# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1314 data_leuu11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H62 K2 O3 Si3' _chemical_formula_weight 657.29 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorthombic _symmetry_space_group_name_H-M Pna2(1) 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 17.298(1) _cell_length_b 20.032(1) _cell_length_c 11.727(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4064(2) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used '4 still frames' _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Rigaku RU-200 rotating-anode generator powered at 50kV / 90mA ; _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS IIc' _diffrn_measurement_method ; Take 60 oscillation frames in the range of 0 - 180\%, \D\f = 3\%, 8 min. per frame. Crystal to detector distance is 69.667 mm, background level -40. ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5680 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 24.00 _reflns_number_total 5680 _reflns_number_gt 5179 _reflns_threshold_expression >2sigma(I) _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^)+(0.1298P)^2^+3.6304P] 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 0.65(11) _refine_ls_number_reflns 5680 _refine_ls_number_parameters 362 _refine_ls_number_restraints 319 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.2684 _refine_ls_wR_factor_gt 0.2606 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K 0.74048(9) 0.92227(8) 0.17595(16) 0.0765(4) Uani 1 1 d . . . K2 K 0.49761(10) 0.74267(9) 0.33749(19) 0.0942(6) Uani 1 1 d . . . Si1 Si 0.97615(14) 0.92806(14) 0.1437(2) 0.0992(8) Uani 1 1 d DU . . C1 C 0.9727(7) 0.8862(6) 0.0018(8) 0.137(4) Uani 1 1 d DU . . H1A H 1.0030 0.9112 -0.0519 0.205 Uiso 1 1 calc R . . H1B H 0.9201 0.8840 -0.0241 0.205 Uiso 1 1 calc R . . H1C H 0.9932 0.8418 0.0083 0.205 Uiso 1 1 calc R . . C2 C 1.0805(5) 0.9311(8) 0.1863(15) 0.186(6) Uani 1 1 d DU . . H2A H 1.1096 0.9540 0.1287 0.279 Uiso 1 1 calc R . . H2B H 1.0998 0.8864 0.1946 0.279 Uiso 1 1 calc R . . H2C H 1.0854 0.9544 0.2575 0.279 Uiso 1 1 calc R . . C3 C 0.9455(8) 1.0172(5) 0.1255(13) 0.189(6) Uani 1 1 d DU . . H3A H 0.9764 1.0378 0.0674 0.283 Uiso 1 1 calc R . . H3B H 0.9523 1.0407 0.1961 0.283 Uiso 1 1 calc R . . H3C H 0.8920 1.0187 0.1036 0.283 Uiso 1 1 calc R . . C4 C 0.9203(4) 0.8851(3) 0.2545(6) 0.0721(18) Uani 1 1 d D . . C5 C 0.8694(3) 0.8329(3) 0.2349(6) 0.0694(17) Uani 1 1 d D . . H5 H 0.8687 0.8174 0.1602 0.083 Uiso 1 1 calc R . . C6 C 0.8196(4) 0.8003(4) 0.3080(6) 0.0746(19) Uani 1 1 d D . . C7 C 0.8218(5) 0.8259(4) 0.4291(6) 0.090(2) Uani 1 1 d D . . H7A H 0.7707 0.8216 0.4622 0.108 Uiso 1 1 calc R . . H7B H 0.8568 0.7983 0.4733 0.108 Uiso 1 1 calc R . . C8 C 0.8472(7) 0.8970(5) 0.4380(8) 0.121(3) Uani 1 1 d D . . H8A H 0.8541 0.9077 0.5180 0.145 Uiso 1 1 calc R . . H8B H 0.8061 0.9252 0.4090 0.145 Uiso 1 1 calc R . . C9 C 0.9219(5) 0.9141(5) 0.3743(7) 0.116(3) Uani 1 1 d D . . H9A H 0.9278 0.9622 0.3701 0.139 Uiso 1 1 calc R . . H9B H 0.9658 0.8962 0.4156 0.139 Uiso 1 1 calc R . . Si2 Si 0.74383(11) 0.74256(10) 0.2582(2) 0.0729(5) Uani 1 1 d DU . . C10 C 0.7237(6) 0.6862(6) 0.3849(10) 0.128(3) Uani 1 1 d DU . . H10A H 0.6846 0.6543 