Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof Glen Deacon' _publ_contact_author_address ; School of Chemistry Monash University Wellington Rd Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email GLEN.DEACON@SCI.MONASH.EDU.AU _publ_section_title ; Hydrocarbon soluble, polymetallic lanthanoid aryloxides constructed utilizing ligands with distal tert-butyl groups ; loop_ _publ_author_name 'Glen Deacon' 'William J. Evans' 'Craig M. Forsyth' 'Rita Harika' 'Peter C. Junk' 'Joseph W. Ziller' data_c:\mydocu~1\craig\laoar\xtaldog\rh424\rh4la _database_code_depnum_ccdc_archive 'CCDC 236327' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Hexakis(3,5-di-tert-butlyphenolato)hexakis(tetrahydrofuran) dilanthanum(III)].5tetrahydrofuran ; _chemical_name_common ; (Hexakis(3,5-di-tert-butlyphenolato)hexakis(tetrahydrofuran) dilanthanum(iii)).5tetrahydrofuran ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H214 La2 O17' _chemical_formula_weight 2302.81 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 15.9309(3) _cell_length_b 16.3120(3) _cell_length_c 26.0616(5) _cell_angle_alpha 87.556(1) _cell_angle_beta 82.746(1) _cell_angle_gamma 72.781(1) _cell_volume 6417.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 83121 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 28.29 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method '1 deg frames in phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83121 _diffrn_reflns_av_R_equivalents 0.1353 _diffrn_reflns_av_sigmaI/netI 0.2831 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.29 _reflns_number_total 27877 _reflns_number_gt 12419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'POVRAY 3.0' _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^)+(0.0459P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27877 _refine_ls_number_parameters 1380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2011 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.170 _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 La1 La 0.19847(2) 0.778326(19) 0.288094(12) 0.02026(10) Uani 1 1 d . . . La2 La 0.37161(2) 0.535031(18) 0.262656(12) 0.01845(10) Uani 1 1 d . . . O1 O 0.2653(2) 0.8136(2) 0.35236(14) 0.0283(10) Uani 1 1 d . . . O2 O 0.1013(2) 0.8002(2) 0.22793(13) 0.0277(10) Uani 1 1 d . . . O3 O 0.3905(2) 0.3923(2) 0.27512(13) 0.0260(9) Uani 1 1 d . . . O4 O 0.5144(2) 0.5436(2) 0.25127(13) 0.0247(9) Uani 1 1 d . . . O5 O 0.2430(2) 0.62838(19) 0.31878(12) 0.0183(9) Uani 1 1 d . . . O6 O 0.3159(2) 0.68301(19) 0.22764(12) 0.0175(8) Uani 1 1 d . . . O7 O 0.1014(3) 0.9399(2) 0.30987(17) 0.0503(12) Uani 1 1 d . . . O8 O 0.2728(2) 0.8823(2) 0.23837(13) 0.0300(10) Uani 1 1 d . . . O9 O 0.0578(2) 0.7689(2) 0.34737(14) 0.0280(9) Uani 1 1 d . . . O10 O 0.4235(2) 0.5150(2) 0.35305(13) 0.0249(9) Uani 1 1 d . . . O11 O 0.4298(2) 0.4919(2) 0.16487(13) 0.0239(9) Uani 1 1 d . . . O12 O 0.2397(2) 0.5073(2) 0.22142(13) 0.0244(9) Uani 1 1 d . . . O13 O 0.2131(4) 1.2381(4) 0.1691(2) 0.0936(18) Uani 1 1 d . . . O14 O 0.3925(4) 1.0462(4) 0.0438(3) 0.113(2) Uani 1 1 d . . . O15 O 0.2163(5) 1.4606(5) 0.0645(4) 0.178(4) Uani 1 1 d . . . O16 O -0.1826(5) 0.8939(5) 0.3103(3) 0.136(3) Uani 1 1 d . . . O17 O 0.1333(8) 0.6783(5) -0.0828(3) 0.190(4) Uani 1 1 d . . . C1 C 0.2968(4) 0.8402(3) 0.3911(2) 0.0277(15) Uani 1 1 d . . . C2 C 0.2402(4) 0.8953(3) 0.4293(2) 0.0299(15) Uani 1 1 d . . . H2 H 0.1786 0.9143 0.4265 0.036 Uiso 1 1 calc R . . C3 C 0.2710(4) 0.9232(3) 0.4711(2) 0.0305(15) Uani 1 1 d . . . C4 C 0.3625(4) 0.8952(3) 0.4735(2) 0.0312(15) Uani 1 1 d . . . H4 H 0.3853 0.9145 0.5011 0.037 Uiso 1 1 calc R . . C5 C 0.4212(4) 0.8403(3) 0.4371(2) 0.0266(14) Uani 1 1 d . . . C6 C 0.3883(3) 0.8133(3) 0.3962(2) 0.0212(13) Uani 1 1 d . . . H6 H 0.4281 0.7760 0.3710 0.025 Uiso 1 1 calc R . . C7 C 0.2099(4) 0.9860(4) 0.5111(2) 0.0417(17) Uani 1 1 d . . . C8 C 0.2209(6) 1.0757(4) 0.5021(3) 0.122(4) Uani 1 1 d . . . H8A H 0.1802 1.1155 0.5275 0.183 Uiso 1 1 calc R . . H8B H 0.2078 1.0954 0.4671 0.183 Uiso 1 1 calc R . . H8C H 0.2820 1.0737 0.5058 0.183 Uiso 1 1 calc R . . C9 C 0.1139(5) 0.9934(5) 0.5108(3) 0.117(4) Uani 1 1 d . . . H9A H 0.0783 1.0354 0.5367 0.175 Uiso 1 1 calc R . . H9B H 0.1044 0.9374 0.5190 0.175 Uiso 1 1 calc R . . H9C H 0.0964 1.0122 0.4765 0.175 Uiso 1 1 calc R . . C10 C 0.2321(5) 0.9605(6) 0.5648(3) 0.113(3) Uani 1 1 d . . . H10A H 0.1919 1.0020 0.5896 0.169 Uiso 1 1 calc R . . H10B H 0.2933 0.9596 0.5672 0.169 Uiso 1 1 calc R . . H10C H 0.2256 0.9033 0.5728 0.169 Uiso 1 1 calc R . . C11 C 0.5189(4) 0.8060(3) 0.4455(2) 0.0312(15) Uani 1 1 d . . . C12 C 0.5767(4) 0.7619(4) 0.3979(3) 0.054(2) Uani 1 1 d . . . H12A H 0.6383 0.7404 0.4053 0.081 Uiso 1 1 calc R . . H12B H 0.5726 0.8030 0.3691 0.081 Uiso 1 1 calc R . . H12C H 0.5567 0.7139 0.3886 0.081 Uiso 1 1 calc R . . C13 C 0.5258(4) 0.7408(4) 0.4908(2) 0.052(2) Uani 1 1 d . . . H13A H 0.4890 0.7692 0.5218 0.078 Uiso 1 1 calc R . . H13B H 0.5876 0.7190 0.4979 0.078 Uiso 1 1 calc R . . H13C H 0.5053 0.6930 0.4816 0.078 Uiso 1 1 calc R . . C14 C 0.5562(4) 0.8765(3) 0.4612(2) 0.0423(17) Uani 1 1 d . . . H14A H 0.5197 0.9060 0.4919 0.063 Uiso 1 1 calc R . . H14B H 0.5556 0.9178 0.4327 0.063 Uiso 1 1 calc R . . H14C H 0.6171 0.8508 0.4690 0.063 Uiso 1 1 calc R . . C15 C 0.0496(3) 0.8300(4) 0.1910(2) 0.0298(15) Uani 1 1 d . . . C16 C 0.0166(3) 0.7746(3) 0.1644(2) 0.0258(14) Uani 1 1 d . . . H16 H 0.0306 0.7155 0.1737 0.031 Uiso 1 1 calc R . . C17 C -0.0358(3) 0.8048(4) 0.1248(2) 0.0336(16) Uani 1 1 d . . . C18 C -0.0565(4) 0.8930(4) 0.1117(2) 0.0362(16) Uani 1 1 d . . . H18 H -0.0921 0.9139 0.0845 0.043 Uiso 1 1 calc R . . C19 C -0.0263(4) 0.9506(4) 0.1374(2) 0.0354(16) Uani 1 1 d . A . C20 C 0.0269(3) 0.9180(3) 0.1762(2) 0.0297(15) Uani 1 1 d . . . H20 H 0.0490 0.9559 0.1936 0.036 Uiso 1 1 calc R . . C21 C -0.0681(4) 0.7447(4) 0.0933(2) 0.0344(16) Uani 1 1 d . . . C22 C -0.0355(4) 0.6507(4) 0.1098(3) 0.059(2) Uani 1 1 d . . . H22A H -0.0566 0.6449 0.1464 0.088 Uiso 1 1 calc R . . H22B H 0.0294 0.6314 0.1049 0.088 Uiso 1 1 calc R . . H22C H -0.0582 0.6156 0.0888 0.088 Uiso 1 1 calc R . . C23 C -0.0347(4) 0.7513(4) 0.0367(2) 0.0483(18) Uani 1 1 d . . . H23A H -0.0560 0.8110 0.0251 0.072 Uiso 1 1 calc R . . H23B H -0.0567 0.7148 0.0163 0.072 Uiso 1 1 calc R . . H23C H 0.0301 0.7325 0.0322 0.072 Uiso 1 1 calc R . . C24 C -0.1701(4) 0.7742(4) 0.0999(2) 0.057(2) Uani 1 1 d . . . H24A H -0.1923 0.7694 0.1364 0.086 Uiso 1 1 calc R . . H24B H -0.1916 0.7380 0.0789 0.086 Uiso 1 1 calc R . . H24C H -0.1913 0.8341 0.0886 0.086 Uiso 1 1 calc R . . C25 C -0.0479(4) 1.0437(4) 0.1211(3) 0.0407(18) Uani 1 1 d . . . C26 C -0.0816(14) 1.1012(10) 0.1705(6) 0.049(6) Uani 0.452(16) 1 d P A 1 H26A H -0.0375 1.0847 0.1950 0.074 Uiso 0.452(16) 1 calc PR A 1 H26B H -0.1375 1.0931 0.1868 0.074 Uiso 0.452(16) 1 calc PR A 1 H26C H -0.0909 1.1616 0.1607 0.074 Uiso 0.452(16) 1 calc PR A 1 C26' C -0.0076(15) 1.0906(9) 0.1490(10) 0.105(12) Uani 0.548(16) 1 d P A 2 H26D H -0.0238 1.1506 0.1373 0.158 Uiso 0.548(16) 1 calc PR A 2 H26E H 0.0569 1.0660 0.1431 0.158 Uiso 0.548(16) 1 calc PR A 2 H26F H -0.0278 1.0880 0.1860 0.158 Uiso 0.548(16) 1 calc PR A 2 C27 C -0.1146(12) 1.0717(11) 0.0822(8) 0.048(6) Uani 0.452(16) 1 d P A 1 H27A H -0.1244 1.1328 0.0743 0.072 Uiso 0.452(16) 1 calc PR A 1 H27B H -0.1707 1.0620 0.0969 0.072 Uiso 0.452(16) 1 calc PR A 1 H27C H -0.0918 1.0383 0.0504 0.072 Uiso 0.452(16) 1 calc PR A 1 C27' C -0.1485(9) 1.0778(8) 0.1214(8) 0.057(5) Uani 0.548(16) 1 d P A 2 H27D H -0.1687 1.0394 0.1013 0.086 Uiso 0.548(16) 1 calc PR A 2 H27E H -0.1640 1.1354 0.1060 0.086 Uiso 0.548(16) 1 calc PR A 2 H27F H -0.1772 1.0805 0.1571 0.086 Uiso 0.548(16) 1 calc PR A 2 C28 C 0.0359(9) 1.0636(8) 0.0948(7) 0.035(5) Uani 0.452(16) 1 d P A 1 H28A H 0.0821 1.0473 0.1180 0.052 Uiso 0.452(16) 1 calc PR A 1 H28B H 0.0222 1.1252 0.0871 0.052 Uiso 0.452(16) 1 calc PR A 1 H28C H 0.0567 1.0311 0.0626 0.052 Uiso 0.452(16) 1 calc PR A 1 C28' C -0.0123(12) 1.0468(8) 0.0618(6) 0.079(7) Uani 0.548(16) 1 d P A 2 H28D H -0.0400 1.0145 0.0419 0.119 Uiso 0.548(16) 1 calc PR A 2 H28E H 0.0520 1.0211 0.0571 0.119 Uiso 0.548(16) 1 calc PR A 2 H28F H -0.0270 1.1065 0.0499 0.119 Uiso 0.548(16) 1 calc PR A 2 C29 C 0.4178(3) 0.3088(3) 0.2656(2) 0.0250(14) Uani 1 1 d . . . C30 C 0.4535(3) 0.2769(3) 0.2160(2) 0.0230(14) Uani 1 1 d . . . H30 H 0.4575 0.3168 0.1889 0.028 Uiso 1 1 calc R . . C31 C 0.4837(3) 0.1889(3) 0.2045(2) 0.0245(14) Uani 1 1 d . . . C32 C 0.4767(3) 0.1319(3) 0.2462(2) 0.0253(14) Uani 1 1 d . . . H32 H 0.4976 0.0719 0.2399 0.030 Uiso 1 1 calc R . . C33 C 0.4403(4) 0.1602(3) 0.2960(2) 0.0260(14) Uani 1 1 d . . . C34 C 0.4097(3) 0.2492(3) 0.3053(2) 0.0255(14) Uani 1 1 d . . . H34 H 0.3832 0.2695 0.3389 0.031 Uiso 1 1 calc R . . C35 C 0.5243(4) 0.1583(3) 0.1500(2) 0.0304(15) Uani 1 1 d . . . C36 C 0.5350(4) 0.0623(3) 0.1425(2) 0.0528(19) Uani 1 1 d . . . H36A H 0.5612 0.0456 0.1071 0.079 Uiso 1 1 calc R . . H36B H 0.4769 0.0523 0.1490 0.079 Uiso 1 1 calc R . . H36C H 0.5737 0.0281 0.1669 0.079 Uiso 1 1 calc R . . C37 C 0.4643(4) 0.2095(3) 0.1108(2) 0.0422(17) Uani 1 1 d . . . H37A H 0.4903 0.1898 0.0758 0.063 Uiso 1 1 calc R . . H37B H 0.4587 0.2706 0.1137 0.063 Uiso 1 1 calc R . . H37C H 0.4057 0.2007 0.1181 0.063 Uiso 1 1 calc R . . C38 C 0.6161(4) 0.1727(4) 0.1397(2) 0.0420(17) Uani 1 1 d . . . H38A H 0.6431 0.1532 0.1048 0.063 Uiso 1 1 calc R . . H38B H 0.6538 0.1400 0.1650 0.063 Uiso 1 1 calc R . . H38C H 0.6100 0.2339 0.1428 0.063 Uiso 1 1 calc R . . C39 C 0.4311(4) 0.0979(3) 0.3411(2) 0.0364(16) Uani 1 1 d . . . C40 C 0.4578(6) 0.1232(4) 0.3890(2) 0.102(4) Uani 1 1 d . . . H40A H 0.4497 0.0830 0.4169 0.153 Uiso 1 1 calc R . . H40B H 0.4211 0.1813 0.3987 0.153 Uiso 1 1 calc R . . H40C H 0.5201 0.1219 0.3831 0.153 Uiso 1 1 calc R . . C41 C 0.3320(5) 0.0971(4) 0.3489(3) 0.077(3) Uani 1 1 d . . . H41A H 0.3168 0.0787 0.3169 0.116 Uiso 1 1 calc R . . H41B H 0.2934 0.1550 0.3578 0.116 Uiso 1 1 calc R . . H41C H 0.3238 0.0572 0.3770 0.116 Uiso 1 1 calc R . . C42 C 0.4827(4) 0.0046(3) 0.3266(2) 0.057(2) Uani 1 1 d . . . H42A H 0.4627 -0.0111 0.2954 0.085 Uiso 1 1 calc R . . H42B H 0.4723 -0.0336 0.3551 0.085 Uiso 1 1 calc R . . H42C H 0.5461 -0.0009 0.3200 0.085 Uiso 1 1 calc R . . C43 C 0.5941(4) 0.4981(3) 0.2636(2) 0.0252(14) Uani 1 1 d . . . C44 C 0.6160(3) 0.4097(3) 0.27214(19) 0.0239(14) Uani 1 1 d . . . H44 H 0.5732 0.3809 0.2686 0.029 Uiso 1 1 calc R . . C45 C 0.6984(4) 0.3622(3) 0.2857(2) 0.0270(14) Uani 1 1 d . B . C46 C 0.7598(3) 0.4056(3) 0.2915(2) 0.0280(15) Uani 1 1 d . . . H46 H 0.8162 0.3742 0.3010 0.034 Uiso 1 1 calc R . . C47 C 0.7409(3) 0.4933(3) 0.28378(19) 0.0245(14) Uani 1 1 d . . . C48 C 0.6581(3) 0.5395(3) 0.27013(19) 0.0234(14) Uani 1 1 d . . . H48 H 0.6445 0.5999 0.2652 0.028 Uiso 1 1 calc R . . C49 C 0.7192(4) 0.2650(3) 0.2953(2) 0.0309(15) Uani 1 1 d . . . C50 C 0.6551(8) 0.2529(6) 0.3451(5) 0.067(4) Uani 0.667(11) 1 d P B 1 H50A H 0.6687 0.2788 0.3750 0.101 Uiso 0.667(11) 1 calc PR B 1 H50B H 0.6636 0.1916 0.3516 0.101 Uiso 0.667(11) 1 calc PR B 1 H50C H 0.5935 0.2809 0.3392 0.101 Uiso 0.667(11) 1 calc PR B 1 C50' C 0.6416(13) 0.2322(12) 0.2956(11) 0.053(8) Uani 0.333(11) 1 d P B 2 H50D H 0.6183 0.2444 0.2621 0.080 Uiso 0.333(11) 1 calc PR B 2 H50E H 0.5955 0.2605 0.3231 0.080 Uiso 0.333(11) 1 calc PR B 2 H50F H 0.6596 0.1701 0.3018 0.080 Uiso 0.333(11) 1 calc PR B 2 C51 C 0.6967(8) 0.2234(5) 0.2510(4) 0.053(4) Uani 0.667(11) 1 d P B 1 H51A H 0.7101 0.1615 0.2574 0.079 Uiso 0.667(11) 1 calc PR B 1 H51B H 0.7316 0.2338 0.2190 0.079 Uiso 0.667(11) 1 calc PR B 1 H51C H 0.6335 0.2476 0.2476 0.079 Uiso 0.667(11) 1 calc PR B 1 C51' C 0.7963(15) 0.2189(11) 0.2514(8) 0.055(8) Uani 0.333(11) 1 d P B 2 H51D H 0.8475 0.2400 0.2525 0.082 Uiso 0.333(11) 1 calc PR B 2 H51E H 0.7751 0.2316 0.2174 0.082 Uiso 0.333(11) 1 calc PR B 2 H51F H 0.8135 0.1567 0.2573 0.082 Uiso 0.333(11) 1 calc PR B 2 C52 C 0.8111(7) 0.2229(6) 0.3084(5) 0.058(4) Uani 0.667(11) 1 d P B 1 H52A H 0.8218 0.2523 0.3378 0.088 Uiso 0.667(11) 1 calc PR B 1 H52B H 0.8539 0.2262 0.2784 0.088 Uiso 0.667(11) 1 calc PR B 1 H52C H 0.8176 0.1626 0.3174 0.088 Uiso 0.667(11) 1 calc PR B 1 C52' C 0.7491(14) 0.2452(10) 0.3481(8) 0.038(6) Uani 0.333(11) 1 d P B 2 H52D H 0.7989 0.2678 0.3507 0.056 Uiso 0.333(11) 1 calc PR B 2 H52E H 0.7678 0.1829 0.3535 0.056 Uiso 0.333(11) 1 calc PR B 2 H52F H 0.7001 0.2719 0.3745 0.056 Uiso 0.333(11) 1 calc PR B 2 C53 C 0.8069(3) 0.5430(4) 0.2914(2) 0.0305(15) Uani 1 1 d . . . C54 C 0.7672(4) 0.6074(4) 0.3353(2) 0.0454(18) Uani 1 1 d . . . H54A H 0.8087 0.6397 0.3400 0.068 Uiso 1 1 calc R . . H54B H 0.7563 0.5765 0.3673 0.068 Uiso 1 1 calc R . . H54C H 0.7113 0.6471 0.3267 0.068 Uiso 1 1 calc R . . C55 C 0.8964(3) 0.4836(4) 0.3043(2) 0.0438(18) Uani 1 1 d . . . H55A H 0.9225 0.4423 0.2763 0.066 Uiso 1 1 calc R . . H55B H 0.8876 0.4528 0.3367 0.066 Uiso 1 1 calc R . . H55C H 0.9363 0.5180 0.3082 0.066 Uiso 1 1 calc R . . C56 C 0.8252(4) 0.5924(3) 0.2414(2) 0.0399(17) Uani 1 1 d . . . H56A H 0.8513 0.5517 0.2131 0.060 Uiso 1 1 calc R . . H56B H 0.8664 0.6246 0.2469 0.060 Uiso 1 1 calc R . . H56C H 0.7696 0.6324 0.2326 0.060 Uiso 1 1 calc R . . C57 C 0.2223(3) 0.5954(3) 0.3661(2) 0.0183(13) Uani 1 1 d . . . C58 C 0.2312(3) 0.6318(3) 0.4111(2) 0.0227(14) Uani 1 1 d . . . H58 H 0.2503 0.6819 0.4092 0.027 Uiso 1 1 calc R . . C59 C 0.2126(3) 0.5962(3) 0.4596(2) 0.0243(14) Uani 1 1 d . . . C60 C 0.1848(3) 0.5223(4) 0.4603(2) 0.0288(15) Uani 1 1 d . . . H60 H 0.1711 0.4976 0.4928 0.035 Uiso 1 1 calc R . . C61 C 0.1765(3) 0.4837(3) 0.4157(2) 0.0245(14) Uani 1 1 d . . . C62 C 0.1953(3) 0.5213(3) 0.3684(2) 0.0213(14) Uani 1 1 d . . . H62 H 0.1896 0.4962 0.3373 0.026 Uiso 1 1 calc R . . C63 C 0.2222(4) 0.6371(4) 0.5096(2) 0.0306(15) Uani 1 1 d . . . C64 C 0.1455(4) 0.7195(4) 0.5208(2) 0.059(2) Uani 1 1 d . . . H64A H 0.1522 0.7455 0.5527 0.089 Uiso 1 1 calc R . . H64B H 0.0893 0.7056 0.5250 0.089 Uiso 1 1 calc R . . H64C H 0.1462 0.7599 0.4920 0.089 Uiso 1 1 calc R . . C65 C 0.3085(4) 0.6619(4) 0.5040(2) 0.0472(18) Uani 1 1 d . . . H65A H 0.3134 0.6885 0.5361 0.071 Uiso 1 1 calc R . . H65B H 0.3085 0.7027 0.4753 0.071 Uiso 1 1 calc R . . H65C H 0.3590 0.6104 0.4971 0.071 Uiso 1 1 calc R . . C66 C 0.2231(4) 0.5769(4) 0.5563(2) 0.060(2) Uani 1 1 d . . . H66A H 0.2290 0.6058 0.5872 0.090 Uiso 1 1 calc R . . H66B H 0.2731 0.5248 0.5501 0.090 Uiso 1 1 calc R . . H66C H 0.1677 0.5613 0.5614 0.090 Uiso 1 1 calc R . . C67 C 0.1486(4) 0.4005(4) 0.4194(2) 0.0353(16) Uani 1 1 d . . . C68 C 0.0572(5) 0.4164(4) 0.4481(3) 0.086(3) Uani 1 1 d . . . H68A H 0.0552 0.4416 0.4819 0.129 Uiso 1 1 calc R . . H68B H 0.0429 0.3620 0.4531 0.129 Uiso 1 1 calc R . . H68C H 0.0141 0.4560 0.4281 0.129 Uiso 1 1 calc R . . C69 C 0.1506(5) 0.3625(4) 0.3668(3) 0.067(2) Uani 1 1 d . . . H69A H 0.2104 0.3502 0.3483 0.101 Uiso 1 1 calc R . . H69B H 0.1088 0.4036 0.3467 0.101 Uiso 1 1 calc R . . H69C H 0.1338 0.3093 0.3715 0.101 Uiso 1 1 calc R . . C70 C 0.2123(5) 0.3310(4) 0.4492(3) 0.087(3) Uani 1 1 d . . . H70A H 0.2133 0.3524 0.4836 0.130 Uiso 1 1 calc R . . H70B H 0.2719 0.3169 0.4303 0.130 Uiso 1 1 calc R . . H70C H 0.1923 0.2795 0.4526 0.130 Uiso 1 1 calc R . . C71 C 0.3484(3) 0.7020(3) 0.1789(2) 0.0165(13) Uani 1 1 d . . . C72 C 0.2945(3) 0.7230(3) 0.1395(2) 0.0193(13) Uani 1 1 d . . . H72 H 0.2337 0.7260 0.1467 0.023 Uiso 1 1 calc R . . C73 C 0.3280(3) 0.7398(3) 0.0898(2) 0.0205(13) Uani 1 1 d . . . C74 C 0.4173(4) 0.7371(3) 0.0809(2) 0.0258(14) Uani 1 1 d . . . H74 H 0.4414 0.7483 0.0470 0.031 Uiso 1 1 calc R . . C75 C 0.4716(3) 0.7186(3) 0.1199(2) 0.0226(14) Uani 1 1 d . . . C76 C 0.4367(3) 0.7002(3) 0.1691(2) 0.0205(13) Uani 1 1 d . . . H76 H 0.4734 0.6864 0.1962 0.025 Uiso 1 1 calc R . . C77 C 0.2673(3) 0.7585(3) 0.0464(2) 0.0250(14) Uani 1 1 d . . . C78 C 0.3172(4) 0.7679(3) -0.00665(19) 0.0347(16) Uani 1 1 d . . . H78A H 0.3432 0.8152 -0.0057 0.052 Uiso 1 1 calc R . . H78B H 0.2760 0.7802 -0.0328 0.052 Uiso 1 1 calc R . . H78C H 0.3642 0.7145 -0.0153 0.052 Uiso 1 1 calc R . . C79 C 0.1919(4) 0.8406(3) 0.0582(2) 0.0366(16) Uani 1 1 d . . . H79A H 0.2163 0.8887 0.0604 0.055 Uiso 1 1 calc R . . H79B H 0.1574 0.8341 0.0912 0.055 Uiso 1 1 calc R . . H79C H 0.1535 0.8518 0.0306 0.055 Uiso 1 1 calc R . . C80 C 0.2294(4) 0.6831(3) 0.0428(2) 0.0332(16) Uani 1 1 d . . . H80A H 0.1907 0.6945 0.0153 0.050 Uiso 1 1 calc R . . H80B H 0.1953 0.6762 0.0759 0.050 Uiso 1 1 calc R . . H80C H 0.2780 0.6305 0.0349 0.050 Uiso 1 1 calc R . . C81 C 0.5685(4) 0.7192(3) 0.1076(2) 0.0286(15) Uani 1 1 d . . . C82 C 0.5721(4) 0.8083(4) 0.0884(2) 0.054(2) Uani 1 1 d . . . H82A H 0.5412 0.8236 0.0576 0.081 Uiso 1 1 calc R . . H82B H 0.6340 0.8077 0.0798 0.081 Uiso 1 1 calc R . . H82C H 0.5434 0.8506 0.1156 0.081 Uiso 1 1 calc R . . C83 C 0.6160(4) 0.6529(4) 0.0653(3) 0.057(2) Uani 1 1 d . . . H83A H 0.5852 0.6664 0.0344 0.086 Uiso 1 1 calc R . . H83B H 0.6160 0.5954 0.0779 0.086 Uiso 1 1 calc R . . H83C H 0.6772 0.6545 0.0567 0.086 Uiso 1 1 calc R . . C84 C 0.6186(4) 0.6963(4) 0.1547(2) 0.055(2) Uani 1 1 d . . . H84A H 0.6175 0.6392 0.1674 0.083 Uiso 1 1 calc R . . H84B H 0.5905 0.7386 0.1819 0.083 Uiso 1 1 calc R . . H84C H 0.6801 0.6964 0.1451 0.083 Uiso 1 1 calc R . . C85 C 0.1402(4) 1.0059(4) 0.3202(3) 0.051(2) Uani 1 1 d . . . H85A H 0.1602 1.0312 0.2874 0.061 Uiso 1 1 calc R . . H85B H 0.1916 0.9820 0.3397 0.061 Uiso 1 1 calc R . . C86 C 0.0684(6) 1.0732(4) 0.3520(3) 0.083(3) Uani 1 1 d . . . H86A H 0.0801 1.0714 0.3885 0.100 Uiso 1 1 calc R . . H86B H 0.0636 1.1315 0.3378 0.100 Uiso 1 1 calc R . . C87 C -0.0087(7) 1.0500(6) 0.3477(6) 0.187(7) Uani 1 1 d . . . H87A H -0.0530 1.0992 0.3336 0.224 Uiso 1 1 calc R . . H87B H -0.0342 1.0364 0.3825 0.224 Uiso 1 1 calc R . . C88 C 0.0090(4) 0.9760(5) 0.3141(2) 0.059(2) Uani 1 1 d . . . H88A H -0.0215 0.9345 0.3297 0.071 Uiso 1 1 calc R . . H88B H -0.0108 0.9940 0.2798 0.071 Uiso 1 1 calc R . . C89 C 0.2511(4) 0.9318(3) 0.1917(2) 0.0366(17) Uani 1 1 d . . . H89A H 0.2109 0.9899 0.2004 0.044 Uiso 1 1 calc R . . H89B H 0.2221 0.9028 0.1699 0.044 Uiso 1 1 calc R . . C90 C 0.3386(4) 0.9371(4) 0.1642(2) 0.0398(17) Uani 1 1 d . . . H90A H 0.3310 0.9891 0.1422 0.048 Uiso 1 1 calc R . . H90B H 0.3687 0.8857 0.1427 0.048 Uiso 1 1 calc R . . C91 C 0.3891(4) 0.9412(4) 0.2091(2) 0.0418(17) Uani 1 1 d . . . H91A H 0.3734 1.0005 0.2223 0.050 Uiso 1 1 calc R . . H91B H 0.4538 0.9205 0.1988 0.050 Uiso 1 1 calc R . . C92 C 0.3593(4) 0.8820(3) 0.2492(2) 0.0346(16) Uani 1 1 d . . . H92A H 0.4009 0.8233 0.2462 0.041 Uiso 1 1 calc R . . H92B H 0.3565 0.9034 0.2845 0.041 Uiso 1 1 calc R . . C93 C 0.0072(4) 0.7151(4) 0.3338(3) 0.0499(19) Uani 1 1 d . . . H93A H 0.0469 0.6581 0.3224 0.060 Uiso 1 1 calc R . . H93B H -0.0276 0.7414 0.3053 0.060 Uiso 1 1 calc R . . C94 C -0.0533(4) 0.7064(5) 0.3815(3) 0.062(2) Uani 1 1 d . . . H94A H -0.1128 0.7479 0.3808 0.074 Uiso 1 1 calc R . . H94B H -0.0592 0.6476 0.3847 0.074 Uiso 1 1 calc R . . C95 C -0.0091(4) 0.7254(4) 0.4248(2) 0.0459(18) Uani 1 1 d . . . H95A H 0.0362 0.6736 0.4354 0.055 Uiso 1 1 calc R . . H95B H -0.0525 0.7488 0.4551 0.055 Uiso 1 1 calc R . . C96 C 0.0326(4) 0.7920(4) 0.4003(2) 0.0428(17) Uani 1 1 d . . . H96A H -0.0103 0.8500 0.4036 0.051 Uiso 1 1 calc R . . H96B H 0.0850 0.7916 0.4172 0.051 Uiso 1 1 calc R . . C97 C 0.4661(3) 0.5713(3) 0.3738(2) 0.0287(15) Uani 1 1 d . . . H97A H 0.4230 0.6149 0.3968 0.034 Uiso 1 1 calc R . . H97B H 0.4938 0.6009 0.3457 0.034 Uiso 1 1 calc R . . C98 C 0.5353(4) 0.5118(4) 0.4037(2) 0.0406(17) Uani 1 1 d . . . H98A H 0.5500 0.5429 0.4315 0.049 Uiso 1 1 calc R . . H98B H 0.5900 0.4846 0.3807 0.049 Uiso 1 1 calc R . . C99 C 0.4902(4) 0.4455(4) 0.4261(2) 0.051(2) Uani 1 1 d . . . H99A H 0.5342 0.3887 0.4295 0.061 Uiso 1 1 calc R . . H99B H 0.4571 0.4633 0.4606 0.061 Uiso 1 1 calc R . . C100 C 0.4284(4) 0.4424(3) 0.3877(2) 0.0347(16) Uani 1 1 d . . . H10D H 0.4509 0.3881 0.3681 0.042 Uiso 1 1 calc R . . H10E H 0.3690 0.4457 0.4058 0.042 Uiso 1 1 calc R . . C101 C 0.5234(4) 0.4692(3) 0.1449(2) 0.0279(15) Uani 1 1 d . . . H10F H 0.5580 0.4215 0.1654 0.034 Uiso 1 1 calc R . . H10G H 0.5462 0.5191 0.1468 0.034 Uiso 1 1 calc R . . C102 C 0.5306(4) 0.4422(4) 0.0892(2) 0.0377(16) Uani 1 1 d . . . H10H H 0.5800 0.4568 0.0676 0.045 Uiso 1 1 calc R . . H10I H 0.5386 0.3799 0.0866 0.045 Uiso 1 1 calc R . . C103 C 0.4416(4) 0.4950(4) 0.0738(2) 0.0354(16) Uani 1 1 d . . . H10J H 0.4415 0.5546 0.0648 0.042 Uiso 1 1 calc R . . H10K H 0.4259 0.4690 0.0441 0.042 Uiso 1 1 calc R . . C104 C 0.3791(4) 0.4924(3) 0.1219(2) 0.0336(16) Uani 1 1 d . . . H10L H 0.3264 0.5434 0.1235 0.040 Uiso 1 1 calc R . . H10M H 0.3596 0.4401 0.1226 0.040 Uiso 1 1 calc R . . C105 C 0.2227(3) 0.4243(3) 0.2192(2) 0.0283(15) Uani 1 1 d . . . H10N H 0.2360 0.3912 0.2514 0.034 Uiso 1 1 calc R . . H10O H 0.2599 0.3905 0.1896 0.034 Uiso 1 1 calc R . . C106 C 0.1250(4) 0.4438(3) 0.2128(3) 0.0431(18) Uani 1 1 d . . . H10P H 0.1172 0.4312 0.1772 0.052 Uiso 1 1 calc R . . H10Q H 0.0962 0.4097 0.2375 0.052 Uiso 1 1 calc R . . C107 C 0.0873(4) 0.5383(3) 0.2241(3) 0.0447(18) Uani 1 1 d . . . H10R H 0.0366 0.5649 0.2045 0.054 Uiso 1 1 calc R . . H10S H 0.0679 0.5484 0.2615 0.054 Uiso 1 1 calc R . . C108 C 0.1636(3) 0.5728(3) 0.2066(2) 0.0318(16) Uani 1 1 d . . . H10T H 0.1691 0.5820 0.1686 0.038 Uiso 1 1 calc R . . H10U H 0.1563 0.6278 0.2238 0.038 Uiso 1 1 calc R . . C109 C 0.1288(5) 1.2224(5) 0.1689(3) 0.076(3) Uani 1 1 d . . . H10V H 0.1365 1.1679 0.1510 0.091 Uiso 1 1 calc R . . H10W H 0.0885 1.2696 0.1509 0.091 Uiso 1 1 calc R . . C110 C 0.0915(5) 1.2172(5) 0.2245(3) 0.071(2) Uani 1 1 d . . . H11A H 0.0735 1.1642 0.2308 0.085 Uiso 1 1 calc R . . H11B H 0.0393 1.2673 0.2335 0.085 Uiso 1 1 calc R . . C111 C 0.1650(6) 1.2165(5) 0.2559(3) 0.077(3) Uani 1 1 d . . . H11C H 0.1548 1.2726 0.2726 0.092 Uiso 1 1 calc R . . H11D H 0.1725 1.1708 0.2827 0.092 Uiso 1 1 calc R . . C112 C 0.2432(5) 1.1982(4) 0.2145(4) 0.073(3) Uani 1 1 d . . . H11E H 0.2897 1.2211 0.2247 0.087 Uiso 1 1 calc R . . H11F H 0.2686 1.1356 0.2092 0.087 Uiso 1 1 calc R . . C113 C 0.3741(5) 0.9838(4) 0.0116(3) 0.070(2) Uani 1 1 d . . . H11G H 0.3664 0.9345 0.0331 0.084 Uiso 1 1 calc R . . H11H H 0.4245 0.9622 -0.0155 0.084 Uiso 1 1 calc R . . C114 C 0.2932(6) 1.0248(5) -0.0125(3) 0.073(3) Uani 1 1 d . . . H11I H 0.2609 0.9834 -0.0184 0.088 Uiso 1 1 calc R . . H11J H 0.3057 1.0539 -0.0454 0.088 Uiso 1 1 calc R . . C115 C 0.2429(5) 1.0895(5) 0.0304(3) 0.080(3) Uani 1 1 d . . . H11K H 0.2013 1.1403 0.0159 0.096 Uiso 1 1 calc R . . H11L H 0.2094 1.0626 0.0571 0.096 Uiso 1 1 calc R . . C116 C 0.3124(5) 1.1128(4) 0.0516(3) 0.066(2) Uani 1 1 d . . . H11M H 0.3202 1.1660 0.0346 0.079 Uiso 1 1 calc R . . H11N H 0.2956 1.1242 0.0891 0.079 Uiso 1 1 calc R . . C117 C 0.1662(8) 1.4871(6) 0.0236(4) 0.141(5) Uani 1 1 d . . . H11O H 0.2057 1.4845 -0.0092 0.170 Uiso 1 1 calc R . . H11P H 0.1284 1.5470 0.0290 0.170 Uiso 1 1 calc R . . C118 C 0.1132(7) 1.4323(6) 0.0213(5) 0.149(5) Uani 1 1 d . . . H11Q H 0.1094 1.4193 -0.0150 0.179 Uiso 1 1 calc R . . H11R H 0.0528 1.4577 0.0390 0.179 Uiso 1 1 calc R . . C119 C 0.1609(8) 1.3556(6) 0.0484(4) 0.148(5) Uani 1 1 d . . . H11S H 0.1205 1.3410 0.0770 0.178 Uiso 1 1 calc R . . H11T H 0.1824 1.3065 0.0243 0.178 Uiso 1 1 calc R . . C120 C 0.2337(6) 1.3711(5) 0.0685(3) 0.080(3) Uani 1 1 d . . . H12D H 0.2363 1.3519 0.1050 0.096 Uiso 1 1 calc R . . H12E H 0.2903 1.3413 0.0478 0.096 Uiso 1 1 calc R . . C121 C -0.1910(9) 0.9479(8) 0.2691(6) 0.209(8) Uani 1 1 d . . . H12F H -0.1330 0.9354 0.2475 0.251 Uiso 1 1 calc R . . H12G H -0.2058 1.0074 0.2818 0.251 Uiso 1 1 calc R . . C122 C -0.2563(7) 0.9437(9) 0.2370(4) 0.140(5) Uani 1 1 d . . . H12H H -0.2319 0.9383 0.2000 0.168 Uiso 1 1 calc R . . H12I H -0.3089 0.9949 0.2415 0.168 Uiso 1 1 calc R . . C123 C -0.2775(10) 0.8667(8) 0.2563(6) 0.175(6) Uani 1 1 d . . . H12J H -0.2416 0.8155 0.2361 0.210 Uiso 1 1 calc R . . H12K H -0.3411 0.8724 0.2564 0.210 Uiso 1 1 calc R . . C124 C -0.2522(8) 0.8635(8) 0.3110(7) 0.208(8) Uani 1 1 d . . . H12L H -0.3028 0.8987 0.3344 0.249 Uiso 1 1 calc R . . H12M H -0.2370 0.8037 0.3241 0.249 Uiso 1 1 calc R . . C125 C 0.0736(6) 0.6642(6) -0.1146(6) 0.116(4) Uani 1 1 d . . . H12N H 0.0301 0.6403 -0.0935 0.139 Uiso 1 1 calc R . . H12O H 0.0409 0.7195 -0.1295 0.139 Uiso 1 1 calc R . . C126 C 0.1149(7) 0.6119(8) -0.1513(5) 0.185(7) Uani 1 1 d . . . H12P H 0.1120 0.6430 -0.1848 0.222 Uiso 1 1 calc R . . H12Q H 0.0861 0.5661 -0.1528 0.222 Uiso 1 1 calc R . . C127 C 0.2084(6) 0.5732(6) -0.1427(4) 0.105(3) Uani 1 1 d . . . H12R H 0.2175 0.5158 -0.1264 0.126 Uiso 1 1 calc R . . H12S H 0.2482 0.5679 -0.1756 0.126 Uiso 1 1 calc R . . C128 C 0.2233(6) 0.6311(7) -0.1094(4) 0.116(4) Uani 1 1 d . . . H12T H 0.2509 0.6716 -0.1291 0.139 Uiso 1 1 calc R . . H12U H 0.2627 0.6003 -0.0838 0.139 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 0.0194(2) 0.01922(19) 0.0190(2) -0.00299(16) -0.00324(17) 0.00000(16) La2 0.0173(2) 0.01672(18) 0.0194(2) -0.00120(16) -0.00114(16) -0.00236(15) O1 0.031(2) 0.028(2) 0.026(2) -0.0086(19) -0.006(2) -0.0056(19) O2 0.029(2) 0.032(2) 0.018(2) -0.0002(18) -0.0160(19) 0.0032(18) O3 0.039(3) 0.0077(19) 0.028(2) -0.0019(18) -0.002(2) -0.0018(18) O4 0.019(2) 0.029(2) 0.026(2) 0.0011(19) -0.0032(19) -0.0052(18) O5 0.018(2) 0.0187(19) 0.014(2) -0.0025(17) 0.0027(17) -0.0006(16) O6 0.018(2) 0.0198(19) 0.013(2) -0.0004(17) -0.0015(17) -0.0024(17) O7 0.036(3) 0.035(3) 0.069(3) -0.018(2) -0.013(3) 0.012(2) O8 0.038(3) 0.025(2) 0.028(2) 0.0025(19) -0.007(2) -0.0098(19) O9 0.024(2) 0.031(2) 0.029(3) -0.010(2) -0.003(2) -0.0085(19) O10 0.024(2) 0.026(2) 0.026(2) 0.0026(19) -0.0089(19) -0.0076(18) O11 0.019(2) 0.027(2) 0.022(2) -0.0020(18) 0.0033(19) -0.0028(18) O12 0.020(2) 0.021(2) 0.032(2) -0.0052(18) -0.0030(19) -0.0059(18) O13 0.085(5) 0.124(5) 0.073(4) -0.004(4) -0.001(4) -0.035(4) O14 0.093(5) 0.113(5) 0.136(6) 0.005(5) -0.016(5) -0.036(5) O15 0.219(9) 0.095(6) 0.265(11) 0.055(6) -0.138(8) -0.081(6) O16 0.112(6) 0.133(6) 0.163(7) 0.053(6) -0.023(5) -0.041(5) O17 0.188(10) 0.192(8) 0.109(7) -0.044(6) -0.028(7) 0.081(8) C1 0.037(4) 0.019(3) 0.028(4) 0.003(3) -0.005(3) -0.011(3) C2 0.033(4) 0.031(3) 0.028(4) 0.001(3) -0.011(3) -0.011(3) C3 0.036(4) 0.029(3) 0.027(4) -0.006(3) 0.000(3) -0.011(3) C4 0.038(4) 0.036(4) 0.027(4) -0.004(3) -0.011(3) -0.018(3) C5 0.026(4) 0.023(3) 0.029(4) -0.002(3) 0.002(3) -0.008(3) C6 0.020(4) 0.019(3) 0.022(3) -0.005(3) 0.000(3) -0.003(3) C7 0.037(4) 0.051(4) 0.037(4) -0.020(3) 0.008(3) -0.015(4) C8 0.147(9) 0.056(6) 0.139(9) -0.056(6) 0.066(7) -0.019(6) C9 0.031(5) 0.175(9) 0.137(9) -0.127(7) 0.025(5) -0.018(6) C10 0.086(7) 0.184(9) 0.030(5) -0.039(6) -0.003(5) 0.023(6) C11 0.033(4) 0.027(3) 0.033(4) -0.002(3) -0.010(3) -0.005(3) C12 0.032(4) 0.062(5) 0.066(5) -0.017(4) -0.013(4) -0.005(4) C13 