Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Malcolm H. Chisholm' 'Chu-Chieh Lin' 'Judith C. Gallucci' 'Bao-Tsan Ko' _publ_contact_author_name 'Prof Malcolm Chisholm' _publ_contact_author_address ; Department of Chemistry The Ohio State University 100 West 18th Avenue Columbus Ohio 43210-1185 ; _publ_contact_author_email 'CHISHOLM@CHEMISTRY.OHIO-STATE.EDU' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Binolate Complexes of Lithium, Zinc, Aluminu, and titanium: [(mu3,mu3-Biphenolate)2Li4("BuLi)4]m (mu2, mu2-Biphenolate)Li2(me3-OCH(iPr)2)2-Li2L2], [(mu2, mu2-Biphenolate)Zn(me-OCH(iPr)2)2Zn2Et2], [(mu2-Biphenolate)AIMe(mu2-OCH(iPr)2)AIMe2], and [(Biphenolate) Ti2Cl6] (where Biphenolate = racemic 5, 5', 6, 6'tetramethyl-3,3'-di-tert-butyl-1, 1'-bi-2-phenolte, L = Tetrahydrofuran or Cyclohexene Oxide). Preparations, Structures and Studies of Lactide Polymerization ; data_Chisholm996 _database_code_CSD 185856 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H50 Li4 O2' _chemical_formula_weight 494.48 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.0434(2) _cell_length_b 16.0320(2) _cell_length_c 20.3345(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.116(1) _cell_angle_gamma 90.00 _cell_volume 6244.81(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_method ? _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ;The molecule is a dimer of lithium clusters and it contains a crystallographic two-fold axis. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50528 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7168 _reflns_number_observed 5288 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). The two hydrogen atoms bonded to C25 and to C29 were refined isotropically. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+4.0730P] 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 7168 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_obs 0.0499 _refine_ls_wR_factor_all 0.1394 _refine_ls_wR_factor_obs 0.1247 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max 0.024 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.277 _refine_diff_density_min -0.230 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O -0.07801(5) 0.38328(6) 0.29804(5) 0.0231(2) Uani 1 d . . O2 O 0.09835(5) 0.25602(6) 0.31133(5) 0.0220(2) Uani 1 d . . C1 C 0.03388(7) 0.36977(8) 0.37995(7) 0.0215(3) Uani 1 d . . C2 C 0.09517(7) 0.40416(9) 0.42481(7) 0.0224(3) Uani 1 d . . C3 C 0.10160(7) 0.49110(9) 0.43066(7) 0.0244(3) Uani 1 d . . C4 C 0.04472(7) 0.53946(9) 0.39564(7) 0.0249(3) Uani 1 d . . H4 H 0.04861(7) 0.59820(9) 0.40174(7) 0.030 Uiso 1 calc R . C5 C -0.01763(7) 0.50823(9) 0.35224(7) 0.0232(3) Uani 1 d . . C6 C -0.02194(7) 0.42066(9) 0.34134(7) 0.0211(3) Uani 1 d . . C7 C 0.02376(7) 0.27679(8) 0.38166(7) 0.0203(3) Uani 1 d . . C8 C -0.01711(7) 0.24602(9) 0.42247(7) 0.0228(3) Uani 1 d . . C9 C -0.02097(7) 0.16003(9) 0.43162(7) 0.0246(3) Uani 1 d . . C10 C 0.01858(7) 0.10826(9) 0.40313(7) 0.0243(3) Uani 1 d . . H10 H 0.01676(7) 0.04999(9) 0.41094(7) 0.029 Uiso 1 calc R . C11 C 0.06083(7) 0.13555(9) 0.36386(7) 0.0217(3) Uani 1 d . . C12 C 0.06135(7) 0.22247(9) 0.35035(7) 0.0199(3) Uani 1 d . . C13 C 0.15171(8) 0.34851(9) 0.46890(7) 0.0284(3) Uani 1 d . . H13A H 0.1469(3) 0.3454(5) 0.5154(2) 0.043 Uiso 1 calc R . H13B H 0.19758(8) 0.3716(4) 0.4711(4) 0.043 Uiso 1 calc R . H13C H 0.1473(3) 0.2925(2) 0.4488(3) 0.043 Uiso 1 calc R . C14 C 0.16728(8) 0.53302(10) 0.47449(8) 0.0317(3) Uani 1 d . . H14A H 0.20611(15) 0.5203(6) 0.4560(3) 0.048 Uiso 1 calc R . H14B H 0.1782(3) 0.5124(5) 0.52185(15) 0.048 Uiso 1 calc R . H14C H 0.1601(2) 0.59350(11) 0.4740(5) 0.048 Uiso 1 calc R . C15 C -0.07993(8) 0.56719(9) 0.32212(8) 0.0286(3) Uani 1 d . . C16 C -0.06059(10) 0.65918(10) 0.33788(11) 0.0464(5) Uani 1 d . . H16A H -0.0454(7) 0.6677(2) 0.38782(11) 0.070 Uiso 1 calc R . H16B H -0.1014(2) 0.69423(12) 0.3171(6) 0.070 Uiso 1 calc R . H16C H -0.0227(5) 0.6743(2) 0.3188(6) 0.070 Uiso 1 calc R . C17 C -0.13676(9) 0.54629(12) 0.35624(10) 0.0447(4) Uani 1 d . . H17A H -0.1191(3) 0.5572(8) 0.40577(15) 0.067 Uiso 1 calc R . H17B H -0.1496(5) 0.4873(2) 0.3486(6) 0.067 Uiso 1 calc R . H17C H -0.1779(3) 0.5810(6) 0.3361(5) 0.067 Uiso 1 calc R . C18 C -0.10919(9) 0.56001(11) 0.24391(8) 0.0381(4) Uani 1 d . . H18A H -0.07110(13) 0.5655(7) 0.22309(9) 0.057 Uiso 1 calc R . H18B H -0.1435(5) 0.6043(5) 0.22658(11) 0.057 Uiso 1 calc R . H18C H -0.1317(5) 0.5055(3) 0.23192(9) 0.057 Uiso 1 calc R . C19 C -0.05424(8) 0.30539(10) 0.45768(8) 0.0300(3) Uani 1 d . . H19A H -0.10339(15) 0.3099(5) 0.4305(3) 0.045 Uiso 1 calc R . H19B H -0.0322(4) 0.3605(2) 0.4617(5) 0.045 Uiso 1 calc R . H19C H -0.0512(5) 0.2842(4) 0.5037(2) 0.045 Uiso 1 calc R . C20 C -0.06491(8) 0.12285(10) 0.47317(9) 0.0343(4) Uani 1 d . . H20A H -0.11406(11) 0.1371(6) 0.4517(3) 0.051 Uiso 1 calc R . H20B H -0.0496(4) 0.1452(5) 0.5201(2) 0.051 Uiso 1 calc R . H20C H -0.0595(5) 0.06206(12) 0.4747(5) 0.051 Uiso 1 calc R . C21 C 0.10962(7) 0.07334(9) 0.34305(8) 0.0271(3) Uani 1 d . . C22 C 0.09489(10) -0.01746(10) 0.35867(11) 0.0445(5) Uani 1 d . . H22A H 0.1026(7) -0.0241(2) 0.40825(13) 0.067 Uiso 1 calc R . H22B H 0.1263(5) -0.05475(12) 0.3437(6) 0.067 Uiso 1 calc R . H22C H 0.0464(2) -0.0315(3) 0.3340(5) 0.067 Uiso 1 calc R . C23 C 0.10369(8) 0.07605(10) 0.26608(8) 0.0318(3) Uani 1 d . . H23A H 0.1338(4) 0.0331(5) 0.25564(13) 0.048 Uiso 1 calc R . H23B H 0.1183(5) 0.1310(2) 0.25441(14) 0.048 Uiso 1 calc R . H23C H 0.05517(14) 0.0658(7) 0.23906(8) 0.048 Uiso 1 calc R . C24 C 0.18482(8) 0.09292(12) 0.38621(9) 0.0386(4) Uani 1 d . . H24A H 0.1896(2) 0.0834(7) 0.43498(10) 0.058 Uiso 1 calc R . H24B H 0.1956(2) 0.1513(2) 0.3793(5) 0.058 Uiso 1 calc R . H24C H 0.21725(9) 0.0565(5) 0.3718(4) 0.058 Uiso 1 calc R . C25 C 0.22848(8) 0.38673(10) 0.32874(8) 0.0284(3) Uani 1 d . . H25A H 0.2187(9) 0.4264(11) 0.3619(9) 0.035(4) Uiso 1 d . . H25B H 0.2498(10) 0.4231(12) 0.3007(10) 0.051(5) Uiso 1 d . . C26 C 0.28581(8) 0.32714(10) 0.37158(8) 0.0322(4) Uani 1 d . . H26A H 0.26549(8) 0.29462(10) 0.40238(8) 0.039 Uiso 1 calc R . H26B H 0.29719(8) 0.28710(10) 0.33940(8) 0.039 Uiso 1 calc R . C27 C 0.35424(9) 0.36526(12) 0.41564(9) 0.0420(4) Uani 1 d . . H27A H 0.34374(9) 0.40761(12) 0.44661(9) 0.050 Uiso 1 calc R . H27B H 0.38280(9) 0.32105(12) 0.44469(9) 0.050 Uiso 1 calc R . C28 C 0.39591(10) 0.40541(14) 0.37364(12) 0.0578(6) Uani 1 d . . H28A H 0.4414(3) 0.4230(9) 0.40406(15) 0.087 Uiso 1 calc R . H28B H 0.3707(4) 0.4542(6) 0.3496(6) 0.087 Uiso 1 calc R . H28C H 0.4029(7) 0.3653(3) 0.3399(5) 0.087 Uiso 1 calc R . C29 C 0.19273(8) 0.23679(10) 0.20150(8) 0.0276(3) Uani 1 d . . H29A H 0.1588(9) 0.2064(11) 0.1633(9) 0.035(4) Uiso 1 d . . H29B H 0.2211(9) 0.1899(11) 0.2312(9) 0.040(5) Uiso 1 d . . C30 C 0.24244(8) 0.28226(10) 0.16816(8) 0.0313(3) Uani 1 d . . H30A H 0.21873(8) 0.33328(10) 0.14537(8) 0.038 Uiso 1 calc R . H30B H 0.28420(8) 0.30018(10) 0.20524(8) 0.038 Uiso 1 calc R . C31 C 0.26678(8) 0.23246(10) 0.11555(8) 0.0319(3) Uani 1 d . . H31A H 0.28762(8) 0.17947(10) 0.13708(8) 0.038 Uiso 1 calc R . H31B H 0.22554(8) 0.21828(10) 0.07646(8) 0.038 Uiso 1 calc R . C32 C 0.31966(10) 0.27718(12) 0.08784(10) 0.0474(5) Uani 1 d . . H32A H 0.3313(5) 0.2420(4) 0.0534(5) 0.071 Uiso 1 calc R . H32B H 0.3620(3) 0.2884(8) 0.1257(2) 0.071 Uiso 1 calc R . H32C H 0.2998(3) 0.3300(4) 0.0666(6) 0.071 Uiso 1 calc R . Li1 Li 0.10686(13) 0.3782(2) 0.30433(13) 0.0276(5) Uani 1 d . . Li2 Li 0.08025(13) 0.2609(2) 0.21005(12) 0.0281(5) Uani 1 d . . Li3 Li 0.19091(12) 0.2596(2) 0.30696(13) 0.0289(5) Uani 1 d . . Li4 Li -0.17501(12) 0.3676(2) 0.28065(13) 0.0293(5) Uani 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 0.0212(5) 0.0247(5) 0.0226(5) -0.0025(4) 0.0049(4) -0.0004(4) O2 0.0215(5) 0.0239(5) 0.0224(5) 0.0012(4) 0.0093(4) -0.0007(4) C1 0.0240(7) 0.0217(7) 0.0199(7) -0.0017(5) 0.0084(6) -0.0004(5) C2 0.0230(7) 0.0261(7) 0.0189(7) -0.0001(6) 0.0074(5) 0.0001(6) C3 0.0260(7) 0.0260(7) 0.0214(7) -0.0032(6) 0.0073(6) -0.0032(6) C4 0.0316(8) 0.0198(7) 0.0252(7) -0.0026(6) 0.0115(6) -0.0012(6) C5 0.0268(7) 0.0236(7) 0.0216(7) -0.0003(6) 0.0108(6) 0.0018(6) C6 0.0211(7) 0.0256(7) 0.0183(6) -0.0018(6) 0.0084(5) 0.0005(5) C7 0.0185(6) 0.0224(7) 0.0187(6) -0.0003(5) 0.0032(5) 0.0000(5) C8 0.0211(7) 0.0276(7) 0.0195(7) 0.0001(6) 0.0054(5) 0.0010(6) C9 0.0216(7) 0.0298(8) 0.0225(7) 0.0042(6) 0.0065(6) -0.0002(6) C10 0.0232(7) 0.0220(7) 0.0263(7) 0.0041(6) 0.0054(6) -0.0003(6) C11 0.0186(6) 0.0240(7) 0.0207(7) 0.0007(5) 0.0028(5) 0.0009(5) C12 0.0171(6) 0.0240(7) 0.0170(6) 0.0009(5) 0.0026(5) -0.0010(5) C13 0.0279(8) 0.0299(8) 0.0246(7) -0.0014(6) 0.0034(6) -0.0001(6) C14 0.0322(8) 0.0294(8) 0.0311(8) -0.0034(7) 0.0056(7) -0.0060(6) C15 0.0283(8) 0.0258(8) 0.0323(8) -0.0005(6) 0.0100(6) 0.0058(6) C16 0.0441(10) 0.0276(9) 0.0608(12) -0.0022(8) 0.0052(9) 0.0111(8) C17 0.0401(10) 0.0475(11) 0.0545(11) 0.0024(9) 0.0263(9) 0.0119(8) C18 0.0390(9) 0.0377(9) 0.0342(9) 0.0069(7) 0.0057(7) 0.0103(7) C19 0.0325(8) 0.0332(8) 0.0279(8) -0.0015(6) 0.0144(6) 0.0022(6) C20 0.0349(9) 0.0347(9) 0.0389(9) 0.0100(7) 0.0195(7) 0.0024(7) C21 0.0279(8) 0.0233(7) 0.0321(8) 0.0041(6) 0.0119(6) 0.0045(6) C22 0.0550(11) 0.0251(8) 0.0643(12) 0.0093(8) 0.0345(10) 0.0107(8) C23 0.0378(9) 0.0268(8) 0.0335(8) -0.0042(6) 0.0145(7) 0.0023(7) C24 0.0281(8) 0.0496(11) 0.0379(9) 0.0059(8) 0.0093(7) 0.0114(7) C25 0.0265(8) 0.0306(8) 0.0279(8) 0.0014(7) 0.0077(6) -0.0024(6) C26 0.0261(8) 0.0346(8) 0.0339(8) 0.0047(7) 0.0056(6) -0.0036(6) C27 0.0310(9) 0.0469(10) 0.0394(9) 0.0047(8) -0.0028(7) -0.0055(8) C28 0.0344(10) 0.0592(13) 0.0751(15) 0.0115(11) 0.0086(10) -0.0158(9) C29 0.0260(7) 0.0302(8) 0.0271(8) 0.0020(7) 0.0089(6) 0.0012(6) C30 0.0313(8) 0.0327(8) 0.0326(8) -0.0025(7) 0.0136(7) -0.0003(6) C31 0.0358(8) 0.0315(8) 0.0324(8) -0.0014(7) 0.0161(7) -0.0006(7) C32 0.0535(11) 0.0475(11) 0.0538(11) -0.0122(9) 0.0355(10) -0.0092(9) Li1 0.0280(13) 0.0291(13) 0.0264(12) -0.0006(10) 0.0090(10) -0.0005(10) Li2 0.0274(13) 0.0292(13) 0.0260(12) 0.0001(10) 0.0054(10) 0.0007(10) Li3 0.0232(12) 0.0338(14) 0.0304(13) 0.0019(11) 0.0091(10) 0.0003(10) Li4 0.0235(12) 0.0348(14) 0.0305(13) -0.0017(11) 0.0090(10) 0.0003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.347(2) . ? O1 Li4 1.888(3) . ? O1 Li2 1.967(3) 2 ? O1 Li1 1.992(3) 2 ? O2 C12 1.347(2) . ? O2 Li3 1.884(3) . ? O2 Li1 1.975(3) . ? O2 Li2 1.985(3) . ? C1 C2 1.409(2) . ? C1 C6 1.420(2) . ? C1 C7 1.506(2) . ? C1 Li1 2.418(3) . ? C2 C3 1.402(2) . ? C2 C13 1.512(2) . ? C2 Li1 2.563(3) . ? C3 C4 1.389(2) . ? C3 C14 1.513(2) . ? C4 C5 1.394(2) . ? C4 H4 0.95 . ? C5 C6 1.420(2) . ? C5 C15 1.542(2) . ? C7 C8 1.415(2) . ? C7 C12 1.419(2) . ? C7 Li2 2.366(3) 2 ? C8 C9 1.396(2) . ? C8 C19 1.512(2) . ? C8 Li2 2.629(3) 2 ? C9 C10 1.387(2) . ? C9 C20 1.511(2) . ? C10 C11 1.394(2) . ? C10 H10 0.95 . ? C11 C12 1.421(2) . ? C11 C21 1.541(2) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C18 1.529(2) . ? C15 C16 1.535(2) . ? C15 C17 1.535(2) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C23 1.535(2) . ? C21 C24 1.537(2) . ? C21 C22 1.537(2) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.550(2) . ? C25 Li3 2.172(3) . ? C25 Li4 2.188(3) 2 ? C25 Li1 2.344(3) . ? C25 H25A 0.99(2) . ? C25 H25B 1.00(2) . ? C26 C27 1.528(2) . ? C26 Li3 2.246(3) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.504(3) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C30 1.543(2) . ? C29 Li4 2.175(3) 2 ? C29 Li3 2.186(3) . ? C29 Li2 2.344(3) . ? C29 H29A 1.00(2) . ? C29 H29B 1.03(2) . ? C30 C31 1.525(2) . ? C30 Li4 2.368(3) 2 ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.519(2) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? Li1 O1 1.992(3) 2 ? Li1 Li4 2.504(3) 2 ? Li1 Li3 2.530(3) . ? Li1 Li2 2.625(3) . ? Li2 O1 1.967(3) 2 ? Li2 C7 2.367(3) 2 ? Li2 Li3 2.496(3) . ? Li2 Li4 2.521(4) 2 ? Li2 C8 2.629(3) 2 ? Li3 Li4 2.436(4) 2 ? Li4 C29 2.175(3) 2 ? Li4 C25 2.188(3) 2 ? Li4 C30 2.368(3) 2 ? Li4 Li3 2.436(4) 2 ? Li4 Li1 2.504(3) 2 ? Li4 Li2 2.521(4) 2 ? 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 C6 O1 Li4 142.83(11) . . ? C6 O1 Li2 119.48(11) . 2 ? Li4 O1 Li2 81.64(11) . 2 ? C6 O1 Li1 129.13(11) . 2 ? Li4 O1 Li1 80.36(11) . 2 ? Li2 O1 Li1 83.06(11) 2 2 ? C12 O2 Li3 139.49(11) . . ? C12 O2 Li1 120.84(11) . . ? Li3 O2 Li1 81.90(11) . . ? C12 O2 Li2 131.51(11) . . ? Li3 O2 Li2 80.31(11) . . ? Li1 O2 Li2 83.05(11) . . ? C2 C1 C6 121.87(12) . . ? C2 C1 C7 118.03(12) . . ? C6 C1 C7 119.46(12) . . ? C2 C1 Li1 79.32(10) . . ? C6 C1 Li1 98.17(10) . . ? C7 C1 Li1 100.40(10) . . ? C3 C2 C1 119.01(13) . . ? C3 C2 C13 120.15(12) . . ? C1 C2 C13 120.76(12) . . ? C3 C2 Li1 102.17(11) . . ? C1 C2 Li1 67.98(9) . . ? C13 C2 Li1 101.97(10) . . ? C4 C3 C2 118.05(13) . . ? C4 C3 C14 119.64(13) . . ? C2 C3 C14 122.29(13) . . ? C3 C4 C5 124.87(13) . . ? C3 C4 H4 117.56(8) . . ? C5 C4 H4 117.56(8) . . ? C4 C5 C6 117.13(13) . . ? C4 C5 C15 120.12(12) . . ? C6 C5 C15 122.63(12) . . ? O1 C6 C1 118.41(12) . . ? O1 C6 C5 122.85(12) . . ? C1 C6 C5 118.68(12) . . ? C8 C7 C12 121.64(12) . . ? C8 C7 C1 117.61(12) . . ? C12 C7 C1 120.27(12) . . ? C8 C7 Li2 84.09(10) . 2 ? C12 C7 Li2 92.38(10) . 2 ? C1 C7 Li2 100.45(10) . 2 ? C9 C8 C7 119.11(12) . . ? C9 C8 C19 120.27(12) . . ? C7 C8 C19 120.59(13) . . ? C9 C8 Li2 101.39(11) . 2 ? C7 C8 Li2 63.54(9) . 2 ? C19 C8 Li2 105.81(10) . 2 ? C10 C9 C8 118.32(13) . . ? C10 C9 C20 119.76(13) . . ? C8 C9 C20 121.89(13) . . ? C9 C10 C11 124.72(13) . . ? C9 C10 H10 117.64(8) . . ? C11 C10 H10 117.64(8) . . ? C10 C11 C12 117.31(12) . . ? C10 C11 C21 119.72(12) . . ? C12 C11 C21 122.70(12) . . ? O2 C12 C7 118.44(12) . . ? O2 C12 C11 122.83(12) . . ? C7 C12 C11 118.68(12) . . ? C2 C13 H13A 109.47(8) . . ? C2 C13 H13B 109.47(8) . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.47(8) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.47(8) . . ? C3 C14 H14B 109.47(8) . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.47(8) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C16 106.60(14) . . ? C18 C15 C17 110.20(14) . . ? C16 C15 C17 106.90(14) . . ? C18 C15 C5 112.64(12) . . ? C16 C15 C5 112.39(13) . . ? C17 C15 C5 107.97(13) . . ? C15 C16 H16A 109.47(10) . . ? C15 C16 H16B 109.47(9) . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.47(10) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.47(9) . . ? C15 C17 H17B 109.47(9) . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.47(9) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.47(9) . . ? C15 C18 H18B 109.47(8) . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.47(9) . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 H19A 109.47(8) . . ? C8 C19 H19B 109.47(8) . . ? H19A C19 H19B 109.5 . . ? C8 C19 H19C 109.47(8) . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C9 C20 H20A 109.47(8) . . ? C9 C20 H20B 109.47(8) . . ? H20A C20 H20B 109.5 . . ? C9 C20 H20C 109.47(8) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 C21 C24 110.18(12) . . ? C23 C21 C22 105.99(13) . . ? C24 C21 C22 106.93(13) . . ? C23 C21 C11 113.38(12) . . ? C24 C21 C11 107.83(12) . . ? C22 C21 C11 112.36(12) . . ? C21 C22 H22A 109.47(10) . . ? C21 C22 H22B 109.47(8) . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.47(9) . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.47(8) . . ? C21 C23 H23B 109.47(8) . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.47(8) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.47(8) . . ? C21 C24 H24B 109.47(9) . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.47(8) . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 Li3 72.03(10) . . ? C26 C25 Li4 123.03(13) . 2 ? Li3 C25 Li4 67.94(11) . 2 ? C26 C25 Li1 129.47(12) . . ? Li3 C25 Li1 68.01(10) . . ? Li4 C25 Li1 66.97(10) 2 . ? C26 C25 H25A 106.1(10) . . ? Li3 C25 H25A 128.0(10) . . ? Li4 C25 H25A 130.4(10) 2 . ? Li1 C25 H25A 77.2(10) . . ? C26 C25 H25B 108.1(11) . . ? Li3 C25 H25B 127.8(11) . . ? Li4 C25 H25B 70.3(11) 2 . ? Li1 C25 H25B 120.5(11) . . ? H25A C25 H25B 102.7(15) . . ? C27 C26 C25 118.17(14) . . ? C27 C26 Li3 174.48(14) . . ? C25 C26 Li3 66.93(10) . . ? C27 C26 H26A 107.77(9) . . ? C25 C26 H26A 107.77(8) . . ? Li3 C26 H26A 71.40(8) . . ? C27 C26 H26B 107.77(10) . . ? C25 C26 H26B 107.77(9) . . ? Li3 C26 H26B 67.74(8) . . ? H26A C26 H26B 107.1 . . ? C28 C27 C26 113.0(2) . . ? C28 C27 H27A 108.98(12) . . ? C26 C27 H27A 108.98(10) . . ? C28 C27 H27B 108.98(11) . . ? C26 C27 H27B 108.98(9) . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.47(10) . . ? C27 C28 H28B 109.47(11) . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.47(12) . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Li4 77.07(11) . 2 ? C30 C29 Li3 123.44(12) . . ? Li4 C29 Li3 67.93(10) 2 . ? C30 C29 Li2 135.56(12) . . ? Li4 C29 Li2 67.69(10) 2 . ? Li3 C29 Li2 66.77(10) . . ? C30 C29 H29A 105.6(10) . . ? Li4 C29 H29A 119.6(10) 2 . ? Li3 C29 H29A 130.0(10) . . ? Li2 C29 H29A 71.9(10) . . ? C30 C29 H29B 106.7(10) . . ? Li4 C29 H29B 134.3(10) 2 . ? Li3 C29 H29B 73.3(10) . . ? Li2 C29 H29B 117.2(10) . . ? H29A C29 H29B 103.5(14) . . ? C31 C30 C29 116.23(13) . . ? C31 C30 Li4 162.20(13) . 2 ? C29 C30 Li4 63.51(10) . 2 ? C31 C30 H30A 108.23(9) . . ? C29 C30 H30A 108.23(8) . . ? Li4 C30 H30A 58.07(7) 2 . ? C31 C30 H30B 108.23(9) . . ? C29 C30 H30B 108.23(8) . . ? Li4 C30 H30B 87.79(7) 2 . ? H30A C30 H30B 107.4 . . ? C32 C31 C30 114.54(13) . . ? C32 C31 H31A 108.63(10) . . ? C30 C31 H31A 108.63(9) . . ? C32 C31 H31B 108.63(10) . . ? C30 C31 H31B 108.63(9) . . ? H31A C31 H31B 107.6 . . ? C31 C32 H32A 109.47(9) . . ? C31 C32 H32B 109.47(10) . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.47(10) . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 Li1 O1 96.40(11) . 2 ? O2 Li1 C25 98.58(11) . . ? O1 Li1 C25 100.54(11) 2 . ? O2 Li1 C1 79.49(9) . . ? O1 Li1 C1 128.55(12) 2 . ? C25 Li1 C1 130.89(12) . . ? O2 Li1 Li4 93.36(11) . 2 ? O1 Li1 Li4 48.01(8) 2 2 ? C25 Li1 Li4 53.53(9) . 2 ? C1 Li1 Li4 171.92(13) . 2 ? O2 Li1 Li3 47.51(8) . . ? O1 Li1 Li3 92.27(11) 2 . ? C25 Li1 Li3 52.77(9) . . ? C1 Li1 Li3 117.93(12) . . ? Li4 Li1 Li3 57.89(10) 2 . ? O2 Li1 C2 93.34(10) . . ? O1 Li1 C2 155.84(13) 2 . ? C25 Li1 C2 99.79(10) . . ? C1 Li1 C2 32.70(5) . . ? Li4 Li1 C2 153.21(13) 2 . ? Li3 Li1 C2 110.46(11) . . ? O2 Li1 Li2 48.64(8) . . ? O1 Li1 Li2 48.08(8) 2 . ? C25 Li1 Li2 99.88(11) . . ? C1 Li1 Li2 113.18(11) . . ? Li4 Li1 Li2 58.82(10) 2 . ? Li3 Li1 Li2 57.89(9) . . ? C2 Li1 Li2 139.33(12) . . ? O2 Li1 H25A 112.5(4) . . ? O1 Li1 H25A 116.8(4) 2 . ? C25 Li1 H25A 24.4(4) . . ? C1 Li1 H25A 111.8(5) . . ? Li4 Li1 H25A 74.4(5) 2 . ? Li3 Li1 H25A 72.7(4) . . ? C2 Li1 H25A 79.1(5) . . ? Li2 Li1 H25A 124.2(5) . . ? O1 Li2 O2 96.85(11) 2 . ? O1 Li2 C29 99.05(11) 2 . ? O2 Li2 C29 100.62(11) . . ? O1 Li2 C7 80.44(9) 2 2 ? O2 Li2 C7 132.18(13) . 2 ? C29 Li2 C7 127.07(12) . 2 ? O1 Li2 Li3 93.88(11) 2 . ? O2 Li2 Li3 48.08(8) . . ? C29 Li2 Li3 53.60(9) . . ? C7 Li2 Li3 174.32(13) 2 . ? O1 Li2 Li4 47.81(8) 2 2 ? O2 Li2 Li4 92.61(11) . 2 ? C29 Li2 Li4 52.96(9) . 2 ? C7 Li2 Li4 117.13(12) 2 2 ? Li3 Li2 Li4 58.11(10) . 2 ? O1 Li2 Li1 48.87(8) 2 . ? O2 Li2 Li1 48.31(8) . . ? C29 Li2 Li1 100.33(11) . . ? C7 Li2 Li1 116.18(12) 2 . ? Li3 Li2 Li1 59.15(9) . . ? Li4 Li2 Li1 58.20(9) 2 . ? O1 Li2 C8 90.73(10) 2 2 ? O2 Li2 C8 161.03(13) . 2 ? C29 Li2 C8 95.29(10) . 2 ? C7 Li2 C8 32.38(5) 2 2 ? Li3 Li2 C8 148.89(12) . 2 ? Li4 Li2 C8 105.27(11) 2 2 ? Li1 Li2 C8 138.31(12) . 2 ? O1 Li2 H29A 110.8(5) 2 . ? O2 Li2 H29A 119.2(5) . . ? C29 Li2 H29A 24.9(5) . . ? C7 Li2 H29A 105.9(5) 2 . ? Li3 Li2 H29A 76.1(5) . . ? Li4 Li2 H29A 71.8(5) 2 . ? Li1 Li2 H29A 124.9(5) . . ? C8 Li2 H29A 73.5(5) 2 . ? O2 Li3 C25 107.83(13) . . ? O2 Li3 C29 110.00(13) . . ? C25 Li3 C29 104.61(12) . . ? O2 Li3 C26 131.55(14) . . ? C25 Li3 C26 41.03(7) . . ? C29 Li3 C26 113.50(12) . . ? O2 Li3 Li4 97.90(12) . 2 ? C25 Li3 Li4 56.34(10) . 2 ? C29 Li3 Li4 55.81(9) . 2 ? C26 Li3 Li4 89.51(11) . 2 ? O2 Li3 Li2 51.61(9) . . ? C25 Li3 Li2 109.09(12) . . ? C29 Li3 Li2 59.64(9) . . ? C26 Li3 Li2 149.37(14) . . ? Li4 Li3 Li2 61.45(10) 2 . ? O2 Li3 Li1 50.60(9) . . ? C25 Li3 Li1 59.22(9) . . ? C29 Li3 Li1 107.96(12) . . ? C26 Li3 Li1 95.41(12) . . ? Li4 Li3 Li1 60.52(10) 2 . ? Li2 Li3 Li1 62.96(10) . . ? O2 Li3 H29B 120.7(5) . . ? C25 Li3 H29B 119.0(5) . . ? C29 Li3 H29B 27.4(5) . . ? C26 Li3 H29B 107.7(5) . . ? Li4 Li3 H29B 81.2(5) 2 . ? Li2 Li3 H29B 79.0(5) . . ? Li1 Li3 H29B 135.1(5) . . ? O1 Li4 C29 107.88(13) . 2 ? O1 Li4 C25 109.94(13) . 2 ? C29 Li4 C25 104.47(12) 2 2 ? O1 Li4 C30 133.17(14) . 2 ? C29 Li4 C30 39.42(7) 2 2 ? C25 Li4 C30 110.84(12) 2 2 ? O1 Li4 Li3 97.91(12) . 2 ? C29 Li4 Li3 56.26(10) 2 2 ? C25 Li4 Li3 55.72(9) 2 2 ? C30 Li4 Li3 86.70(11) 2 2 ? O1 Li4 Li1 51.63(9) . 2 ? C29 Li4 Li1 109.25(12) 2 2 ? C25 Li4 Li1 59.49(9) 2 2 ? C30 Li4 Li1 147.17(14) 2 2 ? Li3 Li4 Li1 61.59(10) 2 2 ? O1 Li4 Li2 50.55(9) . 2 ? C29 Li4 Li2 59.35(9) 2 2 ? C25 Li4 Li2 107.71(12) 2 2 ? C30 Li4 Li2 95.18(11) 2 2 ? Li3 Li4 Li2 60.44(10) 2 2 ? Li1 Li4 Li2 62.98(10) 2 2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.0(2) . . . . ? C7 C1 C2 C3 -171.76(12) . . . . ? Li1 C1 C2 C3 92.05(13) . . . . ? C6 C1 C2 C13 175.83(12) . . . . ? C7 C1 C2 C13 5.1(2) . . . . ? Li1 C1 C2 C13 -91.13(13) . . . . ? C6 C1 C2 Li1 -93.04(14) . . . . ? C7 C1 C2 Li1 96.19(13) . . . . ? Li1 C1 C2 Li1 0.0 . . . . ? C1 C2 C3 C4 4.8(2) . . . . ? C13 C2 C3 C4 -172.07(13) . . . . ? Li1 C2 C3 C4 76.17(14) . . . . ? C1 C2 C3 C14 -176.43(13) . . . . ? C13 C2 C3 C14 6.7(2) . . . . ? Li1 C2 C3 C14 -105.03(14) . . . . ? C2 C3 C4 C5 -3.2(2) . . . . ? C14 C3 C4 C5 178.00(13) . . . . ? C3 C4 C5 C6 -2.4(2) . . . . ? C3 C4 C5 C15 173.62(13) . . . . ? Li4 O1 C6 C1 117.9(2) . . . . ? Li2 O1 C6 C1 -0.1(2) 2 . . . ? Li1 O1 C6 C1 -106.4(2) 2 . . . ? Li4 O1 C6 C5 -59.3(2) . . . . ? Li2 O1 C6 C5 -177.26(13) 2 . . . ? Li1 O1 C6 C5 76.4(2) 2 . . . ? C2 C1 C6 O1 178.13(12) . . . . ? C7 C1 C6 O1 -11.2(2) . . . . ? Li1 C1 C6 O1 95.68(13) . . . . ? C2 C1 C6 C5 -4.6(2) . . . . ? C7 C1 C6 C5 166.04(12) . . . . ? Li1 C1 C6 C5 -87.07(13) . . . . ? C4 C5 C6 O1 -176.75(12) . . . . ? C15 C5 C6 O1 7.3(2) . . . . ? C4 C5 C6 C1 6.1(2) . . . . ? C15 C5 C6 C1 -169.78(12) . . . . ? C2 C1 C7 C8 96.14(15) . . . . ? C6 C1 C7 C8 -74.9(2) . . . . ? Li1 C1 C7 C8 179.49(11) . . . . ? C2 C1 C7 C12 -76.1(2) . . . . ? C6 C1 C7 C12 112.90(14) . . . . ? Li1 C1 C7 C12 7.26(15) . . . . ? C2 C1 C7 Li2 -175.11(12) . . . 