data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dietmar Stalke' _publ_contact_author_email DSTALKE@CHEMIE.UNI-GOETTINGEN.DE _publ_section_title ; The first asymmetric organolithium tetramers with simple ether donor bases ; loop_ _publ_author_name 'Dietmar Stalke' 'Julian Henn' 'Kathrin Meindl' 'Sushil Kumar Pandey' 'Tanja Tatic' # Attachment 'dee.cif' data_dee _database_code_depnum_ccdc_archive 'CCDC 764771' #TrackingRef 'dee.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H64 Li4 O2 Si4' _chemical_formula_weight 524.87 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.882(7) _cell_length_b 19.081(13) _cell_length_c 18.544(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.018(9) _cell_angle_gamma 90.00 _cell_volume 3719(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9063 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 29.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9412 _exptl_absorpt_correction_T_max 0.9742 _exptl_absorpt_process_details ? _exptl_special_details ; Intensities were measured with a Bruker APEX II area detector ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 145981 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 31.95 _reflns_number_total 24602 _reflns_number_gt 21555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (v2.2-0, Bruker 2007)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.46a, Bruker 2007)' _computing_data_reduction 'Bruker AXS SAINT (v 7.46a, Bruker 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.3.1, Bruker 2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0405P)^2^+0.3059P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 24602 _refine_ls_number_parameters 767 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.60519(19) 0.07549(11) 0.54576(12) 0.0263(4) Uani 1 1 d . . . Li2 Li 0.77729(19) 0.03252(10) 0.47549(11) 0.0245(4) Uani 1 1 d . A . Li3 Li 0.72210(19) 0.16064(10) 0.47915(12) 0.0260(4) Uani 1 1 d . A . Li4 Li 0.56402(19) 0.08386(10) 0.40263(12) 0.0255(4) Uani 1 1 d . A . Li5 Li 0.4031(2) 0.83065(11) -0.03631(12) 0.0284(4) Uani 1 1 d . . . Li6 Li 0.22038(19) 0.78820(10) 0.02612(12) 0.0260(4) Uani 1 1 d . B . Li7 Li 0.27551(19) 0.91666(10) 0.02370(11) 0.0256(4) Uani 1 1 d . B . Li8 Li 0.42890(19) 0.84123(11) 0.10525(12) 0.0277(4) Uani 1 1 d . B . Si1 Si 0.86258(3) 0.175229(17) 0.642997(18) 0.02540(7) Uani 1 1 d . . . Si2 Si 0.43417(3) -0.046307(16) 0.396928(18) 0.02264(6) Uani 1 1 d . . . Si3 Si 0.43635(3) 0.239971(16) 0.40604(2) 0.02585(7) Uani 1 1 d . . . Si4 Si 0.90113(3) 0.145032(16) 0.364374(18) 0.02400(7) Uani 1 1 d . A . Si5 Si 0.15275(3) 0.929088(18) -0.143222(19) 0.02847(7) Uani 1 1 d . . . Si6 Si 0.56324(3) 0.710200(17) 0.116970(19) 0.02482(7) Uani 1 1 d . . . Si7 Si 0.55932(3) 0.998317(16) 0.099213(19) 0.02523(7) Uani 1 1 d . . . Si8 Si 0.08913(3) 0.904523(16) 0.132361(18) 0.02234(6) Uani 1 1 d . . . C4 C 0.65623(16) -0.03003(9) 0.68471(9) 0.0489(4) Uani 1 1 d D A . H4A H 0.6690 -0.0418 0.6357 0.073 Uiso 1 1 calc R . . H4B H 0.6595 -0.0729 0.7142 0.073 Uiso 1 1 calc R . . H4C H 0.7233 0.0021 0.7107 0.073 Uiso 1 1 calc R . . C3 C 0.52879(18) 0.00438(9) 0.67467(10) 0.0498(4) Uani 1 1 d D . . H3A H 0.5161 0.0171 0.7223 0.060 Uiso 0.786(4) 1 d PR A 1 H3B H 0.4622 -0.0272 0.6505 0.060 Uiso 0.786(4) 1 d PR A 1 H3C H 0.5288 0.0286 0.7200 0.060 Uiso 0.214(4) 1 d PR A 2 H3D H 0.4656 -0.0318 0.6680 0.060 Uiso 0.214(4) 1 d PR A 2 O1 O 0.52657(19) 0.06503(10) 0.63012(12) 0.0285(4) Uani 0.786(4) 1 d PD A 1 C2 C 0.43927(16) 0.11591(9) 0.64438(9) 0.0330(4) Uani 0.786(4) 1 d PD A 1 H2A H 0.4484 0.1598 0.6178 0.040 Uiso 0.786(4) 1 calc PR A 1 H2B H 0.4615 0.1264 0.6985 0.040 Uiso 0.786(4) 1 calc PR A 1 C1 C 0.30333(19) 0.09233(15) 0.62037(13) 0.0537(6) Uani 0.786(4) 1 d PD A 1 H1A H 0.2829 0.0776 0.5680 0.080 Uiso 0.786(4) 1 calc PR A 1 H1B H 0.2475 0.1311 0.6260 0.080 Uiso 0.786(4) 1 calc PR A 1 H1C H 0.2908 0.0528 0.6515 0.080 Uiso 0.786(4) 1 calc PR A 1 O1' O 0.4873(7) 0.0555(4) 0.6103(4) 0.0312(15) Uani 0.214(4) 1 d PD A 2 C2' C 0.3609(6) 0.0863(4) 0.5959(4) 0.046(2) Uani 0.214(4) 1 d PD A 2 H2C H 0.3049 0.0536 0.6141 0.055 Uiso 0.214(4) 1 calc PR A 2 H2D H 0.3260 0.0911 0.5413 0.055 Uiso 0.214(4) 1 calc PR A 2 C1' C 0.3555(8) 0.1570(5) 0.6315(5) 0.058(3) Uani 0.214(4) 1 d PD A 2 H1D H 0.3826 0.1522 0.6860 0.087 Uiso 0.214(4) 1 calc PR A 2 H1E H 0.2682 0.1749 0.6166 0.087 Uiso 0.214(4) 1 calc PR A 2 H1F H 0.4122 0.1896 0.6151 0.087 Uiso 0.214(4) 1 calc PR A 2 C13 C 0.58035(11) -0.01657(6) 0.46423(7) 0.0247(2) Uani 1 1 d . A . C14 C 0.43579(14) -0.13936(7) 0.36387(9) 0.0379(3) Uani 1 1 d . A . H14A H 0.5077 -0.1460 0.3419 0.057 Uiso 1 1 calc R . . H14B H 0.3561 -0.1493 0.3263 0.057 Uiso 1 1 calc R . . H14C H 0.4444 -0.1713 0.4063 0.057 Uiso 1 1 calc R . . C15 C 0.40345(17) 0.00948(8) 0.30996(8) 0.0465(4) Uani 1 1 d . A . H15A H 0.3770 0.0565 0.3210 0.070 Uiso 1 1 calc R . . H15B H 0.3360 -0.0119 0.2706 0.070 Uiso 1 1 calc R . . H15C H 0.4815 0.0128 0.2931 0.070 Uiso 1 1 calc R . . C16 C 0.29235(14) -0.03610(10) 0.43537(11) 0.0505(4) Uani 1 1 d . A . H16A H 0.3030 -0.0654 0.4800 0.076 Uiso 1 1 calc R . . H16B H 0.2156 -0.0506 0.3977 0.076 Uiso 1 1 calc R . . H16C H 0.2841 0.0131 0.4486 0.076 Uiso 1 1 calc R . . C21 C 0.75073(10) 0.10799(6) 0.37652(6) 0.0230(2) Uani 1 1 d . . . C24 C 0.89816(13) 0.24370(7) 0.36564(8) 0.0336(3) Uani 1 1 d . . . H24A H 0.8296 0.2607 0.3240 0.050 Uiso 1 1 calc R A . H24B H 0.9798 0.2619 0.3607 0.050 Uiso 1 1 calc R . . H24C H 0.8835 0.2599 0.4129 0.050 Uiso 1 1 calc R . . C23 C 1.04265(12) 0.11891(7) 0.44197(8) 0.0355(3) Uani 1 1 d . . . H23A H 1.0365 0.1409 0.4887 0.053 Uiso 1 1 calc R A . H23B H 1.1209 0.1344 0.4300 0.053 Uiso 1 1 calc R . . H23C H 1.0442 0.0678 0.4476 0.053 Uiso 1 1 calc R . . C22 C 0.93991(15) 0.11845(9) 0.27496(8) 0.0430(3) Uani 1 1 d . . . H22A H 0.9458 0.0673 0.2730 0.065 Uiso 1 1 calc R A . H22B H 1.0214 0.1392 0.2731 0.065 Uiso 1 1 calc R . . H22C H 0.8727 0.1350 0.2323 0.065 Uiso 1 1 calc R . . C5 C 0.81882(11) 0.09954(6) 0.57987(6) 0.0236(2) Uani 1 1 d . A . C7 C 0.74567(13) 0.19111(7) 0.69991(7) 0.0334(3) Uani 1 1 d . A . H7A H 0.6628 0.2035 0.6667 0.050 Uiso 1 1 calc R . . H7B H 0.7760 0.2296 0.7350 0.050 Uiso 1 1 calc R . . H7C H 0.7371 0.1485 0.7278 0.050 Uiso 1 1 calc R . . C8 C 0.86400(16) 0.25695(7) 0.58552(8) 0.0402(3) Uani 1 1 d . A . H8A H 0.9263 0.2514 0.5561 0.060 Uiso 1 1 calc R . . H8B H 0.8872 0.2974 0.6188 0.060 Uiso 1 1 calc R . . H8C H 0.7793 0.2644 0.5519 0.060 Uiso 1 1 calc R . . C33 C 0.18835(11) 0.85470(6) -0.07791(7) 0.0250(2) Uani 1 1 d . B . C35 C 0.15868(16) 1.01324(7) -0.08813(9) 0.0420(3) Uani 1 1 d . B . H35A H 0.0954 1.0112 -0.0590 0.063 Uiso 1 1 calc R . . H35B H 0.1400 1.0531 -0.1226 0.063 Uiso 1 1 calc R . . H35C H 0.2437 1.0189 -0.0543 0.063 Uiso 1 1 calc R . . C36 C 0.27160(14) 0.93747(8) -0.20049(8) 0.0382(3) Uani 1 1 d . B . H36A H 0.3571 0.9429 -0.1672 0.057 Uiso 1 1 calc R . . H36B H 0.2508 0.9786 -0.2331 0.057 Uiso 1 1 calc R . . H36C H 0.2688 0.8953 -0.2310 0.057 Uiso 1 1 calc R . . C34 C -0.00889(15) 0.92701(11) -0.21135(10) 0.0558(5) Uani 1 1 d . B . H34A H -0.0176 0.8841 -0.2412 0.084 Uiso 1 1 calc R . . H34B H -0.0186 0.9679 -0.2444 0.084 Uiso 1 1 calc R . . H34C H -0.0747 0.9280 -0.1840 0.084 Uiso 1 1 calc R . . C17 C 0.51245(11) 0.16910(6) 0.46940(7) 0.0262(2) Uani 1 1 d . A 1 C18 C 0.31103(13) 0.29051(7) 0.43761(9) 0.0389(3) Uani 1 1 d . A 1 H18A H 0.2460 0.2581 0.4456 0.058 Uiso 1 1 calc R A 1 H18B H 0.2715 0.3248 0.3993 0.058 Uiso 1 1 calc R A 1 H18C H 0.3504 0.3149 0.4844 0.058 Uiso 1 1 calc R A 1 C20 C 0.56010(14) 0.30455(7) 0.39355(10) 0.0410(3) Uani 1 1 d . A 1 H20A H 0.5994 0.3271 0.4415 0.061 Uiso 1 1 calc R A 1 H20B H 0.5198 0.3402 0.3571 0.061 Uiso 1 1 calc R A 1 H20C H 0.6255 0.2799 0.3756 0.061 Uiso 1 1 calc R A 1 C19 C 0.35189(14) 0.20605(8) 0.31066(8) 0.0390(3) Uani 1 1 d . A 1 H19A H 0.4129 0.1818 0.2888 0.059 Uiso 1 1 calc R A 1 H19B H 0.3141 0.2454 0.2785 0.059 Uiso 1 1 calc R A 1 H19C H 0.2848 0.1734 0.3151 0.059 Uiso 1 1 calc R A 1 C41 C 0.48490(12) 0.92552(6) 0.03839(7) 0.0278(2) Uani 1 1 d . B 1 C42 C 0.68468(13) 1.04765(7) 0.06592(9) 0.0376(3) Uani 1 1 d . B 1 H42A H 0.7508 1.0150 0.0600 0.056 Uiso 1 1 calc R B 1 H42B H 0.7228 1.0836 0.1027 0.056 Uiso 1 1 calc R B 1 H42C H 0.6455 1.0700 0.0179 0.056 Uiso 1 1 calc R B 1 C44 C 0.43700(14) 1.06435(7) 0.11020(9) 0.0370(3) Uani 1 1 d . B 1 H44A H 0.4007 1.0875 0.0622 0.055 Uiso 1 1 calc R B 1 H44B H 0.4773 1.0994 0.1474 0.055 Uiso 1 1 calc R B 1 H44C H 0.3693 1.0405 0.1267 0.055 Uiso 1 1 calc R B 1 C43 C 0.64263(15) 0.96380(8) 0.19422(8) 0.0430(3) Uani 1 1 d . B 1 H43A H 0.5813 0.9392 0.2156 0.065 Uiso 1 1 calc R B 1 H43B H 0.6801 1.0029 0.2268 0.065 Uiso 1 1 calc R B 1 H43C H 0.7100 0.9313 0.1898 0.065 Uiso 1 1 calc R B 1 C37 C 0.42058(11) 0.74006(6) 0.04684(7) 0.0264(2) Uani 1 1 d . B 1 C39 C 0.57861(17) 0.75910(8) 0.20768(8) 0.0465(4) Uani 1 1 d . B 1 H39A H 0.5958 0.8087 0.2006 0.070 Uiso 1 1 calc R B 1 H39B H 0.6488 0.7392 0.2465 0.070 Uiso 1 1 calc R B 1 H39C H 0.4992 0.7548 0.2229 0.070 Uiso 1 1 calc R B 1 C38 C 0.56318(15) 0.61457(7) 0.14173(8) 0.0401(3) Uani 1 1 d . B 1 H38A H 0.4900 0.6045 0.1617 0.060 Uiso 1 1 calc R B 1 H38B H 0.6420 0.6032 0.1794 0.060 Uiso 1 1 calc R B 1 H38C H 0.5575 0.5862 0.0969 0.060 Uiso 1 1 calc R B 1 C40 C 0.71111(14) 0.72675(11) 0.08668(10) 0.0537(4) Uani 1 1 d . B 1 H40A H 0.7049 0.7034 0.0388 0.081 Uiso 1 1 calc R B 1 H40B H 0.7846 0.7083 0.1243 0.081 Uiso 1 1 calc R B 1 H40C H 0.7216 0.7773 0.0810 0.081 Uiso 1 1 calc R B 1 O4 O 0.09581(8) 0.71240(4) 0.01492(5) 0.02742(17) Uani 1 1 d . B 1 C31 C 0.06350(13) 0.67456(7) 0.07466(8) 0.0339(3) Uani 1 1 d . B 1 H31A H -0.0256 0.6582 0.0575 0.041 Uiso 1 1 calc R B 1 H31B H 0.0692 0.7067 0.1173 0.041 Uiso 1 1 calc R B 1 C30 C 0.05000(12) 0.68045(7) -0.05734(7) 0.0309(2) Uani 1 1 d . B 1 H30A H 0.0535 0.6288 -0.0517 0.037 Uiso 1 1 calc R B 1 H30B H 0.1064 0.6938 -0.0893 0.037 Uiso 1 1 calc R B 1 C29 C -0.08436(14) 0.70217(9) -0.09507(10) 0.0473(4) Uani 1 1 d . B 1 H29A H -0.1413 0.6867 -0.0650 0.071 Uiso 1 1 calc R B 1 H29B H -0.1107 0.6807 -0.1447 0.071 Uiso 1 1 calc R B 1 H29C H -0.0885 0.7533 -0.1001 0.071 Uiso 1 1 calc R B 1 C32 C 0.14896(15) 0.61241(8) 0.10075(9) 0.0449(3) Uani 1 1 d . B 1 H32A H 0.1440 0.5804 0.0588 0.067 Uiso 1 1 calc R B 1 H32B H 0.1215 0.5879 0.1404 0.067 Uiso 1 1 calc R B 1 H32C H 0.2369 0.6285 0.1201 0.067 Uiso 1 1 calc R B 1 C45 C 0.23926(11) 0.86364(6) 0.12483(7) 0.0237(2) Uani 1 1 d . B 1 C48 C 0.09559(12) 1.00277(7) 0.12622(8) 0.0313(3) Uani 1 1 d . B 1 H48A H 0.1648 1.0206 0.1670 0.047 Uiso 1 1 calc R B 1 H48B H 0.0146 1.0227 0.1303 0.047 Uiso 1 1 calc R B 1 H48C H 0.1107 1.0162 0.0782 0.047 Uiso 1 1 calc R B 1 C47 C -0.04966(12) 0.87626(8) 0.05468(9) 0.0391(3) Uani 1 1 d . B 1 H47A H -0.0403 0.8951 0.0072 0.059 Uiso 1 1 calc R B 1 H47B H -0.1286 0.8939 0.0641 0.059 Uiso 1 1 calc R B 1 H47C H -0.0526 0.8250 0.0522 0.059 Uiso 1 1 calc R B 1 C46 C 0.04419(14) 0.88515(8) 0.22177(8) 0.0407(3) Uani 1 1 d . B 1 H46A H 0.0302 0.8347 0.2254 0.061 Uiso 1 1 calc R B 1 H46B H -0.0340 0.9105 0.2221 0.061 Uiso 1 1 calc R B 1 H46C H 0.1130 0.9002 0.2644 0.061 Uiso 1 1 calc R B 1 C6 C 1.02346(14) 0.16940(10) 0.71149(9) 0.0481(4) Uani 1 1 d . A 1 H6A H 1.0267 0.1278 0.7430 0.072 Uiso 1 1 calc R A 1 H6B H 1.0382 0.2114 0.7429 0.072 Uiso 1 1 calc R A 1 H6C H 1.0893 0.1659 0.6843 0.072 Uiso 1 1 calc R A 1 C28 C 0.37128(17) 0.73223(9) -0.17771(9) 0.0513(4) Uani 1 1 d . B 1 H28A H 0.3674 0.7088 -0.1313 0.077 Uiso 1 1 calc R B 1 H28B H 0.3630 0.6973 -0.2174 0.077 Uiso 1 1 calc R B 1 H28C H 0.3017 0.7663 -0.1920 0.077 Uiso 1 1 calc R B 1 C27 C 0.49512(19) 0.76911(10) -0.16616(9) 0.0543(4) Uani 1 1 d . B 1 H27A H 0.5618 0.7353 -0.1610 0.065 Uiso 0.740(4) 1 d PR C 1 H27B H 0.4938 0.7975 -0.2092 0.065 Uiso 0.740(4) 1 d PR C 1 H27C H 0.5084 0.7850 -0.2127 0.065 Uiso 0.260(4) 1 d PR C 2 H27D H 0.5646 0.7398 -0.1413 0.065 Uiso 0.260(4) 1 d PR C 2 O3 O 0.52315(18) 0.81434(11) -0.09971(11) 0.0284(4) Uani 0.740(4) 1 d PD B 1 C26 C 0.64747(17) 0.84616(12) -0.08276(11) 0.0377(5) Uani 0.740(4) 1 d PD B 1 H26A H 0.7075 0.8137 -0.0977 0.045 Uiso 0.740(4) 1 calc PR C 1 H26B H 0.6776 0.8534 -0.0282 0.045 Uiso 