0.044(5) 0.048(4) 0.067(5) 0.012(4) -0.020(4) -0.013(4) C14 0.032(4) 0.047(4) 0.050(5) -0.002(4) -0.012(4) -0.012(3) C15 0.020(4) 0.038(4) 0.024(4) 0.001(3) -0.002(3) 0.001(3) C16 0.020(3) 0.029(3) 0.029(4) 0.002(3) -0.004(3) -0.007(3) C17 0.019(4) 0.044(4) 0.037(4) -0.002(3) -0.001(3) -0.009(3) C18 0.024(4) 0.052(4) 0.028(4) 0.007(3) -0.005(3) -0.005(3) C19 0.022(4) 0.050(4) 0.033(4) 0.005(3) -0.005(3) -0.008(3) C20 0.023(4) 0.032(3) 0.035(4) -0.004(3) -0.009(3) -0.005(3) C21 0.026(4) 0.051(4) 0.035(4) 0.005(3) -0.013(3) -0.020(3) C22 0.074(5) 0.055(5) 0.065(5) 0.001(4) -0.038(5) -0.034(4) C23 0.040(4) 0.064(5) 0.044(5) -0.001(4) 0.002(4) -0.022(4) C24 0.048(5) 0.091(5) 0.046(5) 0.002(4) -0.010(4) -0.038(4) C25 0.043(5) 0.028(4) 0.048(5) 0.009(4) -0.007(4) -0.005(3) C26 0.072(15) 0.030(9) 0.042(11) 0.001(8) -0.019(11) -0.004(10) C26' 0.13(2) 0.031(9) 0.19(3) 0.048(14) -0.12(2) -0.045(14) C27 0.030(13) 0.052(11) 0.050(13) 0.016(10) -0.009(11) 0.008(9) C27' 0.040(11) 0.029(7) 0.097(15) -0.008(9) -0.014(10) 0.003(7) C28 0.031(10) 0.030(9) 0.042(12) 0.003(8) 0.006(9) -0.012(7) C28' 0.110(17) 0.058(10) 0.067(13) 0.026(9) 0.000(11) -0.028(10) C29 0.023(4) 0.024(3) 0.029(4) 0.008(3) -0.009(3) -0.007(3) C30 0.036(4) 0.018(3) 0.019(3) 0.005(3) -0.006(3) -0.014(3) C31 0.021(4) 0.020(3) 0.032(4) -0.002(3) -0.004(3) -0.005(3) C32 0.022(4) 0.020(3) 0.032(4) 0.002(3) -0.004(3) -0.002(3) C33 0.027(4) 0.022(3) 0.029(4) 0.002(3) -0.007(3) -0.007(3) C34 0.026(4) 0.027(3) 0.019(3) -0.005(3) 0.004(3) -0.004(3) C35 0.045(4) 0.027(3) 0.017(3) -0.003(3) 0.000(3) -0.007(3) C36 0.090(6) 0.033(4) 0.027(4) -0.011(3) 0.016(4) -0.013(4) C37 0.054(5) 0.043(4) 0.032(4) -0.005(3) -0.009(4) -0.015(3) C38 0.035(4) 0.058(4) 0.026(4) 0.001(3) 0.006(3) -0.008(3) C39 0.060(5) 0.022(3) 0.023(4) 0.003(3) 0.004(3) -0.009(3) C40 0.254(11) 0.053(5) 0.028(4) 0.018(4) -0.059(6) -0.074(6) C41 0.091(7) 0.079(6) 0.062(6) 0.032(5) 0.011(5) -0.039(5) C42 0.107(6) 0.025(4) 0.034(4) 0.011(3) -0.005(4) -0.014(4) C43 0.021(4) 0.034(4) 0.017(3) -0.002(3) 0.001(3) -0.004(3) C44 0.024(4) 0.026(3) 0.025(3) -0.004(3) -0.007(3) -0.009(3) C45 0.029(4) 0.025(3) 0.027(4) -0.003(3) -0.008(3) -0.006(3) C46 0.018(3) 0.026(3) 0.031(4) 0.001(3) -0.006(3) 0.008(3) C47 0.017(3) 0.043(4) 0.014(3) -0.006(3) 0.000(3) -0.009(3) C48 0.024(4) 0.029(3) 0.018(3) 0.001(3) 0.000(3) -0.010(3) C49 0.023(4) 0.026(3) 0.039(4) -0.005(3) -0.010(3) 0.002(3) C50 0.093(11) 0.044(7) 0.063(9) 0.011(7) -0.017(8) -0.014(7) C50' 0.041(15) 0.028(12) 0.08(2) 0.007(14) -0.002(15) -0.005(11) C51 0.065(10) 0.024(5) 0.058(8) -0.015(6) -0.022(8) 0.014(6) C51' 0.069(19) 0.031(12) 0.038(14) -0.020(10) 0.017(13) 0.018(11) C52 0.048(8) 0.025(6) 0.100(13) -0.005(7) -0.025(8) 0.000(6) C52' 0.027(15) 0.021(10) 0.053(15) -0.009(10) 0.002(12) 0.009(10) C53 0.015(4) 0.043(4) 0.030(4) 0.000(3) 0.005(3) -0.007(3) C54 0.028(4) 0.051(4) 0.059(5) -0.012(4) -0.003(4) -0.014(3) C55 0.022(4) 0.053(4) 0.058(5) 0.008(4) -0.009(3) -0.011(3) C56 0.031(4) 0.044(4) 0.050(4) 0.006(4) -0.005(3) -0.019(3) C57 0.012(3) 0.021(3) 0.017(3) -0.001(3) -0.001(3) 0.001(3) C58 0.017(3) 0.028(3) 0.023(3) 0.000(3) -0.001(3) -0.007(3) C59 0.012(3) 0.038(4) 0.018(3) -0.008(3) 0.002(3) -0.001(3) C60 0.028(4) 0.043(4) 0.015(3) 0.006(3) 0.000(3) -0.011(3) C61 0.016(3) 0.028(3) 0.029(4) 0.001(3) 0.000(3) -0.006(3) C62 0.019(3) 0.029(3) 0.018(3) -0.001(3) -0.005(3) -0.009(3) C63 0.031(4) 0.044(4) 0.019(3) 0.000(3) 0.000(3) -0.016(3) C64 0.073(6) 0.065(5) 0.039(5) -0.025(4) -0.013(4) -0.013(4) C65 0.051(5) 0.073(5) 0.024(4) -0.005(4) -0.007(3) -0.026(4) C66 0.082(6) 0.097(6) 0.019(4) 0.006(4) -0.010(4) -0.053(5) C67 0.043(4) 0.041(4) 0.025(4) 0.001(3) 0.009(3) -0.022(3) C68 0.075(6) 0.069(5) 0.122(7) -0.042(5) 0.054(5) -0.056(5) C69 0.100(7) 0.055(5) 0.061(6) -0.011(4) 0.009(5) -0.050(5) C70 0.131(8) 0.049(5) 0.091(7) 0.022(5) -0.040(6) -0.035(5) C71 0.021(4) 0.011(3) 0.016(3) 0.002(3) 0.000(3) -0.004(3) C72 0.018(3) 0.015(3) 0.024(3) 0.003(3) 0.004(3) -0.006(3) C73 0.019(4) 0.012(3) 0.027(4) -0.003(3) 0.006(3) -0.002(3) C74 0.030(4) 0.028(3) 0.017(3) 0.006(3) 0.002(3) -0.007(3) C75 0.015(3) 0.016(3) 0.033(4) 0.005(3) 0.000(3) -0.002(3) C76 0.022(4) 0.018(3) 0.021(3) 0.002(3) -0.006(3) -0.004(3) C77 0.028(4) 0.027(3) 0.015(3) -0.001(3) 0.004(3) -0.002(3) C78 0.038(4) 0.047(4) 0.019(4) -0.003(3) -0.007(3) -0.011(3) C79 0.032(4) 0.038(4) 0.030(4) 0.005(3) 0.002(3) 0.002(3) C80 0.037(4) 0.047(4) 0.017(3) 0.002(3) -0.007(3) -0.013(3) C81 0.024(4) 0.032(3) 0.029(4) 0.009(3) -0.003(3) -0.008(3) C82 0.031(4) 0.054(4) 0.078(5) 0.029(4) -0.005(4) -0.019(3) C83 0.027(4) 0.073(5) 0.067(5) 0.000(4) 0.011(4) -0.014(4) C84 0.021(4) 0.083(5) 0.064(5) 0.028(4) -0.007(4) -0.022(4) C85 0.073(5) 0.023(4) 0.055(5) -0.005(4) -0.016(4) -0.006(4) C86 0.129(8) 0.037(5) 0.054(6) -0.018(4) 0.004(6) 0.018(5) C87 0.080(8) 0.087(8) 0.37(2) -0.103(10) 0.110(10) -0.033(7) C88 0.047(5) 0.073(5) 0.029(4) 0.006(4) 0.000(4) 0.024(4) C89 0.049(5) 0.023(3) 0.035(4) 0.001(3) -0.008(4) -0.004(3) C90 0.058(5) 0.032(4) 0.030(4) 0.001(3) -0.005(4) -0.014(3) C91 0.057(5) 0.036(4) 0.038(4) 0.002(3) 0.001(4) -0.026(4) C92 0.047(4) 0.034(4) 0.030(4) -0.003(3) -0.009(3) -0.020(3) C93 0.034(4) 0.064(5) 0.056(5) -0.018(4) -0.014(4) -0.014(4) C94 0.037(5) 0.086(6) 0.069(6) 0.007(5) -0.006(4) -0.029(4) C95 0.037(4) 0.061(4) 0.038(4) 0.000(4) 0.005(4) -0.016(4) C96 0.052(5) 0.050(4) 0.025(4) -0.012(3) 0.006(4) -0.016(4) C97 0.031(4) 0.034(3) 0.019(3) -0.001(3) 0.001(3) -0.008(3) C98 0.036(4) 0.049(4) 0.039(4) -0.004(3) -0.015(4) -0.012(3) C99 0.057(5) 0.047(4) 0.051(5) 0.014(4) -0.025(4) -0.014(4) C100 0.036(4) 0.035(4) 0.035(4) 0.011(3) -0.006(3) -0.016(3) C101 0.022(4) 0.028(3) 0.027(4) 0.000(3) 0.008(3) -0.002(3) C102 0.042(4) 0.041(4) 0.026(4) -0.004(3) 0.014(3) -0.014(3) C103 0.039(4) 0.040(4) 0.022(4) 0.000(3) 0.002(3) -0.006(3) C104 0.034(4) 0.035(4) 0.034(4) 0.007(3) -0.013(3) -0.009(3) C105 0.025(4) 0.021(3) 0.040(4) 0.000(3) 0.004(3) -0.012(3) C106 0.032(4) 0.028(4) 0.071(5) -0.008(4) -0.010(4) -0.008(3) C107 0.023(4) 0.038(4) 0.072(5) 0.001(4) -0.004(4) -0.009(3) C108 0.029(4) 0.024(3) 0.040(4) 0.006(3) -0.013(3) -0.002(3) C109 0.067(6) 0.101(6) 0.082(7) -0.003(5) -0.026(5) -0.052(5) C110 0.067(6) 0.058(5) 0.080(7) 0.012(5) 0.020(5) -0.021(4) C111 0.143(9) 0.069(6) 0.047(6) 0.025(5) -0.029(6) -0.070(6) C112 0.073(6) 0.038(4) 0.117(8) 0.021(5) -0.051(6) -0.017(4) C113 0.074(6) 0.045(5) 0.087(7) -0.014(5) 0.014(5) -0.019(5) C114 0.126(8) 0.053(5) 0.046(5) 0.005(4) -0.026(6) -0.028(5) C115 0.066(6) 0.061(5) 0.105(8) 0.001(5) -0.020(6) -0.001(5) C116 0.046(5) 0.061(5) 0.075(6) -0.014(5) -0.004(5) 0.010(5) C117 0.165(12) 0.080(8) 0.122(10) 0.030(8) 0.040(9) 0.024(8) C118 0.188(12) 0.074(7) 0.221(14) -0.008(8) -0.133(11) -0.048(8) C119 0.249(13) 0.107(8) 0.161(11) 0.069(8) -0.147(10) -0.122(9) C120 0.100(8) 0.072(6) 0.051(6) 0.001(5) 0.009(5) -0.006(5) C121 0.236(16) 0.218(14) 0.233(16) 0.158(13) -0.107(13) -0.146(13) C122 0.118(10) 0.205(14) 0.100(9) 0.062(9) -0.017(7) -0.060(9) C123 0.275(18) 0.095(9) 0.140(12) -0.037(9) -0.028(13) -0.025(11) C124 0.128(11) 0.197(13) 0.33(2) 0.167(15) -0.072(13) -0.099(10) C125 0.033(6) 0.088(7) 0.214(15) -0.034(8) -0.014(8) 0.004(5) C126 0.064(9) 0.212(13) 0.229(16) -0.158(12) -0.017(9) 0.057(8) C127 0.064(7) 0.135(8) 0.086(7) -0.073(6) -0.002(6) 0.021(6) C128 0.071(8) 0.157(10) 0.092(9) -0.040(7) -0.005(7) 0.012(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 La1 O1 2.273(4) . ? La1 O2 2.285(3) . ? La1 O5 2.465(3) . ? La1 O6 2.478(3) . ? La1 O8 2.563(3) . ? La1 O9 2.596(4) . ? La1 O7 2.674(4) . ? La1 La2 4.1327(4) . ? La2 O3 2.272(3) . ? La2 O4 2.302(3) . ? La2 O6 2.489(3) . ? La2 O5 2.499(3) . ? La2 O10 2.570(3) . ? La2 O12 2.636(3) . ? La2 O11 2.649(3) . ? O1 C1 1.323(6) . ? O2 C15 1.327(5) . ? O3 C29 1.325(6) . ? O4 C43 1.339(5) . ? O5 C57 1.366(5) . ? O6 C71 1.370(5) . ? O7 C88 1.407(7) . ? O7 C85 1.440(6) . ? O8 C92 1.441(6) . ? O8 C89 1.451(5) . ? O9 C96 1.422(6) . ? O9 C93 1.437(6) . ? O10 C97 1.449(5) . ? O10 C100 1.449(5) . ? O11 C101 1.457(6) . ? O11 C104 1.460(5) . ? O12 C108 1.441(5) . ? O12 C105 1.462(5) . ? O13 C112 1.396(7) . ? O13 C109 1.439(7) . ? O14 C116 1.408(8) . ? O14 C113 1.462(8) . ? O15 C117 1.389(11) . ? O15 C120 1.405(8) . ? O16 C124 1.338(10) . ? O16 C121 1.356(10) . ? O17 C125 1.411(10) . ? O17 C128 1.506(11) . ? C1 C2 1.409(7) . ? C1 C6 1.414(7) . ? C2 C3 1.394(7) . ? C3 C4 1.402(7) . ? C3 C7 1.525(8) . ? C4 C5 1.387(7) . ? C5 C6 1.388(7) . ? C5 C11 1.531(7) . ? C7 C9 1.498(8) . ? C7 C10 1.499(8) . ? C7 C8 1.530(8) . ? C11 C12 1.517(8) . ? C11 C14 1.532(7) . ? C11 C13 1.547(7) . ? C15 C16 1.415(7) . ? C15 C20 1.421(6) . ? C16 C17 1.392(7) . ? C17 C18 1.415(7) . ? C17 C21 1.539(7) . ? C18 C19 1.404(7) . ? C19 C20 1.389(6) . ? C19 C25 1.509(7) . ? C21 C23 1.513(7) . ? C21 C22 1.528(7) . ? C21 C24 1.541(7) . ? C25 C26' 1.408(16) . ? C25 C27 1.520(16) . ? C25 C27' 1.533(14) . ? C25 C28 1.537(14) . ? C25 C26 1.567(18) . ? C25 C28' 1.580(15) . ? C29 C30 1.400(7) . ? C29 C34 1.408(6) . ? C30 C31 1.406(7) . ? C31 C32 1.413(6) . ? C31 C35 1.524(7) . ? C32 C33 1.393(7) . ? C33 C34 1.410(7) . ? C33 C39 1.540(7) . ? C35 C37 1.533(6) . ? C35 C38 1.538(7) . ? C35 C36 1.542(7) . ? C39 C40 1.482(7) . ? C39 C42 1.537(8) . ? C39 C41 1.571(8) . ? C43 C44 1.395(6) . ? C43 C48 1.409(6) . ? C44 C45 1.394(6) . ? C45 C46 1.391(6) . ? C45 C49 1.536(7) . ? C46 C47 1.383(6) . ? C47 C48 1.395(6) . ? C47 C53 1.539(7) . ? C49 C50' 1.484(19) . ? C49 C51 1.495(10) . ? C49 C52 1.498(10) . ? C49 C52' 1.506(18) . ? C49 C50 1.590(12) . ? C49 C51' 1.60(2) . ? C53 C54 1.530(7) . ? C53 C55 1.538(7) . ? C53 C56 1.544(6) . ? C57 C58 1.377(7) . ? C57 C62 1.395(6) . ? C58 C59 1.404(6) . ? C59 C60 1.401(7) . ? C59 C63 1.534(7) . ? C60 C61 1.385(7) . ? C61 C62 1.391(6) . ? C61 C67 1.544(7) . ? C63 C66 1.529(6) . ? C63 C65 1.533(7) . ? C63 C64 1.535(8) . ? C67 C68 1.505(8) . ? C67 C69 1.521(8) . ? C67 C70 1.535(7) . ? C71 C72 1.388(6) . ? C71 C76 1.389(6) . ? C72 C73 1.385(7) . ? C73 C74 1.400(6) . ? C73 C77 1.542(7) . ? C74 C75 1.383(6) . ? C75 C76 1.390(7) . ? C75 C81 1.540(7) . ? C77 C79 1.523(7) . ? C77 C78 1.531(7) . ? C77 C80 1.532(6) . ? C81 C84 1.521(7) . ? C81 C82 1.532(6) . ? C81 C83 1.537(8) . ? C85 C86 1.515(9) . ? C86 C87 1.408(10) . ? C87 C88 1.458(11) . ? C89 C90 1.510(7) . ? C90 C91 1.515(7) . ? C91 C92 1.520(6) . ? C93 C94 1.502(8) . ? C94 C95 1.493(8) . ? C95 C96 1.513(7) . ? C97 C98 1.511(6) . ? C98 C99 1.526(7) . ? C99 C100 1.502(7) . ? C101 C102 1.518(7) . ? C102 C103 1.517(7) . ? C103 C104 1.506(7) . ? C105 C106 1.522(6) . ? C106 C107 1.507(7) . ? C107 C108 1.498(7) . ? C109 C110 1.503(9) . ? C110 C111 1.509(8) . ? C111 C112 1.508(10) . ? C113 C114 1.470(9) . ? C114 C115 1.541(9) . ? C115 C116 1.449(8) . ? C117 C118 1.407(12) . ? C118 C119 1.463(10) . ? C119 C120 1.423(9) . ? C121 C122 1.432(12) . ? C122 C123 1.450(12) . ? C123 C124 1.525(15) . ? C125 C126 1.286(12) . ? C126 C127 1.478(11) . ? C127 C128 1.398(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 O1 La1 O2 156.75(12) . . ? O1 La1 O5 88.60(11) . . ? O2 La1 O5 112.43(11) . . ? O1 La1 O6 107.35(11) . . ? O2 La1 O6 90.53(11) . . ? O5 La1 O6 67.40(10) . . ? O1 La1 O8 80.43(11) . . ? O2 La1 O8 89.63(11) . . ? O5 La1 O8 137.40(11) . . ? O6 La1 O8 76.87(11) . . ? O1 La1 O9 95.42(12) . . ? O2 La1 O9 80.27(12) . . ? O5 La1 O9 77.74(10) . . ? O6 La1 O9 137.21(10) . . ? O8 La1 O9 143.88(11) . . ? O1 La1 O7 77.25(12) . . ? O2 La1 O7 79.62(12) . . ? O5 La1 O7 146.40(12) . . ? O6 La1 O7 145.87(11) . . ? O8 La1 O7 70.53(12) . . ? O9 La1 O7 73.54(12) . . ? O1 La1 La2 96.39(8) . . ? O2 La1 La2 106.60(9) . . ? O5 La1 La2 33.89(8) . . ? O6 La1 La2 33.78(6) . . ? O8 La1 La2 106.41(8) . . ? O9 La1 La2 109.72(7) . . ? O7 La1 La2 173.24(9) . . ? O3 La2 O4 103.04(12) . . ? O3 La2 O6 159.69(11) . . ? O4 La2 O6 90.87(10) . . ? O3 La2 O5 113.81(11) . . ? O4 La2 O5 126.94(11) . . ? O6 La2 O5 66.71(10) . . ? O3 La2 O10 79.55(11) . . ? O4 La2 O10 74.17(11) . . ? O6 La2 O10 118.97(10) . . ? O5 La2 O10 76.48(10) . . ? O3 La2 O12 75.96(10) . . ? O4 La2 O12 148.02(12) . . ? O6 La2 O12 84.39(9) . . ? O5 La2 O12 79.81(10) . . ? O10 La2 O12 135.07(10) . . ? O3 La2 O11 84.55(11) . . ? O4 La2 O11 75.19(11) . . ? O6 La2 O11 84.81(10) . . ? O5 La2 O11 142.22(10) . . ? O10 La2 O11 141.05(10) . . ? O12 La2 O11 72.89(10) . . ? O3 La2 La1 145.08(9) . . ? O4 La2 La1 109.08(8) . . ? O6 La2 La1 33.61(8) . . ? O5 La2 La1 33.37(6) . . ? O10 La2 La1 96.14(8) . . ? O12 La2 La1 83.71(7) . . ? O11 La2 La1 116.35(7) . . ? C1 O1 La1 174.3(4) . . ? C15 O2 La1 166.5(3) . . ? C29 O3 La2 159.2(4) . . ? C43 O4 La2 138.2(3) . . ? C57 O5 La1 129.1(3) . . ? C57 O5 La2 116.2(3) . . ? La1 O5 La2 112.74(12) . . ? C71 O6 La1 127.9(3) . . ? C71 O6 La2 119.5(3) . . ? La1 O6 La2 112.61(12) . . ? C88 O7 C85 108.3(5) . . ? C88 O7 La1 129.1(4) . . ? C85 O7 La1 122.6(3) . . ? C92 O8 C89 109.8(4) . . ? C92 O8 La1 118.9(3) . . ? C89 O8 La1 129.9(3) . . ? C96 O9 C93 108.9(4) . . ? C96 O9 La1 128.3(3) . . ? C93 O9 La1 120.6(3) . . ? C97 O10 C100 108.6(3) . . ? C97 O10 La2 123.2(3) . . ? C100 O10 La2 127.6(3) . . ? C101 O11 C104 108.4(4) . . ? C101 O11 La2 122.4(3) . . ? C104 O11 La2 129.0(3) . . ? C108 O12 C105 108.0(3) . . ? C108 O12 La2 125.5(3) . . ? C105 O12 La2 125.5(3) . . ? C112 O13 C109 103.6(5) . . ? C116 O14 C113 105.0(6) . . ? C117 O15 C120 106.7(8) . . ? C124 O16 C121 102.9(9) . . ? C125 O17 C128 104.3(8) . . ? O1 C1 C2 121.2(5) . . ? O1 C1 C6 121.4(6) . . ? C2 C1 C6 117.3(5) . . ? C3 C2 C1 122.7(6) . . ? C2 C3 C4 117.0(6) . . ? C2 C3 C7 122.4(6) . . ? C4 C3 C7 120.4(5) . . ? C5 C4 C3 122.7(5) . . ? C4 C5 C6 118.8(5) . . ? C4 C5 C11 119.2(5) . . ? C6 C5 C11 121.9(6) . . ? C5 C6 C1 121.4(5) . . ? C9 C7 C10 107.2(6) . . ? C9 C7 C3 113.5(5) . . ? C10 C7 C3 111.4(6) . . ? C9 C7 C8 107.9(6) . . ? C10 C7 C8 106.0(6) . . ? C3 C7 C8 110.5(5) . . ? C12 C11 C5 112.4(5) . . ? C12 C11 C14 108.0(5) . . ? C5 C11 C14 112.5(5) . . ? C12 C11 C13 109.2(5) . . ? C5 C11 C13 107.6(4) . . ? C14 C11 C13 106.9(5) . . ? O2 C15 C16 120.9(5) . . ? O2 C15 C20 121.3(5) . . ? C16 C15 C20 117.8(5) . . ? C17 C16 C15 121.3(5) . . ? C16 C17 C18 118.6(5) . . ? C16 C17 C21 122.2(5) . . ? C18 C17 C21 119.2(5) . . ? C19 C18 C17 122.1(5) . . ? C20 C19 C18 117.7(5) . . ? C20 C19 C25 122.0(5) . . ? C18 C19 C25 120.3(5) . . ? C19 C20 C15 122.5(5) . . ? C23 C21 C22 108.1(6) . . ? C23 C21 C17 109.0(4) . . ? C22 C21 C17 112.9(4) . . ? C23 C21 C24 108.9(4) . . ? C22 C21 C24 109.3(5) . . ? C17 C21 C24 108.6(5) . . ? C26' C25 C19 112.4(7) . . ? C26' C25 C27 131.7(9) . . ? C19 C25 C27 115.6(8) . . ? C26' C25 C27' 117.1(12) . . ? C19 C25 C27' 107.4(7) . . ? C27 C25 C27' 41.7(7) . . ? C26' C25 C28 61.7(10) . . ? C19 C25 C28 110.2(7) . . ? C27 C25 C28 105.0(10) . . ? C27' C25 C28 138.9(8) . . ? C26' C25 C26 47.5(9) . . ? C19 C25 C26 108.8(7) . . ? C27 C25 C26 109.4(10) . . ? C27' C25 C26 74.8(9) . . ? C28 C25 C26 107.5(10) . . ? C26' C25 C28' 108.5(11) . . ? C19 C25 C28' 107.7(7) . . ? C27 C25 C28' 61.4(8) . . ? C27' C25 C28' 103.0(9) . . ? C28 C25 C28' 49.7(7) . . ? C26 C25 C28' 142.3(8) . . ? O3 C29 C30 121.5(4) . . ? O3 C29 C34 120.6(5) . . ? C30 C29 C34 117.9(5) . . ? C29 C30 C31 123.2(5) . . ? C30 C31 C32 116.5(5) . . ? C30 C31 C35 120.6(5) . . ? C32 C31 C35 122.9(5) . . ? C33 C32 C31 122.7(5) . . ? C32 C33 C34 118.5(5) . . ? C32 C33 C39 122.5(5) . . ? C34 C33 C39 119.0(5) . . ? C29 C34 C33 121.2(5) . . ? C31 C35 C37 109.4(5) . . ? C31 C35 C38 108.5(4) . . ? C37 C35 C38 110.1(4) . . ? C31 C35 C36 112.4(4) . . ? C37 C35 C36 107.9(5) . . ? C38 C35 C36 108.6(5) . . ? C40 C39 C42 111.1(5) . . ? C40 C39 C33 111.8(5) . . ? C42 C39 C33 111.6(5) . . ? C40 C39 C41 111.4(6) . . ? C42 C39 C41 103.6(5) . . ? C33 C39 C41 107.1(4) . . ? O4 C43 C44 122.0(5) . . ? O4 C43 C48 120.2(5) . . ? C44 C43 C48 117.8(5) . . ? C45 C44 C43 122.2(5) . . ? C46 C45 C44 118.1(5) . . ? C46 C45 C49 121.5(5) . . ? C44 C45 C49 120.3(5) . . ? C47 C46 C45 121.7(5) . . ? C46 C47 C48 119.2(5) . . ? C46 C47 C53 122.6(5) . . ? C48 C47 C53 118.2(5) . . ? C47 C48 C43 121.0(5) . . ? C50' C49 C51 53.9(10) . . ? C50' C49 C52 131.7(8) . . ? C51 C49 C52 113.1(8) . . ? C50' C49 C52' 105.8(12) . . ? C51 C49 C52' 141.3(8) . . ? C52 C49 C52' 52.1(8) . . ? C50' C49 C45 113.9(8) . . ? C51 C49 C45 110.0(5) . . ? C52 C49 C45 113.9(5) . . ? C52' C49 C45 108.5(8) . . ? C50' C49 C50 54.2(10) . . ? C51 C49 C50 107.3(8) . . ? C52 C49 C50 105.6(7) . . ? C52' C49 C50 56.9(8) . . ? C45 C49 C50 106.4(6) . . ? C50' C49 C51' 110.7(13) . . ? C51 C49 C51' 60.8(9) . . ? C52 C49 C51' 59.5(8) . . ? C52' C49 C51' 110.8(11) . . ? C45 C49 C51' 107.2(7) . . ? C50 C49 C51' 146.4(8) . . ? C54 C53 C55 108.8(5) . . ? C54 C53 C47 109.2(4) . . ? C55 C53 C47 112.5(4) . . ? C54 C53 C56 108.8(5) . . ? C55 C53 C56 107.2(4) . . ? C47 C53 C56 110.2(4) . . ? O5 C57 C58 121.3(4) . . ? O5 C57 C62 118.8(5) . . ? C58 C57 C62 119.9(5) . . ? C57 C58 C59 121.1(5) . . ? C60 C59 C58 117.3(5) . . ? C60 C59 C63 121.7(5) . . ? C58 C59 C63 121.0(5) . . ? C61 C60 C59 122.8(5) . . ? C60 C61 C62 118.1(5) . . ? C60 C61 C67 119.9(5) . . ? C62 C61 C67 122.0(5) . . ? C61 C62 C57 120.9(5) . . ? C66 C63 C65 107.8(4) . . ? C66 C63 C59 112.4(5) . . ? C65 C63 C59 110.5(5) . . ? C66 C63 C64 108.6(5) . . ? C65 C63 C64 107.5(5) . . ? C59 C63 C64 109.8(4) . . ? C68 C67 C69 109.0(5) . . ? C68 C67 C70 107.6(5) . . ? C69 C67 C70 106.2(5) . . ? C68 C67 C61 110.5(5) . . ? C69 C67 C61 113.0(4) . . ? C70 C67 C61 110.3(5) . . ? O6 C71 C72 120.9(4) . . ? O6 C71 C76 119.1(4) . . ? C72 C71 C76 120.0(5) . . ? C73 C72 C71 121.0(5) . . ? C72 C73 C74 117.9(5) . . ? C72 C73 C77 119.6(5) . . ? C74 C73 C77 122.5(5) . . ? C75 C74 C73 122.0(5) . . ? C74 C75 C76 118.9(5) . . ? C74 C75 C81 119.2(5) . . ? C76 C75 C81 121.9(5) . . ? C71 C76 C75 120.2(5) . . ? C79 C77 C78 108.7(4) . . ? C79 C77 C80 109.6(4) . . ? C78 C77 C80 107.1(4) . . ? C79 C77 C73 110.0(5) . . ? C78 C77 C73 112.4(4) . . ? C80 C77 C73 109.0(4) . . ? C84 C81 C82 108.3(5) . . ? C84 C81 C83 107.8(5) . . ? C82 C81 C83 109.1(5) . . ? C84 C81 C75 112.1(4) . . ? C82 C81 C75 110.0(4) . . ? C83 C81 C75 109.4(5) . . ? O7 C85 C86 106.3(6) . . ? C87 C86 C85 103.4(7) . . ? C86 C87 C88 112.0(8) . . ? O7 C88 C87 104.4(7) . . ? O8 C89 C90 105.1(4) . . ? C89 C90 C91 101.9(5) . . ? C90 C91 C92 103.2(4) . . ? O8 C92 C91 105.8(4) . . ? O9 C93 C94 106.6(5) . . ? C95 C94 C93 104.1(5) . . ? C94 C95 C96 101.6(5) . . ? O9 C96 C95 106.0(5) . . ? O10 C97 C98 104.1(4) . . ? C97 C98 C99 102.9(4) . . ? C100 C99 C98 104.3(4) . . ? O10 C100 C99 107.5(4) . . ? O11 C101 C102 106.7(4) . . ? C103 C102 C101 101.6(5) . . ? C104 C103 C102 102.9(4) . . ? O11 C104 C103 105.2(4) . . ? O12 C105 C106 106.4(4) . . ? C107 C106 C105 104.0(4) . . ? C108 C107 C106 103.2(5) . . ? O12 C108 C107 104.3(4) . . ? O13 C109 C110 107.0(6) . . ? C109 C110 C111 105.7(6) . . ? C112 C111 C110 100.8(6) . . ? O13 C112 C111 107.5(6) . . ? O14 C113 C114 109.5(6) . . ? C113 C114 C115 99.2(6) . . ? C116 C115 C114 103.7(7) . . ? O14 C116 C115 110.3(6) . . ? O15 C117 C118 108.4(8) . . ? C117 C118 C119 102.4(8) . . ? C120 C119 C118 109.5(7) . . ? O15 C120 C119 103.7(7) . . ? O16 C121 C122 115.5(9) . . ? C121 C122 C123 101.7(9) . . ? C122 C123 C124 100.1(10) . . ? O16 C124 C123 109.0(11) . . ? C126 C125 O17 110.8(9) . . ? C125 C126 C127 110.3(10) . . ? C128 C127 C126 103.4(8) . . ? C127 C128 O17 105.5(8) . . ? _diffrn_measured_fraction_theta_max 0.874 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.888 _refine_diff_density_max 1.068 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.119 #====END data_RH4ND.CIF _database_code_depnum_ccdc_archive 'CCDC 236328' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [Nonakis(3,5-di-tert-phenolato)tetrakis(tetrahydrofuran) trineodymium(III)].4tetrahydrofuran ; _chemical_name_common ; (Nonakis(3,5-di-tert-phenolato)tetrakis(tetrahydrofuran) trineodymium(iii)).4tetrahydrofuran ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C158 H253 Nd3 O17' _chemical_formula_weight 2857.32 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.207(3) _cell_length_b 21.974(4) _cell_length_c 24.703(5) _cell_angle_alpha 75.44(3) _cell_angle_beta 89.35(3) _cell_angle_gamma 88.29(3) _cell_volume 7986(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 116050 _cell_measurement_theta_min 1.11 _cell_measurement_theta_max 28.28 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3034 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116050 _diffrn_reflns_av_R_equivalents 0.0692 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.28 _reflns_number_total 36783 _reflns_number_gt 23950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1323P)^2^+0.4423P] 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 36783 _refine_ls_number_parameters 1604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.2149 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.021 _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 0.808120(18) 0.805770(13) 0.812280(12) 0.021 Uani 1 1 d . . . Nd2 Nd 0.934510(18) 0.781620(13) 0.688030(13) 0.023 Uani 1 1 d . . . Nd3 Nd 0.746160(17) 0.677730(13) 0.747600(12) 0.020 Uani 1 1 d . . . O1 O 0.8409(3) 0.78090(18) 0.90060(17) 0.033 Uani 1 1 d . . . O2 O 0.7488(3) 0.89806(17) 0.80888(17) 0.031 Uani 1 1 d . . . O3 O 0.9420(2) 0.83588(17) 0.76071(17) 0.030 Uani 1 1 d . . . O4 O 0.7814(2) 0.79673(16) 0.71185(15) 0.022 Uani 1 1 d . . . O5 O 0.8816(2) 0.71106(16) 0.78228(15) 0.021 Uani 1 1 d . . . O6 O 0.6893(2) 0.73466(16) 0.81324(16) 0.024 Uani 1 1 d . . . O7 O 1.0009(2) 0.78804(18) 0.60842(17) 0.031 Uani 1 1 d . . . O8 O 0.8531(2) 0.69328(17) 0.67339(16) 0.027 Uani 1 1 d . . . O9 O 0.9135(2) 0.89708(18) 0.63616(17) 0.031 Uani 1 1 d . . . O10 O 1.0874(2) 0.74697(18) 0.72325(17) 0.031 Uani 1 1 d . . . O11 O 0.7062(2) 0.58952(17) 0.73242(17) 0.031 Uani 1 1 d . . . O12 O 0.6000(2) 0.71513(18) 0.70299(18) 0.031 Uani 1 1 d . . . O13 O 0.7699(2) 0.59989(16) 0.84175(16) 0.026 Uani 1 1 d . . . O14 O 1.4025(13) 1.1444(7) 0.8370(6) 0.248 Uani 1 1 d . . . O15 O 0.7210(10) 1.3354(7) 0.9354(7) 0.238 Uani 1 1 d . . . O16 O 0.4834(12) 0.1832(10) 0.6553(9) 0.286 Uani 1 1 d . . . O17 O 0.7699(6) 0.6191(5) 1.2744(4) 0.147 Uani 1 1 d . . . C1 C 0.8297(4) 0.7632(3) 0.9565(2) 0.029 Uani 1 1 d . . . C2 C 0.7596(4) 0.7267(3) 0.9794(2) 0.030 Uani 1 1 d . . . H2 H 0.7188 0.7148 0.9553 0.036 Uiso 1 1 calc R . . C3 C 0.7478(4) 0.7072(3) 1.0366(3) 0.031 Uani 1 1 d . . . C4 C 0.8092(4) 0.7247(3) 1.0717(3) 0.037 Uani 1 1 d . . . H4 H 0.8025 0.7108 1.1111 0.044 Uiso 1 1 calc R . . C5 C 0.8803(4) 0.7624(3) 1.0494(3) 0.035 Uani 1 1 d . . . C6 C 0.8898(4) 0.7804(3) 0.9920(3) 0.033 Uani 1 1 d . . . H6 H 0.9384 0.8051 0.9763 0.040 Uiso 1 1 calc R . . C7 C 0.6706(4) 0.6682(3) 1.0635(3) 0.045 Uani 1 1 d . . . C8 C 0.6136(5) 0.6489(4) 1.0201(3) 0.068 Uani 1 1 d . . . H8A H 0.5647 0.6239 1.0390 0.102 Uiso 1 1 calc R . . H8B H 0.6494 0.6238 1.0000 0.102 Uiso 1 1 calc R . . H8C H 0.5902 0.6867 0.9935 0.102 Uiso 1 1 calc R . . C9 C 0.7046(6) 0.6074(4) 1.1056(4) 0.071 Uani 1 1 d . . . H9A H 0.6545 0.5824 1.1227 0.106 Uiso 1 1 calc R . . H9B H 0.7389 0.6186 1.1349 0.106 Uiso 1 1 calc R . . H9C H 0.7419 0.5827 1.0860 0.106 Uiso 1 1 calc R . . C10 C 0.6156(5) 0.7076(5) 1.0950(4) 0.080 Uani 1 1 d . . . H10A H 0.5651 0.6836 1.1127 0.120 Uiso 1 1 calc R . . H10B H 0.5947 0.7464 1.0687 0.120 Uiso 1 1 calc R . . H10C H 0.6518 0.7181 1.1237 0.120 Uiso 1 1 calc R . . C11 C 0.9449(5) 0.7817(3) 1.0892(3) 0.043 Uani 1 1 d . . . C12 C 0.9968(6) 0.7243(4) 1.1207(4) 0.070 Uani 1 1 d . . . H12A H 0.9563 0.6926 1.1409 0.104 Uiso 1 1 calc R . . H12B H 1.0360 0.7361 1.1474 0.104 Uiso 1 1 calc R . . H12C H 1.0319 0.7071 1.0943 0.104 Uiso 1 1 calc R . . C13 C 0.8905(6) 0.8120(4) 1.1302(3) 0.062 Uani 1 1 d . . . H13A H 0.8488 0.7815 1.1511 0.093 Uiso 1 1 calc R . . H13B H 0.8581 0.8494 1.1089 0.093 Uiso 1 1 calc R . . H13C H 0.9304 0.8240 1.1564 0.093 Uiso 1 1 calc R . . C14 C 1.0080(6) 0.8309(4) 1.0584(3) 0.068 Uani 1 1 d . . . H14A H 1.0476 0.8419 1.0853 0.102 Uiso 1 1 calc R . . H14B H 0.9746 0.8686 1.0385 0.102 Uiso 1 1 calc R . . H14C H 1.0426 0.8141 1.0314 0.102 Uiso 1 1 calc R . . C15 C 0.7442(4) 0.9474(3) 0.8323(3) 0.029 Uani 1 1 d . . . C16 C 0.7171(4) 0.9392(3) 0.8879(3) 0.032 Uani 1 1 d . . . H16 H 0.7016 0.8986 0.9091 0.039 Uiso 1 1 calc R . . C17 C 0.7124(4) 0.9890(3) 0.9122(3) 0.035 Uani 1 1 d . . . C18 C 0.7358(4) 1.0491(3) 0.8801(3) 0.041 Uani 1 1 d . . . H18 H 0.7323 1.0837 0.8967 0.049 Uiso 1 1 calc R . . C19 C 0.7635(4) 1.0589(3) 0.8256(3) 0.040 Uani 1 1 d . . . C20 C 0.7685(4) 1.0069(3) 0.8016(3) 0.036 Uani 1 1 d . . . H20 H 0.7885 1.0125 0.7642 0.043 Uiso 1 1 calc R . . C21 C 0.6872(5) 0.9769(4) 0.9745(3) 0.049 Uani 1 1 d . . . C22 C 0.7594(6) 0.9340(5) 1.0105(3) 0.075 Uani 1 1 d . . . H22A H 0.7435 0.9261 1.0502 0.113 Uiso 1 1 calc R . . H22B H 0.8160 0.9550 1.0041 0.113 Uiso 1 1 calc R . . H22C H 0.7642 0.8940 0.9999 0.113 Uiso 1 1 calc R . . C23 C 0.6006(5) 0.9409(5) 0.9859(4) 0.078 Uani 1 1 d . . . H23A H 0.5851 0.9335 1.0256 0.117 Uiso 1 1 calc R . . H23B H 0.6083 0.9004 0.9763 0.117 Uiso 1 1 calc R . . H23C H 0.5535 0.9657 0.9631 0.117 Uiso 1 1 calc R . . C24 C 0.6759(6) 1.0389(4) 0.9926(4) 0.077 Uani 1 1 d . . . H24A H 0.6596 1.0296 1.0323 0.116 Uiso 1 1 calc R . . H24B H 0.6296 1.0652 0.9703 0.116 Uiso 1 1 calc R . . H24C H 0.7314 1.0613 0.9868 0.116 Uiso 1 1 calc R . . C25 C 0.7920(6) 1.1230(3) 0.7903(3) 0.058 Uani 1 1 d . . . C26 C 0.7763(9) 1.1735(4) 0.8212(5) 0.108 Uani 1 1 d . . . H26A H 0.7132 1.1778 0.8282 0.162 Uiso 1 1 calc R . . H26B H 0.7979 1.2135 0.7986 0.162 Uiso 1 1 calc R . . H26C H 0.8077 1.1619 0.8569 0.162 Uiso 1 1 calc R . . C27 C 0.8922(7) 1.1204(4) 0.7808(4) 0.093 Uani 1 1 d . . . H27A H 0.9068 1.0885 0.7605 0.140 Uiso 1 1 calc R . . H27B H 0.9222 1.1095 0.8171 0.140 Uiso 1 1 calc R . . H27C H 0.9113 1.1616 0.7590 0.140 Uiso 1 1 calc R . . C28 C 0.7456(6) 1.1382(3) 0.7340(4) 0.079 Uani 1 1 d . . . H28A H 0.7590 1.1049 0.7150 0.119 Uiso 1 1 calc R . . H28B H 0.7660 1.1784 0.7109 0.119 Uiso 1 1 calc R . . H28C H 0.6819 1.1412 0.7398 0.119 Uiso 1 1 calc R . . C29 C 1.0019(4) 0.8776(3) 0.7684(3) 0.033 Uani 1 1 d . . . C30 C 1.0014(3) 0.8974(3) 0.8176(3) 0.033 Uani 1 1 d . . . H30 H 0.9588 0.8815 0.8457 0.039 Uiso 1 1 calc R . . C31 C 1.0617(3) 0.9399(3) 0.8264(3) 0.031 Uani 1 1 d . . . C32 C 1.1241(4) 0.9615(3) 0.7847(3) 0.035 Uani 1 1 d . . . H32 H 1.1665 0.9900 0.7905 0.042 Uiso 1 1 calc R . . C33 C 1.1267(3) 0.9429(3) 0.7348(3) 0.033 Uani 1 1 d . . . C34 C 1.0639(3) 0.9004(3) 0.7269(3) 0.031 Uani 1 1 d . . . H34 H 1.0638 0.8871 0.6932 0.037 Uiso 1 1 calc R . . C35 C 1.0627(4) 0.9593(3) 0.8818(3) 0.044 Uani 1 1 d . . . C36 C 0.9702(4) 0.9608(3) 0.9070(3) 0.049 Uani 1 1 d . . . H36A H 0.9737 0.9732 0.9424 0.074 Uiso 1 