2 ? C6 C1 C7 Li2 13.89(15) . . . 2 ? Li1 C1 C7 Li2 -91.75(10) . . . 2 ? C12 C7 C8 C9 -0.6(2) . . . . ? C1 C7 C8 C9 -172.69(12) . . . . ? Li2 C7 C8 C9 88.59(14) 2 . . . ? C12 C7 C8 C19 177.44(12) . . . . ? C1 C7 C8 C19 5.3(2) . . . . ? Li2 C7 C8 C19 -93.41(13) 2 . . . ? C12 C7 C8 Li2 -89.16(13) . . . 2 ? C1 C7 C8 Li2 98.72(13) . . . 2 ? Li2 C7 C8 Li2 0.0 2 . . 2 ? C7 C8 C9 C10 3.4(2) . . . . ? C19 C8 C9 C10 -174.65(13) . . . . ? Li2 C8 C9 C10 69.27(14) 2 . . . ? C7 C8 C9 C20 -178.59(13) . . . . ? C19 C8 C9 C20 3.4(2) . . . . ? Li2 C8 C9 C20 -112.67(14) 2 . . . ? C8 C9 C10 C11 -2.0(2) . . . . ? C20 C9 C10 C11 179.87(13) . . . . ? C9 C10 C11 C12 -2.2(2) . . . . ? C9 C10 C11 C21 172.00(13) . . . . ? Li3 O2 C12 C7 121.7(2) . . . . ? Li1 O2 C12 C7 5.3(2) . . . . ? Li2 O2 C12 C7 -104.6(2) . . . . ? Li3 O2 C12 C11 -55.5(2) . . . . ? Li1 O2 C12 C11 -171.95(13) . . . . ? Li2 O2 C12 C11 78.2(2) . . . . ? C8 C7 C12 O2 179.02(11) . . . . ? C1 C7 C12 O2 -9.1(2) . . . . ? Li2 C7 C12 O2 94.50(12) 2 . . . ? C8 C7 C12 C11 -3.7(2) . . . . ? C1 C7 C12 C11 168.25(12) . . . . ? Li2 C7 C12 C11 -88.19(13) 2 . . . ? C10 C11 C12 O2 -177.91(12) . . . . ? C21 C11 C12 O2 8.1(2) . . . . ? C10 C11 C12 C7 4.9(2) . . . . ? C21 C11 C12 C7 -169.10(12) . . . . ? C4 C5 C15 C18 127.93(15) . . . . ? C6 C5 C15 C18 -56.3(2) . . . . ? C4 C5 C15 C16 7.5(2) . . . . ? C6 C5 C15 C16 -176.73(14) . . . . ? C4 C5 C15 C17 -110.2(2) . . . . ? C6 C5 C15 C17 65.6(2) . . . . ? C10 C11 C21 C23 130.55(14) . . . . ? C12 C11 C21 C23 -55.6(2) . . . . ? C10 C11 C21 C24 -107.18(15) . . . . ? C12 C11 C21 C24 66.7(2) . . . . ? C10 C11 C21 C22 10.4(2) . . . . ? C12 C11 C21 C22 -175.74(14) . . . . ? Li3 C25 C26 C27 177.7(2) . . . . ? Li4 C25 C26 C27 130.7(2) 2 . . . ? Li1 C25 C26 C27 -143.3(2) . . . . ? Li3 C25 C26 Li3 0.0 . . . . ? Li4 C25 C26 Li3 -47.02(13) 2 . . . ? Li1 C25 C26 Li3 39.02(15) . . . . ? C25 C26 C27 C28 -66.5(2) . . . . ? Li3 C26 C27 C28 90.7(15) . . . . ? Li4 C29 C30 C31 -160.12(15) 2 . . . ? Li3 C29 C30 C31 147.74(14) . . . . ? Li2 C29 C30 C31 -122.4(2) . . . . ? Li4 C29 C30 Li4 0.0 2 . . 2 ? Li3 C29 C30 Li4 -52.14(13) . . . 2 ? Li2 C29 C30 Li4 37.8(2) . . . 2 ? C29 C30 C31 C32 -175.78(15) . . . . ? Li4 C30 C31 C32 99.5(4) 2 . . . ? C12 O2 Li1 O1 -128.75(11) . . . 2 ? Li3 O2 Li1 O1 87.21(12) . . . 2 ? Li2 O2 Li1 O1 6.07(11) . . . 2 ? C12 O2 Li1 C25 129.53(11) . . . . ? Li3 O2 Li1 C25 -14.50(11) . . . . ? Li2 O2 Li1 C25 -95.65(11) . . . . ? C12 O2 Li1 C1 -0.66(13) . . . . ? Li3 O2 Li1 C1 -144.69(10) . . . . ? Li2 O2 Li1 C1 134.16(10) . . . . ? C12 O2 Li1 Li4 -176.85(10) . . . 2 ? Li3 O2 Li1 Li4 39.11(11) . . . 2 ? Li2 O2 Li1 Li4 -42.03(11) . . . 2 ? C12 O2 Li1 Li3 144.03(14) . . . . ? Li3 O2 Li1 Li3 0.0 . . . . ? Li2 O2 Li1 Li3 -81.15(11) . . . . ? C12 O2 Li1 C2 29.10(14) . . . . ? Li3 O2 Li1 C2 -114.93(11) . . . . ? Li2 O2 Li1 C2 163.92(10) . . . . ? C12 O2 Li1 Li2 -134.82(13) . . . . ? Li3 O2 Li1 Li2 81.15(11) . . . . ? Li2 O2 Li1 Li2 0.0 . . . . ? C26 C25 Li1 O2 -26.8(2) . . . . ? Li3 C25 Li1 O2 13.41(10) . . . . ? Li4 C25 Li1 O2 87.83(12) 2 . . . ? C26 C25 Li1 O1 -125.0(2) . . . 2 ? Li3 C25 Li1 O1 -84.80(12) . . . 2 ? Li4 C25 Li1 O1 -10.37(11) 2 . . 2 ? C26 C25 Li1 C1 56.7(2) . . . . ? Li3 C25 Li1 C1 96.9(2) . . . . ? Li4 C25 Li1 C1 171.3(2) 2 . . . ? C26 C25 Li1 Li4 -114.7(2) . . . 2 ? Li3 C25 Li1 Li4 -74.43(11) . . . 2 ? Li4 C25 Li1 Li4 0.0 2 . . 2 ? C26 C25 Li1 Li3 -40.2(2) . . . . ? Li3 C25 Li1 Li3 0.0 . . . . ? Li4 C25 Li1 Li3 74.43(11) 2 . . . ? C26 C25 Li1 C2 68.1(2) . . . . ? Li3 C25 Li1 C2 108.33(11) . . . . ? Li4 C25 Li1 C2 -177.25(12) 2 . . . ? C26 C25 Li1 Li2 -76.1(2) . . . . ? Li3 C25 Li1 Li2 -35.90(11) . . . . ? Li4 C25 Li1 Li2 38.53(11) 2 . . . ? C2 C1 Li1 O2 113.48(11) . . . . ? C6 C1 Li1 O2 -125.47(10) . . . . ? C7 C1 Li1 O2 -3.37(11) . . . . ? C2 C1 Li1 O1 -156.7(2) . . . 2 ? C6 C1 Li1 O1 -35.6(2) . . . 2 ? C7 C1 Li1 O1 86.5(2) . . . 2 ? C2 C1 Li1 C25 21.2(2) . . . . ? C6 C1 Li1 C25 142.2(2) . . . . ? C7 C1 Li1 C25 -95.7(2) . . . . ? C2 C1 Li1 Li4 141.6(9) . . . 2 ? C6 C1 Li1 Li4 -97.4(9) . . . 2 ? C7 C1 Li1 Li4 24.7(9) . . . 2 ? C2 C1 Li1 Li3 84.64(14) . . . . ? C6 C1 Li1 Li3 -154.31(13) . . . . ? C7 C1 Li1 Li3 -32.21(15) . . . . ? C2 C1 Li1 C2 0.0 . . . . ? C6 C1 Li1 C2 121.05(12) . . . . ? C7 C1 Li1 C2 -116.85(12) . . . . ? C2 C1 Li1 Li2 149.34(13) . . . . ? C6 C1 Li1 Li2 -89.62(13) . . . . ? C7 C1 Li1 Li2 32.49(14) . . . . ? C3 C2 Li1 O2 178.78(11) . . . . ? C1 C2 Li1 O2 -64.60(11) . . . . ? C13 C2 Li1 O2 53.97(12) . . . . ? C3 C2 Li1 O1 -67.5(3) . . . 2 ? C1 C2 Li1 O1 49.1(3) . . . 2 ? C13 C2 Li1 O1 167.7(3) . . . 2 ? C3 C2 Li1 C25 79.47(12) . . . . ? C1 C2 Li1 C25 -163.91(12) . . . . ? C13 C2 Li1 C25 -45.34(12) . . . . ? C3 C2 Li1 C1 -116.61(13) . . . . ? C1 C2 Li1 C1 0.0 . . . . ? C13 C2 Li1 C1 118.57(13) . . . . ? C3 C2 Li1 Li4 74.6(3) . . . 2 ? C1 C2 Li1 Li4 -168.8(3) . . . 2 ? C13 C2 Li1 Li4 -50.3(3) . . . 2 ? C3 C2 Li1 Li3 133.25(12) . . . . ? C1 C2 Li1 Li3 -110.14(13) . . . . ? C13 C2 Li1 Li3 8.43(14) . . . . ? C3 C2 Li1 Li2 -162.6(2) . . . . ? C1 C2 Li1 Li2 -46.0(2) . . . . ? C13 C2 Li1 Li2 72.6(2) . . . . ? C12 O2 Li2 O1 119.42(13) . . . 2 ? Li3 O2 Li2 O1 -89.07(12) . . . 2 ? Li1 O2 Li2 O1 -6.15(11) . . . 2 ? C12 O2 Li2 C29 -139.99(12) . . . . ? Li3 O2 Li2 C29 11.52(11) . . . . ? Li1 O2 Li2 C29 94.44(11) . . . . ? C12 O2 Li2 C7 36.1(2) . . . 2 ? Li3 O2 Li2 C7 -172.4(2) . . . 2 ? Li1 O2 Li2 C7 -89.4(2) . . . 2 ? C12 O2 Li2 Li3 -151.5(2) . . . . ? Li3 O2 Li2 Li3 0.0 . . . . ? Li1 O2 Li2 Li3 82.92(11) . . . . ? C12 O2 Li2 Li4 167.23(12) . . . 2 ? Li3 O2 Li2 Li4 -41.26(11) . . . 2 ? Li1 O2 Li2 Li4 41.66(11) . . . 2 ? C12 O2 Li2 Li1 125.57(15) . . . . ? Li3 O2 Li2 Li1 -82.92(11) . . . . ? Li1 O2 Li2 Li1 0.0 . . . . ? C12 O2 Li2 C8 6.6(5) . . . 2 ? Li3 O2 Li2 C8 158.1(4) . . . 2 ? Li1 O2 Li2 C8 -119.0(4) . . . 2 ? C30 C29 Li2 O1 -26.6(2) . . . 2 ? Li4 C29 Li2 O1 13.57(10) 2 . . 2 ? Li3 C29 Li2 O1 88.15(12) . . . 2 ? C30 C29 Li2 O2 -125.4(2) . . . . ? Li4 C29 Li2 O2 -85.21(12) 2 . . . ? Li3 C29 Li2 O2 -10.64(11) . . . . ? C30 C29 Li2 C7 58.2(2) . . . 2 ? Li4 C29 Li2 C7 98.4(2) 2 . . 2 ? Li3 C29 Li2 C7 173.0(2) . . . 2 ? C30 C29 Li2 Li3 -114.8(2) . . . . ? Li4 C29 Li2 Li3 -74.58(11) 2 . . . ? Li3 C29 Li2 Li3 0.0 . . . . ? C30 C29 Li2 Li4 -40.2(2) . . . 2 ? Li4 C29 Li2 Li4 0.0 2 . . 2 ? Li3 C29 Li2 Li4 74.58(11) . . . 2 ? C30 C29 Li2 Li1 -76.2(2) . . . . ? Li4 C29 Li2 Li1 -36.04(11) 2 . . . ? Li3 C29 Li2 Li1 38.54(11) . . . . ? C30 C29 Li2 C8 65.0(2) . . . 2 ? Li4 C29 Li2 C8 105.16(11) 2 . . 2 ? Li3 C29 Li2 C8 179.73(12) . . . 2 ? O2 Li1 Li2 O1 171.88(14) . . . 2 ? O1 Li1 Li2 O1 0.0 2 . . 2 ? C25 Li1 Li2 O1 -95.34(11) . . . 2 ? C1 Li1 Li2 O1 121.77(13) . . . 2 ? Li4 Li1 Li2 O1 -59.50(10) 2 . . 2 ? Li3 Li1 Li2 O1 -128.78(13) . . . 2 ? C2 Li1 Li2 O1 146.8(2) . . . 2 ? O2 Li1 Li2 O2 0.0 . . . . ? O1 Li1 Li2 O2 -171.88(14) 2 . . . ? C25 Li1 Li2 O2 92.78(11) . . . . ? C1 Li1 Li2 O2 -50.11(11) . . . . ? Li4 Li1 Li2 O2 128.62(13) 2 . . . ? Li3 Li1 Li2 O2 59.33(9) . . . . ? C2 Li1 Li2 O2 -25.1(2) . . . . ? O2 Li1 Li2 C29 -95.08(11) . . . . ? O1 Li1 Li2 C29 93.04(11) 2 . . . ? C25 Li1 Li2 C29 -2.30(13) . . . . ? C1 Li1 Li2 C29 -145.19(11) . . . . ? Li4 Li1 Li2 C29 33.54(10) 2 . . . ? Li3 Li1 Li2 C29 -35.75(10) . . . . ? C2 Li1 Li2 C29 -120.2(2) . . . . ? O2 Li1 Li2 C7 124.34(14) . . . 2 ? O1 Li1 Li2 C7 -47.54(11) 2 . . 2 ? C25 Li1 Li2 C7 -142.88(11) . . . 2 ? C1 Li1 Li2 C7 74.23(15) . . . 2 ? Li4 Li1 Li2 C7 -107.04(14) 2 . . 2 ? Li3 Li1 Li2 C7 -176.32(15) . . . 2 ? C2 Li1 Li2 C7 99.2(2) . . . 2 ? O2 Li1 Li2 Li3 -59.33(9) . . . . ? O1 Li1 Li2 Li3 128.78(13) 2 . . . ? C25 Li1 Li2 Li3 33.45(10) . . . . ? C1 Li1 Li2 Li3 -109.44(13) . . . . ? Li4 Li1 Li2 Li3 69.29(11) 2 . . . ? Li3 Li1 Li2 Li3 0.0 . . . . ? C2 Li1 Li2 Li3 -84.4(2) . . . . ? O2 Li1 Li2 Li4 -128.62(13) . . . 2 ? O1 Li1 Li2 Li4 59.50(10) 2 . . 2 ? C25 Li1 Li2 Li4 -35.84(10) . . . 2 ? C1 Li1 Li2 Li4 -178.73(14) . . . 2 ? Li4 Li1 Li2 Li4 0.0 2 . . 2 ? Li3 Li1 Li2 Li4 -69.29(11) . . . 2 ? C2 Li1 Li2 Li4 -153.7(2) . . . 2 ? O2 Li1 Li2 C8 154.7(2) . . . 2 ? O1 Li1 Li2 C8 -17.2(2) 2 . . 2 ? C25 Li1 Li2 C8 -112.5(2) . . . 2 ? C1 Li1 Li2 C8 104.6(2) . . . 2 ? Li4 Li1 Li2 C8 -76.7(2) 2 . . 2 ? Li3 Li1 Li2 C8 -146.0(2) . . . 2 ? C2 Li1 Li2 C8 129.6(2) . . . 2 ? C12 O2 Li3 C25 -112.8(2) . . . . ? Li1 O2 Li3 C25 16.30(12) . . . . ? Li2 O2 Li3 C25 100.58(13) . . . . ? C12 O2 Li3 C29 133.7(2) . . . . ? Li1 O2 Li3 C29 -97.22(13) . . . . ? Li2 O2 Li3 C29 -12.94(13) . . . . ? C12 O2 Li3 C26 -73.5(3) . . . . ? Li1 O2 Li3 C26 55.6(2) . . . . ? Li2 O2 Li3 C26 139.9(2) . . . . ? C12 O2 Li3 Li4 -169.88(14) . . . 2 ? Li1 O2 Li3 Li4 -40.80(12) . . . 2 ? Li2 O2 Li3 Li4 43.48(12) . . . 2 ? C12 O2 Li3 Li2 146.6(2) . . . . ? Li1 O2 Li3 Li2 -84.28(11) . . . . ? Li2 O2 Li3 Li2 0.0 . . . . ? C12 O2 Li3 Li1 -129.1(2) . . . . ? Li1 O2 Li3 Li1 0.0 . . . . ? Li2 O2 Li3 Li1 84.28(11) . . . . ? C26 C25 Li3 O2 133.77(15) . . . . ? Li4 C25 Li3 O2 -87.67(13) 2 . . . ? Li1 C25 Li3 O2 -14.62(11) . . . . ? C26 C25 Li3 C29 -109.16(13) . . . . ? Li4 C25 Li3 C29 29.40(11) 2 . . . ? Li1 C25 Li3 C29 102.45(12) . . . . ? C26 C25 Li3 C26 0.0 . . . . ? Li4 C25 Li3 C26 138.56(13) 2 . . . ? Li1 C25 Li3 C26 -148.39(13) . . . . ? C26 C25 Li3 Li4 -138.56(13) . . . 2 ? Li4 C25 Li3 Li4 0.0 2 . . 2 ? Li1 C25 Li3 Li4 73.05(10) . . . 2 ? C26 C25 Li3 Li2 -171.61(14) . . . . ? Li4 C25 Li3 Li2 -33.05(12) 2 . . . ? Li1 C25 Li3 Li2 40.00(11) . . . . ? C26 C25 Li3 Li1 148.39(13) . . . . ? Li4 C25 Li3 Li1 -73.05(10) 2 . . . ? Li1 C25 Li3 Li1 0.0 . . . . ? C30 C29 Li3 O2 142.10(14) . . . . ? Li4 C29 Li3 O2 85.97(13) 2 . . . ? Li2 C29 Li3 O2 11.73(12) . . . . ? C30 C29 Li3 C25 26.5(2) . . . . ? Li4 C29 Li3 C25 -29.60(11) 2 . . . ? Li2 C29 Li3 C25 -103.83(12) . . . . ? C30 C29 Li3 C26 -16.0(2) . . . . ? Li4 C29 Li3 C26 -72.14(13) 2 . . . ? Li2 C29 Li3 C26 -146.38(15) . . . . ? C30 C29 Li3 Li4 56.13(14) . . . 2 ? Li4 C29 Li3 Li4 0.0 2 . . 2 ? Li2 C29 Li3 Li4 -74.24(10) . . . 2 ? C30 C29 Li3 Li2 130.4(2) . . . . ? Li4 C29 Li3 Li2 74.24(10) 2 . . . ? Li2 C29 Li3 Li2 0.0 . . . . ? C30 C29 Li3 Li1 88.4(2) . . . . ? Li4 C29 Li3 Li1 32.28(11) 2 . . . ? Li2 C29 Li3 Li1 -41.96(11) . . . . ? C27 C26 Li3 O2 135.1(14) . . . . ? C25 C26 Li3 O2 -66.7(2) . . . . ? C27 C26 Li3 C25 -158.2(15) . . . . ? C25 C26 Li3 C25 0.0 . . . . ? C27 C26 Li3 C29 -72.9(15) . . . . ? C25 C26 Li3 C29 85.37(14) . . . . ? C27 C26 Li3 Li4 -124.8(14) . . . 2 ? C25 C26 Li3 Li4 33.43(11) . . . 2 ? C27 C26 Li3 Li2 -142.5(14) . . . . ? C25 C26 Li3 Li2 15.7(3) . . . . ? C27 C26 Li3 Li1 174.9(14) . . . . ? C25 C26 Li3 Li1 -26.90(11) . . . . ? O1 Li2 Li3 O2 95.72(12) 2 . . . ? O2 Li2 Li3 O2 0.0 . . . . ? C29 Li2 Li3 O2 -165.89(14) . . . . ? C7 Li2 Li3 O2 95.2(13) 2 . . . ? Li4 Li2 Li3 O2 129.11(13) 2 . . . ? Li1 Li2 Li3 O2 59.68(9) . . . . ? C8 Li2 Li3 O2 -166.4(3) 2 . . . ? O1 Li2 Li3 C25 -2.27(14) 2 . . . ? O2 Li2 Li3 C25 -98.00(13) . . . . ? C29 Li2 Li3 C25 96.12(13) . . . . ? C7 Li2 Li3 C25 -2.8(14) 2 . . . ? Li4 Li2 Li3 C25 31.11(11) 2 . . . ? Li1 Li2 Li3 C25 -38.32(11) . . . . ? C8 Li2 Li3 C25 95.6(2) 2 . . . ? O1 Li2 Li3 C29 -98.39(11) 2 . . . ? O2 Li2 Li3 C29 165.89(14) . . . . ? C29 Li2 Li3 C29 0.0 . . . . ? C7 Li2 Li3 C29 -98.9(13) 2 . . . ? Li4 Li2 Li3 C29 -65.00(10) 2 . . . ? Li1 Li2 Li3 C29 -134.44(12) . . . . ? C8 Li2 Li3 C29 -0.5(2) 2 . . . ? O1 Li2 Li3 C26 -13.1(3) 2 . . . ? O2 Li2 Li3 C26 -108.8(3) . . . . ? C29 Li2 Li3 C26 85.3(3) . . . . ? C7 Li2 Li3 C26 -13.6(15) 2 . . . ? Li4 Li2 Li3 C26 20.3(3) 2 . . . ? Li1 Li2 Li3 C26 -49.2(3) . . . . ? C8 Li2 Li3 C26 84.8(4) 2 . . . ? O1 Li2 Li3 Li4 -33.39(10) 2 . . 2 ? O2 Li2 Li3 Li4 -129.11(13) . . . 2 ? C29 Li2 Li3 Li4 65.00(10) . . . 2 ? C7 Li2 Li3 Li4 -33.9(13) 2 . . 2 ? Li4 Li2 Li3 Li4 0.0 2 . . 2 ? Li1 Li2 Li3 Li4 -69.43(11) . . . 2 ? C8 Li2 Li3 Li4 64.5(2) 2 . . 2 ? O1 Li2 Li3 Li1 36.05(10) 2 . . . ? O2 Li2 Li3 Li1 -59.68(9) . . . . ? C29 Li2 Li3 Li1 134.44(12) . . . . ? C7 Li2 Li3 Li1 35.6(13) 2 . . . ? Li4 Li2 Li3 Li1 69.43(11) 2 . . . ? Li1 Li2 Li3 Li1 0.0 . . . . ? C8 Li2 Li3 Li1 133.9(2) 2 . . . ? O2 Li1 Li3 O2 0.0 . . . . ? O1 Li1 Li3 O2 -96.60(11) 2 . . . ? C25 Li1 Li3 O2 161.88(14) . . . . ? C1 Li1 Li3 O2 40.03(12) . . . . ? Li4 Li1 Li3 O2 -131.97(13) 2 . . . ? C2 Li1 Li3 O2 75.07(11) . . . . ? Li2 Li1 Li3 O2 -61.11(10) . . . . ? O2 Li1 Li3 C25 -161.88(14) . . . . ? O1 Li1 Li3 C25 101.52(11) 2 . . . ? C25 Li1 Li3 C25 0.0 . . . . ? C1 Li1 Li3 C25 -121.85(14) . . . . ? Li4 Li1 Li3 C25 66.14(10) 2 . . . ? C2 Li1 Li3 C25 -86.81(11) . . . . ? Li2 Li1 Li3 C25 137.00(12) . . . . ? O2 Li1 Li3 C29 101.48(13) . . . . ? O1 Li1 Li3 C29 4.88(14) 2 . . . ? C25 Li1 Li3 C29 -96.64(12) . . . . ? C1 Li1 Li3 C29 141.51(12) . . . . ? Li4 Li1 Li3 C29 -30.49(11) 2 . . . ? C2 Li1 Li3 C29 176.55(10) . . . . ? Li2 Li1 Li3 C29 40.36(11) . . . . ? O2 Li1 Li3 C26 -141.66(14) . . . . ? O1 Li1 Li3 C26 121.74(11) 2 . . . ? C25 Li1 Li3 C26 20.22(8) . . . . ? C1 Li1 Li3 C26 -101.63(13) . . . . ? Li4 Li1 Li3 C26 86.36(11) 2 . . . ? C2 Li1 Li3 C26 -66.59(13) . . . . ? Li2 Li1 Li3 C26 157.22(13) . . . . ? O2 Li1 Li3 Li4 131.97(13) . . . 2 ? O1 Li1 Li3 Li4 35.38(10) 2 . . 2 ? C25 Li1 Li3 Li4 -66.14(10) . . . 2 ? C1 Li1 Li3 Li4 172.01(15) . . . 2 ? Li4 Li1 Li3 Li4 0.0 2 . . 2 ? C2 Li1 Li3 Li4 -152.95(13) . . . 2 ? Li2 Li1 Li3 Li4 70.86(11) . . . 2 ? O2 Li1 Li3 Li2 61.11(10) . . . . ? O1 Li1 Li3 Li2 -35.48(10) 2 . . . ? C25 Li1 Li3 Li2 -137.00(12) . . . . ? C1 Li1 Li3 Li2 101.15(13) . . . . ? Li4 Li1 Li3 Li2 -70.86(11) 2 . . . ? C2 Li1 Li3 Li2 136.19(13) . . . . ? Li2 Li1 Li3 Li2 0.0 . . . . ? C6 O1 Li4 C29 -112.6(2) . . . 2 ? Li2 O1 Li4 C29 16.42(12) 2 . . 2 ? Li1 O1 Li4 C29 100.74(13) 2 . . 2 ? C6 O1 Li4 C25 134.1(2) . . . 2 ? Li2 O1 Li4 C25 -96.93(14) 2 . . 2 ? Li1 O1 Li4 C25 -12.61(13) 2 . . 2 ? C6 O1 Li4 C30 -76.7(3) . . . 2 ? Li2 O1 Li4 C30 52.3(2) 2 . . 2 ? Li1 O1 Li4 C30 136.6(2) 2 . . 2 ? C6 O1 Li4 Li3 -169.6(2) . . . 2 ? Li2 O1 Li4 Li3 -40.60(12) 2 . . 2 ? Li1 O1 Li4 Li3 43.72(12) 2 . . 2 ? C6 O1 Li4 Li1 146.7(2) . . . 2 ? Li2 O1 Li4 Li1 -84.32(11) 2 . . 2 ? Li1 O1 Li4 Li1 0.0 2 . . 2 ? C6 O1 Li4 Li2 -129.0(2) . . . 2 ? Li2 O1 Li4 Li2 0.0 2 . . 2 ? Li1 O1 Li4 Li2 84.32(11) 2 . . 2 ? #END OF CIF data_Chisholm979 _database_code_CSD 185857 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H78 Li4 O6' _chemical_formula_weight 754.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8871(1) _cell_length_b 12.3753(2) _cell_length_c 19.6433(3) _cell_angle_alpha 75.397(1) _cell_angle_beta 77.010(1) _cell_angle_gamma 67.596(1) _cell_volume 2343.14(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method ? _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41117 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8253 _reflns_number_observed 6091 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The THF ligands are disordered with two carbon atoms from each THF group disordered over two sites: C39, C40, C44 and C45. The occupancy factors were refined and restricted to sum to one for each THF group. The occupancy factor for the major component for one THF group (C39A and C40A) refined to 0.63(1), while that for the major component in the other THF group (C44A and C45A) refined to 0.57(1). All disordered carbon atoms were kept isotropic. The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+1.1192P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8252 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_obs 0.0589 _refine_ls_wR_factor_all 0.1614 _refine_ls_wR_factor_obs 0.1446 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.031 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.023 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.449 _refine_diff_density_min -0.389 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.07107(13) 0.89702(11) 0.28856(7) 0.0309(3) Uani 1 d . . O2 O 0.40099(14) 0.82586(12) 0.20324(7) 0.0362(3) Uani 1 d . . O3 O 0.33164(13) 0.93693(11) 0.32349(7) 0.0322(3) Uani 1 d . . O4 O 0.27498(13) 0.70935(11) 0.35663(7) 0.0328(3) Uani 1 d . . O5 O 0.08116(15) 0.63962(12) 0.27004(9) 0.0460(4) Uani 1 d . . O6 O 0.4486(2) 1.07990(14) 0.16836(9) 0.0544(4) Uani 1 d . . C1 C 0.1426(2) 0.9877(2) 0.17308(10) 0.0320(5) Uani 1 d . . C2 C 0.0618(2) 0.9956(2) 0.24025(10) 0.0291(4) Uani 1 d . . C3 C -0.0278(2) 1.1089(2) 0.25404(11) 0.0321(5) Uani 1 d . . C4 C -0.0208(2) 1.2077(2) 0.20252(11) 0.0370(5) Uani 1 d . . H4 H -0.0793(2) 1.2839(2) 0.21159(11) 0.044 Uiso 1 calc R . C5 C 0.0657(2) 1.2024(2) 0.13898(12) 0.0403(5) Uani 1 d . . C6 C 0.1467(2) 1.0902(2) 0.12291(11) 0.0384(5) Uani 1 d . . C7 C 0.2091(2) 0.8686(2) 0.14969(10) 0.0334(5) Uani 1 d . . C8 C 0.1383(2) 0.8377(2) 0.11041(11) 0.0391(5) Uani 1 d . . C9 C 0.2038(2) 0.7389(2) 0.07755(12) 0.0448(6) Uani 1 d . . C10 C 0.3384(2) 0.6760(2) 0.08365(12) 0.0448(6) Uani 1 d . . H10 H 0.3831(2) 0.6111(2) 0.05927(12) 0.054 Uiso 1 calc R . C11 C 0.4121(2) 0.7015(2) 0.12301(11) 0.0362(5) Uani 1 d . . C12 C 0.3429(2) 0.7980(2) 0.16041(10) 0.0329(5) Uani 1 d . . C13 C -0.1334(2) 1.1206(2) 0.32113(12) 0.0396(5) Uani 1 d . . C14 C -0.2251(2) 1.0519(2) 0.32129(14) 0.0546(6) Uani 1 d . . H14A H -0.2917(11) 1.0577(13) 0.3643(5) 0.082 Uiso 1 calc R . H14B H -0.1709(3) 0.9682(4) 0.3204(9) 0.082 Uiso 1 calc R . H14C H -0.2711(13) 1.0861(10) 0.2792(5) 0.082 Uiso 1 calc R . C15 C -0.0695(2) 1.0711(2) 0.38977(12) 0.0495(6) Uani 1 d . . H15A H -0.0295(14) 0.9843(3) 0.3958(5) 0.074 Uiso 1 calc R . H15B H -0.1386(4) 1.0930(12) 0.4304(2) 0.074 Uiso 1 calc R . H15C H 0.0003(11) 1.1045(11) 0.3869(4) 0.074 Uiso 1 calc R . C16 C -0.2217(3) 1.2502(2) 0.3239(2) 0.0713(9) Uani 1 d . . H16A H -0.2884(14) 1.2534(3) 0.3669(6) 0.107 Uiso 1 calc R . H16B H -0.2676(16) 1.2845(6) 0.2818(6) 0.107 Uiso 1 calc R . H16C H -0.1655(4) 1.2955(5) 0.3248(11) 0.107 Uiso 1 calc R . C17 C 0.0662(3) 1.3173(2) 0.08758(13) 0.0532(6) Uani 1 d . . H17A H 0.0550(17) 1.3127(6) 0.0404(2) 0.080 Uiso 1 calc R . H17B H 0.1517(7) 1.3286(8) 0.0847(7) 0.080 Uiso 1 calc R . H17C H -0.0078(10) 1.3845(3) 0.1046(5) 0.080 Uiso 1 calc R . C18 C 0.2355(3) 1.0785(2) 0.05195(12) 0.0549(7) Uani 1 d . . H18A H 0.1797(3) 1.0991(15) 0.0146(2) 0.082 Uiso 1 calc R . H18B H 0.2977(12) 0.9964(4) 0.0537(3) 0.082 Uiso 1 calc R . H18C H 0.2866(13) 1.1324(11) 0.0416(4) 0.082 Uiso 1 calc R . C19 C 0.5634(2) 0.6332(2) 0.12237(12) 0.0420(5) Uani 1 d . . C20 C 0.6397(3) 0.7207(2) 0.0996(2) 0.0630(7) Uani 1 d . . H20A H 0.6155(14) 0.7715(11) 0.0540(5) 0.095 Uiso 1 calc R . H20B H 0.7364(3) 0.6765(2) 0.0943(10) 0.095 Uiso 1 calc R . H20C H 0.6159(15) 0.7701(11) 0.1357(5) 0.095 Uiso 1 calc R . C21 C 0.5940(3) 0.5609(2) 0.19522(15) 0.0662(8) Uani 1 d . . H21A H 0.5474(16) 0.5030(12) 0.2096(5) 0.099 Uiso 1 calc R . H21B H 0.5633(18) 0.6141(3) 0.2298(3) 0.099 Uiso 1 calc R . H21C H 0.6909(3) 0.5188(14) 0.1933(3) 0.099 Uiso 1 calc R . C22 C 0.6204(3) 0.5476(3) 0.0691(2) 0.0701(8) Uani 1 d . . H22A H 0.5974(18) 0.5913(4) 0.0220(3) 0.105 Uiso 1 calc R . H22B H 0.5819(16) 0.4840(10) 0.0847(6) 0.105 Uiso 1 calc R . H22C H 0.7183(3) 0.5128(14) 0.0667(8) 0.105 Uiso 1 calc R . C23 C 0.1338(3) 0.7026(3) 0.03346(15) 0.0629(7) Uani 1 d . . H23A H 0.1068(17) 0.7666(7) -0.0072(6) 0.094 Uiso 1 calc R . H23B H 0.0541(11) 0.6878(16) 0.0627(3) 0.094 Uiso 1 calc R . H23C H 0.1952(7) 0.6301(10) 0.0163(8) 0.094 Uiso 1 calc R . C24 C -0.0071(2) 0.9118(2) 0.10354(13) 0.0500(6) Uani 1 d . . H24A H -0.0115(2) 0.9758(9) 0.0619(5) 0.075 Uiso 1 calc R . H24B H -0.0503(5) 0.9462(12) 0.1464(4) 0.075 Uiso 1 calc R . H24C H -0.0536(5) 0.8613(4) 0.0979(9) 0.075 Uiso 1 calc R . C25 C 0.3894(2) 0.9936(2) 0.35479(11) 0.0311(4) Uani 1 d . . H25 H 0.4429(2) 1.0325(2) 0.31502(11) 0.037 Uiso 1 calc R . C26 C 0.2809(2) 1.0938(2) 0.39016(11) 0.0367(5) Uani 1 d . . H26 H 0.2151(2) 1.0599(2) 0.42362(11) 0.044 Uiso 1 calc R . C27 C 0.2058(2) 1.1926(2) 0.33461(14) 0.0498(6) Uani 1 d . . H27A H 0.2660(5) 1.2335(10) 0.3048(6) 0.075 Uiso 1 calc R . H27B H 0.1286(10) 1.2496(8) 0.35845(14) 0.075 Uiso 1 calc R . H27C H 0.1745(15) 1.1584(3) 0.3049(6) 0.075 Uiso 1 calc R . C28 C 0.3376(2) 1.1475(2) 0.43241(14) 0.0506(6) Uani 1 d . . H28A H 0.4130(11) 1.1691(13) 0.4026(3) 0.076 Uiso 1 calc R . H28B H 0.3687(15) 1.0891(6) 0.4746(5) 0.076 Uiso 1 calc R . H28C H 0.2674(5) 1.2187(9) 0.4471(8) 0.076 Uiso 1 calc R . C29 C 0.4887(2) 0.9044(2) 0.40422(11) 0.0373(5) Uani 1 d . . H29 H 0.5282(2) 0.9508(2) 0.42227(11) 0.045 Uiso 1 calc R . C30 C 0.4215(2) 0.8391(2) 0.46859(12) 0.0484(6) Uani 1 d . . H30A H 0.3722(13) 0.8003(12) 0.45282(12) 0.073 Uiso 1 calc R . H30B H 0.3589(12) 0.8960(3) 0.4982(4) 0.073 Uiso 1 calc R . H30C H 0.4900(3) 0.7790(10) 0.4963(5) 0.073 Uiso 1 calc R . C31 C 0.6040(2) 0.8173(2) 0.36395(15) 0.0538(6) Uani 1 d . . H31A H 0.6384(11) 0.8609(3) 0.3197(5) 0.081 Uiso 1 calc R . H31B H 0.5718(5) 0.7605(10) 0.3529(8) 0.081 Uiso 1 calc R . H31C H 0.6759(7) 0.7742(11) 0.3933(4) 0.081 Uiso 1 calc R . C32 C 0.2796(2) 0.6243(2) 0.42005(11) 0.0366(5) Uani 1 d . . H32 H 0.3015(2) 0.6562(2) 0.45605(11) 0.044 Uiso 1 calc R . C33 C 0.1425(2) 0.6094(2) 0.44974(12) 0.0456(6) Uani 1 d . . H33 H 0.1192(2) 0.5753(2) 0.41543(12) 0.055 Uiso 1 calc R . C34 C 0.0334(3) 0.7287(2) 0.45784(15) 0.0608(7) Uani 1 d . . H34A H 0.0211(13) 0.7790(7) 0.4108(2) 0.091 Uiso 1 calc R . H34B H 0.0599(9) 0.7679(8) 0.4868(8) 0.091 Uiso 1 calc R . H34C H -0.0509(5) 0.7162(3) 0.4811(9) 0.091 Uiso 1 calc R . C35 C 0.1452(3) 0.5249(3) 0.52193(14) 0.0686(8) Uani 1 d . . H35A H 0.1811(19) 0.5505(11) 0.5542(4) 0.103 Uiso 1 calc R . H35B H 0.2024(16) 0.4440(4) 0.5155(2) 0.103 Uiso 1 calc R . H35C H 0.0538(4) 0.5264(14) 0.5422(5) 0.103 Uiso 1 calc R . C36 C 0.3935(2) 0.5055(2) 0.41167(13) 0.0441(6) Uani 1 d . . H36 H 0.3900(2) 0.4496(2) 0.45818(13) 0.053 Uiso 1 calc R . C37 C 0.3769(2) 0.4488(2) 0.35544(15) 0.0547(7) Uani 