 0.0750(15) 0.357(3) 0.4049(9) 0.30(2) Uani 1 1 d . . . H28A H 0.0938 0.3300 0.3765 0.444 Uiso 1 1 calc R . . H28B H 0.0351 0.4082 0.3947 0.444 Uiso 1 1 calc R . . H28C H 0.0612 0.2862 0.4220 0.444 Uiso 1 1 calc R . . C29 C 0.1787(7) 0.8787(15) 0.1519(6) 0.065(4) Uani 1 1 d . . . C30 C 0.2368(9) 0.9449(19) 0.1339(6) 0.139(9) Uani 1 1 d . . . H30A H 0.2584 1.0005 0.1589 0.209 Uiso 1 1 calc R . . H30B H 0.2189 0.9904 0.1048 0.209 Uiso 1 1 calc R . . H30C H 0.2707 0.8864 0.1265 0.209 Uiso 1 1 calc R . . C31 C 0.1275(8) 0.9736(16) 0.1633(6) 0.109(6) Uani 1 1 d . . . H31A H 0.0886 0.9335 0.1741 0.164 Uiso 1 1 calc R . . H31B H 0.1114 1.0210 0.1343 0.164 Uiso 1 1 calc R . . H31C H 0.1498 1.0271 0.1888 0.164 Uiso 1 1 calc R . . C32 C 0.1430(11) 0.7964(19) 0.1118(6) 0.165(10) Uani 1 1 d . . . H32A H 0.1049 0.7546 0.1231 0.248 Uiso 1 1 calc R . . H32B H 0.1756 0.7369 0.1033 0.248 Uiso 1 1 calc R . . H32C H 0.1255 0.8450 0.0834 0.248 Uiso 1 1 calc R . . C33 C 0.2355(10) 0.4416(17) 0.1712(7) 0.086(5) Uani 1 1 d . . . C34 C 0.2790(15) 0.3403(18) 0.1925(8) 0.216(15) Uani 1 1 d . . . H34A H 0.3258 0.3693 0.2028 0.324 Uiso 1 1 calc R . . H34B H 0.2792 0.2766 0.1684 0.324 Uiso 1 1 calc R . . H34C H 0.2609 0.3082 0.2204 0.324 Uiso 1 1 calc R . . C35 C 0.2634(16) 0.483(2) 0.1292(8) 0.221(15) Uani 1 1 d . . . H35A H 0.3111 0.5066 0.1389 0.331 Uiso 1 1 calc R . . H35B H 0.2370 0.5520 0.1148 0.331 Uiso 1 1 calc R . . H35C H 0.2607 0.4174 0.1055 0.331 Uiso 1 1 calc R . . C36 C 0.1668(11) 0.401(3) 0.1558(13) 0.37(3) Uani 1 1 d . . . H36A H 0.1476 0.3721 0.1837 0.553 Uiso 1 1 calc R . . H36B H 0.1668 0.3357 0.1325 0.553 Uiso 1 1 calc R . . H36C H 0.1391 0.4683 0.1408 0.553 Uiso 1 1 calc R . . C37 C 0.4535(7) 1.0336(12) 0.3930(5) 0.051(4) Uani 1 1 d . . . C38 C 0.5311(7) 1.0094(13) 0.3999(6) 0.098(6) Uani 1 1 d . . . H38A H 0.5430 0.9482 0.4250 0.147 Uiso 1 1 calc R . . H38B H 0.5558 1.0842 0.4096 0.147 Uiso 1 1 calc R . . H38C H 0.5436 0.9806 0.3696 0.147 Uiso 1 1 calc R . . C39 C 0.4374(7) 1.1324(12) 0.3541(5) 0.081(5) Uani 1 1 d . . . H39A H 0.3885 1.1507 0.3492 0.122 Uiso 1 1 calc R . . H39B H 0.4502 1.1037 