0.740(4) 1 calc PR C 1 C25 C 0.6488(3) 0.91641(19) -0.12225(16) 0.0688(10) Uani 0.740(4) 1 d PD B 1 H25A H 0.6168 0.9099 -0.1763 0.103 Uiso 0.740(4) 1 calc PR C 1 H25B H 0.7360 0.9345 -0.1108 0.103 Uiso 0.740(4) 1 calc PR C 1 H25C H 0.5944 0.9499 -0.1049 0.103 Uiso 0.740(4) 1 calc PR C 1 O3' O 0.4816(7) 0.8236(3) -0.1235(4) 0.0378(13) Uani 0.260(4) 1 d PD B 2 C26' C 0.5606(6) 0.8769(4) -0.1403(4) 0.0483(17) Uani 0.260(4) 1 d PD B 2 H26C H 0.5495 0.9195 -0.1122 0.058 Uiso 0.260(4) 1 calc PR C 2 H26D H 0.5298 0.8881 -0.1941 0.058 Uiso 0.260(4) 1 calc PR C 2 C25' C 0.6945(6) 0.8618(5) -0.1243(4) 0.065(3) Uani 0.260(4) 1 d PD B 2 H25D H 0.7222 0.8386 -0.0756 0.097 Uiso 0.260(4) 1 calc PR C 2 H25E H 0.7419 0.9056 -0.1234 0.097 Uiso 0.260(4) 1 calc PR C 2 H25F H 0.7106 0.8309 -0.1630 0.097 Uiso 0.260(4) 1 calc PR C 2 C9 C 1.07582(15) -0.06154(9) 0.58428(9) 0.0455(3) Uani 1 1 d . . . H9A H 1.1327 -0.0707 0.5521 0.068 Uiso 1 1 calc R . . H9B H 1.1035 -0.0891 0.6302 0.068 Uiso 1 1 calc R . . H9C H 1.0784 -0.0116 0.5968 0.068 Uiso 1 1 calc R . . C10 C 0.94233(12) -0.08185(7) 0.54400(8) 0.0323(3) Uani 1 1 d . A . H10A H 0.9395 -0.1327 0.5332 0.039 Uiso 1 1 calc R . . H10B H 0.8853 -0.0726 0.5767 0.039 Uiso 1 1 calc R . . O2 O 0.89691(8) -0.04371(4) 0.47497(5) 0.02673(16) Uani 1 1 d . . . C11 C 0.92455(13) -0.07598(7) 0.41086(8) 0.0329(3) Uani 1 1 d . A . H11A H 1.0107 -0.0969 0.4258 0.040 Uiso 1 1 calc R . . H11B H 0.9248 -0.0395 0.3729 0.040 Uiso 1 1 calc R . . C12 C 0.82935(14) -0.13228(8) 0.37646(9) 0.0423(3) Uani 1 1 d . . . H12A H 0.8277 -0.1682 0.4140 0.063 Uiso 1 1 calc R A . H12B H 0.8541 -0.1538 0.3343 0.063 Uiso 1 1 calc R . . H12C H 0.7446 -0.1113 0.3588 0.063 Uiso 1 1 calc R . . H13B H 0.6430(18) -0.0468(10) 0.4571(10) 0.050(5) Uiso 1 1 d . . . H13A H 0.5683(16) -0.0307(9) 0.5148(10) 0.049(5) Uiso 1 1 d . . . H5B H 0.8895(17) 0.0889(10) 0.5632(9) 0.045(5) Uiso 1 1 d . . . H5A H 0.8168(16) 0.0644(9) 0.6107(9) 0.036(4) Uiso 1 1 d . . . H17A H 0.5484(16) 0.1921(9) 0.5180(10) 0.042(5) Uiso 1 1 d . . . H17B H 0.4420(17) 0.1401(10) 0.4764(9) 0.045(5) Uiso 1 1 d . . . H41A H 0.4532(18) 0.9433(10) -0.0138(11) 0.052(5) Uiso 1 1 d . . . H41B H 0.5584(19) 0.8954(11) 0.0382(10) 0.059(6) Uiso 1 1 d . . . H45A H 0.3081(16) 0.8869(9) 0.1669(9) 0.040(4) Uiso 1 1 d . . . H37A H 0.4345(18) 0.7219(10) -0.0011(11) 0.057(5) Uiso 1 1 d . . . H37B H 0.3574(18) 0.7107(11) 0.0541(10) 0.053(5) Uiso 1 1 d . . . H33B H 0.1099(16) 0.8472(9) -0.0649(9) 0.040(4) Uiso 1 1 d . . . H33A H 0.1872(17) 0.8175(10) -0.1069(10) 0.048(5) Uiso 1 1 d . . . H21B H 0.7434(19) 0.0563(10) 0.3594(10) 0.053(5) Uiso 1 1 d . . . H21A H 0.6805(17) 0.1352(9) 0.3386(9) 0.044(5) Uiso 1 1 d . . . H45B H 0.238(2) 0.8149(12) 0.1413(11) 0.068(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.0245(9) 0.0279(10) 0.0288(10) 0.0014(8) 0.0112(8) 0.0029(7) Li2 0.0242(9) 0.0221(9) 0.0270(10) -0.0026(7) 0.0063(8) 0.0016(7) Li3 0.0258(9) 0.0229(9) 0.0297(10) -0.0007(7) 0.0078(8) -0.0008(7) Li4 0.0223(9) 0.0248(9) 0.0296(10) 0.0015(7) 0.0071(8) -0.0001(7) Li5 0.0257(10) 0.0297(10) 0.0325(10) -0.0038(8) 0.0123(8) -0.0026(8) Li6 0.0230(9) 0.0237(9) 0.0312(10) 0.0002(7) 0.0070(8) -0.0023(7) Li7 0.0236(9) 0.0227(9) 0.0315(10) -0.0006(8) 0.0089(8) -0.0009(7) Li8 0.0232(9) 0.0254(10) 0.0331(11) -0.0025(8) 0.0049(8) -0.0001(8) Si1 0.02650(15) 0.02482(15) 0.02400(15) -0.00524(12) 0.00493(12) -0.00115(12) Si2 0.01918(14) 0.02166(14) 0.02727(15) -0.00251(12) 0.00638(11) -0.00300(11) Si3 0.02182(15) 0.02087(15) 0.03529(17) 0.00195(12) 0.00815(13) 0.00391(11) Si4 0.02059(14) 0.02528(16) 0.02754(16) -0.00052(12) 0.00877(12) -0.00287(11) Si5 0.02819(16) 0.03117(17) 0.02507(16) 0.00451(13) 0.00515(13) 0.00030(13) Si6 0.02211(15) 0.02393(15) 0.02874(15) 0.00182(12) 0.00717(12) 0.00422(11) Si7 0.02119(15) 0.02161(15) 0.03227(17) -0.00066(12) 0.00580(12) -0.00516(11) Si8 0.01867(14) 0.02312(15) 0.02660(15) 0.00125(11) 0.00833(12) 0.00208(11) C4 0.0505(9) 0.0525(9) 0.0430(8) 0.0132(7) 0.0106(7) -0.0001(7) C3 0.0629(11) 0.0456(8) 0.0500(9) 0.0107(7) 0.0311(8) -0.0004(8) O1 0.0292(9) 0.0281(8) 0.0323(10) -0.0014(6) 0.0155(7) -0.0004(6) C2 0.0302(8) 0.0408(9) 0.0316(8) -0.0042(7) 0.0145(7) 0.0053(7) C1 0.0289(10) 0.0812(17) 0.0512(12) -0.0077(12) 0.0109(9) 0.0034(10) O1' 0.035(4) 0.028(2) 0.036(4) -0.008(2) 0.018(3) -0.017(2) C2' 0.025(3) 0.067(5) 0.055(4) 0.002(4) 0.028(3) -0.004(3) C1' 0.035(4) 0.082(7) 0.057(5) -0.023(4) 0.012(3) 0.008(4) C13 0.0214(5) 0.0212(5) 0.0301(6) -0.0020(4) 0.0043(4) -0.0010(4) C14 0.0359(7) 0.0273(6) 0.0469(8) -0.0103(5) 0.0043(6) -0.0046(5) C15 0.0565(10) 0.0399(8) 0.0336(7) 0.0042(6) -0.0052(7) -0.0131(7) C16 0.0284(7) 0.0589(10) 0.0708(11) -0.0126(8) 0.0250(7) -0.0056(7) C21 0.0188(5) 0.0257(5) 0.0247(5) 0.0002(4) 0.0059(4) -0.0013(4) C24 0.0330(6) 0.0272(6) 0.0393(7) 0.0015(5) 0.0071(5) -0.0046(5) C23 0.0203(5) 0.0380(7) 0.0472(8) 0.0068(6) 0.0072(5) -0.0019(5) C22 0.0406(8) 0.0530(9) 0.0430(8) -0.0101(7) 0.0245(6) -0.0092(7) C5 0.0238(5) 0.0222(5) 0.0249(5) -0.0036(4) 0.0065(4) 0.0003(4) C7 0.0409(7) 0.0307(6) 0.0310(6) -0.0047(5) 0.0135(5) 0.0046(5) C8 0.0569(9) 0.0285(6) 0.0386(7) -0.0058(5) 0.0185(7) -0.0117(6) C33 0.0243(5) 0.0244(5) 0.0264(6) 0.0000(4) 0.0068(4) -0.0020(4) C35 0.0567(9) 0.0304(7) 0.0418(8) 0.0053(6) 0.0180(7) 0.0087(6) C36 0.0441(8) 0.0422(7) 0.0310(6) 0.0010(5) 0.0148(6) -0.0087(6) C34 0.0369(8) 0.0772(13) 0.0447(9) 0.0193(9) -0.0047(7) -0.0004(8) C17 0.0249(5) 0.0228(5) 0.0321(6) 0.0023(4) 0.0097(5) 0.0048(4) C18 0.0314(7) 0.0291(6) 0.0576(9) -0.0028(6) 0.0140(6) 0.0097(5) C20 0.0334(7) 0.0309(6) 0.0594(9) 0.0101(6) 0.0133(7) -0.0012(5) C19 0.0418(8) 0.0389(7) 0.0344(7) 0.0031(6) 0.0065(6) 0.0021(6) C41 0.0234(5) 0.0243(5) 0.0366(6) -0.0046(5) 0.0095(5) -0.0052(4) C42 0.0287(6) 0.0306(6) 0.0544(9) 0.0013(6) 0.0121(6) -0.0097(5) C44 0.0342(7) 0.0303(6) 0.0486(8) -0.0056(6) 0.0146(6) -0.0011(5) C43 0.0441(8) 0.0415(8) 0.0376(7) 0.0036(6) 0.0000(6) -0.0059(6) C37 0.0211(5) 0.0228(5) 0.0347(6) 0.0007(4) 0.0060(4) 0.0022(4) C39 0.0578(10) 0.0379(7) 0.0356(7) -0.0067(6) -0.0029(7) 0.0108(7) C38 0.0499(8) 0.0280(6) 0.0413(8) 0.0054(5) 0.0099(6) 0.0103(6) C40 0.0228(7) 0.0738(12) 0.0666(11) 0.0230(9) 0.0153(7) 0.0094(7) O4 0.0255(4) 0.0241(4) 0.0348(4) -0.0044(3) 0.0115(3) -0.0064(3) C31 0.0335(6) 0.0308(6) 0.0423(7) -0.0007(5) 0.0188(5) -0.0056(5) C30 0.0274(6) 0.0265(5) 0.0391(7) -0.0085(5) 0.0091(5) -0.0030(5) C29 0.0315(7) 0.0490(9) 0.0545(9) -0.0090(7) -0.0015(6) 0.0015(6) C32 0.0381(7) 0.0452(8) 0.0530(9) 0.0138(7) 0.0145(7) 0.0007(6) C45 0.0193(5) 0.0252(5) 0.0265(5) -0.0014(4) 0.0060(4) 0.0027(4) C48 0.0297(6) 0.0260(6) 0.0396(7) 0.0040(5) 0.0111(5) 0.0039(5) C47 0.0194(6) 0.0459(8) 0.0499(8) -0.0125(6) 0.0052(5) 0.0016(5) C46 0.0381(7) 0.0475(8) 0.0440(8) 0.0138(6) 0.0243(6) 0.0103(6) C6 0.0340(7) 0.0615(10) 0.0422(8) -0.0208(7) -0.0021(6) 0.0027(7) C28 0.0586(10) 0.0509(9) 0.0377(8) -0.0144(7) 0.0007(7) 0.0182(8) C27 0.0734(12) 0.0554(10) 0.0419(8) -0.0083(7) 0.0292(8) 0.0127(9) O3 0.0253(8) 0.0374(8) 0.0229(9) -0.0010(6) 0.0071(6) 0.0067(6) C26 0.0222(8) 0.0587(12) 0.0337(10) -0.0009(8) 0.0100(7) 0.0059(8) C25 0.0470(14) 0.102(2) 0.0587(15) 0.0272(16) 0.0157(12) -0.0236(15) O3' 0.048(4) 0.038(3) 0.037(3) -0.003(2) 0.028(3) -0.002(3) C26' 0.038(3) 0.062(4) 0.049(4) 0.012(3) 0.018(3) -0.003(3) C25' 0.037(3) 0.103(7) 0.061(5) -0.035(5) 0.024(3) -0.011(4) C9 0.0354(7) 0.0496(9) 0.0464(8) 0.0049(7) 0.0011(6) -0.0024(6) C10 0.0288(6) 0.0270(6) 0.0411(7) 0.0066(5) 0.0089(5) -0.0002(5) O2 0.0246(4) 0.0237(4) 0.0323(4) 0.0014(3) 0.0081(3) 0.0044(3) C11 0.0321(6) 0.0278(6) 0.0444(7) -0.0034(5) 0.0197(6) 0.0031(5) C12 0.0343(7) 0.0494(8) 0.0442(8) -0.0142(7) 0.0118(6) -0.0040(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O1 1.978(3) . ? Li1 O1' 2.005(8) . ? Li1 C13 2.287(3) . ? Li1 C5 2.292(3) . ? Li1 C17 2.340(3) . ? Li1 Li3 2.569(3) . ? Li1 Li4 2.580(3) . ? Li1 Li2 2.672(3) . ? Li1 H13A 2.116(18) . ? Li1 H5A 2.315(17) . ? Li1 H17A 2.330(17) . ? Li1 H17B 2.268(17) . ? Li2 O2 1.953(2) . ? Li2 C5 2.266(3) . ? Li2 C21 2.291(3) . ? Li2 C13 2.298(3) . ? Li2 Li3 2.523(3) . ? Li2 Li4 2.559(3) . ? Li2 H13B 2.070(19) . ? Li2 H5B 2.066(17) . ? Li2 H21B 2.137(19) . ? Li3 C5 2.222(3) . ? Li3 C21 2.244(3) . ? Li3 C17 2.247(3) . ? Li3 Li4 2.420(3) . ? Li3 H17A 2.271(17) . ? Li4 C17 2.203(3) . ? Li4 C13 2.214(3) . ? Li4 C21 2.255(3) . ? Li4 H21A 2.181(17) . ? Li5 O3 1.996(3) . ? Li5 O3' 2.019(6) . ? Li5 C37 2.291(3) . ? Li5 C33 2.309(3) . ? Li5 C41 2.313(3) . ? Li5 Li8 2.575(3) . ? Li5 Li7 2.580(3) . ? Li5 Li6 2.672(3) . ? Li5 H41A 2.231(19) . ? Li5 H41B 2.25(2) . ? Li5 H37A 2.18(2) . ? Li6 O4 1.956(2) . ? Li6 C33 2.259(3) . ? Li6 C45 2.296(3) . ? Li6 C37 2.303(3) . ? Li6 Li7 2.527(3) . ? Li6 Li8 2.569(3) . ? Li6 H37B 2.068(19) . ? Li6 H33B 2.124(17) . ? Li6 H45B 2.16(2) . ? Li7 C33 2.219(3) . ? Li7 C41 2.230(3) . ? Li7 C45 2.254(3) . ? Li7 Li8 2.416(3) . ? Li7 H41A 2.275(19) . ? Li8 C37 2.204(3) . ? Li8 C41 2.211(3) . ? Li8 C45 2.227(3) . ? Li8 H45A 2.139(16) . ? Si1 C5 1.8422(14) . ? Si1 C7 1.8761(16) . ? Si1 C6 1.8810(18) . ? Si1 C8 1.8911(17) . ? Si2 C13 1.8387(15) . ? Si2 C16 1.8702(17) . ? Si2 C14 1.8798(17) . ? Si2 C15 1.8884(18) . ? Si3 C17 1.8414(14) . ? Si3 C18 1.8831(15) . ? Si3 C20 1.8834(16) . ? Si3 C19 1.8839(18) . ? Si4 C21 1.8493(15) . ? Si4 C23 1.8820(16) . ? Si4 C24 1.8832(18) . ? Si4 C22 1.8834(17) . ? Si5 C33 1.8407(15) . ? Si5 C36 1.8808(16) . ? Si5 C34 1.8814(18) . ? Si5 C35 1.8952(18) . ? Si6 C37 1.8383(15) . ? Si6 C40 1.8635(18) . ? Si6 C38 1.8817(18) . ? Si6 C39 1.8927(18) . ? Si7 C41 1.8395(15) . ? Si7 C43 1.8793(18) . ? Si7 C44 1.8818(17) . ? Si7 C42 1.8880(15) . ? Si8 C45 1.8480(15) . ? Si8 C47 1.8760(16) . ? Si8 C48 1.8805(18) . ? Si8 C46 1.8828(17) . ? C4 C3 1.502(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C3 O1 1.418(3) . ? C3 O1' 1.516(8) . ? C3 H3A 0.9599 . ? C3 H3B 0.9599 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? O1 C2 1.430(2) . ? C2 C1 1.499(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O1' C2' 1.456(9) . ? C2' C1' 1.509(10) . ? C2' H2C 0.9900 . ? C2' H2D 0.9900 . ? C1' H1D 0.9800 . ? C1' H1E 0.9800 . ? C1' H1F 0.9800 . ? C13 H13B 0.927(19) . ? C13 H13A 1.017(18) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 H21B 1.033(19) . ? C21 H21A 1.035(18) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C5 H5B 0.922(18) . ? C5 H5A 0.885(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C33 H33B 0.956(17) . ? C33 H33A 0.889(19) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C17 H17A 0.988(18) . ? C17 H17B 0.981(18) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C41 H41A 0.999(19) . ? C41 H41B 0.99(2) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C37 H37A 1.001(19) . ? C37 H37B 0.923(19) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O4 C30 1.4385(17) . ? O4 C31 1.4401(16) . ? C31 C32 1.507(2) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C30 C29 1.506(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C45 H45A 1.031(17) . ? C45 H45B 0.98(2) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C28 C27 1.486(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 O3 1.470(3) . ? C27 H27A 0.9565 . ? C27 H27B 0.9610 . ? C27 H27C 0.9597 . ? C27 H27D 0.9576 . ? O3 C26 1.441(3) . ? C26 C25 1.529(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O3' C26' 1.417(8) . ? C26' C25' 1.439(9) . ? C26' H26C 0.9900 . ? C26' H26D 0.9900 . ? C25' H25D 0.9800 . ? C25' H25E 0.9800 . ? C25' H25F 0.9800 . ? C9 C10 1.502(2) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 O2 1.4439(17) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O2 C11 1.4382(16) . ? C11 C12 1.514(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 O1' 14.96(17) . . ? O1 Li1 C13 116.36(12) . . ? O1' Li1 C13 105.3(2) . . ? O1 Li1 C5 114.69(12) . . ? O1' Li1 C5 129.3(2) . . ? C13 Li1 C5 105.90(9) . . ? O1 Li1 C17 110.40(11) . . ? O1' Li1 C17 105.3(2) . . ? C13 Li1 C17 103.16(10) . . ? C5 Li1 C17 105.17(9) . . ? O1 Li1 Li3 144.46(12) . . ? O1' Li1 Li3 151.7(2) . . ? C13 Li1 Li3 98.99(10) . . ? C5 Li1 Li3 54.04(7) . . ? C17 Li1 Li3 54.25(8) . . ? O1 Li1 Li4 145.54(13) . . ? O1' Li1 Li4 131.2(2) . . ? C13 Li1 Li4 53.72(8) . . ? C5 Li1 Li4 99.49(9) . . ? C17 Li1 