Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Kenneth Henderson' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Notre Dame 251 Nieuwland Science Hall Notre Dame Indiana 46556 UNITED STATES OF AMERICA ; _publ_contact_author_email KHENDERS@ND.EDU _publ_section_title ; Use of tetrameric cubane aggregates of lithium aryloxides as secondary building units in controlling network assembly ; loop_ _publ_author_name 'Kenneth Henderson' 'Dugald J. MacDougall' 'J. Jacob Morris' 'Bruce C. Noll' data_bcn16m _database_code_depnum_ccdc_archive 'CCDC 239838' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 Li2 O5' _chemical_formula_sum 'C18 H22 Li2 O5' _chemical_formula_weight 332.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' 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 13.0937(9) _cell_length_b 17.7646(12) _cell_length_c 15.7526(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.853(4) _cell_angle_gamma 90.00 _cell_volume 3651.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7784 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 36.39 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9145 _exptl_absorpt_correction_T_max 0.9857 _exptl_absorpt_process_details 'Blessing, R. H. Acta Cryst. (1995) A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30134 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 33.00 _reflns_number_total 6840 _reflns_number_gt 5889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2/SAINT' _computing_data_reduction 'Bruker SAINT/SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.6141P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6840 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.52118(6) 0.52537(4) 0.08365(4) 0.01982(13) Uani 1 1 d . . . C2 C 0.54229(5) 0.42946(4) -0.01707(4) 0.01784(12) Uani 1 1 d . . . C3 C 0.51221(5) 0.22433(4) 0.09769(4) 0.01635(12) Uani 1 1 d . . . C4 C 0.59102(6) 0.22817(4) 0.04228(5) 0.02177(14) Uani 1 1 d . . . C5 C 0.59552(8) 0.17658(5) -0.02415(5) 0.03075(18) Uani 1 1 d . . . C6 C 0.52240(9) 0.12020(5) -0.03742(6) 0.0350(2) Uani 1 1 d . . . C7 C 0.44598(8) 0.11478(5) 0.01781(6) 0.03056(18) Uani 1 1 d . . . C8 C 0.44054(6) 0.16545(4) 0.08462(5) 0.02206(14) Uani 1 1 d . . . C9 C 0.30955(5) 0.43543(4) 0.23041(4) 0.01518(12) Uani 1 1 d . . . C10 C 0.27606(5) 0.47013(4) 0.15263(5) 0.01858(13) Uani 1 1 d . . . C11 C 0.19009(5) 0.51668(4) 0.14551(6) 0.02452(15) Uani 1 1 d . . . C12 C 0.13417(6) 0.52941(5) 0.21521(7) 0.02958(18) Uani 1 1 d . . . C13 C 0.16465(6) 0.49442(5) 0.29201(6) 0.02904(17) Uani 1 1 d . . . C14 C 0.25076(5) 0.44792(4) 0.30005(5) 0.02109(14) Uani 1 1 d . . . C15 C 0.20042(7) 0.27481(5) 0.14880(6) 0.0331(2) Uani 1 1 d . . . C16 C 0.13759(6) 0.21254(5) 0.10569(5) 0.02436(15) Uani 1 1 d . . . C17 C 0.13639(6) 0.14897(4) 0.23547(5) 0.02221(14) Uani 1 1 d . . . C18 C 0.19831(6) 0.21092(5) 0.27984(5) 0.02362(15) Uani 1 1 d . . . H4 H 0.6417(9) 0.2691(6) 0.0496(8) 0.027(3) Uiso 1 1 d . . . H5 H 0.6526(11) 0.1812(8) -0.0643(10) 0.045(4) Uiso 1 1 d . . . H6 H 0.5240(11) 0.0860(8) -0.0860(10) 0.046(4) Uiso 1 1 d . . . H7 H 0.3946(12) 0.0736(9) 0.0084(11) 0.053(4) Uiso 1 1 d . . . H8 H 0.3846(9) 0.1608(6) 0.1245(8) 0.028(3) Uiso 1 1 d . . . H10 H 0.3147(8) 0.4609(6) 0.1028(8) 0.025(3) Uiso 1 1 d . . . H11 H 0.1660(9) 0.5403(7) 0.0881(8) 0.032(3) Uiso 1 1 d . . . H12 H 0.0753(10) 0.5624(7) 0.2093(9) 0.037(3) Uiso 1 1 d . . . H13 H 0.1239(10) 0.5012(8) 0.3417(9) 0.041(3) Uiso 1 1 d . . . H14 H 0.2722(9) 0.4227(7) 0.3526(8) 0.026(3) Uiso 1 1 d . . . H1A H 0.5938(8) 0.5378(6) 0.0852(7) 0.017(2) Uiso 1 1 d . . . H2A H 0.6141(9) 0.4419(6) -0.0162(8) 0.025(3) Uiso 1 1 d . . . H15A H 0.1542(11) 0.3123(8) 0.1711(9) 0.041(3) Uiso 1 1 d . . . H16A H 0.1840(9) 0.1730(7) 0.0840(8) 0.031(3) Uiso 1 1 d . . . H17A H 0.1823(9) 0.1100(6) 0.2174(7) 0.024(3) Uiso 1 1 d . . . H18A H 0.2445(9) 0.1911(7) 0.3288(8) 0.028(3) Uiso 1 1 d . . . H1B H 0.4999(8) 0.5326(6) 0.1403(8) 0.025(3) Uiso 1 1 d . . . H2B H 0.5294(8) 0.3768(7) -0.0262(7) 0.025(3) Uiso 1 1 d . . . H15B H 0.2499(11) 0.2982(8) 0.1070(9) 0.045(4) Uiso 1 1 d . . . H16B H 0.0906(9) 0.2333(7) 0.0568(8) 0.029(3) Uiso 1 1 d . . . H17B H 0.0903(10) 0.1279(8) 0.2773(9) 0.042(3) Uiso 1 1 d . . . H18B H 0.1532(10) 0.2511(7) 0.3013(9) 0.037(3) Uiso 1 1 d . . . Li1 Li 0.39890(10) 0.28282(7) 0.24028(8) 0.0195(2) Uani 1 1 d . . . Li2 Li 0.50559(9) 0.38260(7) 0.16566(8) 0.0179(2) Uani 1 1 d . . . O1 O 0.51102(4) 0.44607(3) 0.06589(3) 0.01790(11) Uani 1 1 d . . . O2 O 0.50504(4) 0.27426(3) 0.15981(3) 0.01760(10) Uani 1 1 d . . . O3 O 0.39319(4) 0.39260(3) 0.23737(3) 0.01628(10) Uani 1 1 d . . . O4 O 0.26226(4) 0.24548(3) 0.22128(4) 0.02671(13) Uani 1 1 d . . . O5 O 0.07472(4) 0.17753(3) 0.16342(4) 0.02121(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0310(3) 0.0141(3) 0.0136(3) -0.0003(2) -0.0023(2) -0.0005(2) C2 0.0251(3) 0.0144(3) 0.0138(3) 0.0006(2) 0.0007(2) 0.0006(2) C3 0.0213(3) 0.0145(3) 0.0125(3) -0.0003(2) -0.0029(2) 0.0026(2) C4 0.0240(3) 0.0234(3) 0.0178(3) 0.0030(2) 0.0012(2) 0.0057(2) C5 0.0416(4) 0.0335(4) 0.0177(3) 0.0022(3) 0.0056(3) 0.0166(3) C6 0.0581(6) 0.0263(4) 0.0195(4) -0.0078(3) -0.0025(3) 0.0145(4) C7 0.0477(5) 0.0177(3) 0.0246(4) -0.0066(3) -0.0072(3) 0.0000(3) C8 0.0300(3) 0.0164(3) 0.0190(3) -0.0028(2) -0.0020(3) -0.0019(2) C9 0.0143(2) 0.0133(3) 0.0176(3) 0.0007(2) -0.0003(2) -0.00173(19) C10 0.0178(3) 0.0184(3) 0.0189(3) 0.0021(2) -0.0022(2) -0.0003(2) C11 0.0185(3) 0.0221(3) 0.0316(4) 0.0050(3) -0.0062(3) 0.0009(2) C12 0.0155(3) 0.0267(4) 0.0466(5) 0.0035(3) 0.0026(3) 0.0041(3) C13 0.0209(3) 0.0290(4) 0.0388(5) 0.0015(3) 0.0121(3) 0.0023(3) C14 0.0197(3) 0.0220(3) 0.0223(3) 0.0023(2) 0.0056(2) -0.0008(2) C15 0.0343(4) 0.0267(4) 0.0351(5) 0.0120(3) -0.0162(3) -0.0127(3) C16 0.0248(3) 0.0263(4) 0.0208(3) 0.0057(3) -0.0054(3) -0.0074(3) C17 0.0200(3) 0.0249(3) 0.0210(3) 0.0049(3) -0.0026(2) -0.0050(2) C18 0.0221(3) 0.0292(4) 0.0189(3) -0.0040(3) -0.0015(2) -0.0019(3) Li1 0.0215(5) 0.0180(6) 0.0185(6) 0.0004(4) -0.0024(4) -0.0028(4) Li2 0.0217(5) 0.0167(5) 0.0150(5) 0.0017(4) 0.0001(4) 0.0000(4) O1 0.0278(2) 0.0131(2) 0.0127(2) 0.00155(15) 0.00120(17) -0.00069(17) O2 0.0230(2) 0.0151(2) 0.0141(2) -0.00360(16) -0.00179(17) 0.00011(16) O3 0.0162(2) 0.0152(2) 0.0170(2) 0.00091(16) -0.00056(16) 0.00217(15) O4 0.0231(2) 0.0276(3) 0.0276(3) 0.0071(2) -0.0092(2) -0.0102(2) O5 0.0175(2) 0.0228(3) 0.0223(3) 0.00251(19) -0.00430(18) -0.00401(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.4402(8) . ? C1 C2 1.5122(10) 5_665 ? C1 H1A 0.974(10) . ? C1 H1B 0.966(12) . ? C2 O1 1.4330(8) . ? C2 C1 1.5122(9) 5_665 ? C2 H2A 0.964(11) . ? C2 H2B 0.960(12) . ? C3 O2 1.3300(8) . ? C3 C4 1.4085(10) . ? C3 C8 1.4087(10) . ? C4 C5 1.3959(12) . ? C4 H4 0.985(12) . ? C5 C6 1.3892(15) . ? C5 H5 1.022(15) . ? C6 C7 1.3838(15) . ? C6 H6 0.980(15) . ? C7 C8 1.3912(11) . ? C7 H7 0.997(15) . ? C8 H8 1.007(12) . ? C9 O3 1.3305(8) . ? C9 C10 1.4080(9) . ? C9 C14 1.4099(10) . ? C10 C11 1.3935(10) . ? C10 H10 0.983(11) . ? C11 C12 1.3889(13) . ? C11 H11 1.023(13) . ? C12 C13 1.3883(13) . ? C12 H12 0.967(13) . ? C13 C14 1.3947(11) . ? C13 H13 0.991(14) . ? C14 H14 0.962(12) . ? C15 O4 1.4403(10) . ? C15 C16 1.5058(11) . ? C15 H15A 0.984(14) . ? C15 H15B 1.048(14) . ? C16 O5 1.4205(10) . ? C16 H16A 1.006(12) . ? C16 H16B 1.014(12) . ? C17 O5 1.4293(9) . ? C17 C18 1.5036(11) . ? C17 H17A 0.974(11) . ? C17 H17B 1.002(14) . ? C18 O4 1.4350(10) . ? C18 H18A 1.003(12) . ? C18 H18B 1.004(13) . ? Li1 O4 1.9079(13) . ? Li1 O2 1.9359(13) 2_655 ? Li1 O3 1.9522(14) . ? Li1 O2 1.9645(14) . ? Li1 Li2 2.5668(17) 2_655 ? Li1 Li2 2.5987(18) . ? Li1 Li1 2.639(3) 2_655 ? Li2 O2 1.9269(13) . ? Li2 O3 1.9377(14) . ? Li2 O1 1.9403(13) . ? Li2 O3 1.9440(13) 2_655 ? Li2 Li1 2.5669(17) 2_655 ? Li2 Li2 2.673(2) 2_655 ? O2 Li1 1.9358(13) 2_655 ? O3 Li2 1.9440(13) 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 O1 C1 C2 110.37(5) . 5_665 ? O1 C1 H1A 107.5(6) . . ? C2 C1 H1A 112.0(6) 5_665 . ? O1 C1 H1B 106.3(7) . . ? C2 C1 H1B 112.7(7) 5_665 . ? H1A C1 H1B 107.7(9) . . ? O1 C2 C1 109.91(6) . 