0.3238 0.122 Uiso 1 1 calc R . . H39C H 0.4634 1.2054 0.3646 0.122 Uiso 1 1 calc R . . C40 C 0.4358(8) 1.0880(13) 0.4409(5) 0.093(6) Uani 1 1 d . . . H40A H 0.3867 1.1044 0.4371 0.140 Uiso 1 1 calc R . . H40B H 0.4612 1.1632 0.4483 0.140 Uiso 1 1 calc R . . H40C H 0.4484 1.0304 0.4672 0.140 Uiso 1 1 calc R . . C41 C 0.5403(8) 0.6257(13) 0.4112(6) 0.065(4) Uani 1 1 d . . . C42 C 0.5279(7) 0.4890(14) 0.4021(6) 0.098(6) Uani 1 1 d . . . H42A H 0.4945 0.4599 0.4216 0.147 Uiso 1 1 calc R . . H42B H 0.5709 0.4452 0.4110 0.147 Uiso 1 1 calc R . . H42C H 0.5103 0.4756 0.3679 0.147 Uiso 1 1 calc R . . C43 C 0.5947(7) 0.6639(15) 0.3813(6) 0.107(6) Uani 1 1 d . . . H43A H 0.5792 0.6439 0.3474 0.160 Uiso 1 1 calc R . . H43B H 0.6374 0.6214 0.3928 0.160 Uiso 1 1 calc R . . H43C H 0.6022 0.7511 0.3845 0.160 Uiso 1 1 calc R . . C44 C 0.5622(8) 0.6528(17) 0.4645(6) 0.123(8) Uani 1 1 d . . . H44A H 0.5264 0.6266 0.4825 0.185 Uiso 1 1 calc R . . H44B H 0.5696 0.7397 0.4689 0.185 Uiso 1 1 calc R . . H44C H 0.6047 0.6097 0.4764 0.185 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 Y1 0.0421(7) 0.0359(7) 0.0447(8) -0.0014(7) 0.0100(6) -0.0038(6) Y2 0.0414(8) 0.0475(8) 0.0674(10) -0.0060(8) 0.0090(7) -0.0017(7) Y3 0.0429(8) 0.0491(9) 0.0644(10) 0.0013(8) 0.0024(7) -0.0043(7) O1 0.038(5) 0.042(5) 0.043(5) 0.001(4) 0.017(4) 0.001(4) O2 0.043(5) 0.042(5) 0.031(5) 0.008(4) 0.003(4) -0.002(4) O3 0.030(5) 0.050(5) 0.054(6) -0.002(5) -0.001(4) -0.010(4) O4 0.033(4) 0.030(4) 0.031(5) -0.004(4) 0.004(4) 0.002(4) O5 0.041(5) 0.020(4) 0.054(6) -0.003(4) 0.013(4) 0.002(4) O6 0.064(6) 0.113(8) 0.054(6) -0.008(6) 0.020(5) 0.019(6) O7 0.089(7) 0.055(6) 0.071(7) 0.013(6) 0.016(6) -0.023(6) O8 0.070(6) 0.084(7) 0.048(6) 0.011(6) 0.018(5) 0.016(6) O9 0.062(6) 0.075(7) 0.085(8) -0.024(6) 0.023(6) 0.003(5) O10 0.046(5) 0.041(5) 0.061(6) -0.008(5) 0.004(5) -0.022(4) O11 0.046(5) 0.069(6) 0.051(6) 0.011(5) 0.009(4) 0.017(5) C1 0.056(9) 0.054(9) 0.046(9) -0.008(8) 0.028(8) -0.004(8) C2 0.047(10) 0.38(3) 0.089(14) 0.105(19) 0.029(9) 0.057(16) C3 0.086(12) 0.19(2) 0.092(14) -0.052(15) 0.050(11) -0.051(14) C4 0.161(18) 