Li4 52.94(7) . . ? Li3 Li1 Li4 56.06(8) . . ? O1 Li1 Li2 148.88(12) . . ? O1' Li1 Li2 150.5(2) . . ? C13 Li1 Li2 54.54(7) . . ? C5 Li1 Li2 53.64(7) . . ? C17 Li1 Li2 100.71(9) . . ? Li3 Li1 Li2 57.50(8) . . ? Li4 Li1 Li2 58.27(8) . . ? O1 Li1 H13A 91.6(5) . . ? O1' Li1 H13A 82.7(5) . . ? C13 Li1 H13A 26.3(5) . . ? C5 Li1 H13A 112.0(5) . . ? C17 Li1 H13A 123.0(5) . . ? Li3 Li1 H13A 123.9(5) . . ? Li4 Li1 H13A 79.1(5) . . ? Li2 Li1 H13A 71.4(5) . . ? O1 Li1 H5A 98.9(4) . . ? O1' Li1 H5A 112.1(5) . . ? C13 Li1 H5A 101.8(4) . . ? C5 Li1 H5A 22.1(4) . . ? C17 Li1 H5A 126.8(4) . . ? Li3 Li1 H5A 76.0(4) . . ? Li4 Li1 H5A 115.1(4) . . ? Li2 Li1 H5A 59.8(4) . . ? H13A Li1 H5A 98.4(6) . . ? O1 Li1 H17A 97.3(4) . . ? O1' Li1 H17A 98.0(5) . . ? C13 Li1 H17A 127.4(4) . . ? C5 Li1 H17A 93.5(4) . . ? C17 Li1 H17A 24.4(4) . . ? Li3 Li1 H17A 55.0(4) . . ? Li4 Li1 H17A 75.4(4) . . ? Li2 Li1 H17A 111.4(4) . . ? H13A Li1 H17A 146.5(6) . . ? H5A Li1 H17A 111.9(6) . . ? O1 Li1 H17B 93.9(4) . . ? O1' Li1 H17B 85.1(5) . . ? C13 Li1 H17B 95.8(5) . . ? C5 Li1 H17B 129.5(5) . . ? C17 Li1 H17B 24.5(5) . . ? Li3 Li1 H17B 78.2(5) . . ? Li4 Li1 H17B 58.7(4) . . ? Li2 Li1 H17B 115.8(4) . . ? H13A Li1 H17B 107.5(7) . . ? H5A Li1 H17B 150.7(6) . . ? H17A Li1 H17B 39.8(6) . . ? O2 Li2 C5 116.03(11) . . ? O2 Li2 C21 114.20(10) . . ? C5 Li2 C21 106.58(10) . . ? O2 Li2 C13 107.63(11) . . ? C5 Li2 C13 106.41(9) . . ? C21 Li2 C13 105.20(9) . . ? O2 Li2 Li3 152.29(11) . . ? C5 Li2 Li3 54.98(7) . . ? C21 Li2 Li3 55.32(8) . . ? C13 Li2 Li3 100.05(9) . . ? O2 Li2 Li4 142.82(11) . . ? C5 Li2 Li4 100.83(9) . . ? C21 Li2 Li4 55.08(7) . . ? C13 Li2 Li4 53.93(8) . . ? Li3 Li2 Li4 56.87(8) . . ? O2 Li2 Li1 141.52(11) . . ? C5 Li2 Li1 54.56(7) . . ? C21 Li2 Li1 103.82(9) . . ? C13 Li2 Li1 54.17(8) . . ? Li3 Li2 Li1 59.19(7) . . ? Li4 Li2 Li1 59.05(9) . . ? O2 Li2 H13B 84.1(5) . . ? C5 Li2 H13B 121.9(5) . . ? C21 Li2 H13B 113.0(5) . . ? C13 Li2 H13B 23.8(5) . . ? Li3 Li2 H13B 123.4(5) . . ? Li4 Li2 H13B 71.8(5) . . ? Li1 Li2 H13B 75.5(5) . . ? O2 Li2 H5B 97.7(5) . . ? C5 Li2 H5B 24.0(5) . . ? C21 Li2 H5B 103.3(5) . . ? C13 Li2 H5B 129.1(5) . . ? Li3 Li2 H5B 64.5(5) . . ? Li4 Li2 H5B 119.1(5) . . ? Li1 Li2 H5B 78.6(5) . . ? H13B Li2 H5B 139.3(7) . . ? O2 Li2 H21B 95.4(5) . . ? C5 Li2 H21B 133.2(5) . . ? C21 Li2 H21B 26.7(5) . . ? C13 Li2 H21B 94.7(5) . . ? Li3 Li2 H21B 80.9(5) . . ? Li4 Li2 H21B 59.4(5) . . ? Li1 Li2 H21B 117.8(5) . . ? H13B Li2 H21B 93.4(7) . . ? H5B Li2 H21B 126.5(7) . . ? C5 Li3 C21 109.78(10) . . ? C5 Li3 C17 110.81(10) . . ? C21 Li3 C17 108.97(10) . . ? C5 Li3 Li4 106.57(10) . . ? C21 Li3 Li4 57.68(8) . . ? C17 Li3 Li4 56.19(8) . . ? C5 Li3 Li2 56.62(8) . . ? C21 Li3 Li2 57.11(7) . . ? C17 Li3 Li2 108.14(9) . . ? Li4 Li3 Li2 62.32(9) . . ? C5 Li3 Li1 56.61(8) . . ? C21 Li3 Li1 108.63(10) . . ? C17 Li3 Li1 57.67(7) . . ? Li4 Li3 Li1 62.20(9) . . ? Li2 Li3 Li1 63.32(9) . . ? C5 Li3 H17A 97.1(4) . . ? C21 Li3 H17A 134.2(5) . . ? C17 Li3 H17A 25.2(4) . . ? Li4 Li3 H17A 79.8(5) . . ? Li2 Li3 H17A 119.2(4) . . ? Li1 Li3 H17A 57.2(4) . . ? C17 Li4 C13 110.31(11) . . ? C17 Li4 C21 110.17(10) . . ? C13 Li4 C21 109.34(9) . . ? C17 Li4 Li3 57.94(8) . . ? C13 Li4 Li3 105.77(11) . . ? C21 Li4 Li3 57.25(8) . . ? C17 Li4 Li2 108.31(10) . . ? C13 Li4 Li2 57.02(7) . . ? C21 Li4 Li2 56.43(8) . . ? Li3 Li4 Li2 60.82(9) . . ? C17 Li4 Li1 57.93(8) . . ? C13 Li4 Li1 56.38(8) . . ? C21 Li4 Li1 107.92(10) . . ? Li3 Li4 Li1 61.74(9) . . ? Li2 Li4 Li1 62.68(8) . . ? C17 Li4 H21A 104.0(5) . . ? C13 Li4 H21A 133.6(5) . . ? C21 Li4 H21A 26.9(5) . . ? Li3 Li4 H21A 67.8(5) . . ? Li2 Li4 H21A 83.3(5) . . ? Li1 Li4 H21A 128.1(5) . . ? O3 Li5 O3' 16.37(18) . . ? O3 Li5 C37 109.01(12) . . ? O3' Li5 C37 120.7(2) . . ? O3 Li5 C33 126.48(13) . . ? O3' Li5 C33 110.3(2) . . ? C37 Li5 C33 105.99(9) . . ? O3 Li5 C41 105.40(12) . . ? O3' Li5 C41 110.8(2) . . ? C37 Li5 C41 103.62(11) . . ? C33 Li5 C41 104.11(10) . . ? O3 Li5 Li8 134.24(13) . . ? O3' Li5 Li8 149.8(2) . . ? C37 Li5 Li8 53.48(8) . . ? C33 Li5 Li8 99.14(9) . . ? C41 Li5 Li8 53.46(7) . . ? O3 Li5 Li7 149.39(13) . . ? O3' Li5 Li7 140.7(2) . . ? C37 Li5 Li7 98.62(10) . . ? C33 Li5 Li7 53.62(8) . . ? C41 Li5 Li7 53.89(8) . . ? Li8 Li5 Li7 55.89(8) . . ? O3 Li5 Li6 151.90(13) . . ? O3' Li5 Li6 147.5(2) . . ? C37 Li5 Li6 54.64(7) . . ? C33 Li5 Li6 53.35(8) . . ? C41 Li5 Li6 101.07(10) . . ? Li8 Li5 Li6 58.60(8) . . ? Li7 Li5 Li6 57.47(8) . . ? O3 Li5 H41A 95.5(5) . . ? O3' Li5 H41A 94.6(5) . . ? C37 Li5 H41A 128.9(5) . . ? C33 Li5 H41A 92.8(5) . . ? C41 Li5 H41A 25.3(5) . . ? Li8 Li5 H41A 77.1(5) . . ? Li7 Li5 H41A 55.9(5) . . ? Li6 Li5 H41A 112.6(5) . . ? O3 Li5 H41B 86.8(5) . . ? O3' Li5 H41B 97.0(5) . . ? C37 Li5 H41B 94.7(5) . . ? C33 Li5 H41B 129.0(5) . . ? C41 Li5 H41B 24.9(5) . . ? Li8 Li5 H41B 57.7(5) . . ? Li7 Li5 H41B 77.8(5) . . ? Li6 Li5 H41B 115.1(5) . . ? H41A Li5 H41B 41.3(7) . . ? O3 Li5 H37A 87.3(5) . . ? O3' Li5 H37A 96.4(5) . . ? C37 Li5 H37A 25.7(5) . . ? C33 Li5 H37A 110.9(5) . . ? C41 Li5 H37A 124.1(5) . . ? Li8 Li5 H37A 78.5(5) . . ? Li7 Li5 H37A 122.5(5) . . ? Li6 Li5 H37A 70.0(5) . . ? H41A Li5 H37A 148.3(7) . . ? H41B Li5 H37A 107.7(7) . . ? O4 Li6 C33 112.04(11) . . ? O4 Li6 C45 117.69(10) . . ? C33 Li6 C45 106.91(10) . . ? O4 Li6 C37 108.80(11) . . ? C33 Li6 C37 107.24(9) . . ? C45 Li6 C37 103.40(9) . . ? O4 Li6 Li7 151.24(12) . . ? C33 Li6 Li7 54.89(8) . . ? C45 Li6 Li7 55.48(8) . . ? C37 Li6 Li7 99.86(9) . . ? O4 Li6 Li8 146.83(12) . . ? C33 Li6 Li8 100.64(10) . . ? C45 Li6 Li8 54.15(7) . . ? C37 Li6 Li8 53.45(8) . . ? Li7 Li6 Li8 56.60(8) . . ? O4 Li6 Li5 138.66(11) . . ? C33 Li6 Li5 55.06(8) . . ? C45 Li6 Li5 103.44(10) . . ? C37 Li6 Li5 54.23(8) . . ? Li7 Li6 Li5 59.44(8) . . ? Li8 Li6 Li5 58.80(9) . . ? O4 Li6 H37B 86.1(6) . . ? C33 Li6 H37B 123.9(5) . . ? C45 Li6 H37B 109.8(5) . . ? C37 Li6 H37B 23.6(5) . . ? Li7 Li6 H37B 122.6(6) . . ? Li8 Li6 H37B 70.5(5) . . ? Li5 Li6 H37B 75.9(5) . . ? O4 Li6 H33B 94.2(5) . . ? C33 Li6 H33B 24.9(5) . . ? C45 Li6 H33B 102.5(5) . . ? C37 Li6 H33B 131.3(5) . . ? Li7 Li6 H33B 63.9(5) . . ? Li8 Li6 H33B 118.6(5) . . ? Li5 Li6 H33B 80.0(5) . . ? H37B Li6 H33B 143.3(7) . . ? O4 Li6 H45B 99.3(6) . . ? C33 Li6 H45B 131.9(6) . . ? C45 Li6 H45B 25.2(6) . . ? C37 Li6 H45B 95.2(6) . . ? Li7 Li6 H45B 80.1(6) . . ? Li8 Li6 H45B 60.1(6) . . ? Li5 Li6 H45B 118.1(6) . . ? H37B Li6 H45B 92.6(8) . . ? H33B Li6 H45B 123.3(7) . . ? C33 Li7 C41 110.03(9) . . ? C33 Li7 C45 109.82(10) . . ? C41 Li7 C45 109.03(10) . . ? C33 Li7 Li8 106.75(11) . . ? C41 Li7 Li8 56.66(8) . . ? C45 Li7 Li8 56.85(8) . . ? C33 Li7 Li6 56.42(8) . . ? C41 Li7 Li6 108.13(10) . . ? C45 Li7 Li6 57.06(7) . . ? Li8 Li7 Li6 62.59(9) . . ? C33 Li7 Li5 56.91(8) . . ? C41 Li7 Li5 56.92(8) . . ? C45 Li7 Li5 107.64(10) . . ? Li8 Li7 Li5 61.93(9) . . ? Li6 Li7 Li5 63.09(9) . . ? C33 Li7 H41A 94.0(5) . . ? C41 Li7 H41A 25.6(5) . . ? C45 Li7 H41A 134.5(5) . . ? Li8 Li7 H41A 79.7(5) . . ? Li6 Li7 H41A 116.5(5) . . ? Li5 Li7 H41A 54.3(5) . . ? C37 Li8 C41 110.11(11) . . ? C37 Li8 C45 109.06(10) . . ? C41 Li8 C45 110.69(10) . . ? C37 Li8 Li7 106.29(11) . . ? C41 Li8 Li7 57.43(9) . . ? C45 Li8 Li7 57.90(8) . . ? C37 Li8 Li6 57.09(8) . . ? C41 Li8 Li6 107.29(11) . . ? C45 Li8 Li6 56.65(8) . . ? Li7 Li8 Li6 60.82(9) . . ? C37 Li8 Li5 56.67(8) . . ? C41 Li8 Li5 57.21(8) . . ? C45 Li8 Li5 108.67(10) . . ? Li7 Li8 Li5 62.18(9) . . ? Li6 Li8 Li5 62.60(8) . . ? C37 Li8 H45A 131.9(5) . . ? C41 Li8 H45A 107.4(5) . . ? C45 Li8 H45A 27.2(4) . . ? Li7 Li8 H45A 70.8(5) . . ? Li6 Li8 H45A 83.8(5) . . ? Li5 Li8 H45A 131.1(5) . . ? C5 Si1 C7 112.51(7) . . ? C5 Si1 C6 115.14(7) . . ? C7 Si1 C6 106.13(9) . . ? C5 Si1 C8 109.07(8) . . ? C7 Si1 C8 106.84(7) . . ? C6 Si1 C8 106.69(9) . . ? C13 Si2 C16 111.30(8) . . ? C13 Si2 C14 115.67(6) . . ? C16 Si2 C14 107.52(8) . . ? C13 Si2 C15 109.65(7) . . ? C16 Si2 C15 106.61(9) . . ? C14 Si2 C15 105.57(8) . . ? C17 Si3 C18 114.83(7) . . ? C17 Si3 C20 109.95(7) . . ? C18 Si3 C20 107.56(8) . . ? C17 Si3 C19 112.09(7) . . ? C18 Si3 C19 104.56(8) . . ? C20 Si3 C19 107.44(8) . . ? C21 Si4 C23 112.35(7) . . ? C21 Si4 C24 111.22(6) . . ? C23 Si4 C24 105.58(6) . . ? C21 Si4 C22 114.30(6) . . ? C23 Si4 C22 106.03(8) . . ? C24 Si4 C22 106.78(7) . . ? C33 Si5 C36 112.26(7) . . ? C33 Si5 C34 115.23(7) . . ? C36 Si5 C34 106.42(9) . . ? C33 Si5 C35 109.07(8) . . ? C36 Si5 C35 107.45(7) . . ? C34 Si5 C35 105.97(9) . . ? C37 Si6 C40 111.78(8) . . ? C37 Si6 C38 114.80(7) . . ? C40 Si6 C38 107.02(8) . . ? C37 Si6 C39 109.87(7) . . ? C40 Si6 C39 107.46(9) . . ? C38 Si6 C39 105.47(8) . . ? C41 Si7 C43 109.81(8) . . ? C41 Si7 C44 111.14(7) . . ? C43 Si7 C44 108.43(8) . . ? C41 Si7 C42 114.62(7) . . ? C43 Si7 C42 105.51(8) . . ? C44 Si7 C42 107.03(8) . . ? C45 Si8 C47 111.85(7) . . ? C45 Si8 C48 111.63(6) . . ? C47 Si8 C48 105.99(7) . . ? C45 Si8 C46 114.84(6) . . ? C47 Si8 C46 106.18(8) . . ? C48 Si8 C46 105.75(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C3 C4 107.74(15) . . ? O1 C3 O1' 20.0(2) . . ? C4 C3 O1' 117.1(3) . . ? O1 C3 H3A 110.2 . . ? C4 C3 H3A 110.1 . . ? O1' C3 H3A 118.5 . . ? O1 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? O1' C3 H3B 90.1 . . ? H3A C3 H3B 108.5 . . ? O1 C3 H3C 96.5 . . ? C4 C3 H3C 108.1 . . ? O1' C3 H3C 108.2 . . ? H3A C3 H3C 16.1 . . ? H3B C3 H3C 122.8 . . ? O1 C3 H3D 127.5 . . ? C4 C3 H3D 108.0 . . ? O1' C3 H3D 107.7 . . ? H3A C3 H3D 91.8 . . ? H3B C3 H3D 19.7 . . ? H3C C3 H3D 107.3 . . ? C3 O1 C2 110.98(17) . . ? C3 O1 Li1 126.68(15) . . ? C2 O1 Li1 121.47(15) . . ? O1 C2 C1 113.14(18) . . ? O1 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? O1 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C2' O1' C3 118.6(6) . . ? C2' O1' Li1 122.3(5) . . ? C3 O1' Li1 119.1(4) . . ? O1' C2' C1' 115.0(6) . . ? O1' C2' H2C 108.5 . . ? C1' C2' H2C 108.5 . . ? O1' C2' H2D 108.5 . . ? C1' C2' H2D 108.5 . . ? H2C C2' H2D 107.5 . . ? C2' C1' H1D 109.5 . . ? C2' C1' H1E 109.5 . . ? H1D C1' H1E 109.5 . . ? C2' C1' H1F 109.5 . . ? H1D C1' H1F 109.5 . . ? H1E C1' H1F 109.5 . . ? Si2 C13 Li4 88.69(8) . . ? Si2 C13 Li1 128.23(8) . . ? Li4 C13 Li1 69.90(10) . . ? Si2 C13 Li2 144.07(9) . . ? Li4 C13 Li2 69.05(8) . . ? Li1 C13 Li2 71.29(8) . . ? Si2 C13 H13B 104.5(11) . . ? Li4 C13 H13B 115.3(11) . . ? Li1 C13 H13B 127.3(11) . . ? Li2 C13 H13B 64.1(12) . . ? Si2 C13 H13A 104.4(10) . . ? Li4 C13 H13A 133.9(10) . . ? Li1 C13 H13A 67.4(10) . . ? Li2 C13 H13A 111.4(10) . . ? H13B C13 H13A 104.0(15) . . ? Si2 C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si4 C21 Li3 104.71(8) . . ? Si4 C21 Li4 168.33(8) . . ? Li3 C21 Li4 65.07(8) . . ? Si4 C21 Li2 113.94(8) . . ? Li3 C21 Li2 67.58(9) . . ? Li4 C21 Li2 68.49(8) . . ? Si4 C21 H21B 109.1(11) . . ? Li3 C21 H21B 132.2(10) . . ? Li4 C21 H21B 82.5(11) . . ? Li2 C21 H21B 68.3(10) . . ? Si4 C21 H21A 104.3(10) . . ? Li3 C21 H21A 96.4(9) . . ? Li4 C21 H21A 72.5(10) . . ? Li2 C21 H21A 141.0(10) . . ? H21B C21 H21A 106.6(14) . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C5 Li3 96.37(9) . . ? Si1 C5 Li2 161.24(9) . . ? Li3 C5 Li2 68.40(9) . . ? Si1 C5 Li1 114.15(7) . . ? Li3 C5 Li1 69.36(8) . . ? Li2 C5 Li1 71.80(8) . . ? Si1 C5 H5B 106.5(11) . . ? Li3 C5 H5B 95.1(11) . . ? Li2 C5 H5B 65.7(11) . . ? Li1 C5 H5B 137.5(11) . . ? Si1 C5 H5A 103.3(10) . . ? Li3 C5 H5A 148.7(11) . . ? Li2 C5 H5A 95.2(10) . . ? Li1 C5 H5A 80.4(11) . . ? H5B C5 H5A 102.2(15) . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C33 Li7 96.81(9) . . ? Si5 C33 Li6 162.63(9) . . ? Li7 C33 Li6 68.69(9) . . ? Si5 C33 Li5 113.29(8) . . ? Li7 C33 Li5 69.46(8) . . ? Li6 C33 Li5 71.59(8) . . ? Si5 C33 H33B 103.4(10) . . ? Li7 C33 H33B 94.5(10) . . ? Li6 C33 H33B 69.6(10) . . ? Li5 C33 H33B 141.1(10) . . ? Si5 C33 H33A 104.6(12) . . ? Li7 C33 H33A 151.1(12) . . ? Li6 C33 H33A 92.4(12) . . ? Li5 C33 H33A 84.1(12) . . ? H33B C33 H33A 99.1(15) . . ? Si5 C35 H35A 109.5 . . ? Si5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si5 C36 H36A 109.5 . . ? Si5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si5 C34 H34A 109.5 . . ? Si5 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si5 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si3 C17 Li4 108.76(9) . . ? Si3 C17 Li3 112.55(8) . . ? Li4 C17 Li3 65.87(8) . . ? Si3 C17 Li1 177.47(9) . . ? Li4 C17 Li1 69.13(9) . . ? Li3 C17 Li1 68.09(8) . . ? Si3 C17 H17A 105.3(10) . . ? Li4 C17 H17A 137.9(10) . . ? Li3 C17 H17A 78.7(10) . . ? Li1 C17 H17A 77.3(10) . . ? Si3 C17 H17B 105.1(10) . . ? Li4 C17 H17B 88.8(10) . . ? Li3 C17 H17B 139.5(10) . . ? Li1 C17 H17B 73.6(10) . . ? H17A C17 H17B 105.6(14) . . ? Si3 C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? Si3 C18 H18C 109.5 . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19B 109.5 . . ? Si3 C19 H19C 109.5 . . ? Si7 C41 Li8 110.31(10) . . ? Si7 C41 Li7 113.93(8) . . ? Li8 C41 Li7 65.92(8) . . ? Si7 C41 Li5 176.56(9) . . ? Li8 C41 Li5 69.34(10) . . ? Li7 C41 Li5 69.19(8) . . ? Si7 C41 H41A 108.9(11) . . ? Li8 C41 H41A 135.6(11) . . ? Li7 C41 H41A 79.7(11) . . ? Li5 C41 H41A 72.7(11) . . ? Si7 C41 H41B 102.4(11) . . ? Li8 C41 H41B 85.4(11) . . ? Li7 C41 H41B 139.4(12) . . ? Li5 C41 H41B 74.2(11) . . ? H41A C41 H41B 105.8(15) . . ? Si7 C42 H42A 109.5 . . ? Si7 C42 H42B 109.5 . . ? Si7 C42 H42C 109.5 . . ? Si7 C44 H44A 109.5 . . ? Si7 C44 H44B 109.5 . . ? Si7 C44 H44C 109.5 . . ? Si7 C43 H43A 109.5 . . ? Si7 C43 H43B 109.5 . . ? Si7 C43 H43C 109.5 . . ? Si6 C37 Li8 90.24(8) . . ? Si6 C37 Li5 128.14(9) . . ? Li8 C37 Li5 69.85(10) . . ? Si6 C37 Li6 146.16(9) . . ? Li8 C37 Li6 69.46(8) . . ? Li5 C37 Li6 71.13(8) . . ? Si6 C37 H37A 103.1(11) . . ? Li8 C37 H37A 138.0(11) . . ? Li5 C37 H37A 70.7(11) . . ? Li6 C37 H37A 110.1(11) . . ? Si6 C37 H37B 103.5(12) . . ? Li8 C37 H37B 113.3(12) . . ? Li5 C37 H37B 128.4(12) . . ? Li6 C37 H37B 63.8(12) . . ? H37A C37 H37B 102.1(15) . . ? Si6 C39 H39A 109.5 . . ? Si6 C39 H39B 109.5 . . ? Si6 C39 H39C 109.5 . . ? Si6 C38 H38A 109.5 . . ? Si6 C38 H38B 109.5 . . ? Si6 C38 H38C 109.5 . . ? Si6 C40 H40A 109.5 . . ? Si6 C40 H40B 109.5 . . ? Si6 C40 H40C 109.5 . . ? C30 O4 C31 114.17(10) . . ? C30 O4 Li6 118.40(10) . . ? C31 O4 Li6 126.12(10) . . ? O4 C31 C32 112.83(11) . . ? O4 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? O4 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? O4 C30 C29 112.11(11) . . ? O4 C30 H30A 109.2 . . ? C29 C30 H30A 109.2 . . ? O4 C30 H30B 109.2 . . ? C29 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? Si8 C45 Li8 165.43(9) . . ? Si8 C45 Li7 102.84(8) . . ? Li8 C45 Li7 65.24(8) . . ? Si8 C45 Li6 115.26(8) . . ? Li8 C45 Li6 69.20(8) . . ? Li7 C45 Li6 67.47(9) . . ? Si8 C45 H45A 104.1(9) . . ? Li8 C45 H45A 71.6(9) . . ? Li7 C45 H45A 100.7(9) . . ? Li6 C45 H45A 140.4(9) . . ? Si8 C45 H45B 107.2(13) . . ? Li8 C45 H45B 87.4(13) . . ? Li7 C45 H45B 134.8(12) . . ? Li6 C45 H45B 69.4(12) . . ? H45A C45 H45B 103.7(15) . . ? Si8 C48 H48A 109.5 . . ? Si8 C48 H48B 109.5 . . ? Si8 C48 H48C 109.5 . . ? Si8 C47 H47A 109.5 . . ? Si8 C47 H47B 109.5 . . ? Si8 C47 H47C 109.5 . . ? Si8 C46 H46A 109.5 . . ? Si8 C46 H46B 109.5 . . ? Si8 C46 H46C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? O3 C27 C28 112.47(15) . . ? O3 C27 H27A 108.9 . . ? C28 C27 H27A 109.4 . . ? O3 C27 H27B 108.7 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 108.1 . . ? O3 C27 H27C 121.4 . . ? C28 C27 H27C 111.2 . . ? H27A C27 H27C 90.9 . . ? H27B C27 H27C 18.2 . . ? O3 C27 H27D 88.4 . . ? C28 C27 H27D 111.5 . . ? H27A C27 H27D 22.2 . . ? H27B C27 H27D 124.7 . . ? H27C C27 H27D 109.4 . . ? C26 O3 C27 114.16(17) . . ? C26 O3 Li5 121.79(16) . . ? C27 O3 Li5 124.05(16) . . ? O3 C26 C25 112.92(18) . . ? O3 C26 H26A 109.0 . . ? C25 C26 H26A 109.0 . . ? O3 C26 H26B 109.0 . . ? C25 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C26' O3' Li5 122.3(5) . . ? O3' C26' C25' 116.8(7) . . ? O3' C26' H26C 108.1 . . ? C25' C26' H26C 108.1 . . ? O3' C26' H26D 108.1 . . ? C25' C26' H26D 108.1 . . ? H26C C26' H26D 107.3 . . ? C26' C25' H25D 109.5 . . ? C26' C25' H25E 109.5 . . ? H25D C25' H25E 109.5 . . ? C26' C25' H25F 109.5 . . ? H25D C25' H25F 109.5 . . ? H25E C25' H25F 109.5 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2 C10 C9 112.07(11) . . ? O2 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? O2 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C11 O2 C10 114.84(10) . . ? C11 O2 Li2 127.25(10) . . ? C10 O2 Li2 116.51(10) . . ? O2 C11 C12 112.66(11) . . ? O2 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? O2 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 31.95 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.449 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.039 # Attachment 'dme.cif' data_dme _database_code_depnum_ccdc_archive 'CCDC 764772' #TrackingRef 'dme.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H42 Li2 O4 Si2' _chemical_formula_weight 368.56 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.4667(8) _cell_length_b 18.3838(13) _cell_length_c 19.2670(14) _cell_angle_alpha 90.00 _cell_angle_beta 92.8900(10) _cell_angle_gamma 90.00 _cell_volume 3702.6(5) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.437 _cell_measurement_theta_max 26.048 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details SADABS-2004/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex II with D8-Goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65904 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7276 _reflns_number_gt 6605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2.1-0' _computing_cell_refinement 'SAINT V7.34A' _computing_data_reduction 'SAINT V7.34A' _computing_structure_solution 'SHELXS in SHELXTL ver. 6.10' _computing_structure_refinement 'SHELXL in SHELXTL ver. 6.10' _computing_molecular_graphics 'XP in SHELXTL ver. 6.10' _computing_publication_material 'XP in SHELXTL ver. 6.10' _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^)+(0.0415P)^2^+0.9453P] 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 7276 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.90378(3) -0.119568(15) 0.182938(15) 0.02220(8) Uani 1 1 d . . . Si2 Si 0.42455(3) 0.101647(16) 0.145045(15) 0.02242(8) Uani 1 1 d . . . Si3 Si 0.22140(3) 0.634844(15) 0.003401(15) 0.02108(8) Uani 1 1 d . . . O1 O 0.52455(8) -0.16004(4) 0.20090(4) 0.02960(18) Uani 1 1 d . . . O2 O 0.52506(8) -0.06254(4) 0.30470(4) 0.02857(17) Uani 1 1 d . . . O3 O 0.80522(8) 0.06688(4) 0.07057(4) 0.02832(17) Uani 1 1 d . . . O4 O 0.79395(7) 0.13753(4) 0.19143(4) 0.02646(17) Uani 1 1 d . . . O5 O -0.17316(7) 0.63883(4) -0.01937(4) 0.02851(17) Uani 1 1 d . . . O6 O -0.12577(7) 0.58896(4) 0.10901(4) 0.02913(17) Uani 1 1 d . . . Li1 Li 0.60486(18) -0.05934(10) 0.21026(10) 0.0265(4) Uani 1 1 d . . . Li2 Li 0.71310(17) 0.03779(10) 0.15433(9) 0.0256(4) Uani 1 1 d . . . Li3 Li -0.05522(17) 0.55552(9) 0.01789(10) 0.0257(4) Uani 1 1 d . . . C1 C 0.81339(10) -0.04685(6) 0.22254(6) 0.0240(2) Uani 1 1 d . . . H101 H 0.8087(12) -0.0590(7) 0.2706(7) 0.029 Uiso 1 1 d . . . H102 H 0.8649(12) -0.0021(7) 0.2223(6) 0.029 Uiso 1 1 d . . . C2 C 1.08334(11) -0.11695(7) 0.19945(7) 0.0370(3) Uani 1 1 d . . . H2A H 1.1164 -0.0704 0.1834 0.056 Uiso 1 1 calc R . . H2B H 1.1224 -0.1568 0.1742 0.056 Uiso 1 1 calc R . . H2C H 1.1042 -0.1223 0.2493 0.056 Uiso 1 1 calc R . . C3 C 0.87987(12) -0.11905(7) 0.08544(6) 0.0330(3) Uani 1 1 d . . . H3A H 0.7891 -0.1266 0.0724 0.050 Uiso 1 1 calc R . . H3B H 0.9305 -0.1582 0.0659 0.050 Uiso 1 1 calc R . . H3C H 0.9075 -0.0721 0.0673 0.050 Uiso 1 1 calc R . . C4 C 0.85269(12) -0.21212(6) 0.21335(6) 0.0330(3) Uani 1 1 d . . . H4A H 0.8709 -0.2163 0.2636 0.050 Uiso 1 1 calc R . . H4B H 0.8999 -0.2498 0.1894 0.050 Uiso 1 1 calc R . . H4C H 0.7607 -0.2184 0.2029 0.050 Uiso 1 1 calc R . . C5 C 0.50688(10) 0.01546(6) 0.13387(6) 0.0244(2) Uani 1 1 d . . . H105 H 0.5128(12) 0.0060(7) 0.0853(7) 0.029 Uiso 1 1 d . . . H106 H 0.4504(12) -0.0225(7) 0.1496(6) 0.029 Uiso 1 1 d . . . C6 C 0.49691(11) 0.17575(6) 0.09225(6) 0.0322(3) Uani 1 1 d . . . H6A H 0.5866 0.1828 0.1080 0.048 Uiso 1 1 calc R . . H6B H 0.4496 0.2211 0.0982 0.048 Uiso 1 1 calc R . . H6C H 0.4923 0.1619 0.0431 0.048 Uiso 1 1 calc R . . C7 C 0.43658(12) 0.12976(7) 0.23920(6) 0.0346(3) Uani 1 1 d . . . H7A H 0.4026 0.0909 0.2678 0.052 Uiso 1 1 calc R . . H7B H 0.3870 0.1743 0.2452 0.052 Uiso 1 1 calc R . . H7C H 0.5264 0.1387 0.2535 0.052 Uiso 1 1 calc R . . C8 C 0.24657(11) 0.10519(7) 0.12205(7) 0.0350(3) Uani 1 1 d . . . H8A H 0.2319 0.1020 0.0715 0.053 Uiso 1 1 calc R . . H8B H 0.2115 0.1511 0.1387 0.053 Uiso 1 1 calc R . . H8C H 0.2042 0.0643 0.1441 0.053 Uiso 1 1 calc R . . C11 C 0.47397(16) -0.19042(8) 0.13771(7) 0.0492(4) Uani 1 1 d . . . H11A H 0.4654 -0.2432 0.1430 0.074 Uiso 1 1 calc R . . H11B H 0.5318 -0.1800 0.1005 0.074 Uiso 1 1 calc R . . H11C H 0.3898 -0.1691 0.1260 0.074 Uiso 1 1 calc R . . C12 C 0.44334(11) -0.17136(7) 0.25717(7) 0.0336(3) Uani 1 1 d . . . H12A H 0.4301 -0.2240 0.2648 0.040 Uiso 1 1 calc R . . H12B H 0.3590 -0.1482 0.2471 0.040 Uiso 1 1 calc R . . C13 C 0.50908(12) -0.13757(6) 0.31971(6) 0.0318(3) Uani 1 1 d . . . H13A H 0.4568 -0.1436 0.3607 0.038 Uiso 1 1 calc R . . H13B H 0.5933 -0.1609 0.3297 0.038 Uiso 1 1 calc R . . C14 C 0.58037(14) -0.02362(7) 0.36301(6) 0.0398(3) Uani 1 1 d . . . H14A H 0.5202 -0.0230 0.4004 0.060 Uiso 1 1 calc R . . H14B H 0.5989 0.0264 0.3491 0.060 Uiso 1 1 calc R . . H14C H 0.6599 -0.0476 0.3795 0.060 Uiso 1 1 calc R . . C15 C 0.75805(14) 0.05471(8) 0.00082(6) 0.0405(3) Uani 1 1 d . . . H15A H 0.7014 0.0948 -0.0141 0.061 Uiso 1 1 calc R . . H15B H 0.7103 0.0088 -0.0017 0.061 Uiso 1 1 calc R . . H15C H 0.8300 0.0521 -0.0297 0.061 Uiso 1 1 calc R . . C16 C 0.87045(12) 0.13467(6) 0.07852(6) 0.0335(3) Uani 1 1 d . . . H16A H 0.8139 0.1749 0.0620 0.040 Uiso 1 1 calc R . . H16B H 0.9477 0.1348 0.0509 0.040 Uiso 1 1 calc R . . C17 C 0.90734(11) 0.14428(7) 0.15384(6) 0.0329(3) Uani 1 1 d . . . H17A H 0.9703 0.1067 0.1693 0.039 Uiso 1 1 calc R . . H17B H 0.9464 0.1928 0.1620 0.039 Uiso 1 1 calc R . . C18 C 0.81838(12) 0.15354(7) 0.26332(6) 0.0350(3) Uani 1 1 d . . . H18A H 0.8861 0.1215 0.2825 0.053 Uiso 1 1 calc R . . H18B H 0.7402 0.1458 0.2883 0.053 Uiso 1 1 calc R . . H18C H 0.8456 0.2043 0.2685 0.053 Uiso 1 1 calc R . . C21 C 0.15269(10) 0.54656(6) 0.02250(6) 0.0252(2) Uani 1 1 d . . . H121 H 0.1584(12) 0.5402(7) 0.0727(7) 0.030 Uiso 1 1 d . . . H122 H 0.2109(12) 0.5120(7) 0.0046(7) 0.030 Uiso 1 1 d . . . C22 C 0.14279(11) 0.71005(6) 0.05215(6) 0.0278(2) Uani 1 1 d . . . H22A H 0.0573 0.7194 0.0309 0.042 Uiso 1 1 calc R . . H22B H 0.1946 0.7543 0.0501 0.042 Uiso 1 1 calc R . . H22C H 0.1355 0.6955 0.1007 0.042 Uiso 1 1 calc R . . C23 C 0.20187(11) 0.65597(7) -0.09239(6) 0.0317(3) Uani 1 1 d . . . H23A H 0.2408 0.6171 -0.1190 0.047 Uiso 1 1 calc R . . H23B H 0.2440 0.7023 -0.1019 0.047 Uiso 1 1 calc R . . H23C H 0.1106 0.6595 -0.1061 0.047 Uiso 1 1 calc R . . C24 C 0.39911(10) 0.64559(6) 0.02508(6) 0.0300(2) Uani 1 1 d . . . H24A H 0.4157 0.6414 0.0754 0.045 Uiso 1 1 calc R . . H24B H 0.4273 0.6934 0.0095 0.045 Uiso 1 1 calc R . . H24C H 0.4461 0.6075 0.0016 0.045 Uiso 1 1 calc R . . C31 C -0.15806(12) 0.68389(7) -0.07848(7) 0.0382(3) Uani 1 1 d . . . H31A H -0.2407 0.7055 -0.0930 0.057 Uiso 1 1 calc R . . H31B H -0.1267 0.6546 -0.1165 0.057 Uiso 1 1 calc R . . H31C H -0.0964 0.7226 -0.0666 0.057 Uiso 1 1 calc R . . C32 C -0.22751(11) 0.67709(6) 0.03660(7) 0.0323(3) Uani 1 1 d . . . H32A H -0.3106 0.6988 0.0209 0.039 Uiso 1 1 calc R . . H32B H -0.1695 0.7166 0.0533 0.039 Uiso 1 1 calc R . . C33 C -0.24600(11) 0.62356(6) 0.09357(7) 0.0322(3) Uani 1 1 d . . . H33A H -0.2753 0.6488 0.1353 0.039 Uiso 1 1 calc R . . H33B H -0.3112 0.5870 0.0786 0.039 Uiso 1 1 calc R . . C34 C -0.12975(13) 0.54124(7) 0.16730(7) 0.0397(3) Uani 1 1 d . . . H34A H -0.1437 0.5697 0.2093 0.060 Uiso 1 1 calc R . . H34B H -0.0485 0.5149 0.1731 0.060 Uiso 1 1 calc R . . H34C H -0.1998 0.5064 0.1595 0.060 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 Si1 0.02126(15) 0.02112(14) 0.02422(15) 0.00062(11) 0.00122(11) 0.00291(11) Si2 0.01869(14) 0.02144(15) 0.02734(15) 0.00042(11) 0.00336(11) 0.00198(11) Si3 0.01926(14) 0.01932(14) 0.02474(15) -0.00187(11) 0.00183(11) -0.00191(10) O1 0.0311(4) 0.0248(4) 0.0326(4) -0.0028(3) -0.0022(3) -0.0037(3) O2 0.0332(4) 0.0258(4) 0.0267(4) 0.0004(3) 0.0016(3) -0.0035(3) O3 0.0334(4) 0.0263(4) 0.0255(4) 0.0026(3) 0.0041(3) -0.0010(3) O4 0.0221(4) 0.0272(4) 0.0301(4) -0.0029(3) 0.0018(3) -0.0025(3) O5 