# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email Peter.Junk@monash.edu _publ_contact_author_name 'Peter Junk' loop_ _publ_author_name 'Shima Hamidi' 'Glen Deacon' 'Peter Junk' 'Paul Neumann' # Attachment '- 3.EuIII.cif' data_ortro _database_code_depnum_ccdc_archive 'CCDC 845097' #TrackingRef '- 3.EuIII.cif' _audit_creation_method 'CrysAlisPro, Oxford Diffraction Ltd.,' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H91 Eu O8' _chemical_formula_sum 'C56 H91 Eu O8' _chemical_formula_weight 1044.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 25.0773(4) _cell_length_b 22.1250(3) _cell_length_c 19.9043(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11043.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 22711 _cell_measurement_theta_min 1.9157 _cell_measurement_theta_max 32.3141 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4432 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7560 _exptl_absorpt_correction_T_max 0.7560 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59568 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12690 _reflns_number_gt 9806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.,' _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^)+(0.0437P)^2^+42.2764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12690 _refine_ls_number_parameters 566 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1308 _refine_ls_wR_factor_gt 0.1138 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.198621(8) 0.401345(8) 0.261690(10) 0.02117(7) Uani 1 1 d . . . O2 O 0.20108(12) 0.30396(13) 0.25602(16) 0.0299(7) Uani 1 1 d . . . O3 O 0.27492(12) 0.42681(14) 0.22048(15) 0.0285(6) Uani 1 1 d . . . O6 O 0.11780(12) 0.39574(14) 0.33512(16) 0.0330(7) Uani 1 1 d . . . O1 O 0.14328(12) 0.42438(13) 0.18253(15) 0.0290(6) Uani 1 1 d . . . C13 C 0.19830(17) 0.24672(19) 0.2340(2) 0.0291(9) Uani 1 1 d . . . C18 C 0.15997(18) 0.20732(19) 0.2617(3) 0.0331(9) Uani 1 1 d . . . O4 O 0.19285(12) 0.50709(13) 0.30749(16) 0.0302(7) Uani 1 1 d . . . C2 C 0.11248(17) 0.3845(2) 0.0780(2) 0.0299(9) Uani 1 1 d . . . C17 C 0.1560(2) 0.1486(2) 0.2353(3) 0.0411(11) Uani 1 1 d . . . H17 H 0.1300 0.1217 0.2529 0.049 Uiso 1 1 calc R . . C48 C 0.1134(2) 0.3805(3) 0.4060(3) 0.0443(12) Uani 1 1 d . . . H48A H 0.1255 0.4148 0.4343 0.053 Uiso 1 1 calc R . . H48B H 0.1355 0.3447 0.4167 0.053 Uiso 1 1 calc R . . O5 O 0.23712(15) 0.38298(17) 0.37471(17) 0.0449(9) Uani 1 1 d . . . C3 C 0.08669(17) 0.3948(2) 0.0172(2) 0.0346(10) Uani 1 1 d . . . H3 H 0.0827 0.3624 -0.0136 0.041 Uiso 1 1 calc R . . C14 C 0.23321(18) 0.22647(19) 0.1836(2) 0.0323(10) Uani 1 1 d . . . C6 C 0.09826(17) 0.49100(19) 0.1068(2) 0.0298(9) Uani 1 1 d . . . C4 C 0.06675(18) 0.4508(2) 0.0006(2) 0.0392(12) Uani 1 1 d . . . H4 H 0.0490 0.4569 -0.0410 0.047 Uiso 1 1 calc R . . C11 C 0.10362(19) 0.5429(2) 0.1558(3) 0.0377(11) Uani 1 1 d . . . H11 H 0.1297 0.5305 0.1912 0.045 Uiso 1 1 calc R . . C5 C 0.07288(17) 0.4981(2) 0.0451(2) 0.0360(11) Uani 1 1 d . . . H5 H 0.0593 0.5367 0.0333 0.043 Uiso 1 1 calc R . . C1 C 0.11872(16) 0.43318(19) 0.1236(2) 0.0263(9) Uani 1 1 d . . . C8 C 0.1314(2) 0.3224(2) 0.0980(2) 0.0366(11) Uani 1 1 d . . . H8 H 0.1624 0.3277 0.1290 0.044 Uiso 1 1 calc R . . C38 C 0.1609(2) 0.6029(2) 0.3416(3) 0.0474(13) Uani 1 1 d . . . H38A H 0.1534 0.6249 0.3838 0.057 Uiso 1 1 calc R . . H38B H 0.1375 0.6188 0.3056 0.057 Uiso 1 1 calc R . . C40 C 0.2274(2) 0.5538(2) 0.2792(3) 0.0390(11) Uani 1 1 d . . . H40A H 0.2174 0.5625 0.2321 0.047 Uiso 1 1 calc R . . H40B H 0.2652 0.5408 0.2804 0.047 Uiso 1 1 calc R . . C39 C 0.2192(2) 0.6083(2) 0.3222(3) 0.0435(12) Uani 1 1 d . . . H39A H 0.2261 0.6460 0.2968 0.052 Uiso 1 1 calc R . . H39B H 0.2426 0.6073 0.3623 0.052 Uiso 1 1 calc R . . C16 C 0.1890(2) 0.1292(2) 0.1844(3) 0.0417(12) Uani 1 1 d . . . H16 H 0.1852 0.0896 0.1665 0.050 Uiso 1 1 calc R . . C45 C 0.06474(18) 0.4004(2) 0.3076(3) 0.0432(12) Uani 1 1 d . . . H45A H 0.0557 0.3638 0.2814 0.052 Uiso 1 1 calc R . . H45B H 0.0618 0.4362 0.2779 0.052 Uiso 1 1 calc R . . C12 C 0.1248(3) 0.6006(2) 0.1229(3) 0.0543(15) Uani 1 1 d . . . H12A H 0.0977 0.6171 0.0926 0.081 Uiso 1 1 calc R . . H12B H 0.1571 0.5911 0.0972 0.081 Uiso 1 1 calc R . . H12C H 0.1333 0.6304 0.1577 0.081 Uiso 1 1 calc R . . C15 C 0.2276(2) 0.1677(2) 0.1593(3) 0.0391(11) Uani 1 1 d . . . H15 H 0.2507 0.1539 0.1248 0.047 Uiso 1 1 calc R . . C23 C 0.1240(2) 0.2267(2) 0.3189(3) 0.0413(12) Uani 1 1 d . . . H23 H 0.1274 0.2715 0.3234 0.050 Uiso 1 1 calc R . . C37 C 0.1531(2) 0.5357(2) 0.3505(3) 0.0433(12) Uani 1 1 d . . . H37A H 0.1586 0.5240 0.3980 0.052 Uiso 1 1 calc R . . H37B H 0.1167 0.5236 0.3368 0.052 Uiso 1 1 calc R . . C47 C 0.0549(2) 0.3673(3) 0.4183(3) 0.0507(14) Uani 1 1 d . . . H47A H 0.0466 0.3241 0.4105 0.061 Uiso 1 1 calc R . . H47B H 0.0441 0.3785 0.4645 0.061 Uiso 1 1 calc R . . C7 C 0.1501(2) 0.2834(3) 0.0394(3) 0.0563(16) Uani 1 1 d . . . H7A H 0.1197 0.2741 0.0102 0.084 Uiso 1 1 calc R . . H7B H 0.1653 0.2457 0.0567 0.084 Uiso 1 1 calc R . . H7C H 0.1772 0.3053 0.0137 0.084 Uiso 1 1 calc R . . C46 C 0.0286(2) 0.4067(3) 0.3674(4) 0.0595(17) Uani 1 1 d . . . H46A H 0.0268 0.4491 0.3829 0.071 Uiso 1 1 calc R . . H46B H -0.0079 0.3922 0.3570 0.071 Uiso 1 1 calc R . . C35 C 0.2616(2) 0.4314(2) 0.0799(2) 0.0395(11) Uani 1 1 d . . . H35 H 0.2371 0.4045 0.1059 0.047 Uiso 1 1 calc R . . C20 C 0.2773(2) 0.2682(2) 0.1588(3) 0.0382(11) Uani 1 1 d . . . H20 H 0.2619 0.3098 0.1565 0.046 Uiso 1 1 calc R . . C21 C 0.3223(2) 0.2701(2) 0.2106(3) 0.0438(12) Uani 1 1 d . . . H21A H 0.3371 0.2295 0.2164 0.066 Uiso 1 1 calc R . . H21B H 0.3082 0.2846 0.2537 0.066 Uiso 1 1 calc R . . H21C H 0.3504 0.2976 0.1951 0.066 Uiso 1 1 calc R . . C25 C 0.31945(19) 0.4281(2) 0.1836(3) 0.0357(11) Uani 1 1 d . . . C9 C 0.0877(2) 0.2891(2) 0.1370(3) 0.0494(13) Uani 1 1 d . . . H9A H 0.0778 0.3128 0.1767 0.074 Uiso 1 1 calc R . . H9B H 0.1010 0.2494 0.1512 0.074 Uiso 1 1 calc R . . H9C H 0.0564 0.2838 0.1082 0.074 Uiso 1 1 calc R . . C30 C 0.3694(2) 0.4279(3) 0.2148(3) 0.0500(14) Uani 1 1 d . . . C32 C 0.3743(2) 0.4285(2) 0.2905(3) 0.0474(13) Uani 1 1 d . . . H32 H 0.3397 0.4134 0.3090 0.057 Uiso 1 1 calc R . . C34 C 0.2399(2) 0.4959(2) 0.0848(3) 0.0415(11) Uani 1 1 d . . . H34A H 0.2370 0.5075 0.1322 0.062 Uiso 1 1 calc R . . H34B H 0.2047 0.4978 0.0637 0.062 Uiso 1 1 calc R . . H34C H 0.2642 0.5237 0.0617 0.062 Uiso 1 1 calc R . . C26 C 0.3157(2) 0.4281(3) 0.1125(3) 0.0473(13) Uani 1 1 d . . . C41 C 0.2602(3) 0.4279(3) 0.4191(3) 0.071(2) Uani 1 1 d . . . H41A H 0.2333 0.4433 0.4513 0.085 Uiso 1 1 calc R . . H41B H 0.2749 0.4623 0.3932 0.085 Uiso 1 1 calc R . . C22 C 0.0649(2) 0.2129(3) 0.3056(4) 0.0574(16) Uani 1 1 d . . . H22A H 0.0532 0.2344 0.2652 0.086 Uiso 1 1 calc R . . H22B H 0.0436 0.2263 0.3441 0.086 Uiso 1 1 calc R . . H22C H 0.0602 0.1693 0.2992 0.086 Uiso 1 1 calc R . . C10 C 0.0509(2) 0.5556(3) 0.1902(3) 0.0542(15) Uani 1 1 d . . . H10A H 0.0247 0.5689 0.1568 0.081 Uiso 1 1 calc R . . H10B H 0.0558 0.5875 0.2239 0.081 Uiso 1 1 calc R . . H10C H 0.0381 0.5188 0.2122 0.081 Uiso 1 1 calc R . . C24 C 0.1420(3) 0.1989(3) 0.3852(3) 0.0641(17) Uani 1 1 d . . . H24A H 0.1361 0.1551 0.3840 0.096 Uiso 1 1 calc R . . H24B H 0.1214 0.2165 0.4222 0.096 Uiso 1 1 calc R . . H24C H 0.1800 0.2071 0.3921 0.096 Uiso 1 1 calc R . . C19 C 0.2985(2) 0.2533(2) 0.0888(3) 0.0477(13) Uani 1 1 d . . . H19A H 0.3156 0.2135 0.0894 0.072 Uiso 1 1 calc R . . H19B H 0.3246 0.2840 0.0753 0.072 Uiso 1 1 calc R . . H19C H 0.2689 0.2530 0.0566 0.072 Uiso 1 1 calc R . . C42 C 0.3050(3) 0.3931(5) 0.4559(4) 0.097(4) Uani 1 1 d . . . H42A H 0.3398 0.4134 0.4495 0.117 Uiso 1 1 calc R . . H42B H 0.2974 0.3905 0.5046 0.117 Uiso 1 1 calc R . . C33 C 0.4181(3) 0.3865(3) 0.3167(4) 0.071(2) Uani 1 1 d . . . H33A H 0.4531 0.4029 0.3047 0.107 Uiso 1 1 calc R . . H33B H 0.4139 0.3463 0.2966 0.107 Uiso 1 1 calc R . . H33C H 0.4154 0.3832 0.3657 0.107 Uiso 1 1 calc R . . C43 C 0.3057(3) 0.3309(4) 0.4248(4) 0.084(3) Uani 1 1 d . . . H43A H 0.3323 0.3286 0.3882 0.101 Uiso 1 1 calc R . . H43B H 0.3142 0.2998 0.4589 0.101 Uiso 1 1 calc R . . C27 C 0.3622(3) 0.4268(4) 0.0752(4) 0.076(2) Uani 1 1 d . . . H27 H 0.3599 0.4265 0.0276 0.091 Uiso 1 1 calc R . . C44 C 0.2521(3) 0.3227(3) 0.3990(4) 0.078(2) Uani 1 1 d . . . H44A H 0.2276 0.3089 0.4348 0.093 Uiso 1 1 calc R . . H44B H 0.2517 0.2929 0.3619 0.093 Uiso 1 1 calc R . . C36 C 0.2601(3) 0.4105(3) 0.0059(3) 0.0587(17) Uani 1 1 d . . . H36A H 0.2827 0.4371 -0.0213 0.088 Uiso 1 1 calc R . . H36B H 0.2234 0.4122 -0.0107 0.088 Uiso 1 1 calc R . . H36C H 0.2734 0.3689 0.0028 0.088 Uiso 1 1 calc R . . C29 C 0.4151(2) 0.4271(4) 0.1737(4) 0.082(2) Uani 1 1 d . . . H29 H 0.4493 0.4274 0.1941 0.098 Uiso 1 1 calc R . . C31 C 0.3819(3) 0.4926(3) 0.3171(5) 0.087(3) Uani 1 1 d . . . H31A H 0.4151 0.5094 0.2991 0.130 Uiso 1 1 calc R . . H31B H 0.3837 0.4917 0.3663 0.130 Uiso 1 1 calc R . . H31C H 0.3518 0.5178 0.3030 0.130 Uiso 1 1 calc R . . C28 C 0.4113(3) 0.4260(5) 0.1050(5) 0.100(3) Uani 1 1 d . . . H28 H 0.4427 0.4246 0.0782 0.120 Uiso 1 1 calc R . . O7' O 0.0510(6) 0.2625(7) -0.0909(7) 0.120(6) Uiso 0.555(19) 1 d P A 1 C73 C -0.0231(4) 0.2491(5) -0.1589(5) 0.102(3) Uiso 1 1 d D A . H73A H -0.0503 0.2738 -0.1821 0.122 Uiso 1 1 calc R . . H73B H -0.0187 0.2105 -0.1835 0.122 Uiso 1 1 calc R . . C74 C 0.0282(4) 0.2820(5) -0.1556(6) 0.120(4) Uiso 1 1 d D . . H74A H 0.0225 0.3263 -0.1563 0.144 Uiso 1 1 calc R A 1 H74B H 0.0518 0.2706 -0.1934 0.144 Uiso 1 1 calc R A 1 C72 C -0.0389(5) 0.2377(6) -0.0892(5) 0.132(4) Uiso 1 1 d D . . H72A H -0.0587 0.1992 -0.0850 0.158 Uiso 1 1 calc R A 1 H72B H -0.0612 0.2710 -0.0714 0.158 Uiso 1 1 calc R A 1 C71' C 0.0142(8) 0.2347(10) -0.0541(10) 0.103(6) Uiso 0.555(19) 1 d P A 1 H71A H 0.0115 0.2543 -0.0095 0.123 Uiso 0.555(19) 1 calc PR A 1 H71B H 0.0245 0.1919 -0.0473 0.123 Uiso 0.555(19) 1 calc PR A 1 C76 C 0.0467(5) 0.0957(5) 0.1319(6) 0.128(4) Uiso 1 1 d D . . H76A H 0.0703 0.0631 0.1483 0.154 Uiso 1 1 calc R B 1 H76B H 0.0436 0.1264 0.1679 0.154 Uiso 1 1 calc R B 1 O7 O 0.0209(9) 0.3109(10) -0.0924(8) 0.152(10) Uiso 0.445(19) 1 d PD A 2 C71 C -0.0025(15) 0.2691(17) -0.0458(11) 0.177(16) Uiso 0.445(19) 1 d PD A 2 H71C H -0.0214 0.2903 -0.0091 0.212 Uiso 0.445(19) 1 calc PR A 2 H71D H 0.0245 0.2415 -0.0265 0.212 Uiso 0.445(19) 1 calc PR A 2 C77 C 0.0705(9) 0.1235(15) 0.0726(9) 0.144(9) Uiso 0.65(4) 1 d PD C 1 H77A H 0.0656 0.1678 0.0746 0.173 Uiso 0.65(4) 1 calc PR C 1 H77B H 0.1092 0.1150 0.0718 0.173 Uiso 0.65(4) 1 calc PR C 1 C78 C 0.0460(7) 0.1000(19) 0.0124(10) 0.155(10) Uiso 0.65(4) 1 d PD C 1 H78A H 0.0664 0.0662 -0.0075 0.186 Uiso 0.65(4) 1 calc PR C 1 H78B H 0.0395 0.1317 -0.0217 0.186 Uiso 0.65(4) 1 calc PR C 1 O8 O -0.0035(6) 0.0798(8) 0.0457(7) 0.281(8) Uiso 1 1 d D . . C75 C -0.0052(5) 0.0712(7) 0.1180(7) 0.170(6) Uiso 1 1 d D C . H75A H -0.0341 0.0946 0.1395 0.204 Uiso 1 1 calc R . . H75B H -0.0081 0.0280 0.1307 0.204 Uiso 1 1 calc R . . C102 C 0.0778(9) 0.088(2) 0.0710(9) 0.099(12) Uiso 0.35(4) 1 d PD C 2 H10D H 0.1076 0.0603 0.0800 0.119 Uiso 0.35(4) 1 calc PR C 2 H10E H 0.0932 0.1279 0.0583 0.119 Uiso 0.35(4) 1 calc PR C 2 C103 C 0.0464(7) 0.0651(18) 0.0147(12) 0.092(11) Uiso 0.35(4) 1 d PD C 2 H10F H 0.0526 0.0875 -0.0277 0.110 Uiso 0.35(4) 1 calc PR C 2 H10G H 0.0512 0.0212 0.0074 0.110 Uiso 0.35(4) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.02612(11) 0.01847(10) 0.01892(11) 0.00084(7) -0.00062(8) 0.00208(7) O2 0.0359(16) 0.0198(14) 0.0342(17) 0.0004(12) 0.0001(13) 0.0036(12) O3 0.0284(15) 0.0306(15) 0.0265(16) 0.0016(13) -0.0012(12) 0.0022(12) O6 0.0305(16) 0.0387(18) 0.0298(17) 0.0025(14) 0.0067(13) 0.0033(13) O1 0.0336(16) 0.0272(15) 0.0262(16) -0.0012(12) -0.0074(12) 0.0044(12) C13 0.036(2) 0.024(2) 0.027(2) 0.0025(17) -0.0078(19) 0.0065(17) C18 0.034(2) 0.0214(19) 0.044(3) 0.0049(19) -0.005(2) 0.0057(17) O4 0.0352(16) 0.0246(15) 0.0307(17) -0.0047(12) 0.0050(13) -0.0020(12) C2 0.029(2) 0.037(2) 0.023(2) -0.0017(18) -0.0012(17) 0.0028(18) C17 0.038(2) 0.027(2) 0.058(3) 0.004(2) -0.006(2) 0.0018(19) C48 0.047(3) 0.046(3) 0.040(3) 0.000(2) 0.015(2) 0.001(2) O5 0.058(2) 0.049(2) 0.0275(18) -0.0026(16) -0.0107(16) 0.0202(18) C3 0.029(2) 0.054(3) 0.020(2) -0.003(2) -0.0010(17) 0.003(2) C14 0.036(2) 0.025(2) 0.036(3) 0.0023(19) -0.0053(19) 0.0056(17) C6 0.026(2) 0.030(2) 0.034(2) 0.0089(18) -0.0010(17) -0.0015(17) C4 0.031(2) 0.062(3) 0.024(2) 0.012(2) -0.0029(18) 0.004(2) C11 0.038(2) 0.025(2) 0.050(3) 0.003(2) -0.007(2) 0.0030(18) C5 0.028(2) 0.041(3) 0.039(3) 0.018(2) -0.0017(19) 0.0035(19) C1 0.027(2) 0.029(2) 0.023(2) 0.0033(17) -0.0032(16) 0.0013(16) C8 0.042(3) 0.034(2) 0.033(3) -0.009(2) -0.008(2) 0.009(2) C38 0.058(3) 0.030(2) 0.055(4) -0.008(2) 0.014(3) 0.005(2) C40 0.041(3) 0.028(2) 0.048(3) -0.004(2) 0.006(2) -0.0044(19) C39 0.067(3) 0.028(2) 0.036(3) -0.002(2) 0.008(2) -0.006(2) C16 0.044(3) 0.024(2) 0.056(3) -0.006(2) -0.014(2) 0.0026(19) C45 0.028(2) 0.048(3) 0.054(3) 0.004(2) 0.007(2) 0.000(2) C12 0.063(4) 0.025(2) 0.075(4) 0.003(3) 0.004(3) -0.006(2) C15 0.043(3) 0.030(2) 0.045(3) -0.005(2) -0.005(2) 0.013(2) C23 0.041(3) 0.028(2) 0.054(3) 0.004(2) 0.008(2) 0.000(2) C37 0.047(3) 0.032(2) 0.051(3) -0.008(2) 0.016(2) 0.003(2) C47 0.060(3) 0.046(3) 0.046(3) -0.007(3) 0.021(3) -0.011(3) C7 0.060(4) 0.057(4) 0.052(4) -0.024(3) -0.011(3) 0.020(3) C46 0.042(3) 0.058(4) 0.079(5) -0.010(3) 0.026(3) -0.002(3) C35 0.048(3) 0.046(3) 0.024(2) 0.005(2) 0.009(2) 0.007(2) C20 0.043(3) 0.025(2) 0.046(3) 0.003(2) 0.003(2) 0.0058(19) C21 0.039(3) 0.034(3) 0.058(3) -0.001(2) -0.001(2) 0.005(2) C25 0.033(2) 0.029(2) 0.045(3) 0.011(2) 0.008(2) 0.0048(18) C9 0.056(3) 0.040(3) 0.052(3) 0.005(2) -0.007(3) 0.006(2) C30 0.031(2) 0.052(3) 0.067(4) 0.025(3) 0.004(2) 0.002(2) C32 0.036(3) 0.041(3) 0.065(4) 0.009(3) -0.011(2) -0.001(2) C34 0.052(3) 0.039(3) 0.034(3) 0.005(2) 0.000(2) 0.005(2) C26 0.044(3) 0.050(3) 0.048(3) 0.014(3) 0.015(2) 0.008(2) C41 0.081(5) 0.091(5) 0.040(3) -0.030(3) -0.036(3) 0.038(4) C22 0.040(3) 0.051(3) 0.081(5) 0.003(3) 0.013(3) -0.001(2) C10 0.057(3) 0.046(3) 0.059(4) -0.010(3) 0.010(3) 0.003(3) C24 0.075(4) 0.064(4) 0.053(4) 0.011(3) 0.015(3) 0.008(3) C19 0.056(3) 0.040(3) 0.048(3) 0.004(2) 0.012(3) 0.015(2) C42 0.070(5) 0.184(10) 0.038(4) -0.033(5) -0.027(3) 0.060(6) C33 0.049(4) 0.085(5) 0.080(5) 0.024(4) -0.025(3) 0.017(3) C43 0.071(5) 0.092(6) 0.089(6) 0.042(5) -0.009(4) 0.023(4) C27 0.065(4) 0.105(6) 0.057(4) 0.038(4) 0.028(3) 0.020(4) C44 0.116(6) 0.065(4) 0.052(4) 0.017(3) -0.014(4) 0.036(4) C36 0.091(5) 0.051(3) 0.034(3) 0.003(3) 0.007(3) 0.016(3) C29 0.027(3) 0.121(7) 0.096(6) 0.042(5) 0.005(3) 0.004(3) C31 0.087(5) 0.055(4) 0.118(7) 0.015(4) -0.043(5) -0.012(4) C28 0.051(4) 0.152(8) 0.096(7) 0.054(6) 0.041(4) 0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O3 2.157(3) . ? Eu1 O2 2.158(3) . ? Eu1 O1 2.161(3) . ? Eu1 O5 2.481(3) . ? Eu1 O6 2.502(3) . ? Eu1 O4 2.515(3) . ? O2 C13 1.342(5) . ? O3 C25 1.337(5) . ? O6 C45 1.443(6) . ? O6 C48 1.455(6) . ? O1 C1 1.339(5) . ? C13 C14 1.405(6) . ? C13 C18 1.410(6) . ? C18 C17 1.406(6) . ? C18 C23 1.515(7) . ? O4 C37 1.457(5) . ? O4 C40 1.462(5) . ? C2 C3 1.390(6) . ? C2 C1 1.417(6) . ? C2 C8 1.508(6) . ? C17 C16 1.376(8) . ? C48 C47 1.517(7) . ? O5 C41 1.450(7) . ? O5 C44 1.468(7) . ? C3 C4 1.377(7) . ? C14 C15 1.393(6) . ? C14 C20 1.523(6) . ? C6 C5 1.392(6) . ? C6 C1 1.418(6) . ? C6 C11 1.513(7) . ? C4 C5 1.378(7) . ? C11 C10 1.516(7) . ? C11 C12 1.529(7) . ? C8 C7 1.525(7) . ? C8 C9 1.532(8) . ? C38 C37 1.510(7) . ? C38 C39 1.518(8) . ? C40 C39 1.492(7) . ? C16 C15 1.382(7) . ? C45 C46 1.503(8) . ? C23 C22 1.535(7) . ? C23 C24 1.525(8) . ? C47 C46 1.490(9) . ? C35 C26 1.504(8) . ? C35 C34 1.531(7) . ? C35 C36 1.544(7) . ? C20 C19 1.527(7) . ? C20 C21 1.530(7) . ? C25 C30 1.398(7) . ? C25 C26 1.417(8) . ? C30 C29 1.407(8) . ? C30 C32 1.512(9) . ? C32 C33 1.532(7) . ? C32 C31 1.525(9) . ? C26 C27 1.382(8) . ? C41 C42 1.548(9) . ? C42 C43 1.508(12) . ? C43 C44 1.451(11) . ? C27 C28 1.368(11) . ? C29 C28 1.372(12) . ? O7' C71' 1.33(2) . ? O7' C74 1.472(16) . ? C73 C72 1.464(8) . ? C73 C74 1.480(8) . ? C74 O7 1.421(9) . ? C72 C71 1.437(10) . ? C72 C71' 1.51(2) . ? C76 C75 1.438(7) . ? C76 C102 1.450(10) . ? C76 C77 1.458(9) . ? O7 C71 1.435(10) . ? C77 C78 1.443(10) . ? C78 O8 1.476(10) . ? O8 C103 1.433(10) . ? O8 C75 1.452(7) . ? C102 C103 1.463(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Eu1 O2 102.45(11) . . ? O3 Eu1 O1 103.35(11) . . ? O2 Eu1 O1 102.46(11) . . ? O3 Eu1 O5 92.43(12) . . ? O2 Eu1 O5 82.69(12) . . ? O1 Eu1 O5 161.73(12) . . ? O3 Eu1 O6 162.52(11) . . ? O2 Eu1 O6 90.24(11) . . ? O1 Eu1 O6 85.26(11) . . ? O5 Eu1 O6 77.14(12) . . ? O3 Eu1 O4 86.89(10) . . ? O2 Eu1 O4 161.65(11) . . ? O1 Eu1 O4 90.46(11) . . ? O5 Eu1 O4 81.15(11) . . ? O6 Eu1 O4 77.75(10) . . ? C13 O2 Eu1 163.3(3) . . ? C25 O3 Eu1 162.8(3) . . ? C45 O6 C48 108.4(4) . . ? C45 O6 Eu1 121.4(3) . . ? C48 O6 Eu1 129.7(3) . . ? C1 O1 Eu1 165.6(3) . . ? O2 C13 C14 120.1(4) . . ? O2 C13 C18 119.4(4) . . ? C14 C13 C18 120.5(4) . . ? C17 C18 C13 118.3(5) . . ? C17 C18 C23 120.0(4) . . ? C13 C18 C23 121.7(4) . . ? C37 O4 C40 108.9(3) . . ? C37 O4 Eu1 131.0(3) . . ? C40 O4 Eu1 119.0(2) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 C8 121.7(4) . . ? C1 C2 C8 119.3(4) . . ? C16 C17 C18 121.4(5) . . ? O6 C48 C47 105.9(4) . . ? C41 O5 C44 108.7(5) . . ? C41 O5 Eu1 126.5(4) . . ? C44 O5 Eu1 123.2(4) . . ? C4 C3 C2 121.7(5) . . ? C15 C14 C13 118.8(4) . . ? C15 C14 C20 121.8(4) . . ? C13 C14 C20 119.4(4) . . ? C5 C6 C1 118.3(4) . . ? C5 C6 C11 121.6(4) . . ? C1 C6 C11 120.1(4) . . ? C5 C4 C3 119.2(4) . . ? C10 C11 C6 110.8(4) . . ? C10 C11 C12 110.0(4) . . ? C6 C11 C12 112.9(4) . . ? C4 C5 C6 122.2(4) . . ? O1 C1 C6 120.2(4) . . ? O1 C1 C2 120.1(4) . . ? C6 C1 C2 119.7(4) . . ? C2 C8 C7 114.2(4) . . ? C2 C8 C9 110.3(4) . . ? C7 C8 C9 109.6(5) . . ? C37 C38 C39 103.4(4) . . ? O4 C40 C39 105.6(4) . . ? C40 C39 C38 102.4(4) . . ? C17 C16 C15 119.7(5) . . ? O6 C45 C46 105.2(5) . . ? C14 C15 C16 121.4(5) . . ? C18 C23 C22 112.9(5) . . ? C18 C23 C24 111.1(4) . . ? C22 C23 C24 110.8(5) . . ? O4 C37 C38 105.7(4) . . ? C46 C47 C48 101.9(4) . . ? C47 C46 C45 102.6(5) . . ? C26 C35 C34 109.8(5) . . ? C26 C35 C36 114.8(5) . . ? C34 C35 C36 109.3(4) . . ? C19 C20 C14 114.7(4) . . ? C19 C20 C21 111.4(4) . . ? C14 C20 C21 109.5(4) . . ? O3 C25 C30 120.3(5) . . ? O3 C25 C26 119.5(4) . . ? C30 C25 C26 120.2(5) . . ? C25 C30 C29 118.1(6) . . ? C25 C30 C32 121.0(5) . . ? C29 C30 C32 120.9(5) . . ? C30 C32 C33 113.0(5) . . ? C30 C32 C31 111.4(5) . . ? C33 C32 C31 110.9(5) . . ? C27 C26 C25 118.6(6) . . ? C27 C26 C35 121.9(6) . . ? C25 C26 C35 119.4(4) . . ? O5 C41 C42 103.7(6) . . ? C43 C42 C41 105.6(6) . . ? C44 C43 C42 104.4(6) . . ? C28 C27 C26 121.9(7) . . ? C43 C44 O5 103.9(6) . . ? C28 C29 C30 121.6(6) . . ? C29 C28 C27 119.5(6) . . ? C71' O7' C74 110.4(13) . . ? C72 C73 C74 106.2(9) . . ? O7 C74 C73 98.5(12) . . ? O7 C74 O7' 53.8(10) . . ? C73 C74 O7' 103.4(10) . . ? C71 C72 C73 108.2(13) . . ? C71 C72 C71' 34.9(18) . . ? C73 C72 C71' 101.9(11) . . ? O7' C71' C72 109.7(15) . . ? C75 C76 C102 106.4(14) . . ? C75 C76 C77 112.0(13) . . ? C102 C76 C77 31.9(15) . . ? C74 O7 C71 109.6(18) . . ? O7 C71 C72 100.6(16) . . ? C78 C77 C76 110.3(15) . . ? C77 C78 O8 95.4(15) . . ? C103 O8 C75 115.0(18) . . ? C103 O8 C78 30.8(15) . . ? C75 O8 C78 120.6(15) . . ? C76 C75 O8 96.6(12) . . ? C76 C102 C103 113.0(17) . . ? O8 C103 C102 93.4(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.780 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.104 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_theta 29.97 _reflns_odcompleteness_iscentric 1 _chemical_oxdiff_formula 'C20 H20 Eu1 O3' data_ortr2.cif _database_code_depnum_ccdc_archive 'CCDC 845098' #TrackingRef '- 10.Ladme.cif' _audit_creation_method 'CrysAlisPro, Oxford Diffraction Ltd.,' _chemical_name_systematic ; ? ; _chemical_name_common LaDME _chemical_melting_point ? _chemical_formula_moiety LaDME _chemical_formula_sum 'C44 H71 La O7' _chemical_formula_weight 850.92 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.1036(2) _cell_length_b 13.4935(3) _cell_length_c 25.6718(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4539.12(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 12670 _cell_measurement_theta_min 2.1621 _cell_measurement_theta_max 32.3176 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94464 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3389 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44155 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.1621 _diffrn_reflns_theta_max 32.3176 _reflns_number_total 10427 _reflns_number_gt 9653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd.,' _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^)+(0.0259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_coef none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.009(9) _refine_ls_number_reflns 10427 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.003 _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 La1 La 0.959409(10) 0.489807(10) 0.111256(5) 0.01351(4) Uani 1 1 d . . . C10 C 0.5285(2) 0.4655(3) 0.15809(13) 0.0430(9) Uani 1 1 d . . . H10A H 0.4610 0.4814 0.1439 0.065 Uiso 1 1 calc R . . H10B H 0.5235 0.4574 0.1959 0.065 Uiso 1 1 calc R . . H10C H 0.5533 0.4038 0.1424 0.065 Uiso 1 1 calc R . . O2 O 0.97691(12) 0.49990(15) 0.19995(6) 0.0195(4) Uani 1 1 d . . . O3 O 1.03496(14) 0.44789(12) 0.03321(6) 0.0176(4) Uani 1 1 d . . . O1 O 0.79639(13) 0.52913(14) 0.09069(6) 0.0187(4) Uani 1 1 d . . . C18 C 0.90549(17) 0.4990(2) 0.28494(9) 0.0182(5) Uani 1 1 d . . . C30 C 1.09602(18) 0.4801(2) -0.05304(10) 0.0185(6) Uani 1 1 d . . . C14 C 1.09017(18) 0.4930(3) 0.27327(9) 0.0172(5) Uani 1 1 d . . . C25 C 1.0416(2) 0.42152(18) -0.01693(9) 0.0161(5) Uani 1 1 d . . . O5 O 0.85901(16) 0.32658(15) 0.13515(8) 0.0288(5) Uani 1 1 d . . . O4 O 1.06694(16) 0.33042(16) 0.13725(8) 0.0283(5) Uani 1 1 d . . . C17 C 0.92094(18) 0.4976(2) 0.33845(9) 0.0205(5) Uani 1 1 d . . . H17 H 0.8634 0.5000 0.3609 0.025 Uiso 1 1 calc R . . C16 C 1.01792(18) 0.4927(2) 0.36002(9) 0.0212(6) Uani 1 1 d . . . H16 H 1.0271 0.4909 0.3967 0.025 Uiso 1 1 calc R . . C15 C 1.10093(18) 0.4906(2) 0.32676(9) 0.0197(5) Uani 1 1 d . . . H15 H 1.1676 0.4873 0.3412 0.024 Uiso 1 1 calc R . . C23 C 0.79778(18) 0.4983(3) 0.26255(9) 0.0238(6) Uani 1 1 d . . . H23 H 0.8027 0.5160 0.2248 0.029 Uiso 1 1 calc R . . C13 C 0.99064(18) 0.4977(2) 0.25130(9) 0.0174(5) Uani 1 1 d . . . O6 O 0.95407(17) 0.68320(14) 0.13115(7) 0.0276(5) Uani 1 1 d . . . C4 C 0.5408(2) 0.6047(2) 0.00385(11) 0.0265(6) Uani 1 1 d . . . H4 H 0.4825 0.6222 -0.0161 0.032 Uiso 1 1 calc R . . C29 C 1.0966(2) 0.4534(2) -0.10555(11) 0.0254(6) Uani 1 1 d . . . H29 H 1.1323 0.4938 -0.1298 0.030 Uiso 1 1 calc R . . C19 C 1.2546(2) 0.5777(3) 0.24795(13) 0.0310(8) Uani 1 1 d . . . H19A H 1.2750 0.5788 0.2847 0.047 Uiso 1 1 calc R . . H19B H 1.2185 0.6392 0.2394 0.047 Uiso 1 1 calc R . . H19C H 1.3155 0.5719 0.2260 0.047 Uiso 1 1 calc R . . C20 C 1.18432(18) 0.4892(2) 0.23818(9) 0.0198(5) Uani 1 1 d . . . H20 H 1.1603 0.4933 0.2013 0.024 Uiso 1 1 calc R . . C7 C 0.8253(2) 0.5476(3) -0.07430(11) 0.0334(8) Uani 1 1 d . . . H7A H 0.7869 0.4866 -0.0810 0.050 Uiso 1 1 calc R . . H7B H 0.8956 0.5396 -0.0867 0.050 Uiso 1 1 calc R . . H7C H 0.7929 0.6029 -0.0927 0.050 Uiso 1 1 calc R . . C3 C 0.6349(2) 0.5953(2) -0.01945(11) 0.0214(6) Uani 1 1 d . . . H3 H 0.6408 0.6054 -0.0559 0.026 Uiso 1 1 calc R . . C2 C 0.7214(2) 0.5713(2) 0.00903(10) 0.0186(6) Uani 1 1 d . . . C37 C 1.1331(3) 0.2730(3) 0.10495(13) 0.0389(9) Uani 1 1 d . . . H37A H 1.1949 0.2557 0.1245 0.058 Uiso 1 1 calc R . . H37B H 1.1519 0.3116 0.0741 0.058 Uiso 1 1 calc R . . H37C H 1.0980 0.2122 0.0942 0.058 Uiso 1 1 calc R . . C39 C 0.9122(3) 0.2396(2) 0.15267(14) 0.0374(9) Uani 1 1 d . . . H39A H 0.9235 0.1937 0.1231 0.045 Uiso 1 1 calc R . . H39B H 0.8714 0.2047 0.1795 0.045 Uiso 1 1 calc R . . C42 C 1.1327(3) 0.6943(3) 0.12650(14) 0.0395(9) Uani 1 1 d . . . H42A H 1.1301 0.7303 0.0929 0.047 Uiso 1 1 calc R . . H42B H 1.1955 0.7144 0.1451 0.047 Uiso 1 1 calc R . . C43 C 1.0414(3) 0.7189(2) 0.15838(13) 0.0365(8) Uani 1 1 d . . . H43A H 1.0463 0.6870 0.1930 0.044 Uiso 1 1 calc R . . H43B H 1.0364 0.7915 0.1634 0.044 Uiso 1 1 calc R . . C11 C 0.6022(2) 0.5492(3) 0.14568(11) 0.0293(7) Uani 1 1 d . . . H11 H 0.6700 0.5316 0.1610 0.035 Uiso 1 1 calc R . . C26 C 0.9923(2) 0.3346(2) -0.03518(11) 0.0212(6) Uani 1 1 d . . . C28 C 1.0469(2) 0.3702(2) -0.12323(11) 0.0311(7) Uani 1 1 d . . . H28 H 1.0482 0.3532 -0.1591 0.037 Uiso 1 1 calc R . . C35 C 1.1555(2) 0.5707(2) -0.03563(11) 0.0225(6) Uani 1 1 d . . . H35 H 1.1297 0.5906 -0.0005 0.027 Uiso 1 1 calc R . . C5 C 0.5328(2) 0.5884(2) 0.05672(11) 0.0259(6) Uani 1 1 d . . . H5 H 0.4679 0.5945 0.0728 0.031 Uiso 1 1 calc R . . C27 C 0.9951(2) 0.3118(2) -0.08786(11) 0.0284(7) Uani 1 1 d . . . H27 H 0.9605 0.2543 -0.0999 0.034 Uiso 1 1 calc R . . C44 C 0.8615(3) 0.7165(3) 0.15568(14) 0.0393(9) Uani 1 1 d . . . H44A H 0.8591 0.6919 0.1916 0.059 Uiso 1 1 calc R . . H44B H 0.8026 0.6913 0.1363 0.059 Uiso 1 1 calc R . . H44C H 0.8599 0.7891 0.1559 0.059 Uiso 1 1 calc R . . C1 C 0.7125(2) 0.5536(2) 0.06317(10) 0.0185(6) Uani 1 1 d . . . C38 C 1.0118(3) 0.2717(2) 0.17498(12) 0.0329(9) Uani 1 1 d . . . H38A H 1.0000 0.3113 0.2069 0.039 Uiso 1 1 calc R . . H38B H 1.0528 0.2128 0.1846 0.039 Uiso 1 1 calc R . . C6 C 0.6167(2) 0.5634(2) 0.08725(11) 0.0215(6) Uani 1 1 d . . . C32 C 0.9350(2) 0.2672(2) 0.00148(12) 0.0309(8) Uani 1 1 d . . . H32 H 0.9475 0.2913 0.0378 0.037 Uiso 1 1 calc R . . C36 C 1.1458(3) 0.6594(2) -0.07169(12) 0.0349(8) Uani 1 1 d . . . H36A H 1.1812 0.6455 -0.1045 0.052 Uiso 1 1 calc R . . H36B H 1.1765 0.7177 -0.0551 0.052 Uiso 1 1 calc R . . H36C H 1.0735 0.6724 -0.0787 0.052 Uiso 1 1 calc R . . O7 O 1.13358(14) 0.59005(15) 0.11743(8) 0.0272(5) Uani 1 1 d . . . C40 C 0.7535(2) 0.3048(3) 0.12420(14) 0.0406(9) Uani 1 1 d . . . H40A H 0.7493 0.2464 0.1016 0.061 Uiso 1 1 calc R . . H40B H 0.7220 0.3616 0.1066 0.061 Uiso 1 1 calc R . . H40C H 0.7173 0.2916 0.1569 0.061 Uiso 1 1 calc R . . C21 C 1.2426(3) 0.3925(3) 0.24418(14) 0.0351(9) Uani 1 1 d . . . H21A H 1.2988 0.3906 0.2190 0.053 Uiso 1 1 calc R . . H21B H 1.1964 0.3367 0.2378 0.053 Uiso 1 1 calc R . . H21C H 1.2701 0.3879 0.2796 0.053 Uiso 1 1 calc R . . C41 C 1.2309(2) 0.5553(3) 0.10119(13) 0.0427(9) Uani 1 1 d . . . H41A H 1.2562 0.5970 0.0727 0.064 Uiso 1 1 calc R . . H41B H 1.2250 0.4867 0.0891 0.064 Uiso 1 1 calc R . . H41C H 1.2787 0.5584 0.1305 0.064 Uiso 1 1 calc R . . C8 C 0.8262(2) 0.5690(2) -0.01540(11) 0.0220(7) Uani 1 1 d . . . H8 H 0.8658 0.5149 0.0019 0.026 Uiso 1 1 calc R . . C9 C 0.8817(2) 0.6667(3) -0.00470(12) 0.0343(8) Uani 1 1 d . . . H9A H 0.8496 0.7200 -0.0248 0.051 Uiso 1 1 calc R . . H9B H 0.9534 0.6604 -0.0149 0.051 Uiso 1 1 calc R . . H9C H 0.8776 0.6822 0.0325 0.051 Uiso 1 1 calc R . . C22 C 0.7276(2) 0.5737(3) 0.28856(13) 0.0357(8) Uani 1 1 d . . . H22A H 0.7208 0.5577 0.3256 0.054 Uiso 1 1 calc R . . H22B H 0.6603 0.5715 0.2720 0.054 Uiso 1 1 calc R . . H22C H 0.7566 0.6402 0.2848 0.054 Uiso 1 1 calc R . . C31 C 0.9731(3) 0.1601(2) -0.00174(14) 0.0520(10) Uani 1 1 d . . . H31A H 0.9518 0.1310 -0.0350 0.078 Uiso 1 1 calc R . . H31B H 0.9440 0.1216 0.0270 0.078 Uiso 1 1 calc R . . H31C H 1.0477 0.1592 0.0007 0.078 Uiso 1 1 calc R . . C34 C 1.2687(2) 0.5431(3) -0.03014(12) 0.0327(8) Uani 1 1 d . . . H34A H 1.2756 0.4871 -0.0061 0.049 Uiso 1 1 calc R . . H34B H 1.3067 0.6001 -0.0165 0.049 Uiso 1 1 calc R . . H34C H 1.2961 0.5246 -0.0643 0.049 Uiso 1 1 calc R . . C33 C 0.8204(3) 0.2728(3) -0.00868(14) 0.0523(11) Uani 1 1 d . . . H33A H 0.7963 0.3404 -0.0021 0.079 Uiso 1 1 calc R . . H33B H 0.7848 0.2267 0.0146 0.079 Uiso 1 1 calc R . . H33C H 0.8065 0.2549 -0.0450 0.079 Uiso 1 1 calc R . . C24 C 0.7529(3) 0.3945(3) 0.26614(14) 0.0374(9) Uani 1 1 d . . . H24A H 0.7999 0.3470 0.2500 0.056 Uiso 1 1 calc R . . H24B H 0.6873 0.3927 0.2479 0.056 Uiso 1 1 calc R . . H24C H 0.7426 0.3770 0.3028 0.056 Uiso 1 1 calc R . . C12 C 0.5661(3) 0.6460(3) 0.17127(13) 0.0436(10) Uani 1 1 d . . . H12A H 0.5012 0.6666 0.1556 0.065 Uiso 1 1 calc R . . H12B H 0.6174 0.6978 0.1658 0.065 Uiso 1 1 calc R . . H12C H 0.5566 0.6353 0.2087 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01263(6) 0.01486(6) 0.01302(6) 0.00143(6) 0.00053(6) 0.00057(7) C10 0.0266(17) 0.061(2) 0.0413(19) 0.0188(17) 0.0095(15) -0.0006(18) O2 0.0210(9) 0.0229(10) 0.0145(8) 0.0009(8) -0.0005(6) 0.0011(10) O3 0.0188(9) 0.0194(9) 0.0146(8) -0.0008(7) 0.0022(8) -0.0006(9) O1 0.0155(9) 0.0213(11) 0.0193(9) 0.0009(8) -0.0027(7) 0.0023(8) C18 0.0199(12) 0.0135(14) 0.0212(12) 0.0022(12) 0.0012(9) -0.0011(13) C30 0.0151(12) 0.0216(16) 0.0187(12) -0.0023(12) 0.0008(10) 0.0054(13) C14 0.0205(12) 0.0131(14) 0.0181(12) -0.0005(13) 0.0010(9) -0.0002(14) C25 0.0138(12) 0.0185(12) 0.0162(12) -0.0006(9) -0.0014(12) 0.0063(13) O5 0.0261(12) 0.0158(11) 0.0446(13) 0.0062(10) 0.0065(10) -0.0022(9) O4 0.0325(13) 0.0277(12) 0.0247(11) 0.0046(9) 0.0077(9) 0.0127(10) C17 0.0250(12) 0.0193(14) 0.0171(12) 0.0011(13) 0.0051(10) -0.0008(13) C16 0.0287(14) 0.0207(14) 0.0143(12) 0.0013(12) 0.0000(9) -0.0044(14) C15 0.0215(13) 0.0179(14) 0.0196(12) -0.0005(12) -0.0019(10) -0.0031(13) C23 0.0196(12) 0.0334(18) 0.0184(12) 0.0031(15) 0.0011(10) 0.0012(16) C13 0.0247(12) 0.0135(13) 0.0140(11) 0.0002(12) -0.0019(9) 0.0012(12) O6 0.0325(12) 0.0183(10) 0.0320(11) -0.0018(8) -0.0087(11) 0.0013(11) C4 0.0169(14) 0.0286(15) 0.0339(16) -0.0012(12) -0.0114(14) 0.0035(15) C29 0.0229(14) 0.0333(16) 0.0200(15) 0.0014(13) 0.0043(12) 0.0049(12) C19 0.0246(18) 0.041(2) 0.0278(19) 0.0032(15) 0.0018(14) -0.0052(15) C20 0.0188(12) 0.0236(15) 0.0171(12) -0.0001(12) 0.0009(9) 0.0021(13) C7 0.0245(16) 0.054(2) 0.0217(16) -0.0033(15) -0.0039(12) 0.0100(15) C3 0.0223(15) 0.0220(16) 0.0199(15) -0.0016(12) -0.0051(12) 0.0042(13) C2 0.0165(14) 0.0174(15) 0.0220(15) -0.0001(11) -0.0013(11) 0.0013(12) C37 0.041(2) 0.046(2) 0.0305(19) 0.0039(17) 0.0064(16) 0.0234(16) C39 0.053(2) 0.0166(16) 0.042(2) 0.0085(15) 0.0168(17) 0.0020(15) C42 0.044(2) 0.0306(19) 0.044(2) 0.0084(15) -0.0133(18) -0.0182(17) C43 0.050(2) 0.0216(15) 0.0381(19) -0.0034(13) -0.016(2) -0.006(2) C11 0.0199(16) 0.042(2) 0.0261(16) 0.0077(14) 0.0011(12) 0.0003(14) C26 0.0224(14) 0.0187(14) 0.0224(15) -0.0013(11) -0.0003(11) 0.0008(11) C28 0.0344(17) 0.0396(17) 0.0192(15) -0.0088(12) 0.0017(14) 0.0058(17) C35 0.0219(15) 0.0283(17) 0.0173(15) -0.0001(12) 0.0042(11) -0.0027(13) C5 0.0139(14) 0.0305(16) 0.0333(16) -0.0002(12) 0.0026(13) -0.0007(14) C27 0.0323(17) 0.0262(16) 0.0265(16) -0.0093(13) -0.0023(13) -0.0003(13) C44 0.046(2) 0.0240(18) 0.048(2) -0.0123(16) -0.0014(18) 0.0101(17) C1 0.0172(14) 0.0152(13) 0.0232(15) -0.0012(11) -0.0043(11) -0.0003(11) C38 0.046(2) 0.0284(17) 0.0239(17) 0.0101(13) 0.0089(14) 0.0159(15) C6 0.0183(14) 0.0210(16) 0.0252(15) -0.0006(12) 0.0004(12) 0.0005(12) C32 0.041(2) 0.0242(16) 0.0272(16) -0.0046(13) -0.0027(14) -0.0113(14) C36 0.043(2) 0.0280(18) 0.0336(18) 0.0044(14) 0.0127(15) -0.0098(16) O7 0.0214(10) 0.0330(12) 0.0272(11) 0.0054(10) -0.0015(9) -0.0085(9) C40 0.039(2) 0.034(2) 0.049(2) 0.0002(16) 0.0081(16) -0.0186(16) C21 0.034(2) 0.038(2) 0.034(2) 0.0024(16) 0.0115(16) 0.0131(16) C41 0.0177(15) 0.076(3) 0.035(2) 0.0008(17) 0.0056(14) -0.0024(16) C8 0.0175(14) 0.0306(18) 0.0179(15) -0.0031(12) -0.0034(11) 0.0053(13) C9 0.0240(16) 0.048(2) 0.0304(18) -0.0017(15) 0.0050(14) -0.0090(16) C22 0.0257(17) 0.049(2) 0.0320(19) 0.0006(16) -0.0023(14) 0.0125(16) C31 0.088(3) 0.0220(16) 0.046(2) -0.0002(15) 0.003(2) -0.014(2) C34 0.0201(15) 0.048(2) 0.0302(17) -0.0102(15) 0.0049(13) -0.0035(15) C33 0.039(2) 0.078(3) 0.039(2) 0.010(2) -0.0007(17) -0.028(2) C24 0.0263(19) 0.042(2) 0.044(2) 0.0016(17) -0.0047(15) -0.0067(16) C12 0.047(2) 0.060(2) 0.0241(17) 0.0011(16) 0.0029(15) 0.0154(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.2635(17) . ? La1 O2 2.2924(15) . ? La1 O3 2.3052(16) . ? La1 O5 2.638(2) . ? La1 O7 2.6577(18) . ? La1 O4 2.656(2) . ? La1 O6 2.6600(18) . ? C10 C11 1.520(4) . ? O2 C13 1.331(3) . ? O3 C25 1.338(3) . ? O1 C1 1.348(3) . ? C18 C17 1.389(3) . ? C18 C13 1.411(3) . ? C18 C23 1.524(3) . ? C30 C29 1.396(4) . ? C30 C25 1.412(4) . ? C30 C35 1.516(4) . ? C14 C15 1.381(3) . ? C14 C13 1.422(3) . ? C14 C20 1.528(3) . ? C25 C26 1.419(4) . ? O5 C39 1.437(4) . ? O5 C40 1.441(4) . ? O4 C37 1.429(4) . ? O4 C38 1.444(4) . ? C17 C16 1.388(3) . ? C16 C15 1.383(3) . ? C23 C24 1.522(5) . ? C23 C22 1.525(4) . ? O6 C43 1.425(4) . ? O6 C44 1.439(4) . ? C4 C3 1.376(4) . ? C4 C5 1.379(4) . ? C29 C28 1.375(4) . ? C19 C20 1.529(4) . ? C20 C21 1.520(4) . ? C7 C8 1.539(4) . ? C3 C2 1.387(4) . ? C2 C1 1.415(4) . ? C2 C8 1.510(4) . ? C39 C38 1.491(5) . ? C42 O7 1.426(4) . ? C42 C43 1.487(5) . ? C11 C6 1.524(4) . ? C11 C12 1.537(5) . ? C26 C27 1.388(4) . ? C26 C32 1.508(4) . ? C28 C27 1.381(4) . ? C35 C36 1.519(4) . ? C35 C34 1.536(4) . ? C5 C6 1.391(4) . ? C1 C6 1.405(4) . ? C32 C33 1.527(4) . ? C32 C31 1.531(5) . ? O7 C41 1.422(3) . ? C8 C9 1.530(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 La1 O2 108.19(6) . . ? O1 La1 O3 105.07(6) . . ? O2 La1 O3 146.60(6) . . ? O1 La1 O5 77.25(7) . . ? O2 La1 O5 82.45(7) . . ? O3 La1 O5 102.21(6) . . ? O1 La1 O7 134.83(7) . . ? O2 La1 O7 79.90(6) . . ? O3 La1 O7 78.93(6) . . ? O5 La1 O7 147.07(6) . . ? O1 La1 O4 138.51(7) . . ? O2 La1 O4 75.26(6) . . ? O3 La1 O4 77.99(6) . . ? O5 La1 O4 61.97(6) . . ? O7 La1 O4 86.65(6) . . ? O1 La1 O6 77.88(7) . . ? O2 La1 O6 75.74(6) . . ? O3 La1 O6 114.76(6) . . ? O5 La1 O6 139.58(7) . . ? O7 La1 O6 60.78(7) . . ? O4 La1 O6 139.46(7) . . ? C13 O2 La1 174.88(18) . . ? C25 O3 La1 158.30(17) . . ? C1 O1 La1 161.72(16) . . ? C17 C18 C13 119.3(2) . . ? C17 C18 C23 120.5(2) . . ? C13 C18 C23 120.1(2) . . ? C29 C30 C25 119.5(3) . . ? C29 C30 C35 119.4(3) . . ? C25 C30 C35 121.1(2) . . ? C15 C14 C13 119.3(2) . . ? C15 C14 C20 120.2(2) . . ? C13 C14 C20 120.5(2) . . ? O3 C25 C26 120.5(2) . . ? O3 C25 C30 121.0(2) . . ? C26 C25 C30 118.5(2) . . ? C39 O5 C40 111.1(2) . . ? C39 O5 La1 120.87(18) . . ? C40 O5 La1 127.12(19) . . ? C37 O4 C38 113.3(2) . . ? C37 O4 La1 127.99(18) . . ? C38 O4 La1 110.32(16) . . ? C16 C17 C18 121.9(2) . . ? C15 C16 C17 118.4(2) . . ? C14 C15 C16 122.2(2) . . ? C18 C23 C24 109.9(3) . . ? C18 C23 C22 112.9(3) . . ? C24 C23 C22 110.7(3) . . ? O2 C13 C18 119.9(2) . . ? O2 C13 C14 121.2(2) . . ? C18 C13 C14 118.9(2) . . ? C43 O6 C44 110.9(2) . . ? C43 O6 La1 113.88(17) . . ? C44 O6 La1 114.39(18) . . ? C3 C4 C5 118.8(3) . . ? C28 C29 C30 121.8(3) . . ? C21 C20 C19 110.6(2) . . ? C21 C20 C14 112.0(3) . . ? C19 C20 C14 111.3(2) . . ? C4 C3 C2 121.6(3) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 C8 121.9(2) . . ? C1 C2 C8 118.7(2) . . ? O5 C39 C38 107.9(3) . . ? O7 C42 C43 108.4(3) . . ? O6 C43 C42 107.5(3) . . ? C10 C11 C6 112.3(3) . . ? C10 C11 C12 110.2(3) . . ? C6 C11 C12 110.6(3) . . ? C27 C26 C25 119.5(3) . . ? C27 C26 C32 119.2(3) . . ? C25 C26 C32 121.3(2) . . ? C27 C28 C29 118.8(3) . . ? C30 C35 C36 114.4(2) . . ? C30 C35 C34 109.2(2) . . ? C36 C35 C34 109.1(3) . . ? C4 C5 C6 122.2(3) . . ? C28 C27 C26 121.8(3) . . ? O1 C1 C6 121.4(2) . . ? O1 C1 C2 119.2(2) . . ? C6 C1 C2 119.4(2) . . ? O4 C38 C39 109.9(3) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C11 119.1(3) . . ? C1 C6 C11 122.1(3) . . ? C26 C32 C33 110.7(3) . . ? C26 C32 C31 111.9(3) . . ? C33 C32 C31 110.9(3) . . ? C41 O7 C42 112.4(3) . . ? C41 O7 La1 125.82(19) . . ? C42 O7 La1 120.33(19) . . ? C2 C8 C7 113.9(2) . . ? C2 C8 C9 109.8(2) . . ? C7 C8 C9 110.0(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.541 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.064 # Attachment '- 2.NdTHF3SQ.CIF' data_ndthf3.cif _database_code_depnum_ccdc_archive 'CCDC 845099' #TrackingRef '- 2.NdTHF3SQ.