# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Makoto Yasuda' _publ_contact_author_email yasuda@chem.eng.osaka-u.ac.jp loop_ _publ_author_name H.Nakajima M.Yasuda A.Baba data_(1aLi3)2(THF)6 _database_code_depnum_ccdc_archive 'CCDC 861321' #TrackingRef '- all-CIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C78 H90 Li6 O12' _chemical_formula_moiety 'C78 H90 Li6 O12' _chemical_formula_weight 1261.21 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_Int_Tables_number 205 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, z, x' 'z, x, y' 'x+1/2, y, -z+1/2' 'y+1/2, z, -x+1/2' 'z+1/2, x, -y+1/2' 'y+1/2, -z+1/2, -x' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' '-x, y+1/2, -z+1/2' '-y, z+1/2, -x+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' '-y, -z, -x' '-z, -x, -y' '-x-1/2, -y, z-1/2' '-y-1/2, -z, x-1/2' '-z-1/2, -x, y-1/2' '-y-1/2, z-1/2, x' '-z-1/2, x-1/2, y' 'z, -x-1/2, y-1/2' 'x, -y-1/2, z-1/2' 'y, -z-1/2, x-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.2239(12) _cell_length_b 19.2239(12) _cell_length_c 19.2239(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7104.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 10974 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 30.41 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9701 _exptl_absorpt_correction_T_max 0.9774 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 3341 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 23.49 _reflns_number_total 1758 _reflns_number_gt 1229 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DELU C10 > C17 SIMU 0.04 0.08 C10 > C17 SAME C14 > C17 SAME C13 < C10 ; _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^)+(0.1201P)^2^+10.2345P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1758 _refine_ls_number_parameters 182 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_gt 0.1069 _refine_ls_wR_factor_ref 0.2869 _refine_ls_wR_factor_gt 0.2622 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.061 _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 O1 O 0.42101(15) 0.44898(15) 0.06844(15) 0.0626(10) Uani 1 1 d . . . O2 O 0.4681(2) 0.28540(18) 0.0167(2) 0.0859(12) Uani 1 1 d . . . C1 C 0.3722(2) 0.4405(2) 0.1166(2) 0.0630(13) Uani 1 1 d . . . C2 C 0.3392(3) 0.4979(3) 0.1450(3) 0.0907(19) Uani 1 1 d . . . H1 H 0.3514 0.5419 0.1291 0.109 Uiso 1 1 calc R . . C3 C 0.2881(3) 0.4923(3) 0.1968(4) 0.101(2) Uani 1 1 d . . . C4 C 0.2702(3) 0.4269(3) 0.2203(3) 0.0896(18) Uani 1 1 d . . . H2 H 0.2373 0.4219 0.2555 0.108 Uiso 1 1 calc R . . C5 C 0.3006(3) 0.3701(3) 0.1919(3) 0.0866(17) Uani 1 1 d . . . H3 H 0.2876 0.3261 0.2073 0.104 Uiso 1 1 calc R . . C6 C 0.3508(3) 0.3761(3) 0.1404(3) 0.0781(15) Uani 1 1 d . . . H4 H 0.3703 0.3361 0.1215 0.094 Uiso 1 1 calc R . . C7 C 0.2508(5) 0.5556(4) 0.2256(6) 0.179(5) Uani 1 1 d . . . H5 H 0.2030 0.5550 0.2095 0.214 Uiso 1 1 calc R . . H6 H 0.2500 0.5523 0.2760 0.214 Uiso 1 1 calc R . . C8 C 0.2834(5) 0.6244(3) 0.2054(5) 0.103(2) Uani 1 1 d . . . C9 C 0.3407(5) 0.6479(5) 0.2395(3) 0.107(2) Uani 1 1 d . . . H7 H 0.3564 0.6246 0.2789 0.128 Uiso 1 1 calc R . . C10 C 0.4595(11) 0.2316(6) -0.0373(6) 0.129(5) Uani 0.623(10) 1 d PDU A 1 H10A H 0.4112 0.2295 -0.0517 0.155 Uiso 0.623(10) 1 calc PR A 1 H10B H 0.4875 0.2434 -0.0776 0.155 Uiso 0.623(10) 1 calc PR A 1 C11 C 0.4790(14) 0.1705(8) -0.0128(8) 0.182(7) Uani 0.623(10) 1 d PDU A 1 H11A H 0.5228 0.1559 -0.0332 0.218 Uiso 0.623(10) 1 calc PR A 1 H11B H 0.4440 0.1353 -0.0218 0.218 Uiso 0.623(10) 1 calc PR A 1 C12 C 0.4872(14) 0.1845(7) 0.0698(8) 0.195(7) Uani 0.623(10) 1 d PDU A 1 H12A H 0.4500 0.1620 0.0954 0.234 Uiso 0.623(10) 1 calc PR A 1 H12B H 0.5314 0.1666 0.0865 0.234 Uiso 0.623(10) 1 calc PR A 1 C13 C 0.4843(6) 0.2510(5) 0.0775(5) 0.091(3) Uani 0.623(10) 1 d PDU A 1 H13A H 0.5288 0.2675 0.0945 0.109 Uiso 0.623(10) 1 calc PR A 1 H13B H 0.4494 0.2619 0.1124 0.109 Uiso 0.623(10) 1 calc PR A 1 C14 C 0.4165(12) 0.2511(9) -0.0080(16) 0.131(8) Uani 0.377(10) 1 d PDU A 2 H14A H 0.4142 0.2596 -0.0577 0.158 Uiso 0.377(10) 1 calc PR A 2 H14B H 0.3741 0.2693 0.0124 0.158 Uiso 0.377(10) 1 calc PR A 2 C15 C 0.4178(12) 0.1838(9) 0.0021(16) 0.154(7) Uani 0.377(10) 1 d PDU A 2 H15A H 0.4059 0.1590 -0.0403 0.185 Uiso 0.377(10) 1 calc PR A 2 H15B H 0.3853 0.1704 0.0384 0.185 Uiso 0.377(10) 1 calc PR A 2 C16 C 0.4966(13) 0.1674(10) 0.025(2) 0.171(9) Uani 0.377(10) 1 d PDU A 2 H16A H 0.4979 0.1447 0.0702 0.205 Uiso 0.377(10) 1 calc PR A 2 H16B H 0.5196 0.1380 -0.0088 0.205 Uiso 0.377(10) 1 calc PR A 2 C17 C 0.5261(11) 0.2288(11) 0.0280(17) 0.153(7) Uani 0.377(10) 1 d PDU A 2 H17A H 0.5614 0.2328 -0.0079 0.184 Uiso 0.377(10) 1 calc PR A 2 H17B H 0.5482 0.2353 0.0729 0.184 Uiso 0.377(10) 1 calc PR A 2 Li1 Li 0.4803(4) 0.3905(4) 0.0093(4) 0.065(2) Uani 1 1 d . A . 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 O1 0.0603(19) 0.0642(19) 0.063(2) -0.0009(15) 0.0106(16) 0.0019(15) O2 0.109(3) 0.062(2) 0.086(3) 0.002(2) -0.008(2) -0.001(2) C1 0.059(3) 0.066(3) 0.063(3) 0.002(2) 0.005(2) -0.005(2) C2 0.089(4) 0.067(3) 0.116(5) 0.009(3) 0.044(4) 0.000(3) C3 0.094(4) 0.090(4) 0.119(5) 0.003(4) 0.051(4) 0.004(3) C4 0.076(4) 0.096(4) 0.097(4) 0.012(3) 0.034(3) -0.005(3) C5 0.090(4) 0.083(4) 0.086(4) 0.018(3) 0.011(3) -0.016(3) C6 0.089(4) 0.066(3) 0.079(4) -0.003(3) 0.009(3) -0.008(3) C7 0.180(8) 0.093(5) 0.264(11) -0.004(6) 0.155(9) 0.008(5) C8 0.093(6) 0.083(4) 0.131(6) -0.005(5) 0.055(5) 0.023(4) C9 0.108(6) 0.138(7) 0.074(4) -0.004(5) 0.026(5) 0.054(5) C10 0.223(16) 0.068(7) 0.096(7) -0.014(6) -0.009(9) 0.012(8) C11 0.298(17) 0.101(8) 0.146(10) -0.026(7) -0.060(13) 0.051(11) C12 0.365(18) 0.094(8) 0.126(9) 0.010(8) -0.044(13) 0.026(12) C13 0.127(8) 0.066(5) 0.079(6) 0.019(5) -0.020(6) -0.007(6) C14 0.149(17) 0.065(9) 0.18(2) 0.009(13) -0.049(15) -0.023(11) C15 0.198(15) 0.063(8) 0.202(18) -0.018(12) -0.009(16) -0.009(11) C16 0.245(16) 0.073(10) 0.20(2) -0.014(15) -0.04(2) 0.044(11) C17 0.189(15) 0.093(11) 0.179(18) -0.004(13) -0.032(15) 0.015(12) Li1 0.070(5) 0.058(5) 0.068(5) -0.005(4) 0.001(4) -0.002(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 O1 C1 1.329(5) . ? O1 Li1 1.963(8) . ? O1 Li1 1.965(8) 23_565 ? O1 Li1 1.967(9) 6 ? O2 C14 1.283(19) . ? O2 C13 1.379(9) . ? O2 C10 1.476(12) . ? O2 C17 1.57(2) . ? O2 Li1 2.038(8) . ? C1 C6 1.383(6) . ? C1 C2 1.385(7) . ? C1 Li1 2.749(9) 6 ? C2 C3 1.402(7) . ? C2 H1 0.9300 . ? C3 C4 1.379(8) . ? C3 C7 1.517(9) . ? C4 C5 1.353(8) . ? C4 H2 0.9300 . ? C5 C6 1.387(7) . ? C5 H3 0.9300 . ? C6 H4 0.9300 . ? C7 C8 1.513(9) . ? C7 H5 0.9700 . ? C7 H6 0.9700 . ? C8 C9 1.361(8) . ? C8 C9 1.365(8) 18_665 ? C9 C8 1.365(8) 11_655 ? C9 H7 0.9300 . ? C10 C11 1.319(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.618(17) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.288(13) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.309(16) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.61(2) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.310(17) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? Li1 O1 1.964(8) 6 ? Li1 O1 1.967(9) 23_565 ? Li1 Li1 2.646(12) 6 ? Li1 Li1 2.646(12) 23_565 ? Li1 C1 2.749(9) 23_565 ? Li1 Li1 3.382(13) 18_665 ? Li1 Li1 3.382(13) 11_655 ? 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 C1 O1 Li1 138.0(4) . . ? C1 O1 Li1 116.1(4) . 23_565 ? Li1 O1 Li1 84.7(3) . 23_565 ? C1 O1 Li1 111.6(3) . 6 ? Li1 O1 Li1 84.6(3) . 6 ? Li1 O1 Li1 118.7(4) 23_565 6 ? C14 O2 C13 104.0(11) . . ? C14 O2 C10 44.9(13) . . ? C13 O2 C10 106.6(7) . . ? C14 O2 C17 104.1(12) . . ? C13 O2 C17 52.5(12) . . ? C10 O2 C17 72.0(11) . . ? C14 O2 Li1 124.9(8) . . ? C13 O2 Li1 120.6(5) . . ? C10 O2 Li1 131.2(6) . . ? C17 O2 Li1 127.9(8) . . ? O1 C1 C6 123.4(4) . . ? O1 C1 C2 120.0(4) . . ? C6 C1 C2 116.6(5) . . ? O1 C1 Li1 41.7(2) . 6 ? C6 C1 Li1 123.4(4) . 6 ? C2 C1 Li1 103.7(4) . 6 ? C1 C2 C3 122.6(5) . . ? C1 C2 H1 118.7 . . ? C3 C2 H1 118.7 . . ? C4 C3 C2 118.6(5) . . ? C4 C3 C7 119.5(5) . . ? C2 C3 C7 121.9(6) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H2 120.2 . . ? C3 C4 H2 120.2 . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H3 119.3 . . ? C6 C5 H3 119.3 . . ? C1 C6 C5 121.2(5) . . ? C1 C6 H4 119.4 . . ? C5 C6 H4 119.4 . . ? C8 C7 C3 114.3(5) . . ? C8 C7 H5 108.7 . . ? C3 C7 H5 108.7 . . ? C8 C7 H6 108.7 . . ? C3 C7 H6 108.7 . . ? H5 C7 H6 107.6 . . ? C9 C8 C9 119.2(8) . 18_665 ? C9 C8 C7 120.1(12) . . ? C9 C8 C7 120.3(12) 18_665 . ? C8 C9 C8 120.8(8) . 11_655 ? C8 C9 H7 119.6 . . ? C8 C9 H7 119.6 11_655 . ? C11 C10 O2 109.9(10) . . ? C11 C10 H10A 109.7 . . ? O2 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? O2 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C10 C11 C12 103.4(11) . . ? C10 C11 H11A 111.1 . . ? C12 C11 H11A 111.1 . . ? C10 C11 H11B 111.1 . . ? C12 C11 H11B 111.1 . . ? H11A C11 H11B 109.1 . . ? C13 C12 C11 105.8(10) . . ? C13 C12 H12A 110.6 . . ? C11 C12 H12A 110.6 . . ? C13 C12 H12B 110.6 . . ? C11 C12 H12B 110.6 . . ? H12A C12 H12B 108.7 . . ? C12 C13 O2 112.9(9) . . ? C12 C13 H13A 109.0 . . ? O2 C13 H13A 109.0 . . ? C12 C13 H13B 109.0 . . ? O2 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? O2 C14 C15 116.1(15) . . ? O2 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? O2 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 104.5(14) . . ? C14 C15 H15A 110.8 . . ? C16 C15 H15A 110.8 . . ? C14 C15 H15B 110.8 . . ? C16 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C17 C16 C15 104.1(14) . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16B 110.9 . . ? C15 C16 H16B 110.9 . . ? H16A C16 H16B 109.0 . . ? C16 C17 O2 108.1(14) . . ? C16 C17 H17A 110.1 . . ? O2 C17 H17A 110.1 . . ? C16 C17 H17B 110.1 . . ? O2 C17 H17B 110.1 . . ? H17A C17 H17B 108.4 . . ? O1 Li1 O1 95.4(4) . 6 ? O1 Li1 O1 95.3(4) . 23_565 ? O1 Li1 O1 119.7(4) 6 23_565 ? O1 Li1 O2 117.4(4) . . ? O1 Li1 O2 111.5(4) 6 . ? O1 Li1 O2 115.0(4) 23_565 . ? O1 Li1 Li1 47.7(3) . 6 ? O1 Li1 Li1 47.62(15) 6 6 ? O1 Li1 Li1 115.5(3) 23_565 6 ? O2 Li1 Li1 128.3(4) . 6 ? O1 Li1 Li1 47.7(3) . 23_565 ? O1 Li1 Li1 115.6(3) 6 23_565 ? O1 Li1 Li1 47.61(15) 23_565 23_565 ? O2 Li1 Li1 131.4(4) . 23_565 ? Li1 Li1 Li1 79.4(4) 6 23_565 ? O1 Li1 C1 115.0(4) . 23_565 ? O1 Li1 C1 130.2(4) 6 23_565 ? O1 Li1 C1 26.71(16) 23_565 23_565 ? O2 Li1 C1 89.2(3) . 23_565 ? Li1 Li1 C1 142.1(3) 6 23_565 ? Li1 Li1 C1 69.6(2) 23_565 23_565 ? O1 Li1 Li1 90.2(2) . 18_665 ? O1 Li1 Li1 90.3(2) 6 18_665 ? O1 Li1 Li1 30.6(2) 23_565 18_665 ? O2 Li1 Li1 141.4(4) . 18_665 ? Li1 Li1 Li1 90.0 6 18_665 ? Li1 Li1 Li1 50.3(2) 23_565 18_665 ? C1 Li1 Li1 53.4(3) 23_565 18_665 ? O1 Li1 Li1 90.3(2) . 11_655 ? O1 Li1 Li1 30.7(2) 6 11_655 ? O1 Li1 Li1 90.2(2) 23_565 11_655 ? O2 Li1 Li1 138.6(4) . 11_655 ? Li1 Li1 Li1 50.3(2) 6 11_655 ? Li1 Li1 Li1 90.0 23_565 11_655 ? C1 Li1 Li1 107.1(2) 23_565 11_655 ? Li1 Li1 Li1 60.0 18_665 11_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.293 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.047 data_(1bLi3)2(THF)6 _database_code_depnum_ccdc_archive 'CCDC 861322' #TrackingRef '- all-CIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C84 H102 Li6 O12 ' _chemical_formula_moiety 'C84 H102 Li6 O12 ' _chemical_formula_weight 1345.37 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_space_group_name_Hall '-P 2ac 2ab 3' _symmetry_Int_Tables_number 205 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, z, x' 'z, x, y' 'x+1/2, y, -z+1/2' 'y+1/2, z, -x+1/2' 'z+1/2, x, -y+1/2' 'y+1/2, -z+1/2, -x' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' '-x, y+1/2, -z+1/2' '-y, z+1/2, -x+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' '-y, -z, -x' '-z, -x, -y' '-x-1/2, -y, z-1/2' '-y-1/2, -z, x-1/2' '-z-1/2, -x, y-1/2' '-y-1/2, z-1/2, x' '-z-1/2, x-1/2, y' 'z, -x-1/2, y-1/2' 'x, -y-1/2, z-1/2' 'y, -z-1/2, x-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.5449(6) _cell_length_b 19.5449(6) _cell_length_c 19.5449(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7466.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 31107 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9411 _exptl_absorpt_correction_T_max 0.9699 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 4179 _diffrn_reflns_av_R_equivalents 0.0104 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 24.97 _reflns_number_total 2190 _reflns_number_gt 1763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1662P)^2^+4.1433P] 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 2190 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0845 _refine_ls_wR_factor_ref 0.2687 _refine_ls_wR_factor_gt 0.2544 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 O1 O 0.42206(10) 0.05109(10) 0.56756(9) 0.0537(6) Uani 1 1 d . . . O2 O 0.28879(12) 0.01590(13) 0.47018(16) 0.0852(9) Uani 1 1 d . . . C1 C 0.37375(14) 0.05971(14) 0.61506(14) 0.0524(7) Uani 1 1 d . . . C2 C 0.34404(15) 0.00286(15) 0.64729(15) 0.0559(8) Uani 1 1 d . . . C3 C 0.29452(15) 0.00914(16) 0.69786(16) 0.0605(8) Uani 1 1 d . . . C4 C 0.27349(18) 0.07478(18) 0.71665(18) 0.0706(10) Uani 1 1 d . . . C5 C 0.30125(19) 0.13095(18) 0.6855(2) 0.0761(10) Uani 1 1 d . . . C6 C 0.35113(18) 0.12425(16) 0.63511(18) 0.0676(9) Uani 1 1 d . . . C7 C 0.29094(16) -0.12073(16) 0.70734(16) 0.0616(8) Uani 1 1 d . . . C8 C 0.26305(15) -0.15050(17) 0.64881(17) 0.0632(9) Uani 1 1 d . . . C9 C 0.2633(2) -0.05306(19) 0.7326(2) 0.0796(11) Uani 1 1 d . . . C10 C 0.2027(2) -0.1169(3) 0.6137(3) 0.0960(13) Uani 1 1 d . . . H7 H 0.1609 -0.1343 0.6326 0.115 Uiso 1 1 calc R . . H8 H 0.2042 -0.1267 0.5656 0.115 Uiso 1 1 calc R . . H9 H 0.2048 -0.0683 0.6205 0.115 Uiso 1 1 calc R . . C11 C 0.2510(3) 0.0702(3) 0.4974(4) 0.136(2) Uani 1 1 d . . . H10 H 0.2564 0.0707 0.5468 0.163 Uiso 1 1 calc R . . H11 H 0.2690 0.1130 0.4798 0.163 Uiso 1 1 calc R . . C12 C 0.1854(4) 0.0660(5) 0.4824(6) 0.219(5) Uani 1 1 d . . . H12 H 0.1730 0.1014 0.4499 0.263 Uiso 1 1 calc R . . H13 H 0.1581 0.0721 0.5234 0.263 Uiso 1 1 calc R . . C13 C 0.1727(2) -0.0008(3) 0.4532(4) 0.137(3) Uani 1 1 d . . . H14 H 0.1425 0.0023 0.4139 0.164 Uiso 1 1 calc R . . H15 H 0.1524 -0.0313 0.4867 0.164 Uiso 1 1 calc R . . C14 C 0.2434(2) -0.0256(2) 0.4323(3) 0.0983(13) Uani 1 1 d . . . H16 H 0.2495 -0.0735 