5_665 ? O1 C2 H2A 107.1(7) . . ? C1 C2 H2A 111.5(7) 5_665 . ? O1 C2 H2B 106.1(7) . . ? C1 C2 H2B 109.5(7) 5_665 . ? H2A C2 H2B 112.6(10) . . ? O2 C3 C4 121.65(6) . . ? O2 C3 C8 121.01(6) . . ? C4 C3 C8 117.34(6) . . ? C5 C4 C3 120.82(8) . . ? C5 C4 H4 120.1(7) . . ? C3 C4 H4 119.0(7) . . ? C6 C5 C4 120.92(8) . . ? C6 C5 H5 119.7(8) . . ? C4 C5 H5 119.3(8) . . ? C7 C6 C5 118.77(8) . . ? C7 C6 H6 120.8(8) . . ? C5 C6 H6 120.4(8) . . ? C6 C7 C8 121.11(8) . . ? C6 C7 H7 118.2(9) . . ? C8 C7 H7 120.7(9) . . ? C7 C8 C3 120.99(8) . . ? C7 C8 H8 120.3(7) . . ? C3 C8 H8 118.7(7) . . ? O3 C9 C10 121.03(6) . . ? O3 C9 C14 121.72(6) . . ? C10 C9 C14 117.25(6) . . ? C11 C10 C9 121.32(7) . . ? C11 C10 H10 120.1(7) . . ? C9 C10 H10 118.6(7) . . ? C12 C11 C10 120.61(7) . . ? C12 C11 H11 119.3(7) . . ? C10 C11 H11 120.1(7) . . ? C13 C12 C11 118.95(7) . . ? C13 C12 H12 121.6(8) . . ? C11 C12 H12 119.4(8) . . ? C12 C13 C14 120.99(8) . . ? C12 C13 H13 119.9(8) . . ? C14 C13 H13 119.0(8) . . ? C13 C14 C9 120.86(7) . . ? C13 C14 H14 121.9(7) . . ? C9 C14 H14 117.2(7) . . ? O4 C15 C16 109.92(7) . . ? O4 C15 H15A 106.5(9) . . ? C16 C15 H15A 109.2(8) . . ? O4 C15 H15B 107.8(8) . . ? C16 C15 H15B 110.6(8) . . ? H15A C15 H15B 112.8(12) . . ? O5 C16 C15 110.92(7) . . ? O5 C16 H16A 108.1(7) . . ? C15 C16 H16A 110.1(7) . . ? O5 C16 H16B 107.4(7) . . ? C15 C16 H16B 110.4(7) . . ? H16A C16 H16B 109.9(10) . . ? O5 C17 C18 110.83(6) . . ? O5 C17 H17A 110.0(7) . . ? C18 C17 H17A 109.5(7) . . ? O5 C17 H17B 108.8(8) . . ? C18 C17 H17B 107.4(8) . . ? H17A C17 H17B 110.3(10) . . ? O4 C18 C17 109.60(6) . . ? O4 C18 H18A 107.4(7) . . ? C17 C18 H18A 111.5(7) . . ? O4 C18 H18B 107.7(7) . . ? C17 C18 H18B 111.6(7) . . ? H18A C18 H18B 108.9(10) . . ? O4 Li1 O2 129.52(7) . 2_655 ? O4 Li1 O3 108.07(7) . . ? O2 Li1 O3 96.81(6) 2_655 . ? O4 Li1 O2 125.25(7) . . ? O2 Li1 O2 94.13(6) 2_655 . ? O3 Li1 O2 95.16(6) . . ? O4 Li1 Li2 137.33(7) . 2_655 ? O2 Li1 Li2 48.21(4) 2_655 2_655 ? O3 Li1 Li2 48.65(4) . 2_655 ? O2 Li1 Li2 95.11(6) . 2_655 ? O4 Li1 Li2 134.35(7) . . ? O2 Li1 Li2 94.83(6) 2_655 . ? O3 Li1 Li2 47.84(4) . . ? O2 Li1 Li2 47.49(4) . . ? Li2 Li1 Li2 62.33(6) 2_655 . ? O4 Li1 Li1 159.45(5) . 2_655 ? O2 Li1 Li1 47.87(4) 2_655 2_655 ? O3 Li1 Li1 92.22(4) . 2_655 ? O2 Li1 Li1 46.96(4) . 2_655 ? Li2 Li1 Li1 59.87(5) 2_655 2_655 ? Li2 Li1 Li1 58.68(5) . 2_655 ? O2 Li2 O3 96.86(6) . . ? O2 Li2 O1 122.81(7) . . ? O3 Li2 O1 120.04(7) . . ? O2 Li2 O3 97.37(6) . 2_655 ? O3 Li2 O3 91.98(6) . 2_655 ? O1 Li2 O3 120.94(7) . 2_655 ? O2 Li2 Li1 48.50(4) . 2_655 ? O3 Li2 Li1 94.81(6) . 2_655 ? O1 Li2 Li1 145.02(7) . 2_655 ? O3 Li2 Li1 48.93(4) 2_655 2_655 ? O2 Li2 Li1 48.72(4) . . ? O3 Li2 Li1 48.32(4) . . ? O1 Li2 Li1 145.15(7) . . ? O3 Li2 Li1 93.66(6) 2_655 . ? Li1 Li2 Li1 61.45(6) 2_655 . ? O2 Li2 Li2 92.71(4) . 2_655 ? O3 Li2 Li2 46.57(4) . 2_655 ? O1 Li2 Li2 144.47(4) . 2_655 ? O3 Li2 Li2 46.37(4) 2_655 2_655 ? Li1 Li2 Li2 59.42(5) 2_655 2_655 ? Li1 Li2 Li2 58.25(5) . 2_655 ? C2 O1 C1 110.46(5) . . ? C2 O1 Li2 130.69(6) . . ? C1 O1 Li2 114.85(6) . . ? C3 O2 Li2 134.52(6) . . ? C3 O2 Li1 124.69(6) . 2_655 ? Li2 O2 Li1 83.29(6) . 2_655 ? C3 O2 Li1 128.62(6) . . ? Li2 O2 Li1 83.79(6) . . ? Li1 O2 Li1 85.17(6) 2_655 . ? C9 O3 Li2 131.68(6) . . ? C9 O3 Li2 128.22(6) . 2_655 ? Li2 O3 Li2 87.06(6) . 2_655 ? C9 O3 Li1 127.08(6) . . ? Li2 O3 Li1 83.84(6) . . ? Li2 O3 Li1 82.42(5) 2_655 . ? C18 O4 C15 110.18(6) . . ? C18 O4 Li1 129.67(6) . . ? C15 O4 Li1 117.09(6) . . ? C16 O5 C17 110.17(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 33.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.498 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.059 _ccdc_chemical_compound_source_recrystallisation 'dioxane, C4H8O2' data_lw1 _database_code_depnum_ccdc_archive 'CCDC 239840' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H112 Li8 O18, 2(C4 H8 O2)' _chemical_formula_sum 'C92 H128 Li8 O22' _chemical_formula_weight 1641.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3172(3) _cell_length_b 15.2696(3) _cell_length_c 24.5935(6) _cell_angle_alpha 74.1940(10) _cell_angle_beta 84.9940(10) _cell_angle_gamma 62.5070(10) _cell_volume 4584.39(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9130 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.75 _exptl_crystal_description cube _exptl_crystal_colour clear _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9726 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details 'Blessing R.H. Acta Cryst. (1995) A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91923 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.86 _diffrn_reflns_theta_max 28.28 _reflns_number_total 22586 _reflns_number_gt 16431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2/SAINT' _computing_data_reduction 'Bruker SAINT/SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Hydrogens were placed at calculated geometries and allowed to ride on the position of the parent atom. Thermal parameters for hydrogen were set to 1.2 \\times the equivalent isotropic U of the parent atom, 1.5 \\times for methyl hydrogens. The largest peak in the final difference map, 0.98 e^-^/A\%^3^, represents a small degree of unmodeled disorder in ethyl group C75-C76. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+1.2125P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22586 _refine_ls_number_parameters 1107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1782 _refine_ls_wR_factor_gt 0.1584 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.6565(2) 0.6093(2) 0.90323(11) 0.0222(5) Uani 1 1 d . . . Li2 Li 0.6105(2) 0.7707(2) 0.81816(11) 0.0220(5) Uani 1 1 d . . . Li3 Li 0.5749(2) 0.6281(2) 0.80548(11) 0.0213(5) Uani 1 1 d . . . Li4 Li 0.7728(2) 0.5924(2) 0.81320(11) 0.0217(5) Uani 1 1 d . . . Li5 Li 0.2209(2) 0.4204(2) 0.67301(12) 0.0221(5) Uani 1 1 d . . . Li6 Li 0.4125(2) 0.3973(2) 0.68752(11) 0.0206(5) Uani 1 1 d . . . Li7 Li 0.3495(2) 0.4030(2) 0.58843(11) 0.0216(5) Uani 1 1 d . . . Li8 Li 0.3929(2) 1.2450(2) 0.67578(11) 0.0215(5) Uani 1 1 d . . . O1 O 0.52434(8) 0.70794(8) 0.85999(5) 0.0214(2) Uani 1 1 d . . . O2 O 0.73808(8) 0.67995(8) 0.86370(5) 0.0204(2) Uani 1 1 d . . . O3 O 0.69793(8) 0.51827(8) 0.85401(5) 0.0206(2) Uani 1 1 d . . . O4 O 0.65413(8) 0.69096(8) 0.76060(4) 0.0190(2) Uani 1 1 d . . . O5 O 0.67742(9) 0.56543(9) 0.98664(5) 0.0254(2) Uani 1 1 d . . . O6 O 0.71652(11) 0.48967(10) 1.10557(5) 0.0339(3) Uani 1 1 d . . . O7 O 0.55401(9) 0.91868(8) 0.79193(5) 0.0234(2) Uani 1 1 d . . . O8 O 0.45163(9) 1.09699(8) 0.70266(5) 0.0223(2) Uani 1 1 d . . . O9 O 0.50080(9) 0.59532(9) 0.75951(5) 0.0229(2) Uani 1 1 d . . . O10 O 0.47702(9) 0.43785(9) 0.73388(5) 0.0226(2) Uani 1 1 d . . . O11 O 0.90310(9) 0.53215(9) 0.77392(5) 0.0260(3) Uani 1 1 d . . . O12 O 1.08146(9) 0.47927(9) 0.70606(5) 0.0256(3) Uani 1 1 d . . . O13 O 0.33346(8) 0.33094(8) 0.73018(4) 0.0192(2) Uani 1 1 d . . . O14 O 0.29242(8) 0.49998(8) 0.63403(5) 0.0201(2) Uani 1 1 d . . . O15 O 0.27176(8) 0.32743(8) 0.62490(5) 0.0210(2) Uani 1 1 d . . . O16 O 0.47830(8) 0.31238(8) 0.63675(4) 0.0205(2) Uani 1 1 d . . . O17 O 0.33478(9) 0.43474(8) 0.50534(5) 0.0249(2) Uani 1 1 d . . . O18 O 0.28709(11) 0.49604(10) 0.38739(5) 0.0353(3) Uani 1 1 d . . . C1 C 0.42475(12) 0.75291(11) 0.87454(6) 0.0186(3) Uani 1 1 d . . . C2 C 0.39822(13) 0.74449(12) 0.93167(7) 0.0230(3) Uani 1 1 d . . . H2 H 0.4520 0.7029 0.9606 0.028 Uiso 1 1 calc R . . C3 C 0.29479(13) 0.79596(13) 0.94626(7) 0.0251(3) Uani 1 1 d . . . H3 H 0.2795 0.7889 0.9851 0.030 Uiso 1 1 calc R . . C4 C 0.21261(12) 0.85776(12) 0.90554(7) 0.0228(3) Uani 1 1 d . . . C5 C 0.23785(12) 0.86315(12) 0.84906(7) 0.0230(3) Uani 1 1 d . . . H5 H 0.1833 0.9031 0.8204 0.028 Uiso 1 1 calc R . . C6 C 0.34105(12) 0.81150(12) 0.83371(6) 0.0211(3) Uani 1 1 d . . . H6 H 0.3552 0.8159 0.7949 0.025 Uiso 1 1 calc R . . C7 C 0.10179(13) 0.91953(14) 0.92237(8) 0.0291(4) Uani 1 1 d . . . H7A H 0.0833 0.8752 0.9542 0.035 Uiso 1 1 calc R . . H7B H 0.0517 0.9429 0.8901 0.035 Uiso 1 1 calc R . . C8 C 0.09008(14) 1.01199(14) 0.93998(8) 0.0312(4) Uani 1 1 d . . . H8A H 0.1361 0.9890 0.9735 0.047 Uiso 1 1 calc R . . H8B H 0.0167 1.0512 0.9488 0.047 Uiso 1 1 calc R . . H8C H 0.1099 1.0553 0.9090 0.047 Uiso 1 1 calc R . . C9 C 0.79403(12) 0.69748(11) 0.89595(6) 0.0186(3) Uani 1 1 d . . . C10 C 0.88738(12) 0.61845(12) 0.92524(7) 0.0210(3) Uani 1 1 d . . . H10 H 0.9124 0.5512 0.9211 0.025 Uiso 1 1 calc R . . C11 C 0.94396(13) 0.63672(13) 0.96015(7) 0.0245(3) Uani 1 1 d . . . H11 H 1.0067 0.5815 0.9796 0.029 Uiso 1 1 calc R . . C12 C 0.91080(14) 0.73417(13) 0.96721(7) 0.0265(3) Uani 1 1 d . . . C13 C 0.81864(14) 0.81254(13) 0.93805(7) 0.0263(3) Uani 1 1 d . . . H13 H 0.7942 0.8797 0.9421 0.032 Uiso 1 1 calc R . . C14 C 0.76133(13) 0.79534(12) 0.90309(7) 0.0227(3) Uani 1 1 d . . . H14 H 0.6988 0.8509 0.8836 0.027 Uiso 1 1 calc R . . C15 C 0.97135(16) 0.75339(16) 1.00628(9) 0.0380(4) Uani 1 1 d . . . H15A H 1.0453 0.7294 0.9949 0.046 Uiso 1 1 calc R . . H15B H 0.9405 0.8279 1.0019 0.046 Uiso 1 1 calc R . . C16 C 0.9701(2) 0.70108(18) 1.06685(9) 0.0529(6) Uani 1 1 d . . . H16A H 0.8976 0.7153 1.0767 0.079 Uiso 1 1 calc R . . H16B H 0.9981 0.7264 1.0907 0.079 Uiso 1 1 calc R . . H16C H 1.0138 0.6271 1.0731 0.079 Uiso 1 1 calc R . . C17 C 0.70511(12) 0.42488(11) 0.86594(6) 0.0182(3) Uani 1 1 d . . . C18 C 0.62228(13) 0.40478(13) 0.89024(7) 0.0238(3) Uani 1 1 d . . . H18 H 0.5600 0.4589 0.8987 0.029 Uiso 1 1 calc R . . C19 C 0.62947(14) 0.30739(14) 0.90216(7) 0.0274(4) Uani 1 1 d . . . H19 H 0.5715 0.2967 0.9180 0.033 Uiso 1 1 calc R . . C20 C 0.71900(15) 0.22588(13) 0.89142(7) 0.0272(4) Uani 1 1 d . . . C21 C 0.80086(14) 0.24565(13) 0.86717(8) 0.0311(4) Uani 1 1 d . . . H21 H 0.8633 0.1909 0.8593 0.037 Uiso 1 1 calc R . . C22 C 0.79482(13) 0.34247(12) 0.85399(7) 0.0256(3) Uani 1 1 d . . . H22 H 0.8521 0.3530 0.8367 0.031 Uiso 1 1 calc R . . C23 C 0.72756(19) 0.11951(14) 0.90325(8) 0.0394(5) Uani 1 1 d . . . H23A H 0.6716 0.1152 0.9288 0.047 Uiso 1 1 calc R . . H23B H 0.7965 0.0688 0.9228 0.047 Uiso 1 1 calc R . . C24 C 0.71733(16) 0.09285(14) 0.84968(8) 0.0359(4) Uani 1 1 d . . . H24A H 0.6489 0.1425 0.8303 0.054 Uiso 1 1 calc R . . H24B H 0.7226 0.0240 0.8594 0.054 Uiso 1 1 calc R . . H24C H 0.7739 0.0948 0.8247 0.054 Uiso 1 1 calc R . . C25 C 0.65175(12) 0.74689(11) 0.70828(6) 0.0179(3) Uani 1 1 d . . . C26 C 0.73541(12) 0.76963(12) 0.68886(7) 0.0226(3) Uani 1 1 d . . . H26 H 0.7961 0.7421 0.7131 0.027 Uiso 1 1 calc R . . C27 C 0.73124(13) 0.83151(13) 0.63504(7) 0.0251(3) Uani 1 1 d . . . H27 H 0.7892 0.8453 0.6233 0.030 Uiso 1 1 calc R . . C28 C 0.64401(14) 0.87391(12) 0.59787(7) 0.0251(3) Uani 1 1 d . . . C29 C 0.56185(13) 0.84940(13) 0.61622(7) 0.0251(3) Uani 1 1 d . . . H29 H 0.5023 0.8758 0.5914 0.030 Uiso 1 1 calc R . . C30 C 0.56494(12) 0.78726(12) 0.67005(6) 0.0213(3) Uani 1 1 d . . . H30 H 0.5078 0.7719 0.6811 0.026 Uiso 1 1 calc R . . C31 C 0.63643(16) 0.94869(14) 0.54139(7) 0.0329(4) Uani 1 1 d . . . H31A H 0.6000 0.9386 0.5130 0.039 Uiso 1 1 calc R . . H31B H 0.7083 0.9346 0.5286 0.039 Uiso 1 1 calc R . . C32 C 0.57689(19) 1.05941(15) 0.54479(8) 0.0410(5) Uani 1 1 d . . . H32A H 0.5063 1.0731 0.5583 0.061 Uiso 1 1 calc R . . H32B H 0.5709 1.1054 0.5072 0.061 Uiso 1 1 calc R . . H32C H 0.6152 1.0708 0.5711 0.061 Uiso 1 1 calc R . . C33 C 0.65399(14) 0.48441(13) 1.01909(7) 0.0281(4) Uani 1 1 d . . . H33A H 0.6625 0.4382 0.9955 0.034 Uiso 1 1 calc R . . H33B H 0.5799 0.5140 1.0303 0.034 Uiso 1 1 calc R . . C34 C 0.72632(16) 0.42438(14) 1.07115(7) 0.0323(4) Uani 1 1 d . . . H34A H 0.7086 0.3697 1.0932 0.039 Uiso 1 1 calc R . . H34B H 0.8001 0.3917 1.0598 0.039 Uiso 1 1 calc R . . C35 C 0.74209(15) 0.56878(14) 1.07349(7) 0.0302(4) Uani 1 1 d . . . H35A H 0.8163 0.5377 1.0627 0.036 Uiso 1 1 calc R . . H35B H 0.7346 0.6145 1.0972 0.036 Uiso 1 1 calc R . . C36 C 0.67129(14) 0.63032(13) 1.02108(7) 0.0276(4) Uani 1 1 d . . . H36A H 0.5977 0.6662 1.0319 0.033 Uiso 1 1 calc R . . H36B H 0.6923 0.6826 0.9990 0.033 Uiso 1 1 calc R . . C37 C 0.61013(12) 0.96996(12) 0.75841(7) 0.0240(3) Uani 1 1 d . . . H37A H 0.6841 0.9195 0.7560 0.029 Uiso 1 1 calc R . . H37B H 0.6104 1.0201 0.7767 0.029 Uiso 1 1 calc R . . C38 C 0.55970(12) 1.02430(12) 0.69981(7) 0.0225(3) Uani 1 1 d . . . H38A H 0.5987 1.0602 0.6774 0.027 Uiso 1 1 calc R . . H38B H 0.5629 0.9738 0.6807 0.027 Uiso 1 1 calc R . . C39 C 0.39562(12) 1.04466(12) 0.73587(7) 0.0245(3) Uani 1 1 d . . . H39A H 0.3969 0.9937 0.7177 0.029 Uiso 1 1 calc R . . H39B H 0.3212 1.0944 0.7380 0.029 Uiso 1 1 calc R . . C40 C 0.44598(13) 0.99170(12) 0.79452(7) 0.0250(3) Uani 1 1 d . . . H40A H 0.4429 1.0429 0.8131 0.030 Uiso 1 1 calc R . . H40B H 0.4069 0.9563 0.8173 0.030 Uiso 1 1 calc R . . C41 C 0.56314(13) 0.54538(13) 0.71760(7) 0.0256(3) Uani 1 1 d . . . H41A H 0.6328 0.5446 0.7168 0.031 Uiso 1 1 calc R . . H41B H 0.5275 0.5838 0.6798 0.031 Uiso 1 1 calc R . . C42 C 0.57778(13) 0.43759(13) 0.73122(7) 0.0248(3) Uani 1 1 d . . . H42A H 0.6191 0.4044 0.7018 0.030 Uiso 1 1 calc R . . H42B H 0.6174 0.3980 0.7680 0.030 Uiso 1 1 calc R . . C43 C 0.41428(13) 0.48806(13) 0.77550(7) 0.0248(3) Uani 1 1 d . . . H43A H 0.4494 0.4496 0.8135 0.030 Uiso 1 1 calc R . . H43B H 0.3445 0.4891 0.7760 0.030 Uiso 1 1 calc R . . C44 C 0.39999(12) 0.59567(13) 0.76209(7) 0.0252(3) Uani 1 1 d . . . H44A H 0.3604 0.6355 0.7253 0.030 Uiso 1 1 calc R . . H44B H 0.3588 0.6288 0.7916 0.030 Uiso 1 1 calc R . . C45 C 1.00883(13) 0.47932(15) 0.79806(8) 0.0331(4) Uani 1 1 d . . . H45A H 1.0334 0.4046 0.8074 0.040 Uiso 1 1 calc R . . H45B H 1.0099 0.4977 0.8335 0.040 Uiso 1 1 calc R . . C46 C 1.08143(13) 0.50665(13) 0.75775(7) 0.0280(4) Uani 1 1 d . . . H46A H 1.0584 0.5811 0.7493 0.034 Uiso 1 1 calc R . . H46B H 1.1537 0.4700 0.7752 0.034 Uiso 1 1 calc R . . C47 C 0.97573(13) 0.53129(15) 0.68100(8) 0.0326(4) Uani 1 1 d . . . H47A H 0.9756 0.5106 0.6462 0.039 Uiso 1 1 calc R . . H47B H 0.9510 0.6062 0.6704 0.039 Uiso 1 1 calc R . . C48 C 0.90227(13) 0.50513(14) 0.72229(8) 0.0297(4) Uani 1 1 d . . . H48A H 0.8298 0.5424 0.7051 0.036 Uiso 1 1 calc R . . H48B H 0.9243 0.4309 0.7308 0.036 Uiso 1 1 calc R . . C49 C 0.35596(15) 0.36149(13) 0.47381(7) 0.0301(4) Uani 1 1 d . . . H49A H 0.3495 0.3016 0.4985 0.036 Uiso 1 1 calc R . . H49B H 0.4290 0.3375 0.4609 0.036 Uiso 1 1 calc R . . C50 C 0.27992(16) 0.40849(14) 0.42333(7) 0.0330(4) Uani 1 1 d . . . H50A H 0.2961 0.3573 0.4018 0.040 Uiso 1 1 calc R . . H50B H 0.2072 0.4290 0.4363 0.040 Uiso 1 1 calc R . . C51 C 0.26269(15) 0.56942(14) 0.41876(7) 0.0324(4) Uani 1 1 d . . . H51A H 0.1895 0.5915 0.4313 0.039 Uiso 1 1 calc R . . H51B H 0.2674 0.6303 0.3941 0.039 Uiso 1 1 calc R . . C52 C 0.33712(14) 0.52547(13) 0.46955(7) 0.0268(3) Uani 1 1 d . . . H52A H 0.4096 0.5086 0.4569 0.032 Uiso 1 1 calc R . . H52B H 0.3170 0.5770 0.4913 0.032 Uiso 1 1 calc R . . C53 C 0.33480(12) 0.27582(11) 0.78278(6) 0.0183(3) Uani 1 1 d . . . C54 C 0.41500(13) 0.24588(12) 0.82308(7) 0.0223(3) Uani 1 1 d . . . H54 H 0.4681 0.2675 0.8133 0.027 Uiso 1 1 calc R . . C55 C 0.41743(14) 0.18490(13) 0.87707(7) 0.0272(4) Uani 1 1 d . . . H55 H 0.4724 0.1659 0.9035 0.033 Uiso 1 1 calc R . . C56 C 0.34204(14) 0.15094(13) 0.89349(7) 0.0277(4) Uani 1 1 d . . . C57 C 0.26139(14) 0.18233(13) 0.85390(7) 0.0272(4) Uani 1 1 d . . . H57 H 0.2080 0.1612 0.8642 0.033 Uiso 1 1 calc R . . C58 C 0.25695(12) 0.24364(12) 0.79985(7) 0.0223(3) Uani 1 1 d . . . H58 H 0.2004 0.2641 0.7741 0.027 Uiso 1 1 calc R . . C59 C 0.35057(18) 0.07739(16) 0.95066(8) 0.0396(5) Uani 1 1 d . . . H59A H 0.2794 0.0857 0.9616 0.048 Uiso 1 1 calc R . . H59B H 0.3791 0.0945 0.9793 0.048 Uiso 1 1 calc R . . C60 C 0.4212(2) -0.03304(17) 0.95024(9) 0.0550(6) Uani 1 1 d . . . H60A H 0.3877 -0.0535 0.9263 0.082 Uiso 1 1 calc R . . H60B H 0.4321 -0.0770 0.9889 0.082 Uiso 1 1 calc R . . H60C H 0.4892 -0.0400 0.9353 0.082 Uiso 1 1 calc R . . C61 C 0.27967(12) 0.59441(11) 0.62713(6) 0.0178(3) Uani 1 1 d . . . C62 C 0.35378(12) 0.62575(12) 