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common SQ _chemical_melting_point ? _chemical_formula_moiety 'C56 H91 Nd O8' _chemical_formula_sum 'C56 H91 Nd O8' _chemical_formula_weight 1036.53 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 25.234(2) _cell_length_b 22.3796(15) _cell_length_c 20.0280(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11310.4(15) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 171113 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4408 _exptl_absorpt_coefficient_mu 0.966 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8766 _exptl_absorpt_correction_T_max 0.9624 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 171113 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12783 _reflns_number_gt 8737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12783 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.014 1287 544 2 0.500 0.500 -0.037 1287 543 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.199513(9) 0.401421(10) 0.263202(12) 0.03183(10) Uani 1 1 d . . . O1 O 0.14431(12) 0.42479(14) 0.18300(16) 0.0405(7) Uani 1 1 d . . . C1 C 0.11871(16) 0.4339(2) 0.1244(2) 0.0371(10) Uani 1 1 d . . . O2 O 0.27640(12) 0.42651(14) 0.22182(15) 0.0383(7) Uani 1 1 d . . . C2 C 0.11155(18) 0.3857(2) 0.0787(3) 0.0445(11) Uani 1 1 d . . . O3 O 0.20232(12) 0.30386(15) 0.25631(18) 0.0464(8) Uani 1 1 d . . . C3 C 0.08660(18) 0.3955(2) 0.0192(3) 0.0447(12) Uani 1 1 d . . . H3 H 0.0825 0.3634 -0.0114 0.054 Uiso 1 1 calc R . . O5 O 0.23801(15) 0.38201(17) 0.37862(18) 0.0595(10) Uani 1 1 d . . . C4 C 0.06713(19) 0.4516(3) 0.0028(3) 0.0552(14) Uani 1 1 d . . . H4 H 0.0495 0.4578 -0.0385 0.066 Uiso 1 1 calc R . . O4 O 0.11733(12) 0.39586(14) 0.33698(18) 0.0469(9) Uani 1 1 d . . . C5 C 0.07360(17) 0.4981(2) 0.0469(3) 0.0482(12) Uani 1 1 d . . . H5 H 0.0604 0.5364 0.0353 0.058 Uiso 1 1 calc R . . O6 O 0.19354(12) 0.50773(14) 0.31135(17) 0.0448(8) Uani 1 1 d . . . C6 C 0.09876(17) 0.49083(19) 0.1077(2) 0.0406(10) Uani 1 1 d . . . C7 C 0.1509(3) 0.2864(3) 0.0392(3) 0.084(2) Uani 1 1 d . . . H7A H 0.1212 0.2791 0.0087 0.126 Uiso 1 1 calc R . . H7B H 0.1646 0.2481 0.0556 0.126 Uiso 1 1 calc R . . H7C H 0.1791 0.3078 0.0156 0.126 Uiso 1 1 calc R . . C8 C 0.1317(2) 0.3241(2) 0.0985(3) 0.0540(14) Uani 1 1 d . . . H8 H 0.1624 0.3298 0.1293 0.065 Uiso 1 1 calc R . . C9 C 0.0880(2) 0.2915(3) 0.1376(4) 0.0725(18) Uani 1 1 d . . . H9A H 0.0799 0.3138 0.1785 0.109 Uiso 1 1 calc R . . H9B H 0.1003 0.2513 0.1494 0.109 Uiso 1 1 calc R . . H9C H 0.0561 0.2886 0.1100 0.109 Uiso 1 1 calc R . . C10 C 0.0521(2) 0.5557(3) 0.1910(3) 0.0735(17) Uani 1 1 d . . . H10A H 0.0576 0.5869 0.2247 0.110 Uiso 1 1 calc R . . H10B H 0.0390 0.5193 0.2128 0.110 Uiso 1 1 calc R . . H10C H 0.0261 0.5694 0.1581 0.110 Uiso 1 1 calc R . . C11 C 0.1045(2) 0.5422(2) 0.1561(3) 0.0509(13) Uani 1 1 d . . . H11 H 0.1304 0.5297 0.1912 0.061 Uiso 1 1 calc R . . C12 C 0.1261(3) 0.5987(2) 0.1235(4) 0.076(2) Uani 1 1 d . . . H12A H 0.1610 0.5904 0.1043 0.115 Uiso 1 1 calc R . . H12B H 0.1293 0.6303 0.1572 0.115 Uiso 1 1 calc R . . H12C H 0.1019 0.6118 0.0881 0.115 Uiso 1 1 calc R . . C14 C 0.3180(2) 0.4287(3) 0.1159(3) 0.0611(15) Uani 1 1 d . . . C15 C 0.3642(3) 0.4264(4) 0.0779(4) 0.097(2) Uani 1 1 d . . . H15 H 0.3618 0.4242 0.0306 0.116 Uiso 1 1 calc R . . C16 C 0.4134(3) 0.4274(5) 0.1081(5) 0.138(4) Uani 1 1 d . . . H16 H 0.4447 0.4276 0.0816 0.166 Uiso 1 1 calc R . . C17 C 0.4170(3) 0.4279(4) 0.1765(5) 0.106(3) Uani 1 1 d . . . H17 H 0.4509 0.4268 0.1971 0.127 Uiso 1 1 calc R . . C19 C 0.2415(2) 0.4938(2) 0.0870(3) 0.0583(14) Uani 1 1 d . . . H19A H 0.2382 0.5049 0.1341 0.087 Uiso 1 1 calc R . . H19B H 0.2065 0.4950 0.0658 0.087 Uiso 1 1 calc R . . H19C H 0.2653 0.5220 0.0644 0.087 Uiso 1 1 calc R . . C20 C 0.2639(2) 0.4318(3) 0.0818(3) 0.0596(14) Uani 1 1 d . . . H20 H 0.2396 0.4048 0.1072 0.072 Uiso 1 1 calc R . . C21 C 0.2626(4) 0.4114(3) 0.0085(3) 0.089(2) Uani 1 1 d . . . H21A H 0.2889 0.4340 -0.0171 0.134 Uiso 1 1 calc R . . H21B H 0.2272 0.4186 -0.0101 0.134 Uiso 1 1 calc R . . H21C H 0.2708 0.3687 0.0061 0.134 Uiso 1 1 calc R . . C22 C 0.3811(3) 0.4943(3) 0.3194(5) 0.113(3) Uani 1 1 d . . . H22A H 0.4155 0.5098 0.3048 0.169 Uiso 1 1 calc R . . H22B H 0.3795 0.4945 0.3683 0.169 Uiso 1 1 calc R . . H22C H 0.3528 0.5196 0.3015 0.169 Uiso 1 1 calc R . . C23 C 0.3742(2) 0.4300(3) 0.2937(4) 0.0744(18) Uani 1 1 d . . . H23 H 0.3396 0.4149 0.3112 0.089 Uiso 1 1 calc R . . C24 C 0.4181(3) 0.3877(4) 0.3204(4) 0.105(3) Uani 1 1 d . . . H24A H 0.4530 0.4048 0.3105 0.157 Uiso 1 1 calc R . . H24B H 0.4149 0.3486 0.2987 0.157 Uiso 1 1 calc R . . H24C H 0.4141 0.3830 0.3688 0.157 Uiso 1 1 calc R . . C25 C 0.19990(18) 0.2470(2) 0.2344(3) 0.0454(12) Uani 1 1 d . . . C26 C 0.1615(2) 0.2081(2) 0.2618(3) 0.0511(13) Uani 1 1 d . . . C27 C 0.1576(2) 0.1502(2) 0.2351(3) 0.0598(15) Uani 1 1 d . . . H27 H 0.1315 0.1236 0.2520 0.072 Uiso 1 1 calc R . . C28 C 0.1906(2) 0.1315(2) 0.1857(3) 0.0574(15) Uani 1 1 d . . . H28 H 0.1871 0.0922 0.1683 0.069 Uiso 1 1 calc R . . C29 C 0.2287(2) 0.1686(2) 0.1607(3) 0.0549(13) Uani 1 1 d . . . H29 H 0.2518 0.1544 0.1268 0.066 Uiso 1 1 calc R . . C30 C 0.23422(18) 0.2271(2) 0.1842(3) 0.0459(12) Uani 1 1 d . . . C31 C 0.0657(2) 0.2133(3) 0.3036(4) 0.091(2) Uani 1 1 d . . . H31A H 0.0537 0.2365 0.2650 0.136 Uiso 1 1 calc R . . H31B H 0.0445 0.2239 0.3428 0.136 Uiso 1 1 calc R . . H31C H 0.0616 0.1705 0.2942 0.136 Uiso 1 1 calc R . . C32 C 0.1251(2) 0.2273(2) 0.3177(3) 0.0607(15) Uani 1 1 d . . . H32 H 0.1285 0.2716 0.3221 0.073 Uiso 1 1 calc R . . C33 C 0.1426(3) 0.1996(3) 0.3847(4) 0.090(2) Uani 1 1 d . . . H33A H 0.1249 0.2204 0.4215 0.134 Uiso 1 1 calc R . . H33B H 0.1811 0.2037 0.3896 0.134 Uiso 1 1 calc R . . H33C H 0.1330 0.1572 0.3855 0.134 Uiso 1 1 calc R . . C34 C 0.3237(2) 0.2688(3) 0.2119(3) 0.0672(16) Uani 1 1 d . . . H34A H 0.3090 0.2752 0.2566 0.101 Uiso 1 1 calc R . . H34B H 0.3483 0.3013 0.2010 0.101 Uiso 1 1 calc R . . H34C H 0.3427 0.2306 0.2108 0.101 Uiso 1 1 calc R . . C35 C 0.2786(2) 0.2676(2) 0.1606(3) 0.0541(13) Uani 1 1 d . . . H35 H 0.2638 0.3090 0.1584 0.065 Uiso 1 1 calc R . . C36 C 0.3003(3) 0.2531(3) 0.0913(3) 0.079(2) Uani 1 1 d . . . H36A H 0.3190 0.2148 0.0926 0.118 Uiso 1 1 calc R . . H36B H 0.3249 0.2846 0.0773 0.118 Uiso 1 1 calc R . . H36C H 0.2710 0.2507 0.0594 0.118 Uiso 1 1 calc R . . C41 C 0.2557(4) 0.3236(3) 0.4006(4) 0.107(3) Uani 1 1 d . . . H41A H 0.2306 0.3068 0.4336 0.129 Uiso 1 1 calc R . . H41B H 0.2581 0.2959 0.3622 0.129 Uiso 1 1 calc R . . C42 C 0.3062(3) 0.3317(5) 0.4299(5) 0.130(4) Uani 1 1 d . . . H42A H 0.3345 0.3280 0.3960 0.156 Uiso 1 1 calc R . . H42B H 0.3123 0.3017 0.4654 0.156 Uiso 1 1 calc R . . C43 C 0.3049(4) 0.3950(5) 0.4592(4) 0.131(5) Uani 1 1 d . . . H43A H 0.2993 0.3938 0.5081 0.157 Uiso 1 1 calc R . . H43B H 0.3385 0.4163 0.4500 0.157 Uiso 1 1 calc R . . C44 C 0.2593(3) 0.4252(4) 0.4249(4) 0.102(3) Uani 1 1 d . . . H44A H 0.2320 0.4372 0.4577 0.122 Uiso 1 1 calc R . . H44B H 0.2715 0.4613 0.4008 0.122 Uiso 1 1 calc R . . C37 C 0.1127(2) 0.3810(3) 0.4062(3) 0.0569(14) Uani 1 1 d . . . H37A H 0.1246 0.4148 0.4344 0.068 Uiso 1 1 calc R . . H37B H 0.1346 0.3456 0.4169 0.068 Uiso 1 1 calc R . . C38 C 0.0541(2) 0.3678(3) 0.4185(3) 0.0723(18) Uani 1 1 d . . . H38A H 0.0462 0.3248 0.4128 0.087 Uiso 1 1 calc R . . H38B H 0.0430 0.3807 0.4637 0.087 Uiso 1 1 calc R . . C39 C 0.0283(3) 0.4043(4) 0.3658(5) 0.109(3) Uani 1 1 d . . . H39A H -0.0067 0.3876 0.3538 0.131 Uiso 1 1 calc R . . H39B H 0.0235 0.4461 0.3809 0.131 Uiso 1 1 calc R . . C40 C 0.0645(2) 0.4017(3) 0.3089(3) 0.0687(18) Uani 1 1 d . . . H40A H 0.0561 0.3669 0.2802 0.082 Uiso 1 1 calc R . . H40B H 0.0618 0.4385 0.2818 0.082 Uiso 1 1 calc R . . C45 C 0.2287(2) 0.5538(2) 0.2844(4) 0.0655(16) Uani 1 1 d . . . H45A H 0.2662 0.5411 0.2884 0.079 Uiso 1 1 calc R . . H45B H 0.2208 0.5608 0.2366 0.079 Uiso 1 1 calc R . . C46 C 0.2197(3) 0.6078(2) 0.3227(4) 0.077(2) Uani 1 1 d . . . H46A H 0.2248 0.6438 0.2947 0.092 Uiso 1 1 calc R . . H46B H 0.2439 0.6100 0.3615 0.092 Uiso 1 1 calc R . . C47 C 0.1632(3) 0.6025(2) 0.3450(4) 0.0664(17) Uani 1 1 d . . . H47A H 0.1387 0.6187 0.3108 0.080 Uiso 1 1 calc R . . H47B H 0.1574 0.6239 0.3876 0.080 Uiso 1 1 calc R . . C48 C 0.1553(2) 0.5351(2) 0.3536(3) 0.0614(15) Uani 1 1 d . . . H48A H 0.1611 0.5232 0.4007 0.074 Uiso 1 1 calc R . . H48B H 0.1190 0.5232 0.3403 0.074 Uiso 1 1 calc R . . C18 C 0.3703(2) 0.4302(3) 0.2176(3) 0.0626(15) Uiso 1 1 d . . . C13 C 0.32096(19) 0.4288(2) 0.1862(2) 0.0417(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.03440(15) 0.02973(16) 0.03138(15) 0.00081(9) 0.00117(10) 0.00213(9) O1 0.0368(16) 0.0430(17) 0.0418(18) -0.0054(15) -0.0088(14) 0.0085(14) C1 0.026(2) 0.044(3) 0.042(3) 0.005(2) 0.0000(19) 0.0046(18) O2 0.0331(16) 0.0455(18) 0.0364(18) 0.0012(14) 0.0027(13) 0.0006(14) C2 0.038(3) 0.052(3) 0.043(3) -0.003(2) -0.002(2) 0.004(2) O3 0.050(2) 0.032(2) 0.057(2) -0.0019(15) -0.0001(15) 0.0049(13) C3 0.032(2) 0.061(3) 0.041(3) -0.003(2) -0.004(2) 0.001(2) O5 0.069(2) 0.067(2) 0.043(2) 0.0055(18) -0.0117(18) 0.0241(19) C4 0.035(3) 0.088(4) 0.042(3) 0.010(3) -0.007(2) -0.002(3) O4 0.0298(16) 0.058(2) 0.053(2) 0.0025(16) 0.0122(15) 0.0035(13) C5 0.033(2) 0.052(3) 0.060(3) 0.020(3) -0.001(2) 0.004(2) O6 0.0472(18) 0.0364(18) 0.051(2) -0.0090(15) 0.0103(15) -0.0030(14) C6 0.030(2) 0.039(3) 0.053(3) 0.006(2) -0.001(2) -0.0016(18) C7 0.104(5) 0.073(4) 0.074(5) -0.029(3) -0.010(4) 0.040(4) C8 0.061(3) 0.043(3) 0.058(3) -0.018(2) -0.018(3) 0.016(2) C9 0.062(4) 0.051(3) 0.104(5) 0.010(3) -0.002(3) 0.009(3) C10 0.068(4) 0.068(4) 0.085(5) -0.007(3) 0.016(3) 0.006(3) C11 0.053(3) 0.032(3) 0.068(4) 0.002(2) -0.010(3) 0.007(2) C12 0.077(4) 0.032(3) 0.121(6) -0.004(3) 0.007(4) -0.012(3) C14 0.044(3) 0.070(4) 0.070(4) 0.009(3) 0.017(3) 0.002(3) C15 0.066(4) 0.153(7) 0.072(5) 0.025(5) 0.020(4) 0.011(5) C16 0.065(5) 0.228(11) 0.122(8) 0.061(8) 0.052(5) 0.027(6) C17 0.038(3) 0.165(8) 0.114(7) 0.058(6) 0.012(4) 0.012(4) C19 0.061(3) 0.056(3) 0.058(3) 0.012(3) 0.005(3) 0.006(3) C20 0.062(3) 0.069(4) 0.048(3) 0.008(3) 0.009(3) 0.006(3) C21 0.135(7) 0.085(5) 0.049(4) -0.001(3) 0.014(4) 0.012(4) C22 0.119(6) 0.065(5) 0.154(8) 0.007(5) -0.043(6) -0.020(4) C23 0.042(3) 0.083(5) 0.098(5) 0.017(4) -0.012(3) -0.010(3) C24 0.088(5) 0.126(6) 0.101(6) 0.025(5) -0.040(5) 0.037(5) C25 0.049(3) 0.032(3) 0.056(3) 0.002(2) -0.014(2) 0.009(2) C26 0.053(3) 0.031(3) 0.069(4) 0.007(2) -0.005(3) 0.006(2) C27 0.058(3) 0.031(3) 0.090(5) 0.006(3) -0.015(3) 0.002(2) C28 0.054(3) 0.038(3) 0.080(4) -0.006(3) -0.014(3) 0.007(2) C29 0.059(3) 0.046(3) 0.060(3) -0.005(3) -0.009(3) 0.021(3) C30 0.040(3) 0.042(3) 0.055(3) -0.001(2) -0.006(2) 0.014(2) C31 0.064(4) 0.081(5) 0.127(7) -0.001(4) 0.017(4) 0.000(3) C32 0.063(3) 0.041(3) 0.079(4) 0.005(3) 0.017(3) -0.005(2) C33 0.100(5) 0.090(5) 0.079(5) 0.018(4) 0.009(4) -0.002(4) C34 0.057(3) 0.056(4) 0.088(4) 0.009(3) -0.015(3) 0.012(3) C35 0.056(3) 0.032(3) 0.074(4) 0.004(2) 0.014(3) 0.012(2) C36 0.109(5) 0.060(4) 0.067(4) 0.005(3) 0.023(4) 0.023(3) C41 0.160(8) 0.070(5) 0.091(6) 0.036(4) -0.025(6) 0.031(5) C42 0.100(6) 0.170(10) 0.121(8) 0.052(7) -0.012(6) 0.072(6) C43 0.108(7) 0.221(13) 0.064(5) -0.030(6) -0.034(5) 0.093(7) C44 0.113(6) 0.127(6) 0.064(4) -0.039(5) -0.053(4) 0.049(5) C37 0.061(3) 0.062(3) 0.047(3) -0.001(3) 0.008(3) 0.002(3) C38 0.070(4) 0.073(4) 0.074(4) -0.016(3) 0.027(3) -0.017(3) C39 0.052(4) 0.133(7) 0.142(9) 0.031(6) 0.038(5) 0.010(4) C40 0.033(3) 0.105(5) 0.068(4) 0.016(3) 0.003(3) 0.002(3) C45 0.056(3) 0.045(3) 0.095(5) -0.006(3) 0.012(3) -0.007(2) C46 0.123(6) 0.040(3) 0.067(4) -0.012(3) 0.023(4) -0.008(3) C47 0.084(4) 0.037(3) 0.078(5) -0.009(3) 0.020(4) 0.006(3) C48 0.056(3) 0.055(3) 0.074(4) -0.014(3) 0.016(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O2 2.183(3) . ? Nd1 O1 2.189(3) . ? Nd1 O3 2.189(3) . ? Nd1 O5 2.545(3) . ? Nd1 O4 2.550(3) . ? Nd1 O6 2.572(3) . ? O1 C1 1.355(5) . ? C1 C6 1.411(6) . ? C1 C2 1.425(7) . ? O2 C13 1.333(6) . ? C2 C3 1.365(7) . ? C2 C8 1.523(7) . ? O3 C25 1.348(6) . ? C3 C4 1.388(7) . ? O5 C44 1.442(8) . ? O5 C41 1.449(7) . ? C4 C5 1.374(7) . ? O4 C37 1.431(6) . ? O4 C40 1.452(6) . ? C5 C6 1.382(7) . ? O6 C48 1.421(6) . ? O6 C45 1.464(6) . ? C6 C11 1.510(7) . ? C7 C8 1.536(7) . ? C8 C9 1.535(8) . ? C10 C11 1.526(7) . ? C11 C12 1.524(7) . ? C14 C15 1.393(8) . ? C14 C13 1.409(8) . ? C14 C20 1.528(8) . ? C15 C16 1.381(12) . ? C16 C17 1.374(12) . ? C17 C18 1.437(9) . ? C19 C20 1.501(8) . ? C20 C21 1.538(8) . ? C22 C23 1.539(10) . ? C23 C18 1.526(9) . ? C23 C24 1.552(8) . ? C25 C30 1.398(7) . ? C25 C26 1.415(7) . ? C26 C27 1.403(7) . ? C26 C32 1.510(7) . ? C27 C28 1.360(8) . ? C28 C29 1.364(8) . ? C29 C30 1.400(7) . ? C30 C35 1.517(7) . ? C31 C32 1.557(8) . ? C32 C33 1.542(9) . ? C34 C35 1.533(8) . ? C35 C36 1.527(8) . ? C41 C42 1.413(11) . ? C42 C43 1.535(12) . ? C43 C44 1.502(9) . ? C37 C38 1.527(8) . ? C38 C39 1.486(10) . ? C39 C40 1.460(10) . ? C45 C46 1.452(8) . ? C46 C47 1.497(9) . ? C47 C48 1.532(7) . ? C18 C13 1.397(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Nd1 O1 103.03(11) . . ? O2 Nd1 O3 101.76(12) . . ? O1 Nd1 O3 102.27(12) . . ? O2 Nd1 O5 92.84(12) . . ? O1 Nd1 O5 161.81(12) . . ? O3 Nd1 O5 82.80(13) . . ? O2 Nd1 O4 162.84(11) . . ? O1 Nd1 O4 85.37(12) . . ? O3 Nd1 O4 90.81(11) . . ? O5 Nd1 O4 77.04(12) . . ? O2 Nd1 O6 87.51(11) . . ? O1 Nd1 O6 90.96(11) . . ? O3 Nd1 O6 161.51(11) . . ? O5 Nd1 O6 80.77(12) . . ? O4 Nd1 O6 77.30(10) . . ? C1 O1 Nd1 167.1(3) . . ? O1 C1 C6 120.7(4) . . ? O1 C1 C2 120.2(4) . . ? C6 C1 C2 119.1(4) . . ? C13 O2 Nd1 164.3(3) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 C8 121.7(4) . . ? C1 C2 C8 118.4(4) . . ? C25 O3 Nd1 163.9(3) . . ? C2 C3 C4 120.9(5) . . ? C44 O5 C41 107.1(5) . . ? C44 O5 Nd1 127.7(4) . . ? C41 O5 Nd1 123.2(4) . . ? C5 C4 C3 119.4(5) . . ? C37 O4 C40 108.7(4) . . ? C37 O4 Nd1 129.8(3) . . ? C40 O4 Nd1 121.2(3) . . ? C4 C5 C6 122.1(4) . . ? C48 O6 C45 109.2(4) . . ? C48 O6 Nd1 131.4(3) . . ? C45 O6 Nd1 118.5(3) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C11 121.3(4) . . ? C1 C6 C11 120.1(4) . . ? C2 C8 C9 108.9(4) . . ? C2 C8 C7 113.7(5) . . ? C9 C8 C7 111.1(5) . . ? C6 C11 C12 113.1(5) . . ? C6 C11 C10 111.2(4) . . ? C12 C11 C10 110.1(4) . . ? C15 C14 C13 120.1(6) . . ? C15 C14 C20 120.3(6) . . ? C13 C14 C20 119.5(5) . . ? C16 C15 C14 120.8(7) . . ? C17 C16 C15 119.7(7) . . ? C16 C17 C18 121.3(7) . . ? C19 C20 C21 109.4(5) . . ? C19 C20 C14 110.3(5) . . ? C21 C20 C14 115.6(5) . . ? C18 C23 C22 109.7(6) . . ? C18 C23 C24 113.0(6) . . ? C22 C23 C24 111.9(6) . . ? O3 C25 C30 120.4(5) . . ? O3 C25 C26 119.1(5) . . ? C30 C25 C26 120.5(5) . . ? C27 C26 C25 117.9(5) . . ? C27 C26 C32 120.2(5) . . ? C25 C26 C32 122.0(5) . . ? C28 C27 C26 121.2(5) . . ? C29 C28 C27 120.7(5) . . ? C28 C29 C30 121.1(5) . . ? C25 C30 C29 118.5(5) . . ? C25 C30 C35 119.5(4) . . ? C29 C30 C35 121.9(5) . . ? C26 C32 C33 110.9(5) . . ? C26 C32 C31 113.2(5) . . ? C33 C32 C31 110.6(5) . . ? C30 C35 C36 115.0(5) . . ? C30 C35 C34 110.5(5) . . ? C36 C35 C34 110.3(5) . . ? C42 C41 O5 106.8(7) . . ? C41 C42 C43 105.0(7) . . ? C44 C43 C42 104.8(7) . . ? O5 C44 C43 106.2(6) . . ? O4 C37 C38 106.3(5) . . ? C39 C38 C37 101.7(5) . . ? C40 C39 C38 104.9(5) . . ? O4 C40 C39 106.0(6) . . ? C46 C45 O6 107.2(5) . . ? C45 C46 C47 103.9(5) . . ? C46 C47 C48 103.7(4) . . ? O6 C48 C47 105.6(4) . . ? C13 C18 C17 118.1(6) . . ? C13 C18 C23 120.4(5) . . ? C17 C18 C23 121.3(6) . . ? O2 C13 C18 120.8(5) . . ? O2 C13 C14 119.4(4) . . ? C18 C13 C14 119.9(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.818 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.112 # Attachment '- 13.Yb(DIP)(DME).CIF' data_Yb(DIP)3(DME)2,2.CIF _database_code_depnum_ccdc_archive 'CCDC 845100' #TrackingRef '- 13.Yb(DIP)(DME).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Yb(DIP)3DME2 _chemical_melting_point ? _chemical_formula_moiety 'C88 H142 O14 Yb2' _chemical_formula_sum 'C88 H142 O14 Yb2' _chemical_formula_weight 1770.10 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' 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 P21/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 22.0514(5) _cell_length_b 18.9710(4) _cell_length_c 23.2542(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.2020(10) _cell_angle_gamma 90.00 _cell_volume 8802.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 74411 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3688 _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7807 _exptl_absorpt_correction_T_max 0.9378 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74411 _diffrn_reflns_av_R_equivalents 0.2136 _diffrn_reflns_av_sigmaI/netI 0.2270 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19092 _reflns_number_gt 9137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 19092 _refine_ls_number_parameters 969 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1744 _refine_ls_R_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1224 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.947 _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 Yb1 Yb 0.018329(19) 0.42772(2) 0.709367(18) 0.01496(12) Uani 1 1 d . . . Yb2 Yb 0.47687(2) 0.59938(2) 0.290151(19) 0.01713(12) Uani 1 1 d . . . O2 O 0.0787(3) 0.4127(3) 0.8047(3) 0.0202(16) Uani 1 1 d . . . O3 O 0.0740(3) 0.3807(3) 0.6685(3) 0.0181(15) Uani 1 1 d . . . O1 O 0.0186(3) 0.5379(3) 0.6966(3) 0.0200(16) Uani 1 1 d . . . O4 O -0.0716(3) 0.4145(3) 0.6023(3) 0.0206(16) Uani 1 1 d . . . O5 O -0.1711(4) 0.3070(4) 0.5277(4) 0.059(3) Uani 1 1 d . . . O7 O -0.0802(3) 0.4424(3) 0.7266(3) 0.0186(15) Uani 1 1 d . . . O6 O -0.0326(3) 0.3173(3) 0.7139(3) 0.0209(16) Uani 1 1 d . . . O8 O 0.4268(3) 0.5540(3) 0.3384(3) 0.0205(15) Uani 1 1 d . . . O9 O 0.4097(3) 0.5842(3) 0.1966(3) 0.0205(16) Uani 1 1 d . . . O10 O 0.4819(3) 0.7078(3) 0.3061(3) 0.0150(15) Uani 1 1 d . . . O11 O 0.6716(3) 0.4794(4) 0.4515(3) 0.038(2) Uani 1 1 d . . . O12 O 0.5739(3) 0.5877(3) 0.3926(3) 0.0232(16) Uani 1 1 d . . . O13 O 0.5239(3) 0.4886(3) 0.2782(3) 0.0259(17) Uani 1 1 d . . . O14 O 0.5684(3) 0.6163(3) 0.2620(3) 0.0228(16) Uani 1 1 d . . . C13 C 0.1161(4) 0.3894(5) 0.8657(4) 0.023(2) Uani 1 1 d . . . C18 C 0.1769(5) 0.3520(6) 0.8780(5) 0.031(3) Uani 1 1 d . . . C17 C 0.2140(6) 0.3275(7) 0.9399(5) 0.055(4) Uani 1 1 d . . . H17 H 0.2538 0.3015 0.9491 0.066 Uiso 1 1 calc R . . C16 C 0.1948(6) 0.3397(8) 0.9872(6) 0.074(5) Uani 1 1 d . . . H16 H 0.2213 0.3226 1.0288 0.089 Uiso 1 1 calc R . . C15 C 0.1367(5) 0.3772(7) 0.9749(5) 0.048(4) Uani 1 1 d . . . H15 H 0.1233 0.3847 1.0082 0.058 Uiso 1 1 calc R . . C14 C 0.0975(4) 0.4042(5) 0.9144(4) 0.027(3) Uani 1 1 d . . . C23 C 0.2381(5) 0.2689(6) 0.8343(5) 0.046(3) Uani 1 1 d . . . H23A H 0.2416 0.2573 0.7947 0.069 Uiso 1 1 calc R . . H23B H 0.2142 0.2311 0.8447 0.069 Uiso 1 1 calc R . . H23C H 0.2832 0.2738 0.8687 0.069 Uiso 1 1 calc R . . C22 C 0.1999(5) 0.3382(6) 0.8260(5) 0.033(3) Uani 1 1 d . . . H22 H 0.1594 0.3368 0.7843 0.039 Uiso 1 1 calc R . . C24 C 0.2439(6) 0.3984(6) 0.8246(6) 0.051(4) Uani 1 1 d . . . H24A H 0.2183 0.4424 0.8157 0.077 Uiso 1 1 calc R . . H24B H 0.2591 0.3899 0.7913 0.077 Uiso 1 1 calc R . . H24C H 0.2827 0.4019 0.8659 0.077 Uiso 1 1 calc R . . C20 C -0.0166(5) 0.3944(5) 0.9131(5) 0.032(3) Uani 1 1 d . . . H20A H -0.0280 0.3544 0.8837 0.048 Uiso 1 1 calc R . . H20B H -0.0573 0.4210 0.9059 0.048 Uiso 1 1 calc R . . H20C H 0.0038 0.3770 0.9570 0.048 Uiso 1 1 calc R . . C19 C 0.0331(5) 0.4427(5) 0.9018(5) 0.026(2) Uani 1 1 d . . . H19 H 0.0124 0.4589 0.8566 0.031 Uiso 1 1 calc R . . C21 C 0.0450(6) 0.5078(6) 0.9460(6) 0.052(4) Uani 1 1 d . . . H21A H 0.0605 0.4920 0.9901 0.077 Uiso 1 1 calc R . . H21B H 0.0030 0.5341 0.9334 0.077 Uiso 1 1 calc R . . H21C H 0.0791 0.5384 0.9424 0.077 Uiso 1 1 calc R . . C25 C 0.1242(4) 0.3553(5) 0.6556(4) 0.022(2) Uani 1 1 d . . . C26 C 0.1295(4) 0.2816(5) 0.6476(4) 0.019(2) Uani 1 1 d . . . C27 C 0.1835(4) 0.2574(5) 0.6366(4) 0.022(2) Uani 1 1 d . . . H27 H 0.1870 0.2083 0.6304 0.026 Uiso 1 1 calc R . . C28 C 0.2315(5) 0.3017(5) 0.6345(5) 0.032(3) Uani 1 1 d . . . H28 H 0.2682 0.2837 0.6279 0.039 Uiso 1 1 calc R . . C29 C 0.2255(4) 0.3736(5) 0.6423(4) 0.026(3) Uani 1 1 d . . . H29 H 0.2588 0.4044 0.6408 0.032 Uiso 1 1 calc R . . C30 C 0.1729(4) 0.4019(5) 0.6520(4) 0.017(2) Uani 1 1 d . . . C35 C 0.2257(5) 0.5240(6) 0.6757(6) 0.046(3) Uani 1 1 d . . . H35A H 0.2600 0.5058 0.7158 0.069 Uiso 1 1 calc R . . H35B H 0.2162 0.5733 0.6812 0.069 Uiso 1 1 calc R . . H35C H 0.2420 0.5208 0.6426 0.069 Uiso 1 1 calc R . . C34 C 0.1619(4) 0.4805(5) 0.6561(5) 0.023(2) Uani 1 1 d . . . H34 H 0.1443 0.4877 0.6889 0.028 Uiso 1 1 calc R . . C36 C 0.1089(5) 0.5062(5) 0.5927(5) 0.035(3) Uani 1 1 d . . . H36A H 0.1260 0.5023 0.5602 0.052 Uiso 1 1 calc R . . H36B H 0.0980 0.5556 0.5966 0.052 Uiso 1 1 calc R . . H36C H 0.0684 0.4774 0.5803 0.052 Uiso 1 1 calc R . . C33 C 0.1020(5) 0.1743(5) 0.6969(5) 0.041(3) Uani 1 1 d . . . H33A H 0.1326 0.1434 0.6881 0.061 Uiso 1 1 calc R . . H33B H 0.0643 0.1465 0.6964 0.061 Uiso 1 1 calc R . . H33C H 0.1259 0.1962 0.7387 0.061 Uiso 1 1 calc R . . C31 C 0.0755(4) 0.2318(5) 0.6459(4) 0.024(2) Uani 1 1 d . . . H31 H 0.0417 0.2600 0.6541 0.029 Uiso 1 1 calc R . . C32 C 0.0395(5) 0.1981(5) 0.5800(5) 0.035(3) Uani 1 1 d . . . H32A H 0.0214 0.2352 0.5478 0.052 Uiso 1 1 calc R . . H32B H 0.0028 0.1683 0.5790 0.052 Uiso 1 1 calc R . . H32C H 0.0713 0.1693 0.5709 0.052 Uiso 1 1 calc R . . C1 C 0.0470(4) 0.5965(4) 0.6877(4) 0.0122(19) Uani 1 1 d U . . C6 C 0.1112(4) 0.6187(5) 0.7333(4) 0.017(2) Uani 1 1 d . . . C5 C 0.1420(4) 0.6759(5) 0.7205(4) 0.021(2) Uani 1 1 d . . . H5 H 0.1856 0.6896 0.7504 0.025 Uiso 1 1 calc R . . C4 C 0.1101(4) 0.7138(5) 0.6643(4) 0.023(2) Uani 1 1 d U . . H4 H 0.1314 0.7533 0.6556 0.027 Uiso 1 1 calc R . . C3 C 0.0476(4) 0.6932(5) 0.6220(4) 0.018(2) Uani 1 1 d U . . H3 H 0.0262 0.7195 0.5838 0.022 Uiso 1 1 calc R . . C2 C 0.0137(4) 0.6366(5) 0.6313(4) 0.015(2) Uani 1 1 d U . . C11 C 0.1047(5) 0.5976(6) 0.8370(4) 0.032(3) Uani 1 1 d . . . H11A H 0.1096 0.6481 0.8466 0.049 Uiso 1 1 calc R . . H11B H 0.1235 0.5706 0.8767 0.049 Uiso 1 1 calc R . . H11C H 0.0571 0.5861 0.8134 0.049 Uiso 1 1 calc R . . C10 C 0.1423(4) 0.5786(5) 0.7961(4) 0.025(3) Uani 1 1 d . . . H10 H 0.1364 0.5270 0.7865 0.030 Uiso 1 1 calc R . . C12 C 0.2178(4) 0.5932(5) 0.8345(5) 0.033(3) Uani 1 1 d . . . H12A H 0.2415 0.5830 0.8082 0.050 Uiso 1 1 calc R . . H12B H 0.2354 0.5632 0.8724 0.050 Uiso 1 1 calc R . . H12C H 0.2244 0.6429 0.8475 0.050 Uiso 1 1 calc R . . C8 C -0.1072(5) 0.6421(5) 0.6111(5) 0.036(3) Uani 1 1 d . . . H8A H -0.0951 0.6212 0.6531 0.054 Uiso 1 1 calc R . . H8B H -0.1527 0.6275 0.5822 0.054 Uiso 1 1 calc R . . H8C H -0.1053 0.6936 0.6148 0.054 Uiso 1 1 calc R . . C7 C -0.0578(5) 0.6170(5) 0.5848(4) 0.024(3) Uani 1 1 d . . . H7 H -0.0608 0.5645 0.5810 0.029 Uiso 1 1 calc R . . C9 C -0.0781(5) 0.6482(6) 0.5180(4) 0.033(3) Uani 1 1 d . . . H9A H -0.0788 0.6997 0.5202 0.049 Uiso 1 1 calc R . . H9B H -0.1228 0.6310 0.4894 0.049 Uiso 1 1 calc R . . H9C H -0.0456 0.6336 0.5018 0.049 Uiso 1 1 calc R . . C37 C -0.1325(4) 0.4539(5) 0.5811(4) 0.020(2) Uani 1 1 d . . . H37A H -0.1402 0.4784 0.5415 0.030 Uiso 1 1 calc R . . H37B H -0.1291 0.4885 0.6136 0.030 Uiso 1 1 calc R . . H37C H -0.1699 0.4218 0.5737 0.030 Uiso 1 1 calc R . . C38 C -0.0669(5) 0.3715(6) 0.5538(4) 0.030(3) Uani 1 1 d . . . H38A H -0.0192 0.3618 0.5646 0.036 Uiso 1 1 calc R . . H38B H -0.0862 0.3971 0.5129 0.036 Uiso 1 1 calc R . . C39 C -0.1064(6) 0.2978(6) 0.5467(5) 0.054(4) Uani 1 1 d . . . H39A H -0.0988 0.2674 0.5158 0.064 Uiso 1 1 calc R . . H39B H -0.0879 0.2732 0.5882 0.064 Uiso 1 1 calc R . . C40 C -0.2030(5) 0.2393(6) 0.5156(5) 0.053(4) Uani 1 1 d . . . H40A H -0.1855 0.2104 0.4911 0.079 Uiso 1 1 calc R . . H40B H -0.2515 0.2452 0.4914 0.079 Uiso 1 1 calc R . . H40C H -0.1937 0.2159 0.5561 0.079 Uiso 1 1 calc R . . C44 C -0.1000(4) 0.5063(5) 0.7473(4) 0.022(2) Uani 1 1 d . . . H44A H -0.1474 0.5156 0.7204 0.033 Uiso 1 1 calc R . . H44B H -0.0728 0.5456 0.7440 0.033 Uiso 1 1 calc R . . H44C H -0.0932 0.5010 0.7915 0.033 Uiso 1 1 calc R . . C43 C -0.1139(4) 0.3807(5) 0.7365(4) 0.022(2) Uani 1 1 d . . . H43A H -0.1623 0.3902 0.7219 0.027 Uiso 1 1 calc R . . H43B H -0.0946 0.3682 0.7822 0.027 Uiso 1 1 calc R . . C42 C -0.1035(4) 0.3229(5) 0.6994(4) 0.023(2) Uani 1 1 d . . . H42A H -0.1194 0.2780 0.7099 0.028 Uiso 1 1 calc R . . H42B H -0.1297 0.3321 0.6535 0.028 Uiso 1 1 calc R . . C41 C 0.0059(4) 0.2700(5) 0.7656(4) 0.023(2) Uani 1 1 d U . . H41A H 0.0023 0.2851 0.8043 0.034 Uiso 1 1 calc R . . H41B H 0.0530 0.2709 0.7727 0.034 Uiso 1 1 calc R . . H41C H -0.0117 0.2220 0.7546 0.034 Uiso 1 1 calc R . . C45 C 0.3796(4) 0.5295(5) 0.3548(4) 0.019(2) Uani 1 1 d . . . C46 C 0.3712(4) 0.4568(5) 0.3614(4) 0.017(2) Uani 1 1 d . . . C47 C 0.3199(4) 0.4335(5) 0.3753(4) 0.023(2) Uani 1 1 d . . . H47 H 0.3124 0.3844 0.3769 0.027 Uiso 1 1 calc R . . C48 C 0.2792(5) 0.4814(5) 0.3868(4) 0.025(2) Uani 1 1 d U . . H48 H 0.2449 0.4651 0.3979 0.030 Uiso 1 1 calc R . . C49 C 0.2881(4) 0.5522(5) 0.3824(4) 0.023(2) Uani 1 1 d . . . H49 H 0.2592 0.5842 0.3902 0.027 Uiso 1 1 calc R . . C50 C 0.3378(4) 0.5789(5) 0.3670(4) 0.021(2) Uani 1 1 d . . . C51 C 0.2903(5) 0.7034(6) 0.3541(5) 0.037(3) Uani 1 1 d . . . H51A H 0.2539 0.6922 0.3126 0.056 Uiso 1 1 calc R . . H51B H 0.3032 0.7529 0.3548 0.056 Uiso 1 1 calc R . . H51C H 0.2751 0.6952 0.3875 0.056 Uiso 1 1 calc R . . C52 C 0.3509(4) 0.6561(5) 0.3658(4) 0.021(2) Uani 1 1 d . . . H52 H 0.3641 0.6645 0.3302 0.025 Uiso 1 1 calc R . . C53 C 0.4100(5) 0.6794(5) 0.4278(4) 0.028(3) Uani 1 1 d . . . H53A H 0.3992 0.6703 0.4639 0.043 Uiso 1 1 calc R . . H53B H 0.4183 0.7298 0.4256 0.043 Uiso 1 1 calc R . . H53C H 0.4502 0.6527 0.4334 0.043 Uiso 1 1 calc R . . C54 C 0.4603(6) 0.3684(7) 0.4158(6) 0.061(4) Uani 1 1 d . . . H54A H 0.4840 0.4037 0.4485 0.091 Uiso 1 1 calc R . . H54B H 0.4930 0.3367 0.4110 0.091 Uiso 1 1 calc R . . H54C H 0.4302 0.3411 0.4284 0.091 Uiso 1 1 calc R . . C55 C 0.4199(5) 0.4050(5) 0.3533(5) 0.032(3) Uani 1 1 d . . . H55 H 0.4514 0.4322 0.3410 0.038 Uiso 1 1 calc R . . C56 C 0.3837(6) 0.3508(6) 0.3014(6) 0.057(4) Uani 1 1 d . . . H56A H 0.4168 0.3211 0.2951 0.086 Uiso 1 1 calc R . . H56B H 0.3561 0.3751 0.2616 0.086 Uiso 1 1 calc R . . H56C H 0.3551 0.3212 0.3142 0.086 Uiso 1 1 calc R . . C57 C 0.3632(5) 0.5684(5) 0.1380(4) 0.026(3) Uani 1 1 d . . . C58 C 0.3019(5) 0.5378(6) 0.1300(5) 0.037(3) Uani 1 1 d . . . C59 C 0.2546(6) 0.5229(9) 0.0685(6) 0.101(7) Uani 1 1 d . . . H59 H 0.2137 0.5009 0.0626 0.121 Uiso 1 1 calc R . . C60 C 0.2657(9) 0.5392(9) 0.0170(8) 0.100(6) Uani 1 1 d U . . H60 H 0.2313 0.5315 -0.0244 0.120 Uiso 1 1 calc R . . C61 C 0.3280(6) 0.5675(9) 0.0239(6) 0.087(6) Uani 1 1 d . . . H61 H 0.3369 0.5752 -0.0121 0.104 Uiso 1 1 calc R . . C62 C 0.3750(5) 0.5834(6) 0.0838(5) 0.033(3) Uani 1 1 d . . . C63 C 0.2528(5) 0.5798(6) 0.2024(5) 0.053(4) Uani 1 1 d . . . H63A H 0.2833 0.6202 0.2175 0.080 Uiso 1 1 calc R . . H63B H 0.2401 0.5645 0.2360 0.080 Uiso 1 1 calc R . . H63C H 0.2126 0.5936 0.1648 0.080 Uiso 1 1 calc R . . C64 C 0.2880(5) 0.5191(6) 0.1853(5) 0.033(3) Uani 1 1 d . . . H64 H 0.3322 0.5115 0.2225 0.040 Uiso 1 1 calc R . . C65 C 0.2466(6) 0.4525(7) 0.1772(5) 0.058(4) Uani 1 1 d . . . H65A H 0.2016 0.4596 0.1432 0.087 Uiso 1 1 calc R . . H65B H 0.2433 0.4420 0.2171 0.087 Uiso 1 1 calc R . . H65C H 0.2683 0.4130 0.1662 0.087 Uiso 1 1 calc R . . C66 C 0.4319(6) 0.6787(6) 0.0491(5) 0.050(4) Uani 1 1 d . . . H66A H 0.4134 0.6652 0.0042 0.075 Uiso 1 1 calc R . . H66B H 0.4757 0.7013 0.0613 0.075 Uiso 1 1 calc R . . H66C H 0.4014 0.7118 0.0557 0.075 Uiso 1 1 calc R . . C67 C 0.4403(5) 0.6125(6) 0.0902(5) 0.031(3) Uani 1 1 d . . . H67 H 0.4674 0.6254 0.1357 0.038 Uiso 1 1 calc R . . C68 C 0.4798(5) 0.5576(6) 0.0709(5) 0.044(3) Uani 1 1 d . . . H68A H 0.4861 0.5149 0.0964 0.066 Uiso 1 1 calc R . . H68B H 0.5237 0.5772 0.0782 0.066 Uiso 1 1 calc R . . H68C H 0.4549 0.5461 0.0258 0.066 Uiso 1 1 calc R . . C69 C 0.4557(4) 0.7664(5) 0.3177(4) 0.018(2) Uani 1 1 d . . . C70 C 0.3908(4) 0.7905(5) 0.2746(4) 0.019(2) Uani 1 1 d . . . C71 C 0.3641(4) 0.8492(5) 0.2903(5) 0.024(2) Uani 1 1 d . . . H71 H 0.3211 0.8652 0.2613 0.029 Uiso 1 1 calc R . . C72 C 0.3969(5) 0.8856(5) 0.3462(5) 0.028(3) Uani 1 1 d . . . H72 H 0.3762 0.9245 0.3563 0.033 Uiso 1 1 calc R . . C73 C 0.4605(4) 0.8644(5) 0.3871(4) 