0.4437 0.118 Uiso 1 1 calc R . . H17 H 0.2505 -0.0196 0.3835 0.118 Uiso 1 1 calc R . . Li1 Li 0.3923(2) 0.0094(2) 0.4818(3) 0.0579(12) Uani 1 1 d . . . H1 H 0.3559(14) -0.0431(15) 0.6314(14) 0.051(7) Uiso 1 1 d . . . H2 H 0.2391(19) 0.0850(18) 0.751(2) 0.082(11) Uiso 1 1 d . . . H3 H 0.2904(19) 0.178(2) 0.7006(19) 0.083(11) Uiso 1 1 d . . . H4 H 0.3676(17) 0.1658(19) 0.6118(18) 0.074(10) Uiso 1 1 d . . . H5 H 0.216(3) -0.052(3) 0.723(2) 0.122(18) Uiso 1 1 d . . . H6 H 0.272(2) -0.051(2) 0.788(2) 0.099(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0533(11) 0.0536(11) 0.0542(11) 0.0070(8) 0.0112(8) -0.0008(8) O2 0.0619(14) 0.0778(16) 0.116(2) -0.0166(15) 0.0026(13) 0.0014(11) C1 0.0501(15) 0.0540(15) 0.0530(15) 0.0032(12) 0.0034(12) 0.0029(12) C2 0.0566(16) 0.0490(15) 0.0621(17) 0.0021(12) 0.0135(13) 0.0037(12) C3 0.0564(16) 0.0644(18) 0.0608(17) 0.0005(14) 0.0150(13) 0.0028(13) C4 0.0665(19) 0.074(2) 0.071(2) -0.0057(16) 0.0214(16) 0.0118(16) C5 0.082(2) 0.0616(19) 0.085(2) -0.0042(17) 0.0139(19) 0.0197(17) C6 0.075(2) 0.0511(17) 0.076(2) 0.0069(15) 0.0114(17) 0.0070(15) C7 0.0607(18) 0.0623(18) 0.0619(18) 0.0080(14) 0.0220(14) -0.0076(14) C8 0.0512(16) 0.0698(19) 0.0685(19) 0.0155(15) 0.0120(14) -0.0099(14) C9 0.081(3) 0.072(2) 0.085(3) 0.0023(18) 0.040(2) -0.0001(18) C10 0.066(2) 0.112(3) 0.110(3) 0.014(3) -0.005(2) 0.003(2) C11 0.085(3) 0.120(4) 0.203(6) -0.073(4) -0.029(4) 0.037(3) C12 0.110(5) 0.210(9) 0.338(14) -0.119(10) -0.044(7) 0.053(6) C13 0.076(3) 0.116(4) 0.218(7) 0.053(4) -0.060(3) -0.020(3) C14 0.107(3) 0.077(2) 0.111(3) -0.013(2) -0.018(3) 0.019(2) Li1 0.056(3) 0.056(3) 0.062(3) 0.002(2) 0.009(2) -0.008(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 O1 C1 1.335(3) . ? O1 Li1 1.953(5) . ? O1 Li1 1.970(5) 21_566 ? O1 Li1 1.985(5) 7_556 ? O2 C11 1.399(5) . ? O2 C14 1.412(5) . ? O2 Li1 2.041(6) . ? C1 C6 1.393(4) . ? C1 C2 1.403(4) . ? C1 Li1 2.776(5) 7_556 ? C2 C3 1.389(4) . ? C2 H1 0.98(3) . ? C3 C4 1.396(5) . ? C3 C9 1.520(5) . ? C4 C5 1.368(5) . ? C4 H2 0.97(4) . ? C5 C6 1.391(5) . ? C5 H3 0.98(4) . ? C6 H4 0.99(4) . ? C7 C8 1.394(4) . ? C7 C8 1.395(5) 7_556 ? C7 C9 1.511(5) . ? C8 C7 1.395(5) 9_645 ? C8 C10 1.515(5) . ? C9 H5 0.94(5) . ? C9 H6 1.10(4) . ? C10 H7 0.9600 . ? C10 H8 0.9600 . ? C10 H9 0.9600 . ? C11 C12 1.319(8) . ? C11 H10 0.9700 . ? C11 H11 0.9700 . ? C12 C13 1.447(9) . ? C12 H12 0.9700 . ? C12 H13 0.9700 . ? C13 C14 1.521(7) . ? C13 H14 0.9700 . ? C13 H15 0.9700 . ? C14 H16 0.9700 . ? C14 H17 0.9700 . ? Li1 O1 1.969(5) 19_655 ? Li1 O1 1.985(5) 9_645 ? Li1 Li1 2.653(7) 19_655 ? Li1 Li1 2.653(7) 21_566 ? Li1 C1 2.776(5) 9_645 ? Li1 Li1 3.364(9) 9_645 ? Li1 Li1 3.364(9) 7_556 ? 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 C1 O1 Li1 116.1(2) . . ? C1 O1 Li1 138.6(2) . 21_566 ? Li1 O1 Li1 85.1(2) . 21_566 ? C1 O1 Li1 112.0(2) . 7_556 ? Li1 O1 Li1 117.4(3) . 7_556 ? Li1 O1 Li1 84.3(2) 21_566 7_556 ? C11 O2 C14 107.7(3) . . ? C11 O2 Li1 121.9(3) . . ? C14 O2 Li1 130.2(3) . . ? O1 C1 C6 122.3(3) . . ? O1 C1 C2 120.3(2) . . ? C6 C1 C2 117.4(3) . . ? O1 C1 Li1 41.53(15) . 7_556 ? C6 C1 Li1 125.6(2) . 7_556 ? C2 C1 Li1 100.8(2) . 7_556 ? C3 C2 C1 122.5(3) . . ? C3 C2 H1 118.2(17) . . ? C1 C2 H1 119.1(17) . . ? C2 C3 C4 118.3(3) . . ? C2 C3 C9 121.8(3) . . ? C4 C3 C9 120.0(3) . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H2 115(2) . . ? C3 C4 H2 125(2) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H3 122(2) . . ? C6 C5 H3 117(2) . . ? C5 C6 C1 120.4(3) . . ? C5 C6 H4 119(2) . . ? C1 C6 H4 121(2) . . ? C8 C7 C8 119.8(3) . 7_556 ? C8 C7 C9 119.6(3) . . ? C8 C7 C9 120.1(3) 7_556 . ? C7 C8 C7 120.2(3) . 9_645 ? C7 C8 C10 119.7(3) . . ? C7 C8 C10 120.0(3) 9_645 . ? C7 C9 C3 114.3(3) . . ? C7 C9 H5 108(3) . . ? C3 C9 H5 106(3) . . ? C7 C9 H6 107(2) . . ? C3 C9 H6 110(2) . . ? H5 C9 H6 111(4) . . ? C8 C10 H7 109.5 . . ? C8 C10 H8 109.5 . . ? H7 C10 H8 109.5 . . ? C8 C10 H9 109.5 . . ? H7 C10 H9 109.5 . . ? H8 C10 H9 109.5 . . ? C12 C11 O2 112.4(5) . . ? C12 C11 H10 109.1 . . ? O2 C11 H10 109.1 . . ? C12 C11 H11 109.1 . . ? O2 C11 H11 109.1 . . ? H10 C11 H11 107.9 . . ? C11 C12 C13 108.2(6) . . ? C11 C12 H12 110.1 . . ? C13 C12 H12 110.1 . . ? C11 C12 H13 110.1 . . ? C13 C12 H13 110.1 . . ? H12 C12 H13 108.4 . . ? C12 C13 C14 103.7(4) . . ? C12 C13 H14 111.0 . . ? C14 C13 H14 111.0 . . ? C12 C13 H15 111.0 . . ? C14 C13 H15 111.0 . . ? H14 C13 H15 109.0 . . ? O2 C14 C13 104.3(4) . . ? O2 C14 H16 110.9 . . ? C13 C14 H16 110.9 . . ? O2 C14 H17 110.9 . . ? C13 C14 H17 110.9 . . ? H16 C14 H17 108.9 . . ? O1 Li1 O1 95.8(2) . 19_655 ? O1 Li1 O1 121.3(3) . 9_645 ? O1 Li1 O1 94.8(2) 19_655 9_645 ? O1 Li1 O2 111.4(3) . . ? O1 Li1 O2 117.1(3) 19_655 . ? O1 Li1 O2 114.2(2) 9_645 . ? O1 Li1 Li1 115.80(17) . 19_655 ? O1 Li1 Li1 47.2(2) 19_655 19_655 ? O1 Li1 Li1 47.62(10) 9_645 19_655 ? O2 Li1 Li1 131.1(2) . 19_655 ? O1 Li1 Li1 47.71(10) . 21_566 ? O1 Li1 Li1 48.1(2) 19_655 21_566 ? O1 Li1 Li1 115.35(17) 9_645 21_566 ? O2 Li1 Li1 129.1(2) . 21_566 ? Li1 Li1 Li1 78.7(3) 19_655 21_566 ? O1 Li1 C1 131.7(2) . 9_645 ? O1 Li1 C1 114.1(2) 19_655 9_645 ? O1 Li1 C1 26.49(10) 9_645 9_645 ? O2 Li1 C1 88.60(19) . 9_645 ? Li1 Li1 C1 69.58(15) 19_655 9_645 ? Li1 Li1 C1 141.75(17) 21_566 9_645 ? O1 Li1 Li1 91.27(16) . 9_645 ? O1 Li1 Li1 90.72(16) 19_655 9_645 ? O1 Li1 Li1 31.03(16) 9_645 9_645 ? O2 Li1 Li1 140.7(2) . 9_645 ? Li1 Li1 Li1 50.66(13) 19_655 9_645 ? Li1 Li1 Li1 90.0 21_566 9_645 ? C1 Li1 Li1 53.40(17) 9_645 9_645 ? O1 Li1 Li1 31.60(16) . 7_556 ? O1 Li1 Li1 91.26(16) 19_655 7_556 ? O1 Li1 Li1 90.71(16) 9_645 7_556 ? O2 Li1 Li1 138.8(2) . 7_556 ? Li1 Li1 Li1 90.0 19_655 7_556 ? Li1 Li1 Li1 50.66(13) 21_566 7_556 ? C1 Li1 Li1 107.35(16) 9_645 7_556 ? Li1 Li1 Li1 59.998(1) 9_645 7_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.639 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.060 data_(1cLi3)2(THF)6 _database_code_depnum_ccdc_archive 'CCDC 861323' #TrackingRef '- all-CIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C93 H117 Li6 O12 ' _chemical_formula_moiety 'C93 H117 Li6 O12 ' _chemical_formula_weight 1468.59 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' 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 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 12.3152(5) _cell_length_b 15.6985(7) _cell_length_c 22.3318(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.3100(10) _cell_angle_gamma 90.00 _cell_volume 4305.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 24128 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1578 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9582 _exptl_absorpt_correction_T_max 0.9650 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 14822 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7426 _reflns_number_gt 5356 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX 1.39 0.02 C46 C49 C49 C47 C47 C46_$1 DANG 2.42 0.04 C46 C47 C49 C46_$1 C49 C47_$1 ; _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^)+(0.1429P)^2^+1.1361P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7426 _refine_ls_number_parameters 515 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 O1 O 0.83733(12) 0.06350(10) 0.50003(7) 0.0415(4) Uani 1 1 d . . . O2 O 1.10226(13) 0.11650(10) 0.51504(7) 0.0462(4) Uani 1 1 d . . . O3 O 1.01454(13) -0.05245(10) 0.59536(7) 0.0450(4) Uani 1 1 d . . . O4 O 0.75267(14) -0.06635(13) 0.60228(9) 0.0612(5) Uani 1 1 d . . . O5 O 0.92718(18) 0.25336(12) 0.44328(11) 0.0728(6) Uani 1 1 d . . . O6 O 1.26583(17) 0.03603(15) 0.62317(9) 0.0700(6) Uani 1 1 d . . . C1 C 0.7660(2) -0.1288(2) 0.64853(16) 0.0740(9) Uani 1 1 d . . . H1 H 0.8009 -0.1041 0.6849 0.089 Uiso 1 1 calc R . . H2 H 0.8104 -0.1757 0.6360 0.089 Uiso 1 1 calc R . . C2 C 1.1479(3) 0.2527(3) 0.81772(19) 0.0946(12) Uani 1 1 d . . . H3 H 1.1787 0.3070 0.8090 0.114 Uiso 1 1 calc R . . H4 H 1.1987 0.2211 0.8438 0.114 Uiso 1 1 calc R . . H5 H 1.0817 0.2610 0.8370 0.114 Uiso 1 1 calc R . . C3 C 0.8511(4) 0.3065(2) 0.4654(2) 0.1089(16) Uani 1 1 d . . . H6 H 0.8545 0.3028 0.5088 0.131 Uiso 1 1 calc R . . H7 H 0.7785 0.2900 0.4497 0.131 Uiso 1 1 calc R . . C4 C 0.8748(7) 0.3947(3) 0.4467(4) 0.174(3) Uani 1 1 d . . . H8 H 0.8159 0.4165 0.4197 0.208 Uiso 1 1 calc R . . H9 H 0.8841 0.4319 0.4813 0.208 Uiso 1 1 calc R . . C5 C 0.9691(7) 0.3898(4) 0.4182(5) 0.226(5) Uani 1 1 d . . . H10 H 1.0263 0.4206 0.4413 0.271 Uiso 1 1 calc R . . H11 H 0.9584 0.4163 0.3789 0.271 Uiso 1 1 calc R . . C6 C 1.0005(4) 0.3045(3) 0.4117(3) 0.1243(19) Uani 1 1 d . . . H12 H 1.0748 0.2963 0.4284 0.149 Uiso 1 1 calc R . . H13 H 0.9964 0.2889 0.3695 0.149 Uiso 1 1 calc R . . C7 C 0.68101(18) 0.21360(15) 0.58501(10) 0.0414(5) Uani 1 1 d . . . C8 C 0.79926(19) 0.25075(15) 0.67896(10) 0.0431(5) Uani 1 1 d . . . C9 C 0.9228(2) 0.16787(16) 0.74569(10) 0.0465(6) Uani 1 1 d . . . C10 C 0.75671(17) 0.11535(14) 0.51387(10) 0.0384(5) Uani 1 1 d . . . C11 C 0.76236(18) 0.15857(14) 0.56882(10) 0.0395(5) Uani 1 1 d . . . H14 H 0.8230 0.1502 0.5956 0.047 Uiso 1 1 calc R . . C12 C 0.81884(19) 0.18212(15) 0.71883(10) 0.0430(5) Uani 1 1 d . . . C13 C 0.7245(2) 0.12472(16) 0.73150(11) 0.0506(6) Uani 1 1 d . . . H15 H 0.7523 0.0688 0.7430 0.061 Uiso 1 1 calc R . . H16 H 0.6770 0.1183 0.6951 0.061 Uiso 1 1 calc R . . C14 C 0.9909(2) 0.28841(16) 0.69144(11) 0.0499(6) Uani 1 1 d . . . C15 C 0.9861(2) 0.01407(16) 0.75010(11) 0.0481(6) Uani 1 1 d . . . C16 C 1.01944(18) -0.05510(15) 0.65492(10) 0.0427(5) Uani 1 1 d . . . C17 C 0.8858(2) 0.30387(15) 0.66516(11) 0.0474(6) Uani 1 1 d . . . C18 C 1.0967(2) 0.22507(16) 0.58920(11) 0.0488(6) Uani 1 1 d . . . H17 H 1.0415 0.1958 0.6067 0.059 Uiso 1 1 calc R . . C19 C 1.1395(2) 0.18996(15) 0.53810(11) 0.0471(6) Uani 1 1 d . . . C20 C 0.6408(2) -0.0423(2) 0.59451(14) 0.0622(7) Uani 1 1 d . . . H18 H 0.6086 -0.0618 0.5559 0.075 Uiso 1 1 calc R . . H19 H 0.6334 0.0191 0.5965 0.075 Uiso 1 1 calc R . . C21 C 0.5911(2) 0.22533(19) 0.54547(13) 0.0603(7) Uani 1 1 d . . . H20 H 0.5354 0.2614 0.5555 0.072 Uiso 1 1 calc R . . C22 C 0.9463(2) 0.09029(18) 0.78471(11) 0.0534(6) Uani 1 1 d . . . H21 H 0.8806 0.0743 0.8033 0.064 Uiso 1 1 calc R . . H22 H 1.0011 0.1049 0.8165 0.064 Uiso 1 1 calc R . . C23 C 0.6591(2) 0.15955(19) 0.78109(13) 0.0596(7) Uani 1 1 d . . . H23 H 0.6891 0.1387 0.8192 0.072 Uiso 1 1 calc R . . H24 H 0.5847 0.1413 0.7745 0.072 Uiso 1 1 calc R . . H25 H 0.6620 0.2207 0.7809 0.072 Uiso 1 1 calc R . . C24 C 0.8637(3) 0.37687(18) 0.62224(13) 0.0634(7) Uani 1 1 d . . . H26 H 0.8064 0.3609 0.5921 0.076 Uiso 1 1 calc R . . H27 H 0.9288 0.3890 0.6019 0.076 Uiso 1 1 calc R . . C25 C 1.0862(2) 0.33907(18) 0.67026(14) 0.0611(7) Uani 1 1 d . . . H28 H 1.1434 0.3416 0.7026 0.073 Uiso 1 1 calc R . . H29 H 1.0624 0.3969 0.6614 0.073 Uiso 1 1 calc R . . C26 C 0.98122(19) 0.01354(15) 0.68775(10) 0.0426(5) Uani 1 1 d . . . H30 H 0.9515 0.0604 0.6670 0.051 Uiso 1 1 calc R . . C27 C 1.0296(3) -0.0568(2) 0.78112(12) 0.0678(8) Uani 1 1 d . . . H31 H 1.0327 -0.0584 0.8228 0.081 Uiso 1 1 calc R . . C28 C 1.0679(3) -0.1242(2) 0.74968(14) 0.0794(10) Uani 1 1 d . . . H32 H 1.0972 -0.1711 0.7707 0.095 Uiso 1 1 calc R . . C29 C 1.1331(2) 0.30142(16) 0.61467(13) 0.0539(6) Uani 1 1 d . . . C30 C 0.6894(2) 0.26063(16) 0.64469(11) 0.0482(6) Uani 1 1 d . . . H33 H 0.6755 0.3207 0.6374 0.058 Uiso 1 1 calc R . . H34 H 0.6335 0.2395 0.6692 0.058 Uiso 1 1 calc R . . C31 C 1.0097(2) 0.22074(17) 0.73137(11) 0.0504(6) Uani 1 1 d . . . C32 C 0.6652(2) 0.12979(19) 0.47445(12) 0.0583(7) Uani 1 1 d . . . H35 H 0.6591 0.1031 0.4371 0.070 Uiso 1 1 calc R . . C33 C 0.5835(3) 0.1835(2) 0.49068(15) 0.0729(9) Uani 1 1 d . . . H36 H 0.5223 0.1918 0.4643 0.087 Uiso 1 1 calc R . . C34 C 1.2230(3) 0.23513(19) 0.51358(15) 0.0694(9) Uani 1 1 d . . . H37 H 1.2533 0.2145 0.4795 0.083 Uiso 1 1 calc R . . C35 C 1.1236(2) 0.2034(2) 0.75950(15) 0.0674(8) Uani 1 1 d . . . H38 H 1.1763 0.2190 0.7313 0.081 Uiso 1 1 calc R . . H39 H 1.1314 0.1429 0.7676 0.081 Uiso 1 1 calc R . . C36 C 0.6560(3) -0.1585(3) 0.65889(19) 0.0897(12) Uani 1 1 d . . . H40 H 0.6516 -0.1758 0.7003 0.108 Uiso 1 1 calc R . . H41 H 0.6350 -0.2061 0.6328 0.108 Uiso 1 1 calc R . . C37 C 0.5864(2) -0.0839(2) 0.64457(15) 0.0698(8) Uani 1 1 d . . . H42 H 0.5847 -0.0461 0.6789 0.084 Uiso 1 1 calc R . . H43 H 0.5126 -0.1009 0.6317 0.084 Uiso 1 1 calc R . . C38 C 1.0640(3) -0.12441(18) 0.68758(12) 0.0618(7) Uani 1 1 d . . . H44 H 1.0910 -0.1708 0.6675 0.074 Uiso 1 1 calc R . . C39 C 0.8295(4) 0.4565(2) 0.65479(19) 0.0881(11) Uani 1 1 d . . . H45 H 0.7517 0.4572 0.6558 0.106 Uiso 1 1 calc R . . H46 H 0.8525 0.5061 0.6340 0.106 Uiso 1 1 calc R . . H47 H 0.8627 0.4565 0.6951 0.106 Uiso 1 1 calc R . . C40 C 1.2167(3) 0.3444(2) 0.58875(16) 0.0741(9) Uani 1 1 d . . . H48 H 1.2422 0.3959 0.6049 0.089 Uiso 1 1 calc R . . C41 C 1.2613(3) 0.3110(2) 0.53972(17) 0.0850(11) Uani 1 1 d . . . H49 H 1.3184 0.3395 0.5235 0.102 Uiso 1 1 calc R . . C42 C 1.3598(3) 0.0799(3) 0.60391(18) 0.0857(10) Uani 1 1 d . . . H50 H 1.3404 0.1145 0.5687 0.103 Uiso 1 1 calc R . . H51 H 1.4160 0.0398 0.5946 0.103 Uiso 1 1 calc R . . C43 C 1.2790(3) 0.0246(3) 0.68541(15) 0.0893(11) Uani 1 1 d . . . H52 H 1.2972 -0.0341 0.6950 0.107 Uiso 1 1 calc R . . H53 H 1.2123 0.0391 0.7036 0.107 Uiso 1 1 calc R . . C44 C 1.3705(3) 0.0831(4) 0.7083(2) 0.1076(16) Uani 1 1 d . . . H54 H 1.3473 0.1199 0.7399 0.129 Uiso 1 1 calc R . . H55 H 1.4332 0.0505 0.7240 0.129 Uiso 1 1 calc R . . C45 C 1.3969(4) 0.1338(3) 0.6555(3) 0.1135(15) Uani 1 1 d . . . H56 H 1.3587 0.1878 0.6543 0.136 Uiso 1 1 calc R . . H57 H 1.4746 0.1444 0.6561 0.136 Uiso 1 1 calc R . . C46 C 0.0384(19) -0.0376(15) 0.0522(4) 0.286(16) Uani 0.50 1 d PD . . H46A H 0.0674 -0.0743 0.0820 0.343 Uiso 0.50 1 calc PR . . C47 C 0.0690(15) 0.0439(10) -0.0312(11) 0.175(6) Uani 0.50 1 d PD . . H47A H 0.1206 0.0622 -0.0567 0.210 Uiso 0.50 1 calc PR . . C49 C 0.1013(13) 0.0226(8) 0.0288(12) 0.191(8) Uani 0.50 1 d PD . . H49A H 0.1605 0.0477 0.0504 0.230 Uiso 0.50 1 calc PR . . Li1 Li 1.1359(3) 0.0146(3) 0.56562(18) 0.0483(9) Uani 1 1 d . . . Li51 Li 0.8711(3) -0.0357(2) 0.55131(17) 0.0460(9) Uani 1 1 d . . . Li53 Li 0.9579(3) 0.1299(3) 0.46973(19) 0.0495(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0431(8) 