0.100(15) 0.141(18) 0.009(13) 0.110(15) -0.022(13) C5 0.036(7) 0.077(10) 0.024(8) 0.015(8) 0.009(6) -0.008(7) C6 0.063(10) 0.117(13) 0.044(9) -0.002(9) -0.008(8) -0.001(9) C7 0.094(12) 0.129(15) 0.052(11) 0.007(11) 0.019(9) -0.019(12) C8 0.085(11) 0.080(12) 0.061(11) -0.025(9) 0.007(9) 0.023(10) C9 0.051(9) 0.070(11) 0.056(11) 0.001(9) -0.002(8) -0.007(8) C10 0.042(8) 0.125(14) 0.096(13) -0.036(12) 0.019(9) -0.022(10) C11 0.054(9) 0.120(15) 0.086(13) -0.008(12) -0.013(9) -0.009(10) C12 0.084(12) 0.062(11) 0.153(18) -0.013(11) -0.017(12) -0.033(10) C13 0.046(8) 0.027(7) 0.044(9) 0.007(7) 0.009(7) 0.006(6) C14 0.048(8) 0.044(8) 0.054(10) 0.007(7) 0.004(7) 0.003(7) C15 0.060(9) 0.049(9) 0.051(10) 0.005(7) 0.004(8) 0.015(7) C16 0.072(10) 0.033(8) 0.058(11) -0.016(7) 0.013(8) 0.001(7) C17 0.061(9) 0.033(8) 0.064(11) -0.008(7) 0.012(8) 0.000(7) C18 0.087(11) 0.022(7) 0.099(13) -0.009(8) 0.019(10) -0.001(8) C19 0.067(10) 0.051(9) 0.078(11) -0.010(8) 0.027(9) 0.021(8) C20 0.084(11) 0.061(10) 0.072(12) 0.015(9) 0.027(9) 0.019(9) C21 0.068(11) 0.101(14) 0.075(13) -0.013(11) 0.033(10) 0.022(10) C22 0.15(2) 0.21(3) 0.25(3) -0.03(2) 0.13(2) 0.01(2) C23 0.25(3) 0.092(16) 0.31(3) 0.071(19) 0.22(3) 0.106(18) C24 0.137(19) 0.50(5) 0.096(18) -0.14(3) -0.014(15) 0.15(3) C25 0.098(14) 0.077(13) 0.094(15) 0.022(12) 0.042(12) -0.008(11) C26 0.30(4) 0.085(17) 0.34(4) 0.10(2) 0.19(3) 0.02(2) C27 0.40(4) 0.101(18) 0.28(4) 0.00(2) 0.28(4) -0.04(2) C28 0.31(4) 0.32(4) 0.21(3) 0.13(3) -0.10(3) -0.28(3) C29 0.055(10) 0.096(12) 0.049(11) -0.006(10) 0.024(9) 0.001(9) C30 0.092(14) 0.22(2) 0.106(17) 0.087(16) 0.020(12) 0.016(15) C31 0.109(14) 0.151(18) 0.068(13) 0.037(12) 0.018(11) 0.049(13) C32 0.25(3) 0.15(2) 0.079(15) -0.027(15) -0.032(16) 0.00(2) C33 0.104(14) 0.083(14) 0.070(14) -0.042(11) 0.013(11) -0.004(11) C34 0.42(4) 0.096(17) 0.13(2) -0.048(16) 0.02(2) 0.10(2) C35 0.45(5) 0.13(2) 0.11(2) -0.039(17) 0.12(3) -0.03(3) C36 0.091(17) 0.47(5) 0.55(6) -0.48(5) 0.08(3) -0.09(3) C37 0.052(9) 0.058(9) 0.044(10) -0.001(8) 0.014(7) -0.011(8) C38 0.064(11) 0.049(10) 0.172(19) -0.015(11) -0.005(12) -0.023(9) C39 0.081(11) 