1 calc R . . H36B H 0.9453 0.9189 0.9140 0.074 Uiso 1 1 calc R . . H36C H 0.9326 0.9911 0.8809 0.074 Uiso 1 1 calc R . . C37 C 1.0986(6) 1.0254(4) 0.8735(5) 0.089 Uani 1 1 d . . . H37A H 1.0988 1.0366 0.9095 0.133 Uiso 1 1 calc R . . H37B H 1.0612 1.0556 0.8470 0.133 Uiso 1 1 calc R . . H37C H 1.1587 1.0262 0.8587 0.133 Uiso 1 1 calc R . . C38 C 1.1191(5) 0.9093(4) 0.9236(4) 0.067 Uani 1 1 d . . . H38A H 1.1210 0.9204 0.9596 0.101 Uiso 1 1 calc R . . H38B H 1.1790 0.9079 0.9088 0.101 Uiso 1 1 calc R . . H38C H 1.0929 0.8680 0.9289 0.101 Uiso 1 1 calc R . . C39 C 1.1967(4) 0.9637(3) 0.6892(3) 0.041 Uani 1 1 d . . . C40 C 1.1544(5) 0.9837(4) 0.6316(3) 0.062 Uani 1 1 d . . . H40A H 1.2001 0.9968 0.6031 0.092 Uiso 1 1 calc R . . H40B H 1.1128 1.0190 0.6304 0.092 Uiso 1 1 calc R . . H40C H 1.1231 0.9483 0.6243 0.092 Uiso 1 1 calc R . . C41 C 1.2585(4) 0.9071(4) 0.6876(3) 0.055 Uani 1 1 d . . . H41A H 1.3033 0.9203 0.6585 0.083 Uiso 1 1 calc R . . H41B H 1.2242 0.8735 0.6792 0.083 Uiso 1 1 calc R . . H41C H 1.2872 0.8915 0.7239 0.083 Uiso 1 1 calc R . . C42 C 1.2499(5) 1.0188(4) 0.6992(4) 0.073 Uani 1 1 d . . . H42A H 1.2941 1.0310 0.6696 0.109 Uiso 1 1 calc R . . H42B H 1.2794 1.0055 0.7356 0.109 Uiso 1 1 calc R . . H42C H 1.2101 1.0547 0.6990 0.109 Uiso 1 1 calc R . . C43 C 0.7269(3) 0.8350(3) 0.6735(2) 0.025 Uani 1 1 d . . . C44 C 0.7236(3) 0.8267(3) 0.6186(2) 0.025 Uani 1 1 d . . . H44 H 0.7590 0.7944 0.6091 0.030 Uiso 1 1 calc R . . C45 C 0.6701(3) 0.8645(3) 0.5787(2) 0.029 Uani 1 1 d . . . C46 C 0.6170(4) 0.9106(3) 0.5946(3) 0.032 Uani 1 1 d . . . H46 H 0.5791 0.9365 0.5675 0.039 Uiso 1 1 calc R . . C47 C 0.6175(3) 0.9198(3) 0.6482(3) 0.029 Uani 1 1 d . . . C48 C 0.6734(3) 0.8816(3) 0.6875(2) 0.027 Uani 1 1 d . . . H48 H 0.6753 0.8874 0.7243 0.032 Uiso 1 1 calc R . . C49 C 0.6652(4) 0.8566(3) 0.5189(2) 0.037 Uani 1 1 d . . . C50 C 0.7284(5) 0.8034(5) 0.5092(3) 0.080 Uani 1 1 d . . . H50A H 0.7133 0.7634 0.5351 0.120 Uiso 1 1 calc R . . H50B H 0.7892 0.8134 0.5158 0.120 Uiso 1 1 calc R . . H50C H 0.7227 0.8000 0.4706 0.120 Uiso 1 1 calc R . . C51 C 0.5742(4) 0.8401(4) 0.5062(3) 0.048 Uani 1 1 d . . . H51A H 0.5585 0.8002 0.5320 0.072 Uiso 1 1 calc R . . H51B H 0.5721 0.8360 0.4677 0.072 Uiso 1 1 calc R . . H51C H 0.5325 0.8734 0.5107 0.072 Uiso 1 1 calc R . . C52 C 0.6893(5) 0.9200(4) 0.4780(3) 0.068 Uani 1 1 d . . . H52A H 0.7490 0.9309 0.4859 0.102 Uiso 1 1 calc R . . H52B H 0.6476 0.9531 0.4827 0.102 Uiso 1 1 calc R . . H52C H 0.6866 0.9160 0.4394 0.102 Uiso 1 1 calc R . . C53 C 0.5597(4) 0.9694(3) 0.6665(3) 0.035 Uani 1 1 d . . . C54 C 0.4991(5) 1.0043(3) 0.6205(3) 0.050 Uani 1 1 d . . . H54A H 0.5341 1.0258 0.5881 0.076 Uiso 1 1 calc R . . H54B H 0.4632 1.0354 0.6339 0.076 Uiso 1 1 calc R . . H54C H 0.4606 0.9745 0.6096 0.076 Uiso 1 1 calc R . . C55 C 0.6173(5) 1.0164(3) 0.6847(4) 0.053 Uani 1 1 d . . . H55A H 0.6540 1.0377 0.6531 0.080 Uiso 1 1 calc R . . H55B H 0.6550 0.9941 0.7157 0.080 Uiso 1 1 calc R . . H55C H 0.5798 1.0475 0.6969 0.080 Uiso 1 1 calc R . . C56 C 0.5038(5) 0.9375(3) 0.7162(3) 0.052 Uani 1 1 d . . . H56A H 0.4658 0.9072 0.7055 0.078 Uiso 1 1 calc R . . H56B H 0.4673 0.9692 0.7283 0.078 Uiso 1 1 calc R . . H56C H 0.5420 0.9154 0.7470 0.078 Uiso 1 1 calc R . . C57 C 0.9448(3) 0.6689(3) 0.8110(2) 0.025 Uani 1 1 d . . . C58 C 0.9821(3) 0.6778(3) 0.8600(2) 0.026 Uani 1 1 d . . . H58 H 0.9634 0.7127 0.8738 0.032 Uiso 1 1 calc R . . C59 C 1.0454(3) 0.6363(3) 0.8883(2) 0.028 Uani 1 1 d . . . C60 C 1.0697(4) 0.5850(3) 0.8678(3) 0.032 Uani 1 1 d . . . H60 H 1.1125 0.5558 0.8878 0.038 Uiso 1 1 calc R . . C61 C 1.0344(4) 0.5740(3) 0.8192(3) 0.029 Uani 1 1 d . . . C62 C 0.9715(3) 0.6169(2) 0.7907(3) 0.026 Uani 1 1 d . . . H62 H 0.9464 0.6111 0.7574 0.031 Uiso 1 1 calc R . . C63 C 1.0843(4) 0.6475(3) 0.9418(3) 0.033 Uani 1 1 d . . . C64 C 1.0191(5) 0.6230(3) 0.9901(3) 0.048 Uani 1 1 d . . . H64A H 1.0093 0.5783 0.9936 0.073 Uiso 1 1 calc R . . H64B H 0.9631 0.6467 0.9822 0.073 Uiso 1 1 calc R . . H64C H 1.0434 0.6284 1.0251 0.073 Uiso 1 1 calc R . . C65 C 1.1724(5) 0.6102(4) 0.9577(3) 0.063 Uani 1 1 d . . . H65A H 1.1634 0.5654 0.9610 0.094 Uiso 1 1 calc R . . H65B H 1.1929 0.6159 0.9936 0.094 Uiso 1 1 calc R . . H65C H 1.2164 0.6257 0.9287 0.094 Uiso 1 1 calc R . . C66 C 1.1000(5) 0.7168(3) 0.9369(3) 0.049 Uani 1 1 d . . . H66A H 1.1247 0.7218 0.9720 0.073 Uiso 1 1 calc R . . H66B H 1.0441 0.7407 0.9294 0.073 Uiso 1 1 calc R . . H66C H 1.1413 0.7326 0.9062 0.073 Uiso 1 1 calc R . . C67 C 1.0647(4) 0.5158(3) 0.8004(3) 0.038 Uani 1 1 d . . . C68 C 1.1631(4) 0.5186(3) 0.7867(3) 0.044 Uani 1 1 d . . . H68A H 1.1818 0.4810 0.7745 0.067 Uiso 1 1 calc R . . H68B H 1.1962 0.5203 0.8201 0.067 Uiso 1 1 calc R . . H68C H 1.1743 0.5562 0.7567 0.067 Uiso 1 1 calc R . . C69 C 1.0495(5) 0.4563(3) 0.8476(4) 0.062 Uani 1 1 d . . . H69A H 1.0685 0.4191 0.8351 0.092 Uiso 1 1 calc R . . H69B H 0.9868 0.4537 0.8572 0.092 Uiso 1 1 calc R . . H69C H 1.0835 0.4583 0.8805 0.092 Uiso 1 1 calc R . . C70 C 1.0156(4) 0.5105(3) 0.7480(3) 0.053 Uani 1 1 d . . . H70A H 1.0362 0.4726 0.7372 0.079 Uiso 1 1 calc R . . H70B H 1.0268 0.5476 0.7173 0.079 Uiso 1 1 calc R . . H70C H 0.9523 0.5081 0.7559 0.079 Uiso 1 1 calc R . . C71 C 0.6099(3) 0.7240(3) 0.8393(2) 0.025 Uani 1 1 d . . . C72 C 0.5760(3) 0.6636(2) 0.8507(2) 0.022 Uani 1 1 d . . . H72 H 0.6090 0.6308 0.8405 0.027 Uiso 1 1 calc R . . C73 C 0.4952(3) 0.6509(2) 0.8766(2) 0.024 Uani 1 1 d . . . C74 C 0.4484(3) 0.7003(3) 0.8901(2) 0.029 Uani 1 1 d . . . H74 H 0.3924 0.6925 0.9075 0.035 Uiso 1 1 calc R . . C75 C 0.4811(3) 0.7611(3) 0.8792(3) 0.029 Uani 1 1 d . . . C76 C 0.5637(3) 0.7715(3) 0.8544(2) 0.027 Uani 1 1 d . . . H76 H 0.5882 0.8120 0.8480 0.033 Uiso 1 1 calc R . . C77 C 0.4553(3) 0.5849(3) 0.8891(2) 0.026 Uani 1 1 d . . . C78 C 0.5238(4) 0.5344(3) 0.8812(3) 0.041 Uani 1 1 d . . . H78A H 0.5737 0.5332 0.9062 0.061 Uiso 1 1 calc R . . H78B H 0.5446 0.5447 0.8423 0.061 Uiso 1 1 calc R . . H78C H 0.4966 0.4931 0.8899 0.061 Uiso 1 1 calc R . . C79 C 0.3784(4) 0.5862(3) 0.8505(3) 0.041 Uani 1 1 d . . . H79A H 0.3532 0.5443 0.8584 0.061 Uiso 1 1 calc R . . H79B H 0.3987 0.5982 0.8116 0.061 Uiso 1 1 calc R . . H79C H 0.3336 0.6167 0.8566 0.061 Uiso 1 1 calc R . . C80 C 0.4239(4) 0.5656(3) 0.9513(3) 0.035 Uani 1 1 d . . . H80A H 0.4741 0.5650 0.9760 0.053 Uiso 1 1 calc R . . H80B H 0.3990 0.5236 0.9593 0.053 Uiso 1 1 calc R . . H80C H 0.3790 0.5960 0.9576 0.053 Uiso 1 1 calc R . . C81 C 0.4261(4) 0.8133(3) 0.8951(3) 0.049 Uani 1 1 d . . . C82 C 0.3391(7) 0.8202(7) 0.8597(8) 0.177 Uani 1 1 d . . . H82A H 0.3537 0.8325 0.8198 0.266 Uiso 1 1 calc R . . H82B H 0.3001 0.8525 0.8690 0.266 Uiso 1 1 calc R . . H82C H 0.3093 0.7800 0.8683 0.266 Uiso 1 1 calc R . . C83 C 0.4013(14) 0.7974(5) 0.9531(6) 0.232 Uani 1 1 d . . . H83A H 0.3755 0.7557 0.9628 0.348 Uiso 1 1 calc R . . H83B H 0.3580 0.8286 0.9599 0.348 Uiso 1 1 calc R . . H83C H 0.4534 0.7970 0.9762 0.348 Uiso 1 1 calc R . . C84 C 0.4669(6) 0.8769(3) 0.8767(4) 0.082 Uani 1 1 d . . . H84A H 0.4858 0.8843 0.8376 0.124 Uiso 1 1 calc R . . H84B H 0.5178 0.8783 0.9003 0.124 Uiso 1 1 calc R . . H84C H 0.4235 0.9096 0.8803 0.124 Uiso 1 1 calc R . . C85 C 1.0464(4) 0.7966(3) 0.5599(3) 0.033 Uani 1 1 d . . . C86 C 1.0054(4) 0.7914(3) 0.5117(3) 0.038 Uani 1 1 d . . . H86 H 0.9454 0.7802 0.5132 0.046 Uiso 1 1 calc R . . C87 C 1.0501(4) 0.8021(3) 0.4617(3) 0.046 Uani 1 1 d . . . C88 C 1.1401(4) 0.8156(3) 0.4608(3) 0.043 Uani 1 1 d . . . H88 H 1.1726 0.8212 0.4268 0.052 Uiso 1 1 calc R . . C89 C 1.1822(4) 0.8209(3) 0.5094(3) 0.037 Uani 1 1 d . . . C90 C 1.1337(4) 0.8125(3) 0.5584(3) 0.034 Uani 1 1 d . . . H90 H 1.1608 0.8178 0.5913 0.040 Uiso 1 1 calc R . . C91 C 1.0056(5) 0.8019(5) 0.4064(4) 0.071 Uani 1 1 d . . . C92 C 1.0079(8) 0.8723(5) 0.3666(5) 0.118 Uani 1 1 d . . . H92A H 0.9766 0.9013 0.3849 0.177 Uiso 1 1 calc R . . H92B H 0.9794 0.8735 0.3309 0.177 Uiso 1 1 calc R . . H92C H 1.0692 0.8849 0.3597 0.177 Uiso 1 1 calc R . . C93 C 1.0561(5) 0.7598(4) 0.3751(3) 0.061 Uani 1 1 d . . . H93A H 1.0260 0.7610 0.3399 0.092 Uiso 1 1 calc R . . H93B H 1.0587 0.7165 0.3983 0.092 Uiso 1 1 calc R . . H93C H 1.1160 0.7750 0.3669 0.092 Uiso 1 1 calc R . . C94 C 0.9121(6) 0.7801(9) 0.4149(5) 0.189 Uani 1 1 d . . . H94A H 0.8785 0.8070 0.4344 0.283 Uiso 1 1 calc R . . H94B H 0.9120 0.7365 0.4374 0.283 Uiso 1 1 calc R . . H94C H 0.8852 0.7827 0.3785 0.283 Uiso 1 1 calc R . . C95 C 1.2811(4) 0.8352(3) 0.5091(3) 0.048 Uani 1 1 d . . . C96 C 1.3258(5) 0.8368(5) 0.4538(4) 0.073 Uani 1 1 d . . . H96A H 1.2953 0.8678 0.4239 0.109 Uiso 1 1 calc R . . H96B H 1.3238 0.7952 0.4463 0.109 Uiso 1 1 calc R . . H96C H 1.3872 0.8485 0.4554 0.109 Uiso 1 1 calc R . . C97 C 1.3248(5) 0.7867(5) 0.5560(4) 0.096 Uani 1 1 d . . . H97A H 1.2955 0.7871 0.5914 0.145 Uiso 1 1 calc R . . H97B H 1.3869 0.7966 0.5580 0.145 Uiso 1 1 calc R . . H97C H 1.3205 0.7450 0.5489 0.145 Uiso 1 1 calc R . . C98 C 1.2896(5) 0.9009(4) 0.5200(4) 0.072 Uani 1 1 d . . . H98A H 1.2612 0.9326 0.4896 0.109 Uiso 1 1 calc R . . H98B H 1.3520 0.9103 0.5216 0.109 Uiso 1 1 calc R . . H98C H 1.2611 0.9016 0.5556 0.109 Uiso 1 1 calc R . . C99 C 0.8655(4) 0.6605(3) 0.6325(2) 0.027 Uani 1 1 d . . . C100 C 0.7933(4) 0.6462(3) 0.6047(3) 0.036 Uani 1 1 d . . . H100 H 0.7360 0.6594 0.6133 0.043 Uiso 1 1 calc R . . C101 C 0.8046(4) 0.6132(3) 0.5651(3) 0.041 Uani 1 1 d . . . C102 C 0.8892(5) 0.5948(3) 0.5524(3) 0.047 Uani 1 1 d . . . H102 H 0.8969 0.5717 0.5249 0.057 Uiso 1 1 calc R . . C103 C 0.9617(5) 0.6094(3) 0.5788(3) 0.041 Uani 1 1 d . . . C104 C 0.9489(4) 0.6425(3) 0.6196(3) 0.033 Uani 1 1 d . . . H104 H 0.9981 0.6528 0.6386 0.040 Uiso 1 1 calc R . . C105 C 0.7256(5) 0.5973(4) 0.5325(3) 0.059 Uani 1 1 d . . . C106 C 0.6400(7) 0.6082(9) 0.5574(6) 0.188 Uani 1 1 d . . . H10D H 0.6405 0.5873 0.5974 0.281 Uiso 1 1 calc R . . H10E H 0.5933 0.5911 0.5390 0.281 Uiso 1 1 calc R . . H10F H 0.6293 0.6535 0.5523 0.281 Uiso 1 1 calc R . . C107 C 0.7333(12) 0.5237(6) 0.5387(7) 0.178 Uani 1 1 d . . . H10G H 0.7282 0.5015 0.5783 0.267 Uiso 1 1 calc R . . H10H H 0.7904 0.5131 0.5241 0.267 Uiso 1 1 calc R . . H10I H 0.6860 0.5111 0.5176 0.267 Uiso 1 1 calc R . . C108 C 0.7307(10) 0.6297(9) 0.4733(5) 0.196 Uani 1 1 d . . . H10J H 0.7880 0.6203 0.4583 0.294 Uiso 1 1 calc R . . H10K H 0.7237 0.6752 0.4689 0.294 Uiso 1 1 calc R . . H10L H 0.6838 0.6154 0.4530 0.294 Uiso 1 1 calc R . . C109 C 1.0530(5) 0.5885(3) 0.5623(3) 0.051 Uani 1 1 d . . . C110 C 1.0561(6) 0.5160(4) 0.5756(4) 0.068 Uani 1 1 d . . . H11A H 1.0438 0.4987 0.6154 0.102 Uiso 1 1 calc R . . H11B H 1.1146 0.5014 0.5665 0.102 Uiso 1 1 calc R . . H11C H 1.0118 0.5019 0.5532 0.102 Uiso 1 1 calc R . . C111 C 1.0708(6) 0.6145(4) 0.5012(4) 0.067 Uani 1 1 d . . . H11D H 1.1296 0.6003 0.4920 0.101 Uiso 1 1 calc R . . H11E H 1.0679 0.6605 0.4923 0.101 Uiso 1 1 calc R . . H11F H 1.0267 0.5995 0.4793 0.101 Uiso 1 1 calc R . . C112 C 1.1278(5) 0.6107(4) 0.5940(4) 0.060 Uani 1 1 d . . . H11G H 1.1192 0.5943 0.6344 0.090 Uiso 1 1 calc R . . H11H H 1.1271 0.6568 0.5848 0.090 Uiso 1 1 calc R . . H11I H 1.1845 0.5951 0.5830 0.090 Uiso 1 1 calc R . . C113 C 0.9302(4) 0.9198(3) 0.5760(3) 0.040 Uani 1 1 d . . . H11J H 0.8952 0.8963 0.5549 0.048 Uiso 1 1 calc R . . H11K H 0.9933 0.9142 0.5676 0.048 Uiso 1 1 calc R . . C114 C 0.9030(4) 0.9892(3) 0.5605(3) 0.046 Uani 1 1 d . . . H11L H 0.8751 1.0013 0.5232 0.055 Uiso 1 1 calc R . . H11M H 0.9543 1.0159 0.5605 0.055 Uiso 1 1 calc R . . C115 C 0.8375(4) 0.9950(3) 0.6063(3) 0.045 Uani 1 1 d . . . H11N H 0.8339 1.0383 0.6112 0.054 Uiso 1 1 calc R . . H11O H 0.7781 0.9821 0.5985 0.054 Uiso 1 1 calc R . . C116 C 0.8787(4) 0.9492(3) 0.6568(3) 0.035 Uani 1 1 d . . . H11P H 0.9263 0.9693 0.6724 0.042 Uiso 1 1 calc R . . H11Q H 0.8340 0.9346 0.6863 0.042 Uiso 1 1 calc R . . C117 C 1.1336(4) 0.7023(3) 0.6986(3) 0.038 Uani 1 1 d . . . H11R H 1.1317 0.7161 0.6572 0.045 Uiso 1 1 calc R . . H11S H 1.1076 0.6603 0.7109 0.045 Uiso 1 1 calc R . . C118 C 1.2280(4) 0.7008(3) 0.7197(3) 0.045 Uani 1 1 d . . . H11T H 1.2589 0.6604 0.7200 0.054 Uiso 1 1 calc R . . H11U H 1.2620 0.7360 0.6969 0.054 Uiso 1 1 calc R . . C119 C 1.2122(4) 0.7081(3) 0.7786(3) 0.049 Uani 1 1 d . . . H11V H 1.1948 0.6679 0.8042 0.058 Uiso 1 1 calc R . . H11W H 1.2651 0.7234 0.7934 0.058 Uiso 1 1 calc R . . C120 C 1.1383(4) 0.7561(3) 0.7702(3) 0.035 Uani 1 1 d . . . H12D H 1.1012 0.7498 0.8043 0.041 Uiso 1 1 calc R . . H12E H 1.1615 0.7991 0.7616 0.041 Uiso 1 1 calc R . . C121 C 0.6852(4) 0.5341(3) 0.7234(2) 0.033 Uani 1 1 d . . . C122 C 0.7494(4) 0.4929(3) 0.7134(3) 0.036 Uani 1 1 d . . . H122 H 0.8093 0.5039 0.7133 0.043 Uiso 1 1 calc R . . C123 C 0.7286(4) 0.4349(3) 0.7033(3) 0.039 Uani 1 1 d . . . C124 C 0.6390(4) 0.4212(3) 0.7024(3) 0.043 Uani 1 1 d . . . H124 H 0.6233 0.3826 0.6950 0.051 Uiso 1 1 calc R . . C125 C 0.5717(4) 0.4624(3) 0.7122(3) 0.045 Uani 1 1 d . . . C126 C 0.5960(4) 0.5189(3) 0.7231(3) 0.034 Uani 1 1 d . . . H126 H 0.5520 0.5474 0.7304 0.041 Uiso 1 1 calc R . . C127 C 0.8009(5) 0.3897(3) 0.6944(4) 0.057 Uani 1 1 d . . . C128 C 0.8514(6) 0.3667(5) 0.7494(4) 0.085 Uani 1 1 d . . . H12H H 0.8985 0.3369 0.7449 0.127 Uiso 1 1 calc R . . H12G H 0.8110 0.3458 0.7790 0.127 Uiso 1 1 calc R . . H12F H 0.8769 0.4027 0.7596 0.127 Uiso 1 1 calc R . . C129 C 0.8665(6) 0.4220(4) 0.6505(4) 0.082 Uani 1 1 d . . . H12K H 0.9125 0.3915 0.6457 0.124 Uiso 1 1 calc R . . H12J H 0.8932 0.4564 0.6625 0.124 Uiso 1 1 calc R . . H12I H 0.8362 0.4388 0.6148 0.124 Uiso 1 1 calc R . . C130 C 0.7660(6) 0.3301(4) 0.6820(5) 0.091 Uani 1 1 d . . . H13D H 0.8155 0.3025 0.6770 0.137 Uiso 1 1 calc R . . H13E H 0.7308 0.3415 0.6477 0.137 Uiso 1 1 calc R . . H13F H 0.7292 0.3083 0.7132 0.137 Uiso 1 1 calc R . . C131 C 0.4754(5) 0.4452(4) 0.7102(4) 0.062 Uani 1 1 d . . . C132 C 0.4573(7) 0.3829(5) 0.7478(6) 0.125 Uani 1 1 d . . . H13G H 0.4970 0.3510 0.7386 0.187 Uiso 1 1 calc R . . H13H H 0.3962 0.3722 0.7431 0.187 Uiso 1 1 calc R . . H13I H 0.4667 0.3842 0.7867 0.187 Uiso 1 1 calc R . . C133 C 0.4123(6) 0.4892(6) 0.7269(7) 0.147 Uani 1 1 d . . . H13J H 0.4280 0.4940 0.7639 0.220 Uiso 1 1 calc R . . H13K H 0.3529 0.4729 0.7281 0.220 Uiso 1 1 calc R . . H13L H 0.4142 0.5302 0.6997 0.220 Uiso 1 1 calc R . . C134 C 0.4533(7) 0.4365(6) 0.6537(5) 0.112 Uani 1 1 d . . . H13M H 0.4958 0.4068 0.6436 0.168 Uiso 1 1 calc R . . H13N H 0.4558 0.4771 0.6259 0.168 Uiso 1 1 calc R . . H13O H 0.3940 0.4201 0.6545 0.168 Uiso 1 1 calc R . . C135 C 0.5408(4) 0.7651(3) 0.7089(3) 0.045 Uani 1 1 d . . . H13P H 0.5534 0.7781 0.7435 0.054 Uiso 1 1 calc R . . H13Q H 0.5461 0.8021 0.6765 0.054 Uiso 1 1 calc R . . C136 C 0.4556(5) 0.7404(4) 0.7112(4) 0.070 Uani 1 1 d . . . H13R H 0.4127 0.7734 0.6922 0.084 Uiso 1 1 calc R . . H13S H 0.4367 0.7242 0.7506 0.084 Uiso 1 1 calc R . . C137 C 0.4614(5) 0.6866(4) 0.6813(4) 0.072 Uani 1 1 d . . . H13T H 0.4464 0.6458 0.7070 0.086 Uiso 1 1 calc R . . H13U H 0.4221 0.6952 0.6485 0.086 Uiso 1 1 calc R . . C138 C 0.5587(4) 0.6871(3) 0.6637(3) 0.039 Uani 1 1 d . . . H13V H 0.5824 0.6439 0.6667 0.047 Uiso 1 1 calc R . . H13W H 0.5668 0.7126 0.6249 0.047 Uiso 1 1 calc R . . C139 C 0.7782(4) 0.6129(3) 0.8968(2) 0.029 Uani 1 1 d . . . H13$ H 0.7218 0.6298 0.9083 0.034 Uiso 1 1 calc R . . H13 H 0.8243 0.6440 0.8961 0.034 Uiso 1 1 calc R . . C140 C 0.8026(8) 0.5513(4) 0.9360(4) 0.091 Uani 1 1 d . . . H14D H 0.8541 0.5561 0.9587 0.109 Uiso 1 1 calc R . . H14E H 0.7530 0.5363 0.9617 0.109 Uiso 1 1 calc R . . C141 C 0.8223(8) 0.5096(4) 0.9055(4) 0.095 Uani 1 1 d . . . H14F H 0.7978 0.4683 0.9240 0.114 Uiso 1 1 calc R . . H14G H 0.8870 0.5042 0.9031 0.114 Uiso 1 1 calc R . . C142 C 0.7848(4) 0.5324(3) 0.8479(3) 0.036 Uani 1 1 d . . . H14H H 0.8268 0.5245 0.8194 0.043 Uiso 1 1 calc R . . H14I H 0.7290 0.5116 0.8447 0.043 Uiso 1 1 calc R . . C143 C 1.3622(9) 1.0890(8) 0.8201(7) 0.154 Uani 1 1 d . . . H14J H 1.3358 1.0597 0.8530 0.185 Uiso 1 1 calc R . . H14K H 1.3159 1.1040 0.7916 0.185 Uiso 1 1 calc R . . C144 C 1.4297(7) 1.0597(5) 0.7986(5) 0.102 Uani 1 1 d . . . H14L H 1.4168 1.0149 0.8022 0.122 Uiso 1 1 calc R . . H14M H 1.4394 1.0805 0.7586 0.122 Uiso 1 1 calc R . . C145 C 1.5014(9) 1.0648(7) 0.8296(6) 0.137 Uani 1 1 d . . . H14N H 1.5555 1.0605 0.8080 0.164 Uiso 1 1 calc R . . H14O H 1.5023 1.0303 0.8642 0.164 Uiso 1 1 calc R . . C146 C 1.5007(9) 1.1217(7) 0.8435(8) 0.148 Uani 1 1 d . . . H14P H 1.5388 1.1519 0.8179 0.178 Uiso 1 1 calc R . . H14Q H 1.5209 1.1165 0.8824 0.178 Uiso 1 1 calc R . . C147 C 0.7200(10) 1.2843(7) 0.9091(6) 0.143 Uani 1 1 d . . . H14R H 0.7774 1.2787 0.8914 0.171 Uiso 1 1 calc R . . H14S H 0.7048 1.2444 0.9361 0.171 Uiso 1 1 calc R . . C148 C 0.6533(7) 1.3045(6) 0.8685(7) 0.125 Uani 1 1 d . . . H14T H 0.5968 1.2842 0.8811 0.150 Uiso 1 1 calc R . . H14U H 0.6705 1.2963 0.8321 0.150 Uiso 1 1 calc R . . C149 C 0.6481(10) 1.3793(5) 0.8649(6) 0.125 Uani 1 1 d . . . H14V H 0.6933 1.4019 0.8391 0.150 Uiso 1 1 calc R . . H14W H 0.5893 1.3976 0.8521 0.150 Uiso 1 1 calc R . . C150 C 0.6629(10) 1.3826(7) 0.9171(6) 0.135 Uani 1 1 d . . . H15A H 0.6083 1.3765 0.9398 0.162 Uiso 1 1 calc R . . H15B H 0.6878 1.4236 0.9178 0.162 Uiso 1 1 calc R . . C151 C 0.4792(13) 0.2383(10) 0.6718(10) 0.222 Uani 1 1 d . . . H15C H 0.4833 0.2307 0.7130 0.266 Uiso 1 1 calc R . . H15D H 0.5256 0.2673 0.6538 0.266 Uiso 1 1 calc R . . C152 C 0.4017(15) 0.2589(10) 0.6538(14) 0.313 Uani 1 1 d . . . H15E H 0.4063 0.2893 0.6168 0.376 Uiso 1 1 calc R . . H15F H 0.3727 0.2806 0.6801 0.376 Uiso 1 1 calc R . . C153 C 0.3527(13) 0.2076(11) 0.6495(11) 0.246 Uani 1 1 d . . . H15G H 0.3085 0.1984 0.6800 0.296 Uiso 1 1 calc R . . H15H H 0.3209 0.2180 0.6134 0.296 Uiso 1 1 calc R . . C154 C 0.4009(11) 0.1613(7) 0.6523(8) 0.159 Uani 1 1 d . . . H15I H 0.3948 0.1448 0.6188 0.190 Uiso 1 1 calc R . . H15J H 0.3874 0.1275 0.6861 0.190 Uiso 1 1 calc R . . C155 C 0.7971(9) 0.6732(6) 1.2451(4) 0.119 Uani 1 1 d . . . H15K H 0.7466 0.7027 1.2330 0.143 Uiso 1 1 calc R . . H15L H 0.8293 0.6680 1.2114 0.143 Uiso 1 1 calc R . . C156 C 0.8596(12) 0.6990(8) 1.2838(5) 0.207 Uani 1 1 d . . . H15M H 0.9160 0.7125 1.2647 0.248 Uiso 1 1 calc R . . H15N H 0.8315 0.7348 1.2957 0.248 Uiso 1 1 calc R . . C157 C 0.8726(9) 0.6451(6) 1.3306(6) 0.137 Uani 1 1 d . . . H15O H 0.9302 0.6239 1.3276 0.164 Uiso 1 1 calc R . . H15P H 0.8705 0.6579 1.3663 0.164 Uiso 1 1 calc R . . C158 C 0.8025(8) 0.6047(7) 1.3277(6) 0.133 Uani 1 1 d . . . H15Q H 0.8239 0.5604 1.3383 0.159 Uiso 1 1 calc R . . H15R H 0.7553 0.6100 1.3542 0.159 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 0.021 0.018 0.025 -0.008 0.003 -0.002 Nd2 0.017 0.023 0.028 -0.008 0.004 -0.001 Nd3 0.017 0.018 0.026 -0.008 0.001 -0.001 O1 0.043 0.029 0.028 -0.011 -0.002 -0.002 O2 0.037 0.023 0.034 -0.011 -0.001 0.005 O3 0.026 0.026 0.041 -0.013 0.005 -0.007 O4 0.022 0.021 0.021 -0.003 -0.002 0.001 O5 0.014 0.020 0.027 -0.002 -0.004 0.004 O6 0.021 0.023 0.031 -0.010 0.010 -0.002 O7 0.031 0.034 0.029 -0.008 0.015 -0.002 O8 0.023 0.028 0.032 -0.014 0.002 0.000 O9 0.032 0.026 0.034 -0.006 0.006 0.001 O10 0.019 0.035 0.039 -0.008 0.001 0.003 O11 0.033 0.022 0.042 -0.015 -0.002 -0.003 O12 0.019 0.031 0.044 -0.013 -0.006 0.001 O13 0.028 0.018 0.032 -0.005 0.003 0.001 O14 0.412 0.182 0.170 -0.088 -0.001 0.069 O15 0.282 0.211 0.278 -0.173 -0.126 0.076 O16 0.232 0.304 0.371 -0.182 0.025 0.047 O17 0.136 0.182 0.138 -0.063 -0.018 -0.040 C1 0.034 0.028 0.026 -0.011 -0.002 0.001 C2 0.032 0.035 0.028 -0.014 -0.002 -0.001 C3 0.034 0.033 0.029 -0.012 0.002 -0.003 C4 0.050 0.040 0.022 -0.011 0.001 -0.005 C5 0.048 0.026 0.032 -0.009 -0.005 0.000 C6 0.039 0.025 0.035 -0.006 -0.005 -0.005 C7 0.044 0.057 0.038 -0.020 0.001 -0.011 C8 0.057 0.096 0.054 -0.020 0.012 -0.042 C9 0.072 0.066 0.067 0.000 -0.002 -0.033 C10 0.056 0.122 0.071 -0.037 0.018 -0.024 C11 0.057 0.034 0.037 -0.009 -0.017 -0.008 C12 0.075 0.063 0.077 -0.028 -0.042 0.004 C13 0.086 0.054 0.057 -0.032 -0.011 -0.021 C14 0.084 0.076 0.046 -0.015 -0.020 -0.042 C15 0.028 0.023 0.037 -0.011 -0.001 0.003 C16 0.036 0.030 0.031 -0.008 0.004 0.002 C17 0.033 0.044 0.033 -0.019 0.003 0.008 C18 0.055 0.035 0.040 -0.024 -0.004 0.006 C19 0.053 0.024 0.044 -0.010 -0.002 -0.002 C20 0.046 0.029 0.033 -0.009 -0.001 0.002 C21 0.053 0.065 0.037 -0.026 0.001 0.016 C22 0.077 0.114 0.034 -0.020 -0.009 0.038 C23 0.060 0.133 0.052 -0.044 0.016 -0.007 C24 0.098 0.097 0.056 -0.058 0.007 0.010 C25 0.092 0.025 0.053 -0.005 -0.013 -0.005 C26 0.197 0.028 0.099 -0.014 -0.035 -0.015 C27 0.111 0.068 0.085 0.016 -0.021 -0.050 C28 0.111 0.030 0.083 0.016 -0.030 -0.017 C29 0.022 0.033 0.048 -0.016 0.006 -0.009 C30 0.020 0.036 0.046 -0.017 0.008 -0.010 C31 0.016 0.032 0.049 -0.019 -0.004 -0.003 C32 0.020 0.029 0.057 -0.010 -0.003 -0.009 C33 0.018 0.029 0.053 -0.009 0.002 -0.009 C34 0.021 0.033 0.041 -0.015 0.003 -0.006 C35 0.035 0.041 0.063 -0.026 0.003 -0.011 C36 0.046 0.056 0.053 -0.029 -0.002 -0.006 C37 0.098 0.074 0.120 -0.071 0.040 -0.042 C38 0.049 0.103 0.060 -0.042 -0.013 0.011 C39 0.032 0.044 0.043 -0.003 0.000 -0.013 C40 0.043 0.067 0.061 0.012 0.007 -0.019 C41 0.033 0.066 0.061 -0.006 0.013 0.001 C42 0.064 0.081 0.080 -0.028 0.028 -0.050 C43 0.016 0.025 0.032 -0.002 -0.004 -0.002 C44 0.016 0.029 0.028 -0.004 0.003 0.002 C45 0.021 0.040 0.024 -0.004 0.004 0.000 C46 0.022 0.034 0.032 0.006 -0.006 0.004 C47 0.018 0.030 0.036 -0.002 -0.001 0.000 C48 0.025 0.028 0.027 -0.007 -0.001 0.001 C49 0.029 0.058 0.018 -0.001 -0.003 0.002 C50 0.069 0.147 0.024 -0.030 -0.007 0.056 C51 0.039 0.064 0.041 -0.016 0.004 -0.006 C52 0.061 0.107 0.025 0.008 -0.001 -0.032 C53 0.022 0.029 0.052 -0.006 -0.006 0.011 C54 0.045 0.049 0.054 -0.008 -0.015 0.020 C55 0.048 0.041 0.074 -0.021 -0.013 0.015 C56 0.046 0.044 0.059 -0.003 0.014 0.017 C57 0.016 0.025 0.033 -0.005 0.007 -0.001 C58 0.023 0.027 0.027 -0.005 -0.004 0.003 C59 0.025 0.026 0.028 0.002 0.005 0.002 C60 0.021 0.028 0.040 0.004 -0.002 0.007 C61 0.024 0.020 0.043 -0.007 0.002 0.000 C62 0.017 0.024 0.038 -0.011 0.000 -0.001 C63 0.028 0.040 0.026 0.001 -0.007 0.008 C64 0.054 0.056 0.035 -0.010 0.005 -0.002 C65 0.045 0.099 0.043 -0.020 -0.015 0.032 C66 0.052 0.052 0.038 -0.003 -0.017 -0.010 C67 0.028 0.025 0.059 -0.011 0.003 0.007 C68 0.033 0.038 0.065 -0.021 0.003 0.006 C69 0.055 0.026 0.102 -0.014 0.018 0.001 C70 0.041 0.043 0.085 -0.037 -0.008 0.014 C71 0.019 0.026 0.031 -0.013 0.006 -0.001 C72 0.017 0.023 0.027 -0.008 0.005 0.004 C73 0.024 0.026 0.025 -0.013 0.003 -0.004 C74 0.016 0.037 0.034 -0.011 0.007 0.000 C75 0.022 0.030 0.040 -0.020 0.005 0.006 C76 0.022 0.021 0.041 -0.012 0.008 -0.003 C77 0.019 0.025 0.032 -0.003 0.003 -0.003 C78 0.039 0.023 0.055 -0.001 0.010 -0.005 C79 0.038 0.037 0.045 -0.003 -0.007 -0.011 C80 0.033 0.033 0.035 0.001 0.003 0.000 C81 0.042 0.033 0.078 -0.024 0.027 0.001 C82 0.073 0.160 0.353 -0.173 -0.070 0.078 C83 0.462 0.063 0.139 0.011 0.208 0.092 C84 0.094 0.037 0.121 -0.034 0.057 0.009 C85 0.035 0.026 0.038 -0.011 0.008 0.001 C86 0.031 0.048 0.043 -0.026 0.007 -0.003 C87 0.042 0.056 0.048 -0.027 0.011 0.002 C88 0.046 0.044 0.038 -0.009 0.010 0.004 C89 0.032 0.036 0.038 -0.001 0.009 0.000 C90 0.028 0.036 0.033 -0.004 0.004 0.000 C91 0.045 0.135 0.061 -0.075 0.006 0.003 C92 0.169 0.112 0.091 -0.065 -0.060 0.092 C93 0.079 0.069 0.043 -0.029 0.009 -0.001 C94 0.047 0.478 0.115 -0.208 0.015 -0.039 C95 0.032 0.057 0.045 0.007 0.013 -0.003 C96 0.046 0.110 0.060 -0.017 0.024 -0.018 C97 0.027 0.136 0.089 0.039 0.010 0.015 C98 0.048 0.086 0.080 -0.013 0.006 -0.023 C99 0.039 0.020 0.024 -0.007 0.003 -0.002 C100 0.041 0.039 0.034 -0.020 0.003 -0.001 C101 0.053 0.045 0.032 -0.021 0.006 -0.004 C102 0.072 0.043 0.037 -0.028 0.007 -0.006 C103 0.057 0.031 0.038 -0.014 0.019 -0.001 C104 0.033 0.034 0.037 -0.016 0.011 -0.002 C105 0.071 0.075 0.045 -0.037 0.001 -0.013 C106 0.079 0.410 0.149 -0.201 0.019 -0.096 C107 0.244 0.113 0.195 -0.061 -0.105 -0.046 C108 0.153 0.363 0.058 -0.015 -0.043 -0.118 C109 0.065 0.040 0.055 -0.026 0.028 -0.001 C110 0.079 0.049 0.083 -0.033 0.028 0.011 C111 0.083 0.056 0.071 -0.032 0.035 -0.001 C112 0.046 0.062 0.081 -0.037 0.021 0.004 C113 0.043 0.039 0.035 -0.002 0.009 -0.002 C114 0.045 0.037 0.049 -0.001 0.010 -0.003 C115 0.036 0.036 0.057 -0.001 0.001 0.003 C116 0.034 0.029 0.044 -0.012 0.008 0.001 C117 0.040 0.031 0.038 -0.003 0.009 -0.004 C118 0.024 0.045 0.062 -0.006 0.000 0.000 C119 0.037 0.042 0.063 -0.005 -0.014 0.001 C120 0.022 0.035 0.043 -0.001 -0.005 -0.004 C121 0.057 0.021 0.025 -0.010 0.000 -0.006 C122 0.035 0.023 0.051 -0.015 0.003 -0.006 C123 0.056 0.023 0.040 -0.010 0.008 -0.003 C124 0.059 0.030 0.046 -0.019 0.013 -0.020 C125 0.048 0.040 0.055 -0.025 0.016 -0.015 C126 0.032 0.034 0.040 -0.015 0.006 -0.010 C127 0.051 0.031 0.095 -0.029 0.016 0.000 C128 0.078 0.075 0.095 -0.013 0.017 0.016 C129 0.108 0.056 0.077 -0.012 0.048 0.021 C130 0.093 0.047 0.154 -0.062 0.018 -0.001 C131 0.047 0.067 0.089 -0.050 0.022 -0.027 C132 0.085 0.112 0.169 -0.012 0.028 -0.066 C133 0.059 0.183 0.260 -0.165 0.041 -0.051 C134 0.082 0.146 0.123 -0.060 -0.023 -0.009 C135 0.018 0.045 0.079 -0.029 -0.008 0.008 C136 0.033 0.074 0.114 -0.047 -0.005 0.013 C137 0.039 0.082 0.116 -0.064 -0.024 0.004 C138 0.049 0.048 0.022 -0.013 -0.005 -0.004 C139 0.032 0.031 0.024 -0.009 0.005 -0.005 C140 0.182 0.030 0.055 -0.004 -0.042 0.025 C141 0.173 0.053 0.048 -0.001 -0.025 0.063 C142 0.049 0.019 0.038 -0.004 -0.002 0.009 C143 0.123 0.203 0.168 -0.103 0.038 -0.052 C144 0.108 0.090 0.111 -0.031 -0.030 0.005 C145 0.122 0.127 0.144 0.002 -0.041 -0.028 C146 0.099 0.146 0.209 -0.061 -0.019 -0.007 C147 0.172 0.118 0.141 -0.046 -0.022 0.067 C148 0.076 0.119 0.213 -0.103 0.020 -0.002 C149 0.190 0.070 0.110 -0.013 -0.033 0.018 C150 0.154 0.135 0.138 -0.080 -0.042 0.069 C151 0.192 0.223 0.305 -0.169 -0.091 0.047 C152 0.236 0.165 0.578 -0.162 -0.240 0.053 C153 0.166 0.267 0.370 -0.201 -0.122 0.057 C154 0.137 0.109 0.243 -0.067 -0.001 -0.011 C155 0.170 0.130 0.052 0.001 0.005 -0.092 C156 0.274 0.247 0.076 0.023 -0.051 -0.178 C157 0.149 0.144 0.117 -0.025 -0.038 -0.061 C158 0.114 0.160 0.123 -0.027 -0.032 -0.037 _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 O1 2.172(4) . ? Nd1 O2 2.177(4) . ? Nd1 O3 2.409(4) . ? Nd1 O6 2.420(3) . ? Nd1 O4 2.576(4) . ? Nd1 O5 2.597(4) . ? Nd1 Nd3 3.7161(10) . ? Nd1 Nd2 3.7445(11) . ? Nd2 O7 2.175(4) . ? Nd2 O3 2.397(4) . ? Nd2 O4 2.429(4) . ? Nd2 O8 2.437(4) . ? Nd2 O10 2.519(4) . ? Nd2 O9 2.551(4) . ? Nd2 O5 2.587(4) . ? Nd2 Nd3 3.7665(13) . ? Nd3 O11 2.170(4) . ? Nd3 O8 2.402(4) . ? Nd3 O6 2.422(4) . ? Nd3 O5 2.440(3) . ? Nd3 O12 2.514(4) . ? Nd3 O13 2.539(4) . ? Nd3 O4 2.611(3) . ? O1 C1 1.346(7) . ? O2 C15 1.351(7) . ? O3 C29 1.359(6) . ? O4 C43 1.367(6) . ? O5 C57 1.386(6) . ? O6 C71 1.360(6) . ? O7 C85 1.352(7) . ? O8 C99 1.389(7) . ? O9 C116 1.450(7) . ? O9 C113 1.465(7) . ? O10 C117 1.442(7) . ? O10 C120 1.460(7) . ? O11 C121 1.340(6) . ? O12 C138 1.433(7) . ? O12 C135 1.434(7) . ? O13 C142 1.463(7) . ? O13 C139 1.466(7) . ? O14 C143 1.531(17) . ? O14 C146 1.556(19) . ? O15 C150 1.335(16) . ? O15 C147 1.433(15) . ? O16 C154 1.366(19) . ? O16 C151 1.37(2) . ? O17 C155 1.303(12) . ? O17 C158 1.370(14) . ? C1 C2 1.381(8) . ? C1 C6 1.398(8) . ? C2 C3 1.382(8) . ? C3 C4 1.406(8) . ? C3 C7 1.520(8) . ? C4 C5 1.402(8) . ? C5 C6 1.379(9) . ? C5 C11 1.540(8) . ? C7 C10 1.529(11) . ? C7 C8 1.533(10) . ? C7 C9 1.552(11) . ? C11 C12 1.511(10) . ? C11 C14 1.517(10) . ? C11 C13 1.563(11) . ? C15 C20 1.394(8) . ? C15 C16 1.397(8) . ? C16 C17 1.372(8) . ? C17 C18 1.413(9) . ? C17 C21 1.543(9) . ? C18 C19 1.373(9) . ? C19 C20 1.412(8) . ? C19 C25 1.531(9) . ? C21 C24 1.542(11) . ? C21 C23 1.543(11) . ? C21 C22 1.556(10) . ? C25 C26 1.509(12) . ? C25 C28 1.523(11) . ? C25 C27 1.540(13) . ? C29 C30 1.390(9) . ? C29 C34 1.392(8) . ? C30 C31 1.386(7) . ? C31 C32 1.396(8) . ? C31 C35 1.532(9) . ? C32 C33 1.391(9) . ? C33 C34 1.403(7) . ? C33 C39 1.535(9) . ? C35 C37 1.530(9) . ? C35 C36 1.535(9) . ? C35 C38 1.549(11) . ? C39 C40 1.524(10) . ? C39 C41 1.545(10) . ? C39 C42 1.548(9) . ? C43 C48 1.399(8) . ? C43 C44 1.414(8) . ? C44 C45 1.375(8) . ? C45 C46 1.406(8) . ? C45 C49 1.532(8) . ? C46 C47 1.390(9) . ? C47 C48 1.391(8) . ? C47 C53 1.531(8) . ? C49 C51 1.496(8) . ? C49 C50 1.553(10) . ? C49 C52 1.554(10) . ? C53 C54 1.509(9) . ? C53 C56 1.517(9) . ? C53 C55 1.527(9) . ? C57 C58 1.402(8) . ? C57 C62 1.405(8) . ? C58 C59 1.374(8) . ? C59 C60 1.386(8) . ? C59 C63 1.533(8) . ? C60 C61 1.396(9) . ? C61 C62 1.388(8) . ? C61 C67 1.525(8) . ? C63 C66 1.523(9) . ? C63 C64 1.542(9) . ? C63 C65 1.551(9) . ? C67 C68 1.530(8) . ? C67 C70 1.533(10) . ? C67 C69 1.538(10) . ? C71 C76 1.367(7) . ? C71 C72 1.399(7) . ? C72 C73 1.381(7) . ? C73 C74 1.388(8) . ? C73 C77 1.547(7) . ? C74 C75 1.401(8) . ? C75 C76 1.389(7) . ? C75 C81 1.528(8) . ? C77 C79 1.511(8) . ? C77 C78 1.547(8) . ? C77 C80 1.559(8) . ? C81 C83 1.435(13) . ? C81 C84 1.506(10) . ? C81 C82 1.577(13) . ? C85 C90 1.381(8) . ? C85 C86 1.381(9) . ? C86 C87 1.373(9) . ? C87 C88 1.408(9) . ? C87 C91 1.533(10) . ? C88 C89 1.401(9) . ? C89 C90 1.384(8) . ? C89 C95 1.545(9) . ? C91 C94 1.509(12) . ? C91 C93 1.533(10) . ? C91 C92 1.612(15) . ? C95 C97 1.507(11) . ? C95 C96 1.511(10) . ? C95 C98 1.543(11) . ? C99 C104 1.374(8) . ? C99 C100 1.385(8) . ? C100 C101 1.363(8) . ? C101 C102 1.393(10) . ? C101 C105 1.549(10) . ? C102 C103 1.373(10) . ? C103 C104 1.392(8) . ? C103 C109 1.532(9) . ? C105 C108 1.458(14) . ? C105 C106 1.471(13) . ? C105 C107 1.587(15) . ? C109 C111 1.497(11) . ? C109 C110 1.543(10) . ? C109 C112 1.546(11) . ? C113 C114 1.522(9) . ? C114 C115 1.526(10) . ? C115 C116 1.520(9) . ? C117 C118 1.529(9) . ? C118 C119 1.519(10) . ? C119 C120 1.498(9) . ? C121 C122 1.374(9) . ? C121 C126 1.407(8) . ? C122 C123 1.404(8) . ? C123 C124 1.406(9) . ? C123 C127 1.512(9) . ? C124 C125 1.404(9) . ? C125 C126 1.398(8) . ? C125 C131 1.529(9) . ? C127 C129 1.519(11) . ? C127 C130 1.527(10) . ? C127 C128 1.533(13) . ? C131 C133 1.471(13) . ? C131 C132 1.480(13) . ? C131 C134 1.498(13) . ? C135 C136 1.414(9) . ? C136 C137 1.543(11) . ? C137 C138 1.537(10) . ? C139 C140 1.494(9) . ? C140 C141 1.351(12) . ? C141 C142 1.498(10) . ? C143 C144 1.366(16) . ? C144 C145 1.363(14) . ? C145 C146 1.377(17) . ? C147 C148 1.415(17) . ? C148 C149 1.624(15) . ? C149 C150 1.331(16) . ? C151 C152 1.29(2) . ? C152 C153 1.40(2) . ? C153 C154 1.23(2) . ? C155 C156 1.570(15) . ? C156 C157 1.444(18) . ? C157 C158 1.422(14) . ? 