0.3649 0.193 Uiso 1 1 calc R . . H10B H 0.7062 0.7126 0.4481 0.193 Uiso 1 1 calc R . . H10C H 0.7703 0.6631 0.4058 0.193 Uiso 1 1 calc R . . C11 C 0.7785(6) 0.6852(6) 0.1426(9) 0.127(3) Uani 1 1 d DU . . H11A H 0.7372 0.6561 0.1200 0.190 Uiso 1 1 calc R . . H11B H 0.8210 0.6590 0.1705 0.190 Uiso 1 1 calc R . . H11C H 0.7951 0.7110 0.0782 0.190 Uiso 1 1 calc R . . C12 C 0.6537(4) 0.7864(3) 0.2146(5) 0.0678(17) Uani 1 1 d D . . C13 C 0.6243(3) 0.8360(3) 0.2828(5) 0.0598(15) Uani 1 1 d D . . H13 H 0.6495 0.8412 0.3523 0.072 Uiso 1 1 calc R . . C14 C 0.5634(4) 0.8794(3) 0.2653(6) 0.0760(19) Uani 1 1 d D . . C15 C 0.5211(5) 0.8718(5) 0.1508(7) 0.110(3) Uani 1 1 d D . . H15A H 0.4715 0.8507 0.1644 0.132 Uiso 1 1 calc R . . H15B H 0.5113 0.9158 0.1197 0.132 Uiso 1 1 calc R . . C16 C 0.5640(7) 0.8322(7) 0.0656(8) 0.154(5) Uani 1 1 d D . . H16A H 0.5264 0.8137 0.0130 0.184 Uiso 1 1 calc R . . H16B H 0.5958 0.8630 0.0222 0.184 Uiso 1 1 calc R . . C17 C 0.6137(5) 0.7778(4) 0.1022(7) 0.097(3) Uani 1 1 d D . . H17A H 0.6528 0.7709 0.0441 0.117 Uiso 1 1 calc R . . H17B H 0.5827 0.7375 0.1059 0.117 Uiso 1 1 calc R . . Si3 Si 0.53210(12) 0.94278(11) 0.3636(2) 0.0836(6) Uani 1 1 d DU . . C18 C 0.4391(6) 0.9203(7) 0.4363(11) 0.159(5) Uani 1 1 d DU . . H18A H 0.4247 0.9555 0.4878 0.238 Uiso 1 1 calc R . . H18B H 0.4458 0.8796 0.4782 0.238 Uiso 1 1 calc R . . H18C H 0.3993 0.9145 0.3802 0.238 Uiso 1 1 calc R . . C19 C 0.5148(8) 1.0268(4) 0.2941(10) 0.140(4) Uani 1 1 d DU . . H19A H 0.4983 1.0583 0.3507 0.209 Uiso 1 1 calc R . . H19B H 0.4755 1.0224 0.2368 0.209 Uiso 1 1 calc R . . H19C H 0.5618 1.0421 0.2595 0.209 Uiso 1 1 calc R . . C20 C 0.6050(5) 0.9561(5) 0.4790(8) 0.116(3) Uani 1 1 d DU . . H20A H 0.5870 0.9901 0.5300 0.175 Uiso 1 1 calc R . . H20B H 0.6533 0.9697 0.4457 0.175 Uiso 1 1 calc R . . H20C H 0.6123 0.9152 0.5204 0.175 Uiso 1 1 calc R . . O1 O 0.7541(5) 0.9200(4) -0.0563(6) 0.127(3) Uani 1 1 d DU . . C21 C 0.7560(9) 0.8640(6) -0.1257(10) 0.169(5) Uani 1 1 d DU . . H21A H 0.7121 0.8353 -0.1099 0.203 Uiso 1 1 calc R . . H21B H 0.8030 0.8388 -0.1128 0.203 Uiso 1 1 calc R . . C22 C 0.7530(12) 0.8878(7) -0.2409(11) 0.213(7) Uani 1 1 d DU . . H22A H 0.8004 0.8766 -0.2807 0.255 Uiso 1 1 calc R . . H22B H 0.7100 0.8675 -0.2811 0.255 Uiso 1 1 calc R . . C23 C 0.7438(11) 0.9558(8) -0.2367(11) 0.189(6) Uani 1 1 d DU . . H23A H 0.6921 0.9676 -0.2615 0.227 Uiso 1 1 calc R . . H23B H 0.7805 0.9771 -0.2876 0.227 Uiso 1 1 calc R . . C24 C 0.7560(9) 0.9785(6) -0.1230(11) 0.164(5) Uani 1 1 d DU . . H24A H 0.8056 1.0008 -0.1161 0.197 Uiso 1 1 calc R . . H24B H 0.7155 1.0092 -0.1000 0.197 Uiso 1 1 calc R . . O2 O 0.7442(5) 1.0513(3) 0.2495(7) 0.129(2) Uani 1 1 d DU . . C25 C 0.7329(9) 1.0999(5) 0.1664(11) 0.158(5) Uani 1 1 d DU . . H25A H 0.6823 1.0946 0.1317 0.190 Uiso 1 1 calc R . . H25B H 0.7718 1.0958 0.1073 0.190 Uiso 1 1 calc R . . C26 C 0.7384(12) 1.1630(6) 0.2192(13) 0.216(7) Uani 1 1 d DU . . H26A H 0.7768 1.1902 0.1810 0.259 Uiso 1 1 calc R . . H26B H 0.6890 1.1859 0.2161 0.259 Uiso 1 1 calc R . . C27 C 0.7591(12) 1.1521(6) 0.3281(13) 0.222(7) Uani 1 1 d DU . . H27A H 0.7205 1.1710 0.3787 0.266 Uiso 1 1 calc R . . H27B H 0.8080 1.1741 0.3433 0.266 Uiso 1 1 calc R . . C28 C 0.7665(10) 