0.058(10) 0.098(13) 0.023(10) -0.006(10) -0.029(9) C40 0.111(13) 0.084(12) 0.089(14) -0.037(11) 0.030(11) -0.050(11) C41 0.063(10) 0.063(10) 0.068(12) 0.016(9) 0.014(9) 0.006(9) C42 0.078(12) 0.079(13) 0.130(17) 0.026(12) -0.008(11) 0.026(10) C43 0.070(11) 0.124(15) 0.131(16) 0.041(13) 0.032(11) 0.024(11) C44 0.114(14) 0.167(19) 0.077(14) -0.034(13) -0.019(11) 0.068(14) _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 Y1 O10 2.061(7) . ? Y1 O1 2.271(7) . ? Y1 O2 2.278(7) . ? Y1 O4 2.323(7) . ? Y1 O5 2.381(7) . ? Y1 O11 2.542(8) . ? Y1 Y2 3.463(3) . ? Y1 Y3 3.464(3) . ? Y2 O8 2.163(9) . ? Y2 O9 2.175(9) . ? Y2 O3 2.299(8) . ? Y2 O1 2.330(7) . ? Y2 O5 2.434(8) . ? Y2 O4 2.450(7) . ? Y2 Y3 3.529(3) . ? Y3 O7 2.164(9) . ? Y3 O6 2.190(9) . ? Y3 O3 2.294(8) . ? Y3 O2 2.316(7) . ? Y3 O5 2.413(7) . ? Y3 O4 2.448(7) . ? O1 C1 1.444(13) . ? O2 C5 1.436(13) . ? O3 C9 1.448(14) . ? O4 C13 1.442(12) . ? O5 C17 1.419(13) . ? O6 C21 1.424(15) . ? O7 C25 1.388(16) . ? O8 C29 1.419(16) . ? O9 C33 1.424(16) . ? O10 C37 1.387(13) . ? O11 C41 1.460(14) . ? C1 C2 1.443(17) . ? C1 C3 1.464(17) . ? C1 C4 1.533(18) . ? C5 C8 1.513(17) . ? C5 C7 1.515(16) . ? C5 C6 1.524(15) . ? C9 C11 1.491(17) . ? C9 C12 1.512(17) . ? C9 C10 1.534(17) . ? C13 C16 1.511(15) . ? C13 C14 1.529(15) . ? C13 C15 1.533(15) . ? C17 C20 1.519(16) . ? C17 C18 1.525(15) . ? C17 C19 1.539(16) . ? C21 C23 1.46(2) . ? C21 C24 1.47(2) . ? C21 C22 1.49(2) . ? C25 C27 1.41(2) . ? C25 C26 1.46(2) . ? C25 C28 1.49(2) . ? C29 C30 1.488(19) . ? C29 C31 1.500(18) . ? C29 C32 1.50(2) . ? C33 C36 1.40(2) . ? C33 C35 1.43(2) . ? C33 C34 1.45(2) . ? C37 C38 1.512(16) . ? C37 C39 1.515(16) . ? C37 C40 1.534(17) . ? C41 C44 1.492(18) . ? C41 C43 1.497(18) . ? C41 C42 1.519(19) . ? 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 O10 Y1 O1 105.7(3) . . ? O10 Y1 O2 105.3(3) . . ? O1 Y1 O2 144.3(3) . . ? O10 Y1 O4 110.4(3) . . ? O1 Y1 O4 76.9(2) . . ? O2 Y1 O4 76.1(2) . . ? O10 Y1 O5 178.8(3) . . ? O1 Y1 O5 74.7(3) . . ? O2 Y1 O5 74.0(3) . . ? O4 Y1 O5 68.4(2) . . ? O10 Y1 O11 73.8(3) . . ? O1 Y1 O11 100.7(3) . . ? O2 Y1 O11 104.5(3) . . ? O4 Y1 