Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chi-Tien Chen' _publ_contact_author_address ; Department of Chemistry National Chung Hsing University 250 Kuo Kuang Rd. Taichung 402 TAIWAN ; _publ_contact_author_email CTCHEN@DRAGON.NCHU.EDU.TW _publ_section_title ; Lithium Complexes Supported by Amine Bis-Phenolate Ligands as Efficient Catalysts for Ring-Opening Polymerization of L-Lactide ; loop_ _publ_author_name 'Chi-Tien Chen' 'Chi-An Huang' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 654617' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H108 Li4 N4 O4' _chemical_formula_weight 1073.34 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9896(7) _cell_length_b 32.351(2) _cell_length_c 19.9026(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.376(2) _cell_angle_gamma 90.00 _cell_volume 7044.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4953 _cell_measurement_theta_min 2.247 _cell_measurement_theta_max 21.309 _exptl_crystal_description parallelpiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.412 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40121 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.1032 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.01 _reflns_number_total 13822 _reflns_number_gt 5672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 13822 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1639 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.5818(5) 0.18639(16) 0.6098(2) 0.0514(13) Uani 1 1 d . . . Li2 Li 0.7073(5) 0.14921(16) 0.6972(3) 0.0586(14) Uani 1 1 d . . . Li3 Li 0.6878(5) 0.12144(15) 0.8770(2) 0.0486(12) Uani 1 1 d . . . Li4 Li 0.6249(5) 0.17535(17) 0.7971(3) 0.0595(15) Uani 1 1 d . . . O1 O 0.67100(19) 0.13601(6) 0.61176(10) 0.0561(6) Uani 1 1 d . . . O2 O 0.61105(18) 0.19834(6) 0.70877(9) 0.0459(5) Uani 1 1 d . . . O3 O 0.56231(18) 0.16183(6) 0.87241(9) 0.0496(5) Uani 1 1 d . . . O4 O 0.74818(17) 0.13452(6) 0.78863(9) 0.0453(5) Uani 1 1 d . . . N1 N 0.4102(2) 0.16411(7) 0.61244(12) 0.0478(6) Uani 1 1 d . . . N2 N 0.5173(3) 0.21954(10) 0.52150(14) 0.0673(8) Uani 1 1 d . . . N3 N 0.5898(2) 0.07067(7) 0.84701(11) 0.0429(6) Uani 1 1 d . . . N4 N 0.7548(3) 0.08788(8) 0.96480(12) 0.0559(7) Uani 1 1 d . . . C1 C 0.6263(3) 0.11278(9) 0.55988(15) 0.0514(8) Uani 1 1 d . . . C2 C 0.7031(3) 0.09558(10) 0.51335(15) 0.0556(9) Uani 1 1 d . . . C3 C 0.6460(4) 0.07440(10) 0.45855(17) 0.0651(10) Uani 1 1 d . . . H3A H 0.6954 0.0640 0.4271 0.078 Uiso 1 1 calc R . . C4 C 0.5217(4) 0.06755(10) 0.44693(17) 0.0667(10) Uani 1 1 d . . . C5 C 0.4501(3) 0.08332(10) 0.49466(18) 0.0655(10) Uani 1 1 d . . . H5A H 0.3661 0.0791 0.4891 0.079 Uiso 1 1 calc R . . C6 C 0.5001(3) 0.10524(9) 0.55059(16) 0.0533(8) Uani 1 1 d . . . C7 C 0.4206(3) 0.11910(9) 0.60410(17) 0.0596(9) Uani 1 1 d . . . H7A H 0.3393 0.1079 0.5934 0.072 Uiso 1 1 calc R . . H7B H 0.4529 0.1073 0.6469 0.072 Uiso 1 1 calc R . . C8 C 0.3673(3) 0.17476(9) 0.67866(16) 0.0528(8) Uani 1 1 d . . . H8A H 0.4018 0.1553 0.7123 0.063 Uiso 1 1 calc R . . H8B H 0.2790 0.1720 0.6757 0.063 Uiso 1 1 calc R . . C9 C 0.4018(3) 0.21803(8) 0.70136(14) 0.0434(7) Uani 1 1 d . . . C10 C 0.3122(3) 0.24685(9) 0.71091(15) 0.0490(8) Uani 1 1 d . . . H10A H 0.2305 0.2395 0.7016 0.059 Uiso 1 1 calc R . . C11 C 0.3409(3) 0.28665(9) 0.73419(15) 0.0474(8) Uani 1 1 d . . . C12 C 0.4640(3) 0.29642(9) 0.74479(15) 0.0500(8) Uani 1 1 d . . . H12A H 0.4847 0.3232 0.7583 0.060 Uiso 1 1 calc R . . C13 C 0.5590(3) 0.26891(9) 0.73665(14) 0.0437(7) Uani 1 1 d . . . C14 C 0.5264(3) 0.22821(9) 0.71549(13) 0.0425(7) Uani 1 1 d . . . C15 C 0.3352(3) 0.18431(11) 0.55702(17) 0.0622(9) Uani 1 1 d . . . H15A H 0.2694 0.1658 0.5408 0.075 Uiso 1 1 calc R . . H15B H 0.2988 0.2090 0.5741 0.075 Uiso 1 1 calc R . . C16 C 0.4049(4) 0.19566(14) 0.50044(19) 0.0848(12) Uani 1 1 d . . . H16A H 0.3530 0.2120 0.4684 0.102 Uiso 1 1 calc R . . H16B H 0.4273 0.1707 0.4776 0.102 Uiso 1 1 calc R . . C17 C 0.5948(4) 0.21544(16) 0.4655(2) 0.1133(17) Uani 1 1 d . . . H17A H 0.5598 0.2311 0.4275 0.170 Uiso 1 1 calc R . . H17B H 0.5999 0.1869 0.4531 0.170 Uiso 1 1 calc R . . H17C H 0.6752 0.2257 0.4794 0.170 Uiso 1 1 calc R . . C18 C 0.4929(5) 0.26242(13) 0.5339(2) 0.1161(17) Uani 1 1 d . . . H18A H 0.4635 0.2756 0.4922 0.174 Uiso 1 1 calc R . . H18B H 0.5667 0.2757 0.5522 0.174 Uiso 1 1 calc R . . H18C H 0.4322 0.2646 0.5654 0.174 Uiso 1 1 calc R . . C19 C 0.4645(4) 0.04477(13) 0.3846(2) 0.0891(13) Uani 1 1 d . . . C20 C 0.3589(8) 0.0207(3) 0.3971(3) 0.249(5) Uani 1 1 d . . . H20A H 0.2935 0.0389 0.4066 0.373 Uiso 1 1 calc R . . H20B H 0.3788 0.0029 0.4351 0.373 Uiso 1 1 calc R . . H20C H 0.3338 0.0044 0.3580 0.373 Uiso 1 1 calc R . . C21 C 0.4470(11) 0.0702(2) 0.3288(3) 0.330(8) Uani 1 1 d . . . H21A H 0.3919 0.0921 0.3378 0.495 Uiso 1 1 calc R . . H21B H 0.4128 0.0544 0.2908 0.495 Uiso 1 1 calc R . . H21C H 0.5239 0.0816 0.3191 0.495 Uiso 1 1 calc R . . C22 C 0.5500(8) 0.0095(3) 0.3693(5) 0.295(6) Uani 1 1 d . . . H22A H 0.5159 -0.0053 0.3302 0.442 Uiso 1 1 calc R . . H22B H 0.5595 -0.0090 0.4072 0.442 Uiso 1 1 calc R . . H22C H 0.6282 0.0206 0.3610 0.442 Uiso 1 1 calc R . . C23 C 0.8422(3) 0.09912(11) 0.52459(17) 0.0663(10) Uani 1 1 d . . . C24 C 0.9073(4) 0.07718(14) 0.4688(2) 0.1045(15) Uani 1 1 d . . . H24A H 0.8840 0.0486 0.4667 0.157 Uiso 1 1 calc R . . H24B H 0.9942 0.0793 0.4790 0.157 Uiso 1 1 calc R . . H24C H 0.8841 0.0901 0.4261 0.157 Uiso 1 1 calc R . . C25 C 0.8873(4) 0.07845(12) 0.59150(19) 0.0828(12) Uani 1 1 d . . . H25A H 0.8490 0.0913 0.6276 0.124 Uiso 1 1 calc R . . H25B H 0.9743 0.0815 0.5994 0.124 Uiso 1 1 calc R . . H25C H 0.8668 0.0496 0.5895 0.124 Uiso 1 1 calc R . . C26 C 0.8829(4) 0.14454(12) 0.5253(2) 0.0843(12) Uani 1 1 d . . . H26A H 0.8451 0.1592 0.5598 0.127 Uiso 1 1 calc R . . H26B H 0.8590 0.1568 0.4822 0.127 Uiso 1 1 calc R . . H26C H 0.9702 0.1460 0.5344 0.127 Uiso 1 1 calc R . . C27 C 0.2425(3) 0.31864(10) 0.74687(16) 0.0565(9) Uani 1 1 d . . . C28 C 0.1243(5) 0.29986(18) 0.7540(5) 0.239(5) Uani 1 1 d . . . H28A H 0.0661 0.3210 0.7619 0.359 Uiso 1 1 calc R . . H28B H 0.1314 0.2810 0.7914 0.359 Uiso 1 1 calc R . . H28C H 0.0973 0.2851 0.7135 0.359 Uiso 1 1 calc R . . C29 C 0.2343(7) 0.3499(2) 0.6942(4) 0.231(5) Uani 1 1 d . . . H29A H 0.1725 0.3697 0.7027 0.347 Uiso 1 1 calc R . . H29B H 0.2134 0.3370 0.6512 0.347 Uiso 1 1 calc R . . H29C H 0.3116 0.3637 0.6939 0.347 Uiso 1 1 calc R . . C30 C 0.2751(5) 0.3406(2) 0.8121(3) 0.181(3) Uani 1 1 d . . . H30A H 0.2128 0.3604 0.8194 0.271 Uiso 1 1 calc R . . H30B H 0.3519 0.3545 0.8104 0.271 Uiso 1 1 calc R . . H30C H 0.2817 0.3209 0.8483 0.271 Uiso 1 1 calc R . . C31 C 0.6929(3) 0.28220(10) 0.75119(16) 0.0535(8) Uani 1 1 d . . . C32 C 0.7617(3) 0.27581(11) 0.68865(17) 0.0687(10) Uani 1 1 d . . . H32A H 0.7559 0.2473 0.6751 0.103 Uiso 1 1 calc R . . H32B H 0.8461 0.2831 0.6990 0.103 Uiso 1 1 calc R . . H32C H 0.7263 0.2930 0.6526 0.103 Uiso 1 1 calc R . . C33 C 0.7552(3) 0.25691(12) 0.80983(17) 0.0730(11) Uani 1 1 d . . . H33A H 0.7494 0.2280 0.7990 0.109 Uiso 1 1 calc R . . H33B H 0.7155 0.2622 0.8499 0.109 Uiso 1 1 calc R . . H33C H 0.8397 0.2647 0.8173 0.109 Uiso 1 1 calc R . . C34 C 0.7052(4) 0.32788(11) 0.7709(2) 0.0872(13) Uani 1 1 d . . . H34A H 0.6628 0.3329 0.8102 0.131 Uiso 1 1 calc R . . H34B H 0.6704 0.3447 0.7343 0.131 Uiso 1 1 calc R . . H34C H 0.7901 0.3347 0.7807 0.131 Uiso 1 1 calc R . . C35 C 0.4810(3) 0.14840(9) 0.91345(14) 0.0427(7) Uani 1 1 d . . . C36 C 0.4484(3) 0.17214(8) 0.96893(14) 0.0442(7) Uani 1 1 d . . . C37 C 0.3730(3) 0.15358(9) 1.01229(15) 0.0477(8) Uani 1 1 d . . . H37A H 0.3526 0.1689 1.0492 0.057 Uiso 1 1 calc R . . C38 C 0.3253(3) 0.11366(9) 1.00462(15) 0.0466(8) Uani 1 1 d . . . C39 C 0.3531(3) 0.09247(9) 0.94781(15) 0.0484(8) Uani 1 1 d . . . H39A H 0.3196 0.0664 0.9394 0.058 Uiso 1 1 calc R . . C40 C 0.4296(3) 0.10893(9) 0.90264(14) 0.0431(7) Uani 1 1 d . . . C41 C 0.4600(3) 0.08405(10) 0.84222(15) 0.0501(8) Uani 1 1 d . . . H41A H 0.4078 0.0598 0.8380 0.060 Uiso 1 1 calc R . . H41B H 0.4427 0.1006 0.8018 0.060 Uiso 1 1 calc R . . C42 C 0.6285(3) 0.05819(9) 0.78051(14) 0.0482(8) Uani 1 1 d . . . H42A H 0.5890 0.0758 0.7456 0.058 Uiso 1 1 calc R . . H42B H 0.6030 0.0299 0.7708 0.058 Uiso 1 1 calc R . . C43 C 0.7653(3) 0.06137(9) 0.77967(14) 0.0448(7) Uani 1 1 d . . . C44 C 0.8363(3) 0.02633(10) 0.77418(15) 0.0521(8) Uani 1 1 d . . . H44A H 0.7981 0.0007 0.7698 0.063 Uiso 1 1 calc R . . C45 C 0.9629(3) 0.02835(10) 0.77498(15) 0.0554(9) Uani 1 1 d . . . C46 C 1.0146(3) 0.06738(10) 0.78278(16) 0.0560(9) Uani 1 1 d . . . H46A H 1.0993 0.0693 0.7842 0.067 Uiso 1 1 calc R . . C47 C 0.9491(3) 0.10387(9) 0.78867(14) 0.0460(8) Uani 1 1 d . . . C48 C 0.8203(3) 0.10073(9) 0.78535(13) 0.0425(7) Uani 1 1 d . . . C49 C 0.6178(3) 0.03894(9) 0.89858(15) 0.0511(8) Uani 1 1 d . . . H49A H 0.6831 0.0215 0.8852 0.061 Uiso 1 1 calc R . . H49B H 0.5463 0.0217 0.9015 0.061 Uiso 1 1 calc R . . C50 C 0.6559(3) 0.05728(10) 0.96758(16) 0.0580(9) Uani 1 1 d . . . H50A H 0.5858 0.0705 0.9848 0.070 Uiso 1 1 calc R . . H50B H 0.6832 0.0353 0.9985 0.070 Uiso 1 1 calc R . . C51 C 0.7662(4) 0.11287(12) 1.02658(18) 0.0904(13) Uani 1 1 d . . . H51A H 0.7976 0.0960 1.0640 0.136 Uiso 1 1 calc R . . H51B H 0.6874 0.1235 1.0349 0.136 Uiso 1 1 calc R . . H51C H 0.8211 0.1355 1.0213 0.136 Uiso 1 1 calc R . . C52 C 0.8714(3) 0.06682(11) 0.95762(18) 0.0723(10) Uani 1 1 d . . . H52A H 0.8975 0.0526 0.9988 0.108 Uiso 1 1 calc R . . H52B H 0.9320 0.0868 0.9481 0.108 Uiso 1 1 calc R . . H52C H 0.8608 0.0473 0.9212 0.108 Uiso 1 1 calc R . . C53 C 0.2478(3) 0.09579(9) 1.05715(17) 0.0554(9) Uani 1 1 d . . . C54 C 0.1961(3) 0.05327(10) 1.0361(2) 0.0767(12) Uani 1 1 d . . . H54A H 0.1454 0.0557 0.9943 0.115 Uiso 1 1 calc R . . H54B H 0.1483 0.0429 1.0704 0.115 Uiso 1 1 calc R . . H54C H 0.2622 0.0346 1.0303 0.115 Uiso 1 1 calc R . . C55 C 0.3278(4) 0.09109(13) 1.12422(19) 0.0868(13) Uani 1 1 d . . . H55A H 0.3955 0.0732 1.1179 0.130 Uiso 1 1 calc R . . H55B H 0.2800 0.0794 1.1575 0.130 Uiso 1 1 calc R . . H55C H 0.3577 