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 Nd1 O2 97.23(15) . . ? O1 Nd1 O3 107.45(15) . . ? O2 Nd1 O3 100.27(14) . . ? O1 Nd1 O6 99.79(14) . . ? O2 Nd1 O6 107.23(13) . . ? O3 Nd1 O6 138.15(12) . . ? O1 Nd1 O4 161.20(13) . . ? O2 Nd1 O4 101.12(13) . . ? O3 Nd1 O4 73.33(12) . . ? O6 Nd1 O4 70.89(12) . . ? O1 Nd1 O5 100.09(14) . . ? O2 Nd1 O5 161.72(13) . . ? O3 Nd1 O5 68.96(12) . . ? O6 Nd1 O5 75.53(11) . . ? O4 Nd1 O5 62.17(11) . . ? O1 Nd1 Nd3 118.10(10) . . ? O2 Nd1 Nd3 132.25(10) . . ? O3 Nd1 Nd3 98.49(9) . . ? O6 Nd1 Nd3 39.89(9) . . ? O4 Nd1 Nd3 44.61(8) . . ? O5 Nd1 Nd3 40.85(7) . . ? O1 Nd1 Nd2 130.93(11) . . ? O2 Nd1 Nd2 118.95(11) . . ? O3 Nd1 Nd2 38.71(9) . . ? O6 Nd1 Nd2 99.60(9) . . ? O4 Nd1 Nd2 40.10(8) . . ? O5 Nd1 Nd2 43.64(8) . . ? Nd3 Nd1 Nd2 60.64(2) . . ? O7 Nd2 O3 135.52(13) . . ? O7 Nd2 O4 132.14(14) . . ? O3 Nd2 O4 76.23(12) . . ? O7 Nd2 O8 88.98(14) . . ? O3 Nd2 O8 135.47(13) . . ? O4 Nd2 O8 71.96(12) . . ? O7 Nd2 O10 80.76(15) . . ? O3 Nd2 O10 80.82(13) . . ? O4 Nd2 O10 146.88(13) . . ? O8 Nd2 O10 110.99(13) . . ? O7 Nd2 O9 76.20(14) . . ? O3 Nd2 O9 76.40(13) . . ? O4 Nd2 O9 81.16(12) . . ? O8 Nd2 O9 126.84(13) . . ? O10 Nd2 O9 116.24(13) . . ? O7 Nd2 O5 147.92(13) . . ? O3 Nd2 O5 69.31(12) . . ? O4 Nd2 O5 64.26(11) . . ? O8 Nd2 O5 69.14(12) . . ? O10 Nd2 O5 85.48(12) . . ? O9 Nd2 O5 135.66(12) . . ? O7 Nd2 Nd1 168.10(11) . . ? O3 Nd2 Nd1 38.93(9) . . ? O4 Nd2 Nd1 43.08(9) . . ? O8 Nd2 Nd1 97.87(9) . . ? O10 Nd2 Nd1 105.56(10) . . ? O9 Nd2 Nd1 91.92(9) . . ? O5 Nd2 Nd1 43.86(8) . . ? O7 Nd2 Nd3 126.96(10) . . ? O3 Nd2 Nd3 97.38(9) . . ? O4 Nd2 Nd3 43.51(8) . . ? O8 Nd2 Nd3 38.56(9) . . ? O10 Nd2 Nd3 118.33(9) . . ? O9 Nd2 Nd3 123.11(9) . . ? O5 Nd2 Nd3 40.02(7) . . ? Nd1 Nd2 Nd3 59.31(2) . . ? O11 Nd3 O8 92.16(14) . . ? O11 Nd3 O6 130.25(13) . . ? O8 Nd3 O6 137.49(12) . . ? O11 Nd3 O5 133.22(13) . . ? O8 Nd3 O5 72.20(12) . . ? O6 Nd3 O5 78.48(12) . . ? O11 Nd3 O12 81.98(14) . . ? O8 Nd3 O12 106.77(13) . . ? O6 Nd3 O12 80.38(13) . . ? O5 Nd3 O12 144.42(12) . . ? O11 Nd3 O13 76.95(14) . . ? O8 Nd3 O13 122.93(13) . . ? O6 Nd3 O13 76.90(12) . . ? O5 Nd3 O13 75.94(12) . . ? O12 Nd3 O13 126.08(13) . . ? O11 Nd3 O4 150.98(14) . . ? O8 Nd3 O4 69.40(12) . . ? O6 Nd3 O4 70.26(12) . . ? O5 Nd3 O4 63.75(11) . . ? O12 Nd3 O4 82.29(12) . . ? O13 Nd3 O4 131.73(11) . . ? O11 Nd3 Nd1 165.04(11) . . ? O8 Nd3 Nd1 99.28(9) . . ? O6 Nd3 Nd1 39.85(8) . . ? O5 Nd3 Nd1 44.12(8) . . ? O12 Nd3 Nd1 103.67(9) . . ? O13 Nd3 Nd1 88.69(8) . . ? O4 Nd3 Nd1 43.86(8) . . ? O11 Nd3 Nd2 130.63(11) . . ? O8 Nd3 Nd2 39.23(9) . . ? O6 Nd3 Nd2 98.98(8) . . ? O5 Nd3 Nd2 42.97(8) . . ? O12 Nd3 Nd2 114.22(9) . . ? O13 Nd3 Nd2 117.23(8) . . ? O4 Nd3 Nd2 39.84(8) . . ? Nd1 Nd3 Nd2 60.05(2) . . ? C1 O1 Nd1 159.4(4) . . ? C15 O2 Nd1 146.2(4) . . ? C29 O3 Nd2 129.2(4) . . ? C29 O3 Nd1 128.2(4) . . ? Nd2 O3 Nd1 102.36(13) . . ? C43 O4 Nd2 119.8(3) . . ? C43 O4 Nd1 126.0(3) . . ? Nd2 O4 Nd1 96.81(12) . . ? C43 O4 Nd3 119.0(3) . . ? Nd2 O4 Nd3 96.65(12) . . ? Nd1 O4 Nd3 91.52(11) . . ? C57 O5 Nd3 122.8(3) . . ? C57 O5 Nd2 114.6(3) . . ? Nd3 O5 Nd2 97.01(12) . . ? C57 O5 Nd1 127.5(3) . . ? Nd3 O5 Nd1 95.02(11) . . ? Nd2 O5 Nd1 92.50(11) . . ? C71 O6 Nd1 135.8(3) . . ? C71 O6 Nd3 123.9(3) . . ? Nd1 O6 Nd3 100.26(12) . . ? C85 O7 Nd2 174.5(4) . . ? C99 O8 Nd3 129.1(3) . . ? C99 O8 Nd2 128.7(3) . . ? Nd3 O8 Nd2 102.21(14) . . ? C116 O9 C113 108.5(4) . . ? C116 O9 Nd2 129.1(3) . . ? C113 O9 Nd2 122.3(3) . . ? C117 O10 C120 109.2(4) . . ? C117 O10 Nd2 117.2(3) . . ? C120 O10 Nd2 133.1(3) . . ? C121 O11 Nd3 177.5(4) . . ? C138 O12 C135 105.2(4) . . ? C138 O12 Nd3 123.5(4) . . ? C135 O12 Nd3 131.4(3) . . ? C142 O13 C139 108.6(4) . . ? C142 O13 Nd3 122.9(3) . . ? C139 O13 Nd3 128.3(3) . . ? C143 O14 C146 100.2(11) . . ? C150 O15 C147 116.9(12) . . ? C154 O16 C151 110.5(16) . . ? C155 O17 C158 111.5(10) . . ? O1 C1 C2 120.3(5) . . ? O1 C1 C6 120.6(5) . . ? C2 C1 C6 119.1(5) . . ? C1 C2 C3 121.2(5) . . ? C2 C3 C4 118.7(5) . . ? C2 C3 C7 122.9(5) . . ? C4 C3 C7 118.4(5) . . ? C5 C4 C3 121.1(6) . . ? C6 C5 C4 118.2(5) . . ? C6 C5 C11 122.4(5) . . ? C4 C5 C11 119.5(6) . . ? C5 C6 C1 121.7(5) . . ? C3 C7 C10 107.6(6) . . ? C3 C7 C8 112.0(6) . . ? C10 C7 C8 110.0(7) . . ? C3 C7 C9 110.0(6) . . ? C10 C7 C9 109.0(7) . . ? C8 C7 C9 108.1(6) . . ? C12 C11 C14 109.2(7) . . ? C12 C11 C5 109.3(5) . . ? C14 C11 C5 112.3(6) . . ? C12 C11 C13 111.0(6) . . ? C14 C11 C13 106.9(6) . . ? C5 C11 C13 108.2(6) . . ? O2 C15 C20 120.2(5) . . ? O2 C15 C16 120.6(5) . . ? C20 C15 C16 119.2(5) . . ? C17 C16 C15 121.1(6) . . ? C16 C17 C18 118.9(6) . . ? C16 C17 C21 119.1(6) . . ? C18 C17 C21 121.8(6) . . ? C19 C18 C17 121.7(6) . . ? C18 C19 C20 118.4(6) . . ? C18 C19 C25 123.0(6) . . ? C20 C19 C25 118.6(6) . . ? C15 C20 C19 120.7(6) . . ? C24 C21 C17 111.5(7) . . ? C24 C21 C23 109.1(7) . . ? C17 C21 C23 110.1(6) . . ? C24 C21 C22 110.1(7) . . ? C17 C21 C22 109.2(6) . . ? C23 C21 C22 106.7(7) . . ? C26 C25 C28 112.3(7) . . ? C26 C25 C19 111.1(7) . . ? C28 C25 C19 109.7(6) . . ? C26 C25 C27 105.4(8) . . ? C28 C25 C27 109.3(8) . . ? C19 C25 C27 108.8(6) . . ? O3 C29 C30 120.1(5) . . ? O3 C29 C34 119.9(5) . . ? C30 C29 C34 120.0(5) . . ? C31 C30 C29 121.2(5) . . ? C30 C31 C32 117.8(6) . . ? C30 C31 C35 120.7(5) . . ? C32 C31 C35 121.4(5) . . ? C33 C32 C31 122.7(5) . . ? C32 C33 C34 118.0(5) . . ? C32 C33 C39 123.8(5) . . ? C34 C33 C39 118.1(6) . . ? C29 C34 C33 120.2(6) . . ? C37 C35 C31 111.0(6) . . ? C37 C35 C36 106.7(6) . . ? C31 C35 C36 112.0(5) . . ? C37 C35 C38 111.9(7) . . ? C31 C35 C38 107.5(6) . . ? C36 C35 C38 107.8(6) . . ? C40 C39 C33 110.7(5) . . ? C40 C39 C41 105.6(6) . . ? C33 C39 C41 109.3(5) . . ? C40 C39 C42 109.2(6) . . ? C33 C39 C42 111.3(6) . . ? C41 C39 C42 110.6(6) . . ? O4 C43 C48 121.4(5) . . ? O4 C43 C44 119.4(5) . . ? C48 C43 C44 119.3(5) . . ? C45 C44 C43 121.1(5) . . ? C44 C45 C46 117.9(5) . . ? C44 C45 C49 122.3(5) . . ? C46 C45 C49 119.9(5) . . ? C47 C46 C45 122.9(5) . . ? C46 C47 C48 118.1(5) . . ? C46 C47 C53 123.7(5) . . ? C48 C47 C53 118.2(5) . . ? C47 C48 C43 120.8(6) . . ? C51 C49 C45 110.6(5) . . ? C51 C49 C50 107.0(6) . . ? C45 C49 C50 112.5(5) . . ? C51 C49 C52 109.1(6) . . ? C45 C49 C52 108.1(6) . . ? C50 C49 C52 109.4(6) . . ? C54 C53 C56 108.2(5) . . ? C54 C53 C55 109.2(5) . . ? C56 C53 C55 108.0(6) . . ? C54 C53 C47 112.0(6) . . ? C56 C53 C47 109.4(5) . . ? C55 C53 C47 110.0(5) . . ? O5 C57 C58 120.4(5) . . ? O5 C57 C62 119.5(5) . . ? C58 C57 C62 120.1(5) . . ? C59 C58 C57 120.4(5) . . ? C58 C59 C60 118.3(6) . . ? C58 C59 C63 118.9(5) . . ? C60 C59 C63 122.8(5) . . ? C59 C60 C61 123.4(5) . . ? C62 C61 C60 117.6(5) . . ? C62 C61 C67 122.9(6) . . ? C60 C61 C67 119.5(5) . . ? C61 C62 C57 120.2(5) . . ? C66 C63 C59 112.4(5) . . ? C66 C63 C64 109.2(6) . . ? C59 C63 C64 107.9(5) . . ? C66 C63 C65 108.4(6) . . ? C59 C63 C65 111.7(5) . . ? C64 C63 C65 107.0(5) . . ? C61 C67 C68 110.1(5) . . ? C61 C67 C70 111.6(5) . . ? C68 C67 C70 107.9(6) . . ? C61 C67 C69 109.9(6) . . ? C68 C67 C69 108.1(5) . . ? C70 C67 C69 109.1(6) . . ? O6 C71 C76 120.7(5) . . ? O6 C71 C72 119.1(5) . . ? C76 C71 C72 120.1(5) . . ? C73 C72 C71 121.1(5) . . ? C72 C73 C74 117.8(5) . . ? C72 C73 C77 122.4(5) . . ? C74 C73 C77 119.8(5) . . ? C73 C74 C75 122.2(5) . . ? C76 C75 C74 118.2(5) . . ? C76 C75 C81 122.3(5) . . ? C74 C75 C81 119.5(5) . . ? C71 C76 C75 120.7(5) . . ? C79 C77 C73 109.4(5) . . ? C79 C77 C78 109.1(5) . . ? C73 C77 C78 111.6(4) . . ? C79 C77 C80 110.0(5) . . ? C73 C77 C80 109.5(5) . . ? C78 C77 C80 107.2(5) . . ? C83 C81 C84 112.9(9) . . ? C83 C81 C75 112.5(7) . . ? C84 C81 C75 113.2(5) . . ? C83 C81 C82 107.5(12) . . ? C84 C81 C82 104.3(9) . . ? C75 C81 C82 105.7(6) . . ? O7 C85 C90 119.5(6) . . ? O7 C85 C86 120.4(5) . . ? C90 C85 C86 120.1(6) . . ? C87 C86 C85 121.0(6) . . ? C86 C87 C88 118.8(7) . . ? C86 C87 C91 122.8(6) . . ? C88 C87 C91 118.3(6) . . ? C89 C88 C87 120.5(6) . . ? C90 C89 C88 118.8(6) . . ? C90 C89 C95 120.2(6) . . ? C88 C89 C95 121.0(6) . . ? C85 C90 C89 120.7(6) . . ? C94 C91 C93 108.3(8) . . ? C94 C91 C87 112.1(7) . . ? C93 C91 C87 111.8(7) . . ? C94 C91 C92 110.4(10) . . ? C93 C91 C92 106.2(7) . . ? C87 C91 C92 107.9(7) . . ? C97 C95 C96 111.0(7) . . ? C97 C95 C98 109.2(8) . . ? C96 C95 C98 107.3(6) . . ? C97 C95 C89 108.2(6) . . ? C96 C95 C89 113.2(6) . . ? C98 C95 C89 107.9(6) . . ? C104 C99 C100 120.3(5) . . ? C104 C99 O8 120.2(5) . . ? C100 C99 O8 119.5(5) . . ? C101 C100 C99 120.1(6) . . ? C100 C101 C102 119.3(6) . . ? C100 C101 C105 121.5(6) . . ? C102 C101 C105 119.1(6) . . ? C103 C102 C101 121.5(6) . . ? C102 C103 C104 118.3(6) . . ? C102 C103 C109 118.8(6) . . ? C104 C103 C109 122.9(6) . . ? C99 C104 C103 120.4(6) . . ? C108 C105 C106 112.2(11) . . ? C108 C105 C101 111.1(7) . . ? C106 C105 C101 113.0(6) . . ? C108 C105 C107 108.8(11) . . ? C106 C105 C107 105.5(11) . . ? C101 C105 C107 105.8(8) . . ? C111 C109 C103 111.6(7) . . ? C111 C109 C110 109.0(6) . . ? C103 C109 C110 107.9(6) . . ? C111 C109 C112 106.6(6) . . ? C103 C109 C112 112.5(6) . . ? C110 C109 C112 109.2(7) . . ? O9 C113 C114 106.1(5) . . ? C113 C114 C115 103.6(5) . . ? C116 C115 C114 100.9(5) . . ? O9 C116 C115 105.4(5) . . ? O10 C117 C118 104.5(5) . . ? C119 C118 C117 101.1(5) . . ? C120 C119 C118 102.3(6) . . ? O10 C120 C119 105.9(5) . . ? O11 C121 C122 120.9(5) . . ? O11 C121 C126 119.1(6) . . ? C122 C121 C126 120.0(5) . . ? C121 C122 C123 121.7(6) . . ? C122 C123 C124 117.2(6) . . ? C122 C123 C127 120.4(6) . . ? C124 C123 C127 122.4(6) . . ? C125 C124 C123 122.6(5) . . ? C126 C125 C124 117.9(6) . . ? C126 C125 C131 121.9(6) . . ? C124 C125 C131 120.2(6) . . ? C125 C126 C121 120.6(6) . . ? C123 C127 C129 111.5(6) . . ? C123 C127 C130 113.0(6) . . ? C129 C127 C130 112.1(8) . . ? C123 C127 C128 107.8(7) . . ? C129 C127 C128 107.0(7) . . ? C130 C127 C128 105.0(7) . . ? C133 C131 C132 105.3(9) . . ? C133 C131 C134 111.0(10) . . ? C132 C131 C134 102.9(8) . . ? C133 C131 C125 114.4(6) . . ? C132 C131 C125 112.0(8) . . ? C134 C131 C125 110.6(7) . . ? C136 C135 O12 105.5(5) . . ? C135 C136 C137 106.6(6) . . ? C138 C137 C136 102.2(6) . . ? O12 C138 C137 102.8(5) . . ? O13 C139 C140 105.6(5) . . ? C141 C140 C139 108.3(7) . . ? C140 C141 C142 110.1(7) . . ? O13 C142 C141 103.6(5) . . ? C144 C143 O14 106.1(12) . . ? C145 C144 C143 105.2(13) . . ? C144 C145 C146 111.4(13) . . ? C145 C146 O14 104.0(12) . . ? C148 C147 O15 102.0(11) . . ? C147 C148 C149 100.6(10) . . ? C150 C149 C148 104.2(11) . . ? C149 C150 O15 102.6(12) . . ? C152 C151 O16 99.9(17) . . ? C151 C152 C153 108.2(19) . . ? C154 C153 C152 110.4(18) . . ? C153 C154 O16 103.8(16) . . ? O17 C155 C156 107.0(10) . . ? C157 C156 C155 102.3(11) . . ? C158 C157 C156 105.2(11) . . ? O17 C158 C157 109.5(12) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.921 _refine_diff_density_min -2.829 _refine_diff_density_rms 0.310 #====END data_rh4er _database_code_depnum_ccdc_archive 'CCDC 236329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [hexakis(3,5-di-tert-butylphenolato)tetrakis(tetrahydrofuran) direbium(III)].2tetrahydrofuran ; _chemical_name_common ; (hexakis(3,5-di-tert-butylphenolato)tetrakis(tetrahydrofuran) direbium(iii)).2tetrahydrofuran ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H174 Er2 O12' _chemical_formula_weight 1998.99 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' Er Er -0.2586 4.9576 '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 11.418(2) _cell_length_b 14.904(3) _cell_length_c 16.507(3) _cell_angle_alpha 104.30(3) _cell_angle_beta 94.37(3) _cell_angle_gamma 102.85(3) _cell_volume 2628.3(9) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 42292 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.33 _exptl_crystal_description prismatic _exptl_crystal_colour pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 1.641 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42292 _diffrn_reflns_av_R_equivalents 0.1658 _diffrn_reflns_av_sigmaI/netI 0.2573 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.33 _reflns_number_total 12844 _reflns_number_gt 6761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.1359P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12844 _refine_ls_number_parameters 251 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1880 _refine_ls_R_factor_gt 0.0900 _refine_ls_wR_factor_ref 0.2498 _refine_ls_wR_factor_gt 0.2099 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.165 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.09900(4) 0.42670(3) 0.45064(2) 0.01982(17) Uani 1 1 d . . . O1 O -0.0291(6) 0.3187(5) 0.3595(4) 0.0337(17) Uiso 1 1 d . . . O2 O 0.2352(6) 0.4512(5) 0.3738(4) 0.0280(16) Uiso 1 1 d . . . O3 O 0.0273(5) 0.5548(4) 0.4488(3) 0.0157(13) Uiso 1 1 d U . . O4 O 0.2563(7) 0.5190(6) 0.5624(5) 0.045(2) Uiso 1 1 d . . . O5 O 0.1731(8) 0.3098(6) 0.4960(5) 0.056(2) Uiso 1 1 d . . . O6 O 0.5058(7) 0.8764(6) 0.6715(5) 0.048(2) Uiso 1 1 d . . . C1 C -0.0731(9) 0.2414(7) 0.2955(6) 0.023(2) Uiso 1 1 d . . . C2 C -0.0618(9) 0.1520(7) 0.3009(6) 0.026(2) Uiso 1 1 d . . . H2 H -0.0245 0.1466 0.3523 0.031 Uiso 1 1 calc R . . C3 C -0.1026(8) 0.0712(6) 0.2346(5) 0.020(2) Uiso 1 1 d . . . C4 C -0.1588(8) 0.0813(6) 0.1609(5) 0.021(2) Uiso 1 1 d . . . H4 H -0.1884 0.0263 0.1144 0.025 Uiso 1 1 calc R . . C5 C -0.1732(8) 0.1679(6) 0.1529(5) 0.020(2) Uiso 1 1 d . . . C6 C -0.1298(9) 0.2478(7) 0.2204(6) 0.025(2) Uiso 1 1 d . . . H6 H -0.1389 0.3081 0.2155 0.030 Uiso 1 1 calc R . . C7 C -0.0849(9) -0.0272(7) 0.2385(6) 0.027(2) Uiso 1 1 d . . . C8 C -0.2051(10) -0.1020(8) 0.2155(7) 0.041(3) Uiso 1 1 d . . . H8A H -0.2603 -0.0838 0.2556 0.061 Uiso 1 1 calc R . . H8B H -0.1917 -0.1641 0.2176 0.061 Uiso 1 1 calc R . . H8C H -0.2409 -0.1064 0.1583 0.061 Uiso 1 1 calc R . . C9 C -0.0275(10) -0.0250(8) 0.3258(7) 0.040(3) Uiso 1 1 d . . . H9A H -0.0803 -0.0062 0.3676 0.060 Uiso 1 1 calc R . . H9B H 0.0517 0.0214 0.3404 0.060 Uiso 1 1 calc R . . H9C H -0.0172 -0.0886 0.3254 0.060 Uiso 1 1 calc R . . C10 C 0.0003(10) -0.0555(8) 0.1740(6) 0.035(3) Uiso 1 1 d . . . H10A H 0.0128 -0.1183 0.1746 0.052 Uiso 1 1 calc R . . H10B H 0.0785 -0.0078 0.1890 0.052 Uiso 1 1 calc R . . H10C H -0.0362 -0.0583 0.1175 0.052 Uiso 1 1 calc R . . C11 C -0.2372(9) 0.1744(7) 0.0681(6) 0.026(2) Uiso 1 1 d . . . C12 C -0.3668(10) 0.1079(7) 0.0469(7) 0.035(3) Uiso 1 1 d . . . H12A H -0.4144 0.1277 0.0919 0.053 Uiso 1 1 calc R . . H12B H -0.3625 0.0418 0.0419 0.053 Uiso 1 1 calc R . . H12C H -0.4056 0.1120 -0.0067 0.053 Uiso 1 1 calc R . . C13 C -0.2486(10) 0.2762(8) 0.0712(7) 0.038(3) Uiso 1 1 d . . . H13A H -0.1677 0.3202 0.0839 0.056 Uiso 1 1 calc R . . H13B H -0.2975 0.2967 0.1152 0.056 Uiso 1 1 calc R . . H13C H -0.2880 0.2766 0.0164 0.056 Uiso 1 1 calc R . . C14 C -0.1652(10) 0.1430(7) -0.0029(6) 0.031(2) Uiso 1 1 d . . . H14A H -0.0831 0.1851 0.0095 0.047 Uiso 1 1 calc R . . H14B H -0.2055 0.1467 -0.0561 0.047 Uiso 1 1 calc R . . H14C H -0.1607 0.0770 -0.0077 0.047 Uiso 1 1 calc R . . C15 C 0.2802(8) 0.4451(6) 0.2998(5) 0.020(2) Uiso 1 1 d . . . C16 C 0.2506(9) 0.3598(7) 0.2361(6) 0.023(2) Uiso 1 1 d . . . H16 H 0.1980 0.3048 0.2447 0.028 Uiso 1 1 calc R . . C17 C 0.2966(8) 0.3540(6) 0.1605(5) 0.022(2) Uiso 1 1 d . . . C18 C 0.3763(8) 0.4350(6) 0.1509(6) 0.022(2) Uiso 1 1 d . . . H18 H 0.4120 0.4305 0.1003 0.026 Uiso 1 1 calc R . . C19 C 0.4058(9) 0.5224(7) 0.2123(6) 0.023(2) Uiso 1 1 d . . . C20 C 0.3566(9) 0.5256(7) 0.2864(6) 0.025(2) Uiso 1 1 d . . . H20 H 0.3751 0.5843 0.3294 0.030 Uiso 1 1 calc R . . C21 C 0.2591(10) 0.2633(7) 0.0868(6) 0.032(2) Uiso 1 1 d . . . C22 C 0.1748(10) 0.1814(8) 0.1085(7) 0.036(3) Uiso 1 1 d . . . H22A H 0.1536 0.1253 0.0593 0.054 Uiso 1 1 calc R . . H22B H 0.1009 0.2000 0.1243 0.054 Uiso 1 1 calc R . . H22C H 0.2153 0.1658 0.1558 0.054 Uiso 1 1 calc R . . C23 C 0.3720(10) 0.2315(8) 0.0577(7) 0.043(3) Uiso 1 1 d . . . H23A H 0.4266 0.2839 0.0429 0.064 Uiso 1 1 calc R . . H23B H 0.3472 0.1758 0.0083 0.064 Uiso 1 1 calc R . . H23C H 0.4141 0.2144 0.1035 0.064 Uiso 1 1 calc R . . C24 C 0.1917(10) 0.2870(8) 0.0124(7) 0.038(3) Uiso 1 1 d . . . H24A H 0.2453 0.3392 -0.0033 0.058 Uiso 1 1 calc R . . H24B H 0.1189 0.3064 0.0298 0.058 Uiso 1 1 calc R . . H24C H 0.1683 0.2302 -0.0361 0.058 Uiso 1 1 calc R . . C25 C 0.4915(10) 0.6108(8) 0.1982(6) 0.034(2) Uiso 1 1 d . . . C26 C 0.454(2) 0.6241(16) 0.1103(14) 0.129(8) Uiso 1 1 d . . . H26A H 0.3697 0.6300 0.1062 0.193 Uiso 1 1 calc R . . H26B H 0.4597 0.5685 0.0659 0.193 Uiso 1 1 calc R . . H26C H 0.5074 0.6820 0.1033 0.193 Uiso 1 1 calc R . . C27 C 0.615(2) 0.6031(17) 0.2038(15) 0.135(8) Uiso 1 1 d . . . H27A H 0.6183 0.5411 0.1677 0.202 Uiso 1 1 calc R . . H27B H 0.6447 0.6085 0.2624 0.202 Uiso 1 1 calc R . . H27C H 0.6647 0.6546 0.1851 0.202 Uiso 1 1 calc R . . C28 C 0.4776(19) 0.7007(14) 0.2539(12) 0.112(7) Uiso 1 1 d . . . H28A H 0.3921 0.7023 0.2478 0.168 Uiso 1 1 calc R . . H28B H 0.5265 0.7551 0.2383 0.168 Uiso 1 1 calc R . . H28C H 0.5048 0.7044 0.3126 0.168 Uiso 1 1 calc R . . C29 C 0.0680(8) 0.6122(6) 0.3985(5) 0.020(2) Uiso 1 1 d U . . C30 C 0.0372(8) 0.5806(6) 0.3129(5) 0.0147(18) Uiso 1 1 d . . . H30 H -0.0118 0.5175 0.2886 0.018 Uiso 1 1 calc R . . C31 C 0.0753(8) 0.6379(6) 0.2596(5) 0.019(2) Uiso 1 1 d . . . C32 C 0.1500(8) 0.7305(6) 0.2992(5) 0.020(2) Uiso 1 1 d . . . H32 H 0.1763 0.7720 0.2651 0.024 Uiso 1 1 calc R . . C33 C 0.1866(8) 0.7631(6) 0.3859(5) 0.0180(19) Uiso 1 1 d . . . C34 C 0.1457(8) 0.7029(6) 0.4357(5) 0.0170(19) Uiso 1 1 d . . . H34 H 0.1704 0.7233 0.4950 0.020 Uiso 1 1 calc R . . C35 C 0.0353(8) 0.5998(6) 0.1650(5) 0.021(2) Uiso 1 1 d . . . C36 C 0.0893(10) 0.6698(7) 0.1166(6) 0.034(3) Uiso 1 1 d . . . H36A H 0.0610 0.6418 0.0562 0.051 Uiso 1 1 calc R . . H36B H 0.1780 0.6837 0.1266 0.051 Uiso 1 1 calc R . . H36C H 0.0637 0.7292 0.1359 0.051 Uiso 1 1 calc R . . C37 C 0.0763(9) 0.5078(7) 0.1322(6) 0.028(2) Uiso 1 1 d . . . H37A H 0.0507 0.4829 0.0711 0.042 Uiso 1 1 calc R . . H37B H 0.0396 0.4601 0.1604 0.042 Uiso 1 1 calc R . . H37C H 0.1649 0.5217 0.1439 0.042 Uiso 1 1 calc R . . C38 C -0.1024(9) 0.5774(7) 0.1461(6) 0.029(2) Uiso 1 1 d . . . H38A H -0.1274 0.5527 0.0850 0.044 Uiso 1 1 calc R . . H38B H -0.1294 0.6359 0.1671 0.044 Uiso 1 1 calc R . . H38C H -0.1390 0.5294 0.1741 0.044 Uiso 1 1 calc R . . C39 C 0.2731(9) 0.8614(7) 0.4267(6) 0.025(2) Uiso 1 1 d . . . C40 C 0.3902(9) 0.8466(7) 0.4674(6) 0.033(2) Uiso 1 1 d . . . H40A H 0.4465 0.9090 0.4944 0.049 Uiso 1 1 calc R . . H40B H 0.4278 0.8096 0.4239 0.049 Uiso 1 1 calc R . . H40C H 0.3711 0.8119 0.5099 0.049 Uiso 1 1 calc R . . C41 C 0.2134(9) 0.9189(7) 0.4964(6) 0.030(2) Uiso 1 1 d . . . H41A H 0.2687 0.9817 0.5231 0.045 Uiso 1 1 calc R . . H41B H 0.1963 0.8840 0.5390 0.045 Uiso 1 1 calc R . . H41C H 0.1375 0.9273 0.4710 0.045 Uiso 1 1 calc R . . C42 C 0.3055(10) 0.9188(7) 0.3642(6) 0.033(2) Uiso 1 1 d . . . H42A H 0.3608 0.9807 0.3937 0.049 Uiso 1 1 calc R . . H42B H 0.2316 0.9289 0.3377 0.049 Uiso 1 1 calc R . . H42C H 0.3451 0.8839 0.3208 0.049 Uiso 1 1 calc R . . C43 C 0.381(3) 0.525(2) 0.5506(18) 0.177(11) Uiso 1 1 d . . . H43A H 0.3937 0.5282 0.4926 0.212 Uiso 1 1 calc R . . H43B H 0.4072 0.4699 0.5618 0.212 Uiso 1 1 calc R . . C44 C 0.4475(13) 0.6193(10) 0.6165(8) 0.060(4) Uiso 1 1 d . . . H44A H 0.5324 0.6191 0.6339 0.072 Uiso 1 1 calc R . . H44B H 0.4476 0.6751 0.5941 0.072 Uiso 1 1 calc R . . C45 C 0.3755(12) 0.6210(9) 0.6886(8) 0.052(3) Uiso 1 1 d . . . H45A H 0.3725 0.6872 0.7166 0.062 Uiso 1 1 calc R . . H45B H 0.4114 0.5942 0.7307 0.062 Uiso 1 1 calc R . . C46 C 0.2510(11) 0.5605(9) 0.6498(7) 0.044(3) Uiso 1 1 d . . . H46A H 0.2258 0.5097 0.6784 0.053 Uiso 1 1 calc R . . H46B H 0.1915 0.6002 0.6554 0.053 Uiso 1 1 calc R . . C47 C 0.2446(16) 0.2522(13) 0.4355(11) 0.088(5) Uiso 1 1 d . . . H47A H 0.1887 0.2036 0.3883 0.105 Uiso 1 1 calc R . . H47B H 0.3032 0.2952 0.4121 0.105 Uiso 1 1 calc R . . C48 C 0.3042(13) 0.2092(10) 0.4851(9) 0.062(4) Uiso 1 1 d . . . H48A H 0.3805 0.2541 0.5170 0.074 Uiso 1 1 calc R . . H48B H 0.3237 0.1517 0.4498 0.074 Uiso 1 1 calc R . . C49 C 0.2188(12) 0.1827(9) 0.5434(8) 0.050(3) Uiso 1 1 d . . . H49A H 0.2630 0.1845 0.5980 0.060 Uiso 1 1 calc R . . H49B H 0.1649 0.1179 0.5185 0.060 Uiso 1 1 calc R . . C50 C 0.1469(12) 0.2582(9) 0.5547(8) 0.052(3) Uiso 1 1 d . . . H50A H 0.0589 0.2274 0.5461 0.062 Uiso 1 1 calc R . . H50B H 0.1690 0.3016 0.6126 0.062 Uiso 1 1 calc R . . C51 C 0.4185(12) 0.9210(10) 0.7104(8) 0.057(4) Uiso 1 1 d . . . H51A H 0.3590 0.8749 0.7303 0.068 Uiso 1 1 calc R . . H51B H 0.3743 0.9451 0.6698 0.068 Uiso 1 1 calc R . . C52 C 0.4884(11) 1.0031(8) 0.7842(7) 0.043(3) Uiso 1 1 d . . . H52A H 0.4418 1.0110 0.8326 0.052 Uiso 1 1 calc R . . H52B H 0.5078 1.0638 0.7679 0.052 Uiso 1 1 calc R . . C53 C 0.6037(11) 0.9730(8) 0.8059(7) 0.041(3) Uiso 1 1 d . . . H53A H 0.6769 1.0225 0.8043 0.049 Uiso 1 1 calc R . . H53B H 0.6073 0.9620 0.8627 0.049 Uiso 1 1 calc R . . C54 C 0.5938(12) 0.8805(9) 0.7377(8) 0.051(3) Uiso 1 1 d . . . H54A H 0.6729 0.8800 0.7172 0.061 Uiso 1 1 calc R . . H54B H 0.5691 0.8247 0.7606 0.061 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 Er1 0.0290(3) 0.0188(2) 0.0144(2) 0.00312(16) 0.00897(17) 0.01105(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 Er1 O1 2.101(7) . ? Er1 O2 2.107(7) . ? Er1 O3 2.244(6) . ? Er1 O3 2.286(6) 2_566 ? Er1 O5 2.348(9) . ? Er1 O4 2.380(8) . ? Er1 Er1 3.6798(14) 2_566 ? O1 C1 1.325(11) . ? O2 C15 1.351(11) . ? O3 C29 1.367(11) . ? O3 Er1 2.286(6) 2_566 ? O4 C43 1.43(3) . ? O4 C46 1.434(13) . ? O5 C50 1.389(14) . ? O5 C47 1.553(19) . ? O6 C54 1.407(14) . ? O6 C51 1.425(15) . ? C1 C6 1.388(12) . ? C1 C2 1.391(13) . ? C2 C3 1.373(13) . ? C3 C4 1.389(12) . ? C3 C7 1.541(13) . ? C4 C5 1.374(12) . ? C5 C6 1.380(13) . ? C5 C11 1.563(12) . ? C7 C8 1.517(14) . ? C7 C9 1.526(14) . ? C7 C10 1.541(14) . ? C11 C14 1.521(14) . ? C11 C13 1.541(14) . ? C11 C12 1.546(14) . ? C15 C16 1.390(12) . ? C15 C20 1.394(13) . ? C16 C17 1.382(13) . ? C17 C18 1.393(13) . ? C17 C21 1.530(13) . ? C18 C19 1.392(12) . ? C19 C20 1.379(13) . ? C19 C25 1.535(14) . ? C21 C22 1.513(14) . ? C21 C23 1.540(16) . ? C21 C24 1.554(14) . ? C25 C27 1.43(2) . ? C25 C28 1.47(2) . ? C25 C26 1.56(2) . ? C29 C30 1.365(12) . ? C29 C34 1.403(12) . ? C30 C31 1.398(12) . ? C31 C32 1.416(12) . ? C31 C35 1.519(12) . ? C32 C33 1.391(12) . ? C33 C34 1.392(12) . ? C33 C39 1.531(12) . ? C35 C36 1.520(13) . ? C35 C38 1.524(13) . ? C35 C37 1.533(13) . ? C39 C42 1.511(14) . ? C39 C40 1.535(14) . ? C39 C41 1.555(14) . ? C43 C44 1.54(3) . ? C44 C45 1.495(18) . ? C45 C46 1.500(17) . ? C47 C48 1.38(2) . ? C48 C49 1.482(18) . ? C49 C50 1.519(17) . ? C51 C52 1.517(16) . ? C52 C53 1.527(16) . ? C53 C54 1.525(16) . ? 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 Er1 O2 97.9(3) . . ? O1 Er1 O3 101.0(2) . . ? O2 Er1 O3 97.4(2) . . ? O1 Er1 O3 95.7(2) . 2_566 ? O2 Er1 O3 163.8(2) . 2_566 ? O3 Er1 O3 71.4(2) . 2_566 ? O1 Er1 O5 89.9(3) . . ? O2 Er1 O5 94.1(3) . . ? O3 Er1 O5 162.8(3) . . ? O3 Er1 O5 94.6(3) 2_566 . ? O1 Er1 O4 166.9(3) . . ? O2 Er1 O4 83.7(3) . . ? O3 Er1 O4 91.6(2) . . ? O3 Er1 O4 85.1(2) 2_566 . ? O5 Er1 O4 77.0(3) . . ? O1 Er1 Er1 100.3(2) . 2_566 ? O2 Er1 Er1 132.44(18) . 2_566 ? O3 Er1 Er1 36.07(15) . 2_566 ? O3 Er1 Er1 35.31(14) 2_566 2_566 ? O5 Er1 Er1 129.2(2) . 