0.60006(7) 0.0218(3) Uani 1 1 d . . . H62 H 0.4146 0.5786 0.5859 0.026 Uiso 1 1 calc R . . C63 C 0.34011(13) 0.72434(12) 0.59349(7) 0.0233(3) Uani 1 1 d . . . H63 H 0.3920 0.7429 0.5751 0.028 Uiso 1 1 calc R . . C64 C 0.25230(13) 0.79656(12) 0.61313(7) 0.0222(3) Uani 1 1 d . . . C65 C 0.17896(12) 0.76568(12) 0.64046(7) 0.0230(3) Uani 1 1 d . . . H65 H 0.1185 0.8132 0.6546 0.028 Uiso 1 1 calc R . . C66 C 0.19179(12) 0.66742(12) 0.64761(7) 0.0213(3) Uani 1 1 d . . . H66 H 0.1403 0.6491 0.6667 0.026 Uiso 1 1 calc R . . C67 C 0.23749(15) 0.90401(12) 0.60665(7) 0.0283(4) Uani 1 1 d . . . H67A H 0.1668 0.9539 0.5889 0.034 Uiso 1 1 calc R . . H67B H 0.2905 0.9151 0.5810 0.034 Uiso 1 1 calc R . . C68 C 0.24809(16) 0.92404(14) 0.66258(8) 0.0352(4) Uani 1 1 d . . . H68A H 0.1932 0.9172 0.6875 0.053 Uiso 1 1 calc R . . H68B H 0.2403 0.9935 0.6556 0.053 Uiso 1 1 calc R . . H68C H 0.3176 0.8744 0.6807 0.053 Uiso 1 1 calc R . . C69 C 0.21863(12) 0.30557(12) 0.59342(6) 0.0197(3) Uani 1 1 d . . . C70 C 0.12574(13) 0.38189(12) 0.56268(7) 0.0248(3) Uani 1 1 d . . . H70 H 0.0999 0.4504 0.5647 0.030 Uiso 1 1 calc R . . C71 C 0.07052(14) 0.35941(13) 0.52929(8) 0.0293(4) Uani 1 1 d . . . H71 H 0.0078 0.4130 0.5090 0.035 Uiso 1 1 calc R . . C72 C 0.10503(14) 0.26017(13) 0.52498(7) 0.0275(4) Uani 1 1 d . . . C73 C 0.19598(14) 0.18428(13) 0.55632(7) 0.0259(3) Uani 1 1 d . . . H73 H 0.2205 0.1156 0.5549 0.031 Uiso 1 1 calc R . . C74 C 0.25226(13) 0.20536(12) 0.58963(7) 0.0237(3) Uani 1 1 d . . . H74 H 0.3144 0.1512 0.6102 0.028 Uiso 1 1 calc R . . C75 C 0.04881(16) 0.23493(17) 0.48638(9) 0.0384(4) Uani 1 1 d . . . H75A H 0.0748 0.2476 0.4478 0.046 Uiso 1 1 calc R . . H75B H 0.0689 0.1610 0.4996 0.046 Uiso 1 1 calc R . . C76 C -0.06826(18) 0.29284(17) 0.48274(10) 0.0503(6) Uani 1 1 d . . . H76A H -0.0951 0.2860 0.5209 0.076 Uiso 1 1 calc R . . H76B H -0.0970 0.2654 0.4607 0.076 Uiso 1 1 calc R . . H76C H -0.0898 0.3653 0.4642 0.076 Uiso 1 1 calc R . . C77 C 0.57948(11) 0.26312(11) 0.62541(6) 0.0178(3) Uani 1 1 d . . . C78 C 0.61156(12) 0.26452(12) 0.56966(6) 0.0199(3) Uani 1 1 d . . . H78 H 0.5608 0.3053 0.5391 0.024 Uiso 1 1 calc R . . C79 C 0.71580(12) 0.20753(12) 0.55832(7) 0.0225(3) Uani 1 1 d . . . H79 H 0.7346 0.2099 0.5201 0.027 Uiso 1 1 calc R . . C80 C 0.79389(12) 0.14682(12) 0.60138(7) 0.0216(3) Uani 1 1 d . . . C81 C 0.76367(12) 0.14922(12) 0.65648(7) 0.0220(3) Uani 1 1 d . . . H81 H 0.8155 0.1109 0.6867 0.026 Uiso 1 1 calc R . . C82 C 0.65930(12) 0.20633(12) 0.66858(6) 0.0207(3) Uani 1 1 d . . . H82 H 0.6417 0.2069 0.7067 0.025 Uiso 1 1 calc R . . C83 C 0.90536(13) 0.07789(13) 0.58848(8) 0.0287(4) Uani 1 1 d . . . H83A H 0.9509 0.0482 0.6234 0.034 Uiso 1 1 calc R . . H83B H 0.9325 0.1195 0.5601 0.034 Uiso 1 1 calc R . . C84 C 0.91249(15) -0.00830(15) 0.56609(9) 0.0362(4) Uani 1 1 d . . . H84A H 0.8868 -0.0505 0.5942 0.054 Uiso 1 1 calc R . . H84B H 0.9860 -0.0506 0.5587 0.054 Uiso 1 1 calc R . . H84C H 0.8693 0.0206 0.5309 0.054 Uiso 1 1 calc R . . O19 O 0.03067(11) 0.11692(10) 0.17895(5) 0.0343(3) Uani 1 1 d . . . O20 O -0.01657(11) 0.24533(10) 0.25151(6) 0.0353(3) Uani 1 1 d . . . C85 C 0.06344(18) 0.2305(2) 0.69147(9) 0.0527(6) Uani 1 1 d . . . H85A H 0.1388 0.1801 0.6939 0.063 Uiso 1 1 calc R . . H85B H 0.0550 0.2954 0.6646 0.063 Uiso 1 1 calc R . . C86 C -0.0018(2) 0.1915(2) 0.66991(9) 0.0586(7) Uani 1 1 d . . . H86A H -0.0769 0.2432 0.6657 0.070 Uiso 1 1 calc R . . H86B H 0.0217 0.1796 0.6324 0.070 Uiso 1 1 calc R . . C87 C -0.02317(16) 0.11626(15) 0.76257(8) 0.0365(4) Uani 1 1 d . . . H87A H -0.0157 0.0520 0.7898 0.044 Uiso 1 1 calc R . . H87B H -0.0982 0.1676 0.7598 0.044 Uiso 1 1 calc R . . C88 C 0.04321(15) 0.15402(15) 0.78294(8) 0.0356(4) Uani 1 1 d . . . H88A H 0.0222 0.1640 0.8211 0.043 Uiso 1 1 calc R . . H88B H 0.1181 0.1022 0.7859 0.043 Uiso 1 1 calc R . . O21 O 0.03188(12) 0.24709(11) 0.74584(7) 0.0454(4) Uani 1 1 d . . . O22 O 0.00928(12) 0.09857(12) 0.70853(7) 0.0475(4) Uani 1 1 d . . . C89 C -0.04267(15) 0.22268(14) 0.16169(8) 0.0317(4) Uani 1 1 d . . . H89A H -0.0970 0.2328 0.1351 0.038 Uiso 1 1 calc R . . H89B H -0.0056 0.2625 0.1418 0.038 Uiso 1 1 calc R . . C90 C -0.09421(15) 0.26027(15) 0.21193(8) 0.0372(4) Uani 1 1 d . . . H90A H -0.1444 0.3339 0.1994 0.045 Uiso 1 1 calc R . . H90B H -0.1343 0.2229 0.2306 0.045 Uiso 1 1 calc R . . C91 C 0.05725(14) 0.14003(14) 0.26800(8) 0.0312(4) Uani 1 1 d . . . H91A H 0.0209 0.0995 0.2879 0.037 Uiso 1 1 calc R . . H91B H 0.1119 0.1297 0.2945 0.037 Uiso 1 1 calc R . . C92 C 0.10808(14) 0.10379(14) 0.21721(8) 0.0321(4) Uani 1 1 d . . . H92A H 0.1461 0.1430 0.1980 0.038 Uiso 1 1 calc R . . H92B H 0.1599 0.0306 0.2293 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0252(13) 0.0202(13) 0.0202(13) -0.0045(10) -0.0001(10) -0.0097(11) Li2 0.0244(13) 0.0158(12) 0.0223(13) -0.0037(10) -0.0021(10) -0.0064(11) Li3 0.0227(12) 0.0231(13) 0.0193(13) -0.0060(10) 0.0009(10) -0.0112(11) Li4 0.0197(12) 0.0196(13) 0.0224(13) -0.0043(10) 0.0001(10) -0.0068(11) Li5 0.0208(12) 0.0200(13) 0.0252(14) -0.0066(11) 0.0026(10) -0.0090(11) Li6 0.0242(13) 0.0225(13) 0.0188(12) -0.0073(10) 0.0028(10) -0.0130(11) Li7 0.0248(13) 0.0206(13) 0.0191(13) -0.0039(10) -0.0014(10) -0.0102(11) Li8 0.0224(12) 0.0175(12) 0.0213(13) -0.0031(10) -0.0033(10) -0.0068(11) O1 0.0186(5) 0.0223(6) 0.0204(5) -0.0072(4) 0.0022(4) -0.0062(4) O2 0.0231(5) 0.0181(5) 0.0201(5) -0.0045(4) -0.0040(4) -0.0088(4) O3 0.0245(5) 0.0151(5) 0.0215(5) -0.0041(4) 0.0004(4) -0.0086(4) O4 0.0228(5) 0.0183(5) 0.0149(5) -0.0033(4) 0.0011(4) -0.0093(4) O5 0.0353(6) 0.0251(6) 0.0155(5) -0.0029(4) 0.0018(5) -0.0149(5) O6 0.0483(8) 0.0344(7) 0.0172(6) -0.0029(5) -0.0010(5) -0.0190(6) O7 0.0267(6) 0.0153(5) 0.0219(6) -0.0021(4) -0.0025(4) -0.0052(5) O8 0.0248(5) 0.0141(5) 0.0224(6) -0.0017(4) -0.0031(4) -0.0052(4) O9 0.0238(5) 0.0293(6) 0.0238(6) -0.0134(5) 0.0045(4) -0.0161(5) O10 0.0246(5) 0.0280(6) 0.0228(6) -0.0120(5) 0.0037(4) -0.0158(5) O11 0.0188(5) 0.0249(6) 0.0291(6) -0.0076(5) 0.0049(5) -0.0062(5) O12 0.0182(5) 0.0240(6) 0.0313(6) -0.0096(5) 0.0055(5) -0.0062(5) O13 0.0209(5) 0.0187(5) 0.0167(5) -0.0031(4) 0.0016(4) -0.0091(4) O14 0.0230(5) 0.0140(5) 0.0221(5) -0.0046(4) 0.0003(4) -0.0076(4) O15 0.0226(5) 0.0185(5) 0.0225(6) -0.0046(4) -0.0053(4) -0.0094(4) O16 0.0169(5) 0.0213(5) 0.0198(5) -0.0061(4) 0.0015(4) -0.0057(4) O17 0.0351(6) 0.0205(6) 0.0175(5) -0.0029(4) -0.0004(5) -0.0122(5) O18 0.0479(8) 0.0334(7) 0.0168(6) -0.0037(5) 0.0004(5) -0.0135(6) C1 0.0199(7) 0.0171(7) 0.0177(7) -0.0056(6) 0.0015(6) -0.0071(6) C2 0.0247(8) 0.0244(8) 0.0173(7) -0.0049(6) -0.0005(6) -0.0092(7) C3 0.0284(8) 0.0296(9) 0.0192(8) -0.0095(7) 0.0072(6) -0.0142(7) C4 0.0219(7) 0.0222(8) 0.0268(8) -0.0101(6) 0.0057(6) -0.0110(6) C5 0.0222(7) 0.0214(8) 0.0238(8) -0.0044(6) -0.0019(6) -0.0089(6) C6 0.0234(7) 0.0225(8) 0.0160(7) -0.0048(6) 0.0016(6) -0.0095(6) C7 0.0230(8) 0.0298(9) 0.0361(10) -0.0150(8) 0.0102(7) -0.0114(7) C8 0.0285(8) 0.0300(9) 0.0318(9) -0.0142(8) 0.0042(7) -0.0077(7) C9 0.0230(7) 0.0194(7) 0.0153(7) -0.0041(6) 0.0017(6) -0.0116(6) C10 0.0231(7) 0.0173(7) 0.0230(8) -0.0070(6) -0.0002(6) -0.0085(6) C11 0.0232(7) 0.0251(8) 0.0247(8) -0.0059(6) -0.0027(6) -0.0104(7) C12 0.0329(9) 0.0293(9) 0.0254(8) -0.0105(7) 0.0023(7) -0.0194(7) C13 0.0382(9) 0.0207(8) 0.0252(8) -0.0091(6) 0.0031(7) -0.0163(7) C14 0.0282(8) 0.0175(7) 0.0204(8) -0.0042(6) -0.0001(6) -0.0091(6) C15 0.0421(11) 0.0418(11) 0.0415(11) -0.0182(9) -0.0044(9) -0.0235(9) C16 0.0677(15) 0.0496(13) 0.0429(13) -0.0162(11) -0.0144(11) -0.0230(12) C17 0.0233(7) 0.0163(7) 0.0150(7) -0.0034(5) -0.0020(5) -0.0089(6) C18 0.0253(8) 0.0263(8) 0.0204(8) -0.0088(6) 0.0056(6) -0.0115(7) C19 0.0374(9) 0.0349(9) 0.0189(8) -0.0041(7) 0.0035(7) -0.0259(8) C20 0.0435(10) 0.0221(8) 0.0201(8) -0.0024(6) -0.0047(7) -0.0189(8) C21 0.0314(9) 0.0190(8) 0.0394(10) -0.0094(7) -0.0014(7) -0.0071(7) C22 0.0206(7) 0.0218(8) 0.0343(9) -0.0091(7) 0.0032(6) -0.0090(7) C23 0.0652(13) 0.0275(9) 0.0329(10) -0.0005(8) -0.0091(9) -0.0295(10) C24 0.0461(11) 