Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Eisen, Moris S.' 'Lisovskii, Anatoli' _publ_contact_author_name 'Prof Moris S Eisen' _publ_contact_author_address ; Prof Moris S Eisen Department of Chemistry & Inst of Catalysis Science & Technology Technion - Israel Institute of Technology Technion City Haifa 32000 ISRAEL ; data_complex1 _database_code_CSD 156013 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex-1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H60 Li2 N4 O Si4' _chemical_formula_weight 643.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Si' 'Si' 0.0817 0.0704 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.752(3) _cell_length_b 10.695(3) _cell_length_c 36.613(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.79(3) _cell_angle_gamma 90.00 _cell_volume 4196(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 9.6 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.168 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9359 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Philips PW 1100 four-cicle diffractometer' _diffrn_measurement_method \w/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '120 min' _diffrn_standards_decay_% '8.7, 2.1, 4.6' _diffrn_reflns_number 7583 _diffrn_reflns_av_R_equivalents 0.1611 _diffrn_reflns_av_sigmaI/netI 0.4854 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7279 _reflns_number_gt 1666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Philips PW 1100/20 (Philips, 1973)' _computing_cell_refinement 'Philips PW 1100/20 (Philips, 1973)' _computing_data_reduction 'PROCN (Philips, 1973)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TEXSAN v.1.10 (MSC, 2000)' _computing_publication_material ? _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^)+(0.0154P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7279 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2635 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.049 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 0.0711(4) 0.0892(4) 0.34148(14) 0.060(2) Uani 1 1 d . . . Li2 Li 0.1610(4) 0.2117(5) 0.39373(16) 0.076(2) Uani 1 1 d . . . Si1 Si 0.35487(7) 0.04116(8) 0.36042(2) 0.0539(3) Uani 1 1 d . . . Si2 Si 0.16541(8) -0.08088(8) 0.40271(2) 0.0584(3) Uani 1 1 d . . . Si3 Si -0.09145(9) 0.29063(11) 0.43730(2) 0.0817(4) Uani 1 1 d . . . Si4 Si 0.06301(8) 0.35046(9) 0.29862(2) 0.0633(4) Uani 1 1 d . . . N1 N 0.21050(17) 0.03697(17) 0.37594(5) 0.0369(8) Uani 1 1 d . . . N2 N -0.01646(18) 0.2604(2) 0.39897(6) 0.0539(9) Uani 1 1 d . . . N3 N 0.03957(17) 0.27612(19) 0.33909(5) 0.0439(8) Uani 1 1 d . . . N4 N 0.2738(2) 0.3339(2) 0.42310(7) 0.0858(11) Uani 1 1 d . . . C1 C -0.0311(2) 0.3098(2) 0.36611(7) 0.0433(10) Uani 1 1 d . . . C2 C -0.1287(2) 0.4108(2) 0.35776(6) 0.0430(10) Uani 1 1 d . . . C3 C -0.2496(2) 0.3759(2) 0.34647(7) 0.0490(11) Uani 1 1 d . . . H3 H -0.2680 0.2902 0.3440 0.059 Uiso 1 1 calc . . . C4 C -0.3447(2) 0.4612(3) 0.33867(7) 0.0566(11) Uani 1 1 d . . . H4 H -0.4264 0.4329 0.3324 0.068 Uiso 1 1 calc . . . C5 C -0.3198(2) 0.5890(3) 0.34004(7) 0.0608(12) Uani 1 1 d . . . C6 C -0.2000(2) 0.6248(2) 0.35103(7) 0.0552(11) Uani 1 1 d . . . H6 