0.1177 1.1392 0.130 Uiso 1 1 calc R . . C56 C 0.1399(3) 0.12445(10) 1.06773(18) 0.0661(10) Uani 1 1 d . . . H56A H 0.0888 0.1271 1.0261 0.099 Uiso 1 1 calc R . . H56B H 0.1703 0.1512 1.0820 0.099 Uiso 1 1 calc R . . H56C H 0.0933 0.1130 1.1016 0.099 Uiso 1 1 calc R . . C57 C 0.4905(3) 0.21709(9) 0.97829(16) 0.0528(8) Uani 1 1 d . . . C58 C 0.4428(4) 0.23715(10) 1.04038(18) 0.0741(11) Uani 1 1 d . . . H58A H 0.3551 0.2361 1.0363 0.111 Uiso 1 1 calc R . . H58B H 0.4691 0.2654 1.0436 0.111 Uiso 1 1 calc R . . H58C H 0.4742 0.2225 1.0802 0.111 Uiso 1 1 calc R . . C59 C 0.4413(4) 0.24217(10) 0.91618(17) 0.0737(11) Uani 1 1 d . . . H59A H 0.4694 0.2301 0.8764 0.111 Uiso 1 1 calc R . . H59B H 0.4700 0.2701 0.9208 0.111 Uiso 1 1 calc R . . H59C H 0.3536 0.2419 0.9125 0.111 Uiso 1 1 calc R . . C60 C 0.6299(3) 0.22032(11) 0.98777(19) 0.0725(10) Uani 1 1 d . . . H60A H 0.6639 0.2083 0.9496 0.109 Uiso 1 1 calc R . . H60B H 0.6601 0.2058 1.0280 0.109 Uiso 1 1 calc R . . H60C H 0.6533 0.2489 0.9916 0.109 Uiso 1 1 calc R . . C61 C 1.0424(3) -0.00986(11) 0.7673(2) 0.0701(10) Uani 1 1 d . . . C62 C 1.1296(6) -0.01528(19) 0.8283(4) 0.199(3) Uani 1 1 d . . . H62A H 1.1790 -0.0393 0.8230 0.298 Uiso 1 1 calc R . . H62B H 1.0851 -0.0187 0.8672 0.298 Uiso 1 1 calc R . . H62C H 1.1812 0.0086 0.8342 0.298 Uiso 1 1 calc R . . C63 C 0.9701(5) -0.04888(15) 0.7606(5) 0.205(4) Uani 1 1 d . . . H63A H 1.0242 -0.0718 0.7563 0.307 Uiso 1 1 calc R . . H63B H 0.9126 -0.0473 0.7213 0.307 Uiso 1 1 calc R . . H63C H 0.9270 -0.0526 0.8000 0.307 Uiso 1 1 calc R . . C64 C 1.1142(7) -0.00472(18) 0.7087(3) 0.209(4) Uani 1 1 d . . . H64A H 1.1643 -0.0287 0.7043 0.313 Uiso 1 1 calc R . . H64B H 1.1652 0.0193 0.7151 0.313 Uiso 1 1 calc R . . H64C H 1.0597 -0.0014 0.6684 0.313 Uiso 1 1 calc R . . C65 C 1.0150(3) 0.14589(10) 0.79619(16) 0.0543(8) Uani 1 1 d . . . C66 C 0.9862(3) 0.16750(11) 0.86097(18) 0.0757(11) Uani 1 1 d . . . H66A H 1.0096 0.1500 0.8989 0.113 Uiso 1 1 calc R . . H66B H 0.9001 0.1731 0.8590 0.113 Uiso 1 1 calc R . . H66C H 1.0307 0.1930 0.8657 0.113 Uiso 1 1 calc R . . C67 C 0.9776(3) 0.17360(10) 0.73550(17) 0.0692(10) Uani 1 1 d . . . H67A H 0.8905 0.1773 0.7313 0.104 Uiso 1 1 calc R . . H67B H 1.0018 0.1609 0.6952 0.104 Uiso 1 1 calc R . . H67C H 1.0169 0.2000 0.7418 0.104 Uiso 1 1 calc R . . C68 C 1.1554(3) 0.14120(12) 0.8009(2) 0.0863(13) Uani 1 1 d . . . H68A H 1.1819 0.1239 0.8387 0.129 Uiso 1 1 calc R . . H68B H 1.1929 0.1679 0.8069 0.129 Uiso 1 1 calc R . . H68C H 1.1787 0.1289 0.7602 0.129 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 Li1 0.051(3) 0.064(3) 0.039(3) 0.004(3) 0.006(2) -0.001(3) Li2 0.072(4) 0.060(3) 0.042(3) -0.008(3) -0.002(3) 0.008(3) Li3 0.053(3) 0.053(3) 0.040(3) 0.003(2) 0.006(2) 0.001(2) Li4 0.072(4) 0.066(3) 0.041(3) 0.004(3) 0.015(3) 0.011(3) O1 0.0648(15) 0.0586(13) 0.0440(13) -0.0127(11) -0.0002(11) 0.0057(11) O2 0.0521(13) 0.0465(11) 0.0392(11) 0.0004(9) 0.0057(9) 0.0068(10) O3 0.0581(13) 0.0497(12) 0.0436(12) 0.0044(10) 0.0189(10) 0.0046(10) O4 0.0466(12) 0.0476(12) 0.0419(12) 0.0028(9) 0.0045(9) 0.0078(10) N1 0.0549(16) 0.0435(15) 0.0447(15) 0.0006(12) 0.0035(12) -0.0025(12) N2 0.0561(19) 0.084(2) 0.0612(19) 0.0251(16) 0.0020(15) -0.0031(17) N3 0.0402(14) 0.0480(14) 0.0403(14) -0.0038(12) 0.0027(11) 0.0049(12) N4 0.0662(19) 0.0546(16) 0.0447(16) -0.0020(13) -0.0060(13) 0.0058(15) C1 0.072(2) 0.0459(18) 0.0356(18) -0.0057(15) -0.0015(16) 0.0018(17) C2 0.074(2) 0.054(2) 0.0397(19) -0.0057(16) 0.0057(17) 0.0055(18) C3 0.091(3) 0.060(2) 0.044(2) -0.0110(17) 0.0075(19) 0.004(2) C4 0.092(3) 0.055(2) 0.053(2) -0.0169(18) 0.001(2) -0.004(2) C5 0.074(3) 0.056(2) 0.064(2) -0.0062(19) -0.008(2) -0.0054(19) C6 0.065(2) 0.0451(18) 0.049(2) -0.0074(16) 0.0035(17) -0.0004(17) C7 0.069(2) 0.049(2) 0.060(2) -0.0050(16) 0.0048(18) -0.0099(17) C8 0.052(2) 0.055(2) 0.053(2) -0.0018(16) 0.0120(16) -0.0060(16) C9 0.0477(19) 0.0418(17) 0.0417(18) 0.0016(14) 0.0091(14) 0.0009(15) C10 0.0446(19) 0.055(2) 0.0474(19) -0.0003(15) 0.0068(14) -0.0036(16) C11 0.052(2) 0.0473(18) 0.0440(18) 0.0013(15) 0.0084(15) 0.0035(16) C12 0.059(2) 0.0438(18) 0.0484(19) -0.0012(15) 0.0100(16) -0.0006(16) C13 0.0470(19) 0.0492(18) 0.0356(16) 0.0017(14) 0.0067(14) 0.0003(15) C14 0.053(2) 0.0454(18) 0.0297(16) 0.0054(13) 0.0085(14) 0.0029(15) C15 0.061(2) 0.064(2) 0.059(2) 0.0038(18) -0.0065(18) -0.0044(18) C16 0.083(3) 0.106(3) 0.064(3) 0.019(2) -0.003(2) 0.005(3) C17 0.103(4) 0.162(5) 0.079(3) 0.040(3) 0.028(3) 0.018(3) C18 0.174(5) 0.075(3) 0.095(3) 0.020(3) -0.013(3) 0.009(3) C19 0.121(4) 0.080(3) 0.062(3) -0.032(2) -0.012(2) -0.014(3) C20 0.303(11) 0.329(11) 0.116(5) -0.105(6) 0.030(6) -0.228(10) C21 0.71(2) 0.164(6) 0.078(4) 0.038(4) -0.178(8) -0.184(10) C22 0.257(10) 0.300(11) 0.303(11) -0.251(10) -0.101(8) 0.073(9) C23 0.072(3) 0.074(2) 0.053(2) -0.0127(19) 0.0096(18) 0.009(2) C24 0.100(3) 0.131(4) 0.085(3) -0.036(3) 0.026(3) 0.017(3) C25 0.081(3) 0.092(3) 0.074(3) -0.001(2) 0.000(2) 0.021(2) C26 0.082(3) 0.087(3) 0.086(3) -0.008(2) 0.018(2) -0.007(2) C27 0.059(2) 0.056(2) 0.055(2) -0.0041(17) 0.0089(17) 0.0119(17) C28 0.092(4) 0.122(5) 0.524(15) -0.088(7) 0.138(7) 0.005(4) C29 0.291(9) 0.212(7) 0.212(7) 0.134(6) 0.134(7) 0.196(7) C30 0.146(5) 0.222(7) 0.167(6) -0.110(5) -0.017(4) 0.105(5) C31 0.053(2) 0.057(2) 0.051(2) -0.0028(16) 0.0041(16) -0.0077(16) C32 0.063(2) 0.078(2) 0.067(2) 0.009(2) 0.0186(19) -0.0072(19) C33 0.059(2) 0.102(3) 0.055(2) 0.001(2) -0.0075(18) -0.013(2) C34 0.069(3) 0.070(3) 0.123(4) -0.021(2) 0.010(2) -0.018(2) C35 0.0436(18) 0.0457(18) 0.0395(17) 0.0069(14) 0.0075(14) 0.0040(14) C36 0.0464(18) 0.0440(17) 0.0430(17) 0.0027(14) 0.0084(14) 0.0067(14) C37 0.0539(19) 0.0455(18) 0.0455(18) -0.0009(15) 0.0138(15) 0.0027(15) C38 0.0449(18) 0.0458(18) 0.0504(19) 0.0037(15) 0.0110(15) 0.0006(15) C39 0.0417(18) 0.0497(18) 0.054(2) -0.0004(15) 0.0053(15) 0.0001(15) C40 0.0379(17) 0.0477(18) 0.0436(18) -0.0039(14) 0.0032(14) 0.0060(14) C41 0.0401(18) 0.0583(19) 0.0512(19) -0.0057(16) 0.0016(14) 0.0016(15) C42 0.0481(19) 0.0542(19) 0.0422(18) -0.0125(15) 0.0039(14) 0.0004(15) C43 0.0460(19) 0.0524(19) 0.0360(17) -0.0058(14) 0.0039(13) 0.0045(16) C44 0.059(2) 0.0492(19) 0.0485(19) -0.0062(15) 0.0096(16) 0.0065(17) C45 0.061(2) 0.057(2) 0.050(2) 0.0053(16) 0.0166(16) 0.0170(18) C46 0.049(2) 0.065(2) 0.056(2) 0.0110(17) 0.0136(16) 0.0105(18) C47 0.0417(18) 0.058(2) 0.0391(17) 0.0077(15) 0.0074(14) 0.0049(16) C48 0.0477(19) 0.0492(18) 0.0309(16) 0.0049(14) 0.0051(13) 0.0087(16) C49 0.0498(19) 0.0470(18) 0.056(2) 0.0030(16) 0.0042(16) -0.0001(15) C50 0.069(2) 0.057(2) 0.048(2) 0.0080(17) 0.0055(17) 0.0138(19) C51 0.130(4) 0.081(3) 0.055(2) -0.017(2) -0.020(2) 0.020(3) C52 0.061(2) 0.086(3) 0.068(2) 0.009(2) -0.0066(19) 0.006(2) C53 0.056(2) 0.052(2) 0.060(2) 0.0079(17) 0.0178(17) 0.0000(17) C54 0.087(3) 0.053(2) 0.096(3) 0.002(2) 0.039(2) -0.006(2) C55 0.081(3) 0.112(3) 0.068(3) 0.032(2) 0.011(2) -0.002(2) C56 0.062(2) 0.061(2) 0.078(3) -0.0027(19) 0.0250(19) -0.0018(18) C57 0.066(2) 0.0446(18) 0.050(2) -0.0009(15) 0.0179(17) 0.0017(16) C58 0.107(3) 0.050(2) 0.069(2) -0.0125(18) 0.034(2) -0.007(2) C59 0.100(3) 0.051(2) 0.074(3) 0.0139(19) 0.028(2) 0.012(2) C60 0.078(3) 0.068(2) 0.074(3) -0.010(2) 0.019(2) -0.016(2) C61 0.068(2) 0.065(2) 0.080(3) 0.008(2) 0.024(2) 0.029(2) C62 0.216(7) 0.151(6) 0.212(7) -0.025(5) -0.075(6) 0.127(5) C63 0.123(5) 0.070(3) 0.435(12) -0.030(5) 0.095(6) 0.028(3) C64 0.282(8) 0.147(5) 0.228(7) 0.060(5) 0.191(7) 0.133(6) C65 0.0456(19) 0.061(2) 0.056(2) 0.0075(17) 0.0050(16) -0.0023(16) C66 0.079(3) 0.082(3) 0.064(2) -0.006(2) -0.003(2) -0.016(2) C67 0.073(2) 0.068(2) 0.068(2) 0.0135(19) 0.0082(19) -0.0080(19) C68 0.052(2) 0.083(3) 0.124(4) 0.019(2) 0.004(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O1 1.900(6) . ? Li1 O2 2.004(5) . ? Li1 N1 2.024(6) . ? Li1 N2 2.123(6) . ? Li1 Li2 2.434(7) . ? Li1 C14 2.621(6) . ? Li1 C1 2.643(6) . ? Li2 O1 1.762(5) . ? Li2 O4 1.894(6) . ? Li2 O2 1.935(6) . ? Li2 Li4 2.414(7) . ? Li2 C48 2.583(6) . ? Li3 O3 1.896(5) . ? Li3 O4 1.983(5) . ? Li3 N3 2.023(6) . ? Li3 N4 2.129(5) . ? Li3 Li4 2.418(7) . ? Li3 C48 2.529(5) . ? Li3 C35 2.600(6) . ? Li4 O3 1.763(5) . ? Li4 O2 1.901(5) . ? Li4 O4 1.911(6) . ? Li4 C14 2.530(6) . ? O1 C1 1.333(3) . ? O2 C14 1.357(3) . ? O3 C35 1.339(3) . ? O4 C48 1.355(3) . ? N1 C15 1.467(4) . ? N1 C7 1.471(4) . ? N1 C8 1.482(4) . ? N2 C18 1.438(5) . ? N2 C17 1.470(5) . ? N2 C16 1.485(5) . ? N3 C49 1.464(4) . ? N3 C42 1.484(3) . ? N3 C41 1.485(3) . ? N4 C51 1.467(4) . ? N4 C52 1.470(4) . ? N4 C50 1.476(4) . ? C1 C6 1.404(4) . ? C1 C2 1.424(4) . ? C2 C3 1.388(4) . ? C2 C23 1.528(5) . ? C3 C4 1.382(5) . ? C3 H3A 0.9300 . ? C4 C5 1.386(5) . ? C4 C19 1.526(5) . ? C5 C6 1.389(4) . ? C5 H5A 0.9300 . ? C6 C7 1.507(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.508(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.382(4) . ? C9 C14 1.411(4) . ? C10 C11 1.394(4) . ? C10 H10A 0.9300 . ? C11 C12 1.387(4) . ? C11 C27 1.535(4) . ? C12 C13 1.392(4) . ? C12 H12A 0.9300 . ? C13 C14 1.418(4) . ? C13 C31 1.535(4) . ? C15 C16 1.466(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C21 1.380(7) . ? C19 C20 1.438(7) . ? C19 C22 1.527(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C25 1.530(5) . ? C23 C26 1.536(5) . ? C23 C24 1.548(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.453(6) . ? C27 C29 1.453(6) . ? C27 C30 1.493(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.529(4) . ? C31 C34 1.532(4) . ? C31 C33 1.533(4) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.404(4) . ? C35 C36 1.418(4) . ? C36 C37 1.388(4) . ? C36 C57 1.532(4) . ? C37 C38 1.397(4) . ? C37 H37A 0.9300 . ? C38 C39 1.381(4) . ? C38 C53 1.523(4) . ? C39 C40 1.393(4) . ? C39 H39A 0.9300 . ? C40 C41 1.510(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.508(4) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.386(4) . ? C43 C48 1.410(4) . ? C44 C45 1.392(4) . ? C44 H44A 0.9300 . ? C45 C46 1.388(4) . ? C45 C61 1.530(4) . ? C46 C47 1.394(4) . ? C46 H46A 0.9300 . ? C47 C48 1.414(4) . ? C47 C65 1.541(4) . ? C49 C50 1.518(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.532(4) . ? C53 C56 1.535(4) . ? C53 C55 1.535(5) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C60 1.530(5) . ? C57 C58 1.531(4) . ? C57 C59 1.534(4) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C64 1.478(6) . ? C61 C62 1.485(7) . ? C61 C63 1.491(6) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.526(4) . ? C65 C67 1.529(4) . ? C65 C68 1.545(4) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? 