1.0819(6) 0.3500(11) 0.174(5) Uani 1 1 d DU . . H28A H 0.8194 1.0705 0.3690 0.209 Uiso 1 1 calc R . . H28B H 0.7331 1.0684 0.4124 0.209 Uiso 1 1 calc R . . O3 O 0.5109(5) 0.7437(5) 0.5674(7) 0.164(4) Uani 1 1 d DU . . C29 C 0.5689(10) 0.7801(10) 0.6200(11) 0.234(7) Uani 1 1 d DU . . H29A H 0.5680 0.8260 0.5937 0.281 Uiso 1 1 calc R . . H29B H 0.6191 0.7612 0.6025 0.281 Uiso 1 1 calc R . . C30 C 0.5546(12) 0.7773(12) 0.7403(12) 0.270(8) Uani 1 1 d DU . . H30A H 0.5990 0.7587 0.7795 0.324 Uiso 1 1 calc R . . H30B H 0.5452 0.8218 0.7699 0.324 Uiso 1 1 calc R . . C31 C 0.4917(13) 0.7381(11) 0.7570(12) 0.258(8) Uani 1 1 d DU . . H31A H 0.4471 0.7652 0.7765 0.310 Uiso 1 1 calc R . . H31B H 0.5010 0.7067 0.8183 0.310 Uiso 1 1 calc R . . C32 C 0.4790(12) 0.7040(10) 0.6532(11) 0.238(7) Uani 1 1 d DU . . H32A H 0.5039 0.6606 0.6548 0.286 Uiso 1 1 calc R . . H32B H 0.4241 0.6976 0.6403 0.286 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 K1 0.0842(10) 0.0696(8) 0.0756(10) 0.0060(8) -0.0002(8) -0.0025(7) K2 0.0983(13) 0.1013(13) 0.0829(12) -0.0002(9) -0.0015(8) -0.0344(10) Si1 0.0792(14) 0.1099(18) 0.108(2) 0.0070(14) 0.0106(12) -0.0047(12) C1 0.133(8) 0.180(9) 0.097(6) 0.019(6) 0.026(5) 0.009(8) C2 0.091(6) 0.210(13) 0.257(16) -0.030(12) 0.000(8) -0.053(6) C3 0.230(12) 0.112(6) 0.225(13) 0.066(7) 0.130(11) 0.024(8) C4 0.070(4) 0.066(4) 0.080(5) -0.001(3) 0.010(3) -0.002(3) C5 0.058(3) 0.085(4) 0.066(4) 0.008(3) 0.001(3) 0.016(3) C6 0.060(4) 0.098(5) 0.066(4) -0.002(3) -0.009(3) 0.005(3) C7 0.079(5) 0.124(7) 0.068(5) -0.006(4) -0.007(4) 0.009(4) C8 0.164(10) 0.123(8) 0.076(6) -0.030(5) -0.005(6) 0.001(7) C9 0.132(7) 0.152(8) 0.063(5) -0.007(5) -0.021(5) 0.066(6) Si2 0.0658(11) 0.0707(11) 0.0822(14) -0.0025(10) 0.0019(9) -0.0047(9) C10 0.110(7) 0.123(7) 0.152(8) 0.056(6) 0.010(6) 0.018(6) C11 0.112(7) 0.134(8) 0.135(7) -0.053(6) -0.007(6) 0.033(6) C12 0.066(4) 0.079(4) 0.059(4) -0.004(3) -0.002(3) -0.010(3) C13 0.055(3) 0.071(4) 0.052(4) 0.000(3) 0.004(3) -0.003(3) C14 0.064(4) 0.081(4) 0.082(5) 0.011(4) -0.022(3) -0.005(3) C15 0.123(7) 0.113(7) 0.094(6) -0.023(5) -0.040(5) 0.016(5) C16 0.155(9) 0.217(13) 0.089(7) -0.042(7) -0.055(6) 0.085(9) C17 0.099(6) 0.103(6) 0.089(6) -0.017(4) -0.013(5) -0.006(5) Si3 0.0724(12) 0.0893(13) 0.0891(15) 0.0029(11) 0.0090(11) 0.0112(10) C18 0.090(6) 0.212(13) 0.175(12) -0.021(8) 0.050(6) 0.009(7) C19 0.201(11) 0.083(5) 0.136(9) -0.009(5) -0.019(7) 0.054(6) C20 0.114(6) 0.132(8) 0.104(6) -0.037(5) -0.011(5) 0.023(6) O1 0.165(7) 0.124(5) 0.093(4) 0.017(3) 0.016(4) -0.015(4) C21 0.241(14) 0.149(7) 0.117(8) -0.011(6) 0.012(9) -0.030(9) C22 0.308(18) 0.216(10) 0.113(7) -0.007(8) 0.049(10) -0.050(14) C23 0.231(15) 0.214(10) 0.124(7) 0.045(8) -0.024(9) -0.053(12) C24 0.205(13) 0.157(7) 0.130(8) 0.036(6) 0.005(9) -0.003(8) O2 0.178(7) 0.096(4) 0.112(5) -0.017(4) -0.013(4) 0.002(4) C25 0.216(12) 0.118(7) 0.139(7) 0.002(6) -0.035(9) 0.009(8) C26 0.342(19) 0.107(6) 0.198(11) 0.002(7) 0.009(13) 0.005(11) C27 0.40(2) 0.113(6) 0.157(9) -0.029(7) 0.027(12) -0.077(10) C28 0.279(16) 0.127(7) 0.118(7) -0.025(6) -0.012(9) -0.025(9) O3 0.190(8) 0.211(10) 0.091(5) -0.012(4) 0.007(4) -0.069(7) C29 0.254(13) 0.321(17) 0.128(8) -0.005(11) -0.021(9) -0.122(11) C30 