H -0.1817 0.7107 0.3525 0.066 Uiso 1 1 calc . . . C7 C -0.1059(2) 0.5409(3) 0.35990(7) 0.0607(12) Uani 1 1 d . . . H7 H -0.0254 0.5701 0.3675 0.073 Uiso 1 1 calc . . . C8 C -0.4192(2) 0.6844(3) 0.33016(8) 0.0950(15) Uani 1 1 d . . . H8A H -0.5006 0.6482 0.3330 0.143 Uiso 1 1 calc R . . H8B H -0.4148 0.7102 0.3049 0.143 Uiso 1 1 calc R . . H8C H -0.4066 0.7564 0.3461 0.143 Uiso 1 1 calc R . . C9 C 0.3340(3) 0.4187(2) 0.43313(7) 0.0617(12) Uani 1 1 d . . . C10 C 0.4135(3) 0.5192(2) 0.44369(7) 0.0558(11) Uani 1 1 d . . . C11 C 0.3877(3) 0.5898(3) 0.47270(8) 0.0774(13) Uani 1 1 d . . . H11 H 0.3161 0.5710 0.4847 0.093 Uiso 1 1 calc . . . C12 C 0.4622(3) 0.6889(3) 0.48555(7) 0.0766(13) Uani 1 1 d . . . H12 H 0.4445 0.7341 0.5065 0.092 Uiso 1 1 calc . . . C13 C 0.5636(3) 0.7187(3) 0.46631(8) 0.0820(14) Uani 1 1 d . . . C14 C 0.5911(2) 0.6490(3) 0.43791(8) 0.0719(13) Uani 1 1 d . . . H14 H 0.6622 0.6689 0.4258 0.086 Uiso 1 1 calc . . . C15 C 0.5180(2) 0.5479(3) 0.42562(7) 0.0693(13) Uani 1 1 d . . . H15 H 0.5390 0.5000 0.4055 0.083 Uiso 1 1 calc . . . C16 C 0.6511(3) 0.8272(3) 0.47674(9) 0.1322(17) Uani 1 1 d . . . H16A H 0.6352 0.8578 0.5009 0.198 Uiso 1 1 calc R . . H16B H 0.6369 0.8940 0.4589 0.198 Uiso 1 1 calc R . . H16C H 0.7369 0.7990 0.4771 0.198 Uiso 1 1 calc R . . C17 C -0.1544(3) 0.0153(5) 0.29174(9) 0.171(2) Uani 1 1 d D . . H17A H -0.1511 0.0906 0.2766 0.205 Uiso 1 1 calc . . . H17B H -0.1872 -0.0525 0.2757 0.205 Uiso 1 1 calc . . . C18 C -0.2355(3) 0.0357(3) 0.31688(8) 0.1308(18) Uani 1 1 d D . . H18A H -0.3122 0.0698 0.3051 0.196 Uiso 1 1 calc R . . H18B H -0.1998 0.0945 0.3350 0.196 Uiso 1 1 calc R . . H18C H -0.2532 -0.0425 0.3288 0.196 Uiso 1 1 calc R . . C19 C 0.0059(4) -0.1404(4) 0.29436(9) 0.142(2) Uani 1 1 d D . . H19A H 0.0835 -0.1628 0.3088 0.170 Uiso 1 1 calc . . . H19B H -0.0585 -0.1994 0.3008 0.170 Uiso 1 1 calc . . . C20 C 0.0241(3) -0.1563(4) 0.25725(8) 0.174(2) Uani 1 1 d D . . H20A H 0.0269 -0.2448 0.2516 0.261 Uiso 1 1 calc R . . H20B H 0.1022 -0.1174 0.2520 0.261 Uiso 1 1 calc R . . H20C H -0.0442 -0.1175 0.2424 0.261 Uiso 1 1 calc R . . C1S1 C 0.4856(2) -0.0180(3) 0.39410(7) 0.0719(13) Uani 1 1 d . . . H1S1 H 0.4722 -0.1057 0.3992 0.108 Uiso 1 1 calc R . . H2S1 H 0.4865 0.0296 0.4167 0.108 Uiso 1 1 calc R . . H3S1 H 0.5649 -0.0079 0.3836 0.108 Uiso 1 1 calc R . . C2S1 C 0.3634(2) -0.0497(3) 0.31655(7) 0.0751(13) Uani 1 1 d . . . H4S1 H 0.3476 -0.1374 0.3210 0.113 Uiso 1 1 calc R . . H5S1 H 0.4458 -0.0402 0.3080 0.113 Uiso 1 1 calc R . . H6S1 H 0.3012 -0.0181 0.2981 0.113 Uiso 1 1 calc R . . C3S1 C 0.4041(2) 0.2039(2) 0.34932(8) 0.0731(13) Uani 1 1 d . . . H7S1 H 0.4473 0.2415 0.3709 0.110 Uiso 1 1 calc R . . H8S1 H 0.3311 0.2534 0.3416 0.110 Uiso 1 1 calc R . . H9S1 H 0.4596 0.2011 0.3297 0.110 Uiso 1 1 calc R . . C1S2 C 0.2106(3) -0.2427(3) 0.38805(8) 0.0887(15) Uani 1 1 d . . . H1S2 H 0.1758 -0.2580 0.3631 0.133 Uiso 1 1 calc R . . H2S2 H 0.1783 -0.3042 0.4043 0.133 Uiso 1 1 calc R . . H3S2 H 0.3008 -0.2492 0.3892 0.133 Uiso 1 1 calc R . . C2S2 C -0.0094(2) -0.0828(3) 0.40249(7) 0.0784(13) Uani 1 1 d . . . H4S2 H -0.0454 -0.1139 0.3791 0.118 Uiso 1 1 calc R . . H5S2 H -0.0393 