0.0225(9) 0.0416(11) -0.0084(8) -0.0077(9) -0.0161(8) C25 0.0227(7) 0.0148(7) 0.0161(7) -0.0055(5) 0.0021(6) -0.0078(6) C26 0.0216(7) 0.0206(8) 0.0235(8) -0.0053(6) 0.0022(6) -0.0085(6) C27 0.0258(8) 0.0242(8) 0.0258(8) -0.0069(7) 0.0074(6) -0.0126(7) C28 0.0353(9) 0.0223(8) 0.0168(7) -0.0064(6) 0.0055(6) -0.0125(7) C29 0.0317(8) 0.0249(8) 0.0180(8) -0.0045(6) -0.0038(6) -0.0122(7) C30 0.0245(7) 0.0222(8) 0.0193(7) -0.0056(6) 0.0007(6) -0.0121(6) C31 0.0446(10) 0.0350(10) 0.0184(8) -0.0045(7) 0.0053(7) -0.0197(9) C32 0.0721(15) 0.0323(10) 0.0221(9) 0.0008(7) 0.0002(9) -0.0308(10) C33 0.0348(9) 0.0304(9) 0.0210(8) -0.0026(7) 0.0015(7) -0.0188(8) C34 0.0424(10) 0.0253(9) 0.0245(9) -0.0004(7) -0.0021(7) -0.0144(8) C35 0.0365(9) 0.0338(9) 0.0230(8) -0.0083(7) 0.0004(7) -0.0177(8) C36 0.0347(9) 0.0234(8) 0.0223(8) -0.0068(7) 0.0024(7) -0.0110(7) C37 0.0213(7) 0.0201(8) 0.0307(9) -0.0071(6) -0.0045(6) -0.0082(6) C38 0.0247(8) 0.0158(7) 0.0246(8) -0.0059(6) 0.0029(6) -0.0072(6) C39 0.0209(7) 0.0197(8) 0.0316(9) -0.0059(7) -0.0031(6) -0.0081(6) C40 0.0285(8) 0.0175(7) 0.0256(8) -0.0056(6) 0.0041(6) -0.0082(7) C41 0.0293(8) 0.0339(9) 0.0230(8) -0.0140(7) 0.0077(6) -0.0196(7) C42 0.0230(8) 0.0309(9) 0.0270(8) -0.0144(7) 0.0052(6) -0.0147(7) C43 0.0261(8) 0.0323(9) 0.0250(8) -0.0136(7) 0.0074(6) -0.0185(7) C44 0.0218(7) 0.0297(9) 0.0284(8) -0.0130(7) 0.0019(6) -0.0125(7) C45 0.0238(8) 0.0322(10) 0.0304(9) -0.0048(8) 0.0017(7) -0.0043(7) C46 0.0221(8) 0.0273(9) 0.0329(9) -0.0112(7) 0.0032(7) -0.0084(7) C47 0.0236(8) 0.0342(10) 0.0298(9) -0.0079(8) 0.0005(7) -0.0050(7) C48 0.0219(8) 0.0296(9) 0.0383(10) -0.0152(8) 0.0063(7) -0.0098(7) C49 0.0414(10) 0.0215(8) 0.0237(8) -0.0066(7) 0.0019(7) -0.0112(8) C50 0.0447(11) 0.0348(10) 0.0228(9) -0.0100(7) 0.0014(7) -0.0196(9) C51 0.0401(10) 0.0241(9) 0.0225(8) -0.0004(7) -0.0009(7) -0.0088(8) C52 0.0311(8) 0.0249(8) 0.0231(8) -0.0027(7) 0.0024(7) -0.0139(7) C53 0.0204(7) 0.0145(7) 0.0174(7) -0.0053(6) 0.0026(6) -0.0057(6) C54 0.0263(8) 0.0235(8) 0.0209(8) -0.0053(6) 0.0008(6) -0.0148(7) C55 0.0364(9) 0.0278(9) 0.0184(8) -0.0049(7) -0.0034(7) -0.0156(8) C56 0.0380(9) 0.0266(9) 0.0181(8) -0.0057(6) 0.0072(7) -0.0155(8) C57 0.0280(8) 0.0268(8) 0.0284(9) -0.0059(7) 0.0088(7) -0.0159(7) C58 0.0196(7) 0.0203(8) 0.0254(8) -0.0064(6) 0.0021(6) -0.0077(6) C59 0.0576(13) 0.0451(12) 0.0197(9) -0.0023(8) 0.0079(8) -0.0307(10) C60 0.0869(18) 0.0394(12) 0.0266(10) 0.0089(9) 0.0011(11) -0.0283(13) C61 0.0204(7) 0.0152(7) 0.0149(7) -0.0025(5) -0.0027(5) -0.0059(6) C62 0.0228(7) 0.0200(7) 0.0211(8) -0.0077(6) 0.0047(6) -0.0079(6) C63 0.0286(8) 0.0237(8) 0.0199(8) -0.0047(6) 0.0043(6) -0.0148(7) C64 0.0305(8) 0.0160(7) 0.0187(7) -0.0029(6) -0.0021(6) -0.0098(6) C65 0.0227(7) 0.0176(7) 0.0244(8) -0.0074(6) 0.0016(6) -0.0048(6) C66 0.0206(7) 0.0208(8) 0.0216(8) -0.0050(6) 0.0024(6) -0.0094(6) C67 0.0369(9) 0.0184(8) 0.0296(9) -0.0047(7) -0.0007(7) -0.0130(7) C68 0.0436(10) 0.0248(9) 0.0394(10) -0.0110(8) -0.0049(8) -0.0150(8) C69 0.0216(7) 0.0202(7) 0.0190(7) -0.0047(6) -0.0005(6) -0.0109(6) C70 0.0268(8) 0.0176(7) 0.0289(9) -0.0043(6) -0.0069(7) -0.0089(7) C71 0.0292(8) 0.0249(8) 0.0324(9) -0.0044(7) -0.0102(7) -0.0109(7) C72 0.0310(9) 0.0300(9) 0.0284(9) -0.0095(7) -0.0002(7) -0.0184(8) C73 0.0331(9) 0.0204(8) 0.0280(8) -0.0097(7) 0.0039(7) -0.0140(7) C74 0.0246(8) 0.0190(8) 0.0251(8) -0.0061(6) -0.0007(6) -0.0077(6) C75 0.0441(11) 0.0457(11) 0.0393(11) -0.0184(9) -0.0011(9) -0.0276(10) C76 0.0543(13) 0.0401(12) 0.0568(14) -0.0092(10) -0.0207(11) -0.0197(11) C77 0.0194(7) 0.0145(7) 0.0195(7) -0.0040(6) 0.0009(6) -0.0079(6) C78 0.0216(7) 0.0206(7) 0.0164(7) -0.0032(6) -0.0008(6) -0.0093(6) C79 0.0238(7) 0.0247(8) 0.0197(7) -0.0069(6) 0.0046(6) -0.0116(7) C80 0.0201(7) 0.0196(7) 0.0256(8) -0.0061(6) 0.0035(6) -0.0098(6) C81 0.0212(7) 0.0207(8) 0.0210(8) -0.0009(6) -0.0024(6) -0.0092(6) C82 0.0234(7) 0.0218(8) 0.0160(7) -0.0029(6) 0.0007(6) -0.0107(6) C83 0.0215(8) 0.0270(9) 0.0351(9) -0.0087(7) 0.0060(7) -0.0096(7) C84 0.0281(9) 0.0342(10) 0.0427(11) -0.0187(9) 0.0048(8) -0.0073(8) O19 0.0439(7) 0.0270(6) 0.0302(7) -0.0072(5) -0.0062(6) -0.0136(6) O20 0.0422(7) 0.0263(6) 0.0337(7) -0.0118(5) -0.0016(6) -0.0098(6) C85 0.0448(12) 0.0647(15) 0.0415(12) 0.0042(11) 0.0042(10) -0.0294(12) C86 0.0616(15) 0.104(2) 0.0262(11) -0.0123(12) 0.0081(10) -0.0546(16) C87 0.0408(10) 0.0350(10) 0.0345(10) -0.0044(8) -0.0005(8) -0.0202(9) C88 0.0348(10) 0.0372(10) 0.0351(10) -0.0047(8) -0.0037(8) -0.0183(8) O21 0.0483(9) 0.0348(8) 0.0530(9) -0.0083(7) 0.0038(7) -0.0209(7) O22 0.0443(8) 0.0528(9) 0.0500(9) -0.0252(8) -0.0019(7) -0.0188(7) C89 0.0352(9) 0.0263(9) 0.0292(9) -0.0005(7) -0.0059(7) -0.0128(8) C90 0.0302(9) 0.0314(10) 0.0413(11) -0.0059(8) -0.0013(8) -0.0084(8) C91 0.0310(9) 0.0293(9) 0.0283(9) -0.0063(7) -0.0023(7) -0.0096(8) C92 0.0296(9) 0.0314(9) 0.0291(9) -0.0061(7) -0.0011(7) -0.0095(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O3 1.943(3) . ? Li1 O1 1.957(3) . ? Li1 O2 1.967(3) . ? Li1 O5 1.980(3) . ? Li2 O2 1.920(3) . ? Li2 O7 1.945(3) . ? Li2 O1 1.958(3) . ? Li2 O4 1.990(3) . ? Li3 O4 1.908(3) . ? Li3 O9 1.913(3) . ? Li3 O1 1.927(3) . ? Li3 O3 1.972(3) . ? Li4 O3 1.937(3) . ? Li4 O2 1.939(3) . ? Li4 O4 1.946(3) . ? Li4 O11 1.961(3) . ? Li5 O13 1.938(3) . ? Li5 O15 1.939(3) . ? Li5 O14 1.946(3) . ? Li5 O12 1.978(3) 1_455 ? Li5 Li8 2.662(4) 1_545 ? Li6 O10 1.907(3) . ? Li6 O16 1.917(3) . ? Li6 O13 1.918(3) . ? Li6 O14 1.982(3) . ? Li6 Li8 2.560(4) 1_545 ? Li7 O14 1.935(3) . ? Li7 O15 1.955(3) . ? Li7 O16 1.964(3) . ? Li7 O17 1.974(3) . ? Li7 Li8 2.617(4) 1_545 ? Li8 O15 1.914(3) 1_565 ? Li8 O8 1.944(3) . ? Li8 O16 1.974(3) 1_565 ? Li8 O13 1.991(3) 1_565 ? Li8 Li6 2.560(4) 1_565 ? Li8 Li7 2.617(4) 1_565 ? Li8 Li5 2.662(4) 1_565 ? Li8 C53 2.788(3) 1_565 ? O1 C1 1.3317(18) . ? O2 C9 1.3293(18) . ? O3 C17 1.3312(18) . ? O4 C25 1.3298(17) . ? O5 C36 1.439(2) . ? O5 C33 1.442(2) . ? O6 C34 1.428(2) . ? O6 C35 1.433(2) . ? O7 C37 1.433(2) . ? O7 C40 1.4383(19) . ? O8 C38 1.4383(19) . ? O8 C39 1.439(2) . ? O9 C44 1.4367(19) . ? O9 C41 1.4421(19) . ? O10 C42 1.4367(19) . ? O10 C43 1.4400(19) . ? O11 C45 1.436(2) . ? O11 C48 1.441(2) . ? O12 C46 1.442(2) . ? O12 C47 1.445(2) . ? O12 Li5 1.978(3) 1_655 ? O13 C53 1.3336(18) . ? O13 Li8 1.991(3) 1_545 ? O14 C61 1.3306(17) . ? O15 C69 1.3294(17) . ? O15 Li8 1.914(3) 1_545 ? O16 C77 1.3340(18) . ? O16 Li8 1.974(3) 1_545 ? O17 C49 1.436(2) . ? O17 C52 1.4382(19) . ? O18 C51 1.427(2) . ? O18 C50 1.430(2) . ? C1 C6 1.406(2) . ? C1 C2 1.410(2) . ? C2 C3 1.388(2) . ? C2 H2 0.9500 . ? C3 C4 1.394(2) . ? C3 H3 0.9500 . ? C4 C5 1.394(2) . ? C4 C7 1.515(2) . ? C5 C6 1.392(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.520(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.402(2) . ? C9 C10 1.402(2) . ? C10 C11 1.390(2) . ? C10 H10 0.9500 . ? C11 C12 1.394(2) . ? C11 H11 0.9500 . ? C12 C13 1.388(2) . ? C12 C15 1.515(2) . ? C13 C14 1.388(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.489(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.401(2) . ? C17 C18 1.404(2) . ? C18 C19 1.391(2) . ? C18 H18 0.9500 . ? C19 C20 1.382(3) . ? C19 H19 0.9500 . ? C20 C21 1.388(3) . ? C20 C23 1.517(2) . ? C21 C22 1.387(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.518(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.406(2) . ? C25 C30 1.411(2) . ? C26 C27 1.389(2) . ? C26 H26 0.9500 . ? C27 C28 1.395(2) . ? C27 H27 0.9500 . ? C28 C29 1.396(2) . ? C28 C31 1.514(2) . ? C29 C30 1.394(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.525(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.506(2) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.504(2) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.505(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.504(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.503(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.502(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.494(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.509(2) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.507(2) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.504(2) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C58 