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 Li1 O2 96.3(2) . . ? O1 Li1 N1 100.0(2) . . ? O2 Li1 N1 96.1(2) . . ? O1 Li1 N2 125.6(3) . . ? O2 Li1 N2 136.6(3) . . ? N1 Li1 N2 87.8(2) . . ? O1 Li1 Li2 45.94(18) . . ? O2 Li1 Li2 50.57(17) . . ? N1 Li1 Li2 105.8(3) . . ? N2 Li1 Li2 164.6(3) . . ? O1 Li1 C14 125.7(2) . . ? O2 Li1 C14 30.57(11) . . ? N1 Li1 C14 82.86(19) . . ? N2 Li1 C14 108.6(2) . . ? Li2 Li1 C14 80.8(2) . . ? O1 Li1 C1 28.59(12) . . ? O2 Li1 C1 121.6(2) . . ? N1 Li1 C1 84.0(2) . . ? N2 Li1 C1 101.7(2) . . ? Li2 Li1 C1 73.2(2) . . ? C14 Li1 C1 146.3(2) . . ? O1 Li2 O4 151.4(3) . . ? O1 Li2 O2 103.7(3) . . ? O4 Li2 O2 100.0(2) . . ? O1 Li2 Li4 144.2(3) . . ? O4 Li2 Li4 50.94(19) . . ? O2 Li2 Li4 50.38(18) . . ? O1 Li2 Li1 50.83(19) . . ? O4 Li2 Li1 151.4(3) . . ? O2 Li2 Li1 53.12(19) . . ? Li4 Li2 Li1 100.6(3) . . ? O1 Li2 C48 124.0(3) . . ? O4 Li2 C48 30.59(12) . . ? O2 Li2 C48 130.6(2) . . ? Li4 Li2 C48 81.2(2) . . ? Li1 Li2 C48 171.7(3) . . ? O3 Li3 O4 96.5(2) . . ? O3 Li3 N3 100.4(2) . . ? O4 Li3 N3 97.2(2) . . ? O3 Li3 N4 125.8(3) . . ? O4 Li3 N4 135.9(3) . . ? N3 Li3 N4 87.8(2) . . ? O3 Li3 Li4 46.30(17) . . ? O4 Li3 Li4 50.29(17) . . ? N3 Li3 Li4 106.3(3) . . ? N4 Li3 Li4 164.5(3) . . ? O3 Li3 C48 127.8(2) . . ? O4 Li3 C48 32.16(11) . . ? N3 Li3 C48 84.19(19) . . ? N4 Li3 C48 106.2(2) . . ? Li4 Li3 C48 82.2(2) . . ? O3 Li3 C35 29.71(11) . . ? O4 Li3 C35 123.4(2) . . ? N3 Li3 C35 84.24(19) . . ? N4 Li3 C35 100.7(2) . . ? Li4 Li3 C35 74.8(2) . . ? C48 Li3 C35 150.2(2) . . ? O3 Li4 O2 151.6(4) . . ? O3 Li4 O4 103.9(3) . . ? O2 Li4 O4 100.7(2) . . ? O3 Li4 Li2 145.1(3) . . ? O2 Li4 Li2 51.64(18) . . ? O4 Li4 Li2 50.32(18) . . ? O3 Li4 Li3 51.04(18) . . ? O2 Li4 Li3 152.1(3) . . ? O4 Li4 Li3 52.97(18) . . ? Li2 Li4 Li3 100.5(3) . . ? O3 Li4 C14 122.4(3) . . ? O2 Li4 C14 31.80(12) . . ? O4 Li4 C14 132.5(2) . . ? Li2 Li4 C14 83.1(2) . . ? Li3 Li4 C14 171.3(3) . . ? C1 O1 Li2 156.6(3) . . ? C1 O1 Li1 108.4(2) . . ? Li2 O1 Li1 83.2(2) . . ? C14 O2 Li4 100.6(2) . . ? C14 O2 Li2 169.9(3) . . ? Li4 O2 Li2 78.0(2) . . ? C14 O2 Li1 100.7(2) . . ? Li4 O2 Li1 145.6(2) . . ? Li2 O2 Li1 76.3(2) . . ? C35 O3 Li4 159.4(3) . . ? C35 O3 Li3 105.7(2) . . ? Li4 O3 Li3 82.7(2) . . ? C48 O4 Li2 104.1(2) . . ? C48 O4 Li4 169.9(2) . . ? Li2 O4 Li4 78.7(2) . . ? C48 O4 Li3 96.7(2) . . ? Li2 O4 Li3 146.8(3) . . ? Li4 O4 Li3 76.7(2) . . ? C15 N1 C7 113.6(3) . . ? C15 N1 C8 111.2(2) . . ? C7 N1 C8 111.4(2) . . ? C15 N1 Li1 106.3(2) . . ? C7 N1 Li1 105.5(2) . . ? C8 N1 Li1 108.4(2) . . ? C18 N2 C17 110.3(3) . . ? C18 N2 C16 112.7(3) . . ? C17 N2 C16 105.4(3) . . ? C18 N2 Li1 113.5(3) . . ? C17 N2 Li1 114.2(3) . . ? C16 N2 Li1 100.1(2) . . ? C49 N3 C42 112.1(2) . . ? C49 N3 C41 112.8(2) . . ? C42 N3 C41 112.1(2) . . ? C49 N3 Li3 106.9(2) . . ? C42 N3 Li3 107.1(2) . . ? C41 N3 Li3 105.3(2) . . ? C51 N4 C52 109.3(3) . . ? C51 N4 C50 110.1(3) . . ? C52 N4 C50 110.2(2) . . ? C51 N4 Li3 113.8(2) . . ? C52 N4 Li3 113.2(2) . . ? C50 N4 Li3 100.0(2) . . ? O1 C1 C6 119.2(3) . . ? O1 C1 C2 121.8(3) . . ? C6 C1 C2 119.0(3) . . ? O1 C1 Li1 43.02(17) . . ? C6 C1 Li1 89.5(2) . . ? C2 C1 Li1 137.6(3) . . ? C3 C2 C1 116.9(3) . . ? C3 C2 C23 121.7(3) . . ? C1 C2 C23 121.4(3) . . ? C4 C3 C2 125.3(3) . . ? C4 C3 H3A 117.3 . . ? C2 C3 H3A 117.3 . . ? C3 C4 C5 116.2(3) . . ? C3 C4 C19 122.6(4) . . ? C5 C4 C19 121.1(4) . . ? C4 C5 C6 122.0(3) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 120.4(3) . . ? C5 C6 C7 120.4(3) . . ? C1 C6 C7 119.1(3) . . ? N1 C7 C6 115.5(3) . . ? N1 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? N1 C8 C9 112.9(2) . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C14 120.4(3) . . ? C10 C9 C8 120.3(3) . . ? C14 C9 C8 119.3(3) . . ? C9 C10 C11 121.8(3) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C12 C11 C10 116.6(3) . . ? C12 C11 C27 120.9(3) . . ? C10 C11 C27 122.4(3) . . ? C11 C12 C13 124.6(3) . . ? C11 C12 H12A 117.7 . . ? C13 C12 H12A 117.7 . . ? C12 C13 C14 117.2(3) . . ? C12 C13 C31 121.0(3) . . ? C14 C13 C31 121.8(3) . . ? O2 C14 C9 118.4(3) . . ? O2 C14 C13 122.3(3) . . ? C9 C14 C13 119.3(3) . . ? O2 C14 Li4 47.60(16) . . ? C9 C14 Li4 108.6(2) . . ? C13 C14 Li4 110.9(2) . . ? O2 C14 Li1 48.71(16) . . ? C9 C14 Li1 90.8(2) . . ? C13 C14 Li1 130.3(2) . . ? Li4 C14 Li1 92.79(19) . . ? C16 C15 N1 113.1(3) . . ? C16 C15 H15A 109.0 . . ? N1 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? N1 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 N2 113.2(3) . . ? C15 C16 H16A 108.9 . . ? N2 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? N2 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 114.0(6) . . ? C21 C19 C4 112.5(4) . . ? C20 C19 C4 113.5(4) . . ? C21 C19 C22 109.0(7) . . ? C20 C19 C22 98.7(6) . . ? C4 C19 C22 108.0(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 C25 109.4(3) . . ? C2 C23 C26 111.1(3) . . ? C25 C23 C26 109.9(3) . . ? C2 C23 C24 112.6(3) . . ? C25 C23 C24 106.9(3) . . ? C26 C23 C24 106.9(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 111.5(5) . . ? C28 C27 C30 104.9(5) . . ? C29 C27 C30 106.9(5) . . ? C28 C27 C11 112.6(3) . . ? C29 C27 C11 110.3(3) . . ? C30 C27 C11 110.3(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C34 107.5(3) . . ? C32 C31 C33 109.2(3) . . ? C34 C31 C33 107.3(3) . . ? C32 C31 C13 110.3(3) . . ? C34 C31 C13 112.2(3) . . ? C33 C31 C13 110.2(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C40 118.9(3) . . ? O3 C35 C36 122.1(3) . . ? C40 C35 C36 119.0(3) . . ? O3 C35 Li3 44.57(16) . . ? C40 C35 Li3 90.1(2) . . ? C36 C35 Li3 133.6(2) . . ? C37 C36 C35 117.3(3) . . ? C37 C36 C57 121.8(3) . . ? C35 C36 C57 120.9(2) . . ? C36 C37 C38 124.9(3) . . ? C36 C37 H37A 117.6 . . ? C38 C37 H37A 117.6 . . ? C39 C38 C37 116.0(3) . . ? C39 C38 C53 123.7(3) . . ? C37 C38 C53 120.3(3) . . ? C38 C39 C40 122.1(3) . . ? C38 C39 H39A 118.9 . . ? C40 C39 H39A 118.9 . . ? C39 C40 C35 120.4(3) . . ? C39 C40 C41 120.1(3) . . ? C35 C40 C41 119.4(3) . . ? N3 C41 C40 112.7(2) . . ? N3 C41 H41A 109.0 . . ? C40 C41 H41A 109.0 . . ? N3 C41 H41B 109.0 . . ? C40 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? N3 C42 C43 111.2(2) . . ? N3 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? N3 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C44 C43 C48 120.3(3) . . ? C44 C43 C42 120.9(3) . . ? C48 C43 C42 118.8(3) . . ? C43 C44 C45 122.0(3) . . ? C43 C44 H44A 119.0 . . ? C45 C44 H44A 119.0 . . ? C46 C45 C44 116.3(3) . . ? C46 C45 C61 121.0(3) . . ? C44 C45 C61 122.7(3) . . ? C45 C46 C47 124.8(3) . . ? C45 C46 H46A 117.6 . . ? C47 C46 H46A 117.6 . . ? C46 C47 C48 117.3(3) . . ? C46 C47 C65 120.9(3) . . ? C48 C47 C65 121.8(3) . . ? O4 C48 C43 119.0(3) . . ? O4 C48 C47 121.8(3) . . ? C43 C48 C47 119.2(3) . . ? O4 C48 Li3 51.16(16) . . ? C43 C48 Li3 91.5(2) . . ? C47 C48 Li3 126.1(2) . . ? O4 C48 Li2 45.34(16) . . ? C43 C48 Li2 108.6(2) . . ? C47 C48 Li2 113.8(2) . . ? Li3 C48 Li2 93.25(19) . . ? N3 C49 C50 112.5(2) . . ? N3 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? N3 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? N4 C50 C49 111.7(3) . . ? N4 C50 H50A 109.3 . . ? C49 C50 H50A 109.3 . . ? N4 C50 H50B 109.3 . . ? C49 C50 H50B 109.3 . . ? H50A C50 H50B 107.9 . . ? N4 C51 H51A 109.5 . . ? N4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N4 C52 H52A 109.5 . . ? N4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C38 C53 C54 111.7(3) . . ? C38 C53 C56 110.7(2) . . ? C54 C53 C56 108.0(3) . . ? C38 C53 C55 108.9(3) . . ? C54 C53 C55 108.5(3) . . ? C56 C53 C55 109.1(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C60 C57 C58 106.7(3) . . ? C60 C57 C36 111.6(3) . . ? C58 C57 C36 112.2(2) . . ? C60 C57 C59 109.7(3) . . ? C58 C57 C59 107.7(3) . . ? C36 C57 C59 108.9(3) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C64 C61 C62 107.9(5) . . ? C64 C61 C63 110.2(5) . . ? C62 C61 C63 105.7(5) . . ? C64 C61 C45 109.9(3) . . ? C62 C61 C45 110.2(4) . . ? C63 C61 C45 112.9(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C67 109.7(3) . . ? C66 C65 C47 110.7(3) . . ? C67 C65 C47 110.6(3) . . ? C66 C65 C68 106.2(3) . . ? C67 C65 C68 107.4(3) . . ? C47 C65 C68 112.1(3) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C65 C68 H68A 109.5 . . ? C65 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C65 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.484 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.042 #==END data_compound_3E0.5_C6H14E0.7C5H12 _database_code_depnum_ccdc_archive 'CCDC 654618' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H66.40 Li2 N O3' _chemical_formula_weight 617.