0.0013 0.4063 0.118 Uiso 1 1 calc R . . H6S2 H -0.0336 -0.1369 0.4220 0.118 Uiso 1 1 calc R . . C3S2 C 0.2274(2) -0.0676(3) 0.45162(7) 0.0808(14) Uani 1 1 d . . . H7S2 H 0.1901 0.0041 0.4627 0.121 Uiso 1 1 calc R . . H8S2 H 0.3173 -0.0572 0.4530 0.121 Uiso 1 1 calc R . . H9S2 H 0.2072 -0.1429 0.4647 0.121 Uiso 1 1 calc R . . C1S3 C 0.0038(3) 0.2153(3) 0.47552(7) 0.1163(17) Uani 1 1 d . . . H1S3 H 0.0865 0.2522 0.4778 0.174 Uiso 1 1 calc R . . H2S3 H 0.0103 0.1265 0.4707 0.174 Uiso 1 1 calc R . . H3S3 H -0.0356 0.2278 0.4981 0.174 Uiso 1 1 calc R . . C2S3 C -0.0993(3) 0.4619(3) 0.45002(8) 0.1241(17) Uani 1 1 d . . . H4S3 H -0.1625 0.5032 0.4338 0.186 Uiso 1 1 calc R . . H5S3 H -0.0189 0.5008 0.4476 0.186 Uiso 1 1 calc R . . H6S3 H -0.1206 0.4695 0.4752 0.186 Uiso 1 1 calc R . . C3S3 C -0.2501(2) 0.2228(4) 0.43467(8) 0.1269(19) Uani 1 1 d . . . H7S3 H -0.3067 0.2756 0.4195 0.190 Uiso 1 1 calc R . . H8S3 H -0.2784 0.2176 0.4591 0.190 Uiso 1 1 calc R . . H9S3 H -0.2486 0.1398 0.4241 0.190 Uiso 1 1 calc R . . C1S4 C 0.1746(3) 0.4868(3) 0.30594(9) 0.1009(15) Uani 1 1 d . . . H1S4 H 0.2577 0.4557 0.3133 0.151 Uiso 1 1 calc R . . H2S4 H 0.1471 0.5409 0.3249 0.151 Uiso 1 1 calc R . . H3S4 H 0.1763 0.5336 0.2833 0.151 Uiso 1 1 calc R . . C2S4 C -0.0777(2) 0.4078(3) 0.27021(7) 0.0957(14) Uani 1 1 d . . . H4S4 H -0.1155 0.4758 0.2829 0.143 Uiso 1 1 calc R . . H5S4 H -0.1373 0.3401 0.2662 0.143 Uiso 1 1 calc R . . H6S4 H -0.0533 0.4373 0.2468 0.143 Uiso 1 1 calc R . . C3S4 C 0.1345(2) 0.2307(3) 0.26909(7) 0.0700(12) Uani 1 1 d . . . H7S4 H 0.2109 0.1990 0.2817 0.105 Uiso 1 1 calc R . . H8S4 H 0.1531 0.2690 0.2462 0.105 Uiso 1 1 calc R . . H9S4 H 0.0763 0.1622 0.2641 0.105 Uiso 1 1 calc R . . O1 O -0.03040(15) -0.01620(19) 0.30509(5) 0.0732(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.040(3) 0.040(3) 0.099(4) -0.007(3) 0.004(3) -0.007(3) Li2 0.039(3) 0.073(4) 0.115(5) -0.019(4) -0.002(3) -0.022(3) Si1 0.0430(5) 0.0520(6) 0.0661(6) 0.0041(6) 0.0011(5) 0.0037(5) Si2 0.0670(6) 0.0530(6) 0.0538(6) 0.0017(6) -0.0035(5) -0.0029(6) Si3 0.0672(6) 0.1248(9) 0.0554(6) 0.0082(7) 0.0181(5) 0.0169(7) Si4 0.0717(6) 0.0682(7) 0.0519(6) 0.0151(6) 0.0161(5) 0.0251(6) N1 0.0457(13) 0.0222(13) 0.0427(14) 0.0059(12) 0.0021(12) -0.0026(12) N2 0.0527(15) 0.0615(16) 0.0467(15) 0.0223(14) -0.0008(13) 0.0207(14) N3 0.0363(13) 0.0529(15) 0.0424(14) -0.0075(14) 0.0035(11) 0.0212(13) N4 0.106(2) 0.0612(18) 0.090(2) -0.0173(18) 0.0074(17) -0.0008(17) C1 0.0276(16) 0.0434(19) 0.0579(19) -0.0152(17) -0.0019(15) -0.0029(16) C2 0.0302(16) 0.062(2) 0.0361(17) -0.0059(18) -0.0022(14) -0.0014(17) C3 0.0506(19) 0.0271(18) 0.068(2) -0.0057(17) 0.0009(17) 0.0066(16) C4 0.0360(17) 0.066(2) 0.069(2) -0.003(2) 0.0125(16) -0.0012(18) C5 0.0496(19) 0.065(2) 0.070(2) 0.002(2) 0.0148(17) 0.0011(18) C6 0.071(2) 0.0239(18) 0.073(2) 0.0042(17) 0.0140(18) 0.0160(17) C7 0.065(2) 0.043(2) 0.074(2) -0.0071(19) 0.0064(18) -0.0097(19) C8 0.092(3) 0.077(3) 0.116(3) 0.018(2) 0.010(2) 0.039(2) C9 0.094(2) 0.0297(18) 0.062(2) -0.0036(18) 0.0091(19) 0.0164(19) C10 0.091(2) 0.0327(18) 0.0419(19) -0.0156(17) -0.0045(17) 0.0062(18) C11 0.082(2) 0.057(2) 