# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email m.murugesu@uOttawa.ca _publ_contact_author_name 'Murale Murugesu' _publ_author_name 'Murale Murugesu' data_mm085 _database_code_depnum_ccdc_archive 'CCDC 864752' #TrackingRef 'mm085.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 Na2 O2 Si2' _chemical_formula_weight 438.70 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' Na Na 0.0362 0.0249 '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 Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.3962(2) _cell_length_b 20.1718(4) _cell_length_c 17.1472(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2558.27(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9939 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9689 _exptl_absorpt_correction_T_max 0.9725 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (650 frames), at phi = 120.00 deg (650 frames), and at phi = 240.00 deg (650 frames). Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20049 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1576 _reflns_number_gt 1322 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0665P)^2^+2.7777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1576 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Na1 Na 0.26106(11) 0.07342(4) 0.7500 0.0292(2) Uani 1 2 d S . . Si1 Si 0.0000 0.13857(3) 0.54614(4) 0.02544(19) Uani 1 2 d S . . O1 O 0.5000 -0.00349(11) 0.7500 0.0264(5) Uani 1 4 d S . . O2 O 0.5000 0.15376(11) 0.7500 0.0293(5) Uani 1 4 d S . . C1 C 0.0000 0.15614(10) 0.70882(13) 0.0214(4) Uani 1 2 d S . . H1 H 0.0000 0.1999 0.6884 0.026 Uiso 1 2 calc SR . . C2 C 0.0000 0.10761(11) 0.64824(12) 0.0222(4) Uani 1 2 d S . . C3 C 0.0000 0.03680(11) 0.65081(13) 0.0254(5) Uani 1 2 d S . . H3 H 0.0000 0.0181 0.5999 0.031 Uiso 1 2 calc SR . . C4 C 0.0000 -0.01249(10) 0.70872(14) 0.0256(5) Uani 1 2 d S . . H4 H 0.0000 -0.0560 0.6875 0.031 Uiso 1 2 calc SR . . C5 C 0.0000 0.23152(13) 0.54104(15) 0.0377(6) Uani 1 2 d S . . H5A H 0.0000 0.2456 0.4863 0.057 Uiso 1 2 calc SR . . H5B H 0.1082 0.2488 0.5671 0.057 Uiso 0.50 1 calc PR . . H5C H -0.1082 0.2488 0.5671 0.057 Uiso 0.50 1 calc PR . . C6 C 0.2038(3) 0.10879(10) 0.49093(11) 0.0397(4) Uani 1 1 d . . . H6A H 0.1997 0.1260 0.4375 0.060 Uiso 1 1 calc R . . H6B H 0.2041 0.0602 0.4896 0.060 Uiso 1 1 calc R . . H6C H 0.3137 0.1246 0.5168 0.060 Uiso 1 1 calc R . . C7 C 0.5000 -0.04532(14) 0.68111(16) 0.0404(6) Uani 1 2 d S . . H7A H 0.6088 -0.0368 0.6490 0.048 Uiso 0.50 1 calc PR . . H7B H 0.3912 -0.0368 0.6490 0.048 Uiso 0.50 1 calc PR . . C8 C 0.5000 -0.11371(18) 0.7104(3) 0.111(2) Uani 1 2 d S . . H8A H 0.3916 -0.1373 0.6909 0.133 Uiso 0.50 1 calc PR . . H8B H 0.6084 -0.1373 0.6909 0.133 Uiso 0.50 1 calc PR . . C9 C 0.5000 0.19546(14) 0.68126(16) 0.0410(6) Uani 1 2 d S . . H9A H 0.3913 0.1868 0.6492 0.049 Uiso 0.50 1 calc PR . . H9B H 0.6087 0.1868 0.6492 0.049 Uiso 0.50 1 calc PR . . C10 C 0.5000 0.26415(19) 0.7093(3) 0.111(2) Uani 1 2 d S . . H10A H 0.6085 0.2876 0.6897 0.133 Uiso 0.50 1 calc PR . . H10B H 0.3915 0.2876 0.6897 0.133 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0182(4) 0.0269(5) 0.0427(5) 0.000 0.000 0.0005(3) Si1 0.0290(3) 0.0254(3) 0.0219(3) -0.0007(2) 0.000 0.000 O1 0.0237(10) 0.0248(11) 0.0307(12) 0.000 0.000 0.000 O2 0.0276(11) 0.0256(11) 0.0346(13) 0.000 0.000 0.000 C1 0.0196(9) 0.0198(9) 0.0249(11) 0.0017(8) 0.000 0.000 C2 0.0200(9) 0.0240(11) 0.0227(10) -0.0001(9) 0.000 0.000 C3 0.0248(10) 0.0261(11) 0.0255(11) -0.0044(9) 0.000 0.000 C4 0.0237(9) 0.0189(10) 0.0343(12) -0.0041(9) 0.000 0.000 C5 0.0546(16) 0.0285(12) 0.0299(12) 0.0040(10) 0.000 0.000 C6 0.0434(10) 0.0404(10) 0.0352(9) -0.0028(8) 0.0122(8) -0.0016(8) C7 0.0404(14) 0.0431(15) 0.0376(15) -0.0118(12) 0.000 0.000 C8 0.224(8) 0.0286(17) 0.080(3) -0.0132(18) 0.000 0.000 C9 0.0425(14) 0.0445(15) 0.0360(14) 0.0075(12) 0.000 0.000 C10 0.233(8) 0.0321(18) 0.068(3) 0.0125(18) 0.000 0.000 _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 Na1 O1 2.3516(17) . ? Na1 O2 2.3978(18) . ? Na1 C1 2.6478(17) 10_557 ? Na1 C1 2.6478(17) . ? Na1 C3 2.6771(17) 10_557 ? Na1 C3 2.6771(17) . ? Na1 C4 2.6893(17) 10_557 ? Na1 C4 2.6893(17) . ? Na1 C2 2.6923(16) 10_557 ? Na1 C2 2.6923(16) . ? Na1 Na1 3.5345(17) 3_656 ? Na1 Na1 3.8617(17) 3_556 ? Si1 C2 1.859(2) . ? Si1 C5 1.877(3) . ? Si1 C6 1.8784(19) . ? Si1 C6 1.8785(19) 12 ? O1 C7 1.452(3) 10_557 ? O1 C7 1.452(3) . ? O1 Na1 2.3516(17) 3_656 ? O2 C9 1.448(3) . ? O2 C9 1.448(3) 10_557 ? O2 Na1 2.3977(18) 3_656 ? C1 C1 1.412(4) 10_557 ? C1 C2 1.427(3) . ? C1 Na1 2.6478(17) 3_556 ? C2 C3 1.429(3) . ? C2 Na1 2.6923(16) 3_556 ? C3 C4 1.405(3) . ? C3 Na1 2.6771(17) 3_556 ? C4 C4 1.416(5) 10_557 ? C4 Na1 2.6894(17) 3_556 ? C7 C8 1.468(5) . ? C8 C8 1.360(10) 10_557 ? C9 C10 1.467(5) . ? C10 C10 1.397(9) 10_557 ? 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 Na1 O2 83.80(7) . . ? O1 Na1 C1 164.53(5) . 