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 31.642(3) _cell_length_b 17.4448(18) _cell_length_c 20.959(2) _cell_angle_alpha 90.00 _cell_angle_beta 129.874(2) _cell_angle_gamma 90.00 _cell_volume 8878.7(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5730 _cell_measurement_theta_min 2.243 _cell_measurement_theta_max 25.488 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.923 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2723 _exptl_absorpt_coefficient_mu 0.056 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49632 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 26.01 _reflns_number_total 8704 _reflns_number_gt 5075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1300P)^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 8704 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2422 _refine_ls_wR_factor_gt 0.2022 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.11612(13) 0.26969(19) 0.3712(2) 0.0602(8) Uani 1 1 d . . . Li2 Li 0.03019(14) 0.3026(2) 0.2338(2) 0.0692(9) Uani 1 1 d . . . N N 0.10870(6) 0.16367(9) 0.39950(10) 0.0562(4) Uani 1 1 d . . . O1 O 0.04735(5) 0.31434(7) 0.34007(8) 0.0570(4) Uani 1 1 d . . . O2 O 0.08902(6) 0.25343(8) 0.26128(9) 0.0618(4) Uani 1 1 d . . . O3 O 0.18990(6) 0.27131(9) 0.48259(10) 0.0777(5) Uani 1 1 d . . . C1 C 0.06212(7) 0.31282(11) 0.41690(12) 0.0551(5) Uani 1 1 d . . . C2 C 0.06679(8) 0.37991(12) 0.45846(13) 0.0617(5) Uani 1 1 d . . . C3 C 0.08099(9) 0.37143(14) 0.53641(14) 0.0704(6) Uani 1 1 d . . . H3A H 0.0843 0.4156 0.5641 0.085 Uiso 1 1 calc R . . C4 C 0.09052(10) 0.30168(15) 0.57520(14) 0.0726(6) Uani 1 1 d . . . C5 C 0.08590(9) 0.23721(14) 0.53268(14) 0.0689(6) Uani 1 1 d . . . H5A H 0.0920 0.1893 0.5568 0.083 Uiso 1 1 calc R . . C6 C 0.07253(8) 0.24131(12) 0.45561(13) 0.0602(5) Uani 1 1 d . . . C7 C 0.06790(9) 0.16851(12) 0.41173(14) 0.0636(5) Uani 1 1 d . . . H7A H 0.0724 0.1246 0.4440 0.076 Uiso 1 1 calc R . . H7B H 0.0313 0.1658 0.3580 0.076 Uiso 1 1 calc R . . C8 C 0.08967(9) 0.11362(11) 0.32819(13) 0.0601(5) Uani 1 1 d . . . H8A H 0.0509 0.1233 0.2831 0.072 Uiso 1 1 calc R . . H8B H 0.0934 0.0605 0.3449 0.072 Uiso 1 1 calc R . . C9 C 0.12086(8) 0.12533(11) 0.29651(12) 0.0563(5) Uani 1 1 d . . . C10 C 0.15082(9) 0.06548(11) 0.29899(13) 0.0619(5) Uani 1 1 d . . . H10A H 0.1533 0.0194 0.3235 0.074 Uiso 1 1 calc R . . C11 C 0.17724(9) 0.07232(12) 0.26603(14) 0.0650(5) Uani 1 1 d . . . C12 C 0.17074(9) 0.14185(13) 0.22855(14) 0.0673(6) Uani 1 1 d . . . H12A H 0.1874 0.1473 0.2050 0.081 Uiso 1 1 calc R . . C13 C 0.14135(8) 0.20389(12) 0.22354(13) 0.0610(5) Uani 1 1 d . . . C14 C 0.11635(7) 0.19632(11) 0.26025(12) 0.0545(5) Uani 1 1 d . . . C15 C 0.16410(9) 0.14167(14) 0.47444(14) 0.0741(6) Uani 1 1 d . . . H15A H 0.1842 0.1198 0.4582 0.089 Uiso 1 1 calc R . . H15B H 0.1610 0.1026 0.5042 0.089 Uiso 1 1 calc R . . C16 C 0.19584(10) 0.20891(17) 0.53135(15) 0.0839(7) Uani 1 1 d . . . H16A H 0.1817 0.2229 0.5594 0.101 Uiso 1 1 calc R . . H16B H 0.2344 0.1956 0.5731 0.101 Uiso 1 1 calc R . . C17 C 0.21765(12) 0.33789(19) 0.5328(2) 0.1205(12) Uani 1 1 d . . . H17A H 0.2528 0.3234 0.5839 0.181 Uiso 1 1 calc R . . H17B H 0.1959 0.3614 0.5446 0.181 Uiso 1 1 calc R . . H17C H 0.2229 0.3736 0.5035 0.181 Uiso 1 1 calc R . . C18 C 0.10546(12) 0.29548(17) 0.66029(16) 0.0900(8) Uani 1 1 d . . . C19 C 0.16542(17) 0.2667(2) 0.7238(2) 0.1406(14) Uani 1 1 d . . . H19A H 0.1683 0.2169 0.7075 0.211 Uiso 1 1 calc R . . H19B H 0.1756 0.2636 0.7779 0.211 Uiso 1 1 calc R . . H19C H 0.1896 0.3017 0.7256 0.211 Uiso 1 1 calc R . . C20 C 0.0674(3) 0.2396(4) 0.6553(3) 0.223(3) Uani 1 1 d . . . H20A H 0.0691 0.1912 0.6352 0.335 Uiso 1 1 calc R . . H20B H 0.0304 0.2589 0.6180 0.335 Uiso 1 1 calc R . . H20C H 0.0784 0.2328 0.7096 0.335 Uiso 1 1 calc R . . C21 C 0.1053(2) 0.3729(2) 0.6937(2) 0.1535(17) Uani 1 1 d . . . H21A H 0.1149 0.3661 0.7471 0.230 Uiso 1 1 calc R . . H21B H 0.0693 0.3953 0.6559 0.230 Uiso 1 1 calc R . . H21C H 0.1317 0.4062 0.6992 0.230 Uiso 1 1 calc R . . C22 C 0.05539(10) 0.45970(13) 0.41931(15) 0.0716(6) Uani 1 1 d . . . C23 C 0.06354(14) 0.52390(16) 0.4769(2) 0.1075(10) Uani 1 1 d . . . H23A H 0.1007 0.5225 0.5286 0.161 Uiso 1 1 calc R . . H23B H 0.0384 0.5165 0.4874 0.161 Uiso 1 1 calc R . . H23C H 0.0567 0.5727 0.4507 0.161 Uiso 1 1 calc R . . C24 C 0.09495(11) 0.47673(15) 0.40246(17) 0.0881(7) Uani 1 1 d . . . H24A H 0.0912 0.4379 0.3666 0.132 Uiso 1 1 calc R . . H24B H 0.1321 0.4770 0.4540 0.132 Uiso 1 1 calc R . . H24C H 0.0864 0.5259 0.3762 0.132 Uiso 1 1 calc R . . C25 C -0.00429(11) 0.46519(15) 0.33860(17) 0.0857(7) Uani 1 1 d . . . H25A H -0.0112 0.4257 0.3010 0.129 Uiso 1 1 calc R . . H25B H -0.0104 0.5145 0.3136 0.129 Uiso 1 1 calc R . . H25C H -0.0287 0.4588 0.3506 0.129 Uiso 1 1 calc R . . C26 C 0.20993(10) 0.00659(14) 0.26703(16) 0.0784(7) Uani 1 1 d . . . C27 C 0.26487(14) 0.0343(2) 0.2948(3) 0.1417(15) Uani 1 1 d . . . H27A H 0.2862 0.0553 0.3498 0.213 Uiso 1 1 calc R . . H27B H 0.2588 0.0730 0.2572 0.213 Uiso 1 1 calc R . . H27C H 0.2844 -0.0080 0.2950 0.213 Uiso 1 1 calc R . . C28 C 0.22112(19) -0.0580(2) 0.3252(3) 0.1447(15) Uani 1 1 d . . . H28A H 0.2422 -0.0386 0.3808 0.217 Uiso 1 1 calc R . . H28B H 0.2414 -0.0980 0.3240 0.217 Uiso 1 1 calc R . . H28C H 0.1868 -0.0781 0.3073 0.217 Uiso 1 1 calc R . . C29 C 0.17734(15) -0.0277(2) 0.1809(2) 0.1256(12) Uani 1 1 d . . . H29A H 0.1980 -0.0688 0.1820 0.188 Uiso 1 1 calc R . . H29B H 0.1705 0.0110 0.1427 0.188 Uiso 1 1 calc R . . H29C H 0.1429 -0.0470 0.1634 0.188 Uiso 1 1 calc R . . C30 C 0.13370(10) 0.27787(14) 0.17689(16) 0.0749(6) Uani 1 1 d . . . C31 C 0.16400(15) 0.2743(2) 0.1417(2) 0.1179(12) Uani 1 1 d . . . H31A H 0.2027 0.2674 0.1864 0.177 Uiso 1 1 calc R . . H31B H 0.1581 0.3213 0.1131 0.177 Uiso 1 1 calc R . . H31C H 0.1501 0.2322 0.1036 0.177 Uiso 1 1 calc R . . C32 C 0.07243(12) 0.28881(18) 0.10257(17) 0.0956(8) Uani 1 1 d . . . H32A H 0.0520 0.2922 0.1219 0.143 Uiso 1 1 calc R . . H32B H 0.0594 0.2460 0.0655 0.143 Uiso 1 1 calc R . . H32C H 0.0675 0.3351 0.0738 0.143 Uiso 1 1 calc R . . C33 C 0.15565(13) 0.34804(16) 0.23433(19) 0.0998(9) Uani 1 1 d . . . H33A H 0.1374 0.3519 0.2572 0.150 Uiso 1 1 calc R . . H33B H 0.1486 0.3935 0.2031 0.150 Uiso 1 1 calc R . . H33C H 0.1946 0.3426 0.2786 0.150 Uiso 1 1 calc R . . C34 C 0.0059(6) 0.0405(9) 0.6459(10) 0.60(3) Uani 1 1 d . . . H34A H -0.0101 0.0790 0.6575 0.895 Uiso 1 1 calc R . . H34B H 0.0449 0.0487 0.6806 0.895 Uiso 1 1 calc R . . H34C H -0.0011 -0.0093 0.6569 0.895 Uiso 1 1 calc R . . C35 C -0.0222(8) 0.0460(8) 0.546(2) 0.57(3) Uani 1 1 d . . . H35A H -0.0618 0.0389 0.5104 0.678 Uiso 1 1 calc R . . H35B H -0.0152 0.0961 0.5343 0.678 Uiso 1 1 calc R . . C36 C 0.0003(10) -0.0100(19) 0.5292(15) 0.52(2) Uani 1 1 d . . . H36A H 0.0380 -0.0197 0.5788 0.622 Uiso 1 1 calc R . . H36B H -0.0204 -0.0572 0.5142 0.622 Uiso 1 1 calc R . . C37 C 0.1001(9) -0.2691(12) 0.3891(10) 0.392(12) Uani 0.70 1 d P . . H37A H 0.0635 -0.2496 0.3478 0.587 Uiso 0.70 1 calc PR . . H37B H 0.1018 -0.2976 0.4299 0.587 Uiso 0.70 1 calc PR . . H37C H 0.1095 -0.3021 0.3632 0.587 Uiso 0.70 1 calc PR . . C38 C 0.1447(15) -0.1960(11) 0.435(2) 0.374(15) Uani 0.70 1 d P . . H38A H 0.1341 -0.1782 0.3830 0.449 Uiso 0.70 1 calc PR . . H38B H 0.1208 -0.1668 0.4403 0.449 Uiso 0.70 1 calc PR . . C39 C 0.1927(9) -0.133(2) 0.4870(9) 0.38(2) Uani 0.70 1 d P . . H39A H 0.2073 -0.1436 0.4588 0.451 Uiso 0.70 1 calc PR . . H39B H 0.1685 -0.0901 0.4567 0.451 Uiso 0.70 1 calc PR . . C40 C 0.2335(11) -0.0929(11) 0.5441(13) 0.359(14) Uani 0.70 1 d P . . H40A H 0.2612 -0.1323 0.5647 0.431 Uiso 0.70 1 calc PR . . H40B H 0.2258 -0.0954 0.5819 0.431 Uiso 0.70 1 calc PR . . C41 C 0.2712(5) -0.0302(8) 0.5841(9) 0.260(6) Uani 0.70 1 d P . . H41A H 0.2572 0.0120 0.5461 0.390 Uiso 0.70 1 calc PR . . H41B H 0.3062 -0.0457 0.6014 0.390 Uiso 0.70 1 calc PR . . H41C H 0.2753 -0.0148 0.6319 0.390 Uiso 0.70 1 calc PR . . 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 Li1 0.0519(18) 0.0589(19) 0.067(2) 0.0002(16) 0.0371(17) 0.0013(14) Li2 0.0561(19) 0.082(2) 0.069(2) 0.0081(19) 0.0399(18) 0.0133(17) N 0.0536(9) 0.0562(10) 0.0570(9) -0.0006(7) 0.0347(8) 0.0032(7) O1 0.0521(7) 0.0590(8) 0.0565(8) -0.0039(6) 0.0333(6) 0.0013(6) O2 0.0608(8) 0.0613(8) 0.0702(9) 0.0073(7) 0.0452(8) 0.0123(6) O3 0.0531(9) 0.0821(11) 0.0797(10) -0.0181(9) 0.0342(8) -0.0051(7) C1 0.0441(10) 0.0638(12) 0.0561(11) -0.0052(10) 0.0315(9) 0.0010(9) C2 0.0523(11) 0.0640(13) 0.0639(12) -0.0091(10) 0.0350(10) 0.0012(9) C3 0.0655(13) 0.0763(15) 0.0671(13) -0.0142(12) 0.0413(12) 0.0042(11) C4 0.0683(14) 0.0861(17) 0.0656(13) -0.0002(12) 0.0440(12) 0.0137(12) C5 0.0726(14) 0.0732(14) 0.0714(14) 0.0037(11) 0.0509(12) 0.0088(11) C6 0.0568(12) 0.0635(13) 0.0645(12) -0.0033(10) 0.0408(10) 0.0023(9) C7 0.0716(13) 0.0578(12) 0.0739(13) -0.0018(10) 0.0524(12) -0.0033(10) C8 0.0639(12) 0.0538(11) 0.0700(13) -0.0033(10) 0.0463(11) -0.0032(9) C9 0.0534(11) 0.0559(12) 0.0609(11) -0.0049(9) 0.0372(10) -0.0021(9) C10 0.0651(12) 0.0517(11) 0.0690(12) -0.0057(10) 0.0430(11) -0.0008(9) C11 0.0603(12) 0.0656(13) 0.0719(13) -0.0077(11) 0.0437(11) 0.0027(10) C12 0.0612(12) 0.0783(15) 0.0759(14) -0.0013(12) 0.0503(12) 0.0031(11) C13 0.0538(11) 0.0665(13) 0.0652(12) 0.0001(10) 0.0394(10) 0.0000(9) C14 0.0459(10) 0.0571(11) 0.0571(11) -0.0037(9) 0.0314(9) -0.0001(8) C15 0.0680(14) 0.0775(15) 0.0647(13) 0.0071(12) 0.0370(12) 0.0135(11) C16 0.0633(14) 0.107(2) 0.0639(14) -0.0025(14) 0.0328(12) 0.0113(13) C17 0.0711(17) 0.109(2) 0.133(3) -0.054(2) 0.0430(18) -0.0256(16) C18 0.101(2) 0.108(2) 0.0718(15) 0.0001(14) 0.0604(16) 0.0149(16) C19 0.151(3) 0.163(3) 0.078(2) 0.010(2) 0.060(2) 0.039(3) C20 0.270(7) 0.342(8) 0.145(4) -0.085(4) 0.173(5) -0.157(6) C21 0.215(4) 0.167(4) 0.098(2) 0.007(2) 0.110(3) 0.064(3) C22 0.0741(14) 0.0601(13) 0.0788(14) -0.0087(11) 0.0481(13) 0.0040(10) C23 0.140(3) 0.0681(16) 0.117(2) -0.0175(15) 0.083(2) 0.0070(16) C24 0.0867(17) 0.0725(16) 0.1047(19) -0.0071(14) 0.0612(16) -0.0095(12) C25 0.0815(16) 0.0723(15) 0.0961(17) 0.0088(13) 0.0536(15) 0.0198(12) C26 0.0797(15) 0.0700(15) 0.0965(17) -0.0073(13) 0.0616(14) 0.0094(12) C27 0.095(2) 0.113(2) 0.222(4) -0.038(3) 0.103(3) 0.0097(18) C28 0.195(4) 0.117(3) 0.166(3) 0.041(3) 0.136(3) 0.081(3) C29 0.134(3) 0.118(2) 0.122(2) -0.037(2) 0.081(2) 0.013(2) C30 0.0717(15) 0.0788(15) 0.0883(16) 0.0167(13) 0.0578(14) 0.0070(12) C31 0.137(3) 0.119(2) 0.163(3) 0.045(2) 0.126(3) 0.026(2) C32 0.0881(18) 0.110(2) 0.0875(18) 0.0307(16) 0.0555(16) 0.0163(15) C33 0.103(2) 0.0783(17) 0.115(2) 0.0099(16) 0.0687(18) -0.0119(15) C34 0.182(9) 0.49(2) 0.57(3) 0.38(3) -0.007(14) -0.093(12) C35 0.221(13) 0.202(9) 0.79(6) 0.008(19) 0.10(2) -0.078(9) C36 0.39(3) 0.61(5) 0.59(5) 0.23(4) 0.33(3) -0.08(3) C37 0.72(4) 0.295(18) 0.38(2) 0.007(16) 0.45(3) 0.01(2) C38 0.67(5) 0.234(16) 0.50(4) 0.041(19) 0.50(4) 0.01(2) C39 0.29(2) 0.66(6) 0.164(11) 0.08(2) 0.139(13) 0.14(3) C40 0.55(4) 0.246(16) 0.29(2) 0.063(18) 0.27(3) -0.02(2) C41 0.253(12) 