0.092(2) -0.020(2) -0.002(2) -0.002(2) C12 0.104(2) 0.086(3) 0.042(2) -0.014(2) 0.0181(18) 0.028(2) C13 0.127(3) 0.060(2) 0.055(2) -0.0292(19) -0.013(2) 0.022(2) C14 0.0325(19) 0.075(2) 0.107(3) 0.037(2) -0.0024(19) 0.0042(19) C15 0.072(2) 0.085(3) 0.055(2) 0.008(2) 0.0271(17) 0.003(2) C16 0.155(3) 0.076(3) 0.147(3) 0.007(3) -0.096(3) -0.030(3) C17 0.052(2) 0.350(6) 0.109(3) -0.004(4) -0.002(2) 0.024(4) C18 0.089(3) 0.128(3) 0.169(3) -0.081(3) -0.029(3) 0.030(3) C19 0.167(4) 0.127(4) 0.127(3) 0.022(3) -0.012(3) 0.011(3) C20 0.154(4) 0.254(5) 0.115(3) -0.007(4) 0.020(3) 0.034(4) C1S1 0.054(2) 0.077(2) 0.079(2) 0.011(2) -0.0227(18) 0.013(2) C2S1 0.077(2) 0.084(2) 0.063(2) -0.036(2) -0.0007(18) 0.025(2) C3S1 0.0451(19) 0.074(2) 0.101(3) -0.001(2) 0.0101(18) -0.0278(19) C1S2 0.115(3) 0.053(2) 0.095(3) -0.005(2) -0.006(2) 0.000(2) C2S2 0.075(2) 0.092(3) 0.068(2) 0.018(2) 0.0043(19) -0.016(2) C3S2 0.088(2) 0.077(3) 0.077(2) 0.008(2) 0.006(2) -0.007(2) C1S3 0.117(3) 0.178(4) 0.056(2) 0.036(3) 0.020(2) 0.046(3) C2S3 0.176(3) 0.112(3) 0.090(3) -0.023(3) 0.041(3) 0.041(3) C3S3 0.068(2) 0.221(4) 0.097(3) 0.001(3) 0.033(2) -0.002(3) C1S4 0.114(3) 0.050(2) 0.143(3) 0.045(2) 0.039(2) -0.007(2) C2S4 0.103(2) 0.137(3) 0.048(2) 0.041(2) 0.0167(19) 0.067(2) C3S4 0.085(2) 0.077(2) 0.0504(19) 0.0097(19) 0.0233(18) 0.017(2) O1 0.0527(12) 0.0991(17) 0.0659(14) 0.0086(14) -0.0075(11) 0.0030(13) _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 N1 1.958(5) . ? Li1 O1 1.998(5) . ? Li1 N3 2.029(5) . ? Li1 Li2 2.450(7) . ? Li1 C1 2.785(5) . ? Li1 Si2 2.997(5) . ? Li1 Si1 3.115(5) . ? Li2 N2 2.003(5) . ? Li2 N4 2.029(6) . ? Li2 N1 2.063(6) . ? Li2 N3 2.397(6) . ? Li2 C1 2.458(5) . ? Li2 Si1 3.095(5) . ? Li2 Si2 3.146(6) . ? Si1 N1 1.698(2) . ? Si1 C3S1 1.874(3) . ? Si1 C2S1 1.886(3) . ? Si1 C1S1 1.899(3) . ? Si2 N1 1.692(2) . ? Si2 C3S2 1.863(3) . ? Si2 C2S2 1.879(3) . ? Si2 C1S2 1.888(3) . ? Si3 N2 1.707(2) . ? Si3 C3S3 1.849(3) . ? Si3 C1S3 1.848(3) . ? Si3 C2S3 1.894(3) . ? Si4 N3 1.718(2) . ? Si4 C2S4 1.866(3) . ? Si4 C3S4 1.882(3) . ? Si4 C1S4 1.893(3) . ? N2 C1 1.311(3) . ? N3 C1 1.346(3) . ? N4 C9 1.156(4) . ? C1 C2 1.519(3) . ? C2 C3 1.382(3) . ? C2 C7 1.413(4) . ? C3 C4 1.382(3) . ? C4 C5 1.393(4) . ? C5 C6 1.371(4) . ? C5 C8 1.500(4) . ? C6 C7 1.372(4) . ? C9 C10 1.407(4) . ? C10 C11 1.350(4) . ? C10 C15 1.385(4) . ? C11 C12 1.387(4) . ? C12 C13 1.384(4) . ? C13 C14 1.333(4) . ? C13 C16 1.522(4) . ? C14 C15 1.389(4) . ? C17 C18 1.337(4) . ? C17 O1 1.422(3) . ? C19 C20 1.399(4) . ? C19 O1 1.448(4) . ? 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 N1 Li1 O1 127.9(3) . . ? N1 Li1 N3 115.1(2) . . ? O1 Li1 N3 116.6(2) . . ? N1 Li1 Li2 54.43(18) . . ? O1 Li1 Li2 168.6(3) . . ? N3 Li1 Li2 63.91(19) . . ? N1 Li1 C1 109.5(2) . . ? O1 Li1 C1 119.1(2) . . ? N3 Li1 C1 27.09(10) . . ? Li2 Li1 C1 55.57(16) . . ? N1 Li1 Si2 32.01(10) . . ? O1 Li1 Si2 106.76(19) . . ? N3 Li1 Si2 132.5(2) . . ? Li2 Li1 Si2 69.73(18) . . ? C1 Li1 Si2 112.96(18) . . ? N1 Li1 Si1 29.14(9) . . ? O1 Li1 Si1 121.7(2) . . ? N3 Li1 Si1 109.21(18) . . ? Li2 Li1 Si1 66.35(16) . . ? C1 Li1 Si1 118.24(16) . . ? Si2 Li1 Si1 57.95(9) . . ? N2 Li2 N4 108.3(3) . . ? N2 Li2 N1 