1.404(2) . ? C53 C54 1.406(2) . ? C53 Li8 2.787(3) 1_545 ? C54 C55 1.391(2) . ? C54 H54 0.9500 . ? C55 C56 1.387(2) . ? C55 H55 0.9500 . ? C56 C57 1.394(3) . ? C56 C59 1.515(2) . ? C57 C58 1.389(2) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.516(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.404(2) . ? C61 C66 1.407(2) . ? C62 C63 1.390(2) . ? C62 H62 0.9500 . ? C63 C64 1.391(2) . ? C63 H63 0.9500 . ? C64 C65 1.392(2) . ? C64 C67 1.518(2) . ? C65 C66 1.387(2) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C68 1.522(2) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.401(2) . ? C69 C74 1.404(2) . ? C70 C71 1.391(2) . ? C70 H70 0.9500 . ? C71 C72 1.392(2) . ? C71 H71 0.9500 . ? C72 C73 1.389(2) . ? C72 C75 1.522(2) . ? C73 C74 1.387(2) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 C76 1.488(3) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.405(2) . ? C77 C82 1.407(2) . ? C78 C79 1.387(2) . ? C78 H78 0.9500 . ? C79 C80 1.395(2) . ? C79 H79 0.9500 . ? C80 C81 1.391(2) . ? C80 C83 1.516(2) . ? C81 C82 1.394(2) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.519(3) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? O19 C92 1.424(2) . ? O19 C89 1.425(2) . ? O20 C91 1.420(2) . ? O20 C90 1.438(2) . ? C85 O21 1.425(3) . ? C85 C86 1.511(3) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 O22 1.423(3) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 O22 1.424(2) . ? C87 C88 1.494(3) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 O21 1.409(2) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 C90 1.496(3) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C90 H90A 0.9900 . ? C90 H90B 0.9900 . ? C91 C92 1.498(2) . ? C91 H91A 0.9900 . ? C91 H91B 0.9900 . ? C92 H92A 0.9900 . ? C92 H92B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Li1 O1 93.79(12) . . ? O3 Li1 O2 93.69(12) . . ? O1 Li1 O2 95.07(12) . . ? O3 Li1 O5 125.46(14) . . ? O1 Li1 O5 126.31(15) . . ? O2 Li1 O5 114.51(14) . . ? O2 Li2 O7 125.33(15) . . ? O2 Li2 O1 96.54(12) . . ? O7 Li2 O1 121.00(14) . . ? O2 Li2 O4 92.77(12) . . ? O7 Li2 O4 118.21(14) . . ? O1 Li2 O4 95.94(12) . . ? O4 Li3 O9 111.26(14) . . ? O4 Li3 O1 99.78(13) . . ? O9 Li3 O1 130.61(15) . . ? O4 Li3 O3 93.96(12) . . ? O9 Li3 O3 120.17(14) . . ? O1 Li3 O3 93.80(12) . . ? O3 Li4 O2 94.79(12) . . ? O3 Li4 O4 93.89(12) . . ? O2 Li4 O4 93.56(12) . . ? O3 Li4 O11 124.43(14) . . ? O2 Li4 O11 129.40(15) . . ? O4 Li4 O11 111.94(14) . . ? O13 Li5 O15 93.75(12) . . ? O13 Li5 O14 94.38(12) . . ? O15 Li5 O14 94.49(12) . . ? O13 Li5 O12 112.44(14) . 1_455 ? O15 Li5 O12 129.26(15) . 1_455 ? O14 Li5 O12 124.03(14) . 1_455 ? O13 Li5 Li8 48.20(9) . 1_545 ? O15 Li5 Li8 45.91(8) . 1_545 ? O14 Li5 Li8 91.79(12) . 1_545 ? O12 Li5 Li8 142.74(14) 1_455 1_545 ? O10 Li6 O16 128.18(15) . . ? O10 Li6 O13 112.47(14) . . ? O16 Li6 O13 100.09(12) . . ? O10 Li6 O14 121.08(14) . . ? O16 Li6 O14 94.37(12) . . ? O13 Li6 O14 93.86(12) . . ? O10 Li6 Li8 143.52(15) . 1_545 ? O16 Li6 Li8 49.83(9) . 1_545 ? O13 Li6 Li8 50.34(9) . 1_545 ? O14 Li6 Li8 94.04(12) . 1_545 ? O14 Li7 O15 94.29(12) . . ? O14 Li7 O16 94.35(12) . . ? O15 Li7 O16 95.13(12) . . ? O14 Li7 O17 126.65(15) . . ? O15 Li7 O17 110.51(13) . . ? O16 Li7 O17 127.56(15) . . ? O14 Li7 Li8 93.39(12) . 1_545 ? O15 Li7 Li8 46.77(9) . 1_545 ? O16 Li7 Li8 48.51(9) . 1_545 ? O17 Li7 Li8 138.02(14) . 1_545 ? O15 Li8 O8 123.05(14) 1_565 . ? O15 Li8 O16 96.15(12) 1_565 1_565 ? O8 Li8 O16 121.96(14) . 1_565 ? O15 Li8 O13 92.85(12) 1_565 1_565 ? O8 Li8 O13 120.06(14) . 1_565 ? O16 Li8 O13 95.70(12) 1_565 1_565 ? O15 Li8 Li6 94.52(12) 1_565 1_565 ? O8 Li8 Li6 142.33(14) . 1_565 ? O16 Li8 Li6 47.91(9) 1_565 1_565 ? O13 Li8 Li6 47.86(9) 1_565 1_565 ? O15 Li8 Li7 48.10(9) 1_565 1_565 ? O8 Li8 Li7 146.60(15) . 1_565 ? O16 Li8 Li7 48.20(9) 1_565 1_565 ? O13 Li8 Li7 93.34(12) 1_565 1_565 ? Li6 Li8 Li7 61.23(10) 1_565 1_565 ? O15 Li8 Li5 46.68(9) 1_565 1_565 ? O8 Li8 Li5 143.98(15) . 1_565 ? O16 Li8 Li5 93.99(12) 1_565 1_565 ? O13 Li8 Li5 46.53(9) 1_565 1_565 ? Li6 Li8 Li5 60.76(10) 1_565 1_565 ? Li7 Li8 Li5 60.00(10) 1_565 1_565 ? O15 Li8 C53 108.40(12) 1_565 1_565 ? O8 Li8 C53 93.85(11) . 1_565 ? O16 Li8 C53 113.82(12) 1_565 1_565 ? O13 Li8 C53 26.24(6) 1_565 1_565 ? Li6 Li8 C53 69.17(9) 1_565 1_565 ? Li7 Li8 C53 119.51(12) 1_565 1_565 ? Li5 Li8 C53 66.84(9) 1_565 1_565 ? C1 O1 Li3 125.67(12) . . ? C1 O1 Li1 133.15(12) . . ? Li3 O1 Li1 86.13(12) . . ? C1 O1 Li2 129.01(12) . . ? Li3 O1 Li2 82.24(12) . . ? Li1 O1 Li2 83.70(12) . . ? C9 O2 Li2 131.17(12) . . ? C9 O2 Li4 134.59(12) . . ? Li2 O2 Li4 87.48(12) . . ? C9 O2 Li1 116.63(12) . . ? Li2 O2 Li1 84.45(12) . . ? Li4 O2 Li1 85.36(12) . . ? C17 O3 Li4 139.20(13) . . ? C17 O3 Li1 128.04(12) . . ? Li4 O3 Li1 86.06(12) . . ? C17 O3 Li3 115.75(12) . . ? Li4 O3 Li3 85.00(12) . . ? Li1 O3 Li3 85.26(12) . . ? C25 O4 Li3 139.07(12) . . ? C25 O4 Li4 130.50(12) . . ? Li3 O4 Li4 86.53(12) . . ? C25 O4 Li2 113.54(12) . . ? Li3 O4 Li2 81.90(12) . . ? Li4 O4 Li2 85.34(12) . . ? C36 O5 C33 110.45(12) . . ? C36 O5 Li1 124.60(12) . . ? C33 O5 Li1 119.87(13) . . ? C34 O6 C35 109.29(13) . . ? C37 O7 C40 109.52(11) . . ? C37 O7 Li2 124.15(13) . . ? C40 O7 Li2 125.53(13) . . ? C38 O8 C39 109.40(11) . . ? C38 O8 Li8 126.06(12) . . ? C39 O8 Li8 124.00(12) . . ? C44 O9 C41 110.55(11) . . ? C44 O9 Li3 134.11(12) . . ? C41 O9 Li3 114.64(12) . . ? C42 O10 C43 110.78(11) . . ? C42 O10 Li6 130.89(12) . . ? C43 O10 Li6 117.94(12) . . ? C45 O11 C48 109.16(13) . . ? C45 O11 Li4 126.80(13) . . ? C48 O11 Li4 121.00(12) . . ? C46 O12 C47 109.80(12) . . ? C46 O12 Li5 115.01(12) . 1_655 ? C47 O12 Li5 131.68(13) . 1_655 ? C53 O13 Li6 137.82(12) . . ? C53 O13 Li5 132.38(12) . . ? Li6 O13 Li5 86.50(12) . . ? C53 O13 Li8 112.45(12) . 1_545 ? Li6 O13 Li8 81.79(12) . 1_545 ? Li5 O13 Li8 85.27(11) . 1_545 ? C61 O14 Li7 134.09(12) . . ? C61 O14 Li5 136.36(12) . . ? Li7 O14 Li5 85.72(12) . . ? C61 O14 Li6 111.81(12) . . ? Li7 O14 Li6 84.63(11) . . ? Li5 O14 Li6 84.56(12) . . ? C69 O15 Li8 133.19(12) . 1_545 ? C69 O15 Li5 130.08(12) . . ? Li8 O15 Li5 87.40(12) 1_545 . ? C69 O15 Li7 119.79(12) . . ? Li8 O15 Li7 85.13(12) 1_545 . ? Li5 O15 Li7 85.36(12) . . ? C77 O16 Li6 130.69(12) . . ? C77 O16 Li7 132.86(12) . . ? Li6 O16 Li7 85.58(12) . . ? C77 O16 Li8 124.63(12) . 1_545 ? Li6 O16 Li8 82.25(12) . 1_545 ? Li7 O16 Li8 83.29(12) . 1_545 ? C49 O17 C52 110.71(12) . . ? C49 O17 Li7 125.24(12) . . ? C52 O17 Li7 120.91(12) . . ? C51 O18 C50 108.94(13) . . ? O1 C1 C6 121.63(13) . . ? O1 C1 C2 121.60(14) . . ? C6 C1 C2 116.76(14) . . ? C3 C2 C1 121.09(15) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 121.93(15) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 117.17(14) . . ? C3 C4 C7 120.90(15) . . ? C5 C4 C7 121.88(15) . . ? C6 C5 C4 121.61(15) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 121.32(14) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? C4 C7 C8 112.31(14) . . ? C4 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C4 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C14 121.52(14) . . ? O2 C9 C10 121.44(13) . . ? C14 C9 C10 117.02(14) . . ? C11 C10 C9 121.17(14) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 121.51(15) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 117.36(15) . . ? C13 C12 C15 121.25(16) . . ? C11 C12 C15 121.38(16) . . ? C14 C13 C12 121.73(15) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C9 121.21(15) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? C16 C15 C12 112.98(17) . . ? C16 C15 H15A 109.0 . . ? C12 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C12 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C22 121.65(14) . . ? O3 C17 C18 121.48(14) . . ? C22 C17 C18 116.86(14) . . ? C19 C18 C17 121.42(15) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C20 C19 C18 121.51(16) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 