O11 175.5(3) . . ? O5 Y1 O11 107.3(3) . . ? O10 Y1 Y2 135.0(2) . . ? O1 Y1 Y2 41.83(18) . . ? O2 Y1 Y2 102.68(19) . . ? O4 Y1 Y2 44.96(17) . . ? O5 Y1 Y2 44.62(18) . . ? O11 Y1 Y2 130.9(2) . . ? O10 Y1 Y3 134.8(2) . . ? O1 Y1 Y3 103.03(19) . . ? O2 Y1 Y3 41.46(18) . . ? O4 Y1 Y3 44.88(17) . . ? O5 Y1 Y3 44.09(17) . . ? O11 Y1 Y3 133.13(19) . . ? Y2 Y1 Y3 61.25(6) . . ? O8 Y2 O9 85.9(3) . . ? O8 Y2 O3 107.5(3) . . ? O9 Y2 O3 102.4(3) . . ? O8 Y2 O1 101.6(3) . . ? O9 Y2 O1 107.1(3) . . ? O3 Y2 O1 139.6(3) . . ? O8 Y2 O5 168.9(3) . . ? O9 Y2 O5 104.7(3) . . ? O3 Y2 O5 73.7(3) . . ? O1 Y2 O5 72.6(2) . . ? O8 Y2 O4 103.9(3) . . ? O9 Y2 O4 170.0(3) . . ? O3 Y2 O4 73.0(2) . . ? O1 Y2 O4 73.3(2) . . ? O5 Y2 O4 65.6(2) . . ? O8 Y2 Y1 126.4(3) . . ? O9 Y2 Y1 132.6(2) . . ? O3 Y2 Y1 99.1(2) . . ? O1 Y2 Y1 40.55(18) . . ? O5 Y2 Y1 43.41(17) . . ? O4 Y2 Y1 42.06(15) . . ? O8 Y2 Y3 131.8(2) . . ? O9 Y2 Y3 127.3(3) . . ? O3 Y2 Y3 39.74(19) . . ? O1 Y2 Y3 99.90(19) . . ? O5 Y2 Y3 43.05(17) . . ? O4 Y2 Y3 43.90(16) . . ? Y1 Y2 Y3 59.40(6) . . ? O7 Y3 O6 84.4(4) . . ? O7 Y3 O3 103.7(3) . . ? O6 Y3 O3 109.2(3) . . ? O7 Y3 O2 106.1(3) . . ? O6 Y3 O2 100.1(3) . . ? O3 Y3 O2 139.8(3) . . ? O7 Y3 O5 104.4(3) . . ? O6 Y3 O5 169.8(3) . . ? O3 Y3 O5 74.2(3) . . ? O2 Y3 O5 72.8(3) . . ? O7 Y3 O4 170.3(3) . . ? O6 Y3 O4 105.4(3) . . ? O3 Y3 O4 73.1(2) . . ? O2 Y3 O4 73.0(2) . . ? O5 Y3 O4 65.9(2) . . ? O7 Y3 Y1 131.7(3) . . ? O6 Y3 Y1 126.6(3) . . ? O3 Y3 Y1 99.2(2) . . ? O2 Y3 Y1 40.65(18) . . ? O5 Y3 Y1 43.36(17) . . ? O4 Y3 Y1 42.03(16) . . ? O7 Y3 Y2 128.3(3) . . ? O6 Y3 Y2 133.8(2) . . ? O3 Y3 Y2 39.85(19) . . ? O2 Y3 Y2 99.98(19) . . ? O5 Y3 Y2 43.51(18) . . ? O4 Y3 Y2 43.94(16) . . ? Y1 Y3 Y2 59.35(6) . . ? C1 O1 Y1 132.0(7) . . ? C1 O1 Y2 130.2(7) . . ? Y1 O1 Y2 97.6(3) . . ? C5 O2 Y1 131.3(6) . . ? C5 O2 Y3 130.8(6) . . ? Y1 O2 Y3 97.9(3) . . ? C9 O3 Y3 130.8(8) . . ? C9 O3 Y2 128.7(8) . . ? Y3 O3 Y2 100.4(3) . . ? C13 O4 Y1 124.2(6) . . ? C13 O4 Y3 123.0(6) . . ? Y1 O4 Y3 93.1(2) . . ? C13 O4 Y2 122.6(6) . . ? Y1 O4 Y2 93.0(2) . . ? Y3 O4 Y2 92.2(2) . . ? C17 O5 Y1 122.8(7) . . ? C17 O5 Y3 123.9(7) . . ? Y1 