2_566 ? O4 Er1 Er1 87.9(2) . 2_566 ? C1 O1 Er1 159.1(7) . . ? C15 O2 Er1 155.1(6) . . ? C29 O3 Er1 121.1(5) . . ? C29 O3 Er1 130.0(5) . 2_566 ? Er1 O3 Er1 108.6(2) . 2_566 ? C43 O4 C46 108.9(13) . . ? C43 O4 Er1 119.8(12) . . ? C46 O4 Er1 130.5(7) . . ? C50 O5 C47 104.4(10) . . ? C50 O5 Er1 136.2(8) . . ? C47 O5 Er1 117.1(8) . . ? C54 O6 C51 105.9(9) . . ? O1 C1 C6 120.9(9) . . ? O1 C1 C2 121.1(8) . . ? C6 C1 C2 118.1(8) . . ? C3 C2 C1 122.4(9) . . ? C2 C3 C4 117.3(9) . . ? C2 C3 C7 122.8(8) . . ? C4 C3 C7 119.9(8) . . ? C5 C4 C3 122.4(8) . . ? C4 C5 C6 118.7(8) . . ? C4 C5 C11 119.8(8) . . ? C6 C5 C11 121.5(8) . . ? C5 C6 C1 121.1(9) . . ? C8 C7 C9 108.7(9) . . ? C8 C7 C3 110.8(8) . . ? C9 C7 C3 112.1(8) . . ? C8 C7 C10 109.1(9) . . ? C9 C7 C10 108.6(9) . . ? C3 C7 C10 107.5(8) . . ? C14 C11 C13 108.3(8) . . ? C14 C11 C12 108.7(8) . . ? C13 C11 C12 107.4(8) . . ? C14 C11 C5 109.4(8) . . ? C13 C11 C5 112.8(8) . . ? C12 C11 C5 110.2(8) . . ? O2 C15 C16 120.9(8) . . ? O2 C15 C20 119.8(8) . . ? C16 C15 C20 119.2(8) . . ? C17 C16 C15 120.7(9) . . ? C16 C17 C18 118.2(8) . . ? C16 C17 C21 122.2(8) . . ? C18 C17 C21 119.5(8) . . ? C19 C18 C17 122.7(9) . . ? C20 C19 C18 117.2(9) . . ? C20 C19 C25 121.7(9) . . ? C18 C19 C25 121.0(8) . . ? C19 C20 C15 121.8(9) . . ? C22 C21 C17 112.8(8) . . ? C22 C21 C23 109.0(9) . . ? C17 C21 C23 110.2(8) . . ? C22 C21 C24 108.2(8) . . ? C17 C21 C24 108.0(8) . . ? C23 C21 C24 108.6(9) . . ? C27 C25 C28 112.7(15) . . ? C27 C25 C19 111.3(13) . . ? C28 C25 C19 112.2(11) . . ? C27 C25 C26 109.0(15) . . ? C28 C25 C26 100.4(13) . . ? C19 C25 C26 110.7(11) . . ? C30 C29 O3 120.7(8) . . ? C30 C29 C34 120.2(8) . . ? O3 C29 C34 119.0(7) . . ? C29 C30 C31 122.2(8) . . ? C30 C31 C32 116.3(8) . . ? C30 C31 C35 119.8(8) . . ? C32 C31 C35 123.8(8) . . ? C33 C32 C31 122.6(8) . . ? C32 C33 C34 118.5(8) . . ? C32 C33 C39 121.7(8) . . ? C34 C33 C39 119.8(7) . . ? C33 C34 C29 120.0(8) . . ? C31 C35 C36 112.8(7) . . ? C31 C35 C38 110.0(8) . . ? C36 C35 C38 108.2(8) . . ? C31 C35 C37 109.2(7) . . ? C36 C35 C37 107.6(8) . . ? C38 C35 C37 109.0(8) . . ? C42 C39 C33 113.0(8) . . ? C42 C39 C40 108.5(8) . . ? C33 C39 C40 108.3(8) . . ? C42 C39 C41 108.8(8) . . ? C33 C39 C41 109.1(8) . . ? C40 C39 C41 109.0(8) . . ? O4 C43 C44 102.5(19) . . ? C45 C44 C43 103.4(15) . . ? C44 C45 C46 105.1(10) . . ? O4 C46 C45 107.3(10) . . ? C48 C47 O5 104.9(13) . . ? C47 C48 C49 105.3(13) . . ? C48 C49 C50 103.7(11) . . ? O5 C50 C49 108.6(11) . . ? O6 C51 C52 106.4(10) . . ? C51 C52 C53 103.6(10) . . ? C54 C53 C52 104.2(9) . . ? O6 C54 C53 107.2(10) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.350 _refine_diff_density_min -2.772 _refine_diff_density_rms 0.255 #====END data_rh4yb _database_code_depnum_ccdc_archive 'CCDC 236330' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [hexakis(3,5-di-tert-butylphenolato)tetrakis(tetrahydrofuran) diytterbium(III)].2tetrahydrofuran ; _chemical_name_common ; (hexakis(3,5-di-tert-butylphenolato)tetrakis(tetrahydrofuran) diytterbium(iii)).2tetrahydrofuran ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H174 O12 Yb2' _chemical_formula_weight 2010.55 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4229(1) _cell_length_b 14.8761(2) _cell_length_c 16.4841(2) _cell_angle_alpha 104.385(1) _cell_angle_beta 94.283(1) _cell_angle_gamma 102.832(1) _cell_volume 2620.40(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 45551 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.35 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 1.830 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45551 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.35 _reflns_number_total 12735 _reflns_number_gt 11085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction 'X -Seed' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0631P)^2^+5.4861P] 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 12735 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.342 _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 Yb1 Yb 0.097911(14) 0.427730(11) 0.450573(9) 0.01860(6) Uani 1 1 d . . . O1 O -0.0281(3) 0.3211(2) 0.36131(18) 0.0348(7) Uani 1 1 d . . . O2 O 0.2312(3) 0.4509(2) 0.37377(18) 0.0305(7) Uani 1 1 d . . . O3 O 0.0256(2) 0.55536(18) 0.44992(16) 0.0190(5) Uani 1 1 d . . . O4 O 0.2555(3) 0.5225(3) 0.5598(2) 0.0407(9) Uani 1 1 d . . . O5 O 0.1730(3) 0.3111(3) 0.4959(3) 0.0571(12) Uani 1 1 d . . . O6 O 0.5043(3) 0.8742(3) 0.6710(2) 0.0494(9) Uani 1 1 d . . . C1 C -0.0717(4) 0.2433(3) 0.2960(3) 0.0261(8) Uani 1 1 d . . . C2 C -0.0603(4) 0.1535(3) 0.3023(3) 0.0250(8) Uani 1 1 d . . . H2 H -0.0234 0.1483 0.3540 0.030 Uiso 1 1 calc R . . C3 C -0.1015(4) 0.0720(3) 0.2353(3) 0.0238(8) Uani 1 1 d . . . C4 C -0.1592(3) 0.0815(3) 0.1607(2) 0.0225(8) Uani 1 1 d . . . H4 H -0.1893 0.0261 0.1144 0.027 Uiso 1 1 calc R . . C5 C -0.1736(3) 0.1696(3) 0.1525(2) 0.0225(8) Uani 1 1 d . . . C6 C -0.1293(4) 0.2500(3) 0.2203(3) 0.0250(8) Uani 1 1 d . . . H6 H -0.1381 0.3105 0.2155 0.030 Uiso 1 1 calc R . . C7 C -0.0827(4) -0.0259(3) 0.2391(3) 0.0267(8) Uani 1 1 d . . . C8 C -0.2044(4) -0.1016(3) 0.2172(4) 0.0389(11) Uani 1 1 d . . . H8A H -0.1909 -0.1637 0.2199 0.058 Uiso 1 1 calc R . . H8B H -0.2410 -0.1069 0.1600 0.058 Uiso 1 1 calc R . . H8C H -0.2589 -0.0826 0.2577 0.058 Uiso 1 1 calc R . . C9 C -0.0260(5) -0.0243(4) 0.3270(3) 0.0390(11) Uani 1 1 d . . . H9A H -0.0160 -0.0882 0.3263 0.058 Uiso 1 1 calc R . . H9B H -0.0791 -0.0055 0.3687 0.058 Uiso 1 1 calc R . . H9C H 0.0533 0.0220 0.3421 0.058 Uiso 1 1 calc R . . C10 C 0.0025(5) -0.0545(4) 0.1755(3) 0.0400(11) Uani 1 1 d . . . H10A H 0.0154 -0.1171 0.1769 0.060 Uiso 1 1 calc R . . H10B H 0.0804 -0.0065 0.1903 0.060 Uiso 1 1 calc R . . H10C H -0.0337 -0.0583 0.1185 0.060 Uiso 1 1 calc R . . C11 C -0.2376(4) 0.1748(3) 0.0683(3) 0.0254(8) Uani 1 1 d . . . C12 C -0.3659(4) 0.1084(4) 0.0484(3) 0.0336(10) Uani 1 1 d . . . H12A H -0.4131 0.1289 0.0936 0.050 Uiso 1 1 calc R . . H12B H -0.3612 0.0424 0.0441 0.050 Uiso 1 1 calc R . . H12C H -0.4054 0.1114 -0.0054 0.050 Uiso 1 1 calc R . . C13 C -0.2491(5) 0.2761(3) 0.0712(3) 0.0376(10) Uani 1 1 d . . . H13A H -0.2948 0.2979 0.1170 0.056 Uiso 1 1 calc R . . H13B H -0.2917 0.2756 0.0171 0.056 Uiso 1 1 calc R . . H13C H -0.1681 0.3196 0.0812 0.056 Uiso 1 1 calc R . . C14 C -0.1658(4) 0.1428(3) -0.0037(3) 0.0324(9) Uani 1 1 d . . . H14A H -0.1583 0.0777 -0.0070 0.049 Uiso 1 1 calc R . . H14B H -0.0849 0.1866 0.0071 0.049 Uiso 1 1 calc R . . H14C H -0.2083 0.1438 -0.0573 0.049 Uiso 1 1 calc R . . C15 C 0.2779(4) 0.4460(3) 0.3014(3) 0.0246(8) Uani 1 1 d . . . C16 C 0.2482(4) 0.3601(3) 0.2364(3) 0.0251(8) Uani 1 1 d . . . H16 H 0.1943 0.3053 0.2444 0.030 Uiso 1 1 calc R . . C17 C 0.2959(3) 0.3534(3) 0.1608(3) 0.0239(8) Uani 1 1 d . . . C18 C 0.3760(3) 0.4348(3) 0.1506(3) 0.0254(8) Uani 1 1 d . . . H18 H 0.4114 0.4303 0.0999 0.030 Uiso 1 1 calc R . . C19 C 0.4052(4) 0.5223(3) 0.2130(3) 0.0255(8) Uani 1 1 d . A . C20 C 0.3550(4) 0.5264(3) 0.2883(3) 0.0260(8) Uani 1 1 d . . . H20 H 0.3739 0.5852 0.3315 0.031 Uiso 1 1 calc R . . C21 C 0.2586(4) 0.2632(3) 0.0861(3) 0.0297(9) Uani 1 1 d . . . C22 C 0.1737(4) 0.1800(3) 0.1080(3) 0.0360(10) Uani 1 1 d . . . H22A H 0.1016 0.1996 0.1270 0.054 Uiso 1 1 calc R . . H22B H 0.2159 0.1622 0.1533 0.054 Uiso 1 1 calc R . . H22C H 0.1493 0.1248 0.0579 0.054 Uiso 1 1 calc R . . C23 C 0.3723(5) 0.2311(4) 0.0576(3) 0.0387(11) Uani 1 1 d . . . H23A H 0.3477 0.1736 0.0096 0.058 Uiso 1 1 calc R . . H23B H 0.4157 0.2168 0.1045 0.058 Uiso 1 1 calc R . . H23C H 0.4257 0.2826 0.0406 0.058 Uiso 1 1 calc R . . C24 C 0.1926(5) 0.2867(4) 0.0126(3) 0.0394(11) Uani 1 1 d . . . H24A H 0.1206 0.3075 0.0302 0.059 Uiso 1 1 calc R . . H24B H 0.1680 0.2295 -0.0357 0.059 Uiso 1 1 calc R . . H24C H 0.2469 0.3381 -0.0038 0.059 Uiso 1 1 calc R . . C25 C 0.4909(4) 0.6110(3) 0.1983(3) 0.0349(10) Uani 1 1 d . . . C26 C 0.4431(9) 0.6234(7) 0.1096(6) 0.055(3) Uani 0.622(11) 1 d P A 1 H26A H 0.3598 0.6304 0.1098 0.083 Uiso 0.622(11) 1 calc PR A 1 H26B H 0.4449 0.5669 0.0644 0.083 Uiso 0.622(11) 1 calc PR A 1 H26C H 0.4952 0.6806 0.0999 0.083 Uiso 0.622(11) 1 calc PR A 1 C27 C 0.6128(7) 0.5992(7) 0.1973(8) 0.060(3) Uani 0.622(11) 1 d P A 1 H27A H 0.6657 0.6560 0.1876 0.090 Uiso 0.622(11) 1 calc PR A 1 H27B H 0.6133 0.5425 0.1519 0.090 Uiso 0.622(11) 1 calc PR A 1 H27C H 0.6422 0.5910 0.2517 0.090 Uiso 0.622(11) 1 calc PR A 1 C28 C 0.4863(10) 0.7055(7) 0.2633(8) 0.049(3) Uani 0.622(11) 1 d P A 1 H28A H 0.4030 0.7128 0.2599 0.074 Uiso 0.622(11) 1 calc PR A 1 H28B H 0.5398 0.7601 0.2505 0.074 Uiso 0.622(11) 1 calc PR A 1 H28C H 0.5131 0.7032 0.3205 0.074 Uiso 0.622(11) 1 calc PR A 1 C29 C 0.0690(3) 0.6133(3) 0.3999(2) 0.0180(7) Uani 1 1 d . . . C30 C 0.0365(3) 0.5808(3) 0.3130(2) 0.0188(7) Uani 1 1 d . . . H30 H -0.0134 0.5179 0.2887 0.023 Uiso 1 1 calc R . . C31 C 0.0760(3) 0.6387(3) 0.2608(2) 0.0193(7) Uani 1 1 d . . . C32 C 0.1505(3) 0.7303(3) 0.2990(2) 0.0205(7) Uani 1 1 d . . . H32 H 0.1771 0.7713 0.2644 0.025 Uiso 1 1 calc R . . C33 C 0.1870(3) 0.7635(3) 0.3858(3) 0.0208(7) Uani 1 1 d . . . C34 C 0.1446(3) 0.7036(3) 0.4366(2) 0.0198(7) Uani 1 1 d . . . H34 H 0.1677 0.7250 0.4961 0.024 Uiso 1 1 calc R . . C35 C 0.0361(3) 0.5995(3) 0.1653(2) 0.0219(7) Uani 1 1 d . . . C36 C 0.0886(4) 0.6711(3) 0.1169(3) 0.0322(9) Uani 1 1 d . . . H36A H 0.0603 0.6433 0.0563 0.048 Uiso 1 1 calc R . . H36B H 0.1774 0.6859 0.1266 0.048 Uiso 1 1 calc R . . H36C H 0.0620 0.7301 0.1367 0.048 Uiso 1 1 calc R . . C37 C 0.0778(4) 0.5074(3) 0.1323(3) 0.0275(8) Uani 1 1 d . . . H37A H 0.0516 0.4820 0.0713 0.041 Uiso 1 1 calc R . . H37B H 0.0420 0.4598 0.1611 0.041 Uiso 1 1 calc R . . H37C H 0.1664 0.5218 0.1436 0.041 Uiso 1 1 calc R . . C38 C -0.1029(4) 0.5764(4) 0.1464(3) 0.0330(10) Uani 1 1 d . . . H38A H -0.1281 0.5512 0.0853 0.049 Uiso 1 1 calc R . . H38B H -0.1302 0.6349 0.1673 0.049 Uiso 1 1 calc R . . H38C H -0.1390 0.5284 0.1747 0.049 Uiso 1 1 calc R . . C39 C 0.2740(4) 0.8621(3) 0.4283(3) 0.0249(8) Uani 1 1 d . . . C40 C 0.3915(4) 0.8473(3) 0.4682(3) 0.0345(10) Uani 1 1 d . . . H40A H 0.4475 0.9097 0.4955 0.052 Uiso 1 1 calc R . . H40B H 0.4290 0.8107 0.4241 0.052 Uiso 1 1 calc R . . H40C H 0.3730 0.8119 0.5104 0.052 Uiso 1 1 calc R . . C41 C 0.2153(4) 0.9200(3) 0.4975(3) 0.0325(9) Uani 1 1 d . . . H41A H 0.2713 0.9825 0.5245 0.049 Uiso 1 1 calc R . . H41B H 0.1970 0.8850 0.5401 0.049 Uiso 1 1 calc R . . H41C H 0.1401 0.9293 0.4721 0.049 Uiso 1 1 calc R . . C42 C 0.3053(4) 0.9205(3) 0.3646(3) 0.0358(10) Uani 1 1 d . . . H42A H 0.3609 0.9826 0.3939 0.054 Uiso 1 1 calc R . . H42B H 0.2309 0.9309 0.3390 0.054 Uiso 1 1 calc R . . H42C H 0.3440 0.8855 0.3204 0.054 Uiso 1 1 calc R . . C43 C 0.3748(8) 0.5554(16) 0.5499(6) 0.308(17) Uani 1 1 d . . . H43A H 0.4092 0.4992 0.5322 0.369 Uiso 1 1 calc R . . H43B H 0.3759 0.5859 0.5029 0.369 Uiso 1 1 calc R . . C44 C 0.4483(5) 0.6176(5) 0.6166(4) 0.0561(15) Uani 1 1 d . . . H44A H 0.4727 0.6819 0.6070 0.067 Uiso 1 1 calc R . . H44B H 0.5220 0.5958 0.6284 0.067 Uiso 1 1 calc R . . C45 C 0.3741(5) 0.6195(5) 0.6877(4) 0.0560(16) Uani 1 1 d . . . H45A H 0.3697 0.6857 0.7150 0.067 Uiso 1 1 calc R . . H45B H 0.4090 0.5933 0.7307 0.067 Uiso 1 1 calc R . . C46 C 0.2507(5) 0.5575(5) 0.6468(3) 0.0507(15) Uani 1 1 d . . . H46A H 0.2280 0.5035 0.6723 0.061 Uiso 1 1 calc R . . H46B H 0.1894 0.5954 0.6554 0.061 Uiso 1 1 calc R . . C47 C 0.2615(12) 0.2719(12) 0.4505(11) 0.237(11) Uani 1 1 d . . . H47A H 0.2246 0.2395 0.3912 0.284 Uiso 1 1 calc R . . H47B H 0.3306 0.3253 0.4498 0.284 Uiso 1 1 calc R . . C48 C 0.3028(6) 0.2109(5) 0.4824(5) 0.0623(17) Uani 1 1 d . . . H48A H 0.3859 0.2407 0.5129 0.075 Uiso 1 1 calc R . . H48B H 0.3045 0.1535 0.4372 0.075 Uiso 1 1 calc R . . C49 C 0.2169(5) 0.1844(4) 0.5424(5) 0.0546(15) Uani 1 1 d . . . H49A H 0.1634 0.1192 0.5180 0.066 Uiso 1 1 calc R . . H49B H 0.2616 0.1869 0.5971 0.066 Uiso 1 1 calc R . . C50 C 0.1450(7) 0.2588(5) 0.5535(4) 0.0588(18) Uani 1 1 d . . . H50A H 0.0572 0.2275 0.5437 0.071 Uiso 1 1 calc R . . H50B H 0.1655 0.3016 0.6118 0.071 Uiso 1 1 calc R . . C51 C 0.4188(5) 0.9212(6) 0.7109(4) 0.0628(18) Uani 1 1 d . . . H51A H 0.3585 0.8759 0.7311 0.075 Uiso 1 1 calc R . . H51B H 0.3755 0.9459 0.6704 0.075 Uiso 1 1 calc R . . C52 C 0.4898(5) 1.0033(4) 0.7848(4) 0.0467(13) Uani 1 1 d . . . H52A H 0.4440 1.0113 0.8337 0.056 Uiso 1 1 calc R . . H52B H 0.5093 1.0642 0.7687 0.056 Uiso 1 1 calc R . . C53 C 0.6056(5) 0.9716(4) 0.8051(3) 0.0419(11) Uani 1 1 d . . . H53A H 0.6789 1.0197 0.8013 0.050 Uiso 1 1 calc R . . H53B H 0.6114 0.9623 0.8626 0.050 Uiso 1 1 calc R . . C54 C 0.5917(6) 0.8774(5) 0.7381(4) 0.0538(14) Uani 1 1 d . . . H54A H 0.6701 0.8738 0.7173 0.065 Uiso 1 1 calc R . . H54B H 0.5644 0.8227 0.7620 0.065 Uiso 1 1 calc R . . C26' C 0.5468(15) 0.5894(11) 0.1161(9) 0.054(5) Uani 0.378(11) 1 d P A 2 H26D H 0.5843 0.5357 0.1137 0.081 Uiso 0.378(11) 1 calc PR A 2 H26E H 0.6085 0.6461 0.1144 0.081 Uiso 0.378(11) 1 calc PR A 2 H26F H 0.4833 0.5724 0.0676 0.081 Uiso 0.378(11) 1 calc PR A 2 C27' C 0.6108(15) 0.6405(14) 0.2708(11) 0.066(6) Uani 0.378(11) 1 d P A 2 H27D H 0.6473 0.5860 0.2656 0.099 Uiso 0.378(11) 1 calc PR A 2 H27E H 0.5862 0.6579 0.3271 0.099 Uiso 0.378(11) 1 calc PR A 2 H27F H 0.6701 0.6952 0.2628 0.099 Uiso 0.378(11) 1 calc PR A 2 C28' C 0.4363(18) 0.6888(12) 0.2055(17) 0.064(6) Uani 0.378(11) 1 d P A 2 H28D H 0.4013 0.7001 0.2586 0.096 Uiso 0.378(11) 1 calc PR A 2 H28E H 0.3721 0.6737 0.1578 0.096 Uiso 0.378(11) 1 calc PR A 2 H28F H 0.4976 0.7465 0.2053 0.096 Uiso 0.378(11) 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 Yb1 0.02267(9) 0.01967(9) 0.01655(9) 0.00622(6) 0.00573(6) 0.00911(6) O1 0.058(2) 0.0191(15) 0.0207(14) -0.0033(11) 0.0050(14) 0.0061(14) O2 0.0389(17) 0.0386(17) 0.0235(15) 0.0139(13) 0.0154(13) 0.0194(14) O3 0.0284(13) 0.0131(12) 0.0179(12) 0.0075(10) 0.0058(10) 0.0056(10) O4 0.0184(14) 0.069(2) 0.0233(15) -0.0038(15) -0.0005(12) 0.0075(15) O5 0.043(2) 0.074(3) 0.096(3) 0.067(3) 0.038(2) 0.040(2) O6 0.044(2) 0.066(3) 0.0374(19) 0.0146(18) -0.0001(16) 0.0142(18) C1 0.035(2) 0.0188(19) 0.0221(19) 0.0003(15) 0.0102(16) 0.0050(16) C2 0.0269(19) 0.026(2) 0.0213(19) 0.0055(15) 0.0026(15) 0.0060(16) C3 0.0239(18) 0.0215(19) 0.027(2) 0.0054(15) 0.0082(15) 0.0065(15) C4 0.0239(18) 0.0203(18) 0.0198(18) 0.0010(14) 0.0022(15) 0.0036(14) C5 0.0211(17) 0.0215(19) 0.0253(19) 0.0068(15) 0.0096(15) 0.0037(14) C6 0.030(2) 0.0197(19) 0.027(2) 0.0072(15) 0.0099(16) 0.0082(15) C7 0.033(2) 0.0198(19) 0.028(2) 0.0056(16) 0.0049(17) 0.0083(16) C8 0.036(2) 0.025(2) 0.056(3) 0.016(2) 0.003(2) 0.0026(18) C9 0.053(3) 0.032(2) 0.036(2) 0.011(2) 0.000(2) 0.019(2) C10 0.043(3) 0.034(3) 0.048(3) 0.011(2) 0.016(2) 0.018(2) C11 0.0260(19) 0.027(2) 0.025(2) 0.0101(16) 0.0054(16) 0.0054(16) C12 0.024(2) 0.046(3) 0.033(2) 0.018(2) 0.0015(17) 0.0059(18) C13 0.048(3) 0.037(3) 0.033(2) 0.017(2) 0.003(2) 0.014(2) C14 0.034(2) 0.039(3) 0.025(2) 0.0098(18) 0.0065(17) 0.0075(19) C15 0.0223(18) 0.035(2) 0.0226(19) 0.0129(17) 0.0074(15) 0.0119(16) C16 0.0229(18) 0.029(2) 0.029(2) 0.0122(17) 0.0084(16) 0.0099(16) C17 0.0205(17) 0.030(2) 0.0244(19) 0.0108(16) 0.0032(15) 0.0096(15) C18 0.0210(18) 0.036(2) 0.0213(19) 0.0098(16) 0.0079(15) 0.0075(16) C19 0.0210(18) 0.033(2) 0.025(2) 0.0112(17) 0.0043(15) 0.0075(16) C20 0.0236(19) 0.030(2) 0.024(2) 0.0046(16) 0.0046(15) 0.0080(16) C21 0.031(2) 0.029(2) 0.031(2) 0.0075(17) 0.0051(17) 0.0118(17) C22 0.037(2) 0.027(2) 0.040(3) 0.0050(19) 0.004(2) 0.0058(18) C23 0.045(3) 0.039(3) 0.039(3) 0.009(2) 0.013(2) 0.024(2) C24 0.047(3) 0.037(3) 0.031(2) 0.0052(19) -0.006(2) 0.012(2) C25 0.033(2) 0.035(2) 0.036(2) 0.0103(19) 0.0141(19) 0.0034(19) C26 0.059(6) 0.059(6) 0.057(6) 0.037(5) 0.016(5) 0.009(5) C27 0.025(4) 0.055(6) 0.104(10) 0.029(6) 0.023(5) 0.007(4) C28 0.042(5) 0.035(5) 0.064(7) 0.011(5) 0.020(5) -0.003(4) C29 0.0182(16) 0.0190(17) 0.0222(18) 0.0110(14) 0.0105(14) 0.0068(13) C30 0.0189(16) 0.0179(17) 0.0208(18) 0.0068(14) 0.0040(14) 0.0047(13) C31 0.0180(16) 0.0224(18) 0.0215(18) 0.0093(14) 0.0048(14) 0.0085(14) C32 0.0207(17) 0.0213(18) 0.0242(19) 0.0131(15) 0.0054(14) 0.0060(14) C33 0.0179(16) 0.0173(17) 0.029(2) 0.0089(15) 0.0062(15) 0.0045(13) C34 0.0220(17) 0.0182(18) 0.0202(18) 0.0056(14) 0.0058(14) 0.0054(14) C35 0.0257(18) 0.0235(19) 0.0188(18) 0.0085(15) 0.0021(15) 0.0082(15) C36 0.043(2) 0.035(2) 0.021(2) 0.0128(17) 0.0022(18) 0.0074(19) C37 0.036(2) 0.026(2) 0.0203(19) 0.0047(16) 0.0010(16) 0.0107(17) C38 0.025(2) 0.047(3) 0.027(2) 0.0098(19) -0.0038(17) 0.0104(18) C39 0.0263(19) 0.0170(18) 0.029(2) 0.0058(15) 0.0011(16) 0.0010(15) C40 0.027(2) 0.029(2) 0.043(3) 0.0110(19) -0.0048(19) -0.0005(17) C41 0.039(2) 0.020(2) 0.036(2) 0.0057(17) 0.0039(19) 0.0056(17) C42 0.039(2) 0.023(2) 0.042(3) 0.0138(19) 0.005(2) -0.0045(18) C43 0.040(4) 0.67(4) 0.047(5) -0.055(12) 0.016(4) -0.093(11) C44 0.027(2) 0.063(4) 0.070(4) 0.014(3) 0.004(3) 0.000(2) C45 0.035(3) 0.061(4) 0.046(3) -0.013(3) 0.005(2) -0.009(2) C46 0.031(2) 0.069(4) 0.034(3) -0.006(2) 0.006(2) -0.003(2) C47 0.211(12) 0.347(19) 0.42(2) 0.36(2) 0.274(16) 0.255(15) C48 0.070(4) 0.057(4) 0.079(5) 0.025(3) 0.034(4) 0.039(3) C49 0.055(3) 0.042(3) 0.089(5) 0.039(3) 0.024(3) 0.028(3) C50 0.089(5) 0.057(4) 0.066(4) 0.044(3) 0.044(4) 0.051(3) C51 0.042(3) 0.103(6) 0.046(3) 0.017(3) 0.003(3) 0.027(3) C52 0.050(3) 0.055(3) 0.049(3) 0.026(3) 0.023(3) 0.022(3) C53 0.038(3) 0.046(3) 0.039(3) 0.013(2) 0.003(2) 0.006(2) C54 0.057(3) 0.058(4) 0.041(3) 0.008(3) -0.012(3) 0.016(3) C26' 0.062(10) 0.049(9) 0.031(7) 0.006(6) 0.014(7) -0.023(7) C27' 0.055(9) 0.071(12) 0.045(9) 0.023(8) -0.018(7) -0.038(8) C28' 0.057(11) 0.037(9) 0.113(18) 0.033(11) 0.041(12) 0.017(8) _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 O1 2.064(3) . ? Yb1 O2 2.076(3) . ? Yb1 O3 2.234(3) . ? Yb1 O3 2.246(3) 2_566 ? Yb1 O5 2.349(3) . ? Yb1 O4 2.366(3) . ? Yb1 C29 3.152(4) . ? Yb1 Yb1 3.6362(3) 2_566 ? O1 C1 1.339(5) . ? O2 C15 1.335(5) . ? O3 C29 1.375(4) . ? O3 Yb1 2.246(3) 2_566 ? O4 C43 1.379(9) . ? O4 C46 1.408(6) . ? O5 C50 1.383(6) . ? O5 C47 1.442(9) . ? O6 C54 1.416(6) . ? O6 C51 1.430(7) . ? C1 C2 1.399(6) . ? C1 C6 1.402(6) . ? C2 C3 1.383(6) . ? C3 C4 1.404(6) . ? C3 C7 1.534(6) . ? C4 C5 1.394(6) . ? C5 C6 1.386(6) . ? C5 C11 1.547(6) . ? C7 C10 1.531(6) . ? C7 C9 1.535(6) . ? C7 C8 1.535(6) . ? C11 C13 1.531(6) . ? C11 C14 1.531(6) . ? C11 C12 1.535(6) . ? C15 C20 1.394(6) . ? C15 C16 1.403(6) . ? C16 C17 1.388(6) . ? C17 C18 1.401(6) . ? C17 C21 1.532(6) . ? C18 C19 1.398(6) . ? C19 C20 1.400(6) . ? C19 C25 1.542(6) . ? C21 C22 1.532(6) . ? C21 C24 1.533(6) . ? C21 C23 1.547(6) . ? C25 C28' 1.417(17) . ? C25 C27 1.443(9) . ? C25 C26' 1.533(15) . ? C25 C28 1.556(11) . ? C25 C26 1.590(10) . ? C25 C27' 1.651(15) . ? C29 C30 1.385(5) . ? C29 C34 1.386(5) . ? C30 C31 1.394(5) . ? C31 C32 1.399(5) . ? C31 C35 1.532(5) . ? C32 C33 1.390(5) . ? C33 C34 1.403(5) . ? C33 C39 1.539(5) . ? C35 C36 1.531(5) . ? C35 C37 1.535(6) . ? C35 C38 1.539(5) . ? C39 C40 1.534(6) . ? C39 C42 1.536(6) . ? C39 C41 1.542(6) . ? C43 C44 1.334(11) . ? C44 C45 1.495(8) . ? C45 C46 1.504(7) . ? C47 C48 1.309(10) . ? C48 C49 1.505(8) . ? C49 C50 1.502(7) . ? C51 C52 1.519(9) . ? C52 C53 1.541(7) . ? C53 C54 1.523(8) . ? 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 Yb1 O2 97.63(13) . . ? O1 Yb1 O3 101.16(12) . . ? O2 Yb1 O3 98.01(11) . . ? O1 Yb1 O3 95.43(11) . 2_566 ? O2 Yb1 O3 164.66(11) . 2_566 ? O3 Yb1 O3 71.49(10) . 2_566 ? O1 Yb1 O5 90.00(15) . . ? O2 Yb1 O5 93.89(12) . . ? O3 Yb1 O5 162.40(14) . . ? O3 Yb1 O5 94.12(11) 2_566 . ? O1 Yb1 O4 167.87(13) . . ? O2 Yb1 O4 83.16(12) . . ? O3 Yb1 O4 90.68(12) . . ? O3 Yb1 O4 85.76(10) 2_566 . ? O5 Yb1 O4 77.87(16) . . ? O1 Yb1 C29 102.01(11) . . ? O2 Yb1 C29 75.84(10) . . ? O3 Yb1 C29 22.26(9) . . ? O3 Yb1 C29 93.62(9) 2_566 . ? O5 Yb1 C29 165.03(12) . . ? O4 Yb1 C29 89.95(12) . . ? O1 Yb1 Yb1 100.22(10) . 2_566 ? O2 Yb1 Yb1 132.94(8) . 2_566 ? O3 Yb1 Yb1 35.85(6) . 2_566 ? O3 Yb1 Yb1 35.64(6) 2_566 2_566 ? O5 Yb1 Yb1 129.06(10) . 2_566 ? O4 Yb1 Yb1 87.80(8) . 2_566 ? C29 Yb1 Yb1 58.01(6) . 2_566 ? C1 O1 Yb1 158.7(3) . . ? C15 O2 Yb1 156.7(3) . . ? C29 O3 Yb1 119.7(2) . . ? C29 O3 Yb1 131.3(2) . 2_566 ? Yb1 O3 Yb1 108.51(10) . 2_566 ? C43 O4 C46 105.1(5) . . ? C43 O4 Yb1 125.7(4) . . ? C46 O4 Yb1 129.3(3) . . ? C50 O5 C47 105.9(4) . . ? C50 O5 Yb1 135.6(3) . . ? C47 O5 Yb1 118.1(4) . . ? C54 O6 C51 105.1(4) . . ? O1 C1 C2 120.2(4) . . ? O1 C1 C6 121.0(4) . . ? C2 C1 C6 118.8(4) . . ? C3 C2 C1 121.7(4) . . ? C2 C3 C4 117.8(4) . . ? C2 C3 C7 122.5(4) . . ? C4 C3 C7 119.7(4) . . ? C5 C4 C3 122.1(4) . . ? C6 C5 C4 118.6(4) . . ? C6 C5 C11 122.1(4) . . ? C4 C5 C11 119.3(3) . . ? C5 C6 C1 121.0(4) . . ? C10 C7 C3 108.3(3) . . ? C10 C7 C9 108.3(4) . . ? C3 C7 C9 112.5(3) . . ? C10 C7 C8 109.8(4) . . ? C3 C7 C8 110.5(4) . . ? C9 C7 C8 107.4(4) . . ? C13 C11 C14 108.2(4) . . ? C13 C11 C12 107.7(4) . . ? C14 C11 C12 108.8(4) . . ? C13 C11 C5 112.4(3) . . ? C14 C11 C5 109.7(3) . . ? C12 C11 C5 110.0(3) . . ? O2 C15 C20 120.7(4) . . ? O2 C15 C16 120.5(4) . . ? C20 C15 C16 118.8(4) . . ? C17 C16 C15 121.4(4) . . ? C16 C17 C18 118.4(4) . . ? C16 C17 C21 122.9(4) . . ? C18 C17 C21 118.6(4) . . ? C19 C18 C17 121.9(4) . . ? C18 C19 C20 118.1(4) . . ? C18 C19 C25 120.3(4) . . ? C20 C19 C25 121.6(4) . . ? C15 C20 C19 121.4(4) . . ? C17 C21 C22 112.2(4) . . ? C17 C21 C24 108.6(4) . . ? C22 C21 C24 108.5(4) . . ? C17 C21 C23 110.0(4) . . ? C22 C21 C23 108.5(4) . . ? C24 C21 C23 109.0(4) . . ? C28' C25 C27 135.6(9) . . ? C28' C25 C26' 111.9(12) . . ? C27 C25 C26' 58.0(8) . . ? C28' C25 C19 112.3(7) . . ? C27 C25 C19 110.7(5) . . ? C26' C25 C19 113.6(6) . . ? C28' C25 C28 39.6(10) . . ? C27 C25 C28 111.8(7) . . ? C26' C25 C28 133.4(7) . . ? C19 C25 C28 112.2(5) . . ? C28' C25 C26 66.5(12) . . ? C27 C25 C26 109.3(7) . . ? C26' C25 C26 53.0(8) . . ? C19 C25 C26 108.3(5) . . ? C28 C25 C26 104.2(7) . . ? C28' C25 C27' 110.2(13) . . ? C27 C25 C27' 45.8(8) . . ? C26' C25 C27' 102.0(10) . . ? C19 C25 C27' 106.1(6) . . ? C28 C25 C27' 72.7(9) . . ? C26 C25 C27' 143.7(7) . . ? O3 C29 C30 119.6(3) . . ? O3 C29 C34 119.9(3) . . ? C30 C29 C34 120.4(3) . . ? O3 C29 Yb1 37.99(15) . . ? C30 C29 Yb1 103.2(2) . . ? C34 C29 Yb1 123.7(3) . . ? C29 C30 C31 121.1(3) . . ? C30 C31 C32 117.8(3) . . ? C30 C31 C35 118.8(3) . . ? C32 C31 C35 123.4(3) . . ? C33 C32 C31 122.2(3) . . ? C32 C33 C34 118.5(3) . . ? C32 C33 C39 122.9(3) . . ? C34 C33 C39 118.6(3) . . ? C29 C34 C33 120.0(3) . . ? C36 C35 C31 112.3(3) . . ? C36 C35 C37 108.5(3) . . ? C31 C35 C37 109.5(3) . . ? C36 C35 C38 107.7(3) . . ? C31 C35 C38 109.7(3) . . ? C37 C35 C38 109.0(3) . . ? C40 C39 C42 108.7(4) . . ? C40 C39 C33 108.9(3) . . ? C42 C39 C33 111.8(3) . . ? C40 C39 C41 109.5(4) . . ? C42 C39 C41 108.0(4) . . ? C33 C39 C41 110.0(3) . . ? C44 C43 O4 117.5(7) . . ? C43 C44 C45 104.2(5) . . ? C44 C45 C46 104.7(4) . . ? O4 C46 C45 108.0(4) . . ? C48 C47 O5 114.1(7) . . ? C47 C48 C49 105.9(5) . . ? C50 C49 C48 103.8(4) . . ? O5 C50 C49 108.3(5) . . ? O6 C51 C52 107.1(5) . . ? C51 C52 C53 103.1(5) . . ? C54 C53 C52 104.2(4) . . ? O6 C54 C53 107.3(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.729 _refine_diff_density_min -2.264 _refine_diff_density_rms 0.152 #====END data_La4H2O.CIF _database_code_depnum_ccdc_archive 'CCDC 236331' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [(Aqua)dodecakis(3,5-di-tert-butylphenolato)tetrakislanthanum(III)] ; _chemical_name_common ;((Aqua)dodecakis(3,5-di-tert- butylphenolato)tetrakislanthanum(iii)) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H254 La4 O13' _chemical_formula_weight 3035.34 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.5273(11) _cell_length_b 18.8403(6) _cell_length_c 29.0828(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.3970(10) _cell_angle_gamma 90.00 _cell_volume 17491.