0.0276(4) 0.0228(4) 0.0353(4) 0.0024(3) 0.0027(3) 0.0031(3) O6 0.0262(4) 0.0300(4) 0.0314(4) -0.0022(3) 0.0045(3) 0.0006(3) Li1 0.0285(9) 0.0229(9) 0.0282(9) 0.0012(7) 0.0029(7) -0.0023(7) Li2 0.0243(9) 0.0246(9) 0.0282(9) 0.0022(7) 0.0031(7) 0.0002(7) Li3 0.0227(9) 0.0225(9) 0.0321(9) -0.0017(7) 0.0030(7) 0.0007(7) C1 0.0251(5) 0.0217(5) 0.0251(5) -0.0001(4) 0.0009(4) 0.0018(4) C2 0.0251(6) 0.0407(7) 0.0453(7) -0.0049(6) 0.0008(5) 0.0043(5) C3 0.0417(7) 0.0309(6) 0.0266(6) -0.0009(5) 0.0039(5) 0.0073(5) C4 0.0377(6) 0.0236(5) 0.0381(7) 0.0034(5) 0.0048(5) 0.0034(5) C5 0.0226(5) 0.0216(5) 0.0288(6) 0.0003(4) 0.0006(4) 0.0009(4) C6 0.0322(6) 0.0255(6) 0.0396(6) 0.0060(5) 0.0076(5) 0.0035(5) C7 0.0338(6) 0.0381(7) 0.0325(6) -0.0050(5) 0.0069(5) 0.0049(5) C8 0.0226(6) 0.0337(6) 0.0487(7) -0.0009(5) 0.0008(5) 0.0042(5) C11 0.0671(10) 0.0365(7) 0.0424(8) -0.0102(6) -0.0132(7) -0.0078(7) C12 0.0252(6) 0.0284(6) 0.0473(7) 0.0021(5) 0.0036(5) -0.0070(5) C13 0.0322(6) 0.0298(6) 0.0338(6) 0.0073(5) 0.0064(5) -0.0046(5) C14 0.0528(8) 0.0385(7) 0.0282(6) -0.0067(5) 0.0023(5) -0.0064(6) C15 0.0517(8) 0.0441(7) 0.0259(6) -0.0001(5) 0.0032(5) 0.0036(6) C16 0.0339(6) 0.0288(6) 0.0389(7) 0.0058(5) 0.0124(5) -0.0046(5) C17 0.0241(6) 0.0326(6) 0.0425(7) -0.0005(5) 0.0061(5) -0.0078(5) C18 0.0324(6) 0.0377(6) 0.0346(6) -0.0102(5) -0.0018(5) 0.0000(5) C21 0.0203(5) 0.0193(5) 0.0359(6) -0.0014(4) 0.0018(4) -0.0008(4) C22 0.0346(6) 0.0220(5) 0.0270(5) -0.0003(4) 0.0038(5) 0.0015(4) C23 0.0320(6) 0.0358(6) 0.0275(6) -0.0021(5) 0.0043(5) -0.0032(5) C24 0.0229(5) 0.0295(6) 0.0375(6) -0.0007(5) 0.0006(5) -0.0061(4) C31 0.0334(6) 0.0378(7) 0.0425(7) 0.0126(5) -0.0056(5) -0.0008(5) C32 0.0246(6) 0.0235(5) 0.0491(7) -0.0044(5) 0.0059(5) 0.0046(4) C33 0.0230(6) 0.0312(6) 0.0430(7) -0.0066(5) 0.0092(5) 0.0009(4) C34 0.0446(7) 0.0425(7) 0.0318(6) 0.0021(5) 0.0006(5) -0.0052(6) _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 Si1 C1 1.8268(11) . ? Si1 C3 1.8825(12) . ? Si1 C4 1.8856(12) . ? Si1 C2 1.8908(12) . ? Si2 C5 1.8215(11) . ? Si2 C6 1.8819(12) . ? Si2 C7 1.8844(12) . ? Si2 C8 1.8941(12) . ? Si3 C21 1.8202(11) . ? Si3 C22 1.8837(11) . ? Si3 C23 1.8870(12) . ? Si3 C24 1.8960(11) . ? O1 C11 1.4175(15) . ? O1 C12 1.4261(14) . ? O1 Li1 2.0374(19) . ? O2 C13 1.4209(13) . ? O2 C14 1.4296(14) . ? O2 Li1 2.041(2) . ? O3 C16 1.4255(14) . ? O3 C15 1.4258(14) . ? O3 Li2 1.9944(19) . ? O4 C18 1.4264(14) . ? O4 C17 1.4265(13) . ? O4 Li2 2.128(2) . ? O5 C31 1.4236(14) . ? O5 C32 1.4293(14) . ? O5 Li3 2.0726(19) . ? O6 C34 1.4275(15) . ? O6 C33 1.4279(14) . ? O6 Li3 2.034(2) . ? Li1 C1 2.196(2) . ? Li1 C5 2.226(2) . ? Li1 C13 2.781(2) . ? Li1 H106 2.061(12) . ? Li2 C5 2.213(2) . ? Li2 C1 2.261(2) . ? Li2 H102 2.137(12) . ? Li3 C21 2.180(2) . ? Li3 C21 2.256(2) 3_565 ? Li3 Li3 2.461(3) 3_565 ? C1 H101 0.956(13) . ? C1 H102 0.983(13) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H105 0.957(13) . ? C5 H106 0.973(13) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.4927(17) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.4932(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 Li3 2.256(2) 3_565 ? C21 H121 0.973(13) . ? C21 H122 0.957(13) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.4940(17) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 Si1 C3 111.56(5) . . ? C1 Si1 C4 111.69(5) . . ? C3 Si1 C4 106.81(6) . . ? C1 Si1 C2 116.25(5) . . ? C3 Si1 C2 104.41(6) . . ? C4 Si1 C2 105.41(6) . . ? C5 Si2 C6 111.11(5) . . ? C5 Si2 C7 110.08(5) . . ? C6 Si2 C7 108.22(6) . . ? C5 Si2 C8 117.89(5) . . ? C6 Si2 C8 105.46(6) . . ? C7 Si2 C8 103.47(6) . . ? C21 Si3 C22 111.51(5) . . ? C21 Si3 C23 110.90(5) . . ? C22 Si3 C23 107.94(5) . . ? C21 Si3 C24 116.20(5) . . ? C22 Si3 C24 105.18(5) . . ? C23 Si3 C24 104.52(5) . . ? C11 O1 C12 112.60(10) . . ? C11 O1 Li1 124.64(9) . . ? C12 O1 Li1 108.93(8) . . ? C13 O2 C14 111.90(9) . . ? C13 O2 Li1 105.49(8) . . ? C14 O2 Li1 121.24(9) . . ? C16 O3 C15 112.32(9) . . ? C16 O3 Li2 113.32(8) . . ? C15 O3 Li2 124.20(9) . . ? C18 O4 C17 111.23(9) . . ? C18 O4 Li2 123.55(8) . . ? C17 O4 Li2 103.38(8) . . ? C31 O5 C32 112.45(9) . . ? C31 O5 Li3 128.23(9) . . ? C32 O5 Li3 110.80(8) . . ? C34 O6 C33 112.16(9) . . ? C34 O6 Li3 121.31(9) . . ? C33 O6 Li3 108.02(8) . . ? O1 Li1 O2 82.37(7) . . ? O1 Li1 C1 120.54(9) . . ? O2 Li1 C1 110.87(9) . . ? O1 Li1 C5 109.18(9) . . ? O2 Li1 C5 114.30(9) . . ? C1 Li1 C5 115.40(9) . . ? O1 Li1 C13 55.55(5) . . ? O2 Li1 C13 29.50(4) . . ? C1 Li1 C13 111.52(8) . . ? C5 Li1 C13 130.47(9) . . ? O1 Li1 H106 86.6(4) . . ? O2 Li1 H106 99.8(4) . . ? C1 Li1 H106 140.7(4) . . ? C5 Li1 H106 25.9(4) . . ? C13 Li1 H106 107.3(4) . . ? O3 Li2 O4 80.82(7) . . ? O3 Li2 C5 114.37(9) . . ? O4 Li2 C5 125.98(9) . . ? O3 Li2 C1 115.19(9) . . ? O4 Li2 C1 103.45(8) . . ? C5 Li2 C1 113.33(9) . . ? O3 Li2 H102 102.3(3) . . ? O4 Li2 H102 79.6(4) . . ? C5 Li2 H102 137.2(4) . . ? C1 Li2 H102 25.6(4) . . ? O6 Li3 O5 80.78(7) . . ? O6 Li3 C21 113.13(9) . . ? O5 Li3 C21 130.23(9) . . ? O6 Li3 C21 111.82(9) . 3_565 ? O5 Li3 C21 104.13(8) . 3_565 ? C21 Li3 C21 112.61(8) . 3_565 ? O6 Li3 Li3 133.52(13) . 3_565 ? O5 Li3 Li3 142.73(13) . 3_565 ? C21 Li3 Li3 57.78(8) . 3_565 ? C21 Li3 Li3 54.83(7) 3_565 3_565 ? Si1 C1 Li1 114.29(7) . . ? Si1 C1 Li2 119.74(7) . . ? Li1 C1 Li2 65.13(7) . . ? Si1 C1 H101 106.6(8) . . ? Li1 C1 H101 88.9(7) . . ? Li2 C1 H101 132.8(8) . . ? Si1 C1 H102 108.3(7) . . ? Li1 C1 H102 129.0(7) . . ? Li2 C1 H102 70.1(7) . . ? H101 C1 H102 104.8(10) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 Li2 106.29(7) . . ? Si2 C5 Li1 131.61(8) . . ? Li2 C5 Li1 65.43(7) . . ? Si2 C5 H105 109.1(8) . . ? Li2 C5 H105 95.6(8) . . ? Li1 C5 H105 118.9(8) . . ? Si2 C5 H106 106.8(7) . . ? Li2 C5 H106 132.8(7) . . ? Li1 C5 H106 67.5(7) . . ? H105 C5 H106 104.2(10) . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O1 C12 C13 106.55(9) . . ? O1 C12 H12A 110.4 . . ? C13 C12 H12A 110.4 . . ? O1 C12 H12B 110.4 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? O2 C13 C12 107.09(9) . . ? O2 C13 Li1 45.01(6) . . ? C12 C13 Li1 76.83(7) . . ? O2 C13 H13A 110.3 . . ? C12 C13 H13A 110.3 . . ? Li1 C13 H13A 153.9 . . ? O2 C13 H13B 110.3 . . ? C12 C13 H13B 110.3 . . ? Li1 C13 H13B 91.2 . . ? H13A C13 H13B 108.6 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 H15A 109.5 . . ? O3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O3 C16 C17 107.87(9) . . ? O3 C16 H16A 110.1 . . ? C17 C16 H16A 110.1 . . ? O3 C16 H16B 110.1 . . ? C17 C16 H16B 110.1 . . ? H16A C16 H16B 108.4 . . ? O4 C17 C16 107.59(9) . . ? O4 C17 H17A 110.2 . . ? C16 C17 H17A 110.2 . . ? O4 C17 H17B 110.2 . . ? C16 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si3 C21 Li3 109.16(7) . . ? Si3 C21 Li3 148.05(8) . 3_565 ? Li3 C21 Li3 67.39(8) . 3_565 ? Si3 C21 H121 107.7(8) . . ? Li3 C21 H121 93.5(7) . . ? Li3 C21 H121 104.3(8) 3_565 . ? Si3 C21 H122 104.7(8) . . ? Li3 C21 H122 133.5(8) . . ? Li3 C21 H122 67.0(8) 3_565 . ? H121 C21 H122 105.7(10) . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C32 C33 107.54(9) . . ? O5 C32 H32A 110.2 . . ? C33 C32 H32A 110.2 . . ? O5 C32 H32B 110.2 . . ? C33 C32 H32B 110.2 . . ? H32A C32 H32B 108.5 . . ? O6 C33 C32 107.51(9) . . ? O6 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? O6 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? O6 C34 H34A 109.5 . . ? O6 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O6 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 C11 O1 Li1 O2 146.26(11) . . . . ? C12 O1 Li1 O2 9.31(9) . . . . ? C11 O1 Li1 C1 -103.97(13) . . . . ? C12 O1 Li1 C1 119.07(11) . . . . ? C11 O1 Li1 C5 33.12(15) . . . . ? C12 O1 Li1 C5 -103.84(10) . . . . ? C11 O1 Li1 C13 159.61(12) . . . . ? C12 O1 Li1 C13 22.65(7) . . . . ? C13 O2 Li1 O1 22.75(9) . . . . ? C14 O2 Li1 O1 151.13(9) . . . . ? C13 O2 Li1 C1 -97.09(10) . . . . ? C14 O2 Li1 C1 31.29(13) . . . . ? C13 O2 Li1 C5 130.40(10) . . . . ? C14 O2 Li1 C5 -101.23(12) . . . . ? C14 O2 Li1 C13 128.38(12) . . . . ? C16 O3 Li2 O4 -0.82(10) . . . . ? C15 O3 Li2 O4 -143.27(9) . . . . ? C16 O3 Li2 C5 124.64(10) . . . . ? C15 O3 Li2 C5 -17.82(14) . . . . ? C16 O3 Li2 C1 -101.44(11) . . . . ? C15 O3 Li2 C1 116.10(11) . . . . ? C18 O4 Li2 O3 -155.46(8) . . . . ? C17 O4 Li2 O3 -28.28(9) . . . . ? C18 O4 Li2 C5 91.02(13) . . . . ? C17 O4 Li2 C5 -141.80(11) . . . . ? C18 O4 Li2 C1 -41.59(12) . . . . ? C17 O4 Li2 C1 85.59(9) . . . . ? C34 O6 Li3 O5 155.84(9) . . . . ? C33 O6 Li3 O5 24.38(9) . . . . ? C34 O6 Li3 C21 -74.20(12) . . . . ? C33 O6 Li3 C21 154.33(9) . . . . ? C34 O6 Li3 C21 54.22(13) . . . 3_565 ? C33 O6 Li3 C21 -77.25(10) . . . 3_565 ? C34 O6 Li3 Li3 -7.4(2) . . . 3_565 ? C33 O6 Li3 Li3 -138.87(16) . . . 3_565 ? C31 O5 Li3 O6 150.34(10) . . . . ? C32 O5 Li3 O6 5.33(9) . . . . ? C31 O5 Li3 C21 37.76(18) . . . . ? C32 O5 Li3 C21 -107.25(13) . . . . ? C31 O5 Li3 C21 -99.33(12) . . . 3_565 ? C32 O5 Li3 C21 115.67(9) . . . 3_565 ? C31 O5 Li3 Li3 -49.9(3) . . . 3_565 ? C32 O5 Li3 Li3 165.14(19) . . . 3_565 ? C3 Si1 C1 Li1 66.38(9) . . . . ? C4 Si1 C1 Li1 -53.07(9) . . . . ? C2 Si1 C1 Li1 -174.07(8) . . . . ? C3 Si1 C1 Li2 -7.73(10) . . . . ? C4 Si1 C1 Li2 -127.19(8) . . . . ? C2 Si1 C1 Li2 111.81(9) . . . . ? O1 Li1 C1 Si1 28.35(13) . . . . ? O2 Li1 C1 Si1 121.78(8) . . . . ? C5 Li1 C1 Si1 -106.26(9) . . . . ? C13 Li1 C1 Si1 90.10(9) . . . . ? O1 Li1 C1 Li2 141.35(12) . . . . ? O2 Li1 C1 Li2 -125.23(10) . . . . ? C5 Li1 C1 Li2 6.73(9) . . . . ? C13 Li1 C1 Li2 -156.91(10) . . . . ? O3 Li2 C1 Si1 -36.14(12) . . . . ? O4 Li2 C1 Si1 -122.19(8) . . . . ? C5 Li2 C1 Si1 98.25(10) . . . . ? O3 Li2 C1 Li1 -141.05(11) . . . . ? O4 Li2 C1 Li1 132.90(10) . . . . ? C5 Li2 C1 Li1 -6.66(8) . . . . ? C6 Si2 C5 Li2 51.74(8) . . . . ? C7 Si2 C5 Li2 -68.12(8) . . . . ? C8 Si2 C5 Li2 173.58(7) . . . . ? C6 Si2 C5 Li1 123.08(10) . . . . ? C7 Si2 C5 Li1 3.22(11) . . . . ? C8 Si2 C5 Li1 -115.08(10) . . . . ? O3 Li2 C5 Si2 -89.84(10) . . . . ? O4 Li2 C5 Si2 6.61(13) . . . . ? C1 Li2 C5 Si2 135.39(8) . . . . ? O3 Li2 C5 Li1 141.33(11) . . . . ? O4 Li2 C5 Li1 -122.22(12) . . . . ? C1 Li2 C5 Li1 6.56(8) . . . . ? O1 Li1 C5 Si2 123.25(9) . . . . ? O2 Li1 C5 Si2 33.09(14) . . . . ? C1 Li1 C5 Si2 -97.23(11) . . . . ? C13 Li1 C5 Si2 62.62(15) . . . . ? O1 Li1 C5 Li2 -146.38(11) . . . . ? O2 Li1 C5 Li2 123.46(11) . . . . ? C1 Li1 C5 Li2 -6.86(9) . . . . ? C13 Li1 C5 Li2 152.99(13) . . . . ? C11 O1 C12 C13 179.34(10) . . . . ? Li1 O1 C12 C13 -38.12(12) . . . . ? C14 O2 C13 C12 176.38(10) . . . . ? Li1 O2 C13 C12 -49.87(11) . . . . ? C14 O2 C13 Li1 -133.75(11) . . . . ? O1 C12 C13 O2 59.80(12) . . . . ? O1 C12 C13 Li1 26.06(8) . . . . ? O1 Li1 C13 O2 -152.30(11) . . . . ? C1 Li1 C13 O2 94.63(11) . . . . ? C5 Li1 C13 O2 -65.84(12) . . . . ? O1 Li1 C13 C12 -20.95(7) . . . . ? O2 Li1 C13 C12 131.36(11) . . . . ? C1 Li1 C13 C12 -134.02(10) . . . . ? C5 Li1 C13 C12 65.52(12) . . . . ? C15 O3 C16 C17 176.00(10) . . . . ? Li2 O3 C16 C17 29.01(12) . . . . ? C18 O4 C17 C16 -173.92(9) . . . . ? Li2 O4 C17 C16 51.51(11) . . . . ? O3 C16 C17 O4 -55.01(12) . . . . ? C22 Si3 C21 Li3 45.52(9) . . . . ? C23 Si3 C21 Li3 -74.81(8) . . . . ? C24 Si3 C21 Li3 166.04(7) . . . . ? C22 Si3 C21 Li3 123.28(14) . . . 3_565 ? C23 Si3 C21 Li3 2.95(15) . . . 3_565 ? C24 Si3 C21 Li3 -116.20(14) . . . 3_565 ? O6 Li3 C21 Si3 -86.06(10) . . . . ? O5 Li3 C21 Si3 11.59(15) . . . . ? C21 Li3 C21 Si3 145.93(9) 3_565 . . . ? Li3 Li3 C21 Si3 145.93(9) 3_565 . . . ? O6 Li3 C21 Li3 128.01(14) . . . 3_565 ? O5 Li3 C21 Li3 -134.34(17) . . . 3_565 ? C21 Li3 C21 Li3 0.0 3_565 . . 3_565 ? C31 O5 C32 C33 176.61(9) . . . . ? Li3 O5 C32 C33 -32.56(12) . . . . ? C34 O6 C33 C32 174.68(10) . . . . ? Li3 O6 C33 C32 -49.06(11) . . . . ? O5 C32 C33 O6 54.13(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.344 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.035 # Attachment '2_cif.cif' data_tbuome_ungeschnitten _database_code_depnum_ccdc_archive 'CCDC 764773' #TrackingRef '2_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H68 Li4 O2 Si4' _chemical_formula_weight 552.92 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' 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' _cell_length_a 21.569(3) _cell_length_b 10.6442(14) _cell_length_c 17.116(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3929.