0.026(3) Uani 1 1 d . . . H73 H 0.4844 0.8903 0.4251 0.031 Uiso 1 1 calc R . . C74 C 0.4901(4) 0.8065(5) 0.3742(4) 0.019(2) Uani 1 1 d . . . C75 C 0.6116(5) 0.8122(5) 0.3970(5) 0.033(3) Uani 1 1 d . . . H75A H 0.6002 0.7962 0.3536 0.049 Uiso 1 1 calc R . . H75B H 0.6564 0.7951 0.4254 0.049 Uiso 1 1 calc R . . H75C H 0.6112 0.8639 0.3980 0.049 Uiso 1 1 calc R . . C76 C 0.5610(4) 0.7838(5) 0.4187(5) 0.029(3) Uani 1 1 d . . . H76 H 0.5625 0.7312 0.4163 0.035 Uiso 1 1 calc R . . C77 C 0.5807(5) 0.8028(6) 0.4892(5) 0.043(3) Uani 1 1 d . . . H77A H 0.6217 0.7776 0.5163 0.064 Uiso 1 1 calc R . . H77B H 0.5444 0.7893 0.5006 0.064 Uiso 1 1 calc R . . H77C H 0.5884 0.8537 0.4951 0.064 Uiso 1 1 calc R . . C78 C 0.3934(5) 0.7658(6) 0.1695(5) 0.042(3) Uani 1 1 d . . . H78A H 0.3928 0.8164 0.1610 0.063 Uiso 1 1 calc R . . H78B H 0.3706 0.7403 0.1293 0.063 Uiso 1 1 calc R . . H78C H 0.4398 0.7495 0.1912 0.063 Uiso 1 1 calc R . . C79 C 0.3574(4) 0.7521(5) 0.2116(4) 0.023(2) Uani 1 1 d . . . H79 H 0.3615 0.7005 0.2214 0.028 Uiso 1 1 calc R . . C80 C 0.2828(4) 0.7681(6) 0.1765(5) 0.040(3) Uani 1 1 d . . . H80A H 0.2619 0.7640 0.2060 0.060 Uiso 1 1 calc R . . H80B H 0.2619 0.7345 0.1416 0.060 Uiso 1 1 calc R . . H80C H 0.2767 0.8161 0.1594 0.060 Uiso 1 1 calc R . . C81 C 0.6999(5) 0.4125(6) 0.4533(5) 0.049(4) Uani 1 1 d . . . H81A H 0.7008 0.3860 0.4899 0.074 Uiso 1 1 calc R . . H81B H 0.7457 0.4179 0.4572 0.074 Uiso 1 1 calc R . . H81C H 0.6728 0.3868 0.4141 0.074 Uiso 1 1 calc R . . C82 C 0.6054(5) 0.4724(6) 0.4441(5) 0.040(3) Uani 1 1 d . . . H82A H 0.6047 0.4435 0.4793 0.048 Uiso 1 1 calc R . . H82B H 0.5784 0.4479 0.4037 0.048 Uiso 1 1 calc R . . C83 C 0.5754(5) 0.5430(6) 0.4442(5) 0.036(3) Uani 1 1 d . . . H83A H 0.5291 0.5367 0.4400 0.043 Uiso 1 1 calc R . . H83B H 0.6017 0.5667 0.4853 0.043 Uiso 1 1 calc R . . C84 C 0.6353(4) 0.6264(5) 0.4108(5) 0.027(3) Uani 1 1 d . . . H84A H 0.6456 0.6512 0.4508 0.041 Uiso 1 1 calc R . . H84B H 0.6305 0.6606 0.3776 0.041 Uiso 1 1 calc R . . H84C H 0.6718 0.5936 0.4164 0.041 Uiso 1 1 calc R . . C85 C 0.4839(5) 0.4418(5) 0.2280(5) 0.035(3) Uani 1 1 d . . . H85A H 0.4835 0.4580 0.1878 0.052 Uiso 1 1 calc R . . H85B H 0.4379 0.4412 0.2243 0.052 Uiso 1 1 calc R . . H85C H 0.5028 0.3942 0.2374 0.052 Uiso 1 1 calc R . . C86 C 0.5909(5) 0.4953(5) 0.2860(4) 0.027(3) Uani 1 1 d . . . H86A H 0.6056 0.4508 0.2736 0.032 Uiso 1 1 calc R . . H86B H 0.6207 0.5049 0.3312 0.032 Uiso 1 1 calc R . . C87 C 0.5957(5) 0.5558(5) 0.2447(4) 0.025(2) Uani 1 1 d . . . H87A H 0.6429 0.5642 0.2528 0.030 Uiso 1 1 calc R . . H87B H 0.5697 0.5447 0.1991 0.030 Uiso 1 1 calc R . . C88 C 0.5843(5) 0.6809(5) 0.2384(5) 0.030(3) Uani 1 1 d . . . H88A H 0.6330 0.6853 0.2543 0.045 Uiso 1 1 calc R . . H88B H 0.5668 0.7211 0.2531 0.045 Uiso 1 1 calc R . . H88C H 0.5638 0.6800 0.1918 0.045 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 0.0154(2) 0.0120(3) 0.0157(2) 0.00111(17) 0.00477(16) 0.00048(17) Yb2 0.0172(2) 0.0132(3) 0.0200(2) 0.00041(18) 0.00693(17) 0.00076(17) O2 0.020(3) 0.016(4) 0.020(3) 0.001(3) 0.004(3) 0.001(3) O3 0.025(4) 0.013(4) 0.017(3) 0.000(3) 0.009(3) 0.001(3) O1 0.020(3) 0.013(4) 0.025(4) 0.001(3) 0.008(3) -0.001(3) O4 0.020(3) 0.023(4) 0.018(3) 0.000(3) 0.007(3) 0.005(3) O5 0.047(5) 0.049(6) 0.065(6) -0.011(4) 0.008(5) -0.008(4) O7 0.019(3) 0.011(4) 0.027(4) 0.005(3) 0.011(3) -0.002(3) O6 0.018(3) 0.020(4) 0.022(3) 0.002(3) 0.006(3) -0.001(3) O8 0.020(3) 0.017(4) 0.027(4) 0.002(3) 0.013(3) -0.004(3) O9 0.017(3) 0.024(4) 0.017(3) 0.000(3) 0.004(3) -0.002(3) O10 0.013(3) 0.013(4) 0.022(3) -0.005(3) 0.011(3) 0.003(3) O11 0.032(4) 0.039(5) 0.039(4) 0.003(4) 0.010(4) 0.008(3) O12 0.019(3) 0.024(4) 0.024(4) 0.008(3) 0.008(3) 0.004(3) O13 0.020(4) 0.032(5) 0.024(4) 0.000(3) 0.009(3) -0.001(3) O14 0.025(4) 0.017(4) 0.033(4) 0.003(3) 0.018(3) 0.003(3) C13 0.018(5) 0.029(7) 0.022(5) -0.005(4) 0.008(4) -0.014(4) C18 0.021(6) 0.045(8) 0.024(5) 0.004(5) 0.008(5) 0.006(5) C17 0.034(7) 0.100(12) 0.038(7) 0.020(7) 0.022(6) 0.024(7) C16 0.023(7) 0.161(16) 0.030(7) 0.030(8) 0.003(6) 0.029(8) C15 0.021(6) 0.105(11) 0.024(6) 0.009(6) 0.015(5) 0.008(6) C14 0.014(5) 0.043(7) 0.021(5) 0.004(5) 0.005(4) 0.002(4) C23 0.053(8) 0.037(8) 0.041(7) -0.005(6) 0.014(6) 0.006(6) C22 0.031(6) 0.041(8) 0.024(5) 0.001(5) 0.009(5) 0.020(5) C24 0.065(9) 0.045(9) 0.051(8) 0.017(6) 0.032(7) 0.023(7) C20 0.023(6) 0.043(8) 0.028(6) 0.006(5) 0.009(5) 0.004(5) C19 0.027(6) 0.026(7) 0.029(5) 0.004(5) 0.017(5) -0.006(4) C21 0.085(10) 0.033(8) 0.066(9) -0.017(6) 0.061(8) -0.018(6) C25 0.021(5) 0.022(7) 0.015(5) -0.003(4) 0.002(4) 0.005(4) C26 0.012(5) 0.019(6) 0.027(5) 0.003(4) 0.010(4) 0.000(4) C27 0.023(5) 0.010(6) 0.029(5) -0.006(4) 0.009(4) -0.003(4) C28 0.026(6) 0.023(7) 0.037(6) -0.010(5) 0.005(5) 0.004(5) C29 0.015(5) 0.022(7) 0.037(6) -0.010(5) 0.006(4) -0.001(4) C30 0.012(5) 0.017(6) 0.021(5) 0.001(4) 0.005(4) -0.003(4) C35 0.045(7) 0.022(7) 0.080(9) -0.022(6) 0.035(7) -0.012(5) C34 0.024(5) 0.009(6) 0.034(6) 0.007(4) 0.010(4) 0.006(4) C36 0.046(7) 0.019(7) 0.035(6) 0.008(5) 0.014(5) 0.010(5) C33 0.042(7) 0.025(7) 0.072(9) 0.017(6) 0.039(6) 0.004(5) C31 0.026(5) 0.017(6) 0.032(6) -0.003(4) 0.014(5) 0.000(4) C32 0.025(6) 0.030(7) 0.052(7) -0.007(5) 0.019(5) -0.017(5) C1 0.013(2) 0.012(2) 0.012(2) -0.0010(10) 0.0056(11) 0.0001(10) C6 0.020(5) 0.016(6) 0.018(5) -0.001(4) 0.012(4) 0.009(4) C5 0.019(5) 0.012(6) 0.033(6) -0.008(4) 0.012(4) -0.004(4) C4 0.023(2) 0.022(2) 0.023(2) -0.0001(10) 0.0099(13) 0.0000(10) C3 0.019(2) 0.018(2) 0.018(2) 0.0005(10) 0.0079(12) -0.0002(10) C2 0.015(2) 0.016(2) 0.016(2) -0.0001(10) 0.0072(12) -0.0002(10) C11 0.023(5) 0.057(8) 0.018(5) 0.006(5) 0.009(4) -0.004(5) C10 0.020(5) 0.028(7) 0.020(5) 0.002(4) 0.001(4) -0.002(4) C12 0.026(6) 0.036(7) 0.030(6) 0.008(5) 0.005(5) -0.005(5) C8 0.024(6) 0.031(7) 0.041(7) -0.006(5) 0.003(5) 0.002(5) C7 0.027(6) 0.013(6) 0.028(5) 0.004(4) 0.006(5) 0.003(4) C9 0.030(6) 0.041(8) 0.028(6) 0.006(5) 0.013(5) 0.001(5) C37 0.016(5) 0.020(6) 0.027(5) 0.000(4) 0.012(4) 0.004(4) C38 0.026(6) 0.042(8) 0.022(5) -0.003(5) 0.010(5) 0.007(5) C39 0.048(8) 0.054(10) 0.035(7) -0.020(6) -0.005(6) 0.026(6) C40 0.048(7) 0.040(9) 0.047(7) -0.001(6) -0.003(6) -0.025(6) C44 0.025(5) 0.014(6) 0.029(5) -0.008(4) 0.013(4) 0.005(4) C43 0.016(5) 0.030(7) 0.026(5) -0.002(4) 0.013(4) 0.001(4) C42 0.020(5) 0.028(7) 0.022(5) 0.001(4) 0.010(4) -0.006(4) C41 0.023(2) 0.023(2) 0.023(2) 0.0002(10) 0.0104(13) -0.0001(10) C45 0.018(5) 0.018(6) 0.018(5) 0.002(4) 0.005(4) -0.005(4) C46 0.008(4) 0.026(6) 0.015(4) -0.007(4) 0.003(4) -0.001(4) C47 0.026(5) 0.008(6) 0.032(6) 0.005(4) 0.010(4) -0.003(4) C48 0.025(2) 0.025(2) 0.025(2) 0.0010(10) 0.0108(13) -0.0004(10) C49 0.018(5) 0.016(6) 0.040(6) 0.001(4) 0.018(5) 0.002(4) C50 0.018(5) 0.021(6) 0.020(5) -0.002(4) 0.005(4) -0.002(4) C51 0.037(7) 0.030(8) 0.049(7) -0.003(5) 0.023(6) 0.008(5) C52 0.019(5) 0.021(6) 0.023(5) 0.010(4) 0.010(4) -0.002(4) C53 0.030(6) 0.040(7) 0.016(5) -0.003(4) 0.010(4) -0.010(5) C54 0.052(8) 0.050(10) 0.092(11) 0.024(8) 0.042(8) 0.022(7) C55 0.042(7) 0.007(6) 0.051(7) 0.001(5) 0.024(6) 0.004(5) C56 0.068(9) 0.040(9) 0.086(10) -0.015(7) 0.053(8) -0.012(7) C57 0.028(6) 0.028(7) 0.020(5) -0.001(4) 0.008(4) -0.008(4) C58 0.037(7) 0.040(8) 0.030(6) 0.002(5) 0.011(5) -0.013(5) C59 0.054(9) 0.21(2) 0.021(6) -0.005(9) 0.001(6) -0.088(11) C60 0.100(6) 0.101(6) 0.100(6) 0.0003(10) 0.042(3) -0.0008(10) C61 0.039(8) 0.193(18) 0.026(7) 0.008(8) 0.011(6) -0.047(9) C62 0.021(6) 0.055(8) 0.019(5) 0.005(5) 0.004(4) 0.001(5) C63 0.039(7) 0.072(10) 0.037(7) -0.016(6) 0.005(6) 0.001(6) C64 0.026(6) 0.049(8) 0.026(6) -0.013(5) 0.013(5) -0.013(5) C65 0.060(9) 0.069(10) 0.037(7) -0.002(6) 0.013(6) -0.032(7) C66 0.077(9) 0.045(9) 0.037(7) -0.006(6) 0.033(7) -0.004(6) C67 0.033(6) 0.035(8) 0.029(6) 0.003(5) 0.016(5) -0.001(5) C68 0.054(8) 0.043(9) 0.042(7) 0.016(6) 0.028(6) 0.014(6) C69 0.015(5) 0.009(6) 0.034(5) -0.002(4) 0.015(4) -0.005(4) C70 0.016(5) 0.015(6) 0.028(5) 0.006(4) 0.012(4) 0.005(4) C71 0.017(5) 0.025(7) 0.037(6) 0.014(5) 0.017(5) 0.010(4) C72 0.030(6) 0.018(7) 0.044(7) 0.002(5) 0.024(5) 0.002(4) C73 0.025(6) 0.024(7) 0.026(5) 0.002(4) 0.007(4) -0.003(4) C74 0.019(5) 0.010(6) 0.036(6) 0.000(4) 0.019(4) -0.005(4) C75 0.023(6) 0.032(7) 0.040(6) 0.004(5) 0.010(5) -0.005(5) C76 0.018(5) 0.027(7) 0.035(6) -0.007(5) 0.004(5) -0.013(4) C77 0.032(6) 0.054(9) 0.031(6) -0.006(5) 0.003(5) 0.005(5) C78 0.044(7) 0.050(9) 0.035(6) 0.003(6) 0.019(5) 0.024(6) C79 0.017(5) 0.022(6) 0.022(5) -0.005(4) 0.000(4) 0.008(4) C80 0.023(6) 0.048(8) 0.033(6) -0.012(5) -0.003(5) 0.003(5) C81 0.038(7) 0.052(9) 0.036(7) -0.007(6) -0.005(6) 0.016(6) C82 0.029(6) 0.041(8) 0.046(7) 0.025(6) 0.014(5) -0.001(5) C83 0.042(7) 0.044(8) 0.021(5) 0.013(5) 0.012(5) 0.006(5) C84 0.016(5) 0.028(7) 0.036(6) 0.004(5) 0.010(5) 0.001(4) C85 0.034(6) 0.014(7) 0.051(7) -0.001(5) 0.013(5) 0.002(4) C86 0.032(6) 0.029(7) 0.016(5) -0.010(4) 0.006(4) 0.002(5) C87 0.024(5) 0.033(7) 0.023(5) 0.003(5) 0.014(4) 0.009(4) C88 0.029(6) 0.033(7) 0.034(6) 0.002(5) 0.018(5) 0.006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O3 2.049(6) . ? Yb1 O2 2.063(6) . ? Yb1 O1 2.111(6) . ? Yb1 O7 2.386(6) . ? Yb1 O6 2.401(6) . ? Yb1 O4 2.447(5) . ? Yb2 O9 2.065(5) . ? Yb2 O8 2.068(6) . ? Yb2 O10 2.085(6) . ? Yb2 O14 2.395(7) . ? Yb2 O13 2.412(7) . ? Yb2 O12 2.441(6) . ? O2 C13 1.375(10) . ? O3 C25 1.353(11) . ? O1 C1 1.334(10) . ? O4 C37 1.429(9) . ? O4 C38 1.430(11) . ? O5 C39 1.315(12) . ? O5 C40 1.435(12) . ? O7 C44 1.439(10) . ? O7 C43 1.457(11) . ? O6 C41 1.449(9) . ? O6 C42 1.457(10) . ? O8 C45 1.335(11) . ? O9 C57 1.344(10) . ? O10 C69 1.332(10) . ? O11 C82 1.403(11) . ? O11 C81 1.408(12) . ? O12 C84 1.437(10) . ? O12 C83 1.458(11) . ? O13 C86 1.416(11) . ? O13 C85 1.433(10) . ? O14 C87 1.432(11) . ? O14 C88 1.443(11) . ? C13 C14 1.386(14) . ? C13 C18 1.433(13) . ? C18 C17 1.397(13) . ? C18 C22 1.521(14) . ? C17 C16 1.357(16) . ? C16 C15 1.384(15) . ? C15 C14 1.399(13) . ? C14 C19 1.510(13) . ? C23 C22 1.530(13) . ? C22 C24 1.508(15) . ? C20 C19 1.534(13) . ? C19 C21 1.557(14) . ? C25 C30 1.421(13) . ? C25 C26 1.422(13) . ? C26 C27 1.397(13) . ? C26 C31 1.506(12) . ? C27 C28 1.369(13) . ? C28 C29 1.389(13) . ? C29 C30 1.382(13) . ? C30 C34 1.520(12) . ? C35 C34 1.524(13) . ? C34 C36 1.521(11) . ? C33 C31 1.531(13) . ? C31 C32 1.534(12) . ? C1 C2 1.421(11) . ? C1 C6 1.425(11) . ? C6 C5 1.378(13) . ? C6 C10 1.525(12) . ? C5 C4 1.392(12) . ? C4 C3 1.367(11) . ? C3 C2 1.377(12) . ? C2 C7 1.529(11) . ? C11 C10 1.548(14) . ? C10 C12 1.542(11) . ? C8 C7 1.534(14) . ? C7 C9 1.540(13) . ? C38 C39 1.618(15) . ? C43 C42 1.472(13) . ? C45 C46 1.409(13) . ? C45 C50 1.425(13) . ? C46 C47 1.375(13) . ? C46 C55 1.525(13) . ? C47 C48 1.382(13) . ? C48 C49 1.367(12) . ? C49 C50 1.385(13) . ? C50 C52 1.496(13) . ? C51 C52 1.534(13) . ? C52 C53 1.541(11) . ? C54 C55 1.512(14) . ? C55 C56 1.527(14) . ? C57 C58 1.409(13) . ? C57 C62 1.421(14) . ? C58 C59 1.392(13) . ? C58 C64 1.487(14) . ? C59 C60 1.36(2) . ? C60 C61 1.417(19) . ? C61 C62 1.369(14) . ? C62 C67 1.488(14) . ? C63 C64 1.533(15) . ? C64 C65 1.524(14) . ? C66 C67 1.541(14) . ? C67 C68 1.542(14) . ? C69 C74 1.425(12) . ? C69 C70 1.429(11) . ? C70 C71 1.379(13) . ? C70 C79 1.517(12) . ? C71 C72 1.373(13) . ? C72 C73 1.377(12) . ? C73 C74 1.374(13) . ? C74 C76 1.524(12) . ? C75 C76 1.507(14) . ? C76 C77 1.548(13) . ? C78 C79 1.521(14) . ? C79 C80 1.522(11) . ? C82 C83 1.495(14) . ? C86 C87 1.528(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 O3 Yb1 O2 101.5(2) . . ? O3 Yb1 O1 109.1(2) . . ? O2 Yb1 O1 104.4(2) . . ? O3 Yb1 O7 153.7(2) . . ? O2 Yb1 O7 93.0(2) . . ? O1 Yb1 O7 88.0(2) . . ? O3 Yb1 O6 91.4(2) . . ? O2 Yb1 O6 86.1(2) . . ? O1 Yb1 O6 154.1(2) . . ? O7 Yb1 O6 67.6(2) . . ? O3 Yb1 O4 82.5(2) . . ? O2 Yb1 O4 162.1(2) . . ? O1 Yb1 O4 90.5(2) . . ? O7 Yb1 O4 77.4(2) . . ? O6 Yb1 O4 76.3(2) . . ? O9 Yb2 O8 101.7(2) . . ? O9 Yb2 O10 106.6(2) . . ? O8 Yb2 O10 108.3(2) . . ? O9 Yb2 O14 92.3(2) . . ? O8 Yb2 O14 155.8(2) . . ? O10 Yb2 O14 85.9(2) . . ? O9 Yb2 O13 84.7(2) . . ? O8 Yb2 O13 93.1(2) . . ? O10 Yb2 O13 152.6(2) . . ? O14 Yb2 O13 68.4(2) . . ? O9 Yb2 O12 162.3(2) . . ? O8 Yb2 O12 83.2(2) . . ? O10 Yb2 O12 87.6(2) . . ? O14 Yb2 O12 77.8(2) . . ? O13 Yb2 O12 78.0(2) . . ? C13 O2 Yb1 169.1(6) . . ? C25 O3 Yb1 165.1(5) . . ? C1 O1 Yb1 151.3(6) . . ? C37 O4 C38 113.6(6) . . ? C37 O4 Yb1 122.1(5) . . ? C38 O4 Yb1 124.1(5) . . ? C39 O5 C40 108.5(9) . . ? C44 O7 C43 112.0(7) . . ? C44 O7 Yb1 125.6(5) . . ? C43 O7 Yb1 119.7(5) . . ? C41 O6 C42 115.4(7) . . ? C41 O6 Yb1 117.2(5) . . ? C42 O6 Yb1 113.7(5) . . ? C45 O8 Yb2 164.0(5) . . ? C57 O9 Yb2 173.7(6) . . ? C69 O10 Yb2 149.8(6) . . ? C82 O11 C81 110.0(8) . . ? C84 O12 C83 111.5(7) . . ? C84 O12 Yb2 124.5(5) . . ? C83 O12 Yb2 124.0(6) . . ? C86 O13 C85 114.1(7) . . ? C86 O13 Yb2 112.5(5) . . ? C85 O13 Yb2 119.2(5) . . ? C87 O14 C88 112.0(8) . . ? C87 O14 Yb2 118.2(6) . . ? C88 O14 Yb2 125.9(5) . . ? O2 C13 C14 121.4(9) . . ? O2 C13 C18 117.7(9) . . ? C14 C13 C18 120.9(9) . . ? C17 C18 C13 117.3(10) . . ? C17 C18 C22 121.0(9) . . ? C13 C18 C22 121.8(8) . . ? C16 C17 C18 122.0(11) . . ? C17 C16 C15 120.1(11) . . ? C16 C15 C14 121.1(11) . . ? C13 C14 C15 118.5(9) . . ? C13 C14 C19 121.4(8) . . ? C15 C14 C19 119.9(10) . . ? C24 C22 C18 108.8(9) . . ? C24 C22 C23 109.2(9) . . ? C18 C22 C23 113.6(9) . . ? C14 C19 C20 111.1(9) . . ? C14 C19 C21 112.1(8) . . ? C20 C19 C21 107.0(9) . . ? O3 C25 C30 120.1(9) . . ? O3 C25 C26 120.0(9) . . ? C30 C25 C26 119.9(9) . . ? C27 C26 C25 118.1(9) . . ? C27 C26 C31 120.9(9) . . ? C25 C26 C31 120.8(9) . . ? C28 C27 C26 122.4(10) . . ? C27 C28 C29 118.8(10) . . ? C30 C29 C28 122.3(10) . . ? C29 C30 C25 118.4(9) . . ? C29 C30 C34 124.0(9) . . ? C25 C30 C34 117.5(9) . . ? C30 C34 C36 109.4(8) . . ? C30 C34 C35 113.4(8) . . ? C36 C34 C35 110.2(9) . . ? C26 C31 C33 112.9(7) . . ? C26 C31 C32 110.8(8) . . ? C33 C31 C32 110.0(9) . . ? O1 C1 C2 119.8(7) . . ? O1 C1 C6 120.9(7) . . ? C2 C1 C6 119.2(8) . . ? C5 C6 C1 119.8(8) . . ? C5 C6 C10 122.5(8) . . ? C1 C6 C10 117.6(8) . . ? C6 C5 C4 120.7(8) . . ? C3 C4 C5 118.7(9) . . ? C4 C3 C2 124.0(8) . . ? C3 C2 C1 117.4(7) . . ? C3 C2 C7 122.9(8) . . ? C1 C2 C7 119.6(8) . . ? C6 C10 C12 113.6(8) . . ? C6 C10 C11 109.3(8) . . ? C12 C10 C11 109.3(8) . . ? C2 C7 C8 109.7(8) . . ? C2 C7 C9 112.9(8) . . ? C8 C7 C9 109.4(8) . . ? O4 C38 C39 111.0(9) . . ? O5 C39 C38 112.3(9) . . ? O7 C43 C42 106.7(8) . . ? O6 C42 C43 109.8(7) . . ? O8 C45 C46 121.7(9) . . ? O8 C45 C50 118.6(9) . . ? C46 C45 C50 119.7(9) . . ? C47 C46 C45 120.0(9) . . ? C47 C46 C55 121.0(9) . . ? C45 C46 C55 119.0(9) . . ? C46 C47 C48 120.1(9) . . ? C49 C48 C47 120.4(10) . . ? C48 C49 C50 122.1(9) . . ? C49 C50 C45 117.5(9) . . ? C49 C50 C52 122.9(9) . . ? C45 C50 C52 119.5(9) . . ? C50 C52 C51 114.5(8) . . ? C50 C52 C53 110.9(7) . . ? C51 C52 C53 108.9(8) . . ? C54 C55 C46 109.5(9) . . ? C54 C55 C56 110.2(10) . . ? C46 C55 C56 111.9(9) . . ? O9 C57 C58 120.0(9) . . ? O9 C57 C62 120.4(9) . . ? C58 C57 C62 119.5(9) . . ? C59 C58 C57 118.5(11) . . ? C59 C58 C64 120.0(10) . . ? C57 C58 C64 121.5(9) . . ? C60 C59 C58 121.5(13) . . ? C59 C60 C61 121.0(15) . . ? C62 C61 C60 118.5(14) . . ? C61 C62 C57 120.8(10) . . ? C61 C62 C67 117.7(11) . . ? C57 C62 C67 121.4(8) . . ? C58 C64 C65 115.1(9) . . ? C58 C64 C63 111.1(10) . . ? C65 C64 C63 108.2(10) . . ? C62 C67 C66 112.7(9) . . ? C62 C67 C68 111.3(9) . . ? C66 C67 C68 107.6(10) . . ? O10 C69 C74 121.7(7) . . ? O10 C69 C70 121.1(8) . . ? C74 C69 C70 117.2(8) . . ? C71 C70 C69 119.0(8) . . ? C71 C70 C79 124.0(8) . . ? C69 C70 C79 116.9(8) . . ? C72 C71 C70 123.0(9) . . ? C71 C72 C73 118.6(10) . . ? C74 C73 C72 121.3(9) . . ? C73 C74 C69 120.8(8) . . ? C73 C74 C76 121.5(8) . . ? C69 C74 C76 117.7(8) . . ? C75 C76 C74 111.3(8) . . ? C75 C76 C77 110.9(8) . . ? C74 C76 C77 113.4(9) . . ? C70 C79 C78 111.5(8) . . ? C70 C79 C80 113.0(8) . . ? C78 C79 C80 111.2(8) . . ? O11 C82 C83 110.7(9) . . ? O12 C83 C82 112.1(9) . . ? O13 C86 C87 109.6(7) . . ? O14 C87 C86 106.0(8) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 1.577 _refine_diff_density_min -2.903 _refine_diff_density_rms 0.213 # Attachment '- Nd.tol.2b.CIF' data_D:\neodymium.CIF _database_code_depnum_ccdc_archive 'CCDC 845101' #TrackingRef '- Nd.tol.2b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Nd structure' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H83 Nd O6' _chemical_formula_weight 984.45 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9370(4) _cell_length_b 35.5722(15) _cell_length_c 13.3069(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.671(2) _cell_angle_gamma 90.00 _cell_volume 5151.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8579 _exptl_absorpt_correction_T_max 0.9492 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31755 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.61 _reflns_number_total 10651 _reflns_number_gt 7359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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. Carbon atom 39 suffers from slightly higher thermal motion than its neighbours as may be expected for a carbon on a THF molecule. ; _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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10651 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Nd1 Nd 0.04547(2) 0.854028(6) 0.498276(18) 0.01352(7) Uani 1 1 d . . . O1 O 0.1789(3) 0.81121(8) 0.5586(2) 0.0180(7) Uani 1 1 d . . . O2 O 0.1243(3) 0.90825(8) 0.5567(2) 0.0174(7) Uani 1 1 d . . . O3 O 0.0775(3) 0.85480(9) 0.3388(2) 0.0198(7) Uani 1 1 d . . . O4 O -0.1170(3) 0.80360(9) 0.4449(2) 0.0232(8) Uani 1 1 d . . . O5 O -0.1499(3) 0.89359(9) 0.4672(2) 0.0267(8) Uani 1 1 d . . . O6 O -0.0544(3) 0.84477(8) 0.6595(2) 0.0248(8) Uani 1 1 d . . . C1 C 0.2759(4) 0.78811(12) 0.5751(3) 0.0160(10) Uani 1 1 d . . . C2 C 0.3880(4) 0.80170(12) 0.6241(3) 0.0176(10) Uani 1 1 d . . . C3 C 0.4864(4) 0.77682(13) 0.6407(3) 0.0231(11) Uani 1 1 d . . . H3 H 0.5617 0.7857 0.6739 0.028 Uiso 1 1 calc R . . C4 C 0.4778(4) 0.73991(12) 0.6107(3) 0.0213(11) Uani 1 1 d . . . H4 H 0.5464 0.7236 0.6228 0.026 Uiso 1 1 calc R . . C5 C 0.3684(4) 0.72687(12) 0.5627(3) 0.0211(11) Uani 1 1 d . . . H5 H 0.3624 0.7013 0.5426 0.025 Uiso 1 1 calc R . . C6 C 0.2671(4) 0.75006(12) 0.5428(3) 0.0161(10) Uani 1 1 d . . . C7 C 0.5242(4) 0.85919(13) 0.6606(4) 0.0344(13) Uani 1 1 d . . . H7A H 0.5787 0.8474 0.7145 0.052 Uiso 1 1 calc R . . H7B H 0.5198 0.8863 0.6730 0.052 Uiso 1 1 calc R . . H7C H 0.5564 0.8548 0.5955 0.052 Uiso 1 1 calc R . . C8 C 0.3958(4) 0.84212(12) 0.6589(4) 0.0240(12) Uani 1 1 d . . . H8 H 0.3404 0.8571 0.6098 0.029 Uiso 1 1 calc R . . C9 C 0.3464(5) 0.84573(13) 0.7614(4) 0.0323(13) Uani 1 1 d . . . H9A H 0.2617 0.8364 0.7568 0.048 Uiso 1 1 calc R . . H9B H 0.3480 0.8722 0.7819 0.048 Uiso 1 1 calc R . . H9C H 0.3976 0.8309 0.8114 0.048 Uiso 1 1 calc R . . C10 C 0.0586(5) 0.72495(15) 0.5656(4) 0.0410(15) Uani 1 1 d . . . H10A H 0.0929 0.7038 0.6064 0.062 Uiso 1 1 calc R . . H10B H -0.0202 0.7175 0.5297 0.062 Uiso 1 1 calc R . . H10C H 0.0459 0.7464 0.6097 0.062 Uiso 1 1 calc R . . C11 C 0.1464(4) 0.73596(12) 0.4903(4) 0.0242(11) Uani 1 1 d . . . H11 H 0.1081 0.7574 0.4499 0.029 Uiso 1 1 calc R . . C12 C 0.1610(5) 0.70373(13) 0.4174(4) 0.0347(13) Uani 1 1 d . . . H12A H 0.1840 0.6808 0.4556 0.052 Uiso 1 1 calc R . . H12B H 0.2253 0.7100 0.3738 0.052 Uiso 1 1 calc R . . H12C H 0.0831 0.6996 0.3757 0.052 Uiso 1 1 calc R . . C13 C 0.2258(4) 0.92912(11) 0.5789(3) 0.0148(10) Uani 1 1 d . . . C14 C 0.2959(4) 0.94132(12) 0.5016(3) 0.0199(11) Uani 1 1 d . . . C15 C 0.4079(4) 0.95893(12) 0.5276(4) 0.0233(11) Uani 1 1 d . . . H15 H 0.4575 0.9661 0.4760 0.028 Uiso 1 1 calc R . . C16 C 0.4484(4) 0.96624(13) 0.6280(4) 0.0269(12) Uani 1 1 d . . . H16 H 0.5267 0.9773 0.6451 0.032 Uiso 1 1 calc R . . C17 C 0.3748(4) 0.95739(12) 0.7025(4) 0.0239(11) Uani 1 1 d . . . H17 H 0.4017 0.9634 0.7707 0.029 Uiso 1 1 calc R . . C18 C 0.2620(4) 0.93979(12) 0.6805(3) 0.0188(10) Uani 1 1 d . . . C19 C 0.3322(5) 0.93841(14) 0.3133(4) 0.0320(13) Uani 1 1 d . . . H19A H 0.2892 0.9330 0.2467 0.048 Uiso 1 1 calc R . . H19B H 0.3951 0.9192 0.3302 0.048 Uiso 1 1 calc R . . H19C H 0.3712 0.9632 0.3121 0.048 Uiso 1 1 calc R . . C20 C 0.2406(4) 0.93820(13) 0.3922(3) 0.0226(11) Uani 1 1 d . . . H20 H 0.1944 0.9139 0.3852 0.027 Uiso 1 1 calc R . . C21 C 0.1483(5) 0.96979(16) 0.3702(4) 0.0450(16) Uani 1 1 d . . . H21A H 0.1917 0.9939 0.3711 0.067 Uiso 1 1 calc R . . H21B H 0.0903 0.9699 0.4218 0.067 Uiso 1 1 calc R . . H21C H 0.1034 0.9659 0.3036 0.067 Uiso 1 1 calc R . . C22 C 0.2291(5) 0.93729(14) 0.8689(3) 0.0339(13) Uani 1 1 d . . . H22A H 0.3017 0.9211 0.8799 0.051 Uiso 1 1 calc R . . H22B H 0.1683 0.9296 0.9142 0.051 Uiso 1 1 calc R . . H22C H 0.2529 0.9635 0.8827 0.051 Uiso 1 1 calc R . . C23 C 0.1732(4) 0.93363(13) 0.7587(3) 0.0224(11) Uani 1 1 d . . . H23 H 0.1396 0.9076 0.7493 0.027 Uiso 1 1 calc R . . C24 C 0.0653(4) 0.96107(13) 0.7408(4) 0.0313(12) Uani 1 1 d . . . H24A H 0.0947 0.9868 0.7535 0.047 Uiso 1 1 calc R . . H24B H 0.0033 0.9550 0.7866 0.047 Uiso 1 1 calc R . . H24C H 0.0288 0.9589 0.6707 0.047 Uiso 1 1 calc R . . C25 C 0.1209(4) 0.85415(13) 0.2483(3) 0.0177(9) Uani 1 1 d . . . C26 C 0.2274(4) 0.83328(12) 0.2336(3) 0.0200(10) Uani 1 1 d . . . C27 C 0.2701(4) 0.83271(14) 0.1386(4) 0.0280(12) Uani 1 1 d . . . H27 H 0.3419 0.8187 0.1288 0.034 Uiso 1 1 calc R . . C28 C 0.2106(4) 0.85211(17) 0.0584(3) 0.0370(13) Uani 1 1 d . . . H28 H 0.2406 0.8514 -0.0062 0.044 Uiso 1 1 calc R . . C29 C 0.1074(5) 0.87246(14) 0.0733(4) 0.0308(13) Uani 1 1 d . . . H29 H 0.0665 0.8858 0.0179 0.037 Uiso 1 1 calc R . . C30 C 0.0609(4) 0.87427(12) 0.1657(3) 0.0206(11) Uani 1 1 d . . . C31 C -0.1691(4) 0.87531(14) 0.1409(4) 0.0358(14) Uani 1 1 d . . . H31A H -0.1682 0.8699 0.0688 0.054 Uiso 1 1 calc R . . H31B H -0.2417 0.8904 0.1513 0.054 Uiso 1 1 calc R . . H31C H -0.1719 0.8517 0.1784 0.054 Uiso 1 1 calc R . . C32 C -0.0531(4) 0.89706(12) 0.1787(3) 0.0245(11) Uani 1 1 d . . . H32 H -0.0557 0.9018 0.2526 0.029 Uiso 1 1 calc R . . C33 C -0.0552(5) 0.93512(13) 0.1257(4) 0.0417(15) Uani 1 1 d . . . H33A H 0.0223 0.9483 0.1447 0.062 Uiso 1 1 calc R . . H33B H -0.1237 0.9501 0.1460 0.062 Uiso 1 1 calc R . . H33C H -0.0654 0.9313 0.0524 0.062 Uiso 1 1 calc R . . C34 C 0.3495(5) 0.77480(13) 0.2895(4) 0.0380(14) Uani 1 1 d . . . H34A H 0.2854 0.7603 0.2502 0.057 Uiso 1 1 calc R . . H34B H 0.3800 0.7606 0.3499 0.057 Uiso 1 1 calc R . . H34C H 0.4173 0.7796 0.2483 0.057 Uiso 1 1 calc R . . C35 C 0.2962(4) 0.81221(12) 0.3209(3) 0.0202(10) Uani 1 1 d . . . H35 H 0.2362 0.8066 0.3709 0.024 Uiso 1 1 calc R . . C36 C 0.3979(5) 0.83640(14) 0.3743(4) 0.0353(14) Uani 1 1 d . . . H36A H 0.4540 0.8445 0.3255 0.053 Uiso 1 1 calc R . . H36B H 0.4435 0.8217 0.4279 0.053 Uiso 1 1 calc R . . H36C H 0.3616 0.8585 0.4038 0.053 Uiso 1 1 calc R . . C37 C -0.2127(5) 0.78698(14) 0.4991(4) 0.0321(13) Uani 1 1 d . . . H37A H -0.2676 0.8067 0.5217 0.039 Uiso 1 1 calc R . . H37B H -0.1761 0.7730 0.5590 0.039 Uiso 1 1 calc R . . C38 C -0.2836(6) 0.76055(17) 0.4253(4) 0.0497(17) Uani 1 1 d . . . H38A H -0.2658 0.7340 0.4440 0.060 Uiso 1 1 calc R . . H38B H -0.3731 0.7649 0.4243 0.060 Uiso 1 1 calc R . . C39 C -0.2419(7) 0.7691(2) 0.3285(5) 0.101(3) Uani 1 1 d . . . H39A H -0.3008 0.7863 0.2904 0.122 Uiso 1 1 calc R . . H39B H -0.2365 0.7458 0.2887 0.122 Uiso 1 1 calc R . . C40 C -0.1223(4) 0.78677(14) 0.3446(3) 0.0291(12) Uani 1 1 d . . . H40A H -0.1131 0.8062 0.2927 0.035 Uiso 1 1 calc R . . H40B H -0.0562 0.7679 0.3416 0.035 Uiso 1 1 calc R . . C41 C -0.2594(5) 0.88397(15) 0.4031(4) 0.0395(14) Uani 1 1 d . . . H41A H -0.3148 0.8684 0.4404 0.047 Uiso 1 1 calc R . . H41B H -0.2382 0.8698 0.3432 0.047 Uiso 1 1 calc R . . C42 C -0.3201(6) 0.92055(18) 0.3716(5) 0.075(3) Uani 1 1 d . . . H42A H -0.3429 0.9211 0.2978 0.090 Uiso 1 1 calc R . . H42B H -0.3950 0.9245 0.4064 0.090 Uiso 1 1 calc R . . C43 C -0.2259(6) 0.95003(18) 0.4021(5) 0.067(2) Uani 1 1 d . . . H43A H -0.1723 0.9548 0.3476 0.080 Uiso 1 1 calc R . . H43B H -0.2650 0.9739 0.4199 0.080 Uiso 1 1 calc R . . C44 C -0.1579(5) 0.93326(14) 0.4890(5) 0.0493(18) Uani 1 1 d . . . H44A H -0.2010 0.9373 0.5501 0.059 Uiso 1 1 calc R . . H44B H -0.0748 0.9444 0.5004 0.059 Uiso 1 1 calc R . . C45 C -0.0239(5) 0.81589(13) 0.7346(4) 0.0319(13) Uani 1 1 d . . . H45A H 0.0533 0.8029 0.7221 0.038 Uiso 1 1 calc R . . H45B H -0.0906 0.7970 0.7341 0.038 Uiso 1 1 calc R . . C46 C -0.0090(5) 0.83670(14) 0.8335(4) 0.0315(13) Uani 1 1 d . . . H46A H 0.0737 0.8481 0.8456 0.038 Uiso 1 1 calc R . . H46B H -0.0228 0.8199 0.8906 0.038 Uiso 1 1 calc R . . C47 C -0.1079(5) 0.86659(14) 0.8185(4) 0.0336(13) Uani 1 1 d . . . H47A H -0.0827 0.8897 0.8565 0.040 Uiso 1 1 calc R . . H47B H -0.1862 0.8574 0.8411 0.040 Uiso 1 1 calc R . . C48 C -0.1216(4) 0.87408(14) 0.7055(4) 0.0285(12) Uani 1 1 d . . . H48A H -0.2094 0.8735 0.6788 0.034 Uiso 1 1 calc R . . H48B H -0.0876 0.8991 0.6910 0.034 Uiso 1 1 calc R . . C49 C 0.6316(5) 0.94253(16) -0.0598(4) 0.0384(14) Uani 1 1 d . . . C50 C 0.6043(6) 0.96319(16) 0.0242(5) 0.0497(17) Uani 1 1 d . . . H50 H 0.6329 0.9883 0.0323 0.060 Uiso 1 1 calc R . . C51 C 0.5358(5) 0.94745(16) 0.0963(4) 0.0448(16) Uani 1 1 d . . . H51 H 0.5193 0.9618 0.1536 0.054 Uiso 1 1 calc R . . C52 C 0.4923(5) 0.91158(15) 0.0857(4) 0.0387(14) Uani 1 1 d . . . H52 H 0.4445 0.9010 0.1344 0.046 Uiso 1 1 calc R . . C53 C 0.5189(5) 0.89099(15) 0.0030(4) 0.0377(15) Uani 1 1 d . . . H53 H 0.4898 0.8659 -0.0051 0.045 Uiso 1 1 calc R . . C54 C 0.5873(5) 0.90652(16) -0.0679(4) 0.0365(14) Uani 1 1 d . . . H54 H 0.6043 0.8918 -0.1244 0.044 Uiso 1 1 calc R . . C55 C 0.7058(6) 0.95943(19) -0.1368(5) 0.065(2) Uani 1 1 d . . . H55A H 0.7929 0.9593 -0.1111 0.098 Uiso 1 1 calc R . . H55B H 0.6790 0.9854 -0.1505 0.098 Uiso 1 1 calc R . . H55C H 0.6942 0.9447 -0.1993 0.098 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 Nd1 0.01483(12) 0.01441(11) 0.01116(11) -0.00052(12) 0.00050(8) 0.00056(13) O1 0.0159(18) 0.0197(17) 0.0181(17) 0.0016(13) 0.0004(14) 0.0055(13) O2 0.0134(17) 0.0169(16) 0.0219(18) -0.0033(13) 0.0015(13) -0.0025(13) O3 0.0261(17) 0.0207(15) 0.0129(15) -0.0015(14) 0.0038(13) 0.0003(16) O4 0.024(2) 0.0298(19) 0.0167(18) -0.0087(14) 0.0044(14) -0.0071(15) O5 0.0210(19) 0.0270(19) 0.030(2) -0.0047(15) -0.0067(15) 0.0070(15) O6 0.037(2) 0.0208(19) 0.0182(17) -0.0002(13) 0.0131(15) 0.0004(14) C1 0.023(3) 0.017(2) 0.008(2) 0.0054(17) 0.0032(19) 0.002(2) C2 0.019(3) 0.018(2) 0.015(2) 0.0005(18) 0.000(2) 0.0021(19) C3 0.023(3) 0.029(3) 0.016(2) 0.001(2) -0.004(2) 0.004(2) C4 0.024(3) 0.019(3) 0.022(3) 0.005(2) 0.007(2) 0.010(2) C5 0.030(3) 0.017(2) 0.018(3) 0.0031(19) 0.012(2) 0.005(2) C6 0.017(3) 0.016(2) 0.016(2) 0.0047(18) 0.0058(19) -0.0021(19) C7 0.039(3) 0.025(3) 0.038(3) -0.004(2) -0.003(2) -0.004(2) C8 0.022(3) 0.019(2) 0.029(3) -0.0038(19) -0.006(2) 0.002(2) C9 0.032(3) 0.032(3) 0.032(3) -0.015(2) 0.001(2) 0.008(2) C10 0.039(4) 0.043(3) 0.043(4) -0.010(3) 0.015(3) -0.016(3) C11 0.027(3) 0.016(2) 0.029(3) -0.002(2) -0.001(2) -0.004(2) C12 0.039(3) 0.033(3) 0.033(3) -0.006(2) 0.007(3) -0.010(3) C13 0.015(3) 0.012(2) 0.017(2) 0.0004(18) 0.0010(19) 0.0024(18) C14 0.021(3) 0.014(2) 0.024(3) 0.000(2) -0.001(2) -0.001(2) C15 0.026(3) 0.023(3) 0.021(3) 0.006(2) 0.005(2) -0.001(2) C16 0.020(3) 0.023(3) 0.035(3) 0.005(2) -0.009(2) -0.008(2) C17 0.028(3) 0.022(3) 0.021(3) -0.001(2) -0.006(2) -0.001(2) C18 0.023(3) 0.015(2) 0.017(2) 0.0018(18) -0.002(2) 0.000(2) C19 0.035(3) 0.034(3) 0.028(3) 0.000(2) 0.009(2) -0.009(3) C20 0.026(3) 0.026(3) 0.016(2) -0.001(2) 0.005(2) -0.005(2) C21 0.046(4) 0.064(4) 0.024(3) 0.004(3) -0.001(3) 0.020(3) C22 0.043(3) 0.039(3) 0.019(3) -0.002(2) 0.003(2) 0.000(3) C23 0.030(3) 0.016(2) 0.020(3) 0.0005(19) 0.000(2) -0.001(2) C24 0.036(3) 0.028(3) 0.030(3) -0.003(2) 0.007(2) 0.005(2) C25 0.021(2) 0.015(2) 0.017(2) -0.004(2) 0.0033(18) -0.005(2) C26 0.024(3) 0.024(3) 0.013(2) 0.0006(19) 0.001(2) -0.006(2) C27 0.021(3) 0.044(3) 0.019(3) -0.002(2) 0.005(2) 0.006(2) C28 0.029(3) 0.069(4) 0.015(2) 0.004(3) 0.008(2) -0.003(3) C29 0.030(3) 0.048(3) 0.013(3) 0.005(2) 0.000(2) 0.004(3) C30 0.020(3) 0.024(3) 0.017(3) -0.003(2) 0.000(2) -0.001(2) C31 0.028(3) 0.044(3) 0.034(3) -0.008(3) -0.002(3) 0.011(3) C32 0.037(3) 0.023(3) 0.013(2) -0.0046(19) -0.003(2) 0.007(2) C33 0.066(4) 0.022(3) 0.035(3) 0.000(2) -0.002(3) 0.009(3) C34 0.052(4) 0.028(3) 0.037(3) 0.004(2) 0.015(3) 0.009(3) C35 0.019(3) 0.025(3) 0.017(2) 0.0036(19) 0.007(2) 0.002(2) C36 0.036(3) 0.035(3) 0.033(3) 0.010(2) -0.009(3) -0.002(2) C37 0.034(3) 0.043(3) 0.021(3) -0.004(2) 0.010(2) -0.017(3) C38 0.049(4) 0.053(4) 0.047(4) -0.010(3) 0.006(3) -0.028(3) C39 0.115(7) 0.145(8) 0.049(5) -0.051(5) 0.031(5) -0.106(6) C40 0.035(3) 0.036(3) 0.016(3) -0.010(2) -0.002(2) 0.002(2) C41 0.026(3) 0.051(4) 0.039(4) -0.007(3) -0.009(3) 0.003(3) C42 0.072(5) 0.070(5) 0.073(5) -0.035(4) -0.045(4) 0.044(4) C43 0.085(5) 0.052(4) 0.058(5) 0.008(3) -0.013(4) 0.033(4) C44 0.046(4) 0.028(3) 0.069(5) -0.008(3) -0.020(3) 0.016(3) C45 0.053(4) 0.017(3) 0.027(3) 0.004(2) 0.012(3) -0.002(2) C46 0.038(3) 0.040(3) 0.017(3) -0.003(2) 0.008(2) -0.003(3) C47 0.038(3) 0.042(3) 0.023(3) -0.005(2) 0.017(2) 0.002(3) C48 0.024(3) 0.040(3) 0.022(3) -0.008(2) 0.008(2) -0.001(2) C49 0.029(3) 0.047(4) 0.038(4) 0.011(3) -0.004(3) 0.006(3) C50 0.052(4) 0.029(3) 0.064(5) -0.004(3) -0.013(3) 0.000(3) C51 0.049(4) 0.043(4) 0.041(4) -0.018(3) -0.003(3) 0.016(3) C52 0.038(4) 0.044(4) 0.032(3) -0.005(3) -0.002(3) 0.007(3) C53 0.037(4) 0.035(3) 0.039(3) -0.006(3) -0.008(3) 0.002(3) C54 0.028(3) 0.047(4) 0.033(3) -0.007(3) -0.005(3) 0.005(3) C55 0.048(4) 0.079(5) 0.067(5) 0.031(4) 0.000(4) 0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.185(3) . ? Nd1 O1 2.205(3) . ? Nd1 O2 2.222(3) . ? Nd1 O6 2.523(3) . ? Nd1 O5 2.558(3) . ? Nd1 O4 2.575(3) . ? O1 C1 1.343(5) . ? O2 C13 1.344(5) . ? O3 C25 1.337(5) . ? O4 C37 1.454(5) . ? O4 C40 1.459(5) . ? O5 C41 1.442(5) . ? O5 C44 1.445(6) . ? O6 C48 1.446(5) . ? O6 C45 1.450(5) . ? C1 C2 1.416(6) . ? C1 C6 1.420(6) . ? C2 C3 1.394(6) . ? C2 C8 1.511(6) . ? C3 C4 1.373(6) . ? C4 C5 1.380(6) . ? C5 C6 1.386(6) . ? C6 C11 1.516(6) . ? C7 C8 1.528(6) . ? C8 C9 1.521(6) . ? C10 C11 1.507(7) . ? C11 C12 1.521(6) . ? C13 C14 1.410(6) . ? C13 C18 1.422(6) . ? C14 C15 1.389(6) . ? C14 C20 1.524(6) . ? C15 C16 1.391(6) . ? C16 C17 1.373(7) . ? C17 C18 1.389(6) . ? C18 C23 1.508(6) . ? C19 C20 1.521(6) . ? C20 C21 1.520(6) . ? C22 C23 1.538(6) . ? C23 C24 1.533(6) . ? C25 C26 1.411(6) . ? C25 C30 1.418(6) . ? C26 C27 1.391(6) . ? C26 C35 1.518(6) . ? C27 C28 1.379(6) . ? C28 C29 1.372(7) . ? C29 C30 1.378(6) . ? C30 C32 1.511(6) . ? C31 C32 1.528(6) . ? C32 C33 1.526(6) . ? C34 C35 1.528(6) . ? C35 C36 1.525(6) . ? C37 C38 1.516(6) . ? C38 C39 1.442(8) . ? C39 C40 1.448(7) . ? C41 C42 1.501(7) . ? C42 C43 1.498(9) . ? C43 C44 1.441(7) . ? C45 C46 1.504(6) . ? C46 C47 1.516(7) . ? C47 C48 1.520(6) . ? C49 C54 1.370(7) . ? C49 C50 1.394(8) . ? C49 C55 1.496(8) . ? C50 C51 1.392(8) . ? C51 C52 1.364(7) . ? C52 C53 1.376(7) . ? C53 C54 1.377(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O1 101.45(11) . . ? O3 Nd1 O2 103.60(11) . . ? O1 Nd1 O2 104.61(11) . . ? O3 Nd1 O6 162.13(10) . . ? O1 Nd1 O6 85.81(10) . . ? O2 Nd1 O6 90.08(10) . . ? O3 Nd1 O5 92.73(11) . . ? O1 Nd1 O5 162.01(11) . . ? O2 Nd1 O5 82.41(10) . . ? O6 Nd1 O5 77.54(10) . . ? O3 Nd1 O4 85.04(10) . . ? O1 Nd1 O4 91.90(10) . . ? O2 Nd1 O4 159.17(10) . . ? O6 Nd1 O4 78.36(10) . . ? O5 Nd1 O4 78.23(10) . . ? C1 O1 Nd1 165.0(3) . . ? C13 O2 Nd1 147.1(3) . . ? C25 O3 Nd1 168.3(3) . . ? C37 O4 C40 108.8(3) . . ? C37 O4 Nd1 131.1(3) . . ? C40 O4 Nd1 120.1(3) . . ? C41 O5 C44 106.7(4) . . ? C41 O5 Nd1 126.7(3) . . ? C44 O5 Nd1 124.9(3) . . ? C48 O6 C45 108.1(4) . . ? C48 O6 Nd1 123.2(3) . . ? C45 O6 Nd1 126.1(3) . . ? O1 C1 C2 120.0(4) . . ? O1 C1 C6 120.3(4) . . ? C2 C1 C6 119.6(4) . . ? C3 C2 C1 118.4(4) . . ? C3 C2 C8 122.4(4) . . ? C1 C2 C8 119.1(4) . . ? C4 C3 C2 122.1(4) . . ? C3 C4 C5 119.1(4) . . ? C4 C5 C6 121.9(4) . . ? C5 C6 C1 118.7(4) . . ? C5 C6 C11 122.3(4) . . ? C1 C6 C11 119.0(4) . . ? C2 C8 C9 109.9(4) . . ? C2 C8 C7 114.0(4) . . ? C9 C8 C7 111.1(4) . . ? C10 C11 C6 111.3(4) . . ? C10 C11 C12 110.0(4) . . ? C6 C11 C12 113.7(4) . . ? O2 C13 C14 120.4(4) . . ? O2 C13 C18 120.1(4) . . ? C14 C13 C18 119.4(4) . . ? C15 C14 C13 119.1(4) . . ? C15 C14 C20 121.8(4) . . ? C13 C14 C20 118.8(4) . . ? C14 C15 C16 120.9(5) . . ? C17 C16 C15 119.8(4) . . ? C16 C17 C18 121.5(4) . . ? C17 C18 C13 118.6(4) . . ? C17 C18 C23 122.6(4) . . ? C13 C18 C23 118.6(4) . . ? C21 C20 C19 109.5(4) . . ? C21 C20 C14 108.9(4) . . ? C19 C20 C14 115.7(4) . . ? C18 C23 C24 109.8(4) . . ? C18 C23 C22 115.1(4) . . ? C24 C23 C22 108.8(4) . . ? O3 C25 C26 120.4(4) . . ? O3 C25 C30 120.7(4) . . ? C26 C25 C30 118.9(4) . . ? C27 C26 C25 119.3(4) . . ? C27 C26 C35 120.2(4) . . ? C25 C26 C35 120.5(4) . . ? C28 C27 C26 121.4(5) . . ? C29 C28 C27 118.9(5) . . ? C28 C29 C30 122.4(4) . . ? C29 C30 C25 119.0(4) . . ? C29 C30 C32 120.6(4) . . ? C25 C30 C32 120.4(4) . . ? C30 C32 C33 113.4(4) . . ? C30 C32 C31 111.0(4) . . ? C33 C32 C31 108.9(4) . . ? C26 C35 C36 111.2(4) . . ? C26 C35 C34 113.2(4) . . ? C36 C35 C34 109.8(4) . . ? O4 C37 C38 106.2(4) . . ? C39 C38 C37 105.1(5) . . ? C38 C39 C40 108.7(5) . . ? C39 C40 O4 105.5(4) . . ? O5 C41 C42 106.1(4) . . ? C43 C42 C41 105.0(5) . . ? C44 C43 C42 102.3(5) . . ? C43 C44 O5 106.3(5) . . ? O6 C45 C46 104.6(4) . . ? C45 C46 C47 102.5(4) . . ? C46 C47 C48 104.6(4) . . ? O6 C48 C47 106.8(4) . . ? C54 C49 C50 117.1(6) . . ? C54 C49 C55 122.2(6) . . ? C50 C49 C55 120.7(6) . . ? C51 C50 C49 120.8(5) . . ? C52 C51 C50 120.7(6) . . ? C51 C52 C53 118.8(6) . . ? C52 C53 C54 120.4(5) . . ? C49 C54 C53 122.2(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.61 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.871 _refine_diff_density_min -1.377 _refine_diff_density_rms 0.114 # Attachment '- 11.dydme2.cif' data_dydme2.CIF _database_code_depnum_ccdc_archive 'CCDC 845102' #TrackingRef '- 11.dydme2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common refine _chemical_melting_point ? _chemical_formula_moiety 'C44 H71 Dy O7' _chemical_formula_sum 'C44 H71 Dy O7' _chemical_formula_weight 874.