117.18(15) . . ? C19 C20 C23 122.23(17) . . ? C21 C20 C23 120.55(17) . . ? C22 C21 C20 122.36(16) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C21 C22 C17 120.65(16) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? C20 C23 C24 112.45(15) . . ? C20 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C20 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 C26 121.29(14) . . ? O4 C25 C30 121.73(14) . . ? C26 C25 C30 116.97(14) . . ? C27 C26 C25 121.42(15) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 121.57(15) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C29 117.40(15) . . ? C27 C28 C31 120.90(16) . . ? C29 C28 C31 121.59(16) . . ? C30 C29 C28 121.70(15) . . ? C30 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C29 C30 C25 120.90(15) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C28 C31 C32 111.91(14) . . ? C28 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C28 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C33 C34 110.58(14) . . ? O5 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? O5 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? O6 C34 C33 110.63(14) . . ? O6 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? O6 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? O6 C35 C36 111.13(14) . . ? O6 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? O6 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? O5 C36 C35 110.84(14) . . ? O5 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? O5 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? O7 C37 C38 110.70(13) . . ? O7 C37 H37A 109.5 . . ? C38 C37 H37A 109.5 . . ? O7 C37 H37B 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? O8 C38 C37 110.12(13) . . ? O8 C38 H38A 109.6 . . ? C37 C38 H38A 109.6 . . ? O8 C38 H38B 109.6 . . ? C37 C38 H38B 109.6 . . ? H38A C38 H38B 108.2 . . ? O8 C39 C40 109.89(13) . . ? O8 C39 H39A 109.7 . . ? C40 C39 H39A 109.7 . . ? O8 C39 H39B 109.7 . . ? C40 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? O7 C40 C39 110.10(13) . . ? O7 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? O7 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.2 . . ? O9 C41 C42 110.10(13) . . ? O9 C41 H41A 109.6 . . ? C42 C41 H41A 109.6 . . ? O9 C41 H41B 109.6 . . ? C42 C41 H41B 109.6 . . ? H41A C41 H41B 108.2 . . ? O10 C42 C41 110.04(13) . . ? O10 C42 H42A 109.7 . . ? C41 C42 H42A 109.7 . . ? O10 C42 H42B 109.7 . . ? C41 C42 H42B 109.7 . . ? H42A C42 H42B 108.2 . . ? O10 C43 C44 110.26(13) . . ? O10 C43 H43A 109.6 . . ? C44 C43 H43A 109.6 . . ? O10 C43 H43B 109.6 . . ? C44 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? O9 C44 C43 110.16(13) . . ? O9 C44 H44A 109.6 . . ? C43 C44 H44A 109.6 . . ? O9 C44 H44B 109.6 . . ? C43 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? O11 C45 C46 110.77(14) . . ? O11 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? O11 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? O12 C46 C45 110.05(14) . . ? O12 C46 H46A 109.7 . . ? C45 C46 H46A 109.6 . . ? O12 C46 H46B 109.7 . . ? C45 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? O12 C47 C48 110.17(14) . . ? O12 C47 H47A 109.6 . . ? C48 C47 H47A 109.6 . . ? O12 C47 H47B 109.6 . . ? C48 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? O11 C48 C47 110.75(14) . . ? O11 C48 H48A 109.5 . . ? C47 C48 H48A 109.5 . . ? O11 C48 H48B 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 108.1 . . ? O17 C49 C50 110.56(14) . . ? O17 C49 H49A 109.5 . . ? C50 C49 H49A 109.5 . . ? O17 C49 H49B 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 108.1 . . ? O18 C50 C49 110.51(15) . . ? O18 C50 H50A 109.5 . . ? C49 C50 H50A 109.5 . . ? O18 C50 H50B 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? O18 C51 C52 111.12(14) . . ? O18 C51 H51A 109.4 . . ? C52 C51 H51A 109.4 . . ? O18 C51 H51B 109.4 . . ? C52 C51 H51B 109.4 . . ? H51A C51 H51B 108.0 . . ? O17 C52 C51 110.80(14) . . ? O17 C52 H52A 109.5 . . ? C51 C52 H52A 109.5 . . ? O17 C52 H52B 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 108.1 . . ? O13 C53 C58 121.18(14) . . ? O13 C53 C54 121.57(14) . . ? C58 C53 C54 117.24(14) . . ? O13 C53 Li8 41.31(8) . 1_545 ? C58 C53 Li8 107.26(11) . 1_545 ? C54 C53 Li8 118.24(11) . 1_545 ? C55 C54 C53 120.74(15) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C56 C55 C54 122.02(15) . . ? C56 C55 H55 119.0 . . ? C54 C55 H55 119.0 . . ? C55 C56 C57 117.20(15) . . ? C55 C56 C59 121.51(17) . . ? C57 C56 C59 121.18(16) . . ? C58 C57 C56 121.82(15) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C57 C58 C53 120.94(15) . . ? C57 C58 H58 119.5 . . ? C53 C58 H58 119.5 . . ? C56 C59 C60 112.12(16) . . ? C56 C59 H59A 109.2 . . ? C60 C59 H59A 109.2 . . ? C56 C59 H59B 109.2 . . ? C60 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O14 C61 C62 121.89(13) . . ? O14 C61 C66 121.47(14) . . ? C62 C61 C66 116.64(14) . . ? C63 C62 C61 121.43(14) . . ? C63 C62 H62 119.3 . . ? C61 C62 H62 119.3 . . ? C62 C63 C64 121.63(15) . . ? C62 C63 H63 119.2 . . ? C64 C63 H63 119.2 . . ? C63 C64 C65 117.23(14) . . ? C63 C64 C67 121.89(15) . . ? C65 C64 C67 120.87(15) . . ? C66 C65 C64 121.80(14) . . ? C66 C65 H65 119.1 . . ? C64 C65 H65 119.1 . . ? C65 C66 C61 121.27(14) . . ? C65 C66 H66 119.4 . . ? C61 C66 H66 119.4 . . ? C64 C67 C68 113.17(14) . . ? C64 C67 H67A 108.9 . . ? C68 C67 H67A 108.9 . . ? C64 C67 H67B 108.9 . . ? C68 C67 H67B 108.9 . . ? H67A C67 H67B 107.8 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O15 C69 C70 121.27(14) . . ? O15 C69 C74 121.83(14) . . ? C70 C69 C74 116.90(14) . . ? C71 C70 C69 121.40(15) . . ? C71 C70 H70 119.3 . . ? C69 C70 H70 119.3 . . ? C70 C71 C72 121.50(16) . . ? C70 C71 H71 119.3 . . ? C72 C71 H71 119.3 . . ? C73 C72 C71 117.05(15) . . ? C73 C72 C75 120.65(16) . . ? C71 C72 C75 122.27(16) . . ? C74 C73 C72 122.21(15) . . ? C74 C73 H73 118.9 . . ? C72 C73 H73 118.9 . . ? C73 C74 C69 120.92(15) . . ? C73 C74 H74 119.5 . . ? C69 C74 H74 119.5 . . ? C76 C75 C72 115.89(17) . . ? C76 C75 H75A 108.3 . . ? C72 C75 H75A 108.3 . . ? C76 C75 H75B 108.3 . . ? C72 C75 H75B 108.3 . . ? H75A C75 H75B 107.4 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O16 C77 C78 121.55(13) . . ? O16 C77 C82 121.82(13) . . ? C78 C77 C82 116.62(13) . . ? C79 C78 C77 121.32(14) . . ? C79 C78 H78 119.3 . . ? C77 C78 H78 119.3 . . ? C78 C79 C80 121.91(14) . . ? C78 C79 H79 119.0 . . ? C80 C79 H79 119.0 . . ? C81 C80 C79 117.04(14) . . ? C81 C80 C83 121.85(15) . . ? C79 C80 C83 121.06(15) . . ? C80 C81 C82 121.71(14) . . ? C80 C81 H81 119.1 . . ? C82 C81 H81 119.1 . . ? C81 C82 C77 121.23(14) . . ? C81 C82 H82 119.4 . . ? C77 C82 H82 119.4 . . ? C80 C83 C84 112.90(14) . . ? C80 C83 H83A 109.0 . . ? C84 C83 H83A 109.0 . . ? C80 C83 H83B 109.0 . . ? C84 C83 H83B 109.0 . . ? H83A C83 H83B 107.8 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C92 O19 C89 108.80(13) . . ? C91 O20 C90 109.37(14) . . ? O21 C85 C86 110.81(17) . . ? O21 C85 H85A 109.5 . . ? C86 C85 H85A 109.5 . . ? O21 C85 H85B 109.5 . . ? C86 C85 H85B 109.5 . . ? H85A C85 H85B 108.1 . . ? O22 C86 C85 109.77(19) . . ? O22 C86 H86A 109.7 . . ? C85 C86 H86A 109.7 . . ? O22 C86 H86B 109.7 . . ? C85 C86 H86B 109.7 . . ? H86A C86 H86B 108.2 . . ? O22 C87 C88 109.51(16) . . ? O22 C87 H87A 109.8 . . ? C88 C87 H87A 109.8 . . ? O22 C87 H87B 109.8 . . ? C88 C87 H87B 109.8 . . ? H87A C87 H87B 108.2 . . ? O21 C88 C87 111.05(16) . . ? O21 C88 H88A 109.4 . . ? C87 C88 H88A 109.4 . . ? O21 C88 H88B 109.4 . . ? C87 C88 H88B 109.4 . . ? H88A C88 H88B 108.0 . . ? C88 O21 C85 108.30(16) . . ? C86 O22 C87 109.19(16) . . ? O19 C89 C90 110.33(15) . . ? O19 C89 H89A 109.6 . . ? C90 C89 H89A 109.6 . . ? O19 C89 H89B 109.6 . . ? C90 C89 H89B 109.6 . . ? H89A C89 H89B 108.1 . . ? O20 C90 C89 110.58(15) . . ? O20 C90 H90A 109.5 . . ? C89 C90 H90A 109.5 . . ? O20 C90 H90B 109.5 . . ? C89 C90 H90B 109.5 . . ? H90A C90 H90B 108.1 . . ? O20 C91 C92 110.31(15) . . ? O20 C91 H91A 109.6 . . ? C92 C91 H91A 109.6 . . ? O20 C91 H91B 109.6 . . ? C92 C91 