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 94007 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 28.31 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6376 _exptl_absorpt_coefficient_mu 1.009 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94007 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.31 _reflns_number_total 21312 _reflns_number_gt 13486 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART/SAINT _computing_cell_refinement SMART/SAINT _computing_data_reduction SMART/SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0788P)^2^+111.3960P] 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 21312 _refine_ls_number_parameters 956 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1475 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 La1 La 0.210056(9) 0.634923(16) 0.011981(12) 0.02873(9) Uani 1 1 d . . . La2 La 0.321599(10) 0.673010(17) 0.022623(13) 0.03263(10) Uani 1 1 d . . . O1 O 0.27906(15) 0.6488(4) 0.07293(19) 0.093(2) Uani 1 1 d . . . O2 O 0.25560(16) 0.6163(3) -0.0318(2) 0.0702(17) Uani 1 1 d . . . O3 O 0.1691(2) 0.7107(3) -0.0586(2) 0.103(3) Uani 1 1 d . . . O4 O 0.1915(3) 0.7448(3) 0.0448(3) 0.119(3) Uani 1 1 d . . . O5 O 0.19068(14) 0.5284(2) 0.02348(17) 0.0473(11) Uani 1 1 d . . . O6 O 0.38409(14) 0.6273(3) 0.0453(2) 0.0708(16) Uani 1 1 d . . . C25 C 0.3321(2) 0.5519(4) -0.1368(3) 0.0563(18) Uani 1 1 d . . . C26 C 0.3709(3) 0.5961(5) -0.1045(4) 0.084(3) Uani 1 1 d . . . H26A H 0.3867 0.6105 -0.1247 0.126 Uiso 1 1 calc R . . H26B H 0.3888 0.5672 -0.0764 0.126 Uiso 1 1 calc R . . H26C H 0.3616 0.6383 -0.0919 0.126 Uiso 1 1 calc R . . C27 C 0.3032(3) 0.5974(5) -0.1803(4) 0.085(3) Uani 1 1 d . . . H27A H 0.3184 0.6122 -0.2011 0.128 Uiso 1 1 calc R . . H27B H 0.2942 0.6394 -0.1671 0.128 Uiso 1 1 calc R . . H27C H 0.2786 0.5694 -0.2003 0.128 Uiso 1 1 calc R . . C28 C 0.3474(3) 0.4884(5) -0.1580(3) 0.066(2) Uani 1 1 d . . . H28A H 0.3629 0.5053 -0.1779 0.099 Uiso 1 1 calc R . . H28B H 0.3233 0.4601 -0.1789 0.099 Uiso 1 1 calc R . . H28C H 0.3659 0.4589 -0.1306 0.099 Uiso 1 1 calc R . . C1 C 0.3070(2) 0.6136(5) 0.1136(3) 0.071(3) Uani 1 1 d . . . C2 C 0.3045(2) 0.5402(5) 0.1189(3) 0.066(2) Uani 1 1 d . . . H2 H 0.2830 0.5143 0.0941 0.079 Uiso 1 1 calc R . . C3 C 0.3333(2) 0.5040(4) 0.1601(3) 0.0555(19) Uani 1 1 d . . . C4 C 0.3646(2) 0.5448(4) 0.1945(2) 0.0516(18) Uani 1 1 d . . . H4 H 0.3845 0.5216 0.2226 0.062 Uiso 1 1 calc R . . C5 C 0.3683(2) 0.6174(4) 0.1900(3) 0.061(2) Uani 1 1 d . A . C6 C 0.3389(2) 0.6522(5) 0.1486(3) 0.068(3) Uani 1 1 d . . . H6 H 0.3410 0.7019 0.1446 0.082 Uiso 1 1 calc R . . C7 C 0.3285(3) 0.4240(5) 0.1660(4) 0.074(2) Uani 1 1 d . . . C8 C 0.3291(5) 0.3822(8) 0.1198(5) 0.148(6) Uani 1 1 d . . . H8A H 0.3069 0.4001 0.0896 0.222 Uiso 1 1 calc R . . H8B H 0.3246 0.3316 0.1237 0.222 Uiso 1 1 calc R . . H8C H 0.3563 0.3888 0.1171 0.222 Uiso 1 1 calc R . . C9 C 0.3636(3) 0.3938(5) 0.2113(5) 0.104(4) Uani 1 1 d . . . H9A H 0.3593 0.3427 0.2135 0.156 Uiso 1 1 calc R . . H9B H 0.3636 0.4173 0.2414 0.156 Uiso 1 1 calc R . . H9C H 0.3906 0.4019 0.2082 0.156 Uiso 1 1 calc R . . C10 C 0.2872(3) 0.4081(5) 0.1710(4) 0.096(3) Uani 1 1 d . . . H10A H 0.2640 0.4265 0.1419 0.144 Uiso 1 1 calc R . . H10B H 0.2868 0.4307 0.2012 0.144 Uiso 1 1 calc R . . H10C H 0.2841 0.3566 0.1732 0.144 Uiso 1 1 calc R . . C11 C 0.4032(3) 0.6614(5) 0.2284(4) 0.081(3) Uani 1 1 d . . . C12 C 0.3937(10) 0.7503(13) 0.2278(11) 0.081(10) Uani 0.396(15) 1 d P A 2 H12A H 0.3651 0.7581 0.2262 0.122 Uiso 0.396(15) 1 calc PR A 2 H12B H 0.3968 0.7719 0.1987 0.122 Uiso 0.396(15) 1 calc PR A 2 H12C H 0.4137 0.7720 0.2582 0.122 Uiso 0.396(15) 1 calc PR A 2 C13 C 0.4309(5) 0.6881(10) 0.1963(7) 0.098(7) Uani 0.604(15) 1 d P A 1 H13A H 0.4416 0.6466 0.1846 0.147 Uiso 0.604(15) 1 calc PR A 1 H13B H 0.4544 0.7172 0.2176 0.147 Uiso 0.604(15) 1 calc PR A 1 H13C H 0.4131 0.7162 0.1677 0.147 Uiso 0.604(15) 1 calc PR A 1 C14 C 0.4354(5) 0.6120(8) 0.2658(5) 0.085(6) Uani 0.604(15) 1 d P A 1 H14A H 0.4455 0.5773 0.2477 0.127 Uiso 0.604(15) 1 calc PR A 1 H14B H 0.4223 0.5871 0.2856 0.127 Uiso 0.604(15) 1 calc PR A 1 H14C H 0.4591 0.6402 0.2878 0.127 Uiso 0.604(15) 1 calc PR A 1 C15 C 0.2699(2) 0.5632(4) -0.0534(3) 0.0492(17) Uani 1 1 d . . . C16 C 0.2644(2) 0.4918(4) -0.0442(2) 0.0481(16) Uani 1 1 d . . . H16 H 0.2500 0.4797 -0.0232 0.058 Uiso 1 1 calc R . . C17 C 0.2797(2) 0.4388(4) -0.0653(2) 0.0482(16) Uani 1 1 d . . . C18 C 0.3011(2) 0.4591(3) -0.0954(2) 0.0480(16) Uani 1 1 d . . . H18 H 0.3115 0.4230 -0.1105 0.058 Uiso 1 1 calc R . . C19 C 0.3080(2) 0.5287(3) -0.1044(2) 0.0425(14) Uani 1 1 d . . . C20 C 0.2921(2) 0.5816(3) -0.0826(3) 0.0469(16) Uani 1 1 d . . . H20 H 0.2965 0.6302 -0.0878 0.056 Uiso 1 1 calc R . . C21 C 0.2729(3) 0.3604(4) -0.0570(3) 0.071(2) Uani 1 1 d . . . C22 C 0.2445(4) 0.3502(6) -0.0275(4) 0.104(4) Uani 1 1 d . . . H22A H 0.2407 0.2994 -0.0234 0.156 Uiso 1 1 calc R . . H22B H 0.2172 0.3723 -0.0455 0.156 Uiso 1 1 calc R . . H22C H 0.2576 0.3724 0.0053 0.156 Uiso 1 1 calc R . . C23 C 0.3160(3) 0.3271(5) -0.0287(4) 0.097(3) Uani 1 1 d . . . H23A H 0.3125 0.2767 -0.0226 0.146 Uiso 1 1 calc R . . H23B H 0.3296 0.3516 0.0032 0.146 Uiso 1 1 calc R . . H23C H 0.3333 0.3315 -0.0485 0.146 Uiso 1 1 calc R . . C24 C 0.2515(3) 0.3241(4) -0.1078(4) 0.089(3) Uani 1 1 d . . . H24A H 0.2465 0.2741 -0.1028 0.134 Uiso 1 1 calc R . . H24B H 0.2696 0.3276 -0.1266 0.134 Uiso 1 1 calc R . . H24C H 0.2247 0.3477 -0.1263 0.134 Uiso 1 1 calc R . . C29 C 0.1408(2) 0.6679(3) -0.0928(3) 0.058(2) Uani 1 1 d . . . C30 C 0.1537(2) 0.6244(4) -0.1217(3) 0.0543(19) Uani 1 1 d . . . H30 H 0.1823 0.6247 -0.1175 0.065 Uiso 1 1 calc R . . C31 C 0.12622(19) 0.5799(3) -0.1568(2) 0.0408(14) Uani 1 1 d . . . C32 C 0.08447(19) 0.5798(3) -0.1617(2) 0.0387(13) Uani 1 1 d . . . H32 H 0.0652 0.5492 -0.1854 0.046 Uiso 1 1 calc R . . C33 C 0.0703(2) 0.6235(4) -0.1327(2) 0.0447(15) Uani 1 1 d . C . C34 C 0.0991(2) 0.6679(4) -0.0981(2) 0.0531(18) Uani 1 1 d . . . H34 H 0.0902 0.6983 -0.0780 0.064 Uiso 1 1 calc R . . C35 C 0.1406(2) 0.5313(4) -0.1898(3) 0.0595(19) Uani 1 1 d . . . C36 C 0.1479(5) 0.4582(6) -0.1677(5) 0.141(6) Uani 1 1 d . . . H36A H 0.1670 0.4609 -0.1327 0.212 Uiso 1 1 calc R . . H36B H 0.1603 0.4282 -0.1860 0.212 Uiso 1 1 calc R . . H36C H 0.1212 0.4376 -0.1699 0.212 Uiso 1 1 calc R . . C37 C 0.1843(3) 0.5604(9) -0.1902(5) 0.134(5) Uani 1 1 d . . . H37A H 0.2056 0.5593 -0.1563 0.201 Uiso 1 1 calc R . . H37B H 0.1806 0.6093 -0.2026 0.201 Uiso 1 1 calc R . . H37C H 0.1932 0.5304 -0.2118 0.201 Uiso 1 1 calc R . . C38 C 0.1121(3) 0.5369(6) -0.2428(3) 0.094(3) Uani 1 1 d . . . H38A H 0.1219 0.5051 -0.2628 0.142 Uiso 1 1 calc R . . H38B H 0.1120 0.5859 -0.2542 0.142 Uiso 1 1 calc R . . H38C H 0.0837 0.5233 -0.2465 0.142 Uiso 1 1 calc R . . C39 C 0.0238(3) 0.6255(5) -0.1399(4) 0.076(3) Uani 1 1 d . . . C43 C 0.1800(4) 0.7139(4) 0.0801(3) 0.068(3) Uani 1 1 d . . . C44 C 0.2078(3) 0.7045(4) 0.1274(3) 0.063(2) Uani 1 1 d . . . H44 H 0.2356 0.7217 0.1365 0.076 Uiso 1 1 calc R . . C45 C 0.1966(2) 0.6708(4) 0.1625(3) 0.0544(18) Uani 1 1 d . . . C46 C 0.1565(2) 0.6455(5) 0.1481(3) 0.065(2) Uani 1 1 d . . . H46 H 0.1484 0.6229 0.1723 0.077 Uiso 1 1 calc R . . C47 C 0.1267(3) 0.6517(5) 0.0988(3) 0.075(3) Uani 1 1 d . . . C48 C 0.1398(4) 0.6879(4) 0.0659(3) 0.081(3) Uani 1 1 d . . . H48 H 0.1207 0.6950 0.0326 0.098 Uiso 1 1 calc R . . C49 C 0.2273(3) 0.6607(6) 0.2164(4) 0.093(3) Uani 1 1 d . . . C50 C 0.2667(5) 0.7003(10) 0.2268(6) 0.195(9) Uani 1 1 d . . . H50A H 0.2603 0.7476 0.2118 0.293 Uiso 1 1 calc R . . H50B H 0.2842 0.6746 0.2126 0.293 Uiso 1 1 calc R . . H50C H 0.2817 0.7048 0.2628 0.293 Uiso 1 1 calc R . . C51 C 0.2105(7) 0.7087(12) 0.2492(5) 0.217(10) Uani 1 1 d . . . H51A H 0.2090 0.7581 0.2382 0.325 Uiso 1 1 calc R . . H51B H 0.2296 0.7052 0.2842 0.325 Uiso 1 1 calc R . . H51C H 0.1826 0.6925 0.2457 0.325 Uiso 1 1 calc R . . C52 C 0.2308(6) 0.5884(8) 0.2312(6) 0.291(17) Uani 1 1 d . . . H52A H 0.2028 0.5685 0.2232 0.436 Uiso 1 1 calc R . . H52B H 0.2468 0.5851 0.2672 0.436 Uiso 1 1 calc R . . H52C H 0.2453 0.5618 0.2136 0.436 Uiso 1 1 calc R . . C53 C 0.0828(4) 0.6209(8) 0.0813(6) 0.132(6) Uani 1 1 d . . . C54 C 0.0742(3) 0.5812(7) 0.1205(6) 0.147(6) Uani 1 1 d . . . H54A H 0.0457 0.5621 0.1066 0.221 Uiso 1 1 calc R . . H54B H 0.0770 0.6133 0.1481 0.221 Uiso 1 1 calc R . . H54C H 0.0943 0.5421 0.1325 0.221 Uiso 1 1 calc R . . C55 C 0.0764(5) 0.5631(9) 0.0370(7) 0.189(9) Uani 1 1 d . . . H55A H 0.0816 0.5860 0.0097 0.284 Uiso 1 1 calc R . . H55B H 0.0477 0.5449 0.0247 0.284 Uiso 1 1 calc R . . H55C H 0.0961 0.5237 0.0501 0.284 Uiso 1 1 calc R . . C56 C 0.0508(4) 0.6730(9) 0.0578(7) 0.191(9) Uani 1 1 d . . . H56A H 0.0565 0.6963 0.0309 0.286 Uiso 1 1 calc R . . H56B H 0.0508 0.7085 0.0824 0.286 Uiso 1 1 calc R . . H56C H 0.0234 0.6496 0.0441 0.286 Uiso 1 1 calc R . . C57 C 0.16862(19) 0.4700(3) 0.0266(2) 0.0409(14) Uani 1 1 d . . . C58 C 0.1698(2) 0.4464(3) 0.0726(2) 0.0412(14) Uani 1 1 d . . . H58 H 0.1867 0.4704 0.1022 0.049 Uiso 1 1 calc R . . C59 C 0.14641(19) 0.3883(3) 0.0751(2) 0.0392(14) Uani 1 1 d . . . C60 C 0.12223(18) 0.3536(3) 0.0319(2) 0.0397(14) Uani 1 1 d . . . H60 H 0.1066 0.3131 0.0340 0.048 Uiso 1 1 calc R . . C61 C 0.12012(19) 0.3760(3) -0.0145(2) 0.0389(13) Uani 1 1 d . . . C62 C 0.1444(2) 0.4348(3) -0.0164(2) 0.0414(14) Uani 1 1 d . . . H62 H 0.1442 0.4505 -0.0475 0.050 Uiso 1 1 calc R . . C63 C 0.1467(2) 0.3609(4) 0.1256(2) 0.0474(16) Uani 1 1 d . . . C64 C 0.1641(3) 0.2857(5) 0.1347(3) 0.070(2) Uani 1 1 d . . . H64A H 0.1928 0.2857 0.1356 0.105 Uiso 1 1 calc R . . H64B H 0.1465 0.2546 0.1078 0.105 Uiso 1 1 calc R . . H64C H 0.1643 0.2684 0.1666 0.105 Uiso 1 1 calc R . . C65 C 0.1730(3) 0.4074(5) 0.1690(3) 0.072(3) Uani 1 1 d . . . H65A H 0.2019 0.4091 0.1707 0.108 Uiso 1 1 calc R . . H65B H 0.1728 0.3876 0.2001 0.108 Uiso 1 1 calc R . . H65C H 0.1614 0.4556 0.1643 0.108 Uiso 1 1 calc R . . C66 C 0.1018(2) 0.3603(4) 0.1241(3) 0.061(2) Uani 1 1 d . . . H66A H 0.0902 0.4085 0.1179 0.091 Uiso 1 1 calc R . . H66B H 0.1020 0.3433 0.1560 0.091 Uiso 1 1 calc R . . H66C H 0.0844 0.3287 0.0974 0.091 Uiso 1 1 calc R . . C67 C 0.0924(2) 0.3400(4) -0.0633(3) 0.0507(17) Uani 1 1 d . . . C68 C 0.0617(3) 0.3935(5) -0.0976(3) 0.084(3) Uani 1 1 d . . . H68A H 0.0773 0.4334 -0.1038 0.125 Uiso 1 1 calc R . . H68B H 0.0431 0.4111 -0.0818 0.125 Uiso 1 1 calc R . . H68C H 0.0451 0.3705 -0.1292 0.125 Uiso 1 1 calc R . . C69 C 0.0666(3) 0.2794(5) -0.0554(3) 0.085(3) Uani 1 1 d . . . H69A H 0.0494 0.2584 -0.0875 0.127 Uiso 1 1 calc R . . H69B H 0.0483 0.2974 -0.0391 0.127 Uiso 1 1 calc R . . H69C H 0.0854 0.2431 -0.0342 0.127 Uiso 1 1 calc R . . C70 C 0.1201(3) 0.3095(4) -0.0894(3) 0.073(2) Uani 1 1 d . . . H70A H 0.1369 0.3477 -0.0953 0.110 Uiso 1 1 calc R . . H70B H 0.1023 0.2883 -0.1212 0.110 Uiso 1 1 calc R . . H70C H 0.1387 0.2731 -0.0682 0.110 Uiso 1 1 calc R . . C71 C 0.42267(19) 0.5991(4) 0.0609(3) 0.0482(16) Uani 1 1 d . . . C72 C 0.4526(2) 0.6273(3) 0.0454(3) 0.0473(16) Uani 1 1 d . B . H72 H 0.4457 0.6668 0.0235 0.057 Uiso 1 1 calc R . . C73 C 0.4923(2) 0.5991(3) 0.0611(3) 0.0528(18) Uani 1 1 d . . . C74 C 0.5011(2) 0.5403(3) 0.0923(3) 0.0542(19) Uani 1 1 d . B . H74 H 0.5282 0.5199 0.1030 0.065 Uiso 1 1 calc R . . C75 C 0.4722(2) 0.5104(3) 0.1084(3) 0.0495(16) Uani 1 1 d . . . C76 C 0.4326(2) 0.5403(4) 0.0920(3) 0.0528(17) Uani 1 1 d . B . H76 H 0.4119 0.5203 0.1022 0.063 Uiso 1 1 calc R . . C81 C 0.4831(3) 0.4452(4) 0.1429(3) 0.081(3) Uani 1 1 d . B . C78 C 0.5510(9) 0.5705(15) 0.0313(13) 0.048(5) Uani 0.484(14) 1 d P B 1 H78A H 0.5597 0.5290 0.0532 0.072 Uiso 0.484(14) 1 calc PR B 1 H78B H 0.5754 0.5903 0.0264 0.072 Uiso 0.484(14) 1 calc PR B 1 H78C H 0.5299 0.5562 -0.0009 0.072 Uiso 0.484(14) 1 calc PR B 1 C42 C -0.0004(5) 0.5642(14) -0.1724(7) 0.104(8) Uani 0.650(17) 1 d P C 1 H42A H 0.0138 0.5194 -0.1591 0.156 Uiso 0.650(17) 1 calc PR C 1 H42B H -0.0019 0.5709 -0.2065 0.156 Uiso 0.650(17) 1 calc PR C 1 H42C H -0.0288 0.5630 -0.1726 0.156 Uiso 0.650(17) 1 calc PR C 1 C79 C 0.5659(4) 0.6533(7) 0.1057(6) 0.050(4) Uani 0.484(14) 1 d P B 1 H79A H 0.5748 0.6130 0.1287 0.074 Uiso 0.484(14) 1 calc PR B 1 H79B H 0.5544 0.6906 0.1202 0.074 Uiso 0.484(14) 1 calc PR B 1 H79C H 0.5900 0.6718 0.0996 0.074 Uiso 0.484(14) 1 calc PR B 1 C84 C 0.5238(6) 0.4210(9) 0.1636(7) 0.085(6) Uani 0.632(16) 1 d P B 1 H84A H 0.5251 0.3795 0.1845 0.127 Uiso 0.632(16) 1 calc PR B 1 H84B H 0.5418 0.4586 0.1840 0.127 Uiso 0.632(16) 1 calc PR B 1 H84C H 0.5334 0.4077 0.1371 0.127 Uiso 0.632(16) 1 calc PR B 1 C82 C 0.4687(6) 0.4698(9) 0.1915(6) 0.096(6) Uani 0.632(16) 1 d P B 1 H82A H 0.4398 0.4875 0.1781 0.144 Uiso 0.632(16) 1 calc PR B 1 H82B H 0.4875 0.5073 0.2110 0.144 Uiso 0.632(16) 1 calc PR B 1 H82C H 0.4707 0.4286 0.2128 0.144 Uiso 0.632(16) 1 calc PR B 1 C40 C 0.0250(5) 0.6088(10) -0.0832(6) 0.094(6) Uani 0.650(17) 1 d P C 1 H40A H 0.0367 0.5614 -0.0726 0.140 Uiso 0.650(17) 1 calc PR C 1 H40B H -0.0035 0.6108 -0.0837 0.140 Uiso 0.650(17) 1 calc PR C 1 H40C H 0.0425 0.6443 -0.0598 0.140 Uiso 0.650(17) 1 calc PR C 1 C41 C 0.0066(5) 0.6965(11) -0.1545(8) 0.104(7) Uani 0.650(17) 1 d P C 1 H41A H 0.0242 0.7312 -0.1305 0.155 Uiso 0.650(17) 1 calc PR C 1 H41B H -0.0219 0.6984 -0.1551 0.155 Uiso 0.650(17) 1 calc PR C 1 H41C H 0.0061 0.7075 -0.1877 0.155 Uiso 0.650(17) 1 calc PR C 1 C83 C 0.4498(7) 0.3851(9) 0.1174(8) 0.103(7) Uani 0.632(16) 1 d P B 1 H83A H 0.4217 0.4060 0.1034 0.154 Uiso 0.632(16) 1 calc PR B 1 H83B H 0.4508 0.3492 0.1422 0.154 Uiso 0.632(16) 1 calc PR B 1 H83C H 0.4563 0.3628 0.0907 0.154 Uiso 0.632(16) 1 calc PR B 1 C84' C 0.5296(8) 0.4660(14) 0.1809(9) 0.068(7) Uani 0.368(16) 1 d P B 2 H84D H 0.5452 0.4873 0.1624 0.102 Uiso 0.368(16) 1 calc PR B 2 H84E H 0.5442 0.4232 0.1981 0.102 Uiso 0.368(16) 1 calc PR B 2 H84F H 0.5278 0.5001 0.2054 0.102 Uiso 0.368(16) 1 calc PR B 2 C83' C 0.5008(7) 0.3825(10) 0.1076(8) 0.060(7) Uani 0.368(16) 1 d P B 2 H1 H 0.5207 0.4059 0.0960 0.090 Uiso 0.368(16) 1 calc PR B 2 H3 H 0.4767 0.3656 0.0789 0.090 Uiso 0.368(16) 1 calc PR B 2 H5 H 0.5145 0.3421 0.1289 0.090 Uiso 0.368(16) 1 calc PR B 2 C82' C 0.4578(9) 0.4156(17) 0.1564(15) 0.100(16) Uani 0.368(16) 1 d P B 2 H82D H 0.4713 0.3752 0.1778 0.151 Uiso 0.368(16) 1 calc PR B 2 H82E H 0.4341 0.3986 0.1273 0.151 Uiso 0.368(16) 1 calc PR B 2 H82F H 0.4477 0.4492 0.1751 0.151 Uiso 0.368(16) 1 calc PR B 2 C40' C -0.0024(8) 0.6442(19) -0.2049(13) 0.109(14) Uani 0.350(17) 1 d P C 2 H40D H 0.0058 0.6915 -0.2121 0.163 Uiso 0.350(17) 1 calc PR C 2 H40E H -0.0328 0.6429 -0.2138 0.163 Uiso 0.350(17) 1 calc PR C 2 H40F H 0.0055 0.6086 -0.2243 0.163 Uiso 0.350(17) 1 calc PR C 2 C42' C 0.0043(11) 0.5642(14) -0.1430(16) 0.080(11) Uani 0.350(17) 1 d P C 2 H42D H 0.0182 0.5275 -0.1551 0.119 Uiso 0.350(17) 1 calc PR C 2 H42E H -0.0249 0.5688 -0.1660 0.119 Uiso 0.350(17) 1 calc PR C 2 H42F H 0.0052 0.5508 -0.1100 0.119 Uiso 0.350(17) 1 calc PR C 2 C41' C 0.0109(10) 0.6888(17) -0.1179(16) 0.097(12) Uani 0.350(17) 1 d P C 2 H41D H 0.0304 0.7280 -0.1148 0.145 Uiso 0.350(17) 1 calc PR C 2 H41E H 0.0114 0.6765 -0.0849 0.145 Uiso 0.350(17) 1 calc PR C 2 H41F H -0.0175 0.7032 -0.1395 0.145 Uiso 0.350(17) 1 calc PR C 2 O7 O 0.2500 0.7500 0.0000 0.0408(14) Uani 1 2 d S . . C14' C 0.4015(7) 0.6481(9) 0.2856(6) 0.055(6) Uani 0.396(15) 1 d P A 2 H14D H 0.3728 0.6557 0.2838 0.083 Uiso 0.396(15) 1 calc PR A 2 H14E H 0.4205 0.6814 0.3095 0.083 Uiso 0.396(15) 1 calc PR A 2 H14F H 0.4101 0.5993 0.2965 0.083 Uiso 0.396(15) 1 calc PR A 2 C13' C 0.4418(6) 0.6527(11) 0.2306(8) 0.061(6) Uani 0.396(15) 1 d P A 2 H13D H 0.4609 0.6835 0.2565 0.092 Uiso 0.396(15) 1 calc PR A 2 H13E H 0.4430 0.6649 0.1984 0.092 Uiso 0.396(15) 1 calc PR A 2 H13F H 0.4502 0.6030 0.2386 0.092 Uiso 0.396(15) 1 calc PR A 2 C12' C 0.3883(7) 0.7164(13) 0.2430(9) 0.120(10) Uani 0.604(15) 1 d P A 1 H12D H 0.4113 0.7432 0.2674 0.181 Uiso 0.604(15) 1 calc PR A 1 H12E H 0.3688 0.7008 0.2582 0.181 Uiso 0.604(15) 1 calc PR A 1 H12F H 0.3734 0.7468 0.2143 0.181 Uiso 0.604(15) 1 calc PR A 1 C77 C 0.5319(5) 0.6285(8) 0.0559(7) 0.037(4) Uani 0.484(14) 1 d P B 1 C79' C 0.4938(5) 0.6434(9) -0.0256(6) 0.069(5) Uani 0.516(14) 1 d P B 2 H79D H 0.4689 0.6727 -0.0320 0.104 Uiso 0.516(14) 1 calc PR B 2 H79E H 0.4855 0.5969 -0.0413 0.104 Uiso 0.516(14) 1 calc PR B 2 H79F H 0.5124 0.6668 -0.0393 0.104 Uiso 0.516(14) 1 calc PR B 2 C77' C 0.5172(6) 0.6336(11) 0.0313(8) 0.054(5) Uani 0.516(14) 1 d P B 2 C80 C 0.5204(6) 0.6925(10) 0.0246(9) 0.066(6) Uani 0.484(14) 1 d P B 1 H80A H 0.4986 0.6806 -0.0077 0.098 Uiso 0.484(14) 1 calc PR B 1 H80B H 0.5452 0.7107 0.0197 0.098 Uiso 0.484(14) 1 calc PR B 1 H80C H 0.5098 0.7288 0.0409 0.098 Uiso 0.484(14) 1 calc PR B 1 C78' C 0.5299(9) 0.7085(15) 0.0539(8) 0.125(13) Uani 0.516(14) 1 d P B 2 H78D H 0.5450 0.7045 0.0900 0.188 Uiso 0.516(14) 1 calc PR B 2 H78E H 0.5048 0.7375 0.0468 0.188 Uiso 0.516(14) 1 calc PR B 2 H78F H 0.5482 0.7310 0.0392 0.188 Uiso 0.516(14) 1 calc PR B 2 C80' C 0.5538(14) 0.587(3) 0.0388(18) 0.14(2) Uani 0.516(14) 1 d P B 2 H80D H 0.5688 0.5780 0.0744 0.216 Uiso 0.516(14) 1 calc PR B 2 H80E H 0.5727 0.6100 0.0254 0.216 Uiso 0.516(14) 1 calc PR B 2 H80F H 0.5441 0.5416 0.0216 0.216 Uiso 0.516(14) 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 0.02629(16) 0.03012(16) 0.03187(17) 0.00124(13) 0.01341(13) -0.00572(12) La2 0.02280(16) 0.03293(17) 0.0426(2) 0.00258(14) 0.01295(14) -0.00064(12) O1 0.033(3) 0.181(7) 0.048(3) 0.066(4) -0.004(2) -0.028(3) O2 0.059(3) 0.074(3) 0.104(4) -0.062(3) 0.061(3) -0.036(3) O3 0.113(5) 0.039(3) 0.074(4) -0.002(3) -0.058(4) -0.011(3) O4 0.278(10) 0.039(3) 0.123(5) 0.028(3) 0.169(7) 0.034(4) O5 0.060(3) 0.033(2) 0.060(3) -0.003(2) 0.034(2) -0.018(2) O6 0.029(2) 0.075(4) 0.107(5) 0.013(3) 0.024(3) 0.018(2) C25 0.057(4) 0.062(4) 0.065(5) -0.001(4) 0.039(4) 0.014(4) C26 0.068(6) 0.094(7) 0.115(8) -0.026(6) 0.064(6) -0.013(5) C27 0.097(7) 0.097(7) 0.092(7) 0.033(6) 0.069(6) 0.035(6) C28 0.065(5) 0.086(6) 0.063(5) -0.004(4) 0.041(4) 0.020(4) C1 0.038(4) 0.132(8) 0.038(4) 0.039(4) 0.007(3) -0.024(4) C2 0.040(4) 0.124(8) 0.034(4) -0.001(4) 0.015(3) -0.028(4) C3 0.038(4) 0.088(6) 0.045(4) -0.008(4) 0.022(3) -0.017(4) C4 0.037(3) 0.072(5) 0.036(3) 0.021(3) 0.003(3) -0.008(3) C5 0.044(4) 0.077(5) 0.046(4) 0.030(4) -0.002(3) -0.019(4) C6 0.041(4) 0.093(6) 0.054(4) 0.047(4) -0.001(3) -0.023(4) C7 0.052(5) 0.084(6) 0.085(6) -0.015(5) 0.025(5) -0.014(4) C8 0.153(13) 0.162(13) 0.158(13) -0.090(11) 0.093(11) -0.054(10) C9 0.059(6) 0.060(6) 0.169(11) -0.005(6) 0.015(6) 0.002(4) C10 0.057(5) 0.084(7) 0.150(10) 0.031(7) 0.042(6) -0.005(5) C11 0.055(5) 0.065(5) 0.080(6) 0.034(5) -0.023(4) -0.022(4) C12 0.086(18) 0.046(14) 0.082(17) 0.039(13) -0.002(13) -0.006(12) C13 0.062(10) 0.110(14) 0.093(13) 0.024(11) -0.002(9) -0.041(9) C14 0.083(11) 0.076(10) 0.049(8) 0.013(7) -0.027(8) -0.014(8) C15 0.038(3) 0.060(4) 0.059(4) -0.035(3) 0.029(3) -0.019(3) C16 0.046(4) 0.064(4) 0.030(3) -0.010(3) 0.010(3) -0.012(3) C17 0.053(4) 0.048(4) 0.036(3) 0.002(3) 0.008(3) 0.003(3) C18 0.053(4) 0.043(4) 0.045(4) -0.005(3) 0.015(3) 0.013(3) C19 0.039(3) 0.047(4) 0.042(4) -0.004(3) 0.017(3) 0.006(3) C20 0.041(4) 0.041(3) 0.067(5) -0.016(3) 0.030(3) -0.006(3) C21 0.096(7) 0.044(4) 0.066(5) 0.018(4) 0.023(5) 0.011(4) C22 0.116(9) 0.087(7) 0.121(9) 0.046(7) 0.059(8) 0.000(6) C23 0.107(8) 0.079(7) 0.080(7) 0.034(5) 0.007(6) 0.023(6) C24 0.098(7) 0.045(5) 0.108(8) 0.005(5) 0.020(6) 0.003(5) C29 0.063(5) 0.031(3) 0.040(4) 0.004(3) -0.025(3) -0.010(3) C30 0.030(3) 0.051(4) 0.061(5) 0.010(3) -0.007(3) -0.004(3) C31 0.037(3) 0.049(4) 0.029(3) 0.005(3) 0.004(3) 0.004(3) C32 0.038(3) 0.043(3) 0.030(3) -0.004(2) 0.007(3) -0.007(3) C33 0.045(4) 0.053(4) 0.033(3) -0.003(3) 0.011(3) 0.000(3) C34 0.076(5) 0.043(4) 0.027(3) -0.008(3) 0.004(3) 0.006(3) C35 0.052(4) 0.079(5) 0.047(4) 0.004(4) 0.019(3) 0.016(4) C36 0.269(18) 0.083(8) 0.118(10) 0.024(7) 0.125(12) 0.083(10) C37 0.065(7) 0.248(17) 0.107(9) -0.011(10) 0.052(7) -0.008(9) C38 0.103(8) 0.132(9) 0.053(5) -0.007(5) 0.035(5) 0.025(7) C39 0.057(5) 0.092(7) 0.091(7) -0.015(5) 0.042(5) 0.002(5) C43 0.136(8) 0.036(4) 0.071(6) 0.006(4) 0.082(6) 0.013(5) C44 0.073(5) 0.048(4) 0.093(6) 0.007(4) 0.059(5) 0.007(4) C45 0.058(5) 0.064(5) 0.047(4) 0.010(3) 0.028(4) 0.010(4) C46 0.058(5) 0.091(6) 0.057(5) 0.030(4) 0.035(4) 0.016(4) C47 0.056(5) 0.084(6) 0.076(6) 0.030(5) 0.013(4) 0.004(4) C48 0.140(9) 0.054(5) 0.042(4) 0.017(4) 0.025(5) 0.023(5) C49 0.077(7) 0.099(8) 0.080(7) 0.019(6) 0.003(5) 0.002(6) C50 0.128(13) 0.215(19) 0.164(15) -0.032(14) -0.033(11) -0.049(13) C51 0.27(2) 0.29(3) 0.063(9) -0.025(12) 0.026(12) 0.06(2) C52 0.32(3) 0.097(10) 0.206(18) 0.074(11) -0.180(18) -0.053(13) C53 0.072(7) 0.126(11) 0.168(14) 0.067(10) 0.010(8) 0.008(7) C54 0.066(7) 0.117(10) 0.251(18) 0.052(11) 0.052(9) -0.014(7) C55 0.142(14) 0.159(15) 0.193(18) -0.045(14) -0.019(13) -0.005(12) C56 0.079(9) 0.197(17) 0.26(2) 0.086(15) 0.027(11) 0.066(10) C57 0.042(3) 0.030(3) 0.059(4) -0.003(3) 0.029(3) -0.014(2) C58 0.046(4) 0.039(3) 0.045(4) -0.002(3) 0.025(3) -0.013(3) C59 0.035(3) 0.043(3) 0.047(4) 0.004(3) 0.024(3) -0.003(3) C60 0.035(3) 0.034(3) 0.051(4) 0.006(3) 0.017(3) -0.010(2) C61 0.039(3) 0.037(3) 0.042(3) 0.004(3) 0.016(3) -0.009(2) C62 0.049(4) 0.035(3) 0.045(4) 0.003(3) 0.024(3) -0.009(3) C63 0.049(4) 0.057(4) 0.046(4) 0.002(3) 0.029(3) -0.011(3) C64 0.080(6) 0.075(6) 0.057(5) 0.017(4) 0.028(4) 0.004(5) C65 0.078(6) 0.104(7) 0.046(4) -0.011(4) 0.037(4) -0.036(5) C66 0.063(5) 0.066(5) 0.072(5) 0.003(4) 0.046(4) -0.016(4) C67 0.053(4) 0.043(4) 0.047(4) 0.005(3) 0.010(3) -0.014(3) C68 0.069(6) 0.085(6) 0.073(6) 0.018(5) 0.001(5) -0.008(5) C69 0.100(7) 0.075(6) 0.061(5) -0.002(4) 0.009(5) -0.052(5) C70 0.092(7) 0.058(5) 0.059(5) -0.013(4) 0.017(5) -0.017(4) C71 0.027(3) 0.049(4) 0.069(5) 0.007(3) 0.019(3) 0.006(3) C72 0.042(4) 0.042(4) 0.060(4) 0.010(3) 0.021(3) 0.005(3) C73 0.041(4) 0.036(3) 0.094(6) 0.004(3) 0.040(4) 0.001(3) C74 0.026(3) 0.039(3) 0.093(6) 0.000(3) 0.017(3) 0.001(3) C75 0.049(4) 0.037(3) 0.059(4) -0.001(3) 0.017(3) -0.002(3) C76 0.046(4) 0.053(4) 0.069(5) 0.008(3) 0.033(4) -0.002(3) C81 0.099(7) 0.048(5) 0.071(6) 0.012(4) 0.004(5) 0.005(5) C78 0.034(10) 0.049(9) 0.066(13) -0.003(9) 0.026(9) 0.010(7) C42 0.031(7) 0.20(2) 0.091(14) -0.029(14) 0.029(9) -0.027(9) C79 0.027(7) 0.038(7) 0.088(12) -0.012(7) 0.028(7) -0.010(5) C84 0.106(13) 0.067(11) 0.081(12) 0.035(9) 0.036(10) 0.038(10) C82 0.178(19) 0.064(10) 0.076(11) 0.018(8) 0.082(12) 0.006(10) C40 0.095(12) 0.131(15) 0.082(11) 0.020(10) 0.066(10) 0.034(10) C41 0.077(11) 0.150(18) 0.094(14) 0.039(13) 0.044(11) 0.055(11) C83 0.17(2) 0.056(9) 0.099(14) 0.007(9) 0.064(14) -0.014(10) C84' 0.073(16) 0.053(15) 0.057(14) 0.013(11) 0.001(11) -0.008(12) C83' 0.075(15) 0.039(10) 0.075(15) 0.009(9) 0.039(12) 0.014(9) C82' 0.071(17) 0.09(2) 0.16(4) 0.09(3) 0.07(2) 0.020(16) C40' 0.039(14) 0.14(3) 0.13(3) 0.05(2) 0.016(16) -0.004(16) C42' 0.070(19) 0.043(13) 0.15(4) -0.026(18) 0.07(2) -0.010(12) C41' 0.08(2) 0.09(2) 0.14(3) -0.04(2) 0.05(2) -0.024(16) O7 0.021(3) 0.030(3) 0.074(4) 0.009(3) 0.021(3) -0.003(2) C14' 0.076(14) 0.043(10) 0.035(9) 0.002(7) 0.009(9) -0.019(9) C13' 0.044(11) 0.064(13) 0.066(15) 0.005(11) 0.010(10) -0.007(9) C12' 0.089(14) 0.102(19) 0.11(2) -0.061(16) -0.027(14) 0.006(14) C77 0.031(9) 0.034(7) 0.052(10) 0.015(8) 0.022(7) 0.012(6) C79' 0.085(12) 0.069(10) 0.071(11) 0.004(8) 0.049(10) -0.017(9) C77' 0.039(10) 0.064(11) 0.060(12) 0.017(10) 0.019(8) 0.002(8) C80 0.065(12) 0.049(10) 0.105(17) 0.026(11) 0.057(12) 0.004(8) C78' 0.18(3) 0.14(2) 0.065(14) -0.028(14) 0.053(16) -0.11(2) C80' 0.11(3) 0.21(5) 0.14(4) 0.10(3) 0.08(3) 0.05(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 La1 O5 2.181(4) . ? La1 O1 2.381(5) . ? La1 O2 2.397(4) . ? La1 O3 2.457(5) . ? La1 O4 2.465(5) . ? La1 O7 2.6628(3) . ? La1 C43 2.964(7) . ? La1 C29 3.136(6) . ? La1 La2 3.8031(5) 7_565 ? La1 La2 3.8124(4) . ? La2 O6 2.178(4) . ? La2 O3 2.397(5) 7_565 ? La2 O4 2.402(5) 7_565 ? La2 O2 2.468(5) . ? La2 O1 2.478(5) . ? La2 O7 2.7219(3) . ? La2 C15 3.057(6) . ? La2 C1 3.085(6) . ? La2 La1 3.8031(5) 7_565 ? O1 C1 1.378(8) . ? O2 C15 1.370(7) . ? O3 C29 1.361(7) . ? O3 La2 2.397(5) 7_565 ? O4 C43 1.366(8) . ? O4 La2 2.402(5) 7_565 ? O5 C57 1.361(6) . ? O6 C71 1.343(7) . ? C25 C28 1.528(10) . ? C25 C27 1.539(11) . ? C25 C19 1.541(9) . ? C25 C26 1.552(11) . ? C1 C6 1.387(11) . ? C1 C2 1.397(13) . ? C2 C3 1.408(11) . ? C3 C4 1.391(9) . ? C3 C7 1.532(12) . ? C4 C5 1.386(10) . ? C5 C6 1.405(9) . ? C5 C11 1.536(11) . ? C7 C10 1.517(12) . ? C7 C9 1.522(13) . ? C7 C8 1.565(14) . ? C11 C12' 1.30(2) . ? C11 C13' 1.32(2) . ? C11 C14 1.538(15) . ? C11 C13 1.65(2) . ? C11 C12 1.71(3) . ? C11 C14' 1.71(2) . ? C15 C20 1.386(9) . ? C15 C16 1.399(10) . ? C16 C17 1.378(10) . ? C17 C18 1.399(10) . ? C17 C21 1.529(10) . ? C18 C19 1.374(9) . ? C19 C20 1.399(8) . ? C21 C23 1.534(12) . ? C21 C24 1.537(12) . ? C21 C22 1.541(14) . ? C29 C30 1.364(11) . ? C29 C34 1.388(11) . ? C30 C31 1.381(9) . ? C31 C32 1.394(9) . ? C31 C35 1.537(10) . ? C32 C33 1.395(9) . ? C33 C34 1.392(9) . ? C33 C39 1.537(10) . ? C35 C38 1.484(11) . ? C35 C36 1.500(13) . ? C35 C37 1.609(13) . ? C39 C42' 1.32(3) . ? C39 C41 1.46(2) . ? C39 C41' 1.50(3) . ? C39 C42 1.52(2) . ? C39 C40 1.666(16) . ? C39 C40' 1.79(3) . ? C43 C44 1.356(12) . ? C43 C48 1.377(13) . ? C44 C45 1.376(10) . ? C45 C46 1.370(11) . ? C45 C49 1.534(12) . ? C46 C47 1.416(11) . ? C47 C48 1.386(13) . ? C47 C53 1.518(15) . ? C49 C52 1.419(16) . ? C49 C50 1.478(18) . ? C49 C51 1.58(2) . ? C53 C56 1.440(16) . ? C53 C54 1.484(18) . ? C53 C55 1.64(2) . ? C57 C62 1.381(9) . ? C57 C58 1.394(8) . ? C58 C59 1.379(8) . ? C59 C60 1.380(9) . ? C59 C63 1.552(8) . ? C60 C61 1.389(8) . ? C61 C62 1.403(8) . ? C61 C67 1.536(9) . ? C63 C65 1.522(10) . ? C63 C64 1.523(11) . ? C63 C66 1.534(9) . ? C67 C69 1.520(10) . ? C67 C68 1.525(11) . ? C67 C70 1.541(12) . ? C71 C72 1.384(9) . ? C71 C76 1.386(9) . ? C72 C73 1.374(9) . ? C73 C74 1.390(10) . ? C73 C77 1.535(17) . ? C73 C77' 1.578(19) . ? C74 C75 1.374(10) . ? C75 C76 1.385(9) . ? C75 C81 1.539(10) . ? C81 C82' 1.22(2) . ? C81 C84 1.378(18) . ? C81 C83 1.58(2) . ? C81 C84' 1.61(2) . ? C81 C82 1.731(18) . ? C81 C83' 1.82(2) . ? C78 C77 1.58(3) . ? C79 C77 1.55(2) . ? O7 La1 2.6628(3) 7_565 ? O7 La2 2.7219(3) 7_565 ? C77 C80 1.47(2) . ? C79' C77' 1.55(3) . ? C77' C80' 1.49(4) . ? C77' C78' 1.55(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 La1 O1 105.4(2) . . ? O5 La1 O2 104.38(17) . . ? O1 La1 O2 74.8(2) . . ? O5 La1 O3 123.37(18) . . ? O1 La1 O3 130.7(2) . . ? O2 La1 O3 85.8(3) . . ? O5 La1 O4 124.99(18) . . ? O1 La1 O4 87.3(3) . . ? O2 La1 O4 130.45(19) . . ? O3 La1 O4 71.6(2) . . ? O5 La1 O7 166.82(12) . . ? O1 La1 O7 65.58(13) . . ? O2 La1 O7 64.68(12) . . ? O3 La1 O7 65.14(14) . . ? O4 La1 O7 65.84(16) . . ? O5 La1 C43 98.81(19) . . ? O1 La1 C43 87.3(3) . . ? O2 La1 C43 153.7(2) . . ? O3 La1 C43 91.7(3) . . ? O4 La1 C43 27.20(18) . . ? O7 La1 C43 90.56(16) . . ? O5 La1 C29 99.59(17) . . ? O1 La1 C29 151.37(19) . . ? O2 La1 C29 85.7(2) . . ? O3 La1 C29 24.52(16) . . ? O4 La1 C29 89.7(2) . . ? O7 La1 C29 87.28(13) . . ? C43 La1 C29 102.6(3) . . ? O5 La1 La2 147.36(13) . 7_565 ? O1 La1 La2 101.39(18) . 7_565 ? O2 La1 La2 100.33(15) . 7_565 ? O3 La1 La2 37.85(12) . 7_565 ? O4 La1 La2 38.02(12) . 7_565 ? O7 La1 La2 45.701(7) . 7_565 ? C43 La1 La2 63.95(14) . 7_565 ? C29 La1 La2 61.20(12) . 7_565 ? O5 La1 La2 121.34(12) . . ? O1 La1 La2 39.24(13) . . ? O2 La1 La2 39.07(11) . . ? O3 La1 La2 101.56(19) . . ? O4 La1 La2 102.4(2) . . ? O7 La1 La2 45.557(7) . . ? C43 La1 La2 116.8(2) . . ? C29 La1 La2 114.48(17) . . ? La2 La1 La2 91.258(9) 7_565 . ? O6 La2 O3 106.1(2) . 7_565 ? O6 La2 O4 111.0(3) . 7_565 ? O3 La2 O4 73.7(2) 7_565 7_565 ? O6 La2 O2 126.1(2) . . ? O3 La2 O2 127.8(2) 7_565 . ? O4 La2 O2 85.1(3) 7_565 . ? O6 La2 O1 119.3(2) . . ? O3 La2 O1 85.5(3) 7_565 . ? O4 La2 O1 129.1(2) 7_565 . ? O2 La2 O1 71.88(18) . . ? O6 La2 O7 170.80(15) . . ? O3 La2 O7 64.93(15) 7_565 . ? O4 La2 O7 65.68(18) 7_565 . ? O2 La2 O7 62.88(12) . . ? O1 La2 O7 63.43(14) . . ? O6 La2 C15 100.9(2) . . ? O3 La2 C15 151.48(19) 7_565 . ? O4 La2 C15 88.2(2) 7_565 . ? O2 La2 C15 26.03(16) . . ? O1 La2 C15 89.4(2) . . ? O7 La2 C15 87.71(13) . . ? O6 La2 C1 93.6(2) . . ? O3 La2 C1 89.8(3) 7_565 . ? O4 La2 C1 153.1(2) 7_565 . ? O2 La2 C1 88.87(19) . . ? O1 La2 C1 25.85(19) . . ? O7 La2 C1 88.31(17) . . ? C15 La2 C1 97.7(2) . . ? O6 La2 La1 127.41(15) . 7_565 ? O3 La2 La1 38.97(12) 7_565 7_565 ? O4 La2 La1 39.20(13) 7_565 7_565 ? O2 La2 La1 98.06(14) . 7_565 ? O1 La2 La1 98.97(18) . 7_565 ? O7 La2 La1 44.440(7) . 7_565 ? C15 La2 La1 115.02(15) . 7_565 ? C1 La2 La1 116.6(2) . 7_565 ? O6 La2 La1 143.46(15) . . ? O3 La2 La1 99.82(19) 7_565 . ? O4 La2 La1 100.7(2) 7_565 . ? O2 La2 La1 37.74(10) . . ? O1 La2 La1 37.42(11) . . ? O7 La2 La1 44.302(7) . . ? C15 La2 La1 61.38(11) . . ? C1 La2 La1 60.75(13) . . ? La1 La2 La1 88.742(9) 7_565 . ? C1 O1 La1 139.5(5) . . ? C1 O1 La2 102.5(4) . . ? La1 O1 La2 103.34(19) . . ? C15 O2 La1 140.8(4) . . ? C15 O2 La2 101.7(4) . . ? La1 O2 La2 103.19(17) . . ? C29 O3 La2 143.1(5) . 7_565 ? C29 O3 La1 106.9(4) . . ? La2 O3 La1 103.18(19) 7_565 . ? C43 O4 La2 150.6(7) . 