1 d . . H37A H 0.3697(17) 0.5051(6) 0.3102(3) 0.082 Uiso 1 calc R . H37B H 0.2954(9) 0.4279(14) 0.3705(4) 0.082 Uiso 1 calc R . H37C H 0.4550(8) 0.3768(9) 0.3495(7) 0.082 Uiso 1 calc R . C38 C 0.5291(2) 0.5212(2) 0.39645(14) 0.0492(6) Uani 1 d . . H38A H 0.5342(6) 0.5635(13) 0.4311(5) 0.074 Uiso 1 calc R . H38B H 0.5405(7) 0.5673(12) 0.3484(3) 0.074 Uiso 1 calc R . H38C H 0.6003(2) 0.4431(2) 0.4000(8) 0.074 Uiso 1 calc R . C39A C 0.3991(5) 1.2062(4) 0.1417(3) 0.0559(15) Uiso 0.635(13) d P 1 H39A H 0.3171(5) 1.2472(4) 0.1722(3) 0.067 Uiso 0.635(13) calc PR 1 H39B H 0.3804(5) 1.2241(4) 0.0923(3) 0.067 Uiso 0.635(13) calc PR 1 C40A C 0.5172(6) 1.2398(5) 0.1458(5) 0.083(2) Uiso 0.635(13) d P 1 H40A H 0.5241(6) 1.2389(5) 0.1953(5) 0.100 Uiso 0.635(13) calc PR 1 H40B H 0.5129(6) 1.3185(5) 0.1163(5) 0.100 Uiso 0.635(13) calc PR 1 C39B C 0.4279(10) 1.2034(7) 0.1676(7) 0.060(3) Uiso 0.365(13) d P 2 H39C H 0.4466(10) 1.2130(7) 0.2124(7) 0.072 Uiso 0.365(13) calc PR 2 H39D H 0.3353(10) 1.2556(7) 0.1600(7) 0.072 Uiso 0.365(13) calc PR 2 C40B C 0.5299(10) 1.2294(9) 0.1049(8) 0.079(4) Uiso 0.365(13) d P 2 H40C H 0.4991(10) 1.2397(9) 0.0592(8) 0.095 Uiso 0.365(13) calc PR 2 H40D H 0.5472(10) 1.3017(9) 0.1063(8) 0.095 Uiso 0.365(13) calc PR 2 C41 C 0.6364(4) 1.1348(4) 0.1138(2) 0.1098(14) Uani 1 d . . H41A H 0.6496(4) 1.1524(4) 0.0612(2) 0.132 Uiso 0.635(13) calc PR 1 H41B H 0.7216(4) 1.1199(4) 0.1307(2) 0.132 Uiso 0.635(13) calc PR 1 H41C H 0.6866(4) 1.1413(4) 0.1479(2) 0.132 Uiso 0.365(13) calc PR 2 H41D H 0.6964(4) 1.1247(4) 0.0680(2) 0.132 Uiso 0.365(13) calc PR 2 C42 C 0.5879(3) 1.0311(3) 0.1422(2) 0.0844(10) Uani 1 d . . H42A H 0.6009(3) 0.9869(3) 0.1041(2) 0.101 Uiso 1 calc R . H42B H 0.6377(3) 0.9760(3) 0.1809(2) 0.101 Uiso 1 calc R . C43 C 0.1221(3) 0.5373(2) 0.2372(2) 0.0610(7) Uani 1 d . . H43A H 0.1650(3) 0.4642(2) 0.2705(2) 0.073 Uiso 0.572(14) calc PR 1 H43B H 0.1876(3) 0.5447(2) 0.1939(2) 0.073 Uiso 0.572(14) calc PR 1 H43C H 0.1946(3) 0.4703(2) 0.2598(2) 0.073 Uiso 0.428(14) calc PR 2 H43D H 0.1527(3) 0.5563(2) 0.1857(2) 0.073 Uiso 0.428(14) calc PR 2 C44A C 0.0003(5) 0.5313(6) 0.2188(5) 0.065(2) Uiso 0.572(14) d P 1 H44A H 0.0064(5) 0.4478(6) 0.2237(5) 0.078 Uiso 0.572(14) calc PR 1 H44B H -0.0143(5) 0.5735(6) 0.1697(5) 0.078 Uiso 0.572(14) calc PR 1 C45A C -0.1107(6) 0.5936(8) 0.2733(5) 0.075(2) Uiso 0.572(14) d P 1 H45A H -0.1969(6) 0.6329(8) 0.2540(5) 0.090 Uiso 0.572(14) calc PR 1 H45B H -0.1228(6) 0.5364(8) 0.3174(5) 0.090 Uiso 0.572(14) calc PR 1 C44B C -0.0103(8) 0.5087(8) 0.2514(8) 0.074(3) Uiso 0.428(14) d P 2 H44A' H -0.0238(8) 0.4622(8) 0.2997(8) 0.088 Uiso 0.428(14) calc PR 2 H44B' H -0.0125(8) 0.4658(8) 0.2157(8) 0.088 Uiso 0.428(14) calc PR 2 C45B C -0.1173(7) 0.6409(9) 0.2431(6) 0.065(3) Uiso 0.428(14) d P 2 H45A' H -0.1138(7) 0.6841(9) 0.1933(6) 0.078 Uiso 0.428(14) calc PR 2 H45B' H -0.2101(7) 0.6427(9) 0.2626(6) 0.078 Uiso 0.428(14) calc PR 2 C46 C -0.0624(2) 0.6839(2) 0.2872(2) 0.0622(7) Uani 1 d . . H46A H -0.1008(2) 0.7623(2) 0.2571(2) 0.075 Uiso 0.572(14) calc PR 1 H46B H -0.0890(2) 0.6926(2) 0.3377(2) 0.075 Uiso 0.572(14) calc PR 1 H46C H -0.0962(2) 0.7720(2) 0.2780(2) 0.075 Uiso 0.428(14) calc PR 2 H46D H -0.0896(2) 0.6554(2) 0.3381(2) 0.075 Uiso 0.428(14) calc PR 2 Li1 Li 0.1861(3) 0.8788(3) 0.3545(2) 0.0350(8) Uani 1 d . . Li2 Li 0.4016(3) 0.7791(3) 0.3017(2) 0.0350(8) Uani 1 d . . Li3 Li 0.1732(3) 0.7383(3) 0.2827(2) 0.0374(8) Uani 1 d . . Li4 Li 0.3423(4) 0.9809(3) 0.2230(2) 0.0382(8) Uani 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 0.0305(7) 0.0260(7) 0.0329(7) -0.0051(6) -0.0017(6) -0.0079(5) O2 0.0414(8) 0.0342(7) 0.0338(8) -0.0119(6) -0.0044(6) -0.0108(6) O3 0.0359(8) 0.0320(7) 0.0338(8) -0.0088(6) -0.0047(6) -0.0154(6) O4 0.0323(8) 0.0259(7) 0.0377(8) -0.0006(6) -0.0042(6) -0.0109(6) O5 0.0424(9) 0.0386(8) 0.0630(10) -0.0195(7) -0.0047(8) -0.0159(7) O6 0.0654(11) 0.0431(9) 0.0541(10) -0.0031(8) 0.0053(9) -0.0298(8) C1 0.0351(11) 0.0306(10) 0.0318(11) -0.0073(9) -0.0065(9) -0.0110(9) C2 0.0291(10) 0.0270(10) 0.0337(11) -0.0070(8) -0.0068(8) -0.0103(8) C3 0.0286(10) 0.0280(10) 0.0397(12) -0.0088(9) -0.0072(9) -0.0069(8) C4 0.0384(12) 0.0265(10) 0.0464(13) -0.0095(9) -0.0128(10) -0.0061(9) C5 0.0507(13) 0.0317(11) 0.0415(13) -0.0011(9) -0.0148(11) -0.0166(10) C6 0.0485(13) 0.0366(12) 0.0325(12) -0.0047(9) -0.0076(10) -0.0173(10) C7 0.0412(12) 0.0323(11) 0.0265(11) -0.0088(8) 0.0012(9) -0.0139(9) C8 0.0447(13) 0.0417(12) 0.0328(12) -0.0104(9) -0.0017(10) -0.0167(10) C9 0.0523(15) 0.0502(13) 0.0400(13) -0.0206(11) -0.0002(11) -0.0224(11) C10 0.0524(15) 0.0429(12) 0.0439(13) -0.0233(10) 0.0069(11) -0.0196(11) C11 0.0429(12) 0.0350(11) 0.0311(11) -0.0114(9) 0.0055(9) -0.0164(9) C12 0.0422(12) 0.0307(10) 0.0254(10) -0.0056(8) 0.0029(9) -0.0162(9) C13 0.0293(11) 0.0312(11) 0.0539(14) -0.0154(10) 0.0018(10) -0.0053(9) C14 0.0380(13) 0.065(2) 0.066(2) -0.0199(13) 0.0004(12) -0.0230(12) C15 0.0409(13) 0.063(2) 0.0459(14) -0.0234(12) 0.0071(11) -0.0188(11) C16 0.056(2) 0.0425(14) 0.088(2) -0.0195(14) 0.0216(15) -0.0001(12) C17 0.078(2) 0.0376(13) 0.0461(14) 0.0016(10) -0.0169(13) -0.0235(12) C18 0.080(2) 0.0459(14) 0.0352(13) -0.0035(11) 0.0027(12) -0.0264(13) C19 0.0407(12) 0.0381(12) 0.0452(13) -0.0182(10) 0.0067(10) -0.0119(10) C20 0.049(2) 0.059(2) 0.079(2) -0.0231(14) 0.0151(14) -0.0238(13) C21 0.054(2) 0.057(2) 0.063(2) -0.0065(13) 0.0003(13) -0.0009(13) C22 0.051(2) 0.073(2) 0.088(2) -0.051(2) 0.0073(14) -0.0094(14) C23 0.065(2) 0.073(2) 0.066(2) -0.0386(15) -0.0069(14) -0.0247(14) C24 0.0500(14) 0.0541(14) 0.0509(15) -0.0175(12) -0.0102(11) -0.0167(11) C25 0.0322(11) 0.0333(10) 0.0326(11) -0.0081(9) -0.0014(8) -0.0172(9) C26 0.0367(12) 0.0374(11) 0.0415(12) -0.0148(10) -0.0022(9) -0.0160(9) C27 0.0483(14) 0.0347(12) 0.068(2) -0.0128(11) -0.0152(12) -0.0107(10) C28 0.0511(14) 0.0511(14) 0.060(2) -0.0267(12) -0.0069(12) -0.0188(11) C29 0.0368(12) 0.0375(11) 0.0432(13) -0.0069(9) -0.0076(10) -0.0182(9) C30 0.0551(15) 0.0518(14) 0.0450(14) 0.0033(11) -0.0151(11) -0.0289(12) C31 0.0378(13) 0.0485(14) 0.072(2) -0.0121(12) -0.0093(12) -0.0099(11) C32 0.0384(12) 0.0325(11) 0.0370(12) 0.0013(9) -0.0051(9) -0.0152(9) C33 0.0438(13) 0.0494(13) 0.0439(13) 0.0026(11) -0.0060(10) -0.0237(11) C34 0.0437(14) 0.073(2) 0.056(2) -0.0099(13) 0.0071(12) -0.0176(13) C35 0.061(2) 0.089(2) 0.056(2) 0.0198(15) -0.0097(13) -0.046(2) C36 0.0465(13) 0.0298(11) 0.0508(14) 0.0039(10) -0.0108(11) -0.0125(10) C37 0.0483(14) 0.0355(12) 0.082(2) -0.0146(12) -0.0102(13) -0.0128(11) C38 0.0381(13) 0.0423(13) 0.061(2) -0.0103(11) -0.0129(11) -0.0028(10) C41 0.076(2) 0.115(3) 0.130(3) 0.028(3) -0.008(2) -0.059(2) C42 0.069(2) 0.067(2) 0.098(2) -0.003(2) 0.021(2) -0.029(2) C43 0.071(2) 0.0455(14) 0.075(2) -0.0244(13) -0.0089(14) -0.0222(13) C46 0.0421(14) 0.068(2) 0.085(2) -0.0260(15) -0.0093(13) -0.0200(13) Li1 0.036(2) 0.032(2) 0.037(2) -0.0071(14) -0.0017(15) -0.0125(14) Li2 0.033(2) 0.034(2) 0.038(2) -0.0070(15) -0.0039(15) -0.0132(14) Li3 0.038(2) 0.031(2) 0.045(2) -0.0092(15) -0.008(2) -0.0114(15) Li4 0.049(2) 0.033(2) 0.035(2) -0.0060(15) -0.004(2) -0.019(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 C2 1.328(2) . ? O1 Li3 1.870(3) . ? O1 Li1 1.914(4) . ? O2 C12 1.334(2) . ? O2 Li2 1.874(4) . ? O2 Li4 1.889(3) . ? O3 C25 1.412(2) . ? O3 Li4 1.901(4) . ? O3 Li1 1.901(4) . ? O3 Li2 1.929(3) . ? O4 C32 1.410(2) . ? O4 Li2 1.891(4) . ? O4 Li3 1.904(4) . ? O4 Li1 1.939(3) . ? O5 C46 1.435(3) . ? O5 C43 1.438(3) . ? O5 Li3 1.938(4) . ? O6 C42 1.427(3) . ? O6 C39A 1.442(5) . ? O6 C39B 1.454(8) . ? O6 Li4 1.963(4) . ? C1 C6 1.405(3) . ? C1 C2 1.415(3) . ? C1 C7 1.512(3) . ? C1 Li4 2.544(4) . ? C2 C3 1.422(3) . ? C2 Li1 2.683(4) . ? C3 C4 1.391(3) . ? C3 C13 1.539(3) . ? C4 C5 1.384(3) . ? C4 H4 0.95 . ? C5 C6 1.403(3) . ? C5 C17 1.523(3) . ? C6 C18 1.513(3) . ? C7 C8 1.406(3) . ? C7 C12 1.416(3) . ? C7 Li3 2.734(4) . ? C8 C9 1.395(3) . ? C8 C24 1.514(3) . ? C9 C10 1.389(3) . ? C9 C23 1.512(3) . ? C10 C11 1.392(3) . ? C10 H10 0.95 . ? C11 C12 1.429(3) . ? C11 C19 1.537(3) . ? C13 C16 1.531(3) . ? C13 C15 1.535(3) . ? C13 C14 1.537(3) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C21 1.517(3) . ? C19 C20 1.528(3) . ? C19 C22 1.539(3) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C29 1.533(3) . ? C25 C26 1.538(3) . ? C25 H25 1.00 . ? C26 C27 1.523(3) . ? C26 C28 1.527(3) . ? C26 H26 1.00 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 C30 1.519(3) . ? C29 C31 1.522(3) . ? C29 H29 1.00 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 C33 1.538(3) . ? C32 C36 1.539(3) . ? C32 H32 1.00 . ? C33 C34 1.521(3) . ? C33 C35 1.534(3) . ? C33 H33 1.00 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 C38 1.516(3) . ? C36 C37 1.524(3) . ? C36 H36 1.00 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39A C40A 1.517(9) . ? C39A H39A 0.99 . ? C39A H39B 0.99 . ? C40A C41 1.589(8) . ? C40A H40A 0.99 . ? C40A H40B 0.99 . ? C39B C40B 1.52(2) . ? C39B H39C 0.99 . ? C39B H39D 0.99 . ? C40B C41 1.304(10) . ? C40B H40C 0.99 . ? C40B H40D 0.99 . ? C41 C42 1.503(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C41 H41C 0.99 . ? C41 H41D 0.99 . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44A 1.483(6) . ? C43 C44B 1.561(9) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C43 H43C 0.99 . ? C43 H43D 0.99 . ? C44A C45A 1.525(10) . ? C44A H44A 0.99 . ? C44A H44B 0.99 . ? C45A C46 1.506(7) . ? C45A H45A 0.99 . ? C45A H45B 0.99 . ? C44B C45B 1.600(14) . ? C44B H44A 0.99 . ? C44B H44B 0.99 . ? C45B C46 1.449(7) . ? C45B H45A 0.99 . ? C45B H45B 0.99 . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C46 H46C 0.99 . ? C46 H46D 0.99 . ? Li1 Li2 2.334(5) . ? Li1 Li3 2.558(5) . ? Li1 Li4 3.030(5) . ? Li2 Li4 2.513(5) . ? Li2 Li3 2.836(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 C2 O1 Li3 130.3(2) . . ? C2 O1 Li1 110.36(14) . . ? Li3 O1 Li1 85.04(15) . . ? C12 O2 Li2 130.2(2) . . ? C12 O2 Li4 122.0(2) . . ? Li2 O2 Li4 83.8(2) . . ? C25 O3 Li4 114.82(15) . . ? C25 O3 Li1 133.9(2) . . ? Li4 O3 Li1 105.7(2) . . ? C25 O3 Li2 130.1(2) . . ? Li4 O3 Li2 82.04(15) . . ? Li1 O3 Li2 75.08(14) . . ? C32 O4 Li2 132.1(2) . . ? C32 O4 Li3 127.1(2) . . ? Li2 O4 Li3 96.7(2) . . ? C32 O4 Li1 122.8(2) . . ? Li2 O4 Li1 75.05(15) . . ? Li3 O4 Li1 83.44(15) . . ? C46 O5 C43 109.7(2) . . ? C46 O5 Li3 115.6(2) . . ? C43 O5 Li3 133.9(2) . . ? C42 O6 C39A 110.0(2) . . ? C42 O6 C39B 103.8(4) . . ? C42 O6 Li4 122.7(2) . . ? C39A O6 Li4 126.9(2) . . ? C39B O6 Li4 129.9(4) . . ? C6 C1 C2 121.3(2) . . ? C6 C1 C7 118.2(2) . . ? C2 C1 C7 119.8(2) . . ? C6 C1 Li4 91.02(15) . . ? C2 C1 Li4 91.12(14) . . ? C7 C1 Li4 96.20(14) . . ? O1 C2 C1 119.2(2) . . ? O1 C2 C3 121.8(2) . . ? C1 C2 C3 119.0(2) . . ? O1 C2 Li1 41.98(10) . . ? C1 C2 Li1 116.56(15) . . ? C3 C2 Li1 108.24(14) . . ? C4 C3 C2 117.2(2) . . ? C4 C3 C13 121.6(2) . . ? C2 C3 C13 121.1(2) . . ? C5 C4 C3 124.4(2) . . ? C5 C4 H4 117.78(12) . . ? C3 C4 H4 117.78(12) . . ? C4 C5 C6 118.3(2) . . ? C4 C5 C17 119.5(2) . . ? C6 C5 C17 122.1(2) . . ? C5 C6 C1 119.2(2) . . ? C5 C6 C18 120.8(2) . . ? C1 C6 C18 119.9(2) . . ? C8 C7 C12 121.7(2) . . ? C8 C7 C1 117.2(2) . . ? C12 C7 C1 120.7(2) . . ? C8 C7 Li3 103.39(15) . . ? C12 C7 Li3 78.06(13) . . ? C1 C7 Li3 94.84(13) . . ? C9 C8 C7 119.3(2) . . ? C9 C8 C24 120.6(2) . . ? C7 C8 C24 120.1(2) . . ? C10 C9 C8 118.4(2) . . ? C10 C9 C23 119.8(2) . . ? C8 C9 C23 121.7(2) . . ? C9 C10 C11 124.5(2) . . ? C9 C10 H10 117.73(12) . . ? C11 C10 H10 117.73(12) . . ? C10 C11 C12 117.1(2) . . ? C10 C11 C19 121.1(2) . . ? C12 C11 C19 121.7(2) . . ? O2 C12 C7 119.0(2) . . ? O2 C12 C11 122.4(2) . . ? C7 C12 C11 118.6(2) . . ? C16 C13 C15 106.6(2) . . ? C16 C13 C14 108.0(2) . . ? C15 C13 C14 108.6(2) . . ? C16 C13 C3 112.2(2) . . ? C15 C13 C3 112.3(2) . . ? C14 C13 C3 108.9(2) . . ? C13 C14 H14A 109.47(13) . . ? C13 C14 H14B 109.47(12) . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.47(13) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.47(12) . . ? C13 C15 H15B 109.47(11) . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.47(12) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.47(14) . . ? C13 C16 H16B 109.5(2) . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.47(14) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 C17 H17A 109.47(12) . . ? C5 C17 H17B 109.47(13) . . ? H17A C17 H17B 109.5 . . ? C5 C17 H17C 109.47(13) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C6 C18 H18A 109.47(14) . . ? C6 C18 H18B 109.47(12) . . ? H18A C18 H18B 109.5 . . ? C6 C18 H18C 109.47(12) . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 109.0(2) . . ? C21 C19 C11 111.2(2) . . ? C20 C19 C11 109.8(2) . . ? C21 C19 C22 107.8(2) . . ? C20 C19 C22 106.5(2) . . ? C11 C19 C22 112.4(2) . . ? C19 C20 H20A 109.5(2) . . ? C19 C20 H20B 109.47(13) . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.47(13) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.47(15) . . ? C19 C21 H21B 109.47(13) . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.47(13) . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5(2) . . ? C19 C22 H22B 109.47(14) . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.47(14) . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C9 C23 H23A 109.47(15) . . ? C9 C23 H23B 109.47(14) . . ? H23A C23 H23B 109.5 . . ? C9 C23 H23C 109.47(14) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 C24 H24A 109.47(13) . . ? C8 C24 H24B 109.47(12) . . ? H24A C24 H24B 109.5 . . ? C8 C24 H24C 109.47(12) . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 C29 112.1(2) . . ? O3 C25 C26 111.2(2) . . ? C29 C25 C26 113.5(2) . . ? O3 C25 H25 106.50(10) . . ? C29 C25 H25 106.50(11) . . ? C26 C25 H25 106.50(11) . . ? C27 C26 C28 108.7(2) . . ? C27 C26 C25 110.5(2) . . ? C28 C26 C25 112.9(2) . . ? C27 C26 H26 108.15(12) . . ? C28 C26 H26 108.15(13) . . ? C25 C26 H26 108.15(11) . . ? C26 C27 H27A 109.47(12) . . ? C26 C27 H27B 109.47(12) . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.47(11) . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.47(12) . . ? C26 C28 H28B 109.47(12) . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.47(12) . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C31 111.0(2) . . ? C30 C29 C25 112.8(2) . . ? C31 C29 C25 111.2(2) . . ? C30 C29 H29 107.17(12) . . ? C31 C29 H29 107.17(12) . . ? C25 C29 H29 107.17(10) . . ? C29 C30 H30A 109.47(12) . . ? C29 C30 H30B 109.47(12) . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.47(12) . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.47(13) . . ? C29 C31 H31B 109.47(12) . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.47(13) . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 C32 C33 112.1(2) . . ? O4 C32 C36 111.8(2) . . ? C33 C32 C36 112.8(2) . . ? O4 C32 H32 106.54(10) . . ? C33 C32 H32 106.54(13) . . ? C36 C32 H32 106.54(12) . . ? C34 C33 C35 108.9(2) . . ? C34 C33 C32 111.0(2) . . ? C35 C33 C32 111.8(2) . . ? C34 C33 H33 108.35(14) . . ? C35 C33 H33 108.35(15) . . ? C32 C33 H33 108.35(13) . . ? C33 C34 H34A 109.47(13) . . ? C33 C34 H34B 109.47(14) . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.47(13) . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.47(14) . . ? C33 C35 H35B 109.5(2) . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.47(13) . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C37 111.2(2) . . ? C38 C36 C32 110.7(2) . . ? C37 C36 C32 112.5(2) . . ? C38 C36 H36 107.39(13) . . ? C37 C36 H36 107.39(12) . . ? C32 C36 H36 107.39(11) . . ? C36 C37 H37A 109.47(12) . . ? C36 C37 H37B 109.47(13) . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.47(12) . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.47(13) . . ? C36 C38 H38B 109.47(13) . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.47(12) . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O6 C39A C40A 100.8(4) . . ? O6 C39A H39A 111.6(2) . . ? C40A C39A H39A 111.6(4) . . ? O6 C39A H39B 111.6(3) . . ? C40A C39A H39B 111.6(5) . . ? H39A C39A H39B 109.4 . . ? C39A C40A C41 99.5(5) . . ? C39A C40A H40A 111.9(5) . . ? C41 C40A H40A 111.9(3) . . ? C39A C40A H40B 111.9(3) . . ? C41 C40A H40B 111.9(3) . . ? H40A C40A H40B 109.6 . . ? O6 C39B C40B 102.1(7) . . ? O6 C39B H39C 111.4(5) . . ? C40B C39B H39C 111.4(9) . . ? O6 C39B H39D 111.4(5) . . ? C40B C39B H39D 111.4(6) . . ? H39C C39B H39D 109.2 . . ? C41 C40B C39B 102.9(9) . . ? C41 C40B H40C 111.2(7) . . ? C39B C40B H40C 111.2(9) . . ? C41 C40B H40D 111.2(5) . . ? C39B C40B H40D 111.2(7) . . ? H40C C40B H40D 109.1 . . ? C40B C41 C42 106.6(5) . . ? C42 C41 C40A 102.5(3) . . ? C42 C41 H41A 111.3(2) . . ? C40A C41 H41A 111.3(3) . . ? C42 C41 H41B 111.3(2) . . ? C40A C41 H41B 111.3(3) . . ? H41A C41 H41B 109.2 . . ? C40B C41 H41C 110.4(7) . . ? C42 C41 H41C 110.4(2) . . ? C40B C41 H41D 110.4(6) . . ? C42 C41 H41D 110.4(2) . . ? H41C C41 H41D 108.6 . . ? O6 C42 C41 106.2(3) . . ? O6 C42 H42A 110.5(2) . . ? C41 C42 H42A 110.5(2) . . ? O6 C42 H42B 110.5(2) . . ? C41 C42 H42B 110.5(2) . . ? H42A C42 H42B 108.7 . . ? O5 C43 C44A 107.7(3) . . ? O5 C43 C44B 102.0(4) . . ? O5 C43 H43A 110.17(14) . . ? C44A C43 H43A 110.2(3) . . ? O5 C43 H43B 110.17(13) . . ? C44A C43 H43B 110.2(4) . . ? H43A C43 H43B 108.5 . . ? O5 C43 H43C 111.36(13) . . ? C44B C43 H43C 111.4(4) . . ? O5 C43 H43D 111.36(13) . . ? C44B C43 H43D 111.4(5) . . ? H43C C43 H43D 109.2 . . ? C43 C44A C45A 102.5(5) . . ? C43 C44A H44A 111.3(3) . . ? C45A C44A H44A 111.3(5) . . ? C43 C44A H44B 111.3(4) . . ? C45A C44A H44B 111.3(6) . . ? H44A C44A H44B 109.2 . . ? C46 C45A C44A 104.3(5) . . ? C46 C45A H45A 110.9(3) . . ? C44A C45A H45A 110.9(5) . . ? C46 C45A H45B 110.9(4) . . ? C44A C45A H45B 110.9(6) . . ? H45A C45A H45B 108.9 . . ? C43 C44B C45B 99.8(7) . . ? C43 C44B H44A 111.8(5) . . ? C45B C44B H44A 111.8(8) . . ? C43 C44B H44B 111.8(4) . . ? C45B C44B H44B 111.8(6) . . ? H44A C44B H44B 109.5 . . ? C46 C45B C44B 96.3(7) . . ? C46 C45B H45A 112.5(5) . . ? C44B C45B H45A 112.5(8) . . ? C46 C45B H45B 112.5(4) . . ? C44B C45B H45B 112.5(6) . . ? H45A C45B H45B 110.0 . . ? O5 C46 C45B 107.8(3) . . ? O5 C46 C45A 106.0(3) . . ? O5 C46 H46A 110.53(14) . . ? C45A C46 H46A 110.5(4) . . ? O5 C46 H46B 110.53(13) . . ? C45A C46 H46B 110.5(4) . . ? H46A C46 H46B 108.7 . . ? O5 C46 H46C 110.14(13) . . ? C45B C46 H46C 110.1(4) . . ? O5 C46 H46D 110.14(14) . . ? C45B C46 H46D 110.1(5) . . ? H46C C46 H46D 108.5 . . ? O3 Li1 O1 119.6(2) . . ? O3 Li1 O4 102.4(2) . . ? O1 Li1 O4 94.0(2) . . ? O3 Li1 Li2 53.00(12) . . ? O1 Li1 Li2 104.6(2) . . ? O4 Li1 Li2 51.55(12) . . ? O3 Li1 Li3 116.6(2) . . ? O1 Li1 Li3 46.76(11) . . ? O4 Li1 Li3 47.69(11) . . ? Li2 Li1 Li3 70.72(14) . . ? O3 Li1 C2 95.38(14) . . ? O1 Li1 C2 27.66(7) . . ? O4 Li1 C2 114.0(2) . . ? Li2 Li1 C2 101.5(2) . . ? Li3 Li1 C2 67.44(12) . . ? O3 Li1 Li4 37.16(10) . . ? O1 Li1 Li4 82.88(13) . . ? O4 Li1 Li4 101.51(15) . . ? Li2 Li1 Li4 54.01(12) . . ? Li3 Li1 Li4 88.22(14) . . ? C2 Li1 Li4 61.47(10) . . ? O2 Li2 O4 118.7(2) . . ? O2 Li2 O3 96.8(2) . . ? O4 Li2 O3 103.1(2) . . ? O2 Li2 Li1 106.3(2) . . ? O4 Li2 Li1 53.41(12) . . ? O3 Li2 Li1 51.92(12) . . ? O2 Li2 Li4 48.34(11) . . ? O4 Li2 Li4 124.5(2) . . ? O3 Li2 Li4 48.50(11) . . ? Li1 Li2 Li4 77.28(15) . . ? O2 Li2 Li3 77.27(14) . . ? O4 Li2 Li3 41.81(11) . . ? O3 Li2 Li3 104.5(2) . . ? Li1 Li2 Li3 58.34(13) . . ? Li4 Li2 Li3 93.53(15) . . ? O1 Li3 O4 96.6(2) . . ? O1 Li3 O5 117.4(2) . . ? O4 Li3 O5 127.1(2) . . ? O1 Li3 Li1 48.20(11) . . ? O4 Li3 Li1 48.87(11) . . ? O5 Li3 Li1 148.2(2) . . ? O1 Li3 C7 73.46(12) . . ? O4 Li3 C7 125.3(2) . . ? O5 Li3 C7 103.5(2) . . ? Li1 Li3 C7 98.33(14) . . ? O1 Li3 Li2 89.05(14) . . ? O4 Li3 Li2 41.47(10) . . ? O5 Li3 Li2 153.5(2) . . ? Li1 Li3 Li2 50.94(12) . . ? C7 Li3 Li2 84.04(12) . . ? O2 Li4 O3 97.2(2) . . ? O2 Li4 O6 115.5(2) . . ? O3 Li4 O6 120.9(2) . . ? O2 Li4 Li2 47.85(11) . . ? O3 Li4 Li2 49.46(12) . . ? O6 Li4 Li2 133.1(2) . . ? O2 Li4 C1 78.57(13) . . ? O3 Li4 C1 115.0(2) . . ? O6 Li4 C1 118.7(2) . . ? Li2 Li4 C1 101.63(14) . . ? O2 Li4 Li1 83.33(13) . . ? O3 Li4 Li1 37.16(10) . . ? O6 Li4 Li1 155.6(2) . . ? Li2 Li4 Li1 48.70(11) . . ? C1 Li4 Li1 78.56(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li3 O1 C2 C1 -2.8(3) . . . . ? Li1 O1 C2 C1 98.3(2) . . . . ? Li3 O1 C2 C3 176.8(2) . . . . ? Li1 O1 C2 C3 -82.1(2) . . . . ? Li3 O1 C2 Li1 -101.2(2) . . . . ? Li1 O1 C2 Li1 0.0 . . . . ? C6 C1 C2 O1 -173.4(2) . . . . ? C7 C1 C2 O1 16.3(3) . . . . ? Li4 C1 C2 O1 -81.5(2) . . . . ? C6 C1 C2 C3 7.0(3) . . . . ? C7 C1 C2 C3 -163.3(2) . . . . ? Li4 C1 C2 C3 98.9(2) . . . . ? C6 C1 C2 Li1 -125.7(2) . . . . ? C7 C1 C2 Li1 64.0(2) . . . . ? Li4 C1 C2 Li1 -33.8(2) . . . . ? O1 C2 C3 C4 174.1(2) . . . . ? C1 C2 C3 C4 -6.3(3) . . . . ? Li1 C2 C3 C4 129.9(2) . . . . ? O1 C2 C3 C13 -9.4(3) . . . . ? C1 C2 C3 C13 170.2(2) . . . . ? Li1 C2 C3 C13 -53.6(2) . . . . ? C2 C3 C4 C5 0.9(3) . . . . ? C13 C3 C4 C5 -175.5(2) . . . . ? C3 C4 C5 C6 4.0(3) . . . . ? C3 C4 C5 C17 -178.5(2) . . . . ? C4 C5 C6 C1 -3.3(3) . . . . ? C17 C5 C6 C1 179.3(2) . . . . ? C4 C5 C6 C18 175.4(2) . . . . ? C17 C5 C6 C18 -2.1(3) . . . . ? C2 C1 C6 C5 -2.1(3) . . . . ? C7 C1 C6 C5 168.4(2) . . . . ? Li4 C1 C6 C5 -94.0(2) . . . . ? C2 C1 C6 C18 179.2(2) . . . . ? C7 C1 C6 C18 -10.3(3) . . . . ? Li4 C1 C6 C18 87.3(2) . . . . ? C6 C1 C7 C8 -78.8(2) . . . . ? C2 C1 C7 C8 91.8(2) . . . . ? Li4 C1 C7 C8 -173.3(2) . . . . ? C6 C1 C7 C12 94.5(2) . . . . ? C2 C1 C7 C12 -94.9(2) . . . . ? Li4 C1 C7 C12 -0.1(2) . . . . ? C6 C1 C7 Li3 173.4(2) . . . . ? C2 C1 C7 Li3 -15.9(2) . . . . ? Li4 C1 C7 Li3 78.93(13) . . . . ? C12 C7 C8 C9 -3.9(3) . . . . ? C1 C7 C8 C9 169.3(2) . . . . ? Li3 C7 C8 C9 -88.0(2) . . . . ? C12 C7 C8 C24 176.6(2) . . . . ? C1 C7 C8 C24 -10.2(3) . . . . ? Li3 C7 C8 C24 92.5(2) . . . . ? C7 C8 C9 C10 -1.4(3) . . . . ? C24 C8 C9 C10 178.0(2) . . . . ? C7 C8 C9 C23 -178.8(2) . . . . ? C24 C8 C9 C23 0.7(3) . . . . ? C8 C9 C10 C11 2.8(4) . . . . ? C23 C9 C10 C11 -179.7(2) . . . . ? C9 C10 C11 C12 1.1(3) . . . . ? C9 C10 C11 C19 -175.4(2) . . . . ? Li2 O2 C12 C7 88.2(2) . . . . ? Li4 O2 C12 C7 -23.1(3) . . . . ? Li2 O2 