0.241(11) 0.294(14) 0.130(12) 0.178(11) 0.099(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.895(4) . ? Li1 O3 1.978(4) . ? Li1 O1 1.987(3) . ? Li1 N 2.002(4) . ? Li1 Li2 2.444(5) . ? Li1 C1 2.550(4) . ? Li1 C14 2.658(4) . ? Li1 C15 2.786(4) . ? Li2 O2 1.777(4) . ? Li2 O1 1.894(4) 2 ? Li2 O1 1.936(4) . ? Li2 Li2 2.403(7) 2 ? Li2 C1 2.590(4) 2 ? N C15 1.469(3) . ? N C7 1.471(3) . ? N C8 1.485(2) . ? O1 C1 1.359(2) . ? O1 Li2 1.894(4) 2 ? O2 C14 1.328(2) . ? O3 C16 1.421(3) . ? O3 C17 1.429(3) . ? C1 C6 1.407(3) . ? C1 C2 1.409(3) . ? C1 Li2 2.590(4) 2 ? C2 C3 1.397(3) . ? C2 C22 1.537(3) . ? C3 C4 1.385(3) . ? C3 H3A 0.9300 . ? C4 C5 1.383(3) . ? C4 C18 1.528(3) . ? C5 C6 1.385(3) . ? C5 H5A 0.9300 . ? C6 C7 1.519(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.516(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.389(3) . ? C9 C14 1.412(3) . ? C10 C11 1.390(3) . ? C10 H10A 0.9300 . ? C11 C12 1.387(3) . ? C11 C26 1.535(3) . ? C12 C13 1.386(3) . ? C12 H12A 0.9300 . ? C13 C14 1.420(3) . ? C13 C30 1.542(3) . ? C15 C16 1.507(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C20 1.500(5) . ? C18 C21 1.523(4) . ? C18 C19 1.544(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C25 1.530(3) . ? C22 C24 1.532(3) . ? C22 C23 1.543(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C29 1.514(4) . ? C26 C27 1.515(4) . ? C26 C28 1.525(4) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C32 1.533(4) . ? C30 C33 1.536(4) . ? C30 C31 1.541(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.68(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.38(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C36 1.26(4) 5_556 ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.67(3) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.60(3) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.27(3) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.43(2) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? 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 Li1 O3 135.15(19) . . ? O2 Li1 O1 96.48(16) . . ? O3 Li1 O1 126.67(19) . . ? O2 Li1 N 100.05(17) . . ? O3 Li1 N 86.41(15) . . ? O1 Li1 N 98.49(16) . . ? O2 Li1 Li2 46.23(12) . . ? O3 Li1 Li2 165.2(2) . . ? O1 Li1 Li2 50.52(12) . . ? N Li1 Li2 108.23(17) . . ? O2 Li1 C1 127.66(16) . . ? O3 Li1 C1 96.91(15) . . ? O1 Li1 C1 31.90(8) . . ? N Li1 C1 85.82(14) . . ? Li2 Li1 C1 82.30(13) . . ? O2 Li1 C14 28.03(8) . . ? O3 Li1 C14 112.11(15) . . ? O1 Li1 C14 121.21(16) . . ? N Li1 C14 83.17(13) . . ? Li2 Li1 C14 72.98(13) . . ? C1 Li1 C14 148.09(15) . . ? O2 Li1 C15 114.89(16) . . ? O3 Li1 C15 56.75(11) . . ? O1 Li1 C15 120.40(16) . . ? N Li1 C15 30.48(8) . . ? Li2 Li1 C15 138.06(17) . . ? C1 Li1 C15 96.17(13) . . ? C14 Li1 C15 89.30(12) . . ? O2 Li2 O1 148.9(2) . 2 ? O2 Li2 O1 102.44(18) . . ? O1 Li2 O1 100.95(17) 2 . ? O2 Li2 Li2 140.0(2) . 2 ? O1 Li2 Li2 51.92(14) 2 2 ? O1 Li2 Li2 50.37(14) . 2 ? O2 Li2 Li1 50.35(13) . . ? O1 Li2 Li1 150.2(2) 2 . ? O1 Li2 Li1 52.40(12) . . ? Li2 Li2 Li1 98.8(2) 2 . ? O2 Li2 C1 123.81(19) . 2 ? O1 Li2 C1 30.55(8) 2 2 ? O1 Li2 C1 131.37(17) . 2 ? Li2 Li2 C1 82.26(18) 2 2 ? Li1 Li2 C1 170.3(2) . 2 ? C15 N C7 114.07(17) . . ? C15 N C8 111.02(16) . . ? C7 N C8 111.98(15) . . ? C15 N Li1 105.79(17) . . ? C7 N Li1 106.35(15) . . ? C8 N Li1 107.09(15) . . ? C1 O1 Li2 104.34(15) . 2 ? C1 O1 Li2 172.27(17) . . ? Li2 O1 Li2 77.71(17) 2 . ? C1 O1 Li1 97.53(15) . . ? Li2 O1 Li1 142.93(17) 2 . ? Li2 O1 Li1 77.08(15) . . ? C14 O2 Li2 156.09(18) . . ? C14 O2 Li1 109.89(15) . . ? Li2 O2 Li1 83.41(16) . . ? C16 O3 C17 111.0(2) . . ? C16 O3 Li1 110.47(16) . . ? C17 O3 Li1 125.7(2) . . ? O1 C1 C6 118.43(17) . . ? O1 C1 C2 122.43(18) . . ? C6 C1 C2 119.14(18) . . ? O1 C1 Li1 50.57(11) . . ? C6 C1 Li1 89.39(14) . . ? C2 C1 Li1 130.35(16) . . ? O1 C1 Li2 45.11(11) . 2 ? C6 C1 Li2 107.83(15) . 2 ? C2 C1 Li2 113.60(15) . 2 ? Li1 C1 Li2 91.43(13) . 2 ? C3 C2 C1 117.6(2) . . ? C3 C2 C22 120.65(19) . . ? C1 C2 C22 121.77(18) . . ? C4 C3 C2 124.4(2) . . ? C4 C3 H3A 117.8 . . ? C2 C3 H3A 117.8 . . ? C5 C4 C3 116.3(2) . . ? C5 C4 C18 121.4(2) . . ? C3 C4 C18 122.4(2) . . ? C4 C5 C6 122.5(2) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C1 120.12(19) . . ? C5 C6 C7 120.13(19) . . ? C1 C6 C7 119.74(18) . . ? N C7 C6 113.50(16) . . ? N C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N C8 C9 113.82(16) . . ? N C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 120.72(18) . . ? C10 C9 C8 120.19(18) . . ? C14 C9 C8 118.99(17) . . ? C9 C10 C11 122.05(19) . . ? C9 C10 H10A 119.0 . . ? C11 C10 H10A 119.0 . . ? C12 C11 C10 116.02(19) . . ? C12 C11 C26 121.0(2) . . ? C10 C11 C26 122.9(2) . . ? C13 C12 C11 125.1(2) . . ? C13 C12 H12A 117.5 . . ? C11 C12 H12A 117.5 . . ? C12 C13 C14 117.78(19) . . ? C12 C13 C30 121.77(19) . . ? C14 C13 C30 120.40(18) . . ? O2 C14 C9 119.43(17) . . ? O2 C14 C13 122.26(18) . . ? C9 C14 C13 118.31(17) . . ? O2 C14 Li1 42.08(11) . . ? C9 C14 Li1 90.43(14) . . ? C13 C14 Li1 138.09(16) . . ? N C15 C16 112.08(19) . . ? N C15 Li1 43.73(12) . . ? C16 C15 Li1 75.26(15) . . ? N C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? Li1 C15 H15A 101.3 . . ? N C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? Li1 C15 H15B 146.5 . . ? H15A C15 H15B 107.9 . . ? O3 C16 C15 108.27(19) . . ? O3 C16 H16A 110.0 . . ? C15 C16 H16A 110.0 . . ? O3 C16 H16B 110.0 . . ? C15 C16 H16B 110.0 . . ? H16A C16 H16B 108.4 . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C21 111.7(3) . . ? C20 C18 C4 109.3(3) . . ? C21 C18 C4 112.6(2) . . ? C20 C18 C19 109.6(4) . . ? C21 C18 C19 104.9(3) . . ? C4 C18 C19 108.6(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C22 C24 110.2(2) . . ? C25 C22 C2 110.36(19) . . ? C24 C22 C2 110.61(19) . . ? C25 C22 C23 106.8(2) . . ? C24 C22 C23 106.8(2) . . ? C2 C22 C23 112.0(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C29 C26 C27 108.7(3) . . ? C29 C26 C28 107.0(3) . . ? C27 C26 C28 107.9(3) . . ? C29 C26 C11 109.9(2) . . ? C27 C26 C11 111.3(2) . . ? C28 C26 C11 111.8(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C33 109.8(2) . . ? C32 C30 C31 106.7(2) . . ? C33 C30 C31 107.4(2) . . ? C32 C30 C13 109.32(19) . . ? C33 C30 C13 111.2(2) . . ? C31 C30 C13 112.2(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C34 109(2) . . ? C36 C35 H35A 109.8 . . ? C34 C35 H35A 109.8 . . ? C36 C35 H35B 109.8 . . ? C34 C35 H35B 109.8 . . ? H35A C35 H35B 108.3 . . ? C36 C36 C35 111(4) 5_556 . ? C36 C36 H36A 109.4 5_556 . ? C35 C36 H36A 109.4 . . ? C36 C36 H36B 109.4 5_556 . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C37 173(3) . . ? C39 C38 H38A 92.1 . . ? C37 C38 H38A 92.1 . . ? C39 C38 H38B 92.1 . . ? C37 C38 H38B 92.1 . . ? H38A C38 H38B 103.0 . . ? C40 C39 C38 165(3) . . ? C40 C39 H39A 94.6 . . ? C38 C39 H39A 94.6 . . ? C40 C39 H39B 94.6 . . ? C38 C39 H39B 94.6 . . ? H39A C39 H39B 103.2 . . ? C39 C40 C41 160(2) . . ? C39 C40 H40A 96.1 . . ? C41 C40 H40A 96.1 . . ? C39 C40 H40B 96.1 . . ? C41 C40 H40B 96.1 . . ? H40A C40 H40B 103.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.300 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.044 #==END data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 654619' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H102 Li2 N4 O4' _chemical_formula_weight 1101.46 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.4797(17) _cell_length_b 12.810(2) _cell_length_c 15.438(3) _cell_angle_alpha 95.307(3) _cell_angle_beta 106.674(4) _cell_angle_gamma 103.336(4) _cell_volume 1721.9(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3223 _cell_measurement_theta_min 2.303 _cell_measurement_theta_max 26.031 _exptl_crystal_description parallelepiped _exptl_crystal_colour colcorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.716 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9824 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.05 _reflns_number_total 6670 _reflns_number_gt 4193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 6670 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li Li 0.4565(4) 0.6468(2) 0.5055(2) 0.0458(7) Uani 1 1 d . . . O1 O 0.31906(14) 0.53492(10) 0.39976(8) 0.0434(3) Uani 1 1 d . . . H1 H 0.359(3) 0.466(2) 0.3918(19) 0.099(9) Uiso 1 1 d . . . O2 O 0.59029(14) 0.63090(9) 0.61790(8) 0.0419(3) Uani 1 1 d . . . N1 N 0.62206(16) 0.70602(11) 0.44615(10) 0.0389(4) Uani 1 1 d . . . N2 N 0.39868(19) 0.79388(12) 0.48577(11) 0.0504(4) Uani 1 1 d . . . C1 C 0.2941(2) 0.58012(14) 0.32076(12) 0.0394(4) Uani 1 1 d . . . C2 C 0.1472(2) 0.57998(15) 0.26666(13) 0.0451(5) Uani 1 1 d . . . C3 C 0.1371(2) 0.62848(17) 0.18843(14) 0.0533(5) Uani 1 1 d . . . H3A H 0.0405 0.6294 0.1521 0.064 Uiso 1 1 calc R . . C4 C 0.2607(3) 0.67515(17) 0.16139(13) 0.0531(5) Uani 1 1 d . . . C5 C 0.4035(2) 0.67458(16) 0.21740(13) 0.0487(5) Uani 1 1 d . . . H5A H 0.4893 0.7057 0.2014 0.058 Uiso 1 1 calc R . . C6 C 0.4226(2) 0.62921(14) 0.29636(12) 0.0408(4) Uani 1 1 d . . . C7 C 0.5803(2) 0.63391(15) 0.35705(12) 0.0425(4) Uani 1 1 d . . . H7A H 0.5848 0.5611 0.3677 0.051 Uiso 1 1 calc R . . H7B H 0.6538 0.6602 0.3261 0.051 Uiso 1 1 calc R . . C8 C 0.7717(2) 0.70214(15) 0.50779(12) 0.0429(4) Uani 1 1 d . . . H8A H 0.8516 0.7360 0.4837 0.051 Uiso 1 1 calc R . . H8B H 0.7726 0.6267 0.5090 0.051 Uiso 1 1 calc R . . C9 C 0.8054(2) 0.75919(14) 0.60421(12) 0.0405(4) Uani 1 1 d . . . C10 C 0.9355(2) 0.84602(15) 0.64374(13) 0.0447(4) Uani 1 1 d . . . H10A H 0.9991 0.8691 0.6093 0.054 Uiso 1 1 calc R . . C11 C 0.9732(2) 0.89937(15) 0.73353(13) 0.0472(5) Uani 1 1 d . A . C12 C 0.8697(2) 0.86489(15) 0.78016(13) 0.0484(5) Uani 1 1 d . . . H12A H 0.8904 0.9015 0.8392 0.058 Uiso 1 1 calc R . . C13 C 0.7378(2) 0.77945(14) 0.74440(13) 0.0434(4) Uani 1 1 d . . . C14 C 0.7082(2) 0.72184(13) 0.65532(12) 0.0391(4) Uani 1 1 d . . . C15 C 0.6199(2) 0.81796(15) 0.43328(14) 0.0466(5) Uani 1 1 d . . . H15A H 0.6380 0.8299 0.3758 0.056 Uiso 1 1 calc R . . H15B H 0.7028 0.8682 0.4823 0.056 Uiso 1 1 calc R . . C16 C 0.4723(2) 0.84291(14) 0.43231(13) 0.0464(5) Uani 1 1 d . . . C17 C 0.4210(3) 