7_565 ? C43 O4 La1 97.2(4) . . ? La2 O4 La1 102.78(19) 7_565 . ? C57 O5 La1 165.1(4) . . ? C71 O6 La2 178.0(5) . . ? C28 C25 C27 108.7(7) . . ? C28 C25 C19 112.0(6) . . ? C27 C25 C19 109.1(6) . . ? C28 C25 C26 108.3(6) . . ? C27 C25 C26 109.8(8) . . ? C19 C25 C26 108.9(6) . . ? O1 C1 C6 118.6(8) . . ? O1 C1 C2 121.2(7) . . ? C6 C1 C2 120.1(7) . . ? O1 C1 La2 51.7(3) . . ? C6 C1 La2 95.5(4) . . ? C2 C1 La2 119.4(6) . . ? C1 C2 C3 121.4(7) . . ? C4 C3 C2 116.6(7) . . ? C4 C3 C7 123.4(7) . . ? C2 C3 C7 120.0(7) . . ? C5 C4 C3 123.5(6) . . ? C4 C5 C6 118.6(7) . . ? C4 C5 C11 122.6(6) . . ? C6 C5 C11 118.8(7) . . ? C1 C6 C5 119.8(8) . . ? C10 C7 C9 108.1(9) . . ? C10 C7 C3 110.6(7) . . ? C9 C7 C3 112.3(7) . . ? C10 C7 C8 107.7(9) . . ? C9 C7 C8 106.8(10) . . ? C3 C7 C8 111.2(9) . . ? C12' C11 C13' 127.0(15) . . ? C12' C11 C5 111.7(11) . . ? C13' C11 C5 117.7(14) . . ? C12' C11 C14 121.5(15) . . ? C13' C11 C14 56.2(12) . . ? C5 C11 C14 110.1(8) . . ? C12' C11 C13 109.2(17) . . ? C13' C11 C13 43.4(11) . . ? C5 C11 C13 102.4(9) . . ? C14 C11 C13 99.5(12) . . ? C12' C11 C12 28(2) . . ? C13' C11 C12 108.0(15) . . ? C5 C11 C12 115.3(12) . . ? C14 C11 C12 133.3(13) . . ? C13 C11 C12 81.1(14) . . ? C12' C11 C14' 68.5(17) . . ? C13' C11 C14' 110.1(13) . . ? C5 C11 C14' 108.8(8) . . ? C14 C11 C14' 60.4(10) . . ? C13 C11 C14' 147.1(10) . . ? C12 C11 C14' 94.4(14) . . ? O2 C15 C20 118.6(6) . . ? O2 C15 C16 121.0(6) . . ? C20 C15 C16 120.3(6) . . ? O2 C15 La2 52.2(3) . . ? C20 C15 La2 88.2(4) . . ? C16 C15 La2 126.6(5) . . ? C17 C16 C15 120.5(6) . . ? C16 C17 C18 117.7(6) . . ? C16 C17 C21 121.4(7) . . ? C18 C17 C21 120.9(7) . . ? C19 C18 C17 123.3(6) . . ? C18 C19 C20 117.9(6) . . ? C18 C19 C25 123.9(6) . . ? C20 C19 C25 118.2(6) . . ? C15 C20 C19 120.2(6) . . ? C17 C21 C23 107.7(8) . . ? C17 C21 C24 108.9(6) . . ? C23 C21 C24 110.3(8) . . ? C17 C21 C22 112.2(7) . . ? C23 C21 C22 110.0(8) . . ? C24 C21 C22 107.8(9) . . ? O3 C29 C30 119.6(8) . . ? O3 C29 C34 120.5(8) . . ? C30 C29 C34 119.9(6) . . ? O3 C29 La1 48.5(3) . . ? C30 C29 La1 99.9(4) . . ? C34 C29 La1 118.9(5) . . ? C29 C30 C31 121.9(7) . . ? C30 C31 C32 117.8(6) . . ? C30 C31 C35 122.0(6) . . ? C32 C31 C35 120.2(6) . . ? C31 C32 C33 121.7(6) . . ? C34 C33 C32 118.2(6) . . ? C34 C33 C39 120.4(7) . . ? C32 C33 C39 121.3(6) . . ? C29 C34 C33 120.4(7) . . ? C38 C35 C36 116.6(9) . . ? C38 C35 C31 111.3(6) . . ? C36 C35 C31 108.8(7) . . ? C38 C35 C37 102.6(8) . . ? C36 C35 C37 108.1(9) . . ? C31 C35 C37 109.1(8) . . ? C42' C39 C41 129.8(18) . . ? C42' C39 C41' 120(2) . . ? C41 C39 C41' 40.6(15) . . ? C42' C39 C42 32.0(18) . . ? C41 C39 C42 116.6(14) . . ? C41' C39 C42 133.2(15) . . ? C42' C39 C33 117.8(15) . . ? C41 C39 C33 110.4(10) . . ? C41' C39 C33 115.1(13) . . ? C42 C39 C33 111.4(9) . . ? C42' C39 C40 73.8(19) . . ? C41 C39 C40 108.3(11) . . ? C41' C39 C40 68.0(18) . . ? C42 C39 C40 105.7(12) . . ? C33 C39 C40 103.3(8) . . ? C42' C39 C40' 94(2) . . ? C41 C39 C40' 61.7(14) . . ? C41' C39 C40' 100(2) . . ? C42 C39 C40' 63.8(14) . . ? C33 C39 C40' 103.4(11) . . ? C40 C39 C40' 153.3(12) . . ? C44 C43 O4 121.4(10) . . ? C44 C43 C48 120.2(7) . . ? O4 C43 C48 118.3(10) . . ? C44 C43 La1 108.6(6) . . ? O4 C43 La1 55.6(3) . . ? C48 C43 La1 100.9(6) . . ? C43 C44 C45 121.4(8) . . ? C46 C45 C44 118.1(7) . . ? C46 C45 C49 119.5(7) . . ? C44 C45 C49 122.4(8) . . ? C45 C46 C47 122.7(7) . . ? C48 C47 C46 116.0(8) . . ? C48 C47 C53 120.2(10) . . ? C46 C47 C53 123.8(9) . . ? C43 C48 C47 121.6(8) . . ? C52 C49 C50 117.1(13) . . ? C52 C49 C45 112.0(10) . . ? C50 C49 C45 111.7(11) . . ? C52 C49 C51 112.0(16) . . ? C50 C49 C51 96.3(13) . . ? C45 C49 C51 106.2(9) . . ? C56 C53 C54 111.4(14) . . ? C56 C53 C47 112.8(12) . . ? C54 C53 C47 113.6(11) . . ? C56 C53 C55 103.4(13) . . ? C54 C53 C55 105.2(13) . . ? C47 C53 C55 109.7(13) . . ? O5 C57 C62 119.2(6) . . ? O5 C57 C58 120.6(6) . . ? C62 C57 C58 120.2(5) . . ? C59 C58 C57 120.0(6) . . ? C58 C59 C60 119.4(6) . . ? C58 C59 C63 121.5(6) . . ? C60 C59 C63 119.1(5) . . ? C59 C60 C61 122.0(5) . . ? C60 C61 C62 117.9(6) . . ? C60 C61 C67 123.2(5) . . ? C62 C61 C67 118.9(5) . . ? C57 C62 C61 120.5(6) . . ? C65 C63 C64 108.6(7) . . ? C65 C63 C66 107.8(6) . . ? C64 C63 C66 109.0(6) . . ? C65 C63 C59 112.3(5) . . ? C64 C63 C59 109.4(6) . . ? C66 C63 C59 109.5(6) . . ? C69 C67 C68 107.2(7) . . ? C69 C67 C61 112.7(6) . . ? C68 C67 C61 110.2(6) . . ? C69 C67 C70 107.7(7) . . ? C68 C67 C70 109.4(7) . . ? C61 C67 C70 109.5(6) . . ? O6 C71 C72 120.4(6) . . ? O6 C71 C76 120.3(6) . . ? C72 C71 C76 119.3(6) . . ? C73 C72 C71 121.1(6) . . ? C72 C73 C74 117.8(6) . . ? C72 C73 C77 129.7(8) . . ? C74 C73 C77 111.8(8) . . ? C72 C73 C77' 109.9(9) . . ? C74 C73 C77' 131.2(9) . . ? C77 C73 C77' 26.2(6) . . ? C75 C74 C73 122.9(6) . . ? C74 C75 C76 117.7(6) . . ? C74 C75 C81 121.3(7) . . ? C76 C75 C81 121.0(7) . . ? C75 C76 C71 121.1(6) . . ? C82' C81 C84 116.3(15) . . ? C82' C81 C75 123.1(14) . . ? C84 C81 C75 120.3(11) . . ? C82' C81 C83 49(2) . . ? C84 C81 C83 114.0(13) . . ? C75 C81 C83 108.1(9) . . ? C82' C81 C84' 122(2) . . ? C84 C81 C84' 36.6(10) . . ? C75 C81 C84' 100.7(11) . . ? C83 C81 C84' 148.3(13) . . ? C82' C81 C82 53(2) . . ? C84 C81 C82 107.0(11) . . ? C75 C81 C82 104.0(8) . . ? C83 C81 C82 101.1(12) . . ? C84' C81 C82 84.0(13) . . ? C82' C81 C83' 109(2) . . ? C84 C81 C83' 61.7(12) . . ? C75 C81 C83' 101.7(9) . . ? C83 C81 C83' 67.1(11) . . ? C84' C81 C83' 94.8(15) . . ? C82 C81 C83' 154.0(10) . . ? La1 O7 La1 180.0 . 7_565 ? La1 O7 La2 89.859(10) . 7_565 ? La1 O7 La2 90.141(10) 7_565 7_565 ? La1 O7 La2 90.141(10) . . ? La1 O7 La2 89.859(10) 7_565 . ? La2 O7 La2 180.0 7_565 . ? C80 C77 C73 108.5(13) . . ? C80 C77 C79 105.1(15) . . ? C73 C77 C79 113.8(12) . . ? C80 C77 C78 110(2) . . ? C73 C77 C78 109.7(16) . . ? C79 C77 C78 109.3(15) . . ? C80' C77' C78' 113(3) . . ? C80' C77' C79' 107(2) . . ? C78' C77' C79' 107.1(17) . . ? C80' C77' C73 107(2) . . ? C78' C77' C73 105.6(16) . . ? C79' C77' C73 117.6(13) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.057 _refine_diff_density_min -1.111 _refine_diff_density_rms 0.156 #====END data_RH1NdHOAr.CIF _database_code_depnum_ccdc_archive 'CCDC 236332' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common rhNdHOAr _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C172 H263 Nd3 O13' _chemical_formula_weight 2971.54 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 15.9373(6) _cell_length_b 18.8756(7) _cell_length_c 29.4560(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.3130(10) _cell_angle_gamma 90.00 _cell_volume 8846.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 95126 _cell_measurement_theta_min 0.69 _cell_measurement_theta_max 28.30 _exptl_crystal_description prismatic _exptl_crystal_colour blue _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3158 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.721 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95126 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 0.69 _diffrn_reflns_theta_max 28.30 _reflns_number_total 41246 _reflns_number_gt 37195 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART/SAINT _computing_cell_refinement SMART/SAINT _computing_data_reduction SMART/SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0898P)^2^+20.6899P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.019(11) _refine_ls_number_reflns 41246 _refine_ls_number_parameters 853 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1478 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Nd1 Nd 0.75188(2) 0.585982(15) 0.776253(10) 0.02885(7) Uani 1 1 d . . . Nd2 Nd 0.692738(17) 0.397467(14) 0.794062(9) 0.02303(6) Uani 1 1 d . . . Nd3 Nd 0.802250(15) 0.451871(13) 0.689447(8) 0.01885(6) Uani 1 1 d . . . O1 O 0.6257(4) 0.6591(3) 0.7528(2) 0.0561(14) Uani 1 1 d . . . H1A H 0.6042 0.6426 0.7283 0.084 Uiso 1 1 calc R . . O2 O 0.7965(3) 0.6674(3) 0.82184(17) 0.0465(12) Uani 1 1 d . . . O3 O 0.5609(3) 0.3566(2) 0.78829(15) 0.0346(9) Uani 1 1 d . . . O4 O 0.7534(3) 0.3240(2) 0.84169(15) 0.0360(10) Uani 1 1 d . . . O5 O 0.6776(2) 0.3956(3) 0.64508(13) 0.0318(8) Uani 1 1 d . . . H5A H 0.6462 0.3765 0.6634 0.048 Uiso 1 1 calc R . . O6 O 0.8524(2) 0.4642(2) 0.62302(12) 0.0269(8) Uani 1 1 d . . . O7 O 0.6790(3) 0.5147(2) 0.82591(15) 0.0347(9) Uani 1 1 d . . . O8 O 0.7572(2) 0.3502(2) 0.72999(13) 0.0255(8) Uani 1 1 d . . . O9 O 0.8145(2) 0.5770(2) 0.70401(13) 0.0264(8) Uani 1 1 d . . . O10 O 0.6762(2) 0.48959(19) 0.72807(13) 0.0239(7) Uiso 1 1 d . . . O11 O 0.8207(2) 0.4722(2) 0.77494(12) 0.0240(8) Uani 1 1 d . . . O12 O 0.5657(3) 0.3309(3) 0.69957(16) 0.0441(11) Uani 1 1 d . . . H12 H 0.5586 0.3355 0.7274 0.053 Uiso 1 1 calc R . . O13 O 0.9467(2) 0.4092(2) 0.71021(14) 0.0315(9) Uani 1 1 d . . . C1 C 0.5924(5) 0.7274(4) 0.7604(3) 0.0468(16) Uiso 1 1 d . . . C2 C 0.5368(5) 0.7559(5) 0.7284(3) 0.0534(18) Uiso 1 1 d . . . H2A H 0.5187 0.7301 0.7019 0.064 Uiso 1 1 calc R . . C3 C 0.5075(6) 0.8243(5) 0.7361(3) 0.062(2) Uiso 1 1 d . . . C4 C 0.5331(6) 0.8596(6) 0.7754(3) 0.065(2) Uiso 1 1 d . . . H4A H 0.5124 0.9061 0.7802 0.078 Uiso 1 1 calc R . . C5 C 0.5877(6) 0.8300(5) 0.8080(3) 0.060(2) Uiso 1 1 d . . . C6 C 0.6212(5) 0.7638(5) 0.8000(3) 0.0559(19) Uiso 1 1 d . . . H6A H 0.6625 0.7435 0.8206 0.067 Uiso 1 1 calc R . . C7 C 0.4485(7) 0.8580(6) 0.6963(4) 0.080(3) Uiso 1 1 d . . . C8 C 0.5011(9) 0.8694(8) 0.6558(5) 0.102(4) Uiso 1 1 d . . . H8A H 0.4661 0.8900 0.6307 0.152 Uiso 1 1 calc R . . H8B H 0.5238 0.8239 0.6462 0.152 Uiso 1 1 calc R . . H8C H 0.5475 0.9017 0.6642 0.152 Uiso 1 1 calc R . . C9 C 0.3750(8) 0.8088(7) 0.6841(5) 0.091(3) Uiso 1 1 d . . . H9A H 0.3386 0.8303 0.6599 0.137 Uiso 1 1 calc R . . H9B H 0.3428 0.8009 0.7110 0.137 Uiso 1 1 calc R . . H9C H 0.3964 0.7634 0.6735 0.137 Uiso 1 1 calc R . . C10 C 0.4158(10) 0.9290(9) 0.7121(6) 0.117(5) Uiso 1 1 d . . . H10A H 0.3785 0.9496 0.6880 0.176 Uiso 1 1 calc R . . H10B H 0.4632 0.9611 0.7190 0.176 Uiso 1 1 calc R . . H10C H 0.3846 0.9221 0.7395 0.176 Uiso 1 1 calc R . . C11 C 0.6215(8) 0.8720(7) 0.8494(5) 0.088(3) Uiso 1 1 d . . . C12 C 0.7090(13) 0.9034(14) 0.8411(8) 0.174(8) Uiso 1 1 d . . . H12A H 0.7294 0.9304 0.8679 0.261 Uiso 1 1 calc R . . H12B H 0.7046 0.9347 0.8145 0.261 Uiso 1 1 calc R . . H12C H 0.7483 0.8648 0.8356 0.261 Uiso 1 1 calc R . . C13 C 0.6443(7) 0.8266(6) 0.8907(4) 0.076(3) Uiso 1 1 d . . . H13A H 0.5939 0.8024 0.9004 0.114 Uiso 1 1 calc R . . H13B H 0.6675 0.8566 0.9155 0.114 Uiso 1 1 calc R . . H13C H 0.6863 0.7913 0.8830 0.114 Uiso 1 1 calc R . . C14 C 0.5758(11) 0.9395(10) 0.8587(6) 0.129(5) Uiso 1 1 d . . . H14A H 0.5176 0.9287 0.8654 0.193 Uiso 1 1 calc R . . H14B H 0.5759 0.9703 0.8319 0.193 Uiso 1 1 calc R . . H14C H 0.6039 0.9637 0.8848 0.193 Uiso 1 1 calc R . . C15 C 0.8231(5) 0.6994(4) 0.8611(3) 0.0457(16) Uiso 1 1 d . . . C16 C 0.8014(5) 0.6741(5) 0.9021(3) 0.0561(19) Uiso 1 1 d . . . H16A H 0.7669 0.6331 0.9031 0.067 Uiso 1 1 calc R . . C17 C 0.8284(6) 0.7067(5) 0.9421(3) 0.065(2) Uiso 1 1 d . . . C18 C 0.8790(7) 0.7648(6) 0.9414(4) 0.078(3) Uiso 1 1 d . . . H18A H 0.8967 0.7871 0.9693 0.094 Uiso 1 1 calc R . . C19 C 0.9053(7) 0.7923(6) 0.9003(4) 0.073(3) Uiso 1 1 d . . . C20 C 0.8732(6) 0.7589(5) 0.8598(3) 0.063(2) Uiso 1 1 d . . . H20A H 0.8864 0.7779 0.8312 0.075 Uiso 1 1 calc R . . C21 C 0.7965(7) 0.6844(6) 0.9880(4) 0.078(3) Uiso 1 1 d . . . C22 C 0.8658(15) 0.6637(15) 1.0195(9) 0.189(10) Uiso 1 1 d . . . H22A H 0.9062 0.7028 1.0230 0.283 Uiso 1 1 calc R . . H22B H 0.8938 0.6219 1.0077 0.283 Uiso 1 1 calc R . . H22C H 0.8442 0.6525 1.0492 0.283 Uiso 1 1 calc R . . C23 C 0.7374(10) 0.6158(8) 0.9850(6) 0.115(5) Uiso 1 1 d . . . H23A H 0.7203 0.6037 1.0155 0.172 Uiso 1 1 calc R . . H23B H 0.7683 0.5760 0.9727 0.172 Uiso 1 1 calc R . . H23C H 0.6874 0.6257 0.9651 0.172 Uiso 1 1 calc R . . C24 C 0.7432(18) 0.7387(17) 1.0040(10) 0.219(12) Uiso 1 1 d . . . H24A H 0.7748 0.7831 1.0072 0.329 Uiso 1 1 calc R . . H24B H 0.7233 0.7249 1.0336 0.329 Uiso 1 1 calc R . . H24C H 0.6950 0.7453 0.9822 0.329 Uiso 1 1 calc R . . C25 C 0.9688(8) 0.8588(7) 0.9027(5) 0.089(3) Uiso 1 1 d . . . C26 C 0.9241(11) 0.9185(9) 0.9190(6) 0.123(5) Uiso 1 1 d . . . H26A H 0.9070 0.9086 0.9498 0.184 Uiso 1 1 calc R . . H26B H 0.8742 0.9274 0.8989 0.184 Uiso 1 1 calc R . . H26C H 0.9606 0.9603 0.9196 0.184 Uiso 1 1 calc R . . C27 C 1.0459(10) 0.8428(9) 0.9287(6) 0.114(5) Uiso 1 1 d . . . H27A H 1.0333 0.8316 0.9601 0.172 Uiso 1 1 calc R . . H27B H 1.0834 0.8839 0.9286 0.172 Uiso 1 1 calc R . . H27C H 1.0732 0.8020 0.9152 0.172 Uiso 1 1 calc R . . C28 C 0.9926(10) 0.8761(8) 0.8528(5) 0.109(4) Uiso 1 1 d . . . H28A H 1.0312 0.9166 0.8533 0.163 Uiso 1 1 calc R . . H28B H 0.9416 0.8878 0.8342 0.163 Uiso 1 1 calc R . . H28C H 1.0199 0.8348 0.8399 0.163 Uiso 1 1 calc R . . C29 C 0.5033(4) 0.3261(4) 0.8147(2) 0.0409(15) Uiso 1 1 d . . . C30 C 0.5183(6) 0.2595(5) 0.8336(3) 0.061(2) Uiso 1 1 d . . . H30A H 0.5676 0.2345 0.8265 0.073 Uiso 1 1 calc R . . C31 C 0.4629(7) 0.2280(6) 0.8629(4) 0.073(3) Uiso 1 1 d . . . C32 C 0.3901(6) 0.2648(6) 0.8700(4) 0.070(2) Uiso 1 1 d . . . H32A H 0.3488 0.2426 0.8872 0.084 Uiso 1 1 calc R . . C33 C 0.3733(6) 0.3343(5) 0.8531(3) 0.064(2) Uiso 1 1 d . . . C34 C 0.4329(5) 0.3641(5) 0.8252(3) 0.0537(18) Uiso 1 1 d . . . H34A H 0.4245 0.4106 0.8134 0.064 Uiso 1 1 calc R . . C35 C 0.4860(9) 0.1536(7) 0.8857(5) 0.091(3) Uiso 1 1 d . . . C36 C 0.5749(17) 0.1333(16) 0.8925(10) 0.217(12) Uiso 1 1 d . . . H36A H 0.5997 0.1294 0.8630 0.325 Uiso 1 1 calc R . . H36B H 0.5792 0.0876 0.9083 0.325 Uiso 1 1 calc R . . H36C H 0.6052 0.1695 0.9109 0.325 Uiso 1 1 calc R . . C37 C 0.450(2) 0.101(2) 0.8515(12) 0.274(17) Uiso 1 1 d . . . H37A H 0.4786 0.1054 0.8231 0.411 Uiso 1 1 calc R . . H37B H 0.3898 0.1098 0.8457 0.411 Uiso 1 1 calc R . . H37C H 0.4582 0.0527 0.8635 0.411 Uiso 1 1 calc R . . C38 C 0.4501(18) 0.1578(17) 0.9343(10) 0.216(12) Uiso 1 1 d . . . H38A H 0.3907 0.1714 0.9314 0.324 Uiso 1 1 calc R . . H38B H 0.4818 0.1931 0.9527 0.324 Uiso 1 1 calc R . . H38C H 0.4556 0.1114 0.9492 0.324 Uiso 1 1 calc R . . C39 C 0.2942(8) 0.3712(7) 0.8653(4) 0.085(3) Uiso 1 1 d . . . C40 C 0.3030(10) 0.3983(10) 0.9148(5) 0.118(5) Uiso 1 1 d . . . H40A H 0.3497 0.4321 0.9181 0.178 Uiso 1 1 calc R . . H40B H 0.3141 0.3582 0.9355 0.178 Uiso 1 1 calc R . . H40C H 0.2508 0.4218 0.9225 0.178 Uiso 1 1 calc R . . C41 C 0.2670(13) 0.4301(11) 0.8354(7) 0.151(7) Uiso 1 1 d . . . H41A H 0.3101 0.4672 0.8369 0.227 Uiso 1 1 calc R . . H41B H 0.2141 0.4495 0.8453 0.227 Uiso 1 1 calc R . . H41C H 0.2588 0.4130 0.8040 0.227 Uiso 1 1 calc R . . C42 C 0.2195(11) 0.3194(10) 0.8599(6) 0.132(6) Uiso 1 1 d . . . H42A H 0.2138 0.3024 0.8285 0.198 Uiso 1 1 calc R . . H42B H 0.1678 0.3437 0.8675 0.198 Uiso 1 1 calc R . . H42C H 0.2296 0.2790 0.8805 0.198 Uiso 1 1 calc R . . C43 C 0.7989(4) 0.2692(4) 0.8598(2) 0.0404(14) Uiso 1 1 d . . . C44 C 0.7835(6) 0.2455(5) 0.9032(3) 0.059(2) Uiso 1 1 d . . . H44A H 0.7412 0.2677 0.9196 0.071 Uiso 1 1 calc R . . C45 C 0.8293(7) 0.1896(7) 0.9230(4) 0.081(3) Uiso 1 1 d . . . C46 C 0.8941(8) 0.1617(7) 0.8984(5) 0.089(3) Uiso 1 1 d . . . H46A H 0.9290 0.1261 0.9123 0.107 Uiso 1 1 calc R . . C47 C 0.9100(6) 0.1829(5) 0.8552(3) 0.060(2) Uiso 1 1 d . . . C48 C 0.8626(5) 0.2381(4) 0.8368(3) 0.0455(16) Uiso 1 1 d . . . H48A H 0.8740 0.2552 0.8074 0.055 Uiso 1 1 calc R . . C49 C 0.8216(11) 0.1646(10) 0.9752(6) 0.121(5) Uiso 1 1 d . . . C50 C 0.7749(13) 0.2240(12) 1.0002(7) 0.152(7) Uiso 1 1 d . . . H50A H 0.7672 0.2093 1.0316 0.228 Uiso 1 1 calc R . . H50B H 0.7199 0.2324 0.9845 0.228 Uiso 1 1 calc R . . H50C H 0.8082 0.2676 1.0003 0.228 Uiso 1 1 calc R . . C51 C 0.9135(13) 0.1740(13) 1.0027(8) 0.167(8) Uiso 1 1 d . . . H51A H 0.9101 0.1572 1.0340 0.251 Uiso 1 1 calc R . . H51B H 0.9296 0.2242 1.0030 0.251 Uiso 1 1 calc R . . H51C H 0.9557 0.1463 0.9876 0.251 Uiso 1 1 calc R . . C52 C 0.7810(15) 0.0873(14) 0.9682(8) 0.183(9) Uiso 1 1 d . . . H52A H 0.7730 0.0659 0.9979 0.275 Uiso 1 1 calc R . . H52B H 0.8187 0.0575 0.9512 0.275 Uiso 1 1 calc R . . H52C H 0.7266 0.0914 0.9511 0.275 Uiso 1 1 calc R . . C53 C 0.9822(8) 0.1523(7) 0.8310(4) 0.088(3) Uiso 1 1 d D . . C54 C 1.0505(15) 0.2083(12) 0.8419(8) 0.232(13) Uiso 1 1 d D . . H54A H 1.1025 0.1944 0.8280 0.348 Uiso 1 1 calc R . . H54B H 1.0609 0.2120 0.8749 0.348 Uiso 1 1 calc R . . H54C H 1.0317 0.2543 0.8296 0.348 Uiso 1 1 calc R . . C55 C 1.0199(18) 0.0873(12) 0.8497(8) 0.233(13) Uiso 1 1 d D . . H55A H 0.9794 0.0483 0.8460 0.350 Uiso 1 1 calc R . . H55B H 1.0353 0.0941 0.8822 0.350 Uiso 1 1 calc R . . H55C H 1.0703 0.0758 0.8337 0.350 Uiso 1 1 calc R . . C56 C 0.9685(8) 0.1540(8) 0.7804(4) 0.097(4) Uiso 1 1 d D . . H56A H 0.9227 0.1216 0.7709 0.146 Uiso 1 1 calc R . . H56B H 1.0201 0.1394 0.7665 0.146 Uiso 1 1 calc R . . H56C H 0.9536 0.2023 0.7706 0.146 Uiso 1 1 calc R . . C57 C 0.6390(4) 0.3930(3) 0.6010(2) 0.0331(12) Uiso 1 1 d . . . C58 C 0.6900(4) 0.3819(3) 0.5651(2) 0.0367(13) Uiso 1 1 d . . . H58A H 0.7492 0.3785 0.5704 0.044 Uiso 1 1 calc R . . C59 C 0.6532(4) 0.3758(4) 0.5209(2) 0.0412(15) Uiso 1 1 d . . . C60 C 0.5651(5) 0.3782(4) 0.5148(3) 0.0464(16) Uiso 1 1 d . . . H60A H 0.5395 0.3727 0.4851 0.056 Uiso 1 1 calc R . . C61 C 0.5149(4) 0.3881(4) 0.5508(3) 0.0459(15) Uiso 1 1 d . . . C62 C 0.5522(4) 0.3966(4) 0.5946(2) 0.0413(14) Uiso 1 1 d . . . H62A H 0.5185 0.4048 0.6196 0.050 Uiso 1 1 calc R . . C63 C 0.7076(5) 0.3621(4) 0.4793(3) 0.0496(17) Uiso 1 1 d . . . C64 C 0.6867(7) 0.2877(6) 0.4605(4) 0.070(2) Uiso 1 1 d . . . H64A H 0.7020 0.2521 0.4837 0.106 Uiso 1 1 calc R . . H64B H 0.7183 0.2791 0.4334 0.106 Uiso 1 1 calc R . . H64C H 0.6263 0.2846 0.4522 0.106 Uiso 1 1 calc R . . C65 C 0.6836(8) 0.4188(7) 0.4427(4) 0.085(3) Uiso 1 1 d . . . H65A H 0.7166 0.4112 0.4161 0.128 Uiso 1 1 calc R . . H65B H 0.6954 0.4661 0.4552 0.128 Uiso 1 1 calc R . . H65C H 0.6236 0.4149 0.4337 0.128 Uiso 1 1 calc R . . C66 C 0.7990(6) 0.3704(5) 0.4899(3) 0.066(2) Uiso 1 1 d . . . H66A H 0.8180 0.3353 0.5127 0.098 Uiso 1 1 calc R . . H66B H 0.8105 0.4182 0.5017 0.098 Uiso 1 1 calc R . . H66C H 0.8291 0.3632 0.4621 0.098 Uiso 1 1 calc R . . C67 C 0.4175(5) 0.3929(5) 0.5429(3) 0.0576(19) Uiso 1 1 d . . . C68 C 0.3796(9) 0.3362(8) 0.5755(5) 0.100(4) Uiso 1 1 d . . . H68A H 0.3181 0.3373 0.5718 0.151 Uiso 1 1 calc R . . H68B H 0.3974 0.3473 0.6071 0.151 Uiso 1 1 calc R . . H68C H 0.3998 0.2889 0.5678 0.151 Uiso 1 1 calc R . . C69 C 0.3923(9) 0.4667(8) 0.5512(5) 0.104(4) Uiso 1 1 d . . . H69A H 0.4193 0.4982 0.5300 0.155 Uiso 1 1 calc R . . H69B H 0.4096 0.4800 0.5825 0.155 Uiso 1 1 calc R . . H69C H 0.3311 0.4709 0.5465 0.155 Uiso 1 1 calc R . . C70 C 0.3890(9) 0.3714(8) 0.4948(5) 0.108(4) Uiso 1 1 d . . . H70A H 0.4113 0.4050 0.4732 0.163 Uiso 1 1 calc R . . H70B H 0.3274 0.3716 0.4916 0.163 Uiso 1 1 calc R . . H70C H 0.4098 0.3237 0.4886 0.163 Uiso 1 1 calc R . . C71 C 0.8868(3) 0.4865(3) 0.58514(19) 0.0260(11) Uiso 1 1 d . . . C72 C 0.9542(3) 0.4498(3) 0.56757(18) 0.0283(10) Uiso 1 1 d . . . H72A H 0.9746 0.4077 0.5821 0.034 Uiso 1 1 calc R . . C73 C 0.9914(4) 0.4742(3) 0.5292(2) 0.0319(12) Uiso 1 1 d . . . C74 C 0.9586(4) 0.5351(3) 0.5071(2) 0.0335(12) Uiso 1 1 d . . . H74A H 0.9835 0.5518 0.4807 0.040 Uiso 1 1 calc R . . C75 C 0.8903(4) 0.5714(3) 0.5233(2) 0.0322(12) Uiso 1 1 d . . . C76 C 0.8555(4) 0.5463(3) 0.5622(2) 0.0294(11) Uiso 1 1 d . . . H76A H 0.8090 0.5707 0.5736 0.035 Uiso 1 1 calc R . . C77 C 1.0665(5) 0.4331(4) 0.5105(3) 0.0465(16) Uiso 1 1 d . . . C78 C 1.0319(11) 0.3757(9) 0.4785(6) 0.124(5) Uiso 1 1 d . . . H78A H 0.9992 0.3974 0.4530 0.186 Uiso 1 1 calc R . . H78B H 0.9957 0.3439 0.4949 0.186 Uiso 1 1 calc R . . H78C H 1.0785 0.3486 0.4669 0.186 Uiso 1 1 calc R . . C79 C 1.1150(8) 0.3891(7) 0.5481(4) 0.094(3) Uiso 1 1 d . . . H79A H 1.1616 0.3639 0.5349 0.141 Uiso 1 1 calc R . . H79B H 1.0768 0.3547 0.5609 0.141 Uiso 1 1 calc R . . H79C H 1.1373 0.4209 0.5722 0.141 Uiso 1 1 calc R . . C80 C 1.1285(10) 0.4810(9) 0.4905(5) 0.112(5) Uiso 1 1 d . . . H80A H 1.1003 0.5096 0.4664 0.168 Uiso 1 1 calc R . . H80B H 1.1730 0.4526 0.4778 0.168 Uiso 1 1 calc R . . H80C H 1.1532 0.5122 0.5143 0.168 Uiso 1 1 calc R . . C81 C 0.8503(4) 0.6352(4) 0.4967(2) 0.0410(14) Uiso 1 1 d . . . C82 C 0.7738(6) 0.6089(5) 0.4684(3) 0.058(2) Uiso 1 1 d . . . H82A H 0.7479 0.6486 0.4514 0.087 Uiso 1 1 calc R . . H82B H 0.7331 0.5887 0.4885 0.087 Uiso 1 1 calc R . . H82C H 0.7911 0.5725 0.4471 0.087 Uiso 1 1 calc R . . C83 C 0.8220(5) 0.6927(4) 0.5298(3) 0.0466(16) Uiso 1 1 d . . . H83A H 0.7970 0.7324 0.5124 0.070 Uiso 1 1 calc R . . H83B H 0.8707 0.7095 0.5486 0.070 Uiso 1 1 calc R . . H83C H 0.7803 0.6728 0.5494 0.070 Uiso 1 1 calc R . . C84 C 0.9096(5) 0.6699(4) 0.4645(3) 0.0502(17) Uiso 1 1 d . . . H84A H 0.8808 0.7096 0.4488 0.075 Uiso 1 1 calc R . . H84B H 0.9264 0.6350 0.4422 0.075 Uiso 1 1 calc R . . H84C H 0.9596 0.6875 0.4820 0.075 Uiso 1 1 calc R . . C85 C 0.6286(4) 0.5192(3) 0.8609(2) 0.0353(13) Uiso 1 1 d . . . C86 C 0.5673(5) 0.5744(4) 0.8616(3) 0.0483(17) Uiso 1 1 d . . . H86A H 0.5638 0.6078 0.8374 0.058 Uiso 1 1 calc R . . C87 C 0.5130(5) 0.5809(5) 0.8961(3) 0.059(2) Uiso 1 1 d . . . C88 C 0.5198(5) 0.5284(5) 0.9312(3) 0.0524(18) Uiso 1 1 d . . . H88A H 0.4826 0.5307 0.9552 0.063 Uiso 1 1 calc R . . C89 C 0.5788(5) 0.4742(5) 0.9314(3) 0.0534(19) Uiso 1 1 d . . . C90 C 0.6334(5) 0.4702(4) 0.8956(3) 0.0446(16) Uiso 1 1 d . . . H90A H 0.6740 0.4333 0.8953 0.054 Uiso 1 1 calc R . . C91 C 0.4447(7) 0.6398(6) 0.8973(4) 0.076(3) Uiso 1 1 d . . . C92 C 0.3532(9) 0.6035(8) 0.8969(5) 0.106(4) Uiso 1 1 d . . . H92A H 0.3100 0.6404 0.8975 0.160 Uiso 1 1 calc R . . H92B H 0.3500 0.5731 0.9238 0.160 Uiso 1 1 calc R . . H92C H 0.3439 0.5749 0.8694 0.160 Uiso 1 1 calc R . . C93 C 0.4426(8) 0.6853(7) 0.8559(5) 0.093(4) Uiso 1 1 d . . . H93A H 0.4967 0.7094 0.8542 0.139 Uiso 1 1 calc R . . H93B H 0.3978 0.7206 0.8576 0.139 Uiso 1 1 calc R . . H93C H 0.4318 0.6559 0.8288 0.139 Uiso 1 1 calc R . . C94 C 0.4631(8) 0.6836(7) 0.9392(4) 0.090(3) Uiso 1 1 d . . . H94A H 0.5192 0.7045 0.9382 0.134 Uiso 1 1 calc R . . H94B H 0.4610 0.6534 0.9661 0.134 Uiso 1 1 calc R . . H94C H 0.4212 0.7213 0.9406 0.134 Uiso 1 1 calc R . . C95 C 0.5854(6) 0.4163(5) 0.9691(3) 0.061(2) Uiso 1 1 d . . . C96 C 0.6754(8) 0.4126(8) 0.9892(5) 0.094(4) Uiso 1 1 d . . . H96A H 0.7136 0.4045 0.9648 0.141 Uiso 1 1 calc R . . H96B H 0.6807 0.3737 1.0112 0.141 Uiso 1 1 calc R . . H96C H 0.6900 0.4574 1.0046 0.141 Uiso 1 1 calc R . . C97 C 0.5210(8) 0.4279(7) 1.0059(5) 0.097(4) Uiso 1 1 d . . . H97A H 0.4640 0.4280 0.9915 0.145 Uiso 1 1 calc R . . H97B H 0.5320 0.4734 1.0211 0.145 Uiso 1 1 calc R . . H97C H 0.5262 0.3895 1.0284 0.145 Uiso 1 1 calc R . . C98 C 0.5639(7) 0.3434(6) 0.9471(4) 0.073(3) Uiso 1 1 d . . . H98A H 0.6030 0.3335 0.9234 0.110 Uiso 1 1 calc R . . H98B H 0.5063 0.3443 0.9335 0.110 Uiso 1 1 calc R . . H98C H 0.5688 0.3063 0.9703 0.110 Uiso 1 1 calc R . . C99 C 0.7656(4) 0.2812(3) 0.7156(2) 0.0282(11) Uiso 1 1 d . . . C100 C 0.7232(4) 0.2273(3) 0.7365(2) 0.0324(12) Uiso 1 1 d . . . H10D H 0.6876 0.2383 0.7603 0.039 Uiso 1 1 calc R . . C101 C 0.7323(5) 0.1568(4) 0.7230(3) 0.0436(16) Uiso 1 1 d . . . C102 C 0.7862(4) 0.1433(4) 0.6876(2) 0.0412(14) Uiso 1 1 d . . . H10E H 0.7929 0.0958 0.6777 0.049 Uiso 1 1 calc R . . C103 C 0.8296(4) 0.1963(4) 0.6669(2) 0.0377(13) Uiso 1 1 d . . . C104 C 0.8169(4) 0.2653(3) 0.6808(2) 0.0315(12) Uiso 1 1 d . . . H10F H 0.8442 0.3028 0.6661 0.038 Uiso 1 1 calc R . . C105 C 0.6858(5) 0.0987(4) 0.7486(3) 0.0518(18) Uiso 1 1 d . . . C106 C 0.5906(6) 0.1108(5) 0.7408(3) 0.064(2) Uiso 1 1 d . . . H10G H 0.5759 0.1572 0.7530 0.096 Uiso 1 1 calc R . . H10H H 0.5603 0.0736 0.7563 0.096 Uiso 1 1 calc R . . H10I H 0.5751 0.1093 0.7082 0.096 Uiso 1 1 calc R . . C107 C 0.7000(6) 0.0255(5) 0.7280(3) 0.065(2) Uiso 1 1 d . . . H10J H 0.6695 -0.0102 0.7447 0.098 Uiso 1 1 calc R . . H10K H 0.7601 0.0144 0.7301 0.098 Uiso 1 1 calc R . . H10L H 0.6793 0.0254 0.6960 0.098 Uiso 1 1 calc R . . C108 C 0.7097(6) 0.1003(6) 0.7985(3) 0.070(2) Uiso 1 1 d . . . H10M H 0.7004 0.1480 0.8104 0.105 Uiso 1 1 calc R . . H10N H 0.7691 0.0877 0.8036 0.105 Uiso 1 1 calc R . . H10O H 0.6751 0.0662 0.8142 0.105 Uiso 1 1 calc R . . C109 C 0.8898(5) 0.1806(4) 0.6286(3) 0.0489(17) Uiso 1 1 d . . . C110 C 0.9744(10) 0.2043(9) 0.6434(6) 0.117(5) Uiso 1 1 d . . . H11A H 1.0129 0.1948 0.6193 0.175 Uiso 1 1 calc R . . H11B H 0.9935 0.1787 0.6710 0.175 Uiso 1 1 calc R . . H11C H 0.9736 0.2552 0.6497 0.175 Uiso 1 1 calc R . . C111 C 0.9004(12) 0.1063(11) 0.6191(7) 0.143(7) Uiso 1 1 d . . . H11D H 0.9388 0.1008 0.5945 0.215 Uiso 1 1 calc R . . H11E H 0.8458 0.0854 0.6098 0.215 Uiso 1 1 calc R . . H11F H 0.9239 0.0823 0.6464 0.215 Uiso 1 1 calc R . . C112 C 0.8601(11) 0.2190(9) 0.5873(6) 0.121(5) Uiso 1 1 d . . . H11G H 0.8978 0.2094 0.5629 0.182 Uiso 1 1 calc R . . H11H H 0.8595 0.2700 0.5935 0.182 Uiso 1 1 calc R . . H11I H 0.8032 0.2032 0.5778 0.182 Uiso 1 1 calc R . . C113 C 0.8566(3) 0.6341(3) 0.68667(18) 0.0239(10) Uiso 1 1 d . . . C114 C 0.9317(3) 0.6249(3) 0.66617(18) 0.0256(10) Uiso 1 1 d . . . H11J H 0.9531 0.5785 0.6622 0.031 Uiso 1 1 calc R . . C115 C 0.9767(4) 0.6836(3) 0.6512(2) 0.0294(11) Uiso 1 1 d . . . C116 C 0.9437(4) 0.7509(4) 0.6582(2) 0.0409(14) Uiso 1 1 d . . . H11K H 0.9737 0.7912 0.6486 0.049 Uiso 1 1 calc R . . C117 C 0.8678(4) 0.7607(4) 0.6789(2) 0.0379(13) Uiso 1 1 d . A . C118 C 0.8253(4) 0.7007(3) 0.6931(2) 0.0352(13) Uiso 1 1 d . . . H11L H 0.7738 0.7061 0.7074 0.042 Uiso 1 1 calc R . . C119 C 1.0620(4) 0.6769(3) 0.6297(2) 0.0354(13) Uiso 1 1 d . . . C120 C 1.1282(5) 0.7152(5) 0.6585(3) 0.0521(18) Uiso 1 1 d . . . H12D H 1.1120 0.7651 0.6614 0.078 Uiso 1 1 calc R . . H12E H 1.1820 0.7123 0.6441 0.078 Uiso 1 1 calc R . . H12F H 1.1337 0.6934 0.6887 0.078 Uiso 1 1 calc R . . C121 C 1.0554(5) 0.7083(5) 0.5816(3) 0.0528(18) Uiso 1 1 d . . . H12G H 1.0387 0.7582 0.5832 0.079 Uiso 1 1 calc R . . H12H H 1.0133 0.6820 0.5628 0.079 Uiso 1 1 calc R . . H12I H 1.1101 0.7048 0.5682 0.079 Uiso 1 1 calc R . . C122 C 1.0883(4) 0.5985(4) 0.6249(2) 0.0386(14) Uiso 1 1 d . . . H12J H 1.1425 0.5961 0.6109 0.058 Uiso 1 1 calc R . . H12K H 1.0456 0.5734 0.6057 0.058 Uiso 1 1 calc R . . H12L H 1.0933 0.5764 0.6550 0.058 Uiso 1 1 calc R . . C123 C 0.8354(5) 0.8358(5) 0.6869(3) 0.0538(19) Uiso 1 1 d . . . C124 C 0.8108(15) 0.8693(13) 0.6396(8) 0.083(6) Uiso 0.50 1 d P A 1 H12M H 0.7686 0.8394 0.6234 0.125 Uiso 0.50 1 calc PR A 1 H12N H 0.8607 0.8728 0.6219 0.125 Uiso 0.50 1 calc PR A 1 H12O H 0.7874 0.9167 0.6439 0.125 Uiso 0.50 1 calc PR A 1 C125 C 0.7529(12) 0.8373(11) 0.7181(7) 0.063(5) Uiso 0.50 1 d P A 1 H12P H 0.7060 0.8127 0.7020 0.095 Uiso 0.50 1 calc PR A 1 H12Q H 0.7370 0.8865 0.7237 0.095 Uiso 0.50 1 calc PR A 1 H12R H 0.7667 0.8135 0.7472 0.095 Uiso 0.50 1 calc PR A 1 C126 C 0.9011(13) 0.8753(11) 0.7171(7) 0.070(5) Uiso 0.50 1 d P A 1 H12S H 0.9109 0.8497 0.7459 0.104 Uiso 0.50 1 calc PR A 1 H12T H 0.8808 0.9231 0.7233 0.104 Uiso 0.50 1 calc PR A 1 H12U H 0.9538 0.8783 0.7016 0.104 Uiso 0.50 1 calc PR A 1 C127 C 0.6086(3) 0.5186(3) 0.70342(18) 0.0249(10) Uiso 1 1 d . . . C128 C 0.5278(4) 0.5104(3) 0.7178(2) 0.0319(12) Uiso 1 1 d . . . H12V H 0.5190 0.4833 0.7443 0.038 Uiso 1 1 calc R . . C129 C 0.4586(4) 0.5420(4) 0.6935(2) 0.0398(14) Uiso 1 1 d . . . C130 C 0.4739(4) 0.5814(4) 0.6554(2) 0.0397(14) Uiso 