C12 C11 -93.9(2) . . . . ? Li4 O2 C12 C11 154.9(2) . . . . ? C8 C7 C12 O2 -174.2(2) . . . . ? C1 C7 C12 O2 12.9(3) . . . . ? Li3 C7 C12 O2 -75.7(2) . . . . ? C8 C7 C12 C11 7.8(3) . . . . ? C1 C7 C12 C11 -165.2(2) . . . . ? Li3 C7 C12 C11 106.3(2) . . . . ? C10 C11 C12 O2 175.8(2) . . . . ? C19 C11 C12 O2 -7.8(3) . . . . ? C10 C11 C12 C7 -6.2(3) . . . . ? C19 C11 C12 C7 170.2(2) . . . . ? C4 C3 C13 C16 -1.8(3) . . . . ? C2 C3 C13 C16 -178.2(2) . . . . ? C4 C3 C13 C15 -122.0(2) . . . . ? C2 C3 C13 C15 61.7(2) . . . . ? C4 C3 C13 C14 117.6(2) . . . . ? C2 C3 C13 C14 -58.7(2) . . . . ? C10 C11 C19 C21 -115.2(2) . . . . ? C12 C11 C19 C21 68.5(3) . . . . ? C10 C11 C19 C20 124.0(2) . . . . ? C12 C11 C19 C20 -52.2(3) . . . . ? C10 C11 C19 C22 5.8(3) . . . . ? C12 C11 C19 C22 -170.5(2) . . . . ? Li4 O3 C25 C29 -128.6(2) . . . . ? Li1 O3 C25 C29 82.3(2) . . . . ? Li2 O3 C25 C29 -27.7(3) . . . . ? Li4 O3 C25 C26 103.1(2) . . . . ? Li1 O3 C25 C26 -46.0(3) . . . . ? Li2 O3 C25 C26 -156.0(2) . . . . ? O3 C25 C26 C27 -64.9(2) . . . . ? C29 C25 C26 C27 167.6(2) . . . . ? O3 C25 C26 C28 173.0(2) . . . . ? C29 C25 C26 C28 45.5(2) . . . . ? O3 C25 C29 C30 -65.0(2) . . . . ? C26 C25 C29 C30 62.1(2) . . . . ? O3 C25 C29 C31 60.5(2) . . . . ? C26 C25 C29 C31 -172.5(2) . . . . ? Li2 O4 C32 C33 171.8(2) . . . . ? Li3 O4 C32 C33 -36.4(3) . . . . ? Li1 O4 C32 C33 72.1(2) . . . . ? Li2 O4 C32 C36 -60.4(3) . . . . ? Li3 O4 C32 C36 91.4(2) . . . . ? Li1 O4 C32 C36 -160.1(2) . . . . ? O4 C32 C33 C34 -53.3(3) . . . . ? C36 C32 C33 C34 179.4(2) . . . . ? O4 C32 C33 C35 -175.1(2) . . . . ? C36 C32 C33 C35 57.6(3) . . . . ? O4 C32 C36 C38 63.8(2) . . . . ? C33 C32 C36 C38 -168.8(2) . . . . ? O4 C32 C36 C37 -61.3(2) . . . . ? C33 C32 C36 C37 66.1(2) . . . . ? C42 O6 C39A C40A -38.9(6) . . . . ? C39B O6 C39A C40A 41.3(10) . . . . ? Li4 O6 C39A C40A 148.0(4) . . . . ? O6 C39A C40A C41 44.4(6) . . . . ? C42 O6 C39B C40B 31.4(11) . . . . ? C39A O6 C39B C40B -76.1(12) . . . . ? Li4 O6 C39B C40B -170.0(6) . . . . ? O6 C39B C40B C41 -43.7(14) . . . . ? C39B C40B C41 C42 36.8(12) . . . . ? C39B C40B C41 C40A -49.8(11) . . . . ? C39A C40A C41 C40B 65.5(10) . . . . ? C39A C40A C41 C42 -36.0(6) . . . . ? C39A O6 C42 C41 15.1(5) . . . . ? C39B O6 C42 C41 -10.9(6) . . . . ? Li4 O6 C42 C41 -171.4(3) . . . . ? C40B C41 C42 O6 -17.6(8) . . . . ? C40A C41 C42 O6 14.1(5) . . . . ? C46 O5 C43 C44A 12.3(5) . . . . ? Li3 O5 C43 C44A -157.5(4) . . . . ? C46 O5 C43 C44B -11.7(6) . . . . ? Li3 O5 C43 C44B 178.5(5) . . . . ? O5 C43 C44A C45A -26.9(8) . . . . ? C44B C43 C44A C45A 52.7(11) . . . . ? C43 C44A C45A C46 31.0(9) . . . . ? O5 C43 C44B C45B 36.3(9) . . . . ? C44A C43 C44B C45B -70.4(12) . . . . ? C43 C44B C45B C46 -47.1(10) . . . . ? C43 O5 C46 C45B -21.1(6) . . . . ? Li3 O5 C46 C45B 150.8(5) . . . . ? C43 O5 C46 C45A 8.0(5) . . . . ? Li3 O5 C46 C45A 179.9(4) . . . . ? C44B C45B C46 O5 42.2(9) . . . . ? C44B C45B C46 C45A -48.4(9) . . . . ? C44A C45A C46 O5 -24.5(8) . . . . ? C44A C45A C46 C45B 73.5(10) . . . . ? C25 O3 Li1 O1 141.8(2) . . . . ? Li4 O3 Li1 O1 -9.2(2) . . . . ? Li2 O3 Li1 O1 -86.3(2) . . . . ? C25 O3 Li1 O4 -116.2(2) . . . . ? Li4 O3 Li1 O4 92.8(2) . . . . ? Li2 O3 Li1 O4 15.7(2) . . . . ? C25 O3 Li1 Li2 -131.9(2) . . . . ? Li4 O3 Li1 Li2 77.1(2) . . . . ? Li2 O3 Li1 Li2 0.0 . . . . ? C25 O3 Li1 Li3 -164.9(2) . . . . ? Li4 O3 Li1 Li3 44.1(2) . . . . ? Li2 O3 Li1 Li3 -32.9(2) . . . . ? C25 O3 Li1 C2 127.7(2) . . . . ? Li4 O3 Li1 C2 -23.3(2) . . . . ? Li2 O3 Li1 C2 -100.37(15) . . . . ? C25 O3 Li1 Li4 151.0(2) . . . . ? Li4 O3 Li1 Li4 0.0 . . . . ? Li2 O3 Li1 Li4 -77.1(2) . . . . ? C2 O1 Li1 O3 -31.4(2) . . . . ? Li3 O1 Li1 O3 99.9(2) . . . . ? C2 O1 Li1 O4 -138.13(14) . . . . ? Li3 O1 Li1 O4 -6.8(2) . . . . ? C2 O1 Li1 Li2 -86.9(2) . . . . ? Li3 O1 Li1 Li2 44.4(2) . . . . ? C2 O1 Li1 Li3 -131.3(2) . . . . ? Li3 O1 Li1 Li3 0.0 . . . . ? C2 O1 Li1 C2 0.0 . . . . ? Li3 O1 Li1 C2 131.3(2) . . . . ? C2 O1 Li1 Li4 -37.03(15) . . . . ? Li3 O1 Li1 Li4 94.27(14) . . . . ? C32 O4 Li1 O3 114.8(2) . . . . ? Li2 O4 Li1 O3 -16.0(2) . . . . ? Li3 O4 Li1 O3 -114.8(2) . . . . ? C32 O4 Li1 O1 -123.7(2) . . . . ? Li2 O4 Li1 O1 105.5(2) . . . . ? Li3 O4 Li1 O1 6.7(2) . . . . ? C32 O4 Li1 Li2 130.8(2) . . . . ? Li2 O4 Li1 Li2 0.0 . . . . ? Li3 O4 Li1 Li2 -98.8(2) . . . . ? C32 O4 Li1 Li3 -130.4(2) . . . . ? Li2 O4 Li1 Li3 98.8(2) . . . . ? Li3 O4 Li1 Li3 0.0 . . . . ? C32 O4 Li1 C2 -143.5(2) . . . . ? Li2 O4 Li1 C2 85.7(2) . . . . ? Li3 O4 Li1 C2 -13.1(2) . . . . ? C32 O4 Li1 Li4 152.75(15) . . . . ? Li2 O4 Li1 Li4 21.97(14) . . . . ? Li3 O4 Li1 Li4 -76.8(2) . . . . ? O1 C2 Li1 O3 152.9(2) . . . . ? C1 C2 Li1 O3 47.9(2) . . . . ? C3 C2 Li1 O3 -89.5(2) . . . . ? O1 C2 Li1 O1 0.0 . . . . ? C1 C2 Li1 O1 -105.1(2) . . . . ? C3 C2 Li1 O1 117.5(2) . . . . ? O1 C2 Li1 O4 46.8(2) . . . . ? C1 C2 Li1 O4 -58.3(2) . . . . ? C3 C2 Li1 O4 164.3(2) . . . . ? O1 C2 Li1 Li2 99.6(2) . . . . ? C1 C2 Li1 Li2 -5.4(2) . . . . ? C3 C2 Li1 Li2 -142.8(2) . . . . ? O1 C2 Li1 Li3 36.34(14) . . . . ? C1 C2 Li1 Li3 -68.7(2) . . . . ? C3 C2 Li1 Li3 153.9(2) . . . . ? O1 C2 Li1 Li4 137.1(2) . . . . ? C1 C2 Li1 Li4 32.1(2) . . . . ? C3 C2 Li1 Li4 -105.30(15) . . . . ? C12 O2 Li2 O4 -15.2(3) . . . . ? Li4 O2 Li2 O4 112.2(2) . . . . ? C12 O2 Li2 O3 -124.2(2) . . . . ? Li4 O2 Li2 O3 3.2(2) . . . . ? C12 O2 Li2 Li1 -72.0(2) . . . . ? Li4 O2 Li2 Li1 55.4(2) . . . . ? C12 O2 Li2 Li4 -127.4(2) . . . . ? Li4 O2 Li2 Li4 0.0 . . . . ? C12 O2 Li2 Li3 -20.8(2) . . . . ? Li4 O2 Li2 Li3 106.58(14) . . . . ? C32 O4 Li2 O2 149.5(2) . . . . ? Li3 O4 Li2 O2 -8.2(2) . . . . ? Li1 O4 Li2 O2 -89.6(2) . . . . ? C32 O4 Li2 O3 -105.1(2) . . . . ? Li3 O4 Li2 O3 97.2(2) . . . . ? Li1 O4 Li2 O3 15.8(2) . . . . ? C32 O4 Li2 Li1 -120.9(2) . . . . ? Li3 O4 Li2 Li1 81.3(2) . . . . ? Li1 O4 Li2 Li1 0.0 . . . . ? C32 O4 Li2 Li4 -153.4(2) . . . . ? Li3 O4 Li2 Li4 48.9(2) . . . . ? Li1 O4 Li2 Li4 -32.4(2) . . . . ? C32 O4 Li2 Li3 157.7(2) . . . . ? Li3 O4 Li2 Li3 0.0 . . . . ? Li1 O4 Li2 Li3 -81.3(2) . . . . ? C25 O3 Li2 O2 -119.0(2) . . . . ? Li4 O3 Li2 O2 -3.2(2) . . . . ? Li1 O3 Li2 O2 105.5(2) . . . . ? C25 O3 Li2 O4 119.3(2) . . . . ? Li4 O3 Li2 O4 -124.8(2) . . . . ? Li1 O3 Li2 O4 -16.2(2) . . . . ? C25 O3 Li2 Li1 135.5(2) . . . . ? Li4 O3 Li2 Li1 -108.6(2) . . . . ? Li1 O3 Li2 Li1 0.0 . . . . ? C25 O3 Li2 Li4 -115.9(2) . . . . ? Li4 O3 Li2 Li4 0.0 . . . . ? Li1 O3 Li2 Li4 108.6(2) . . . . ? C25 O3 Li2 Li3 162.4(2) . . . . ? Li4 O3 Li2 Li3 -81.7(2) . . . . ? Li1 O3 Li2 Li3 26.9(2) . . . . ? O3 Li1 Li2 O2 -85.8(2) . . . . ? O1 Li1 Li2 O2 30.5(2) . . . . ? O4 Li1 Li2 O2 114.0(2) . . . . ? Li3 Li1 Li2 O2 63.2(2) . . . . ? C2 Li1 Li2 O2 2.3(2) . . . . ? Li4 Li1 Li2 O2 -39.09(13) . . . . ? O3 Li1 Li2 O4 160.3(2) . . . . ? O1 Li1 Li2 O4 -83.4(2) . . . . ? O4 Li1 Li2 O4 0.0 . . . . ? Li3 Li1 Li2 O4 -50.74(12) . . . . ? C2 Li1 Li2 O4 -111.7(2) . . . . ? Li4 Li1 Li2 O4 -153.1(2) . . . . ? O3 Li1 Li2 O3 0.0 . . . . ? O1 Li1 Li2 O3 116.3(2) . . . . ? O4 Li1 Li2 O3 -160.3(2) . . . . ? Li3 Li1 Li2 O3 149.0(2) . . . . ? C2 Li1 Li2 O3 88.07(14) . . . . ? Li4 Li1 Li2 O3 46.68(12) . . . . ? O3 Li1 Li2 Li4 -46.68(12) . . . . ? O1 Li1 Li2 Li4 69.6(2) . . . . ? O4 Li1 Li2 Li4 153.1(2) . . . . ? Li3 Li1 Li2 Li4 102.32(15) . . . . ? C2 Li1 Li2 Li4 41.39(14) . . . . ? Li4 Li1 Li2 Li4 0.0 . . . . ? O3 Li1 Li2 Li3 -149.0(2) . . . . ? O1 Li1 Li2 Li3 -32.69(13) . . . . ? O4 Li1 Li2 Li3 50.74(12) . . . . ? Li3 Li1 Li2 Li3 0.0 . . . . ? C2 Li1 Li2 Li3 -60.93(13) . . . . ? Li4 Li1 Li2 Li3 -102.32(15) . . . . ? C2 O1 Li3 O4 119.6(2) . . . . ? Li1 O1 Li3 O4 7.0(2) . . . . ? C2 O1 Li3 O5 -102.3(2) . . . . ? Li1 O1 Li3 O5 145.1(2) . . . . ? C2 O1 Li3 Li1 112.6(2) . . . . ? Li1 O1 Li3 Li1 0.0 . . . . ? C2 O1 Li3 C7 -5.3(2) . . . . ? Li1 O1 Li3 C7 -117.92(12) . . . . ? C2 O1 Li3 Li2 78.7(2) . . . . ? Li1 O1 Li3 Li2 -33.86(14) . . . . ? C32 O4 Li3 O1 119.7(2) . . . . ? Li2 O4 Li3 O1 -81.0(2) . . . . ? Li1 O4 Li3 O1 -6.9(2) . . . . ? C32 O4 Li3 O5 -12.3(3) . . . . ? Li2 O4 Li3 O5 147.0(2) . . . . ? Li1 O4 Li3 O5 -139.0(2) . . . . ? C32 O4 Li3 Li1 126.6(2) . . . . ? Li2 O4 Li3 Li1 -74.03(15) . . . . ? Li1 O4 Li3 Li1 0.0 . . . . ? C32 O4 Li3 C7 -165.9(2) . . . . ? Li2 O4 Li3 C7 -6.5(2) . . . . ? Li1 O4 Li3 C7 67.5(2) . . . . ? C32 O4 Li3 Li2 -159.4(2) . . . . ? Li2 O4 Li3 Li2 0.0 . . . . ? Li1 O4 Li3 Li2 74.03(15) . . . . ? C46 O5 Li3 O1 -17.9(3) . . . . ? C43 O5 Li3 O1 151.4(2) . . . . ? C46 O5 Li3 O4 105.8(3) . . . . ? C43 O5 Li3 O4 -84.8(3) . . . . ? C46 O5 Li3 Li1 36.0(4) . . . . ? C43 O5 Li3 Li1 -154.6(3) . . . . ? C46 O5 Li3 C7 -96.1(2) . . . . ? C43 O5 Li3 C7 73.2(3) . . . . ? C46 O5 Li3 Li2 159.8(4) . . . . ? C43 O5 Li3 Li2 -30.9(6) . . . . ? O3 Li1 Li3 O1 -106.8(2) . . . . ? O1 Li1 Li3 O1 0.0 . . . . ? O4 Li1 Li3 O1 170.8(2) . . . . ? Li2 Li1 Li3 O1 -134.2(2) . . . . ? C2 Li1 Li3 O1 -22.19(9) . . . . ? Li4 Li1 Li3 O1 -81.89(14) . . . . ? O3 Li1 Li3 O4 82.5(2) . . . . ? O1 Li1 Li3 O4 -170.8(2) . . . . ? O4 Li1 Li3 O4 0.0 . . . . ? Li2 Li1 Li3 O4 55.08(13) . . . . ? C2 Li1 Li3 O4 167.1(2) . . . . ? Li4 Li1 Li3 O4 107.35(15) . . . . ? O3 Li1 Li3 O5 178.9(3) . . . . ? O1 Li1 Li3 O5 -74.4(3) . . . . ? O4 Li1 Li3 O5 96.4(4) . . . . ? Li2 Li1 Li3 O5 151.5(4) . . . . ? C2 Li1 Li3 O5 -96.5(4) . . . . ? Li4 Li1 Li3 O5 -156.2(3) . . . . ? O3 Li1 Li3 C7 -47.9(2) . . . . ? O1 Li1 Li3 C7 58.88(12) . . . . ? O4 Li1 Li3 C7 -130.4(2) . . . . ? Li2 Li1 Li3 C7 -75.29(14) . . . . ? C2 Li1 Li3 C7 36.69(10) . . . . ? Li4 Li1 Li3 C7 -23.02(13) . . . . ? O3 Li1 Li3 Li2 27.4(2) . . . . ? O1 Li1 Li3 Li2 134.2(2) . . . . ? O4 Li1 Li3 Li2 -55.08(13) . . . . ? Li2 Li1 Li3 Li2 0.0 . . . . ? C2 Li1 Li3 Li2 111.97(14) . . . . ? Li4 Li1 Li3 Li2 52.27(12) . . . . ? C8 C7 Li3 O1 -108.9(2) . . . . ? C12 C7 Li3 O1 131.0(2) . . . . ? C1 C7 Li3 O1 10.63(14) . . . . ? C8 C7 Li3 O4 164.7(2) . . . . ? C12 C7 Li3 O4 44.6(2) . . . . ? C1 C7 Li3 O4 -75.8(2) . . . . ? C8 C7 Li3 O5 6.2(2) . . . . ? C12 C7 Li3 O5 -114.0(2) . . . . ? C1 C7 Li3 O5 125.6(2) . . . . ? C8 C7 Li3 Li1 -150.6(2) . . . . ? C12 C7 Li3 Li1 89.3(2) . . . . ? C1 C7 Li3 Li1 -31.1(2) . . . . ? C8 C7 Li3 Li2 160.4(2) . . . . ? C12 C7 Li3 Li2 40.26(13) . . . . ? C1 C7 Li3 Li2 -80.14(14) . . . . ? O2 Li2 Li3 O1 -86.22(15) . . . . ? O4 Li2 Li3 O1 101.2(2) . . . . ? O3 Li2 Li3 O1 7.6(2) . . . . ? Li1 Li2 Li3 O1 32.33(14) . . . . ? Li4 Li2 Li3 O1 -40.4(2) . . . . ? O2 Li2 Li3 O4 172.6(2) . . . . ? O4 Li2 Li3 O4 0.0 . . . . ? O3 Li2 Li3 O4 -93.6(2) . . . . ? Li1 Li2 Li3 O4 -68.8(2) . . . . ? Li4 Li2 Li3 O4 -141.5(2) . . . . ? O2 Li2 Li3 O5 95.8(4) . . . . ? O4 Li2 Li3 O5 -76.8(4) . . . . ? O3 Li2 Li3 O5 -170.4(4) . . . . ? Li1 Li2 Li3 O5 -145.7(5) . . . . ? Li4 Li2 Li3 O5 141.6(4) . . . . ? O2 Li2 Li3 Li1 -118.6(2) . . . . ? O4 Li2 Li3 Li1 68.8(2) . . . . ? O3 Li2 Li3 Li1 -24.76(14) . . . . ? Li1 Li2 Li3 Li1 0.0 . . . . ? Li4 Li2 Li3 Li1 -72.7(2) . . . . ? O2 Li2 Li3 C7 -12.75(11) . . . . ? O4 Li2 Li3 C7 174.6(2) . . . . ? O3 Li2 Li3 C7 81.04(15) . . . . ? Li1 Li2 Li3 C7 105.80(14) . . . . ? Li4 Li2 Li3 C7 33.09(13) . . . . ? C12 O2 Li4 O3 131.1(2) . . . . ? Li2 O2 Li4 O3 -3.2(2) . . . . ? C12 O2 Li4 O6 -99.6(2) . . . . ? Li2 O2 Li4 O6 126.1(2) . . . . ? C12 O2 Li4 Li2 134.3(2) . . . . ? Li2 O2 Li4 Li2 0.0 . . . . ? C12 O2 Li4 C1 16.9(2) . . . . ? Li2 O2 Li4 C1 -117.40(14) . . . . ? C12 O2 Li4 Li1 96.5(2) . . . . ? Li2 O2 Li4 Li1 -37.78(13) . . . . ? C25 O3 Li4 O2 133.8(2) . . . . ? Li1 O3 Li4 O2 -68.8(2) . . . . ? Li2 O3 Li4 O2 3.1(2) . . . . ? C25 O3 Li4 O6 8.2(3) . . . . ? Li1 O3 Li4 O6 165.6(2) . . . . ? Li2 O3 Li4 O6 -122.5(2) . . . . ? C25 O3 Li4 Li2 130.7(2) . . . . ? Li1 O3 Li4 Li2 -72.0(2) . . . . ? Li2 O3 Li4 Li2 0.0 . . . . ? C25 O3 Li4 C1 -145.47(15) . . . . ? Li1 O3 Li4 C1 11.9(2) . . . . ? Li2 O3 Li4 C1 83.9(2) . . . . ? C25 O3 Li4 Li1 -157.4(2) . . . . ? Li1 O3 Li4 Li1 0.0 . . . . ? Li2 O3 Li4 Li1 72.0(2) . . . . ? C42 O6 Li4 O2 -28.4(3) . . . . ? C39A O6 Li4 O2 143.9(4) . . . . ? C39B O6 Li4 O2 176.6(7) . . . . ? C42 O6 Li4 O3 88.3(3) . . . . ? C39A O6 Li4 O3 -99.4(4) . . . . ? C39B O6 Li4 O3 -66.8(8) . . . . ? C42 O6 Li4 Li2 26.8(4) . . . . ? C39A O6 Li4 Li2 -160.9(4) . . . . ? C39B O6 Li4 Li2 -128.2(7) . . . . ? C42 O6 Li4 C1 -119.0(3) . . . . ? C39A O6 Li4 C1 53.3(4) . . . . ? C39B O6 Li4 C1 86.0(7) . . . . ? C42 O6 Li4 Li1 109.7(5) . . . . ? C39A O6 Li4 Li1 -78.0(6) . . . . ? C39B O6 Li4 Li1 -45.4(9) . . . . ? O2 Li2 Li4 O2 0.0 . . . . ? O4 Li2 Li4 O2 -99.7(2) . . . . ? O3 Li2 Li4 O2 -175.8(2) . . . . ? Li1 Li2 Li4 O2 -125.9(2) . . . . ? Li3 Li2 Li4 O2 -69.49(14) . . . . ? O2 Li2 Li4 O3 175.8(2) . . . . ? O4 Li2 Li4 O3 76.1(2) . . . . ? O3 Li2 Li4 O3 0.0 . . . . ? Li1 Li2 Li4 O3 49.87(13) . . . . ? Li3 Li2 Li4 O3 106.3(2) . . . . ? O2 Li2 Li4 O6 -87.1(3) . . . . ? O4 Li2 Li4 O6 173.2(2) . . . . ? O3 Li2 Li4 O6 97.1(3) . . . . ? Li1 Li2 Li4 O6 147.0(2) . . . . ? Li3 Li2 Li4 O6 -156.6(2) . . . . ? O2 Li2 Li4 C1 62.68(14) . . . . ? O4 Li2 Li4 C1 -37.0(2) . . . . ? O3 Li2 Li4 C1 -113.1(2) . . . . ? Li1 Li2 Li4 C1 -63.2(2) . . . . ? Li3 Li2 Li4 C1 -6.8(2) . . . . ? O2 Li2 Li4 Li1 125.9(2) . . . . ? O4 Li2 Li4 Li1 26.2(2) . . . . ? O3 Li2 Li4 Li1 -49.87(13) . . . . ? Li1 Li2 Li4 Li1 0.0 . . . . ? Li3 Li2 Li4 Li1 56.42(13) . . . . ? C6 C1 Li4 O2 -126.5(2) . . . . ? C2 C1 Li4 O2 112.12(15) . . . . ? C7 C1 Li4 O2 -7.99(15) . . . . ? C6 C1 Li4 O3 140.8(2) . . . . ? C2 C1 Li4 O3 19.4(2) . . . . ? C7 C1 Li4 O3 -100.7(2) . . . . ? C6 C1 Li4 O6 -13.5(2) . . . . ? C2 C1 Li4 O6 -134.9(2) . . . . ? C7 C1 Li4 O6 105.0(2) . . . . ? C6 C1 Li4 Li2 -168.8(2) . . . . ? C2 C1 Li4 Li2 69.9(2) . . . . ? C7 C1 Li4 Li2 -50.2(2) . . . . ? C6 C1 Li4 Li1 148.06(15) . . . . ? C2 C1 Li4 Li1 26.71(13) . . . . ? C7 C1 Li4 Li1 -93.41(13) . . . . ? O3 Li1 Li4 O2 111.3(2) . . . . ? O1 Li1 Li4 O2 -76.73(14) . . . . ? O4 Li1 Li4 O2 16.0(2) . . . . ? Li2 Li1 Li4 O2 37.20(14) . . . . ? Li3 Li1 Li4 O2 -30.12(15) . . . . ? C2 Li1 Li4 O2 -95.29(13) . . . . ? O3 Li1 Li4 O3 0.0 . . . . ? O1 Li1 Li4 O3 171.9(2) . . . . ? O4 Li1 Li4 O3 -95.4(2) . . . . ? Li2 Li1 Li4 O3 -74.1(2) . . . . ? Li3 Li1 Li4 O3 -141.5(2) . . . . ? C2 Li1 Li4 O3 153.4(2) . . . . ? O3 Li1 Li4 O6 -31.3(4) . . . . ? O1 Li1 Li4 O6 140.7(4) . . . . ? O4 Li1 Li4 O6 -126.6(4) . . . . ? Li2 Li1 Li4 O6 -105.4(5) . . . . ? Li3 Li1 Li4 O6 -172.7(4) . . . . ? C2 Li1 Li4 O6 122.1(5) . . . . ? O3 Li1 Li4 Li2 74.1(2) . . . . ? O1 Li1 Li4 Li2 -113.9(2) . . . . ? O4 Li1 Li4 Li2 -21.23(14) . . . . ? Li2 Li1 Li4 Li2 0.0 . . . . ? Li3 Li1 Li4 Li2 -67.3(2) . . . . ? C2 Li1 Li4 Li2 -132.5(2) . . . . ? O3 Li1 Li4 C1 -169.0(2) . . . . ? O1 Li1 Li4 C1 2.90(11) . . . . ? O4 Li1 Li4 C1 95.61(15) . . . . ? Li2 Li1 Li4 C1 116.8(2) . . . . ? Li3 Li1 Li4 C1 49.52(12) . . . . ? C2 Li1 Li4 C1 -15.65(8) . . . . ? #END OF CIF data_Chisholm1004 _database_code_CSD 185858 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C50 H82 Li4 O6' _chemical_formula_weight 806.92 _chemical_melting_point ? _chemical_compound_source ? 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 17.6377(3) _cell_length_b 11.5509(2) _cell_length_c 12.6251(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2572.13(7) _cell_formula_units_Z 2 _cell_measurement_temperature 270(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_method ? _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ;Earlier crystals self-destructed at 150 K and 220 K. Data collection appeared stable at 270 K. ; _diffrn_ambient_temperature 270(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16757 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2568 _reflns_number_observed 1992 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;There is a crystallographic two-fold axis through the molecule. Both the cyclohexene oxide group and the OCH(i-propyl)~2~ group are disordered. Several restraints were used in the least-squares refinement in order to control these groups. The following bond lengths in the cyclohexene oxide group were restrained to 1.54\%A with the DFIX command: C22-C23, C23-C24 and C24-C25. The OCH(i-propyl)~2~ group was modeled in terms of two positions each for C13, C17, C18 and C19. The SADI restraint was used for the following bond lengths: C13A-C14, C13A-C17A, C13B-C14, C13B-C17B and a separate SADI restraint was used for the bond lengths: C14-C15, C14-C16, C17A-C18A, C17A-C19A, C17B-C18B, and C17B-C19B. The following atoms were kept isotropic: C17A, C18A, C19A, C17B, C18B and C19B. The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For some methyl groups, the torsion angle which defines the orientation of the group about the C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1694P)^2^+0.3190P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2568 _refine_ls_number_parameters 279 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_obs 0.0783 _refine_ls_wR_factor_all 0.2498 _refine_ls_wR_factor_obs 0.2213 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max -0.023 _refine_ls_shift/esd_mean 0.004 _refine_diff_density_max 0.329 _refine_diff_density_min -0.211 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.58754(15) 0.0633(2) 0.7669(2) 0.0745(7) Uani 1 d . . O2 O 0.5556(2) -0.0984(2) 0.6048(2) 0.0809(8) Uani 1 d . . O3 O 0.6941(2) -0.1585(3) 0.7759(3) 0.1035(11) Uani 1 d . . C1 C 0.5524(2) 0.1229(3) 0.8423(3) 0.0670(9) Uani 1 d . . C2 C 0.5018(2) 0.0657(3) 0.9102(3) 0.0666(9) Uani 1 d . . C3 C 0.4592(2) 0.1267(3) 0.9849(4) 0.0784(11) Uani 1 d . . C4 C 0.4689(3) 0.2456(4) 0.9955(4) 0.0876(12) Uani 1 d . . C5 C 0.5220(3) 0.2987(3) 0.9324(4) 0.0913(14) Uani 1 d . . H5 H 0.5291(3) 0.3779(3) 0.9409(4) 0.110 Uiso 1 calc R . C6 C 0.5658(2) 0.2427(3) 0.8571(4) 0.0825(11) Uani 1 d . . C7 C 0.4053(3) 0.0617(5) 1.0588(4) 0.1012(15) Uani 1 d . . H7A H 0.4288(10) 0.0523(33) 1.1269(11) 0.152 Uiso 1 calc R . H7B H 0.3941(19) -0.0130(16) 1.0294(18) 0.152 Uiso 1 calc R . H7C H 0.3592(10) 0.1050(19) 1.0666(27) 0.152 Uiso 1 calc R . C8 C 0.4270(4) 0.3159(4) 1.0773(5) 0.122(2) Uani 1 d . . H8A H 0.4403(23) 0.3961(8) 1.0701(28) 0.183 Uiso 1 calc R . H8B H 0.4405(23) 0.2894(31) 1.1469(6) 0.183 Uiso 1 calc R . H8C H 0.3733(4) 0.3069(36) 1.0672(27) 0.183 Uiso 1 calc R . C9 C 0.6309(4) 0.3050(4) 0.7994(5) 0.104(2) Uani 1 d . . C10 C 0.6221(5) 0.3027(7) 0.6811(5) 0.142(3) Uani 1 d . . H10A H 0.5753(5) 0.3398(7) 0.6618(5) 0.213 Uiso 1 calc R . H10B H 0.6215(5) 0.2238(7) 0.6569(5) 0.213 Uiso 1 calc R . H10C H 0.6637(5) 0.3429(7) 0.6488(5) 0.213 Uiso 1 calc R . C11 C 0.7049(3) 0.2461(6) 0.8287(6) 0.131(2) Uani 1 d . . H11A H 0.7110(3) 0.2472(6) 0.9043(6) 0.197 Uiso 1 calc R . H11B H 0.7464(3) 0.2865(6) 0.7962(6) 0.197 Uiso 1 calc R . H11C H 0.7041(3) 0.1674(6) 0.8043(6) 0.197 Uiso 1 calc R . C12 C 0.6372(6) 0.4332(5) 0.8343(8) 0.190(4) Uani 1 d . . H12A H 0.6429(6) 0.4370(5) 0.9099(8) 0.286 Uiso 1 calc R . H12B H 0.5921(6) 0.4740(5) 0.8138(8) 0.286 Uiso 1 calc R . H12C H 0.6804(6) 0.4681(5) 0.8010(8) 0.286 Uiso 1 calc R . C13A C 0.5767(7) -0.1448(10) 0.5081(10) 0.092(4) Uani 0.50 d PD 1 H13A H 0.5413(7) -0.1199(10) 0.4529(10) 0.111 Uiso 0.50 calc PR 1 C13B C 0.6093(8) -0.1613(10) 0.5384(10) 0.087(3) Uani 0.50 d PD 2 H13B H 0.6575(8) -0.1690(10) 0.5762(10) 0.105 Uiso 0.50 calc PR 2 C14 C 0.5777(7) -0.2807(5) 0.5156(7) 0.177(4) Uani 1 d D . H14A H 0.5253(7) -0.2994(5) 0.4962(7) 0.212 Uiso 0.50 calc PR 1 H14B H 0.5242(7) -0.2755(5) 0.4954(7) 0.212 Uiso 0.50 calc PR 2 C15 C 0.5857(7) -0.3446(6) 0.6143(10) 0.190(4) Uani 1 d D . H15A H 0.5591(7) -0.3049(6) 0.6697(10) 0.285 Uiso 1 calc R . H15B H 0.6385(7) -0.3503(6) 0.6324(10) 0.285 Uiso 1 calc R . H15C H 0.5650(7) -0.4209(6) 0.6058(10) 0.285 Uiso 1 calc R . C16 C 0.6212(12) -0.3502(13) 0.4354(12) 0.319(12) Uani 1 d D . H16A H 0.6183(12) -0.3127(13) 0.3677(12) 0.478 Uiso 1 calc R . H16B H 0.5997(12) -0.4264(13) 0.4304(12) 0.478 Uiso 1 calc R . H16C H 0.6732(12) -0.3558(13) 0.4570(12) 0.478 Uiso 1 calc R . C17A C 0.6586(9) -0.0941(16) 0.4853(16) 0.162(6) Uiso 0.50 d PD 1 H17A H 0.6940(9) -0.1455(16) 0.5223(16) 0.194 Uiso 0.50 calc PR 1 C18A C 0.6809(13) 0.0234(18) 0.5146(20) 0.197(8) Uiso 0.50 d PD 1 H18A H 0.6676(13) 0.0374(18) 0.5872(20) 0.295 Uiso 0.50 calc PR 1 H18B H 0.6549(13) 0.0779(18) 0.4700(20) 0.295 Uiso 0.50 calc PR 1 H18C H 0.7346(13) 0.0321(18) 0.5057(20) 0.295 Uiso 0.50 calc PR 1 C19A C 0.6850(19) -0.0897(31) 0.3750(22) 0.286(16) Uiso 0.50 d PD 1 H19A H 0.6749(19) -0.1624(31) 0.3411(22) 0.429 Uiso 0.50 calc PR 1 H19B H 0.7385(19) -0.0747(31) 0.3738(22) 0.429 Uiso 0.50 calc PR 1 H19C H 0.6589(19) -0.0290(31) 0.3381(22) 0.429 Uiso 0.50 calc PR 1 C17B C 0.6222(7) -0.0964(11) 0.4377(9) 0.108(3) Uiso 0.50 d PD 2 H17B H 0.6616(7) -0.1383(11) 0.3986(9) 0.130 Uiso 0.50 calc PR 2 C18B C 0.5567(12) -0.0900(22) 0.3691(18) 0.198(8) Uiso 0.50 d PD 2 H18D H 0.5363(12) -0.1662(22) 0.3587(18) 0.297 Uiso 0.50 calc PR 2 H18E H 0.5714(12) -0.0581(22) 0.3020(18) 0.297 Uiso 0.50 calc PR 2 H18F H 0.5189(12) -0.0414(22) 0.4010(18) 0.297 Uiso 0.50 calc PR 2 C19B C 0.6476(13) 0.0227(17) 0.4473(20) 0.203(9) Uiso 0.50 d PD 2 H19D H 0.6915(13) 0.0258(17) 0.4922(20) 0.304 Uiso 0.50 calc PR 2 H19E H 0.6078(13) 0.0688(17) 0.4775(20) 0.304 Uiso 0.50 calc PR 2 H19F H 0.6603(13) 0.0522(17) 0.3784(20) 0.304 Uiso 0.50 calc PR 2 C20 C 0.7447(4) -0.1008(6) 0.8460(6) 0.130(2) Uani 1 d . . H20 H 0.7215(4) -0.0474(6) 0.8969(6) 0.156 Uiso 1 calc R . C21 C 0.7283(4) -0.2240(7) 0.8616(6) 0.128(2) Uani 1 d . . H21 H 0.6953(4) -0.2437(7) 0.9213(6) 0.154 Uiso 1 calc R . C22 C 0.7846(4) -0.3131(7) 0.8293(9) 0.157(3) Uani 1 d D . H22A H 0.7936(4) -0.3647(7) 0.8885(9) 0.188 Uiso 1 calc R . H22B H 0.7634(4) -0.3587(7) 0.7720(9) 0.188 Uiso 1 calc R . C23 C 0.8577(5) -0.2635(9) 0.7945(12) 0.194(5) Uani 1 d D . H23A H 0.8882(5) -0.2505(9) 0.8572(12) 0.233 Uiso 1 calc R . H23B H 0.8835(5) -0.3218(9) 0.7526(12) 0.233 Uiso 1 calc R . C24 C 0.8576(6) -0.1603(11) 0.7356(15) 0.254(8) Uani 1 d D . H24A H 0.8345(6) -0.1743(11) 0.6671(15) 0.305 Uiso 1 calc R . H24B H 0.9094(6) -0.1354(11) 0.7239(15) 0.305 Uiso 1 calc R . C25 C 0.8125(5) -0.0610(8) 0.7947(12) 0.196(5) Uani 1 d D . H25A H 0.8454(5) -0.0261(8) 0.8473(12) 0.235 Uiso 1 calc R . H25B H 0.7991(5) -0.0015(8) 