0.313(16) 0.371(19) 0.126(8) -0.038(12) -0.022(11) -0.118(14) C31 0.343(18) 0.34(2) 0.092(7) 0.003(9) -0.001(10) -0.131(15) C32 0.318(16) 0.286(16) 0.111(9) 0.025(8) -0.022(11) -0.125(12) _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 K1 O2 2.726(7) . ? K1 O1 2.734(8) . ? K1 C13 2.932(6) . ? K1 C5 2.942(6) . ? K1 C12 3.141(7) . ? K1 C6 3.201(7) . ? K1 C4 3.329(7) . ? K1 C14 3.350(7) . ? K1 Si2 3.727(3) . ? K2 O3 2.706(9) . ? K2 C5 2.942(6) 3_465 ? K2 C13 2.951(6) . ? K2 C4 3.048(7) 3_465 ? K2 C14 3.084(7) . ? K2 C12 3.184(7) . ? K2 C6 3.215(7) 3_465 ? K2 C15 3.412(11) . ? K2 C9 3.429(9) 3_465 ? K2 C17 3.484(10) . ? K2 C7 3.505(9) 3_465 ? Si1 C4 1.833(7) . ? Si1 C1 1.865(9) . ? Si1 C2 1.873(9) . ? Si1 C3 1.875(9) . ? C4 C5 1.386(9) . ? C4 C9 1.520(10) . ? C4 K2 3.048(7) 3_565 ? C5 C6 1.380(9) . ? C5 K2 2.942(6) 3_565 ? C6 C7 1.510(9) . ? C6 Si2 1.844(7) . ? C6 K2 3.215(7) 3_565 ? C7 C8 1.493(12) . ? C7 K2 3.505(9) 3_565 ? C8 C9 1.533(13) . ? C9 K2 3.429(9) 3_565 ? Si2 C12 1.860(7) . ? Si2 C11 1.876(9) . ? Si2 C10 1.899(9) . ? C12 C13 1.374(8) . ? C12 C17 1.498(9) . ? C13 C14 1.381(9) . ? C14 C15 1.536(10) . ? C14 Si3 1.799(8) . ? C15 C16 1.476(12) . ? C16 C17 1.453(12) . ? Si3 C20 1.869(8) . ? Si3 C18 1.875(9) . ? Si3 C19 1.893(8) . ? O1 C21 1.386(12) . ? O1 C24 1.410(11) . ? C21 C22 1.434(14) . ? C22 C23 1.372(17) . ? C23 C24 1.425(14) . ? O2 C28 1.383(12) . ? O2 C25 1.391(11) . ? C25 C26 1.410(13) . ? C26 C27 1.344(17) . ? C27 C28 1.437(13) . ? O3 C29 1.385(12) . ? O3 C32 1.396(13) . ? C29 C30 1.434(14) . ? C30 C31 1.355(17) . ? C31 C32 1.413(15) . ? 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 K1 O1 109.2(2) . . ? O2 K1 C13 116.1(2) . . ? O1 K1 C13 118.4(2) . . ? O2 K1 C5 119.0(2) . . ? O1 K1 C5 99.1(2) . . ? C13 K1 C5 93.48(19) . . ? O2 K1 C12 142.0(2) . . ? O1 K1 C12 99.8(2) . . ? C13 K1 C12 25.86(16) . . ? C5 K1 C12 78.53(17) . . ? O2 K1 C6 124.1(2) . . ? O1 K1 C6 115.6(2) . . ? C13 K1 C6 68.68(17) . . ? C5 K1 C6 25.52(17) . . ? C12 K1 C6 58.20(18) . . ? O2 K1 C4 95.9(2) . . ? O1 K1 C4 101.0(2) . . ? C13 K1 C4 113.00(17) . . ? C5 K1 C4 24.56(16) . . ? C12 K1 C4 102.29(17) . . ? C6 K1 C4 45.22(16) . . ? O2 K1 C14 99.6(2) . . ? O1 K1 C14 112.7(2) . . ? C13 K1 C14 24.25(16) . . ? C5 K1 C14 117.64(17) . . ? C12 K1 C14 45.23(17) . . ? C6 K1 C14 92.53(17) . . ? C4 K1 C14 135.31(17) . . ? O2 K1 Si2 146.48(19) . . ? O1 K1 Si2 103.91(18) . . ? C13 K1 Si2 47.99(12) . . ? C5 K1 Si2 48.70(14) . . ? C12 K1 Si2 29.90(12) . . ? C6 K1 Si2 29.64(13) . . ? C4 K1 Si2 72.42(12) . . ? C14 K1 Si2 71.67(12) . . ? O3 K2 C5 118.4(2) . 3_465 ? O3 K2 C13 98.5(2) . . ? C5 K2 C13 142.8(2) 3_465 . ? O3 K2 C4 111.2(2) . 3_465 ? C5 K2 C4 26.69(17) 3_465 3_465 ? C13 K2 C4 142.04(19) . 3_465 ? O3 K2 C14 103.6(2) . . ? C5 K2 C14 128.5(2) 3_465 . ? C13 K2 C14 26.34(16) . . ? C4 K2 C14 145.1(2) 3_465 . ? O3 K2 C12 112.1(2) . . ? C5 K2 C12 126.55(19) 3_465 . ? C13 K2 C12 25.52(16) . . ? C4 K2 C12 117.28(18) 3_465 . ? C14 K2 C12 47.05(18) . . ? O3 K2 C6 101.0(2) . 3_465 ? C5 K2 C6 25.41(17) 3_465 3_465 ? C13 K2 C6 149.02(19) . 3_465 ? C4 K2 C6 47.22(18) 3_465 3_465 ? C14 K2 C6 124.16(19) . 3_465 ? C12 K2 C6 146.83(18) . 