10_557 ? O2 Na1 C1 96.41(6) . 10_557 ? O1 Na1 C1 164.53(5) . . ? O2 Na1 C1 96.40(6) . . ? C1 Na1 C1 30.93(9) 10_557 . ? O1 Na1 C3 111.10(6) . 10_557 ? O2 Na1 C3 135.90(5) . 10_557 ? C1 Na1 C3 58.57(6) 10_557 10_557 ? C1 Na1 C3 79.48(6) . 10_557 ? O1 Na1 C3 111.10(6) . . ? O2 Na1 C3 135.90(5) . . ? C1 Na1 C3 79.48(6) 10_557 . ? C1 Na1 C3 58.57(6) . . ? C3 Na1 C3 78.89(8) 10_557 . ? O1 Na1 C4 96.57(6) . 10_557 ? O2 Na1 C4 164.73(5) . 10_557 ? C1 Na1 C4 79.18(6) 10_557 10_557 ? C1 Na1 C4 87.29(5) . 10_557 ? C3 Na1 C4 30.35(7) 10_557 10_557 ? C3 Na1 C4 58.10(7) . 10_557 ? O1 Na1 C4 96.57(6) . . ? O2 Na1 C4 164.73(5) . . ? C1 Na1 C4 87.29(5) 10_557 . ? C1 Na1 C4 79.18(6) . . ? C3 Na1 C4 58.10(7) 10_557 . ? C3 Na1 C4 30.36(7) . . ? C4 Na1 C4 30.52(10) 10_557 . ? O1 Na1 C2 135.07(5) . 10_557 ? O2 Na1 C2 110.82(6) . 10_557 ? C1 Na1 C2 30.99(7) 10_557 10_557 ? C1 Na1 C2 59.23(6) . 10_557 ? C3 Na1 C2 30.87(7) 10_557 10_557 ? C3 Na1 C2 88.01(5) . 10_557 ? C4 Na1 C2 58.64(6) 10_557 10_557 ? C4 Na1 C2 79.67(6) . 10_557 ? O1 Na1 C2 135.07(5) . . ? O2 Na1 C2 110.82(6) . . ? C1 Na1 C2 59.23(6) 10_557 . ? C1 Na1 C2 30.99(7) . . ? C3 Na1 C2 88.01(5) 10_557 . ? C3 Na1 C2 30.87(7) . . ? C4 Na1 C2 79.68(6) 10_557 . ? C4 Na1 C2 58.64(6) . . ? C2 Na1 C2 80.80(8) 10_557 . ? O1 Na1 Na1 41.28(5) . 3_656 ? O2 Na1 Na1 42.52(5) . 3_656 ? C1 Na1 Na1 136.82(4) 10_557 3_656 ? C1 Na1 Na1 136.82(4) . 3_656 ? C3 Na1 Na1 136.16(4) 10_557 3_656 ? C3 Na1 Na1 136.16(4) . 3_656 ? C4 Na1 Na1 135.89(4) 10_557 3_656 ? C4 Na1 Na1 135.89(4) . 3_656 ? C2 Na1 Na1 135.82(4) 10_557 3_656 ? C2 Na1 Na1 135.82(4) . 3_656 ? O1 Na1 Na1 138.72(5) . 3_556 ? O2 Na1 Na1 137.48(5) . 3_556 ? C1 Na1 Na1 43.18(4) 10_557 3_556 ? C1 Na1 Na1 43.18(4) . 3_556 ? C3 Na1 Na1 43.84(4) 10_557 3_556 ? C3 Na1 Na1 43.84(4) . 3_556 ? C4 Na1 Na1 44.11(4) 10_557 3_556 ? C4 Na1 Na1 44.11(4) . 3_556 ? C2 Na1 Na1 44.18(4) 10_557 3_556 ? C2 Na1 Na1 44.18(4) . 3_556 ? Na1 Na1 Na1 180.0 3_656 3_556 ? C2 Si1 C5 112.30(11) . . ? C2 Si1 C6 111.55(8) . . ? C5 Si1 C6 107.22(8) . . ? C2 Si1 C6 111.55(8) . 12 ? C5 Si1 C6 107.22(8) . 12 ? C6 Si1 C6 106.70(13) . 12 ? C7 O1 C7 108.9(3) 10_557 . ? C7 O1 Na1 112.55(7) 10_557 . ? C7 O1 Na1 112.55(7) . . ? C7 O1 Na1 112.55(7) 10_557 3_656 ? C7 O1 Na1 112.55(7) . 3_656 ? Na1 O1 Na1 97.44(9) . 3_656 ? C9 O2 C9 109.0(3) . 10_557 ? C9 O2 Na1 113.12(8) . 3_656 ? C9 O2 Na1 113.12(8) 10_557 3_656 ? C9 O2 Na1 113.12(8) . . ? C9 O2 Na1 113.12(8) 10_557 . ? Na1 O2 Na1 94.96(9) 3_656 . ? C1 C1 C2 136.70(12) 10_557 . ? C1 C1 Na1 74.53(5) 10_557 3_556 ? C2 C1 Na1 76.23(9) . 3_556 ? C1 C1 Na1 74.53(5) 10_557 . ? C2 C1 Na1 76.22(9) . . ? Na1 C1 Na1 93.64(8) 3_556 . ? C3 C2 C1 131.5(2) . . ? C3 C2 Si1 111.39(15) . . ? C1 C2 Si1 117.07(16) . . ? C3 C2 Na1 73.98(9) . 3_556 ? C1 C2 Na1 72.78(9) . 3_556 ? Si1 C2 Na1 134.15(4) . 3_556 ? C3 C2 Na1 73.98(9) . . ? C1 C2 Na1 72.78(9) . . ? Si1 C2 Na1 134.15(4) . . ? Na1 C2 Na1 91.64(7) 3_556 . ? C2 C3 C4 136.8(2) . . ? C2 C3 Na1 75.15(9) . . ? C4 C3 Na1 75.30(10) . . ? C2 C3 Na1 75.15(9) . 3_556 ? C4 C3 Na1 75.30(10) . 3_556 ? Na1 C3 Na1 92.31(7) . 3_556 ? C4 C4 C3 134.96(13) 10_557 . ? C4 C4 Na1 74.74(5) 10_557 . ? C3 C4 Na1 74.34(9) . . ? C4 C4 Na1 74.74(5) 10_557 3_556 ? C3 C4 Na1 74.34(9) . 3_556 ? Na1 C4 Na1 91.77(7) . 3_556 ? O1 C7 C8 105.6(3) . . ? C8 C8 C7 110.0(2) 10_557 . ? O2 C9 C10 106.4(3) . . ? C10 C10 C9 109.1(2) 10_557 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Na1 O1 C7 118.23(13) . . . 10_557 ? C1 Na1 O1 C7 26.6(3) 10_557 . . 10_557 ? C1 Na1 O1 C7 -150.2(2) . . . 10_557 ? C3 Na1 O1 C7 -18.85(14) 10_557 . . 10_557 ? C3 Na1 O1 C7 -104.69(13) . . . 10_557 ? C4 Na1 O1 C7 -46.40(14) 10_557 . . 10_557 ? C4 Na1 O1 C7 -77.13(14) . . . 10_557 ? C2 Na1 O1 C7 4.82(17) 10_557 . . 10_557 ? C2 Na1 O1 C7 -128.35(13) . . . 10_557 ? Na1 Na1 O1 C7 118.23(13) 3_656 . . 10_557 ? Na1 Na1 O1 C7 -61.77(13) 3_556 . . 10_557 ? O2 Na1 O1 C7 -118.23(13) . . . . ? C1 Na1 O1 C7 150.2(2) 10_557 . . . ? C1 Na1 O1 C7 -26.6(3) . . . . ? C3 Na1 O1 C7 104.69(13) 10_557 . . . ? C3 Na1 O1 C7 18.85(14) . . . . ? C4 Na1 O1 C7 77.13(14) 10_557 . . . ? C4 Na1 O1 C7 46.40(14) . . . . ? C2 Na1 O1 C7 128.36(13) 10_557 . . . ? C2 Na1 O1 C7 -4.82(17) . . . . ? Na1 Na1 O1 C7 -118.23(13) 3_656 . . . ? Na1 Na1 O1 C7 61.77(13) 3_556 . . . ? O2 Na1 O1 Na1 0.0 . . . 3_656 ? C1 Na1 O1 Na1 -91.6(2) 10_557 . . 3_656 ? C1 Na1 O1 Na1 91.6(2) . . . 3_656 ? C3 Na1 O1 Na1 -137.08(5) 10_557 . . 3_656 ? C3 Na1 O1 Na1 137.08(5) . . . 3_656 ? C4 Na1 O1 Na1 -164.63(5) 10_557 . . 3_656 ? C4 Na1 O1 Na1 164.64(5) . . . 3_656 ? C2 Na1 O1 Na1 -113.41(8) 10_557 . . 3_656 ? C2 Na1 O1 Na1 113.41(8) . . . 3_656 ? Na1 Na1 O1 Na1 180.0 3_556 . . 3_656 ? O1 Na1 O2 C9 117.74(13) . . . . ? C1 Na1 O2 C9 -77.82(14) 10_557 . . . ? C1 Na1 O2 C9 -46.69(14) . . . . ? C3 Na1 O2 C9 -128.17(13) 10_557 . . . ? C3 Na1 O2 C9 3.66(17) . . . . ? C4 Na1 O2 C9 -150.0(2) 10_557 . . . ? C4 Na1 O2 C9 25.5(3) . . . . ? C2 Na1 O2 C9 -106.15(13) 10_557 . . . ? C2 Na1 O2 C9 -18.36(14) . . . . ? Na1 Na1 O2 C9 117.74(13) 3_656 . . . ? Na1 Na1 O2 C9 -62.26(13) 3_556 . . . ? O1 Na1 O2 C9 -117.74(13) . . . 