O5 Y3 92.5(2) . . ? C17 O5 Y2 123.4(7) . . ? Y1 O5 Y2 92.0(2) . . ? Y3 O5 Y2 93.4(2) . . ? C21 O6 Y3 178.8(9) . . ? C25 O7 Y3 178.0(11) . . ? C29 O8 Y2 179.1(9) . . ? C33 O9 Y2 178.4(10) . . ? C37 O10 Y1 176.4(8) . . ? C41 O11 Y1 169.9(8) . . ? C2 C1 O1 111.3(11) . . ? C2 C1 C3 113.0(14) . . ? O1 C1 C3 109.1(11) . . ? C2 C1 C4 107.6(15) . . ? O1 C1 C4 108.8(10) . . ? C3 C1 C4 106.9(14) . . ? O2 C5 C8 109.3(10) . . ? O2 C5 C7 109.4(10) . . ? C8 C5 C7 109.8(11) . . ? O2 C5 C6 108.9(10) . . ? C8 C5 C6 109.3(11) . . ? C7 C5 C6 110.1(11) . . ? O3 C9 C11 110.4(11) . . ? O3 C9 C12 107.5(11) . . ? C11 C9 C12 111.7(13) . . ? O3 C9 C10 108.2(11) . . ? C11 C9 C10 109.6(12) . . ? C12 C9 C10 109.3(13) . . ? O4 C13 C16 109.8(9) . . ? O4 C13 C14 109.0(9) . . ? C16 C13 C14 110.6(10) . . ? O4 C13 C15 108.5(9) . . ? C16 C13 C15 110.3(10) . . ? C14 C13 C15 108.7(10) . . ? O5 C17 C20 109.5(10) . . ? O5 C17 C18 109.4(10) . . ? C20 C17 C18 109.7(11) . . ? O5 C17 C19 108.7(10) . . ? C20 C17 C19 110.0(11) . . ? C18 C17 C19 109.5(11) . . ? O6 C21 C23 110.6(14) . . ? O6 C21 C24 112.4(14) . . ? C23 C21 C24 111.9(19) . . ? O6 C21 C22 108.9(15) . . ? C23 C21 C22 106.2(17) . . ? C24 C21 C22 106.5(18) . . ? O7 C25 C27 113.7(17) . . ? O7 C25 C26 111.7(15) . . ? C27 C25 C26 107(2) . . ? O7 C25 C28 110.7(16) . . ? C27 C25 C28 111(2) . . ? C26 C25 C28 102(2) . . ? O8 C29 C30 112.4(12) . . ? O8 C29 C31 110.6(12) . . ? C30 C29 C31 107.5(15) . . ? O8 C29 C32 108.4(14) . . ? C30 C29 C32 109.2(15) . . ? C31 C29 C32 108.5(14) . . ? C36 C33 O9 109.2(15) . . ? C36 C33 C35 109(2) . . ? O9 C33 C35 109.8(16) . . ? C36 C33 C34 110(2) . . ? O9 C33 C34 111.7(15) . . ? C35 C33 C34 107.0(19) . . ? O10 C37 C38 110.8(11) . . ? O10 C37 C39 112.0(10) . . ? C38 C37 C39 107.5(12) . . ? O10 C37 C40 111.4(10) . . ? C38 C37 C40 108.3(12) . . ? C39 C37 C40 106.6(12) . . ? O11 C41 C44 109.9(12) . . ? O11 C41 C43 107.4(11) . . ? C44 C41 C43 111.8(14) . . ? O11 C41 C42 109.2(12) . . ? C44 C41 C42 111.7(14) . . ? C43 C41 C42 106.8(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.483 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.115