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 0.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9752 _exptl_absorpt_correction_T_max 0.9833 _exptl_absorpt_process_details 'SADABS 2008/2 (Bruker AXS, 2008)' _exptl_special_details ; Intensities were measured with a Bruker APEX II area detector ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38585 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.51 _reflns_number_total 7279 _reflns_number_gt 6202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (v2.2-0, Bruker 2007)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.46a, Bruker 2007)' _computing_data_reduction 'Bruker AXS SAINT (v 7.46a, Bruker 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.3.1, Bruker 2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0873P)^2^+2.0319P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(16) _refine_ls_number_reflns 7279 _refine_ls_number_parameters 566 _refine_ls_number_restraints 1007 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.092 _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 0.3643(3) 0.5924(7) 0.1790(4) 0.0535(9) Uani 1 1 d U . . Li2 Li 0.2866(3) 0.7706(6) 0.1222(4) 0.0424(8) Uani 1 1 d U A . Li3 Li 0.4025(3) 0.7506(5) 0.0775(4) 0.0437(7) Uani 1 1 d U A . Li4 Li 0.3297(3) 0.5967(6) 0.0356(4) 0.0461(8) Uani 1 1 d U A . O2 O 0.22136(15) 0.8748(3) 0.1777(2) 0.0464(8) Uani 0.795(6) 1 d PDU A 1 C6 C 0.2037(4) 0.8253(7) 0.2511(5) 0.061(2) Uani 0.795(6) 1 d PDU A 1 H6A H 0.2181 0.7382 0.2553 0.091 Uiso 0.795(6) 1 calc PR A 1 H6B H 0.1585 0.8277 0.2559 0.091 Uiso 0.795(6) 1 calc PR A 1 H6C H 0.2224 0.8756 0.2928 0.091 Uiso 0.795(6) 1 calc PR A 1 C7 C 0.2027(2) 1.0048(4) 0.1651(4) 0.0519(11) Uani 0.795(6) 1 d PDU A 1 C9 C 0.2349(3) 1.0925(6) 0.2220(5) 0.080(2) Uani 0.795(6) 1 d PDU A 1 H9A H 0.2206 1.0745 0.2752 0.119 Uiso 0.795(6) 1 calc PR A 1 H9B H 0.2250 1.1797 0.2087 0.119 Uiso 0.795(6) 1 calc PR A 1 H9C H 0.2798 1.0798 0.2190 0.119 Uiso 0.795(6) 1 calc PR A 1 C8 C 0.1323(3) 1.0194(7) 0.1681(6) 0.066(2) Uani 0.795(6) 1 d PDU A 1 H8A H 0.1176 1.0013 0.2211 0.099 Uiso 0.795(6) 1 calc PR A 1 H8B H 0.1131 0.9606 0.1312 0.099 Uiso 0.795(6) 1 calc PR A 1 H8C H 0.1210 1.1056 0.1538 0.099 Uiso 0.795(6) 1 calc PR A 1 C10 C 0.2252(3) 1.0333(7) 0.0820(4) 0.0645(17) Uani 0.795(6) 1 d PDU A 1 H10A H 0.2045 0.9767 0.0451 0.097 Uiso 0.795(6) 1 calc PR A 1 H10B H 0.2701 1.0209 0.0791 0.097 Uiso 0.795(6) 1 calc PR A 1 H10C H 0.2152 1.1206 0.0688 0.097 Uiso 0.795(6) 1 calc PR A 1 O2' O 0.2273(6) 0.9207(13) 0.1386(8) 0.0485(19) Uani 0.205(6) 1 d PDU A 2 C6' C 0.2429(14) 1.038(2) 0.1031(16) 0.059(5) Uani 0.205(6) 1 d PDU A 2 H6D H 0.2656 1.0225 0.0544 0.088 Uiso 0.205(6) 1 calc PR A 2 H6E H 0.2689 1.0869 0.1388 0.088 Uiso 0.205(6) 1 calc PR A 2 H6F H 0.2049 1.0848 0.0916 0.088 Uiso 0.205(6) 1 calc PR A 2 C7' C 0.1932(7) 0.9417(16) 0.2115(9) 0.052(2) Uani 0.205(6) 1 d PDU A 2 C9' C 0.1270(8) 0.983(3) 0.1928(19) 0.058(5) Uani 0.205(6) 1 d PDU A 2 H9D H 0.1282 1.0599 0.1612 0.088 Uiso 0.205(6) 1 calc PR A 2 H9E H 0.1047 0.9996 0.2416 0.088 Uiso 0.205(6) 1 calc PR A 2 H9F H 0.1058 0.9166 0.1637 0.088 Uiso 0.205(6) 1 calc PR A 2 C8' C 0.2246(9) 1.039(2) 0.2631(12) 0.056(4) Uani 0.205(6) 1 d PDU A 2 H8D H 0.2273 1.1193 0.2349 0.083 Uiso 0.205(6) 1 calc PR A 2 H8E H 0.2664 1.0106 0.2767 0.083 Uiso 0.205(6) 1 calc PR A 2 H8F H 0.2003 1.0511 0.3109 0.083 Uiso 0.205(6) 1 calc PR A 2 C10' C 0.1892(17) 0.810(2) 0.249(2) 0.061(5) Uani 0.205(6) 1 d PDU A 2 H10D H 0.1683 0.7527 0.2125 0.092 Uiso 0.205(6) 1 calc PR A 2 H10E H 0.1658 0.8150 0.2975 0.092 Uiso 0.205(6) 1 calc PR A 2 H10F H 0.2312 0.7791 0.2592 0.092 Uiso 0.205(6) 1 calc PR A 2 O1 O 0.39724(15) 0.4863(4) 0.2672(2) 0.0617(10) Uani 0.803(5) 1 d PDU B 1 C1 C 0.4538(3) 0.4204(7) 0.2565(4) 0.0629(17) Uani 0.803(5) 1 d PDU B 1 H1A H 0.4733 0.4477 0.2077 0.094 Uiso 0.803(5) 1 calc PR B 1 H1B H 0.4454 0.3300 0.2540 0.094 Uiso 0.803(5) 1 calc PR B 1 H1C H 0.4816 0.4380 0.3004 0.094 Uiso 0.803(5) 1 calc PR B 1 C2 C 0.3614(2) 0.4556(5) 0.3369(3) 0.0663(13) Uani 0.803(5) 1 d PDU B 1 C3 C 0.4032(4) 0.4486(10) 0.4071(4) 0.0722(18) Uani 0.803(5) 1 d PDU B 1 H3A H 0.4241 0.5295 0.4143 0.108 Uiso 0.803(5) 1 calc PR B 1 H3B H 0.4342 0.3825 0.3992 0.108 Uiso 0.803(5) 1 calc PR B 1 H3C H 0.3784 0.4293 0.4536 0.108 Uiso 0.803(5) 1 calc PR B 1 C4 C 0.3245(3) 0.3378(6) 0.3246(6) 0.092(2) Uani 0.803(5) 1 d PDU B 1 H4A H 0.3527 0.2658 0.3206 0.138 Uiso 0.803(5) 1 calc PR B 1 H4B H 0.3003 0.3452 0.2763 0.138 Uiso 0.803(5) 1 calc PR B 1 H4C H 0.2963 0.3253 0.3689 0.138 Uiso 0.803(5) 1 calc PR B 1 C5 C 0.3168(2) 0.5689(6) 0.3476(3) 0.0707(15) Uani 0.803(5) 1 d PDU B 1 H5A H 0.3410 0.6465 0.3524 0.106 Uiso 0.803(5) 1 calc PR B 1 H5B H 0.2920 0.5567 0.3949 0.106 Uiso 0.803(5) 1 calc PR B 1 H5C H 0.2893 0.5751 0.3022 0.106 Uiso 0.803(5) 1 calc PR B 1 O1' O 0.3593(6) 0.5289(14) 0.2999(9) 0.070(2) Uani 0.197(5) 1 d PDU B 2 C1' C 0.2939(7) 0.523(3) 0.3130(19) 0.090(5) Uani 0.197(5) 1 d PDU B 2 H1D H 0.2741 0.5984 0.2921 0.135 Uiso 0.197(5) 1 calc PR B 2 H1E H 0.2858 0.5170 0.3693 0.135 Uiso 0.197(5) 1 calc PR B 2 H1F H 0.2769 0.4484 0.2868 0.135 Uiso 0.197(5) 1 calc PR B 2 C2' C 0.3920(6) 0.4202(16) 0.3313(9) 0.066(2) Uani 0.197(5) 1 d PDU B 2 C3' C 0.3504(12) 0.3059(18) 0.327(2) 0.092(5) Uani 0.197(5) 1 d PDU B 2 H3D H 0.3367 0.2935 0.2729 0.138 Uiso 0.197(5) 1 calc PR B 2 H3E H 0.3141 0.3185 0.3606 0.138 Uiso 0.197(5) 1 calc PR B 2 H3F H 0.3733 0.2316 0.3444 0.138 Uiso 0.197(5) 1 calc PR B 2 C4' C 0.4087(15) 0.450(3) 0.4155(10) 0.070(5) Uani 0.197(5) 1 d PDU B 2 H4D H 0.3711 0.4482 0.4477 0.104 Uiso 0.197(5) 1 calc PR B 2 H4E H 0.4274 0.5338 0.4182 0.104 Uiso 0.197(5) 1 calc PR B 2 H4F H 0.4382 0.3875 0.4349 0.104 Uiso 0.197(5) 1 calc PR B 2 C5' C 0.4498(9) 0.401(3) 0.2820(16) 0.067(5) Uani 0.197(5) 1 d PDU B 2 H5D H 0.4378 0.3792 0.2285 0.101 Uiso 0.197(5) 1 calc PR B 2 H5E H 0.4747 0.3329 0.3043 0.101 Uiso 0.197(5) 1 calc PR B 2 H5F H 0.4742 0.4787 0.2814 0.101 Uiso 0.197(5) 1 calc PR B 2 C23 C 0.42532(18) 0.5496(4) 0.0666(3) 0.0496(7) Uani 1 1 d DU A . Si4 Si 0.42808(5) 0.38394(9) 0.02969(8) 0.0446(3) Uani 1 1 d DU . . C26 C 0.50360(18) 0.2992(4) 0.0443(3) 0.0550(10) Uani 1 1 d DU B . H26A H 0.5015 0.2164 0.0194 0.083 Uiso 1 1 calc R . . H26B H 0.5115 0.2890 0.1003 0.083 Uiso 1 1 calc R . . H26C H 0.5373 0.3481 0.0207 0.083 Uiso 1 1 calc R . . C25 C 0.4101(2) 0.3850(4) -0.0771(3) 0.0624(10) Uani 1 1 d DU B . H25A H 0.3713 0.4306 -0.0861 0.094 Uiso 1 1 calc R . . H25B H 0.4058 0.2984 -0.0958 0.094 Uiso 1 1 calc R . . H25C H 0.4439 0.4264 -0.1055 0.094 Uiso 1 1 calc R . . C24 C 0.36898(19) 0.2810(4) 0.0791(3) 0.0632(11) Uani 1 1 d DU B . H24A H 0.3272 0.3120 0.0672 0.095 Uiso 1 1 calc R . . H24B H 0.3757 0.2828 0.1357 0.095 Uiso 1 1 calc R . . H24C H 0.3732 0.1946 0.0601 0.095 Uiso 1 1 calc R . . C11 C 0.2618(4) 0.5595(8) 0.1348(4) 0.0426(10) Uani 0.637(14) 1 d PDU A 1 H11A H 0.2792 0.4802 0.1503 0.051 Uiso 0.637(14) 1 d PR A 1 H11B H 0.2447 0.5957 0.1809 0.051 Uiso 0.637(14) 1 d PR A 1 Si1 Si 0.1927(2) 0.5170(5) 0.0714(3) 0.0475(8) Uani 0.637(14) 1 d PDU A 1 C12 C 0.1353(5) 0.4084(10) 0.1173(9) 0.099(3) Uani 0.637(14) 1 d PDU A 1 H12A H 0.1170 0.4487 0.1633 0.148 Uiso 0.637(14) 1 calc PR A 1 H12B H 0.1562 0.3306 0.1331 0.148 Uiso 0.637(14) 1 calc PR A 1 H12C H 0.1025 0.3887 0.0796 0.148 Uiso 0.637(14) 1 calc PR A 1 C13 C 0.1495(7) 0.6623(11) 0.0434(11) 0.056(3) Uani 0.637(14) 1 d PDU A 1 H13A H 0.1365 0.7070 0.0907 0.083 Uiso 0.637(14) 1 calc PR A 1 H13B H 0.1130 0.6394 0.0126 0.083 Uiso 0.637(14) 1 calc PR A 1 H13C H 0.1766 0.7168 0.0123 0.083 Uiso 0.637(14) 1 calc PR A 1 C14 C 0.2213(4) 0.4438(10) -0.0221(5) 0.069(3) Uani 0.637(14) 1 d PDU A 1 H14A H 0.2487 0.3731 -0.0098 0.103 Uiso 0.637(14) 1 calc PR A 1 H14B H 0.2441 0.5066 -0.0525 0.103 Uiso 0.637(14) 1 calc PR A 1 H14C H 0.1858 0.4136 -0.0526 0.103 Uiso 0.637(14) 1 calc PR A 1 C11' C 0.2698(6) 0.5780(15) 0.1163(9) 0.0451(13) Uani 0.363(14) 1 d PDU A 2 H11C H 0.2827 0.4971 0.1350 0.054 Uiso 0.363(14) 1 d PR A 2 H11D H 0.2475 0.6153 0.1590 0.054 Uiso 0.363(14) 1 d PR A 2 Si1' Si 0.2011(4) 0.5339(9) 0.0484(7) 0.0546(18) Uani 0.363(14) 1 d PDU A 2 C12' C 0.1524(9) 0.3948(15) 0.0693(16) 0.099(5) Uani 0.363(14) 1 d PDU A 2 H12D H 0.1791 0.3225 0.0807 0.149 Uiso 0.363(14) 1 calc PR A 2 H12E H 0.1264 0.3760 0.0238 0.149 Uiso 0.363(14) 1 calc PR A 2 H12F H 0.1259 0.4121 0.1146 0.149 Uiso 0.363(14) 1 calc PR A 2 C13' C 0.1484(11) 0.672(2) 0.0360(19) 0.054(4) Uani 0.363(14) 1 d PDU A 2 H13D H 0.1724 0.7446 0.0187 0.081 Uiso 0.363(14) 1 calc PR A 2 H13E H 0.1283 0.6907 0.0860 0.081 Uiso 0.363(14) 1 calc PR A 2 H13F H 0.1167 0.6518 -0.0032 0.081 Uiso 0.363(14) 1 calc PR A 2 C14' C 0.2365(7) 0.5107(17) -0.0524(9) 0.066(3) Uani 0.363(14) 1 d PDU A 2 H14D H 0.2627 0.4354 -0.0522 0.100 Uiso 0.363(14) 1 calc PR A 2 H14E H 0.2618 0.5841 -0.0659 0.100 Uiso 0.363(14) 1 calc PR A 2 H14F H 0.2034 0.5008 -0.0911 0.100 Uiso 0.363(14) 1 calc PR A 2 C15 C 0.3255(3) 0.7736(11) -0.0128(5) 0.0453(14) Uani 0.60(2) 1 d PDU A 1 H15A H 0.2953 0.8402 0.0007 0.054 Uiso 0.60(2) 1 d PR A 1 H15B H 0.3032 0.7149 -0.0478 0.054 Uiso 0.60(2) 1 d PR A 1 Si2 Si 0.3844(3) 0.8625(5) -0.0715(4) 0.0405(11) Uani 0.60(2) 1 d PDU A 1 C18 C 0.3580(9) 1.0126(12) -0.1187(11) 0.065(4) Uani 0.60(2) 1 d PDU A 1 H18A H 0.3909 1.0447 -0.1528 0.098 Uiso 0.60(2) 1 calc PR A 1 H18B H 0.3488 1.0749 -0.0782 0.098 Uiso 0.60(2) 1 calc PR A 1 H18C H 0.3206 0.9965 -0.1497 0.098 Uiso 0.60(2) 1 calc PR A 1 C16 C 0.4160(7) 0.7597(11) -0.1487(6) 0.064(3) Uani 0.60(2) 1 d PDU A 1 H16A H 0.4457 0.8071 -0.1805 0.096 Uiso 0.60(2) 1 calc PR A 1 H16B H 0.3821 0.7297 -0.1819 0.096 Uiso 0.60(2) 1 calc PR A 1 H16C H 0.4369 0.6878 -0.1247 0.096 Uiso 0.60(2) 1 calc PR A 1 C17 C 0.4516(5) 0.9101(12) -0.0073(8) 0.068(3) Uani 0.60(2) 1 d PDU A 1 H17A H 0.4838 0.9496 -0.0393 0.102 Uiso 0.60(2) 1 calc PR A 1 H17B H 0.4687 0.8355 0.0185 0.102 Uiso 0.60(2) 1 calc PR A 1 H17C H 0.4372 0.9698 0.0323 0.102 Uiso 0.60(2) 1 calc PR A 1 C15' C 0.3328(6) 0.8167(17) 0.0026(8) 0.0479(16) Uani 0.40(2) 1 d PDU A 2 H15C H 0.2931 0.8051 -0.0216 0.057 Uiso 0.40(2) 1 d PR A 2 H15D H 0.3291 0.8926 0.0325 0.057 Uiso 0.40(2) 1 d PR A 2 Si2' Si 0.3856(3) 0.8594(8) -0.0789(6) 0.0369(13) Uani 0.40(2) 1 d PDU A 2 C18' C 0.3672(14) 1.0087(19) -0.1340(16) 0.060(4) Uani 0.40(2) 1 d PDU A 2 H18D H 0.4023 1.0310 -0.1675 0.090 Uiso 0.40(2) 1 calc PR A 2 H18E H 0.3595 1.0769 -0.0967 0.090 Uiso 0.40(2) 1 calc PR A 2 H18F H 0.3302 0.9957 -0.1662 0.090 Uiso 0.40(2) 1 calc PR A 2 C16' C 0.3912(9) 0.7338(15) -0.1522(8) 0.058(3) Uani 0.40(2) 1 d PDU A 2 H16D H 0.4200 0.7592 -0.1935 0.087 Uiso 0.40(2) 1 calc PR A 2 H16E H 0.3501 0.7184 -0.1749 0.087 Uiso 0.40(2) 1 calc PR A 2 H16F H 0.4063 0.6567 -0.1273 0.087 Uiso 0.40(2) 1 calc PR A 2 C17' C 0.4675(6) 0.883(2) -0.0383(11) 0.069(4) Uani 0.40(2) 1 d PDU A 2 H17D H 0.4932 0.9255 -0.0776 0.104 Uiso 0.40(2) 1 calc PR A 2 H17E H 0.4858 0.8015 -0.0256 0.104 Uiso 0.40(2) 1 calc PR A 2 H17F H 0.4655 0.9351 0.0089 0.104 Uiso 0.40(2) 1 calc PR A 2 C19 C 0.37455(17) 0.8109(4) 0.1929(3) 0.0531(8) Uani 1 1 d DU A . H19A H 0.3487 0.7889 0.2387 0.064 Uiso 1 1 d R . . H19B H 0.3561 0.8894 0.1724 0.064 Uiso 1 1 d R . . Si3 Si 0.44643(5) 0.86950(10) 0.24009(8) 0.0423(2) Uani 1 1 d DU . . C20 C 0.4482(4) 0.8415(12) 0.3477(4) 0.096(3) Uani 0.763(9) 1 d PDU B 1 H20A H 0.4392 0.7529 0.3583 0.145 Uiso 0.763(9) 1 calc PR B 1 H20B H 0.4170 0.8944 0.3732 0.145 Uiso 0.763(9) 1 calc PR B 1 H20C H 0.4894 0.8625 0.3680 0.145 Uiso 0.763(9) 1 calc PR B 1 C21 C 0.4605(5) 1.0377(6) 0.2244(8) 0.125(4) Uani 0.763(9) 1 d PDU B 1 H21A H 0.4988 1.0624 0.2509 0.187 Uiso 0.763(9) 1 calc PR B 1 H21B H 0.4257 1.0861 0.2457 0.187 Uiso 0.763(9) 1 calc PR B 1 H21C H 0.4643 1.0543 0.1683 0.187 Uiso 0.763(9) 1 calc PR B 1 C22 C 0.5171(2) 0.7814(7) 0.2063(5) 0.071(2) Uani 0.763(9) 1 d PDU B 1 H22A H 0.5119 0.6917 0.2176 0.107 Uiso 0.763(9) 1 calc PR B 1 H22B H 0.5537 0.8132 0.2338 0.107 Uiso 0.763(9) 1 calc PR B 1 H22C H 0.5224 0.7932 0.1499 0.107 Uiso 0.763(9) 1 calc PR B 1 C20' C 0.4379(12) 0.950(3) 0.3380(11) 0.105(7) Uani 0.237(9) 1 d PDU B 2 H20D H 0.4109 1.0231 0.3325 0.158 Uiso 0.237(9) 