0.7438(12) 0.235 Uiso 1 calc R . Li1 Li 0.5935(4) -0.0963(6) 0.7439(6) 0.081(2) Uani 1 d . . Li2 Li 0.5494(4) 0.0684(6) 0.6275(6) 0.081(2) Uani 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 0.082(2) 0.0619(13) 0.080(2) 0.0034(13) 0.0005(13) -0.0057(12) O2 0.098(2) 0.0656(14) 0.079(2) -0.0068(13) 0.0111(15) 0.0068(13) O3 0.104(2) 0.092(2) 0.114(2) 0.005(2) -0.016(2) 0.021(2) C1 0.075(2) 0.051(2) 0.075(2) 0.006(2) -0.014(2) -0.003(2) C2 0.076(2) 0.047(2) 0.077(2) -0.001(2) -0.008(2) -0.0024(14) C3 0.087(2) 0.061(2) 0.088(2) -0.007(2) -0.003(2) 0.000(2) C4 0.098(3) 0.060(2) 0.105(3) -0.018(2) -0.008(3) 0.010(2) C5 0.111(3) 0.045(2) 0.119(3) -0.007(2) -0.021(3) -0.001(2) C6 0.096(3) 0.054(2) 0.097(3) 0.007(2) -0.018(2) -0.011(2) C7 0.110(3) 0.091(3) 0.103(3) -0.010(3) 0.025(3) -0.002(3) C8 0.139(4) 0.079(3) 0.148(5) -0.038(3) 0.009(4) 0.011(3) C9 0.123(4) 0.067(2) 0.123(4) 0.019(3) -0.015(3) -0.034(3) C10 0.167(6) 0.134(5) 0.126(5) 0.047(4) -0.018(4) -0.056(5) C11 0.104(4) 0.140(5) 0.150(5) 0.031(5) -0.010(4) -0.044(4) C12 0.266(11) 0.076(3) 0.230(9) -0.009(5) 0.049(9) -0.074(5) C13A 0.090(8) 0.110(8) 0.077(7) 0.012(5) 0.004(6) 0.033(6) C13B 0.090(8) 0.092(6) 0.080(7) 0.002(5) 0.013(6) 0.019(6) C14 0.286(11) 0.086(4) 0.157(6) -0.042(5) 0.071(7) 0.013(6) C15 0.243(11) 0.082(4) 0.244(11) -0.012(6) 0.040(10) 0.019(5) C16 0.484(30) 0.189(11) 0.283(17) -0.074(11) 0.205(19) 0.027(15) C20 0.133(5) 0.122(5) 0.133(5) -0.031(4) -0.024(4) 0.018(4) C21 0.126(4) 0.137(5) 0.121(4) 0.032(4) 0.003(4) 0.034(4) C22 0.131(5) 0.131(5) 0.208(8) 0.037(6) 0.003(5) 0.047(4) C23 0.134(6) 0.143(7) 0.304(14) -0.023(9) 0.027(8) 0.027(6) C24 0.159(8) 0.189(10) 0.415(23) 0.069(14) 0.125(12) 0.024(8) C25 0.145(6) 0.135(6) 0.307(14) -0.038(8) -0.018(9) -0.025(6) Li1 0.089(4) 0.068(3) 0.086(4) 0.002(3) -0.002(3) 0.007(3) Li2 0.092(4) 0.065(3) 0.085(4) 0.006(3) 0.010(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.328(5) . ? O1 Li1 1.869(7) . ? O1 Li2 1.886(8) . ? O2 C13A 1.384(13) . ? O2 C13B 1.459(12) . ? O2 Li1 1.879(8) . ? O2 Li2 1.905(8) 2_655 ? O2 Li2 1.950(7) . ? O3 C20 1.422(7) . ? O3 C21 1.452(7) . ? O3 Li1 1.955(8) . ? C1 C2 1.403(5) . ? C1 C6 1.416(5) . ? C1 Li2 2.785(8) . ? C2 C3 1.396(6) . ? C2 C2 1.519(7) 2_655 ? C2 Li1 2.713(8) 2_655 ? C3 C4 1.391(6) . ? C3 C7 1.529(7) . ? C4 C5 1.374(7) . ? C4 C8 1.508(7) . ? C5 C6 1.385(7) . ? C5 H5 0.93 . ? C6 C9 1.539(7) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 C10 1.502(9) . ? C9 C11 1.517(9) . ? C9 C12 1.550(8) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13A C14 1.573(13) . ? C13A C17A 1.59(2) . ? C13A H13A 0.98 . ? C13B C17B 1.492(14) . ? C13B C14 1.515(13) . ? C13B Li1 2.715(14) . ? C13B H13B 0.98 . ? C14 C15 1.455(12) . ? C14 C16 1.502(12) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C17A C18A 1.46(2) . ? C17A C19A 1.47(2) . ? C17A H17A 0.98 . ? C18A H18A 0.96 . ? C18A H18B 0.96 . ? C18A H18C 0.96 . ? C19A H19A 0.96 . ? C19A H19B 0.96 . ? C19A H19C 0.96 . ? C17B C18B 1.45(2) . ? C17B C19B 1.45(2) . ? C17B H17B 0.98 . ? C18B H18D 0.96 . ? C18B H18E 0.96 . ? C18B H18F 0.96 . ? C19B H19D 0.96 . ? C19B H19E 0.96 . ? C19B H19F 0.96 . ? C20 C25 1.436(12) . ? C20 C21 1.465(10) . ? C20 H20 0.98 . ? C21 C22 1.487(10) . ? C21 H21 0.98 . ? C22 C23 1.478(12) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.404(14) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 C25 1.582(14) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? Li1 Li2 2.527(9) . ? Li1 C2 2.713(8) 2_655 ? Li1 Li2 2.936(10) 2_655 ? Li2 O2 1.906(8) 2_655 ? Li2 Li2 2.352(14) 2_655 ? Li2 Li1 2.936(10) 2_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 130.5(3) . . ? C1 O1 Li2 119.1(3) . . ? Li1 O1 Li2 84.6(3) . . ? C13A O2 Li1 137.1(6) . . ? C13B O2 Li1 108.2(6) . . ? C13A O2 Li2 117.6(6) . 2_655 ? C13B O2 Li2 143.8(6) . 2_655 ? Li1 O2 Li2 101.8(3) . 2_655 ? C13A O2 Li2 121.8(5) . . ? C13B O2 Li2 127.8(5) . . ? Li1 O2 Li2 82.6(3) . . ? Li2 O2 Li2 75.2(3) 2_655 . ? C20 O3 C21 61.3(4) . . ? C20 O3 Li1 121.7(4) . . ? C21 O3 Li1 136.3(4) . . ? O1 C1 C2 119.4(3) . . ? O1 C1 C6 121.6(4) . . ? C2 C1 C6 119.0(4) . . ? O1 C1 Li2 36.3(2) . . ? C2 C1 Li2 118.5(3) . . ? C6 C1 Li2 110.7(3) . . ? C3 C2 C1 121.2(3) . . ? C3 C2 C2 118.8(3) . 2_655 ? C1 C2 C2 119.8(3) . 2_655 ? C3 C2 Li1 97.1(3) . 2_655 ? C1 C2 Li1 81.9(3) . 2_655 ? C2 C2 Li1 96.0(2) 2_655 2_655 ? C4 C3 C2 119.8(4) . . ? C4 C3 C7 120.2(4) . . ? C2 C3 C7 119.9(4) . . ? C5 C4 C3 117.9(4) . . ? C5 C4 C8 119.5(4) . . ? C3 C4 C8 122.5(5) . . ? C4 C5 C6 124.7(3) . . ? C4 C5 H5 117.6(2) . . ? C6 C5 H5 117.6(2) . . ? C5 C6 C1 117.0(4) . . ? C5 C6 C9 121.5(4) . . ? C1 C6 C9 121.2(4) . . ? C3 C7 H7A 109.5(3) . . ? C3 C7 H7B 109.5(2) . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5(3) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5(3) . . ? C4 C8 H8B 109.5(3) . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5(3) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C11 108.9(7) . . ? C10 C9 C6 112.7(5) . . ? C11 C9 C6 108.5(4) . . ? C10 C9 C12 107.9(6) . . ? C11 C9 C12 107.3(6) . . ? C6 C9 C12 111.4(6) . . ? C9 C10 H10A 109.5(5) . . ? C9 C10 H10B 109.5(4) . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5(4) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5(4) . . ? C9 C11 H11B 109.5(3) . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5(3) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5(4) . . ? C9 C12 H12B 109.5(5) . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5(4) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13A C14 109.7(8) . . ? O2 C13A C17A 105.2(11) . . ? C14 C13A C17A 111.7(10) . . ? O2 C13A H13A 110.1(5) . . ? C14 C13A H13A 110.1(7) . . ? C17A C13A H13A 110.1(9) . . ? O2 C13B C17B 109.8(9) . . ? O2 C13B C14 108.9(8) . . ? C17B C13B C14 110.6(9) . . ? O2 C13B Li1 41.1(4) . . ? C17B C13B Li1 133.7(8) . . ? C14 C13B Li1 113.3(7) . . ? O2 C13B H13B 109.2(6) . . ? C17B C13B H13B 109.2(7) . . ? C14 C13B H13B 109.2(7) . . ? Li1 C13B H13B 69.4(3) . . ? C15 C14 C16 104.8(9) . . ? C15 C14 C13B 105.3(9) . . ? C16 C14 C13B 115.2(11) . . ? C15 C14 C13A 124.0(8) . . ? C16 C14 C13A 119.9(10) . . ? C15 C14 H14A 101.2(7) . . ? C16 C14 H14A 101.2(9) . . ? C13A C14 H14A 101.2(7) . . ? C15 C14 H14B 110.4(7) . . ? C16 C14 H14B 110.4(9) . . ? C13B C14 H14B 110.4(7) . . ? C14 C15 H15A 109.5(4) . . ? C14 C15 H15B 109.5(7) . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5(5) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5(8) . . ? C14 C16 H16B 109.5(8) . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5(9) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18A C17A C19A 97.0(21) . . ? C18A C17A C13A 122.8(16) . . ? C19A C17A C13A 118.3(19) . . ? C18A C17A H17A 105.7(12) . . ? C19A C17A H17A 105.7(16) . . ? C13A C17A H17A 105.7(8) . . ? C17A C18A H18A 109.5(13) . . ? C17A C18A H18B 109.5(13) . . ? H18A C18A H18B 109.5 . . ? C17A C18A H18C 109.5(11) . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C17A C19A H19A 109.5(16) . . ? C17A C19A H19B 109.5(16) . . ? H19A C19A H19B 109.5 . . ? C17A C19A H19C 109.5(16) . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C18B C17B C19B 104.3(15) . . ? C18B C17B C13B 114.4(13) . . ? C19B C17B C13B 116.9(14) . . ? C18B C17B H17B 106.9(11) . . ? C19B C17B H17B 106.9(11) . . ? C13B C17B H17B 106.9(7) . . ? C17B C18B H18D 109.5(11) . . ? C17B C18B H18E 109.5(10) . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5(11) . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5(11) . . ? C17B C19B H19E 109.5(11) . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5(11) . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? O3 C20 C25 113.1(8) . . ? O3 C20 C21 60.4(4) . . ? C25 C20 C21 122.4(7) . . ? O3 C20 H20 116.2(3) . . ? C25 C20 H20 116.2(5) . . ? C21 C20 H20 116.2(4) . . ? O3 C21 C20 58.4(4) . . ? O3 C21 C22 115.7(7) . . ? C20 C21 C22 120.3(7) . . ? O3 C21 H21 116.6(3) . . ? C20 C21 H21 116.6(4) . . ? C22 C21 H21 116.6(5) . . ? C23 C22 C21 113.3(7) . . ? C23 C22 H22A 108.9(6) . . ? C21 C22 H22A 108.9(5) . . ? C23 C22 H22B 108.9(7) . . ? C21 C22 H22B 108.9(5) . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 119.0(9) . . ? C24 C23 H23A 107.6(10) . . ? C22 C23 H23A 107.6(7) . . ? C24 C23 H23B 107.6(8) . . ? C22 C23 H23B 107.6(5) . . ? H23A C23 H23B 107.0 . . ? C23 C24 C25 111.5(11) . . ? C23 C24 H24A 109.3(10) . . ? C25 C24 H24A 109.3(8) . . ? C23 C24 H24B 109.3(7) . . ? C25 C24 H24B 109.3(5) . . ? H24A C24 H24B 108.0 . . ? C20 C25 C24 113.5(7) . . ? C20 C25 H25A 108.9(6) . . ? C24 C25 H25A 108.9(8) . . ? C20 C25 H25B 108.9(6) . . ? C24 C25 H25B 108.9(8) . . ? H25A C25 H25B 107.7 . . ? O1 Li1 O2 97.9(3) . . ? O1 Li1 O3 112.4(4) . . ? O2 Li1 O3 120.8(4) . . ? O1 Li1 Li2 48.0(2) . . ? O2 Li1 Li2 49.9(2) . . ? O3 Li1 Li2 132.5(4) . . ? O1 Li1 C2 73.5(3) . 2_655 ? O2 Li1 C2 120.3(3) . 2_655 ? O3 Li1 C2 116.7(3) . 2_655 ? Li2 Li1 C2 99.3(3) . 2_655 ? O1 Li1 C13B 115.3(4) . . ? O2 Li1 C13B 30.7(3) . . ? O3 Li1 C13B 90.2(4) . . ? Li2 Li1 C13B 71.6(4) . . ? C2 Li1 C13B 147.0(4) 2_655 . ? O1 Li1 Li2 85.5(3) . 2_655 ? O2 Li1 Li2 39.4(2) . 2_655 ? O3 Li1 Li2 157.3(4) . 2_655 ? Li2 Li1 Li2 50.3(3) . 2_655 ? C2 Li1 Li2 80.9(3) 2_655 2_655 ? C13B Li1 Li2 68.9(4) . 2_655 ? O1 Li2 O2 119.5(4) . 2_655 ? O1 Li2 O2 94.9(3) . . ? O2 Li2 O2 102.2(4) 2_655 . ? O1 Li2 Li2 104.1(2) . 2_655 ? O2 Li2 Li2 53.3(3) 2_655 2_655 ? O2 Li2 Li2 51.5(3) . 2_655 ? O1 Li2 Li1 47.4(2) . . ? O2 Li2 Li1 121.6(4) 2_655 . ? O2 Li2 Li1 47.5(2) . . ? Li2 Li2 Li1 73.9(3) 2_655 . ? O1 Li2 C1 24.64(15) . . ? O2 Li2 C1 97.1(3) 2_655 . ? O2 Li2 C1 111.4(3) . . ? Li2 Li2 C1 99.6(2) 2_655 . ? Li1 Li2 C1 66.3(3) . . ? O1 Li2 Li1 80.9(3) . 2_655 ? O2 Li2 Li1 38.8(2) 2_655 2_655 ? O2 Li2 Li1 103.3(3) . 2_655 ? Li2 Li2 Li1 55.8(3) 2_655 2_655 ? Li1 Li2 Li1 93.2(3) . 2_655 ? C1 Li2 Li1 60.3(2) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 O1 C1 C2 -10.4(6) . . . . ? Li2 O1 C1 C2 99.1(4) . . . . ? Li1 O1 C1 C6 168.4(4) . . . . ? Li2 O1 C1 C6 -82.1(5) . . . . ? Li1 O1 C1 Li2 -109.5(5) . . . . ? Li2 O1 C1 Li2 0.000(2) . . . . ? O1 C1 C2 C3 -174.9(4) . . . . ? C6 C1 C2 C3 6.3(5) . . . . ? Li2 C1 C2 C3 -133.2(4) . . . . ? O1 C1 C2 C2 10.9(5) . . . 2_655 ? C6 C1 C2 C2 -167.9(4) . . . 2_655 ? Li2 C1 C2 C2 52.6(5) . . . 2_655 ? O1 C1 C2 Li1 -81.4(3) . . . 2_655 ? C6 C1 C2 Li1 99.8(4) . . . 2_655 ? Li2 C1 C2 Li1 -39.8(3) . . . 2_655 ? C1 C2 C3 C4 -2.5(6) . . . . ? C2 C2 C3 C4 171.8(4) 2_655 . . . ? Li1 C2 C3 C4 -87.3(4) 2_655 . . . ? C1 C2 C3 C7 -179.2(4) . . . . ? C2 C2 C3 C7 -4.9(6) 2_655 . . . ? Li1 C2 C3 C7 96.0(4) 2_655 . . . ? C2 C3 C4 C5 -1.4(7) . . . . ? C7 C3 C4 C5 175.3(4) . . . . ? C2 C3 C4 C8 -177.6(5) . . . . ? C7 C3 C4 C8 -0.9(7) . . . . ? C3 C4 C5 C6 1.4(7) . . . . ? C8 C4 C5 C6 177.7(5) . . . . ? C4 C5 C6 C1 2.3(7) . . . . ? C4 C5 C6 C9 -172.3(4) . . . . ? O1 C1 C6 C5 175.1(4) . . . . ? C2 C1 C6 C5 -6.1(6) . . . . ? Li2 C1 C6 C5 136.3(4) . . . . ? O1 C1 C6 C9 -10.2(6) . . . . ? C2 C1 C6 C9 168.6(4) . . . . ? Li2 C1 C6 C9 -49.0(5) . . . . ? C5 C6 C9 C10 -123.2(6) . . . . ? C1 C6 C9 C10 62.4(7) . . . . ? C5 C6 C9 C11 116.1(5) . . . . ? C1 C6 C9 C11 -58.3(6) . . . . ? C5 C6 C9 C12 -1.8(8) . . . . ? C1 C6 C9 C12 -176.2(6) . . . . ? C13B O2 C13A C14 67.4(14) . . . . ? Li1 O2 C13A C14 62.6(13) . . . . ? Li2 O2 C13A C14 -91.9(9) 2_655 . . . ? Li2 O2 C13A C14 179.0(7) . . . . ? C13B O2 C13A C17A -52.8(15) . . . . ? Li1 O2 C13A C17A -57.6(13) . . . . ? Li2 O2 C13A C17A 147.9(9) 2_655 . . . ? Li2 O2 C13A C17A 58.8(11) . . . . ? C13A O2 C13B C17B 48.7(14) . . . . ? Li1 O2 C13B C17B -134.7(8) . . . . ? Li2 O2 C13B C17B 80.8(12) 2_655 . . . ? Li2 O2 C13B C17B -40.0(13) . . . . ? C13A O2 C13B C14 -72.5(16) . . . . ? Li1 O2 C13B C14 104.0(9) . . . . ? Li2 O2 C13B C14 -40.4(14) 2_655 . . . ? Li2 O2 C13B C14 -161.2(7) . . . . ? C13A O2 C13B Li1 -176.6(14) . . . . ? Li1 O2 C13B Li1 0.000(2) . . . . ? Li2 O2 C13B Li1 -144.5(9) 2_655 . . . ? Li2 O2 C13B Li1 94.8(7) . . . . ? O2 C13B C14 C15 -73.3(11) . . . . ? C17B C13B C14 C15 165.9(10) . . . . ? Li1 C13B C14 C15 -29.4(11) . . . . ? O2 C13B C14 C16 171.7(11) . . . . ? C17B C13B C14 C16 50.9(16) . . . . ? Li1 C13B C14 C16 -144.3(10) . . . . ? O2 C13B C14 C13A 64.9(16) . . . . ? C17B C13B C14 C13A -55.9(15) . . . . ? Li1 C13B C14 C13A 108.9(18) . . . . ? O2 C13A C14 C15 -22.7(16) . . . . ? C17A C13A C14 C15 93.5(15) . . . . ? O2 C13A C14 C16 -160.7(12) . . . . ? C17A C13A C14 C16 -44.5(18) . . . . ? O2 C13A C14 C13B -73.5(17) . . . . ? C17A C13A C14 C13B 42.7(15) . . . . ? O2 C13A C17A C18A -36.4(22) . . . . ? C14 C13A C17A C18A -155.3(18) . . . . ? O2 C13A C17A C19A -157.2(21) . . . . ? C14 C13A C17A C19A 83.9(23) . . . . ? O2 C13B C17B C18B -66.6(15) . . . . ? C14 C13B C17B C18B 53.6(18) . . . . ? Li1 C13B C17B C18B -106.9(15) . . . . ? O2 C13B C17B C19B 55.7(18) . . . . ? C14 C13B C17B C19B 175.9(14) . . . . ? Li1 C13B C17B C19B 15.4(22) . . . . ? C21 O3 C20 C25 115.3(8) . . . . ? Li1 O3 C20 C25 -115.6(7) . . . . ? C21 O3 C20 C21 0.0 . . . . ? Li1 O3 C20 C21 129.0(5) . . . . ? C20 O3 C21 C20 0.000(1) . . . . ? Li1 O3 C21 C20 -107.1(7) . . . . ? C20 O3 C21 C22 -111.1(8) . . . . ? Li1 O3 C21 C22 141.7(6) . . . . ? O3 C20 C21 O3 0.000(1) . . . . ? C25 C20 C21 O3 -100.0(9) . . . . ? O3 C20 C21 C22 103.3(8) . . . . ? C25 C20 C21 C22 3.3(13) . . . . ? O3 C21 C22 C23 73.7(11) . . . . ? C20 C21 C22 C23 6.8(13) . . . . ? C21 C22 C23 C24 -37.8(17) . . . . ? C22 C23 C24 C25 54.3(18) . . . . ? O3 C20 C25 C24 -55.8(13) . . . . ? C21 C20 C25 C24 12.7(16) . . . . ? C23 C24 C25 C20 -39.8(18) . . . . ? C1 O1 Li1 O2 123.9(4) . . . . ? Li2 O1 Li1 O2 -0.2(4) . . . . ? C1 O1 Li1 O3 -108.1(5) . . . . ? Li2 O1 Li1 O3 127.8(4) . . . . ? C1 O1 Li1 Li2 124.1(4) . . . . ? Li2 O1 Li1 Li2 0.000(1) . . . . ? C1 O1 Li1 C2 4.6(4) . . . 2_655 ? Li2 O1 Li1 C2 -119.6(3) . . . 2_655 ? C1 O1 Li1 C13B 150.4(4) . . . . ? Li2 O1 Li1 C13B 26.3(5) . . . . ? C1 O1 Li1 Li2 86.4(4) . . . 2_655 ? Li2 O1 Li1 Li2 -37.8(3) . . . 2_655 ? C13A O2 Li1 O1 130.1(8) . . . . ? C13B O2 Li1 O1 127.6(5) . . . . ? Li2 O2 Li1 O1 -72.9(4) 2_655 . . . ? Li2 O2 Li1 O1 0.2(3) . . . . ? C13A O2 Li1 O3 8.0(10) . . . . ? C13B O2 Li1 O3 5.6(7) . . . . ? Li2 O2 Li1 O3 165.1(4) 2_655 . . . ? Li2 O2 Li1 O3 -121.8(5) . . . . ? C13A O2 Li1 Li2 129.8(9) . . . . ? C13B O2 Li1 Li2 127.4(6) . . . . ? Li2 O2 Li1 Li2 -73.1(3) 2_655 . . . ? Li2 O2 Li1 Li2 0.000(1) . . . . ? C13A O2 Li1 C2 -154.5(8) . . . 2_655 ? C13B O2 Li1 C2 -156.9(5) . . . 2_655 ? Li2 O2 Li1 C2 2.6(4) 2_655 . . 2_655 ? Li2 O2 Li1 C2 75.7(4) . . . 2_655 ? C13A O2 Li1 C13B 2.4(10) . . . . ? C13B O2 Li1 C13B 0.000(2) . . . . ? Li2 O2 Li1 C13B 159.5(6) 2_655 . . . ? Li2 O2 Li1 C13B -127.4(6) . . . . ? C13A O2 Li1 Li2 -157.1(9) . . . 2_655 ? C13B O2 Li1 Li2 -159.5(6) . . . 2_655 ? Li2 O2 Li1 Li2 0.000(1) 2_655 . . 2_655 ? Li2 O2 Li1 Li2 73.1(3) . . . 2_655 ? C20 O3 Li1 O1 23.1(7) . . . . ? C21 O3 Li1 O1 103.2(7) . . . . ? C20 O3 Li1 O2 137.8(6) . . . . ? C21 O3 Li1 O2 -142.0(6) . . . . ? C20 O3 Li1 Li2 75.9(7) . . . . ? C21 O3 Li1 Li2 156.0(6) . . . . ? C20 O3 Li1 C2 -59.1(6) . . . 2_655 ? C21 O3 Li1 C2 21.1(8) . . . 2_655 ? C20 O3 Li1 C13B 140.7(5) . . . . ? C21 O3 Li1 C13B -139.2(6) . . . . ? C20 O3 Li1 Li2 162.9(10) . . . 2_655 ? C21 O3 Li1 Li2 -116.9(11) . . . 2_655 ? O2 C13B Li1 O1 -60.2(6) . . . . ? C17B C13B Li1 O1 7.4(14) . . . . ? C14 C13B Li1 O1 -152.7(8) . . . . ? O2 C13B Li1 O2 0.000(4) . . . . ? C17B C13B Li1 O2 67.6(12) . . . . ? C14 C13B Li1 O2 -92.5(10) . . . . ? O2 C13B Li1 O3 -175.2(6) . . . . ? C17B C13B Li1 O3 -107.6(13) . . . . ? C14 C13B Li1 O3 92.3(9) . . . . ? O2 C13B Li1 Li2 -39.9(4) . . . . ? C17B C13B Li1 Li2 27.7(12) . . . . ? C14 C13B Li1 Li2 -132.3(9) . . . . ? O2 C13B Li1 C2 38.5(8) . . . 2_655 ? C17B C13B Li1 C2 106.1(13) . . . 2_655 ? C14 C13B Li1 C2 -54.0(12) . . . 2_655 ? O2 C13B Li1 Li2 13.8(4) . . . 2_655 ? C17B C13B Li1 Li2 81.4(13) . . . 2_655 ? C14 C13B Li1 Li2 -78.7(9) . . . 2_655 ? C1 O1 Li2 O2 -26.7(5) . . . 2_655 ? Li1 O1 Li2 O2 107.3(4) . . . 2_655 ? C1 O1 Li2 O2 -133.7(3) . . . . ? Li1 O1 Li2 O2 0.2(3) . . . . ? C1 O1 Li2 Li2 -82.2(5) . . . 2_655 ? Li1 O1 Li2 Li2 51.8(5) . . . 2_655 ? C1 O1 Li2 Li1 -133.9(4) . . . . ? Li1 O1 Li2 Li1 0.000(1) . . . . ? C1 O1 Li2 C1 0.000(3) . . . . ? Li1 O1 Li2 C1 133.9(4) . . . . ? C1 O1 Li2 Li1 -31.0(4) . . . 2_655 ? Li1 O1 Li2 Li1 102.9(3) . . . 2_655 ? C13A O2 Li2 O1 -142.3(7) . . . . ? C13B O2 Li2 O1 -107.5(8) . . . . ? Li1 O2 Li2 O1 -0.2(3) . . . . ? Li2 O2 Li2 O1 104.1(2) 2_655 . . . ? C13A O2 Li2 O2 96.1(7) . . . 2_655 ? C13B O2 Li2 O2 130.8(7) . . . 2_655 ? Li1 O2 Li2 O2 -121.9(4) . . . 2_655 ? Li2 O2 Li2 O2 -17.5(5) 2_655 . . 2_655 ? C13A O2 Li2 Li2 113.6(7) . . . 2_655 ? C13B O2 Li2 Li2 148.4(8) . . . 2_655 ? Li1 O2 Li2 Li2 -104.3(3) . . . 2_655 ? Li2 O2 Li2 Li2 0.0 2_655 . . 2_655 ? C13A O2 Li2 Li1 -142.1(7) . . . . ? C13B O2 Li2 Li1 -107.3(8) . . . . ? Li1 O2 Li2 Li1 0.000(1) . . . . ? Li2 O2 Li2 Li1 104.3(3) 2_655 . . . ? C13A O2 Li2 C1 -161.2(7) . . . . ? C13B O2 Li2 C1 -126.4(7) . . . . ? Li1 O2 Li2 C1 -19.1(4) . . . . ? Li2 O2 Li2 C1 85.2(3) 2_655 . . . ? C13A O2 Li2 Li1 135.9(7) . . . 2_655 ? C13B O2 Li2 Li1 170.6(7) . . . 2_655 ? Li1 O2 Li2 Li1 -82.1(4) . . . 2_655 ? Li2 O2 Li2 Li1 22.3(4) 2_655 . . 2_655 ? O1 Li1 Li2 O1 0.000(2) . . . . ? O2 Li1 Li2 O1 179.7(5) . . . . ? O3 Li1 Li2 O1 -82.5(5) . . . . ? C2 Li1 Li2 O1 57.7(3) 2_655 . . . ? C13B Li1 Li2 O1 -155.0(4) . . . . ? Li2 Li1 Li2 O1 127.5(4) 2_655 . . . ? O1 Li1 Li2 O2 -102.7(5) . . . 2_655 ? O2 Li1 Li2 O2 77.0(4) . . . 2_655 ? O3 Li1 Li2 O2 174.8(4) . . . 2_655 ? C2 Li1 Li2 O2 -45.0(5) 2_655 . . 2_655 ? C13B Li1 Li2 O2 102.3(5) . . . 2_655 ? Li2 Li1 Li2 O2 24.8(4) 2_655 . . 2_655 ? O1 Li1 Li2 O2 -179.7(5) . . . . ? O2 Li1 Li2 O2 0.000(1) . . . . ? O3 Li1 Li2 O2 97.8(6) . . . . ? C2 Li1 Li2 O2 -122.0(4) 2_655 . . . ? C13B Li1 Li2 O2 25.3(3) . . . . ? Li2 Li1 Li2 O2 -52.2(2) 2_655 . . . ? O1 Li1 Li2 Li2 -127.5(4) . . . 2_655 ? O2 Li1 Li2 Li2 52.2(2) . . . 2_655 ? O3 Li1 Li2 Li2 150.0(6) . . . 2_655 ? C2 Li1 Li2 Li2 -69.8(3) 2_655 . . 2_655 ? C13B Li1 Li2 Li2 77.5(4) . . . 2_655 ? Li2 Li1 Li2 Li2 0.0 2_655 . . 2_655 ? O1 Li1 Li2 C1 -19.1(2) . . . . ? O2 Li1 Li2 C1 160.6(4) . . . . ? O3 Li1 Li2 C1 -101.6(5) . . . . ? C2 Li1 Li2 C1 38.5(2) 2_655 . . . ? C13B Li1 Li2 C1 -174.1(4) . . . . ? Li2 Li1 Li2 C1 108.4(3) 2_655 . . . ? O1 Li1 Li2 Li1 -74.6(2) . . . 2_655 ? O2 Li1 Li2 Li1 105.1(4) . . . 2_655 ? O3 Li1 Li2 Li1 -157.1(5) . . . 2_655 ? C2 Li1 Li2 Li1 -16.9(3) 2_655 . . 2_655 ? C13B Li1 Li2 Li1 130.4(4) . . . 2_655 ? Li2 Li1 Li2 Li1 53.0(3) 2_655 . . 2_655 ? O1 C1 Li2 O1 0.000(4) . . . . ? C2 C1 Li2 O1 -101.8(4) . . . . ? C6 C1 Li2 O1 115.6(4) . . . . ? O1 C1 Li2 O2 156.8(5) . . . 2_655 ? C2 C1 Li2 O2 55.0(4) . . . 2_655 ? C6 C1 Li2 O2 -87.6(4) . . . 2_655 ? O1 C1 Li2 O2 50.7(4) . . . . ? C2 C1 Li2 O2 -51.1(5) . . . . ? C6 C1 Li2 O2 166.2(4) . . . . ? O1 C1 Li2 Li2 103.0(5) . . . 2_655 ? C2 C1 Li2 Li2 1.2(5) . . . 2_655 ? C6 C1 Li2 Li2 -141.4(4) . . . 2_655 ? O1 C1 Li2 Li1 35.4(3) . . . . ? C2 C1 Li2 Li1 -66.4(4) . . . . ? C6 C1 Li2 Li1 151.0(3) . . . . ? O1 C1 Li2 Li1 144.2(4) . . . 2_655 ? C2 C1 Li2 Li1 42.4(3) . . . 2_655 ? C6 C1 Li2 Li1 -100.3(3) . . . 2_655 ? #END OF CIF data_chisholm987 _database_code_CSD 185859 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H72 O4 Zn3' _chemical_formula_weight 837.11 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.1517(1) _cell_length_b 17.2776(2) _cell_length_c 21.8457(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.283(1) _cell_angle_gamma 90.00 _cell_volume 4444.78(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method ? _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.641 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ;The molecule contains a crystallographic two-fold axis. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33240 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5107 _reflns_number_observed 4192 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;Atom C21, the methyl carbon atom of the ethyl ligand, acquired a very elongated anisotropic displacement parameter. This atom was then modeled as being disordered over two sites: C21A and C21B. The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+1.6257P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5107 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_obs 0.0278 _refine_ls_wR_factor_all 0.0735 _refine_ls_wR_factor_obs 0.0694 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 0.071 _refine_ls_shift/esd_mean 0.004 _refine_diff_density_max 0.451 _refine_diff_density_min -0.223 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.0000 0.611773(15) 0.2500 0.02731(8) Uani 1 d S . Zn2 Zn 0.17920(2) 0.689317(11) 0.343905(9) 0.03390(7) Uani 1 d . . O1 O 0.12621(9) 0.68965(6) 0.25133(5) 0.0272(2) Uani 1 d . . O2 O 0.08899(9) 0.59290(6) 0.33385(5) 0.0308(2) Uani 1 d . . C1 C 0.09523(13) 0.74810(9) 0.20864(7) 0.0263(3) Uani 1 d . . C2 C 0.01658(13) 0.80330(9) 0.21887(8) 0.0282(3) Uani 1 d . . C3 C -0.02824(14) 0.85848(9) 0.17200(8) 0.0316(4) Uani 1 d . . C4 C 0.00713(14) 0.85785(10) 0.11593(8) 0.0342(4) Uani 1 d . . C5 C 0.09044(15) 0.80583(10) 0.10910(8) 0.0338(4) Uani 1 d . . H5 H 0.11591(15) 0.80780(10) 0.07136(8) 0.041 Uiso 1 calc R . C6 C 0.13889(13) 0.75076(9) 0.15464(7) 0.0290(3) Uani 1 d . . C7 C -0.1138(2) 0.91736(11) 0.18198(10) 0.0459(5) Uani 1 d . . H7A H -0.0789(4) 0.9688(2) 0.1870(7) 0.069 Uiso 1 calc R . H7B H -0.1388(9) 0.9041(5) 0.2200(4) 0.069 Uiso 1 calc R . H7C H -0.1794(6) 0.9174(6) 0.1454(3) 0.069 Uiso 1 calc R . C8 C -0.0431(2) 0.91259(12) 0.06245(9) 0.0501(5) Uani 1 d . . H8A H -0.0335(11) 0.96604(13) 0.0778(2) 0.075 Uiso 1 calc R . H8B H -0.1242(3) 0.9014(5) 0.0464(4) 0.075 Uiso 1 calc R . H8C H -0.0044(8) 0.9058(6) 0.0284(3) 0.075 Uiso 1 calc R . C9 C 0.23673(15) 0.69820(10) 0.14686(8) 0.0342(4) Uani 1 d . . C10 C 0.3422(2) 0.71468(13) 0.20086(10) 0.0500(5) Uani 1 d . . H10A H 0.4044(4) 0.6806(6) 0.1967(4) 0.075 Uiso 1 calc R . H10B H 0.3241(4) 0.7052(8) 0.24152(10) 0.075 Uiso 1 calc R . H10C H 0.3652(7) 0.7688(3) 0.1987(4) 0.075 Uiso 1 calc R . C11 C 0.2687(2) 0.71349(14) 0.08425(10) 0.0558(5) Uani 1 d . . H11A H 0.3319(9) 0.6797(6) 0.0812(3) 0.084 Uiso 1 calc R . H11B H 0.2916(12) 0.7677(3) 0.0826(3) 0.084 Uiso 1 calc R . H11C H 0.2031(4) 0.7029(8) 0.04896(10) 0.084 Uiso 1 calc R . C12 C 0.2067(2) 0.61192(10) 0.14828(9) 0.0435(4) Uani 1 d . . H12A H 0.2678(5) 0.58073(11) 0.1388(6) 0.065 Uiso 1 calc R . H12B H 0.1357(6) 0.6017(2) 0.1166(4) 0.065 Uiso 1 calc R . H12C H 0.1976(11) 0.5983(2) 0.1903(2) 0.065 Uiso 1 calc R . C13 C 0.12557(15) 0.52325(10) 0.36850(8) 0.0349(4) Uani 1 d . . H13 H 0.05739(15) 0.48941(10) 0.36448(8) 0.042 Uiso 1 calc R . C14 C 0.1718(2) 0.54185(11) 0.43860(8) 0.0411(4) Uani 1 d . . H14 H 0.2411(2) 0.57460(11) 0.44296(8) 0.049 Uiso 1 calc R . C15 C 0.0866(2) 0.58745(14) 0.46496(9) 0.0546(5) Uani 1 d . . H15A H 0.1202(5) 0.6000(7) 0.5094(2) 0.082 Uiso 1 calc R . H15B H 0.0180(5) 0.5563(3) 0.4617(6) 0.082 Uiso 1 calc R . H15C H 0.0668(9) 0.6354(4) 0.4408(4) 0.082 Uiso 1 calc R . C16 C 0.2065(2) 0.46829(14) 0.47762(10) 0.0608(6) Uani 1 d . . H16A H 0.2750(8) 0.4466(5) 0.4683(6) 0.091 Uiso 1 calc R . H16B H 0.1448(6) 0.4303(4) 0.4669(5) 0.091 Uiso 1 calc R . H16C H 0.2219(13) 0.4809(2) 0.52268(10) 0.091 Uiso 1 calc R . C17 C 0.2109(2) 0.47926(11) 0.33959(10) 0.0472(5) Uani 1 d . . H17 H 0.2398(2) 0.43477(11) 0.36834(10) 0.057 Uiso 1 calc R . C18 C 0.1545(2) 0.44512(14) 0.27548(12) 0.0648(6) Uani 1 d . . H18A H 0.0877(8) 0.4151(8) 0.2786(2) 0.097 Uiso 1 calc R . H18B H 0.2084(5) 0.4112(8) 0.2616(4) 0.097 Uiso 1 calc R . H18C H 0.1312(13) 0.48699(14) 0.2448(2) 0.097 Uiso 1 calc R . C19 C 0.3137(2) 0.52764(13) 0.33595(11) 0.0577(6) Uani 1 d . . H19A H 0.3486(8) 0.5492(7) 0.3777(2) 0.087 Uiso 1 calc R . H19B H 0.2897(3) 0.5699(5) 0.3057(5) 0.087 Uiso 1 calc R . H19C H 0.3689(6) 0.4950(2) 0.3221(7) 0.087 Uiso 1 calc R . C20 C 0.2884(2) 0.74667(12) 0.40805(10) 0.0512(5) Uani 1 d . . H20A H 0.2507(2) 0.79347(12) 0.41932(10) 0.061 Uiso 0.61(2) calc PR 1 H20B H 0.3112(2) 0.71418(12) 0.44644(10) 0.061 Uiso 0.61(2) calc PR 1 H20C H 0.2760(2) 0.80254(12) 0.39885(10) 0.061 Uiso 0.39(2) calc PR 2 H20D H 0.2710(2) 0.73686(12) 0.44932(10) 0.061 Uiso 0.39(2) calc PR 2 C21A C 0.3960(6) 0.7716(8) 0.3882(5) 0.097(4) Uani 0.61(2) d P 1 H21A H 0.3773(9) 0.8139(17) 0.3574(14) 0.117 Uiso 0.61(2) calc PR 1 H21B H 0.4259(19) 0.7276(10) 0.3690(16) 0.117 Uiso 0.61(2) calc PR 1 H21C H 0.4534(13) 0.7893(21) 0.4254(6) 0.117 Uiso 0.61(2) calc PR 1 C21B C 0.4070(9) 0.7306(9) 0.4148(7) 0.087(4) Uani 0.39(2) d P 2 H21D H 0.4182(10) 0.6746(9) 0.4125(25) 0.105 Uiso 0.39(2) calc PR 2 H21E H 0.4509(10) 0.7500(27) 0.4557(12) 0.105 Uiso 0.39(2) calc PR 2 H21F H 0.4327(14) 0.7562(25) 0.3807(15) 0.105 Uiso 0.39(2) calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.03191(15) 0.02615(14) 0.02314(14) 0.000 0.00538(11) 0.000 Zn2 0.03719(12) 0.03412(13) 0.02761(11) -0.00064(8) 0.00271(9) -0.00227(8) O1 0.0308(6) 0.0272(6) 0.0239(5) 0.0027(4) 0.0073(5) 0.0009(4) O2 0.0364(6) 0.0285(6) 0.0253(6) 0.0051(5) 0.0034(5) 0.0021(5) C1 0.0273(8) 0.0254(8) 0.0247(8) 0.0016(6) 0.0037(6) -0.0039(6) C2 0.0280(8) 0.0269(8) 0.0299(8) -0.0005(6) 0.0076(7) -0.0033(6) C3 0.0314(8) 0.0265(8) 0.0353(9) 0.0031(7) 0.0054(7) -0.0015(7) C4 0.0354(9) 0.0324(9) 0.0320(9) 0.0067(7) 0.0029(7) -0.0037(7) C5 0.0389(9) 0.0380(10) 0.0256(8) 0.0026(7) 0.0101(7) -0.0074(7) C6 0.0307(8) 0.0296(9) 0.0272(8) -0.0021(6) 0.0081(7) -0.0043(7) C7 0.0441(11) 0.0403(11) 0.0535(12) 0.0071(9) 0.0126(9) 0.0120(8) C8 0.0554(12) 0.0513(12) 0.0402(11) 0.0162(9) 0.0052(9) 0.0041(10) C9 0.0347(9) 0.0378(10) 0.0337(9) -0.0010(7) 0.0155(7) 0.0005(7) C10 0.0316(10) 0.0612(13) 0.0576(13) -0.0101(10) 0.0119(9) -0.0012(9) C11 0.0666(14) 0.0628(13) 0.0497(12) 0.0079(11) 0.0368(11) 0.0123(11) C12 0.0472(11) 0.0390(10) 0.0465(11) -0.0053(8) 0.0156(9) 0.0058(8) C13 0.0391(9) 0.0317(9) 0.0335(9) 0.0089(7) 0.0084(7) 0.0026(7) C14 0.0400(10) 0.0489(11) 0.0317(9) 0.0125(8) 0.0039(8) -0.0015(8) C15 0.0616(13) 0.0725(15) 0.0293(10) 0.0016(10) 0.0105(9) 0.0003(11) C16 0.0634(14) 0.069(2) 0.0458(12) 0.0284(11) 0.0057(10) 0.0046(11) C17 0.0542(12) 0.0380(11) 0.0522(12) 0.0088(9) 0.0183(10) 0.0149(9) C18 0.079(2) 0.0502(13) 0.072(2) -0.0161(12) 0.0315(13) 0.0049(12) C19 0.0471(12) 0.0625(14) 0.0678(15) 0.0032(11) 0.0225(11) 0.0139(10) C20 0.0488(12) 0.0538(13) 0.0436(11) -0.0084(9) -0.0028(9) -0.0046(10) C21A 0.048(3) 0.133(8) 0.118(7) -0.076(6) 0.035(4) -0.036(4) C21B 0.062(5) 0.081(7) 0.100(8) -0.016(6) -0.017(5) -0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.9115(11) 2 ? Zn1 O2 1.9115(11) . ? Zn1 O1 2.0351(11) . ? Zn1 O1 2.0351(11) 2 ? Zn1 Zn2 2.9225(2) . ? Zn1 Zn2 2.9225(2) 2 ? Zn2 C20 1.947(2) . ? Zn2 O1 1.9653(11) . ? Zn2 O2 1.9764(11) . ? O1 C1 1.363(2) . ? O2 C13 1.433(2) . ? C1 C2 1.407(2) . ? C1 C6 1.409(2) . ? C2 C3 1.407(2) . ? C2 C2 1.511(3) 2 ? C3 C4 1.395(2) . ? C3 C7 1.509(2) . ? C4 C5 1.389(2) . ? C4 C8 1.510(2) . ? C5 C6 1.397(2) . ? C5 H5 0.95 . ? C6 C9 1.538(2) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C11 1.534(2) . ? C9 C12 1.537(2) . ? C9 C10 1.539(3) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.530(2) . ? C13 C17 1.541(3) . ? C13 H13 1.00 . ? C14 C15 1.523(3) . ? C14 C16 1.530(3) . ? C14 H14 1.00 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.518(3) . ? C17 C19 1.521(3) . ? C17 H17 1.00 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 C21B 1.439(11) . ? C20 C21A 1.537(7) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C20 H20C 0.99 . ? C20 H20D 0.99 . ? C21A H21A 0.98 . ? C21A H21B 0.98 . ? C21A H21C 0.98 . ? C21B H21D 0.98 . ? C21B H21E 0.98 . ? C21B H21F 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O2 160.35(7) 2 . ? O2 Zn1 O1 111.88(5) 2 . ? O2 Zn1 O1 81.55(4) . . ? O2 Zn1 O1 81.54(4) 2 2 ? O2 Zn1 O1 111.88(4) . 2 ? O1 Zn1 O1 97.22(6) . 2 ? O2 Zn1 Zn2 153.93(3) 2 . ? O2 Zn1 Zn2 42.11(3) . . ? O1 Zn1 Zn2 42.14(3) . . ? O1 Zn1 Zn2 97.78(3) 2 . ? O2 Zn1 Zn2 42.11(3) 2 2 ? O2 Zn1 Zn2 153.93(3) . 2 ? O1 Zn1 Zn2 97.77(3) . 2 ? O1 Zn1 Zn2 42.14(3) 2 2 ? Zn2 Zn1 Zn2 125.427(12) . 2 ? C20 Zn2 O1 137.00(8) . . ? C20 Zn2 O2 140.35(7) . . ? O1 Zn2 O2 81.73(4) . . ? C20 Zn2 Zn1 175.06(7) . . ? O1 Zn2 Zn1 44.01(3) . . ? O2 Zn2 Zn1 40.43(3) . . ? C1 O1 Zn2 132.17(9) . . ? C1 O1 Zn1 113.59(9) . . ? Zn2 O1 Zn1 93.85(4) . . ? C13 O2 Zn1 132.69(10) . . ? C13 O2 Zn2 123.92(10) . . ? Zn1 O2 Zn2 97.46(5) . . ? O1 C1 C2 118.52(14) . . ? O1 C1 C6 119.98(14) . . ? C2 C1 C6 121.47(14) . . ? C1 C2 C3 120.01(15) . . ? C1 C2 C2 119.06(13) . 2 ? C3 C2 C2 120.92(13) . 2 ? C4 C3 C2 119.1(2) . . ? C4 C3 C7 120.3(2) . . ? C2 C3 C7 120.6(2) . . ? C5 C4 C3 119.34(15) . . ? C5 C4 C8 119.2(2) . . ? C3 C4 C8 121.4(2) . . ? C4 C5 C6 123.7(2) . . ? C4 C5 H5 118.17(10) . . ? C6 C5 H5 118.17(10) . . ? C5 C6 C1 116.04(15) . . ? C5 C6 C9 121.65(14) . . ? C1 C6 C9 122.29(14) . . ? C3 C7 H7A 109.47(10) . . ? C3 C7 H7B 109.47(10) . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.47(10) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.47(11) . . ? C4 C8 H8B 109.47(10) . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.47(11) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C12 107.4(2) . . ? C11 C9 C6 111.68(15) . . ? C12 C9 C6 112.14(14) . . ? C11 C9 C10 107.8(2) . . ? C12 C9 C10 108.7(2) . . ? C6 C9 C10 109.03(14) . . ? C9 C10 H10A 109.47(10) . . ? C9 C10 H10B 109.47(10) . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.47(11) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.47(10) . . ? C9 C11 H11B 109.47(11) . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.47(11) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.47(10) . . ? C9 C12 H12B 109.47(10) . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.47(10) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C14 109.99(14) . . ? O2 C13 C17 110.50(14) . . ? C14 C13 C17 113.3(2) . . ? O2 C13 H13 107.60(8) . . ? C14 C13 H13 107.60(9) . . ? C17 C13 H13 107.60(10) . . ? C15 C14 C13 111.81(15) . . ? C15 C14 C16 109.8(2) . . ? C13 C14 C16 111.5(2) . . ? C15 C14 H14 107.87(12) . . ? C13 C14 H14 107.87(9) . . ? C16 C14 H14 107.87(11) . . ? C14 C15 H15A 109.47(10) . . ? C14 C15 H15B 109.47(12) . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.47(11) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.47(12) . . ? C14 C16 H16B 109.47(11) . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.47(11) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 110.8(2) . . ? C18 C17 C13 111.9(2) . . ? C19 C17 C13 113.2(2) . . ? C18 C17 H17 106.82(12) . . ? C19 C17 H17 106.82(11) . . ? C13 C17 H17 106.82(9) . . ? C17 C18 H18A 109.47(12) . . ? C17 C18 H18B 109.47(12) . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.47(12) . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.47(12) . . ? C17 C19 H19B 109.47(11) . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.47(11) . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21B C20 Zn2 117.6(5) . . ? C21A C20 Zn2 114.6(3) . . ? C21A C20 H20A 108.7(5) . . ? Zn2 C20 H20A 108.62(6) . . ? C21A C20 H20B 108.6(6) . . ? Zn2 C20 H20B 108.62(7) . . ? H20A C20 H20B 107.6 . . ? C21B C20 H20C 107.9(7) . . ? Zn2 C20 H20C 107.91(6) . . ? C21B C20 H20D 107.9(7) . . ? Zn2 C20 H20D 107.91(7) . . ? H20C C20 H20D 107.2 . . ? C20 C21A H21A 109.4(7) . . ? C20 C21A H21B 109.5(4) . . ? H21A C21A H21B 109.5 . . ? C20 C21A H21C 109.5(4) . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C20 C21B H21D 109.5(6) . . ? C20 C21B H21E 109.5(5) . . ? H21D C21B H21E 109.5 . . ? C20 C21B H21F 109.4(8) . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 Zn2 C20 98.8(8) 2 . . . ? O2 Zn1 Zn2 C20 -102.0(8) . . . . ? O1 Zn1 Zn2 C20 104.3(8) . . . . ? O1 Zn1 Zn2 C20 12.2(8) 2 . . . ? Zn2 Zn1 Zn2 C20 46.9(8) 2 . . . ? O2 Zn1 Zn2 O1 -5.55(9) 2 . . . ? O2 Zn1 Zn2 O1 153.62(7) . . . . ? O1 Zn1 Zn2 O1 0.0 . . . . ? O1 Zn1 Zn2 O1 -92.19(7) 2 . . . ? Zn2 Zn1 Zn2 O1 -57.40(4) 2 . . . ? O2 Zn1 Zn2 O2 -159.17(8) 2 . . . ? O2 Zn1 Zn2 O2 0.0 . . . . ? O1 Zn1 Zn2 O2 -153.62(7) . . . . ? O1 Zn1 Zn2 O2 114.19(6) 2 . . . ? Zn2 Zn1 Zn2 O2 148.98(5) 2 . . . ? C20 Zn2 O1 C1 -46.0(2) . . . . ? O2 Zn2 O1 C1 143.95(13) . . . . ? Zn1 Zn2 O1 C1 127.02(14) . . . . ? C20 Zn2 O1 Zn1 -172.97(10) . . . . ? O2 Zn2 O1 Zn1 16.93(4) . . . . ? Zn1 Zn2 O1 Zn1 0.0 . . . . ? O2 Zn1 O1 C1 37.60(11) 2 . . . ? O2 Zn1 O1 C1 -157.31(10) . . . . ? O1 Zn1 O1 C1 -46.15(9) 2 . . . ? Zn2 Zn1 O1 C1 -139.78(11) . . . . ? Zn2 Zn1 O1 C1 -3.63(10) 2 . . . ? O2 Zn1 O1 Zn2 177.38(4) 2 . . . ? O2 Zn1 O1 Zn2 -17.53(4) . . . . ? O1 Zn1 O1 Zn2 93.63(4) 2 . . . ? Zn2 Zn1 O1 Zn2 0.0 . . . . ? Zn2 Zn1 O1 Zn2 136.14(3) 2 . . . ? O2 Zn1 O2 C13 -0.11(13) 2 . . . ? O1 Zn1 O2 C13 -134.88(14) . . . . ? O1 Zn1 O2 C13 130.69(13) 2 . . . ? Zn2 Zn1 O2 C13 -152.4(2) . . . . ? Zn2 Zn1 O2 C13 134.70(12) 2 . . . ? O2 Zn1 O2 Zn2 152.30(4) 2 . . . ? O1 Zn1 O2 Zn2 17.54(4) . . . . ? O1 Zn1 O2 Zn2 -76.89(5) 2 . . . ? Zn2 Zn1 O2 Zn2 0.0 . . . . ? Zn2 Zn1 O2 Zn2 -72.88(9) 2 . . . ? C20 Zn2 O2 C13 -31.8(2) . . . . ? O1 Zn2 O2 C13 137.61(12) . . . . ? Zn1 Zn2 O2 C13 155.79(14) . . . . ? C20 Zn2 O2 Zn1 172.42(10) . . . . ? O1 Zn2 O2 Zn1 -18.18(5) . . . . ? Zn1 Zn2 O2 Zn1 0.0 . . . . ? Zn2 O1 C1 C2 -49.9(2) . . . . ? Zn1 O1 C1 C2 69.68(15) . . . . ? Zn2 O1 C1 C6 132.18(13) . . . . ? Zn1 O1 C1 C6 -108.20(14) . . . . ? O1 C1 C2 C3 -171.91(14) . . . . ? C6 C1 C2 C3 5.9(2) . . . . ? O1 C1 C2 C2 9.4(2) . . . 2 ? C6 C1 C2 C2 -172.76(15) . . . 2 ? C1 C2 C3 C4 -0.5(2) . . . . ? C2 C2 C3 C4 178.1(2) 2 . . . ? C1 C2 C3 C7 179.2(2) . . . . ? C2 C2 C3 C7 -2.2(3) 2 . . . ? C2 C3 C4 C5 -3.7(2) . . . . ? C7 C3 C4 C5 176.6(2) . . . . ? C2 C3 C4 C8 176.4(2) . . . . ? C7 C3 C4 C8 -3.3(3) . . . . ? C3 C4 C5 C6 2.8(3) . . . . ? C8 C4 C5 C6 -177.3(2) . . . . ? C4 C5 C6 C1 2.4(2) . . . . ? C4 C5 C6 C9 -175.7(2) . . . . ? O1 C1 C6 C5 171.11(14) . . . . ? C2 C1 C6 C5 -6.7(2) . . . . ? O1 C1 C6 C9 -10.8(2) . . . . ? C2 C1 C6 C9 171.38(15) . . . . ? C5 C6 C9 C11 -1.3(2) . . . . ? C1 C6 C9 C11 -179.3(2) . . . . ? C5 C6 C9 C12 -121.9(2) . . . . ? C1 C6 C9 C12 60.1(2) . . . . ? C5 C6 C9 C10 117.7(2) . . . . ? C1 C6 C9 C10 -60.3(2) . . . . ? Zn1 O2 C13 C14 -166.98(11) . . . . ? Zn2 O2 C13 C14 46.6(2) . . . . ? Zn1 O2 C13 C17 67.2(2) . . . . ? Zn2 O2 C13 C17 -79.2(2) . . . . ? O2 C13 C14 C15 54.0(2) . . . . ? C17 C13 C14 C15 178.2(2) . . . . ? O2 C13 C14 C16 177.3(2) . . . . ? C17 C13 C14 C16 -58.5(2) . . . . ? O2 C13 C17 C18 -69.6(2) . . . . ? C14 C13 C17 C18 166.4(2) . . . . ? O2 C13 C17 C19 56.5(2) . . . . ? C14 C13 C17 C19 -67.5(2) . . . . ? O1 Zn2 C20 C21B -73.9(9) . . . . ? O2 Zn2 C20 C21B 90.6(9) . . . . ? Zn1 Zn2 C20 C21B -173.2(10) . . . . ? O1 Zn2 C20 C21A -34.7(7) . . . . ? O2 Zn2 C20 C21A 129.8(7) . . . . ? Zn1 Zn2 C20 C21A -133.9(10) . . . . ? #END OF CIF data_Chisholm1000 _database_code_CSD 185860 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H56 Al2 O3' _chemical_formula_weight 566.75 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1bar loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2489(1) _cell_length_b 14.5356(2) _cell_length_c 19.8429(3) _cell_angle_alpha 101.212(1) _cell_angle_beta 103.271(1) _cell_angle_gamma 105.798(1) _cell_volume 3441.50(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular chunk' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.094 _exptl_crystal_density_method ? _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.114 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52871 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.04 _reflns_number_total 12146 _reflns_number_observed 8931 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;There are two molecules in the asymmetric unit and they are labeled as A and B. The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond or the Al-C bond was refined. The other hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+2.4287P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12146 _refine_ls_number_parameters 737 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_obs 0.0537 _refine_ls_wR_factor_all 0.1444 _refine_ls_wR_factor_obs 0.1281 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max -0.017 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.824 _refine_diff_density_min -0.720 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1A Al 0.17137(6) 0.02491(5) 0.21775(4) 0.0296(2) Uani 1 d . . Al2A Al 0.08651(6) -0.18329(5) 0.15532(4) 0.0346(2) Uani 1 d . . O1A O 0.22024(12) -0.07900(11) 0.19045(8) 0.0278(3) Uani 1 d . . O2A O 0.23792(13) 0.07807(11) 0.30885(8) 0.0342(4) Uani 1 d . . O3A O 0.04060(12) -0.07795(11) 0.19106(8) 0.0302(4) Uani 1 d . . C1A C 0.3300(2) -0.0691(2) 0.22451(12) 0.0276(5) Uani 1 d . . C2A C 0.4032(2) -0.0701(2) 0.18384(12) 0.0289(5) Uani 1 d . . C3A C 0.5114(2) -0.0533(2) 0.22238(13) 0.0320(5) Uani 1 d . . H3A H 0.5630(2) -0.0558(2) 0.19642(13) 0.038 Uiso 1 calc R . C4A C 0.5479(2) -0.0332(2) 0.29677(13) 0.0329(5) Uani 1 d . . C5A C 0.4736(2) -0.0319(2) 0.33598(12) 0.0330(5) Uani 1 d . . C6A C 0.3612(2) -0.0536(2) 0.29955(12) 0.0297(5) Uani 1 d . . C7A C 0.2829(2) -0.0567(2) 0.34440(12) 0.0310(5) Uani 1 d . . C8A C 0.2380(2) 0.0202(2) 0.35528(12) 0.0319(5) Uani 1 d . . C9A C 0.1953(2) 0.0391(2) 0.41348(13) 0.0386(6) Uani 1 d . . C10A C 0.1827(2) -0.0323(2) 0.45101(13) 0.0413(6) Uani 1 d . . H10A H 0.1518(2) -0.0230(2) 0.48952(13) 0.050 Uiso 1 calc R . C11A C 0.2125(2) -0.1165(2) 0.43558(12) 0.0376(6) Uani 1 d . . C12A C 0.2676(2) -0.1273(2) 0.38391(12) 0.0349(6) Uani 1 d . . C13A C 0.3701(2) -0.0930(2) 0.10091(12) 0.0328(5) Uani 1 d . . C14A C 0.3046(2) -0.2047(2) 0.06889(14) 0.0454(7) Uani 1 d . . H14A H 0.2424(9) -0.2220(3) 0.0883(7) 0.068 Uiso 1 calc R . H14B H 0.3525(4) -0.2435(2) 0.0816(8) 0.068 Uiso 1 calc R . H14C H 0.2771(12) -0.2197(3) 0.0164(2) 0.068 Uiso 1 calc R . C15A C 0.4712(2) -0.0718(2) 0.07351(14) 0.0437(6) Uani 1 d . . H15A H 0.4473(2) -0.0840(13) 0.0211(2) 0.066 Uiso 1 calc R . H15B H 0.5128(8) -0.1156(9) 0.0861(8) 0.066 Uiso 1 calc R . H15C H 0.5180(7) -0.0023(4) 0.0959(7) 0.066 Uiso 1 calc R . C16A C 0.3044(2) -0.0295(2) 0.07247(14) 0.0486(7) Uani 1 d . . H16A H 0.3445(7) 0.0408(2) 0.0976(7) 0.073 Uiso 1 calc R . H16B H 0.2325(6) -0.0488(10) 0.0809(9) 0.073 Uiso 1 calc R . H16C H 0.2941(14) -0.0401(11) 0.0207(2) 0.073 Uiso 1 calc R . C17A C 0.6687(2) -0.0121(2) 0.33335(15) 0.0483(7) Uani 1 d . . H17A H 0.7066(4) -0.0206(14) 0.2968(2) 0.072 Uiso 1 calc R . H17B H 0.6766(2) -0.0583(9) 0.3626(8) 0.072 Uiso 1 calc R . H17C H 0.7011(4) 0.0564(5) 0.3644(8) 0.072 Uiso 1 calc R . C18A C 0.5150(2) -0.0042(2) 0.41705(13) 0.0471(7) Uani 1 d . . H18A H 0.5310(14) -0.0602(5) 0.43242(14) 0.071 Uiso 1 calc R . H18B H 0.4588(6) 0.0116(13) 0.43712(13) 0.071 Uiso 1 calc R . H18C H 0.5822(9) 0.0538(9) 0.43431(14) 0.071 Uiso 1 calc R . C19A C 0.1709(3) 0.1365(2) 0.4363(2) 0.0531(7) Uani 1 d . . C20A C 0.0815(3) 0.1493(3) 0.3783(2) 0.0762(11) Uani 1 d . . H20A H 0.0691(16) 0.2118(10) 0.3963(6) 0.114 Uiso 1 calc R . H20B H 0.0132(6) 0.0936(10) 0.3665(10) 0.114 Uiso 1 calc R . H20C H 0.1050(9) 0.1509(19) 0.3351(5) 0.114 Uiso 1 calc R . C21A C 0.1339(4) 0.1416(3) 0.5045(2) 0.0933(13) Uani 1 d . . H21A H 0.1919(11) 0.1382(23) 0.5438(5) 0.140 Uiso 1 calc R . H21B H 0.0666(14) 0.0857(13) 0.4950(5) 0.140 Uiso 1 calc R . H21C H 0.1197(25) 0.2043(11) 0.5183(10) 0.140 Uiso 1 calc R . C22A C 0.2774(3) 0.2240(2) 0.4541(2) 0.0750(10) Uani 1 d . . H22A H 0.3348(6) 0.2171(10) 0.4919(9) 0.112 Uiso 1 calc R . H22B H 0.2643(6) 0.2865(3) 0.4708(13) 0.112 Uiso 1 calc R . H22C H 0.3012(11) 0.2244(11) 0.4108(4) 0.112 Uiso 1 calc R . C23A C 0.1899(2) -0.1923(2) 0.47716(14) 0.0498(7) Uani 1 d . . H23A H 0.2596(2) -0.1942(10) 0.5060(8) 0.075 Uiso 1 calc R . H23B H 0.1475(14) -0.2579(3) 0.44349(15) 0.075 Uiso 1 calc R . H23C H 0.1478(14) -0.1739(8) 0.5091(8) 0.075 Uiso 1 calc R . C24A C 0.3105(2) -0.2130(2) 0.37292(15) 0.0473(7) Uani 1 d . . H24A H 0.3449(14) -0.2117(8) 0.3342(7) 0.071 Uiso 1 calc R . H24B H 0.2495(3) -0.2757(2) 0.3598(10) 0.071 Uiso 1 calc R . H24C H 0.3650(11) -0.2077(8) 0.4175(3) 0.071 Uiso 1 calc R . C25A C -0.0695(2) -0.0734(2) 0.18944(13) 0.0344(6) Uani 1 d . . H25A H -0.0592(2) -0.0064(2) 0.22027(13) 0.041 Uiso 1 calc R . C26A C -0.1363(2) -0.0817(2) 0.11307(14) 0.0414(6) Uani 1 d . . H26A H -0.1507(2) -0.1500(2) 0.08245(14) 0.050 Uiso 1 calc R . C27A C -0.0772(2) -0.0073(2) 0.0785(2) 0.0524(7) Uani 1 d . . H27A H -0.0087(8) -0.0184(10) 0.0750(10) 0.079 Uiso 1 calc R . H27B H -0.0605(14) 0.0605(2) 0.1081(6) 0.079 Uiso 1 calc R . H27C H -0.1246(7) -0.0160(10) 0.0303(4) 0.079 Uiso 1 calc R . C28A C -0.2472(2) -0.0698(3) 0.1133(2) 0.0650(9) Uani 1 d . . H28A H -0.2354(2) -0.0051(7) 0.1456(10) 0.098 Uiso 1 calc R . H28B H -0.2890(8) -0.1229(10) 0.1299(12) 0.098 Uiso 1 calc R . H28C H -0.2885(8) -0.0737(17) 0.0644(3) 0.098 Uiso 1 calc R . C29A C -0.1276(2) -0.1507(2) 0.22281(14) 0.0413(6) Uani 1 d . . H29A H -0.1952(2) -0.1355(2) 0.22789(14) 0.050 Uiso 1 calc R . C30A C -0.0591(3) -0.1410(2) 0.2986(2) 0.0557(8) Uani 1 d . . H30A H 0.0067(9) -0.1584(15) 0.2962(2) 0.084 Uiso 1 calc R . H30B H -0.1028(6) -0.1861(11) 0.3200(4) 0.084 Uiso 1 calc R . H30C H -0.0373(14) -0.0724(4) 0.3282(3) 0.084 Uiso 1 calc R . C31A C -0.1669(2) -0.2582(2) 0.1754(2) 0.0542(7) Uani 1 d . . H31A H -0.1047(4) -0.2736(5) 0.1632(9) 0.081 Uiso 1 calc R . H31B H -0.2234(12) -0.2657(4) 0.1311(5) 0.081 Uiso 1 calc R . H31C H -0.1979(15) -0.3037(2) 0.2015(4) 0.081 Uiso 1 calc R . C32A C 0.1871(2) 0.1302(2) 0.17089(15) 0.0453(7) Uani 1 d . . H32A H 0.1455(12) 0.1725(8) 0.1861(8) 0.068 Uiso 1 calc R . H32B H 0.1588(14) 0.1014(2) 0.11857(15) 0.068 Uiso 1 calc R . H32C H 0.2649(3) 0.1702(8) 0.1842(8) 0.068 Uiso 1 calc R . C33A C 0.0236(2) -0.2261(2) 0.05037(15) 0.0528(8) Uani 1 d . . H33A H -0.0567(3) -0.2535(14) 0.03769(15) 0.079 Uiso 1 calc R . H33B H 0.0518(13) -0.2773(11) 0.0300(2) 0.079 Uiso 1 calc R . H33C H 0.0441(14) -0.1691(4) 0.0309(2) 0.079 Uiso 1 calc R . C34A C 0.0991(2) -0.2867(2) 0.2028(2) 0.0532(7) Uani 1 d . . H34A H 0.0386(9) -0.3486(4) 0.1761(6) 0.080 Uiso 1 calc R . H34B H 0.0958(16) -0.2661(7) 0.2521(4) 0.080 Uiso 1 calc R . H34C H 0.1694(7) -0.2974(10) 0.2041(9) 0.080 Uiso 1 calc R . Al1B Al 0.78287(6) 0.51655(5) 0.30904(4) 0.0318(2) Uani 1 d . . Al2B Al 0.73310(7) 0.31040(5) 0.28700(4) 0.0402(2) Uani 1 d . . O1B O 0.79725(13) 0.41080(11) 0.24871(8) 0.0320(4) Uani 1 d . . O2B O 0.70111(13) 0.56806(11) 0.25803(8) 0.0337(4) Uani 1 d . . O3B O 0.70818(13) 0.41698(11) 0.34162(8) 0.0345(4) Uani 1 d . . C1B C 0.8040(2) 0.4192(2) 0.17989(12) 0.0309(5) Uani 1 d . . C2B C 0.8973(2) 0.4148(2) 0.15977(12) 0.0332(5) Uani 1 d . . C3B C 0.8997(2) 0.4334(2) 0.09372(13) 0.0368(6) Uani 1 d . . H3B H 0.9605(2) 0.4288(2) 0.07721(13) 0.044 Uiso 1 calc R . C4B C 0.8189(2) 0.4582(2) 0.05080(13) 0.0353(6) Uani 1 d . . C5B C 0.7262(2) 0.4612(2) 0.07202(13) 0.0337(5) Uani 1 d . . C6B C 0.7164(2) 0.4377(2) 0.13631(12) 0.0302(5) Uani 1 d . . C7B C 0.6096(2) 0.4320(2) 0.15283(12) 0.0305(5) Uani 1 d . . C8B C 0.6054(2) 0.5084(2) 0.20694(12) 0.0312(5) Uani 1 d . . C9B C 0.5058(2) 0.5250(2) 0.20657(13) 0.0367(6) Uani 1 d . . C10B C 0.4108(2) 0.4519(2) 0.15953(13) 0.0404(6) Uani 1 d . . H10B H 0.3420(2) 0.4598(2) 0.15980(13) 0.048 Uiso 1 calc R . C11B C 0.4109(2) 0.3678(2) 0.11208(13) 0.0360(6) Uani 1 d . . C12B C 0.5111(2) 0.3596(2) 0.10637(12) 0.0342(5) Uani 1 d . . C13B C 0.9907(2) 0.3857(2) 0.20272(14) 0.0431(6) Uani 1 d . . C14B C 1.0859(2) 0.3956(3) 0.1691(2) 0.0606(8) Uani 1 d . . H14D H 1.1435(8) 0.3767(16) 0.1979(7) 0.091 Uiso 1 calc R . H14E H 1.1163(12) 0.4646(4) 0.1681(11) 0.091 Uiso 1 calc R . H14F H 1.0583(4) 0.3518(12) 0.1198(4) 0.091 Uiso 1 calc R . C15B C 0.9439(3) 0.2754(2) 0.2000(2) 0.0604(8) Uani 1 d . . H15D H 0.8806(11) 0.2652(4) 0.2188(11) 0.091 Uiso 1 calc R . H15E H 1.0006(6) 0.2562(5) 0.2295(9) 0.091 Uiso 1 calc R . H15F H 0.9206(16) 0.2345(3) 0.1501(2) 0.091 Uiso 1 calc R . C16B C 1.0409(2) 0.4511(2) 0.28060(15) 0.0564(8) Uani 1 d . . H16D H 0.9851(5) 0.4410(11) 0.3059(3) 0.085 Uiso 1 calc R . H16E H 1.0668(15) 0.5211(3) 0.28082(15) 0.085 Uiso 1 calc R . H16F H 1.1029(11) 