122.6(3) . . ? N4 Li2 N1 126.3(3) . . ? N2 Li2 N3 63.13(16) . . ? N4 Li2 N3 121.1(3) . . ? N1 Li2 N3 97.7(2) . . ? N2 Li2 Li1 84.1(2) . . ? N4 Li2 Li1 159.7(3) . . ? N1 Li2 Li1 50.55(17) . . ? N3 Li2 Li1 49.47(16) . . ? N2 Li2 C1 32.18(11) . . ? N4 Li2 C1 112.8(3) . . ? N1 Li2 C1 119.1(2) . . ? N3 Li2 C1 32.16(10) . . ? Li1 Li2 C1 69.14(18) . . ? N2 Li2 Si1 150.4(3) . . ? N4 Li2 Si1 101.32(19) . . ? N1 Li2 Si1 30.93(9) . . ? N3 Li2 Si1 100.3(2) . . ? Li1 Li2 Si1 67.18(17) . . ? C1 Li2 Si1 131.3(2) . . ? N2 Li2 Si2 104.8(2) . . ? N4 Li2 Si2 125.6(2) . . ? N1 Li2 Si2 29.57(10) . . ? N3 Li2 Si2 112.06(19) . . ? Li1 Li2 Si2 63.34(17) . . ? C1 Li2 Si2 118.20(19) . . ? Si1 Li2 Si2 56.67(10) . . ? N1 Si1 C3S1 112.34(11) . . ? N1 Si1 C2S1 112.49(11) . . ? C3S1 Si1 C2S1 105.01(13) . . ? N1 Si1 C1S1 114.95(11) . . ? C3S1 Si1 C1S1 104.04(12) . . ? C2S1 Si1 C1S1 107.18(12) . . ? N1 Si1 Li2 38.65(12) . . ? C3S1 Si1 Li2 75.53(13) . . ? C2S1 Si1 Li2 136.17(13) . . ? C1S1 Si1 Li2 115.25(14) . . ? N1 Si1 Li1 34.18(11) . . ? C3S1 Si1 Li1 95.05(12) . . ? C2S1 Si1 Li1 90.68(13) . . ? C1S1 Si1 Li1 149.06(13) . . ? Li2 Si1 Li1 46.47(13) . . ? N1 Si2 C3S2 113.76(12) . . ? N1 Si2 C2S2 109.91(12) . . ? C3S2 Si2 C2S2 106.41(13) . . ? N1 Si2 C1S2 115.18(12) . . ? C3S2 Si2 C1S2 105.25(13) . . ? C2S2 Si2 C1S2 105.65(13) . . ? N1 Si2 Li1 37.84(11) . . ? C3S2 Si2 Li1 138.10(14) . . ? C2S2 Si2 Li1 74.19(13) . . ? C1S2 Si2 Li1 115.01(13) . . ? N1 Si2 Li2 36.98(12) . . ? C3S2 Si2 Li2 91.48(14) . . ? C2S2 Si2 Li2 90.24(13) . . ? C1S2 Si2 Li2 152.16(14) . . ? Li1 Si2 Li2 46.93(14) . . ? N2 Si3 C3S3 112.34(13) . . ? N2 Si3 C1S3 105.68(13) . . ? C3S3 Si3 C1S3 108.60(15) . . ? N2 Si3 C2S3 114.79(13) . . ? C3S3 Si3 C2S3 109.40(16) . . ? C1S3 Si3 C2S3 105.58(14) . . ? N3 Si4 C2S4 117.52(12) . . ? N3 Si4 C3S4 106.07(12) . . ? C2S4 Si4 C3S4 104.74(12) . . ? N3 Si4 C1S4 111.79(12) . . ? C2S4 Si4 C1S4 107.49(14) . . ? C3S4 Si4 C1S4 108.73(13) . . ? Si2 N1 Si1 121.85(12) . . ? Si2 N1 Li1 110.15(17) . . ? Si1 N1 Li1 116.67(18) . . ? Si2 N1 Li2 113.45(19) . . ? Si1 N1 Li2 110.42(17) . . ? Li1 N1 Li2 75.0(2) . . ? C1 N2 Si3 130.48(19) . . ? C1 N2 Li2 93.4(2) . . ? Si3 N2 Li2 130.3(2) . . ? C1 N3 Si4 129.95(18) . . ? C1 N3 Li1 109.6(2) . . ? Si4 N3 Li1 117.21(18) . . ? C1 N3 Li2 76.42(18) . . ? Si4 N3 Li2 138.05(16) . . ? Li1 N3 Li2 66.6(2) . . ? C9 N4 Li2 165.4(3) . . ? N2 C1 N3 122.3(2) . . ? N2 C1 C2 120.0(2) . . ? N3 C1 C2 117.7(2) . . ? N2 C1 Li2 54.42(18) . . ? N3 C1 Li2 71.42(19) . . ? C2 C1 Li2 158.3(2) . . ? N2 C1 Li1 86.28(19) . . ? N3 C1 Li1 43.34(16) . . ? C2 C1 Li1 145.27(19) . . ? Li2 C1 Li1 55.29(17) . . ? C3 C2 C7 115.9(2) . . ? C3 C2 C1 119.0(2) . . ? C7 C2 C1 125.1(2) . . ? C4 C3 C2 123.0(2) . . ? C3 C4 C5 120.3(2) . . ? C6 C5 C4 117.2(2) . . ? C6 C5 C8 120.9(2) . . ? C4 C5 C8 121.9(2) . . ? C5 C6 C7 122.9(2) . . ? C6 C7 C2 120.7(2) . . ? N4 C9 C10 176.0(3) . . ? C11 C10 C15 118.7(3) . . ? C11 C10 C9 118.9(3) . . ? C15 C10 C9 122.4(2) . . ? C10 C11 C12 122.9(3) . . ? C13 C12 C11 117.4(3) . . ? C14 C13 C12 120.2(3) . . ? C14 C13 C16 116.7(3) . . ? C12 C13 C16 123.0(3) . . ? C13 C14 C15 122.2(3) . . ? C10 C15 C14 118.5(3) . . ? C18 C17 O1 