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.366(3) _cell_length_b 19.1880(10) _cell_length_c 16.638(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.624(7) _cell_angle_gamma 90.00 _cell_volume 4586.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 33363 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 27.12 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 1.673 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71200 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33363 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.12 _reflns_number_total 9554 _reflns_number_gt 8554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.0604P)^2^+7.5894P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_coef none _refine_ls_number_reflns 9554 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Dy1 Dy 0.480490(9) 0.204579(7) 0.290735(8) 0.01596(7) Uani 1 1 d . . . O1 O 0.53912(16) 0.17364(12) 0.40201(13) 0.0206(5) Uani 1 1 d . . . O2 O 0.54616(17) 0.30271(11) 0.27907(14) 0.0210(5) Uani 1 1 d . . . O3 O 0.33948(15) 0.23227(11) 0.31052(13) 0.0208(5) Uani 1 1 d . . . O4 O 0.44281(17) 0.07590(12) 0.28038(15) 0.0276(5) Uani 1 1 d . . . O5 O 0.6051(2) -0.01131(15) 0.2664(2) 0.0453(7) Uani 1 1 d . . . O6 O 0.42995(19) 0.19185(14) 0.14932(15) 0.0296(5) Uani 1 1 d . . . O7 O 0.60231(17) 0.16634(14) 0.19738(15) 0.0303(5) Uani 1 1 d . . . C1 C 0.5675(2) 0.17155(16) 0.47866(18) 0.0190(6) Uani 1 1 d . . . C2 C 0.5128(3) 0.20259(16) 0.5394(2) 0.0239(7) Uani 1 1 d . . . C3 C 0.5470(3) 0.20417(17) 0.6178(2) 0.0283(8) Uani 1 1 d . . . H3 H 0.5116 0.2266 0.6582 0.034 Uiso 1 1 calc R . . C4 C 0.6318(3) 0.1736(2) 0.6387(2) 0.0297(8) Uani 1 1 d . . . H4 H 0.6544 0.1757 0.6925 0.036 Uiso 1 1 calc R . . C5 C 0.6825(2) 0.14014(18) 0.5801(2) 0.0270(7) Uani 1 1 d . . . H5 H 0.7394 0.1180 0.5946 0.032 Uiso 1 1 calc R . . C6 C 0.6523(2) 0.13801(17) 0.49984(19) 0.0218(6) Uani 1 1 d . . . C7 C 0.4162(3) 0.2289(2) 0.5160(2) 0.0288(7) Uani 1 1 d . . . H7 H 0.4220 0.2551 0.4643 0.035 Uiso 1 1 calc R . . C8 C 0.3515(3) 0.1661(2) 0.5002(2) 0.0356(9) Uani 1 1 d . . . H8A H 0.3793 0.1357 0.4597 0.053 Uiso 1 1 calc R . . H8B H 0.2909 0.1827 0.4808 0.053 Uiso 1 1 calc R . . H8C H 0.3434 0.1399 0.5503 0.053 Uiso 1 1 calc R . . C9 C 0.3721(4) 0.2779(3) 0.5770(3) 0.0497(12) Uani 1 1 d . . . H9A H 0.3587 0.2521 0.6264 0.075 Uiso 1 1 calc R . . H9B H 0.3140 0.2968 0.5545 0.075 Uiso 1 1 calc R . . H9C H 0.4151 0.3162 0.5892 0.075 Uiso 1 1 calc R . . C10 C 0.7087(2) 0.10160(18) 0.4362(2) 0.0255(7) Uani 1 1 d . . . H10 H 0.6720 0.1038 0.3848 0.031 Uiso 1 1 calc R . . C11 C 0.8021(3) 0.1377(2) 0.4214(3) 0.0378(9) Uani 1 1 d . . . H11A H 0.7912 0.1864 0.4065 0.057 Uiso 1 1 calc R . . H11B H 0.8345 0.1139 0.3777 0.057 Uiso 1 1 calc R . . H11C H 0.8404 0.1357 0.4705 0.057 Uiso 1 1 calc R . . C12 C 0.7239(3) 0.0244(2) 0.4560(3) 0.0409(10) Uani 1 1 d . . . H12A H 0.7643 0.0203 0.5037 0.061 Uiso 1 1 calc R . . H12B H 0.7534 0.0012 0.4104 0.061 Uiso 1 1 calc R . . H12C H 0.6638 0.0023 0.4667 0.061 Uiso 1 1 calc R . . C13 C 0.5654(2) 0.37054(16) 0.28256(19) 0.0200(6) Uani 1 1 d . . . C14 C 0.5631(2) 0.41108(17) 0.21143(19) 0.0203(6) Uani 1 1 d . . . C15 C 0.5777(2) 0.48264(18) 0.2170(2) 0.0258(7) Uani 1 1 d . . . H15 H 0.5760 0.5101 0.1695 0.031 Uiso 1 1 calc R . . C16 C 0.5949(3) 0.51476(18) 0.2904(2) 0.0304(8) Uani 1 1 d . . . H16 H 0.6026 0.5639 0.2933 0.036 Uiso 1 1 calc R . . C17 C 0.6006(3) 0.47460(18) 0.3592(2) 0.0290(7) Uani 1 1 d . . . H17 H 0.6144 0.4964 0.4092 0.035 Uiso 1 1 calc R . . C18 C 0.5865(2) 0.40262(17) 0.3568(2) 0.0238(7) Uani 1 1 d . . . C19 C 0.5458(2) 0.37487(17) 0.13205(19) 0.0217(6) Uani 1 1 d . . . H19 H 0.4983 0.3377 0.1415 0.026 Uiso 1 1 calc R . . C20 C 0.6351(3) 0.3385(2) 0.1039(2) 0.0339(8) Uani 1 1 d . . . H20A H 0.6837 0.3734 0.0950 0.051 Uiso 1 1 calc R . . H20B H 0.6223 0.3134 0.0537 0.051 Uiso 1 1 calc R . . H20C H 0.6562 0.3054 0.1452 0.051 Uiso 1 1 calc R . . C21 C 0.5074(3) 0.4222(2) 0.0661(2) 0.0360(9) Uani 1 1 d . . . H21A H 0.4507 0.4451 0.0848 0.054 Uiso 1 1 calc R . . H21B H 0.4929 0.3943 0.0182 0.054 Uiso 1 1 calc R . . H21C H 0.5539 0.4576 0.0528 0.054 Uiso 1 1 calc R . . C22 C 0.5970(3) 0.35664(18) 0.4305(2) 0.0319(8) Uani 1 1 d . . . H22 H 0.5482 0.3196 0.4267 0.038 Uiso 1 1 calc R . . C23 C 0.6923(3) 0.3201(2) 0.4284(3) 0.0466(11) Uani 1 1 d . . . H23A H 0.6963 0.2917 0.3796 0.070 Uiso 1 1 calc R . . H23B H 0.6993 0.2901 0.4758 0.070 Uiso 1 1 calc R . . H23C H 0.7418 0.3552 0.4285 0.070 Uiso 1 1 calc R . . C24 C 0.5838(4) 0.3943(2) 0.5101(2) 0.0544(13) Uani 1 1 d . . . H24A H 0.6347 0.4276 0.5185 0.082 Uiso 1 1 calc R . . H24B H 0.5838 0.3603 0.5540 0.082 Uiso 1 1 calc R . . H24C H 0.5243 0.4193 0.5089 0.082 Uiso 1 1 calc R . . C25 C 0.2562(2) 0.25508(16) 0.33435(17) 0.0181(6) Uani 1 1 d . . . C26 C 0.1787(3) 0.20957(17) 0.3356(2) 0.0221(7) Uani 1 1 d . . . C27 C 0.0924(2) 0.2347(2) 0.3585(2) 0.0288(7) Uani 1 1 d . . . H27 H 0.0403 0.2041 0.3585 0.035 Uiso 1 1 calc R . . C28 C 0.0809(3) 0.3041(2) 0.3816(2) 0.0327(8) Uani 1 1 d . . . H28 H 0.0213 0.3210 0.3965 0.039 Uiso 1 1 calc R . . C29 C 0.1572(3) 0.34794(18) 0.3824(2) 0.0272(7) Uani 1 1 d . . . H29 H 0.1495 0.3948 0.3994 0.033 Uiso 1 1 calc R . . C30 C 0.2451(2) 0.32537(17) 0.35906(18) 0.0212(6) Uani 1 1 d . . . C31 C 0.1899(2) 0.13418(17) 0.3090(2) 0.0240(7) Uani 1 1 d . . . H31 H 0.2581 0.1245 0.3046 0.029 Uiso 1 1 calc R . . C32 C 0.1458(3) 0.1230(2) 0.2260(2) 0.0360(9) Uani 1 1 d . . . H32A H 0.0784 0.1307 0.2289 0.054 Uiso 1 1 calc R . . H32B H 0.1577 0.0752 0.2081 0.054 Uiso 1 1 calc R . . H32C H 0.1728 0.1559 0.1877 0.054 Uiso 1 1 calc R . . C33 C 0.1496(3) 0.0823(2) 0.3689(2) 0.0400(10) Uani 1 1 d . . . H33A H 0.1777 0.0901 0.4221 0.060 Uiso 1 1 calc R . . H33B H 0.1631 0.0347 0.3512 0.060 Uiso 1 1 calc R . . H33C H 0.0820 0.0888 0.3719 0.060 Uiso 1 1 calc R . . C34 C 0.3270(3) 0.37484(17) 0.3530(2) 0.0272(7) Uani 1 1 d . . . H34 H 0.3848 0.3473 0.3643 0.033 Uiso 1 1 calc R . . C35 C 0.3335(2) 0.40265(19) 0.2673(2) 0.0302(8) Uani 1 1 d . . . H35A H 0.3417 0.3636 0.2300 0.045 Uiso 1 1 calc R . . H35B H 0.3867 0.4344 0.2634 0.045 Uiso 1 1 calc R . . H35C H 0.2761 0.4278 0.2533 0.045 Uiso 1 1 calc R . . C36 C 0.3255(3) 0.4354(2) 0.4119(3) 0.0427(10) Uani 1 1 d . . . H36A H 0.2740 0.4669 0.3979 0.064 Uiso 1 1 calc R . . H36B H 0.3845 0.4609 0.4093 0.064 Uiso 1 1 calc R . . H36C H 0.3169 0.4176 0.4665 0.064 Uiso 1 1 calc R . . C37 C 0.6619(4) -0.0680(3) 0.2403(4) 0.0590(13) Uani 1 1 d . . . H37A H 0.6816 -0.0958 0.2869 0.088 Uiso 1 1 calc R . . H37B H 0.7169 -0.0497 0.2131 0.088 Uiso 1 1 calc R . . H37C H 0.6261 -0.0974 0.2029 0.088 Uiso 1 1 calc R . . C38 C 0.5255(3) -0.0359(2) 0.3078(3) 0.0399(9) Uani 1 1 d . . . H38A H 0.5450 -0.0665 0.3528 0.048 Uiso 1 1 calc R . . H38B H 0.4853 -0.0632 0.2708 0.048 Uiso 1 1 calc R . . C39 C 0.4722(3) 0.0261(2) 0.3399(3) 0.0376(9) Uani 1 1 d . . . H39A H 0.4165 0.0087 0.3681 0.045 Uiso 1 1 calc R . . H39B H 0.5119 0.0503 0.3802 0.045 Uiso 1 1 calc R . . C40 C 0.3792(3) 0.0436(2) 0.2226(3) 0.0375(9) Uani 1 1 d . . . H40A H 0.4137 0.0111 0.1887 0.056 Uiso 1 1 calc R . . H40B H 0.3505 0.0797 0.1889 0.056 Uiso 1 1 calc R . . H40C H 0.3306 0.0183 0.2515 0.056 Uiso 1 1 calc R . . C41 C 0.3481(3) 0.2248(2) 0.1164(3) 0.0420(10) Uani 1 1 d . . . H41A H 0.3664 0.2649 0.0838 0.063 Uiso 1 1 calc R . . H41B H 0.3083 0.2405 0.1603 0.063 Uiso 1 1 calc R . . H41C H 0.3138 0.1914 0.0828 0.063 Uiso 1 1 calc R . . C42 C 0.4958(3) 0.1739(2) 0.0889(2) 0.0425(10) Uani 1 1 d . . . H42A H 0.5215 0.2169 0.0648 0.051 Uiso 1 1 calc R . . H42B H 0.4646 0.1468 0.0458 0.051 Uiso 1 1 calc R . . C43 C 0.5734(3) 0.1316(2) 0.1255(3) 0.0448(10) Uani 1 1 d . . . H43A H 0.5514 0.0839 0.1380 0.054 Uiso 1 1 calc R . . H43B H 0.6260 0.1281 0.0877 0.054 Uiso 1 1 calc R . . C44 C 0.6946(3) 0.1491(2) 0.2227(3) 0.0393(9) Uani 1 1 d . . . H44A H 0.6976 0.0995 0.2364 0.059 Uiso 1 1 calc R . . H44B H 0.7115 0.1770 0.2700 0.059 Uiso 1 1 calc R . . H44C H 0.7379 0.1591 0.1791 0.059 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 Dy1 0.01841(10) 0.01361(9) 0.01573(9) 0.00121(5) -0.00546(6) -0.00019(5) O1 0.0240(11) 0.0214(11) 0.0163(10) 0.0063(9) -0.0084(8) 0.0042(9) O2 0.0266(12) 0.0148(10) 0.0215(11) 0.0016(8) -0.0060(9) -0.0054(9) O3 0.0201(11) 0.0172(10) 0.0249(11) 0.0038(9) -0.0078(9) 0.0022(9) O4 0.0289(13) 0.0162(11) 0.0376(14) 0.0023(10) -0.0034(10) -0.0041(10) O5 0.0396(16) 0.0305(15) 0.066(2) -0.0015(14) 0.0049(14) 0.0004(13) O6 0.0327(14) 0.0353(13) 0.0205(12) 0.0025(10) -0.0075(10) -0.0044(11) O7 0.0293(13) 0.0301(13) 0.0315(13) -0.0060(11) 0.0026(10) -0.0014(11) C1 0.0239(15) 0.0141(13) 0.0189(14) 0.0026(11) -0.0072(12) -0.0016(12) C2 0.0263(17) 0.0217(16) 0.0238(17) 0.0038(12) -0.0014(13) 0.0013(13) C3 0.036(2) 0.0254(17) 0.0237(17) -0.0015(13) 0.0004(15) -0.0032(14) C4 0.0346(19) 0.0341(19) 0.0201(16) 0.0010(14) -0.0117(14) -0.0031(16) C5 0.0277(17) 0.0270(17) 0.0259(17) 0.0009(13) -0.0135(13) -0.0016(14) C6 0.0242(16) 0.0195(14) 0.0216(15) 0.0032(12) -0.0090(12) 0.0007(13) C7 0.0312(18) 0.0334(19) 0.0218(16) 0.0030(14) 0.0021(14) 0.0112(16) C8 0.0248(18) 0.050(2) 0.0320(19) 0.0150(17) -0.0004(14) -0.0015(17) C9 0.055(3) 0.053(3) 0.040(2) -0.003(2) 0.007(2) 0.025(2) C10 0.0258(16) 0.0228(16) 0.0277(17) -0.0001(13) -0.0091(13) 0.0069(13) C11 0.0282(19) 0.039(2) 0.046(2) -0.0074(18) 0.0001(16) 0.0028(17) C12 0.056(3) 0.0269(19) 0.040(2) 0.0014(16) -0.0055(19) 0.0143(18) C13 0.0219(15) 0.0168(14) 0.0211(15) 0.0000(11) -0.0039(12) 0.0019(12) C14 0.0152(14) 0.0207(15) 0.0249(16) 0.0056(12) -0.0021(11) -0.0005(12) C15 0.0222(16) 0.0231(16) 0.0320(18) 0.0098(14) -0.0017(13) -0.0013(13) C16 0.0290(18) 0.0158(15) 0.046(2) 0.0030(14) -0.0027(15) -0.0027(14) C17 0.0324(18) 0.0188(15) 0.0356(19) -0.0037(14) -0.0077(15) -0.0023(14) C18 0.0272(17) 0.0192(15) 0.0249(16) 0.0006(12) -0.0081(13) -0.0042(13) C19 0.0177(14) 0.0265(16) 0.0209(15) 0.0021(13) -0.0015(11) -0.0004(13) C20 0.0293(19) 0.040(2) 0.0323(19) -0.0016(16) 0.0045(15) 0.0043(16) C21 0.038(2) 0.042(2) 0.0277(18) 0.0091(16) -0.0071(15) 0.0010(18) C22 0.049(2) 0.0205(16) 0.0258(17) 0.0010(14) -0.0145(16) -0.0041(16) C23 0.051(3) 0.036(2) 0.052(3) 0.012(2) -0.027(2) -0.003(2) C24 0.102(4) 0.036(2) 0.025(2) -0.0015(17) -0.014(2) -0.005(3) C25 0.0217(15) 0.0188(14) 0.0136(13) 0.0026(11) -0.0053(11) 0.0033(12) C26 0.0252(17) 0.0234(16) 0.0175(15) 0.0015(12) -0.0069(12) -0.0017(13) C27 0.0238(17) 0.0348(19) 0.0278(17) 0.0061(15) -0.0003(13) -0.0027(15) C28 0.0294(19) 0.038(2) 0.0310(19) 0.0034(15) 0.0064(15) 0.0094(16) C29 0.0357(19) 0.0229(16) 0.0231(16) 0.0001(13) -0.0009(14) 0.0083(14) C30 0.0272(16) 0.0188(15) 0.0175(14) 0.0012(12) -0.0080(12) 0.0009(13) C31 0.0273(16) 0.0212(15) 0.0235(16) 0.0002(12) -0.0052(13) -0.0065(13) C32 0.051(2) 0.0318(19) 0.0251(18) -0.0026(15) -0.0126(16) -0.0068(18) C33 0.065(3) 0.0262(18) 0.0292(19) 0.0050(15) 0.0001(18) -0.0078(19) C34 0.0323(18) 0.0161(15) 0.0329(18) -0.0013(13) -0.0102(14) -0.0002(13) C35 0.0238(17) 0.0240(17) 0.043(2) 0.0089(15) -0.0033(15) -0.0003(14) C36 0.059(3) 0.0238(18) 0.045(2) -0.0122(17) -0.014(2) -0.0058(18) C37 0.046(3) 0.049(3) 0.082(4) -0.014(3) 0.002(3) 0.011(2) C38 0.045(2) 0.0234(18) 0.051(2) 0.0060(17) -0.0054(19) -0.0037(17) C39 0.041(2) 0.0242(18) 0.048(2) 0.0056(16) -0.0049(18) -0.0060(16) C40 0.044(2) 0.0238(17) 0.045(2) -0.0083(16) -0.0065(18) -0.0066(16) C41 0.042(2) 0.046(2) 0.038(2) 0.0047(19) -0.0233(18) 0.001(2) C42 0.053(3) 0.046(2) 0.028(2) -0.0012(18) 0.0038(18) -0.010(2) C43 0.050(3) 0.049(3) 0.035(2) -0.0117(19) 0.0093(18) -0.007(2) C44 0.0297(19) 0.046(2) 0.042(2) 0.0121(18) 0.0074(16) 0.0026(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.111(2) . ? Dy1 O2 2.116(2) . ? Dy1 O3 2.123(2) . ? Dy1 O7 2.464(2) . ? Dy1 O6 2.467(2) . ? Dy1 O4 2.533(2) . ? O1 C1 1.335(4) . ? O2 C13 1.332(4) . ? O3 C25 1.338(4) . ? O4 C39 1.437(5) . ? O4 C40 1.457(4) . ? O5 C38 1.422(5) . ? O5 C37 1.431(5) . ? O6 C42 1.430(5) . ? O6 C41 1.438(5) . ? O7 C44 1.425(5) . ? O7 C43 1.427(5) . ? C1 C2 1.418(5) . ? C1 C6 1.419(4) . ? C2 C3 1.389(5) . ? C2 C7 1.524(5) . ? C3 C4 1.393(5) . ? C4 C5 1.382(5) . ? C5 C6 1.399(4) . ? C6 C10 1.511(5) . ? C7 C9 1.526(5) . ? C7 C8 1.544(6) . ? C10 C11 1.532(5) . ? C10 C12 1.533(5) . ? C13 C18 1.410(4) . ? C13 C14 1.416(4) . ? C14 C15 1.392(5) . ? C14 C19 1.510(4) . ? C15 C16 1.387(5) . ? C16 C17 1.382(5) . ? C17 C18 1.396(5) . ? C18 C22 1.517(5) . ? C19 C21 1.523(5) . ? C19 C20 1.538(5) . ? C22 C24 1.522(5) . ? C22 C23 1.538(6) . ? C25 C26 1.415(5) . ? C25 C30 1.420(4) . ? C26 C27 1.388(5) . ? C26 C31 1.522(4) . ? C27 C28 1.397(5) . ? C28 C29 1.382(6) . ? C29 C30 1.395(5) . ? C30 C34 1.516(5) . ? C31 C33 1.528(5) . ? C31 C32 1.530(5) . ? C34 C36 1.521(5) . ? C34 C35 1.527(5) . ? C38 C39 1.515(6) . ? C42 C43 1.503(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O2 99.01(9) . . ? O1 Dy1 O3 107.86(9) . . ? O2 Dy1 O3 102.63(9) . . ? O1 Dy1 O7 100.94(9) . . ? O2 Dy1 O7 83.50(9) . . ? O3 Dy1 O7 149.03(8) . . ? O1 Dy1 O6 156.81(9) . . ? O2 Dy1 O6 97.32(9) . . ? O3 Dy1 O6 84.33(9) . . ? O7 Dy1 O6 64.73(9) . . ? O1 Dy1 O4 82.44(8) . . ? O2 Dy1 O4 163.00(9) . . ? O3 Dy1 O4 92.92(8) . . ? O7 Dy1 O4 79.61(8) . . ? O6 Dy1 O4 77.19(8) . . ? C1 O1 Dy1 163.9(2) . . ? C13 O2 Dy1 163.4(2) . . ? C25 O3 Dy1 170.2(2) . . ? C39 O4 C40 110.4(3) . . ? C39 O4 Dy1 122.7(2) . . ? C40 O4 Dy1 126.3(2) . . ? C38 O5 C37 111.1(3) . . ? C42 O6 C41 112.5(3) . . ? C42 O6 Dy1 120.3(2) . . ? C41 O6 Dy1 123.4(2) . . ? C44 O7 C43 113.6(3) . . ? C44 O7 Dy1 123.2(2) . . ? C43 O7 Dy1 117.7(2) . . ? O1 C1 C2 120.1(3) . . ? O1 C1 C6 120.2(3) . . ? C2 C1 C6 119.7(3) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 C7 122.9(3) . . ? C1 C2 C7 117.9(3) . . ? C2 C3 C4 121.6(3) . . ? C5 C4 C3 119.1(3) . . ? C4 C5 C6 121.7(3) . . ? C5 C6 C1 118.7(3) . . ? C5 C6 C10 121.3(3) . . ? C1 C6 C10 120.0(3) . . ? C2 C7 C9 114.8(3) . . ? C2 C7 C8 109.2(3) . . ? C9 C7 C8 109.9(4) . . ? C6 C10 C11 112.4(3) . . ? C6 C10 C12 111.8(3) . . ? C11 C10 C12 110.4(3) . . ? O2 C13 C18 120.5(3) . . ? O2 C13 C14 119.8(3) . . ? C18 C13 C14 119.7(3) . . ? C15 C14 C13 118.9(3) . . ? C15 C14 C19 122.4(3) . . ? C13 C14 C19 118.7(3) . . ? C16 C15 C14 121.5(3) . . ? C17 C16 C15 119.4(3) . . ? C16 C17 C18 121.3(3) . . ? C17 C18 C13 119.2(3) . . ? C17 C18 C22 122.6(3) . . ? C13 C18 C22 118.2(3) . . ? C14 C19 C21 114.3(3) . . ? C14 C19 C20 110.2(3) . . ? C21 C19 C20 110.4(3) . . ? C18 C22 C24 114.5(3) . . ? C18 C22 C23 109.1(3) . . ? C24 C22 C23 110.8(4) . . ? O3 C25 C26 120.5(3) . . ? O3 C25 C30 120.0(3) . . ? C26 C25 C30 119.4(3) . . ? C27 C26 C25 119.7(3) . . ? C27 C26 C31 120.5(3) . . ? C25 C26 C31 119.8(3) . . ? C26 C27 C28 121.0(3) . . ? C29 C28 C27 119.2(3) . . ? C28 C29 C30 122.0(3) . . ? C29 C30 C25 118.7(3) . . ? C29 C30 C34 122.0(3) . . ? C25 C30 C34 119.1(3) . . ? C26 C31 C33 112.9(3) . . ? C26 C31 C32 110.6(3) . . ? C33 C31 C32 109.9(3) . . ? C30 C34 C36 114.8(3) . . ? C30 C34 C35 109.6(3) . . ? C36 C34 C35 109.7(3) . . ? O5 C38 C39 108.9(3) . . ? O4 C39 C38 115.1(4) . . ? O6 C42 C43 109.8(3) . . ? O7 C43 C42 107.1(3) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.155 _refine_diff_density_min -1.916 _refine_diff_density_rms 0.116 # Attachment '- 9.euIIlast2.CIF' data_euIIlast2.CIF _database_code_depnum_ccdc_archive 'CCDC 845103' #TrackingRef '- 9.euIIlast2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common EuII _chemical_melting_point ? _chemical_formula_moiety 'C64 H100 Eu2 O8' _chemical_formula_sum 'C64 H100 Eu2 O8' _chemical_formula_weight 1301.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 20.135(10) _cell_length_b 14.588(7) _cell_length_c 22.125(12) _cell_angle_alpha 90.00 _cell_angle_beta 100.403(11) _cell_angle_gamma 90.00 _cell_volume 6392(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 55115 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 1.994 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7959 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55115 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14641 _reflns_number_gt 9461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14641 _refine_ls_number_parameters 702 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.113 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.249406(12) 0.062495(16) 0.237285(10) 0.03444(7) Uani 1 1 d . . . Eu2 Eu 0.258039(13) -0.146380(17) 0.129511(11) 0.04207(8) Uani 1 1 d . A . O1 O 0.31888(15) -0.0114(2) 0.17175(14) 0.0392(7) Uani 1 1 d . . . O2 O 0.18945(16) -0.0797(2) 0.20232(13) 0.0415(8) Uani 1 1 d . . . O3 O 0.32199(16) -0.2358(2) 0.07856(14) 0.0432(8) Uani 1 1 d . . . O4 O 0.21213(18) 0.2019(2) 0.19791(15) 0.0545(9) Uani 1 1 d . . . O5 O 0.34527(17) 0.0976(2) 0.32485(14) 0.0466(8) Uani 1 1 d . . . O6 O 0.16621(18) 0.0795(3) 0.31382(17) 0.0628(11) Uani 1 1 d . . . O7 O 0.2111(3) -0.0605(3) 0.03425(18) 0.0862(15) Uani 1 1 d . . . O8 O 0.16270(19) -0.2642(3) 0.09048(19) 0.0688(11) Uani 1 1 d . . . C1 C 0.3842(2) 0.0122(3) 0.17781(18) 0.0299(10) Uani 1 1 d . . . C2 C 0.4350(2) -0.0430(3) 0.21165(19) 0.0339(10) Uani 1 1 d . . . C3 C 0.5017(2) -0.0163(3) 0.2173(2) 0.0417(11) Uani 1 1 d . . . H3 H 0.5360 -0.0538 0.2399 0.050 Uiso 1 1 calc R . . C4 C 0.5195(3) 0.0633(4) 0.1911(2) 0.0473(13) Uani 1 1 d . . . H4 H 0.5656 0.0807 0.1957 0.057 Uiso 1 1 calc R . . C5 C 0.4702(3) 0.1174(3) 0.1584(2) 0.0411(12) Uani 1 1 d . . . H5 H 0.4828 0.1723 0.1403 0.049 Uiso 1 1 calc R . . C6 C 0.4023(2) 0.0944(3) 0.15096(19) 0.0340(10) Uani 1 1 d . . . C7 C 0.4474(3) -0.2158(4) 0.2154(3) 0.0661(17) Uani 1 1 d . . . H7A H 0.4291 -0.2204 0.1713 0.099 Uiso 1 1 calc R . . H7B H 0.4357 -0.2711 0.2363 0.099 Uiso 1 1 calc R . . H7C H 0.4966 -0.2097 0.2215 0.099 Uiso 1 1 calc R . . C8 C 0.4172(3) -0.1313(3) 0.2420(2) 0.0464(12) Uani 1 1 d . . . H8 H 0.3670 -0.1379 0.2331 0.056 Uiso 1 1 calc R . . C9 C 0.4395(3) -0.1281(4) 0.3121(2) 0.0673(17) Uani 1 1 d . . . H9A H 0.4887 -0.1227 0.3223 0.101 Uiso 1 1 calc R . . H9B H 0.4252 -0.1845 0.3302 0.101 Uiso 1 1 calc R . . H9C H 0.4187 -0.0752 0.3286 0.101 Uiso 1 1 calc R . . C10 C 0.3507(3) 0.1458(5) 0.0453(2) 0.085(2) Uani 1 1 d . . . H10A H 0.3144 0.1825 0.0215 0.127 Uiso 1 1 calc R . . H10B H 0.3445 0.0812 0.0334 0.127 Uiso 1 1 calc R . . H10C H 0.3944 0.1672 0.0372 0.127 Uiso 1 1 calc R . . C11 C 0.3490(3) 0.1556(3) 0.1130(2) 0.0431(12) Uani 1 1 d . . . H11 H 0.3039 0.1330 0.1196 0.052 Uiso 1 1 calc R . . C12 C 0.3552(4) 0.2547(4) 0.1340(3) 0.097(2) Uani 1 1 d . . . H12A H 0.3981 0.2799 0.1267 0.145 Uiso 1 1 calc R . . H12B H 0.3536 0.2579 0.1779 0.145 Uiso 1 1 calc R . . H12C H 0.3178 0.2903 0.1108 0.145 Uiso 1 1 calc R . . C13 C 0.1471(2) -0.1283(3) 0.2301(2) 0.0405(12) Uani 1 1 d . . . C14 C 0.1714(3) -0.1931(4) 0.2750(3) 0.0563(15) Uani 1 1 d . . . C15 C 0.1259(3) -0.2439(5) 0.3027(3) 0.086(2) Uani 1 1 d . . . H15 H 0.1422 -0.2884 0.3332 0.103 Uiso 1 1 calc R . . C16 C 0.0568(3) -0.2291(5) 0.2857(3) 0.085(2) Uani 1 1 d . . . H16 H 0.0261 -0.2644 0.3040 0.102 Uiso 1 1 calc R . . C17 C 0.0328(3) -0.1644(4) 0.2428(3) 0.0634(16) Uani 1 1 d . . . H17 H -0.0145 -0.1539 0.2325 0.076 Uiso 1 1 calc R . . C18 C 0.0766(3) -0.1135(4) 0.2140(2) 0.0462(12) Uani 1 1 d . . . C19 C 0.2468(3) -0.2081(4) 0.2959(3) 0.0663(17) Uani 1 1 d . . . H19 H 0.2706 -0.1573 0.2782 0.080 Uiso 1 1 calc R . . C20 C 0.2689(4) -0.2959(5) 0.2712(4) 0.106(3) Uani 1 1 d . . . H20A H 0.2503 -0.3476 0.2910 0.159 Uiso 1 1 calc R . . H20B H 0.3183 -0.2992 0.2795 0.159 Uiso 1 1 calc R . . H20C H 0.2525 -0.2985 0.2267 0.159 Uiso 1 1 calc R . . C21 C 0.2692(4) -0.2048(6) 0.3662(3) 0.113(3) Uani 1 1 d . . . H21A H 0.2516 -0.2586 0.3846 0.169 Uiso 1 1 calc R . . H21B H 0.2517 -0.1489 0.3823 0.169 Uiso 1 1 calc R . . H21C H 0.3187 -0.2047 0.3764 0.169 Uiso 1 1 calc R . . C22 C 0.0504(3) -0.0449(4) 0.1646(3) 0.0538(14) Uani 1 1 d . . . H22 H 0.0849 0.0046 0.1661 0.065 Uiso 1 1 calc R . . C23 C 0.0407(3) -0.0895(5) 0.1006(3) 0.0752(19) Uani 1 1 d . . . H23A H 0.0837 -0.1155 0.0940 0.113 Uiso 1 1 calc R . . H23B H 0.0255 -0.0431 0.0692 0.113 Uiso 1 1 calc R . . H23C H 0.0069 -0.1383 0.0980 0.113 Uiso 1 1 calc R . . C24 C -0.0169(3) 0.0004(4) 0.1723(3) 0.0737(18) Uani 1 1 d . . . H24A H -0.0524 -0.0463 0.1682 0.111 Uiso 1 1 calc R . . H24B H -0.0292 0.0473 0.1405 0.111 Uiso 1 1 calc R . . H24C H -0.0117 0.0289 0.2130 0.111 Uiso 1 1 calc R . . C25 C 0.3595(2) -0.2831(3) 0.04603(19) 0.0346(10) Uani 1 1 d . . . C26 C 0.4017(2) -0.2374(3) 0.01121(19) 0.0347(10) Uani 1 1 d . . . C27 C 0.4404(3) -0.2891(4) -0.0218(2) 0.0471(13) Uani 1 1 d . . . H27 H 0.4687 -0.2585 -0.0453 0.057 Uiso 1 1 calc R . . C28 C 0.4392(3) -0.3840(4) -0.0217(2) 0.0531(14) Uani 1 1 d . . . H28 H 0.4657 -0.4182 -0.0451 0.064 Uiso 1 1 calc R . . C29 C 0.3986(3) -0.4277(3) 0.0136(2) 0.0504(14) Uani 1 1 d . . . H29 H 0.3986 -0.4928 0.0149 0.060 Uiso 1 1 calc R . . C30 C 0.3580(3) -0.3802(3) 0.0468(2) 0.0399(11) Uani 1 1 d . . . C31 C 0.3147(3) -0.4292(3) 0.0852(2) 0.0541(14) Uani 1 1 d . . . H31 H 0.2796 -0.3849 0.0935 0.065 Uiso 1 1 calc R . . C32 C 0.2785(3) -0.5117(4) 0.0542(3) 0.080(2) Uani 1 1 d . . . H32A H 0.2506 -0.4931 0.0152 0.120 Uiso 1 1 calc R . . H32B H 0.2496 -0.5384 0.0809 0.120 Uiso 1 1 calc R . . H32C H 0.3116 -0.5574 0.0464 0.120 Uiso 1 1 calc R . . C33 C 0.3567(4) -0.4578(5) 0.1480(3) 0.106(3) Uani 1 1 d . . . H33A H 0.3268 -0.4858 0.1733 0.159 Uiso 1 1 calc R . . H33B H 0.3785 -0.4036 0.1690 0.159 Uiso 1 1 calc R . . H33C H 0.3912 -0.5022 0.1415 0.159 Uiso 1 1 calc R . . C34 C 0.4055(2) -0.1339(3) 0.0116(2) 0.0402(11) Uani 1 1 d . . . H34 H 0.3674 -0.1105 0.0307 0.048 Uiso 1 1 calc R . . C35 C 0.3971(3) -0.0935(4) -0.0533(2) 0.0589(15) Uani 1 1 d . . . H35A H 0.4358 -0.1110 -0.0720 0.088 Uiso 1 1 calc R . . H35B H 0.3947 -0.0265 -0.0510 0.088 Uiso 1 1 calc R . . H35C H 0.3555 -0.1171 -0.0783 0.088 Uiso 1 1 calc R . . C36 C 0.4712(3) -0.1005(4) 0.0509(2) 0.0588(15) Uani 1 1 d . . . H36A H 0.4757 -0.1265 0.0922 0.088 Uiso 1 1 calc R . . H36B H 0.4706 -0.0335 0.0534 0.088 Uiso 1 1 calc R . . H36C H 0.5094 -0.1201 0.0322 0.088 Uiso 1 1 calc R . . C37 C 0.1845(3) 0.2839(3) 0.1962(2) 0.0464(12) Uani 1 1 d . . . C38 C 0.1349(3) 0.3086(4) 0.1445(2) 0.0550(14) Uani 1 1 d . . . C39 C 0.1015(3) 0.3923(4) 0.1455(3) 0.0693(17) Uani 1 1 d . . . H39 H 0.0673 0.4084 0.1117 0.083 Uiso 1 1 calc R . . C40 C 0.1166(3) 0.4522(4) 0.1941(3) 0.0668(17) Uani 1 1 d . . . H40 H 0.0924 0.5080 0.1946 0.080 Uiso 1 1 calc R . . C41 C 0.1672(3) 0.4299(4) 0.2415(3) 0.0569(14) Uani 1 1 d . . . H41 H 0.1791 0.4723 0.2743 0.068 Uiso 1 1 calc R . . C42 C 0.2021(3) 0.3470(3) 0.2439(2) 0.0453(12) Uani 1 1 d . . . C43 C 0.1197(3) 0.2449(4) 0.0892(3) 0.0680(17) Uani 1 1 d . . . H43 H 0.1516 0.1919 0.0974 0.082 Uiso 1 1 calc R . . C44 C 0.0492(4) 0.2067(6) 0.0802(4) 0.125(3) Uani 1 1 d . . . H44A H 0.0165 0.2571 0.0736 0.187 Uiso 1 1 calc R . . H44B H 0.0433 0.1720 0.1168 0.187 Uiso 1 1 calc R . . H44C H 0.0418 0.1661 0.0443 0.187 Uiso 1 1 calc R . . C45 C 0.1308(5) 0.2886(6) 0.0306(3) 0.125(3) Uani 1 1 d . . . H45A H 0.1178 0.2456 -0.0035 0.188 Uiso 1 1 calc R . . H45B H 0.1786 0.3046 0.0340 0.188 Uiso 1 1 calc R . . H45C H 0.1032 0.3442 0.0230 0.188 Uiso 1 1 calc R . . C46 C 0.2591(3) 0.3284(4) 0.2975(3) 0.0633(16) Uani 1 1 d . . . H46 H 0.2753 0.2648 0.2916 0.076 Uiso 1 1 calc R . . C47 C 0.2357(5) 0.3288(7) 0.3587(3) 0.134(4) Uani 1 1 d . . . H47A H 0.2746 0.3199 0.3918 0.201 Uiso 1 1 calc R . . H47B H 0.2031 0.2792 0.3596 0.201 Uiso 1 1 calc R . . H47C H 0.2142 0.3877 0.3643 0.201 Uiso 1 1 calc R . . C48 C 0.3177(4) 0.3896(5) 0.2984(3) 0.105(3) Uani 1 1 d . . . H48A H 0.3051 0.4524 0.3075 0.158 Uiso 1 1 calc R . . H48B H 0.3317 0.3881 0.2583 0.158 Uiso 1 1 calc R . . H48C H 0.3551 0.3690 0.3302 0.158 Uiso 1 1 calc R . . C49 C 0.3392(3) 0.0986(4) 0.3882(2) 0.0555(14) Uani 1 1 d . . . H49A H 0.3414 0.0354 0.4047 0.067 Uiso 1 1 calc R . . H49B H 0.2956 0.1260 0.3931 0.067 Uiso 1 1 calc R . . C50 C 0.3971(3) 0.1551(5) 0.4220(2) 0.0704(18) Uani 1 1 d . . . H50A H 0.3833 0.2195 0.4265 0.084 Uiso 1 1 calc R . . H50B H 0.4146 0.1292 0.4631 0.084 Uiso 1 1 calc R . . C51 C 0.4480(3) 0.1481(5) 0.3811(2) 0.080(2) Uani 1 1 d . . . H51A H 0.4765 0.2038 0.3846 0.096 Uiso 1 1 calc R . . H51B H 0.4774 0.0940 0.3921 0.096 Uiso 1 1 calc R . . C52 C 0.4092(3) 0.1389(4) 0.3187(2) 0.0509(13) Uani 1 1 d . . . H52A H 0.4018 0.1997 0.2988 0.061 Uiso 1 1 calc R . . H52B H 0.4335 0.0995 0.2935 0.061 Uiso 1 1 calc R . . C53 C 0.1529(3) 0.0258(5) 0.3649(3) 0.081(2) Uani 1 1 d . . . H53A H 0.1850 0.0425 0.4026 0.098 Uiso 1 1 calc R . . H53B H 0.1586 -0.0402 0.3567 0.098 Uiso 1 1 calc R . . C54 C 0.0831(4) 0.0440(6) 0.3732(4) 0.103(3) Uani 1 1 d . . . H54A H 0.0798 0.0446 0.4173 0.124 Uiso 1 1 calc R . . H54B H 0.0516 -0.0026 0.3518 0.124 Uiso 1 1 calc R . . C55 C 0.0685(4) 0.1369(5) 0.3449(3) 0.088(2) Uani 1 1 d . . . H55A H 0.0838 0.1860 0.3751 0.105 Uiso 1 1 calc R . . H55B H 0.0196 0.1446 0.3290 0.105 Uiso 1 1 calc R . . C56 C 0.1089(3) 0.1381(5) 0.2925(3) 0.079(2) Uani 1 1 d . . . H56A H 0.0816 0.1139 0.2541 0.095 Uiso 1 1 calc R . . H56B H 0.1238 0.2011 0.2850 0.095 Uiso 1 1 calc R . . C57 C 0.2205(5) -0.0815(5) -0.0272(3) 0.101(3) Uani 0.171(10) 1 d P A 2 H57A H 0.2286 -0.1479 -0.0316 0.121 Uiso 0.171(10) 1 calc PR A 2 H57B H 0.2593 -0.0470 -0.0376 0.121 Uiso 0.171(10) 1 calc PR A 2 C58 C 0.1574(13) -0.0534(18) -0.0667(13) 0.009(5) Uani 0.171(10) 1 d PU A 2 H58A H 0.1261 -0.1058 -0.0769 0.010 Uiso 0.171(10) 1 calc PR A 2 H58B H 0.1658 -0.0246 -0.1052 0.010 Uiso 0.171(10) 1 calc PR A 2 C58A C 0.1756(10) -0.0448(14) -0.0641(7) 0.215(11) Uani 0.829(10) 1 d P A 1 H58C H 0.1392 -0.0896 -0.0783 0.258 Uiso 0.829(10) 1 calc PR A 1 H58D H 0.1939 -0.0234 -0.1003 0.258 Uiso 0.829(10) 1 calc PR A 1 C59 C 0.130(2) 0.016(3) -0.025(2) 0.030(8) Uani 0.171(10) 1 d PU A 2 H59A H 0.1242 0.0766 -0.0459 0.036 Uiso 0.171(10) 1 calc PR A 2 H59B H 0.0860 -0.0043 -0.0169 0.036 Uiso 0.171(10) 1 calc PR A 2 C59A C 0.1464(9) 0.0384(13) -0.0328(7) 0.163(8) Uani 0.829(10) 1 d P A 1 H59C H 0.1605 0.0975 -0.0485 0.196 Uiso 0.829(10) 1 calc PR A 1 H59D H 0.0965 0.0361 -0.0389 0.196 Uiso 0.829(10) 1 calc PR A 1 C60 C 0.1767(3) 0.0246(4) 0.0310(3) 0.071(2) Uani 0.171(10) 1 d P A 2 H60A H 0.2081 0.0766 0.0298 0.085 Uiso 0.171(10) 1 calc PR A 2 H60B H 0.1530 0.0327 0.0661 0.085 Uiso 0.171(10) 1 calc PR A 2 C61 C 0.1231(3) -0.3238(5) 0.1220(3) 0.0792(19) Uani 1 1 d . A . H61A H 0.1014 -0.2888 0.1515 0.095 Uiso 1 1 calc R . . H61B H 0.1516 -0.3726 0.1445 0.095 Uiso 1 1 calc R . . C62 C 0.0704(3) -0.3642(4) 0.0710(3) 0.0766(19) Uani 1 1 d . . . H62A H 0.0539 -0.4242 0.0831 0.092 Uiso 1 1 calc R A . H62B H 0.0316 -0.3222 0.0594 0.092 Uiso 1 1 calc R . . C63 C 0.1099(4) -0.3746(5) 0.0196(4) 0.094(2) Uani 1 1 d . A . H63A H 0.0795 -0.3764 -0.0209 0.113 Uiso 1 1 calc R . . H63B H 0.1378 -0.4309 0.0248 0.113 Uiso 1 1 calc R . . C64 C 0.1536(3) -0.2894(5) 0.0261(3) 0.080(2) Uani 1 1 d . A . H64A H 0.1977 -0.3023 0.0141 0.095 Uiso 1 1 calc R . . H64B H 0.1310 -0.2394 -0.0001 0.095 Uiso 1 1 calc R . . C57A C 0.2205(5) -0.0815(5) -0.0272(3) 0.101(3) Uani 0.83 1 d P A 1 H57C H 0.2651 -0.0588 -0.0335 0.121 Uiso 0.829(10) 1 calc PR A 1 H57D H 0.2191 -0.1487 -0.0335 0.121 Uiso 0.829(10) 1 calc PR A 1 C60A C 0.1767(3) 0.0246(4) 0.0310(3) 0.071(2) Uani 0.83 1 d P A 1 H60C H 0.1415 0.0233 0.0569 0.085 Uiso 0.829(10) 1 calc PR A 1 H60D H 0.2087 0.0748 0.0455 0.085 Uiso 0.829(10) 1 calc PR A 1 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 0.03642(13) 0.03345(13) 0.03146(12) -0.00081(11) 0.00078(9) 0.00596(11) Eu2 0.04989(16) 0.03289(14) 0.04618(15) -0.00570(12) 0.01605(12) -0.00051(12) O1 0.0388(19) 0.0284(17) 0.0526(19) 0.0024(15) 0.0143(15) 0.0018(15) O2 0.0403(19) 0.046(2) 0.0395(18) 0.0021(16) 0.0119(14) -0.0072(16) O3 0.051(2) 0.0296(17) 0.053(2) 0.0003(16) 0.0195(16) 0.0009(16) O4 0.068(2) 0.041(2) 0.052(2) 0.0057(17) 0.0054(18) 0.0183(19) O5 0.050(2) 0.052(2) 0.0342(18) 0.0035(16) -0.0028(15) -0.0063(17) O6 0.052(2) 0.082(3) 0.058(2) 0.003(2) 0.0204(19) 0.012(2) O7 0.137(4) 0.072(3) 0.048(2) 0.001(2) 0.014(2) 0.047(3) O8 0.059(3) 0.062(3) 0.086(3) -0.019(2) 0.016(2) -0.013(2) C1 0.036(3) 0.028(2) 0.027(2) -0.0034(19) 0.0112(19) -0.003(2) C2 0.044(3) 0.032(3) 0.028(2) 0.001(2) 0.011(2) 0.004(2) C3 0.040(3) 0.046(3) 0.038(3) -0.004(2) 0.003(2) 0.005(2) C4 0.041(3) 0.054(3) 0.047(3) -0.009(3) 0.009(2) -0.008(3) C5 0.053(3) 0.038(3) 0.034(3) -0.001(2) 0.013(2) -0.014(2) C6 0.049(3) 0.029(2) 0.026(2) -0.007(2) 0.011(2) -0.002(2) C7 0.099(5) 0.039(3) 0.060(4) -0.001(3) 0.013(3) 0.003(3) C8 0.054(3) 0.038(3) 0.048(3) 0.010(2) 0.011(2) 0.007(2) C9 0.104(5) 0.059(4) 0.042(3) 0.013(3) 0.021(3) 0.008(4) C10 0.072(4) 0.135(7) 0.045(3) 0.020(4) 0.002(3) 0.013(4) C11 0.053(3) 0.034(3) 0.043(3) 0.013(2) 0.011(2) -0.002(2) C12 0.109(6) 0.038(4) 0.132(6) 0.011(4) -0.011(5) 0.015(4) C13 0.044(3) 0.038(3) 0.040(3) -0.008(2) 0.010(2) -0.009(2) C14 0.048(3) 0.060(4) 0.061(3) 0.020(3) 0.011(3) -0.008(3) C15 0.074(5) 0.088(5) 0.097(5) 0.045(4) 0.016(4) -0.013(4) C16 0.058(4) 0.090(5) 0.113(6) 0.030(5) 0.030(4) -0.023(4) C17 0.042(3) 0.068(4) 0.080(4) 0.003(4) 0.011(3) -0.011(3) C18 0.045(3) 0.045(3) 0.050(3) -0.004(3) 0.011(2) -0.005(3) C19 0.055(4) 0.066(4) 0.077(4) 0.029(3) 0.008(3) 0.003(3) C20 0.085(6) 0.082(6) 0.153(8) -0.008(5) 0.022(5) 0.004(4) C21 0.104(6) 0.144(8) 0.078(5) 0.010(5) -0.018(4) 0.028(6) C22 0.040(3) 0.049(3) 0.071(4) 0.001(3) 0.008(3) 0.007(3) C23 0.070(4) 0.097(5) 0.058(4) 0.002(4) 0.011(3) 0.020(4) C24 0.059(4) 0.076(5) 0.085(4) -0.007(4) 0.011(3) 0.013(4) C25 0.040(3) 0.033(3) 0.029(2) -0.007(2) 0.000(2) 0.003(2) C26 0.039(3) 0.035(3) 0.029(2) -0.005(2) 0.0030(19) -0.001(2) C27 0.048(3) 0.059(3) 0.033(3) -0.009(3) 0.003(2) 0.003(3) C28 0.061(4) 0.055(3) 0.040(3) -0.020(3) 0.001(3) 0.018(3) C29 0.070(4) 0.030(3) 0.045(3) -0.014(2) -0.005(3) 0.007(3) C30 0.052(3) 0.030(3) 0.032(2) 0.000(2) -0.006(2) 0.001(2) C31 0.069(4) 0.030(3) 0.060(3) 0.001(3) 0.004(3) -0.004(3) C32 0.081(5) 0.048(4) 0.108(5) -0.002(4) 