10_557 ? C1 Na1 O2 C9 46.69(14) 10_557 . . 10_557 ? C1 Na1 O2 C9 77.82(14) . . . 10_557 ? C3 Na1 O2 C9 -3.66(17) 10_557 . . 10_557 ? C3 Na1 O2 C9 128.17(13) . . . 10_557 ? C4 Na1 O2 C9 -25.5(3) 10_557 . . 10_557 ? C4 Na1 O2 C9 150.0(2) . . . 10_557 ? C2 Na1 O2 C9 18.36(14) 10_557 . . 10_557 ? C2 Na1 O2 C9 106.15(13) . . . 10_557 ? Na1 Na1 O2 C9 -117.74(13) 3_656 . . 10_557 ? Na1 Na1 O2 C9 62.26(13) 3_556 . . 10_557 ? O1 Na1 O2 Na1 0.0 . . . 3_656 ? C1 Na1 O2 Na1 164.43(5) 10_557 . . 3_656 ? C1 Na1 O2 Na1 -164.43(5) . . . 3_656 ? C3 Na1 O2 Na1 114.09(8) 10_557 . . 3_656 ? C3 Na1 O2 Na1 -114.09(8) . . . 3_656 ? C4 Na1 O2 Na1 92.2(2) 10_557 . . 3_656 ? C4 Na1 O2 Na1 -92.2(2) . . . 3_656 ? C2 Na1 O2 Na1 136.10(5) 10_557 . . 3_656 ? C2 Na1 O2 Na1 -136.10(5) . . . 3_656 ? Na1 Na1 O2 Na1 180.0 3_556 . . 3_656 ? O1 Na1 C1 C1 178.3(3) . . . 10_557 ? O2 Na1 C1 C1 -91.781(19) . . . 10_557 ? C3 Na1 C1 C1 43.79(5) 10_557 . . 10_557 ? C3 Na1 C1 C1 127.12(5) . . . 10_557 ? C4 Na1 C1 C1 73.35(5) 10_557 . . 10_557 ? C4 Na1 C1 C1 103.01(5) . . . 10_557 ? C2 Na1 C1 C1 18.67(5) 10_557 . . 10_557 ? C2 Na1 C1 C1 147.70(8) . . . 10_557 ? Na1 Na1 C1 C1 -107.15(6) 3_656 . . 10_557 ? Na1 Na1 C1 C1 72.85(6) 3_556 . . 10_557 ? O1 Na1 C1 C2 30.6(3) . . . . ? O2 Na1 C1 C2 120.51(9) . . . . ? C1 Na1 C1 C2 -147.70(8) 10_557 . . . ? C3 Na1 C1 C2 -103.91(10) 10_557 . . . ? C3 Na1 C1 C2 -20.59(9) . . . . ? C4 Na1 C1 C2 -74.36(10) 10_557 . . . ? C4 Na1 C1 C2 -44.69(10) . . . . ? C2 Na1 C1 C2 -129.03(13) 10_557 . . . ? Na1 Na1 C1 C2 105.15(9) 3_656 . . . ? Na1 Na1 C1 C2 -74.86(9) 3_556 . . . ? O1 Na1 C1 Na1 105.5(2) . . . 3_556 ? O2 Na1 C1 Na1 -164.63(5) . . . 3_556 ? C1 Na1 C1 Na1 -72.85(6) 10_557 . . 3_556 ? C3 Na1 C1 Na1 -29.06(7) 10_557 . . 3_556 ? C3 Na1 C1 Na1 54.27(6) . . . 3_556 ? C4 Na1 C1 Na1 0.50(7) 10_557 . . 3_556 ? C4 Na1 C1 Na1 30.16(6) . . . 3_556 ? C2 Na1 C1 Na1 -54.18(6) 10_557 . . 3_556 ? C2 Na1 C1 Na1 74.86(9) . . . 3_556 ? Na1 Na1 C1 Na1 180.0 3_656 . . 3_556 ? C1 C1 C2 C3 0.0 10_557 . . . ? Na1 C1 C2 C3 -48.66(3) 3_556 . . . ? Na1 C1 C2 C3 48.66(3) . . . . ? C1 C1 C2 Si1 180.0 10_557 . . . ? Na1 C1 C2 Si1 131.34(3) 3_556 . . . ? Na1 C1 C2 Si1 -131.34(3) . . . . ? C1 C1 C2 Na1 48.66(3) 10_557 . . 3_556 ? Na1 C1 C2 Na1 97.32(6) . . . 3_556 ? C1 C1 C2 Na1 -48.66(3) 10_557 . . . ? Na1 C1 C2 Na1 -97.32(6) 3_556 . . . ? C5 Si1 C2 C3 180.0 . . . . ? C6 Si1 C2 C3 -59.61(7) . . . . ? C6 Si1 C2 C3 59.61(7) 12 . . . ? C5 Si1 C2 C1 0.0 . . . . ? C6 Si1 C2 C1 120.39(7) . . . . ? C6 Si1 C2 C1 -120.39(7) 12 . . . ? C5 Si1 C2 Na1 91.88(13) . . . 3_556 ? C6 Si1 C2 Na1 -147.73(13) . . . 3_556 ? C6 Si1 C2 Na1 -28.51(17) 12 . . 3_556 ? C5 Si1 C2 Na1 -91.88(13) . . . . ? C6 Si1 C2 Na1 28.51(17) . . . . ? C6 Si1 C2 Na1 147.72(13) 12 . . . ? O1 Na1 C2 C3 46.88(12) . . . . ? O2 Na1 C2 C3 149.44(9) . . . . ? C1 Na1 C2 C3 -125.58(11) 10_557 . . . ? C1 Na1 C2 C3 -144.22(14) . . . . ? C3 Na1 C2 C3 -71.49(11) 10_557 . . . ? C4 Na1 C2 C3 -42.10(10) 10_557 . . . ? C4 Na1 C2 C3 -18.21(9) . . . . ? C2 Na1 C2 C3 -101.67(10) 10_557 . . . ? Na1 Na1 C2 C3 107.19(9) 3_656 . . . ? Na1 Na1 C2 C3 -72.81(9) 3_556 . . . ? O1 Na1 C2 C1 -168.90(10) . . . . ? O2 Na1 C2 C1 -66.34(10) . . . . ? C1 Na1 C2 C1 18.64(8) 10_557 . . . ? C3 Na1 C2 C1 72.73(10) 10_557 . . . ? C3 Na1 C2 C1 144.22(14) . . . . ? C4 Na1 C2 C1 102.12(10) 10_557 . . . ? C4 Na1 C2 C1 126.00(11) . . . . ? C2 Na1 C2 C1 42.54(11) 10_557 . . . ? Na1 Na1 C2 C1 -108.59(9) 3_656 . . . ? Na1 Na1 C2 C1 71.40(9) 3_556 . . . ? O1 Na1 C2 Si1 -57.61(18) . . . . ? O2 Na1 C2 Si1 44.96(16) . . . . ? C1 Na1 C2 Si1 129.94(16) 10_557 . . . ? C1 Na1 C2 Si1 111.30(18) . . . . ? C3 Na1 C2 Si1 -175.97(15) 10_557 . . . ? C3 Na1 C2 Si1 -104.49(18) . . . . ? C4 Na1 C2 Si1 -146.58(15) 10_557 . . . ? C4 Na1 C2 Si1 -122.70(16) . . . . ? C2 Na1 C2 Si1 153.84(11) 10_557 . . . ? Na1 Na1 C2 Si1 2.70(19) 3_656 . . . ? Na1 Na1 C2 Si1 -177.30(19) 3_556 . . . ? O1 Na1 C2 Na1 119.69(7) . . . 3_556 ? O2 Na1 C2 Na1 -137.74(5) . . . 3_556 ? C1 Na1 C2 Na1 -52.76(6) 10_557 . . 3_556 ? C1 Na1 C2 Na1 -71.40(9) . . . 3_556 ? C3 Na1 C2 Na1 1.33(7) 10_557 . . 3_556 ? C3 Na1 C2 Na1 72.81(9) . . . 3_556 ? C4 Na1 C2 Na1 30.72(7) 10_557 . . 3_556 ? C4 Na1 C2 Na1 54.60(6) . . . 3_556 ? C2 Na1 C2 Na1 -28.86(9) 10_557 . . 3_556 ? Na1 Na1 C2 Na1 180.0 3_656 . . 3_556 ? C1 C2 C3 C4 0.0 . . . . ? Si1 C2 C3 C4 180.0 . . . . ? Na1 C2 C3 C4 -48.26(3) 3_556 . . . ? Na1 C2 C3 C4 48.26(3) . . . . ? C1 C2 C3 Na1 -48.26(3) . . . . ? Si1 C2 C3 Na1 131.74(3) . . . . ? Na1 C2 C3 Na1 -96.52(6) 3_556 . . . ? C1 C2 C3 Na1 48.26(3) . . . 3_556 ? Si1 C2 C3 Na1 -131.74(3) . . . 3_556 ? Na1 C2 C3 Na1 96.52(6) . . . 