0.0407(9) 0.0421(8) -0.0036(6) 0.0133(6) 0.0024(7) O2 0.0509(9) 0.0378(9) 0.0516(9) -0.0062(7) 0.0160(7) -0.0036(7) O3 0.0494(9) 0.0447(9) 0.0426(8) -0.0020(7) 0.0156(7) 0.0022(7) O4 0.0487(10) 0.0681(12) 0.0698(12) 0.0258(9) 0.0253(8) 0.0062(9) O5 0.0788(14) 0.0444(11) 0.0995(16) 0.0060(10) 0.0353(12) 0.0023(9) O6 0.0600(12) 0.0856(15) 0.0638(12) -0.0087(10) 0.0015(9) -0.0214(11) C1 0.0584(17) 0.082(2) 0.083(2) 0.0401(18) 0.0192(15) 0.0092(15) C2 0.071(2) 0.109(3) 0.100(3) -0.027(2) -0.0181(19) -0.007(2) C3 0.142(4) 0.063(2) 0.132(3) 0.021(2) 0.081(3) 0.023(2) C4 0.243(7) 0.063(3) 0.236(7) 0.039(3) 0.155(6) 0.031(3) C5 0.241(9) 0.078(4) 0.386(13) 0.041(5) 0.200(9) -0.015(4) C6 0.104(3) 0.079(3) 0.199(6) 0.031(3) 0.073(3) -0.005(2) C7 0.0411(12) 0.0380(12) 0.0461(12) 0.0020(9) 0.0101(10) 0.0018(9) C8 0.0468(13) 0.0392(12) 0.0447(12) -0.0120(9) 0.0124(10) 0.0012(10) C9 0.0511(14) 0.0476(13) 0.0420(12) -0.0128(10) 0.0119(10) 0.0026(11) C10 0.0394(11) 0.0351(11) 0.0416(11) 0.0008(9) 0.0090(9) -0.0006(9) C11 0.0390(11) 0.0413(12) 0.0388(11) -0.0010(9) 0.0068(9) 0.0015(9) C12 0.0472(13) 0.0410(12) 0.0423(12) -0.0112(9) 0.0136(10) -0.0001(10) C13 0.0539(14) 0.0436(13) 0.0555(14) -0.0048(11) 0.0122(11) -0.0047(11) C14 0.0510(14) 0.0457(14) 0.0553(14) -0.0200(11) 0.0185(11) -0.0093(11) C15 0.0506(13) 0.0514(14) 0.0431(12) -0.0005(10) 0.0089(10) 0.0029(11) C16 0.0413(12) 0.0436(13) 0.0443(12) 0.0019(9) 0.0109(9) 0.0015(10) C17 0.0588(15) 0.0386(13) 0.0467(12) -0.0136(10) 0.0171(11) -0.0047(11) C18 0.0472(13) 0.0421(13) 0.0596(14) -0.0090(11) 0.0200(11) -0.0090(10) C19 0.0481(13) 0.0395(13) 0.0555(13) -0.0045(10) 0.0151(11) -0.0040(10) C20 0.0485(15) 0.0632(17) 0.0757(18) 0.0205(14) 0.0101(13) -0.0030(13) C21 0.0492(15) 0.0627(17) 0.0686(17) -0.0127(13) 0.0012(13) 0.0180(13) C22 0.0584(15) 0.0609(16) 0.0415(12) -0.0053(11) 0.0080(11) 0.0055(12) C23 0.0583(16) 0.0574(17) 0.0660(16) -0.0013(13) 0.0239(13) -0.0078(13) C24 0.0800(19) 0.0474(15) 0.0648(16) -0.0023(12) 0.0183(14) -0.0089(14) C25 0.0605(16) 0.0514(16) 0.0741(18) -0.0222(13) 0.0226(14) -0.0164(12) C26 0.0442(12) 0.0425(13) 0.0419(12) 0.0023(9) 0.0091(9) 0.0042(10) C27 0.093(2) 0.0683(19) 0.0420(13) 0.0095(12) 0.0076(13) 0.0187(16) C28 0.114(3) 0.0637(19) 0.0607(17) 0.0155(14) 0.0087(17) 0.0319(19) C29 0.0509(14) 0.0449(14) 0.0680(16) -0.0127(12) 0.0185(12) -0.0104(11) C30 0.0483(14) 0.0441(13) 0.0536(13) -0.0063(10) 0.0129(11) 0.0055(10) C31 0.0462(13) 0.0545(15) 0.0517(13) -0.0190(11) 0.0122(11) -0.0018(11) C32 0.0579(16) 0.0644(17) 0.0514(14) -0.0159(12) -0.0037(12) 0.0097(13) C33 0.0573(17) 0.086(2) 0.0724(19) -0.0191(16) -0.0163(14) 0.0223(16) C34 0.0738(19) 0.0576(17) 0.083(2) -0.0134(15) 0.0434(16) -0.0153(14) C35 0.0459(15) 0.073(2) 0.083(2) -0.0152(15) 0.0039(13) 0.0014(13) C36 0.070(2) 0.099(3) 0.103(3) 0.052(2) 0.0243(18) 0.0045(19) C37 0.0518(16) 0.082(2) 0.0786(19) 0.0165(16) 0.0222(14) -0.0016(15) C38 0.0781(19) 0.0495(15) 0.0591(15) 0.0041(12) 0.0139(13) 0.0186(14) C39 0.117(3) 0.0439(17) 0.104(3) -0.0091(16) 0.015(2) 0.0044(18) C40 0.075(2) 0.0527(17) 0.099(2) -0.0215(16) 0.0365(17) -0.0288(15) C41 0.088(2) 0.067(2) 0.108(3) -0.0196(18) 0.056(2) -0.0356(17) C42 0.0577(18) 0.101(3) 0.098(2) 0.014(2) 0.0048(17) -0.0154(18) C43 0.074(2) 0.129(3) 0.0642(19) -0.008(2) -0.0002(16) -0.015(2) C44 0.056(2) 0.168(5) 0.096(3) -0.054(3) -0.0109(19) 0.004(2) C45 0.081(3) 0.108(3) 0.151(4) -0.028(3) 0.003(3) -0.036(2) C46 0.44(4) 0.39(3) 0.033(4) 0.041(9) 0.056(10) 0.24(3) C47 0.144(12) 0.138(12) 0.24(2) 0.027(12) -0.002(11) -0.018(9) C49 0.187(15) 0.080(8) 0.29(2) -0.063(11) -0.063(17) -0.030(9) Li1 0.053(2) 0.047(2) 0.045(2) -0.0037(16) 0.0108(17) -0.0042(18) Li51 0.049(2) 0.045(2) 0.046(2) 0.0010(16) 0.0176(16) 0.0013(17) Li53 0.052(2) 0.039(2) 0.060(2) -0.0033(17) 0.0206(18) -0.0007(17) _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 O1 C10 1.338(3) . ? O1 Li1 1.958(4) 3_756 ? O1 Li51 1.959(4) . ? O1 Li53 1.975(4) . ? O2 C19 1.330(3) . ? O2 Li1 1.984(5) . ? O2 Li53 1.990(5) . ? O2 Li51 1.997(4) 3_756 ? O3 C16 1.327(3) . ? O3 Li53 1.945(4) 3_756 ? O3 Li51 1.974(5) . ? O3 Li1 1.983(4) . ? O4 C1 1.425(3) . ? O4 C20 1.427(3) . ? O4 Li51 1.975(4) . ? O5 C3 1.374(4) . ? O5 C6 1.433(4) . ? O5 Li53 2.052(5) . ? O6 C43 1.399(4) . ? O6 C42 1.440(4) . ? O6 Li1 2.004(5) . ? C1 C36 1.467(5) . ? C1 H1 0.9700 . ? C1 H2 0.9700 . ? C2 C35 1.523(5) . ? C2 H3 0.9600 . ? C2 H4 0.9600 . ? C2 H5 0.9600 . ? C3 C4 1.481(6) . ? C3 H6 0.9700 . ? C3 H7 0.9700 . ? C4 C5 1.367(8) . ? C4 H8 0.9700 . ? C4 H9 0.9700 . ? C5 C6 1.405(8) . ? C5 H10 0.9700 . ? C5 H11 0.9700 . ? C6 H12 0.9700 . ? C6 H13 0.9700 . ? C7 C21 1.376(4) . ? C7 C11 1.391(3) . ? C7 C30 1.520(3) . ? C8 C17 1.406(3) . ? C8 C12 1.407(3) . ? C8 C30 1.512(4) . ? C9 C12 1.391(4) . ? C9 C31 1.410(4) . ? C9 C22 1.513(4) . ? C10 C32 1.396(4) . ? C10 C11 1.399(3) . ? C10 Li53 2.744(4) . ? C11 H14 0.9300 . ? C12 C13 1.513(3) . ? C13 C23 1.520(3) . ? C13 H15 0.9700 . ? C13 H16 0.9700 . ? C14 C31 1.395(4) . ? C14 C17 1.401(4) . ? C14 C25 1.523(3) . ? C15 C26 1.389(3) . ? C15 C27 1.396(4) . ? C15 C22 1.525(4) . ? C16 C38 1.399(4) . ? C16 C26 1.404(3) . ? C16 Li1 2.768(4) . ? C17 C24 1.506(4) . ? C18 C29 1.387(3) . ? C18 C19 1.405(3) . ? C18 H17 0.9300 . ? C19 C34 1.394(4) . ? C19 Li53 2.776(5) . ? C20 C37 1.495(4) . ? C20 H18 0.9700 . ? C20 H19 0.9700 . ? C21 C33 1.385(4) . ? C21 H20 0.9300 . ? C22 H21 0.9700 . ? C22 H22 0.9700 . ? C23 H23 0.9600 . ? C23 H24 0.9600 . ? C23 H25 0.9600 . ? C24 C39 1.522(4) . ? C24 H26 0.9700 . ? C24 H27 0.9700 . ? C25 C29 1.526(4) . ? C25 H28 0.9700 . ? C25 H29 0.9700 . ? C26 H30 0.9300 . ? C27 C28 1.373(4) . ? C27 H31 0.9300 . ? C28 C38 1.384(4) . ? C28 H32 0.9300 . ? C29 C40 1.393(4) . ? C30 H33 0.9700 . ? C30 H34 0.9700 . ? C31 C35 1.518(4) . ? C32 C33 1.382(4) . ? C32 H35 0.9300 . ? C33 H36 0.9300 . ? C34 C41 1.394(4) . ? C34 H37 0.9300 . ? C35 H38 0.9700 . ? C35 H39 0.9700 . ? C36 C37 1.472(5) . ? C36 H40 0.9700 . ? C36 H41 0.9700 . ? C37 H42 0.9700 . ? C37 H43 0.9700 . ? C38 H44 0.9300 . ? C39 H45 0.9600 . ? C39 H46 0.9600 . ? C39 H47 0.9600 . ? C40 C41 1.366(4) . ? C40 H48 0.9300 . ? C41 H49 0.9300 . ? C42 C45 1.474(6) . ? C42 H50 0.9700 . ? C42 H51 0.9700 . ? C43 C44 1.513(6) . ? C43 H52 0.9700 . ? C43 H53 0.9700 . ? C44 C45 1.478(7) . ? C44 H54 0.9700 . ? C44 H55 0.9700 . ? C45 H56 0.9700 . ? C45 H57 0.9700 . ? C46 C49 1.352(15) . ? C46 C47 1.373(15) 3 ? C46 H46A 0.9300 . ? C47 C46 1.373(15) 3 ? C47 C49 1.410(15) . ? C47 H47A 0.9300 . ? C49 H49A 0.9300 . ? Li1 O1 1.958(4) 3_756 ? Li1 Li51 2.627(5) 3_756 ? Li1 Li53 2.640(6) 3_756 ? Li1 Li51 3.347(6) . ? Li1 Li53 3.458(6) . ? Li51 O2 1.997(4) 3_756 ? Li51 Li1 2.627(5) 3_756 ? Li51 Li53 2.645(5) 3_756 ? Li51 Li53 3.394(5) . ? Li53 O3 1.945(4) 3_756 ? Li53 Li1 2.640(6) 3_756 ? Li53 Li51 2.645(5) 3_756 ? 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 C10 O1 Li1 136.36(19) . 3_756 ? C10 O1 Li51 118.49(16) . . ? Li1 O1 Li51 84.24(17) 3_756 . ? C10 O1 Li53 110.36(17) . . ? Li1 O1 Li53 84.31(17) 3_756 . ? Li51 O1 Li53 119.22(19) . . ? C19 O2 Li1 115.30(19) . . ? C19 O2 Li53 111.96(19) . . ? Li1 O2 Li53 121.02(18) . . ? C19 O2 Li51 140.08(18) . 3_756 ? Li1 O2 Li51 82.60(17) . 3_756 ? Li53 O2 Li51 83.14(17) . 3_756 ? C16 O3 Li53 137.0(2) . 3_756 ? C16 O3 Li51 118.36(16) . . ? Li53 O3 Li51 84.89(18) 3_756 . ? C16 O3 Li1 111.94(18) . . ? Li53 O3 Li1 84.47(17) 3_756 . ? Li51 O3 Li1 115.53(18) . . ? C1 O4 C20 109.13(19) . . ? C1 O4 Li51 122.4(2) . . ? C20 O4 Li51 127.84(19) . . ? C3 O5 C6 108.0(3) . . ? C3 O5 Li53 125.9(2) . . ? C6 O5 Li53 124.1(2) . . ? C43 O6 C42 108.8(3) . . ? C43 O6 Li1 130.0(2) . . ? C42 O6 Li1 120.6(2) . . ? O4 C1 C36 106.0(2) . . ? O4 C1 H1 110.5 . . ? C36 C1 H1 110.5 . . ? O4 C1 H2 110.5 . . ? C36 C1 H2 110.5 . . ? H1 C1 H2 108.7 . . ? C35 C2 H3 109.5 . . ? C35 C2 H4 109.5 . . ? H3 C2 H4 109.5 . . ? C35 C2 H5 109.5 . . ? H3 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? O5 C3 C4 108.2(3) . . ? O5 C3 H6 110.1 . . ? C4 C3 H6 110.1 . . ? O5 C3 H7 110.1 . . ? C4 C3 H7 110.1 . . ? H6 C3 H7 108.4 . . ? C5 C4 C3 105.8(4) . . ? C5 C4 H8 110.6 . . ? C3 C4 H8 110.6 . . ? C5 C4 H9 110.6 . . ? C3 C4 H9 110.6 . . ? H8 C4 H9 108.7 . . ? C4 C5 C6 110.6(4) . . ? C4 C5 H10 109.5 . . ? C6 C5 H10 109.5 . . ? C4 C5 H11 109.5 . . ? C6 C5 H11 109.5 . . ? H10 C5 H11 108.1 . . ? C5 C6 O5 107.1(4) . . ? C5 C6 H12 110.3 . . ? O5 C6 H12 110.3 . . ? C5 C6 H13 110.3 . . ? O5 C6 H13 110.3 . . ? H12 C6 H13 108.5 . . ? C21 C7 C11 118.5(2) . . ? C21 C7 C30 119.7(2) . . ? C11 C7 C30 121.8(2) . . ? C17 C8 C12 119.8(2) . . ? C17 C8 C30 119.5(2) . . ? C12 C8 C30 120.2(2) . . ? C12 C9 C31 119.8(2) . . ? C12 C9 C22 120.5(2) . . ? C31 C9 C22 119.3(2) . . ? O1 C10 C32 122.1(2) . . ? O1 C10 C11 120.6(2) . . ? C32 C10 C11 117.3(2) . . ? O1 C10 Li53 42.44(12) . . ? C32 C10 Li53 117.92(19) . . ? C11 C10 Li53 106.73(17) . . ? C7 C11 C10 122.7(2) . . ? C7 C11 H14 118.7 . . ? C10 C11 H14 118.7 . . ? C9 C12 C8 120.3(2) . . ? C9 C12 C13 121.2(2) . . ? C8 C12 C13 118.5(2) . . ? C12 C13 C23 112.2(2) . . ? C12 C13 H15 109.2 . . ? C23 C13 H15 109.2 . . ? C12 C13 H16 109.2 . . ? C23 C13 H16 109.2 . . ? H15 C13 H16 107.9 . . ? C31 C14 C17 120.3(2) . . ? C31 C14 C25 120.1(3) . . ? C17 C14 C25 119.3(3) . . ? C26 C15 C27 118.6(2) . . ? C26 C15 C22 121.4(2) . . ? C27 C15 C22 120.0(2) . . ? O3 C16 C38 122.2(2) . . ? O3 C16 C26 120.5(2) . . ? C38 C16 C26 117.3(2) . . ? O3 C16 Li1 41.65(13) . . ? C38 C16 Li1 118.64(19) . . ? C26 C16 Li1 106.55(17) . . ? C14 C17 C8 119.8(2) . . ? C14 C17 C24 121.0(2) . . ? C8 C17 C24 119.2(2) . . ? C29 C18 C19 122.9(2) . . ? C29 C18 H17 118.6 . . ? C19 C18 H17 118.6 . . ? O2 C19 C34 122.1(2) . . ? O2 C19 C18 121.0(2) . . ? C34 C19 C18 116.9(2) . . ? O2 C19 Li53 41.65(14) . . ? C34 C19 Li53 122.9(2) . . ? C18 C19 Li53 104.10(18) . . ? O4 C20 C37 106.1(2) . . ? O4 C20 H18 110.5 . . ? C37 C20 H18 110.5 . . ? O4 C20 H19 110.5 . . ? C37 C20 H19 110.5 . . ? H18 C20 H19 108.7 . . ? C7 C21 C33 120.1(2) . . ? C7 C21 H20 120.0 . . ? C33 C21 H20 120.0 . . ? C9 C22 C15 113.24(19) . . ? C9 C22 H21 108.9 . . ? C15 C22 H21 108.9 . . ? C9 C22 H22 108.9 . . ? C15 C22 H22 108.9 . . ? H21 C22 H22 107.7 . . ? C13 C23 H23 109.5 . . ? C13 C23 H24 109.5 . . ? H23 C23 H24 109.5 . . ? C13 C23 H25 109.5 . . ? H23 C23 H25 109.5 . . ? H24 C23 H25 109.5 . . ? C17 C24 C39 111.4(2) . . ? C17 C24 H26 109.3 . . ? C39 C24 H26 109.3 . . ? C17 C24 H27 109.3 . . ? C39 C24 H27 109.3 . . ? H26 C24 H27 108.0 . . ? C14 C25 C29 113.4(2) . . ? C14 C25 H28 108.9 . . ? C29 C25 H28 108.9 . . ? C14 C25 H29 108.9 . . ? C29 C25 H29 108.9 . . ? H28 C25 H29 107.7 . . ? C15 C26 C16 122.5(2) . . ? C15 C26 H30 118.8 . . ? C16 C26 H30 118.8 . . ? C28 C27 C15 119.6(2) . . ? C28 C27 H31 120.2 . . ? C15 C27 H31 120.2 . . ? C27 C28 C38 121.8(3) . . ? C27 C28 H32 119.1 . . ? C38 C28 H32 119.1 . . ? C18 C29 C40 118.3(2) . . ? C18 C29 C25 122.6(2) . . ? C40 C29 C25 119.1(2) . . ? C8 C30 C7 113.14(18) . . ? C8 C30 H33 109.0 . . ? C7 C30 H33 109.0 . . ? C8 C30 H34 109.0 . . ? C7 C30 H34 109.0 . . ? H33 C30 H34 107.8 . . ? C14 C31 C9 120.0(2) . . ? C14 C31 C35 120.4(2) . . ? C9 C31 C35 119.6(3) . . ? C33 C32 C10 120.2(2) . . ? C33 C32 H35 119.9 . . ? C10 C32 H35 119.9 . . ? C32 C33 C21 121.3(3) . . ? C32 C33 H36 119.4 . . ? C21 C33 H36 119.4 . . ? C41 C34 C19 120.5(3) . . ? C41 C34 H37 119.8 . . ? C19 C34 H37 119.8 . . ? C31 C35 C2 112.2(3) . . ? C31 C35 H38 109.2 . . ? C2 C35 H38 109.2 . . ? C31 C35 H39 109.2 . . ? C2 C35 H39 109.2 . . ? H38 C35 H39 107.9 . . ? C1 C36 C37 104.0(3) . . ? C1 C36 H40 110.9 . . ? C37 C36 H40 110.9 . . ? C1 C36 H41 110.9 . . ? C37 C36 H41 110.9 . . ? H40 C36 H41 109.0 . . ? C36 C37 C20 102.9(2) . . ? C36 C37 H42 111.2 . . ? C20 C37 H42 111.2 . . ? C36 C37 H43 111.2 . . ? C20 C37 H43 111.2 . . ? H42 C37 H43 109.1 . . ? C28 C38 C16 120.2(3) . . ? C28 C38 H44 119.9 . . ? C16 C38 H44 119.9 . . ? C24 C39 H45 109.5 . . ? C24 C39 H46 109.5 . . ? H45 C39 H46 109.5 . . ? C24 C39 H47 109.5 . . ? H45 C39 H47 109.5 . . ? H46 C39 H47 109.5 . . ? C41 C40 C29 120.1(3) . . ? C41 C40 H48 119.9 . . ? C29 C40 H48 119.9 . . ? C40 C41 C34 121.3(3) . . ? C40 C41 H49 119.3 . . ? C34 C41 H49 119.3 . . ? O6 C42 C45 104.5(3) . . ? O6 C42 H50 110.9 . . ? C45 C42 H50 110.9 . . ? O6 C42 H51 110.9 . . ? C45 C42 H51 110.9 . . ? H50 C42 H51 108.9 . . ? O6 C43 C44 106.6(3) . . ? O6 C43 H52 110.4 . . ? C44 C43 H52 110.4 . . ? O6 C43 H53 110.4 . . ? C44 C43 H53 110.4 . . ? H52 C43 H53 108.6 . . ? C45 C44 C43 105.0(3) . . ? C45 C44 H54 110.7 . . ? C43 C44 H54 110.7 . . ? C45 C44 H55 110.7 . . ? C43 C44 H55 110.7 . . ? H54 C44 H55 108.8 . . ? C42 C45 C44 104.0(4) . . ? C42 C45 H56 111.0 . . ? C44 C45 H56 111.0 . . ? C42 C45 H57 111.0 . . ? C44 C45 H57 111.0 . . ? H56 C45 H57 109.0 . . ? C49 C46 C47 118.9(13) . 3 ? C49 C46 H46A 120.5 . . ? C47 C46 H46A 120.5 3 . ? C46 C47 C49 120.2(14) 3 . ? C46 C47 H47A 119.9 3 . ? C49 C47 H47A 119.9 . . ? C46 C49 C47 113.8(13) . . ? C46 C49 H49A 123.1 . . ? C47 C49 H49A 123.1 . . ? O1 Li1 O3 95.27(18) 3_756 . ? O1 Li1 O2 96.80(18) 3_756 . ? O3 Li1 O2 119.3(2) . . ? O1 Li1 O6 114.4(2) 3_756 . ? O3 Li1 O6 117.4(2) . . ? O2 Li1 O6 110.6(2) . . ? O1 Li1 Li51 47.89(13) 3_756 3_756 ? O3 Li1 Li51 115.5(2) . 3_756 ? O2 Li1 Li51 48.91(13) . 3_756 ? O6 Li1 Li51 125.5(2) . 3_756 ? O1 Li1 Li53 48.12(13) 3_756 3_756 ? O3 Li1 Li53 47.15(13) . 3_756 ? O2 Li1 Li53 117.1(2) . 3_756 ? O6 Li1 Li53 130.3(2) . 3_756 ? Li51 Li1 Li53 80.22(17) 3_756 3_756 ? O1 Li1 C16 114.67(18) 3_756 . ? O3 Li1 C16 26.41(9) . . ? O2 Li1 C16 129.19(19) . . ? O6 Li1 C16 92.07(16) . . ? Li51 Li1 C16 141.81(19) 3_756 . ? Li53 Li1 C16 68.70(14) 3_756 . ? O1 Li1 Li51 89.92(16) 3_756 . ? O3 Li1 Li51 32.16(11) . . ? O2 Li1 Li51 88.61(16) . . ? O6 Li1 Li51 145.69(19) . . ? Li51 Li1 Li51 88.64(15) 3_756 . ? Li53 Li1 Li51 50.77(13) 3_756 . ? C16 Li1 Li51 54.67(11) . . ? O1 Li1 Li53 89.94(16) 3_756 . ? O3 Li1 Li53 91.55(16) . . ? O2 Li1 Li53 29.54(11) . . ? O6 Li1 Li53 138.4(2) . . ? Li51 Li1 Li53 49.23(13) 3_756 . ? Li53 Li1 Li53 91.27(16) 3_756 . ? C16 Li1 Li53 108.34(15) . . ? Li51 Li1 Li53 59.79(12) . . ? O1 Li51 O3 122.7(2) . . ? O1 Li51 O4 113.4(2) . . ? O3 Li51 O4 110.6(2) . . ? O1 Li51 O2 96.36(18) . 