0.91970(17) 0.38223(15) 0.0601(6) Uani 1 1 d . . . H17A H 0.4729 0.9516 0.3445 0.072 Uiso 1 1 calc R . . C18 C 0.2928(3) 0.9477(2) 0.38933(18) 0.0756(8) Uani 1 1 d . . . H18A H 0.2568 0.9987 0.3565 0.091 Uiso 1 1 calc R . . C19 C 0.2186(3) 0.8990(2) 0.44585(19) 0.0729(7) Uani 1 1 d . . . H19A H 0.1324 0.9172 0.4526 0.088 Uiso 1 1 calc R . . C20 C 0.2745(3) 0.82315(18) 0.49205(17) 0.0623(6) Uani 1 1 d . . . H20A H 0.2234 0.7902 0.5298 0.075 Uiso 1 1 calc R . . C21 C 0.2425(3) 0.7279(2) 0.07450(15) 0.0712(7) Uani 1 1 d . . . C22 C 0.3095(7) 0.8476(3) 0.1030(3) 0.198(3) Uani 1 1 d . . . H22A H 0.2533 0.8765 0.1375 0.297 Uiso 1 1 calc R . . H22B H 0.3041 0.8812 0.0495 0.297 Uiso 1 1 calc R . . H22C H 0.4144 0.8624 0.1404 0.297 Uiso 1 1 calc R . . C23 C 0.3345(6) 0.6868(5) 0.0197(3) 0.191(3) Uani 1 1 d . . . H23A H 0.3245 0.7194 -0.0345 0.286 Uiso 1 1 calc R . . H23B H 0.2970 0.6090 0.0025 0.286 Uiso 1 1 calc R . . H23C H 0.4402 0.7058 0.0565 0.286 Uiso 1 1 calc R . . C24 C 0.0822(4) 0.7016(3) 0.0131(2) 0.1365(17) Uani 1 1 d . . . H24A H 0.0207 0.7271 0.0455 0.205 Uiso 1 1 calc R . . H24B H 0.0434 0.6242 -0.0063 0.205 Uiso 1 1 calc R . . H24C H 0.0787 0.7364 -0.0396 0.205 Uiso 1 1 calc R . . C25 C 0.0010(2) 0.52530(17) 0.28806(14) 0.0513(5) Uani 1 1 d . . . C26 C 0.0103(3) 0.5681(3) 0.38594(18) 0.0877(9) Uani 1 1 d . . . H26A H -0.0822 0.5330 0.3972 0.132 Uiso 1 1 calc R . . H26B H 0.0230 0.6453 0.3933 0.132 Uiso 1 1 calc R . . H26C H 0.0958 0.5529 0.4288 0.132 Uiso 1 1 calc R . . C27 C -0.0210(3) 0.40281(19) 0.2752(2) 0.0815(8) Uani 1 1 d . . . H27A H -0.1122 0.3682 0.2881 0.122 Uiso 1 1 calc R . . H27B H 0.0655 0.3867 0.3164 0.122 Uiso 1 1 calc R . . H27C H -0.0302 0.3762 0.2131 0.122 Uiso 1 1 calc R . . C28 C -0.1431(3) 0.5463(2) 0.22461(19) 0.0784(7) Uani 1 1 d . . . H28A H -0.2305 0.5106 0.2407 0.118 Uiso 1 1 calc R . . H28B H -0.1563 0.5181 0.1621 0.118 Uiso 1 1 calc R . . H28C H -0.1329 0.6232 0.2312 0.118 Uiso 1 1 calc R . . C29 C 1.1226(2) 0.98921(18) 0.78051(15) 0.0597(6) Uani 1 1 d . . . C30 C 1.0843(6) 1.0929(4) 0.8173(6) 0.0960(17) Uani 0.60 1 d P A 1 H30A H 1.1773 1.1494 0.8466 0.144 Uiso 0.60 1 calc PR A 1 H30B H 1.0312 1.0762 0.8608 0.144 Uiso 0.60 1 calc PR A 1 H30C H 1.0207 1.1171 0.7671 0.144 Uiso 0.60 1 calc PR A 1 C31 C 1.2205(6) 0.9504(5) 0.8617(4) 0.0797(15) Uani 0.60 1 d P A 1 H31A H 1.2465 0.8871 0.8398 0.120 Uiso 0.60 1 calc PR A 1 H31B H 1.1641 0.9326 0.9034 0.120 Uiso 0.60 1 calc PR A 1 H31C H 1.3124 1.0072 0.8928 0.120 Uiso 0.60 1 calc PR A 1 C32 C 1.2144(7) 1.0191(7) 0.7189(3) 0.095(2) Uani 0.60 1 d P A 1 H32A H 1.2388 0.9558 0.6954 0.142 Uiso 0.60 1 calc PR A 1 H32B H 1.3072 1.0738 0.7526 0.142 Uiso 0.60 1 calc PR A 1 H32C H 1.1567 1.0469 0.6689 0.142 Uiso 0.60 1 calc PR A 1 C30' C 1.1496(15) 1.0240(14) 0.8772(7) 0.176(7) Uani 0.40 1 d P A 2 H30D H 1.1959 0.9753 0.9119 0.264 Uiso 0.40 1 calc PR A 2 H30E H 1.0541 1.0232 0.8874 0.264 Uiso 0.40 1 calc PR A 2 H30F H 1.2166 1.0964 0.8964 0.264 Uiso 0.40 1 calc PR A 2 C31' C 1.2524(11) 0.9412(15) 0.770(2) 0.299(16) Uani 0.40 1 d P A 2 H31D H 1.2111 0.8657 0.7430 0.449 Uiso 0.40 1 calc PR A 2 H31E H 1.3256 0.9479 0.8298 0.449 Uiso 0.40 1 calc PR A 2 H31F H 1.3018 0.9799 0.7320 0.449 Uiso 0.40 1 calc PR A 2 C32' C 1.1184(16) 1.0859(11) 0.7323(11) 0.166(6) Uani 0.40 1 d P A 2 H32D H 1.1479 1.0746 0.6784 0.248 Uiso 0.40 1 calc PR A 2 H32E H 1.1880 1.1503 0.7728 0.248 Uiso 0.40 1 calc PR A 2 H32F H 1.0167 1.0947 0.7150 0.248 Uiso 0.40 1 calc PR A 2 C33 C 0.6287(2) 0.74767(17) 0.80094(14) 0.0540(5) Uani 1 1 d . . . C34 C 0.6286(3) 0.6352(2) 0.82505(18) 0.0782(8) Uani 1 1 d . . . H34A H 0.7306 0.6351 0.8593 0.117 Uiso 1 1 calc R . . H34B H 0.5929 0.5825 0.7697 0.117 Uiso 1 1 calc R . . H34C H 0.5623 0.6169 0.8613 0.117 Uiso 1 1 calc R . . C35 C 0.4674(3) 0.7503(3) 0.7458(2) 0.0907(9) Uani 1 1 d . . . H35A H 0.4335 0.7012 0.6885 0.136 Uiso 1 1 calc R . . H35B H 0.4686 0.8228 0.7343 0.136 Uiso 1 1 calc R . . H35C H 0.3988 0.7284 0.7801 0.136 Uiso 1 1 calc R . . C36 C 0.6761(3) 0.8274(2) 0.89102(19) 0.0920(9) Uani 1 1 d . . . H36A H 0.7768 0.8277 0.9279 0.138 Uiso 1 1 calc R . . H36B H 0.6051 0.8052 0.9237 0.138 Uiso 1 1 calc R . . H36C H 0.6760 0.8992 0.8779 0.138 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 Li 0.0463(18) 0.0414(16) 0.0495(18) 0.0079(14) 0.0156(14) 0.0109(13) O1 0.0488(8) 0.0397(7) 0.0413(7) 0.0074(6) 0.0145(6) 0.0108(6) O2 0.0416(7) 0.0349(6) 0.0446(7) 0.0038(5) 0.0115(6) 0.0055(5) N1 0.0395(8) 0.0354(8) 0.0405(8) 0.0044(6) 0.0122(7) 0.0092(6) N2 0.0524(10) 0.0414(9) 0.0566(10) 0.0013(8) 0.0163(8) 0.0152(7) C1 0.0456(11) 0.0340(9) 0.0372(9) 0.0020(7) 0.0131(8) 0.0095(8) C2 0.0469(11) 0.0419(10) 0.0432(10) 0.0015(8) 0.0118(9) 0.0113(8) C3 0.0505(12) 0.0554(12) 0.0462(11) 0.0073(9) 0.0039(9) 0.0144(10) C4 0.0622(14) 0.0529(12) 0.0403(11) 0.0095(9) 0.0125(10) 0.0126(10) C5 0.0510(12) 0.0487(11) 0.0422(11) 0.0051(9) 0.0164(9) 0.0045(9) C6 0.0437(11) 0.0379(9) 0.0390(10) 0.0022(8) 0.0122(8) 0.0103(8) C7 0.0438(11) 0.0439(10) 0.0421(10) 0.0035(8) 0.0190(8) 0.0112(8) C8 0.0412(10) 0.0446(10) 0.0451(10) 0.0066(8) 0.0177(8) 0.0113(8) C9 0.0398(10) 0.0387(9) 0.0424(10) 0.0056(8) 0.0114(8) 0.0120(8) C10 0.0396(10) 0.0449(10) 0.0469(11) 0.0087(8) 0.0132(8) 0.0070(8) C11 0.0454(11) 0.0403(10) 0.0482(11) 0.0065(8) 0.0086(9) 0.0051(8) C12 0.0536(12) 0.0422(10) 0.0449(11) 0.0015(8) 0.0131(9) 0.0101(9) C13 0.0457(11) 0.0395(10) 0.0440(10) 0.0051(8) 0.0144(8) 0.0103(8) C14 0.0383(10) 0.0337(9) 0.0424(10) 0.0048(8) 0.0104(8) 0.0082(7) C15 0.0502(12) 0.0381(10) 0.0494(11) 0.0092(8) 0.0144(9) 0.0090(8) C16 0.0527(12) 0.0351(9) 0.0454(11) 0.0009(8) 0.0086(9) 0.0114(8) C17 0.0732(15) 0.0482(12) 0.0555(13) 0.0091(10) 0.0105(11) 0.0223(11) C18 0.0855(19) 0.0623(15) 0.0722(16) 0.0027(13) 0.0011(14) 0.0407(14) C19 0.0637(16) 0.0656(15) 0.0884(18) -0.0020(14) 0.0163(14) 0.0312(12) C20 0.0598(14) 0.0549(13) 0.0741(15) -0.0016(11) 0.0248(12) 0.0195(11) C21 0.0730(16) 0.0817(17) 0.0455(12) 0.0227(12) 0.0079(12) 0.0041(13) C22 0.294(6) 0.097(3) 0.102(3) 0.063(2) -0.035(3) -0.035(3) C23 0.195(5) 0.364(8) 0.089(3) 0.116(4) 0.088(3) 0.135(5) C24 0.111(3) 0.186(4) 0.075(2) 0.069(2) -0.0090(19) -0.001(3) C25 0.0413(11) 0.0564(12) 0.0539(12) 0.0065(10) 0.0130(9) 0.0125(9) C26 0.0629(16) 0.126(2) 0.0725(17) -0.0013(16) 0.0356(13) 0.0114(15) C27 0.0536(15) 0.0572(14) 0.128(2) 0.0166(15) 0.0248(15) 0.0080(11) C28 0.0522(14) 0.0929(19) 0.0938(19) 0.0235(16) 0.0207(13) 0.0270(13) C29 0.0528(13) 0.0569(13) 0.0521(13) 0.0046(10) 0.0073(10) -0.0045(10) C30 0.089(4) 0.048(2) 0.113(5) -0.013(3) 0.002(3) -0.008(2) C31 0.053(3) 0.100(4) 0.066(3) 0.026(3) -0.002(2) 0.004(3) C32 0.062(4) 0.122(5) 0.058(3) 0.010(3) 0.011(3) -0.045(3) C30' 0.130(11) 0.210(15) 0.081(6) -0.046(8) 0.014(7) -0.108(10) C31' 0.039(5) 0.221(17) 0.52(4) -0.22(2) 0.028(12) -0.005(8) C32' 0.111(9) 0.117(9) 0.178(13) 0.054(9) -0.025(9) -0.065(7) C33 0.0562(13) 0.0542(12) 0.0504(12) -0.0002(9) 0.0254(10) 0.0052(10) C34 0.107(2) 0.0666(15) 0.0690(16) 0.0171(13) 0.0475(15) 0.0106(14) C35 0.0649(17) 0.127(3) 0.091(2) 0.0093(18) 0.0418(15) 0.0292(16) C36 0.107(2) 0.0807(18) 0.0822(18) -0.0219(14) 0.0602(17) -0.0097(15) _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 Li O2 1.893(3) . ? Li O1 1.975(3) . ? Li N1 2.069(4) . ? Li N2 2.104(3) . ? O1 C1 1.381(2) . ? O1 H1 1.04(3) . ? O2 C14 1.358(2) . ? N1 C15 1.470(2) . ? N1 C7 1.478(2) . ? N1 C8 1.478(2) . ? N2 C16 1.337(3) . ? N2 C20 1.341(3) . ? C1 C2 1.403(3) . ? C1 C6 1.405(3) . ? C2 C3 1.398(3) . ? C2 C25 1.542(3) . ? C3 C4 1.381(3) . ? C3 H3A 0.9300 . ? C4 C5 1.384(3) . ? C4 C21 1.541(3) . ? C5 C6 1.382(3) . ? C5 H5A 0.9300 . ? C6 C7 1.503(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.507(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.393(2) . ? C9 C14 1.409(3) . ? C10 C11 1.395(3) . ? C10 H10A 0.9300 . ? C11 C12 1.392(3) . ? C11 C29 1.537(3) . ? C12 C13 1.388(3) . ? C12 H12A 0.9300 . ? C13 C14 1.418(3) . ? C13 C33 1.545(3) . ? C15 C16 1.501(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.396(3) . ? C17 C18 1.373(4) . ? C17 H17A 0.9300 . ? C18 C19 1.377(4) . ? C18 H18A 0.9300 . ? C19 C20 1.372(3) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C24 1.483(4) . ? C21 C22 1.488(4) . ? C21 C23 1.519(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C27 1.521(3) . ? C25 C26 1.530(3) . ? C25 C28 1.532(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30' 1.448(10) . ? C29 C32 1.482(6) . ? C29 C32' 1.506(11) . ? C29 C31 1.529(5) . ? C29 C31' 1.536(12) . ? C29 C30 1.555(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 0.9600 . ? C31' H31D 0.9600 . ? C31' H31E 0.9600 . ? C31' H31F 0.9600 . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 0.9600 . ? C33 C34 1.521(3) . ? C33 C36 1.531(3) . ? C33 C35 1.532(3) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 Li O1 129.77(17) . . ? O2 Li N1 97.17(15) . . ? O1 Li N1 97.10(15) . . ? O2 Li N2 121.96(17) . . ? O1 Li N2 107.24(15) . . ? N1 Li N2 84.27(12) . . ? C1 O1 Li 109.79(13) . . ? C1 O1 H1 111.0(15) . . ? Li O1 H1 113.2(15) . . ? C14 O2 Li 111.72(14) . . ? C15 N1 C7 111.08(14) . . ? C15 N1 C8 111.59(14) . . ? C7 N1 C8 111.03(13) . . ? C15 N1 Li 108.01(14) . . ? C7 N1 Li 106.62(14) . . ? C8 N1 Li 108.29(13) . . ? C16 N2 C20 117.64(18) . . ? C16 N2 Li 109.09(15) . . ? C20 N2 Li 129.29(17) . . ? O1 C1 C2 122.25(16) . . ? O1 C1 C6 117.58(16) . . ? C2 C1 C6 120.15(17) . . ? C3 C2 C1 116.76(18) . . ? C3 C2 C25 120.27(18) . . ? C1 C2 C25 122.91(17) . . ? C4 C3 C2 124.51(19) . . ? C4 C3 H3A 117.7 . . ? C2 C3 H3A 117.7 . . ? C3 C4 C5 116.72(18) . . ? C3 C4 C21 122.2(2) . . ? C5 C4 C21 121.1(2) . . ? C6 C5 C4 122.03(18) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C1 119.79(17) . . ? C5 C6 C7 120.28(17) . . ? C1 C6 C7 119.92(16) . . ? N1 C7 C6 111.88(14) . . ? N1 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? N1 C8 C9 112.38(14) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C14 120.20(17) . . ? C10 C9 C8 119.97(17) . . ? C14 C9 C8 119.78(16) . . ? C9 C10 C11 121.87(18) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C12 C11 C10 116.45(17) . . ? C12 C11 C29 121.14(18) . . ? C10 C11 C29 122.39(18) . . ? C13 C12 C11 124.35(18) . . ? C13 C12 H12A 117.8 . . ? C11 C12 H12A 117.8 . . ? C12 C13 C14 117.84(17) . . ? C12 C13 C33 120.72(17) . . ? C14 C13 C33 121.43(16) . . ? O2 C14 C9 118.76(16) . . ? O2 C14 C13 122.23(16) . . ? C9 C14 C13 119.01(16) . . ? N1 C15 C16 113.58(15) . . ? N1 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N1 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? N2 C16 C17 121.9(2) . . ? N2 C16 C15 117.13(16) . . ? C17 C16 C15 120.8(2) . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 118.9(2) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C20 C19 C18 118.6(2) . . ? C20 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? N2 C20 C19 123.6(2) . . ? N2 C20 H20A 118.2 . . ? C19 C20 H20A 118.2 . . ? C24 C21 C22 111.3(3) . . ? C24 C21 C23 107.2(3) . . ? C22 C21 C23 107.3(4) . . ? C24 C21 C4 113.6(2) . . ? C22 C21 C4 108.5(2) . . ? C23 C21 C4 108.7(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 110.0(2) . . ? C27 C25 C28 107.41(19) . . ? C26 C25 C28 106.2(2) . . ? C27 C25 C2 109.01(18) . . ? C26 C25 C2 111.29(17) . . ? C28 C25 C2 112.78(18) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30' C29 C32 132.7(4) . . ? C30' C29 C32' 108.9(10) . . ? C32 C29 C32' 57.1(7) . . ? C30' C29 C31 52.5(8) . . ? C32 C29 C31 108.1(4) . . ? C32' C29 C31 142.2(4) . . ? C30' C29 C31' 108.5(12) . . ? C32 C29 C31' 54.4(11) . . ? C32' C29 C31' 110.7(13) . . ? C31 C29 C31' 59.6(12) . . ? C30' C29 C11 113.7(4) . . ? C32 C29 C11 113.5(3) . . ? C32' C29 C11 108.7(4) . . ? C31 C29 C11 109.0(2) . . ? C31' C29 C11 106.3(5) . . ? C30' C29 C30 57.5(8) . . ? C32 C29 C30 108.4(4) . . ? C32' C29 C30 56.0(8) . . ? C31 C29 C30 108.6(4) . . ? C31' C29 C30 144.6(5) . . ? C11 C29 C30 109.1(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C30' H30D 109.5 . . ? C29 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C29 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C29 C31' H31D 109.5 . . ? C29 C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C29 C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C29 C32' H32D 109.5 . . ? C29 C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C29 C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C34 C33 C36 107.5(2) . . ? C34 C33 C35 110.7(2) . . ? C36 C33 C35 106.9(2) . . ? C34 C33 C13 110.14(19) . . ? C36 C33 C13 112.08(17) . . ? C35 C33 C13 109.39(18) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.359 _refine_diff_density_min -0.242 _refine_diff_density_rms 0.043 #==END data_compound_5_EEt2O _database_code_depnum_ccdc_archive 'CCDC 654620' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H114 Li2 N2 O7' _chemical_formula_weight 1109.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.7520(10) _cell_length_b 13.8559(13) _cell_length_c 14.0999(12) _cell_angle_alpha 99.985(2) _cell_angle_beta 106.680(2) _cell_angle_gamma 108.834(2) _cell_volume 1820.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3063 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.42 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 610 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10349 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.05 _reflns_number_total 7020 _reflns_number_gt 4093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^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 7020 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1939 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.0395(4) 0.6081(3) 0.4182(3) 0.0527(8) Uani 1 1 d . B . O1 O -0.00552(14) 0.65264(11) 0.53691(10) 0.0481(4) Uani 1 1 d . B . O2 O 0.00573(13) 0.46456(11) 0.34866(10) 0.0476(4) Uani 1 1 d . . . O3 O 0.0908(2) 0.71804(14) 0.34112(13) 0.0730(5) Uani 1 1 d . . . O4 O -0.034(4) -0.008(4) -0.024(2) 0.58(3) Uani 0.50 1 d P . . N N 0.25500(17) 0.66278(13) 0.49193(12) 0.0471(4) Uani 1 1 d . . . C1 C 0.0796(2) 0.75718(15) 0.59033(14) 0.0449(5) Uani 1 1 d . . . C2 C 0.0258(2) 0.83525(17) 0.60868(16) 0.0509(5) Uani 1 1 d . . . C3 C 0.1229(2) 0.93761(18) 0.67112(17) 0.0563(6) Uani 1 1 d . . . H3A H 0.0880 0.9897 0.6843 0.068 Uiso 1 1 calc R B . C4 C 0.2670(2) 0.96628(17) 0.71443(17) 0.0554(6) Uani 1 1 d . . . C5 C 0.3170(2) 0.88835(18) 0.68896(16) 0.0548(5) Uani 1 1 d . . . H5A H 0.4139 0.9059 0.7138 0.066 Uiso 1 1 calc R B . C6 C 0.2272(2) 0.78587(16) 0.62807(15) 0.0478(5) Uani 1 1 d . B . C7 C 0.2860(2) 0.70379(17) 0.60354(16) 0.0517(5) Uani 1 1 d . B . H7A H 0.3876 0.7352 0.6401 0.062 Uiso 1 1 calc R . . H7B H 0.2470 0.6446 0.6288 0.062 Uiso 1 1 calc R . . C8 C 0.2935(2) 0.57022(17) 0.47281(15) 0.0503(5) Uani 1 1 d . . . H8A H 0.2525 0.5204 0.5068 0.060 Uiso 1 1 calc R . . H8B H 0.3954 0.5942 0.5033 0.060 Uiso 1 1 calc R . . C9 C 0.2443(2) 0.51333(16) 0.35936(15) 0.0466(5) Uani 1 1 d . . . C10 C 0.3415(2) 0.50808(17) 0.31450(16) 0.0506(5) Uani 1 1 d . . . H10A H 0.4373 0.5408 0.3552 0.061 Uiso 1 1 calc R . . C11 C 0.3006(2) 0.45556(17) 0.21069(16) 0.0495(5) Uani 1 1 d . . . C12 C 0.1575(2) 0.41313(18) 0.15260(16) 0.0510(5) Uani 1 1 d . . . H12A H 0.1284 0.3802 0.0821 0.061 Uiso 1 1 calc R . . C13 C 0.0540(2) 0.41638(16) 0.19264(15) 0.0475(5) Uani 1 1 d . . . C14 C 0.0986(2) 0.46354(16) 0.29929(15) 0.0434(5) Uani 1 1 d . B . C15 C 0.3208(3) 0.7455(2) 0.44860(19) 0.0646(6) Uani 1 1 d . B . H15A H 0.4076 0.7410 0.4453 0.078 Uiso 1 1 calc R A 1 H15B H 0.3452 0.8150 0.4947 0.078 Uiso 1 1 calc R A 1 C16 C 0.2264(7) 0.7363(6) 0.3415(6) 0.0892(18) Uani 0.50 1 d P B 1 H16A H 0.236(8) 0.820(7) 0.327(5) 0.107 Uiso 0.50 1 d P C 1 H16B H 0.200(6) 0.660(5) 0.275(5) 0.107 Uiso 0.50 1 d P D 1 C16' C 0.2314(6) 0.8012(4) 0.4069(4) 0.0572(12) Uani 0.50 1 d P B 2 H16C H 0.225(5) 0.842(4) 0.457(4) 0.069 Uiso 0.50 1 d P E 2 H16D H 0.274(6) 0.850(5) 0.367(4) 0.069 Uiso 0.50 1 d P F 2 C17 C 0.0065(5) 0.7485(4) 0.2649(3) 0.1401(16) Uani 1 1 d . B . H17A H 0.0664 0.8033 0.2456 0.210 Uiso 1 1 calc R . . H17B H -0.0521 0.7751 0.2923 0.210 Uiso 1 1 calc R . . H17C H -0.0520 0.6878 0.2051 0.210 Uiso 1 1 calc R . . C18 C 0.3705(3) 1.07692(19) 0.7878(2) 0.0704(7) Uani 1 1 d . . . C19 C 0.4468(4) 1.0640(3) 0.8923(2) 0.1153(12) Uani 1 1 d . B . H19A H 0.3787 1.0324 0.9213 0.173 Uiso 1 1 calc R . . H19B H 0.5130 1.1327 0.9389 0.173 Uiso 1 1 calc R . . H19C H 0.4962 1.0189 0.8820 0.173 Uiso 1 1 calc R . . C20 C 0.2952(4) 1.1514(2) 0.8078(3) 0.1007(10) Uani 1 1 d . B . H20A H 0.2278 1.1203 0.8375 0.151 Uiso 1 1 calc R . . H20B H 0.2473 1.1610 0.7436 0.151 Uiso 1 1 calc R . . H20C H 0.3636 1.2192 0.8549 0.151 Uiso 1 1 calc R . . C21 C 0.4768(3) 1.1296(2) 0.7408(3) 0.1024(11) Uani 1 1 d . B . H21A H 0.4274 1.1381 0.6763 0.154 Uiso 1 1 calc R . . H21B H 0.5269 1.0855 0.7288 0.154 Uiso 1 1 calc R . . H21C H 0.5426 1.1983 0.7877 0.154 Uiso 1 1 calc R . . C22 C -0.1332(3) 0.81168(19) 0.56710(19) 0.0630(6) Uani 1 1 d . . . C23 C -0.2048(3) 0.7464(3) 0.6251(4) 0.1175(13) Uani 1 1 d . B . H23A H -0.2659 0.6760 0.5796 0.176 Uiso 1 1 calc R . . H23B H -0.2594 0.7795 0.6505 0.176 Uiso 1 1 calc R . . H23C H -0.1348 0.7418 0.6823 0.176 Uiso 1 1 calc R . . C24 C -0.1620(3) 0.9128(2) 0.5762(3) 0.0971(10) Uani 1 1 d . B . H24A H -0.1423 0.9438 0.5235 0.146 Uiso 1 1 calc R . . H24B H -0.1025 0.9627 0.6432 0.146 Uiso 1 1 calc R . . H24C H -0.2593 0.8957 0.5674 0.146 Uiso 1 1 calc R . . C25 C -0.1989(4) 0.7527(4) 0.4508(3) 0.1406(18) Uani 1 1 d . B . H25A H -0.1468 0.7926 0.4155 0.211 Uiso 1 1 calc R . . H25B H -0.2954 0.7451 0.4240 0.211 Uiso 1 1 calc R . . H25C H -0.1955 0.6833 0.4400 0.211 Uiso 1 1 calc R . . C26 C 0.4102(2) 0.4461(2) 0.16466(18) 0.0577(6) Uani 1 1 d . B . C27 C 0.5000(14) 0.3906(9) 0.2284(8) 0.059(3) Uani 0.30 1 d P B 1 H27A H 0.4374 0.3228 0.2278 0.088 Uiso 0.30 1 calc PR B 1 H27B H 0.5518 0.4354 0.2985 0.088 Uiso 0.30 1 calc PR B 1 H27C H 0.5649 0.3802 0.1970 0.088 Uiso 0.30 1 calc PR B 1 C28 C 0.5092(13) 0.5473(9) 0.1773(11) 0.228(7) Uani 0.70 1 d P B 1 H28A H 0.5982 0.5601 0.2288 0.342 Uiso 0.70 1 calc PR B 1 H28B H 0.4762 0.6008 0.1991 0.342 Uiso 0.70 1 calc PR B 1 H28C H 0.5208 0.5503 0.1127 0.342 Uiso 0.70 1 calc PR B 1 C29 C 0.3451(12) 0.3882(11) 0.0552(8) 0.219(6) Uani 0.70 1 d P B 1 H29A H 0.2976 0.3137 0.0466 0.329 Uiso 0.70 1 calc PR B 1 H29B H 0.4167 0.3979 0.0256 0.329 Uiso 0.70 1 calc PR B 1 H29C H 0.2781 0.4148 0.0211 0.329 Uiso 0.70 1 calc PR B 1 C27' C 0.4878(17) 0.3977(15) 0.2203(11) 0.295(10) Uani 0.70 1 d P B 2 H27D H 0.4247 0.3309 0.2213 0.442 Uiso 0.70 1 calc PR B 2 H27E H 0.5415 0.4434 0.2899 0.442 Uiso 0.70 1 calc PR B 2 H27F H 0.5509 0.3853 0.1880 0.442 Uiso 0.70 1 calc PR B 2 C28' C 0.5062(12) 0.5633(10) 0.1666(7) 0.049(3) Uani 0.30 1 d P B 2 H28D H 0.5421 0.6112 0.2351 0.074 Uiso 0.30 1 calc PR B 2 H28E H 0.4501 0.5883 0.1187 0.074 Uiso 0.30 1 calc PR B 2 H28F H 0.5837 0.5603 0.1471 0.074 Uiso 0.30 1 calc PR B 2 C29' C 0.3458(11) 0.3761(6) 0.0484(6) 0.0349(19) Uani 0.30 1 d P B 2 H29D H 0.3013 0.3024 0.0442 0.052 Uiso 0.30 1 calc PR B 2 H29E H 0.4197 0.3849 0.0213 0.052 Uiso 0.30 1 calc PR B 2 H29F H 0.2770 0.3982 0.0087 0.052 Uiso 0.30 1 calc PR B 2 C30 C -0.1036(2) 0.3661(2) 0.12103(17) 0.0622(6) Uani 1 1 d . B . C31 C -0.1238(3) 0.3317(3) 0.00660(19) 0.0871(9) Uani 1 1 d . . . H31A H -0.0874 0.2778 -0.0050 0.131 Uiso 1 1 calc R B . H31B H -0.0741 0.3922 -0.0118 0.131 Uiso 1 1 calc R . . H31C H -0.2226 0.3036 -0.0352 0.131 Uiso 1 1 calc R . . C32 C -0.1831(3) 0.2716(3) 0.1493(2) 0.1074(12) Uani 1 1 d . . . H32A H -0.1432 0.2192 0.1425 0.161 Uiso 1 1 calc R B . H32B H -0.2806 0.2412 0.1039 0.161 Uiso 1 1 calc R . . H32C H -0.1765 0.2941 0.2196 0.161 Uiso 1 1 calc R . . C33 C -0.1668(3) 0.4519(3) 0.1313(3) 0.1032(11) Uani 1 1 d . . . H33A H -0.2649 0.4214 0.0871 0.155 Uiso 1 1 calc R B . H33B H -0.1167 0.5109 0.1112 0.155 Uiso 1 1 calc R . . H33C H -0.1579 0.4765 0.2018 0.155 Uiso 1 1 calc R . . H1 H 0.014(3) 0.409(2) 0.405(2) 0.086(8) Uiso 1 1 d . . . C34 C -0.109(3) -0.012(3) -0.073(2) 0.58(3) Uani 1 1 d . . . H34A H -0.0652 -0.0122 -0.1240 0.691 Uiso 1 1 calc R . . H34B H -0.0885 