3_556 ? O1 Na1 C3 C2 -146.46(9) . . . . ? O2 Na1 C3 C2 -43.06(13) . . . . ? C1 Na1 C3 C2 45.30(9) 10_557 . . . ? C1 Na1 C3 C2 20.66(9) . . . . ? C3 Na1 C3 C2 105.03(10) 10_557 . . . ? C4 Na1 C3 C2 129.03(11) 10_557 . . . ? C4 Na1 C3 C2 148.12(15) . . . . ? C2 Na1 C3 C2 75.31(11) 10_557 . . . ? Na1 Na1 C3 C2 -106.02(9) 3_656 . . . ? Na1 Na1 C3 C2 73.97(9) 3_556 . . . ? O1 Na1 C3 C4 65.42(10) . . . . ? O2 Na1 C3 C4 168.81(10) . . . . ? C1 Na1 C3 C4 -102.82(11) 10_557 . . . ? C1 Na1 C3 C4 -127.46(11) . . . . ? C3 Na1 C3 C4 -43.09(12) 10_557 . . . ? C4 Na1 C3 C4 -19.10(8) 10_557 . . . ? C2 Na1 C3 C4 -72.82(11) 10_557 . . . ? C2 Na1 C3 C4 -148.12(15) . . . . ? Na1 Na1 C3 C4 105.85(10) 3_656 . . . ? Na1 Na1 C3 C4 -74.15(10) 3_556 . . . ? O1 Na1 C3 Na1 139.57(5) . . . 3_556 ? O2 Na1 C3 Na1 -117.03(8) . . . 3_556 ? C1 Na1 C3 Na1 -28.67(7) 10_557 . . 3_556 ? C1 Na1 C3 Na1 -53.31(6) . . . 3_556 ? C3 Na1 C3 Na1 31.06(9) 10_557 . . 3_556 ? C4 Na1 C3 Na1 55.06(6) 10_557 . . 3_556 ? C4 Na1 C3 Na1 74.15(10) . . . 3_556 ? C2 Na1 C3 Na1 1.33(8) 10_557 . . 3_556 ? C2 Na1 C3 Na1 -73.97(9) . . . 3_556 ? Na1 Na1 C3 Na1 180.0 3_656 . . 3_556 ? C2 C3 C4 C4 0.0 . . . 10_557 ? Na1 C3 C4 C4 48.21(3) . . . 10_557 ? Na1 C3 C4 C4 -48.21(3) 3_556 . . 10_557 ? C2 C3 C4 Na1 -48.21(3) . . . . ? Na1 C3 C4 Na1 -96.43(6) 3_556 . . . ? C2 C3 C4 Na1 48.21(3) . . . 3_556 ? Na1 C3 C4 Na1 96.43(6) . . . 3_556 ? O1 Na1 C4 C4 91.803(18) . . . 10_557 ? O2 Na1 C4 C4 -177.7(2) . . . 10_557 ? C1 Na1 C4 C4 -73.16(5) 10_557 . . 10_557 ? C1 Na1 C4 C4 -103.25(5) . . . 10_557 ? C3 Na1 C4 C4 -19.00(6) 10_557 . . 10_557 ? C3 Na1 C4 C4 -146.85(9) . . . 10_557 ? C2 Na1 C4 C4 -42.90(5) 10_557 . . 10_557 ? C2 Na1 C4 C4 -128.35(5) . . . 10_557 ? Na1 Na1 C4 C4 106.35(6) 3_656 . . 10_557 ? Na1 Na1 C4 C4 -73.65(6) 3_556 . . 10_557 ? O1 Na1 C4 C3 -121.35(9) . . . . ? O2 Na1 C4 C3 -30.8(3) . . . . ? C1 Na1 C4 C3 73.69(11) 10_557 . . . ? C1 Na1 C4 C3 43.59(10) . . . . ? C3 Na1 C4 C3 127.85(14) 10_557 . . . ? C4 Na1 C4 C3 146.85(9) 10_557 . . . ? C2 Na1 C4 C3 103.95(11) 10_557 . . . ? C2 Na1 C4 C3 18.50(9) . . . . ? Na1 Na1 C4 C3 -106.80(9) 3_656 . . . ? Na1 Na1 C4 C3 73.19(9) 3_556 . . . ? O1 Na1 C4 Na1 165.46(5) . . . 3_556 ? O2 Na1 C4 Na1 -104.0(2) . . . 3_556 ? C1 Na1 C4 Na1 0.49(7) 10_557 . . 3_556 ? C1 Na1 C4 Na1 -29.60(6) . . . 3_556 ? C3 Na1 C4 Na1 54.66(6) 10_557 . . 3_556 ? C3 Na1 C4 Na1 -73.19(9) . . . 3_556 ? C4 Na1 C4 Na1 73.65(6) 10_557 . . 3_556 ? C2 Na1 C4 Na1 30.76(6) 10_557 . . 3_556 ? C2 Na1 C4 Na1 -54.69(6) . . . 3_556 ? Na1 Na1 C4 Na1 180.0 3_656 . . 3_556 ? C7 O1 C7 C8 0.0 10_557 . . . ? Na1 O1 C7 C8 -125.54(8) . . . . ? Na1 O1 C7 C8 125.54(7) 3_656 . . . ? O1 C7 C8 C8 0.0 . . . 10_557 ? C9 O2 C9 C10 0.0 10_557 . . . ? Na1 O2 C9 C10 -126.74(8) 3_656 . . . ? Na1 O2 C9 C10 126.74(8) . . . . ? O2 C9 C10 C10 0.000(1) . . . 10_557 ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.384 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.055 # Attachment 'mm093-1.cif' data_mm093 _database_code_depnum_ccdc_archive 'CCDC 864753' #TrackingRef 'mm093-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H80 Li4 O4 Si4' _chemical_formula_weight 813.20 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.713(2) _cell_length_b 11.295(3) _cell_length_c 11.483(2) _cell_angle_alpha 99.865(12) _cell_angle_beta 108.105(11) _cell_angle_gamma 97.319(13) _cell_volume 1276.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6085 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.94 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 444 _exptl_absorpt_coefficient_mu 0.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9574 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14794 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.53 _reflns_number_total 6090 _reflns_number_gt 4083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0887P)^2^+0.2472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6090 _refine_ls_number_parameters 280 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.071 _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 0.1130(4) 0.7203(4) 0.8051(4) 0.0503(9) Uani 1 1 d . . . Li2 Li -0.1275(5) 0.9470(5) 0.9080(5) 0.0771(15) Uani 1 1 d . . . O1 O 0.15070(19) 0.55492(15) 0.79676(19) 0.0608(5) Uani 1 1 d . B . O2 O 0.16658(17) 0.75989(15) 0.66868(15) 0.0515(4) Uani 1 1 d . D . Si1 Si 0.33299(6) 0.82213(6) 1.13468(6) 0.04302(18) Uani 1 1 d . . . Si2 Si -0.27658(6) 0.68472(6) 0.65808(6) 0.04465(19) Uani 1 1 d . . . C1 C -0.1207(2) 0.78923(19) 0.76748(19) 0.0372(4) Uani 1 1 d . . . C2 C -0.05969(19) 0.74394(18) 0.87697(19) 0.0365(4) Uani 1 1 d . . . H2A H -0.1185 0.6772 0.8839 0.044 Uiso 1 1 calc R . . C3 C 0.06298(19) 0.77121(18) 0.97642(18) 0.0358(4) Uani 1 1 d . . . H3A H 0.0621 0.7230 1.0364 0.043 Uiso 1 1 calc R . . C4 C 0.1887(2) 0.85229(18) 1.01117(19) 0.0364(4) Uani 1 1 d . . . C5 C 0.2208(2) 0.95952(18) 0.9686(2) 0.0395(5) Uani 1 1 d . . . H5A H 0.3136 