3_756 ? O3 Li51 O2 95.39(17) . 3_756 ? O4 Li51 O2 116.3(2) . 3_756 ? O1 Li51 Li1 47.87(13) . 3_756 ? O3 Li51 Li1 118.23(18) . 3_756 ? O4 Li51 Li1 129.3(2) . 3_756 ? O2 Li51 Li1 48.49(13) 3_756 3_756 ? O1 Li51 Li53 118.53(18) . 3_756 ? O3 Li51 Li53 47.08(13) . 3_756 ? O4 Li51 Li53 126.7(2) . 3_756 ? O2 Li51 Li53 48.32(13) 3_756 3_756 ? Li1 Li51 Li53 81.99(16) 3_756 3_756 ? O1 Li51 Li1 91.75(15) . . ? O3 Li51 Li1 32.31(11) . . ? O4 Li51 Li1 139.3(2) . . ? O2 Li51 Li1 90.41(15) 3_756 . ? Li1 Li51 Li1 91.36(15) 3_756 . ? Li53 Li51 Li1 50.64(13) 3_756 . ? O1 Li51 Li53 30.53(11) . . ? O3 Li51 Li53 93.63(16) . . ? O4 Li51 Li53 140.55(19) . . ? O2 Li51 Li53 90.71(14) 3_756 . ? Li1 Li51 Li53 50.06(13) 3_756 . ? Li53 Li51 Li53 92.63(15) 3_756 . ? Li1 Li51 Li53 61.73(12) . . ? O3 Li53 O1 95.95(19) 3_756 . ? O3 Li53 O2 96.57(18) 3_756 . ? O1 Li53 O2 115.8(2) . . ? O3 Li53 O5 114.5(2) 3_756 . ? O1 Li53 O5 118.0(2) . . ? O2 Li53 O5 112.6(2) . . ? O3 Li53 Li1 48.38(13) 3_756 3_756 ? O1 Li53 Li1 47.57(13) . 3_756 ? O2 Li53 Li1 114.5(2) . 3_756 ? O5 Li53 Li1 131.2(2) . 3_756 ? O3 Li53 Li51 48.03(13) 3_756 3_756 ? O1 Li53 Li51 113.24(19) . 3_756 ? O2 Li53 Li51 48.55(13) . 3_756 ? O5 Li53 Li51 127.5(2) . 3_756 ? Li1 Li53 Li51 78.60(17) 3_756 3_756 ? O3 Li53 C10 115.42(19) 3_756 . ? O1 Li53 C10 27.20(8) . . ? O2 Li53 C10 127.2(2) . . ? O5 Li53 C10 91.73(16) . . ? Li1 Li53 C10 69.46(14) 3_756 . ? Li51 Li53 C10 140.32(19) 3_756 . ? O3 Li53 C19 116.41(18) 3_756 . ? O1 Li53 C19 125.9(2) . . ? O2 Li53 C19 26.39(9) . . ? O5 Li53 C19 87.79(16) . . ? Li1 Li53 C19 140.6(2) 3_756 . ? Li51 Li53 C19 70.63(15) 3_756 . ? C10 Li53 C19 122.86(16) . . ? O3 Li53 Li51 90.10(16) 3_756 . ? O1 Li53 Li51 30.25(11) . . ? O2 Li53 Li51 87.21(16) . . ? O5 Li53 Li51 144.98(18) . . ? Li1 Li53 Li51 49.72(13) 3_756 . ? Li51 Li53 Li51 87.37(15) 3_756 . ? C10 Li53 Li51 54.10(11) . . ? C19 Li53 Li51 103.78(16) . . ? O3 Li53 Li1 89.85(16) 3_756 . ? O1 Li53 Li1 88.24(16) . . ? O2 Li53 Li1 29.44(11) . . ? O5 Li53 Li1 140.1(2) . . ? Li1 Li53 Li1 88.73(16) 3_756 . ? Li51 Li53 Li1 48.78(13) 3_756 . ? C10 Li53 Li1 106.33(15) . . ? C19 Li53 Li1 52.43(11) . . ? Li51 Li53 Li1 58.48(12) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.612 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.080 data_(1dLi3)2(THF)6 _database_code_depnum_ccdc_archive 'CCDC 861324' #TrackingRef '- all-CIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C171 H195 F12 Li12 O24 ' _chemical_formula_moiety 'C171 H195 F12 Li12 O24 ' _chemical_formula_weight 2945.68 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c a' _symmetry_space_group_name_Hall '-P 2a 2ac' _symmetry_Int_Tables_number 54 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x, -y, z+1/2' '-x+1/2, -y, z' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x, y, -z-1/2' 'x-1/2, y, -z' _cell_length_a 31.5198(6) _cell_length_b 16.6893(3) _cell_length_c 31.2344(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16430.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 69063 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 30.5 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6228 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9347 _exptl_absorpt_correction_T_max 0.9915 _exptl_absorpt_process_details multi-scan _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 122224 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14454 _reflns_number_gt 10544 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1618P)^2^+9.6298P] 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 14454 _refine_ls_number_parameters 1108 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2628 _refine_ls_wR_factor_gt 0.2378 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.002 _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 F1 F 0.12357(8) 0.49357(16) 0.41812(7) 0.0897(8) Uani 1 1 d . . . F2 F 0.13077(7) 0.51732(13) 0.04905(6) 0.0731(6) Uani 1 1 d . . . F3 F 0.34255(7) 0.12273(12) 0.23967(7) 0.0714(6) Uani 1 1 d . . . F4 F 0.00324(7) 0.37629(12) 0.09502(7) 0.0731(6) Uani 1 1 d . . . F5 F 0.16984(7) -0.00378(15) -0.14164(8) 0.0857(7) Uani 1 1 d . . . F6 F 0.19315(6) 0.01248(15) 0.10617(8) 0.0817(7) Uani 1 1 d . . . O1 O 0.20376(6) 0.48947(11) 0.29007(6) 0.0430(5) Uani 1 1 d . . . O2 O 0.20475(6) 0.49670(11) 0.18072(6) 0.0401(4) Uani 1 1 d . . . O3 O 0.27241(6) 0.37323(11) 0.23726(6) 0.0427(5) Uani 1 1 d . . . O4 O 0.12435(6) 0.57123(15) 0.23612(7) 0.0581(6) Uani 1 1 d . . . O5 O 0.24576(7) 0.65900(13) 0.13373(7) 0.0539(5) Uani 1 1 d . . . O6 O 0.26263(7) 0.34735(14) 0.34102(8) 0.0630(6) Uani 1 1 d . . . O7 O 0.00349(6) 0.12745(11) 0.02265(6) 0.0435(5) Uani 1 1 d . . . O8 O 0.04845(6) 0.00487(11) -0.05287(6) 0.0414(4) Uani 1 1 d . . . O9 O 0.05928(6) -0.00682(11) 0.03841(6) 0.0413(4) Uani 1 1 d . . . O10 O 0.10277(8) 0.15666(14) -0.00579(8) 0.0626(6) Uani 1 1 d . . . O11 O 0.01257(7) 0.07073(14) 0.12609(6) 0.0558(6) Uani 1 1 d . . . O12 O 0.10094(7) -0.15829(14) -0.01998(8) 0.0619(6) Uani 1 1 d . . . C1 C 0.17192(8) 0.46222(17) 0.31425(9) 0.0416(6) Uani 1 1 d . . . C2 C 0.14444(9) 0.40252(18) 0.29873(10) 0.0468(7) Uani 1 1 d . . . C3 C 0.11082(10) 0.3738(2) 0.32292(10) 0.0528(7) Uani 1 1 d . . . C4 C 0.10361(11) 0.4047(2) 0.36354(11) 0.0599(8) Uani 1 1 d . . . C5 C 0.13054(12) 0.4630(2) 0.37823(10) 0.0603(8) Uani 1 1 d . . . C6 C 0.16492(10) 0.4919(2) 0.35554(10) 0.0524(7) Uani 1 1 d . . . C7 C 0.17546(8) 0.47118(16) 0.15309(9) 0.0377(6) Uani 1 1 d . . . C8 C 0.15138(9) 0.40289(17) 0.16252(9) 0.0432(6) Uani 1 1 d . . . C9 C 0.12049(9) 0.37410(18) 0.13446(10) 0.0485(7) Uani 1 1 d . . . C10 C 0.11332(10) 0.4131(2) 0.09610(11) 0.0529(8) Uani 1 1 d . . . C11 C 0.13733(10) 0.4794(2) 0.08721(10) 0.0517(7) Uani 1 1 d . . . C12 C 0.16809(9) 0.51013(19) 0.11425(10) 0.0460(7) Uani 1 1 d . . . C13 C 0.27149(9) 0.29337(16) 0.23834(9) 0.0413(6) Uani 1 1 d . . . C14 C 0.23267(10) 0.25239(18) 0.23845(11) 0.0505(7) Uani 1 1 d . . . C15 C 0.23048(11) 0.16927(19) 0.23811(12) 0.0583(8) Uani 1 1 d . . . C16 C 0.26804(12) 0.1245(2) 0.23873(13) 0.0624(9) Uani 1 1 d . . . C17 C 0.30573(10) 0.16610(19) 0.23916(10) 0.0532(8) Uani 1 1 d . . . C18 C 0.30908(10) 0.24801(18) 0.23883(10) 0.0478(7) Uani 1 1 d . . . C19 C 0.09819(11) 0.2677(2) 0.26609(11) 0.0574(8) Uani 1 1 d . . . C20 C 0.08624(9) 0.29563(19) 0.22576(11) 0.0526(8) Uani 1 1 d . . . C21 C 0.10561(10) 0.26500(18) 0.18909(11) 0.0525(8) Uani 1 1 d . . . C22 C 0.13842(10) 0.20825(19) 0.19264(12) 0.0571(8) Uani 1 1 d . . . C23 C 0.14981(11) 0.17976(19) 0.23313(13) 0.0616(9) Uani 1 1 d . . . C24 C 0.12940(11) 0.2084(2) 0.26966(12) 0.0625(9) Uani 1 1 d . . . C25 C 0.08120(12) 0.3084(2) 0.30593(12) 0.0700(10) Uani 1 1 d . . . H10 H 0.0770 0.2684 0.3281 0.084 Uiso 1 1 calc R . . H11 H 0.0538 0.3320 0.2995 0.084 Uiso 1 1 calc R . . C26 C 0.05477(12) 0.3636(2) 0.22151(15) 0.0752(11) Uani 1 1 d . . . H12 H 0.0342 0.3602 0.2441 0.090 Uiso 1 1 calc R . . H13 H 0.0406 0.3598 0.1944 0.090 Uiso 1 1 calc R . . H14 H 0.0695 0.4138 0.2233 0.090 Uiso 1 1 calc R . . C27 C 0.09494(11) 0.2995(2) 0.14571(11) 0.0628(9) Uani 1 1 d . . . H15 H 0.0650 0.3127 0.1450 0.075 Uiso 1 1 calc R . . H16 H 0.1000 0.2589 0.1241 0.075 Uiso 1 1 calc R . . C28 C 0.16270(13) 0.1830(3) 0.15359(15) 0.0807(12) Uani 1 1 d . . . H17 H 0.1855 0.2200 0.1486 0.097 Uiso 1 1 calc R . . H18 H 0.1441 0.1827 0.1293 0.097 Uiso 1 1 calc R . . H19 H 0.1741 0.1303 0.1579 0.097 Uiso 1 1 calc R . . C29 C 0.18786(12) 0.1245(2) 0.23718(17) 0.0797(13) Uani 1 1 d . . . H20 H 0.1879 0.0875 0.2133 0.096 Uiso 1 1 calc R . . H21 H 0.1851 0.0934 0.2632 0.096 Uiso 1 1 calc R . . C30 C 0.14200(17) 0.1792(3) 0.31375(16) 0.0998(16) Uani 1 1 d . . . H22 H 0.1716 0.1658 0.3139 0.120 Uiso 1 1 calc R . . H23 H 0.1256 0.1327 0.3210 0.120 Uiso 1 1 calc R . . H24 H 0.1368 0.2207 0.3344 0.120 Uiso 1 1 calc R . . C31 C 0.09786(11) 0.5826(3) 0.19926(12) 0.0673(10) Uani 1 1 d . . . H25 H 0.0983 0.5351 0.1813 0.081 Uiso 1 1 calc R . . H26 H 0.1078 0.6278 0.1825 0.081 Uiso 1 1 calc R . . C32 C 0.05362(11) 0.5981(3) 0.21544(13) 0.0736(11) Uani 1 1 d . . . H27 H 0.0390 0.6373 0.1979 0.088 Uiso 1 1 calc R . . H28 H 0.0370 0.5492 0.2164 0.088 Uiso 1 1 calc R . . C33 C 0.06158(15) 0.6284(5) 0.2575(2) 0.147(3) Uani 1 1 d . . . H29 H 0.0390 0.6119 0.2767 0.176 Uiso 1 1 calc R . . H30 H 0.0623 0.6865 0.2569 0.176 Uiso 1 1 calc R . . C34 C 0.10185(11) 0.5979(3) 0.27304(12) 0.0712(10) Uani 1 1 d . . . H31 H 0.1176 0.6398 0.2876 0.085 Uiso 1 1 calc R . . H32 H 0.0974 0.5539 0.2928 0.085 Uiso 1 1 calc R . . C35 C 0.26450(12) 0.6489(2) 0.09205(11) 0.0668(10) Uani 1 1 d . . . H33 H 0.2595 0.5951 0.0814 0.080 Uiso 1 1 calc R . . H34 H 0.2948 0.6583 0.0932 0.080 Uiso 1 1 calc R . . C36 C 0.2434(2) 0.7090(4) 0.06430(16) 0.140(3) Uani 1 1 d . . . H35 H 0.2647 0.7409 0.0497 0.168 Uiso 1 1 calc R . . H36 H 0.2264 0.6820 0.0428 0.168 Uiso 1 1 calc R . . C37 C 0.2193(3) 0.7556(5) 0.08756(17) 0.186(4) Uani 1 1 d . . . H37 H 0.1907 0.7555 0.0761 0.223 Uiso 1 1 calc R . . H38 H 0.2300 0.8101 0.0865 0.223 Uiso 1 1 calc R . . C38 C 0.21857(14) 0.7274(3) 0.13275(13) 0.0806(12) Uani 1 1 d . . . H39 H 0.2290 0.7688 0.1519 0.097 Uiso 1 1 calc R . . H40 H 0.1900 0.7129 0.1413 0.097 Uiso 1 1 calc R . . C39 C 0.30010(12) 0.3016(3) 0.34897(14) 0.0754(11) Uani 1 1 d . . . H41 H 0.3163 0.3252 0.3722 0.090 Uiso 1 1 calc R . . H42 H 0.3178 0.2999 0.3236 0.090 Uiso 1 1 calc R . . C40 C 0.28604(17) 0.2213(3) 0.36048(18) 0.0996(15) Uani 1 1 d . . . H43 H 0.3060 0.1961 0.3799 0.120 Uiso 1 1 calc R . . H44 H 0.2829 0.1880 0.3352 0.120 Uiso 1 1 calc R . . C41 C 0.24510(17) 0.2341(3) 0.3813(2) 0.119(2) Uani 1 1 d . . . H45 H 0.2485 0.2385 0.4121 0.143 Uiso 1 1 calc R . . H46 H 0.2258 0.1902 0.3752 0.143 Uiso 1 1 calc R . . C42 C 0.22891(14) 0.3102(3) 0.36308(19) 0.1034(18) Uani 1 1 d . . . H47 H 0.2056 0.2995 0.3436 0.124 Uiso 1 1 calc R . . H48 H 0.2187 0.3449 0.3858 0.124 Uiso 1 1 calc R . . C43 C 0.00296(9) 0.20735(17) 0.02229(9) 0.0442(6) Uani 1 1 d . . . C44 C 0.00027(12) 0.24950(19) -0.01638(11) 0.0551(8) Uani 1 1 d . . . C45 C -0.00124(13) 0.3320(2) -0.01831(11) 0.0644(9) Uani 1 1 d . . . C46 C 0.00002(13) 0.3756(2) 0.01998(13) 0.0664(10) Uani 1 1 d . . . C47 C 0.00259(11) 0.3340(2) 0.05732(11) 0.0566(8) Uani 1 1 d . . . C48 C 0.00454(10) 0.25199(19) 0.06016(10) 0.0489(7) Uani 1 1 d . . . C49 C 0.07089(9) 0.03172(17) -0.08601(8) 0.0410(6) Uani 1 1 d . . . C50 C 0.05579(10) 0.09561(19) -0.11056(10) 0.0483(7) Uani 1 1 d . . . C51 C 0.07805(11) 0.1259(2) -0.14528(10) 0.0565(8) Uani 1 1 d . . . C52 C 0.11692(12) 0.0916(2) -0.15628(11) 0.0623(9) Uani 1 1 d . . . C53 C 0.13138(10) 0.0293(2) -0.13176(11) 0.0586(8) Uani 1 1 d . . . C54 C 0.10982(10) -0.0019(2) -0.09700(10) 0.0515(7) Uani 1 1 d . . . C55 C 0.08760(9) -0.03229(17) 0.06691(8) 0.0396(6) Uani 1 1 d . . . C56 C 0.07894(10) -0.09818(18) 0.09268(9) 0.0452(7) Uani 1 1 d . . . C57 C 0.10719(10) -0.12660(19) 0.12323(10) 0.0533(8) Uani 1 1 d . . . C58 C 0.14611(11) -0.0881(2) 0.12819(11) 0.0585(9) Uani 1 1 d . . . C59 C 0.15449(10) -0.0246(2) 0.10214(11) 0.0558(8) Uani 1 1 d . . . C60 C 0.12711(10) 0.0049(2) 0.07187(11) 0.0503(7) Uani 1 1 d . . . C61 C -0.00929(15) 0.3217(2) -0.09912(12) 0.0710(11) Uani 1 1 d . . . C62 C 0.02680(14) 0.2933(2) -0.12074(12) 0.0697(10) Uani 1 1 d . . . C63 C 0.02225(12) 0.2352(2) -0.15249(11) 0.0635(9) Uani 1 1 d . . . C64 C -0.01793(12) 0.2056(2) -0.16255(10) 0.0599(9) Uani 1 1 d . . . C65 C -0.05402(12) 0.2353(2) -0.14159(11) 0.0607(9) Uani 1 1 d . . . C66 C -0.04961(13) 0.2922(2) -0.10919(11) 0.0664(10) Uani 1 1 d . . . C67 C -0.00414(18) 0.3770(2) -0.06066(13) 0.0866(14) Uani 1 1 d . . . H58 H -0.0281 0.4134 -0.0596 0.104 Uiso 1 1 calc R . . H59 H 0.0213 0.4088 -0.0644 0.104 Uiso 1 1 calc R . . C68 C 0.07045(17) 0.3220(3) -0.10732(18) 0.1092(17) Uani 1 1 d . . . H60 H 0.0702 0.3349 -0.0774 0.131 Uiso 1 1 calc R . . H61 H 0.0779 0.3687 -0.1236 0.131 Uiso 1 1 calc R . . H62 H 0.0909 0.2804 -0.1125 0.131 Uiso 1 1 calc R . . C69 C 0.06098(14) 0.1963(3) -0.17163(13) 0.0789(12) Uani 1 1 d . . . H63 H 0.0831 0.2362 -0.1744 0.095 Uiso 1 1 calc R . . H64 H 0.0541 0.1773 -0.2002 0.095 Uiso 1 1 calc R . . C70 C -0.02278(15) 0.1368(3) -0.19400(12) 0.0798(11) Uani 1 1 d . . . H65 H 0.0018 0.1029 -0.1925 0.096 Uiso 1 1 calc R . . H66 H -0.0256 0.1577 -0.2225 0.096 Uiso 1 1 calc R . . H67 H -0.0476 0.1063 -0.1869 0.096 Uiso 1 1 calc R . . C71 C -0.09698(13) 0.1992(3) -0.15079(14) 0.0696(10) Uani 1 1 d . . . C72 C -0.08777(16) 0.3175(3) -0.08398(15) 0.0979(15) Uani 1 1 d . . . H70 H -0.1124 0.3165 -0.1021 0.118 Uiso 1 1 calc R . . H71 H -0.0836 0.3709 -0.0733 0.118 Uiso 1 1 calc R . . H72 H -0.0918 0.2814 -0.0604 0.118 Uiso 1 1 calc R . . C73 C 0.13649(14) 0.1622(3) -0.03518(14) 0.0890(14) Uani 1 1 d . . . H73 H 0.1257 0.1692 -0.0640 0.107 Uiso 1 1 calc R . . H74 H 0.1537 0.1141 -0.0343 0.107 Uiso 1 1 calc R . . C74 C 0.1622(2) 0.2340(4) -0.0218(2) 0.142(3) Uani 1 1 d . . . H75 H 0.1923 0.2221 -0.0224 0.170 Uiso 1 1 calc R . . H76 H 0.1566 0.2794 -0.0403 0.170 Uiso 1 1 calc R . . C75 C 0.1481(3) 0.2499(6) 0.0213(3) 0.233(6) Uani 1 1 d . . . H77 H 0.1678 0.2267 0.0417 0.279 Uiso 1 1 calc R . . H78 H 0.1468 0.3072 0.0263 0.279 Uiso 1 1 calc R . . C76 C 0.10829(16) 0.2163(3) 0.02648(16) 0.0998(17) Uani 1 1 d . . . H79 H 0.0866 0.2573 0.0237 0.120 Uiso 1 1 calc R . . H80 H 0.1059 0.1923 0.0547 0.120 Uiso 1 1 calc R . . C77 C 0.05037(10) 0.0782(2) 0.15176(10) 0.0561(8) Uani 1 1 d . . . H81 H 0.0682 0.1210 0.1410 0.067 Uiso 1 1 calc R . . H82 H 0.0664 0.0287 0.1514 0.067 Uiso 1 1 calc R . . C78 C 0.03557(11) 0.0969(2) 0.19641(10) 0.0569(8) Uani 1 1 d . . . H83 H 0.0299 0.0484 0.2125 0.068 Uiso 1 1 calc R . . H84 H 0.0561 0.1292 0.2118 0.068 Uiso 1 1 calc R . . C79 C -0.00440(13) 0.1428(3) 0.18757(12) 0.0726(10) Uani 1 1 d . . . H85 H -0.0234 0.1411 0.2120 0.087 Uiso 1 1 calc R . . H86 H 0.0018 0.1982 0.1806 0.087 Uiso 1 1 calc R . . C80 C -0.02295(11) 0.1003(2) 0.15026(11) 0.0632(9) Uani 1 1 d . . . H87 H -0.0408 0.0564 0.1597 0.076 Uiso 1 1 calc R . . H88 H -0.0399 0.1367 0.1331 0.076 Uiso 1 1 calc R . . C81 C 