0.0635 -0.0458 0.691 Uiso 1 1 calc R . . C35 C -0.224(3) -0.028(2) -0.1371(18) 0.503(16) Uani 1 1 d . . . H35A H -0.2124 0.0256 -0.1726 0.755 Uiso 1 1 calc R . . H35B H -0.2885 -0.0254 -0.1031 0.755 Uiso 1 1 calc R . . H35C H -0.2598 -0.0971 -0.1861 0.755 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 Li1 0.050(2) 0.056(2) 0.050(2) 0.0117(16) 0.0187(17) 0.0199(17) O1 0.0426(8) 0.0449(8) 0.0455(8) 0.0047(6) 0.0158(6) 0.0081(6) O2 0.0400(7) 0.0512(8) 0.0486(8) 0.0101(7) 0.0211(6) 0.0125(6) O3 0.0770(12) 0.0817(13) 0.0728(12) 0.0380(10) 0.0307(10) 0.0360(10) O4 0.42(7) 0.88(6) 0.26(4) 0.10(4) -0.15(3) 0.33(6) N 0.0446(9) 0.0468(10) 0.0454(10) 0.0085(7) 0.0199(8) 0.0123(8) C1 0.0457(11) 0.0429(11) 0.0386(11) 0.0072(8) 0.0164(9) 0.0098(9) C2 0.0497(12) 0.0513(13) 0.0460(12) 0.0093(9) 0.0169(10) 0.0162(10) C3 0.0618(14) 0.0475(13) 0.0561(14) 0.0105(10) 0.0210(11) 0.0203(11) C4 0.0600(14) 0.0471(12) 0.0486(13) 0.0081(10) 0.0180(11) 0.0129(11) C5 0.0449(12) 0.0560(13) 0.0473(12) 0.0059(10) 0.0118(10) 0.0093(10) C6 0.0450(11) 0.0483(12) 0.0428(11) 0.0068(9) 0.0150(9) 0.0139(10) C7 0.0411(11) 0.0558(13) 0.0468(12) 0.0055(10) 0.0121(9) 0.0134(10) C8 0.0365(10) 0.0560(13) 0.0490(12) 0.0073(10) 0.0121(9) 0.0140(10) C9 0.0420(11) 0.0517(12) 0.0443(11) 0.0102(9) 0.0168(9) 0.0174(10) C10 0.0383(11) 0.0574(13) 0.0534(13) 0.0112(10) 0.0168(10) 0.0181(10) C11 0.0493(12) 0.0542(13) 0.0527(13) 0.0175(10) 0.0259(10) 0.0227(10) C12 0.0501(12) 0.0577(13) 0.0435(12) 0.0114(9) 0.0192(10) 0.0194(10) C13 0.0437(11) 0.0500(12) 0.0454(12) 0.0109(9) 0.0170(9) 0.0154(10) C14 0.0377(10) 0.0459(11) 0.0477(12) 0.0124(9) 0.0191(9) 0.0157(9) C15 0.0607(14) 0.0566(14) 0.0739(17) 0.0171(12) 0.0356(13) 0.0115(12) C16 0.092(5) 0.094(5) 0.087(5) 0.040(4) 0.046(4) 0.025(4) C16' 0.070(3) 0.050(3) 0.055(3) 0.018(2) 0.033(3) 0.019(3) C17 0.151(4) 0.156(4) 0.134(3) 0.088(3) 0.033(3) 0.080(3) C18 0.0696(16) 0.0474(14) 0.0657(16) 0.0019(11) 0.0123(13) 0.0069(12) C19 0.125(3) 0.083(2) 0.068(2) -0.0081(16) -0.0127(19) 0.013(2) C20 0.106(2) 0.0544(17) 0.108(2) -0.0112(15) 0.030(2) 0.0158(16) C21 0.084(2) 0.0656(18) 0.126(3) 0.0101(17) 0.040(2) -0.0009(16) C22 0.0547(13) 0.0610(15) 0.0710(16) 0.0119(12) 0.0198(12) 0.0268(12) C23 0.077(2) 0.117(3) 0.207(4) 0.088(3) 0.081(2) 0.051(2) C24 0.0720(18) 0.079(2) 0.138(3) 0.0286(19) 0.0247(18) 0.0415(16) C25 0.098(2) 0.185(4) 0.090(2) -0.029(3) -0.027(2) 0.085(3) C26 0.0526(13) 0.0748(16) 0.0567(14) 0.0188(12) 0.0305(11) 0.0296(13) C27 0.070(6) 0.092(6) 0.045(5) 0.034(5) 0.020(5) 0.063(6) C28 0.221(10) 0.120(8) 0.374(16) 0.004(8) 0.256(11) 0.011(7) C29 0.138(8) 0.364(15) 0.156(9) -0.014(9) 0.097(7) 0.108(9) C27' 0.372(16) 0.62(3) 0.292(13) 0.329(16) 0.288(13) 0.45(2) C28' 0.040(5) 0.054(6) 0.039(4) 0.021(4) 0.014(4) -0.005(4) C29' 0.048(5) 0.032(3) 0.023(4) -0.002(3) 0.018(4) 0.013(3) C30 0.0451(12) 0.0830(17) 0.0456(13) 0.0129(12) 0.0139(10) 0.0149(12) C31 0.0567(15) 0.124(3) 0.0493(15) 0.0093(15) 0.0091(12) 0.0153(16) C32 0.0731(19) 0.113(3) 0.0673(19) 0.0208(17) 0.0044(15) -0.0262(18) C33 0.0679(18) 0.158(3) 0.085(2) 0.026(2) 0.0138(16) 0.065(2) C34 0.47(5) 0.72(5) 0.38(4) -0.03(4) -0.10(3) 0.37(4) C35 0.51(4) 0.69(4) 0.46(3) 0.09(3) 0.27(3) 0.38(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.924(4) . ? Li1 O1 1.928(4) . ? Li1 O3 2.045(4) . ? Li1 N 2.058(4) . ? Li1 C1 2.726(4) . ? Li1 C14 2.738(4) . ? O1 C1 1.369(2) . ? O2 C14 1.374(2) . ? O2 H1 1.20(3) . ? O3 C17 1.414(4) . ? O3 C16' 1.474(6) . ? O4 O4 0.77(3) 2 ? O4 C34 0.888(19) . ? O4 C34 1.64(3) 2 ? N C15 1.468(3) . ? N C8 1.475(3) . ? N C7 1.475(3) . ? C1 C2 1.401(3) . ? C1 C6 1.413(3) . ? C2 C3 1.400(3) . ? C2 C22 1.540(3) . ? C3 C4 1.381(3) . ? C3 H3A 0.9300 . ? C4 C5 1.391(3) . ? C4 C18 1.532(3) . ? C5 C6 1.379(3) . ? C5 H5A 0.9300 . ? C6 C7 1.505(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.506(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.382(3) . ? C9 C14 1.409(3) . ? C10 C11 1.386(3) . ? C10 H10A 0.9300 . ? C11 C12 1.382(3) . ? C11 C26 1.528(3) . ? C12 C13 1.395(3) . ? C12 H12A 0.9300 . ? C13 C14 1.400(3) . ? C13 C30 1.545(3) . ? C15 C16' 1.474(6) . ? C15 C16 1.515(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 1.19(9) . ? C16 H16B 1.18(7) . ? C16 H16D 1.43(6) . ? C16' H16A 1.21(8) . ? C16' H16C 0.86(5) . ? C16' H16D 1.03(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C21 1.530(4) . ? C18 C19 1.539(4) . ? C18 C20 1.539(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.499(4) . ? C22 C24 1.522(4) . ? C22 C25 1.535(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27' 1.389(11) . ? C26 C28 1.404(10) . ? C26 C29 1.450(11) . ? C26 C29' 1.572(9) . ? C26 C27 1.598(12) . ? C26 C28' 1.609(11) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C27' H27D 0.9600 . ? C27' H27E 0.9600 . ? C27' H27F 0.9600 . ? C28' H28D 0.9600 . ? C28' H28E 0.9600 . ? C28' H28F 0.9600 . ? C29' H29D 0.9600 . ? C29' H29E 0.9600 . ? C29' H29F 0.9600 . ? C30 C32 1.502(4) . ? C30 C31 1.531(3) . ? C30 C33 1.555(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.22(2) . ? C34 O4 1.64(3) 2 ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? 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 Li1 O1 126.6(2) . . ? O2 Li1 O3 115.68(18) . . ? O1 Li1 O3 116.49(18) . . ? O2 Li1 N 97.90(16) . . ? O1 Li1 N 98.08(16) . . ? O3 Li1 N 83.78(15) . . ? O2 Li1 C1 150.50(18) . . ? O1 Li1 C1 28.07(8) . . ? O3 Li1 C1 93.43(14) . . ? N Li1 C1 79.70(13) . . ? O2 Li1 C14 27.90(7) . . ? O1 Li1 C14 149.95(18) . . ? O3 Li1 C14 93.12(14) . . ? N Li1 C14 79.14(12) . . ? C1 Li1 C14 157.02(16) . . ? C1 O1 Li1 110.41(15) . . ? C14 O2 Li1 111.15(15) . . ? C14 O2 H1 108.0(12) . . ? Li1 O2 H1 113.7(13) . . ? C17 O3 C16' 115.5(3) . . ? C17 O3 Li1 131.9(2) . . ? C16' O3 Li1 107.9(2) . . ? O4 O4 C34 166(10) 2 . ? O4 O4 C34 7(6) 2 2 ? C34 O4 C34 174(5) . 2 ? C15 N C8 112.49(16) . . ? C15 N C7 112.84(17) . . ? C8 N C7 109.81(15) . . ? C15 N Li1 107.55(17) . . ? C8 N Li1 107.00(16) . . ? C7 N Li1 106.80(15) . . ? O1 C1 C2 122.64(18) . . ? O1 C1 C6 117.78(17) . . ? C2 C1 C6 119.58(19) . . ? O1 C1 Li1 41.52(11) . . ? C2 C1 Li1 134.38(16) . . ? C6 C1 Li1 92.28(14) . . ? C3 C2 C1 117.3(2) . . ? C3 C2 C22 119.72(19) . . ? C1 C2 C22 122.95(19) . . ? C4 C3 C2 124.3(2) . . ? C4 C3 H3A 117.8 . . ? C2 C3 H3A 117.8 . . ? C3 C4 C5 116.6(2) . . ? C3 C4 C18 123.5(2) . . ? C5 C4 C18 119.9(2) . . ? C6 C5 C4 122.0(2) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C1 119.94(19) . . ? C5 C6 C7 120.18(19) . . ? C1 C6 C7 119.86(18) . . ? N C7 C6 113.38(17) . . ? N C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? N C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N C8 C9 112.93(16) . . ? N C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C14 119.93(18) . . ? C10 C9 C8 120.18(18) . . ? C14 C9 C8 119.88(17) . . ? C9 C10 C11 122.02(19) . . ? C9 C10 H10A 119.0 . . ? C11 C10 H10A 119.0 . . ? C12 C11 C10 116.56(18) . . ? C12 C11 C26 122.66(19) . . ? C10 C11 C26 120.78(19) . . ? C11 C12 C13 124.32(19) . . ? C11 C12 H12A 117.8 . . ? C13 C12 H12A 117.8 . . ? C12 C13 C14 117.39(18) . . ? C12 C13 C30 120.30(18) . . ? C14 C13 C30 122.28(17) . . ? O2 C14 C13 122.63(17) . . ? O2 C14 C9 117.89(17) . . ? C13 C14 C9 119.49(17) . . ? O2 C14 Li1 40.94(11) . . ? C13 C14 Li1 134.33(15) . . ? C9 C14 Li1 92.35(14) . . ? N C15 C16' 114.3(3) . . ? N C15 C16 113.3(3) . . ? C16' C15 C16 45.1(4) . . ? N C15 H15A 108.9 . . ? C16' C15 H15A 135.8 . . ? C16 C15 H15A 108.9 . . ? N C15 H15B 108.9 . . ? C16' C15 H15B 66.3 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C15 C16 H16A 114(3) . . ? C15 C16 H16B 116(3) . . ? H16A C16 H16B 123(5) . . ? C15 C16 H16D 90(2) . . ? H16A C16 H16D 23(4) . . ? H16B C16 H16D 143(4) . . ? O3 C16' C15 106.7(4) . . ? O3 C16' H16A 85(4) . . ? C15 C16' H16A 115(4) . . ? O3 C16' H16C 110(3) . . ? C15 C16' H16C 109(3) . . ? H16A C16' H16C 127(5) . . ? O3 C16' H16D 112(3) . . ? C15 C16' H16D 112(3) . . ? H16A C16' H16D 29(4) . . ? H16C C16' H16D 107(5) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 C18 C4 109.8(2) . . ? C21 C18 C19 110.7(3) . . ? C4 C18 C19 108.5(2) . . ? C21 C18 C20 107.6(2) . . ? C4 C18 C20 112.2(2) . . ? C19 C18 C20 108.0(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C24 109.1(2) . . ? C23 C22 C25 110.5(3) . . ? C24 C22 C25 104.9(2) . . ? C23 C22 C2 109.7(2) . . ? C24 C22 C2 112.5(2) . . ? C25 C22 C2 110.0(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27' C26 C28 105.2(10) . . ? C27' C26 C29 111.4(9) . . ? C28 C26 C29 108.4(8) . . ? C27' C26 C11 108.8(4) . . ? C28 C26 C11 110.9(4) . . ? C29 C26 C11 111.8(4) . . ? C27' C26 C29' 106.3(8) . . ? C28 C26 C29' 110.6(6) . . ? C29 C26 C29' 5.1(8) . . ? C11 C26 C29' 114.5(4) . . ? C27' C26 C27 0.3(10) . . ? C28 C26 C27 105.0(8) . . ? C29 C26 C27 111.3(7) . . ? C11 C26 C27 109.1(5) . . ? C29' C26 C27 106.1(5) . . ? C27' C26 C28' 113.1(9) . . ? C28 C26 C28' 8.0(9) . . ? C29 C26 C28' 103.1(7) . . ? C11 C26 C28' 108.5(5) . . ? C29' C26 C28' 105.8(5) . . ? C27 C26 C28' 112.9(6) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C27' H27D 109.5 . . ? C26 C27' H27E 109.5 . . ? H27D C27' H27E 109.5 . . ? C26 C27' H27F 109.5 . . ? H27D C27' H27F 109.5 . . ? H27E C27' H27F 109.5 . . ? C26 C28' H28D 109.5 . . ? C26 C28' H28E 109.5 . . ? H28D C28' H28E 109.5 . . ? C26 C28' H28F 109.5 . . ? H28D C28' H28F 109.5 . . ? H28E C28' H28F 109.5 . . ? C26 C29' H29D 109.5 . . ? C26 C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C26 C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C32 C30 C31 109.4(2) . . ? C32 C30 C13 110.6(2) . . ? C31 C30 C13 112.21(18) . . ? C32 C30 C33 110.4(3) . . ? C31 C30 C33 105.4(2) . . ? C13 C30 C33 108.8(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O4 C34 C35 171(6) . . ? O4 C34 O4 6(5) . 2 ? C35 C34 O4 173(4) . 2 ? O4 C34 H34A 92.9 . . ? C35 C34 H34A 92.9 . . ? O4 C34 H34A 94.2 2 . ? O4 C34 H34B 92.9 . . ? C35 C34 H34B 92.9 . . ? O4 C34 H34B 86.5 2 . ? H34A C34 H34B 103.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.257 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.040 #==END