0.9945 1.0033 0.047 Uiso 1 1 calc R . . C6 C 0.1485(2) 1.02556(18) 0.8881(2) 0.0412(5) Uani 1 1 d . . . H6A H 0.1969 1.1057 0.8996 0.049 Uiso 1 1 calc R . . C7 C 0.0225(2) 1.0030(2) 0.7947(2) 0.0447(5) Uani 1 1 d . . . H7A H 0.0038 1.0734 0.7627 0.054 Uiso 1 1 calc R . . C8 C -0.0833(2) 0.9019(2) 0.7368(2) 0.0433(5) Uani 1 1 d . . . H8A H -0.1434 0.9109 0.6596 0.052 Uiso 1 1 calc R . . C9 C 0.2953(3) 0.6758(3) 1.1812(3) 0.0786(9) Uani 1 1 d . . . H9A H 0.2181 0.6758 1.2098 0.118 Uiso 1 1 calc R . . H9B H 0.3731 0.6671 1.2495 0.118 Uiso 1 1 calc R . . H9C H 0.2748 0.6072 1.1089 0.118 Uiso 1 1 calc R . . C10 C 0.3873(3) 0.9449(3) 1.2816(3) 0.0778(9) Uani 1 1 d . . . H10A H 0.3125 0.9498 1.3130 0.117 Uiso 1 1 calc R . . H10B H 0.4156 1.0237 1.2634 0.117 Uiso 1 1 calc R . . H10C H 0.4622 0.9258 1.3453 0.117 Uiso 1 1 calc R . . C11 C 0.4809(3) 0.8176(3) 1.0813(3) 0.0765(9) Uani 1 1 d . . . H11A H 0.4564 0.7543 1.0039 0.115 Uiso 1 1 calc R . . H11B H 0.5545 0.7988 1.1468 0.115 Uiso 1 1 calc R . . H11C H 0.5094 0.8974 1.0653 0.115 Uiso 1 1 calc R . . C12 C -0.3577(3) 0.7444(3) 0.5170(3) 0.0707(8) Uani 1 1 d . . . H12A H -0.2935 0.7607 0.4740 0.106 Uiso 1 1 calc R . . H12B H -0.3865 0.8204 0.5433 0.106 Uiso 1 1 calc R . . H12C H -0.4356 0.6835 0.4597 0.106 Uiso 1 1 calc R . . C13 C -0.4022(3) 0.6553(3) 0.7383(3) 0.0692(8) Uani 1 1 d . . . H13A H -0.4244 0.7330 0.7705 0.104 Uiso 1 1 calc R . . H13B H -0.3643 0.6168 0.8082 0.104 Uiso 1 1 calc R . . H13C H -0.4835 0.6007 0.6779 0.104 Uiso 1 1 calc R . . C14 C -0.2405(3) 0.5320(2) 0.5996(3) 0.0580(6) Uani 1 1 d . . . H14A H -0.1750 0.5428 0.5569 0.087 Uiso 1 1 calc R . . H14B H -0.3234 0.4787 0.5406 0.087 Uiso 1 1 calc R . . H14C H -0.2042 0.4946 0.6708 0.087 Uiso 1 1 calc R . . C15 C 0.0958(3) 0.4593(2) 0.8428(3) 0.0665(8) Uani 1 1 d . B . H15A H 0.0075 0.4158 0.7817 0.080 Uiso 1 1 calc R . . H15B H 0.0843 0.4929 0.9235 0.080 Uiso 1 1 calc R . . C16 C 0.1922(4) 0.3740(3) 0.8611(5) 0.1041(13) Uani 1 1 d . . . H16A H 0.1535 0.2950 0.7991 0.125 Uiso 0.50 1 calc PR A 1 H16B H 0.2151 0.3584 0.9468 0.125 Uiso 0.50 1 calc PR A 1 H16C H 0.0007 0.0001 0.0002 0.125 Uiso 0.50 1 d PR A 2 H16D H 0.0007 0.0001 0.0002 0.125 Uiso 0.50 1 d PR A 2 C17 C 0.3177(8) 0.4393(7) 0.8414(9) 0.077(2) Uani 0.50 1 d PU B 1 H17A H 0.3857 0.4851 0.9223 0.092 Uiso 0.50 1 calc PR B 1 H17B H 0.3582 0.3804 0.7975 0.092 Uiso 0.50 1 calc PR B 1 C17' C 0.2539(10) 0.3901(8) 0.7751(8) 0.085(2) Uani 0.50 1 d PU B 2 H17C H 0.2025 0.3340 0.6928 0.101 Uiso 0.50 1 calc PR B 2 H17D H 0.3453 0.3722 0.8038 0.101 Uiso 0.50 1 calc PR B 2 C18 C 0.2607(4) 0.5224(3) 0.7627(4) 0.0873(11) Uani 1 1 d . . . H18A H 0.3287 0.5965 0.7773 0.105 Uiso 0.50 1 calc PR B 1 H18B H 0.2301 0.4810 0.6726 0.105 Uiso 0.50 1 calc PR B 1 H18C H 0.3467 0.5741 0.8204 0.105 Uiso 0.50 1 d PR B 2 H18D H 0.2503 0.5288 0.6754 0.105 Uiso 0.50 1 d PR B 2 C19 C 0.0714(3) 0.7345(3) 0.5436(2) 0.0628(7) Uani 1 1 d . . . H19A H -0.0209 0.7315 0.5449 0.075 Uiso 0.50 1 calc PR C 1 H19B H 0.0762 0.6558 0.4933 0.075 Uiso 0.50 1 calc PR C 1 H19C H -0.0135 0.7596 0.5446 0.075 Uiso 0.50 1 d PR C 2 H19D H 0.0524 0.6459 0.5047 0.075 Uiso 0.50 1 d PR C 2 C20 C 0.118(3) 0.8496(16) 0.488(3) 0.103(5) Uani 0.50 1 d PU D 1 H20A H 0.1009 0.8250 0.3968 0.123 Uiso 0.50 1 calc PR D 1 H20B H 0.0724 0.9184 0.5047 0.123 Uiso 0.50 1 calc PR D 1 C21 C 0.2543(14) 0.8792(14) 0.5570(12) 0.130(5) Uani 0.50 1 d PU D 1 H21A H 0.2880 0.9673 0.5667 0.156 Uiso 0.50 1 calc PR D 1 H21B H 0.3034 0.8315 0.5120 0.156 Uiso 0.50 1 calc PR D 1 C20' C 0.122(3) 0.8063(14) 0.477(2) 0.103(5) Uani 0.50 1 d PU D 2 H20C H 0.0498 0.8311 0.4143 0.123 Uiso 0.50 1 calc PR D 2 H20D H 0.1749 0.7621 0.4332 0.123 Uiso 0.50 1 calc PR D 2 C21' C 0.2159(12) 0.9225(8) 0.5815(10) 0.070(2) Uani 0.50 1 d PU D 2 H21C H 0.2834 0.9664 0.5535 0.084 Uiso 0.50 1 calc PR D 2 H21D H 0.1641 0.9802 0.6109 0.084 Uiso 0.50 1 calc PR D 2 C22 C 0.2764(3) 0.8519(3) 0.6778(3) 0.0673(8) Uani 1 1 d . . . H22A H 0.3614 0.8217 0.7052 0.081 Uiso 0.50 1 calc PR D 1 H22B H 0.2826 0.9265 0.7403 0.081 Uiso 0.50 1 calc PR D 1 H22C H 0.3481 0.8141 0.6581 0.081 Uiso 0.50 1 d PR D 2 H22D H 0.3142 0.9055 0.7632 0.081 Uiso 0.50 1 d PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.060(2) 0.050(2) 0.057(2) 0.0234(18) 0.034(2) 0.0174(18) Li2 0.043(2) 0.113(4) 0.058(3) -0.018(3) 0.013(2) 0.013(2) O1 0.0718(12) 0.0510(9) 0.0896(13) 0.0337(9) 0.0534(11) 0.0277(9) O2 0.0596(10) 0.0578(10) 0.0495(9) 0.0245(8) 0.0274(8) 0.0153(8) Si1 0.0335(3) 0.0447(3) 0.0487(4) 0.0164(3) 0.0086(3) 0.0054(2) Si2 0.0362(3) 0.0529(4) 0.0414(3) 0.0122(3) 0.0078(3) 0.0082(3) C1 0.0339(10) 0.0441(11) 0.0370(10) 0.0124(9) 0.0127(8) 0.0132(8) C2 0.0310(10) 0.0417(11) 0.0397(10) 0.0146(9) 0.0135(8) 0.0058(8) C3 0.0341(10) 0.0422(11) 0.0353(10) 0.0150(8) 0.0142(8) 0.0078(8) C4 0.0364(10) 0.0387(10) 0.0373(10) 0.0111(8) 0.0150(9) 0.0086(8) C5 0.0394(11) 0.0364(10) 