H91B 109.6 . . ? H91A C91 H91B 108.1 . . ? O19 C92 C91 110.38(15) . . ? O19 C92 H92A 109.6 . . ? C91 C92 H92A 109.6 . . ? O19 C92 H92B 109.6 . . ? C91 C92 H92B 109.6 . . ? H92A C92 H92B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.982 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.071 _ccdc_chemical_compound_source_recrystallisation dioxane data_dmd14sq _database_code_depnum_ccdc_archive 'CCDC 239844' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C12 H11 Li O2), 3(C4 H8 O2)' _chemical_formula_sum 'C15 H17 Li O3.50' _chemical_formula_weight 260.23 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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_int_tables_number 88 _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 15.0031(1) _cell_length_b 15.0031(1) _cell_length_c 24.7185(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5563.96(10) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7510 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 31.98 _exptl_crystal_description octahedron _exptl_crystal_colour clear _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8112 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details 'Blessing, R. H. Acta Cryst. (1995) A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18864 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 30.51 _reflns_number_total 4247 _reflns_number_gt 3158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2/SAINT' _computing_data_reduction 'Bruker SAINT/SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The asymmetric unit contains three moieties. In addition to the monomeric unit of the polymer there are two disordered sites of dioxane molecules. One site is disordered across two positions by 2-fold symmetry. The second is disordered across four positions by \=4 symmetry. The asymmetric unit is formulated to be C~12~H~11~O~2~Li^.^0.75(C~4~H~8~O~2~. The solvent sites were modeled using PLATON/SQUEEZE, which found 572 e^_^/unit cell for solvent. As formulated, there are 576 e^_^/unit cell attributed to solvent. On the monomeric unit hydrogens were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom. All non-hydrogen atoms were modeled with parameters for anisotropic thermal motion. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.2880P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4247 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1360 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.47597(10) 0.66657(10) 0.08624(6) 0.0295(3) Uani 1 1 d . . . O1 O 0.59312(4) 0.72312(4) 0.08515(2) 0.02693(16) Uani 1 1 d . . . O2 O 0.47176(4) 0.56974(4) 0.03460(2) 0.03098(17) Uani 1 1 d . . . C1 C 0.65515(6) 0.68654(6) 0.05387(4) 0.0291(2) Uani 1 1 d . . . C2 C 0.68438(7) 0.72750(7) 0.00703(4) 0.0377(2) Uani 1 1 d . . . H2 H 0.6603 0.7838 -0.0029 0.045 Uiso 1 1 calc R . . C3 C 0.74917(7) 0.68751(9) -0.02636(5) 0.0464(3) Uani 1 1 d . . . H3 H 0.7668 0.7166 -0.0588 0.056 Uiso 1 1 calc R . . C4 C 0.78683(7) 0.60819(9) -0.01313(5) 0.0484(3) Uani 1 1 d . . . H4 H 0.8314 0.5830 -0.0357 0.058 Uiso 1 1 calc R . . C5 C 0.75960(7) 0.56294(8) 0.03436(4) 0.0454(3) Uani 1 1 d . . . C6 C 0.79552(10) 0.47900(10) 0.04980(6) 0.0679(5) Uani 1 1 d . . . H6 H 0.8397 0.4520 0.0276 0.082 Uiso 1 1 calc R . . C7 C 0.76844(12) 0.43639(11) 0.09528(6) 0.0809(6) Uani 1 1 d . . . H7 H 0.7942 0.3807 0.1049 0.097 Uiso 1 1 calc R . . C8 C 0.70264(12) 0.47416(9) 0.12816(5) 0.0647(4) Uani 1 1 d . . . H8 H 0.6839 0.4440 0.1600 0.078 Uiso 1 1 calc R . . C9 C 0.66515(8) 0.55429(7) 0.11472(4) 0.0413(3) Uani 1 1 d . . . H9 H 0.6197 0.5786 0.1370 0.050 Uiso 1 1 calc R . . C10 C 0.69305(6) 0.60153(7) 0.06814(4) 0.0343(2) Uani 1 1 d . . . C11 C 0.47573(7) 0.58158(6) -0.02306(4) 0.0318(2) Uani 1 1 d . . . H11A H 0.4897 0.6446 -0.0314 0.038 Uiso 1 1 calc R . . H11B H 0.4170 0.5674 -0.0391 0.038 Uiso 1 1 calc R . . C12 C 0.45410(7) 0.47800(6) 0.04741(4) 0.0319(2) Uani 1 1 d . . . H12A H 0.3948 0.4610 0.0332 0.038 Uiso 1 1 calc R . . H12B H 0.4533 0.4702 0.0872 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0341(8) 0.0332(8) 0.0213(7) -0.0036(6) 0.0006(6) -0.0028(6) O1 0.0280(3) 0.0336(3) 0.0191(3) -0.0025(2) 0.0016(2) 0.0005(2) O2 0.0391(4) 0.0352(3) 0.0187(3) -0.0077(2) 0.0038(3) -0.0063(3) C1 0.0248(4) 0.0395(5) 0.0230(4) -0.0090(4) -0.0017(3) -0.0014(3) C2 0.0368(5) 0.0446(5) 0.0316(5) -0.0043(4) 0.0079(4) -0.0046(4) C3 0.0387(5) 0.0636(7) 0.0368(6) -0.0129(5) 0.0141(4) -0.0111(5) C4 0.0285(5) 0.0751(8) 0.0417(6) -0.0280(6) 0.0026(4) 0.0023(5) C5 0.0362(5) 0.0649(7) 0.0349(6) -0.0223(5) -0.0125(4) 0.0158(5) C6 0.0700(8) 0.0860(10) 0.0477(7) -0.0301(7) -0.0216(6) 0.0470(8) C7 0.1195(13) 0.0796(10) 0.0438(8) -0.0176(7) -0.0304(8) 0.0645(10) C8 0.1081(12) 0.0549(7) 0.0311(6) -0.0058(5) -0.0207(7) 0.0352(7) C9 0.0585(7) 0.0411(5) 0.0242(5) -0.0087(4) -0.0126(4) 0.0140(5) C10 0.0338(5) 0.0451(5) 0.0240(4) -0.0122(4) -0.0105(4) 0.0075(4) C11 0.0390(5) 0.0365(5) 0.0199(4) -0.0058(4) 0.0019(4) -0.0039(4) C12 0.0387(5) 0.0358(5) 0.0211(4) -0.0051(3) 0.0049(4) -0.0063(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.9349(16) . ? Li1 O1 1.9490(16) 15_565 ? Li1 O1 1.9519(16) . ? Li1 O1 1.9531(17) 6_564 ? Li1 Li1 2.605(3) 6_564 ? Li1 Li1 2.658(3) 15_565 ? Li1 Li1 2.658(3) 12_766 ? O1 C1 1.3285(10) . ? O1 Li1 1.9490(16) 12_766 ? O1 Li1 1.9531(17) 6_564 ? O2 C12 1.4370(11) . ? O2 C11 1.4377(11) . ? C1 C2 1.3824(14) . ? C1 C10 1.4402(14) . ? C2 C3 1.4092(14) . ? C2 H2 0.9500 . ? C3 C4 1.3572(18) . ? C3 H3 0.9500 . ? C4 C5 1.4163(18) . ? C4 H4 0.9500 . ? C5 C6 1.4220(18) . ? C5 C10 1.4245(14) . ? C6 C7 1.356(2) . ? C6 H6 0.9500 . ? C7 C8 1.399(2) . ? C7 H7 0.9500 . ? C8 C9 1.3682(16) . ? C8 H8 0.9500 . ? C9 C10 1.4153(15) . ? C9 H9 0.9500 . ? C11 C12 1.5065(13) 9_665 ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C11 1.5065(13) 9_665 ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li1 O1 126.94(9) . 15_565 ? O2 Li1 O1 110.28(8) . . ? O1 Li1 O1 93.78(7) 15_565 . ? O2 Li1 O1 127.58(8) . 6_564 ? O1 Li1 O1 93.74(7) 15_565 6_564 ? O1 Li1 O1 96.28(7) . 6_564 ? O2 Li1 Li1 136.93(5) . 6_564 ? O1 Li1 Li1 94.46(5) 15_565 6_564 ? O1 Li1 Li1 48.17(5) . 6_564 ? O1 Li1 Li1 48.13(6) 6_564 6_564 ? O2 Li1 Li1 156.93(9) . 15_565 ? O1 Li1 Li1 47.09(6) 15_565 15_565 ? O1 Li1 Li1 92.77(5) . 15_565 ? O1 Li1 Li1 47.00(4) 6_564 15_565 ? Li1 Li1 Li1 60.65(3) 6_564 15_565 ? O2 Li1 Li1 138.34(9) . 12_766 ? O1 Li1 Li1 47.13(6) 15_565 12_766 ? O1 Li1 Li1 47.00(4) . 12_766 ? O1 Li1 Li1 92.74(5) 6_564 12_766 ? Li1 Li1 Li1 60.65(3) 6_564 12_766 ? Li1 Li1 Li1 58.69(7) 15_565 12_766 ? C1 O1 Li1 129.90(7) . 12_766 ? C1 O1 Li1 117.34(7) . . ? Li1 O1 Li1 85.91(7) 12_766 . ? C1 O1 Li1 136.88(7) . 6_564 ? Li1 O1 Li1 85.87(7) 12_766 6_564 ? Li1 O1 Li1 83.70(7) . 6_564 ? C12 O2 C11 110.14(6) . . ? C12 O2 Li1 125.44(7) . . ? C11 O2 Li1 124.05(7) . . ? O1 C1 C2 121.74(9) . . ? O1 C1 C10 119.99(9) . . ? C2 C1 C10 118.27(8) . . ? C1 C2 C3 121.34(10) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 121.29(11) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.99(9) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 122.52(11) . . ? C4 C5 C10 119.55(10) . . ? C6 C5 C10 117.93(12) . . ? C7 C6 C5 121.77(12) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 120.16(12) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.33(14) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 121.07(11) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C9 C10 C5 118.72(10) . . ? C9 C10 C1 121.73(9) . . ? C5 C10 C1 119.54(10) . . ? O2 C11 C12 110.59(8) . 9_665 ? O2 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 9_665 . ? O2 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 9_665 . ? H11A C11 H11B 108.1 . . ? O2 C12 C11 110.58(7) . 9_665 ? O2 C12 H12A 109.5 . . ? C11 C12 H12A 109.5 9_665 . ? O2 C12 H12B 109.5 . . ? C11 C12 H12B 109.5 9_665 . ? H12A C12 H12B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.272 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.034 _chemical_compound_source synthesized