0.14097(13) -0.1546(3) -0.00059(15) 0.0914(15) Uani 1 1 d . . . H89 H 0.1386 -0.1610 0.0302 0.110 Uiso 1 1 calc R . . H90 H 0.1547 -0.1038 -0.0067 0.110 Uiso 1 1 calc R . . C82 C 0.1655(2) -0.2230(5) -0.0200(2) 0.175(4) Uani 1 1 d . . . H91 H 0.1927 -0.2043 -0.0304 0.210 Uiso 1 1 calc R . . H92 H 0.1704 -0.2643 0.0013 0.210 Uiso 1 1 calc R . . C83 C 0.1427(2) -0.2527(6) -0.0524(3) 0.201(5) Uani 1 1 d . . . H93 H 0.1420 -0.3107 -0.0506 0.242 Uiso 1 1 calc R . . H94 H 0.1556 -0.2379 -0.0795 0.242 Uiso 1 1 calc R . . C84 C 0.10073(14) -0.2216(3) -0.05024(19) 0.114(2) Uani 1 1 d . . . H95 H 0.0920 -0.2018 -0.0781 0.137 Uiso 1 1 calc R . . H96 H 0.0811 -0.2632 -0.0414 0.137 Uiso 1 1 calc R . . C85 C 0.2460(5) 0.0418(9) 0.0080(4) 0.067(4) Uani 0.25 1 d P . . H97 H 0.2403 0.0653 0.0344 0.080 Uiso 0.25 1 calc PR . . C86 C 0.2459(5) 0.0883(9) -0.0245(6) 0.075(4) Uani 0.25 1 d P . . H98 H 0.2451 0.1439 -0.0258 0.090 Uiso 0.25 1 calc PR . . C87 C 0.2469(6) 0.0400(9) -0.0528(5) 0.077(5) Uani 0.25 1 d P . . H99 H 0.2427 0.0617 -0.0799 0.093 Uiso 0.25 1 calc PR . . C88 C 0.7470(6) 0.4064(10) 0.0249(5) 0.074(4) Uani 0.25 1 d P . . H100 H 0.7467 0.3507 0.0262 0.089 Uiso 0.25 1 calc PR . . C89 C 0.7803(5) 0.4602(11) 0.0236(5) 0.077(5) Uani 0.25 1 d P . . H101 H 0.8068 0.4360 0.0221 0.093 Uiso 0.25 1 calc PR . . C90 C 0.7818(6) 0.5453(10) 0.0239(5) 0.080(5) Uani 0.25 1 d P . . H102 H 0.8089 0.5673 0.0233 0.096 Uiso 0.25 1 calc PR . . Li1 Li 0.18507(15) 0.5392(3) 0.23546(15) 0.0427(10) Uani 1 1 d . . . Li2 Li 0.24751(14) 0.5803(3) 0.18215(15) 0.0422(10) Uani 1 1 d . . . Li3 Li 0.25508(15) 0.4223(3) 0.29204(16) 0.0454(11) Uani 1 1 d . . . Li4 Li 0.05420(15) 0.0783(3) -0.00362(15) 0.0453(11) Uani 1 1 d . . . Li5 Li 0.00790(15) 0.0400(3) 0.06474(14) 0.0437(10) Uani 1 1 d . . . Li6 Li 0.05306(15) -0.0802(3) -0.01050(15) 0.0450(11) Uani 1 1 d . . . H1 H 0.1501(11) 0.382(2) 0.2677(11) 0.058(9) Uiso 1 1 d . . . H2 H 0.0740(14) 0.392(2) 0.3811(13) 0.090(13) Uiso 1 1 d . . . H3 H 0.1826(11) 0.535(2) 0.3701(11) 0.063(10) Uiso 1 1 d . . . H4 H 0.1589(11) 0.3769(19) 0.1905(11) 0.056(9) Uiso 1 1 d . . . H5 H 0.0949(11) 0.396(2) 0.0772(11) 0.060(10) Uiso 1 1 d . . . H6 H 0.1839(10) 0.558(2) 0.1063(10) 0.053(9) Uiso 1 1 d . . . H7 H 0.2092(13) 0.286(2) 0.2380(11) 0.066(11) Uiso 1 1 d . . . H8 H 0.2685(13) 0.064(3) 0.2380(12) 0.079(12) Uiso 1 1 d . . . H9 H 0.3370(11) 0.276(2) 0.2398(10) 0.054(9) Uiso 1 1 d . . . H49 H -0.0017(11) 0.220(2) -0.0401(13) 0.064(10) Uiso 1 1 d . . . H50 H -0.0021(13) 0.429(3) 0.0191(13) 0.082(13) Uiso 1 1 d . . . H51 H 0.0079(10) 0.226(2) 0.0876(12) 0.057(9) Uiso 1 1 d . . . H52 H 0.0294(11) 0.117(2) -0.1057(11) 0.056(9) Uiso 1 1 d . . . H53 H 0.1309(15) 0.108(3) -0.1844(16) 0.106(15) Uiso 1 1 d . . . H54 H 0.1250(12) -0.040(2) -0.0777(13) 0.075(11) Uiso 1 1 d . . . H55 H 0.0546(11) -0.1248(19) 0.0886(11) 0.054(9) Uiso 1 1 d . . . H56 H 0.1639(13) -0.104(2) 0.1469(13) 0.073(11) Uiso 1 1 d . . . H57 H 0.1340(14) 0.046(3) 0.0570(14) 0.084(14) Uiso 1 1 d . . . H68 H -0.0990(14) 0.179(3) -0.1797(15) 0.087(13) Uiso 1 1 d . . . H69 H -0.1178(16) 0.243(3) -0.1418(15) 0.104(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.1013(18) 0.1151(19) 0.0526(12) -0.0210(12) 0.0260(12) -0.0203(15) F2 0.0885(15) 0.0822(14) 0.0486(11) 0.0115(10) -0.0165(10) 0.0052(11) F3 0.0682(12) 0.0607(12) 0.0852(14) 0.0022(10) -0.0043(10) 0.0268(10) F4 0.0850(14) 0.0622(12) 0.0723(13) -0.0288(10) -0.0062(11) 0.0039(10) F5 0.0605(13) 0.1044(17) 0.0923(17) -0.0106(14) 0.0290(12) 0.0077(12) F6 0.0489(11) 0.0996(17) 0.0965(17) -0.0082(13) -0.0169(11) -0.0083(11) O1 0.0382(10) 0.0450(11) 0.0458(11) 0.0018(8) 0.0034(8) -0.0059(8) O2 0.0348(9) 0.0411(10) 0.0442(10) -0.0025(8) -0.0024(8) -0.0038(8) O3 0.0421(10) 0.0353(10) 0.0505(11) 0.0009(8) -0.0017(8) -0.0029(8) O4 0.0389(11) 0.0757(15) 0.0597(14) 0.0027(11) 0.0036(9) 0.0134(10) O5 0.0549(12) 0.0552(12) 0.0516(12) 0.0137(10) 0.0067(10) 0.0104(10) O6 0.0603(13) 0.0655(14) 0.0633(14) 0.0217(12) 0.0015(11) -0.0012(11) O7 0.0539(11) 0.0349(10) 0.0417(10) 0.0031(8) -0.0022(9) 0.0009(8) O8 0.0475(11) 0.0450(10) 0.0319(9) 0.0041(8) 0.0038(8) 0.0008(8) O9 0.0449(10) 0.0444(10) 0.0346(10) 0.0035(8) -0.0012(8) 0.0041(8) O10 0.0671(14) 0.0644(14) 0.0564(13) -0.0124(11) 0.0096(11) -0.0217(12) O11 0.0533(12) 0.0772(15) 0.0368(11) -0.0132(10) 0.0002(9) 0.0009(11) O12 0.0549(13) 0.0619(14) 0.0690(15) -0.0109(11) -0.0085(11) 0.0200(11) C1 0.0363(14) 0.0436(15) 0.0449(15) 0.0046(12) 0.0026(12) -0.0020(11) C2 0.0433(15) 0.0505(16) 0.0466(17) -0.0004(13) 0.0049(13) -0.0092(13) C3 0.0480(16) 0.0589(18) 0.0516(17) 0.0018(14) 0.0085(14) -0.0108(14) C4 0.0543(18) 0.070(2) 0.0555(19) 0.0036(16) 0.0157(15) -0.0099(16) C5 0.069(2) 0.071(2) 0.0417(17) -0.0059(15) 0.0126(15) -0.0026(18) C6 0.0528(17) 0.0576(19) 0.0468(17) -0.0029(14) 0.0030(14) -0.0050(15) C7 0.0307(12) 0.0415(14) 0.0410(14) -0.0057(11) -0.0011(11) 0.0024(11) C8 0.0399(14) 0.0459(15) 0.0437(16) -0.0039(12) -0.0038(12) -0.0024(12) C9 0.0403(15) 0.0526(17) 0.0526(17) -0.0081(14) -0.0034(13) -0.0058(13) C10 0.0465(16) 0.063(2) 0.0492(18) -0.0095(15) -0.0115(14) -0.0010(15) C11 0.0535(17) 0.0602(19) 0.0415(16) -0.0013(13) -0.0074(14) 0.0125(15) C12 0.0422(15) 0.0481(17) 0.0476(17) 0.0002(13) 0.0016(13) 0.0023(13) C13 0.0461(15) 0.0333(14) 0.0445(15) 0.0010(11) -0.0024(12) 0.0000(11) C14 0.0442(16) 0.0374(16) 0.070(2) 0.0034(14) -0.0040(14) 0.0017(13) C15 0.0573(19) 0.0369(16) 0.080(2) 0.0044(15) -0.0054(16) -0.0040(14) C16 0.071(2) 0.0367(17) 0.080(2) 0.0031(16) -0.0064(18) 0.0059(15) C17 0.0539(18) 0.0489(17) 0.0567(19) 0.0019(14) -0.0041(14) 0.0151(14) C18 0.0457(16) 0.0473(17) 0.0504(17) 0.0020(13) -0.0034(13) 0.0042(13) C19 0.0521(18) 0.0566(19) 0.063(2) 0.0015(16) 0.0059(15) -0.0249(15) C20 0.0406(15) 0.0482(17) 0.069(2) -0.0012(15) 0.0008(14) -0.0156(13) C21 0.0463(16) 0.0472(16) 0.0638(19) -0.0042(15) -0.0038(14) -0.0179(13) C22 0.0497(17) 0.0445(17) 0.077(2) -0.0125(16) -0.0006(16) -0.0152(14) C23 0.0530(18) 0.0397(16) 0.092(3) 0.0050(17) -0.0039(18) -0.0140(14) C24 0.061(2) 0.0513(19) 0.075(2) 0.0162(17) -0.0059(17) -0.0226(16) C25 0.059(2) 0.082(2) 0.069(2) -0.0057(19) 0.0154(17) -0.0322(19) C26 0.053(2) 0.073(2) 0.100(3) 0.000(2) 0.010(2) 0.0000(18) C27 0.0582(19) 0.067(2) 0.063(2) -0.0033(17) -0.0121(16) -0.0231(17) C28 0.070(2) 0.076(3) 0.096(3) -0.035(2) 0.007(2) -0.008(2) C29 0.063(2) 0.0408(18) 0.135(4) 0.009(2) -0.012(2) -0.0101(16) C30 0.108(4) 0.098(3) 0.094(3) 0.040(3) -0.018(3) -0.021(3) C31 0.0533(19) 0.083(2) 0.065(2) 0.0155(19) 0.0072(17) 0.0182(18) C32 0.0515(19) 0.087(3) 0.083(3) 0.011(2) 0.0011(18) 0.0198(18) C33 0.056(3) 0.249(8) 0.135(5) -0.111(5) -0.014(3) 0.047(4) C34 0.0517(19) 0.098(3) 0.064(2) -0.011(2) 0.0060(16) 0.0177(19) C35 0.066(2) 0.082(2) 0.0524(19) 0.0119(18) 0.0078(16) 0.0225(19) C36 0.156(5) 0.194(6) 0.069(3) 0.061(4) 0.033(3) 0.113(5) C37 0.294(10) 0.198(7) 0.066(3) 0.048(4) 0.033(4) 0.187(8) C38 0.087(3) 0.093(3) 0.061(2) 0.015(2) 0.009(2) 0.045(2) C39 0.065(2) 0.087(3) 0.075(3) 0.018(2) -0.0002(19) 0.010(2) C40 0.099(3) 0.089(3) 0.111(4) 0.029(3) 0.008(3) 0.017(3) C41 0.091(3) 0.120(4) 0.145(5) 0.080(4) 0.016(3) 0.008(3) C42 0.071(3) 0.108(4) 0.131(4) 0.067(3) 0.023(3) 0.010(2) C43 0.0507(16) 0.0357(14) 0.0462(16) -0.0002(12) -0.0046(13) 0.0004(12) C44 0.081(2) 0.0388(17) 0.0458(18) -0.0025(14) -0.0068(16) -0.0030(15) C45 0.091(3) 0.0400(17) 0.062(2) 0.0049(15) -0.0106(19) 0.0008(16) C46 0.089(3) 0.0362(18) 0.073(2) -0.0063(16) -0.013(2) -0.0014(16) C47 0.0606(19) 0.0493(18) 0.060(2) -0.0158(15) -0.0080(16) 0.0004(14) C48 0.0497(17) 0.0492(18) 0.0479(17) -0.0037(14) -0.0053(13) 0.0004(13) C49 0.0454(15) 0.0452(15) 0.0325(13) -0.0009(11) 0.0002(11) -0.0051(12) C50 0.0480(17) 0.0546(18) 0.0423(16) 0.0083(13) 0.0056(13) -0.0028(14) C51 0.0612(19) 0.066(2) 0.0424(16) 0.0103(15) 0.0080(14) -0.0086(16) C52 0.064(2) 0.073(2) 0.0491(19) 0.0035(17) 0.0146(16) -0.0151(18) C53 0.0483(17) 0.068(2) 0.060(2) -0.0142(17) 0.0156(15) -0.0057(15) C54 0.0505(17) 0.0549(18) 0.0490(17) -0.0051(15) 0.0028(14) -0.0012(14) C55 0.0419(14) 0.0451(15) 0.0319(13) -0.0031(11) 0.0005(11) 0.0077(12) C56 0.0465(16) 0.0489(16) 0.0404(15) 0.0024(13) -0.0041(12) 0.0053(14) C57 0.0591(18) 0.0543(18) 0.0465(17) 0.0040(14) -0.0073(14) 0.0146(15) C58 0.0518(18) 0.070(2) 0.0537(19) -0.0046(17) -0.0164(15) 0.0155(16) C59 0.0438(16) 0.065(2) 0.0586(19) -0.0093(16) -0.0078(14) 0.0023(14) C60 0.0482(17) 0.0527(18) 0.0499(18) -0.0016(15) 0.0014(14) 0.0017(14) C61 0.116(3) 0.0386(17) 0.059(2) 0.0158(15) -0.012(2) 0.0006(19) C62 0.093(3) 0.055(2) 0.061(2) 0.0248(17) -0.007(2) -0.0177(19) C63 0.081(2) 0.059(2) 0.0505(19) 0.0265(16) 0.0051(17) -0.0043(18) C64 0.084(2) 0.0533(18) 0.0420(17) 0.0176(14) -0.0040(16) 0.0015(17) C65 0.081(2) 0.0528(18) 0.0483(18) 0.0199(15) -0.0086(16) 0.0065(17) C66 0.097(3) 0.0462(18) 0.056(2) 0.0160(15) -0.0060(19) 0.0190(18) C67 0.149(4) 0.0416(19) 0.069(2) 0.0104(17) -0.015(3) -0.003(2) C68 0.113(4) 0.104(4) 0.111(4) 0.021(3) -0.006(3) -0.043(3) C69 0.087(3) 0.085(3) 0.065(2) 0.034(2) 0.014(2) -0.004(2) C70 0.106(3) 0.081(3) 0.053(2) -0.0014(19) 0.005(2) -0.003(2) C71 0.072(2) 0.075(3) 0.062(2) 0.022(2) -0.0156(19) 0.011(2) C72 0.122(4) 0.088(3) 0.084(3) 0.004(2) 0.000(3) 0.050(3) C73 0.074(2) 0.114(4) 0.079(3) -0.036(3) 0.023(2) -0.037(2) C74 0.119(4) 0.175(6) 0.131(5) -0.076(4) 0.051(4) -0.095(4) C75 0.158(6) 0.294(11) 0.247(10) -0.210(9) 0.107(6) -0.150(7) C76 0.092(3) 0.121(4) 0.086(3) -0.055(3) 0.019(2) -0.034(3) C77 0.0521(17) 0.068(2) 0.0482(17) -0.0114(15) -0.0021(14) -0.0053(15) C78 0.0637(19) 0.064(2) 0.0433(17) -0.0089(15) -0.0050(14) -0.0036(16) C79 0.077(2) 0.083(3) 0.057(2) -0.0187(19) 0.0050(18) 0.011(2) C80 0.0526(18) 0.087(2) 0.0500(18) -0.0130(17) 0.0012(15) 0.0050(17) C81 0.064(2) 0.133(4) 0.077(3) -0.038(3) -0.014(2) 0.030(3) C82 0.115(4) 0.275(9) 0.134(5) -0.119(6) -0.053(4) 0.124(6) C83 0.100(4) 0.244(9) 0.260(10) -0.179(9) -0.041(5) 0.073(5) C84 0.067(3) 0.130(4) 0.144(5) -0.083(4) -0.027(3) 0.030(3) C85 0.093(11) 0.066(8) 0.040(7) -0.006(6) 0.036(7) -0.013(8) C86 0.066(9) 0.047(8) 0.111(13) 0.003(9) 0.002(9) 0.016(7) C87 0.125(14) 0.052(8) 0.055(9) 0.029(7) 0.007(9) 0.014(9) C88 0.110(13) 0.055(8) 0.058(8) -0.008(7) 0.000(8) 0.004(9) C89 0.052(8) 0.103(13) 0.077(10) -0.031(9) -0.012(7) 0.007(8) C90 0.090(11) 0.076(11) 0.074(10) 0.015(8) -0.046(9) 0.010(9) Li1 0.041(2) 0.042(2) 0.046(3) 0.000(2) 0.0009(19) -0.0019(19) Li2 0.038(2) 0.041(2) 0.048(3) 0.003(2) 0.0011(19) -0.0014(19) Li3 0.044(2) 0.044(3) 0.048(3) 0.004(2) 0.001(2) -0.002(2) Li4 0.049(3) 0.044(3) 0.043(2) 0.003(2) 0.002(2) -0.005(2) Li5 0.047(3) 0.048(3) 0.036(2) 0.002(2) 0.0013(19) 0.002(2) Li6 0.049(3) 0.044(3) 0.041(2) -0.0003(19) -0.005(2) 0.008(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 F1 C5 1.364(4) . ? F2 C11 1.366(4) . ? F3 C17 1.368(4) . ? F4 C47 1.373(4) . ? F5 C53 1.367(4) . ? F6 C59 1.373(4) . ? O1 C1 1.336(3) . ? O1 Li3 1.963(5) 4_565 ? O1 Li3 1.969(5) . ? O1 Li1 1.986(5) . ? O2 C7 1.334(3) . ? O2 Li2 1.940(5) . ? O2 Li1 1.952(5) . ? O2 Li2 1.979(5) 4_565 ? O3 C13 1.333(3) . ? O3 Li3 1.974(5) . ? O3 Li1 1.984(5) 4_565 ? O3 Li2 1.990(5) 4_565 ? O4 C34 1.425(4) . ? O4 C31 1.435(4) . ? O4 Li1 1.987(5) . ? O5 C38 1.427(4) . ? O5 C35 1.439(4) . ? O5 Li2 2.004(5) . ? O6 C42 1.410(5) . ? O6 C39 1.428(4) . ? O6 Li3 1.991(5) . ? O7 C43 1.334(3) . ? O7 Li5 1.969(5) . ? O7 Li4 1.975(5) . ? O7 Li6 1.986(5) 5 ? O8 C49 1.331(3) . ? O8 Li6 1.946(5) . ? O8 Li5 1.963(5) 5 ? O8 Li4 1.975(5) . ? O9 C55 1.330(3) . ? O9 Li4 1.941(5) . ? O9 Li6 1.967(5) . ? O9 Li5 1.977(5) . ? O10 C73 1.407(4) . ? O10 C76 1.428(4) . ? O10 Li4 2.014(5) . ? O11 C80 1.438(4) . ? O11 C77 1.441(4) . ? O11 Li5 1.989(5) . ? O12 C81 1.401(4) . ? O12 C84 1.418(5) . ? O12 Li6 2.016(5) . ? C1 C6 1.399(4) . ? C1 C2 1.406(4) . ? C2 C3 1.387(4) . ? C2 H1 1.04(3) . ? C3 C4 1.388(5) . ? C3 C25 1.531(5) . ? C4 C5 1.370(5) . ? C4 H2 1.10(4) . ? C5 C6 1.381(5) . ? C6 H3 1.02(4) . ? C7 C12 1.396(4) . ? C7 C8 1.401(4) . ? C7 Li2 2.731(5) 4_565 ? C8 C9 1.395(4) . ? C8 H4 1.00(3) . ? C9 C10 1.382(5) . ? C9 C27 1.525(4) . ? C10 C11 1.369(5) . ? C10 H5 0.88(4) . ? C11 C12 1.384(4) . ? C12 H6 0.97(3) . ? C13 C14 1.402(4) . ? C13 C18 1.406(4) . ? C13 Li3 2.777(6) . ? C14 C15 1.389(4) . ? C14 H7 0.93(4) . ? C15 C16 1.400(5) . ? C15 C29 1.537(5) . ? C16 C17 1.376(5) . ? C16 H8 1.00(4) . ? C17 C18 1.371(4) . ? C18 H9 1.00(4) . ? C19 C20 1.395(5) . ? C19 C24 1.401(5) . ? C19 C25 1.515(5) . ? C20 C21 1.395(5) . ? C20 C26 1.512(5) . ? C21 C22 1.407(5) . ? C21 C27 1.510(5) . ? C22 C23 1.398(5) . ? C22 C28 1.500(5) . ? C23 C24 1.394(5) . ? C23 C29 1.518(5) . ? C24 C30 1.514(6) . ? C25 H10 0.9700 . ? C25 H11 0.9700 . ? C26 H12 0.9600 . ? C26 H13 0.9600 . ? C26 H14 0.9600 . ? C27 H15 0.9700 . ? C27 H16 0.9700 . ? C28 H17 0.9600 . ? C28 H18 0.9600 . ? C28 H19 0.9600 . ? C29 H20 0.9700 . ? C29 H21 0.9700 . ? C30 H22 0.9600 . ? C30 H23 0.9600 . ? C30 H24 0.9600 . ? C31 C32 1.506(5) . ? C31 H25 0.9700 . ? C31 H26 0.9700 . ? C32 C33 1.430(6) . ? C32 H27 0.9700 . ? C32 H28 0.9700 . ? C33 C34 1.451(6) . ? C33 H29 0.9700 . ? C33 H30 0.9700 . ? C34 H31 0.9700 . ? C34 H32 0.9700 . ? C35 C36 1.483(5) . ? C35 H33 0.9700 . ? C35 H34 0.9700 . ? C36 C37 1.308(7) . ? C36 H35 0.9700 . ? C36 H36 0.9700 . ? C37 C38 1.488(6) . ? C37 H37 0.9700 . ? C37 H38 0.9700 . ? C38 H39 0.9700 . ? C38 H40 0.9700 . ? C39 C40 1.456(6) . ? C39 H41 0.9700 . ? C39 H42 0.9700 . ? C40 C41 1.461(7) . ? C40 H43 0.9700 . ? C40 H44 0.9700 . ? C41 C42 1.484(6) . ? C41 H45 0.9700 . ? C41 H46 0.9700 . ? C42 H47 0.9700 . ? C42 H48 0.9700 . ? C43 C48 1.399(4) . ? C43 C44 1.400(4) . ? C43 Li6 2.785(6) 5 ? C44 C45 1.379(4) . ? C44 H49 0.89(4) . ? C45 C46 1.401(5) . ? C45 C67 1.524(5) . ? C46 C47 1.359(5) . ? C46 H50 0.90(4) . ? C47 C48 1.373(5) . ? C48 H51 0.96(4) . ? C49 C54 1.392(4) . ? C49 C50 1.397(4) . ? C49 Li4 2.739(6) . ? C50 C51 1.387(4) . ? C50 H52 0.92(3) . ? C51 C52 1.395(5) . ? C51 C69 1.532(5) . ? C52 C53 1.370(5) . ? C52 H53 1.02(5) . ? C53 C54 1.382(5) . ? C54 H54 1.00(4) . ? C55 C56 1.390(4) . ? C55 C60 1.400(4) . ? C55 Li6 2.769(5) . ? C55 Li5 2.788(5) . ? C56 C57 1.388(4) . ? C56 H55 0.90(3) . ? C57 