1 1 d . . . H13D H 0.4276 0.6024 0.6385 0.048 Uiso 1 1 calc R . . C131 C 0.5540(4) 0.5916(4) 0.6407(2) 0.0343(12) Uiso 1 1 d . . . C132 C 0.6221(4) 0.5599(3) 0.6648(2) 0.0308(12) Uiso 1 1 d . . . H13E H 0.6775 0.5662 0.6551 0.037 Uiso 1 1 calc R . . C133 C 0.3700(5) 0.5318(5) 0.7100(3) 0.0547(18) Uiso 1 1 d . . . C134 C 0.3687(7) 0.5645(6) 0.7581(4) 0.071(3) Uiso 1 1 d . . . H13F H 0.3807 0.6153 0.7565 0.106 Uiso 1 1 calc R . . H13G H 0.4114 0.5414 0.7783 0.106 Uiso 1 1 calc R . . H13H H 0.3131 0.5574 0.7700 0.106 Uiso 1 1 calc R . . C135 C 0.3031(6) 0.5677(6) 0.6788(4) 0.074(3) Uiso 1 1 d . . . H13I H 0.3143 0.6187 0.6777 0.110 Uiso 1 1 calc R . . H13J H 0.2476 0.5597 0.6905 0.110 Uiso 1 1 calc R . . H13K H 0.3043 0.5478 0.6481 0.110 Uiso 1 1 calc R . . C136 C 0.3510(6) 0.4524(6) 0.7117(4) 0.072(2) Uiso 1 1 d . . . H13L H 0.3521 0.4323 0.6811 0.108 Uiso 1 1 calc R . . H13M H 0.2953 0.4452 0.7234 0.108 Uiso 1 1 calc R . . H13N H 0.3935 0.4289 0.7318 0.108 Uiso 1 1 calc R . . C137 C 0.5719(5) 0.6357(4) 0.5976(3) 0.0442(15) Uiso 1 1 d . . . C138 C 0.4930(5) 0.6727(5) 0.5773(3) 0.058(2) Uiso 1 1 d . . . H13O H 0.5071 0.6998 0.5504 0.088 Uiso 1 1 calc R . . H13P H 0.4712 0.7049 0.5999 0.088 Uiso 1 1 calc R . . H13Q H 0.4503 0.6372 0.5685 0.088 Uiso 1 1 calc R . . C139 C 0.6059(5) 0.5850(5) 0.5617(3) 0.0504(17) Uiso 1 1 d . . . H13R H 0.6175 0.6120 0.5343 0.076 Uiso 1 1 calc R . . H13S H 0.5640 0.5484 0.5540 0.076 Uiso 1 1 calc R . . H13T H 0.6579 0.5628 0.5740 0.076 Uiso 1 1 calc R . . C140 C 0.6366(5) 0.6925(4) 0.6099(3) 0.0502(17) Uiso 1 1 d . . . H14D H 0.6476 0.7203 0.5828 0.075 Uiso 1 1 calc R . . H14E H 0.6889 0.6702 0.6218 0.075 Uiso 1 1 calc R . . H14F H 0.6152 0.7238 0.6332 0.075 Uiso 1 1 calc R . . C141 C 0.8877(3) 0.4893(3) 0.80478(18) 0.0252(10) Uiso 1 1 d . . . C142 C 0.9426(4) 0.5439(3) 0.7939(2) 0.0311(12) Uiso 1 1 d . . . H14G H 0.9354 0.5666 0.7651 0.037 Uiso 1 1 calc R . . C143 C 1.0072(4) 0.5654(3) 0.8243(2) 0.0362(13) Uiso 1 1 d . . . C144 C 1.0170(5) 0.5313(4) 0.8655(3) 0.0439(15) Uiso 1 1 d . . . H14H H 1.0609 0.5459 0.8866 0.053 Uiso 1 1 calc R . . C145 C 0.9641(4) 0.4754(4) 0.8776(3) 0.0431(15) Uiso 1 1 d . . . C146 C 0.8997(4) 0.4550(4) 0.8466(2) 0.0332(11) Uiso 1 1 d . . . H14I H 0.8634 0.4174 0.8540 0.040 Uiso 1 1 calc R . . C147 C 1.0673(5) 0.6246(4) 0.8125(3) 0.0476(16) Uiso 1 1 d . . . C148 C 1.1406(8) 0.5928(8) 0.7884(5) 0.099(4) Uiso 1 1 d . . . H14J H 1.1193 0.5689 0.7605 0.148 Uiso 1 1 calc R . . H14K H 1.1701 0.5584 0.8085 0.148 Uiso 1 1 calc R . . H14L H 1.1795 0.6305 0.7807 0.148 Uiso 1 1 calc R . . C149 C 1.0998(9) 0.6644(8) 0.8572(5) 0.098(4) Uiso 1 1 d . . . H14M H 1.0519 0.6855 0.8718 0.147 Uiso 1 1 calc R . . H14N H 1.1391 0.7019 0.8495 0.147 Uiso 1 1 calc R . . H14O H 1.1284 0.6307 0.8781 0.147 Uiso 1 1 calc R . . C150 C 1.0246(5) 0.6808(4) 0.7832(3) 0.0504(17) Uiso 1 1 d . . . H15A H 1.0039 0.6599 0.7542 0.076 Uiso 1 1 calc R . . H15B H 1.0647 0.7187 0.7775 0.076 Uiso 1 1 calc R . . H15C H 0.9772 0.7005 0.7988 0.076 Uiso 1 1 calc R . . C151 C 0.9745(5) 0.4382(5) 0.9243(3) 0.056(2) Uiso 1 1 d . . . C152 C 0.9948(9) 0.3622(7) 0.9167(5) 0.097(4) Uiso 1 1 d . . . H15D H 1.0495 0.3585 0.9032 0.145 Uiso 1 1 calc R . . H15E H 0.9513 0.3410 0.8960 0.145 Uiso 1 1 calc R . . H15F H 0.9968 0.3369 0.9458 0.145 Uiso 1 1 calc R . . C153 C 0.8868(8) 0.4332(7) 0.9457(4) 0.089(3) Uiso 1 1 d . . . H15G H 0.8936 0.4099 0.9754 0.134 Uiso 1 1 calc R . . H15H H 0.8481 0.4055 0.9256 0.134 Uiso 1 1 calc R . . H15I H 0.8641 0.4809 0.9495 0.134 Uiso 1 1 calc R . . C154 C 1.0419(11) 0.4656(11) 0.9517(6) 0.135(6) Uiso 1 1 d . . . H15J H 1.0926 0.4667 0.9344 0.203 Uiso 1 1 calc R . . H15K H 1.0517 0.4355 0.9786 0.203 Uiso 1 1 calc R . . H15L H 1.0283 0.5138 0.9613 0.203 Uiso 1 1 calc R . . C155 C 0.5168(5) 0.2744(4) 0.6822(3) 0.0456(16) Uiso 1 1 d . . . C156 C 0.5451(5) 0.2368(4) 0.6468(3) 0.0465(16) Uiso 1 1 d . . . H15M H 0.5966 0.2496 0.6343 0.056 Uiso 1 1 calc R . . C157 C 0.4986(5) 0.1788(4) 0.6285(3) 0.0510(18) Uiso 1 1 d . . . C158 C 0.4209(6) 0.1662(5) 0.6447(3) 0.062(2) Uiso 1 1 d . . . H15N H 0.3871 0.1294 0.6314 0.075 Uiso 1 1 calc R . . C159 C 0.3898(5) 0.2061(5) 0.6805(3) 0.0558(19) Uiso 1 1 d . B . C160 C 0.4394(5) 0.2610(4) 0.6992(3) 0.0499(17) Uiso 1 1 d . . . H16B H 0.4200 0.2889 0.7233 0.060 Uiso 1 1 calc R . . C161 C 0.5341(6) 0.1345(5) 0.5898(3) 0.064(2) Uiso 1 1 d . . . C162 C 0.5769(13) 0.1795(11) 0.5562(7) 0.150(7) Uiso 1 1 d . . . H16C H 0.5367 0.2137 0.5425 0.225 Uiso 1 1 calc R . . H16D H 0.5982 0.1493 0.5324 0.225 Uiso 1 1 calc R . . H16E H 0.6239 0.2049 0.5718 0.225 Uiso 1 1 calc R . . C163 C 0.4708(10) 0.0818(9) 0.5682(6) 0.116(5) Uiso 1 1 d . . . H16F H 0.4244 0.1078 0.5525 0.174 Uiso 1 1 calc R . . H16G H 0.4487 0.0519 0.5920 0.174 Uiso 1 1 calc R . . H16H H 0.4986 0.0521 0.5463 0.174 Uiso 1 1 calc R . . C164 C 0.5973(10) 0.0800(10) 0.6109(6) 0.127(5) Uiso 1 1 d . . . H16I H 0.6445 0.1050 0.6265 0.190 Uiso 1 1 calc R . . H16J H 0.6182 0.0501 0.5868 0.190 Uiso 1 1 calc R . . H16K H 0.5693 0.0503 0.6328 0.190 Uiso 1 1 calc R . . C165 C 0.3053(7) 0.1888(7) 0.6998(4) 0.080(3) Uiso 1 1 d . . . C166 C 0.2339(19) 0.2121(18) 0.6612(11) 0.114(9) Uiso 0.50 1 d P B 1 H16L H 0.2608 0.2347 0.6359 0.171 Uiso 0.50 1 calc PR B 1 H16M H 0.1949 0.2455 0.6743 0.171 Uiso 0.50 1 calc PR B 1 H16N H 0.2029 0.1701 0.6501 0.171 Uiso 0.50 1 calc PR B 1 C167 C 0.3007(16) 0.1161(13) 0.7149(9) 0.087(7) Uiso 0.50 1 d P B 1 H16O H 0.3449 0.1073 0.7387 0.130 Uiso 0.50 1 calc PR B 1 H16P H 0.3085 0.0843 0.6891 0.130 Uiso 0.50 1 calc PR B 1 H16Q H 0.2456 0.1073 0.7269 0.130 Uiso 0.50 1 calc PR B 1 C168 C 0.2823(12) 0.2387(10) 0.7395(7) 0.059(4) Uiso 0.50 1 d P B 1 H16R H 0.3184 0.2279 0.7666 0.089 Uiso 0.50 1 calc PR B 1 H16S H 0.2233 0.2315 0.7460 0.089 Uiso 0.50 1 calc PR B 1 H16T H 0.2907 0.2881 0.7306 0.089 Uiso 0.50 1 calc PR B 1 C266 C 0.2635(16) 0.1264(13) 0.6796(9) 0.087(6) Uiso 0.50 1 d P B 2 H26D H 0.2861 0.0836 0.6947 0.130 Uiso 0.50 1 calc PR B 2 H26E H 0.2735 0.1243 0.6471 0.130 Uiso 0.50 1 calc PR B 2 H26F H 0.2030 0.1294 0.6835 0.130 Uiso 0.50 1 calc PR B 2 C267 C 0.320(2) 0.153(2) 0.7486(12) 0.131(11) Uiso 0.50 1 d P B 2 H26G H 0.3799 0.1505 0.7568 0.197 Uiso 0.50 1 calc PR B 2 H26H H 0.2956 0.1053 0.7477 0.197 Uiso 0.50 1 calc PR B 2 H26I H 0.2919 0.1817 0.7711 0.197 Uiso 0.50 1 calc PR B 2 C268 C 0.2625(17) 0.2510(15) 0.7095(10) 0.097(7) Uiso 0.50 1 d P B 2 H26J H 0.2832 0.2692 0.7392 0.146 Uiso 0.50 1 calc PR B 2 H26K H 0.2022 0.2411 0.7100 0.146 Uiso 0.50 1 calc PR B 2 H26L H 0.2721 0.2865 0.6860 0.146 Uiso 0.50 1 calc PR B 2 C169 C 0.9728(4) 0.3582(4) 0.7459(2) 0.0385(14) Uiso 1 1 d . . . H16U H 0.9384 0.3640 0.7725 0.046 Uiso 1 1 calc R . . H16V H 0.9660 0.3091 0.7344 0.046 Uiso 1 1 calc R . . C170 C 1.0610(7) 0.3730(6) 0.7583(4) 0.079(3) Uiso 1 1 d . . . H17A H 1.0906 0.3304 0.7707 0.095 Uiso 1 1 calc R . . H17B H 1.0673 0.4121 0.7807 0.095 Uiso 1 1 calc R . . C171 C 1.0933(7) 0.3949(7) 0.7109(4) 0.084(3) Uiso 1 1 d . . . H17C H 1.1462 0.4223 0.7143 0.100 Uiso 1 1 calc R . . H17D H 1.1016 0.3531 0.6914 0.100 Uiso 1 1 calc R . . C172 C 1.0223(5) 0.4396(4) 0.6927(3) 0.0483(17) Uiso 1 1 d . . . H17E H 1.0297 0.4892 0.7030 0.058 Uiso 1 1 calc R . . H17F H 1.0188 0.4388 0.6590 0.058 Uiso 1 1 calc R . . C224 C 0.8828(18) 0.8962(17) 0.6645(10) 0.107(8) Uiso 0.50 1 d P A 2 H22D H 0.8570 0.9417 0.6718 0.160 Uiso 0.50 1 calc PR A 2 H22E H 0.8798 0.8895 0.6315 0.160 Uiso 0.50 1 calc PR A 2 H22F H 0.9417 0.8960 0.6760 0.160 Uiso 0.50 1 calc PR A 2 C225 C 0.7367(15) 0.8383(13) 0.6904(9) 0.081(6) Uiso 0.50 1 d P A 2 H22G H 0.7191 0.8872 0.6959 0.121 Uiso 0.50 1 calc PR A 2 H22H H 0.7209 0.8081 0.7156 0.121 Uiso 0.50 1 calc PR A 2 H22I H 0.7091 0.8211 0.6619 0.121 Uiso 0.50 1 calc PR A 2 C226 C 0.8456(19) 0.8448(17) 0.7407(10) 0.108(9) Uiso 0.50 1 d P A 2 H22J H 0.8262 0.8920 0.7491 0.163 Uiso 0.50 1 calc PR A 2 H22K H 0.9049 0.8392 0.7508 0.163 Uiso 0.50 1 calc PR A 2 H22L H 0.8121 0.8086 0.7552 0.163 Uiso 0.50 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 Nd1 0.04203(17) 0.02184(14) 0.02359(13) -0.00167(11) 0.00963(12) 0.00476(12) Nd2 0.02498(13) 0.02479(14) 0.02004(13) 0.00195(11) 0.00754(9) 0.00211(11) Nd3 0.01979(11) 0.02000(12) 0.01715(12) 0.00055(10) 0.00439(8) 0.00092(10) O1 0.061(3) 0.047(3) 0.060(3) -0.004(3) 0.002(3) 0.027(3) O2 0.063(3) 0.036(2) 0.041(3) -0.013(2) 0.009(2) 0.001(2) O3 0.029(2) 0.045(3) 0.030(2) 0.0025(18) 0.0094(17) -0.0065(18) O4 0.039(2) 0.037(2) 0.033(2) 0.0140(18) 0.0059(18) 0.0050(18) O5 0.0278(18) 0.047(2) 0.0209(18) -0.0041(19) 0.0046(14) -0.0068(19) O6 0.0304(18) 0.032(2) 0.0191(17) -0.0007(15) 0.0078(14) -0.0044(16) O7 0.045(2) 0.033(2) 0.028(2) -0.0032(17) 0.0146(18) 0.0048(18) O8 0.0297(19) 0.0228(19) 0.0248(19) -0.0045(15) 0.0086(15) -0.0005(15) O9 0.0289(19) 0.0231(19) 0.0273(19) 0.0051(15) 0.0021(15) -0.0009(15) O11 0.0260(18) 0.032(2) 0.0143(16) -0.0006(14) 0.0013(13) 0.0027(14) O12 0.042(3) 0.060(3) 0.032(2) -0.010(2) 0.0096(19) -0.018(2) O13 0.0281(19) 0.035(2) 0.032(2) 0.0061(17) 0.0032(15) 0.0066(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 O2 2.135(5) . ? Nd1 O7 2.344(4) . ? Nd1 O9 2.408(4) . ? Nd1 O11 2.412(4) . ? Nd1 O1 2.503(5) . ? Nd1 O10 2.566(4) . ? Nd1 C141 2.918(5) . ? Nd1 Nd3 3.7186(4) . ? Nd1 Nd2 3.7259(4) . ? Nd2 O4 2.160(4) . ? Nd2 O3 2.235(4) . ? Nd2 O8 2.375(4) . ? Nd2 O7 2.418(4) . ? Nd2 O11 2.569(4) . ? Nd2 O10 2.610(4) . ? Nd2 Nd3 3.7707(4) . ? Nd3 O6 2.169(4) . ? Nd3 O8 2.393(4) . ? Nd3 O9 2.406(4) . ? Nd3 O10 2.470(4) . ? Nd3 O13 2.482(4) . ? Nd3 O5 2.545(4) . ? Nd3 O11 2.548(3) . ? O1 C1 1.416(9) . ? O2 C15 1.350(9) . ? O3 C29 1.365(8) . ? O4 C43 1.356(8) . ? O5 C57 1.405(7) . ? O6 C71 1.338(7) . ? O7 C85 1.347(8) . ? O8 C99 1.378(7) . ? O9 C113 1.383(7) . ? O10 C127 1.377(6) . ? O11 C141 1.381(6) . ? O12 C155 1.399(9) . ? O13 C172 1.456(9) . ? O13 C169 1.467(8) . ? C1 C2 1.365(11) . ? C1 C6 1.409(12) . ? C2 C3 1.396(13) . ? C3 C4 1.377(13) . ? C3 C7 1.593(15) . ? C4 C5 1.376(13) . ? C5 C6 1.385(13) . ? C5 C11 1.527(16) . ? C7 C8 1.514(17) . ? C7 C10 1.520(19) . ? C7 C9 1.522(17) . ? C11 C14 1.50(2) . ? C11 C13 1.516(17) . ? C11 C12 1.55(2) . ? C15 C16 1.361(12) . ? C15 C20 1.380(12) . ? C16 C17 1.378(13) . ? C17 C18 1.361(15) . ? C17 C21 1.529(15) . ? C18 C19 1.404(16) . ? C19 C20 1.420(14) . ? C19 C25 1.612(17) . ? C21 C24 1.43(3) . ? C21 C22 1.46(3) . ? C21 C23 1.600(19) . ? C25 C26 1.43(2) . ? C25 C27 1.443(19) . ? C25 C28 1.572(19) . ? C29 C34 1.382(11) . ? C29 C30 1.391(12) . ? C30 C31 1.400(14) . ? C31 C32 1.380(14) . ? C31 C35 1.591(17) . ? C32 C33 1.423(14) . ? C33 C34 1.408(13) . ? C33 C39 1.503(15) . ? C35 C36 1.47(3) . ? C35 C37 1.51(4) . ? C35 C38 1.57(3) . ? C39 C41 1.47(2) . ? C39 C42 1.54(2) . ? C39 C40 1.546(19) . ? C43 C48 1.385(10) . ? C43 C44 1.390(11) . ? C44 C45 1.390(15) . ? C45 C46 1.400(17) . ? C45 C49 1.62(2) . ? C46 C47 1.371(16) . ? C47 C48 1.379(12) . ? C47 C53 1.503(16) . ? C49 C50 1.55(3) . ? C49 C52 1.60(3) . ? C49 C51 1.64(3) . ? C53 C55 1.46(2) . ? C53 C56 1.493(17) . ? C53 C54 1.539(9) . ? C57 C58 1.386(9) . ? C57 C62 1.387(9) . ? C58 C59 1.402(9) . ? C59 C60 1.406(10) . ? C59 C63 1.562(11) . ? C60 C61 1.376(10) . ? C61 C62 1.397(10) . ? C61 C67 1.559(11) . ? C63 C66 1.481(12) . ? C63 C64 1.540(13) . ? C63 C65 1.551(14) . ? C67 C69 1.474(17) . ? C67 C70 1.518(17) . ? C67 C68 1.582(17) . ? C71 C76 1.393(8) . ? C71 C72 1.403(8) . ? C72 C73 1.385(8) . ? C73 C74 1.407(9) . ? C73 C77 1.553(10) . ? C74 C75 1.393(8) . ? C75 C76 1.386(8) . ? C75 C81 1.552(9) . ? C77 C80 1.485(17) . ? C77 C78 1.520(18) . ? C77 C79 1.556(15) . ? C81 C82 1.520(11) . ? C81 C84 1.524(11) . ? C81 C83 1.543(10) . ? C85 C90 1.376(10) . ? C85 C86 1.430(10) . ? C86 C87 1.377(12) . ? C87 C88 1.431(12) . ? C87 C91 1.558(14) . ? C88 C89 1.389(12) . ? C89 C90 1.409(11) . ? C89 C95 1.557(13) . ? C91 C93 1.488(17) . ? C91 C94 1.500(17) . ? C91 C92 1.611(18) . ? C95 C96 1.521(15) . ? C95 C97 1.551(16) . ? C95 C98 1.552(14) . ? C99 C104 1.380(8) . ? C99 C100 1.384(8) . ? C100 C101 1.400(10) . ? C101 C102 1.412(10) . ? C101 C105 1.543(11) . ? C102 C103 1.380(10) . ? C103 C104 1.385(9) . ? C103 C109 1.550(10) . ? C105 C108 1.499(13) . ? C105 C107 1.532(13) . ? C105 C106 1.538(12) . ? C109 C111 1.44(2) . ? C109 C110 1.463(17) . ? C109 C112 1.472(18) . ? C113 C118 1.370(9) . ? C113 C114 1.383(8) . ? C114 C115 1.404(8) . ? C115 C116 1.395(9) . ? C115 C119 1.538(9) . ? C116 C117 1.398(9) . ? C117 C118 1.397(9) . ? C117 C123 1.532(11) . ? C119 C120 1.499(10) . ? C119 C121 1.534(10) . ? C119 C122 1.546(9) . ? C123 C126 1.53(2) . ? C123 C224 1.54(3) . ? C123 C124 1.56(3) . ? C123 C225 1.58(2) . ? C123 C226 1.59(3) . ? C123 C125 1.65(2) . ? C127 C128 1.386(8) . ? C127 C132 1.407(8) . ? C128 C129 1.412(9) . ? C129 C130 1.382(10) . ? C129 C133 1.529(11) . ? C130 C131 1.384(9) . ? C131 C132 1.396(8) . ? C131 C137 1.559(10) . ? C133 C135 1.526(13) . ? C133 C136 1.531(14) . ? C133 C134 1.547(13) . ? C137 C140 1.519(11) . ? C137 C138 1.530(11) . ? C137 C139 1.547(11) . ? C141 C146 1.395(8) . ? C141 C142 1.401(8) . ? C142 C143 1.386(9) . ? C143 C144 1.375(10) . ? C143 C147 1.526(10) . ? C144 C145 1.408(11) . ? C145 C146 1.386(9) . ? C145 C151 1.545(11) . ? C147 C150 1.505(11) . ? C147 C148 1.524(15) . ? C147 C149 1.577(16) . ? C151 C154 1.406(19) . ? C151 C152 1.491(16) . ? C151 C153 1.569(15) . ? C155 C156 1.359(11) . ? C155 C160 1.382(11) . ? C156 C157 1.412(11) . ? C157 C158 1.373(12) . ? C157 C161 1.548(13) . ? C158 C159 1.408(13) . ? C159 C160 1.397(12) . ? C159 C165 1.528(14) . ? C161 C162 1.50(2) . ? C161 C163 1.529(18) . ? C161 C164 1.545(19) . ? C165 C268 1.39(3) . ? C165 C167 1.45(3) . ? C165 C266 1.46(3) . ? C165 C168 1.56(2) . ? C165 C267 1.59(4) . ? C165 C166 1.62(3) . ? C169 C170 1.460(13) . ? C170 C171 1.572(16) . ? C171 C172 1.486(14) . ? 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 O7 100.34(18) . . ? O2 Nd1 O9 117.81(17) . . ? O7 Nd1 O9 139.15(14) . . ? O2 Nd1 O11 121.02(17) . . ? O7 Nd1 O11 74.99(13) . . ? O9 Nd1 O11 73.20(12) . . ? O2 Nd1 O1 90.6(2) . . ? O7 Nd1 O1 93.96(18) . . ? O9 Nd1 O1 99.40(16) . . ? O11 Nd1 O1 147.67(17) . . ? O2 Nd1 O10 170.78(17) . . ? O7 Nd1 O10 72.79(14) . . ? O9 Nd1 O10 70.53(12) . . ? O11 Nd1 O10 63.87(12) . . ? O1 Nd1 O10 83.90(16) . . ? O2 Nd1 C141 93.12(18) . . ? O7 Nd1 C141 81.21(15) . . ? O9 Nd1 C141 82.63(14) . . ? O11 Nd1 C141 28.05(13) . . ? O1 Nd1 C141 174.38(18) . . ? O10 Nd1 C141 91.89(13) . . ? O2 Nd1 Nd3 147.67(14) . . ? O7 Nd1 Nd3 99.95(10) . . ? O9 Nd1 Nd3 39.40(9) . . ? O11 Nd1 Nd3 42.83(8) . . ? O1 Nd1 Nd3 112.82(14) . . ? O10 Nd1 Nd3 41.42(8) . . ? C141 Nd1 Nd3 65.55(11) . . ? O2 Nd1 Nd2 132.56(14) . . ? O7 Nd1 Nd2 39.24(10) . . ? O9 Nd1 Nd2 100.26(9) . . ? O11 Nd1 Nd2 43.20(9) . . ? O1 Nd1 Nd2 111.06(15) . . ? O10 Nd1 Nd2 44.43(8) . . ? C141 Nd1 Nd2 63.35(11) . . ? Nd3 Nd1 Nd2 60.863(7) . . ? O4 Nd2 O3 102.18(17) . . ? O4 Nd2 O8 94.43(16) . . ? O3 Nd2 O8 104.93(15) . . ? O4 Nd2 O7 112.47(17) . . ? O3 Nd2 O7 103.88(16) . . ? O8 Nd2 O7 134.85(14) . . ? O4 Nd2 O11 99.43(15) . . ? O3 Nd2 O11 158.04(14) . . ? O8 Nd2 O11 69.32(12) . . ? O7 Nd2 O11 70.91(13) . . ? O4 Nd2 O10 158.96(14) . . ? O3 Nd2 O10 96.85(14) . . ? O8 Nd2 O10 71.84(13) . . ? O7 Nd2 O10 70.84(13) . . ? O11 Nd2 O10 61.19(11) . . ? O4 Nd2 Nd1 126.64(13) . . ? O3 Nd2 Nd1 124.29(12) . . ? O8 Nd2 Nd1 97.04(9) . . ? O7 Nd2 Nd1 37.81(10) . . ? O11 Nd2 Nd1 40.01(8) . . ? O10 Nd2 Nd1 43.48(8) . . ? O4 Nd2 Nd3 119.65(12) . . ? O3 Nd2 Nd3 120.61(11) . . ? O8 Nd2 Nd3 37.90(9) . . ? O7 Nd2 Nd3 97.14(10) . . ? O11 Nd2 Nd3 42.31(8) . . ? O10 Nd2 Nd3 40.67(8) . . ? Nd1 Nd2 Nd3 59.472(7) . . ? O6 Nd3 O8 132.34(13) . . ? O6 Nd3 O9 91.42(14) . . ? O8 Nd3 O9 136.23(13) . . ? O6 Nd3 O10 137.45(14) . . ? O8 Nd3 O10 74.10(12) . . ? O9 Nd3 O10 72.24(12) . . ? O6 Nd3 O13 82.65(14) . . ? O8 Nd3 O13 85.25(13) . . ? O9 Nd3 O13 102.12(14) . . ? O10 Nd3 O13 138.38(13) . . ? O6 Nd3 O5 84.21(13) . . ? O8 Nd3 O5 70.98(14) . . ? O9 Nd3 O5 123.63(14) . . ? O10 Nd3 O5 74.07(12) . . ? O13 Nd3 O5 132.55(15) . . ? O6 Nd3 O11 148.01(13) . . ? O8 Nd3 O11 69.42(13) . . ? O9 Nd3 O11 70.86(12) . . ? O10 Nd3 O11 63.36(12) . . ? O13 Nd3 O11 75.70(13) . . ? O5 Nd3 O11 127.76(12) . . ? O6 Nd3 Nd1 130.74(11) . . ? O8 Nd3 Nd1 96.90(9) . . ? O9 Nd3 Nd1 39.45(9) . . ? O10 Nd3 Nd1 43.40(9) . . ? O13 Nd3 Nd1 106.59(10) . . ? O5 Nd3 Nd1 116.35(9) . . ? O11 Nd3 Nd1 40.07(8) . . ? O6 Nd3 Nd2 168.20(10) . . ? O8 Nd3 Nd2 37.56(9) . . ? O9 Nd3 Nd2 99.11(9) . . ? O10 Nd3 Nd2 43.53(9) . . ? O13 Nd3 Nd2 100.18(9) . . ? O5 Nd3 Nd2 85.52(9) . . ? O11 Nd3 Nd2 42.74(9) . . ? Nd1 Nd3 Nd2 59.665(8) . . ? C1 O1 Nd1 139.6(5) . . ? C15 O2 Nd1 159.5(5) . . ? C29 O3 Nd2 139.7(4) . . ? C43 O4 Nd2 162.7(4) . . ? C57 O5 Nd3 140.9(4) . . ? C71 O6 Nd3 167.3(4) . . ? C85 O7 Nd1 141.4(4) . . ? C85 O7 Nd2 115.2(4) . . ? Nd1 O7 Nd2 102.95(15) . . ? C99 O8 Nd2 130.8(3) . . ? C99 O8 Nd3 124.6(3) . . ? Nd2 O8 Nd3 104.54(14) . . ? C113 O9 Nd3 137.4(3) . . ? C113 O9 Nd1 120.4(3) . . ? Nd3 O9 Nd1 101.15(14) . . ? C127 O10 Nd3 120.3(3) . . ? C127 O10 Nd1 109.8(3) . . ? Nd3 O10 Nd1 95.18(12) . . ? C127 O10 Nd2 134.4(3) . . ? Nd3 O10 Nd2 95.80(12) . . ? Nd1 O10 Nd2 92.09(12) . . ? C141 O11 Nd1 96.8(3) . . ? C141 O11 Nd3 134.8(3) . . ? Nd1 O11 Nd3 97.10(12) . . ? C141 O11 Nd2 125.7(3) . . ? Nd1 O11 Nd2 96.79(12) . . ? Nd3 O11 Nd2 94.95(12) . . ? C172 O13 C169 107.9(5) . . ? C172 O13 Nd3 124.0(4) . . ? C169 O13 Nd3 127.6(3) . . ? C2 C1 C6 123.1(8) . . ? C2 C1 O1 119.0(7) . . ? C6 C1 O1 117.8(7) . . ? C1 C2 C3 117.5(8) . . ? C4 C3 C2 120.0(9) . . ? C4 C3 C7 124.0(9) . . ? C2 C3 C7 116.0(9) . . ? C5 C4 C3 122.2(10) . . ? C4 C5 C6 118.9(9) . . ? C4 C5 C11 121.7(9) . . ? C6 C5 C11 118.8(9) . . ? C5 C6 C1 118.0(8) . . ? C8 C7 C10 109.3(12) . . ? C8 C7 C9 110.7(11) . . ? C10 C7 C9 109.8(11) . . ? C8 C7 C3 107.8(9) . . ? C10 C7 C3 109.0(10) . . ? C9 C7 C3 110.1(10) . . ? C14 C11 C13 115.5(12) . . ? C14 C11 C5 115.7(11) . . ? C13 C11 C5 113.9(10) . . ? C14 C11 C12 98.9(14) . . ? C13 C11 C12 99.6(13) . . ? C5 C11 C12 110.6(13) . . ? O2 C15 C16 121.3(7) . . ? O2 C15 C20 119.5(7) . . ? C16 C15 C20 119.2(8) . . ? C15 C16 C17 121.4(9) . . ? C18 C17 C16 120.2(10) . . ? C18 C17 C21 117.5(10) . . ? C16 C17 C21 122.0(9) . . ? C17 C18 C19 121.1(11) . . ? C18 C19 C20 116.8(10) . . ? C18 C19 C25 118.0(10) . . ? C20 C19 C25 125.2(10) . . ? C15 C20 C19 121.2(9) . . ? C24 C21 C22 115.2(18) . . ? C24 C21 C17 109.2(15) . . ? C22 C21 C17 111.0(13) . . ? C24 C21 C23 103.8(15) . . ? C22 C21 C23 103.9(14) . . ? C17 C21 C23 113.5(10) . . ? C26 C25 C27 114.2(13) . . ? C26 C25 C28 107.6(13) . . ? C27 C25 C28 107.3(12) . . ? C26 C25 C19 107.7(11) . . ? C27 C25 C19 111.9(12) . . ? C28 C25 C19 107.9(11) . . ? O3 C29 C34 119.4(7) . . ? O3 C29 C30 120.2(7) . . ? C34 C29 C30 120.2(8) . . ? C29 C30 C31 122.0(9) . . ? C32 C31 C30 116.5(10) . . ? C32 C31 C35 123.8(10) . . ? C30 C31 C35 119.7(10) . . ? C31 C32 C33 123.6(10) . . ? C34 C33 C32 117.0(9) . . ? C34 C33 C39 123.9(9) . . ? C32 C33 C39 119.1(9) . . ? C29 C34 C33 120.4(8) . . ? C36 C35 C37 104(2) . . ? C36 C35 C38 106.7(17) . . ? C37 C35 C38 120(2) . . ? C36 C35 C31 119.0(16) . . ? C37 C35 C31 103.4(17) . . ? C38 C35 C31 104.7(14) . . ? C41 C39 C33 115.5(13) . . ? C41 C39 C42 102.8(13) . . ? C33 C39 C42 109.6(11) . . ? C41 C39 C40 108.9(13) . . ? C33 C39 C40 110.3(11) . . ? C42 C39 C40 109.5(12) . . ? O4 C43 C48 121.5(6) . . ? O4 C43 C44 119.3(7) . . ? C48 C43 C44 119.2(7) . . ? C45 C44 C43 120.8(9) . . ? C44 C45 C46 117.1(11) . . ? C44 C45 C49 123.4(11) . . ? C46 C45 C49 118.7(12) . . ? C47 C46 C45 123.5(12) . . ? C46 C47 C48 117.3(10) . . ? C46 C47 C53 121.0(10) . . ? C48 C47 C53 121.4(9) . . ? C47 C48 C43 121.9(8) . . ? C50 C49 C52 121.1(17) . . ? C50 C49 C45 107.8(15) . . ? C52 C49 C45 101.3(14) . . ? C50 C49 C51 97.2(15) . . ? C52 C49 C51 120.2(17) . . ? C45 C49 C51 108.8(14) . . ? C55 C53 C56 115.5(14) . . ? C55 C53 C47 116.9(15) . . ? C56 C53 C47 113.1(10) . . ? C55 C53 C54 103.1(13) . . ? C56 C53 C54 104.7(12) . . ? C47 C53 C54 100.9(15) . . ? C58 C57 C62 121.8(6) . . ? C58 C57 O5 117.7(5) . . ? C62 C57 O5 120.4(5) . . ? C57 C58 C59 119.3(6) . . ? C58 C59 C60 118.4(7) . . ? C58 C59 C63 121.4(6) . . ? C60 C59 C63 120.1(6) . . ? C61 C60 C59 121.8(7) . . ? C60 C61 C62 119.4(7) . . ? C60 C61 C67 120.7(7) . . ? C62 C61 C67 119.9(7) . . ? C57 C62 C61 119.2(6) . . ? C66 C63 C64 111.2(8) . . ? C66 C63 C65 105.9(8) . . ? C64 C63 C65 109.8(8) . . ? C66 C63 C59 113.7(7) . . ? C64 C63 C59 108.4(7) . . ? C65 C63 C59 107.7(7) . . ? C69 C67 C70 109.7(10) . . ? C69 C67 C61 108.1(8) . . ? C70 C67 C61 111.5(8) . . ? C69 C67 C68 114.9(10) . . ? C70 C67 C68 106.3(10) . . ? C61 C67 C68 106.3(8) . . ? O6 C71 C76 120.4(5) . . ? O6 C71 C72 120.7(5) . . ? C76 C71 C72 118.8(5) . . ? C73 C72 C71 120.6(5) . . ? C72 C73 C74 118.9(6) . . ? C72 C73 C77 119.9(6) . . ? C74 C73 C77 121.1(6) . . ? C75 C74 C73 121.4(6) . . ? C76 C75 C74 118.2(6) . . ? C76 C75 C81 120.6(5) . . ? C74 C75 C81 121.1(6) . . ? C75 C76 C71 121.9(5) . . ? C80 C77 C78 114.5(10) . . ? C80 C77 C73 112.4(8) . . ? C78 C77 C73 108.5(8) . . ? C80 C77 C79 106.9(9) . . ? C78 C77 C79 102.0(9) . . ? C73 C77 C79 112.0(7) . . ? C82 C81 C84 107.8(6) . . ? C82 C81 C83 108.7(6) . . ? C84 C81 C83 107.7(6) . . ? C82 C81 C75 108.5(6) . . ? C84 C81 C75 113.3(6) . . ? C83 C81 C75 110.8(6) . . ? O7 C85 C90 121.1(6) . . ? O7 C85 C86 119.7(6) . . ? C90 C85 C86 119.2(7) . . ? C87 C86 C85 122.3(8) . . ? C86 C87 C88 116.5(8) . . ? C86 C87 C91 123.3(9) . . ? C88 C87 C91 120.2(8) . . ? C89 C88 C87 122.5(8) . . ? C88 C89 C90 118.8(8) . . ? C88 C89 C95 122.6(8) . . ? C90 C89 C95 118.5(7) . . ? C85 C90 C89 120.7(7) . . ? C93 C91 C94 110.5(11) . . ? C93 C91 C87 112.1(10) . . ? C94 C91 C87 107.9(9) . . ? C93 C91 C92 105.3(10) . . ? C94 C91 C92 111.9(10) . . ? C87 C91 C92 109.2(10) . . ? C96 C95 C97 112.5(9) . . ? C96 C95 C98 107.7(9) . . ? C97 C95 C98 106.2(9) . . ? C96 C95 C89 109.4(8) . . ? C97 C95 C89 112.3(8) . . ? C98 C95 C89 108.6(8) . . ? O8 C99 C104 120.3(5) . . ? O8 C99 C100 120.0(5) . . ? C104 C99 C100 119.7(6) . . ? C99 C100 C101 120.8(6) . . ? C100 C101 C102 117.3(7) . . ? C100 C101 C105 118.5(7) . . ? C102 C101 C105 124.2(7) . . ? C103 C102 C101 122.6(7) . . ? C102 C103 C104 117.7(6) . . ? C102 C103 C109 122.0(6) . . ? C104 C103 C109 120.2(6) . . ? C99 C104 C103 121.9(6) . . ? C108 C105 C107 111.8(8) . . ? C108 C105 C106 109.5(8) . . ? C107 C105 C106 104.0(7) . . ? C108 C105 C101 111.3(7) . . ? C107 C105 C101 111.2(7) . . ? C106 C105 C101 108.6(7) . . ? C111 C109 C110 103.8(12) . . ? C111 C109 C112 110.7(12) . . ? C110 C109 C112 110.1(11) . . ? C111 C109 C103 114.3(10) . . ? C110 C109 C103 108.9(9) . . ? C112 C109 C103 108.9(9) . . ? C118 C113 C114 120.5(5) . . ? C118 C113 O9 118.4(5) . . ? C114 C113 O9 120.9(5) . . ? C113 C114 C115 120.6(5) . . ? C116 C115 C114 118.0(6) . . ? C116 C115 C119 119.0(6) . . ? C114 C115 C119 123.0(5) . . ? C115 C116 C117 121.8(6) . . ? C118 C117 C116 118.1(6) . . ? C118 C117 C123 122.1(6) . . ? C116 C117 C123 119.8(7) . . ? C113 C118 C117 121.1(6) . . ? C120 C119 C121 110.0(6) . . ? C120 C119 C115 109.8(6) . . ? C121 C119 C115 109.5(5) . . ? C120 C119 C122 109.2(6) . . ? C121 C119 C122 106.8(6) . . ? C115 C119 C122 111.5(5) . . ? C126 C123 C117 108.4(10) . . ? C126 C123 C224 63.4(14) . . ? C117 C123 C224 116.2(13) . . ? C126 C123 C124 116.9(14) . . ? C117 C123 C124 107.9(11) . . ? C224 C123 C124 54.6(14) . . ? C126 C123 C225 126.7(14) . . ? C117 C123 C225 112.4(11) . . ? C224 C123 C225 121.4(16) . . ? C124 C123 C225 81.1(14) . . ? C126 C123 C226 48.8(13) . . ? C117 C123 C226 103.6(13) . . ? C224 C123 C226 108.9(17) . . ? C124 C123 C226 148.4(16) . . ? C225 C123 C226 88.7(16) . . ? C126 C123 C125 102.1(12) . . ? C117 C123 C125 112.8(9) . . ? C224 C123 C125 130.9(15) . . ? C124 C123 C125 108.9(13) . . ? C225 C123 C125 30.1(10) . . ? C226 C123 C125 58.8(13) . . ? O10 C127 C128 120.4(5) . . ? O10 C127 C132 119.6(5) . . ? C128 C127 C132 119.8(5) . . ? C127 C128 C129 120.7(6) . . ? C130 C129 C128 118.0(6) . . ? C130 C129 C133 122.3(6) . . ? C128 C129 C133 119.7(6) . . ? C129 C130 C131 122.5(6) . . ? C130 C131 C132 119.2(6) . . ? C130 C131 C137 122.9(6) . . ? C132 C131 C137 117.9(6) . . ? C131 C132 C127 119.8(6) . . ? C135 C133 C129 112.3(7) . . ? C135 C133 C136 108.8(8) . . ? C129 C133 C136 108.7(7) . . ? C135 C133 C134 109.2(8) . . ? C129 C133 C134 107.6(7) . . ? C136 C133 C134 110.2(8) . . ? C140 C137 C138 107.6(7) . . ? C140 C137 C139 109.9(6) . . ? C138 C137 C139 109.1(6) . . ? C140 C137 C131 109.7(6) . . ? C138 C137 C131 112.2(6) . . ? C139 C137 C131 108.4(6) . . ? O11 C141 C146 121.1(5) . . ? O11 C141 C142 119.7(5) . . ? C146 C141 C142 119.2(5) . . ? O11 C141 Nd1 55.2(2) . . ? C146 C141 Nd1 127.3(4) . . ? C142 C141 Nd1 86.3(3) . . ? C143 C142 C141 121.2(6) . . ? C144 C143 C142 118.4(6) . . ? C144 C143 C147 120.3(6) . . ? C142 C143 C147 121.3(6) . . ? C143 C144 C145 122.3(7) . . ? C146 C145 C144 118.2(7) . . ? C146 C145 C151 119.8(7) . . ? C144 C145 C151 122.0(7) . . ? C145 C146 C141 120.7(6) . . ? C150 C147 C148 110.2(8) . . ? C150 C147 C143 112.2(6) . . ? C148 C147 C143 109.0(8) . . ? C150 C147 C149 105.0(8) . . ? C148 C147 C149 110.7(9) . . ? C143 C147 C149 109.8(8) . . ? C154 C151 C152 106.0(11) . . ? C154 C151 C145 112.6(10) . . ? C152 C151 C145 108.5(9) . . ? C154 C151 C153 117.3(11) . . ? C152 C151 C153 102.0(9) . . ? C145 C151 C153 109.5(8) . . ? C156 C155 C160 121.7(7) . . ? C156 C155 O12 118.4(7) . . ? C160 C155 O12 119.8(7) . . ? C155 C156 C157 120.5(7) . . ? C158 C157 C156 117.8(8) . . ? C158 C157 C161 122.5(8) . . ? C156 C157 C161 119.6(7) . . ? C157 C158 C159 122.1(9) . . ? C160 C159 C158 118.4(8) . . ? C160 C159 C165 120.2(8) . . ? C158 C159 C165 121.4(9) . . ? C155 C160 C159 119.4(8) . . ? C162 C161 C163 114.1(12) . . ? C162 C161 C164 109.3(12) . . ? C163 C161 C164 97.7(11) . . ? C162 C161 C157 112.3(11) . . ? C163 C161 C157 113.4(9) . . ? C164 C161 C157 108.7(9) . . ? C268 C165 C167 134.7(18) . . ? C268 C165 C266 123.0(17) . . ? C167 C165 C266 47.9(14) . . ? C268 C165 C159 110.3(15) . . ? C167 C165 C159 112.2(13) . . ? C266 C165 C159 114.2(13) . . ? C268 C165 C168 36.9(13) . . ? C167 C165 C168 109.1(15) . . ? C266 C165 C168 132.1(15) . . ? C159 C165 C168 113.6(11) . . ? C268 C165 C267 103(2) . . ? C167 C165 C267 47.8(16) . . ? C266 C165 C267 93.7(19) . . ? C159 C165 C267 110.1(15) . . ? C168 C165 C267 66.9(16) . . ? C268 C165 C166 65.4(17) . . ? C167 C165 C166 115.2(18) . . ? C266 C165 C166 69.4(16) . . ? C159 C165 C166 106.1(14) . . ? C168 C165 C166 100.1(15) . . ? C267 C165 C166 143.7(19) . . ? C170 C169 O13 106.5(7) . . ? C169 C170 C171 100.7(9) . . ? C172 C171 C170 101.0(8) . . ? O13 C172 C171 106.0(7) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.289 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.132