0.0451(11) 0.0124(9) 0.0170(9) 0.0050(8) C6 0.0481(12) 0.0315(10) 0.0492(12) 0.0143(9) 0.0210(10) 0.0075(9) C7 0.0536(14) 0.0381(11) 0.0500(13) 0.0211(10) 0.0185(11) 0.0181(10) C8 0.0466(12) 0.0480(12) 0.0395(11) 0.0177(9) 0.0124(10) 0.0184(10) C9 0.0595(17) 0.0764(19) 0.088(2) 0.0504(18) -0.0029(15) -0.0007(15) C10 0.0662(19) 0.082(2) 0.0638(18) 0.0062(16) -0.0053(15) 0.0236(16) C11 0.0490(16) 0.096(2) 0.103(2) 0.042(2) 0.0343(17) 0.0322(16) C12 0.0673(18) 0.0715(18) 0.0547(16) 0.0146(14) -0.0047(13) 0.0116(15) C13 0.0382(14) 0.089(2) 0.0759(19) 0.0125(16) 0.0209(13) 0.0030(13) C14 0.0583(15) 0.0520(14) 0.0551(14) 0.0070(12) 0.0133(12) 0.0018(12) C15 0.0713(18) 0.0506(14) 0.088(2) 0.0277(14) 0.0369(16) 0.0082(13) C16 0.132(3) 0.079(2) 0.143(4) 0.066(2) 0.071(3) 0.050(2) C17 0.065(5) 0.073(5) 0.099(6) 0.031(4) 0.023(4) 0.033(4) C17' 0.096(6) 0.085(5) 0.086(5) 0.021(4) 0.034(5) 0.054(5) C18 0.106(3) 0.090(2) 0.120(3) 0.052(2) 0.082(2) 0.059(2) C19 0.0674(17) 0.0696(17) 0.0492(14) 0.0099(13) 0.0205(13) 0.0084(14) C20 0.116(7) 0.100(13) 0.081(10) 0.063(11) 0.008(6) -0.006(10) C21 0.119(10) 0.172(12) 0.080(7) 0.046(8) 0.025(6) -0.046(8) C20' 0.140(9) 0.078(10) 0.055(5) 0.034(8) -0.005(5) -0.033(8) C21' 0.099(6) 0.055(4) 0.082(5) 0.036(4) 0.056(4) 0.013(3) C22 0.0582(16) 0.084(2) 0.0684(17) 0.0254(15) 0.0334(14) 0.0036(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.928(4) . ? Li1 O1 1.953(4) . ? Li1 C3 2.199(4) . ? Li1 C2 2.275(4) . ? Li1 C4 2.402(5) . ? Li1 C1 2.647(5) . ? Li2 C8 2.156(5) . ? Li2 C5 2.181(5) 2_577 ? Li2 C1 2.214(5) . ? Li2 C6 2.393(5) 2_577 ? Li2 C7 2.449(6) . ? Li2 C2 2.494(6) . ? Li2 C4 2.543(6) 2_577 ? Li2 Li2 2.842(9) 2_577 ? O1 C18 1.423(3) . ? O1 C15 1.421(3) . ? O2 C22 1.432(3) . ? O2 C19 1.435(3) . ? Si1 C9 1.857(3) . ? Si1 C4 1.859(2) . ? Si1 C10 1.868(3) . ? Si1 C11 1.872(3) . ? Si2 C1 1.856(2) . ? Si2 C12 1.866(3) . ? Si2 C14 1.874(3) . ? Si2 C13 1.880(3) . ? C1 C8 1.420(3) . ? C1 C2 1.437(3) . ? C2 C3 1.403(3) . ? C3 C4 1.427(3) . ? C4 C5 1.423(3) . ? C4 Li2 2.543(6) 2_577 ? C5 C6 1.396(3) . ? C5 Li2 2.181(5) 2_577 ? C6 C7 1.399(3) . ? C6 Li2 2.393(5) 2_577 ? C7 C8 1.404(3) . ? C15 C16 1.492(5) . ? C16 C17' 1.372(9) . ? C16 C17 1.548(9) . ? C17 C18 1.472(8) . ? C17' C18 1.519(9) . ? C19 C20' 1.38(2) . ? C19 C20 1.63(2) . ? C20 C21 1.39(3) . ? C21 C22 1.427(12) . ? C20' C21' 1.59(2) . ? C21' C22 1.506(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li1 O1 99.49(18) . . ? O2 Li1 C3 152.3(2) . . ? O1 Li1 C3 107.06(18) . . ? O2 Li1 C2 136.6(2) . . ? O1 Li1 C2 112.06(18) . . ? C3 Li1 C2 36.51(9) . . ? O2 Li1 C4 123.2(2) . . ? O1 Li1 C4 116.0(2) . . ? C3 Li1 C4 35.80(9) . . ? C2 Li1 C4 68.42(12) . . ? O2 Li1 C1 103.90(19) . . ? O1 Li1 C1 128.3(2) . . ? C3 Li1 C1 65.46(12) . . ? C2 Li1 C1 32.86(9) . . ? C4 Li1 C1 87.75(13) . . ? C8 Li2 C5 155.1(3) . 2_577 ? C8 Li2 C1 37.89(11) . . ? C5 Li2 C1 152.5(3) 2_577 . ? C8 Li2 C6 169.7(3) . 2_577 ? C5 Li2 C6 35.17(10) 2_577 2_577 ? C1 Li2 C6 135.3(3) . 2_577 ? C8 Li2 C7 34.79(11) . . ? C5 Li2 C7 137.6(3) 2_577 . ? C1 Li2 C7 67.68(14) . . ? C6 Li2 C7 143.3(2) 2_577 . ? C8 Li2 C2 67.12(15) . . ? C5 Li2 C2 135.1(3) 2_577 . ? C1 Li2 C2 34.90(11) . . ? C6 Li2 C2 103.8(2) 2_577 . ? C7 Li2 C2 84.46(15) . . ? C8 Li2 C4 125.2(3) . 2_577 ? C5 Li2 C4 33.98(10) 2_577 2_577 ? C1 Li2 C4 157.3(3) . 2_577 ? C6 Li2 C4 63.69(13) 2_577 2_577 ? C7 Li2 C4 104.5(2) . 2_577 ? C2 Li2 C4 167.3(3) . 2_577 ? C8 Li2 Li2 103.4(2) . 2_577 ? C5 Li2 Li2 89.1(2) 2_577 2_577 ? C1 Li2 Li2 112.8(3) . 2_577 ? C6 Li2 Li2 71.1(2) 2_577 2_577 ? C7 Li2 Li2 73.1(2) . 2_577 ? C2 Li2 Li2 90.8(3) . 2_577 ? C4 Li2 Li2 83.4(2) 2_577 2_577 ? C18 O1 C15 109.4(2) . . ? C18 O1 Li1 121.5(2) . . ? C15 O1 Li1 128.09(18) . . ? C22 O2 C19 108.48(19) . . ? C22 O2 Li1 126.9(2) . . ? C19 O2 Li1 120.6(2) . . ? C9 Si1 C4 113.19(12) . . ? C9 Si1 C10 106.18(16) . . ? C4 Si1 C10 111.36(12) . . ? C9 Si1 C11 107.78(16) . . ? C4 Si1 C11 111.06(12) . . ? C10 Si1 C11 106.93(17) . . ? C1 Si2 C12 112.76(12) . . ? C1 Si2 C14 110.56(11) . . ? C12 Si2 C14 107.03(13) . . ? C1 Si2 C13 111.47(11) . . ? C12 Si2 C13 108.20(15) . . ? C14 Si2 C13 106.52(14) . . ? C8 C1 C2 129.65(19) . . ? C8 C1 Si2 117.62(16) . . ? C2 C1 Si2 112.63(15) . . ? C8 C1 Li2 68.8(2) . . ? C2 C1 Li2 83.2(2) . . ? Si2 C1 Li2 121.09(15) . . ? C8 C1 Li1 96.51(15) . . ? C2 C1 Li1 59.20(13) . . ? Si2 C1 Li1 120.21(13) . . ? Li2 C1 Li1 116.45(18) . . ? C3 C2 C1 137.46(18) . . ? C3 C2 Li1 68.79(15) . . ? C1 C2 Li1 87.94(16) . . ? C3 C2 Li2 99.08(17) . . ? C1 C2 Li2 61.86(16) . . ? Li1 C2 Li2 120.36(17) . . ? C2 C3 C4 136.79(19) . . ? C2 C3 Li1 74.70(16) . . ? C4 C3 Li1 79.90(16) . . ? C5 C4 C3 129.3(2) . . ? C5 C4 Si1 113.07(15) . . ? C3 C4 Si1 117.61(15) . . ? C5 C4 Li1 94.06(15) . . ? C3 C4 Li1 64.30(14) . . ? Si1 C4 Li1 118.40(14) . . ? C5 C4 Li2 58.94(17) . 2_577 ? C3 C4 Li2 100.24(16) . 2_577 ? Si1 C4 Li2 109.76(15) . 