116.7(3) . . ? C20 C19 O1 115.9(3) . . ? C17 O1 C19 113.0(3) . . ? C17 O1 Li1 122.7(3) . . ? C19 O1 Li1 123.6(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.085 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.052 data_complex2 _database_code_CSD 156014 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Complex-2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H82 Li3 N7 Si6' _chemical_formula_weight 970.59 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' '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' 'N' 'N' 0.0061 0.0033 '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 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 13.506(2) _cell_length_b 14.668(4) _cell_length_c 30.918(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6125(3) _cell_formula_units_Z 4 _cell_measurement_temperature 220(1) _cell_measurement_reflns_used 2833 _cell_measurement_theta_min 1.01 _cell_measurement_theta_max 25.35 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.053 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9730 _exptl_absorpt_correction_T_max 0.9949 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27733 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.1516 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5668 _reflns_number_gt 2679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD (Nonius,2000)' _computing_cell_refinement 'DENZO SMN (Otwinowski & Minor, 1997' _computing_data_reduction 'DENZO SMN (Otwinowski & Minor, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Texsan (MSC,2000)' _computing_publication_material ? _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^)+(0.0350P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00147(17) _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 0.00 _refine_ls_number_reflns 5668 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.004 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 0.09291(9) 0.39546(9) 0.63783(5) 0.0458(4) Uani 1 1 d . . . Si2 Si 0.34139(10) 0.69390(9) 0.64519(5) 0.0482(4) Uani 1 1 d . . . Si3 Si 0.65584(10) 0.49571(10) 0.59791(5) 0.0523(4) Uani 1 1 d . . . Si4 Si 0.41691(10) 0.40212(10) 0.73336(5) 0.0513(4) Uani 1 1 d . . . Si5 Si 0.35474(10) 0.67146(10) 0.48704(5) 0.0544(5) Uani 1 1 d . . . Si6 Si 0.38427(10) 0.31458(9) 0.54446(5) 0.0491(4) Uani 1 1 d . . . N1 N 0.1373(3) 0.5382(3) 0.52591(14) 0.0535(12) Uani 1 1 d . . . N2 N 0.1945(2) 0.4642(3) 0.62901(12) 0.0340(10) Uani 1 1 d . . . N3 N 0.2976(3) 0.5896(2) 0.62644(12) 0.0350(10) Uani 1 1 d . . . N4 N 0.4464(3) 0.4430(2) 0.68329(12) 0.0400(11) Uani 1 1 d . . . N5 N 0.5454(2) 0.4931(2) 0.62459(14) 0.0402(11) Uani 1 1 d . . . N6 N 0.3696(2) 0.4319(2) 0.54580(12) 0.0359(10) Uani 1 1 d . . . N7 N 0.3696(2) 0.5788(2) 0.52074(12) 0.0378(10) Uani 1 1 d . . . C1 C 0.0770(4) 0.5285(4) 0.49998(19) 0.0517(16) Uani 1 1 d . . . C2 C 0.0024(4) 0.5139(3) 0.46792(18) 0.0456(14) Uani 1 1 d . . . C3 C 0.0313(4) 0.5012(4) 0.4248(2) 0.0681(17) Uani 1 1 d . . . H3 H 0.0973 0.5059 0.4165 0.102 Uiso 1 1 calc . . . C4 C -0.0418(5) 0.4815(4) 0.39503(19) 0.0758(19) Uani 1 1 d . . . H4 H -0.0235 0.4706 0.3665 0.114 Uiso 1 1 calc . . . C5 C -0.1385(5) 0.4772(3) 0.4056(2) 0.0625(17) Uani 1 1 d . . . C6 C -0.1645(4) 0.4934(4) 0.4481(3) 0.0756(19) Uani 1 1 d . . . H6 H -0.2310 0.4921 0.4558 0.113 Uiso 1 1 calc . . . C7 C -0.0943(4) 0.5115(4) 0.47920(19) 0.0682(17) Uani 1 1 d . . . H7 H -0.1132 0.5220 0.5077 0.102 Uiso 1 1 calc . . . C8 C -0.2178(4) 0.4550(3) 0.3723(2) 0.099(2) Uani 1 1 d . . . H8A H -0.2791 0.4830 0.3807 0.149 Uiso 1 1 calc R . . H8B H -0.2264 0.3901 0.3708 0.149 Uiso 1 1 calc R . . H8C H -0.1978 0.4777 0.3446 0.149 Uiso 1 1 calc R . . C9 C 0.2096(4) 0.5521(3) 0.63742(15) 0.0352(12) Uani 1 1 d . . . C10 C 0.1274(3) 0.6097(3) 0.65578(16) 0.0368(13) Uani 1 1 d . . . C11 C 0.1166(3) 0.6282(3) 0.69912(17) 0.0505(15) Uani 1 1 d . . . H11 H 0.1618 0.6038 0.7186 0.076 Uiso 1 1 calc . . . C12 C 0.0407(4) 0.6819(4) 0.71435(16) 0.0568(15) Uani 1 1 d . . . H12 H 0.0352 0.6927 0.7439 0.085 Uiso 1 1 calc . . . C13 C -0.0268(4) 0.7198(3) 0.68666(19) 0.0511(15) Uani 1 1 d . . . C14 C -0.0158(3) 0.7020(3) 0.64269(17) 0.0497(14) Uani 1 1 d . . . H14 H -0.0603 0.7275 0.6232 0.075 Uiso 1 1 calc . . . C15 C 0.0588(4) 0.6480(3) 0.62758(16) 0.0472(14) Uani 1 1 d . . . H15 H 0.0638 0.6366 0.5981 0.071 Uiso 1 1 calc . . . C16 C -0.1118(3) 0.7783(4) 0.70188(18) 0.0798(19) Uani 1 1 d . . . H16A H -0.1067 0.8377 0.6890 0.120 Uiso 1 1 calc R . . H16B H -0.1093 0.7840 0.7328 0.120 Uiso 1 1 calc R . . H16C H -0.1733 0.7506 0.6936 0.120 Uiso 1 1 calc R . . C17 C 0.5336(4) 0.4663(3) 0.66686(18) 0.0389(13) Uani 1 1 d . . . C18 C 0.6241(3) 0.4659(4) 0.69530(16) 0.0388(13) Uani 1 1 d . . . C19 C 0.6748(4) 0.3869(3) 0.70563(17) 0.0496(14) Uani 1 1 d . . . H19 H 0.6541 0.3318 0.6938 0.074 Uiso 1 1 calc . . . C20 C 0.7563(4) 0.3878(4) 0.73332(18) 0.0500(14) Uani 1 1 d . . . H20 H 0.7890 0.3336 0.7396 0.075 Uiso 1 1 calc . . . C21 C 0.7887(4) 0.4680(5) 0.75146(17) 0.0524(15) Uani 1 1 d . . . C22 C 0.7371(4) 0.5476(4) 0.74226(19) 0.0576(16) Uani 1 1 d . . . H22 H 0.7564 0.6022 0.7550 0.086 Uiso 1 1 calc . . . C23 C 0.6569(4) 0.5462(4) 0.71422(18) 0.0523(15) Uani 1 1 d . . . H23 H 0.6244 0.6005 0.7079 0.078 Uiso 1 1 calc . . . C24 C 0.8771(3) 0.4710(4) 0.78152(17) 0.0761(19) Uani 1 1 d . . . H24A H 0.8946 0.4101 0.7900 0.114 Uiso 1 1 calc R . . H24B H 0.8608 0.5060 0.8068 0.114 Uiso 1 1 calc R . . H24C H 0.9321 0.4989 0.7669 0.114 Uiso 1 1 calc R . . C25 C 0.3734(3) 0.4893(4) 0.51242(16) 0.0362(12) Uani 1 1 d . . . C26 C 0.3764(4) 0.4562(3) 0.46602(16) 0.0425(13) Uani 1 1 d . . . C27 C 0.4583(4) 0.4729(4) 0.4395(2) 0.0669(17) Uani 1 1 d . . . H27 H 0.5131 0.5037 0.4504 0.080 Uiso 1 1 calc . . . C28 C 0.4573(5) 0.4429(5) 0.3964(2) 0.088(2) Uani 1 1 d . . . H28 H 0.5125 0.4533 0.3790 0.132 Uiso 1 1 calc . . . C29 C 0.3778(5) 0.3989(5) 0.3794(2) 0.082(2) Uani 1 1 d . . . C30 C 0.2984(4) 0.3828(4) 0.4052(2) 0.0679(18) Uani 1 1 d . . . H30 H 0.2438 0.3524 0.3939 0.102 Uiso 1 1 calc . . . C31 C 0.2969(4) 0.4108(4) 0.44841(18) 0.0550(15) Uani 1 1 d . . . H31 H 0.2416 0.3987 0.4654 0.083 Uiso 1 1 calc . . . C32 C 0.3779(5) 0.3672(5) 0.33230(18) 0.122(3) Uani 1 1 d . . . H32A H 0.3123 0.3728 0.3206 0.183 Uiso 1 1 calc R . . H32B H 0.3986 0.3046 0.3309 0.183 Uiso 1 1 calc R . . H32C