0.008(4) -0.017(3) C33 0.128(7) 0.104(6) 0.078(5) 0.043(4) -0.006(4) -0.037(5) C34 0.050(3) 0.036(3) 0.037(3) -0.001(2) 0.016(2) -0.002(2) C35 0.073(4) 0.049(3) 0.056(3) 0.010(3) 0.016(3) -0.005(3) C36 0.074(4) 0.052(3) 0.052(3) -0.009(3) 0.015(3) -0.020(3) C37 0.048(3) 0.040(3) 0.053(3) 0.013(3) 0.013(2) 0.010(2) C38 0.059(4) 0.047(3) 0.057(3) 0.002(3) 0.006(3) 0.010(3) C39 0.069(4) 0.054(4) 0.077(4) 0.011(3) -0.010(3) 0.022(3) C40 0.067(4) 0.043(3) 0.089(5) 0.000(3) 0.012(4) 0.020(3) C41 0.071(4) 0.042(3) 0.058(3) -0.002(3) 0.013(3) 0.006(3) C42 0.057(3) 0.034(3) 0.047(3) 0.006(2) 0.013(2) 0.006(2) C43 0.083(5) 0.050(4) 0.061(4) -0.001(3) -0.014(3) 0.019(3) C44 0.134(8) 0.120(7) 0.128(7) -0.041(6) 0.046(6) -0.050(6) C45 0.181(9) 0.120(7) 0.086(6) -0.030(5) 0.058(6) -0.054(7) C46 0.079(4) 0.043(3) 0.063(4) -0.006(3) -0.001(3) 0.007(3) C47 0.149(8) 0.190(10) 0.059(5) 0.041(6) 0.010(5) 0.018(7) C48 0.091(6) 0.099(6) 0.110(6) 0.026(5) -0.027(5) -0.012(5) C49 0.061(4) 0.068(4) 0.036(3) 0.007(3) 0.003(2) -0.013(3) C50 0.086(5) 0.085(5) 0.040(3) -0.008(3) 0.012(3) -0.031(4) C51 0.071(4) 0.121(6) 0.044(3) -0.002(4) -0.001(3) -0.037(4) C52 0.055(3) 0.055(3) 0.042(3) -0.007(3) 0.009(2) -0.007(3) C53 0.077(5) 0.108(6) 0.064(4) 0.023(4) 0.024(3) 0.018(4) C54 0.090(6) 0.121(7) 0.110(6) 0.035(5) 0.049(5) 0.021(5) C55 0.088(5) 0.090(5) 0.098(5) 0.030(4) 0.051(4) 0.032(4) C56 0.068(4) 0.102(5) 0.072(4) 0.006(4) 0.025(3) 0.021(4) C57 0.148(8) 0.096(6) 0.056(4) -0.005(4) 0.015(5) 0.055(5) C58 0.008(5) 0.009(5) 0.009(5) 0.0002(10) 0.0014(14) -0.0005(10) C58A 0.30(2) 0.27(2) 0.073(8) -0.009(10) 0.002(12) 0.204(19) C59 0.030(8) 0.030(8) 0.030(8) 0.0000(10) 0.0055(17) 0.0000(10) C59A 0.200(19) 0.218(19) 0.068(8) 0.024(10) 0.014(9) 0.149(14) C60 0.075(5) 0.060(4) 0.078(5) 0.001(4) 0.016(3) 0.019(3) C61 0.066(4) 0.070(4) 0.103(5) -0.014(4) 0.018(4) -0.022(4) C62 0.055(4) 0.063(4) 0.108(5) -0.009(4) 0.006(4) -0.007(3) C63 0.073(5) 0.080(5) 0.121(6) -0.038(5) -0.005(4) 0.001(4) C64 0.078(5) 0.081(5) 0.076(5) -0.014(4) 0.001(4) -0.012(4) C57A 0.148(8) 0.096(6) 0.056(4) -0.005(4) 0.015(5) 0.055(5) C60A 0.075(5) 0.060(4) 0.078(5) 0.001(4) 0.016(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.285(3) . ? Eu1 O1 2.440(3) . ? Eu1 O2 2.454(3) . ? Eu1 O5 2.528(3) . ? Eu1 O6 2.600(4) . ? Eu1 Eu2 3.8924(14) . ? Eu2 O3 2.271(3) . ? Eu2 O1 2.416(3) . ? Eu2 O7 2.487(4) . ? Eu2 O2 2.500(3) . ? Eu2 O8 2.605(4) . ? O1 C1 1.343(5) . ? O2 C13 1.340(5) . ? O3 C25 1.326(5) . ? O4 C37 1.317(5) . ? O5 C49 1.428(5) . ? O5 C52 1.449(6) . ? O6 C53 1.439(7) . ? O6 C56 1.445(7) . ? O7 C60 1.417(7) . ? O7 C57 1.439(7) . ? O8 C61 1.442(7) . ? O8 C64 1.450(7) . ? C1 C2 1.405(6) . ? C1 C6 1.416(6) . ? C2 C3 1.382(6) . ? C2 C8 1.526(6) . ? C3 C4 1.374(7) . ? C4 C5 1.368(7) . ? C5 C6 1.387(6) . ? C6 C11 1.526(6) . ? C7 C8 1.537(7) . ? C8 C9 1.536(7) . ? C10 C11 1.512(7) . ? C11 C12 1.517(7) . ? C13 C14 1.394(7) . ? C13 C18 1.418(7) . ? C14 C15 1.404(7) . ? C14 C19 1.520(7) . ? C15 C16 1.391(9) . ? C16 C17 1.363(8) . ? C17 C18 1.392(7) . ? C18 C22 1.505(7) . ? C19 C20 1.492(9) . ? C19 C21 1.541(8) . ? C22 C23 1.538(8) . ? C22 C24 1.543(7) . ? C25 C26 1.413(6) . ? C25 C30 1.418(6) . ? C26 C27 1.384(6) . ? C26 C34 1.512(6) . ? C27 C28 1.384(7) . ? C28 C29 1.383(7) . ? C29 C30 1.382(7) . ? C30 C31 1.503(7) . ? C31 C32 1.507(7) . ? C31 C33 1.548(8) . ? C34 C36 1.526(7) . ? C34 C35 1.531(6) . ? C37 C42 1.398(7) . ? C37 C38 1.422(7) . ? C38 C39 1.397(7) . ? C38 C43 1.522(8) . ? C39 C40 1.377(8) . ? C40 C41 1.363(8) . ? C41 C42 1.395(7) . ? C42 C46 1.518(7) . ? C43 C45 1.496(9) . ? C43 C44 1.505(9) . ? C46 C48 1.477(9) . ? C46 C47 1.513(8) . ? C49 C50 1.510(7) . ? C50 C51 1.486(8) . ? C51 C52 1.465(7) . ? C53 C54 1.475(9) . ? C54 C55 1.499(9) . ? C55 C56 1.533(8) . ? C57 C58 1.46(3) . ? C58 C59 1.54(5) . ? C58A C59A 1.56(2) . ? C59 C60 1.42(5) . ? C61 C62 1.523(8) . ? C62 C63 1.508(9) . ? C63 C64 1.515(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu1 O1 110.53(11) . . ? O4 Eu1 O2 121.54(12) . . ? O1 Eu1 O2 75.01(10) . . ? O4 Eu1 O5 105.36(12) . . ? O1 Eu1 O5 96.00(11) . . ? O2 Eu1 O5 132.59(11) . . ? O4 Eu1 O6 87.57(13) . . ? O1 Eu1 O6 159.23(11) . . ? O2 Eu1 O6 87.00(11) . . ? O5 Eu1 O6 88.52(12) . . ? O4 Eu1 Eu2 120.73(9) . . ? O1 Eu1 Eu2 36.51(7) . . ? O2 Eu1 Eu2 38.64(7) . . ? O5 Eu1 Eu2 121.03(8) . . ? O6 Eu1 Eu2 125.37(9) . . ? O3 Eu2 O1 111.52(11) . . ? O3 Eu2 O7 91.82(13) . . ? O1 Eu2 O7 90.33(13) . . ? O3 Eu2 O2 166.44(10) . . ? O1 Eu2 O2 74.59(10) . . ? O7 Eu2 O2 100.39(12) . . ? O3 Eu2 O8 84.63(12) . . ? O1 Eu2 O8 163.28(11) . . ? O7 Eu2 O8 84.65(15) . . ? O2 Eu2 O8 90.60(11) . . ? O3 Eu2 Eu1 147.78(8) . . ? O1 Eu2 Eu1 36.94(7) . . ? O7 Eu2 Eu1 94.16(10) . . ? O2 Eu2 Eu1 37.80(7) . . ? O8 Eu2 Eu1 127.43(9) . . ? C1 O1 Eu2 131.8(3) . . ? C1 O1 Eu1 118.9(2) . . ? Eu2 O1 Eu1 106.55(11) . . ? C13 O2 Eu1 128.3(3) . . ? C13 O2 Eu2 124.1(3) . . ? Eu1 O2 Eu2 103.56(11) . . ? C25 O3 Eu2 175.9(3) . . ? C37 O4 Eu1 158.0(3) . . ? C49 O5 C52 108.8(3) . . ? C49 O5 Eu1 124.4(3) . . ? C52 O5 Eu1 125.5(3) . . ? C53 O6 C56 109.1(4) . . ? C53 O6 Eu1 133.8(3) . . ? C56 O6 Eu1 114.5(3) . . ? C60 O7 C57 106.5(5) . . ? C60 O7 Eu2 126.3(3) . . ? C57 O7 Eu2 126.7(4) . . ? C61 O8 C64 109.9(4) . . ? C61 O8 Eu2 132.5(4) . . ? C64 O8 Eu2 116.6(3) . . ? O1 C1 C2 120.8(4) . . ? O1 C1 C6 119.8(4) . . ? C2 C1 C6 119.4(4) . . ? C3 C2 C1 119.2(4) . . ? C3 C2 C8 120.0(4) . . ? C1 C2 C8 120.8(4) . . ? C4 C3 C2 121.6(5) . . ? C5 C4 C3 119.3(5) . . ? C4 C5 C6 121.9(4) . . ? C5 C6 C1 118.5(4) . . ? C5 C6 C11 120.3(4) . . ? C1 C6 C11 121.1(4) . . ? C2 C8 C9 111.7(4) . . ? C2 C8 C7 111.6(4) . . ? C9 C8 C7 110.4(4) . . ? C10 C11 C12 112.2(5) . . ? C10 C11 C6 110.5(4) . . ? C12 C11 C6 112.3(4) . . ? O2 C13 C14 121.0(4) . . ? O2 C13 C18 119.7(4) . . ? C14 C13 C18 119.3(4) . . ? C13 C14 C15 119.7(5) . . ? C13 C14 C19 121.1(5) . . ? C15 C14 C19 119.1(5) . . ? C16 C15 C14 120.0(6) . . ? C17 C16 C15 120.5(6) . . ? C16 C17 C18 120.9(6) . . ? C17 C18 C13 119.5(5) . . ? C17 C18 C22 121.3(5) . . ? C13 C18 C22 119.2(4) . . ? C20 C19 C14 111.1(6) . . ? C20 C19 C21 110.1(6) . . ? C14 C19 C21 113.4(5) . . ? C18 C22 C23 110.9(4) . . ? C18 C22 C24 113.8(5) . . ? C23 C22 C24 108.3(5) . . ? O3 C25 C26 120.6(4) . . ? O3 C25 C30 119.8(4) . . ? C26 C25 C30 119.6(4) . . ? C27 C26 C25 118.9(4) . . ? C27 C26 C34 121.0(4) . . ? C25 C26 C34 120.2(4) . . ? C26 C27 C28 122.2(5) . . ? C29 C28 C27 118.3(5) . . ? C30 C29 C28 122.4(5) . . ? C29 C30 C25 118.7(5) . . ? C29 C30 C31 121.4(4) . . ? C25 C30 C31 119.9(4) . . ? C30 C31 C32 113.9(5) . . ? C30 C31 C33 110.9(5) . . ? C32 C31 C33 109.5(5) . . ? C26 C34 C36 111.1(4) . . ? C26 C34 C35 112.5(4) . . ? C36 C34 C35 110.4(4) . . ? O4 C37 C42 121.9(5) . . ? O4 C37 C38 119.1(5) . . ? C42 C37 C38 119.0(5) . . ? C39 C38 C37 118.7(5) . . ? C39 C38 C43 121.2(5) . . ? C37 C38 C43 120.1(5) . . ? C40 C39 C38 121.9(5) . . ? C41 C40 C39 118.6(5) . . ? C40 C41 C42 122.5(5) . . ? C41 C42 C37 119.1(5) . . ? C41 C42 C46 119.3(5) . . ? C37 C42 C46 121.6(4) . . ? C45 C43 C44 109.1(6) . . ? C45 C43 C38 113.4(5) . . ? C44 C43 C38 112.4(6) . . ? C48 C46 C47 111.2(6) . . ? C48 C46 C42 113.0(5) . . ? C47 C46 C42 112.7(5) . . ? O5 C49 C50 107.3(4) . . ? C51 C50 C49 102.5(5) . . ? C52 C51 C50 105.7(5) . . ? O5 C52 C51 106.3(4) . . ? O6 C53 C54 108.4(5) . . ? C53 C54 C55 103.3(6) . . ? C54 C55 C56 103.6(5) . . ? O6 C56 C55 104.4(5) . . ? O7 C57 C58 104.9(12) . . ? C57 C58 C59 101(2) . . ? C60 C59 C58 109(3) . . ? O7 C60 C59 102(2) . . ? O8 C61 C62 104.3(5) . . ? C63 C62 C61 101.9(5) . . ? C62 C63 C64 102.9(5) . . ? O8 C64 C63 105.6(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.563 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.102 # Attachment '- 15.SHSQ6z=4 last.CIF' data_SHSQ6z=4.CIF _database_code_depnum_ccdc_archive 'CCDC 845104' #TrackingRef '- 15.SHSQ6z=4 last.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sq2 _chemical_melting_point ? _chemical_formula_moiety 'C43 H67.50 La O6.50' _chemical_formula_sum 'C42 H65 La O6' _chemical_formula_weight 827.38 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.133(2) _cell_length_b 15.232(3) _cell_length_c 25.884(5) _cell_angle_alpha 89.63(3) _cell_angle_beta 79.38(3) _cell_angle_gamma 69.75(3) _cell_volume 4402.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 62811 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 26.69 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1738 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71200 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62811 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 26.69 _reflns_number_total 16469 _reflns_number_gt 15669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.0123P)^2^+27.3372P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_coef none _refine_ls_number_reflns 16469 _refine_ls_number_parameters 955 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1167 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 202 12 2 -0.002 0.500 0.500 294 30 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 La1 La 0.51323(2) 0.946848(16) 0.308014(9) 0.01437(7) Uani 1 1 d . . . O1 O 0.6785(3) 0.8264(2) 0.27363(14) 0.0278(7) Uani 1 1 d . . . C1 C 0.7924(4) 0.7704(3) 0.2569(2) 0.0252(10) Uani 1 1 d . . . C27 C 0.1129(4) 0.8869(4) 0.2481(2) 0.0368(13) Uani 1 1 d . . . H27 H 0.0478 0.8750 0.2696 0.044 Uiso 1 1 calc R . . La2 La 0.54906(2) 0.436257(16) 0.183390(9) 0.01632(7) Uani 1 1 d . . . O2 O 0.4250(3) 0.9266(2) 0.38886(12) 0.0221(7) Uani 1 1 d . . . C2 C 0.8433(4) 0.7583(3) 0.2025(2) 0.0302(11) Uani 1 1 d . . . O3 O 0.3877(3) 0.9236(2) 0.26005(12) 0.0227(7) Uani 1 1 d . . . C3 C 0.9616(5) 0.6985(4) 0.1861(3) 0.0415(14) Uani 1 1 d . . . H3 H 0.9972 0.6908 0.1497 0.050 Uiso 1 1 calc R . . O4 O 0.4032(3) 1.1205(2) 0.28657(14) 0.0286(7) Uani 1 1 d . . . C4 C 1.0277(5) 0.6504(4) 0.2220(3) 0.0486(16) Uani 1 1 d . . . H4 H 1.1081 0.6097 0.2103 0.058 Uiso 1 1 calc R . . O5 O 0.6424(3) 1.0523(2) 0.27598(14) 0.0272(7) Uani 1 1 d . . . C5 C 0.9773(5) 0.6612(4) 0.2745(3) 0.0446(14) Uani 1 1 d . . . H5 H 1.0237 0.6269 0.2987 0.054 Uiso 1 1 calc R . . O6 O 0.6452(3) 0.9865(2) 0.37218(13) 0.0289(8) Uani 1 1 d . . . C6 C 0.8605(4) 0.7208(3) 0.2938(2) 0.0314(11) Uani 1 1 d . . . O7 O 0.6260(3) 0.3719(2) 0.10165(13) 0.0334(8) Uani 1 1 d . . . C7 C 0.7688(5) 0.8086(4) 0.1632(2) 0.0326(11) Uani 1 1 d . . . H7 H 0.6831 0.8204 0.1795 0.039 Uiso 1 1 calc R . . O8 O 0.6765(3) 0.3340(2) 0.22737(12) 0.0239(7) Uani 1 1 d . . . C8 C 0.7808(8) 0.9040(5) 0.1534(3) 0.0580(19) Uani 1 1 d . . . H8A H 0.7600 0.9407 0.1870 0.087 Uiso 1 1 calc R . . H8B H 0.7266 0.9374 0.1302 0.087 Uiso 1 1 calc R . . H8C H 0.8635 0.8953 0.1366 0.087 Uiso 1 1 calc R . . O9 O 0.3786(3) 0.4150(2) 0.22101(12) 0.0231(7) Uani 1 1 d . . . C9 C 0.7953(6) 0.7514(5) 0.1114(3) 0.0524(16) Uani 1 1 d . . . H9A H 0.8746 0.7463 0.0916 0.079 Uiso 1 1 calc R . . H9B H 0.7345 0.7824 0.0905 0.079 Uiso 1 1 calc R . . H9C H 0.7938 0.6885 0.1186 0.079 Uiso 1 1 calc R . . O10 O 0.4162(3) 0.5602(2) 0.12409(12) 0.0278(7) Uani 1 1 d . . . C10 C 0.8029(5) 0.7252(4) 0.3514(2) 0.0325(11) Uani 1 1 d . . . H10 H 0.7283 0.7820 0.3584 0.039 Uiso 1 1 calc R . . O11 O 0.4521(3) 0.6144(2) 0.21654(12) 0.0225(7) Uani 1 1 d . . . C11 C 0.7669(7) 0.6393(5) 0.3617(3) 0.0543(18) Uani 1 1 d . . . H11A H 0.7106 0.6380 0.3393 0.082 Uiso 1 1 calc R . . H11B H 0.7287 0.6421 0.3988 0.082 Uiso 1 1 calc R . . H11C H 0.8384 0.5824 0.3537 0.082 Uiso 1 1 calc R . . O12 O 0.6906(3) 0.5321(2) 0.19670(13) 0.0246(7) Uani 1 1 d . . . C12 C 0.8821(7) 0.7326(6) 0.3893(3) 0.066(2) Uani 1 1 d . . . H12A H 0.9562 0.6778 0.3830 0.099 Uiso 1 1 calc R . . H12B H 0.8395 0.7351 0.4256 0.099 Uiso 1 1 calc R . . H12C H 0.9014 0.7897 0.3835 0.099 Uiso 1 1 calc R . . C13 C 0.3421(4) 0.9284(3) 0.43124(17) 0.0200(9) Uani 1 1 d . . . C14 C 0.3554(4) 0.8490(3) 0.46143(17) 0.0226(9) Uani 1 1 d . . . C15 C 0.2646(5) 0.8531(4) 0.50428(18) 0.0294(11) Uani 1 1 d . . . H15 H 0.2721 0.7996 0.5243 0.035 Uiso 1 1 calc R . . C16 C 0.1645(4) 0.9326(4) 0.51832(19) 0.0310(11) Uani 1 1 d . . . H16 H 0.1042 0.9337 0.5478 0.037 Uiso 1 1 calc R . . C17 C 0.1523(4) 1.0110(4) 0.48919(19) 0.0288(10) Uani 1 1 d . . . H17 H 0.0835 1.0659 0.4991 0.035 Uiso 1 1 calc R . . C18 C 0.2395(4) 1.0104(3) 0.44557(18) 0.0227(9) Uani 1 1 d . . . C19 C 0.4684(5) 0.7628(4) 0.44864(19) 0.0308(11) Uani 1 1 d . . . H19 H 0.5120 0.7672 0.4125 0.037 Uiso 1 1 calc R . . C20 C 0.4442(6) 0.6707(4) 0.4498(2) 0.0451(15) Uani 1 1 d . . . H20A H 0.4105 0.6614 0.4860 0.068 Uiso 1 1 calc R . . H20B H 0.5194 0.6186 0.4372 0.068 Uiso 1 1 calc R . . H20C H 0.3873 0.6730 0.4270 0.068 Uiso 1 1 calc R . . C21 C 0.5492(5) 0.7616(4) 0.4878(2) 0.0411(13) Uani 1 1 d . . . H21A H 0.5734 0.8168 0.4840 0.062 Uiso 1 1 calc R . . H21B H 0.6205 0.7046 0.4806 0.062 Uiso 1 1 calc R . . H21C H 0.5054 0.7627 0.5237 0.062 Uiso 1 1 calc R . . C22 C 0.2276(5) 1.0948(4) 0.4131(2) 0.0301(11) Uani 1 1 d . . . H22 H 0.2619 1.0703 0.3757 0.036 Uiso 1 1 calc R . . C23 C 0.0990(6) 1.1596(5) 0.4147(3) 0.0520(16) Uani 1 1 d . . . H23A H 0.0531 1.1238 0.4036 0.078 Uiso 1 1 calc R . . H23B H 0.0985 1.2099 0.3908 0.078 Uiso 1 1 calc R . . H23C H 0.0625 1.1869 0.4506 0.078 Uiso 1 1 calc R . . C24 C 0.3016(7) 1.1501(5) 0.4276(3) 0.0563(18) Uani 1 1 d . . . H24A H 0.3033 1.1974 0.4019 0.084 Uiso 1 1 calc R . . H24B H 0.3835 1.1075 0.4274 0.084 Uiso 1 1 calc R . . H24C H 0.2658 1.1812 0.4628 0.084 Uiso 1 1 calc R . . C25 C 0.2988(4) 0.9163(3) 0.23920(16) 0.0176(8) Uani 1 1 d U A . C26 C 0.2023(4) 0.8982(3) 0.27116(19) 0.0226(9) Uani 1 1 d . . . C28 C 0.1169(5) 0.8926(4) 0.1949(3) 0.0436(15) Uani 1 1 d . . . H28 H 0.0555 0.8836 0.1799 0.052 Uiso 1 1 calc R . . C29 C 0.2076(7) 0.9109(4) 0.1639(2) 0.0458(16) Uani 1 1 d . A . H29 H 0.2084 0.9158 0.1273 0.055 Uiso 1 1 calc R . . C30 C 0.3010(6) 0.9230(4) 0.1847(2) 0.0383(13) Uani 1 1 d . . . C31 C 0.2020(5) 0.8887(4) 0.3288(2) 0.0354(13) Uani 1 1 d . . . H31 H 0.2388 0.9333 0.3398 0.042 Uiso 1 1 calc R . . C32 C 0.2803(10) 0.7925(5) 0.3389(3) 0.075(3) Uani 1 1 d . . . H32A H 0.2486 0.7462 0.3278 0.112 Uiso 1 1 calc R . . H32B H 0.2818 0.7888 0.3766 0.112 Uiso 1 1 calc R . . H32C H 0.3618 0.7795 0.3190 0.112 Uiso 1 1 calc R . . C33 C 0.0758(7) 0.9164(7) 0.3630(3) 0.080(3) Uani 1 1 d . . . H33A H 0.0270 0.9794 0.3553 0.121 Uiso 1 1 calc R . . H33B H 0.0814 0.9158 0.4003 0.121 Uiso 1 1 calc R . . H33C H 0.0384 0.8716 0.3553 0.121 Uiso 1 1 calc R . . C36 C 0.4592(13) 0.8882(10) 0.0952(6) 0.039(3) Uani 0.449(12) 1 d PU A 1 H36A H 0.4072 0.9117 0.0696 0.058 Uiso 0.449(12) 1 calc PR A 1 H36B H 0.4703 0.8220 0.1002 0.058 Uiso 0.449(12) 1 calc PR A 1 H36C H 0.5371 0.8944 0.0822 0.058 Uiso 0.449(12) 1 calc PR A 1 C37 C 0.2836(5) 1.1524(4) 0.2762(3) 0.0436(14) Uani 1 1 d . . . H37A H 0.2372 1.2131 0.2954 0.065 Uiso 1 1 calc R . . H37B H 0.2454 1.1067 0.2879 0.065 Uiso 1 1 calc R . . H37C H 0.2867 1.1592 0.2384 0.065 Uiso 1 1 calc R . . C38 C 0.4709(5) 1.1764(4) 0.2635(2) 0.0371(13) Uani 1 1 d . . . H38A H 0.4228 1.2439 0.2712 0.045 Uiso 1 1 calc R . . H38B H 0.4928 1.1636 0.2248 0.045 Uiso 1 1 calc R . . C39 C 0.5810(5) 1.1520(3) 0.2864(2) 0.0366(13) Uani 1 1 d . . . H39A H 0.6326 1.1867 0.2698 0.044 Uiso 1 1 calc R . . H39B H 0.5597 1.1683 0.3248 0.044 Uiso 1 1 calc R . . C40 C 0.7556(4) 1.0185(4) 0.2935(2) 0.0370(13) Uani 1 1 d . . . H40A H 0.8046 1.0565 0.2791 0.044 Uiso 1 1 calc R . . H40B H 0.7998 0.9526 0.2799 0.044 Uiso 1 1 calc R . . C41 C 0.7369(5) 1.0241(4) 0.3525(2) 0.0397(13) Uani 1 1 d . . . H41A H 0.8121 0.9876 0.3641 0.048 Uiso 1 1 calc R . . H41B H 0.7121 1.0901 0.3660 0.048 Uiso 1 1 calc R . . C42 C 0.6308(6) 0.9788(5) 0.4282(2) 0.0420(14) Uani 1 1 d . . . H42A H 0.7059 0.9365 0.4367 0.063 Uiso 1 1 calc R . . H42B H 0.5668 0.9537 0.4403 0.063 Uiso 1 1 calc R . . H42C H 0.6099 1.0408 0.4457 0.063 Uiso 1 1 calc R . . C43 C 0.6903(4) 0.3288(3) 0.05495(18) 0.0259(10) Uani 1 1 d . B . C44 C 0.7922(5) 0.3489(4) 0.03095(18) 0.0283(10) Uani 1 1 d . . . C45 C 0.8573(5) 0.3021(5) -0.0170(2) 0.0412(14) Uani 1 1 d . . . H45 H 0.9259 0.3155 -0.0334 0.049 Uiso 1 1 calc R . . C46 C 0.8257(6) 0.2374(5) -0.0412(2) 0.0489(16) Uani 1 1 d . . . H46 H 0.8723 0.2057 -0.0737 0.059 Uiso 1 1 calc R . . C47 C 0.7252(7) 0.2189(4) -0.0177(2) 0.0485(16) Uani 1 1 d . B . H47 H 0.7028 0.1745 -0.0348 0.058 Uiso 1 1 calc R . . C48 C 0.6559(5) 0.2630(4) 0.0299(2) 0.0353(12) Uiso 1 1 d . . . C49 C 0.8255(6) 0.4211(5) 0.0573(2) 0.0466(16) Uani 1 1 d . . . H49 H 0.8078 0.4144 0.0961 0.056 Uiso 1 1 calc R . . C50 C 0.7512(8) 0.5187(5) 0.0472(3) 0.065(2) Uani 1 1 d . . . H50A H 0.7689 0.5285 0.0096 0.097 Uiso 1 1 calc R . . H50B H 0.7701 0.5639 0.0675 0.097 Uiso 1 1 calc R . . H50C H 0.6661 0.5275 0.0580 0.097 Uiso 1 1 calc R . . C51 C 0.9590(8) 0.4074(7) 0.0417(4) 0.084(3) Uani 1 1 d . . . H51A H 1.0071 0.3421 0.0458 0.126 Uiso 1 1 calc R . . H51B H 0.9782 0.4490 0.0645 0.126 Uiso 1 1 calc R . . H51C H 0.9769 0.4223 0.0050 0.126 Uiso 1 1 calc R . . C52' C 0.5431(7) 0.2439(6) 0.0550(3) 0.066(2) Uani 0.412(11) 1 d P B 1 H52' H 0.4938 0.3077 0.0720 0.080 Uiso 0.412(11) 1 calc PR B 1 C55 C 0.2753(4) 0.4090(3) 0.24709(18) 0.0219(9) Uani 1 1 d . C . C56 C 0.1988(4) 0.3842(3) 0.2191(2) 0.0280(10) Uani 1 1 d . . . C57 C 0.0923(5) 0.3782(4) 0.2478(2) 0.0369(13) Uani 1 1 d . C . H57 H 0.0411 0.3612 0.2294 0.044 Uiso 1 1 calc R . . C58 C 0.0589(5) 0.3955(4) 0.3011(3) 0.0399(13) Uani 1 1 d . . . H58 H -0.0146 0.3916 0.3192 0.048 Uiso 1 1 calc R C . C59 C 0.1341(5) 0.4189(3) 0.3282(2) 0.0317(11) Uani 1 1 d . C . H59 H 0.1113 0.4313 0.3653 0.038 Uiso 1 1 calc R . . C60 C 0.2429(4) 0.4249(3) 0.30214(19) 0.0227(9) Uani 1 1 d . . . C61' C 0.2358(5) 0.3623(4) 0.1604(2) 0.0385(15) Uani 0.276(11) 1 d P C 1 H61' H 0.3077 0.3814 0.1516 0.046 Uiso 0.276(11) 1 calc PR C 1 C62 C 0.2045(9) 0.4494(7) 0.1318(3) 0.046(2) Uani 0.724(11) 1 d P C 2 H62A H 0.2300 0.4336 0.0938 0.069 Uiso 0.724(11) 1 calc PR C 2 H62B H 0.2451 0.4898 0.1425 0.069 Uiso 0.724(11) 1 calc PR C 2 H62C H 0.1177 0.4824 0.1402 0.069 Uiso 0.724(11) 1 calc PR C 2 C63 C 0.1721(9) 0.2955(7) 0.1426(4) 0.053(3) Uani 0.724(11) 1 d P C 2 H63A H 0.1940 0.2377 0.1613 0.080 Uiso 0.724(11) 1 calc PR C 2 H63B H 0.1981 0.2802 0.1046 0.080 Uiso 0.724(11) 1 calc PR C 2 H63C H 0.0851 0.3274 0.1510 0.080 Uiso 0.724(11) 1 calc PR C 2 C64 C 0.3234(5) 0.4499(4) 0.33294(19) 0.0305(11) Uani 1 1 d . C . H64 H 0.4047 0.4315 0.3099 0.037 Uiso 1 1 calc R . . C65 C 0.3373(6) 0.3988(5) 0.3835(2) 0.0482(15) Uani 1 1 d . . . H65A H 0.2584 0.4127 0.4062 0.072 Uiso 1 1 calc R C . H65B H 0.3883 0.4197 0.4019 0.072 Uiso 1 1 calc R . . H65C H 0.3742 0.3311 0.3748 0.072 Uiso 1 1 calc R . . C66 C 0.2792(9) 0.5560(5) 0.3455(3) 0.067(2) Uani 1 1 d . . . H66A H 0.2756 0.5883 0.3126 0.100 Uiso 1 1 calc R C . H66B H 0.3345 0.5713 0.3640 0.100 Uiso 1 1 calc R . . H66C H 0.1992 0.5764 0.3679 0.100 Uiso 1 1 calc R . . C67 C 0.7729(4) 0.2785(3) 0.2451(2) 0.0251(10) Uani 1 1 d . . . C68 C 0.7742(4) 0.2837(3) 0.2997(2) 0.0275(11) Uani 1 1 d . . . C69 C 0.8741(5) 0.2246(4) 0.3176(2) 0.0385(13) Uani 1 1 d . . . H69 H 0.8761 0.2271 0.3541 0.046 Uiso 1 1 calc R . . C70 C 0.9705(5) 0.1624(4) 0.2833(3) 0.0464(16) Uani 1 1 d . . . H70 H 1.0385 0.1236 0.2962 0.056 Uiso 1 1 calc R . . C71 C 0.9680(5) 0.1566(4) 0.2303(3) 0.0430(15) Uani 1 1 d . . . H71 H 1.0341 0.1132 0.2071 0.052 Uiso 1 1 calc R . . C72 C 0.8695(5) 0.2139(3) 0.2105(2) 0.0319(11) Uani 1 1 d . . . C73 C 0.6659(5) 0.3503(4) 0.3362(2) 0.0310(11) Uani 1 1 d . . . H73 H 0.5936 0.3455 0.3250 0.037 Uiso 1 1 calc R . . C74 C 0.6588(6) 0.4526(4) 0.3313(2) 0.0458(15) Uani 1 1 d . . . H74A H 0.7274 0.4606 0.3429 0.069 Uiso 1 1 calc R . . H74B H 0.5844 0.4942 0.3534 0.069 Uiso 1 1 calc R . . H74C H 0.6600 0.4684 0.2945 0.069 Uiso 1 1 calc R . . C75 C 0.6581(7) 0.3266(5) 0.3937(2) 0.0515(17) Uani 1 1 d . . . H75A H 0.6552 0.2633 0.3971 0.077 Uiso 1 1 calc R . . H75B H 0.5856 0.3719 0.4150 0.077 Uiso 1 1 calc R . . H75C H 0.7286 0.3294 0.4060 0.077 Uiso 1 1 calc R . . C76 C 0.8617(5) 0.2032(4) 0.1528(2) 0.0386(13) Uani 1 1 d . . . H76 H 0.8120 0.2663 0.1432 0.046 Uiso 1 1 calc R . . C77 C 0.7959(15) 0.1388(10) 0.1469(4) 0.155(7) Uani 1 1 d . . . H77A H 0.7161 0.1629 0.1695 0.233 Uiso 1 1 calc R . . H77B H 0.8402 0.0764 0.1573 0.233 Uiso 1 1 calc R . . H77C H 0.7879 0.1345 0.1101 0.233 Uiso 1 1 calc R . . C78 C 0.9785(8) 0.1741(9) 0.1147(4) 0.111(4) Uani 1 1 d . . . H78A H 1.0297 0.1118 0.1223 0.167 Uiso 1 1 calc R . . H78B H 1.0184 0.2193 0.1180 0.167 Uiso 1 1 calc R . . H78C H 0.9642 0.1722 0.0787 0.167 Uiso 1 1 calc R . . C79 C 0.4162(7) 0.5490(4) 0.0685(2) 0.0473(16) Uani 1 1 d . . . H79A H 0.3350 0.5574 0.0638 0.071 Uiso 1 1 calc R . . H79B H 0.4705 0.4861 0.0547 0.071 Uiso 1 1 calc R . . H79C H 0.4433 0.5960 0.0495 0.071 Uiso 1 1 calc R . . C80 C 0.3399(5) 0.6520(3) 0.1456(2) 0.0308(11) Uani 1 1 d . . . H80A H 0.2587 0.6663 0.1379 0.037 Uiso 1 1 calc R . . H80B H 0.3725 0.6996 0.1299 0.037 Uiso 1 1 calc R . . C81 C 0.3348(5) 0.6533(4) 0.2041(2) 0.0328(11) Uani 1 1 d . . . H81A H 0.2961 0.7187 0.2192 0.039 Uiso 1 1 calc R . . H81B H 0.2852 0.6169 0.2202 0.039 Uiso 1 1 calc R . . C82 C 0.5236(5) 0.6722(3) 0.2036(2) 0.0342(12) Uani 1 1 d . . . H82A H 0.4819 0.7354 0.2215 0.041 Uiso 1 1 calc R . . H82B H 0.5391 0.6788 0.1652 0.041 Uiso 1 1 calc R . . C83 C 0.6382(5) 0.6249(3) 0.2219(2) 0.0305(11) Uani 1 1 d . . . H83A H 0.6931 0.6603 0.2122 0.037 Uiso 1 1 calc R . . H83B H 0.6230 0.6217 0.2606 0.037 Uiso 1 1 calc R . . C84 C 0.8147(4) 0.4898(4) 0.2004(2) 0.0319(11) Uani 1 1 d . . . H84A H 0.8604 0.5258 0.1812 0.048 Uiso 1 1 calc R . . H84B H 0.8462 0.4252 0.1851 0.048 Uiso 1 1 calc R . . H84C H 0.8220 0.4896 0.2375 0.048 Uiso 1 1 calc R . . C63' C 0.284(2) 0.2644(15) 0.1436(8) 0.040(5) Uiso 0.276(11) 1 d P C 1 H63D H 0.3057 0.2575 0.1051 0.060 Uiso 0.276(11) 1 calc PR C 1 H63E H 0.2242 0.2354 0.1558 0.060 Uiso 0.276(11) 1 calc PR C 1 H63F H 0.3557 0.2336 0.1584 0.060 Uiso 0.276(11) 1 calc PR C 1 C62' C 0.155(2) 0.4224(19) 0.1273(10) 0.052(6) Uiso 0.276(11) 1 d P C 1 H62D H 0.1240 0.4875 0.1417 0.077 Uiso 0.276(11) 1 calc PR C 1 H62E H 0.0876 0.4006 0.1272 0.077 Uiso 0.276(11) 1 calc PR C 1 H62F H 0.1992 0.4185 0.0912 0.077 Uiso 0.276(11) 1 calc PR C 1 C61 C 0.2358(5) 0.3623(4) 0.1604(2) 0.0385(15) Uani 0.72 1 d P C 2 H61 H 0.3245 0.3292 0.1515 0.046 Uiso 0.724(11) 1 calc PR C 2 C55' C 0.5791(13) 0.1274(8) 0.0442(5) 0.065(4) Uani 0.588(11) 1 d P B 2 H55A H 0.5997 0.1113 0.0061 0.097 Uiso 0.588(11) 1 calc PR B 2 H55B H 0.5106 0.1094 0.0597 0.097 Uiso 0.588(11) 1 calc PR B 2 H55C H 0.6478 0.0938 0.0602 0.097 Uiso 0.588(11) 1 calc PR B 2 C53 C 0.4490(13) 0.2870(11) 0.0177(6) 0.061(4) Uani 0.588(11) 1 d PU B 2 H53A H 0.4169 0.3555 0.0233 0.092 Uiso 0.588(11) 1 calc PR B 2 H53B H 0.3834 0.2625 0.0260 0.092 Uiso 0.588(11) 1 calc PR B 2 H53C H 0.4890 0.2694 -0.0192 0.092 Uiso 0.588(11) 1 calc PR B 2 C52 C 0.5431(7) 0.2439(6) 0.0550(3) 0.066(2) Uani 0.59 1 d P B 2 H52 H 0.5125 0.2669 0.0929 0.080 Uiso 0.588(11) 1 calc PR B 2 C54' C 0.4629(17) 0.2297(17) 0.0290(8) 0.070(6) Uani 0.412(11) 1 d P B 1 H54A H 0.4568 0.2677 -0.0018 0.104 Uiso 0.412(11) 1 calc PR B 1 H54B H 0.3843 0.2478 0.0524 0.104 Uiso 0.412(11) 1 calc PR B 1 H54C H 0.4894 0.1632 0.0174 0.104 Uiso 0.412(11) 1 calc PR B 1 C54 C 0.5606(14) 0.1868(11) 0.1071(6) 0.045(4) Uani 0.412(11) 1 d PU B 1 H54D H 0.4821 0.1909 0.1274 0.068 Uiso 0.412(11) 1 calc PR B 1 H54E H 0.6009 0.2138 0.1287 0.068 Uiso 0.412(11) 1 calc PR B 1 H54F H 0.6094 0.1210 0.0971 0.068 Uiso 0.412(11) 1 calc PR B 1 C35 C 0.4299(16) 1.0228(10) 0.1581(5) 0.052(4) Uani 0.449(12) 1 d P A 1 H35A H 0.3736 1.0785 0.1459 0.078 Uiso 0.449(12) 1 calc PR A 1 H35B H 0.5110 1.0116 0.1382 0.078 Uiso 0.449(12) 1 calc PR A 1 H35C H 0.4278 1.0328 0.1956 0.078 Uiso 0.449(12) 1 calc PR A 1 C36' C 0.3218(15) 1.0324(10) 0.1105(6) 0.078(5) Uani 0.551(12) 1 d P A 2 H36D H 0.3770 1.0599 0.0903 0.117 Uiso 0.551(12) 1 calc PR A 2 H36E H 0.2555 1.0818 0.1328 0.117 Uiso 0.551(12) 1 calc PR A 2 H36F H 0.2901 1.0026 0.0863 0.117 Uiso 0.551(12) 1 calc PR A 2 C35' C 0.4799(13) 0.8796(10) 0.1192(6) 0.058(4) Uani 0.551(12) 1 d PU A 2 H35D H 0.5320 0.8360 0.1400 0.087 Uiso 0.551(12) 1 calc PR A 2 H35E H 0.5280 0.9054 0.0932 0.087 Uiso 0.551(12) 1 calc PR A 2 H35F H 0.4406 0.8462 0.1010 0.087 Uiso 0.551(12) 1 calc PR A 2 C34' C 0.3986(9) 0.9479(7) 0.1505(4) 0.076(3) Uani 0.449(12) 1 d PU A 1 H34' H 0.4614 0.9063 0.1687 0.092 Uiso 0.449(12) 1 calc PR A 1 C34 C 0.3986(9) 0.9479(7) 0.1505(4) 0.076(3) Uani 0.55 1 d PU A 2 H34 H 0.4380 0.9765 0.1727 0.092 Uiso 0.551(12) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.01278(11) 0.01139(12) 0.02202(13) 0.00090(9) -0.00481(9) -0.00735(9) O1 0.0158(15) 0.0157(15) 0.046(2) -0.0050(14) 0.0005(14) -0.0008(13) C1 0.016(2) 0.011(2) 0.049(3) -0.0017(19) -0.003(2) -0.0075(18) C27 0.016(2) 0.032(3) 0.059(4) -0.020(3) -0.007(2) -0.005(2) La2 0.01873(13) 0.01235(12) 0.01957(12) 0.00260(9) -0.00646(9) -0.00620(10) O2 0.0240(16) 0.0267(17) 0.0207(15) 0.0039(13) -0.0058(13) -0.0148(15) C2 0.022(2) 0.019(2) 0.051(3) -0.002(2) 0.001(2) -0.013(2) O3 0.0189(15) 0.0258(17) 0.0279(16) -0.0045(13) -0.0073(13) -0.0118(14) C3 0.023(3) 0.031(3) 0.064(4) 0.002(3) 0.006(3) -0.009(2) O4 0.0223(17) 0.0203(17) 0.045(2) 0.0116(15) -0.0092(15) -0.0089(15) C4 0.022(3) 0.039(3) 0.078(5) 0.000(3) 0.003(3) -0.007(3) O5 0.0216(16) 0.0222(17) 0.043(2) 0.0050(14) -0.0075(14) -0.0134(15) C5 0.023(3) 0.036(3) 0.072(4) 0.012(3) -0.011(3) -0.006(3) O6 0.0309(18) 0.0340(19) 0.0349(18) 0.0034(15) -0.0160(15) -0.0230(17) C6 0.022(2) 0.021(2) 0.055(3) 0.006(2) -0.010(2) -0.010(2) O7 0.043(2) 0.0238(17) 0.0203(16) -0.0001(13) 0.0059(15) -0.0009(17) C7 0.029(3) 0.026(3) 0.042(3) -0.001(2) -0.004(2) -0.010(2) O8 0.0264(17) 0.0211(16) 0.0294(17) 0.0113(13) -0.0161(14) -0.0096(15) C8 0.086(5) 0.034(3) 0.067(4) 0.018(3) -0.034(4) -0.028(4) O9 0.0193(15) 0.0214(16) 0.0280(17) 0.0047(13) -0.0036(13) -0.0069(14) C9 0.052(4) 0.052(4) 0.046(4) -0.012(3) -0.005(3) -0.012(3) O10 0.042(2) 0.0203(17) 0.0204(16) 0.0009(13) -0.0125(14) -0.0071(16) C10 0.027(3) 0.025(3) 0.048(3) 0.006(2) -0.016(2) -0.008(2) O11 0.0250(16) 0.0114(14) 0.0289(17) 0.0015(12) -0.0109(13) -0.0008(13) C11 0.066(4) 0.044(4) 0.056(4) -0.002(3) 0.005(3) -0.032(4) O12 0.0231(16) 0.0189(16) 0.0350(18) 0.0029(13) -0.0098(14) -0.0096(14) C12 0.061(5) 0.085(6) 0.070(5) -0.001(4) -0.024(4) -0.041(5) C13 0.022(2) 0.028(2) 0.020(2) 0.0004(17) -0.0104(17) -0.017(2) C14 0.029(2) 0.028(2) 0.018(2) 0.0028(17) -0.0111(18) -0.016(2) C15 0.037(3) 0.041(3) 0.023(2) 0.010(2) -0.013(2) -0.026(3) C16 0.026(2) 0.052(3) 0.021(2) 0.005(2) -0.0071(19) -0.020(3) C17 0.021(2) 0.038(3) 0.027(2) -0.001(2) -0.0083(19) -0.009(2) C18 0.023(2) 0.028(2) 0.025(2) 0.0013(18) -0.0110(18) -0.015(2) C19 0.042(3) 0.028(3) 0.026(2) 0.004(2) -0.012(2) -0.014(2) C20 0.067(4) 0.033(3) 0.045(3) 0.006(2) -0.026(3) -0.022(3) C21 0.040(3) 0.044(3) 0.044(3) 0.002(3) -0.018(3) -0.014(3) C22 0.030(3) 0.025(3) 0.041(3) 0.006(2) -0.014(2) -0.013(2) C23 0.035(3) 0.048(4) 0.071(4) 0.026(3) -0.019(3) -0.009(3) C24 0.060(4) 0.034(3) 0.092(5) 0.006(3) -0.033(4) -0.030(3) C25 0.0188(11) 0.0172(11) 0.0185(11) -0.0024(8) -0.0065(8) -0.0070(9) C26 0.018(2) 0.019(2) 0.033(2) -0.0075(18) -0.0067(18) -0.0079(19) C28 0.038(3) 0.032(3) 0.063(4) -0.015(3) -0.038(3) 0.001(3) C29 0.084(5) 0.029(3) 0.036(3) 0.003(2) -0.039(3) -0.020(3) C30 0.070(4) 0.035(3) 0.025(3) 0.001(2) -0.018(3) -0.032(3) C31 0.046(3) 0.044(3) 0.029(3) -0.007(2) -0.001(2) -0.035(3) C32 0.162(9) 0.047(4) 0.045(4) 0.017(3) -0.056(5) -0.056(5) C33 0.078(5) 0.138(8) 0.050(4) -0.028(5) 0.023(4) -0.086(6) C36 0.039(3) 0.039(3) 0.039(3) 0.0020(10) -0.0076(12) -0.0136(15) C37 0.026(3) 0.032(3) 0.070(4) 0.017(3) -0.018(3) -0.003(3) C38 0.043(3) 0.020(2) 0.055(3) 0.013(2) -0.011(3) -0.017(2) C39 0.038(3) 0.018(2) 0.063(4) 0.005(2) -0.010(3) -0.022(2) C40 0.020(2) 0.043(3) 0.059(4) 0.011(3) -0.013(2) -0.023(2) C41 0.034(3) 0.044(3) 0.060(4) 0.008(3) -0.023(3) -0.029(3) C42 0.051(3) 0.055(4) 0.037(3) 0.004(3) -0.023(3) -0.032(3) C43 0.030(2) 0.026(2) 0.020(2) 0.0058(18) -0.0054(19) -0.007(2) C44 0.033(3) 0.035(3) 0.021(2) 0.005(2) -0.010(2) -0.014(2) C45 0.028(3) 0.063(4) 0.023(2) 0.005(2) 0.000(2) -0.006(3) C46 0.056(4) 0.051(4) 0.024(3) -0.008(3) -0.008(3) 0.001(3) C47 0.078(5) 0.034(3) 0.037(3) -0.001(2) -0.026(3) -0.016(3) C49 0.067(4) 0.061(4) 0.033(3) 0.012(3) -0.022(3) -0.043(4) C50 0.090(6) 0.049(4) 0.070(5) -0.005(3) -0.028(4) -0.036(4) C51 0.073(6) 0.085(6) 0.133(8) 0.037(6) -0.055(6) -0.058(5) C52' 0.058(5) 0.071(5) 0.091(6) 0.041(4) -0.027(4) -0.044(4) C55 0.020(2) 0.013(2) 0.031(2) 0.0051(17) -0.0051(18) -0.0025(18) C56 0.021(2) 0.022(2) 0.037(3) -0.001(2) -0.010(2) 0.000(2) C57 0.020(2) 0.027(3) 0.063(4) 0.002(3) -0.017(2) -0.004(2) C58 0.021(2) 0.032(3) 0.061(4) 0.005(3) 0.003(2) -0.008(2) C59 0.026(3) 0.024(2) 0.038(3) 0.003(2) 0.006(2) -0.008(2) C60 0.022(2) 0.014(2) 0.032(2) 0.0035(18) -0.0039(19) -0.0054(19) C61' 0.028(3) 0.042(3) 0.040(3) -0.006(2) -0.015(2) -0.001(3) C62 0.050(5) 0.061(6) 0.031(4) 0.000(4) -0.005(4) -0.027(5) C63 0.060(6) 0.058(6) 0.050(5) -0.008(4) -0.025(4) -0.024(5) C64 0.039(3) 0.032(3) 0.026(2) 0.003(2) -0.009(2) -0.018(2) C65 0.056(4) 0.057(4) 0.039(3) 0.019(3) -0.021(3) -0.024(4) C66 0.117(7) 0.038(4) 0.066(5) 0.009(3) -0.055(5) -0.037(4) C67 0.021(2) 0.015(2) 0.046(3) 0.0142(19) -0.014(2) -0.012(2) C68 0.025(2) 0.024(2) 0.046(3) 0.021(2) -0.022(2) -0.016(2) C69 0.035(3) 0.036(3) 0.059(4) 0.024(3) -0.027(3) -0.021(3) C70 0.022(3) 0.038(3) 0.087(5) 0.036(3) -0.027(3) -0.012(3) C71 0.021(3) 0.027(3) 0.083(5) 0.023(3) -0.012(3) -0.010(2) C72 0.025(2) 0.020(2) 0.056(3) 0.011(2) -0.009(2) -0.013(2) C73 0.036(3) 0.034(3) 0.032(3) 0.015(2) -0.019(2) -0.019(3) C74 0.068(4) 0.030(3) 0.041(3) 0.006(2) -0.013(3) -0.018(3) C75 0.064(4) 0.066(4) 0.037(3) 0.023(3) -0.022(3) -0.032(4) C76 0.035(3) 0.028(3) 0.049(3) 0.002(2) 0.000(3) -0.010(2) C77 0.33(2) 0.197(13) 0.048(5) 0.006(6) -0.026(8) -0.230(15) C78 0.051(5) 0.159(11) 0.076(6) 0.050(7) 0.015(4) 0.009(6) C79 0.081(5) 0.042(3) 0.018(2) -0.001(2) -0.019(3) -0.015(3) C80 0.036(3) 0.021(2) 0.031(3) -0.0013(19) -0.016(2) -0.001(2) C81 0.033(3) 0.028(3) 0.031(3) -0.005(2) -0.011(2) 0.000(2) C82 0.051(3) 0.017(2) 0.037(3) 0.001(2) -0.008(2) -0.016(2) C83 0.036(3) 0.017(2) 0.043(3) 0.003(2) -0.010(2) -0.014(2) C84 0.019(2) 0.036(3) 0.044(3) 0.006(2) -0.009(2) -0.012(2) C61 0.028(3) 0.042(3) 0.040(3) -0.006(2) -0.015(2) -0.001(3) C55' 0.087(10) 0.040(6) 0.077(9) 0.011(6) -0.010(7) -0.037(7) C53 0.061(4) 0.061(4) 0.062(4) 0.0040(10) -0.0115(12) -0.0217(16) C52 0.058(5) 0.071(5) 0.091(6) 0.041(4) -0.027(4) -0.044(4) C54' 0.047(10) 0.090(16) 0.074(13) 0.036(12) -0.005(9) -0.031(11) C54 0.045(4) 0.045(4) 0.045(4) 0.0032(10) -0.0085(12) -0.0158(17) C35 0.084(12) 0.038(8) 0.037(7) -0.004(6) 0.004(7) -0.033(8) C36' 0.082(11) 0.052(8) 0.074(10) 0.033(7) 0.006(8) -0.003(8) C35' 0.058(4) 0.058(4) 0.058(4) 0.0041(10) -0.0107(12) -0.0206(16) C34' 0.077(3) 0.077(3) 0.076(3) 0.0040(7) -0.0145(9) -0.0285(11) C34 0.077(3) 0.077(3) 0.076(3) 0.0040(7) -0.0145(9) -0.0285(11) _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 La1 O1 2.236(3) . ? La1 O2 2.240(3) . ? La1 O3 2.250(3) . ? La1 O4 2.626(3) . ? La1 O5 2.641(3) . ? La1 O6 2.711(3) . ? O1 C1 1.339(5) . ? C1 C2 1.415(7) . ? C1 C6 1.419(8) . ? C27 C28 1.372(9) . ? C27 C26 1.389(6) . ? La2 O7 2.230(3) . ? La2 O9 2.247(3) . ? La2 O8 2.252(3) . ? La2 O11 2.632(3) . ? La2 O12 2.676(3) . ? La2 O10 2.699(3) . ? O2 C13 1.338(5) . ? C2 C3 1.396(7) . ? C2 C7 1.512(8) . ? O3 C25 1.328(5) . ? C3 C4 1.380(10) . ? O4 C38 1.433(6) . ? O4 C37 1.438(6) . ? C4 C5 1.371(9) . ? O5 C39 1.443(6) . ? O5 C40 1.446(6) . ? C5 C6 1.391(7) . ? O6 C41 1.433(6) . ? O6 C42 1.438(6) . ? C6 C10 1.517(8) . ? O7 C43 1.345(6) . ? C7 C9 1.525(8) . ? C7 C8 1.526(8) . ? O8 C67 1.343(6) . ? O9 C55 1.342(5) . ? O10 C80 1.431(6) . ? O10 C79 1.449(6) . ? C10 C12 1.524(8) . ? C10 C11 1.525(7) . ? O11 C82 1.435(6) . ? O11 C81 1.437(6) . ? O12 C83 1.437(6) . ? O12 C84 1.439(6) . ? C13 C14 1.414(6) . ? C13 C18 1.416(7) . ? C14 C15 1.397(7) . ? C14 C19 1.518(7) . ? C15 C16 1.378(8) . ? C16 C17 1.386(7) . ? C17 C18 1.395(7) . ? C18 C22 1.511(7) . ? C19 C20 1.529(7) . ? C19 C21 1.529(7) . ? C22 C24 1.519(7) . ? C22 C23 1.525(8) . ? C25 C30 1.409(6) . ? C25 C26 1.413(6) . ? C26 C31 1.499(7) . ? C28 C29 1.347(9) . ? C29 C30 1.407(8) . ? C30 C34' 1.501(10) . ? C31 C32 1.497(10) . ? C31 C33 1.538(8) . ? C36 C34' 1.606(16) . ? C38 C39 1.489(8) . ? C40 C41 1.501(8) . ? C43 C44 1.408(7) . ? C43 C48 1.413(7) . ? C44 C45 1.389(7) . ? C44 C49 1.501(7) . ? C45 C46 1.368(9) . ? C46 C47 1.377(10) . ? C47 C48 1.385(8) . ? C48 C52' 1.525(8) . ? C49 C50 1.498(10) . ? C49 C51 1.535(10) . ? C52' C54' 1.36(2) . ? C52' C54 1.607(16) . ? C55 C60 1.406(6) . ? C55 C56 1.424(7) . ? C56 C57 1.398(7) . ? C56 C61' 1.506(7) . ? C57 C58 1.364(8) . ? C58 C59 1.384(8) . ? C59 C60 1.399(6) . ? C60 C64 1.511(7) . ? C61' C63' 1.44(2) . ? C61' C62' 1.49(3) . ? C64 C65 1.524(7) . ? C64 C66 1.533(8) . ? C67 C72 1.404(7) . ? C67 C68 1.419(7) . ? C68 C69 1.393(7) . ? C68 C73 1.510(8) . ? C69 C70 1.385(9) . ? C70 C71 1.381(10) . ? C71 C72 1.397(8) . ? C72 C76 1.527(8) . ? C73 C75 1.522(7) . ? C73 C74 1.536(7) . ? C76 C77 1.489(10) . ? C76 C78 1.496(9) . ? C80 C81 1.503(7) . ? C82 C83 1.490(8) . ? C35 C34' 1.347(15) . ? 