C58 1.394(5) . ? C57 C71 1.521(5) 5 ? C58 C59 1.361(5) . ? C58 H56 0.85(4) . ? C59 C60 1.372(5) . ? C60 H57 0.86(4) . ? C61 C66 1.399(6) . ? C61 C62 1.405(6) . ? C61 C67 1.523(5) . ? C62 C63 1.394(5) . ? C62 C68 1.516(6) . ? C63 C64 1.395(5) . ? C63 C69 1.506(6) . ? C64 C65 1.403(5) . ? C64 C70 1.519(5) . ? C65 C66 1.395(5) . ? C65 C71 1.509(5) . ? C66 C72 1.499(6) . ? C67 H58 0.9700 . ? C67 H59 0.9700 . ? C68 H60 0.9600 . ? C68 H61 0.9600 . ? C68 H62 0.9600 . ? C69 H63 0.9700 . ? C69 H64 0.9700 . ? C70 H65 0.9600 . ? C70 H66 0.9600 . ? C70 H67 0.9600 . ? C71 C57 1.521(5) 5 ? C71 H68 0.97(5) . ? C71 H69 1.02(5) . ? C72 H70 0.9600 . ? C72 H71 0.9600 . ? C72 H72 0.9600 . ? C73 C74 1.504(6) . ? C73 H73 0.9700 . ? C73 H74 0.9700 . ? C74 C75 1.443(8) . ? C74 H75 0.9700 . ? C74 H76 0.9700 . ? C75 C76 1.384(7) . ? C75 H77 0.9700 . ? C75 H78 0.9700 . ? C76 H79 0.9700 . ? C76 H80 0.9700 . ? C77 C78 1.503(4) . ? C77 H81 0.9700 . ? C77 H82 0.9700 . ? C78 C79 1.500(5) . ? C78 H83 0.9700 . ? C78 H84 0.9700 . ? C79 C80 1.484(5) . ? C79 H85 0.9700 . ? C79 H86 0.9700 . ? C80 H87 0.9700 . ? C80 H88 0.9700 . ? C81 C82 1.507(7) . ? C81 H89 0.9700 . ? C81 H90 0.9700 . ? C82 C83 1.335(8) . ? C82 H91 0.9700 . ? C82 H92 0.9700 . ? C83 C84 1.422(7) . ? C83 H93 0.9700 . ? C83 H94 0.9700 . ? C84 H95 0.9700 . ? C84 H96 0.9700 . ? C85 C86 1.28(2) . ? C85 C85 1.42(3) 4 ? C85 C87 1.90(2) . ? C85 H97 0.9300 . ? C86 C87 1.20(2) . ? C86 H98 0.9300 . ? C87 C87 1.35(3) 4 ? C87 H99 0.9300 . ? C88 C90 1.21(2) 4_665 ? C88 C89 1.38(2) . ? C88 H100 0.9300 . ? C89 C90 1.42(2) . ? C89 C90 1.96(2) 4_665 ? C89 H101 0.9300 . ? C90 C88 1.21(2) 4_665 ? C90 C89 1.96(2) 4_665 ? C90 H102 0.9300 . ? Li1 O3 1.984(5) 4_565 ? Li1 Li3 2.664(7) 4_565 ? Li1 Li2 2.668(6) . ? Li1 Li2 3.356(7) 4_565 ? Li1 Li3 3.435(7) . ? Li2 O2 1.979(5) 4_565 ? Li2 O3 1.989(5) 4_565 ? Li2 Li2 2.685(9) 4_565 ? Li2 C7 2.731(5) 4_565 ? Li2 Li1 3.356(7) 4_565 ? Li2 Li3 3.434(7) 4_565 ? Li3 O1 1.963(5) 4_565 ? Li3 Li3 2.613(9) 4_565 ? Li3 Li1 2.664(7) 4_565 ? Li3 Li2 3.434(7) 4_565 ? Li4 Li6 2.654(7) . ? Li4 Li5 2.664(7) . ? Li4 Li5 3.373(7) 5 ? Li4 Li6 3.410(7) 5 ? Li5 O8 1.963(5) 5 ? Li5 Li6 2.648(6) 5 ? Li5 Li4 3.373(7) 5 ? Li5 Li6 3.402(7) . ? Li6 O7 1.986(5) 5 ? Li6 Li5 2.648(6) 5 ? Li6 C43 2.785(6) 5 ? Li6 Li4 3.410(7) 5 ? 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 C1 O1 Li3 137.2(2) . 4_565 ? C1 O1 Li3 113.9(2) . . ? Li3 O1 Li3 83.3(2) 4_565 . ? C1 O1 Li1 113.9(2) . . ? Li3 O1 Li1 84.8(2) 4_565 . ? Li3 O1 Li1 120.6(2) . . ? C7 O2 Li2 136.5(2) . . ? C7 O2 Li1 117.6(2) . . ? Li2 O2 Li1 86.5(2) . . ? C7 O2 Li2 109.5(2) . 4_565 ? Li2 O2 Li2 86.5(2) . 4_565 ? Li1 O2 Li2 117.2(2) . 4_565 ? C13 O3 Li3 112.8(2) . . ? C13 O3 Li1 138.7(2) . 4_565 ? Li3 O3 Li1 84.6(2) . 4_565 ? C13 O3 Li2 113.9(2) . 4_565 ? Li3 O3 Li2 120.1(2) . 4_565 ? Li1 O3 Li2 84.3(2) 4_565 4_565 ? C34 O4 C31 108.6(2) . . ? C34 O4 Li1 124.9(2) . . ? C31 O4 Li1 126.0(2) . . ? C38 O5 C35 108.7(2) . . ? C38 O5 Li2 123.8(2) . . ? C35 O5 Li2 126.5(2) . . ? C42 O6 C39 107.7(3) . . ? C42 O6 Li3 124.2(3) . . ? C39 O6 Li3 124.6(3) . . ? C43 O7 Li5 138.4(2) . . ? C43 O7 Li4 114.9(2) . . ? Li5 O7 Li4 85.0(2) . . ? C43 O7 Li6 112.6(2) . 5 ? Li5 O7 Li6 84.1(2) . 5 ? Li4 O7 Li6 118.8(2) . 5 ? C49 O8 Li6 137.3(2) . . ? C49 O8 Li5 117.5(2) . 5 ? Li6 O8 Li5 85.3(2) . 5 ? C49 O8 Li4 110.3(2) . . ? Li6 O8 Li4 85.2(2) . . ? Li5 O8 Li4 117.8(2) 5 . ? C55 O9 Li4 137.9(2) . . ? C55 O9 Li6 112.8(2) . . ? Li4 O9 Li6 85.5(2) . . ? C55 O9 Li5 113.4(2) . . ? Li4 O9 Li5 85.7(2) . . ? Li6 O9 Li5 119.2(2) . . ? C73 O10 C76 108.8(3) . . ? C73 O10 Li4 129.7(3) . . ? C76 O10 Li4 121.4(3) . . ? C80 O11 C77 108.8(2) . . ? C80 O11 Li5 122.5(2) . . ? C77 O11 Li5 128.3(2) . . ? C81 O12 C84 109.0(3) . . ? C81 O12 Li6 125.6(3) . . ? C84 O12 Li6 125.2(3) . . ? O1 C1 C6 121.3(3) . . ? O1 C1 C2 120.6(3) . . ? C6 C1 C2 118.1(3) . . ? C3 C2 C1 121.8(3) . . ? C3 C2 H1 121.6(19) . . ? C1 C2 H1 116.5(19) . . ? C2 C3 C4 119.6(3) . . ? C2 C3 C25 121.6(3) . . ? C4 C3 C25 118.8(3) . . ? C5 C4 C3 118.0(3) . . ? C5 C4 H2 119(2) . . ? C3 C4 H2 122(2) . . ? F1 C5 C4 118.1(3) . . ? F1 C5 C6 117.7(3) . . ? C4 C5 C6 124.2(3) . . ? C5 C6 C1 118.2(3) . . ? C5 C6 H3 116(2) . . ? C1 C6 H3 125(2) . . ? O2 C7 C12 121.9(2) . . ? O2 C7 C8 119.9(2) . . ? C12 C7 C8 118.1(3) . . ? O2 C7 Li2 43.11(15) . 4_565 ? C12 C7 Li2 125.7(2) . 4_565 ? C8 C7 Li2 99.0(2) . 4_565 ? C9 C8 C7 121.8(3) . . ? C9 C8 H4 124.2(19) . . ? C7 C8 H4 114.0(19) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 C27 119.9(3) . . ? C8 C9 C27 120.3(3) . . ? C11 C10 C9 117.8(3) . . ? C11 C10 H5 120(2) . . ? C9 C10 H5 123(2) . . ? F2 C11 C10 117.9(3) . . ? F2 C11 C12 117.8(3) . . ? C10 C11 C12 124.3(3) . . ? C11 C12 C7 118.3(3) . . ? C11 C12 H6 120.5(19) . . ? C7 C12 H6 121.2(19) . . ? O3 C13 C14 120.4(3) . . ? O3 C13 C18 121.3(3) . . ? C14 C13 C18 118.2(3) . . ? O3 C13 Li3 40.96(16) . . ? C14 C13 Li3 102.4(2) . . ? C18 C13 Li3 124.6(2) . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H7 124(2) . . ? C13 C14 H7 114(2) . . ? C14 C15 C16 119.4(3) . . ? C14 C15 C29 121.9(3) . . ? C16 C15 C29 118.7(3) . . ? C17 C16 C15 117.5(3) . . ? C17 C16 H8 119(2) . . ? C15 C16 H8 123(2) . . ? F3 C17 C18 117.5(3) . . ? F3 C17 C16 117.8(3) . . ? C18 C17 C16 124.7(3) . . ? C17 C18 C13 118.2(3) . . ? C17 C18 H9 122.2(19) . . ? C13 C18 H9 119.7(19) . . ? C20 C19 C24 119.8(3) . . ? C20 C19 C25 119.8(3) . . ? C24 C19 C25 120.0(3) . . ? C21 C20 C19 120.1(3) . . ? C21 C20 C26 119.3(3) . . ? C19 C20 C26 120.4(3) . . ? C20 C21 C22 120.2(3) . . ? C20 C21 C27 120.0(3) . . ? C22 C21 C27 119.4(3) . . ? C23 C22 C21 119.3(3) . . ? C23 C22 C28 120.6(3) . . ? C21 C22 C28 120.0(4) . . ? C24 C23 C22 120.4(3) . . ? C24 C23 C29 120.3(4) . . ? C22 C23 C29 119.0(4) . . ? C23 C24 C19 120.1(3) . . ? C23 C24 C30 120.9(4) . . ? C19 C24 C30 118.9(4) . . ? C19 C25 C3 112.9(3) . . ? C19 C25 H10 109.0 . . ? C3 C25 H10 109.0 . . ? C19 C25 H11 109.0 . . ? C3 C25 H11 109.0 . . ? H10 C25 H11 107.8 . . ? C20 C26 H12 109.5 . . ? C20 C26 H13 109.5 . . ? H12 C26 H13 109.5 . . ? C20 C26 H14 109.5 . . ? H12 C26 H14 109.5 . . ? H13 C26 H14 109.5 . . ? C21 C27 C9 113.6(3) . . ? C21 C27 H15 108.8 . . ? C9 C27 H15 108.8 . . ? C21 C27 H16 108.8 . . ? C9 C27 H16 108.8 . . ? H15 C27 H16 107.7 . . ? C22 C28 H17 109.5 . . ? C22 C28 H18 109.5 . . ? H17 C28 H18 109.5 . . ? C22 C28 H19 109.5 . . ? H17 C28 H19 109.5 . . ? H18 C28 H19 109.5 . . ? C23 C29 C15 113.4(3) . . ? C23 C29 H20 108.9 . . ? C15 C29 H20 108.9 . . ? C23 C29 H21 108.9 . . ? C15 C29 H21 108.9 . . ? H20 C29 H21 107.7 . . ? C24 C30 H22 109.5 . . ? C24 C30 H23 109.5 . . ? H22 C30 H23 109.5 . . ? C24 C30 H24 109.5 . . ? H22 C30 H24 109.5 . . ? H23 C30 H24 109.5 . . ? O4 C31 C32 107.0(3) . . ? O4 C31 H25 110.3 . . ? C32 C31 H25 110.3 . . ? O4 C31 H26 110.3 . . ? C32 C31 H26 110.3 . . ? H25 C31 H26 108.6 . . ? C33 C32 C31 101.9(3) . . ? C33 C32 H27 111.4 . . ? C31 C32 H27 111.4 . . ? C33 C32 H28 111.4 . . ? C31 C32 H28 111.4 . . ? H27 C32 H28 109.2 . . ? C32 C33 C34 109.7(4) . . ? C32 C33 H29 109.7 . . ? C34 C33 H29 109.7 . . ? C32 C33 H30 109.7 . . ? C34 C33 H30 109.7 . . ? H29 C33 H30 108.2 . . ? O4 C34 C33 105.9(3) . . ? O4 C34 H31 110.5 . . ? C33 C34 H31 110.5 . . ? O4 C34 H32 110.5 . . ? C33 C34 H32 110.5 . . ? H31 C34 H32 108.7 . . ? O5 C35 C36 105.4(3) . . ? O5 C35 H33 110.7 . . ? C36 C35 H33 110.7 . . ? O5 C35 H34 110.7 . . ? C36 C35 H34 110.7 . . ? H33 C35 H34 108.8 . . ? C37 C36 C35 109.7(4) . . ? C37 C36 H35 109.7 . . ? C35 C36 H35 109.7 . . ? C37 C36 H36 109.7 . . ? C35 C36 H36 109.7 . . ? H35 C36 H36 108.2 . . ? C36 C37 C38 110.3(4) . . ? C36 C37 H37 109.6 . . ? C38 C37 H37 109.6 . . ? C36 C37 H38 109.6 . . ? C38 C37 H38 109.6 . . ? H37 C37 H38 108.1 . . ? O5 C38 C37 105.3(3) . . ? O5 C38 H39 110.7 . . ? C37 C38 H39 110.7 . . ? O5 C38 H40 110.7 . . ? C37 C38 H40 110.7 . . ? H39 C38 H40 108.8 . . ? O6 C39 C40 106.4(3) . . ? O6 C39 H41 110.4 . . ? C40 C39 H41 110.4 . . ? O6 C39 H42 110.4 . . ? C40 C39 H42 110.4 . . ? H41 C39 H42 108.6 . . ? C39 C40 C41 104.2(4) . . ? C39 C40 H43 110.9 . . ? C41 C40 H43 110.9 . . ? C39 C40 H44 110.9 . . ? C41 C40 H44 110.9 . . ? H43 C40 H44 108.9 . . ? C40 C41 C42 104.9(4) . . ? C40 C41 H45 110.8 . . ? C42 C41 H45 110.8 . . ? C40 C41 H46 110.8 . . ? C42 C41 H46 110.8 . . ? H45 C41 H46 108.8 . . ? O6 C42 C41 107.8(4) . . ? O6 C42 H47 110.2 . . ? C41 C42 H47 110.2 . . ? O6 C42 H48 110.2 . . ? C41 C42 H48 110.2 . . ? H47 C42 H48 108.5 . . ? O7 C43 C48 121.7(3) . . ? O7 C43 C44 120.7(3) . . ? C48 C43 C44 117.6(3) . . ? O7 C43 Li6 41.15(16) . 5 ? C48 C43 Li6 122.7(2) . 5 ? C44 C43 Li6 103.3(2) . 5 ? C45 C44 C43 122.8(3) . . ? C45 C44 H49 121(2) . . ? C43 C44 H49 116(2) . . ? C44 C45 C46 118.7(3) . . ? C44 C45 C67 122.1(3) . . ? C46 C45 C67 119.2(3) . . ? C47 C46 C45 118.0(3) . . ? C47 C46 H50 123(3) . . ? C45 C46 H50 119(3) . . ? C46 C47 F4 118.3(3) . . ? C46 C47 C48 124.5(3) . . ? F4 C47 C48 117.1(3) . . ? C47 C48 C43 118.3(3) . . ? C47 C48 H51 120(2) . . ? C43 C48 H51 121(2) . . ? O8 C49 C54 121.6(3) . . ? O8 C49 C50 120.2(3) . . ? C54 C49 C50 118.2(3) . . ? O8 C49 Li4 42.54(15) . . ? C54 C49 Li4 121.0(2) . . ? C50 C49 Li4 103.5(2) . . ? C51 C50 C49 122.3(3) . . ? C51 C50 H52 117(2) . . ? C49 C50 H52 121(2) . . ? C50 C51 C52 119.2(3) . . ? C50 C51 C69 121.4(3) . . ? C52 C51 C69 119.4(3) . . ? C53 C52 C51 117.8(3) . . ? C53 C52 H53 123(3) . . ? C51 C52 H53 119(3) . . ? F5 C53 C52 118.4(3) . . ? F5 C53 C54 117.5(3) . . ? C52 C53 C54 124.1(3) . . ? C53 C54 C49 118.4(3) . . ? C53 C54 H54 119(2) . . ? C49 C54 H54 122(2) . . ? O9 C55 C56 120.6(3) . . ? O9 C55 C60 122.0(3) . . ? C56 C55 C60 117.5(3) . . ? O9 C55 Li6 40.91(15) . . ? C56 C55 Li6 101.5(2) . . ? C60 C55 Li6 125.0(2) . . ? O9 C55 Li5 40.61(15) . . ? C56 C55 Li5 100.4(2) . . ? C60 C55 Li5 127.8(2) . . ? Li6 C55 Li5 75.49(15) . . ? C57 C56 C55 122.8(3) . . ? C57 C56 H55 119(2) . . ? C55 C56 H55 118(2) . . ? C56 C57 C58 118.9(3) . . ? C56 C57 C71 121.7(3) . 5 ? C58 C57 C71 119.4(3) . 5 ? C59 C58 C57 117.6(3) . . ? C59 C58 H56 122(3) . . ? C57 C58 H56 120(3) . . ? C58 C59 C60 124.7(3) . . ? C58 C59 F6 117.9(3) . . ? C60 C59 F6 117.4(3) . . ? C59 C60 C55 118.5(3) . . ? C59 C60 H57 120(3) . . ? C55 C60 H57 121(3) . . ? C66 C61 C62 120.6(4) . . ? C66 C61 C67 119.2(4) . . ? C62 C61 C67 119.8(4) . . ? C63 C62 C61 119.6(4) . . ? C63 C62 C68 120.6(4) . . ? C61 C62 C68 119.7(4) . . ? C62 C63 C64 120.0(4) . . ? C62 C63 C69 119.9(4) . . ? C64 C63 C69 119.6(4) . . ? C63 C64 C65 120.4(3) . . ? C63 C64 C70 120.3(4) . . ? C65 C64 C70 119.2(3) . . ? C66 C65 C64 119.9(4) . . ? C66 C65 C71 119.9(4) . . ? C64 C65 C71 119.8(4) . . ? C65 C66 C61 119.6(4) . . ? C65 C66 C72 119.6(4) . . ? C61 C66 C72 120.8(4) . . ? C61 C67 C45 113.1(3) . . ? C61 C67 H58 109.0 . . ? C45 C67 H58 109.0 . . ? C61 C67 H59 109.0 . . ? C45 C67 H59 109.0 . . ? H58 C67 H59 107.8 . . ? C62 C68 H60 109.5 . . ? C62 C68 H61 109.5 . . ? H60 C68 H61 109.5 . . ? C62 C68 H62 109.5 . . ? H60 C68 H62 109.5 . . ? H61 C68 H62 109.5 . . ? C63 C69 C51 113.7(3) . . ? C63 C69 H63 108.8 . . ? C51 C69 H63 108.8 . . ? C63 C69 H64 108.8 . . ? C51 C69 H64 108.8 . . ? H63 C69 H64 107.7 . . ? C64 C70 H65 109.5 . . ? C64 C70 H66 109.5 . . ? H65 C70 H66 109.5 . . ? C64 C70 H67 109.5 . . ? H65 C70 H67 109.5 . . ? H66 C70 H67 109.5 . . ? C65 C71 C57 113.6(3) . 5 ? C65 C71 H68 112(3) . . ? C57 C71 H68 104(3) 5 . ? C65 C71 H69 104(3) . . ? C57 C71 H69 106(3) 5 . ? H68 C71 H69 118(4) . . ? C66 C72 H70 109.5 . . ? C66 C72 H71 109.5 . . ? H70 C72 H71 109.5 . . ? C66 C72 H72 109.5 . . ? H70 C72 H72 109.5 . . ? H71 C72 H72 109.5 . . ? O10 C73 C74 106.1(3) . . ? O10 C73 H73 110.5 . . ? C74 C73 H73 110.5 . . ? O10 C73 H74 110.5 . . ? C74 C73 H74 110.5 . . ? H73 C73 H74 108.7 . . ? C75 C74 C73 103.9(4) . . ? C75 C74 H75 111.0 . . ? C73 C74 H75 111.0 . . ? C75 C74 H76 111.0 . . ? C73 C74 H76 111.0 . . ? H75 C74 H76 109.0 . . ? C76 C75 C74 108.2(5) . . ? C76 C75 H77 110.1 . . ? C74 C75 H77 110.1 . . ? C76 C75 H78 110.1 . . ? C74 C75 H78 110.1 . . ? H77 C75 H78 108.4 . . ? C75 C76 O10 108.1(4) . . ? C75 C76 H79 110.1 . . ? O10 C76 H79 110.1 . . ? C75 C76 H80 110.1 . . ? O10 C76 H80 110.1 . . ? H79 C76 H80 108.4 . . ? O11 C77 C78 106.1(3) . . ? O11 C77 H81 110.5 . . ? C78 C77 H81 110.5 . . ? O11 C77 H82 110.5 . . ? C78 C77 H82 110.5 . . ? H81 C77 H82 108.7 . . ? C79 C78 C77 101.3(3) . . ? C79 C78 H83 111.5 . . ? C77 C78 H83 111.5 . . ? C79 C78 H84 111.5 . . ? C77 C78 H84 111.5 . . ? H83 C78 H84 109.3 . . ? C80 C79 C78 103.4(3) . . ? C80 C79 H85 111.1 . . ? C78 C79 H85 111.1 . . ? C80 C79 H86 111.1 . . ? C78 C79 H86 111.1 . . ? H85 C79 H86 109.1 . . ? O11 C80 C79 105.6(3) . . ? O11 C80 H87 110.6 . . ? C79 C80 H87 110.6 . . ? O11 C80 H88 110.6 . . ? C79 C80 H88 110.6 . . ? H87 C80 H88 108.7 . . ? O12 C81 C82 104.7(4) . . ? O12 C81 H89 110.8 . . ? C82 C81 H89 110.8 . . ? O12 C81 H90 110.8 . . ? C82 C81 H90 110.8 . . ? H89 C81 H90 108.9 . . ? C83 C82 C81 108.1(4) . . ? C83 C82 H91 110.1 . . ? C81 C82 H91 110.1 . . ? C83 C82 H92 110.1 . . ? C81 C82 H92 110.1 . . ? H91 C82 H92 108.4 . . ? C82 C83 C84 109.2(5) . . ? C82 C83 H93 109.8 . . ? C84 C83 H93 109.8 . . ? C82 C83 H94 109.8 . . ? C84 C83 H94 109.8 . . ? H93 C83 H94 108.3 . . ? O12 C84 C83 107.4(4) . . ? O12 C84 H95 110.2 . . ? C83 C84 H95 110.2 . . ? O12 C84 H96 110.2 . . ? C83 C84 H96 110.2 . . ? H95 C84 H96 108.5 . . ? C86 C85 C85 126.7(10) . 4 ? C86 C85 C87 38.3(9) . . ? C85 C85 C87 88.9(6) 4 . ? C86 C85 H97 116.6 . . ? C85 C85 H97 116.6 4 . ? C87 C85 H97 153.6 . . ? C87 C86 C85 100.3(14) . . ? C87 C86 H98 129.8 . . ? C85 C86 H98 129.8 . . ? C86 C87 C87 132.0(10) . 4 ? C86 C87 C85 41.3(10) . . ? C87 C87 C85 91.0(6) 4 . ? C86 C87 H99 114.0 . . ? C87 C87 H99 114.0 4 . ? C85 C87 H99 154.3 . . ? C90 C88 C89 97.8(15) 4_665 . ? C90 C88 H100 131.1 4_665 . ? C89 C88 H100 131.1 . . ? C88 C89 C90 132.5(16) . . ? C88 C89 C90 37.9(9) . 4_665 ? C90 C89 C90 94.7(13) . 4_665 ? C88 C89 H101 113.8 . . ? C90 C89 H101 113.8 . . ? C90 C89 H101 151.5 4_665 . ? C88 C90 C89 129.6(18) 4_665 . ? C88 C90 C89 44.3(11) 4_665 4_665 ? C89 C90 C89 85.3(13) . 4_665 ? C88 C90 H102 115.2 4_665 . ? C89 C90 H102 115.2 . . ? C89 C90 H102 159.4 4_665 . ? O2 Li1 O3 94.5(2) . 