3_465 ? O3 K2 C15 128.6(3) . . ? C5 K2 C15 102.6(2) 3_465 . ? C13 K2 C15 44.93(19) . . ? C4 K2 C15 118.9(2) 3_465 . ? C14 K2 C15 26.74(18) . . ? C12 K2 C15 53.1(2) . . ? C6 K2 C15 104.4(2) 3_465 . ? O3 K2 C9 85.1(2) . 3_465 ? C5 K2 C9 45.0(2) 3_465 3_465 ? C13 K2 C9 153.0(2) . 3_465 ? C4 K2 C9 26.30(17) 3_465 3_465 ? C14 K2 C9 171.3(2) . 3_465 ? C12 K2 C9 129.2(2) . 3_465 ? C6 K2 C9 53.3(2) 3_465 3_465 ? C15 K2 C9 145.09(19) . 3_465 ? O3 K2 C17 137.6(2) . . ? C5 K2 C17 102.4(2) 3_465 . ? C13 K2 C17 43.29(17) . . ? C4 K2 C17 99.75(19) 3_465 . ? C14 K2 C17 52.46(19) . . ? C12 K2 C17 25.46(16) . . ? C6 K2 C17 121.4(2) 3_465 . ? C15 K2 C17 43.2(2) . . ? C9 K2 C17 120.3(2) 3_465 . ? O3 K2 C7 76.8(2) . 3_465 ? C5 K2 C7 43.10(18) 3_465 3_465 ? C13 K2 C7 163.6(2) . 3_465 ? C4 K2 C7 52.27(18) 3_465 3_465 ? C14 K2 C7 138.8(2) . 3_465 ? C12 K2 C7 169.19(19) . 3_465 ? C6 K2 C7 25.50(16) 3_465 3_465 ? C15 K2 C7 126.7(2) . 3_465 ? C9 K2 C7 43.2(2) 3_465 3_465 ? C17 K2 C7 145.25(18) . 3_465 ? C4 Si1 C1 113.9(5) . . ? C4 Si1 C2 109.5(6) . . ? C1 Si1 C2 106.5(6) . . ? C4 Si1 C3 112.2(4) . . ? C1 Si1 C3 108.5(6) . . ? C2 Si1 C3 105.8(7) . . ? C5 C4 C9 116.9(6) . . ? C5 C4 Si1 124.8(5) . . ? C9 C4 Si1 117.8(6) . . ? C5 C4 K2 72.4(4) . 3_565 ? C9 C4 K2 91.0(5) . 3_565 ? Si1 C4 K2 112.9(3) . 3_565 ? C5 C4 K1 61.9(4) . . ? C9 C4 K1 100.8(4) . . ? Si1 C4 K1 101.0(3) . . ? K2 C4 K1 133.3(2) 3_565 . ? C6 C5 C4 130.6(7) . . ? C6 C5 K1 87.8(4) . . ? C4 C5 K1 93.5(4) . . ? C6 C5 K2 88.4(4) . 3_565 ? C4 C5 K2 80.9(4) . 3_565 ? K1 C5 K2 168.7(3) . 3_565 ? C5 C6 C7 114.1(7) . . ? C5 C6 Si2 122.9(5) . . ? C7 C6 Si2 122.0(5) . . ? C5 C6 K1 66.7(4) . . ? C7 C6 K1 101.9(5) . . ? Si2 C6 K1 91.2(2) . . ? C5 C6 K2 66.2(4) . 3_565 ? C7 C6 K2 88.1(4) . 3_565 ? Si2 C6 K2 123.2(3) . 3_565 ? K1 C6 K2 131.8(2) . 3_565 ? C8 C7 C6 113.4(7) . . ? C8 C7 K2 98.1(6) . 3_565 ? C6 C7 K2 66.4(4) . 3_565 ? C7 C8 C9 115.3(8) . . ? C4 C9 C8 110.5(7) . . ? C4 C9 K2 62.7(4) . 3_565 ? C8 C9 K2 100.3(6) . 3_565 ? C6 Si2 C12 112.8(3) . . ? C6 Si2 C11 112.7(4) . . ? C12 Si2 C11 111.0(4) . . ? C6 Si2 C10 104.8(5) . . ? C12 Si2 C10 110.0(4) . . ? C11 Si2 C10 105.0(5) . . ? C6 Si2 K1 59.2(2) . . ? C12 Si2 K1 57.3(2) . . ? C11 Si2 K1 114.2(4) . . ? C10 Si2 K1 140.8(4) . . ? C13 C12 C17 115.1(6) . . ? C13 C12 Si2 119.4(5) . . ? C17 C12 Si2 125.1(5) . . ? C13 C12 K1 68.5(4) . . ? C17 C12 K1 101.2(5) . . ? Si2 C12 K1 92.8(2) . . ? C13 C12 K2 67.7(4) . . ? C17 C12 K2 88.5(4) . . ? Si2 C12 K2 117.2(3) . . ? K1 C12 K2 135.1(2) . . ? C12 C13 C14 130.6(6) . . ? C12 C13 K1 85.6(4) . . ? C14 C13 K1 95.1(4) . . ? C12 C13 K2 86.8(4) . . ? C14 C13 K2 82.2(4) . . ? K1 C13 K2 167.2(2) . . ? C13 C14 C15 115.5(6) . . ? C13 C14 Si3 125.3(5) . . ? C15 C14 Si3 119.1(5) . . ? C13 C14 K2 71.5(4) . . ? C15 C14 K2 88.7(5) . . ? Si3 C14 K2 109.9(3) . . ? C13 C14 K1 60.7(4) . . ? C15 C14 K1 100.8(5) . . ? Si3 C14 K1 107.1(3) . . ? K2 C14 K1 130.6(2) . . ? C16 C15 C14 113.9(7) . . ? C16 C15 K2 95.0(7) . . ? C14 C15 K2 64.6(5) . . ? C17 C16 C15 120.0(8) . . ? C25 O2 K1 116.0(6) . . ? O2 C25 C26 108.0(10) . . ? C27 C26 C25 106.9(10) . . ? C26 C27 C28 110.6(10) . . ? O2 C28 C27 104.8(10) . . ? C29 O3 C32 105.4(11) . . ? C29 O3 K2 120.6(7) . . ? C32 O3 K2 132.9(8) . . ? O3 C29 C30 107.0(11) . . ? C31 C30 C29 107.7(11) . . ? C30 