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 La1 O2 114.18(13) . . ? O1 La1 O3 98.82(12) . . ? O2 La1 O3 100.38(11) . . ? O1 La1 O4 137.78(12) . . ? O2 La1 O4 107.37(12) . . ? O3 La1 O4 80.29(12) . . ? O1 La1 O5 85.23(11) . . ? O2 La1 O5 131.02(11) . . ? O3 La1 O5 121.49(11) . . ? O4 La1 O5 61.26(10) . . ? O1 La1 O6 86.64(12) . . ? O2 La1 O6 75.95(11) . . ? O3 La1 O6 174.37(11) . . ? O4 La1 O6 96.62(11) . . ? O5 La1 O6 60.08(11) . . ? C1 O1 La1 163.9(3) . . ? O1 C1 C2 120.1(5) . . ? O1 C1 C6 119.7(5) . . ? C2 C1 C6 120.2(4) . . ? C28 C27 C26 121.3(5) . . ? O7 La2 O9 114.83(13) . . ? O7 La2 O8 99.86(13) . . ? O9 La2 O8 99.24(12) . . ? O7 La2 O11 129.49(12) . . ? O9 La2 O11 89.44(11) . . ? O8 La2 O11 120.09(11) . . ? O7 La2 O12 102.59(13) . . ? O9 La2 O12 142.06(11) . . ? O8 La2 O12 79.51(11) . . ? O11 La2 O12 60.54(10) . . ? O7 La2 O10 76.57(12) . . ? O9 La2 O10 86.52(12) . . ? O8 La2 O10 174.14(11) . . ? O11 La2 O10 60.68(10) . . ? O12 La2 O10 96.62(10) . . ? C13 O2 La1 162.3(3) . . ? C3 C2 C1 118.9(5) . . ? C3 C2 C7 121.2(5) . . ? C1 C2 C7 119.9(4) . . ? C25 O3 La1 169.9(3) . . ? C4 C3 C2 120.8(6) . . ? C38 O4 C37 112.6(4) . . ? C38 O4 La1 120.2(3) . . ? C37 O4 La1 122.4(3) . . ? C5 C4 C3 120.0(5) . . ? C39 O5 C40 113.1(4) . . ? C39 O5 La1 115.6(3) . . ? C40 O5 La1 110.9(3) . . ? C4 C5 C6 122.3(6) . . ? C41 O6 C42 111.7(4) . . ? C41 O6 La1 121.4(3) . . ? C42 O6 La1 126.8(3) . . ? C5 C6 C1 117.8(5) . . ? C5 C6 C10 121.3(5) . . ? C1 C6 C10 120.5(4) . . ? C43 O7 La2 170.3(3) . . ? C2 C7 C9 113.7(5) . . ? C2 C7 C8 111.0(5) . . ? C9 C7 C8 110.7(5) . . ? C67 O8 La2 165.8(3) . . ? C55 O9 La2 174.3(3) . . ? C80 O10 C79 111.2(4) . . ? C80 O10 La2 120.9(3) . . ? C79 O10 La2 127.7(3) . . ? C6 C10 C12 113.8(5) . . ? C6 C10 C11 109.1(5) . . ? C12 C10 C11 110.0(6) . . ? C82 O11 C81 113.7(4) . . ? C82 O11 La2 117.6(3) . . ? C81 O11 La2 109.6(3) . . ? C83 O12 C84 111.5(4) . . ? C83 O12 La2 119.5(3) . . ? C84 O12 La2 124.5(3) . . ? O2 C13 C14 120.6(4) . . ? O2 C13 C18 119.6(4) . . ? C14 C13 C18 119.8(4) . . ? C15 C14 C13 118.6(4) . . ? C15 C14 C19 121.0(4) . . ? C13 C14 C19 120.4(4) . . ? C16 C15 C14 121.8(5) . . ? C15 C16 C17 119.6(5) . . ? C16 C17 C18 121.0(5) . . ? C17 C18 C13 119.2(4) . . ? C17 C18 C22 121.8(5) . . ? C13 C18 C22 118.9(4) . . ? C14 C19 C20 113.5(5) . . ? C14 C19 C21 109.2(4) . . ? C20 C19 C21 109.1(5) . . ? C18 C22 C24 111.7(5) . . ? C18 C22 C23 114.4(4) . . ? C24 C22 C23 110.2(5) . . ? O3 C25 C30 120.9(4) . . ? O3 C25 C26 120.3(4) . . ? C30 C25 C26 118.8(4) . . ? C27 C26 C25 119.3(5) . . ? C27 C26 C31 122.1(5) . . ? C25 C26 C31 118.5(4) . . ? C29 C28 C27 120.2(5) . . ? C28 C29 C30 121.4(5) . . ? C29 C30 C25 119.0(5) . . ? C29 C30 C34' 121.1(6) . . ? C25 C30 C34' 119.8(6) . . ? C32 C31 C26 110.9(5) . . ? C32 C31 C33 111.7(6) . . ? C26 C31 C33 113.6(6) . . ? O4 C38 C39 108.1(4) . . ? O5 C39 C38 106.6(4) . . ? O5 C40 C41 111.0(4) . . ? O6 C41 C40 107.7(4) . . ? O7 C43 C44 120.2(4) . . ? O7 C43 C48 119.9(4) . . ? C44 C43 C48 119.8(4) . . ? C45 C44 C43 118.5(5) . . ? C45 C44 C49 122.3(5) . . ? C43 C44 C49 119.1(5) . . ? C46 C45 C44 122.2(5) . . ? C45 C46 C47 118.9(5) . . ? C46 C47 C48 122.1(6) . . ? C47 C48 C43 118.5(5) . . ? C47 C48 C52' 121.8(6) . . ? C43 C48 C52' 119.8(5) . . ? C50 C49 C44 111.6(5) . . ? C50 C49 C51 109.8(6) . . ? C44 C49 C51 113.1(6) . . ? C54' C52' C48 125.8(10) . . ? C54' C52' C54 114.9(11) . . ? C48 C52' C54 111.8(8) . . ? O9 C55 C60 120.7(4) . . ? O9 C55 C56 119.9(4) . . ? C60 C55 C56 119.4(4) . . ? C57 C56 C55 118.1(5) . . ? C57 C56 C61' 122.2(5) . . ? C55 C56 C61' 119.7(4) . . ? C58 C57 C56 122.9(5) . . ? C57 C58 C59 118.8(5) . . ? C58 C59 C60 121.5(5) . . ? C59 C60 C55 119.4(5) . . ? C59 C60 C64 120.2(4) . . ? C55 C60 C64 120.5(4) . . ? C63' C61' C62' 114.4(14) . . ? C63' C61' C56 115.6(10) . . ? C62' C61' C56 116.7(11) . . ? C60 C64 C65 113.8(4) . . ? C60 C64 C66 110.6(5) . . ? C65 C64 C66 109.8(5) . . ? O8 C67 C72 120.6(5) . . ? O8 C67 C68 119.1(4) . . ? C72 C67 C68 120.3(5) . . ? C69 C68 C67 118.4(5) . . ? C69 C68 C73 122.6(5) . . ? C67 C68 C73 118.9(4) . . ? C70 C69 C68 121.2(6) . . ? C71 C70 C69 120.1(5) . . ? C70 C71 C72 120.8(6) . . ? C71 C72 C67 119.1(6) . . ? C71 C72 C76 121.3(5) . . ? C67 C72 C76 119.5(5) . . ? C68 C73 C75 113.8(5) . . ? C68 C73 C74 111.7(4) . . ? C75 C73 C74 109.8(5) . . ? C77 C76 C78 110.8(9) . . ? C77 C76 C72 109.9(5) . . ? C78 C76 C72 115.4(6) . . ? O10 C80 C81 107.3(4) . . ? O11 C81 C80 111.7(4) . . ? O11 C82 C83 106.8(4) . . ? O12 C83 C82 107.5(4) . . ? C35 C34' C30 126.4(9) . . ? C35 C34' C36 116.2(10) . . ? C30 C34' C36 116.8(8) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 26.69 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 1.829 _refine_diff_density_min -2.390 _refine_diff_density_rms 0.108 # Attachment '- 4.ndthf2.cif' data_ndthf2)2.cif _database_code_depnum_ccdc_archive 'CCDC 845105' #TrackingRef '- 4.ndthf2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Refine _chemical_melting_point ? _chemical_formula_moiety 'C44 H67 Nd O5' _chemical_formula_sum 'C44 H67 Nd O5' _chemical_formula_weight 820.22 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.790(2) _cell_length_b 19.391(2) _cell_length_c 12.139(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.018(11) _cell_angle_gamma 90.00 _cell_volume 2165.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15584 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.08 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 1.239 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71200 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15584 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.08 _reflns_number_total 8416 _reflns_number_gt 8121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.0340P)^2^+1.5876P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.051(11) _refine_ls_number_reflns 8416 _refine_ls_number_parameters 468 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.083 _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 Nd1 Nd 0.220960(13) 0.253430(12) 0.288043(11) 0.01909(5) Uani 1 1 d . . . O1 O 0.1417(3) 0.21230(13) 0.1112(2) 0.0275(5) Uani 1 1 d . . . O2 O 0.1566(3) 0.19226(12) 0.4118(2) 0.0236(5) Uani 1 1 d . . . O3 O 0.3378(3) 0.34968(13) 0.3007(2) 0.0298(5) Uani 1 1 d . . . O4 O 0.4600(3) 0.19672(15) 0.3731(3) 0.0356(6) Uani 1 1 d . A . O5 O 0.0150(3) 0.32706(14) 0.2840(3) 0.0319(6) Uani 1 1 d . . . C1 C 0.0575(4) 0.1680(2) 0.0308(3) 0.0294(8) Uani 1 1 d . . . C2 C 0.1136(5) 0.1026(2) 0.0179(3) 0.0348(8) Uani 1 1 d . . . C3 C 0.0206(6) 0.0567(3) -0.0608(4) 0.0507(12) Uani 1 1 d . . . H27 H 0.0562 0.0123 -0.0703 0.061 Uiso 1 1 calc R . . C4 C -0.1184(6) 0.0730(3) -0.1243(4) 0.0597(16) Uani 1 1 d . . . H28 H -0.1792 0.0401 -0.1764 0.072 Uiso 1 1 calc R . . C5 C -0.1729(5) 0.1390(3) -0.1128(4) 0.0542(14) Uani 1 1 d . . . H29 H -0.2704 0.1506 -0.1579 0.065 Uiso 1 1 calc R . . C38A C 0.642(2) 0.1810(14) 0.5543(18) 0.047(7) Uiso 0.26(3) 1 d P A 2 H38C H 0.6091 0.2197 0.5921 0.056 Uiso 0.26(3) 1 calc PR A 2 H38D H 0.7031 0.1491 0.6150 0.056 Uiso 0.26(3) 1 calc PR A 2 C6 C -0.0851(5) 0.1873(3) -0.0361(4) 0.0363(11) Uani 1 1 d . . . C7 C 0.2709(6) 0.0868(2) 0.0867(4) 0.0418(10) Uani 1 1 d . . . H35 H 0.2905 0.1049 0.1678 0.050 Uiso 1 1 calc R . . C8 C 0.3726(5) 0.1244(3) 0.0376(6) 0.0539(13) Uani 1 1 d . . . H36A H 0.3539 0.1097 -0.0435 0.081 Uiso 1 1 calc R . . H36B H 0.4735 0.1138 0.0851 0.081 Uiso 1 1 calc R . . H36C H 0.3564 0.1742 0.0393 0.081 Uiso 1 1 calc R . . C9 C 0.3057(8) 0.0092(3) 0.0987(6) 0.0657(15) Uani 1 1 d . . . H34A H 0.2379 -0.0142 0.1297 0.099 Uiso 1 1 calc R . . H34B H 0.4054 0.0024 0.1523 0.099 Uiso 1 1 calc R . . H34C H 0.2958 -0.0099 0.0216 0.099 Uiso 1 1 calc R . . C10 C -0.1385(4) 0.2594(5) -0.0205(3) 0.0494(13) Uani 1 1 d . . . H32 H -0.1017 0.2696 0.0655 0.059 Uiso 1 1 calc R . . C11 C -0.0744(7) 0.3138(3) -0.0796(5) 0.0571(15) Uani 1 1 d . . . H33A H -0.1125 0.3070 -0.1647 0.086 Uiso 1 1 calc R . . H33B H 0.0318 0.3094 -0.0514 0.086 Uiso 1 1 calc R . . H33C H -0.1011 0.3598 -0.0607 0.086 Uiso 1 1 calc R . . C12 C -0.3044(5) 0.2659(6) -0.0628(5) 0.083(3) Uani 1 1 d . . . H31A H -0.3312 0.3138 -0.0545 0.125 Uiso 1 1 calc R . . H31B H -0.3431 0.2359 -0.0156 0.125 Uiso 1 1 calc R . . H31C H -0.3451 0.2521 -0.1453 0.125 Uiso 1 1 calc R . . C13 C 0.1007(3) 0.15501(17) 0.4794(3) 0.0215(6) Uani 1 1 d . . . C14 C 0.1126(4) 0.17896(19) 0.5921(3) 0.0266(7) Uani 1 1 d . . . C15 C 0.0545(5) 0.1387(2) 0.6606(3) 0.0361(9) Uani 1 1 d . . . H5 H 0.0623 0.1540 0.7369 0.043 Uiso 1 1 calc R . . C16 C -0.0147(5) 0.0766(2) 0.6188(4) 0.0375(9) Uani 1 1 d . . . H4 H -0.0547 0.0500 0.6661 0.045 Uiso 1 1 calc R . . C17 C -0.0251(4) 0.0536(2) 0.5086(4) 0.0336(8) Uani 1 1 d . . . H3 H -0.0722 0.0110 0.4809 0.040 Uiso 1 1 calc R . . C18 C 0.0317(4) 0.09130(18) 0.4374(3) 0.0254(7) Uani 1 1 d . . . C19 C 0.1894(4) 0.2465(3) 0.6372(3) 0.0358(9) Uani 1 1 d . . . H11 H 0.1851 0.2739 0.5662 0.043 Uiso 1 1 calc R . . C20 C 0.3482(7) 0.2346(3) 0.7043(8) 0.095(3) Uani 1 1 d . . . H10A H 0.3585 0.2079 0.7753 0.143 Uiso 1 1 calc R . . H10B H 0.3975 0.2791 0.7262 0.143 Uiso 1 1 calc R . . H10C H 0.3919 0.2090 0.6551 0.143 Uiso 1 1 calc R . . C21 C 0.1162(9) 0.2895(4) 0.7032(9) 0.098(3) Uani 1 1 d . . . H12A H 0.1225 0.2661 0.7763 0.147 Uiso 1 1 calc R . . H12B H 0.0138 0.2961 0.6552 0.147 Uiso 1 1 calc R . . H12C H 0.1643 0.3345 0.7212 0.147 Uiso 1 1 calc R . . C22 C 0.0149(4) 0.0689(2) 0.3143(3) 0.0321(8) Uani 1 1 d . . . H8 H 0.1043 0.0839 0.2988 0.039 Uiso 1 1 calc R . . C23 C -0.1141(6) 0.1048(3) 0.2243(5) 0.0445(13) Uani 1 1 d . . . H9A H -0.2030 0.0943 0.2409 0.067 Uiso 1 1 calc R . . H9B H -0.1242 0.0885 0.1455 0.067 Uiso 1 1 calc R . . H9C H -0.0979 0.1548 0.2288 0.067 Uiso 1 1 calc R . . C24 C 0.0025(5) -0.0095(2) 0.2971(4) 0.0453(10) Uani 1 1 d . . . H7A H 0.0867 -0.0319 0.3546 0.068 Uiso 1 1 calc R . . H7B H -0.0003 -0.0210 0.2177 0.068 Uiso 1 1 calc R . . H7C H -0.0868 -0.0258 0.3080 0.068 Uiso 1 1 calc R . . C25 C 0.4232(4) 0.40498(17) 0.3112(3) 0.0238(7) Uani 1 1 d . . . C26 C 0.5045(4) 0.4298(2) 0.4237(3) 0.0296(8) Uani 1 1 d . . . C27 C 0.5943(4) 0.4858(2) 0.4317(4) 0.0358(9) Uani 1 1 d . . . H15 H 0.6532 0.5016 0.5071 0.043 Uiso 1 1 calc R . . C28 C 0.6016(4) 0.5197(2) 0.3342(4) 0.0385(9) Uani 1 1 d . . . H16 H 0.6622 0.5590 0.3425 0.046 Uiso 1 1 calc R . . C29 C 0.5191(4) 0.49558(19) 0.2231(4) 0.0333(8) Uani 1 1 d . . . H17 H 0.5233 0.5190 0.1556 0.040 Uiso 1 1 calc R . . C30 C 0.4303(3) 0.43744(18) 0.2094(3) 0.0235(7) Uani 1 1 d . . . C31 C 0.4905(5) 0.3919(3) 0.5305(4) 0.0430(10) Uani 1 1 d . . . H20 H 0.4661 0.3427 0.5074 0.052 Uiso 1 1 calc R . . C32 C 0.6255(7) 0.3921(4) 0.6354(5) 0.0712(17) Uani 1 1 d . . . H19A H 0.6469 0.4393 0.6651 0.107 Uiso 1 1 calc R . . H19B H 0.7067 0.3746 0.6136 0.107 Uiso 1 1 calc R . . H19C H 0.6119 0.3626 0.6963 0.107 Uiso 1 1 calc R . . C33 C 0.3624(6) 0.4227(3) 0.5593(5) 0.0521(12) Uani 1 1 d . . . H21A H 0.3541 0.3998 0.6286 0.078 Uiso 1 1 calc R . . H21B H 0.2725 0.4159 0.4926 0.078 Uiso 1 1 calc R . . H21C H 0.3788 0.4722 0.5750 0.078 Uiso 1 1 calc R . . C34 C 0.3457(5) 0.4067(2) 0.0903(4) 0.0338(9) Uani 1 1 d . . . H23 H 0.2470 0.3941 0.0911 0.041 Uiso 1 1 calc R . . C35 C 0.3249(7) 0.4555(3) -0.0120(4) 0.0613(15) Uani 1 1 d . . . H24A H 0.2865 0.4996 0.0042 0.092 Uiso 1 1 calc R . . H24B H 0.2561 0.4353 -0.0835 0.092 Uiso 1 1 calc R . . H24C H 0.4185 0.4632 -0.0227 0.092 Uiso 1 1 calc R . . C36 C 0.4190(5) 0.3401(3) 0.0715(4) 0.0435(10) Uani 1 1 d . . . H22A H 0.5117 0.3513 0.0615 0.065 Uiso 1 1 calc R . . H22B H 0.3555 0.3165 0.0012 0.065 Uiso 1 1 calc R . . H22C H 0.4367 0.3099 0.1397 0.065 Uiso 1 1 calc R . . C37 C 0.4888(6) 0.1361(3) 0.4456(6) 0.0664(18) Uani 1 1 d . . . H37A H 0.4121 0.1311 0.4812 0.080 Uiso 1 1 calc R A 1 H37B H 0.4851 0.0950 0.3963 0.080 Uiso 1 1 calc R A 1 C38 C 0.6195(10) 0.1390(8) 0.5314(10) 0.083(4) Uani 0.74(3) 1 d PU A 1 H38A H 0.6720 0.0947 0.5384 0.100 Uiso 0.74(3) 1 calc PR A 1 H38B H 0.6092 0.1503 0.6077 0.100 Uiso 0.74(3) 1 calc PR A 1 C39 C 0.7041(7) 0.2010(5) 0.4885(9) 0.103(3) Uani 1 1 d . . . H39A H 0.7297 0.2392 0.5460 0.123 Uiso 1 1 calc R A 1 H39B H 0.7938 0.1836 0.4779 0.123 Uiso 1 1 calc R A 1 C40 C 0.5983(5) 0.2234(3) 0.3768(5) 0.0563(14) Uani 1 1 d . A . H40A H 0.5952 0.2744 0.3719 0.068 Uiso 1 1 calc R . . H40B H 0.6245 0.2052 0.3105 0.068 Uiso 1 1 calc R . . C41 C -0.1066(4) 0.3100(2) 0.3211(4) 0.0400(10) Uani 1 1 d . . . H44A H -0.0734 0.2850 0.3967 0.048 Uiso 1 1 calc R . . H44B H -0.1784 0.2812 0.2617 0.048 Uiso 1 1 calc R . . C42 C -0.1713(5) 0.3791(2) 0.3337(4) 0.0383(9) Uani 1 1 d . . . H43A H -0.1177 0.4009 0.4101 0.046 Uiso 1 1 calc R . . H43B H -0.2752 0.3748 0.3252 0.046 Uiso 1 1 calc R . . C43 C -0.1519(5) 0.4194(2) 0.2318(5) 0.0343(10) Uani 1 1 d . . . H42A H -0.2276 0.4071 0.1564 0.041 Uiso 1 1 calc R . . H42B H -0.1548 0.4698 0.2443 0.041 Uiso 1 1 calc R . . C44 C -0.0038(5) 0.3967(2) 0.2350(4) 0.0386(9) Uani 1 1 d . . . H41A H 0.0018 0.3964 0.1551 0.046 Uiso 1 1 calc R . . H41B H 0.0723 0.4279 0.2850 0.046 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 Nd1 0.02091(7) 0.01839(8) 0.01977(7) 0.00003(11) 0.00928(5) -0.00164(10) O1 0.0284(12) 0.0304(14) 0.0221(11) -0.0089(10) 0.0066(10) 0.0000(10) O2 0.0278(11) 0.0201(12) 0.0269(12) 0.0033(9) 0.0145(10) -0.0053(9) O3 0.0240(12) 0.0226(12) 0.0456(15) 0.0027(11) 0.0153(11) -0.0036(10) O4 0.0263(13) 0.0316(14) 0.0478(16) 0.0141(12) 0.0114(12) 0.0039(11) O5 0.0303(13) 0.0258(13) 0.0482(16) 0.0098(11) 0.0247(12) 0.0051(10) C1 0.0318(18) 0.038(2) 0.0221(16) -0.0073(15) 0.0137(14) -0.0092(15) C2 0.048(2) 0.035(2) 0.0278(18) -0.0062(16) 0.0201(17) -0.0096(17) C3 0.071(3) 0.050(3) 0.045(2) -0.022(2) 0.038(2) -0.029(2) C4 0.060(3) 0.088(4) 0.037(2) -0.029(3) 0.026(2) -0.046(3) C5 0.035(2) 0.101(5) 0.026(2) -0.013(2) 0.0109(17) -0.022(2) C6 0.0298(19) 0.065(3) 0.0185(19) -0.008(2) 0.0133(16) -0.0094(19) C7 0.053(3) 0.031(2) 0.047(2) -0.0018(18) 0.025(2) 0.000(2) C8 0.040(2) 0.044(3) 0.086(4) 0.005(3) 0.032(3) 0.005(2) C9 0.096(4) 0.035(3) 0.076(4) 0.005(2) 0.041(3) 0.013(3) C10 0.0349(17) 0.084(4) 0.0276(15) -0.001(3) 0.0089(13) 0.020(3) C11 0.063(3) 0.071(4) 0.044(3) 0.011(3) 0.027(3) 0.020(3) C12 0.035(2) 0.156(9) 0.058(3) 0.007(5) 0.015(2) 0.022(4) C13 0.0194(14) 0.0223(16) 0.0241(15) 0.0033(13) 0.0090(12) 0.0036(12) C14 0.0262(16) 0.0283(17) 0.0275(17) 0.0034(14) 0.0119(14) 0.0043(13) C15 0.047(2) 0.040(2) 0.0269(17) 0.0047(16) 0.0198(17) 0.0055(17) C16 0.047(2) 0.033(2) 0.044(2) 0.0114(17) 0.0305(19) -0.0007(17) C17 0.037(2) 0.0232(17) 0.047(2) 0.0053(16) 0.0219(18) -0.0022(14) C18 0.0250(16) 0.0241(17) 0.0295(17) 0.0014(14) 0.0125(14) 0.0016(13) C19 0.0390(16) 0.033(3) 0.0345(15) -0.006(2) 0.0113(13) 0.003(2) C20 0.057(3) 0.053(4) 0.134(6) 0.004(3) -0.023(4) -0.011(2) C21 0.102(5) 0.076(4) 0.145(7) -0.069(5) 0.080(5) -0.029(4) C22 0.0326(18) 0.035(2) 0.0334(19) -0.0098(16) 0.0172(16) -0.0101(15) C23 0.058(3) 0.036(3) 0.038(2) 0.003(2) 0.014(2) -0.013(2) C24 0.048(2) 0.037(2) 0.051(3) -0.014(2) 0.016(2) -0.0020(19) C25 0.0203(15) 0.0155(15) 0.0365(18) 0.0030(13) 0.0108(14) 0.0022(12) C26 0.0227(16) 0.038(2) 0.0279(17) -0.0021(15) 0.0088(14) 0.0045(14) C27 0.0263(17) 0.037(2) 0.043(2) -0.0170(18) 0.0118(16) -0.0051(16) C28 0.0334(19) 0.0190(17) 0.066(3) -0.0126(18) 0.0206(19) -0.0073(14) C29 0.0328(18) 0.0237(18) 0.051(2) 0.0083(16) 0.0237(17) 0.0031(14) C30 0.0203(15) 0.0215(16) 0.0314(17) 0.0014(13) 0.0123(13) 0.0034(12) C31 0.042(2) 0.052(3) 0.037(2) 0.007(2) 0.0158(18) 0.0066(19) C32 0.061(3) 0.096(5) 0.051(3) 0.026(3) 0.014(3) -0.004(3) C33 0.058(3) 0.058(3) 0.056(3) 0.005(2) 0.041(2) 0.010(2) C34 0.028(2) 0.041(2) 0.033(2) -0.0071(18) 0.0119(17) 0.0063(18) C35 0.068(3) 0.083(4) 0.028(2) 0.010(2) 0.009(2) 0.028(3) C36 0.044(2) 0.040(2) 0.049(2) -0.018(2) 0.019(2) 0.0028(19) C37 0.049(3) 0.052(3) 0.105(5) 0.047(3) 0.034(3) 0.018(2) C38 0.052(4) 0.093(8) 0.087(6) 0.044(5) 0.001(4) 0.000(4) C39 0.045(3) 0.096(6) 0.131(7) 0.017(5) -0.015(4) 0.004(4) C40 0.028(2) 0.051(2) 0.093(4) 0.022(3) 0.025(2) 0.0055(18) C41 0.0311(19) 0.037(2) 0.062(3) 0.009(2) 0.0295(19) 0.0029(16) C42 0.036(2) 0.037(2) 0.051(2) 0.0055(18) 0.0271(19) 0.0104(17) C43 0.032(2) 0.025(2) 0.048(3) 0.0076(19) 0.0158(18) 0.0088(17) C44 0.038(2) 0.027(2) 0.060(3) 0.0123(19) 0.028(2) 0.0106(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O3 2.167(2) . ? Nd1 O1 2.170(2) . ? Nd1 O2 2.171(2) . ? Nd1 O5 2.457(3) . ? Nd1 O4 2.469(3) . ? O1 C1 1.349(4) . ? O2 C13 1.341(4) . ? O3 C25 1.338(4) . ? O4 C40 1.436(5) . ? O4 C37 1.437(5) . ? O5 C41 1.448(4) . ? O5 C44 1.461(5) . ? C1 C6 1.405(6) . ? C1 C2 1.411(6) . ? C2 C3 1.392(6) . ? C2 C7 1.510(7) . ? C3 C4 1.352(8) . ? C4 C5 1.413(9) . ? C5 C6 1.391(7) . ? C38A C39 1.22(2) . ? C38A C37 1.84(2) . ? C6 C10 1.526(10) . ? C7 C8 1.513(7) . ? C7 C9 1.538(7) . ? C10 C11 1.526(10) . ? C10 C12 1.532(6) . ? C13 C14 1.412(5) . ? C13 C18 1.417(5) . ? C14 C15 1.395(5) . ? C14 C19 1.516(7) . ? C15 C16 1.390(6) . ? C16 C17 1.382(6) . ? C17 C18 1.386(5) . ? C18 C22 1.510(5) . ? C19 C21 1.499(8) . ? C19 C20 1.505(7) . ? C22 C23 1.526(7) . ? C22 C24 1.534(6) . ? C25 C26 1.409(5) . ? C25 C30 1.410(5) . ? C26 C27 1.381(6) . ? C26 C31 1.537(6) . ? C27 C28 1.376(7) . ? C28 C29 1.394(6) . ? C29 C30 1.398(5) . ? C30 C34 1.520(5) . ? C31 C32 1.488(7) . ? C31 C33 1.533(6) . ? C34 C35 1.519(7) . ? C34 C36 1.531(6) . ? C37 C38 1.346(11) . ? C38 C39 1.642(14) . ? C39 C40 1.463(9) . ? C41 C42 1.512(6) . ? C42 C43 1.529(6) . ? C43 C44 1.504(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Nd1 O1 112.83(10) . . ? O3 Nd1 O2 133.87(10) . . ? O1 Nd1 O2 113.21(10) . . ? O3 Nd1 O5 84.87(9) . . ? O1 Nd1 O5 100.41(10) . . ? O2 Nd1 O5 84.30(9) . . ? O3 Nd1 O4 87.25(9) . . ? O1 Nd1 O4 102.50(10) . . ? O2 Nd1 O4 85.73(9) . . ? O5 Nd1 O4 157.06(10) . . ? C1 O1 Nd1 150.8(2) . . ? C13 O2 Nd1 173.2(2) . . ? C25 O3 Nd1 173.8(2) . . ? C40 O4 C37 106.9(3) . . ? C40 O4 Nd1 127.0(3) . . ? C37 O4 Nd1 125.4(3) . . ? C41 O5 C44 109.5(3) . . ? C41 O5 Nd1 128.1(2) . . ? C44 O5 Nd1 122.2(2) . . ? O1 C1 C6 119.2(4) . . ? O1 C1 C2 119.2(3) . . ? C6 C1 C2 121.6(4) . . ? C3 C2 C1 117.5(4) . . ? C3 C2 C7 123.6(4) . . ? C1 C2 C7 118.9(4) . . ? C4 C3 C2 122.5(5) . . ? C3 C4 C5 119.7(4) . . ? C6 C5 C4 120.6(5) . . ? C39 C38A C37 98.5(13) . . ? C5 C6 C1 118.1(5) . . ? C5 C6 C10 122.7(4) . . ? C1 C6 C10 119.2(4) . . ? C2 C7 C8 111.6(4) . . ? C2 C7 C9 113.7(5) . . ? C8 C7 C9 110.8(5) . . ? C6 C10 C11 111.1(4) . . ? C6 C10 C12 113.7(7) . . ? C11 C10 C12 110.2(6) . . ? O2 C13 C14 120.0(3) . . ? O2 C13 C18 119.6(3) . . ? C14 C13 C18 120.4(3) . . ? C15 C14 C13 118.6(3) . . ? C15 C14 C19 121.4(3) . . ? C13 C14 C19 120.0(3) . . ? C16 C15 C14 120.9(4) . . ? C17 C16 C15 119.9(4) . . ? C16 C17 C18 121.4(4) . . ? C17 C18 C13 118.6(3) . . ? C17 C18 C22 122.3(3) . . ? C13 C18 C22 119.0(3) . . ? C21 C19 C20 113.0(6) . . ? C21 C19 C14 113.8(4) . . ? C20 C19 C14 110.8(5) . . ? C18 C22 C23 111.1(4) . . ? C18 C22 C24 113.4(4) . . ? C23 C22 C24 110.4(4) . . ? O3 C25 C26 119.5(3) . . ? O3 C25 C30 119.4(3) . . ? C26 C25 C30 121.1(3) . . ? C27 C26 C25 118.2(4) . . ? C27 C26 C31 123.7(4) . . ? C25 C26 C31 118.1(4) . . ? C28 C27 C26 122.3(4) . . ? C27 C28 C29 119.3(4) . . ? C28 C29 C30 121.1(4) . . ? C29 C30 C25 118.1(3) . . ? C29 C30 C34 122.9(4) . . ? C25 C30 C34 118.9(3) . . ? C32 C31 C33 111.1(5) . . ? C32 C31 C26 114.2(4) . . ? C33 C31 C26 108.8(4) . . ? C35 C34 C30 114.2(4) . . ? C35 C34 C36 110.0(4) . . ? C30 C34 C36 110.0(3) . . ? C38 C37 O4 112.0(7) . . ? C38 C37 C38A 25.9(8) . . ? O4 C37 C38A 89.7(9) . . ? C37 C38 C39 103.6(6) . . ? C38A C39 C40 110.4(11) . . ? C38A C39 C38 30.9(11) . . ? C40 C39 C38 103.7(5) . . ? O4 C40 C39 106.4(5) . . ? O5 C41 C42 104.3(3) . . ? C41 C42 C43 101.5(3) . . ? C44 C43 C42 102.4(3) . . ? O5 C44 C43 105.5(3) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.176 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.073 # Attachment '- 8.ybthf2.CIF' data_ybthf2.CIF _database_code_depnum_ccdc_archive 'CCDC 845106' #TrackingRef '- 8.ybthf2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common work _chemical_melting_point ? _chemical_formula_moiety 'C44 H67 O5 Yb' _chemical_formula_sum 'C44 H67 O5 Yb' _chemical_formula_weight 849.02 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' 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.7148(16) _cell_length_b 19.483(3) _cell_length_c 12.344(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.053(11) _cell_angle_gamma 90.00 _cell_volume 2194.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 10375 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 25.00 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7808 _exptl_absorpt_correction_T_max 0.9378 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10375 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6228 _reflns_number_gt 5732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(8) _refine_ls_number_reflns 6228 _refine_ls_number_parameters 463 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Yb1 Yb 0.293307(11) 0.144000(18) 0.214168(11) 0.03799(6) Uani 1 1 d . . . O1 O 0.3611(3) 0.10076(18) 0.3753(3) 0.0539(8) Uani 1 1 d . . . O2 O 0.3566(3) 0.09036(17) 0.0957(3) 0.0498(8) Uani 1 1 d . . . O3 O 0.1789(3) 0.23250(17) 0.2070(3) 0.0520(8) Uani 1 1 d . . . O4 O 0.0679(3) 0.09097(19) 0.1288(3) 0.0610(10) Uani 1 1 d . . . O5 O 0.4897(3) 0.21524(18) 0.2246(3) 0.0588(9) Uani 1 1 d . . . C1 C 0.4344(4) 0.0573(3) 0.4588(4) 0.0513(12) Uani 1 1 d . . . C2 C 0.3724(6) -0.0043(3) 0.4737(4) 0.0621(14) Uani 1 1 d . . . C3 C 0.4542(8) -0.0502(4) 0.5558(6) 0.0877(19) Uani 1 1 d . . . H3 H 0.4115 -0.0924 0.5664 0.105 Uiso 1 1 calc R . . C4 C 0.5986(9) -0.0353(5) 0.6232(6) 0.106(3) Uani 1 1 d . . . H4 H 0.6560 -0.0680 0.6769 0.128 Uiso 1 1 calc R . . C5 C 0.6563(6) 0.0266(5) 0.6112(6) 0.094(2) Uani 1 1 d . . . H5 H 0.7529 0.0377 0.6601 0.112 Uiso 1 1 calc R . . C6 C 0.5807(6) 0.0726(4) 0.5323(5) 0.070(2) Uani 1 1 d . . . C7 C 0.2120(9) -0.0193(5) 0.4036(7) 0.089(3) Uani 1 1 d . . . H7 H 0.1923 0.0016 0.3257 0.106 Uiso 1 1 calc R . . C8 C 0.1137(8) 0.0159(5) 0.4557(10) 0.112(3) Uani 1 1 d . . . H8A H 0.0114 0.0072 0.4083 0.168 Uiso 1 1 calc R . . H8B H 0.1327 0.0654 0.4592 0.168 Uiso 1 1 calc R . . H8C H 0.1324 -0.0018 0.5337 0.168 Uiso 1 1 calc R . . C9 C 0.1759(10) -0.0948(5) 0.3847(9) 0.128(3) Uani 1 1 d . . . H9A H 0.1680 -0.1147 0.4553 0.192 Uiso 1 1 calc R . . H9B H 0.2537 -0.1182 0.3654 0.192 Uiso 1 1 calc R . . H9C H 0.0825 -0.1003 0.3213 0.192 Uiso 1 1 calc R . . C10 C 0.6422(5) 0.1414(9) 0.5176(4) 0.091(2) Uani 1 1 d . . . H10 H 0.6012 0.1531 0.4337 0.109 Uiso 1 1 calc R . . C11 C 0.5869(12) 0.1950(7) 0.5810(11) 0.150(5) Uani 1 1 d . . . H11A H 0.4799 0.1979 0.5472 0.225 Uiso 1 1 calc R . . H11B H 0.6298 0.2397 0.5743 0.225 Uiso 1 1 calc R . . H11C H 0.6152 0.1823 0.6625 0.225 Uiso 1 1 calc R . . C12 C 0.8089(5) 0.1410(11) 0.5514(8) 0.194(6) Uani 1 1 d . . . H12A H 0.8528 0.1238 0.6305 0.291 Uiso 1 1 calc R . . H12B H 0.8437 0.1878 0.5470 0.291 Uiso 1 1 calc R . . H12C H 0.8371 0.1112 0.4986 0.291 Uiso 1 1 calc R . . C13 C 0.4041(4) 0.0515(2) 0.0279(4) 0.0441(11) Uani 1 1 d . . . C14 C 0.3886(4) 0.0722(3) -0.0849(4) 0.0517(12) Uani 1 1 d . . . C15 C 0.4417(5) 0.0304(4) -0.1524(5) 0.0699(16) Uani 1 1 d . . . H15 H 0.4311 0.0443 -0.2286 0.084 Uiso 1 1 calc R . . C16 C 0.5091(6) -0.0305(4) -0.1113(6) 0.0768(18) Uani 1 1 d . . . H16 H 0.5468 -0.0582 -0.1579 0.092 Uiso 1 1 calc R . . C17 C 0.5220(5) -0.0514(3) -0.0015(6) 0.0732(16) Uani 1 1 d . . . H17 H 0.5667 -0.0944 0.0255 0.088 Uiso 1 1 calc R . . C18 C 0.4722(4) -0.0119(3) 0.0709(5) 0.0564(13) Uani 1 1 d . . . C19 C 0.3156(4) 0.1396(6) -0.1309(4) 0.0725(15) Uani 1 1 d . . . H19 H 0.3001 0.1642 -0.0649 0.087 Uiso 1 1 calc R . . C20 C 0.4070(10) 0.1854(6) -0.1762(10) 0.148(4) Uani 1 1 d . . . H20A H 0.4155 0.1653 -0.2464 0.222 Uiso 1 1 calc R . . H20B H 0.5048 0.1902 -0.1179 0.222 Uiso 1 1 calc R . . H20C H 0.3606 0.2306 -0.1939 0.222 Uiso 1 1 calc R . . C21 C 0.1637(8) 0.1272(7) -0.2213(8) 0.160(6) Uani 1 1 d . . . H21A H 0.1233 0.1709 -0.2579 0.239 Uiso 1 1 calc R . . H21B H 0.0986 0.1077 -0.1838 0.239 Uiso 1 1 calc R . . H21C H 0.1722 0.0952 -0.2799 0.239 Uiso 1 1 calc R . . C22 C 0.4923(6) -0.0333(4) 0.1923(6) 0.0773(18) Uani 1 1 d . . . H22 H 0.4132 -0.0108 0.2144 0.093 Uiso 1 1 calc R . . C23 C 0.6363(12) -0.0085(6) 0.2745(8) 0.104(3) Uani 1 1 d . . . H23A H 0.7162 -0.0335 0.2605 0.156 Uiso 1 1 calc R . . H23B H 0.6404 -0.0167 0.3539 0.156 Uiso 1 1 calc R . . H23C H 0.6464 0.0407 0.2629 0.156 Uiso 1 1 calc R . . C24 C 0.4811(8) -0.1104(4) 0.2080(8) 0.120(3) Uani 1 1 d . . . H24A H 0.5601 -0.1337 0.1900 0.180 Uiso 1 1 calc R . . H24B H 0.3862 -0.1269 0.1560 0.180 Uiso 1 1 calc R . . H24C H 0.4899 -0.1202 0.2879 0.180 Uiso 1 1 calc R . . C25 C 0.0969(4) 0.2885(2) 0.1993(4) 0.0458(11) Uani 1 1 d . . . C26 C 0.0173(4) 0.3152(3) 0.0877(5) 0.0581(14) Uani 1 1 d . . . C27 C -0.0673(5) 0.3723(3) 0.0813(6) 0.0733(17) Uani 1 1 d . . . H27 H -0.1227 0.3902 0.0076 0.088 Uiso 1 1 calc R . . C28 C -0.0743(6) 0.4042(3) 0.1775(8) 0.087(2) Uani 1 1 d . . . H28 H -0.1327 0.4442 0.1702 0.105 Uiso 1 1 calc R . . C29 C 0.0032(6) 0.3785(3) 0.2856(7) 0.0781(19) Uani 1 1 d . . . H29 H -0.0028 0.4009 0.3522 0.094 Uiso 1 1 calc R . . C30 C 0.0896(4) 0.3204(3) 0.2978(5) 0.0539(13) Uani 1 1 d . . . C31 C 0.0299(6) 0.2805(4) -0.0192(5) 0.0752(17) Uani 1 1 d . . . H31 H 0.0649 0.2327 0.0041 0.090 Uiso 1 1 calc R . . C32 C 0.1471(9) 0.3151(5) -0.0557(8) 0.126(3) Uani 1 1 d . . . H32A H 0.1561 0.2912 -0.1228 0.189 Uiso 1 1 calc R . . H32B H 0.2410 0.3133 0.0080 0.189 Uiso 1 1 calc R . . H32C H 0.1198 0.3630 -0.0759 0.189 Uiso 1 1 calc R . . C33 C -0.1127(8) 0.2741(6) -0.1151(7) 0.135(3) Uani 1 1 d . . . H33A H -0.1835 0.2508 -0.0871 0.203 Uiso 1 1 calc R . . H33B H -0.0992 0.2474 -0.1779 0.203 Uiso 1 1 calc R . . H33C H -0.1494 0.3199 -0.1433 0.203 Uiso 1 1 calc R . . C34 C 0.1730(7) 0.2881(5) 0.4142(7) 0.073(2) Uani 1 1 d . . . H34 H 0.2677 0.2704 0.4103 0.087 Uiso 1 1 calc R . . C35 C 0.2107(11) 0.3394(6) 0.5163(7) 0.142(4) Uani 1 1 d . . . H35A H 0.2447 0.3827 0.4938 0.213 Uiso 1 1 calc R . . H35B H 0.2880 0.3201 0.5830 0.213 Uiso 1 1 calc R . . H35C H 0.1231 0.3480 0.5366 0.213 Uiso 1 1 calc R . . C36 C 0.0921(8) 0.2284(5) 0.4387(7) 0.096(2) Uani 1 1 d . . . H36A H 0.0078 0.2450 0.4576 0.144 Uiso 1 1 calc R . . H36B H 0.1575 0.2024 0.5041 0.144 Uiso 1 1 calc R . . H36C H 0.0580 0.1987 0.3707 0.144 Uiso 1 1 calc R . . C37 C 0.0401(6) 0.0318(4) 0.0542(8) 0.104(3) Uani 1 1 d . . . H37A H 0.0636 -0.0109 0.1002 0.124 Uiso 1 1 calc R . . H37B H 0.1004 0.0337 0.0039 0.124 Uiso 1 1 calc R . . C38 C -0.1144(6) 0.0343(6) -0.0142(9) 0.152(5) Uani 1 1 d . . . H38A H -0.1273 0.0466 -0.0949 0.182 Uiso 1 1 calc R . . H38B H -0.1598 -0.0112 -0.0140 0.182 Uiso 1 1 calc R . . C39 C -0.1819(6) 0.0845(5) 0.0349(9) 0.129(4) Uani 1 1 d . . . H39A H -0.2609 0.0631 0.0570 0.154 Uiso 1 1 calc R . . H39B H -0.2257 0.1211 -0.0221 0.154 Uiso 1 1 calc R . . C40 C -0.0712(4) 0.1136(3) 0.1362(6) 0.0806(19) Uani 1 1 d . . . H40A H -0.0773 0.1643 0.1352 0.097 Uiso 1 1 calc R . . H40B H -0.0837 0.0965 0.2078 0.097 Uiso 1 1 calc R . . C41 C 0.6125(5) 0.1983(3) 0.1878(7) 0.0805(19) Uani 1 1 d . . . H41A H 0.5780 0.1750 0.1118 0.097 Uiso 1 1 calc R . . H41B H 0.6824 0.1677 0.2445 0.097 Uiso 1 1 calc R . . C42 C 0.6816(6) 0.2639(4) 0.1802(7) 0.091(2) Uani 1 1 d . . . H42A H 0.6373 0.2844 0.1025 0.109 Uiso 1 1 calc R . . H42B H 0.7882 0.2581 0.1969 0.109 Uiso 1 1 calc R . . C43 C 0.6530(8) 0.3078(6) 0.2699(9) 0.085(3) Uani 1 1 d . . . H43A H 0.6514 0.3571 0.2500 0.102 Uiso 1 1 calc R . . H43B H 0.7280 0.3002 0.3468 0.102 Uiso 1 1 calc R . . C44 C 0.5046(6) 0.2841(3) 0.2672(7) 0.0756(18) Uani 1 1 d . . . H44A H 0.4982 0.2854 0.3455 0.091 Uiso 1 1 calc R . . H44B H 0.4266 0.3137 0.2157 0.091 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 0.03562(7) 0.04066(9) 0.03942(8) -0.00020(19) 0.01509(5) 0.00205(15) O1 0.0528(14) 0.063(2) 0.0457(16) 0.0130(16) 0.0168(14) -0.0017(14) O2 0.0510(13) 0.053(2) 0.0508(17) -0.0049(16) 0.0247(14) 0.0044(13) O3 0.0490(13) 0.0433(19) 0.065(2) 0.0010(17) 0.0211(14) 0.0093(13) O4 0.0414(13) 0.063(2) 0.077(2) -0.021(2) 0.0195(15) -0.0038(13) O5 0.0536(14) 0.048(2) 0.089(2) -0.0111(19) 0.0423(17) -0.0057(13) C1 0.058(2) 0.061(3) 0.042(2) 0.004(2) 0.026(2) 0.009(2) C2 0.080(3) 0.063(4) 0.050(3) 0.005(3) 0.032(3) 0.009(3) C3 0.134(5) 0.069(4) 0.079(4) 0.023(4) 0.061(4) 0.025(4) C4 0.116(5) 0.138(8) 0.070(4) 0.044(5) 0.039(4) 0.064(5) C5 0.071(3) 0.150(8) 0.060(4) 0.029(5) 0.023(3) 0.029(4) C6 0.051(2) 0.107(6) 0.051(3) 0.006(4) 0.018(2) 0.008(3) C7 0.127(6) 0.075(6) 0.059(4) 0.005(4) 0.026(5) -0.030(5) C8 0.083(4) 0.100(7) 0.152(9) -0.028(7) 0.038(5) -0.014(5) C9 0.154(6) 0.091(6) 0.147(8) -0.022(6) 0.063(6) -0.044(5) C10 0.063(2) 0.148(7) 0.059(3) 0.010(8) 0.016(2) -0.022(7) C11 0.147(7) 0.146(11) 0.162(11) -0.019(9) 0.060(8) -0.067(7) C12 0.062(3) 0.309(16) 0.189(9) 0.095(15) 0.015(4) -0.042(9) C13 0.0341(16) 0.049(3) 0.049(2) -0.013(2) 0.0140(18) -0.0056(17) C14 0.0423(18) 0.064(3) 0.049(3) -0.010(3) 0.017(2) -0.006(2) C15 0.070(3) 0.093(5) 0.052(3) -0.014(3) 0.027(3) -0.007(3) C16 0.076(3) 0.081(5) 0.088(4) -0.038(4) 0.047(3) -0.007(3) C17 0.071(3) 0.057(4) 0.103(5) -0.013(4) 0.044(3) 0.010(2) C18 0.049(2) 0.055(3) 0.069(3) -0.003(3) 0.025(2) 0.002(2) C19 0.073(2) 0.087(4) 0.056(2) 0.013(6) 0.019(2) 0.005(5) C20 0.142(6) 0.115(8) 0.209(11) 0.062(8) 0.090(8) 0.011(6) C21 0.108(4) 0.140(15) 0.167(8) 0.035(8) -0.036(5) 0.030(6) C22 0.070(3) 0.094(5) 0.076(4) 0.021(4) 0.035(3) 0.032(3) C23 0.142(7) 0.092(8) 0.071(6) 0.015(5) 0.027(5) -0.008(7) C24 0.118(5) 0.096(6) 0.128(7) 0.045(6) 0.021(5) -0.021(4) C25 0.0315(16) 0.041(3) 0.069(3) -0.005(2) 0.0231(19) -0.0047(16) C26 0.047(2) 0.045(3) 0.083(4) 0.010(3) 0.022(2) 0.000(2) C27 0.072(3) 0.052(4) 0.103(5) 0.027(4) 0.039(3) 0.012(2) C28 0.079(3) 0.046(4) 0.149(7) 0.021(4) 0.054(4) 0.020(3) C29 0.076(3) 0.054(4) 0.129(6) -0.028(4) 0.067(4) -0.009(3) C30 0.0433(19) 0.057(3) 0.069(3) -0.012(3) 0.029(2) -0.0112(19) C31 0.084(3) 0.072(4) 0.069(4) 0.010(4) 0.026(3) 0.007(3) C32 0.148(6) 0.128(8) 0.146(7) -0.017(6) 0.108(6) -0.026(6) C33 0.122(5) 0.170(10) 0.091(5) -0.026(6) 0.007(5) -0.005(6) C34 0.067(3) 0.084(6) 0.072(5) -0.014(4) 0.028(3) -0.010(3) C35 0.206(9) 0.144(9) 0.083(5) -0.040(6) 0.058(6) -0.068(8) C36 0.107(5) 0.091(6) 0.093(5) 0.010(5) 0.038(4) -0.011(4) C37 0.057(3) 0.095(6) 0.147(7) -0.070(6) 0.019(4) -0.012(3) C38 0.064(3) 0.201(11) 0.168(9) -0.128(9) 0.010(4) -0.016(5) C39 0.061(3) 0.138(8) 0.168(8) -0.065(7) 0.014(4) -0.007(4) C40 0.043(2) 0.084(4) 0.122(5) -0.030(4) 0.038(3) -0.010(2) C41 0.071(3) 0.072(4) 0.124(5) -0.023(4) 0.067(3) -0.016(3) C42 0.078(3) 0.082(5) 0.135(6) -0.013(5) 0.067(4) -0.028(3) C43 0.069(3) 0.065(5) 0.126(8) -0.008(5) 0.039(4) 0.001(3) C44 0.074(3) 0.057(4) 0.111(5) -0.030(4) 0.051(3) -0.014(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb1 O3 2.037(3) . ? Yb1 O1 2.049(3) . ? Yb1 O2 2.055(3) . ? Yb1 O4 2.322(3) . ? Yb1 O5 2.327(3) . ? O1 C1 1.336(6) . ? O2 C13 1.323(5) . ? O3 C25 1.334(5) . ? O4 C37 1.441(7) . ? O4 C40 1.454(5) . ? O5 C44 1.430(7) . ? O5 C41 1.453(6) . ? C1 C2 1.383(8) . ? C1 C6 1.431(7) . ? C2 C3 1.380(8) . ? C2 C7 1.529(9) . ? C3 C4 1.395(10) . ? C4 C5 1.360(12) . ? C5 C6 1.342(10) . ? C6 C10 1.505(16) . ? C7 C8 1.488(12) . ? C7 C9 1.512(12) . ? C10 C11 1.510(16) . ? C10 C12 1.527(7) . ? C13 C14 1.406(7) . ? C13 C18 1.417(7) . ? C14 C15 1.386(8) . ? C14 C19 1.508(12) . ? C15 C16 1.365(9) . ? C16 C17 1.379(9) . ? C17 C18 1.385(8) . ? C18 C22 1.503(8) . ? C19 C20 1.496(12) . ? C19 C21 1.533(7) . ? C22 C23 1.498(11) . ? C22 C24 1.524(11) . ? C25 C30 1.390(7) . ? C25 C26 1.427(7) . ? C26 C27 1.370(8) . ? C26 C31 1.525(8) . ? C27 C28 1.362(10) . ? C28 C29 1.381(10) . ? C29 C30 1.386(8) . ? C30 C34 1.523(10) . ? C31 C33 1.487(8) . ? C31 C32 1.518(10) . ? C34 C36 1.491(11) . ? C34 C35 1.551(12) . ? C37 C38 1.448(8) . ? C38 C39 1.424(11) . ? C39 C40 1.456(8) . ? C41 C42 1.463(9) . ? C42 C43 1.499(12) . ? C43 C44 1.504(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Yb1 O1 112.28(14) . . ? O3 Yb1 O2 133.74(13) . . ? O1 Yb1 O2 113.97(13) . . ? O3 Yb1 O4 86.63(11) . . ? O1 Yb1 O4 101.36(13) . . ? O2 Yb1 O4 85.20(12) . . ? O3 Yb1 O5 85.55(12) . . ? O1 Yb1 O5 101.93(12) . . ? O2 Yb1 O5 84.45(12) . . ? O4 Yb1 O5 156.69(14) . . ? C1 O1 Yb1 156.7(3) . . ? C13 O2 Yb1 174.3(3) . . ? C25 O3 Yb1 176.7(3) . . ? C37 O4 C40 107.9(4) . . ? C37 O4 Yb1 125.9(3) . . ? C40 O4 Yb1 126.1(3) . . ? C44 O5 C41 109.8(4) . . ? C44 O5 Yb1 123.9(3) . . ? C41 O5 Yb1 126.3(3) . . ? O1 C1 C2 120.8(4) . . ? O1 C1 C6 120.5(5) . . ? C2 C1 C6 118.6(5) . . ? C3 C2 C1 119.5(5) . . ? C3 C2 C7 120.6(6) . . ? C1 C2 C7 119.7(5) . . ? C2 C3 C4 120.7(7) . . ? C5 C4 C3 119.2(6) . . ? C6 C5 C4 121.9(6) . . ? C5 C6 C1 119.9(7) . . ? C5 C6 C10 122.8(6) . . ? C1 C6 C10 117.3(6) . . ? C8 C7 C9 111.4(8) . . ? C8 C7 C2 110.4(7) . . ? C9 C7 C2 114.3(7) . . ? C6 C10 C11 109.1(6) . . ? C6 C10 C12 112.9(12) . . ? C11 C10 C12 113.2(11) . . ? O2 C13 C14 121.4(4) . . ? O2 C13 C18 118.8(4) . . ? C14 C13 C18 119.8(5) . . ? C15 C14 C13 119.5(5) . . ? C15 C14 C19 120.6(5) . . ? C13 C14 C19 119.9(5) . . ? C16 C15 C14 121.1(6) . . ? C15 C16 C17 119.5(6) . . ? C16 C17 C18 122.3(6) . . ? C17 C18 C13 117.7(5) . . ? C17 C18 C22 122.3(5) . . ? C13 C18 C22 120.0(5) . . ? C20 C19 C14 113.4(5) . . ? C20 C19 C21 111.6(7) . . ? C14 C19 C21 110.4(8) . . ? C23 C22 C18 111.0(6) . . ? C23 C22 C24 108.8(6) . . ? C18 C22 C24 114.1(7) . . ? O3 C25 C30 120.8(4) . . ? O3 C25 C26 118.7(5) . . ? C30 C25 C26 120.5(4) . . ? C27 C26 C25 117.9(6) . . ? C27 C26 C31 122.3(6) . . ? C25 C26 C31 119.7(5) . . ? C28 C27 C26 121.9(6) . . ? C27 C28 C29 120.3(5) . . ? C28 C29 C30 120.6(6) . . ? C29 C30 C25 118.8(5) . . ? C29 C30 C34 123.2(6) . . ? C25 C30 C34 118.0(5) . . ? C33 C31 C32 113.0(7) . . ? C33 C31 C26 113.4(6) . . ? C32 C31 C26 110.5(6) . . ? C36 C34 C30 111.5(6) . . ? C36 C34 C35 109.4(8) . . ? C30 C34 C35 113.6(7) . . ? O4 C37 C38 106.0(6) . . ? C39 C38 C37 108.1(6) . . ? C38 C39 C40 108.7(5) . . ? O4 C40 C39 104.9(5) . . ? O5 C41 C42 105.4(5) . . ? C41 C42 C43 104.2(7) . . ? C42 C43 C44 103.2(7) . . ? O5 C44 C43 105.8(6) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.648 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.051 # Attachment '- 12.ydme2.cif' data_ydme2.CIF _database_code_depnum_ccdc_archive 'CCDC 845107' #TrackingRef '- 12.ydme2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Refine _chemical_melting_point ? _chemical_formula_moiety 'C44 H71 O7 Y' _chemical_formula_sum 'C44 H71 O7 Y' _chemical_formula_weight 800.92 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.373(2) _cell_length_b 19.227(2) _cell_length_c 16.652(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.782(9) _cell_angle_gamma 90.00 _cell_volume 4601.