0.4330(11) 0.3049(4) 0.085 Uiso 1 calc R . C17B C 0.8321(2) 0.4798(2) -0.01896(14) 0.0490(7) Uani 1 d . . H17D H 0.8447(15) 0.5506(3) -0.0147(4) 0.074 Uiso 1 calc R . H17E H 0.7652(6) 0.4401(11) -0.0585(2) 0.074 Uiso 1 calc R . H17F H 0.8949(10) 0.4628(13) -0.0288(5) 0.074 Uiso 1 calc R . C18B C 0.6398(2) 0.4916(2) 0.02640(14) 0.0455(7) Uani 1 d . . H18D H 0.5949(10) 0.5125(13) 0.0553(3) 0.068 Uiso 1 calc R . H18E H 0.5927(9) 0.4351(4) -0.0149(5) 0.068 Uiso 1 calc R . H18F H 0.6756(2) 0.5469(9) 0.0092(8) 0.068 Uiso 1 calc R . C19B C 0.5029(2) 0.6241(2) 0.2505(2) 0.0522(8) Uani 1 d . . C20B C 0.5742(4) 0.7093(3) 0.2285(2) 0.0862(12) Uani 1 d . . H20D H 0.5469(14) 0.6986(11) 0.1764(3) 0.129 Uiso 1 calc R . H20E H 0.6506(5) 0.7105(13) 0.2416(14) 0.129 Uiso 1 calc R . H20F H 0.5704(19) 0.7728(3) 0.2536(12) 0.129 Uiso 1 calc R . C21B C 0.3868(3) 0.6297(3) 0.2316(2) 0.112(2) Uani 1 d . . H21D H 0.3563(12) 0.6134(27) 0.1792(3) 0.169 Uiso 1 calc R . H21E H 0.3892(5) 0.6971(8) 0.2534(17) 0.169 Uiso 1 calc R . H21F H 0.3404(8) 0.5821(19) 0.2501(17) 0.169 Uiso 1 calc R . C22B C 0.5460(3) 0.6424(3) 0.3316(2) 0.0749(10) Uani 1 d . . H22D H 0.5017(13) 0.5884(10) 0.3462(2) 0.112 Uiso 1 calc R . H22E H 0.5412(20) 0.7058(9) 0.3560(2) 0.112 Uiso 1 calc R . H22F H 0.6228(7) 0.6448(19) 0.3448(2) 0.112 Uiso 1 calc R . C23B C 0.3035(2) 0.2909(2) 0.06402(14) 0.0469(7) Uani 1 d . . H23D H 0.3008(7) 0.2255(3) 0.0711(7) 0.070 Uiso 1 calc R . H23E H 0.2978(7) 0.2889(10) 0.0136(2) 0.070 Uiso 1 calc R . H23F H 0.2422(2) 0.3084(8) 0.0762(7) 0.070 Uiso 1 calc R . C24B C 0.5118(2) 0.2740(2) 0.04944(14) 0.0442(6) Uani 1 d . . H24D H 0.5876(3) 0.2749(8) 0.0552(6) 0.066 Uiso 1 calc R . H24E H 0.4803(14) 0.2805(7) 0.00156(14) 0.066 Uiso 1 calc R . H24F H 0.4680(12) 0.2111(2) 0.0547(6) 0.066 Uiso 1 calc R . C25B C 0.6517(2) 0.4250(2) 0.3973(2) 0.0495(7) Uani 1 d . . H25B H 0.6421(2) 0.4918(2) 0.4052(2) 0.059 Uiso 1 calc R . C26B C 0.5373(3) 0.3477(3) 0.3709(2) 0.0763(11) Uani 1 d . . H26B H 0.5054(3) 0.3663(3) 0.4105(2) 0.092 Uiso 1 calc R . C27B C 0.4645(4) 0.3541(4) 0.3116(3) 0.139(2) Uani 1 d . . H27D H 0.4747(26) 0.4242(4) 0.3141(13) 0.208 Uiso 1 calc R . H27E H 0.3891(4) 0.3205(30) 0.3108(14) 0.208 Uiso 1 calc R . H27F H 0.4777(25) 0.3223(30) 0.2678(3) 0.208 Uiso 1 calc R . C28B C 0.5320(3) 0.2418(2) 0.3698(2) 0.0802(11) Uani 1 d . . H28D H 0.5560(21) 0.2375(5) 0.4193(2) 0.120 Uiso 1 calc R . H28E H 0.5803(17) 0.2226(7) 0.3432(13) 0.120 Uiso 1 calc R . H28F H 0.4563(5) 0.1970(4) 0.3462(13) 0.120 Uiso 1 calc R . C29B C 0.7233(3) 0.4218(3) 0.4692(2) 0.0645(9) Uani 1 d . . H29B H 0.7314(3) 0.3545(3) 0.4622(2) 0.077 Uiso 1 calc R . C30B C 0.8374(3) 0.4982(3) 0.4937(2) 0.0804(11) Uani 1 d . . H30D H 0.8777(8) 0.4959(14) 0.5410(7) 0.121 Uiso 1 calc R . H30E H 0.8317(3) 0.5646(3) 0.4969(13) 0.121 Uiso 1 calc R . H30F H 0.8767(8) 0.4834(11) 0.4589(8) 0.121 Uiso 1 calc R . C31B C 0.6680(4) 0.4361(4) 0.5288(2) 0.106(2) Uani 1 d . . H31D H 0.5962(13) 0.3839(15) 0.5145(8) 0.159 Uiso 1 calc R . H31E H 0.6581(26) 0.5013(11) 0.5363(13) 0.159 Uiso 1 calc R . H31F H 0.7145(14) 0.4322(26) 0.5736(5) 0.159 Uiso 1 calc R . C32B C 0.9180(2) 0.6171(2) 0.3708(2) 0.0493(7) Uani 1 d . . H32D H 0.9654(7) 0.5856(2) 0.3962(8) 0.074 Uiso 1 calc R . H32E H 0.9016(3) 0.6639(8) 0.4059(7) 0.074 Uiso 1 calc R . H32F H 0.9556(8) 0.6529(9) 0.3417(2) 0.074 Uiso 1 calc R . C33B C 0.6169(3) 0.2061(2) 0.2094(2) 0.0650(9) Uani 1 d . . H33D H 0.5942(13) 0.1464(6) 0.2258(4) 0.097 Uiso 1 calc R . H33E H 0.6441(6) 0.1905(12) 0.1680(5) 0.097 Uiso 1 calc R . H33F H 0.5539(8) 0.2286(7) 0.1952(8) 0.097 Uiso 1 calc R . C34B C 0.8397(3) 0.2741(3) 0.3529(2) 0.0630(9) Uani 1 d . . H34D H 0.8556(14) 0.2182(11) 0.3263(3) 0.095 Uiso 1 calc R . H34E H 0.8094(8) 0.2547(16) 0.3907(7) 0.095 Uiso 1 calc R . H34F H 0.9077(7) 0.3311(6) 0.3749(9) 0.095 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1A 0.0294(4) 0.0284(4) 0.0308(4) 0.0083(3) 0.0077(3) 0.0100(3) Al2A 0.0295(4) 0.0297(4) 0.0389(4) 0.0036(3) 0.0057(3) 0.0087(3) O1A 0.0243(8) 0.0292(8) 0.0272(8) 0.0041(6) 0.0045(7) 0.0097(7) O2A 0.0401(10) 0.0301(9) 0.0308(9) 0.0056(7) 0.0083(7) 0.0131(7) O3A 0.0246(8) 0.0319(9) 0.0337(9) 0.0081(7) 0.0081(7) 0.0100(7) C1A 0.0258(12) 0.0252(12) 0.0297(12) 0.0061(9) 0.0058(10) 0.0081(9) C2A 0.0314(13) 0.0246(12) 0.0300(12) 0.0065(9) 0.0079(10) 0.0098(10) C3A 0.0297(13) 0.0302(13) 0.0365(13) 0.0075(10) 0.0106(11) 0.0113(10) C4A 0.0281(13) 0.0314(13) 0.0361(13) 0.0079(10) 0.0051(11) 0.0097(10) C5A 0.0337(13) 0.0327(13) 0.0296(12) 0.0076(10) 0.0040(11) 0.0114(11) C6A 0.0314(13) 0.0263(12) 0.0305(12) 0.0064(10) 0.0089(10) 0.0094(10) C7A 0.0290(13) 0.0341(13) 0.0254(12) 0.0055(10) 0.0051(10) 0.0076(10) C8A 0.0314(13) 0.0327(13) 0.0267(12) 0.0050(10) 0.0051(10) 0.0083(10) C9A 0.0345(14) 0.046(2) 0.0310(13) 0.0018(11) 0.0075(11) 0.0142(12) C10A 0.0344(14) 0.059(2) 0.0287(13) 0.0074(12) 0.0130(11) 0.0139(13) C11A 0.0298(13) 0.047(2) 0.0282(13) 0.0098(11) 0.0042(10) 0.0047(11) C12A 0.0354(14) 0.0368(14) 0.0280(12) 0.0072(10) 0.0052(11) 0.0099(11) C13A 0.0324(13) 0.0362(13) 0.0302(13) 0.0070(10) 0.0107(10) 0.0125(11) C14A 0.042(2) 0.045(2) 0.0387(15) -0.0011(12) 0.0117(12) 0.0078(13) C15A 0.045(2) 0.051(2) 0.0347(14) 0.0083(12) 0.0175(12) 0.0121(13) C16A 0.060(2) 0.066(2) 0.0344(14) 0.0230(13) 0.0183(13) 0.033(2) C17A 0.0323(14) 0.058(2) 0.047(2) 0.0081(13) 0.0039(12) 0.0131(13) C18A 0.042(2) 0.060(2) 0.0317(14) 0.0091(13) 0.0021(12) 0.0137(13) C19A 0.059(2) 0.053(2) 0.050(2) 0.0014(14) 0.0214(15) 0.028(2) C20A 0.076(2) 0.069(2) 0.085(3) 0.005(2) 0.012(2) 0.050(2) C21A 0.138(4) 0.093(3) 0.084(3) 0.017(2) 0.071(3) 0.067(3) C22A 0.079(2) 0.050(2) 0.078(2) -0.013(2) 0.017(2) 0.020(2) C23A 0.044(2) 0.059(2) 0.0387(15) 0.0201(13) 0.0076(13) 0.0030(14) C24A 0.061(2) 0.044(2) 0.045(2) 0.0202(13) 0.0190(14) 0.0238(14) C25A 0.0268(13) 0.0391(14) 0.0375(14) 0.0083(11) 0.0096(11) 0.0129(11) C26A 0.0288(13) 0.050(2) 0.0428(15) 0.0131(12) 0.0054(11) 0.0129(12) C27A 0.044(2) 0.067(2) 0.050(2) 0.0294(15) 0.0074(13) 0.0208(15) C28A 0.038(2) 0.096(3) 0.069(2) 0.036(2) 0.012(2) 0.030(2) C29A 0.0333(14) 0.049(2) 0.0441(15) 0.0166(12) 0.0152(12) 0.0117(12) C30A 0.056(2) 0.066(2) 0.048(2) 0.0253(15) 0.0187(14) 0.015(2) C31A 0.045(2) 0.049(2) 0.064(2) 0.0194(15) 0.0172(15) 0.0044(13) C32A 0.047(2) 0.0382(15) 0.049(2) 0.0161(12) 0.0101(13) 0.0115(12) C33A 0.039(2) 0.056(2) 0.047(2) -0.0082(14) 0.0037(13) 0.0143(14) C34A 0.047(2) 0.0352(15) 0.071(2) 0.0128(14) 0.0079(15) 0.0127(13) Al1B 0.0325(4) 0.0282(4) 0.0305(4) 0.0054(3) 0.0055(3) 0.0087(3) Al2B 0.0522(5) 0.0303(4) 0.0415(4) 0.0126(3) 0.0170(4) 0.0148(4) O1B 0.0394(9) 0.0290(8) 0.0300(9) 0.0089(7) 0.0112(7) 0.0136(7) O2B 0.0329(9) 0.0269(8) 0.0350(9) 0.0039(7) 0.0029(7) 0.0093(7) O3B 0.0381(10) 0.0320(9) 0.0327(9) 0.0088(7) 0.0115(7) 0.0101(7) C1B 0.0355(13) 0.0254(12) 0.0293(12) 0.0054(10) 0.0090(10) 0.0081(10) C2B 0.0326(13) 0.0310(13) 0.0337(13) 0.0053(10) 0.0090(11) 0.0103(10) C3B 0.0319(14) 0.0369(14) 0.0384(14) 0.0054(11) 0.0135(11) 0.0074(11) C4B 0.0333(14) 0.0320(13) 0.0339(13) 0.0059(10) 0.0084(11) 0.0040(11) C5B 0.0324(13) 0.0309(13) 0.0332(13) 0.0075(10) 0.0060(11) 0.0071(10) C6B 0.0306(13) 0.0249(12) 0.0326(13) 0.0046(10) 0.0090(10) 0.0078(10) C7B 0.0320(13) 0.0309(12) 0.0304(12) 0.0100(10) 0.0097(10) 0.0118(10) C8B 0.0321(13) 0.0292(12) 0.0295(12) 0.0081(10) 0.0067(10) 0.0078(10) C9B 0.0348(14) 0.0405(14) 0.0325(13) 0.0044(11) 0.0097(11) 0.0134(11) C10B 0.0321(14) 0.052(2) 0.0381(14) 0.0104(12) 0.0123(11) 0.0149(12) C11B 0.0317(14) 0.0414(14) 0.0306(13) 0.0096(11) 0.0085(11) 0.0060(11) C12B 0.0373(14) 0.0329(13) 0.0302(13) 0.0084(10) 0.0101(11) 0.0084(11) C13B 0.0394(15) 0.050(2) 0.044(2) 0.0132(13) 0.0124(12) 0.0221(13) C14B 0.044(2) 0.088(2) 0.064(2) 0.026(2) 0.0191(15) 0.038(2) C15B 0.070(2) 0.059(2) 0.074(2) 0.029(2) 0.029(2) 0.041(2) C16B 0.042(2) 0.077(2) 0.047(2) 0.011(2) 0.0014(13) 0.028(2) C17B 0.046(2) 0.060(2) 0.043(2) 0.0208(14) 0.0177(13) 0.0130(14) C18B 0.043(2) 0.055(2) 0.043(2) 0.0216(13) 0.0112(13) 0.0185(13) C19B 0.046(2) 0.057(2) 0.049(2) -0.0041(14) 0.0079(13) 0.0272(14) C20B 0.122(3) 0.050(2) 0.108(3) 0.026(2) 0.046(3) 0.050(2) C21B 0.069(3) 0.123(4) 0.111(3) -0.052(3) -0.005(2) 0.063(3) C22B 0.099(3) 0.071(2) 0.048(2) -0.007(2) 0.016(2) 0.039(2) C23B 0.0364(15) 0.050(2) 0.044(2) 0.0099(13) 0.0086(12) 0.0027(12) C24B 0.043(2) 0.0385(15) 0.0406(15) -0.0005(12) 0.0112(12) 0.0070(12) C25B 0.054(2) 0.043(2) 0.064(2) 0.0183(14) 0.035(2) 0.0201(14) C26B 0.047(2) 0.063(2) 0.126(3) 0.031(2) 0.034(2) 0.020(2) C27B 0.110(4) 0.089(3) 0.148(5) 0.052(3) -0.047(3) -0.018(3) C28B 0.075(2) 0.053(2) 0.120(3) 0.033(2) 0.047(2) 0.010(2) C29B 0.096(3) 0.069(2) 0.048(2) 0.028(2) 0.038(2) 0.037(2) C30B 0.092(3) 0.089(3) 0.044(2) 0.019(2) 0.004(2) 0.018(2) C31B 0.158(5) 0.110(3) 0.071(3) 0.031(2) 0.072(3) 0.043(3) C32B 0.045(2) 0.039(2) 0.050(2) 0.0035(13) 0.0032(13) 0.0071(13) C33B 0.089(2) 0.035(2) 0.057(2) 0.0098(14) 0.020(2) 0.003(2) C34B 0.083(2) 0.072(2) 0.067(2) 0.043(2) 0.038(2) 0.048(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 Al1A O2A 1.731(2) . ? Al1A O1A 1.835(2) . ? Al1A O3A 1.838(2) . ? Al1A C32A 1.929(3) . ? Al1A Al2A 2.8297(10) . ? Al2A O1A 1.866(2) . ? Al2A O3A 1.871(2) . ? Al2A C34A 1.946(3) . ? Al2A C33A 1.958(3) . ? O1A C1A 1.411(3) . ? O2A C8A 1.363(3) . ? O3A C25A 1.471(3) . ? C1A C2A 1.397(3) . ? C1A C6A 1.405(3) . ? C2A C3A 1.391(3) . ? C2A C13A 1.545(3) . ? C3A C4A 1.388(3) . ? C3A H3A 0.95 . ? C4A C5A 1.390(3) . ? C4A C17A 1.516(3) . ? C5A C6A 1.414(3) . ? C5A C18A 1.508(3) . ? C6A C7A 1.511(3) . ? C7A C8A 1.406(3) . ? C7A C12A 1.408(3) . ? C8A C9A 1.411(3) . ? C9A C10A 1.386(4) . ? C9A C19A 1.543(4) . ? C10A C11A 1.386(4) . ? C10A H10A 0.95 . ? C11A C12A 1.398(3) . ? C11A C23A 1.507(4) . ? C12A C24A 1.504(3) . ? C13A C16A 1.530(3) . ? C13A C15A 1.536(3) . ? C13A C14A 1.540(3) . ? C14A H14A 0.98 . ? C14A H14B 0.98 . ? C14A H14C 0.98 . ? C15A H15A 0.98 . ? C15A H15B 0.98 . ? C15A H15C 0.98 . ? C16A H16A 0.98 . ? C16A H16B 0.98 . ? C16A H16C 0.98 . ? C17A H17A 0.98 . ? C17A H17B 0.98 . ? C17A H17C 0.98 . ? C18A H18A 0.98 . ? C18A H18B 0.98 . ? C18A H18C 0.98 . ? C19A C20A 1.530(4) . ? C19A C22A 1.534(5) . ? C19A C21A 1.538(4) . ? C20A H20A 0.98 . ? C20A H20B 0.98 . ? C20A H20C 0.98 . ? C21A H21A 0.98 . ? C21A H21B 0.98 . ? C21A H21C 0.98 . ? C22A H22A 0.98 . ? C22A H22B 0.98 . ? C22A H22C 0.98 . ? C23A H23A 0.98 . ? C23A H23B 0.98 . ? C23A H23C 0.98 . ? C24A H24A 0.98 . ? C24A H24B 0.98 . ? C24A H24C 0.98 . ? C25A C29A 1.531(3) . ? C25A C26A 1.533(3) . ? C25A H25A 1.00 . ? C26A C27A 1.525(4) . ? C26A C28A 1.527(4) . ? C26A H26A 1.00 . ? C27A H27A 0.98 . ? C27A H27B 0.98 . ? C27A H27C 0.98 . ? C28A H28A 0.98 . ? C28A H28B 0.98 . ? C28A H28C 0.98 . ? C29A C30A 1.525(4) . ? C29A C31A 1.536(4) . ? C29A H29A 1.00 . ? C30A H30A 0.98 . ? C30A H30B 0.98 . ? C30A H30C 0.98 . ? C31A H31A 0.98 . ? C31A H31B 0.98 . ? C31A H31C 0.98 . ? C32A H32A 0.98 . ? C32A H32B 0.98 . ? C32A H32C 0.98 . ? C33A H33A 0.98 . ? C33A H33B 0.98 . ? C33A H33C 0.98 . ? C34A H34A 0.98 . ? C34A H34B 0.98 . ? C34A H34C 0.98 . ? Al1B O2B 1.730(2) . ? Al1B O3B 1.836(2) . ? Al1B O1B 1.839(2) . ? Al1B C32B 1.927(3) . ? Al1B Al2B 2.8084(10) . ? Al2B O3B 1.864(2) . ? Al2B O1B 1.866(2) . ? Al2B C33B 1.942(3) . ? Al2B C34B 1.953(3) . ? O1B C1B 1.415(3) . ? O2B C8B 1.362(3) . ? O3B C25B 1.473(3) . ? C1B C2B 1.397(3) . ? C1B C6B 1.403(3) . ? C2B C3B 1.394(3) . ? C2B C13B 1.542(3) . ? C3B C4B 1.383(3) . ? C3B H3B 0.95 . ? C4B C5B 1.395(3) . ? C4B C17B 1.515(3) . ? C5B C6B 1.407(3) . ? C5B C18B 1.510(3) . ? C6B C7B 1.509(3) . ? C7B C12B 1.408(3) . ? C7B C8B 1.409(3) . ? C8B C9B 1.404(3) . ? C9B C10B 1.390(3) . ? C9B C19B 1.547(4) . ? C10B C11B 1.391(4) . ? C10B H10B 0.95 . ? C11B C12B 1.392(3) . ? C11B C23B 1.510(3) . ? C12B C24B 1.513(3) . ? C13B C16B 1.532(4) . ? C13B C15B 1.539(4) . ? C13B C14B 1.544(4) . ? C14B H14D 0.98 . ? C14B H14E 0.98 . ? C14B H14F 0.98 . ? C15B H15D 0.98 . ? C15B H15E 0.98 . ? C15B H15F 0.98 . ? C16B H16D 0.98 . ? C16B H16E 0.98 . ? C16B H16F 0.98 . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? C18B H18D 0.98 . ? C18B H18E 0.98 . ? C18B H18F 0.98 . ? C19B C22B 1.522(4) . ? C19B C21B 1.526(4) . ? C19B C20B 1.542(5) . ? C20B H20D 0.98 . ? C20B H20E 0.98 . ? C20B H20F 0.98 . ? C21B H21D 0.98 . ? C21B H21E 0.98 . ? C21B H21F 0.98 . ? C22B H22D 0.98 . ? C22B H22E 0.98 . ? C22B H22F 0.98 . ? C23B H23D 0.98 . ? C23B H23E 0.98 . ? C23B H23F 0.98 . ? C24B H24D 0.98 . ? C24B H24E 0.98 . ? C24B H24F 0.98 . ? C25B C26B 1.520(4) . ? C25B C29B 1.538(4) . ? C25B H25B 1.00 . ? C26B C27B 1.376(5) . ? C26B C28B 1.517(5) . ? C26B H26B 1.00 . ? C27B H27D 0.98 . ? C27B H27E 0.98 . ? C27B H27F 0.98 . ? C28B H28D 0.98 . ? C28B H28E 0.98 . ? C28B H28F 0.98 . ? C29B C30B 1.514(5) . ? C29B C31B 1.537(5) . ? C29B H29B 1.00 . ? C30B H30D 0.98 . ? C30B H30E 0.98 . ? C30B H30F 0.98 . ? C31B H31D 0.98 . ? C31B H31E 0.98 . ? C31B H31F 0.98 . ? C32B H32D 0.98 . ? C32B H32E 0.98 . ? C32B H32F 0.98 . ? C33B H33D 0.98 . ? C33B H33E 0.98 . ? C33B H33F 0.98 . ? C34B H34D 0.98 . ? C34B H34E 0.98 . ? C34B H34F 0.98 . ? 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 O2A Al1A O1A 106.38(7) . . ? O2A Al1A O3A 117.84(8) . . ? O1A Al1A O3A 81.05(7) . . ? O2A Al1A C32A 107.82(10) . . ? O1A Al1A C32A 120.67(10) . . ? O3A Al1A C32A 120.65(10) . . ? O2A Al1A Al2A 122.61(6) . . ? O1A Al1A Al2A 40.54(5) . . ? O3A Al1A Al2A 40.71(5) . . ? C32A Al1A Al2A 128.99(9) . . ? O1A Al2A O3A 79.39(7) . . ? O1A Al2A C34A 108.51(10) . . ? O3A Al2A C34A 123.74(11) . . ? O1A Al2A C33A 115.09(11) . . ? O3A Al2A C33A 107.92(10) . . ? C34A Al2A C33A 116.69(13) . . ? O1A Al2A Al1A 39.74(5) . . ? O3A Al2A Al1A 39.84(5) . . ? C34A Al2A Al1A 127.51(9) . . ? C33A Al2A Al1A 115.36(10) . . ? C1A O1A Al1A 118.25(13) . . ? C1A O1A Al2A 135.25(13) . . ? Al1A O1A Al2A 99.71(7) . . ? C8A O2A Al1A 120.25(14) . . ? C25A O3A Al1A 128.70(14) . . ? C25A O3A Al2A 131.32(14) . . ? Al1A O3A Al2A 99.45(7) . . ? C2A C1A C6A 123.3(2) . . ? C2A C1A O1A 119.6(2) . . ? C6A C1A O1A 117.0(2) . . ? C3A C2A C1A 115.8(2) . . ? C3A C2A C13A 119.6(2) . . ? C1A C2A C13A 124.5(2) . . ? C4A C3A C2A 123.4(2) . . ? C4A C3A H3A 118.29(14) . . ? C2A C3A H3A 118.29(14) . . ? C3A C4A C5A 119.6(2) . . ? C3A C4A C17A 118.9(2) . . ? C5A C4A C17A 121.6(2) . . ? C4A C5A C6A 119.7(2) . . ? C4A C5A C18A 119.2(2) . . ? C6A C5A C18A 121.1(2) . . ? C1A C6A C5A 118.1(2) . . ? C1A C6A C7A 124.4(2) . . ? C5A C6A C7A 117.5(2) . . ? C8A C7A C12A 119.4(2) . . ? C8A C7A C6A 119.6(2) . . ? C12A C7A C6A 120.3(2) . . ? O2A C8A C7A 118.6(2) . . ? O2A C8A C9A 120.1(2) . . ? C7A C8A C9A 121.3(2) . . ? C10A C9A C8A 116.0(2) . . ? C10A C9A C19A 122.4(2) . . ? C8A C9A C19A 121.5(2) . . ? C11A C10A C9A 123.7(2) . . ? C11A C10A H10A 118.13(15) . . ? C9A C10A H10A 118.13(14) . . ? C10A C11A C12A 119.2(2) . . ? C10A C11A C23A 119.6(2) . . ? C12A C11A C23A 121.2(2) . . ? C11A C12A C7A 119.1(2) . . ? C11A C12A C24A 119.1(2) . . ? C7A C12A C24A 121.9(2) . . ? C16A C13A C15A 105.9(2) . . ? C16A C13A C14A 111.2(2) . . ? C15A C13A C14A 107.2(2) . . ? C16A C13A C2A 112.6(2) . . ? C15A C13A C2A 111.7(2) . . ? C14A C13A C2A 108.1(2) . . ? C13A C14A H14A 109.47(13) . . ? C13A C14A H14B 109.47(14) . . ? H14A C14A H14B 109.5 . . ? C13A C14A H14C 109.47(13) . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C13A C15A H15A 109.47(13) . . ? C13A C15A H15B 109.47(14) . . ? H15A C15A H15B 109.5 . . ? C13A C15A H15C 109.47(13) . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C13A C16A H16A 109.47(15) . . ? C13A C16A H16B 109.47(14) . . ? H16A C16A H16B 109.5 . . ? C13A C16A H16C 109.47(13) . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C4A C17A H17A 109.47(14) . . ? C4A C17A H17B 109.47(15) . . ? H17A C17A H17B 109.5 . . ? C4A C17A H17C 109.47(14) . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C5A C18A H18A 109.47(14) . . ? C5A C18A H18B 109.47(14) . . ? H18A C18A H18B 109.5 . . ? C5A C18A H18C 109.47(14) . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C20A C19A C22A 108.9(3) . . ? C20A C19A C21A 107.5(3) . . ? C22A C19A C21A 107.7(3) . . ? C20A C19A C9A 113.4(2) . . ? C22A C19A C9A 108.3(2) . . ? C21A C19A C9A 110.9(3) . . ? C19A C20A H20A 109.5(2) . . ? C19A C20A H20B 109.5(2) . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5(2) . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5(2) . . ? C19A C21A H21B 109.5(2) . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5(2) . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C19A C22A H22A 109.5(2) . . ? C19A C22A H22B 109.5(2) . . ? H22A C22A H22B 109.5 . . ? C19A C22A H22C 109.5(2) . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C11A C23A H23A 109.47(14) . . ? C11A C23A H23B 109.47(14) . . ? H23A C23A H23B 109.5 . . ? C11A C23A H23C 109.5(2) . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C12A C24A H24A 109.47(14) . . ? C12A C24A H24B 109.47(15) . . ? H24A C24A H24B 109.5 . . ? C12A C24A H24C 109.47(14) . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? O3A C25A C29A 110.7(2) . . ? O3A C25A C26A 110.9(2) . . ? C29A C25A C26A 113.4(2) . . ? O3A C25A H25A 107.17(11) . . ? C29A C25A H25A 107.17(14) . . ? C26A C25A H25A 107.17(14) . . ? C27A C26A C28A 109.5(2) . . ? C27A C26A C25A 113.7(2) . . ? C28A C26A C25A 110.2(2) . . ? C27A C26A H26A 107.8(2) . . ? C28A C26A H26A 107.8(2) . . ? C25A C26A H26A 107.75(14) . . ? C26A C27A H27A 109.47(14) . . ? C26A C27A H27B 109.5(2) . . ? H27A C27A H27B 109.5 . . ? C26A C27A H27C 109.47(14) . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C26A C28A H28A 109.5(2) . . ? C26A C28A H28B 109.5(2) . . ? H28A C28A H28B 109.5 . . ? C26A C28A H28C 109.5(2) . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C30A C29A C25A 112.2(2) . . ? C30A C29A C31A 111.1(2) . . ? C25A C29A C31A 113.9(2) . . ? C30A C29A H29A 106.3(2) . . ? C25A C29A H29A 106.33(13) . . ? C31A C29A H29A 106.33(15) . . ? C29A C30A H30A 109.5(2) . . ? C29A C30A H30B 109.47(15) . . ? H30A C30A H30B 109.5 . . ? C29A C30A H30C 109.5(2) . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C29A C31A H31A 109.47(15) . . ? C29A C31A H31B 109.47(15) . . ? H31A C31A H31B 109.5 . . ? C29A C31A H31C 109.47(15) . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? Al1A C32A H32A 109.47(9) . . ? Al1A C32A H32B 109.47(8) . . ? H32A C32A H32B 109.5 . . ? Al1A C32A H32C 109.47(8) . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? Al2A C33A H33A 109.47(9) . . ? Al2A C33A H33B 109.47(9) . . ? H33A C33A H33B 109.5 . . ? Al2A C33A H33C 109.47(10) . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? Al2A C34A H34A 109.47(9) . . ? Al2A C34A H34B 109.47(9) . . ? H34A C34A H34B 109.5 . . ? Al2A C34A H34C 109.47(9) . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? O2B Al1B O3B 114.95(8) . . ? O2B Al1B O1B 108.69(8) . . ? O3B Al1B O1B 81.83(7) . . ? O2B Al1B C32B 110.90(11) . . ? O3B Al1B C32B 121.00(11) . . ? O1B Al1B C32B 116.02(11) . . ? O2B Al1B Al2B 122.69(6) . . ? O3B Al1B Al2B 40.98(5) . . ? O1B Al1B Al2B 41.07(5) . . ? C32B Al1B Al2B 125.85(9) . . ? O3B Al2B O1B 80.37(7) . . ? O3B Al2B C33B 122.56(13) . . ? O1B Al2B C33B 108.40(11) . . ? O3B Al2B C34B 106.69(12) . . ? O1B Al2B C34B 113.65(12) . . ? C33B Al2B C34B 118.96(15) . . ? O3B Al2B Al1B 40.24(5) . . ? O1B Al2B Al1B 40.34(5) . . ? C33B Al2B Al1B 127.11(10) . . ? C34B Al2B Al1B 113.58(11) . . ? C1B O1B Al1B 117.45(13) . . ? C1B O1B Al2B 136.51(14) . . ? Al1B O1B Al2B 98.59(8) . . ? C8B O2B Al1B 120.12(14) . . ? C25B O3B Al1B 128.40(15) . . ? C25B O3B Al2B 132.75(15) . . ? Al1B O3B Al2B 98.78(8) . . ? C2B C1B C6B 123.0(2) . . ? C2B C1B O1B 120.3(2) . . ? C6B C1B O1B 116.6(2) . . ? C3B C2B C1B 115.3(2) . . ? C3B C2B C13B 119.8(2) . . ? C1B C2B C13B 124.8(2) . . ? C4B C3B C2B 124.0(2) . . ? C4B C3B H3B 118.02(14) . . ? C2B C3B H3B 118.02(14) . . ? C3B C4B C5B 119.4(2) . . ? C3B C4B C17B 119.2(2) . . ? C5B C4B C17B 121.4(2) . . ? C4B C5B C6B 119.2(2) . . ? C4B C5B C18B 119.3(2) . . ? C6B C5B C18B 121.4(2) . . ? C1B C6B C5B 118.8(2) . . ? C1B C6B C7B 124.2(2) . . ? C5B C6B C7B 116.9(2) . . ? C12B C7B C8B 119.6(2) . . ? C12B C7B C6B 119.5(2) . . ? C8B C7B C6B 120.0(2) . . ? O2B C8B C9B 120.8(2) . . ? O2B C8B C7B 118.4(2) . . ? C9B C8B C7B 120.8(2) . . ? C10B C9B C8B 116.5(2) . . ? C10B C9B C19B 121.7(2) . . ? C8B C9B C19B 121.6(2) . . ? C9B C10B C11B 123.6(2) . . ? C9B C10B H10B 118.20(14) . . ? C11B C10B H10B 118.20(14) . . ? C10B C11B C12B 118.8(2) . . ? C10B C11B C23B 120.0(2) . . ? C12B C11B C23B 121.0(2) . . ? C11B C12B C7B 119.4(2) . . ? C11B C12B C24B 119.3(2) . . ? C7B C12B C24B 121.4(2) . . ? C16B C13B C15B 111.1(2) . . ? C16B C13B C2B 112.3(2) . . ? C15B C13B C2B 108.0(2) . . ? C16B C13B C14B 106.6(2) . . ? C15B C13B C14B 106.9(2) . . ? C2B C13B C14B 112.0(2) . . ? C13B C14B H14D 109.47(15) . . ? C13B C14B H14E 109.5(2) . . ? H14D C14B H14E 109.5 . . ? C13B C14B H14F 109.5(2) . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13B C15B H15D 109.47(15) . . ? C13B C15B H15E 109.5(2) . . ? H15D C15B H15E 109.5 . . ? C13B C15B H15F 109.5(2) . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C13B C16B H16D 109.5(2) . . ? C13B C16B H16E 109.5(2) . . ? H16D C16B H16E 109.5 . . ? C13B C16B H16F 109.47(14) . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C4B C17B H17D 109.47(15) . . ? C4B C17B H17E 109.47(14) . . ? H17D C17B H17E 109.5 . . ? C4B C17B H17F 109.47(15) . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C5B C18B H18D 109.47(14) . . ? C5B C18B H18E 109.47(14) . . ? H18D C18B H18E 109.5 . . ? C5B C18B H18F 109.47(14) . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C22B C19B C21B 108.8(3) . . ? C22B C19B C20B 108.7(3) . . ? C21B C19B C20B 106.5(3) . . ? C22B C19B C9B 113.7(2) . . ? C21B C19B C9B 111.1(2) . . ? C20B C19B C9B 107.8(2) . . ? C19B C20B H20D 109.5(2) . . ? C19B C20B H20E 109.5(2) . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5(2) . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19B C21B H21D 109.5(2) . . ? C19B C21B H21E 109.5(2) . . ? H21D C21B H21E 109.5 . . ? C19B C21B H21F 109.5(3) . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C19B C22B H22D 109.5(2) . . ? C19B C22B H22E 109.5(2) . . ? H22D C22B H22E 109.5 . . ? C19B C22B H22F 109.5(2) . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C11B C23B H23D 109.47(14) . . ? C11B C23B H23E 109.47(14) . . ? H23D C23B H23E 109.5 . . ? C11B C23B H23F 109.47(15) . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C12B C24B H24D 109.47(14) . . ? C12B C24B H24E 109.47(14) . . ? H24D C24B H24E 109.5 . . ? C12B C24B H24F 109.47(14) . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? O3B C25B C26B 110.7(3) . . ? O3B C25B C29B 110.7(2) . . ? C26B C25B C29B 113.8(3) . . ? O3B C25B H25B 107.09(12) . . ? C26B C25B H25B 107.1(2) . . ? C29B C25B H25B 107.1(2) . . ? C27B C26B C28B 113.3(4) . . ? C27B C26B C25B 116.8(3) . . ? C28B C26B C25B 116.1(3) . . ? C27B C26B H26B 102.6(3) . . ? C28B C26B H26B 102.6(2) . . ? C25B C26B H26B 102.6(2) . . ? C26B C27B H27D 109.5(2) . . ? C26B C27B H27E 109.5(3) . . ? H27D C27B H27E 109.5 . . ? C26B C27B H27F 109.5(3) . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C26B C28B H28D 109.5(2) . . ? C26B C28B H28E 109.5(2) . . ? H28D C28B H28E 109.5 . . ? C26B C28B H28F 109.5(2) . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C30B C29B C31B 109.3(3) . . ? C30B C29B C25B 112.9(3) . . ? C31B C29B C25B 111.2(3) . . ? C30B C29B H29B 107.8(2) . . ? C31B C29B H29B 107.8(2) . . ? C25B C29B H29B 107.8(2) . . ? C29B C30B H30D 109.5(2) . . ? C29B C30B H30E 109.5(2) . . ? H30D C30B H30E 109.5 . . ? C29B C30B H30F 109.5(2) . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C29B C31B H31D 109.5(2) . . ? C29B C31B H31E 109.5(2) . . ? H31D C31B H31E 109.5 . . ? C29B C31B H31F 109.5(2) . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? Al1B C32B H32D 109.47(9) . . ? Al1B C32B H32E 109.47(9) . . ? H32D C32B H32E 109.5 . . ? Al1B C32B H32F 109.47(9) . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? Al2B C33B H33D 109.47(9) . . ? Al2B C33B H33E 109.47(11) . . ? H33D C33B H33E 109.5 . . ? Al2B C33B H33F 109.47(11) . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? Al2B C34B H34D 109.47(10) . . ? Al2B C34B H34E 109.47(10) . . ? H34D C34B H34E 109.5 . . ? Al2B C34B H34F 109.47(11) . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2A Al1A Al2A O1A -76.54(10) . . . . ? O1A Al1A Al2A O1A 0.0 . . . . ? O3A Al1A Al2A O1A -172.66(11) . . . . ? C32A Al1A Al2A O1A 93.63(14) . . . . ? O2A Al1A Al2A O3A 96.12(11) . . . . ? O1A Al1A Al2A O3A 172.66(11) . . . . ? O3A Al1A Al2A O3A 0.0 . . . . ? C32A Al1A Al2A O3A -93.71(14) . . . . ? O2A Al1A Al2A C34A -3.83(15) . . . . ? O1A Al1A Al2A C34A 72.71(14) . . . . ? O3A Al1A Al2A C34A -99.95(14) . . . . ? C32A Al1A Al2A C34A 166.3(2) . . . . ? O2A Al1A Al2A C33A -175.97(12) . . . . ? O1A Al1A Al2A C33A -99.43(12) . . . . ? O3A Al1A Al2A C33A 87.91(12) . . . . ? C32A Al1A Al2A C33A -5.8(2) . . . . ? O2A Al1A O1A C1A -34.1(2) . . . . ? O3A Al1A O1A C1A -150.7(2) . . . . ? C32A Al1A O1A C1A 88.9(2) . . . . ? Al2A Al1A O1A C1A -155.5(2) . . . . ? O2A Al1A O1A Al2A 121.36(8) . . . . ? O3A Al1A O1A Al2A 4.84(7) . . . . ? C32A Al1A O1A Al2A -115.60(11) . . . . ? Al2A Al1A O1A Al2A 0.0 . . . . ? O3A Al2A O1A C1A 144.0(2) . . . . ? C34A Al2A O1A C1A 21.7(2) . . . . ? C33A Al2A O1A C1A -111.1(2) . . . . ? Al1A Al2A O1A C1A 148.7(2) . . . . ? O3A Al2A O1A Al1A -4.78(7) . . . . ? C34A Al2A O1A Al1A -127.00(11) . . . . ? C33A Al2A O1A Al1A 100.18(11) . . . . ? Al1A Al2A O1A Al1A 0.0 . . . . ? O1A Al1A O2A C8A -50.4(2) . . . . ? O3A Al1A O2A C8A 38.0(2) . . . . ? C32A Al1A O2A C8A 178.8(2) . . . . ? Al2A Al1A O2A C8A -9.2(2) . . . . ? O2A Al1A O3A C25A 79.0(2) . . . . ? O1A Al1A O3A C25A -177.1(2) . . . . ? C32A Al1A O3A C25A -56.7(2) . . . . ? Al2A Al1A O3A C25A -172.3(2) . . . . ? O2A Al1A O3A Al2A -108.69(9) . . . . ? O1A Al1A O3A Al2A -4.82(7) . . . . ? C32A Al1A O3A Al2A 115.64(12) . . . . ? Al2A Al1A O3A Al2A 0.0 . . . . ? O1A Al2A O3A C25A 176.8(2) . . . . ? C34A Al2A O3A C25A -78.0(2) . . . . ? C33A Al2A O3A C25A 63.6(2) . . . . ? Al1A Al2A O3A C25A 172.0(2) . . . . ? O1A Al2A O3A Al1A 4.77(7) . . . . ? C34A Al2A O3A Al1A 110.03(12) . . . . ? C33A Al2A O3A Al1A -108.36(12) . . . . ? Al1A Al2A O3A Al1A 0.0 . . . . ? Al1A O1A C1A C2A -116.9(2) . . . . ? Al2A O1A C1A C2A 98.6(2) . . . . ? Al1A O1A C1A C6A 59.9(2) . . . . ? Al2A O1A C1A C6A -84.6(2) . . . . ? C6A C1A C2A C3A -0.7(3) . . . . ? O1A C1A C2A C3A 175.9(2) . . . . ? C6A C1A C2A C13A 176.3(2) . . . . ? O1A C1A C2A C13A -7.1(3) . . . . ? C1A C2A C3A C4A -2.2(3) . . . . ? C13A C2A C3A C4A -179.4(2) . . . . ? C2A C3A C4A C5A 1.8(4) . . . . ? C2A C3A C4A C17A -177.6(2) . . . . ? C3A C4A C5A C6A 1.7(3) . . . . ? C17A C4A C5A C6A -179.0(2) . . . . ? C3A C4A C5A C18A -176.6(2) . . . . ? C17A C4A C5A C18A 2.8(4) . . . . ? C2A C1A C6A C5A 4.0(3) . . . . ? O1A C1A C6A C5A -172.7(2) . . . . ? C2A C1A C6A C7A -177.2(2) . . . . ? O1A C1A C6A C7A 6.1(3) . . . . ? C4A C5A C6A C1A -4.4(3) . . . . ? C18A C5A C6A C1A 173.8(2) . . . . ? C4A C5A C6A C7A 176.7(2) . . . . ? C18A C5A C6A C7A -5.1(3) . . . . ? C1A C6A C7A C8A -71.0(3) . . . . ? C5A C6A C7A C8A 107.9(2) . . . . ? C1A C6A C7A C12A 118.5(3) . . . . ? C5A C6A C7A C12A -62.6(3) . . . . ? Al1A O2A C8A C7A 59.0(3) . . . . ? Al1A O2A C8A C9A -122.1(2) . . . . ? C12A C7A C8A O2A -169.5(2) . . . . ? C6A C7A C8A O2A 19.9(3) . . . . ? C12A C7A C8A C9A 11.6(3) . . . . ? C6A C7A C8A C9A -159.0(2) . . . . ? O2A C8A C9A C10A 170.2(2) . . . . ? C7A C8A C9A C10A -10.9(3) . . . . ? O2A C8A C9A C19A -13.3(3) . . . . ? C7A C8A C9A C19A 165.6(2) . . . . ? C8A C9A C10A C11A 2.1(4) . . . . ? C19A C9A C10A C11A -174.4(2) . . . . ? C9A C10A C11A C12A 6.1(4) . . . . ? C9A C10A C11A C23A -176.8(2) . . . . ? C10A C11A C12A C7A -5.5(3) . . . . ? C23A C11A C12A C7A 177.5(2) . . . . ? C10A C11A C12A C24A 173.5(2) . . . . ? C23A C11A C12A C24A -3.5(4) . . . . ? C8A C7A C12A C11A -3.0(3) . . . . ? C6A C7A C12A C11A 167.5(2) . . . . ? C8A C7A C12A C24A 178.0(2) . . . . ? C6A C7A C12A C24A -11.5(3) . . . . ? C3A C2A C13A C16A -131.2(2) . . . . ? C1A C2A C13A C16A 51.9(3) . . . . ? C3A C2A C13A C15A -12.3(3) . . . . ? C1A C2A C13A C15A 170.8(2) . . . . ? C3A C2A C13A C14A 105.5(2) . . . . ? C1A C2A C13A C14A -71.4(3) . . . . ? C10A C9A C19A C20A -120.2(3) . . . . ? C8A C9A C19A C20A 63.4(4) . . . . ? C10A C9A C19A C22A 118.7(3) . . . . ? C8A C9A C19A C22A -57.6(3) . . . . ? C10A C9A C19A C21A 0.8(4) . . . . ? C8A C9A C19A C21A -175.5(3) . . . . ? Al1A O3A C25A C29A -134.6(2) . . . . ? Al2A O3A C25A C29A 55.5(3) . . . . ? Al1A O3A C25A C26A 98.6(2) . . . . ? Al2A O3A C25A C26A -71.3(2) . . . . ? O3A C25A C26A C27A -52.8(3) . . . . ? C29A C25A C26A C27A -178.1(2) . . . . ? O3A C25A C26A C28A -176.1(2) . . . . ? C29A C25A C26A C28A 58.6(3) . . . . ? O3A C25A C29A C30A 54.4(3) . . . . ? C26A C25A C29A C30A 179.7(2) . . . . ? O3A C25A C29A C31A -73.0(3) . . . . ? C26A C25A C29A C31A 52.4(3) . . . . ? O2B Al1B Al2B O3B -91.46(11) . . . . ? O3B Al1B Al2B O3B 0.0 . . . . ? O1B Al1B Al2B O3B -172.43(12) . . . . ? C32B Al1B Al2B O3B 97.88(14) . . . . ? O2B Al1B Al2B O1B 80.97(11) . . . . ? O3B Al1B Al2B O1B 172.43(11) . . . . ? O1B Al1B Al2B O1B 0.0 . . . . ? C32B Al1B Al2B O1B -89.69(14) . . . . ? O2B Al1B Al2B C33B 7.2(2) . . . . ? O3B Al1B Al2B C33B 98.7(2) . . . . ? O1B Al1B Al2B C33B -73.8(2) . . . . ? C32B Al1B Al2B C33B -163.5(2) . . . . ? O2B Al1B Al2B C34B -179.70(12) . . . . ? O3B Al1B Al2B C34B -88.24(13) . . . . ? O1B Al1B Al2B C34B 99.33(13) . . . . ? C32B Al1B Al2B C34B 9.6(2) . . . . ? O2B Al1B O1B C1B 36.2(2) . . . . ? O3B Al1B O1B C1B 149.9(2) . . . . ? C32B Al1B O1B C1B -89.6(2) . . . . ? Al2B Al1B O1B C1B 154.9(2) . . . . ? O2B Al1B O1B Al2B -118.67(8) . . . . ? O3B Al1B O1B Al2B -5.01(8) . . . . ? C32B Al1B O1B Al2B 115.58(12) . . . . ? Al2B Al1B O1B Al2B 0.0 . . . . ? O3B Al2B O1B C1B -141.8(2) . . . . ? C33B Al2B O1B C1B -20.6(2) . . . . ? C34B Al2B O1B C1B 114.1(2) . . . . ? Al1B Al2B O1B C1B -146.8(2) . . . . ? O3B Al2B O1B Al1B 4.95(8) . . . . ? C33B Al2B O1B Al1B 126.20(13) . . . . ? C34B Al2B O1B Al1B -99.16(13) . . . . ? Al1B Al2B O1B Al1B 0.0 . . . . ? O3B Al1B O2B C8B -43.1(2) . . . . ? O1B Al1B O2B C8B 46.4(2) . . . . ? C32B Al1B O2B C8B 175.1(2) . . . . ? Al2B Al1B O2B C8B 3.2(2) . . . . ? O2B Al1B O3B C25B -70.7(2) . . . . ? O1B Al1B O3B C25B -177.6(2) . . . . ? C32B Al1B O3B C25B 66.9(2) . . . . ? Al2B Al1B O3B C25B 177.4(2) . . . . ? O2B Al1B O3B Al2B 111.89(9) . . . . ? O1B Al1B O3B Al2B 5.01(8) . . . . ? C32B Al1B O3B Al2B -110.50(12) . . . . ? Al2B Al1B O3B Al2B 0.0 . . . . ? O1B Al2B O3B C25B 177.8(2) . . . . ? C33B Al2B O3B C25B 72.0(2) . . . . ? C34B Al2B O3B C25B -70.3(2) . . . . ? Al1B Al2B O3B C25B -177.2(2) . . . . ? O1B Al2B O3B Al1B -4.96(8) . . . . ? C33B Al2B O3B Al1B -110.71(13) . . . . ? C34B Al2B O3B Al1B 106.99(12) . . . . ? Al1B Al2B O3B Al1B 0.0 . . . . ? Al1B O1B C1B C2B 119.1(2) . . . . ? Al2B O1B C1B C2B -98.5(3) . . . . ? Al1B O1B C1B C6B -57.2(2) . . . . ? Al2B O1B C1B C6B 85.2(2) . . . . ? C6B C1B C2B C3B 2.0(3) . . . . ? O1B C1B C2B C3B -174.1(2) . . . . ? C6B C1B C2B C13B -174.4(2) . . . . ? O1B C1B C2B C13B 9.5(3) . . . . ? C1B C2B C3B C4B 2.2(4) . . . . ? C13B C2B C3B C4B 178.8(2) . . . . ? C2B C3B C4B C5B -2.9(4) . . . . ? C2B C3B C4B C17B 178.2(2) . . . . ? C3B C4B C5B C6B -0.7(3) . . . . ? C17B C4B C5B C6B 178.2(2) . . . . ? C3B C4B C5B C18B 178.0(2) . . . . ? C17B C4B C5B C18B -3.1(4) . . . . ? C2B C1B C6B C5B -5.4(3) . . . . ? O1B C1B C6B C5B 170.8(2) . . . . ? C2B C1B C6B C7B 173.1(2) . . . . ? O1B C1B C6B C7B -10.6(3) . . . . ? C4B C5B C6B C1B 4.7(3) . . . . ? C18B C5B C6B C1B -174.0(2) . . . . ? C4B C5B C6B C7B -174.0(2) . . . . ? C18B C5B C6B C7B 7.3(3) . . . . ? C1B C6B C7B C12B -115.4(3) . . . . ? C5B C6B C7B C12B 63.2(3) . . . . ? C1B C6B C7B C8B 75.2(3) . . . . ? C5B C6B C7B C8B -106.2(3) . . . . ? Al1B O2B C8B C9B 126.6(2) . . . . ? Al1B O2B C8B C7B -55.9(3) . . . . ? C12B C7B C8B O2B 169.9(2) . . . . ? C6B C7B C8B O2B -20.8(3) . . . . ? C12B C7B C8B C9B -12.6(3) . . . . ? C6B C7B C8B C9B 156.8(2) . . . . ? O2B C8B C9B C10B -170.5(2) . . . . ? C7B C8B C9B C10B 12.0(3) . . . . ? O2B C8B C9B C19B 15.4(4) . . . . ? C7B C8B C9B C19B -162.0(2) . . . . ? C8B C9B C10B C11B -2.9(4) . . . . ? C19B C9B C10B C11B 171.2(2) . . . . ? C9B C10B C11B C12B -5.8(4) . . . . ? C9B C10B C11B C23B 178.6(2) . . . . ? C10B C11B C12B C7B 5.3(4) . . . . ? C23B C11B C12B C7B -179.1(2) . . . . ? C10B C11B C12B C24B -173.6(2) . . . . ? C23B C11B C12B C24B 2.0(4) . . . . ? C8B C7B C12B C11B 3.6(3) . . . . ? C6B C7B C12B C11B -165.8(2) . . . . ? C8B C7B C12B C24B -177.5(2) . . . . ? C6B C7B C12B C24B 13.0(3) . . . . ? C3B C2B C13B C16B 127.8(3) . . . . ? C1B C2B C13B C16B -56.0(3) . . . . ? C3B C2B C13B C15B -109.3(3) . . . . ? C1B C2B C13B C15B 66.9(3) . . . . ? C3B C2B C13B C14B 8.0(3) . . . . ? C1B C2B C13B C14B -175.8(2) . . . . ? C10B C9B C19B C22B 120.3(3) . . . . ? C8B C9B C19B C22B -65.9(4) . . . . ? C10B C9B C19B C21B -2.8(4) . . . . ? C8B C9B C19B C21B 170.9(3) . . . . ? C10B C9B C19B C20B -119.1(3) . . . . ? C8B C9B C19B C20B 54.6(3) . . . . ? Al1B O3B C25B C26B 132.2(2) . . . . ? Al2B O3B C25B C26B -51.3(3) . . . . ? Al1B O3B C25B C29B -100.6(2) . . . . ? Al2B O3B C25B C29B 75.9(3) . . . . ? O3B C25B C26B C27B -62.2(5) . . . . ? C29B C25B C26B C27B 172.3(4) . . . . ? O3B C25B C26B C28B 75.6(4) . . . . ? C29B C25B C26B C28B -49.8(4) . . . . ? O3B C25B C29B C30B 53.5(3) . . . . ? C26B C25B C29B C30B 179.0(3) . . . . ? O3B C25B C29B C31B 176.8(3) . . . . ? C26B C25B C29B C31B -57.8(4) . . . . ? #END OF CIF data_Chisholm1012 _database_code_CSD 185861 _audit_creation_method SHELXL-93 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H32 Cl6 O2 Ti2' _chemical_formula_weight 661.00 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.0474(1) _cell_length_b 11.9321(1) _cell_length_c 17.6166(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.018(1) _cell_angle_gamma 90.00 _cell_volume 3104.64(5) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'trapezoidal chunk' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method ? _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; There is a crystallographic two-fold axis through the C-C bond of the 'biphenyl' ligand. ; _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31055 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3565 _reflns_number_observed 3004 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;The Cl atoms appear to be disordered and are modeled in terms of two sites each. A second data set was measured at 150 K and no improvement in the behavior of the Cl atoms was observed. So the present data set at 250 K was used for this structure determination. The methyl group hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded C atom). For each methyl group, the torsion angle which defines its orientation about the C-C bond was refined. The hydrogen atom bonded to C3 was included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded C atom). Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+3.2561P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3564 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_obs 0.0390 _refine_ls_wR_factor_all 0.1126 _refine_ls_wR_factor_obs 0.1060 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.053 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.544 _refine_diff_density_min -0.805 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.62033(3) 0.00923(4) 0.40491(2) 0.04933(15) Uani 1 d . . Cl1A Cl 0.7220(8) -0.1234(9) 0.4457(7) 0.0625(12) Uani 0.50 d P . Cl2A Cl 0.66642(10) 0.13396(15) 0.51269(9) 0.0576(4) Uani 0.50 d P . Cl3A Cl 0.49274(10) -0.05609(15) 0.38950(11) 0.0677(4) Uani 0.50 d P . Cl1B Cl 0.7345(8) -0.1052(9) 0.4508(7) 0.074(2) Uani 0.50 d P . Cl2B Cl 0.6155(2) 0.0942(2) 0.50399(12) 0.1198(10) Uani 0.50 d P . Cl3B Cl 0.4980(2) -0.1073(2) 0.3453(2) 0.1181(9) Uani 0.50 d P . O O 0.62694(9) 0.08338(11) 0.32296(7) 0.0376(3) Uani 1 d . . C1 C 0.60898(12) 0.14678(14) 0.25284(10) 0.0308(3) Uani 1 d . . C2 C 0.66958(11) 0.14637(14) 0.21319(10) 0.0312(3) Uani 1 d . . C3 C 0.64031(12) 0.20706(15) 0.13956(10) 0.0337(4) Uani 1 d . . H3 H 0.67661(12) 0.20557(15) 0.10867(10) 0.040 Uiso 1 calc R . C4 C 0.56128(12) 0.26921(15) 0.10921(10) 0.0348(4) Uani 1 d . . C5 C 0.50576(12) 0.27449(14) 0.15373(11) 0.0342(4) Uani 1 d . . C6 C 0.52902(11) 0.20976(14) 0.22552(10) 0.0311(4) Uani 1 d . . C7 C 0.76115(12) 0.0856(2) 0.24699(11) 0.0375(4) Uani 1 d . . C8 C 0.81767(14) 0.1260(2) 0.33514(13) 0.0516(5) Uani 1 d . . H8A H 0.8769(4) 0.0910(12) 0.3547(4) 0.077 Uiso 1 calc R . H8B H 0.7873(6) 0.1056(13) 0.3712(3) 0.077 Uiso 1 calc R . H8C H 0.8244(10) 0.2067(3) 0.3351(2) 0.077 Uiso 1 calc R . C9 C 0.7474(2) -0.0415(2) 0.24504(13) 0.0476(5) Uani 1 d . . H9A H 0.8058(2) -0.0785(2) 0.2674(10) 0.071 Uiso 1 calc R . H9B H 0.7145(10) -0.0657(3) 0.1886(2) 0.071 Uiso 1 calc R . H9C H 0.7131(10) -0.0609(2) 0.2779(9) 0.071 Uiso 1 calc R . C10 C 0.81681(15) 0.1115(2) 0.19492(15) 0.0535(5) Uani 1 d . . H10A H 0.8749(5) 0.0738(12) 0.2186(7) 0.080 Uiso 1 calc R . H10B H 0.8264(10) 0.1918(3) 0.1945(9) 0.080 Uiso 1 calc R . H10C H 0.7842(6) 0.0854(14) 0.1389(3) 0.080 Uiso 1 calc R . C11 C 0.53706(15) 0.3319(2) 0.02871(13) 0.0494(5) Uani 1 d . . H11A H 0.5393(11) 0.4119(2) 0.0391(2) 0.074 Uiso 1 calc R . H11B H 0.4765(5) 0.3111(11) -0.0088(4) 0.074 Uiso 1 calc R . H11C H 0.5799(7) 0.3129(11) 0.0043(5) 0.074 Uiso 1 calc R . C12 C 0.42381(15) 0.3501(2) 0.12681(14) 0.0509(5) Uani 1 d . . H12A H 0.3824(6) 0.3294(10) 0.0717(4) 0.076 Uiso 1 calc R . H12B H 0.4427(2) 0.4273(2) 0.1268(10) 0.076 Uiso 1 calc R . H12C H 0.3936(7) 0.3422(11) 0.1647(6) 0.076 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0493(2) 0.0653(3) 0.0391(2) 0.0248(2) 0.0234(2) 0.0200(2) Cl1A 0.087(3) 0.0542(15) 0.060(2) 0.0248(11) 0.044(2) 0.0357(15) Cl2A 0.0671(8) 0.0706(9) 0.0330(5) -0.0044(5) 0.0171(6) 0.0058(6) Cl3A 0.0544(7) 0.0679(9) 0.0769(10) 0.0272(7) 0.0215(7) -0.0060(7) Cl1B 0.091(3) 0.082(5) 0.055(2) 0.031(3) 0.035(2) 0.051(3) Cl2B 0.194(3) 0.131(2) 0.0607(11) 0.0393(12) 0.079(2) 0.104(2) Cl3B 0.0855(13) 0.107(2) 0.139(2) 0.059(2) 0.0193(14) -0.0240(12) O 0.0434(7) 0.0417(7) 0.0294(6) 0.0087(5) 0.0160(5) 0.0086(6) C1 0.0367(8) 0.0299(8) 0.0245(7) 0.0027(6) 0.0107(6) 0.0006(7) C2 0.0333(8) 0.0305(8) 0.0277(8) -0.0004(6) 0.0095(6) -0.0013(7) C3 0.0359(9) 0.0357(9) 0.0293(8) 0.0027(7) 0.0127(7) -0.0043(7) C4 0.0370(9) 0.0328(9) 0.0307(8) 0.0054(7) 0.0089(7) -0.0045(7) C5 0.0336(8) 0.0319(9) 0.0329(9) 0.0034(7) 0.0085(7) 0.0003(7) C6 0.0337(8) 0.0291(8) 0.0295(8) -0.0011(6) 0.0115(7) -0.0023(7) C7 0.0369(9) 0.0436(10) 0.0310(8) 0.0027(7) 0.0122(7) 0.0068(8) C8 0.0390(10) 0.0648(14) 0.0410(11) -0.0050(10) 0.0049(8) 0.0055(10) C9 0.0573(12) 0.0419(11) 0.0442(11) 0.0040(8) 0.0205(9) 0.0130(9) C10 0.0431(11) 0.0682(15) 0.0547(13) 0.0126(11) 0.0252(10) 0.0140(10) C11 0.0494(11) 0.0549(12) 0.0409(10) 0.0190(9) 0.0145(9) 0.0030(10) C12 0.0488(12) 0.0493(12) 0.0542(12) 0.0161(10) 0.0197(10) 0.0155(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti O 1.7314(12) . ? Ti Cl2B 2.046(2) . ? Ti Cl3A 2.107(2) . ? Ti Cl1B 2.171(11) . ? Ti Cl1A 2.184(10) . ? Ti Cl2A 2.295(2) . ? Ti Cl3B 2.297(2) . ? Cl2A Cl2B 0.905(3) . ? Cl3A Cl3B 1.019(3) . ? O C1 1.379(2) . ? C1 C6 1.400(2) . ? C1 C2 1.402(2) . ? C2 C3 1.397(2) . ? C2 C7 1.535(2) . ? C3 C4 1.383(3) . ? C3 H3 0.94 . ? C4 C5 1.400(3) . ? C4 C11 1.514(2) . ? C5 C6 1.402(2) . ? C5 C12 1.510(3) . ? C6 C6 1.496(3) 2_655 ? C7 C9 1.531(3) . ? C7 C8 1.538(3) . ? C7 C10 1.541(3) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C8 H8C 0.97 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C9 H9C 0.97 . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C10 H10C 0.97 . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C11 H11C 0.97 . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C12 H12C 0.97 . ? 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 O Ti Cl2B 119.56(9) . . ? O Ti Cl3A 117.06(6) . . ? Cl2B Ti Cl3A 86.20(12) . . ? O Ti Cl1B 108.3(3) . . ? Cl2B Ti Cl1B 107.6(3) . . ? Cl3A Ti Cl1B 116.8(3) . . ? O Ti Cl1A 111.3(3) . . ? Cl2B Ti Cl1A 110.5(3) . . ? Cl3A Ti Cl1A 109.7(3) . . ? Cl1B Ti Cl1A 7.5(7) . . ? O Ti Cl2A 104.68(6) . . ? Cl2B Ti Cl2A 23.17(9) . . ? Cl3A Ti Cl2A 109.21(7) . . ? Cl1B Ti Cl2A 98.5(3) . . ? Cl1A Ti Cl2A 103.9(3) . . ? O Ti Cl3B 104.35(8) . . ? Cl2B Ti Cl3B 112.28(14) . . ? Cl3A Ti Cl3B 26.32(8) . . ? Cl1B Ti Cl3B 103.6(3) . . ? Cl1A Ti Cl3B 96.1(3) . . ? Cl2A Ti Cl3B 135.41(10) . . ? Cl2B Cl2A Ti 62.8(2) . . ? Cl3B Cl3A Ti 87.3(2) . . ? Cl2A Cl2B Ti 94.1(2) . . ? Cl3A Cl3B Ti 66.4(2) . . ? C1 O Ti 165.34(12) . . ? O C1 C6 116.40(15) . . ? O C1 C2 120.11(15) . . ? C6 C1 C2 123.49(15) . . ? C3 C2 C1 114.5(2) . . ? C3 C2 C7 121.9(2) . . ? C1 C2 C7 123.63(15) . . ? C4 C3 C2 124.2(2) . . ? C4 C3 H3 117.92(10) . . ? C2 C3 H3 117.92(10) . . ? C3 C4 C5 119.7(2) . . ? C3 C4 C11 119.2(2) . . ? C5 C4 C11 121.1(2) . . ? C4 C5 C6 118.5(2) . . ? C4 C5 C12 121.2(2) . . ? C6 C5 C12 120.3(2) . . ? C1 C6 C5 119.4(2) . . ? C1 C6 C6 119.7(2) . 2_655 ? C5 C6 C6 120.9(2) . 2_655 ? C9 C7 C2 110.6(2) . . ? C9 C7 C8 110.9(2) . . ? C2 C7 C8 109.9(2) . . ? C9 C7 C10 107.3(2) . . ? C2 C7 C10 111.3(2) . . ? C8 C7 C10 106.7(2) . . ? C7 C8 H8A 109.47(11) . . ? C7 C8 H8B 109.47(12) . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.47(12) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.47(11) . . ? C7 C9 H9B 109.47(10) . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.47(11) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.47(11) . . ? C7 C10 H10B 109.47(12) . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.47(12) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 109.47(12) . . ? C4 C11 H11B 109.47(11) . . ? H11A C11 H11B 109.5 . . ? C4 C11 H11C 109.47(11) . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 H12A 109.47(11) . . ? C5 C12 H12B 109.47(11) . . ? H12A C12 H12B 109.5 . . ? C5 C12 H12C 109.47(11) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O Ti Cl2A Cl2B 133.2(2) . . . . ? Cl2B Ti Cl2A Cl2B 0.0 . . . . ? Cl3A Ti Cl2A Cl2B 7.1(2) . . . . ? Cl1B Ti Cl2A Cl2B -115.3(4) . . . . ? Cl1A Ti Cl2A Cl2B -110.0(4) . . . . ? Cl3B Ti Cl2A Cl2B 4.1(3) . . . . ? O Ti Cl3A Cl3B 66.1(2) . . . . ? Cl2B Ti Cl3A Cl3B -172.5(2) . . . . ? Cl1B Ti Cl3A Cl3B -64.7(4) . . . . ? Cl1A Ti Cl3A Cl3B -62.0(4) . . . . ? Cl2A Ti Cl3A Cl3B -175.3(2) . . . . ? Cl3B Ti Cl3A Cl3B 0.0 . . . . ? Ti Cl2A Cl2B Ti 0.0 . . . . ? O Ti Cl2B Cl2A -54.2(2) . . . . ? Cl3A Ti Cl2B Cl2A -173.3(2) . . . . ? Cl1B Ti Cl2B Cl2A 69.7(4) . . . . ? Cl1A Ti Cl2B Cl2A 77.0(4) . . . . ? Cl2A Ti Cl2B Cl2A 0.0 . . . . ? Cl3B Ti Cl2B Cl2A -176.9(2) . . . . ? Ti Cl3A Cl3B Ti 0.0 . . . . ? O Ti Cl3B Cl3A -122.8(2) . . . . ? Cl2B Ti Cl3B Cl3A 8.1(2) . . . . ? Cl3A Ti Cl3B Cl3A 0.0 . . . . ? Cl1B Ti Cl3B Cl3A 123.9(3) . . . . ? Cl1A Ti Cl3B Cl3A 123.3(3) . . . . ? Cl2A Ti Cl3B Cl3A 6.4(2) . . . . ? Cl2B Ti O C1 -77.1(5) . . . . ? Cl3A Ti O C1 24.7(5) . . . . ? Cl1B Ti O C1 159.3(6) . . . . ? Cl1A Ti O C1 152.0(6) . . . . ? Cl2A Ti O C1 -96.3(5) . . . . ? Cl3B Ti O C1 49.4(5) . . . . ? Ti O C1 C6 17.7(6) . . . . ? Ti O C1 C2 -162.6(4) . . . . ? O C1 C2 C3 175.34(15) . . . . ? C6 C1 C2 C3 -5.1(2) . . . . ? O C1 C2 C7 -5.0(3) . . . . ? C6 C1 C2 C7 174.5(2) . . . . ? C1 C2 C3 C4 4.0(3) . . . . ? C7 C2 C3 C4 -175.6(2) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C2 C3 C4 C11 179.7(2) . . . . ? C3 C4 C5 C6 -4.4(3) . . . . ? C11 C4 C5 C6 176.5(2) . . . . ? C3 C4 C5 C12 174.1(2) . . . . ? C11 C4 C5 C12 -5.0(3) . . . . ? O C1 C6 C5 -178.83(15) . . . . ? C2 C1 C6 C5 1.6(3) . . . . ? O C1 C6 C6 2.9(2) . . . 2_655 ? C2 C1 C6 C6 -176.68(15) . . . 2_655 ? C4 C5 C6 C1 3.3(3) . . . . ? C12 C5 C6 C1 -175.2(2) . . . . ? C4 C5 C6 C6 -178.45(15) . . . 2_655 ? C12 C5 C6 C6 3.1(3) . . . 2_655 ? C3 C2 C7 C9 -113.2(2) . . . . ? C1 C2 C7 C9 67.2(2) . . . . ? C3 C2 C7 C8 124.0(2) . . . . ? C1 C2 C7 C8 -55.6(2) . . . . ? C3 C2 C7 C10 6.0(2) . . . . ? C1 C2 C7 C10 -173.6(2) . . . . ? #END OF CIF