C31 C32 106.3(12) . . ? O3 C32 C31 106.5(11) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.599 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.068 #=END data_leuu08 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H41 Li N2 Si2' _chemical_formula_weight 348.65 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' 'N' 'N' 0.0061 0.0033 '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 Pna2(1) 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 19.325(4) _cell_length_b 8.660(2) _cell_length_c 14.750(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2468.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 10 _exptl_crystal_description 'YELLOW PRISM' _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.30 _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_000 776 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.9578 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ROTATION ANODE' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU AFC7R' _diffrn_measurement_method '\W SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.36 _diffrn_reflns_number 4366 _diffrn_reflns_av_R_equivalents 0.1711 _diffrn_reflns_av_sigmaI/netI 0.1712 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2263 _reflns_number_gt 614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC DIFFRACTOMETER CONTROL' _computing_cell_refinement 'MSC/AFC DIFFRACTOMETER CONTROL' _computing_data_reduction 'MSC/AFC DIFFRACTOMETER CONTROL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.0046(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.2(3) _refine_ls_number_reflns 2263 _refine_ls_number_parameters 203 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.2639 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 0.729 _refine_ls_restrained_S_all 0.866 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.12928(17) 0.0684(3) 0.6153(3) 0.0712(11) Uani 1 1 d . . . H1A H -0.1111 0.0167 0.5612 0.085 Uiso 1 1 calc R . . Li1 Li -0.1314(4) 0.3152(6) 0.6075(5) 0.093(2) Uani 1 1 d . A . C2 C -0.20182(16) 0.0880(4) 0.6164(2) 0.0917(14) Uani 1 1 d D . . C3 C -0.2302(2) 0.1228(5) 0.7119(3) 0.139(2) Uani 1 1 d . . . H3A H -0.2376 0.2333 0.7171 0.167 Uiso 1 1 calc R . . H3B H -0.2748 0.0728 0.7183 0.167 Uiso 1 1 calc R . . C4 C -0.1857(2) 0.0730(5) 0.7864(3) 0.143(2) Uani 1 1 d . . . H4A H -0.1878 -0.0387 0.7905 0.172 Uiso 1 1 calc R . . H4B H -0.2041 0.1146 0.8425 0.172 Uiso 1 1 calc R . . C5 C -0.1119(2) 0.1204(5) 0.7779(3) 0.1270(18) Uani 1 1 d . . . H5A H -0.0847 0.0637 0.8221 0.152 Uiso 1 1 calc R . . H5B H -0.1080 0.2294 0.7924 0.152 Uiso 1 1 calc R . . C6 C -0.08137(18) 0.0925(4) 0.6831(3) 0.0965(14) Uani 1 1 d D . . Si1 Si 0.00959(5) 0.05323(14) 0.67744(10) 0.1094(4) Uani 1 1 d D . . C7 C 0.0370(2) -0.1082(5) 0.7530(4) 0.194(3) Uani 1 1 d D . . H7A H 0.0857 -0.1257 0.7460 0.291 Uiso 1 1 calc R . . H7B H 0.0121 -0.2002 0.7370 0.291 Uiso 1 1 calc R . . H7C H 0.0272 -0.0817 0.8149 0.291 Uiso 1 1 calc R . . C8 C 0.06175(16) 0.2253(5) 0.7135(3) 0.154(2) Uani 1 1 d D . . H8A H 0.1101 0.2026 0.7072 0.231 Uiso 1 1 calc R . . H8B H 0.0517 0.2493 0.7756 0.231 Uiso 1 1 calc R . . H8C H 0.0501 0.3121 0.6760 0.231 Uiso 1 1 calc R . . C9 C 0.03579(18) -0.0040(5) 0.5596(3) 