2_577 ? Li1 C4 Li2 131.26(18) . 2_577 ? C6 C5 C4 135.2(2) . . ? C6 C5 Li2 80.7(2) . 2_577 ? C4 C5 Li2 87.1(2) . 2_577 ? C5 C6 C7 135.8(2) . . ? C5 C6 Li2 64.11(18) . 2_577 ? C7 C6 Li2 110.52(18) . 2_577 ? C6 C7 C8 135.7(2) . . ? C6 C7 Li2 102.25(18) . . ? C8 C7 Li2 61.11(16) . . ? C7 C8 C1 134.4(2) . . ? C7 C8 Li2 84.10(19) . . ? C1 C8 Li2 73.3(2) . . ? O1 C15 C16 106.7(2) . . ? C17' C16 C15 103.1(4) . . ? C17' C16 C17 34.8(4) . . ? C15 C16 C17 105.6(3) . . ? C18 C17 C16 101.6(5) . . ? C16 C17' C18 107.9(5) . . ? O1 C18 C17 107.2(4) . . ? O1 C18 C17' 102.7(4) . . ? C17 C18 C17' 34.5(4) . . ? C20' C19 O2 107.6(10) . . ? C20' C19 C20 16.4(19) . . ? O2 C19 C20 103.1(9) . . ? C21 C20 C19 100.7(15) . . ? C20 C21 C22 109.5(13) . . ? C19 C20' C21' 104.2(16) . . ? C22 C21' C20' 96.0(9) . . ? O2 C22 C21 108.2(6) . . ? O2 C22 C21' 104.1(5) . . ? C21 C22 C21' 29.5(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Li1 O1 C18 34.7(3) . . . . ? C3 Li1 O1 C18 -137.1(3) . . . . ? C2 Li1 O1 C18 -175.6(3) . . . . ? C4 Li1 O1 C18 -99.7(3) . . . . ? C1 Li1 O1 C18 151.0(3) . . . . ? O2 Li1 O1 C15 -157.8(2) . . . . ? C3 Li1 O1 C15 30.3(4) . . . . ? C2 Li1 O1 C15 -8.2(4) . . . . ? C4 Li1 O1 C15 67.7(3) . . . . ? C1 Li1 O1 C15 -41.5(4) . . . . ? O1 Li1 O2 C22 -114.1(3) . . . . ? C3 Li1 O2 C22 49.0(6) . . . . ? C2 Li1 O2 C22 108.9(4) . . . . ? C4 Li1 O2 C22 15.8(4) . . . . ? C1 Li1 O2 C22 112.4(2) . . . . ? O1 Li1 O2 C19 91.1(3) . . . . ? C3 Li1 O2 C19 -105.9(5) . . . . ? C2 Li1 O2 C19 -45.9(4) . . . . ? C4 Li1 O2 C19 -139.0(2) . . . . ? C1 Li1 O2 C19 -42.5(3) . . . . ? C12 Si2 C1 C8 2.5(2) . . . . ? C14 Si2 C1 C8 122.23(17) . . . . ? C13 Si2 C1 C8 -119.48(19) . . . . ? C12 Si2 C1 C2 179.07(16) . . . . ? C14 Si2 C1 C2 -61.16(17) . . . . ? C13 Si2 C1 C2 57.13(19) . . . . ? C12 Si2 C1 Li2 83.2(3) . . . . ? C14 Si2 C1 Li2 -157.0(2) . . . . ? C13 Si2 C1 Li2 -38.7(3) . . . . ? C12 Si2 C1 Li1 -114.45(17) . . . . ? C14 Si2 C1 Li1 5.32(17) . . . . ? C13 Si2 C1 Li1 123.61(16) . . . . ? C5 Li2 C1 C8 136.9(7) 2_577 . . . ? C6 Li2 C1 C8 -168.2(3) 2_577 . . . ? C7 Li2 C1 C8 -23.36(13) . . . . ? C2 Li2 C1 C8 -137.32(19) . . . . ? C4 Li2 C1 C8 50.4(6) 2_577 . . . ? Li2 Li2 C1 C8 -82.5(4) 2_577 . . . ? C8 Li2 C1 C2 137.32(19) . . . . ? C5 Li2 C1 C2 -85.8(7) 2_577 . . . ? C6 Li2 C1 C2 -30.9(3) 2_577 . . . ? C7 Li2 C1 C2 113.96(15) . . . . ? C4 Li2 C1 C2 -172.3(6) 2_577 . . . ? Li2 Li2 C1 C2 54.8(4) 2_577 . . . ? C8 Li2 C1 Si2 -110.3(2) . . . . ? C5 Li2 C1 Si2 26.6(8) 2_577 . . . ? C6 Li2 C1 Si2 81.5(4) 2_577 . . . ? C7 Li2 C1 Si2 -133.65(15) . . . . ? C2 Li2 C1 Si2 112.39(19) . . . . ? C4 Li2 C1 Si2 -59.9(7) 2_577 . . . ? Li2 Li2 C1 Si2 167.2(3) 2_577 . . . ? C8 Li2 C1 Li1 86.73(19) . . . . ? C5 Li2 C1 Li1 -136.4(6) 2_577 . . . ? C6 Li2 C1 Li1 -81.5(3) 2_577 . . . ? C7 Li2 C1 Li1 63.37(19) . . . . ? C2 Li2 C1 Li1 -50.59(16) . . . . ? C4 Li2 C1 Li1 137.1(6) 2_577 . . . ? Li2 Li2 C1 Li1 4.3(4) 2_577 . . . ? O2 Li1 C1 C8 -42.8(2) . . . . ? O1 Li1 C1 C8 -157.1(2) . . . . ? C3 Li1 C1 C8 109.97(16) . . . . ? C2 Li1 C1 C8 132.8(2) . . . . ? C4 Li1 C1 C8 80.94(16) . . . . ? O2 Li1 C1 C2 -175.6(2) . . . . ? O1 Li1 C1 C2 70.0(2) . . . . ? C3 Li1 C1 C2 -22.84(13) . . . . ? C4 Li1 C1 C2 -51.88(14) . . . . ? O2 Li1 C1 Si2 84.52(19) . . . . ? O1 Li1 C1 Si2 -29.8(3) . . . . ? C3 Li1 C1 Si2 -122.70(14) . . . . ? C2 Li1 C1 Si2 -99.86(17) . . . . ? C4 Li1 C1 Si2 -151.74(12) . . . . ? O2 Li1 C1 Li2 -112.3(3) . . . . ? O1 Li1 C1 Li2 133.3(3) . . . . ? C3 Li1 C1 Li2 40.4(2) . . . . ? C2 Li1 C1 Li2 63.3(2) . . . . ? C4 Li1 C1 Li2 11.4(2) . . . . ? C8 C1 C2 C3 -16.3(4) . . . . ? Si2 C1 C2 C3 167.6(2) . . . . ? Li2 C1 C2 C3 -71.4(3) . . . . ? Li1 C1 C2 C3 54.9(2) . . . . ? C8 C1 C2 Li1 -71.2(2) . . . . ? Si2 C1 C2 Li1 112.71(15) . . . . ? Li2 C1 C2 Li1 -126.36(18) . . . . ? C8 C1 C2 Li2 55.2(2) . . . . ? Si2 C1 C2 Li2 -120.92(18) . . . . ? Li1 C1 C2 Li2 126.36(18) . . . . ? O2 Li1 C2 C3 -137.4(3) . . . . ? O1 Li1 C2 C3 89.1(2) . . . . ? C4 Li1 C2 C3 -21.31(12) . . . . ? C1 Li1 C2 C3 -143.60(19) . . . . ? O2 Li1 C2 C1 6.2(3) . . . . ? O1 Li1 C2 C1 -127.3(2) . . . . ? C3 Li1 C2 C1 143.60(19) . . . . ? C4 Li1 C2 C1 122.29(15) . . . . ? O2 Li1 C2 Li2 -49.2(4) . . . . ? O1 Li1 C2 Li2 177.3(2) . . . . ? C3 Li1 C2 Li2 88.2(2) . . . . ? C4 Li1 C2 Li2 66.91(19) . . . . ? C1 Li1 C2 Li2 -55.38(19) . . . . ? C8 Li2 C2 C3 112.66(16) . . . . ? C5 Li2 C2 C3 -81.1(3) 2_577 . . . ? C1 Li2 C2 C3 139.53(18) . . . . ? C6 Li2 C2 C3 -62.3(2) 2_577 . . . ? C7 Li2 C2 C3 81.39(16) . . . . ? C4 Li2 C2 C3 -54.1(10) 2_577 . . . ? Li2 Li2 C2 C3 8.5(3) 2_577 . . . ? C8 Li2 C2 C1 -26.87(13) . . . . ? C5 Li2 C2 C1 139.4(4) 2_577 . . . ? C6 Li2 C2 C1 158.2(2) 2_577 . . . ? C7 Li2 C2 C1 -58.14(15) . . . . ? C4 Li2 C2 C1 166.4(10) 2_577 . . . ? Li2 Li2 C2 C1 -131.1(3) 2_577 . . . ? C8 Li2 C2 Li1 42.0(2) . . . . ? C5 Li2 C2 Li1 -151.8(3) 2_577 . . . ? C1 Li2 C2 Li1 68.9(2) . . . . ? C6 Li2 C2 Li1 -133.0(2) 