4_565 ? O2 Li1 O1 120.4(3) . . ? O3 Li1 O1 94.8(2) 4_565 . ? O2 Li1 O4 114.4(2) . . ? O3 Li1 O4 116.9(3) 4_565 . ? O1 Li1 O4 112.9(2) . . ? O2 Li1 Li3 116.3(2) . 4_565 ? O3 Li1 Li3 47.54(16) 4_565 4_565 ? O1 Li1 Li3 47.22(15) . 4_565 ? O4 Li1 Li3 127.6(2) . 4_565 ? O2 Li1 Li2 46.55(15) . . ? O3 Li1 Li2 47.91(15) 4_565 . ? O1 Li1 Li2 115.1(2) . . ? O4 Li1 Li2 130.4(2) . . ? Li3 Li1 Li2 80.2(2) 4_565 . ? O2 Li1 Li2 31.62(13) . 4_565 ? O3 Li1 Li2 91.38(18) 4_565 4_565 ? O1 Li1 Li2 89.43(19) . 4_565 ? O4 Li1 Li2 140.8(2) . 4_565 ? Li3 Li1 Li2 91.39(18) 4_565 4_565 ? Li2 Li1 Li2 51.40(18) . 4_565 ? O2 Li1 Li3 92.30(19) . . ? O3 Li1 Li3 88.26(18) 4_565 . ? O1 Li1 Li3 29.58(13) . . ? O4 Li1 Li3 140.0(2) . . ? Li3 Li1 Li3 48.75(19) 4_565 . ? Li2 Li1 Li3 89.61(18) . . ? Li2 Li1 Li3 60.73(14) 4_565 . ? O2 Li2 O2 93.5(2) . 4_565 ? O2 Li2 O3 94.7(2) . 4_565 ? O2 Li2 O3 120.8(2) 4_565 4_565 ? O2 Li2 O5 115.8(2) . . ? O2 Li2 O5 115.4(2) 4_565 . ? O3 Li2 O5 112.9(2) 4_565 . ? O2 Li2 Li1 46.92(15) . . ? O2 Li2 Li1 114.1(2) 4_565 . ? O3 Li2 Li1 47.75(15) 4_565 . ? O5 Li2 Li1 128.3(2) . . ? O2 Li2 Li2 47.37(15) . 4_565 ? O2 Li2 Li2 46.16(15) 4_565 4_565 ? O3 Li2 Li2 114.05(16) 4_565 4_565 ? O5 Li2 Li2 130.98(15) . 4_565 ? Li1 Li2 Li2 77.66(19) . 4_565 ? O2 Li2 C7 112.6(2) . 4_565 ? O2 Li2 C7 27.41(10) 4_565 4_565 ? O3 Li2 C7 133.7(2) 4_565 4_565 ? O5 Li2 C7 88.84(18) . 4_565 ? Li1 Li2 C7 141.5(2) . 4_565 ? Li2 Li2 C7 68.52(18) 4_565 4_565 ? O2 Li2 Li1 91.37(18) . 4_565 ? O2 Li2 Li1 31.14(12) 4_565 4_565 ? O3 Li2 Li1 90.12(19) 4_565 4_565 ? O5 Li2 Li1 141.4(2) . 4_565 ? Li1 Li2 Li1 90.3(2) . 4_565 ? Li2 Li2 Li1 50.94(15) 4_565 4_565 ? C7 Li2 Li1 54.19(13) 4_565 4_565 ? O2 Li2 Li3 89.85(18) . 4_565 ? O2 Li2 Li3 91.86(18) 4_565 4_565 ? O3 Li2 Li3 29.84(13) 4_565 4_565 ? O5 Li2 Li3 139.7(2) . 4_565 ? Li1 Li2 Li3 49.86(15) . 4_565 ? Li2 Li2 Li3 89.36(11) 4_565 4_565 ? C7 Li2 Li3 110.45(17) 4_565 4_565 ? Li1 Li2 Li3 60.77(14) 4_565 4_565 ? O1 Li3 O1 96.6(2) 4_565 . ? O1 Li3 O3 95.8(2) 4_565 . ? O1 Li3 O3 115.9(3) . . ? O1 Li3 O6 114.6(3) 4_565 . ? O1 Li3 O6 118.7(3) . . ? O3 Li3 O6 111.9(2) . . ? O1 Li3 Li3 48.45(16) 4_565 4_565 ? O1 Li3 Li3 48.26(16) . 4_565 ? O3 Li3 Li3 116.47(16) . 4_565 ? O6 Li3 Li3 129.67(16) . 4_565 ? O1 Li3 Li1 47.95(16) 4_565 4_565 ? O1 Li3 Li1 115.1(2) . 4_565 ? O3 Li3 Li1 47.87(15) . 4_565 ? O6 Li3 Li1 125.2(2) . 4_565 ? Li3 Li3 Li1 81.2(2) 4_565 4_565 ? O1 Li3 C13 116.0(2) 4_565 . ? O1 Li3 C13 125.1(2) . . ? O3 Li3 C13 26.29(10) . . ? O6 Li3 C13 87.42(19) . . ? Li3 Li3 C13 142.36(12) 4_565 . ? Li1 Li3 C13 69.78(17) 4_565 . ? O1 Li3 Li2 89.65(18) 4_565 4_565 ? O1 Li3 Li2 87.50(18) . 4_565 ? O3 Li3 Li2 30.10(13) . 4_565 ? O6 Li3 Li2 139.7(2) . 4_565 ? Li3 Li3 Li2 90.56(11) 4_565 4_565 ? Li1 Li3 Li2 49.96(15) 4_565 4_565 ? C13 Li3 Li2 52.47(13) . 4_565 ? O1 Li3 Li1 89.00(18) 4_565 . ? O1 Li3 Li1 29.86(12) . . ? O3 Li3 Li1 88.13(19) . . ? O6 Li3 Li1 146.0(2) . . ? Li3 Li3 Li1 50.04(16) 4_565 . ? Li1 Li3 Li1 88.7(2) 4_565 . ? C13 Li3 Li1 104.41(17) . . ? Li2 Li3 Li1 58.50(13) 4_565 . ? O9 Li4 O8 94.6(2) . . ? O9 Li4 O7 95.1(2) . . ? O8 Li4 O7 120.5(3) . . ? O9 Li4 O10 115.8(3) . . ? O8 Li4 O10 116.5(2) . . ? O7 Li4 O10 111.1(2) . . ? O9 Li4 Li6 47.64(15) . . ? O8 Li4 Li6 46.93(15) . . ? O7 Li4 Li6 115.9(2) . . ? O10 Li4 Li6 130.9(3) . . ? O9 Li4 Li5 47.74(15) . . ? O8 Li4 Li5 115.1(2) . . ? O7 Li4 Li5 47.41(15) . . ? O10 Li4 Li5 126.8(3) . . ? Li6 Li4 Li5 79.53(19) . . ? O9 Li4 C49 114.3(2) . . ? O8 Li4 C49 27.11(10) . . ? O7 Li4 C49 131.6(2) . . ? O10 Li4 C49 90.39(19) . . ? Li6 Li4 C49 69.12(17) . . ? Li5 Li4 C49 142.2(2) . . ? O9 Li4 Li5 90.10(18) . 5 ? O8 Li4 Li5 30.97(12) . 5 ? O7 Li4 Li5 90.49(19) . 5 ? O10 Li4 Li5 143.3(2) . 5 ? Li6 Li4 Li5 50.40(15) . 5 ? Li5 Li4 Li5 89.72(18) . 5 ? C49 Li4 Li5 54.09(13) . 5 ? O9 Li4 Li6 90.05(18) . 5 ? O8 Li4 Li6 90.88(19) . 5 ? O7 Li4 Li6 30.68(13) . 5 ? O10 Li4 Li6 138.8(2) . 5 ? Li6 Li4 Li6 90.34(18) . 5 ? Li5 Li4 Li6 49.86(15) . 5 ? C49 Li4 Li6 108.33(18) . 5 ? Li5 Li4 Li6 60.21(14) 5 5 ? O8 Li5 O7 95.3(2) 5 . ? O8 Li5 O9 120.8(3) 5 . ? O7 Li5 O9 94.2(2) . . ? O8 Li5 O11 110.3(2) 5 . ? O7 Li5 O11 117.2(3) . . ? O9 Li5 O11 116.2(2) . . ? O8 Li5 Li6 47.09(16) 5 5 ? O7 Li5 Li6 48.24(16) . 5 ? O9 Li5 Li6 115.4(2) . 5 ? O11 Li5 Li6 127.2(2) . 5 ? O8 Li5 Li4 115.8(2) 5 . ? O7 Li5 Li4 47.60(15) . . ? O9 Li5 Li4 46.61(15) . . ? O11 Li5 Li4 132.1(3) . . ? Li6 Li5 Li4 79.9(2) 5 . ? O8 Li5 C55 130.9(2) 5 . ? O7 Li5 C55 113.6(2) . . ? O9 Li5 C55 25.97(10) . . ? O11 Li5 C55 91.23(19) . . ? Li6 Li5 C55 141.2(2) 5 . ? Li4 Li5 C55 68.27(16) . . ? O8 Li5 Li4 31.18(13) 5 5 ? O7 Li5 Li4 90.86(18) . 5 ? O9 Li5 Li4 90.47(19) . 5 ? O11 Li5 Li4 137.6(2) . 5 ? Li6 Li5 Li4 50.58(16) 5 5 ? Li4 Li5 Li4 90.28(18) . 5 ? C55 Li5 Li4 106.44(18) . 5 ? O8 Li5 Li6 91.31(19) 5 . ? O7 Li5 Li6 90.30(18) . . ? O9 Li5 Li6 30.33(12) . . ? O11 Li5 Li6 141.9(2) . . ? Li6 Li5 Li6 90.62(18) 5 . ? Li4 Li5 Li6 50.11(15) . . ? C55 Li5 Li6 52.01(12) . . ? Li4 Li5 Li6 60.43(14) 5 . ? O8 Li6 O9 94.7(2) . . ? O8 Li6 O7 95.3(2) . 5 ? O9 Li6 O7 119.0(3) . 5 ? O8 Li6 O12 115.3(3) . . ? O9 Li6 O12 116.2(2) . . ? O7 Li6 O12 112.8(2) 5 . ? O8 Li6 Li5 47.64(15) . 5 ? O9 Li6 Li5 114.3(2) . 5 ? O7 Li6 Li5 47.69(15) 5 5 ? O12 Li6 Li5 127.8(2) . 5 ? O8 Li6 Li4 47.86(16) . . ? O9 Li6 Li4 46.82(15) . . ? O7 Li6 Li4 115.1(2) 5 . ? O12 Li6 Li4 130.2(3) . . ? Li5 Li6 Li4 79.02(19) 5 . ? O8 Li6 C55 114.4(2) . . ? O9 Li6 C55 26.29(10) . . ? O7 Li6 C55 129.4(2) 5 . ? O12 Li6 C55 91.17(18) . . ? Li5 Li6 C55 140.4(2) 5 . ? Li4 Li6 C55 68.68(17) . . ? O8 Li6 C43 114.7(2) . 5 ? O9 Li6 C43 129.8(2) . 5 ? O7 Li6 C43 26.23(11) 5 5 ? O12 Li6 C43 87.85(19) . 5 ? Li5 Li6 C43 69.40(17) 5 5 ? Li4 Li6 C43 141.1(2) . 5 ? C55 Li6 C43 125.8(2) . 5 ? O8 Li6 Li5 90.48(18) . . ? O9 Li6 Li5 30.50(12) . . ? O7 Li6 Li5 89.47(19) 5 . ? O12 Li6 Li5 142.7(2) . . ? Li5 Li6 Li5 89.38(18) 5 . ? Li4 Li6 Li5 50.36(15) . . ? C55 Li6 Li5 52.50(12) . . ? C43 Li6 Li5 106.00(18) 5 . ? O8 Li6 Li4 90.42(18) . 5 ? O9 Li6 Li4 89.59(19) . 5 ? O7 Li6 Li4 30.49(13) 5 5 ? O12 Li6 Li4 140.1(2) . 5 ? Li5 Li6 Li4 50.28(15) 5 5 ? Li4 Li6 Li4 89.66(18) . 5 ? C55 Li6 Li4 105.92(17) . 5 ? C43 Li6 Li4 52.80(13) 5 5 ? Li5 Li6 Li4 59.37(14) . 5 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.968 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.096 data_(1bLi3)2(THF)4 _database_code_depnum_ccdc_archive 'CCDC 861325' #TrackingRef '- all-CIF2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C94 H104 Li6 O10 ' _chemical_formula_moiety 'C94 H104 Li6 O10 ' _chemical_formula_weight 1435.50 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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9238(13) _cell_length_b 13.6966(15) _cell_length_c 14.6695(15) _cell_angle_alpha 67.099(2) _cell_angle_beta 64.141(2) _cell_angle_gamma 64.306(2) _cell_volume 2040.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 30.4 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9785 _exptl_absorpt_correction_T_max 0.9856 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 12270 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.1071 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7181 _reflns_number_gt 3197 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+1.2778P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7181 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1967 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2804 _refine_ls_wR_factor_gt 0.2179 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 O1 O 0.6872(2) 0.9104(2) 0.0232(2) 0.0570(8) Uani 1 1 d . . . O2 O 0.4500(3) 0.8587(3) 0.0419(2) 0.0647(9) Uani 1 1 d . . . O3 O 0.3854(3) 1.0532(2) 0.1509(2) 0.0586(8) Uani 1 1 d . . . O4 O 0.1698(3) 0.9560(3) 0.2146(3) 0.0878(12) Uani 1 1 d . . . O5 O 0.2611(4) 1.3187(3) 0.0326(3) 0.0970(13) Uani 1 1 d . . . C1 C 0.7686(4) 0.8540(4) 0.0742(3) 0.0528(11) Uani 1 1 d . . . C2 C 0.7439(4) 0.7735(4) 0.1677(3) 0.0605(13) Uani 1 1 d . . . H1 H 0.6702 0.7604 0.1933 0.073 Uiso 1 1 calc R . . C3 C 0.8241(4) 0.7122(4) 0.2239(3) 0.0603(13) Uani 1 1 d . . . C4 C 0.9329(4) 0.7328(4) 0.1860(4) 0.0695(14) Uani 1 1 d . . . H2 H 0.9881 0.6932 0.2227 0.083 Uiso 1 1 calc R . . C5 C 0.9599(4) 0.8125(5) 0.0933(4) 0.0756(15) Uani 1 1 d . . . H3 H 1.0331 0.8262 0.0685 0.091 Uiso 1 1 calc R . . C6 C 0.8794(4) 0.8718(4) 0.0373(4) 0.0670(14) Uani 1 1 d . . . H4 H 0.8996 0.9239 -0.0254 0.080 Uiso 1 1 calc R . . C7 C 0.4282(4) 0.7604(4) 0.0907(3) 0.0610(13) Uani 1 1 d . . . C8 C 0.4470(4) 0.7008(4) 0.1860(3) 0.0593(12) Uani 1 1 d . . . H5 H 0.4754 0.7300 0.2147 0.071 Uiso 1 1 calc R . . C9 C 0.4254(4) 0.5997(4) 0.2404(4) 0.0631(13) Uani 1 1 d . . . C10 C 0.3833(5) 0.5574(5) 0.1966(4) 0.0859(17) Uani 1 1 d . . . H6 H 0.3679 0.4896 0.2313 0.103 Uiso 1 1 calc R . . C11 C 0.3644(6) 0.6151(6) 0.1022(5) 0.105(2) Uani 1 1 d . . . H7 H 0.3366 0.5855 0.0734 0.125 Uiso 1 1 calc R . . C12 C 0.3855(5) 0.7158(5) 0.0491(4) 0.0847(17) Uani 1 1 d . . . H8 H 0.3712 0.7539 -0.0145 0.102 Uiso 1 1 calc R . . C13 C 0.3521(4) 1.0505(4) 0.2523(3) 0.0538(12) Uani 1 1 d . . . C14 C 0.3748(4) 0.9499(4) 0.3257(3) 0.0589(12) Uani 1 1 d . . . H9 H 0.4125 0.8844 0.3030 0.071 Uiso 1 1 calc R . . C15 C 0.3450(4) 0.9409(4) 0.4309(3) 0.0642(13) Uani 1 1 d . . . C16 C 0.2912(4) 1.0393(5) 0.4629(4) 0.0714(15) Uani 1 1 d . . . H10 H 0.2722 1.0369 0.5325 0.086 Uiso 1 1 calc R . . C17 C 0.2658(5) 1.1401(5) 0.3927(4) 0.0792(16) Uani 1 1 d . . . H11 H 0.2282 1.2053 0.4160 0.095 Uiso 1 1 calc R . . C18 C 0.2945(4) 1.1484(4) 0.2870(4) 0.0686(14) Uani 1 1 d . . . H12 H 0.2757 1.2177 0.2407 0.082 Uiso 1 1 calc R . . C19 C 0.7953(4) 0.6243(4) 0.3262(4) 0.0763(16) Uani 1 1 d . . . H13 H 0.8425 0.5504 0.3136 0.092 Uiso 1 1 calc R . . H14 H 0.8194 0.6320 0.3765 0.092 Uiso 1 1 calc R . . C20 C 0.6621(5) 0.6343(4) 0.3722(3) 0.0662(14) Uani 1 1 d . . . C21 C 0.6201(5) 0.5727(4) 0.3466(3) 0.0633(14) Uani 1 1 d . . . C22 C 0.4950(5) 0.5912(4) 0.3803(3) 0.0641(14) Uani 1 1 d . . . C23 C 0.4125(5) 0.6726(4) 0.4362(3) 0.0631(13) Uani 1 1 d . . . C24 C 0.4553(5) 0.7334(4) 0.4607(3) 0.0644(14) Uani 1 1 d . . . C25 C 0.5805(5) 0.7131(4) 0.4292(3) 0.0660(14) Uani 1 1 d . . . C26 C 0.6271(6) 0.7842(5) 0.4505(4) 0.0960(19) Uani 1 1 d . . . H15 H 0.6454 0.7473 0.5148 0.115 Uiso 1 1 calc R . . H16 H 0.5662 0.8557 0.4558 0.115 Uiso 1 1 calc R . . H17 H 0.6992 0.7946 0.3943 0.115 Uiso 1 1 calc R . . C27 C 0.7050(5) 0.4942(5) 0.2774(4) 0.0925(19) Uani 1 1 d . . . H18 H 0.7115 0.5338 0.2059 0.111 Uiso 1 1 calc R . . H19 H 0.6743 0.4341 0.2963 0.111 Uiso 1 1 calc R . . H20 H 0.7836 0.4645 0.2856 0.111 Uiso 1 1 calc R . . C28 C 0.4468(5) 0.5349(4) 0.3442(4) 0.0734(15) Uani 1 1 d . . . H21 H 0.3711 0.5255 0.3966 0.088 Uiso 1 1 calc R . . H22 H 0.5042 0.4611 0.3383 0.088 Uiso 1 1 calc R . . C29 C 0.2797(5) 0.6984(5) 0.4627(4) 0.0902(18) Uani 1 1 d . . . H23 H 0.2526 0.7568 0.4074 0.108 Uiso 1 1 calc R . . H24 H 0.2373 0.7225 0.5266 0.108 Uiso 1 1 calc R . . H25 H 0.2636 0.6326 0.4714 0.108 Uiso 1 1 calc R . . C30 C 0.3698(5) 0.8297(4) 0.5100(3) 0.0778(16) Uani 1 1 d . . . H26 H 0.4040 0.8346 0.5547 0.093 Uiso 1 1 calc R . . H27 H 0.2937 0.8151 0.5538 0.093 Uiso 1 1 calc R . . C31 C 0.1179(6) 0.8716(6) 0.2415(5) 0.106(2) Uani 1 1 d . . . H28 H 0.1765 0.7982 0.2551 0.127 Uiso 1 1 calc R . . H29 H 0.0945 0.8785 0.1842 0.127 Uiso 1 1 calc R . . C32 C 0.0124(6) 0.8854(7) 0.3340(6) 0.132(3) Uani 1 1 d . . . H30 H 0.0249 0.8216 0.3925 0.158 Uiso 1 1 calc R . . H31 H -0.0590 0.8933 0.3215 0.158 Uiso 1 1 calc R . . C33 C -0.0023(9) 0.9903(10) 0.3559(7) 0.187(5) Uani 1 1 d . . . H32 H -0.0835 1.0424 0.3608 0.225 Uiso 1 1 calc R . . H33 H 0.0114 0.9726 0.4214 0.225 Uiso 1 1 calc R . . C34 C 0.0832(6) 1.0368(7) 0.2732(7) 0.141(3) Uani 1 1 d . . . H34 H 0.1239 1.0593 0.2999 0.169 Uiso 1 1 calc R . . H35 H 0.0433 1.1025 0.2284 0.169 Uiso 1 1 calc R . . C35 C 0.1335(5) 1.3370(6) 0.0686(6) 0.116(2) Uani 1 1 d . . . H36 H 0.1145 1.2701 0.1171 0.139 Uiso 1 1 calc R . . H37 H 0.1047 1.3581 0.0105 0.139 Uiso 1 1 calc R . . C36 C 0.0766(7) 1.4305(8) 0.1222(8) 0.170(4) Uani 1 1 d . . . H38 H -0.0004 1.4792 0.1113 0.204 Uiso 1 1 calc R . . H39 H 0.0641 1.4018 0.1967 0.204 Uiso 1 1 calc R . . C37 C 0.1671(8) 1.4893(8) 0.0709(11) 0.230(7) Uani 1 1 d . . . H40 H 0.1453 1.5526 0.0149 0.276 Uiso 1 1 calc R . . H41 H 0.1707 1.5168 0.1209 0.276 Uiso 1 1 calc R . . C38 C 0.2786(6) 1.4146(6) 0.0310(5) 0.107(2) Uani 1 1 d . . . H42 H 0.3296 1.3933 0.0728 0.128 Uiso 1 1 calc R . . H43 H 0.3187 1.4496 -0.0401 0.128 Uiso 1 1 calc R . . C39 C 0.4019(6) 0.8901(6) 0.7401(4) 0.0843(17) Uani 1 1 d . . . H44 H 0.4597 0.9268 0.7023 0.101 Uiso 1 1 calc R . . C40 C 0.4355(6) 0.7780(7) 0.7542(5) 0.0939(19) Uani 1 1 d . . . H45 H 0.5165 0.7380 0.7267 0.113 Uiso 1 1 calc R . . C41 C 0.3516(7) 0.7239(6) 0.8083(5) 0.0907(18) Uani 1 1 d . . . H46 H 0.3755 0.6471 0.8172 0.109 Uiso 1 1 calc R . . C42 C 0.2353(7) 0.7800(7) 0.8488(5) 0.099(2) Uani 1 1 d . . . H47 H 0.1780 0.7428 0.8857 0.119 Uiso 1 1 calc R . . C43 C 0.2010(6) 0.8933(7) 0.8356(5) 0.107(2) Uani 1 1 d . . . H48 H 0.1199 0.9325 0.8642 0.128 Uiso 1 1 calc R . . C44 C 0.2835(6) 0.9492(5) 0.7814(4) 0.0873(17) Uani 1 1 d . . . H49 H 0.2598 1.0259 0.7727 0.105 Uiso 1 1 calc R . . C45 C 0.0844(6) 0.4639(7) 0.4137(6) 0.107(2) Uani 1 1 d . . . H51 H 0.1417 0.4395 0.3545 0.128 Uiso 1 1 calc R . . C46 C 0.0820(6) 0.5530(7) 0.4339(7) 0.107(2) Uani 1 1 d . . . H50 H 0.1391 0.5891 0.3884 0.128 Uiso 1 1 calc R . . C47 C -0.0004(8) 0.5906(6) 0.5178(8) 0.113(2) Uani 1 1 d . . . H52 H -0.0012 0.6528 0.5300 0.135 Uiso 1 1 calc R . . Li1 Li 0.5550(7) 1.0280(8) 0.0827(6) 0.075(3) Uani 1 1 d . . . Li2 Li 0.3205(7) 0.9780(6) 0.1098(5) 0.060(2) Uani 1 1 d . . . Li3 Li 0.3742(7) 1.1649(7) 0.0203(6) 0.064(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0556(17) 0.0544(18) 0.0518(17) 0.0029(14) -0.0261(15) -0.0147(14) O2 0.0635(19) 0.064(2) 0.0444(16) 0.0030(15) -0.0203(15) -0.0130(16) O3 0.0668(19) 0.0597(19) 0.0412(16) -0.0004(13) -0.0214(14) -0.0197(15) O4 0.081(3) 0.100(3) 0.083(2) -0.026(2) -0.006(2) -0.046(2) O5 0.085(3) 0.085(3) 0.117(3) -0.034(2) -0.026(2) -0.023(2) C1 0.049(3) 