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 33768 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 27.10 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 1.311 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details XDS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71200 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Australian Synchrotron' _diffrn_radiation_monochromator 'Silicon Double Crystal' _diffrn_measurement_device_type 'ADSC Quantum 210r' _diffrn_measurement_method 'Phi Scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33768 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.10 _reflns_number_total 9679 _reflns_number_gt 8420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BluIce (McPhillips, 2002)' _computing_cell_refinement 'XDS (Kabsch, 1993)' _computing_data_reduction 'XDS (Kabsch, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.0678P)^2^+9.6495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method ? _refine_ls_extinction_coef none _refine_ls_number_reflns 9679 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.979637(18) 0.294004(13) 0.791845(15) 0.01688(9) Uani 1 1 d . . . O1 O 0.83970(14) 0.26715(11) 0.81128(13) 0.0217(4) Uani 1 1 d . . . O2 O 1.04490(15) 0.19651(10) 0.77995(13) 0.0223(4) Uani 1 1 d . . . O3 O 1.03721(14) 0.32520(11) 0.90254(12) 0.0226(4) Uani 1 1 d . . . O4 O 0.94236(16) 0.42187(11) 0.78026(14) 0.0286(5) Uani 1 1 d . . . O6 O 1.10077(16) 0.33177(13) 0.70048(14) 0.0302(5) Uani 1 1 d . . . O7 O 0.92946(17) 0.30563(13) 0.65159(13) 0.0305(5) Uani 1 1 d . . . O37 O 1.1040(2) 0.50959(15) 0.7664(2) 0.0482(7) Uani 1 1 d . . . C1 C 0.7565(2) 0.24449(15) 0.83508(16) 0.0196(6) Uani 1 1 d . . . C2 C 0.7455(2) 0.17425(16) 0.85938(18) 0.0230(6) Uani 1 1 d . . . C3 C 0.6582(2) 0.15156(17) 0.88307(19) 0.0298(7) Uani 1 1 d . . . H3 H 0.6505 0.1047 0.8997 0.036 Uiso 1 1 calc R . . C4 C 0.5823(3) 0.19567(19) 0.8829(2) 0.0338(8) Uani 1 1 d . . . H4 H 0.5229 0.1790 0.8984 0.041 Uiso 1 1 calc R . . C5 C 0.5935(2) 0.26452(18) 0.8599(2) 0.0294(7) Uani 1 1 d . . . H5 H 0.5414 0.2949 0.8600 0.035 Uiso 1 1 calc R . . C6 C 0.6795(2) 0.28969(16) 0.83673(17) 0.0221(6) Uani 1 1 d . . . C7 C 0.8273(2) 0.12452(16) 0.8524(2) 0.0281(7) Uani 1 1 d . . . H7 H 0.8853 0.1517 0.8637 0.034 Uiso 1 1 calc R . . C8 C 0.8330(2) 0.09717(17) 0.7668(2) 0.0303(7) Uani 1 1 d . . . H8A H 0.7756 0.0720 0.7531 0.046 Uiso 1 1 calc R . . H8B H 0.8862 0.0656 0.7626 0.046 Uiso 1 1 calc R . . H8C H 0.8407 0.1362 0.7297 0.046 Uiso 1 1 calc R . . C9 C 0.8252(3) 0.06390(19) 0.9114(3) 0.0455(10) Uani 1 1 d . . . H9A H 0.8166 0.0818 0.9659 0.068 Uiso 1 1 calc R . . H9B H 0.8840 0.0383 0.9091 0.068 Uiso 1 1 calc R . . H9C H 0.7736 0.0327 0.8972 0.068 Uiso 1 1 calc R . . C10 C 0.6901(2) 0.36497(15) 0.81021(18) 0.0235(6) Uani 1 1 d . . . H10 H 0.7582 0.3749 0.8059 0.028 Uiso 1 1 calc R . . C11 C 0.6458(3) 0.37586(19) 0.7272(2) 0.0353(8) Uani 1 1 d . . . H11A H 0.6744 0.3441 0.6887 0.053 Uiso 1 1 calc R . . H11B H 0.6556 0.4240 0.7101 0.053 Uiso 1 1 calc R . . H11C H 0.5789 0.3664 0.7297 0.053 Uiso 1 1 calc R . . C12 C 0.6496(3) 0.41672(19) 0.8696(2) 0.0421(9) Uani 1 1 d . . . H12A H 0.5818 0.4115 0.8706 0.063 Uiso 1 1 calc R . . H12B H 0.6653 0.4641 0.8530 0.063 Uiso 1 1 calc R . . H12C H 0.6756 0.4078 0.9233 0.063 Uiso 1 1 calc R . . C13 C 1.0646(2) 0.12893(15) 0.78382(18) 0.0211(6) Uani 1 1 d . . . C14 C 1.06285(19) 0.08842(15) 0.71311(18) 0.0212(6) Uani 1 1 d . . . C15 C 1.0780(2) 0.01710(16) 0.7191(2) 0.0270(7) Uani 1 1 d . . . H15 H 1.0764 -0.0105 0.6718 0.032 Uiso 1 1 calc R . . C16 C 1.0955(2) -0.01461(17) 0.7926(2) 0.0324(7) Uani 1 1 d . . . H16 H 1.1040 -0.0635 0.7958 0.039 Uiso 1 1 calc R . . C17 C 1.1004(2) 0.02561(16) 0.8611(2) 0.0315(7) Uani 1 1 d . . . H17 H 1.1139 0.0040 0.9113 0.038 Uiso 1 1 calc R . . C18 C 1.0860(2) 0.09762(16) 0.85834(19) 0.0256(7) Uani 1 1 d . . . C19 C 1.0456(2) 0.12431(17) 0.63377(19) 0.0244(6) Uani 1 1 d . . . H19 H 0.9988 0.1620 0.6426 0.029 Uiso 1 1 calc R . . C20 C 1.1359(2) 0.1588(2) 0.6055(2) 0.0389(8) Uani 1 1 d . . . H20A H 1.1586 0.1912 0.6469 0.058 Uiso 1 1 calc R . . H20B H 1.1237 0.1843 0.5555 0.058 Uiso 1 1 calc R . . H20C H 1.1830 0.1230 0.5962 0.058 Uiso 1 1 calc R . . C21 C 1.0075(3) 0.0767(2) 0.5676(2) 0.0385(8) Uani 1 1 d . . . H21A H 1.0536 0.0408 0.5555 0.058 Uiso 1 1 calc R . . H21B H 0.9944 0.1042 0.5192 0.058 Uiso 1 1 calc R . . H21C H 0.9500 0.0546 0.5857 0.058 Uiso 1 1 calc R . . C22 C 1.0961(3) 0.14341(17) 0.9317(2) 0.0366(9) Uani 1 1 d . . . H22 H 1.0468 0.1800 0.9279 0.044 Uiso 1 1 calc R . . C23 C 1.1906(3) 0.1805(2) 0.9293(3) 0.0528(12) Uani 1 1 d . . . H23A H 1.2407 0.1460 0.9331 0.079 Uiso 1 1 calc R . . H23B H 1.1958 0.2130 0.9745 0.079 Uiso 1 1 calc R . . H23C H 1.1957 0.2062 0.8787 0.079 Uiso 1 1 calc R . . C24 C 1.0835(4) 0.1057(2) 1.0114(2) 0.0615(15) Uani 1 1 d . . . H24A H 1.0258 0.0786 1.0093 0.092 Uiso 1 1 calc R . . H24B H 1.0804 0.1398 1.0550 0.092 Uiso 1 1 calc R . . H24C H 1.1364 0.0744 1.0210 0.092 Uiso 1 1 calc R . . C25 C 1.0657(2) 0.32764(15) 0.97906(17) 0.0206(6) Uani 1 1 d . . . C26 C 1.1498(2) 0.36173(15) 1.00046(19) 0.0226(6) Uani 1 1 d . . . C27 C 1.1801(2) 0.35994(17) 1.0809(2) 0.0292(7) Uani 1 1 d . . . H27 H 1.2367 0.3824 1.0955 0.035 Uiso 1 1 calc R . . C28 C 1.1297(2) 0.32642(18) 1.13930(19) 0.0314(7) Uani 1 1 d . . . H28 H 1.1525 0.3244 1.1931 0.038 Uiso 1 1 calc R . . C29 C 1.0452(3) 0.29564(17) 1.1185(2) 0.0298(7) Uani 1 1 d . . . H29 H 1.0099 0.2732 1.1588 0.036 Uiso 1 1 calc R . . C30 C 1.0114(2) 0.29706(16) 1.03955(19) 0.0254(6) Uani 1 1 d . . . C31 C 1.2065(2) 0.39819(17) 0.9373(2) 0.0278(7) Uani 1 1 d . . . H31 H 1.1704 0.3956 0.8856 0.033 Uiso 1 1 calc R . . C32 C 1.3003(2) 0.3632(2) 0.9235(2) 0.0399(9) Uani 1 1 d . . . H32A H 1.3376 0.3648 0.9732 0.060 Uiso 1 1 calc R . . H32B H 1.3332 0.3877 0.8808 0.060 Uiso 1 1 calc R . . H32C H 1.2903 0.3147 0.9077 0.060 Uiso 1 1 calc R . . C33 C 1.2205(3) 0.47526(19) 0.9570(2) 0.0448(10) Uani 1 1 d . . . H33A H 1.1601 0.4968 0.9674 0.067 Uiso 1 1 calc R . . H33B H 1.2497 0.4985 0.9114 0.067 Uiso 1 1 calc R . . H33C H 1.2608 0.4797 1.0046 0.067 Uiso 1 1 calc R . . C34 C 0.9146(2) 0.27053(19) 1.0166(2) 0.0316(7) Uani 1 1 d . . . H34 H 0.9201 0.2443 0.9650 0.038 Uiso 1 1 calc R . . C35 C 0.8498(2) 0.3329(2) 1.0008(2) 0.0385(9) Uani 1 1 d . . . H35A H 0.7885 0.3160 0.9832 0.058 Uiso 1 1 calc R . . H35B H 0.8762 0.3623 0.9588 0.058 Uiso 1 1 calc R . . H35C H 0.8435 0.3600 1.0502 0.058 Uiso 1 1 calc R . . C36 C 0.8712(4) 0.2221(3) 1.0772(3) 0.0549(12) Uani 1 1 d . . . H36A H 0.9139 0.1835 1.0887 0.082 Uiso 1 1 calc R . . H36B H 0.8125 0.2037 1.0553 0.082 Uiso 1 1 calc R . . H36C H 0.8590 0.2477 1.1269 0.082 Uiso 1 1 calc R . . C37 C 1.1605(4) 0.5663(3) 0.7410(4) 0.0676(15) Uani 1 1 d . . . H37A H 1.1235 0.5975 0.7067 0.101 Uiso 1 1 calc R . . H37B H 1.2134 0.5485 0.7108 0.101 Uiso 1 1 calc R . . H37C H 1.1834 0.5919 0.7882 0.101 Uiso 1 1 calc R . . C38 C 1.0233(3) 0.53357(19) 0.8077(3) 0.0427(9) Uani 1 1 d . . . H38A H 0.9826 0.5602 0.7704 0.051 Uiso 1 1 calc R . . H38B H 1.0422 0.5646 0.8525 0.051 Uiso 1 1 calc R . . C39 C 0.9708(3) 0.47147(19) 0.8402(2) 0.0398(9) Uani 1 1 d . . . H39A H 1.0107 0.4476 0.8805 0.048 Uiso 1 1 calc R . . H39B H 0.9148 0.4884 0.8681 0.048 Uiso 1 1 calc R . . C40 C 0.8792(3) 0.4532(2) 0.7219(2) 0.0407(9) Uani 1 1 d . . . H40A H 0.8309 0.4792 0.7500 0.061 Uiso 1 1 calc R . . H40B H 0.8502 0.4167 0.6890 0.061 Uiso 1 1 calc R . . H40C H 0.9140 0.4849 0.6873 0.061 Uiso 1 1 calc R . . C41 C 1.1935(2) 0.3477(2) 0.7259(2) 0.0405(9) Uani 1 1 d . . . H41A H 1.2361 0.3397 0.6814 0.061 Uiso 1 1 calc R . . H41B H 1.2111 0.3179 0.7713 0.061 Uiso 1 1 calc R . . H41C H 1.1970 0.3966 0.7424 0.061 Uiso 1 1 calc R . . C42 C 1.0731(3) 0.3652(3) 0.6275(2) 0.0490(10) Uani 1 1 d . . . H42A H 1.1263 0.3678 0.5904 0.059 Uiso 1 1 calc R . . H42B H 1.0514 0.4131 0.6385 0.059 Uiso 1 1 calc R . . C43 C 0.9956(3) 0.3228(2) 0.5905(2) 0.0410(9) Uani 1 1 d . . . H43A H 0.9646 0.3498 0.5472 0.049 Uiso 1 1 calc R . . H43B H 1.0211 0.2797 0.5669 0.049 Uiso 1 1 calc R . . C44 C 0.8474(3) 0.2732(2) 0.6184(2) 0.0431(9) Uani 1 1 d . . . H44A H 0.8140 0.3066 0.5842 0.065 Uiso 1 1 calc R . . H44B H 0.8070 0.2583 0.6621 0.065 Uiso 1 1 calc R . . H44C H 0.8653 0.2328 0.5863 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Y1 0.01901(14) 0.01366(14) 0.01775(14) -0.00223(10) -0.00812(10) -0.00003(10) O1 0.0212(10) 0.0157(10) 0.0281(11) -0.0014(8) -0.0056(8) -0.0005(8) O2 0.0278(11) 0.0138(9) 0.0249(10) -0.0022(8) -0.0101(9) 0.0034(8) O3 0.0242(10) 0.0226(11) 0.0207(10) -0.0042(8) -0.0077(8) -0.0053(9) O4 0.0304(12) 0.0179(10) 0.0375(13) -0.0052(9) -0.0049(10) 0.0024(9) O6 0.0272(12) 0.0324(13) 0.0310(12) 0.0019(10) 0.0006(9) 0.0007(10) O7 0.0325(12) 0.0379(13) 0.0209(11) -0.0046(9) -0.0098(9) 0.0022(10) O37 0.0416(15) 0.0336(14) 0.070(2) 0.0013(14) 0.0016(14) -0.0019(12) C1 0.0238(14) 0.0193(14) 0.0153(13) -0.0014(11) -0.0090(11) -0.0026(11) C2 0.0290(15) 0.0201(14) 0.0198(14) -0.0006(11) -0.0101(12) -0.0033(12) C3 0.0406(19) 0.0243(16) 0.0244(15) 0.0007(12) -0.0032(14) -0.0081(14) C4 0.0310(17) 0.0380(19) 0.0325(18) -0.0022(15) 0.0038(14) -0.0090(15) C5 0.0272(16) 0.0315(17) 0.0293(16) -0.0059(14) 0.0003(13) 0.0027(14) C6 0.0260(15) 0.0229(15) 0.0173(13) -0.0034(11) -0.0068(11) 0.0010(12) C7 0.0320(17) 0.0154(14) 0.0363(17) 0.0041(13) -0.0154(14) -0.0040(12) C8 0.0256(15) 0.0208(15) 0.0445(19) -0.0078(14) -0.0049(14) -0.0018(13) C9 0.060(3) 0.0249(18) 0.051(2) 0.0119(17) -0.019(2) 0.0010(17) C10 0.0273(15) 0.0193(14) 0.0235(15) -0.0006(11) -0.0078(12) 0.0038(12) C11 0.049(2) 0.0299(17) 0.0262(17) 0.0010(14) -0.0117(15) 0.0073(16) C12 0.069(3) 0.0254(18) 0.0315(18) -0.0067(15) -0.0048(18) 0.0081(18) C13 0.0201(14) 0.0161(13) 0.0268(15) -0.0013(11) -0.0091(11) 0.0000(11) C14 0.0152(13) 0.0200(14) 0.0283(15) -0.0044(12) -0.0043(11) 0.0016(11) C15 0.0226(15) 0.0200(15) 0.0383(18) -0.0080(13) -0.0043(13) 0.0036(12) C16 0.0342(18) 0.0165(14) 0.046(2) -0.0026(14) -0.0070(15) 0.0033(13) C17 0.0370(18) 0.0179(15) 0.0393(19) 0.0035(13) -0.0121(15) 0.0030(13) C18 0.0306(16) 0.0178(14) 0.0281(16) -0.0008(12) -0.0122(13) 0.0009(12) C19 0.0202(14) 0.0277(16) 0.0251(15) -0.0044(12) -0.0020(12) 0.0020(12) C20 0.0291(18) 0.048(2) 0.040(2) 0.0042(17) 0.0028(15) -0.0006(16) C21 0.045(2) 0.039(2) 0.0311(18) -0.0105(15) -0.0106(16) 0.0011(17) C22 0.060(2) 0.0191(15) 0.0303(17) -0.0001(13) -0.0245(17) 0.0067(15) C23 0.063(3) 0.033(2) 0.061(3) -0.0096(19) -0.040(2) -0.0001(19) C24 0.124(5) 0.034(2) 0.0252(19) 0.0020(16) -0.023(2) 0.008(3) C25 0.0240(14) 0.0177(14) 0.0199(14) -0.0027(11) -0.0084(11) -0.0014(11) C26 0.0244(15) 0.0173(13) 0.0259(15) -0.0016(11) -0.0120(12) 0.0001(12) C27 0.0287(16) 0.0298(17) 0.0286(16) -0.0008(13) -0.0164(13) -0.0007(13) C28 0.0390(18) 0.0333(18) 0.0216(15) 0.0004(13) -0.0153(13) 0.0037(15) C29 0.0371(18) 0.0285(17) 0.0237(15) 0.0005(13) -0.0044(13) 0.0004(14) C30 0.0294(16) 0.0234(15) 0.0234(15) -0.0040(12) -0.0050(12) -0.0028(13) C31 0.0281(16) 0.0254(16) 0.0294(16) 0.0006(13) -0.0124(13) -0.0071(13) C32 0.0263(17) 0.045(2) 0.048(2) 0.0076(18) -0.0048(16) -0.0044(16) C33 0.065(3) 0.0269(18) 0.042(2) 0.0012(16) -0.0119(19) -0.0186(18) C34 0.0343(18) 0.0369(18) 0.0238(15) -0.0051(14) -0.0010(13) -0.0132(15) C35 0.0267(17) 0.056(2) 0.0325(18) -0.0163(17) -0.0040(14) -0.0010(16) C36 0.063(3) 0.062(3) 0.039(2) 0.003(2) 0.002(2) -0.032(2) C37 0.052(3) 0.051(3) 0.099(4) 0.015(3) 0.001(3) -0.012(2) C38 0.049(2) 0.0226(17) 0.056(2) -0.0073(16) -0.0115(19) 0.0056(16) C39 0.047(2) 0.0258(17) 0.047(2) -0.0114(16) -0.0103(17) 0.0086(16) C40 0.049(2) 0.0292(18) 0.043(2) 0.0093(16) -0.0080(17) 0.0073(16) C41 0.0281(17) 0.051(2) 0.042(2) -0.0106(18) 0.0004(15) -0.0024(16) C42 0.050(2) 0.060(3) 0.037(2) 0.0138(19) 0.0066(18) 0.007(2) C43 0.049(2) 0.052(2) 0.0220(16) 0.0006(16) -0.0017(15) 0.0076(19) C44 0.041(2) 0.048(2) 0.039(2) -0.0025(17) -0.0256(17) 0.0001(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O3 2.098(2) . ? Y1 O1 2.106(2) . ? Y1 O2 2.107(2) . ? Y1 O6 2.438(2) . ? Y1 O7 2.445(2) . ? Y1 O4 2.523(2) . ? O1 C1 1.337(4) . ? O2 C13 1.331(3) . ? O3 C25 1.334(3) . ? O4 C39 1.436(4) . ? O4 C40 1.452(4) . ? O6 C41 1.426(4) . ? O6 C42 1.427(5) . ? O7 C44 1.437(4) . ? O7 C43 1.440(5) . ? O37 C37 1.427(5) . ? O37 C38 1.433(5) . ? C1 C6 1.408(4) . ? C1 C2 1.419(4) . ? C2 C3 1.391(5) . ? C2 C7 1.521(5) . ? C3 C4 1.382(5) . ? C4 C5 1.388(5) . ? C5 C6 1.387(5) . ? C6 C10 1.522(4) . ? C7 C8 1.522(5) . ? C7 C9 1.526(5) . ? C10 C12 1.524(5) . ? C10 C11 1.528(4) . ? C13 C18 1.409(4) . ? C13 C14 1.412(4) . ? C14 C15 1.392(4) . ? C14 C19 1.508(4) . ? C15 C16 1.388(5) . ? C16 C17 1.379(5) . ? C17 C18 1.401(4) . ? C18 C22 1.512(4) . ? C19 C21 1.528(4) . ? C19 C20 1.537(5) . ? C22 C24 1.525(5) . ? C22 C23 1.535(6) . ? C25 C30 1.411(4) . ? C25 C26 1.416(4) . ? C26 C27 1.403(4) . ? C26 C31 1.512(5) . ? C27 C28 1.381(5) . ? C28 C29 1.390(5) . ? C29 C30 1.396(4) . ? C30 C34 1.526(4) . ? C31 C32 1.527(5) . ? C31 C33 1.530(5) . ? C34 C36 1.515(5) . ? C34 C35 1.538(5) . ? C38 C39 1.516(6) . ? C42 C43 1.505(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Y1 O1 107.53(8) . . ? O3 Y1 O2 99.57(8) . . ? O1 Y1 O2 102.93(8) . . ? O3 Y1 O6 100.76(8) . . ? O1 Y1 O6 149.38(8) . . ? O2 Y1 O6 83.32(8) . . ? O3 Y1 O7 157.05(8) . . ? O1 Y1 O7 84.22(8) . . ? O2 Y1 O7 96.75(8) . . ? O6 Y1 O7 65.20(8) . . ? O3 Y1 O4 82.49(8) . . ? O1 Y1 O4 92.77(8) . . ? O2 Y1 O4 162.60(8) . . ? O6 Y1 O4 79.33(8) . . ? O7 Y1 O4 77.19(8) . . ? C1 O1 Y1 170.01(19) . . ? C13 O2 Y1 163.5(2) . . ? C25 O3 Y1 164.09(19) . . ? C39 O4 C40 111.0(3) . . ? C39 O4 Y1 122.4(2) . . ? C40 O4 Y1 125.9(2) . . ? C41 O6 C42 113.8(3) . . ? C41 O6 Y1 123.5(2) . . ? C42 O6 Y1 118.2(2) . . ? C44 O7 C43 112.0(3) . . ? C44 O7 Y1 123.9(2) . . ? C43 O7 Y1 120.4(2) . . ? C37 O37 C38 111.3(3) . . ? O1 C1 C6 120.7(3) . . ? O1 C1 C2 119.9(3) . . ? C6 C1 C2 119.4(3) . . ? C3 C2 C1 118.9(3) . . ? C3 C2 C7 121.7(3) . . ? C1 C2 C7 119.1(3) . . ? C4 C3 C2 121.5(3) . . ? C3 C4 C5 119.4(3) . . ? C6 C5 C4 121.2(3) . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C10 120.4(3) . . ? C1 C6 C10 120.0(3) . . ? C2 C7 C8 109.9(3) . . ? C2 C7 C9 114.1(3) . . ? C8 C7 C9 110.0(3) . . ? C6 C10 C12 113.1(3) . . ? C6 C10 C11 110.5(3) . . ? C12 C10 C11 109.8(3) . . ? O2 C13 C18 120.2(3) . . ? O2 C13 C14 119.8(3) . . ? C18 C13 C14 120.0(3) . . ? C15 C14 C13 118.9(3) . . ? C15 C14 C19 122.5(3) . . ? C13 C14 C19 118.6(3) . . ? C16 C15 C14 121.5(3) . . ? C17 C16 C15 119.3(3) . . ? C16 C17 C18 121.4(3) . . ? C17 C18 C13 118.8(3) . . ? C17 C18 C22 122.4(3) . . ? C13 C18 C22 118.7(3) . . ? C14 C19 C21 114.2(3) . . ? C14 C19 C20 109.7(3) . . ? C21 C19 C20 109.5(3) . . ? C18 C22 C24 114.5(3) . . ? C18 C22 C23 108.9(3) . . ? C24 C22 C23 111.1(3) . . ? O3 C25 C30 120.1(3) . . ? O3 C25 C26 120.4(3) . . ? C30 C25 C26 119.5(3) . . ? C27 C26 C25 118.8(3) . . ? C27 C26 C31 120.8(3) . . ? C25 C26 C31 120.4(3) . . ? C28 C27 C26 121.7(3) . . ? C27 C28 C29 119.2(3) . . ? C28 C29 C30 121.2(3) . . ? C29 C30 C25 119.4(3) . . ? C29 C30 C34 122.3(3) . . ? C25 C30 C34 118.2(3) . . ? C26 C31 C32 112.7(3) . . ? C26 C31 C33 111.8(3) . . ? C32 C31 C33 110.1(3) . . ? C36 C34 C30 114.9(3) . . ? C36 C34 C35 109.8(3) . . ? C30 C34 C35 109.3(3) . . ? O37 C38 C39 109.1(3) . . ? O4 C39 C38 114.4(3) . . ? O6 C42 C43 107.5(3) . . ? O7 C43 C42 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.951 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.091 # Attachment '- 7.ythf2.cif' data_ythf2.CIF _database_code_depnum_ccdc_archive 'CCDC 845108' #TrackingRef '- 7.ythf2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Y(DIP)3(THF)2 _chemical_melting_point ? _chemical_formula_moiety 'C44 H67 O5 Y' _chemical_formula_sum 'C44 H67 O5 Y' _chemical_formula_weight 764.89 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6897(14) _cell_length_b 19.343(3) _cell_length_c 12.182(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.559(9) _cell_angle_gamma 90.00 _cell_volume 2151.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 11351 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 24.99 _exptl_crystal_description colourless _exptl_crystal_colour block _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 1.395 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8504 _exptl_absorpt_correction_T_max 0.9593 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11351 _diffrn_reflns_av_R_equivalents 0.1898 _diffrn_reflns_av_sigmaI/netI 0.3940 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6783 _reflns_number_gt 3233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(13) _refine_ls_number_reflns 6783 _refine_ls_number_parameters 473 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1867 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2260 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 0.779 _refine_ls_restrained_S_all 0.776 _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 Y1 Y 0.71207(10) 0.75161(5) 0.78670(7) 0.0226(3) Uani 1 1 d . A . O1 O 0.6404(8) 0.7106(4) 0.6206(6) 0.034(2) Uani 1 1 d . . . O2 O 0.6494(8) 0.6949(4) 0.9061(6) 0.0274(18) Uani 1 1 d . . . O3 O 0.8275(8) 0.8437(4) 0.7965(6) 0.0270(19) Uani 1 1 d . . . O4 O 0.9368(9) 0.6971(4) 0.8672(7) 0.041(2) Uani 1 1 d . . . O5 O 0.5146(8) 0.8243(4) 0.7795(6) 0.034(2) Uani 1 1 d . . . C1 C 0.5581(13) 0.6660(6) 0.5382(9) 0.029(3) Uani 1 1 d U . . C2 C 0.6187(13) 0.6015(6) 0.5219(9) 0.034(3) Uani 1 1 d . . . C3 C 0.5353(19) 0.5555(7) 0.4426(11) 0.054(4) Uani 1 1 d . . . H3 H 0.5763 0.5123 0.4326 0.065 Uiso 1 1 calc R . . C4 C 0.3914(17) 0.5704(8) 0.3761(12) 0.054(4) Uani 1 1 d . . . H4 H 0.3323 0.5374 0.3233 0.064 Uiso 1 1 calc R . . C5 C 0.3369(15) 0.6347(9) 0.3889(10) 0.057(5) Uani 1 1 d . . . H5 H 0.2392 0.6458 0.3428 0.068 Uiso 1 1 calc R . . C6 C 0.4185(14) 0.6830(8) 0.4658(10) 0.038(4) Uani 1 1 d . . . C7 C 0.7776(17) 0.5861(8) 0.5935(12) 0.050(4) Uani 1 1 d . . . H7 H 0.7941 0.6051 0.6732 0.060 Uiso 1 1 calc R . . C8 C 0.8844(16) 0.6244(8) 0.5451(13) 0.053(4) Uani 1 1 d . . . H8A H 0.8712 0.6077 0.4662 0.079 Uiso 1 1 calc R . . H8B H 0.9853 0.6156 0.5955 0.079 Uiso 1 1 calc R . . H8C H 0.8646 0.6741 0.5427 0.079 Uiso 1 1 calc R . . C9 C 0.814(2) 0.5086(8) 0.6087(12) 0.073(5) Uani 1 1 d . . . H9A H 0.7425 0.4853 0.6373 0.110 Uiso 1 1 calc R . . H9B H 0.9124 0.5023 0.6648 0.110 Uiso 1 1 calc R . . H9C H 0.8088 0.4887 0.5335 0.110 Uiso 1 1 calc R . . C10 C 0.3591(12) 0.7563(11) 0.4808(8) 0.047(3) Uani 1 1 d . . . H10 H 0.3942 0.7667 0.5661 0.056 Uiso 1 1 calc R . . C11 C 0.4239(19) 0.8100(9) 0.4240(14) 0.067(5) Uani 1 1 d . . . H11A H 0.3916 0.8017 0.3399 0.101 Uiso 1 1 calc R . . H11B H 0.5310 0.8075 0.4561 0.101 Uiso 1 1 calc R . . H11C H 0.3915 0.8560 0.4390 0.101 Uiso 1 1 calc R . . C12 C 0.1960(15) 0.7602(14) 0.4396(11) 0.087(6) Uani 1 1 d . . . H12A H 0.1656 0.8023 0.4700 0.131 Uiso 1 1 calc R . . H12B H 0.1569 0.7196 0.4674 0.131 Uiso 1 1 calc R . . H12C H 0.1585 0.7612 0.3542 0.131 Uiso 1 1 calc R . . C13 C 0.5989(11) 0.6549(6) 0.9746(8) 0.020(2) Uani 1 1 d U . . C14 C 0.6103(12) 0.6767(6) 1.0881(9) 0.027(3) Uani 1 1 d . . . C15 C 0.5545(13) 0.6355(6) 1.1552(9) 0.034(3) Uani 1 1 d . . . H15 H 0.5633 0.6501 1.2317 0.041 Uiso 1 1 calc R . . C16 C 0.4856(15) 0.5733(7) 1.1139(10) 0.045(4) Uani 1 1 d . . . H16 H 0.4462 0.5459 1.1611 0.054 Uiso 1 1 calc R . . C17 C 0.4749(13) 0.5515(7) 1.0034(10) 0.037(3) Uani 1 1 d U . . H17 H 0.4297 0.5082 0.9762 0.044 Uiso 1 1 calc R . . C18 C 0.5285(12) 0.5910(6) 0.9298(8) 0.025(3) Uani 1 1 d . . . C19 C 0.6854(12) 0.7439(8) 1.1350(9) 0.036(3) Uani 1 1 d . . . H19 H 0.6941 0.7708 1.0675 0.044 Uiso 1 1 calc R . . C20 C 0.606(2) 0.7875(9) 1.1934(18) 0.117(8) Uani 1 1 d . . . H20A H 0.5042 0.7934 1.1420 0.176 Uiso 1 1 calc R . . H20B H 0.6532 0.8328 1.2112 0.176 Uiso 1 1 calc R . . H20C H 0.6068 0.7651 1.2659 0.176 Uiso 1 1 calc R . . C21 C 0.8368(18) 0.7328(10) 1.2184(15) 0.114(9) Uani 1 1 d . . . H21A H 0.8318 0.7077 1.2869 0.171 Uiso 1 1 calc R . . H21B H 0.8844 0.7776 1.2426 0.171 Uiso 1 1 calc R . . H21C H 0.8935 0.7057 1.1804 0.171 Uiso 1 1 calc R . . C22 C 0.5078(15) 0.5705(6) 0.8074(10) 0.039(3) Uani 1 1 d . . . H22 H 0.5933 0.5888 0.7879 0.047 Uiso 1 1 calc R . . C23 C 0.3711(18) 0.6026(8) 0.7229(11) 0.049(4) Uani 1 1 d . . . H23A H 0.2844 0.5808 0.7322 0.074 Uiso 1 1 calc R . . H23B H 0.3702 0.5956 0.6430 0.074 Uiso 1 1 calc R . . H23C H 0.3701 0.6523 0.7386 0.074 Uiso 1 1 calc R . . C24 C 0.5057(17) 0.4913(7) 0.7915(12) 0.066(5) Uani 1 1 d . . . H24A H 0.5904 0.4709 0.8513 0.099 Uiso 1 1 calc R . . H24B H 0.5099 0.4803 0.7142 0.099 Uiso 1 1 calc R . . H24C H 0.4153 0.4724 0.7988 0.099 Uiso 1 1 calc R . . C25 C 0.9156(12) 0.8992(5) 0.8086(9) 0.022(3) Uani 1 1 d . . . C26 C 0.9947(14) 0.9219(6) 0.9207(10) 0.036(3) Uani 1 1 d . . . C27 C 1.0855(14) 0.9806(7) 0.9311(10) 0.040(3) Uani 1 1 d . . . H27 H 1.1422 0.9969 1.0063 0.048 Uiso 1 1 calc R . . C28 C 1.0925(16) 1.0139(6) 0.8353(12) 0.049(4) Uani 1 1 d . . . H28 H 1.1532 1.0536 0.8441 0.058 Uiso 1 1 calc R . . C29 C 1.0130(14) 0.9911(7) 0.7256(10) 0.038(3) Uani 1 1 d U . . H29 H 1.0195 1.0151 0.6594 0.046 Uiso 1 1 calc R . . C30 C 0.9228(12) 0.9330(6) 0.7100(10) 0.030(3) Uani 1 1 d . . . C31 C 0.9802(14) 0.8868(7) 1.0271(10) 0.039(3) Uani 1 1 d . . . H31 H 0.9509 0.8379 1.0044 0.047 Uiso 1 1 calc R . . C32 C 0.8583(17) 0.9187(9) 1.0620(13) 0.072(5) Uani 1 1 d . . . H32A H 0.8454 0.8922 1.1265 0.107 Uiso 1 1 calc R . . H32B H 0.7671 0.9178 0.9953 0.107 Uiso 1 1 calc R . . H32C H 0.8836 0.9666 1.0866 0.107 Uiso 1 1 calc R . . C33 C 1.1178(16) 0.8839(8) 1.1264(11) 0.061(4) Uani 1 1 d . . . H33A H 1.1549 0.9309 1.1476 0.092 Uiso 1 1 calc R . . H33B H 1.1903 0.8568 1.1049 0.092 Uiso 1 1 calc R . . H33C H 1.0997 0.8621 1.1930 0.092 Uiso 1 1 calc R . . C34 C 0.8394(14) 0.9037(7) 0.5895(10) 0.033(3) Uani 1 1 d . . . H34 H 0.7401 0.8896 0.5895 0.040 Uiso 1 1 calc R . . C35 C 0.8176(17) 0.9559(8) 0.4896(11) 0.064(5) Uani 1 1 d . . . H35A H 0.7858 1.0003 0.5114 0.096 Uiso 1 1 calc R . . H35B H 0.7429 0.9384 0.4190 0.096 Uiso 1 1 calc R . . H35C H 0.9102 0.9620 0.4749 0.096 Uiso 1 1 calc R . . C36 C 0.9169(15) 0.8380(7) 0.5664(11) 0.050(4) Uani 1 1 d . . . H36A H 0.8510 0.8134 0.4988 0.075 Uiso 1 1 calc R . . H36B H 0.9425 0.8079 0.6349 0.075 Uiso 1 1 calc R . . H36C H 1.0061 0.8513 0.5508 0.075 Uiso 1 1 calc R . . C37 C 0.9658(15) 0.6347(8) 0.9397(13) 0.061(2) Uani 0.59(6) 1 d PU A 2 H37A H 0.9129 0.6379 0.9963 0.073 Uiso 0.59(6) 1 calc PR A 2 H37B H 0.9277 0.5939 0.8895 0.073 Uiso 0.59(6) 1 calc PR A 2 C37A C 0.9658(15) 0.6347(8) 0.9397(13) 0.061(2) Uani 0.41(6) 1 d PU A 1 H37C H 0.9780 0.5933 0.8959 0.073 Uiso 0.41(6) 1 calc PR A 1 H37D H 0.8883 0.6261 0.9741 0.073 Uiso 0.41(6) 1 calc PR A 1 C38 C 1.110(3) 0.626(2) 0.998(3) 0.061(2) Uani 0.59(6) 1 d PU A 2 H38A H 1.1461 0.5835 0.9701 0.073 Uiso 0.59(6) 1 calc PR A 2 H38B H 1.1276 0.6206 1.0825 0.073 Uiso 0.59(6) 1 calc PR A 2 C38A C 1.115(4) 0.657(3) 1.035(5) 0.061(2) Uani 0.41(6) 1 d PU A 1 H38C H 1.0970 0.6878 1.0940 0.073 Uiso 0.41(6) 1 calc PR A 1 H38D H 1.1713 0.6164 1.0748 0.073 Uiso 0.41(6) 1 calc PR A 1 C39 C 1.1930(15) 0.6932(8) 0.9737(12) 0.061(2) Uani 1 1 d U . . H39A H 1.2605 0.6616 0.9527 0.073 Uiso 1 1 calc R A 1 H39B H 1.2507 0.7313 1.0216 0.073 Uiso 1 1 calc R A 1 C40 C 1.0817(14) 0.7205(8) 0.8681(12) 0.060(2) Uani 1 1 d U A . H40A H 1.0855 0.7717 0.8681 0.072 Uiso 1 1 calc R B 1 H40B H 1.1006 0.7035 0.7978 0.072 Uiso 1 1 calc R B 1 C41 C 0.3855(14) 0.8060(7) 0.8161(11) 0.042(3) Uani 1 1 d . A . H41A H 0.3136 0.7776 0.7561 0.051 Uiso 1 1 calc R . . H41B H 0.4167 0.7807 0.8910 0.051 Uiso 1 1 calc R . . C42 C 0.3235(14) 0.8749(6) 0.8280(10) 0.039(3) Uani 1 1 d . . . H42A H 0.3762 0.8962 0.9045 0.047 Uiso 1 1 calc R A . H42B H 0.2179 0.8717 0.8177 0.047 Uiso 1 1 calc R . . C43 C 0.3495(17) 0.9154(8) 0.7273(12) 0.044(4) Uani 1 1 d . A . H43A H 0.2771 0.9023 0.6512 0.052 Uiso 1 1 calc R . . H43B H 0.3442 0.9659 0.7385 0.052 Uiso 1 1 calc R . . C44 C 0.4993(15) 0.8940(7) 0.7353(12) 0.044(4) Uani 1 1 d . A . H44A H 0.5112 0.8954 0.6577 0.053 Uiso 1 1 calc R . . H44B H 0.5734 0.9246 0.7889 0.053 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 0.0203(5) 0.0194(5) 0.0252(5) 0.0009(7) 0.0036(3) -0.0011(8) O1 0.036(5) 0.032(5) 0.027(4) -0.006(3) 0.003(3) -0.002(4) O2 0.019(5) 0.027(5) 0.034(4) 0.001(3) 0.005(3) 0.002(4) O3 0.012(4) 0.028(5) 0.037(4) 0.003(3) 0.003(3) -0.003(4) O4 0.035(6) 0.027(5) 0.051(5) 0.009(4) 0.000(4) 0.000(4) O5 0.020(5) 0.025(5) 0.056(5) 0.005(4) 0.012(4) 0.003(4) C1 0.029(3) 0.029(3) 0.029(3) -0.0002(10) 0.0099(13) -0.0006(10) C2 0.037(8) 0.030(8) 0.032(7) -0.001(5) 0.006(5) -0.016(6) C3 0.093(14) 0.038(9) 0.045(8) -0.019(6) 0.039(9) -0.021(9) C4 0.051(11) 0.053(11) 0.065(10) -0.035(7) 0.030(8) -0.027(9) C5 0.029(9) 0.115(16) 0.023(7) 0.006(7) 0.005(5) -0.017(9) C6 0.028(8) 0.057(11) 0.023(7) -0.004(6) -0.001(5) -0.018(7) C7 0.061(12) 0.032(10) 0.060(9) -0.011(6) 0.023(8) 0.004(8) C8 0.040(10) 0.044(11) 0.085(11) 0.004(8) 0.036(8) 0.002(8) C9 0.100(15) 0.055(12) 0.068(11) 0.008(8) 0.032(10) 0.021(10) C10 0.032(7) 0.075(11) 0.027(6) 0.001(9) 0.002(4) 0.007(11) C11 0.075(13) 0.062(13) 0.073(12) 0.006(9) 0.036(10) 0.028(10) C12 0.045(9) 0.142(18) 0.064(9) -0.018(13) 0.002(7) 0.019(15) C13 0.020(3) 0.020(3) 0.020(3) 0.0009(10) 0.0068(12) 0.0003(10) C14 0.025(7) 0.025(7) 0.030(6) 0.010(5) 0.007(5) 0.009(5) C15 0.035(8) 0.032(8) 0.025(6) 0.007(5) -0.003(5) 0.006(6) C16 0.044(9) 0.044(10) 0.049(8) 0.026(6) 0.019(6) 0.017(7) C17 0.037(3) 0.037(3) 0.037(3) 0.0006(10) 0.0122(14) 0.0000(10) C18 0.031(7) 0.019(7) 0.022(6) 0.001(4) 0.006(5) -0.002(5) C19 0.039(7) 0.034(8) 0.032(6) 0.002(6) 0.006(5) 0.003(8) C20 0.18(2) 0.041(12) 0.159(19) -0.048(11) 0.091(18) -0.009(13) C21 0.071(13) 0.07(2) 0.139(16) -0.013(11) -0.042(11) -0.011(10) C22 0.048(10) 0.024(8) 0.053(8) -0.011(6) 0.026(7) -0.011(6) C23 0.073(13) 0.033(9) 0.035(8) -0.003(6) 0.008(7) 0.001(9) C24 0.072(12) 0.029(9) 0.080(10) -0.031(7) 0.003(8) 0.002(8) C25 0.017(7) 0.009(6) 0.040(7) 0.004(5) 0.009(5) -0.007(5) C26 0.046(9) 0.020(7) 0.040(7) -0.013(5) 0.011(6) -0.004(6) C27 0.047(9) 0.023(8) 0.043(8) -0.004(5) 0.007(6) 0.010(7) C28 0.065(11) 0.014(7) 0.069(10) -0.017(6) 0.026(8) -0.008(7) C29 0.038(3) 0.038(3) 0.038(3) 0.0006(10) 0.0129(14) -0.0001(10) C30 0.016(7) 0.025(8) 0.045(7) 0.005(5) 0.007(5) 0.000(5) C31 0.034(9) 0.038(9) 0.037(7) -0.012(5) 0.002(6) -0.009(6) C32 0.078(13) 0.081(13) 0.072(11) 0.010(8) 0.047(9) 0.020(10) C33 0.065(12) 0.050(10) 0.059(9) 0.008(7) 0.008(7) -0.011(8) C34 0.020(8) 0.044(10) 0.034(7) 0.000(6) 0.006(6) 0.004(6) C35 0.081(13) 0.074(12) 0.035(8) 0.013(7) 0.016(7) 0.014(9) C36 0.053(10) 0.033(10) 0.058(9) -0.007(6) 0.010(7) 0.008(8) C37 0.030(5) 0.052(6) 0.089(6) 0.030(4) 0.005(4) 0.003(4) C37A 0.030(5) 0.052(6) 0.089(6) 0.030(4) 0.005(4) 0.003(4) C38 0.030(5) 0.052(6) 0.089(6) 0.030(4) 0.005(4) 0.003(4) C38A 0.030(5) 0.052(6) 0.089(6) 0.030(4) 0.005(4) 0.003(4) C39 0.030(5) 0.052(6) 0.089(6) 0.030(4) 0.005(4) 0.003(4) C40 0.030(5) 0.052(6) 0.089(6) 0.030(4) 0.006(4) 0.003(4) C41 0.034(9) 0.035(8) 0.064(9) 0.007(6) 0.024(7) 0.011(7) C42 0.039(9) 0.032(8) 0.057(8) 0.006(6) 0.029(6) 0.008(6) C43 0.043(10) 0.029(9) 0.048(9) 0.010(6) 0.002(7) 0.000(7) C44 0.048(10) 0.028(8) 0.066(9) 0.029(6) 0.032(7) 0.021(7) _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 O1 2.065(7) . ? Y1 O2 2.068(7) . ? Y1 O3 2.086(7) . ? Y1 O4 2.321(8) . ? Y1 O5 2.352(8) . ? O1 C1 1.360(12) . ? O2 C13 1.345(12) . ? O3 C25 1.348(12) . ? O4 C37 1.466(15) . ? O4 C40 1.472(15) . ? O5 C44 1.440(14) . ? O5 C41 1.504(14) . ? C1 C6 1.384(16) . ? C1 C2 1.420(17) . ? C2 C3 1.363(16) . ? C2 C7 1.524(18) . ? C3 C4 1.39(2) . ? C4 C5 1.38(2) . ? C5 C6 1.372(18) . ? C6 C10 1.56(2) . ? C7 C9 1.536(19) . ? C7 C8 1.541(19) . ? C10 C12 1.491(16) . ? C10 C11 1.50(2) . ? C13 C14 1.414(14) . ? C13 C18 1.429(15) . ? C14 C15 1.375(16) . ? C14 C19 1.506(18) . ? C15 C16 1.387(18) . ? C16 C17 1.382(16) . ? C17 C18 1.403(16) . ? C18 C22 1.490(14) . ? C19 C20 1.48(2) . ? C19 C21 1.494(17) . ? C22 C23 1.513(18) . ? C22 C24 1.543(17) . ? C25 C30 1.389(15) . ? C25 C26 1.395(14) . ? C26 C27 1.416(17) . ? C26 C31 1.511(17) . ? C27 C28 1.355(16) . ? C28 C29 1.373(16) . ? C29 C30 1.397(17) . ? C30 C34 1.527(16) . ? C31 C33 1.471(16) . ? C31 C32 1.514(18) . ? C34 C35 1.540(17) . ? C34 C36 1.549(18) . ? C37 C38 1.35(3) . ? C38 C39 1.61(4) . ? C38A C39 1.41(4) . ? C39 C40 1.472(16) . ? C41 C42 1.488(16) . ? C42 C43 1.546(17) . ? C43 C44 1.481(18) . ? 