0.1407(19) Uani 1 1 d D . . H9A H 0.0848 -0.0224 0.5580 0.211 Uiso 1 1 calc R . . H9B H 0.0243 0.0775 0.5182 0.211 Uiso 1 1 calc R . . H9C H 0.0117 -0.0964 0.5425 0.211 Uiso 1 1 calc R . . Si2 Si -0.25937(5) 0.04638(14) 0.52314(9) 0.1089(4) Uani 1 1 d D . . C10 C -0.32651(17) -0.1047(4) 0.5497(4) 0.173(2) Uani 1 1 d D . . H10A H -0.3550 -0.1217 0.4974 0.260 Uiso 1 1 calc R . . H10B H -0.3548 -0.0701 0.5992 0.260 Uiso 1 1 calc R . . H10C H -0.3039 -0.1994 0.5662 0.260 Uiso 1 1 calc R . . C11 C -0.2105(2) -0.0321(5) 0.4226(3) 0.1462(19) Uani 1 1 d D . . H11A H -0.2424 -0.0533 0.3742 0.219 Uiso 1 1 calc R . . H11B H -0.1872 -0.1256 0.4396 0.219 Uiso 1 1 calc R . . H11C H -0.1771 0.0427 0.4028 0.219 Uiso 1 1 calc R . . C12 C -0.31082(18) 0.2187(4) 0.4872(3) 0.1337(19) Uani 1 1 d D . . H12A H -0.3403 0.1910 0.4374 0.200 Uiso 1 1 calc R . . H12B H -0.2800 0.2997 0.4687 0.200 Uiso 1 1 calc R . . H12C H -0.3386 0.2539 0.5370 0.200 Uiso 1 1 calc R . . C13 C -0.1143(3) 0.5621(5) 0.7499(3) 0.189(3) Uani 1 1 d D A . H13A H -0.1329 0.4933 0.7947 0.283 Uiso 1 1 calc R . . H13B H -0.1216 0.6669 0.7687 0.283 Uiso 1 1 calc R . . H13C H -0.0656 0.5434 0.7432 0.283 Uiso 1 1 calc R . . C14 C -0.2220(3) 0.5672(5) 0.6742(5) 0.206(3) Uani 1 1 d D A . H14A H -0.2414 0.4986 0.7185 0.309 Uiso 1 1 calc R . . H14B H -0.2445 0.5513 0.6169 0.309 Uiso 1 1 calc R . . H14C H -0.2286 0.6721 0.6933 0.309 Uiso 1 1 calc R . . N1 N -0.1483(2) 0.5361(4) 0.6647(2) 0.1446(17) Uani 1 1 d D . . C15 C -0.1462(4) 0.6436(10) 0.5838(6) 0.174 Uiso 0.50 1 d PD A 1 H15A H -0.1431 0.7501 0.6039 0.174 Uiso 0.50 1 calc PR A 1 H15B H -0.1878 0.6319 0.5477 0.174 Uiso 0.50 1 calc PR A 1 C16 C -0.0802(3) 0.5994(6) 0.5257(5) 0.102(2) Uiso 0.50 1 d PD A 1 H16A H -0.0752 0.6696 0.4749 0.123 Uiso 0.50 1 calc PR A 1 H16B H -0.0388 0.6054 0.5627 0.123 Uiso 0.50 1 calc PR A 1 N2 N -0.09100(18) 0.4361(3) 0.4923(2) 0.1094(13) Uani 1 1 d D . . C17 C -0.1288(2) 0.4042(6) 0.4085(3) 0.170(3) Uani 1 1 d D A . H17A H -0.1248 0.2965 0.3939 0.255 Uiso 1 1 calc R . . H17B H -0.1096 0.4648 0.3601 0.255 Uiso 1 1 calc R . . H17C H -0.1766 0.4304 0.4164 0.255 Uiso 1 1 calc R . . C18 C -0.01823(17) 0.4071(5) 0.4729(3) 0.188(3) Uani 1 1 d D A . H18A H -0.0122 0.3009 0.4560 0.281 Uiso 1 1 calc R . . H18B H 0.0089 0.4288 0.5259 0.281 Uiso 1 1 calc R . . H18C H -0.0034 0.4725 0.4240 0.281 Uiso 1 1 calc R . . C15' C -0.10152(17) 0.6379(5) 0.6040(3) 0.106(3) Uiso 0.50 1 d PRD A 2 H15C H -0.0531 0.6155 0.6156 0.127 Uiso 0.50 1 calc PR B 2 H16D H -0.1097 0.7464 0.6163 0.127 Uiso 0.50 1 calc PR C 2 C16' C -0.1206(4) 0.5986(7) 0.5017(5) 0.109(3) Uiso 0.50 1 d PD A 2 H16C H -0.1702 0.5998 0.4920 0.130 Uiso 0.50 1 calc PR A 2 H16D H -0.0987 0.6700 0.4598 0.130 Uiso 0.50 1 calc PR A 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 C1 0.0841(18) 0.0497(17) 0.080(3) 0.000(2) 0.011(2) 0.006(2) Li1 0.118(4) 0.072(3) 0.089(5) 0.026(5) 0.004(5) -0.005(4) C2 0.072(2) 0.102(3) 0.101(3) 0.004(2) -0.021(3) 0.001(2) C3 0.141(3) 0.122(3) 0.155(5) 0.026(3) 0.042(4) 0.017(3) C4 0.167(4) 0.153(4) 0.111(4) 0.022(4) 0.039(4) 0.053(3) C5 0.134(3) 0.147(3) 0.100(4) -0.012(3) -0.008(3) -0.006(3) C6 0.103(2) 0.108(3) 0.078(3) 0.014(3) -0.010(3) -0.011(2) Si1 0.0827(6) 0.1133(8) 