0.054(3) 0.049(2) -0.008(2) -0.022(2) -0.010(2) C2 0.059(3) 0.065(3) 0.055(3) -0.001(2) -0.029(2) -0.019(2) C3 0.057(3) 0.065(3) 0.058(3) -0.007(2) -0.033(2) -0.012(2) C4 0.062(3) 0.069(3) 0.077(3) -0.010(3) -0.043(3) -0.007(3) C5 0.058(3) 0.089(4) 0.079(3) -0.005(3) -0.030(3) -0.029(3) C6 0.060(3) 0.074(3) 0.058(3) -0.004(2) -0.021(2) -0.023(3) C7 0.051(3) 0.063(3) 0.046(2) -0.007(2) -0.019(2) -0.002(2) C8 0.068(3) 0.057(3) 0.049(3) -0.004(2) -0.028(2) -0.016(2) C9 0.068(3) 0.059(3) 0.059(3) -0.005(2) -0.030(2) -0.016(2) C10 0.106(4) 0.081(4) 0.086(4) -0.007(3) -0.045(3) -0.041(3) C11 0.156(6) 0.100(5) 0.099(5) -0.005(4) -0.070(4) -0.065(5) C12 0.104(4) 0.108(5) 0.061(3) -0.013(3) -0.045(3) -0.038(4) C13 0.052(3) 0.061(3) 0.044(2) -0.002(2) -0.019(2) -0.021(2) C14 0.064(3) 0.061(3) 0.048(3) -0.013(2) -0.015(2) -0.021(2) C15 0.067(3) 0.080(4) 0.042(2) -0.010(2) -0.014(2) -0.027(3) C16 0.072(3) 0.092(4) 0.050(3) -0.018(3) -0.021(3) -0.025(3) C17 0.078(4) 0.087(4) 0.073(4) -0.038(3) -0.019(3) -0.015(3) C18 0.069(3) 0.063(3) 0.070(3) -0.014(3) -0.029(3) -0.013(3) C19 0.078(4) 0.074(3) 0.063(3) 0.013(3) -0.041(3) -0.019(3) C20 0.074(3) 0.064(3) 0.046(3) 0.013(2) -0.034(3) -0.018(3) C21 0.073(3) 0.050(3) 0.047(3) 0.007(2) -0.026(3) -0.012(3) C22 0.086(4) 0.055(3) 0.042(2) 0.014(2) -0.031(3) -0.026(3) C23 0.081(4) 0.060(3) 0.042(2) 0.011(2) -0.031(3) -0.027(3) C24 0.080(4) 0.060(3) 0.034(2) 0.003(2) -0.022(2) -0.015(3) C25 0.087(4) 0.067(3) 0.042(2) 0.003(2) -0.034(3) -0.025(3) C26 0.114(5) 0.115(5) 0.072(4) -0.010(3) -0.038(3) -0.051(4) C27 0.101(4) 0.081(4) 0.081(4) -0.006(3) -0.044(3) -0.014(3) C28 0.089(4) 0.062(3) 0.063(3) 0.004(2) -0.031(3) -0.030(3) C29 0.089(4) 0.099(4) 0.071(3) -0.003(3) -0.027(3) -0.033(3) C30 0.098(4) 0.083(4) 0.040(2) 0.000(2) -0.024(3) -0.030(3) C31 0.095(5) 0.099(5) 0.111(5) -0.010(4) -0.030(4) -0.038(4) C32 0.084(5) 0.120(6) 0.128(6) -0.005(5) 0.001(5) -0.036(4) C33 0.154(8) 0.228(12) 0.142(8) -0.092(8) 0.057(7) -0.096(8) C34 0.081(5) 0.175(8) 0.175(8) -0.097(7) -0.002(5) -0.041(5) C35 0.070(4) 0.100(5) 0.171(7) -0.058(5) -0.037(4) -0.003(3) C36 0.086(5) 0.162(8) 0.216(10) -0.104(8) -0.027(6) 0.028(6) C37 0.089(6) 0.156(9) 0.416(19) -0.175(11) 0.024(8) -0.028(6) C38 0.115(5) 0.085(5) 0.111(5) -0.032(4) -0.014(4) -0.039(4) C39 0.085(4) 0.101(5) 0.069(3) -0.011(3) -0.027(3) -0.038(4) C40 0.087(4) 0.114(6) 0.068(4) -0.029(4) -0.023(3) -0.017(4) C41 0.115(5) 0.086(4) 0.075(4) -0.023(3) -0.032(4) -0.031(4) C42 0.104(5) 0.109(6) 0.092(4) -0.002(4) -0.034(4) -0.057(4) C43 0.071(4) 0.115(6) 0.105(5) -0.014(4) -0.015(4) -0.030(4) C44 0.098(5) 0.081(4) 0.078(4) -0.018(3) -0.029(4) -0.024(4) C45 0.095(5) 0.102(6) 0.110(5) -0.017(5) -0.043(4) -0.019(4) C46 0.078(5) 0.095(6) 0.132(7) -0.005(5) -0.046(5) -0.023(4) C47 0.103(5) 0.088(5) 0.141(6) -0.013(5) -0.049(5) -0.030(5) Li1 0.062(5) 0.082(6) 0.053(4) -0.008(4) -0.018(4) -0.007(4) Li2 0.061(4) 0.058(5) 0.045(4) 0.001(3) -0.015(3) -0.020(4) Li3 0.066(5) 0.063(5) 0.058(4) 0.003(4) -0.032(4) -0.019(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 O1 C1 1.340(5) . ? O1 Li1 1.919(9) . ? O1 Li3 1.940(9) 2_675 ? O1 Li2 1.967(7) 2_675 ? O2 C7 1.345(6) . ? O2 Li1 1.887(8) 2_675 ? O2 Li3 1.970(8) 2_675 ? O2 Li2 1.976(8) . ? O3 C13 1.346(5) . ? O3 Li1 1.903(9) . ? O3 Li3 1.950(7) . ? O3 Li2 1.950(9) . ? O4 C31 1.425(7) . ? O4 C34 1.430(8) . ? O4 Li2 1.945(8) . ? O5 C38 1.417(7) . ? O5 C35 1.431(7) . ? O5 Li3 2.001(9) . ? C1 C6 1.388(6) . ? C1 C2 1.395(6) . ? C1 Li1 2.746(9) . ? C2 C3 1.383(6) . ? C2 H1 0.9300 . ? C3 C4 1.381(6) . ? C3 C19 1.528(6) . ? C4 C5 1.387(6) . ? C4 H2 0.9300 . ? C5 C6 1.383(6) . ? C5 H3 0.9300 . ? C6 H4 0.9300 . ? C7 C8 1.384(6) . ? C7 C12 1.387(7) . ? C7 Li3 2.750(9) 2_675 ? C7 Li2 2.759(9) . ? C8 C9 1.384(6) . ? C8 H5 0.9300 . ? C9 C10 1.381(7) . ? C9 C28 1.513(6) . ? C10 C11 1.371(8) . ? C10 H6 0.9300 . ? C11 C12 1.373(8) . ? C11 H7 0.9300 . ? C12 H8 0.9300 . ? C13 C14 1.383(6) . ? C13 C18 1.395(7) . ? C13 Li1 2.714(9) . ? C14 C15 1.385(6) . ? C14 H9 0.9300 . ? C15 C16 1.384(7) . ? C15 C30 1.515(6) . ? C16 C17 1.368(7) . ? C16 H10 0.9300 . ? C17 C18 1.397(7) . ? C17 H11 0.9300 . ? C18 H12 0.9300 . ? C19 C20 1.514(7) . ? C19 H13 0.9700 . ? C19 H14 0.9700 . ? C20 C25 1.386(7) . ? C20 C21 1.403(7) . ? C21 C22 1.404(7) . ? C21 C27 1.499(7) . ? C22 C23 1.404(7) . ? C22 C28 1.511(7) . ? C23 C24 1.391(7) . ? C23 C29 1.490(7) . ? C24 C25 1.403(7) . ? C24 C30 1.505(7) . ? C25 C26 1.524(8) . ? C26 H15 0.9600 . ? C26 H16 0.9600 . ? C26 H17 0.9600 . ? C27 H18 0.9600 . ? C27 H19 0.9600 . ? C27 H20 0.9600 . ? C28 H21 0.9700 . ? C28 H22 0.9700 . ? C29 H23 0.9600 . ? C29 H24 0.9600 . ? C29 H25 0.9600 . ? C30 H26 0.9700 . ? C30 H27 0.9700 . ? C31 C32 1.449(8) . ? C31 H28 0.9700 . ? C31 H29 0.9700 . ? C32 C33 1.508(11) . ? C32 H30 0.9700 . ? C32 H31 0.9700 . ? C33 C34 1.392(10) . ? C33 H32 0.9700 . ? C33 H33 0.9700 . ? C34 H34 0.9700 . ? C34 H35 0.9700 . ? C35 C36 1.504(10) . ? C35 H36 0.9700 . ? C35 H37 0.9700 . ? C36 C37 1.470(12) . ? C36 H38 0.9700 . ? C36 H39 0.9700 . ? C37 C38 1.384(9) . ? C37 H40 0.9700 . ? C37 H41 0.9700 . ? C38 H42 0.9700 . ? C38 H43 0.9700 . ? C39 C40 1.358(8) . ? C39 C44 1.364(8) . ? C39 H44 0.9300 . ? C40 C41 1.357(9) . ? C40 H45 0.9300 . ? C41 C42 1.334(8) . ? C41 H46 0.9300 . ? C42 C43 1.374(9) . ? C42 H47 0.9300 . ? C43 C44 1.360(8) . ? C43 H48 0.9300 . ? C44 H49 0.9300 . ? C45 C46 1.348(10) . ? C45 C47 1.383(9) 2_566 ? C45 H51 0.9300 . ? C46 C47 1.338(10) . ? C46 H50 0.9300 . ? C47 C45 1.383(9) 2_566 ? C47 H52 0.9300 . ? Li1 O2 1.887(8) 2_675 ? Li1 Li3 2.558(11) . ? Li1 Li2 2.584(11) 2_675 ? Li1 Li3 3.147(13) 2_675 ? Li1 Li2 3.217(12) . ? Li2 O1 1.967(7) 2_675 ? Li2 Li1 2.584(11) 2_675 ? Li2 Li3 2.624(11) . ? Li3 O1 1.939(9) 2_675 ? Li3 O2 1.971(8) 2_675 ? Li3 C7 2.750(9) 2_675 ? Li3 Li1 3.147(13) 2_675 ? 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 C1 O1 Li1 113.6(4) . . ? C1 O1 Li3 122.1(3) . 2_675 ? Li1 O1 Li3 109.3(4) . 2_675 ? C1 O1 Li2 136.5(3) . 2_675 ? Li1 O1 Li2 83.3(3) . 2_675 ? Li3 O1 Li2 84.4(3) 2_675 2_675 ? C7 O2 Li1 139.8(4) . 2_675 ? C7 O2 Li3 110.7(3) . 2_675 ? Li1 O2 Li3 83.0(3) 2_675 2_675 ? C7 O2 Li2 111.0(3) . . ? Li1 O2 Li2 83.9(3) 2_675 . ? Li3 O2 Li2 128.9(4) 2_675 . ? C13 O3 Li1 112.2(4) . . ? C13 O3 Li3 138.0(4) . . ? Li1 O3 Li3 83.2(3) . . ? C13 O3 Li2 119.9(3) . . ? Li1 O3 Li2 113.2(4) . . ? Li3 O3 Li2 84.6(3) . . ? C31 O4 C34 107.4(5) . . ? C31 O4 Li2 130.6(5) . . ? C34 O4 Li2 121.7(5) . . ? C38 O5 C35 108.2(5) . . ? C38 O5 Li3 132.4(4) . . ? C35 O5 Li3 118.2(4) . . ? O1 C1 C6 122.4(4) . . ? O1 C1 C2 120.1(4) . . ? C6 C1 C2 117.5(4) . . ? O1 C1 Li1 39.8(3) . . ? C6 C1 Li1 121.9(4) . . ? C2 C1 Li1 105.7(3) . . ? C3 C2 C1 123.0(4) . . ? C3 C2 H1 118.5 . . ? C1 C2 H1 118.5 . . ? C4 C3 C2 118.2(4) . . ? C4 C3 C19 119.6(4) . . ? C2 C3 C19 122.2(4) . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H2 120.0 . . ? C5 C4 H2 120.0 . . ? C6 C5 C4 121.0(5) . . ? C6 C5 H3 119.5 . . ? C4 C5 H3 119.5 . . ? C5 C6 C1 120.3(4) . . ? C5 C6 H4 119.9 . . ? C1 C6 H4 119.9 . . ? O2 C7 C8 120.1(5) . . ? O2 C7 C12 122.1(4) . . ? C8 C7 C12 117.9(5) . . ? O2 C7 Li3 42.1(2) . 2_675 ? C8 C7 Li3 102.5(4) . 2_675 ? C12 C7 Li3 123.5(4) . 2_675 ? O2 C7 Li2 42.0(2) . . ? C8 C7 Li2 103.0(4) . . ? C12 C7 Li2 122.2(4) . . ? Li3 C7 Li2 80.5(3) 2_675 . ? C9 C8 C7 122.8(5) . . ? C9 C8 H5 118.6 . . ? C7 C8 H5 118.6 . . ? C10 C9 C8 117.9(5) . . ? C10 C9 C28 119.7(5) . . ? C8 C9 C28 122.4(5) . . ? C11 C10 C9 120.1(5) . . ? C11 C10 H6 119.9 . . ? C9 C10 H6 119.9 . . ? C10 C11 C12 121.5(6) . . ? C10 C11 H7 119.2 . . ? C12 C11 H7 119.2 . . ? C11 C12 C7 119.8(5) . . ? C11 C12 H8 120.1 . . ? C7 C12 H8 120.1 . . ? O3 C13 C14 120.9(4) . . ? O3 C13 C18 121.4(4) . . ? C14 C13 C18 117.7(4) . . ? O3 C13 Li1 40.5(3) . . ? C14 C13 Li1 105.0(3) . . ? C18 C13 Li1 121.4(4) . . ? C13 C14 C15 124.0(5) . . ? C13 C14 H9 118.0 . . ? C15 C14 H9 118.0 . . ? C16 C15 C14 117.3(5) . . ? C16 C15 C30 119.7(4) . . ? C14 C15 C30 123.0(5) . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H10 119.9 . . ? C15 C16 H10 119.9 . . ? C16 C17 C18 122.1(5) . . ? C16 C17 H11 119.0 . . ? C18 C17 H11 119.0 . . ? C13 C18 C17 118.7(5) . . ? C13 C18 H12 120.7 . . ? C17 C18 H12 120.7 . . ? C20 C19 C3 112.7(4) . . ? C20 C19 H13 109.1 . . ? C3 C19 H13 109.1 . . ? C20 C19 H14 109.1 . . ? C3 C19 H14 109.1 . . ? H13 C19 H14 107.8 . . ? C25 C20 C21 120.2(5) . . ? C25 C20 C19 120.0(6) . . ? C21 C20 C19 119.4(5) . . ? C20 C21 C22 119.1(5) . . ? C20 C21 C27 121.4(5) . . ? C22 C21 C27 119.2(6) . . ? C21 C22 C23 120.5(5) . . ? C21 C22 C28 120.0(5) . . ? C23 C22 C28 119.0(5) . . ? C24 C23 C22 119.8(5) . . ? C24 C23 C29 120.4(5) . . ? C22 C23 C29 119.7(5) . . ? C23 C24 C25 119.7(5) . . ? C23 C24 C30 121.3(5) . . ? C25 C24 C30 118.7(5) . . ? C20 C25 C24 120.7(5) . . ? C20 C25 C26 119.4(5) . . ? C24 C25 C26 119.7(5) . . ? C25 C26 H15 109.5 . . ? C25 C26 H16 109.5 . . ? H15 C26 H16 109.5 . . ? C25 C26 H17 109.5 . . ? H15 C26 H17 109.5 . . ? H16 C26 H17 109.5 . . ? C21 C27 H18 109.5 . . ? C21 C27 H19 109.5 . . ? H18 C27 H19 109.5 . . ? C21 C27 H20 109.5 . . ? H18 C27 H20 109.5 . . ? H19 C27 H20 109.5 . . ? C22 C28 C9 113.2(4) . . ? C22 C28 H21 108.9 . . ? C9 C28 H21 108.9 . . ? C22 C28 H22 108.9 . . ? C9 C28 H22 108.9 . . ? H21 C28 H22 107.8 . . ? C23 C29 H23 109.5 . . ? C23 C29 H24 109.5 . . ? H23 C29 H24 109.5 . . ? C23 C29 H25 109.5 . . ? H23 C29 H25 109.5 . . ? H24 C29 H25 109.5 . . ? C24 C30 C15 113.3(4) . . ? C24 C30 H26 108.9 . . ? C15 C30 H26 108.9 . . ? C24 C30 H27 108.9 . . ? C15 C30 H27 108.9 . . ? H26 C30 H27 107.7 . . ? O4 C31 C32 108.3(6) . . ? O4 C31 H28 110.0 . . ? C32 C31 H28 110.0 . . ? O4 C31 H29 110.0 . . ? C32 C31 H29 110.0 . . ? H28 C31 H29 108.4 . . ? C31 C32 C33 105.4(6) . . ? C31 C32 H30 110.7 . . ? C33 C32 H30 110.7 . . ? C31 C32 H31 110.7 . . ? C33 C32 H31 110.7 . . ? H30 C32 H31 108.8 . . ? C34 C33 C32 106.8(7) . . ? C34 C33 H32 110.4 . . ? C32 C33 H32 110.4 . . ? C34 C33 H33 110.4 . . ? C32 C33 H33 110.4 . . ? H32 C33 H33 108.6 . . ? C33 C34 O4 109.3(8) . . ? C33 C34 H34 109.8 . . ? O4 C34 H34 109.8 . . ? C33 C34 H35 109.8 . . ? O4 C34 H35 109.8 . . ? H34 C34 H35 108.3 . . ? O5 C35 C36 105.0(6) . . ? O5 C35 H36 110.7 . . ? C36 C35 H36 110.7 . . ? O5 C35 H37 110.7 . . ? C36 C35 H37 110.7 . . ? H36 C35 H37 108.8 . . ? C37 C36 C35 102.7(7) . . ? C37 C36 H38 111.2 . . ? C35 C36 H38 111.2 . . ? C37 C36 H39 111.2 . . ? C35 C36 H39 111.2 . . ? H38 C36 H39 109.1 . . ? C38 C37 C36 108.1(7) . . ? C38 C37 H40 110.1 . . ? C36 C37 H40 110.1 . . ? C38 C37 H41 110.1 . . ? C36 C37 H41 110.1 . . ? H40 C37 H41 108.4 . . ? C37 C38 O5 109.2(7) . . ? C37 C38 H42 109.8 . . ? O5 C38 H42 109.8 . . ? C37 C38 H43 109.8 . . ? O5 C38 H43 109.8 . . ? H42 C38 H43 108.3 . . ? C40 C39 C44 120.2(6) . . ? C40 C39 H44 119.9 . . ? C44 C39 H44 119.9 . . ? C41 C40 C39 120.4(6) . . ? C41 C40 H45 119.8 . . ? C39 C40 H45 119.8 . . ? C42 C41 C40 120.5(7) . . ? C42 C41 H46 119.8 . . ? C40 C41 H46 119.8 . . ? C41 C42 C43 119.4(6) . . ? C41 C42 H47 120.3 . . ? C43 C42 H47 120.3 . . ? C44 C43 C42 121.1(6) . . ? C44 C43 H48 119.5 . . ? C42 C43 H48 119.5 . . ? C43 C44 C39 118.5(6) . . ? C43 C44 H49 120.7 . . ? C39 C44 H49 120.7 . . ? C46 C45 C47 119.1(7) . 2_566 ? C46 C45 H51 120.4 . . ? C47 C45 H51 120.4 2_566 . ? C47 C46 C45 121.6(7) . . ? C47 C46 H50 119.2 . . ? C45 C46 H50 119.2 . . ? C46 C47 C45 119.2(8) . 2_566 ? C46 C47 H52 120.4 . . ? C45 C47 H52 120.4 2_566 . ? O2 Li1 O3 98.9(4) 2_675 . ? O2 Li1 O1 98.5(4) 2_675 . ? O3 Li1 O1 134.3(6) . . ? O2 Li1 Li3 49.9(3) 2_675 . ? O3 Li1 Li3 49.2(3) . . ? O1 Li1 Li3 128.3(5) . . ? O2 Li1 Li2 49.5(3) 2_675 2_675 ? O3 Li1 Li2 128.6(5) . 2_675 ? O1 Li1 Li2 49.1(2) . 2_675 ? Li3 Li1 Li2 87.7(3) . 2_675 ? O2 Li1 C13 117.6(4) 2_675 . ? O3 Li1 C13 27.34(17) . . ? O1 Li1 C13 138.5(4) . . ? Li3 Li1 C13 71.5(3) . . ? Li2 Li1 C13 156.0(4) 2_675 . ? O2 Li1 C1 116.4(4) 2_675 . ? O3 Li1 C1 138.9(4) . . ? O1 Li1 C1 26.57(17) . . ? Li3 Li1 C1 154.9(4) . . ? Li2 Li1 C1 70.5(3) 2_675 . ? C13 Li1 C1 126.1(3) . . ? O2 Li1 Li3 94.1(4) 2_675 2_675 ? O3 Li1 Li3 101.2(4) . 2_675 ? O1 Li1 Li3 35.6(3) . 2_675 ? Li3 Li1 Li3 99.1(4) . 2_675 ? Li2 Li1 Li3 53.4(3) 2_675 2_675 ? C13 Li1 Li3 116.9(4) . 2_675 ? C1 Li1 Li3 58.1(2) . 2_675 ? O2 Li1 Li2 94.5(4) 2_675 . ? O3 Li1 Li2 33.9(3) . . ? O1 Li1 Li2 102.9(4) . . ? Li3 Li1 Li2 52.6(3) . . ? Li2 Li1 Li2 100.8(3) 2_675 . ? C13 Li1 Li2 57.1(2) . . ? C1 Li1 Li2 118.1(4) . . ? Li3 Li1 Li2 68.0(3) 2_675 . ? O4 Li2 O3 111.7(4) . . ? O4 Li2 O1 118.2(4) . 2_675 ? O3 Li2 O1 95.0(3) . 2_675 ? O4 Li2 O2 121.9(4) . . ? O3 Li2 O2 111.9(4) . . ? O1 Li2 O2 94.0(3) 2_675 . ? O4 Li2 Li1 139.7(5) . 2_675 ? O3 Li2 Li1 107.5(4) . 2_675 ? O1 Li2 Li1 47.6(2) 2_675 2_675 ? O2 Li2 Li1 46.6(3) . 2_675 ? O4 Li2 Li3 127.8(4) . . ? O3 Li2 Li3 47.7(3) . . ? O1 Li2 Li3 47.4(2) 2_675 . ? O2 Li2 Li3 109.9(3) . . ? Li1 Li2 Li3 74.4(3) 2_675 . ? O4 Li2 C7 95.2(3) . . ? O3 Li2 C7 125.0(4) . . ? O1 Li2 C7 113.6(4) 2_675 . ? O2 Li2 C7 27.06(16) . . ? Li1 Li2 C7 69.3(3) 2_675 . ? Li3 Li2 C7 136.9(3) . . ? O4 Li2 Li1 141.1(4) . . ? O3 Li2 Li1 32.9(2) . . ? O1 Li2 Li1 88.4(3) 2_675 . ? O2 Li2 Li1 80.3(3) . . ? Li1 Li2 Li1 79.2(3) 2_675 . ? Li3 Li2 Li1 50.7(3) . . ? C7 Li2 Li1 99.4(3) . . ? O1 Li3 O3 95.9(4) 2_675 . ? O1 Li3 O2 115.8(4) 2_675 2_675 ? O3 Li3 O2 94.6(3) . 2_675 ? O1 Li3 O5 111.9(4) 2_675 . ? O3 Li3 O5 116.4(4) . . ? O2 Li3 O5 118.7(4) 2_675 . ? O1 Li3 Li1 111.0(4) 2_675 . ? O3 Li3 Li1 47.6(2) . . ? O2 Li3 Li1 47.1(3) 2_675 . ? O5 Li3 Li1 135.6(5) . . ? O1 Li3 Li2 48.2(3) 2_675 . ? O3 Li3 Li2 47.7(3) . . ? O2 Li3 Li2 113.4(4) 2_675 . ? O5 Li3 Li2 126.8(4) . . ? Li1 Li3 Li2 76.7(3) . . ? O1 Li3 C7 128.1(4) 2_675 2_675 ? O3 Li3 C7 114.0(4) . 2_675 ? O2 Li3 C7 27.22(16) 2_675 2_675 ? O5 Li3 C7 92.2(3) . 2_675 ? Li1 Li3 C7 69.8(3) . 2_675 ? Li2 Li3 C7 140.6(4) . 2_675 ? O1 Li3 Li1 35.1(2) 2_675 2_675 ? O3 Li3 Li1 89.0(3) . 2_675 ? O2 Li3 Li1 82.2(3) 2_675 2_675 ? O5 Li3 Li1 143.4(4) . 2_675 ? Li1 Li3 Li1 80.9(4) . 2_675 ? Li2 Li3 Li1 52.2(3) . 2_675 ? C7 Li3 Li1 101.3(3) 2_675 2_675 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.288 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.049