1 calc PR B 2 H20E H 0.4787 0.9763 0.3568 0.158 Uiso 0.237(9) 1 calc PR B 2 H20F H 0.4195 0.8908 0.3756 0.158 Uiso 0.237(9) 1 calc PR B 2 C21' C 0.4920(12) 0.984(3) 0.1788(14) 0.104(7) Uani 0.237(9) 1 d PDU B 2 H21D H 0.4636 1.0434 0.1540 0.156 Uiso 0.237(9) 1 calc PR B 2 H21E H 0.5148 0.9376 0.1383 0.156 Uiso 0.237(9) 1 calc PR B 2 H21F H 0.5214 1.0292 0.2120 0.156 Uiso 0.237(9) 1 calc PR B 2 C22' C 0.5009(10) 0.7389(17) 0.2631(19) 0.100(6) Uani 0.237(9) 1 d PDU B 2 H22D H 0.5066 0.6863 0.2167 0.149 Uiso 0.237(9) 1 calc PR B 2 H22E H 0.4839 0.6880 0.3057 0.149 Uiso 0.237(9) 1 calc PR B 2 H22F H 0.5410 0.7738 0.2791 0.149 Uiso 0.237(9) 1 calc PR B 2 H106 H 0.451(2) 0.532(4) 0.110(3) 0.068(14) Uiso 1 1 d . . . H107 H 0.455(3) 0.596(6) 0.041(4) 0.089(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.053(2) 0.054(2) 0.0539(18) 0.0101(15) -0.0016(16) 0.0060(16) Li2 0.0434(17) 0.0403(18) 0.043(2) 0.0001(15) 0.0028(13) 0.0006(13) Li3 0.0434(17) 0.0381(18) 0.0497(17) -0.0030(15) 0.0004(15) 0.0059(14) Li4 0.0443(18) 0.0436(19) 0.0506(19) -0.0025(14) 0.0056(16) 0.0000(15) O2 0.0415(15) 0.0384(16) 0.059(2) -0.0063(14) 0.0067(15) 0.0006(13) C6 0.055(5) 0.068(4) 0.060(3) -0.001(3) 0.020(3) -0.002(3) C7 0.043(2) 0.031(2) 0.082(3) -0.0146(19) -0.007(2) 0.0014(17) C9 0.061(3) 0.052(3) 0.125(5) -0.037(4) -0.024(4) -0.005(3) C8 0.043(2) 0.047(4) 0.108(6) -0.014(4) -0.012(3) 0.001(2) C10 0.061(4) 0.038(3) 0.095(4) 0.015(3) -0.008(3) -0.004(3) O2' 0.039(3) 0.037(3) 0.070(5) -0.011(3) 0.000(3) -0.003(3) C6' 0.059(11) 0.039(5) 0.077(10) 0.001(8) -0.010(8) 0.003(6) C7' 0.041(4) 0.048(5) 0.068(5) -0.012(4) -0.004(4) 0.006(4) C9' 0.036(5) 0.046(11) 0.093(13) -0.025(9) -0.006(6) 0.005(7) C8' 0.039(8) 0.067(9) 0.061(9) -0.012(7) -0.001(7) -0.002(8) C10' 0.048(11) 0.065(7) 0.071(9) 0.005(7) -0.005(8) -0.003(7) O1 0.0484(18) 0.073(2) 0.0635(18) 0.0273(17) -0.0034(14) -0.0068(15) C1 0.068(3) 0.058(3) 0.063(5) 0.014(3) -0.014(3) 0.010(3) C2 0.058(3) 0.081(3) 0.060(3) 0.030(2) -0.010(2) -0.027(2) C3 0.080(4) 0.077(4) 0.060(3) 0.011(3) -0.015(3) -0.019(3) C4 0.089(5) 0.103(4) 0.083(5) 0.019(4) -0.016(4) -0.055(4) C5 0.056(3) 0.113(4) 0.043(3) 0.011(3) -0.003(2) -0.011(3) O1' 0.054(5) 0.097(4) 0.060(3) 0.027(4) -0.005(3) -0.003(4) C1' 0.061(6) 0.139(11) 0.069(9) 0.019(10) 0.013(7) 0.003(7) C2' 0.063(5) 0.077(5) 0.057(4) 0.025(4) -0.015(4) -0.018(4) C3' 0.108(10) 0.102(6) 0.067(10) 0.014(9) -0.014(10) -0.052(8) C4' 0.075(10) 0.077(10) 0.057(6) 0.023(7) -0.014(6) -0.026(9) C5' 0.070(7) 0.072(10) 0.059(9) 0.024(9) -0.016(7) 0.002(6) C23 0.0478(15) 0.0357(15) 0.065(2) -0.0012(14) 0.0021(17) -0.0015(13) Si4 0.0443(5) 0.0308(5) 0.0586(6) 0.0021(5) 0.0024(5) 0.0006(4) C26 0.0518(18) 0.0411(19) 0.072(3) 0.0072(19) 0.0073(18) 0.0077(16) C25 0.067(3) 0.048(2) 0.072(2) 0.000(2) -0.007(2) 0.0002(18) C24 0.059(2) 0.044(2) 0.086(3) 0.004(2) 0.011(2) -0.0075(18) C11 0.0552(19) 0.038(2) 0.035(3) 0.005(2) 0.0029(17) 0.0124(17) Si1 0.0486(14) 0.0314(15) 0.063(2) 0.0003(13) 0.0046(13) 0.0008(10) C12 0.093(6) 0.067(5) 0.137(10) 0.029(6) 0.022(6) -0.030(5) C13 0.049(5) 0.045(4) 0.074(7) 0.005(4) -0.018(4) -0.003(3) C14 0.058(4) 0.084(6) 0.064(4) -0.026(4) -0.017(3) 0.010(4) C11' 0.052(2) 0.037(3) 0.047(3) 0.014(3) 0.006(2) 0.008(2) Si1' 0.040(2) 0.039(3) 0.085(5) 0.001(3) -0.003(2) -0.0066(16) C12' 0.097(9) 0.055(6) 0.146(12) 0.015(9) 0.001(8) -0.033(6) C13' 0.041(7) 0.060(7) 0.061(9) 0.020(7) 0.006(6) 0.002(6) C14' 0.058(5) 0.066(7) 0.075(5) -0.022(5) -0.012(4) 0.002(4) C15 0.039(3) 0.049(4) 0.0479(19) 0.005(2) 0.0037(17) -0.002(2) Si2 0.058(3) 0.0221(16) 0.0416(17) 0.0044(12) 0.0040(13) -0.0031(14) C18 0.079(8) 0.041(4) 0.077(9) 0.015(4) 0.008(6) 0.006(4) C16 0.081(8) 0.037(5) 0.075(5) -0.002(3) 0.035(5) -0.008(4) C17 0.064(5) 0.066(5) 0.074(6) 0.020(5) -0.008(4) -0.031(4) C15' 0.042(3) 0.049(3) 0.052(3) 0.011(3) 0.004(2) -0.001(3) Si2' 0.018(2) 0.046(3) 0.047(2) -0.0009(18) -0.0017(16) -0.0030(19) C18' 0.068(8) 0.057(5) 0.055(8) 0.010(5) 0.019(6) 0.018(6) C16' 0.079(9) 0.041(6) 0.054(4) -0.005(4) 0.010(5) -0.029(6) C17' 0.051(5) 0.098(10) 0.059(8) 0.020(7) -0.023(5) -0.037(6) C19 0.0396(15) 0.0656(18) 0.0542(17) -0.0100(15) 0.0042(14) 0.0044(15) Si3 0.0388(5) 0.0422(5) 0.0458(6) 0.0015(5) -0.0020(4) -0.0037(4) C20 0.078(5) 0.158(8) 0.054(3) 0.001(4) -0.015(3) -0.017(5) C21 0.125(8) 0.043(3) 0.205(11) 0.026(5) -0.032(7) -0.011(3) C22 0.037(2) 0.085(4) 0.092(5) -0.028(4) -0.012(3) 0.002(3) C20' 0.102(14) 0.138(16) 0.076(9) -0.050(10) 0.001(8) -0.031(12) C21' 0.103(14) 0.092(13) 0.118(13) 0.033(11) 0.017(11) -0.040(10) C22' 0.081(11) 0.082(10) 0.136(16) 0.015(9) -0.046(11) 0.018(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 O1 2.015(7) . ? Li1 O1' 2.180(16) . ? Li1 C11' 2.310(14) . ? Li1 C19 2.349(9) . ? Li1 C11 2.364(10) . ? Li1 C23 2.375(8) . ? Li1 Li3 2.555(9) . ? Li1 Li4 2.566(10) . ? Li1 Li2 2.711(9) . ? Li1 H11A 2.2439 . ? Li1 H11C 2.1664 . ? Li1 H106 2.30(5) . ? Li2 O2 2.028(7) . ? Li2 O2' 2.065(14) . ? Li2 C11' 2.084(16) . ? Li2 C19 2.291(7) . ? Li2 C11 2.320(10) . ? Li2 C15' 2.331(12) . ? Li2 C15 2.459(10) . ? Li2 Li4 2.547(9) . ? Li2 Li3 2.623(8) . ? Li2 H11B 2.3000 . ? Li2 H11D 1.9597 . ? Li2 H15A 2.2166 . ? Li2 H15D 2.2105 . ? Li2 H19B 2.1406 . ? Li3 C15' 2.097(15) . ? Li3 C19 2.163(8) . ? Li3 C23 2.203(7) . ? Li3 C15 2.283(11) . ? Li3 Li4 2.379(9) . ? Li3 Si2' 2.939(12) . ? Li3 H15D 2.3202 . ? Li3 H107 2.10(6) . ? Li4 C11' 1.903(17) . ? Li4 C15 2.059(11) . ? Li4 C23 2.187(7) . ? Li4 C11 2.277(10) . ? Li4 C15' 2.409(17) . ? Li4 C14' 2.674(15) . ? Li4 H11C 2.2467 . ? Li4 H15B 1.9867 . ? O2 C6 1.414(8) . ? O2 C7 1.458(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.517(7) . ? C7 C8 1.528(7) . ? C7 C10 1.532(9) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O2' C6' 1.429(16) . ? O2' C7' 1.465(14) . ? C6' H6D 0.9800 . ? C6' H6E 0.9800 . ? C6' H6F 0.9800 . ? C7' C8' 1.523(14) . ? C7' C9' 1.527(15) . ? C7' C10' 1.539(15) . ? C9' H9D 0.9800 . ? C9' H9E 0.9800 . ? C9' H9F 0.9800 . ? C8' H8D 0.9800 . ? C8' H8E 0.9800 . ? C8' H8F 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? O1 C1 1.418(5) . ? O1 C2 1.458(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C4 1.501(5) . ? C2 C3 1.503(5) . ? C2 C5 1.554(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? O1' C1' 1.430(7) . ? O1' C2' 1.458(6) . ? C1' H1D 0.9800 . ? C1' H1E 0.9800 . ? C1' H1F 0.9800 . ? C2' C3' 1.514(5) . ? C2' C4' 1.519(5) . ? C2' C5' 1.520(5) . ? C3' H3D 0.9800 . ? C3' H3E 0.9800 . ? C3' H3F 0.9800 . ? C4' H4D 0.9800 . ? C4' H4E 0.9800 . ? C4' H4F 0.9800 . ? C5' H5D 0.9800 . ? C5' H5E 0.9800 . ? C5' H5F 0.9800 . ? C23 Si4 1.874(4) . ? C23 H106 0.95(6) . ? C23 H107 0.92(6) . ? Si4 C25 1.869(5) . ? Si4 C26 1.878(4) . ? Si4 C24 1.881(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C11 Si1 1.898(7) . ? C11 H11A 0.9609 . ? C11 H11B 0.9541 . ? C11 H11C 0.8025 . ? C11 H11D 0.7874 . ? Si1 C13 1.868(8) . ? Si1 C12 1.868(8) . ? Si1 C14 1.884(7) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C11' Si1' 1.940(11) . ? C11' H11A 1.2096 . ? C11' H11B 1.2460 . ? C11' H11C 0.9600 . ? C11' H11D 0.9602 . ? Si1' C12' 1.851(11) . ? Si1' C13' 1.868(11) . ? Si1' C14' 1.903(11) . ? C12' H12D 0.9800 . ? C12' H12E 0.9800 . ? C12' H12F 0.9800 . ? C13' H13D 0.9800 . ? C13' H13E 0.9800 . ? C13' H13F 0.9800 . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15 Si2 1.876(7) . ? C15 H15A 0.9901 . ? C15 H15B 0.9899 . ? Si2 C16 1.845(8) . ? Si2 C18 1.879(8) . ? Si2 C17 1.888(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C15' Si2' 1.856(10) . ? C15' H15C 0.9601 . ? C15' H15D 0.9600 . ? Si2' C16' 1.838(11) . ? Si2' C18' 1.891(11) . ? Si2' C17' 1.914(10) . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? C16' H16D 0.9800 . ? C16' H16E 0.9800 . ? C16' H16F 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? C19 Si3 1.856(4) . ? C19 H19A 0.9901 . ? C19 H19B 0.9901 . ? Si3 C21 1.835(6) . ? Si3 C22' 1.863(12) . ? Si3 C20 1.866(7) . ? Si3 C22 1.881(5) . ? Si3 C21' 1.883(11) . ? Si3 C20' 1.889(12) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C20' H20D 0.9800 . ? C20' H20E 0.9800 . ? C20' H20F 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li1 O1' 29.8(4) . . ? O1 Li1 C11' 128.5(5) . . ? O1' Li1 C11' 112.1(6) . . ? O1 Li1 C19 116.5(4) . . ? O1' Li1 C19 102.4(5) . . ? C11' Li1 C19 101.3(5) . . ? O1 Li1 C11 119.1(4) . . ? O1' Li1 C11 102.2(5) . . ? C11' Li1 C11 10.0(4) . . ? C19 Li1 C11 105.5(3) . . ? O1 Li1 C23 107.7(3) . . ? O1' Li1 C23 137.5(5) . . ? C11' Li1 C23 95.8(5) . . ? C19 Li1 C23 102.7(3) . . ? C11 Li1 C23 103.3(3) . . ? O1 Li1 Li3 139.9(4) . . ? O1' Li1 Li3 150.0(6) . . ? C11' Li1 Li3 90.7(4) . . ? C19 Li1 Li3 52.1(2) . . ? C11 Li1 Li3 100.5(3) . . ? C23 Li1 Li3 52.9(2) . . ? O1 Li1 Li4 146.1(4) . . ? O1' Li1 Li4 154.1(5) . . ? C11' Li1 Li4 45.6(4) . . ? C19 Li1 Li4 96.1(3) . . ? C11 Li1 Li4 54.8(3) . . ? C23 Li1 Li4 52.4(2) . . ? Li3 Li1 Li4 55.4(2) . . ? O1 Li1 Li2 151.4(4) . . ? O1' Li1 Li2 121.7(5) . . ? C11' Li1 Li2 48.2(4) . . ? C19 Li1 Li2 53.3(2) . . ? C11 Li1 Li2 53.9(3) . . ? C23 Li1 Li2 100.7(3) . . ? Li3 Li1 Li2 59.7(2) . . ? Li4 Li1 Li2 57.6(2) . . ? O1 Li1 H11A 98.9 . . ? O1' Li1 H11A 90.1 . . ? C11' Li1 H11A 30.8 . . ? C19 Li1 H11A 128.7 . . ? C11 Li1 H11A 23.9 . . ? C23 Li1 H11A 100.0 . . ? Li3 Li1 H11A 117.7 . . ? Li4 Li1 H11A 64.1 . . ? Li2 Li1 H11A 77.8 . . ? O1 Li1 H11C 106.5 . . ? O1' Li1 H11C 98.3 . . ? C11' Li1 H11C 24.5 . . ? C19 Li1 H11C 125.1 . . ? C11 Li1 H11C 19.8 . . ? C23 Li1 H11C 94.5 . . ? Li3 Li1 H11C 109.5 . . ? Li4 Li1 H11C 55.9 . . ? Li2 Li1 H11C 72.6 . . ? H11A Li1 H11C 8.2 . . ? O1 Li1 H106 86.6(14) . . ? O1' Li1 H106 116.1(15) . . ? C11' Li1 H106 117.5(15) . . ? C19 Li1 H106 104.6(12) . . ? C11 Li1 H106 123.8(14) . . ? C23 Li1 H106 23.4(14) . . ? Li3 Li1 H106 64.8(13) . . ? Li4 Li1 H106 75.7(14) . . ? Li2 Li1 H106 121.0(14) . . ? H11A Li1 H106 113.9 . . ? H11C Li1 H106 110.6 . . ? O2 Li2 O2' 23.6(4) . . ? O2 Li2 C11' 116.1(5) . . ? O2' Li2 C11' 131.3(6) . . ? O2 Li2 C19 103.0(3) . . ? O2' Li2 C19 107.2(5) . . ? C11' Li2 C19 110.8(5) . . ? O2 Li2 C11 109.1(3) . . ? O2' Li2 C11 126.4(5) . . ? C11' Li2 C11 8.8(5) . . ? C19 Li2 C11 108.9(3) . . ? O2 Li2 C15' 126.4(5) . . ? O2' Li2 C15' 102.8(6) . . ? C11' Li2 C15' 103.8(7) . . ? C19 Li2 C15' 94.0(5) . . ? C11 Li2 C15' 112.6(6) . . ? O2 Li2 C15 132.0(4) . . ? O2' Li2 C15 109.2(5) . . ? C11' Li2 C15 91.5(6) . . ? C19 Li2 C15 102.2(3) . . ? C11 Li2 C15 100.3(4) . . ? C15' Li2 C15 12.9(4) . . ? O2 Li2 Li4 157.4(3) . . ? O2' Li2 Li4 150.1(5) . . ? C11' Li2 Li4 47.2(5) . . ? C19 Li2 Li4 98.1(3) . . ? C11 Li2 Li4 55.6(3) . . ? C15' Li2 Li4 59.0(5) . . ? C15 Li2 Li4 48.5(3) . . ? O2 Li2 Li3 147.4(3) . . ? O2' Li2 Li3 133.8(5) . . ? C11' Li2 Li3 94.1(5) . . ? C19 Li2 Li3 51.7(2) . . ? C11 Li2 Li3 99.7(3) . . ? C15' Li2 Li3 49.7(4) . . ? C15 Li2 Li3 53.3(3) . . ? Li4 Li2 Li3 54.8(2) . . ? O2 Li2 Li1 130.1(3) . . ? O2' Li2 Li1 151.0(5) . . ? C11' Li2 Li1 55.8(4) . . ? C19 Li2 Li1 55.2(2) . . ? C11 Li2 Li1 55.4(3) . . ? C15' Li2 Li1 101.4(4) . . ? C15 Li2 Li1 97.8(3) . . ? Li4 Li2 Li1 58.3(2) . . ? Li3 Li2 Li1 57.2(2) . . ? O2 Li2 H11B 88.0 . . ? O2' Li2 H11B 108.9 . . ? C11' Li2 H11B 32.5 . . ? C19 Li2 H11B 104.3 . . ? C11 Li2 H11B 23.8 . . ? C15' Li2 H11B 136.3 . . ? C15 Li2 H11B 123.8 . . ? Li4 Li2 H11B 79.1 . . ? Li3 Li2 H11B 115.9 . . ? Li1 Li2 H11B 61.4 . . ? O2 Li2 H11D 90.7 . . ? O2' Li2 H11D 110.0 . . ? C11' Li2 H11D 27.3 . . ? C19 Li2 H11D 110.2 . . ? C11 Li2 H11D 18.9 . . ? C15' Li2 H11D 130.1 . . ? C15 Li2 H11D 117.4 . . ? Li4 Li2 H11D 74.4 . . ? Li3 Li2 H11D 115.8 . . ? Li1 Li2 H11D 64.0 . . ? H11B Li2 H11D 7.3 . . ? O2 Li2 H15A 108.4 . . ? O2' Li2 H15A 85.5 . . ? C11' Li2 H15A 107.3 . . ? C19 Li2 H15A 111.3 . . ? C11 Li2 H15A 115.5 . . ? C15' Li2 H15A 21.3 . . ? C15 Li2 H15A 23.7 . . ? Li4 Li2 H15A 70.5 . . ? Li3 Li2 H15A 70.9 . . ? Li1 Li2 H15A 121.2 . . ? H11B Li2 H15A 135.6 . . ? H11D Li2 H15A 128.3 . . ? O2 Li2 H15D 107.0 . . ? O2' Li2 H15D 84.1 . . ? C11' Li2 H15D 128.1 . . ? C19 Li2 H15D 85.0 . . ? C11 Li2 H15D 136.8 . . ? C15' Li2 H15D 24.2 . . ? C15 Li2 H15D 36.7 . . ? Li4 Li2 H15D 82.6 . . ? Li3 Li2 H15D 56.6 . . ? Li1 Li2 H15D 113.8 . . ? H11B Li2 H15D 160.4 . . ? H11D Li2 H15D 153.8 . . ? H15A Li2 H15D 27.9 . . ? O2 Li2 H19B 88.5 . . ? O2' Li2 H19B 85.5 . . ? C11' Li2 H19B 136.3 . . ? C19 Li2 H19B 25.5 . . ? C11 Li2 H19B 134.2 . . ? C15' Li2 H19B 85.9 . . ? C15 Li2 H19B 97.5 . . ? Li4 Li2 H19B 114.0 . . ? Li3 Li2 H19B 59.8 . . ? Li1 Li2 H19B 80.6 . . ? H11B Li2 H19B 125.3 . . ? H11D Li2 H19B 132.1 . . ? H15A Li2 H19B 96.9 . . ? H15D Li2 H19B 69.0 . . ? C15' Li3 C19 105.0(5) . . ? C15' Li3 C23 115.7(6) . . ? C19 Li3 C23 115.4(3) . . ? C15' Li3 C15 13.6(4) . . ? C19 Li3 C15 112.6(4) . . ? C23 Li3 C15 102.1(4) . . ? C15' Li3 Li4 64.8(6) . . ? C19 Li3 Li4 107.2(3) . . ? C23 Li3 Li4 56.9(2) . . ? C15 Li3 Li4 52.4(3) . . ? C15' Li3 Li1 114.0(4) . . ? C19 Li3 Li1 59.0(3) . . ? C23 Li3 Li1 59.3(3) . . ? C15 Li3 Li1 107.3(3) . . ? Li4 Li3 Li1 62.5(3) . . ? C15' Li3 Li2 57.9(3) . . ? C19 Li3 Li2 56.2(2) . . ? C23 Li3 Li2 108.4(3) . . ? C15 Li3 Li2 59.7(3) . . ? Li4 Li3 Li2 61.0(2) . . ? Li1 Li3 Li2 63.1(2) . . ? C15' Li3 Si2' 38.9(3) . . ? C19 Li3 Si2' 132.9(3) . . ? C23 Li3 Si2' 109.4(3) . . ? C15 Li3 Si2' 41.5(3) . . ? Li4 Li3 Si2' 85.1(3) . . ? Li1 Li3 Si2' 147.0(3) . . ? Li2 Li3 Si2' 96.6(3) . . ? C15' Li3 H15D 24.4 . . ? C19 Li3 H15D 85.4 . . ? C23 Li3 H15D 139.2 . . ? C15 Li3 H15D 37.7 . . ? Li4 Li3 H15D 84.2 . . ? Li1 Li3 H15D 115.8 . . ? Li2 Li3 H15D 52.7 . . ? Si2' Li3 H15D 49.9 . . ? C15' Li3 H107 117.7(17) . . ? C19 Li3 H107 131.2(17) . . ? C23 Li3 H107 24.4(17) . . ? C15 Li3 H107 105.8(16) . . ? Li4 Li3 H107 73.9(16) . . ? Li1 Li3 H107 81.9(17) . . ? Li2 Li3 H107 131.6(17) . . ? Si2' Li3 H107 95.9(17) . . ? H15D Li3 H107 141.2 . . ? C11' Li4 C15 111.0(6) . . ? C11' Li4 C23 116.2(5) . . ? C15 Li4 C23 110.4(4) . . ? C11' Li4 C11 4.6(6) . . ? C15 Li4 C11 115.5(4) . . ? C23 Li4 C11 112.7(4) . . ? C11' Li4 Li3 107.6(5) . . ? C15 Li4 Li3 61.4(4) . . ? C23 Li4 Li3 57.5(2) . . ? C11 Li4 Li3 108.6(3) . . ? C11' Li4 C15' 106.9(6) . . ? C15 Li4 C15' 11.0(4) . . ? C23 Li4 C15' 104.7(4) . . ? C11 Li4 C15' 111.2(4) . . ? Li3 Li4 C15' 51.9(4) . . ? C11' Li4 Li2 53.5(5) . . ? C15 Li4 Li2 63.5(4) . . ? C23 Li4 Li2 111.7(3) . . ? C11 Li4 Li2 57.2(3) . . ? Li3 Li4 Li2 64.2(2) . . ? C15' Li4 Li2 56.0(4) . . ? C11' Li4 Li1 60.1(4) . . ? C15 Li4 Li1 114.5(5) . . ? C23 Li4 Li1 59.3(3) . . ? C11 Li4 Li1 58.1(3) . . ? Li3 Li4 Li1 62.1(3) . . ? C15' Li4 Li1 103.5(5) . . ? Li2 Li4 Li1 64.1(3) . . ? C11' Li4 C14' 82.1(5) . . ? C15 Li4 C14' 93.0(6) . . ? C23 Li4 C14' 140.1(4) . . ? C11 Li4 C14' 82.9(4) . . ? Li3 Li4 C14' 154.4(5) . . ? C15' Li4 C14' 102.8(6) . . ? Li2 Li4 C14' 107.6(4) . . ? Li1 Li4 C14' 138.7(5) . . ? C11' Li4 H11C 25.0 . . ? C15 Li4 H11C 135.8 . . ? C23 Li4 H11C 97.7 . . ? C11 Li4 H11C 20.4 . . ? Li3 Li4 H11C 113.2 . . ? C15' Li4 H11C 130.5 . . ? Li2 Li4 H11C 74.8 . . ? Li1 Li4 H11C 53.0 . . ? C14' Li4 H11C 85.7 . . ? C11' Li4 H15B 113.1 . . ? C15 Li4 H15B 28.3 . . ? C23 Li4 H15B 126.2 . . ? C11 Li4 H15B 117.4 . . ? Li3 Li4 H15B 88.3 . . ? C15' Li4 H15B 39.1 . . ? Li2 Li4 H15B 81.6 . . ? Li1 Li4 H15B 141.5 . . ? C14' Li4 H15B 66.1 . . ? H11C Li4 H15B 135.5 . . ? C6 O2 C7 114.3(5) . . ? C6 O2 Li2 113.5(4) . . ? C7 O2 Li2 129.9(4) . . ? O2 C6 H6A 109.5 . . ? O2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? O2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O2 C7 C9 111.3(5) . . ? O2 C7 C8 111.4(4) . . ? C9 C7 C8 111.7(5) . . ? O2 C7 C10 103.8(5) . . ? C9 C7 C10 109.3(5) . . ? C8 C7 C10 109.0(6) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6' O2' C7' 110.3(15) . . ? C6' O2' Li2 118.2(15) . . ? C7' O2' Li2 123.0(11) . . ? O2' C6' H6D 109.5 . . ? O2' C6' H6E 109.5 . . ? H6D C6' H6E 109.5 . . ? O2' C6' H6F 109.5 . . ? H6D C6' H6F 109.5 . . ? H6E C6' H6F 109.5 . . ? O2' C7' C8' 112.0(13) . . ? O2' C7' C9' 109.6(15) . . ? C8' C7' C9' 109.8(15) . . ? O2' C7' C10' 103.9(16) . . ? C8' C7' C10' 114.0(17) . . ? C9' C7' C10' 107.3(16) . . ? C7' C9' H9D 109.5 . . ? C7' C9' H9E 109.5 . . ? H9D C9' H9E 109.5 . . ? C7' C9' H9F 109.5 . . ? H9D C9' H9F 109.5 . . ? H9E C9' H9F 109.5 . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? C7' C10' H10D 109.5 . . ? C7' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C1 O1 C2 116.7(4) . . ? C1 O1 Li1 118.9(4) . . ? C2 O1 Li1 123.5(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C4 110.7(4) . . ? O1 C2 C3 110.4(4) . . ? C4 C2 C3 112.9(5) . . ? O1 C2 C5 104.5(4) . . ? C4 C2 C5 109.6(4) . . ? C3 C2 C5 108.4(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1' O1' C2' 112.5(8) . . ? C1' O1' Li1 102.3(13) . . ? C2' O1' Li1 124.9(10) . . ? O1' C1' H1D 109.5 . . ? O1' C1' H1E 109.5 . . ? H1D C1' H1E 109.5 . . ? O1' C1' H1F 109.5 . . ? H1D C1' H1F 109.5 . . ? H1E C1' H1F 109.5 . . ? O1' C2' C3' 109.4(7) . . ? O1' C2' C4' 107.4(7) . . ? C3' C2' C4' 110.9(7) . . ? O1' C2' C5' 107.4(7) . . ? C3' C2' C5' 110.5(7) . . ? C4' C2' C5' 111.1(7) . . ? C2' C3' H3D 109.5 . . ? C2' C3' H3E 109.5 . . ? H3D C3' H3E 109.5 . . ? C2' C3' H3F 109.5 . . ? H3D C3' H3F 109.5 . . ? H3E C3' H3F 109.5 . . ? C2' C4' H4D 109.5 . . ? C2' C4' H4E 109.5 . . ? H4D C4' H4E 109.5 . . ? C2' C4' H4F 109.5 . . ? H4D C4' H4F 109.5 . . ? H4E C4' H4F 109.5 . . ? C2' C5' H5D 109.5 . . ? C2' C5' H5E 109.5 . . ? H5D C5' H5E 109.5 . . ? C2' C5' H5F 109.5 . . ? H5D C5' H5F 109.5 . . ? H5E C5' H5F 109.5 . . ? Si4 C23 Li4 99.4(2) . . ? Si4 C23 Li3 161.7(3) . . ? Li4 C23 Li3 65.6(2) . . ? Si4 C23 Li1 118.1(3) . . ? Li4 C23 Li1 68.3(3) . . ? Li3 C23 Li1 67.7(3) . . ? Si4 C23 H106 93(3) . . ? Li4 C23 H106 142(3) . . ? Li3 C23 H106 105(3) . . ? Li1 C23 H106 74(3) . . ? Si4 C23 H107 108(4) . . ? Li4 C23 H107 114(4) . . ? Li3 C23 H107 71(4) . . ? Li1 C23 H107 132(4) . . ? H106 C23 H107 95(4) . . ? C25 Si4 C23 108.5(2) . . ? C25 Si4 C26 108.2(2) . . ? C23 Si4 C26 115.76(19) . . ? C25 Si4 C24 107.6(2) . . ? C23 Si4 C24 112.0(2) . . ? C26 Si4 C24 104.38(19) . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C25 H25A 109.5 . . ? Si4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C11 Li4 96.9(3) . . ? Si1 C11 Li2 111.0(4) . . ? Li4 C11 Li2 67.3(3) . . ? Si1 C11 Li1 162.4(4) . . ? Li4 C11 Li1 67.1(3) . . ? Li2 C11 Li1 70.7(3) . . ? Si1 C11 H11A 104.9 . . ? Li4 C11 H11A 96.2 . . ? Li2 C11 H11A 141.8 . . ? Li1 C11 H11A 71.0 . . ? Si1 C11 H11B 105.4 . . ? Li4 C11 H11B 142.8 . . ? Li2 C11 H11B 76.9 . . ? Li1 C11 H11B 92.1 . . ? H11A C11 H11B 106.1 . . ? Si1 C11 H11C 104.3 . . ? Li4 C11 H11C 77.6 . . ? Li2 C11 H11C 132.2 . . ? Li1 C11 H11C 66.1 . . ? H11A C11 H11C 18.7 . . ? H11B C11 H11C 123.2 . . ? Si1 C11 H11D 100.0 . . ? Li4 C11 H11D 120.9 . . ? Li2 C11 H11D 53.7 . . ? Li1 C11 H11D 94.9 . . ? H11A C11 H11D 132.0 . . ? H11B C11 H11D 26.7 . . ? H11C C11 H11D 147.3 . . ? C13 Si1 C12 106.9(6) . . ? C13 Si1 C14 106.7(7) . . ? C12 Si1 C14 108.6(5) . . ? C13 Si1 C11 109.9(5) . . ? C12 Si1 C11 115.3(5) . . ? C14 Si1 C11 109.1(4) . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Li4 C11' Si1' 96.3(6) . . ? Li4 C11' Li2 79.3(6) . . ? Si1' C11' Li2 113.6(7) . . ? Li4 C11' Li1 74.3(5) . . ? Si1' C11' Li1 165.5(9) . . ? Li2 C11' Li1 76.0(4) . . ? Li4 C11' H11A 108.9 . . ? Si1' C11' H11A 102.1 . . ? Li2 C11' H11A 142.5 . . ? Li1 C11' H11A 71.6 . . ? Li4 C11' H11B 157.5 . . ? Si1' C11' H11B 103.7 . . ? Li2 C11' H11B 83.3 . . ? Li1 C11' H11B 87.8 . . ? H11A C11' H11B 77.1 . . ? Li4 C11' H11C 97.9 . . ? Si1' C11' H11C 101.8 . . ? Li2 C11' H11C 144.6 . . ? Li1 C11' H11C 69.4 . . ? H11A C11' H11C 11.2 . . ? H11B C11' H11C 88.1 . . ? Li4 C11' H11D 148.1 . . ? Si1' C11' H11D 100.0 . . ? Li2 C11' H11D 69.2 . . ? Li1 C11' H11D 93.5 . . ? H11A C11' H11D 94.2 . . ? H11B C11' H11D 17.1 . . ? H11C C11' H11D 105.2 . . ? C12' Si1' C13' 107.7(10) . . ? C12' Si1' C14' 107.5(9) . . ? C13' Si1' C14' 104.1(10) . . ? C12' Si1' C11' 120.7(8) . . ? C13' Si1' C11' 110.0(10) . . ? C14' Si1' C11' 105.6(6) . . ? Si1' C12' H12D 109.5 . . ? Si1' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? Si1' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? Si1' C13' H13D 109.5 . . ? Si1' C13' H13E 109.5 . . ? H13D C13' H13E 109.5 . . ? Si1' C13' H13F 109.5 . . ? H13D C13' H13F 109.5 . . ? H13E C13' H13F 109.5 . . ? Si1' C14' Li4 75.3(5) . . ? Si1' C14' H14D 109.5 . . ? Li4 C14' H14D 81.1 . . ? Si1' C14' H14E 109.5 . . ? Li4 C14' H14E 56.1 . . ? H14D C14' H14E 109.5 . . ? Si1' C14' H14F 109.5 . . ? Li4 C14' H14F 165.1 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? Si2 C15 Li4 130.3(5) . . ? Si2 C15 Li3 85.6(4) . . ? Li4 C15 Li3 66.2(3) . . ? Si2 C15 Li2 137.8(7) . . ? Li4 C15 Li2 68.0(3) . . ? Li3 C15 Li2 67.0(3) . . ? Si2 C15 H15A 102.1 . . ? Li4 C15 H15A 126.1 . . ? Li3 C15 H15A 113.4 . . ? Li2 C15 H15A 64.2 . . ? Si2 C15 H15B 108.9 . . ? Li4 C15 H15B 71.8 . . ? Li3 C15 H15B 134.0 . . ? Li2 C15 H15B 113.2 . . ? H15A C15 H15B 105.8 . . ? Si2 C15 H15C 106.5 . . ? Li4 C15 H15C 120.3 . . ? Li3 C15 H15C 145.0 . . ? Li2 C15 H15C 83.3 . . ? H15A C15 H15C 32.7 . . ? H15B C15 H15C 73.9 . . ? Si2 C15 H15D 79.3 . . ? Li4 C15 H15D 124.5 . . ? Li3 C15 H15D 72.5 . . ? Li2 C15 H15D 62.5 . . ? H15A C15 H15D 45.9 . . ? H15B C15 H15D 151.5 . . ? H15C C15 H15D 77.6 . . ? C16 Si2 C15 109.5(4) . . ? C16 Si2 C18 107.9(6) . . ? C15 Si2 C18 117.0(6) . . ? C16 Si2 C17 107.0(6) . . ? C15 Si2 C17 110.1(5) . . ? C18 Si2 C17 104.7(7) . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2' C15' Li3 95.9(6) . . ? Si2' C15' Li2 166.9(10) . . ? Li3 C15' Li2 72.4(4) . . ? Si2' C15' Li4 115.6(8) . . ? Li3 C15' Li4 63.3(4) . . ? Li2 C15' Li4 65.0(4) . . ? Si2' C15' H15A 119.0 . . ? Li3 C15' H15A 143.7 . . ? Li2 C15' H15A 71.8 . . ? Li4 C15' H15A 105.6 . . ? Si2' C15' H15B 90.4 . . ? Li3 C15' H15B 114.1 . . ? Li2 C15' H15B 99.6 . . ? Li4 C15' H15B 55.3 . . ? H15A C15' H15B 77.7 . . ? Si2' C15' H15C 104.8 . . ? Li3 C15' H15C 149.4 . . ? Li2 C15' H15C 88.3 . . ? Li4 C15' H15C 87.2 . . ? H15A C15' H15C 33.8 . . ? H15B C15' H15C 44.8 . . ? Si2' C15' H15D 104.3 . . ? Li3 C15' H15D 90.9 . . ? Li2 C15' H15D 70.9 . . ? Li4 C15' H15D 133.6 . . ? H15A C15' H15D 72.1 . . ? H15B C15' H15D 149.8 . . ? H15C C15' H15D 105.3 . . ? C16' Si2' C15' 112.0(7) . . ? C16' Si2' C18' 106.5(10) . . ? C15' Si2' C18' 116.8(9) . . ? C16' Si2' C17' 106.5(8) . . ? C15' Si2' C17' 109.0(7) . . ? C18' Si2' C17' 105.3(10) . . ? C16' Si2' Li3 109.1(7) . . ? C15' Si2' Li3 45.2(5) . . ? C18' Si2' Li3 144.3(10) . . ? C17' Si2' Li3 66.9(6) . . ? Si2' C18' H18D 109.5 . . ? Si2' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? Si2' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Si2' C16' H16D 109.5 . . ? Si2' C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? Si2' C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? Si2' C17' H17D 109.5 . . ? Si2' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? Si2' C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? Si3 C19 Li3 105.3(2) . . ? Si3 C19 Li2 169.9(3) . . ? Li3 C19 Li2 72.1(2) . . ? Si3 C19 Li1 117.1(3) . . ? Li3 C19 Li1 68.9(3) . . ? Li2 C19 Li1 71.5(3) . . ? Si3 C19 H19A 101.9 . . ? Li3 C19 H19A 144.1 . . ? Li2 C19 H19A 84.7 . . ? Li1 C19 H19A 78.1 . . ? Si3 C19 H19B 102.0 . . ? Li3 C19 H19B 92.2 . . ? Li2 C19 H19B 68.7 . . ? Li1 C19 H19B 139.6 . . ? H19A C19 H19B 104.7 . . ? C21 Si3 C19 113.7(4) . . ? C21 Si3 C22' 130.9(8) . . ? C19 Si3 C22' 111.6(7) . . ? C21 Si3 C20 107.3(5) . . ? C19 Si3 C20 113.1(3) . . ? C22' Si3 C20 70.0(10) . . ? C21 Si3 C22 107.9(5) . . ? C19 Si3 C22 112.1(2) . . ? C22' Si3 C22 35.1(10) . . ? C20 Si3 C22 102.0(4) . . ? C21 Si3 C21' 37.2(9) . . ? C19 Si3 C21' 114.2(8) . . ? C22' Si3 C21' 105.7(9) . . ? C20 Si3 C21' 130.0(9) . . ? C22 Si3 C21' 74.2(10) . . ? C21 Si3 C20' 72.9(11) . . ? C19 Si3 C20' 117.1(8) . . ? C22' Si3 C20' 102.1(9) . . ? C20 Si3 C20' 36.7(9) . . ? C22 Si3 C20' 125.3(9) . . ? C21' Si3 C20' 104.8(9) . . ? Si3 C20 H20A 109.5 . . ? Si3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C20' H20D 109.5 . . ? Si3 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? Si3 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? Si3 C21' H21D 109.5 . . ? Si3 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? Si3 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? Si3 C22' H22D 109.5 . . ? Si3 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? Si3 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.594 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.051