2_577 . . . ? C7 Li2 C2 Li1 10.7(2) . . . . ? C4 Li2 C2 Li1 -124.8(10) 2_577 . . . ? Li2 Li2 C2 Li1 -62.2(3) 2_577 . . . ? C1 C2 C3 C4 -5.2(4) . . . . ? Li1 C2 C3 C4 56.2(3) . . . . ? Li2 C2 C3 C4 -63.0(3) . . . . ? C1 C2 C3 Li1 -61.3(3) . . . . ? Li2 C2 C3 Li1 -119.15(18) . . . . ? O2 Li1 C3 C2 93.2(5) . . . . ? O1 Li1 C3 C2 -104.2(2) . . . . ? C4 Li1 C3 C2 144.72(19) . . . . ? C1 Li1 C3 C2 20.73(11) . . . . ? O2 Li1 C3 C4 -51.5(5) . . . . ? O1 Li1 C3 C4 111.1(2) . . . . ? C2 Li1 C3 C4 -144.72(19) . . . . ? C1 Li1 C3 C4 -123.99(14) . . . . ? C2 C3 C4 C5 18.6(4) . . . . ? Li1 C3 C4 C5 73.0(2) . . . . ? C2 C3 C4 Si1 -164.6(2) . . . . ? Li1 C3 C4 Si1 -110.12(16) . . . . ? C2 C3 C4 Li1 -54.5(3) . . . . ? C2 C3 C4 Li2 76.6(3) . . . 2_577 ? Li1 C3 C4 Li2 131.05(19) . . . 2_577 ? C9 Si1 C4 C5 -175.35(18) . . . . ? C10 Si1 C4 C5 65.10(19) . . . . ? C11 Si1 C4 C5 -54.0(2) . . . . ? C9 Si1 C4 C3 7.3(2) . . . . ? C10 Si1 C4 C3 -112.24(19) . . . . ? C11 Si1 C4 C3 128.70(18) . . . . ? C9 Si1 C4 Li1 -66.83(19) . . . . ? C10 Si1 C4 Li1 173.63(17) . . . . ? C11 Si1 C4 Li1 54.57(18) . . . . ? C9 Si1 C4 Li2 120.9(2) . . . 2_577 ? C10 Si1 C4 Li2 1.4(2) . . . 2_577 ? C11 Si1 C4 Li2 -117.67(19) . . . 2_577 ? O2 Li1 C4 C5 22.1(3) . . . . ? O1 Li1 C4 C5 144.8(2) . . . . ? C3 Li1 C4 C5 -132.06(19) . . . . ? C2 Li1 C4 C5 -110.37(16) . . . . ? C1 Li1 C4 C5 -83.04(15) . . . . ? O2 Li1 C4 C3 154.2(3) . . . . ? O1 Li1 C4 C3 -83.2(2) . . . . ? C2 Li1 C4 C3 21.69(12) . . . . ? C1 Li1 C4 C3 49.01(13) . . . . ? O2 Li1 C4 Si1 -96.9(2) . . . . ? O1 Li1 C4 Si1 25.8(2) . . . . ? C3 Li1 C4 Si1 108.93(17) . . . . ? C2 Li1 C4 Si1 130.63(13) . . . . ? C1 Li1 C4 Si1 157.95(11) . . . . ? O2 Li1 C4 Li2 73.4(3) . . . 2_577 ? O1 Li1 C4 Li2 -164.0(2) . . . 2_577 ? C3 Li1 C4 Li2 -80.8(2) . . . 2_577 ? C2 Li1 C4 Li2 -59.1(2) . . . 2_577 ? C1 Li1 C4 Li2 -31.8(2) . . . 2_577 ? C3 C4 C5 C6 3.3(4) . . . . ? Si1 C4 C5 C6 -173.6(2) . . . . ? Li1 C4 C5 C6 63.1(3) . . . . ? Li2 C4 C5 C6 -73.7(3) 2_577 . . . ? C3 C4 C5 Li2 77.0(2) . . . 2_577 ? Si1 C4 C5 Li2 -99.93(17) . . . 2_577 ? Li1 C4 C5 Li2 136.81(18) . . . 2_577 ? C4 C5 C6 C7 -17.2(4) . . . . ? Li2 C5 C6 C7 -93.4(3) 2_577 . . . ? C4 C5 C6 Li2 76.2(3) . . . 2_577 ? C5 C6 C7 C8 -4.2(4) . . . . ? Li2 C6 C7 C8 -77.7(3) 2_577 . . . ? C5 C6 C7 Li2 56.8(3) . . . . ? Li2 C6 C7 Li2 -16.7(3) 2_577 . . . ? C8 Li2 C7 C6 -135.8(2) . . . . ? C5 Li2 C7 C6 82.9(4) 2_577 . . . ? C1 Li2 C7 C6 -110.49(18) . . . . ? C6 Li2 C7 C6 26.9(5) 2_577 . . . ? C2 Li2 C7 C6 -78.79(17) . . . . ? C4 Li2 C7 C6 92.0(2) 2_577 . . . ? Li2 Li2 C7 C6 13.7(3) 2_577 . . . ? C5 Li2 C7 C8 -141.4(4) 2_577 . . . ? C1 Li2 C7 C8 25.27(13) . . . . ? C6 Li2 C7 C8 162.6(5) 2_577 . . . ? C2 Li2 C7 C8 56.96(16) . . . . ? C4 Li2 C7 C8 -132.2(2) 2_577 . . . ? Li2 Li2 C7 C8 149.5(3) 2_577 . . . ? C6 C7 C8 C1 17.8(4) . . . . ? Li2 C7 C8 C1 -59.6(3) . . . . ? C6 C7 C8 Li2 77.4(3) . . . . ? C2 C1 C8 C7 2.6(4) . . . . ? Si2 C1 C8 C7 178.6(2) . . . . ? Li2 C1 C8 C7 63.6(3) . . . . ? Li1 C1 C8 C7 -52.3(3) . . . . ? C2 C1 C8 Li2 -61.0(3) . . . . ? Si2 C1 C8 Li2 114.97(19) . . . . ? Li1 C1 C8 Li2 -115.89(18) . . . . ? C5 Li2 C8 C7 88.5(7) 2_577 . . . ? C1 Li2 C8 C7 -140.0(2) . . . . ? C6 Li2 C8 C7 -86.7(16) 2_577 . . . ? C2 Li2 C8 C7 -115.09(16) . . . . ? C4 Li2 C8 C7 61.4(3) 2_577 . . . ? Li2 Li2 C8 C7 -30.0(3) 2_577 . . . ? C5 Li2 C8 C1 -131.6(7) 2_577 . . . ? C6 Li2 C8 C1 53.3(16) 2_577 . . . ? C7 Li2 C8 C1 140.0(2) . . . . ? C2 Li2 C8 C1 24.90(12) . . . . ? C4 Li2 C8 C1 -158.6(3) 2_577 . . . ? Li2 Li2 C8 C1 110.0(3) 2_577 . . . ? C18 O1 C15 C16 11.1(4) . . . . ? Li1 O1 C15 C16 -157.6(3) . . . . ? O1 C15 C16 C17' -27.2(6) . . . . ? O1 C15 C16 C17 8.6(6) . . . . ? C17' C16 C17 C18 66.6(8) . . . . ? C15 C16 C17 C18 -23.9(7) . . . . ? C15 C16 C17' C18 32.3(7) . . . . ? C17 C16 C17' C18 -66.3(8) . . . . ? C15 O1 C18 C17 -27.6(5) . . . . ? Li1 O1 C18 C17 141.9(4) . . . . ? C15 O1 C18 C17' 7.8(5) . . . . ? Li1 O1 C18 C17' 177.4(4) . . . . ? C16 C17 C18 O1 31.1(6) . . . . ? C16 C17 C18 C17' -56.6(7) . . . . ? C16 C17' C18 O1 -26.1(7) . . . . ? C16 C17' C18 C17 75.8(9) . . . . ? C22 O2 C19 C20' 1.3(12) . . . . ? Li1 O2 C19 C20' 160.4(12) . . . . ? C22 O2 C19 C20 -15.0(10) . . . . ? Li1 O2 C19 C20 144.0(10) . . . . ? C20' C19 C20 C21 -80(7) . . . . ? O2 C19 C20 C21 28.2(17) . . . . ? C19 C20 C21 C22 -31.4(18) . . . . ? O2 C19 C20' C21' -27.6(17) . . . . ? C20 C19 C20' C21' 49(6) . . . . ? C19 C20' C21' C22 41.7(16) . . . . ? C19 O2 C22 C21 -3.3(8) . . . . ? Li1 O2 C22 C21 -160.6(7) . . . . ? C19 O2 C22 C21' 27.2(4) . . . . ? Li1 O2 C22 C21' -130.2(4) . . . . ? C20 C21 C22 O2 24.1(15) . . . . ? C20 C21 C22 C21' -62.4(17) . . . . ? C20' C21' C22 O2 -40.0(12) . . . . ? C20' C21' C22 C21 62.2(19) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 28.53 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.328 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.059