0.1321(10) 0.0180(10) -0.0265(9) -0.0097(7) C7 0.135(3) 0.189(4) 0.257(6) 0.115(4) -0.045(5) 0.029(4) C8 0.110(3) 0.172(4) 0.179(4) -0.030(4) -0.047(4) -0.033(3) C9 0.101(2) 0.150(4) 0.171(4) -0.013(4) 0.035(4) 0.012(3) Si2 0.0791(6) 0.1090(7) 0.1385(10) -0.0009(11) -0.0253(9) 0.0033(7) C10 0.123(3) 0.159(4) 0.238(6) 0.031(5) -0.073(4) -0.050(3) C11 0.155(4) 0.172(4) 0.112(3) -0.078(3) -0.036(4) 0.031(4) C12 0.111(3) 0.150(3) 0.140(4) 0.012(4) -0.008(3) 0.021(3) C13 0.296(7) 0.138(4) 0.133(5) -0.013(4) 0.030(6) -0.033(5) C14 0.269(6) 0.125(4) 0.223(6) -0.018(5) 0.044(7) 0.056(5) N1 0.243(4) 0.106(2) 0.085(3) 0.014(2) 0.050(3) 0.005(3) N2 0.147(2) 0.0806(19) 0.100(3) 0.009(2) 0.022(2) -0.004(2) C17 0.174(4) 0.195(5) 0.143(5) 0.017(4) 0.034(5) 0.008(4) C18 0.108(3) 0.281(6) 0.175(5) 0.055(5) 0.045(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.379(5) . ? C1 C2 1.412(4) . ? C1 Li1 2.140(6) . ? Li1 N1 2.116(7) . ? Li1 N2 2.145(7) . ? Li1 C2 2.395(7) . ? Li1 C6 2.428(7) . ? C2 C3 1.541(5) . ? C2 Si2 1.805(4) . ? C3 C4 1.460(6) . ? C4 C5 1.490(5) . ? C5 C6 1.537(6) . ? C6 Si1 1.792(4) . ? Si1 C7 1.864(5) . ? Si1 C8 1.876(4) . ? Si1 C9 1.877(4) . ? Si2 C12 1.870(4) . ? Si2 C10 1.884(4) . ? Si2 C11 1.885(4) . ? C13 N1 1.435(6) . ? C14 N1 1.456(6) . ? N1 C15 1.515(9) . ? N1 C15' 1.548(5) . ? C15 C16 1.582(10) . ? C16 N2 1.512(6) . ? N2 C18 1.457(5) . ? N2 C17 1.462(6) . ? N2 C16' 1.526(6) . ? C15' C16' 1.591(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 129.8(3) . . ? C6 C1 Li1 84.3(3) . . ? C2 C1 Li1 82.0(3) . . ? N1 Li1 C1 152.2(4) . . ? N1 Li1 N2 86.0(2) . . ? C1 Li1 N2 121.5(3) . . ? N1 Li1 C2 129.3(3) . . ? C1 Li1 C2 35.73(14) . . ? N2 Li1 C2 130.6(3) . . ? N1 Li1 C6 126.6(4) . . ? C1 Li1 C6 34.40(15) . . ? N2 Li1 C6 127.3(3) . . ? C2 Li1 C6 63.20(17) . . ? C1 C2 C3 112.8(3) . . ? C1 C2 Si2 125.4(3) . . ? C3 C2 Si2 121.1(2) . . ? C1 C2 Li1 62.3(2) . . ? C3 C2 Li1 95.2(3) . . ? Si2 C2 Li1 118.2(2) . . ? C4 C3 C2 114.9(3) . . ? C3 C4 C5 114.8(4) . . ? C4 C5 C6 113.6(4) . . ? C1 C6 C5 115.2(3) . . ? C1 C6 Si1 126.6(3) . . ? C5 C6 Si1 116.6(3) . . ? C1 C6 Li1 61.3(2) . . ? C5 C6 Li1 98.0(3) . . ? Si1 C6 Li1 121.3(2) . . ? C6 Si1 C7 113.14(19) . . ? C6 Si1 C8 111.29(17) . . ? C7 Si1 C8 105.9(2) . . ? C6 Si1 C9 111.0(2) . . ? C7 Si1 C9 106.2(2) . . ? C8 Si1 C9 109.1(2) . . ? C2 Si2 C12 112.60(17) . . ? C2 Si2 C10 113.8(2) . . ? C12 Si2 C10 104.32(17) . . ? C2 Si2 C11 111.29(17) . . ? C12 Si2 C11 109.3(2) . . ? C10 Si2 C11 105.0(2) . . ? C13 N1 C14 109.6(4) . . ? C13 N1 C15 125.5(5) . . ? C14 N1 C15 89.3(4) . . ? C13 N1 C15' 98.6(4) . . ? C14 N1 C15' 121.4(4) . . ? C15 N1 C15' 34.7(3) . . ? C13 N1 Li1 114.8(3) . . ? C14 N1 Li1 110.8(4) . . ? C15 N1 Li1 103.7(4) . . ? C15' N1 Li1 101.2(3) . . ? N1 C15 C16 107.5(6) . . ? N2 C16 C15 107.0(5) . . ? C18 N2 C17 106.5(3) . . ? C18 N2 C16 95.3(3) . . ? C17 N2 C16 121.4(4) . . ? C18 N2 C16' 122.6(4) . . ? C17 N2 C16' 93.7(4) . . ? C16 N2 C16' 32.8(4) . . ? C18 N2 Li1 115.0(3) . . ? C17 N2 Li1 113.3(3) . . ? C16 N2 Li1 104.4(4) . . ? C16' N2 Li1 104.0(4) . . ? N1 C15' C16' 107.0(4) . . ? N2 C16' C15' 101.3(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.151 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.033