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 Y1 O2 113.8(3) . . ? O1 Y1 O3 112.5(3) . . ? O2 Y1 O3 133.7(3) . . ? O1 Y1 O4 101.5(3) . . ? O2 Y1 O4 85.2(3) . . ? O3 Y1 O4 87.4(3) . . ? O1 Y1 O5 101.0(3) . . ? O2 Y1 O5 85.2(3) . . ? O3 Y1 O5 84.6(3) . . ? O4 Y1 O5 157.5(3) . . ? C1 O1 Y1 152.7(7) . . ? C13 O2 Y1 174.3(7) . . ? C25 O3 Y1 173.7(7) . . ? C37 O4 C40 105.0(9) . . ? C37 O4 Y1 126.3(8) . . ? C40 O4 Y1 128.4(7) . . ? C44 O5 C41 109.8(9) . . ? C44 O5 Y1 123.6(7) . . ? C41 O5 Y1 126.5(6) . . ? O1 C1 C6 121.7(11) . . ? O1 C1 C2 119.4(10) . . ? C6 C1 C2 118.8(11) . . ? C3 C2 C1 119.9(13) . . ? C3 C2 C7 121.5(13) . . ? C1 C2 C7 118.6(10) . . ? C2 C3 C4 121.2(14) . . ? C5 C4 C3 118.0(12) . . ? C6 C5 C4 122.4(14) . . ? C5 C6 C1 119.3(14) . . ? C5 C6 C10 123.2(13) . . ? C1 C6 C10 117.4(10) . . ? C2 C7 C9 113.9(13) . . ? C2 C7 C8 111.5(12) . . ? C9 C7 C8 111.1(12) . . ? C12 C10 C11 111.8(15) . . ? C12 C10 C6 113.3(16) . . ? C11 C10 C6 110.4(10) . . ? O2 C13 C14 120.6(10) . . ? O2 C13 C18 119.2(9) . . ? C14 C13 C18 120.2(9) . . ? C15 C14 C13 119.4(11) . . ? C15 C14 C19 120.7(10) . . ? C13 C14 C19 119.9(9) . . ? C14 C15 C16 121.6(11) . . ? C17 C16 C15 119.2(11) . . ? C16 C17 C18 122.2(12) . . ? C17 C18 C13 117.3(10) . . ? C17 C18 C22 122.7(11) . . ? C13 C18 C22 119.9(9) . . ? C20 C19 C21 107.9(14) . . ? C20 C19 C14 114.2(12) . . ? C21 C19 C14 111.9(13) . . ? C18 C22 C23 111.5(11) . . ? C18 C22 C24 112.4(11) . . ? C23 C22 C24 110.5(11) . . ? O3 C25 C30 119.5(9) . . ? O3 C25 C26 118.5(10) . . ? C30 C25 C26 121.9(11) . . ? C25 C26 C27 117.5(11) . . ? C25 C26 C31 121.3(11) . . ? C27 C26 C31 121.1(10) . . ? C28 C27 C26 120.8(11) . . ? C27 C28 C29 120.8(13) . . ? C28 C29 C30 120.9(12) . . ? C25 C30 C29 118.1(10) . . ? C25 C30 C34 119.6(11) . . ? C29 C30 C34 122.3(10) . . ? C33 C31 C26 113.8(11) . . ? C33 C31 C32 111.2(12) . . ? C26 C31 C32 111.3(11) . . ? C30 C34 C35 113.9(12) . . ? C30 C34 C36 110.2(10) . . ? C35 C34 C36 109.9(11) . . ? C38 C37 O4 112.4(17) . . ? C37 C38 C39 107(2) . . ? C38A C39 C40 106.0(18) . . ? C38A C39 C38 28(2) . . ? C40 C39 C38 100.8(14) . . ? O4 C40 C39 108.2(11) . . ? C42 C41 O5 102.8(10) . . ? C41 C42 C43 101.4(10) . . ? C44 C43 C42 102.9(10) . . ? O5 C44 C43 105.2(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.153 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.098 # Attachment '- SH2C.CIF' data_sh2c _database_code_depnum_ccdc_archive 'CCDC 853842' #TrackingRef '- SH2C.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H32 I2 O4 Yb' _chemical_formula_weight 715.26 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4437(7) _cell_length_b 9.8103(8) _cell_length_c 13.6182(12) _cell_angle_alpha 79.672(5) _cell_angle_beta 87.987(5) _cell_angle_gamma 87.362(4) _cell_volume 1108.20(16) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 7.019 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4863 _exptl_absorpt_correction_T_max 0.8170 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19862 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3817 _reflns_number_gt 3068 _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^)+(0.1588P)^2^+72.0688P] 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 3817 _refine_ls_number_parameters 211 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2754 _refine_ls_wR_factor_gt 0.2472 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.073 _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 1.0000 0.0000 0.5000 0.0267(4) Uani 1 2 d S . . Yb2 Yb 1.0000 0.5000 0.0000 0.0232(4) Uani 1 2 d S . . I4 I 0.76840(15) 0.26449(15) 0.07191(10) 0.0331(4) Uani 1 1 d . . . I2 I 0.76605(17) -0.19850(16) 0.43219(12) 0.0415(5) Uani 1 1 d . . . O1 O 1.1259(15) 0.4474(16) 0.1569(11) 0.031(3) Uani 1 1 d . . . C2 C 1.284(3) 0.486(2) 0.1800(16) 0.036(5) Uani 1 1 d . . . H2A H 1.3376 0.5383 0.1198 0.043 Uiso 1 1 calc R . . H2B H 1.3509 0.4034 0.2066 0.043 Uiso 1 1 calc R . . O2 O 0.8240(15) 0.6603(17) 0.0644(12) 0.037(4) Uani 1 1 d . . . C4 C 1.253(3) 0.577(2) 0.2580(17) 0.037(5) Uani 1 1 d . . . H4A H 1.2215 0.6732 0.2274 0.044 Uiso 1 1 calc R . . H4B H 1.3468 0.5779 0.2995 0.044 Uiso 1 1 calc R . . C3 C 1.115(2) 0.502(2) 0.3187(16) 0.032(5) Uani 1 1 d . . . H3A H 1.1545 0.4422 0.3799 0.039 Uiso 1 1 calc R . . H3B H 1.0358 0.5708 0.3384 0.039 Uiso 1 1 calc R . . C5 C 0.861(3) 0.773(3) 0.1132(19) 0.046(6) Uani 1 1 d . . . H5A H 0.9369 0.8343 0.0713 0.055 Uiso 1 1 calc R . . H5B H 0.9101 0.7371 0.1782 0.055 Uiso 1 1 calc R . . C6 C 0.713(3) 0.852(3) 0.129(2) 0.041(6) Uani 1 1 d . . . H6A H 0.6965 0.9310 0.0731 0.050 Uiso 1 1 calc R . . H6B H 0.7133 0.8875 0.1922 0.050 Uiso 1 1 calc R . . O3 O 0.8128(18) 0.1937(17) 0.4458(12) 0.041(4) Uani 1 1 d . . . C13 C 0.686(3) 0.201(3) 0.3808(17) 0.040(6) Uani 1 1 d . . . H13A H 0.6090 0.1293 0.4065 0.048 Uiso 1 1 calc R . . H13B H 0.7250 0.1877 0.3135 0.048 Uiso 1 1 calc R . . C12 C 0.612(3) 0.346(3) 0.3778(19) 0.046(6) Uani 1 1 d . . . H12A H 0.6555 0.4132 0.3213 0.055 Uiso 1 1 calc R . . H12B H 0.4949 0.3471 0.3731 0.055 Uiso 1 1 calc R . . C11 C 0.659(4) 0.378(3) 0.477(3) 0.061(8) Uani 1 1 d . . . H11A H 0.6796 0.4779 0.4705 0.074 Uiso 1 1 calc R . . H11B H 0.5738 0.3546 0.5277 0.074 Uiso 1 1 calc R . . C10 C 0.802(4) 0.295(4) 0.506(3) 0.082(13) Uani 1 1 d . . . H10A H 0.8965 0.3533 0.4948 0.098 Uiso 1 1 calc R . . H10B H 0.7954 0.2521 0.5775 0.098 Uiso 1 1 calc R . . C8 C 0.653(2) 0.662(3) 0.057(2) 0.047(7) Uani 1 1 d . . . H8A H 0.6134 0.5664 0.0736 0.057 Uiso 1 1 calc R . . H8B H 0.6202 0.7030 -0.0119 0.057 Uiso 1 1 calc R . . C7 C 0.589(3) 0.750(3) 0.131(3) 0.056(8) Uani 1 1 d . . . H7A H 0.4860 0.7960 0.1109 0.068 Uiso 1 1 calc R . . H7B H 0.5771 0.6933 0.1989 0.068 Uiso 1 1 calc R . . O4 O 1.1388(17) 0.0206(19) 0.3416(11) 0.039(4) Uani 1 1 d . . . C14 C 1.307(3) 0.046(5) 0.327(2) 0.083(13) Uani 1 1 d . . . H14A H 1.3281 0.1412 0.3371 0.100 Uiso 1 1 calc R . . H14B H 1.3697 -0.0209 0.3750 0.100 Uiso 1 1 calc R . . C15 C 1.349(3) 0.031(4) 0.229(2) 0.063(8) Uani 1 1 d . . . H15A H 1.4017 -0.0612 0.2284 0.076 Uiso 1 1 calc R . . H15B H 1.4232 0.1029 0.1986 0.076 Uiso 1 1 calc R . . C17 C 1.070(4) 0.003(3) 0.2487(16) 0.049(7) Uani 1 1 d . . . H17A H 0.9742 0.0648 0.2341 0.059 Uiso 1 1 calc R . . H17B H 1.0410 -0.0941 0.2510 0.059 Uiso 1 1 calc R . . C16 C 1.205(3) 0.044(3) 0.1701(18) 0.049(6) Uani 1 1 d . . . H16A H 1.2121 -0.0185 0.1207 0.059 Uiso 1 1 calc R . . H16B H 1.1874 0.1408 0.1345 0.059 Uiso 1 1 calc R . . C1A C 1.042(3) 0.418(3) 0.2542(17) 0.040(5) Uani 1 1 d U . . H1A1 H 1.0534 0.3179 0.2831 0.048 Uiso 1 1 calc R . . H1A2 H 0.9273 0.4432 0.2469 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Yb1 0.0139(6) 0.0335(7) 0.0301(7) 0.0006(5) 0.0005(4) 0.0016(5) Yb2 0.0115(6) 0.0272(7) 0.0305(7) -0.0029(5) -0.0039(4) -0.0013(4) I4 0.0222(7) 0.0333(8) 0.0408(8) 0.0049(6) -0.0073(5) -0.0094(5) I2 0.0304(8) 0.0385(9) 0.0534(10) 0.0007(7) 0.0001(6) -0.0122(6) O1 0.014(7) 0.042(9) 0.040(8) -0.009(7) -0.002(6) -0.008(6) C2 0.026(11) 0.042(13) 0.035(11) 0.005(10) -0.004(9) -0.006(9) O2 0.007(6) 0.050(10) 0.059(10) -0.027(8) -0.004(6) 0.009(6) C4 0.031(12) 0.036(13) 0.044(13) -0.009(10) -0.009(9) -0.005(9) C3 0.021(10) 0.041(13) 0.034(11) -0.005(9) -0.007(8) -0.004(9) C5 0.028(12) 0.070(18) 0.045(13) -0.019(12) 0.004(10) -0.018(12) C6 0.030(12) 0.038(13) 0.062(15) -0.021(11) -0.009(10) -0.014(10) O3 0.029(8) 0.041(10) 0.054(10) -0.008(8) -0.015(7) -0.001(7) C13 0.023(11) 0.058(16) 0.040(12) -0.010(11) -0.014(9) 0.019(10) C12 0.018(10) 0.056(16) 0.053(14) 0.022(12) -0.011(9) 0.004(10) C11 0.062(18) 0.030(14) 0.10(2) -0.024(14) -0.039(16) 0.023(13) C10 0.09(2) 0.09(3) 0.07(2) -0.047(19) -0.053(18) 0.07(2) C8 0.011(10) 0.048(15) 0.091(19) -0.033(14) 0.000(11) -0.005(9) C7 0.022(12) 0.058(18) 0.10(2) -0.038(16) 0.019(12) -0.006(11) O4 0.019(7) 0.066(11) 0.034(8) -0.006(7) -0.004(6) -0.016(7) C14 0.014(12) 0.18(4) 0.048(16) 0.003(19) 0.010(11) -0.038(17) C15 0.022(12) 0.10(3) 0.066(18) -0.020(17) 0.011(12) -0.008(14) C17 0.09(2) 0.028(12) 0.029(11) -0.015(9) -0.015(12) 0.013(12) C16 0.042(14) 0.066(18) 0.036(12) -0.006(12) 0.009(10) 0.013(12) C1A 0.040(5) 0.040(5) 0.040(5) -0.0070(14) -0.0011(10) -0.0018(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 Yb1 O4 2.399(15) . ? Yb1 O4 2.399(15) 2_756 ? Yb1 O3 2.440(16) . ? Yb1 O3 2.440(16) 2_756 ? Yb1 I2 3.1103(15) 2_756 ? Yb1 I2 3.1103(15) . ? Yb2 O2 2.375(14) 2_765 ? Yb2 O2 2.375(14) . ? Yb2 O1 2.382(14) . ? Yb2 O1 2.382(14) 2_765 ? Yb2 I4 3.0970(13) 2_765 ? Yb2 I4 3.0970(13) . ? O1 C2 1.47(2) . ? O1 C1A 1.47(3) . ? C2 C4 1.51(3) . ? O2 C5 1.44(3) . ? O2 C8 1.45(2) . ? C4 C3 1.54(3) . ? C3 C1A 1.48(3) . ? C5 C6 1.47(4) . ? C6 C7 1.47(3) . ? O3 C10 1.40(3) . ? O3 C13 1.40(3) . ? C13 C12 1.53(4) . ? C12 C11 1.51(4) . ? C11 C10 1.45(3) . ? C8 C7 1.52(3) . ? O4 C17 1.45(3) . ? O4 C14 1.45(3) . ? C14 C15 1.41(4) . ? C15 C16 1.46(4) . ? C17 C16 1.55(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Yb1 O4 180.000(2) . 2_756 ? O4 Yb1 O3 94.5(6) . . ? O4 Yb1 O3 85.5(6) 2_756 . ? O4 Yb1 O3 85.5(6) . 2_756 ? O4 Yb1 O3 94.5(6) 2_756 2_756 ? O3 Yb1 O3 180.000(2) . 2_756 ? O4 Yb1 I2 89.9(4) . 2_756 ? O4 Yb1 I2 90.1(4) 2_756 2_756 ? O3 Yb1 I2 90.9(4) . 2_756 ? O3 Yb1 I2 89.1(4) 2_756 2_756 ? O4 Yb1 I2 90.1(4) . . ? O4 Yb1 I2 89.9(4) 2_756 . ? O3 Yb1 I2 89.1(4) . . ? O3 Yb1 I2 90.9(4) 2_756 . ? I2 Yb1 I2 180.00(4) 2_756 . ? O2 Yb2 O2 180.000(1) 2_765 . ? O2 Yb2 O1 90.4(5) 2_765 . ? O2 Yb2 O1 89.6(5) . . ? O2 Yb2 O1 89.6(5) 2_765 2_765 ? O2 Yb2 O1 90.4(5) . 2_765 ? O1 Yb2 O1 180.000(1) . 2_765 ? O2 Yb2 I4 90.4(4) 2_765 2_765 ? O2 Yb2 I4 89.6(4) . 2_765 ? O1 Yb2 I4 90.4(3) . 2_765 ? O1 Yb2 I4 89.6(3) 2_765 2_765 ? O2 Yb2 I4 89.6(4) 2_765 . ? O2 Yb2 I4 90.4(4) . . ? O1 Yb2 I4 89.6(3) . . ? O1 Yb2 I4 90.4(3) 2_765 . ? I4 Yb2 I4 180.0 2_765 . ? C2 O1 C1A 104.7(15) . . ? C2 O1 Yb2 127.2(12) . . ? C1A O1 Yb2 124.6(12) . . ? O1 C2 C4 104.3(17) . . ? C5 O2 C8 107.7(16) . . ? C5 O2 Yb2 128.8(12) . . ? C8 O2 Yb2 123.4(13) . . ? C2 C4 C3 100.8(18) . . ? C1A C3 C4 107.3(18) . . ? O2 C5 C6 108.1(17) . . ? C5 C6 C7 104(2) . . ? C10 O3 C13 113.7(18) . . ? C10 O3 Yb1 115.2(13) . . ? C13 O3 Yb1 128.7(14) . . ? O3 C13 C12 104.3(19) . . ? C11 C12 C13 101.5(17) . . ? C10 C11 C12 108(2) . . ? O3 C10 C11 106(2) . . ? O2 C8 C7 104.5(19) . . ? C6 C7 C8 103(2) . . ? C17 O4 C14 111(2) . . ? C17 O4 Yb1 125.2(14) . . ? C14 O4 Yb1 124.1(14) . . ? C15 C14 O4 107(2) . . ? C14 C15 C16 109(2) . . ? O4 C17 C16 103(2) . . ? C15 C16 C17 104(2) . . ? O1 C1A C3 106.2(18) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 6.125 _refine_diff_density_min -2.093 _refine_diff_density_rms 0.623 # Attachment '- ladipthf3.cif' data_ladipthf3.cif _database_code_depnum_ccdc_archive 'CCDC 853843' #TrackingRef '- ladipthf3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'SH8 La' _chemical_melting_point ? _chemical_formula_moiety 'C52 H83 La O7' _chemical_formula_sum 'C52 H83 La O7' _chemical_formula_weight 959.09 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4044(15) _cell_length_b 35.747(5) _cell_length_c 13.3608(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.540(5) _cell_angle_gamma 90.00 _cell_volume 5399.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 32284 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.180 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.835 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8920 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32284 _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_sigmaI/netI 0.1285 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12385 _reflns_number_gt 6485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12385 _refine_ls_number_parameters 388 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.1982 _refine_ls_R_factor_gt 0.1117 _refine_ls_wR_factor_ref 0.2815 _refine_ls_wR_factor_gt 0.2402 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _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 La1 La 0.42706(5) 0.145205(17) 0.48062(5) 0.0487(2) Uani 1 1 d . B . O1 O 0.3056(5) 0.19028(19) 0.4179(6) 0.056(2) Uani 1 1 d . . . C1 C 0.2126(10) 0.2136(3) 0.4004(8) 0.054(3) Uiso 1 1 d . A . C81 C 0.045(6) -0.0784(15) 0.028(4) 0.37(5) Uiso 0.50 1 d PD . . H81A H -0.0099 -0.0694 -0.0312 0.448 Uiso 0.50 1 calc PR . . H81B H 0.1242 -0.0817 0.0066 0.448 Uiso 0.50 1 calc PR . . O2 O 0.3344(6) 0.0942(2) 0.4163(7) 0.071(2) Uani 1 1 d . . . C2 C 0.2265(10) 0.2502(3) 0.4225(8) 0.056(3) Uiso 1 1 d . . . O3 O 0.3901(8) 0.1466(2) 0.6396(6) 0.078(3) Uani 1 1 d . . . C3 C 0.1285(10) 0.2743(4) 0.4095(9) 0.063(3) Uiso 1 1 d . . . H3 H 0.1373 0.2999 0.4276 0.076 Uiso 1 1 calc R . . O4 O 0.6020(6) 0.1912(2) 0.5400(6) 0.0567(19) Uani 1 1 d . . . C4 C 0.0218(13) 0.2607(4) 0.3711(10) 0.080(4) Uiso 1 1 d . . . H4 H -0.0438 0.2772 0.3601 0.097 Uiso 1 1 calc R . . O5 O 0.6035(7) 0.0984(2) 0.5173(7) 0.074(2) Uani 1 1 d . . . C5 C 0.0053(14) 0.2238(4) 0.3479(11) 0.095(5) Uiso 1 1 d . A . H5 H -0.0711 0.2149 0.3218 0.114 Uiso 1 1 calc R . . O6 O 0.5270(7) 0.1549(2) 0.3197(5) 0.070(2) Uani 1 1 d D . . C6 C 0.1013(12) 0.1990(4) 0.3623(10) 0.078(4) Uiso 1 1 d . . . O7 O 0.763(4) 0.0681(9) 0.123(4) 0.222(16) Uiso 0.50 1 d PD . . C7 C 0.3440(11) 0.2655(3) 0.4610(9) 0.065(3) Uiso 1 1 d . . . H7 H 0.3886 0.2451 0.5008 0.078 Uiso 1 1 calc R . . O8 O 0.050(5) -0.0517(10) 0.111(5) 0.33(3) Uiso 0.50 1 d PD . . C8 C 0.3443(15) 0.2992(5) 0.5309(12) 0.108(5) Uiso 1 1 d . . . H8A H 0.4259 0.3074 0.5513 0.162 Uiso 1 1 calc R . . H8B H 0.3084 0.2922 0.5910 0.162 Uiso 1 1 calc R . . H8C H 0.2989 0.3196 0.4955 0.162 Uiso 1 1 calc R . . C9 C 0.4107(14) 0.2746(5) 0.3764(12) 0.104(5) Uiso 1 1 d . . . H9A H 0.4888 0.2844 0.4032 0.157 Uiso 1 1 calc R . . H9B H 0.3674 0.2935 0.3331 0.157 Uiso 1 1 calc R . . H9C H 0.4202 0.2520 0.3369 0.157 Uiso 1 1 calc R . . C10 C 0.092(2) 0.1591(7) 0.367(2) 0.056(6) Uiso 0.50 1 d P A 1 H10 H 0.1529 0.1475 0.4179 0.067 Uiso 0.50 1 calc PR A 1 C11 C 0.107(2) 0.1499(7) 0.264(2) 0.060(6) Uiso 0.50 1 d P A 1 H11A H 0.1063 0.1227 0.2560 0.090 Uiso 0.50 1 calc PR A 1 H11B H 0.1831 0.1598 0.2493 0.090 Uiso 0.50 1 calc PR A 1 H11C H 0.0428 0.1610 0.2180 0.090 Uiso 0.50 1 calc PR A 1 C12 C -0.035(2) 0.1451(8) 0.375(2) 0.079(7) Uiso 0.50 1 d P A 1 H12A H -0.0531 0.1488 0.4440 0.118 Uiso 0.50 1 calc PR A 1 H12B H -0.0413 0.1185 0.3577 0.118 Uiso 0.50 1 calc PR A 1 H12C H -0.0921 0.1593 0.3280 0.118 Uiso 0.50 1 calc PR A 1 C13 C 0.2505(15) 0.0715(5) 0.4036(14) 0.067(6) Uiso 0.60 1 d PD B 1 C14 C 0.2378(17) 0.0567(6) 0.3069(13) 0.078(6) Uiso 0.60 1 d PD B 1 C15 C 0.147(2) 0.0314(7) 0.2772(13) 0.115(10) Uiso 0.60 1 d PD B 1 H15 H 0.1403 0.0201 0.2123 0.138 Uiso 0.60 1 calc PR B 1 C16 C 0.067(2) 0.0227(9) 0.3426(17) 0.099(12) Uiso 0.60 1 d PD B 1 H16 H 0.0025 0.0065 0.3211 0.119 Uiso 0.60 1 calc PR B 1 C17 C 0.0796(16) 0.0374(6) 0.4391(13) 0.089(7) Uiso 0.60 1 d PD B 1 H17 H 0.0271 0.0301 0.4851 0.106 Uiso 0.60 1 calc PR B 1 C18 C 0.1692(17) 0.0629(6) 0.4687(12) 0.069(6) Uiso 0.60 1 d PD B 1 C19 C 0.389(3) 0.0601(11) 0.218(3) 0.077(10) Uiso 0.40 1 d PD B 2 H19 H 0.4176 0.0846 0.2478 0.093 Uiso 0.40 1 calc PR B 2 C20 C 0.367(3) 0.0657(11) 0.106(3) 0.088(10) Uiso 0.40 1 d P B 2 H20A H 0.3138 0.0872 0.0905 0.131 Uiso 0.40 1 calc PR B 2 H20B H 0.3296 0.0433 0.0736 0.131 Uiso 0.40 1 calc PR B 2 H20C H 0.4417 0.0705 0.0796 0.131 Uiso 0.40 1 calc PR B 2 C21 C 0.482(4) 0.0330(13) 0.247(4) 0.128(18) Uiso 0.40 1 d PD B 2 H21A H 0.5532 0.0399 0.2172 0.192 Uiso 0.40 1 calc PR B 2 H21B H 0.4557 0.0081 0.2236 0.192 Uiso 0.40 1 calc PR B 2 H21C H 0.5008 0.0328 0.3210 0.192 Uiso 0.40 1 calc PR B 2 C22 C 0.199(2) 0.0735(8) 0.580(2) 0.080(7) Uiso 0.60 1 d P B 1 H22 H 0.2322 0.0992 0.5779 0.096 Uiso 0.60 1 calc PR B 1 C23 C 0.093(3) 0.0783(10) 0.636(3) 0.140(12) Uiso 0.60 1 d P B 1 H23A H 0.0308 0.0919 0.5933 0.210 Uiso 0.60 1 calc PR B 1 H23B H 0.1167 0.0925 0.6981 0.210 Uiso 0.60 1 calc PR B 1 H23C H 0.0634 0.0537 0.6529 0.210 Uiso 0.60 1 calc PR B 1 C24 C 0.285(3) 0.0536(9) 0.638(2) 0.118(10) Uiso 0.60 1 d P B 1 H24A H 0.3550 0.0517 0.6023 0.177 Uiso 0.60 1 calc PR B 1 H24B H 0.2561 0.0285 0.6505 0.177 Uiso 0.60 1 calc PR B 1 H24C H 0.3071 0.0666 0.7023 0.177 Uiso 0.60 1 calc PR B 1 C25 C 0.3597(10) 0.1493(3) 0.7289(9) 0.059(3) Uiso 1 1 d . B . C26 C 0.4185(11) 0.1300(4) 0.8073(10) 0.070(3) Uiso 1 1 d . . . C27 C 0.3891(15) 0.1324(5) 0.9059(13) 0.107(5) Uiso 1 1 d . B . H27 H 0.4295 0.1179 0.9592 0.129 Uiso 1 1 calc R . . C28 C 0.2968(17) 0.1573(5) 0.9233(15) 0.120(6) Uiso 1 1 d . . . H28 H 0.2752 0.1602 0.9892 0.144 Uiso 1 1 calc R B . C29 C 0.2385(14) 0.1774(5) 0.8422(12) 0.097(5) Uiso 1 1 d . B . H29 H 0.1796 0.1949 0.8553 0.117 Uiso 1 1 calc R . . C30 C 0.2619(11) 0.1733(4) 0.7428(10) 0.072(3) Uiso 1 1 d . . . C31 C 0.5188(11) 0.1042(4) 0.7947(10) 0.074(4) Uiso 1 1 d . B . H31 H 0.5198 0.1001 0.7208 0.089 Uiso 1 1 calc R . . C32 C 0.6363(13) 0.1210(4) 0.8379(11) 0.095(5) Uiso 1 1 d . . . H32A H 0.7003 0.1038 0.8272 0.143 Uiso 1 1 calc R B . H32B H 0.6372 0.1254 0.9103 0.143 Uiso 1 1 calc R . . H32C H 0.6478 0.1448 0.8040 0.143 Uiso 1 1 calc R . . C33 C 0.525(2) 0.0660(7) 0.8467(18) 0.179(10) Uiso 1 1 d . . . H33A H 0.5944 0.0523 0.8300 0.269 Uiso 1 1 calc R B . H33B H 0.4533 0.0517 0.8234 0.269 Uiso 1 1 calc R . . H33C H 0.5316 0.0695 0.9200 0.269 Uiso 1 1 calc R . . C34 C 0.2009(12) 0.1938(4) 0.6633(10) 0.075(4) Uiso 1 1 d . B . H34 H 0.2501 0.1925 0.6067 0.090 Uiso 1 1 calc R . . C35 C 0.192(3) 0.2335(8) 0.687(2) 0.224(13) Uiso 1 1 d . . . H35A H 0.1535 0.2468 0.6275 0.337 Uiso 1 1 calc R B . H35B H 0.2711 0.2437 0.7068 0.337 Uiso 1 1 calc R . . H35C H 0.1447 0.2365 0.7428 0.337 Uiso 1 1 calc R . . C36 C 0.0860(18) 0.1772(6) 0.6242(16) 0.154(8) Uiso 1 1 d . . . H36A H 0.0474 0.1926 0.5688 0.230 Uiso 1 1 calc R B . H36B H 0.0359 0.1761 0.6784 0.230 Uiso 1 1 calc R . . H36C H 0.0982 0.1519 0.5995 0.230 Uiso 1 1 calc R . . C37 C 0.6035(14) 0.2088(4) 0.6354(11) 0.091(4) Uiso 1 1 d . B . H37A H 0.6404 0.1922 0.6900 0.109 Uiso 1 1 calc R . . H37B H 0.5220 0.2148 0.6482 0.109 Uiso 1 1 calc R . . C38 C 0.6746(15) 0.2441(5) 0.6315(13) 0.108(5) Uiso 1 1 d . . . H38A H 0.6229 0.2657 0.6099 0.130 Uiso 1 1 calc R B . H38B H 0.7200 0.2497 0.6982 0.130 Uiso 1 1 calc R . . C39 C 0.7538(15) 0.2355(5) 0.5566(12) 0.105(5) Uiso 1 1 d . B . H39A H 0.8296 0.2252 0.5898 0.126 Uiso 1 1 calc R . . H39B H 0.7705 0.2584 0.5189 0.126 Uiso 1 1 calc R . . C40 C 0.6892(12) 0.2070(4) 0.4866(11) 0.081(4) Uiso 1 1 d . B . H40A H 0.6520 0.2191 0.4237 0.098 Uiso 1 1 calc R . . H40B H 0.7445 0.1875 0.4688 0.098 Uiso 1 1 calc R . . C41 C 0.560(3) 0.0569(8) 0.532(2) 0.086(8) Uiso 0.50 1 d P B 1 H41A H 0.4948 0.0563 0.5737 0.103 Uiso 0.50 1 calc PR B 1 H41B H 0.5331 0.0450 0.4656 0.103 Uiso 0.50 1 calc PR B 1 C42 C 0.654(4) 0.0406(11) 0.577(3) 0.117(13) Uiso 0.50 1 d P B 1 H42A H 0.6923 0.0269 0.5252 0.140 Uiso 0.50 1 calc PR B 1 H42B H 0.6289 0.0218 0.6239 0.140 Uiso 0.50 1 calc PR B 1 C43 C 0.746(2) 0.0661(7) 0.635(2) 0.062(6) Uiso 0.50 1 d P B 1 H43A H 0.7404 0.0650 0.7086 0.074 Uiso 0.50 1 calc PR B 1 H43B H 0.8269 0.0587 0.6240 0.074 Uiso 0.50 1 calc PR B 1 C44 C 0.716(3) 0.1051(9) 0.594(2) 0.069(8) Uiso 0.50 1 d P B 1 H44A H 0.7811 0.1154 0.5596 0.083 Uiso 0.50 1 calc PR B 1 H44B H 0.6998 0.1225 0.6479 0.083 Uiso 0.50 1 calc PR B 1 C45 C 0.636(2) 0.1374(9) 0.296(2) 0.095(13) Uiso 0.50 1 d PD B 1 H45A H 0.7017 0.1424 0.3507 0.115 Uiso 0.50 1 calc PR B 1 H45B H 0.6255 0.1100 0.2895 0.115 Uiso 0.50 1 calc PR B 1 C46 C 0.663(2) 0.1534(9) 0.2009(19) 0.113(12) Uiso 0.50 1 d PD B 1 H46A H 0.7357 0.1686 0.2124 0.136 Uiso 0.50 1 calc PR B 1 H46B H 0.6746 0.1332 0.1525 0.136 Uiso 0.50 1 calc PR B 1 C47 C 0.562(3) 0.1768(9) 0.1610(14) 0.132(15) Uiso 0.50 1 d PD B 1 H47A H 0.5118 0.1636 0.1061 0.159 Uiso 0.50 1 calc PR B 1 H47B H 0.5900 0.2005 0.1338 0.159 Uiso 0.50 1 calc PR B 1 C48 C 0.496(2) 0.1843(6) 0.2452(14) 0.075(8) Uiso 0.50 1 d PD B 1 H48A H 0.5170 0.2091 0.2749 0.090 Uiso 0.50 1 calc PR B 1 H48B H 0.4097 0.1839 0.2219 0.090 Uiso 0.50 1 calc PR B 1 C71 C 0.761(6) 0.0518(14) 0.222(3) 0.24(3) Uiso 0.50 1 d PD . . H71A H 0.6868 0.0583 0.2486 0.287 Uiso 0.50 1 calc PR . . H71B H 0.8284 0.0615 0.2699 0.287 Uiso 0.50 1 calc PR . . C72 C 0.771(8) 0.0113(13) 0.213(4) 0.42(6) Uiso 0.50 1 d PD . . H72A H 0.8481 0.0025 0.2474 0.507 Uiso 0.50 1 calc PR . . H72B H 0.7072 -0.0013 0.2432 0.507 Uiso 0.50 1 calc PR . . C73 C 0.761(5) 0.0027(10) 0.105(4) 0.22(3) Uiso 0.50 1 d PD . . H73A H 0.8239 -0.0151 0.0917 0.262 Uiso 0.50 1 calc PR . . H73B H 0.6833 -0.0088 0.0817 0.262 Uiso 0.50 1 calc PR . . C74 C 0.774(7) 0.0377(15) 0.052(3) 0.31(4) Uiso 0.50 1 d PD . . H74A H 0.7116 0.0398 -0.0069 0.374 Uiso 0.50 1 calc PR . . H74B H 0.8520 0.0387 0.0272 0.374 Uiso 0.50 1 calc PR . . C82 C 0.003(4) -0.1138(10) 0.064(3) 0.160(17) Uiso 0.50 1 d PD . . H82A H 0.0689 -0.1317 0.0776 0.192 Uiso 0.50 1 calc PR . . H82B H -0.0584 -0.1248 0.0131 0.192 Uiso 0.50 1 calc PR . . C83 C -0.047(7) -0.1059(16) 0.157(5) 0.45(7) Uiso 0.50 1 d PD . . H83A H -0.1343 -0.1092 0.1459 0.544 Uiso 0.50 1 calc PR . . H83B H -0.0139 -0.1232 0.2112 0.544 Uiso 0.50 1 calc PR . . C84 C -0.018(5) -0.0674(16) 0.186(4) 0.24(3) Uiso 0.50 1 d PD . . H84A H 0.0293 -0.0666 0.2534 0.286 Uiso 0.50 1 calc PR . . H84B H -0.0912 -0.0527 0.1883 0.286 Uiso 0.50 1 calc PR . . C10' C 0.0886(19) 0.1567(6) 0.315(2) 0.046(5) Uiso 0.50 1 d P A 2 H10' H 0.1358 0.1401 0.3653 0.055 Uiso 0.50 1 calc PR A 2 C11' C 0.140(3) 0.1514(9) 0.216(2) 0.090(9) Uiso 0.50 1 d P A 2 H11D H 0.2202 0.1621 0.2226 0.135 Uiso 0.50 1 calc PR A 2 H11E H 0.0901 0.1641 0.1612 0.135 Uiso 0.50 1 calc PR A 2 H11F H 0.1442 0.1247 0.2006 0.135 Uiso 0.50 1 calc PR A 2 C12' C -0.035(2) 0.1409(8) 0.300(2) 0.085(8) Uiso 0.50 1 d P A 2 H12D H -0.0722 0.1453 0.3613 0.127 Uiso 0.50 1 calc PR A 2 H12E H -0.0314 0.1140 0.2877 0.127 Uiso 0.50 1 calc PR A 2 H12F H -0.0813 0.1532 0.2426 0.127 Uiso 0.50 1 calc PR A 2 C13' C 0.2601(14) 0.0652(5) 0.3564(14) 0.027(4) Uiso 0.40 1 d PD B 2 C14' C 0.2801(17) 0.0492(6) 0.2658(14) 0.045(6) Uiso 0.40 1 d PD B 2 C15' C 0.203(2) 0.0222(7) 0.2208(15) 0.070(8) Uiso 0.40 1 d PD B 2 H15' H 0.2139 0.0119 0.1573 0.084 Uiso 0.40 1 calc PR B 2 C16' C 0.109(2) 0.0105(8) 0.269(2) 0.094(12) Uiso 0.40 1 d PD B 2 H16' H 0.0595 -0.0094 0.2416 0.113 Uiso 0.40 1 calc PR B 2 C17' C 0.086(2) 0.0276(10) 0.358(2) 0.058(10) Uiso 0.40 1 d PD B 2 H17' H 0.0171 0.0213 0.3870 0.070 Uiso 0.40 1 calc PR B 2 C18' C 0.1646(17) 0.0540(6) 0.4033(14) 0.046(6) Uiso 0.40 1 d PD B 2 C19' C 0.322(3) 0.0644(9) 0.229(2) 0.099(8) Uiso 0.60 1 d P B 1 H19' H 0.3688 0.0868 0.2551 0.118 Uiso 0.60 1 calc PR B 1 C20' C 0.273(3) 0.0740(10) 0.123(3) 0.140(12) Uiso 0.60 1 d P B 1 H20D H 0.2287 0.0975 0.1220 0.211 Uiso 0.60 1 calc PR B 1 H20E H 0.2201 0.0540 0.0943 0.211 Uiso 0.60 1 calc PR B 1 H20F H 0.3381 0.0768 0.0821 0.211 Uiso 0.60 1 calc PR B 1 C21' C 0.412(4) 0.0337(13) 0.224(4) 0.169(16) Uiso 0.60 1 d P B 1 H21D H 0.4495 0.0277 0.2923 0.253 Uiso 0.60 1 calc PR B 1 H21E H 0.4725 0.0422 0.1832 0.253 Uiso 0.60 1 calc PR B 1 H21F H 0.3727 0.0114 0.1930 0.253 Uiso 0.60 1 calc PR B 1 C22' C 0.154(2) 0.0703(8) 0.509(2) 0.050(7) Uiso 0.40 1 d P B 2 H22' H 0.1859 0.0965 0.5109 0.060 Uiso 0.40 1 calc PR B 2 C23' C 0.019(3) 0.0722(10) 0.519(3) 0.082(10) Uiso 0.40 1 d P B 2 H23D H -0.0194 0.0907 0.4718 0.123 Uiso 0.40 1 calc PR B 2 H23E H 0.0093 0.0796 0.5885 0.123 Uiso 0.40 1 calc PR B 2 H23F H -0.0168 0.0476 0.5045 0.123 Uiso 0.40 1 calc PR B 2 C24' C 0.218(4) 0.0502(15) 0.586(4) 0.109(15) Uiso 0.40 1 d P B 2 H24D H 0.3030 0.0525 0.5809 0.164 Uiso 0.40 1 calc PR B 2 H24E H 0.1951 0.0238 0.5803 0.164 Uiso 0.40 1 calc PR B 2 H24F H 0.2020 0.0601 0.6511 0.164 Uiso 0.40 1 calc PR B 2 C41' C 0.600(2) 0.0604(8) 0.477(2) 0.073(7) Uiso 0.50 1 d P B 2 H41C H 0.5240 0.0486 0.4876 0.088 Uiso 0.50 1 calc PR B 2 H41D H 0.6039 0.0614 0.4037 0.088 Uiso 0.50 1 calc PR B 2 C42' C 0.690(3) 0.0397(10) 0.522(3) 0.103(11) Uiso 0.50 1 d P B 2 H42C H 0.6608 0.0214 0.5689 0.124 Uiso 0.50 1 calc PR B 2 H42D H 0.7282 0.0259 0.4710 0.124 Uiso 0.50 1 calc PR B 2 C43' C 0.763(5) 0.0631(17) 0.571(5) 0.20(2) Uiso 0.50 1 d P B 2 H43C H 0.8419 0.0613 0.5477 0.234 Uiso 0.50 1 calc PR B 2 H43D H 0.7723 0.0577 0.6444 0.234 Uiso 0.50 1 calc PR B 2 C44' C 0.712(3) 0.1011(9) 0.550(3) 0.079(9) Uiso 0.50 1 d P B 2 H44C H 0.7218 0.1162 0.6126 0.095 Uiso 0.50 1 calc PR B 2 H44D H 0.7535 0.1139 0.4994 0.095 Uiso 0.50 1 calc PR B 2 C45' C 0.612(2) 0.1325(7) 0.2739(14) 0.063(9) Uiso 0.50 1 d PD B 2 H45C H 0.5950 0.1055 0.2808 0.076 Uiso 0.50 1 calc PR B 2 H45D H 0.6933 0.1375 0.3075 0.076 Uiso 0.50 1 calc PR B 2 C46' C 0.602(3) 0.1428(9) 0.1673(13) 0.113(12) Uiso 0.50 1 d PD B 2 H46C H 0.6747 0.1559 0.1533 0.135 Uiso 0.50 1 calc PR B 2 H46D H 0.5922 0.1201 0.1246 0.135 Uiso 0.50 1 calc PR B 2 C47' C 0.500(3) 0.1671(10) 0.1452(10) 0.108(11) Uiso 0.50 1 d PD B 2 H47C H 0.5239 0.1913 0.1181 0.130 Uiso 0.50 1 calc PR B 2 H47D H 0.4405 0.1554 0.0940 0.130 Uiso 0.50 1 calc PR B 2 C48' C 0.450(3) 0.1731(11) 0.2383(13) 0.128(15) Uiso 0.50 1 d PD B 2 H48C H 0.3691 0.1623 0.2327 0.154 Uiso 0.50 1 calc PR B 2 H48D H 0.4441 0.2002 0.2520 0.154 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 La1 0.0412(3) 0.0420(3) 0.0684(4) 0.0128(3) 0.0279(3) 0.0085(3) O1 0.030(3) 0.044(4) 0.097(6) 0.021(4) 0.015(4) 0.009(3) O2 0.042(4) 0.041(4) 0.132(8) 0.021(5) 0.021(4) -0.007(3) O3 0.113(7) 0.044(4) 0.095(6) 0.013(4) 0.075(5) 0.019(5) O4 0.044(4) 0.064(5) 0.063(5) -0.004(4) 0.010(4) -0.004(3) O5 0.055(5) 0.063(5) 0.100(7) -0.002(5) -0.002(5) 0.025(4) O6 0.080(6) 0.078(6) 0.057(5) 0.007(4) 0.030(4) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O1 2.216(6) . ? La1 O3 2.220(7) . ? La1 O2 2.222(8) . ? La1 O6 2.586(6) . ? La1 O5 2.613(7) . ? La1 O4 2.625(7) . ? O1 C1 1.346(12) . ? C1 C2 1.343(15) . ? C1 C6 1.406(16) . ? C81 C82 1.458(10) . ? C81 O8 1.461(10) . ? O2 C13 1.250(14) . ? O2 C13' 1.502(16) . ? C2 C3 1.405(15) . ? C2 C7 1.477(15) . ? O3 C25 1.289(13) . ? C3 C4 1.349(17) . ? O4 C40 1.417(14) . ? O4 C37 1.421(15) . ? C4 C5 1.360(18) . ? O5 C44' 1.26(3) . ? O5 C41' 1.46(3) . ? O5 C44 1.55(3) . ? O5 C41 1.58(3) . ? C5 C6 1.403(19) . ? O6 C45' 1.455(8) . ? O6 C48 1.458(9) . ? O6 C48' 1.461(9) . ? O6 C45 1.463(9) . ? C6 C10 1.43(3) . ? C6 C10' 1.64(3) . ? O7 C71 1.452(9) . ? O7 C74 1.460(9) . ? C7 C9 1.480(18) . ? C7 C8 1.525(18) . ? O8 C84 1.458(9) . ? C10 C11 1.44(3) . ? C10 C12 1.55(3) . ? C13 C14 1.385(8) . ? C13 C18 1.386(8) . ? C14 C15 1.394(8) . ? C14 C19' 1.53(3) . ? C15 C16 1.380(8) . ? C16 C17 1.383(8) . ? C17 C18 1.388(8) . ? C18 C22 1.52(3) . ? C19 C21 1.450(10) . ? C19 C20 1.50(5) . ? C19 C14' 1.53(4) . ? C22 C24 1.37(4) . ? C22 C23 1.51(4) . ? C25 C26 1.357(16) . ? C25 C30 1.438(16) . ? C26 C27 1.404(19) . ? C26 C31 1.494(17) . ? C27 C28 1.42(2) . ? C28 C29 1.39(2) . ? C29 C30 1.396(18) . ? C30 C34 1.400(17) . ? C31 C32 1.512(18) . ? C31 C33 1.53(2) . ? C34 C35 1.46(3) . ? C34 C36 1.47(2) . ? C37 C38 1.50(2) . ? C38 C39 1.47(2) . ? C39 C40 1.509(19) . ? C41 C42 1.30(4) . ? C42 C43 1.53(4) . ? C43 C44 1.53(4) . ? C45 C46 1.463(9) . ? C46 C47 1.461(9) . ? C47 C48 1.462(9) . ? C71 C72 1.460(9) . ? C72 C73 1.460(10) . ? C73 C74 1.455(9) . ? C82 C83 1.459(9) . ? C83 C84 1.456(9) . ? C10' C12' 1.51(3) . ? C10' C11' 1.53(4) . ? C13' C14' 1.384(8) . ? C13' C18' 1.385(8) . ? C14' C15' 1.391(8) . ? C15' C16' 1.387(8) . ? C16' C17' 1.385(8) . ? C17' C18' 1.387(8) . ? C18' C22' 1.54(3) . ? C19' C20' 1.50(4) . ? C19' C21' 1.51(5) . ? C22' C24' 1.38(6) . ? C22' C23' 1.57(4) . ? C41' C42' 1.34(4) . ? C42' C43' 1.30(6) . ? C43' C44' 1.49(6) . ? C45' C46' 1.461(9) . ? C46' C47' 1.456(9) . ? C47' C48' 1.452(9) . ? 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 La1 O3 99.1(3) . . ? O1 La1 O2 102.0(3) . . ? O3 La1 O2 104.3(3) . . ? O1 La1 O6 84.8(3) . . ? O3 La1 O6 162.3(3) . . ? O2 La1 O6 91.6(3) . . ? O1 La1 O5 164.6(3) . . ? O3 La1 O5 94.2(3) . . ? O2 La1 O5 82.1(3) . . ? O6 La1 O5 80.2(3) . . ? O1 La1 O4 94.1(2) . . ? O3 La1 O4 85.9(3) . . ? O2 La1 O4 159.1(2) . . ? O6 La1 O4 76.5(2) . . ? O5 La1 O4 79.0(2) . . ? C1 O1 La1 162.8(6) . . ? C2 C1 O1 119.8(10) . . ? C2 C1 C6 121.2(11) . . ? O1 C1 C6 119.0(11) . . ? C82 C81 O8 107.1(8) . . ? C13 O2 C13' 27.2(8) . . ? C13 O2 La1 154.6(11) . . ? C13' O2 La1 168.2(10) . . ? C1 C2 C3 120.0(11) . . ? C1 C2 C7 120.9(11) . . ? C3 C2 C7 119.1(11) . . ? C25 O3 La1 174.4(8) . . ? C4 C3 C2 119.3(12) . . ? C40 O4 C37 110.3(10) . . ? C40 O4 La1 130.9(7) . . ? C37 O4 La1 117.9(7) . . ? C3 C4 C5 121.8(15) . . ? C44' O5 C41' 100.2(19) . . ? C44' O5 C44 21.5(19) . . ? C41' O5 C44 111.5(16) . . ? C44' O5 C41 110(2) . . ? C41' O5 C41 34.7(14) . . ? C44 O5 C41 108.2(16) . . ? C44' O5 La1 135.4(17) . . ? C41' O5 La1 123.0(12) . . ? C44 O5 La1 125.0(12) . . ? C41 O5 La1 112.1(12) . . ? C4 C5 C6 120.0(15) . . ? C45' O6 C48 103.1(11) . . ? C45' O6 C48' 107.7(6) . . ? C48 O6 C48' 26(2) . . ? C45' O6 C45 16(2) . . ? C48 O6 C45 107.5(6) . . ? C48' O6 C45 118.6(12) . . ? C45' O6 La1 131.9(9) . . ? C48 O6 La1 124.7(8) . . ? C48' O6 La1 112.9(10) . . ? C45 O6 La1 127.0(8) . . ? C5 C6 C1 117.7(13) . . ? C5 C6 C10 125.1(16) . . ? C1 C6 C10 115.2(15) . . ? C5 C6 C10' 120.3(14) . . ? C1 C6 C10' 120.9(13) . . ? C10 C6 C10' 25.1(11) . . ? C71 O7 C74 108.0(6) . . ? C2 C7 C9 110.5(11) . . ? C2 C7 C8 115.8(11) . . ? C9 C7 C8 109.5(12) . . ? C84 O8 C81 107.4(8) . . ? C6 C10 C11 100(2) . . ? C6 C10 C12 114(2) . . ? C11 C10 C12 103(2) . . ? O2 C13 C14 111.0(14) . . ? O2 C13 C18 128.4(14) . . ? C14 C13 C18 120.3(7) . . ? C13 C14 C15 119.8(7) . . ? C13 C14 C19' 124.6(18) . . ? C15 C14 C19' 115.6(18) . . ? C16 C15 C14 119.6(7) . . ? C15 C16 C17 120.5(7) . . ? C16 C17 C18 120.0(7) . . ? C13 C18 C17 119.6(7) . . ? C13 C18 C22 118.5(15) . . ? C17 C18 C22 119.9(16) . . ? C21 C19 C20 113(4) . . ? C21 C19 C14' 109(3) . . ? C20 C19 C14' 114(3) . . ? C24 C22 C23 110(3) . . ? C24 C22 C18 118(3) . . ? C23 C22 C18 115(2) . . ? O3 C25 C26 120.7(11) . . ? O3 C25 C30 118.2(11) . . ? C26 C25 C30 121.2(11) . . ? C25 C26 C27 122.5(13) . . ? C25 C26 C31 122.3(12) . . ? C27 C26 C31 115.2(13) . . ? C26 C27 C28 117.8(17) . . ? C29 C28 C27 118.9(18) . . ? C28 C29 C30 123.6(16) . . ? C29 C30 C34 121.9(13) . . ? C29 C30 C25 115.8(13) . . ? C34 C30 C25 122.1(12) . . ? C26 C31 C32 111.5(12) . . ? C26 C31 C33 119.3(14) . . ? C32 C31 C33 101.3(14) . . ? C30 C34 C35 112.8(16) . . ? C30 C34 C36 112.8(14) . . ? C35 C34 C36 112.6(17) . . ? O4 C37 C38 106.6(12) . . ? C39 C38 C37 103.4(14) . . ? C38 C39 C40 105.6(14) . . ? O4 C40 C39 106.1(11) . . ? C42 C41 O5 103(3) . . ? C41 C42 C43 116(3) . . ? C44 C43 C42 105(2) . . ? C43 C44 O5 103(2) . . ? C46 C45 O6 107.4(5) . . ? C47 C46 C45 107.4(6) . . ? C46 C47 C48 106.5(7) . . ? O6 C48 C47 106.7(7) . . ? O7 C71 C72 107.8(6) . . ? C73 C72 C71 107.4(8) . . ? C74 C73 C72 107.5(8) . . ? C73 C74 O7 107.4(7) . . ? C81 C82 C83 107.5(8) . . ? C84 C83 C82 107.8(6) . . ? C83 C84 O8 107.8(6) . . ? C12' C10' C11' 108(2) . . ? C12' C10' C6 115.4(19) . . ? C11' C10' C6 115.1(18) . . ? C14' C13' C18' 120.4(7) . . ? C14' C13' O2 127.2(12) . . ? C18' C13' O2 112.3(12) . . ? C13' C14' C15' 119.8(7) . . ? C13' C14' C19 120.1(19) . . ? C15' C14' C19 120.1(19) . . ? C16' C15' C14' 119.6(7) . . ? C17' C16' C15' 120.4(7) . . ? C16' C17' C18' 119.6(7) . . ? C13' C18' C17' 119.9(7) . . ? C13' C18' C22' 117.5(16) . . ? C17' C18' C22' 122.5(16) . . ? C20' C19' C21' 107(3) . . ? C20' C19' C14 120(3) . . ? C21' C19' C14 113(3) . . ? C24' C22' C18' 113(3) . . ? C24' C22' C23' 112(3) . . ? C18' C22' C23' 107(2) . . ? C42' C41' O5 112(3) . . ? C43' C42' C41' 106(4) . . ? C42' C43' C44' 106(5) . . ? O5 C44' C43' 110(3) . . ? O6 C45' C46' 107.4(6) . . ? C47' C46' C45' 107.9(6) . . ? C48' C47' C46' 108.0(5) . . ? C47' C48' O6 107.7(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.168 _refine_diff_density_min -2.630 _refine_diff_density_rms 0.130