H 0.4227 0.4042 0.3158 0.183 Uiso 1 1 calc R . . C33 C 0.4565(3) 0.7192(3) 0.61502(19) 0.0658(18) Uani 1 1 d . . . H33A H 0.4423 0.7218 0.5846 0.099 Uiso 1 1 calc R . . H33B H 0.5043 0.6722 0.6204 0.099 Uiso 1 1 calc R . . H33C H 0.4826 0.7768 0.6243 0.099 Uiso 1 1 calc R . . C34 C 0.3765(3) 0.6849(3) 0.70357(16) 0.0706(17) Uani 1 1 d . . . H34A H 0.4213 0.6348 0.7074 0.106 Uiso 1 1 d R . . H34B H 0.3180 0.6747 0.7206 0.106 Uiso 1 1 d R . . H34C H 0.4079 0.7403 0.7128 0.106 Uiso 1 1 d R . . C35 C 0.2579(3) 0.7943(3) 0.63876(18) 0.0646(16) Uani 1 1 d . . . H35A H 0.2391 0.8002 0.6089 0.097 Uiso 1 1 calc R . . H35B H 0.2919 0.8485 0.6479 0.097 Uiso 1 1 calc R . . H35C H 0.1997 0.7859 0.6561 0.097 Uiso 1 1 calc R . . C36 C 0.1418(4) 0.2797(3) 0.64763(19) 0.083(2) Uani 1 1 d . . . H36A H 0.1778 0.2789 0.6744 0.125 Uiso 1 1 calc R . . H36B H 0.1852 0.2627 0.6244 0.125 Uiso 1 1 calc R . . H36C H 0.0878 0.2372 0.6492 0.125 Uiso 1 1 calc R . . C37 C 0.0101(3) 0.3912(4) 0.59019(16) 0.0743(18) Uani 1 1 d . . . H37A H -0.0183 0.4503 0.5854 0.111 Uiso 1 1 calc R . . H37B H -0.0417 0.3477 0.5953 0.111 Uiso 1 1 calc R . . H37C H 0.0475 0.3732 0.5652 0.111 Uiso 1 1 calc R . . C38 C 0.0134(3) 0.4232(4) 0.68493(17) 0.0717(18) Uani 1 1 d . . . H38A H -0.0313 0.3736 0.6903 0.108 Uiso 1 1 calc R . . H38B H -0.0238 0.4775 0.6789 0.108 Uiso 1 1 calc R . . H38C H 0.0542 0.4328 0.7100 0.108 Uiso 1 1 calc R . . C39 C 0.7151(4) 0.3817(4) 0.59335(19) 0.082(2) Uani 1 1 d . . . H39A H 0.7329 0.3603 0.6216 0.123 Uiso 1 1 calc R . . H39B H 0.7734 0.3863 0.5758 0.123 Uiso 1 1 calc R . . H39C H 0.6695 0.3397 0.5803 0.123 Uiso 1 1 calc R . . C40 C 0.7523(3) 0.5767(4) 0.61713(18) 0.0756(19) Uani 1 1 d . . . H40A H 0.7774 0.5566 0.6446 0.113 Uiso 1 1 calc R . . H40B H 0.7239 0.6363 0.6202 0.113 Uiso 1 1 calc R . . H40C H 0.8054 0.5790 0.5965 0.113 Uiso 1 1 calc R . . C41 C 0.6255(3) 0.5322(4) 0.54154(16) 0.0707(17) Uani 1 1 d . . . H41A H 0.5772 0.4914 0.5295 0.106 Uiso 1 1 calc R . . H41B H 0.6844 0.5308 0.5242 0.106 Uiso 1 1 calc R . . H41C H 0.5992 0.5930 0.5420 0.106 Uiso 1 1 calc R . . C42 C 0.4918(3) 0.4373(3) 0.78048(15) 0.0653(16) Uani 1 1 d . . . H42A H 0.4616 0.4151 0.8065 0.098 Uiso 1 1 calc R . . H42B H 0.4954 0.5027 0.7815 0.098 Uiso 1 1 calc R . . H42C H 0.5574 0.4126 0.7779 0.098 Uiso 1 1 calc R . . C43 C 0.4093(4) 0.2750(3) 0.73053(19) 0.084(2) Uani 1 1 d . . . H43A H 0.3632 0.2577 0.7084 0.126 Uiso 1 1 calc R . . H43B H 0.3874 0.2516 0.7579 0.126 Uiso 1 1 calc R . . H43C H 0.4735 0.2506 0.7239 0.126 Uiso 1 1 calc R . . C44 C 0.2907(3) 0.4460(4) 0.74591(18) 0.0768(19) Uani 1 1 d . . . H44A H 0.2467 0.4317 0.7225 0.115 Uiso 1 1 calc R . . H44B H 0.2934 0.5109 0.7497 0.115 Uiso 1 1 calc R . . H44C H 0.2669 0.4180 0.7720 0.115 Uiso 1 1 calc R . . C45 C 0.2906(3) 0.6500(4) 0.43419(18) 0.0775(19) Uani 1 1 d . . . H45A H 0.3328 0.6143 0.4158 0.116 Uiso 1 1 calc R . . H45B H 0.2762 0.7071 0.4204 0.116 Uiso 1 1 calc R . . H45C H 0.2300 0.6175 0.4393 0.116 Uiso 1 1 calc R . . C46 C 0.4753(4) 0.7271(3) 0.47647(18) 0.0752(19) Uani 1 1 d . . . H46A H 0.5151 0.6883 0.4585 0.113 Uiso 1 1 calc R . . H46B H 0.5089 0.7376 0.5034 0.113 Uiso 1 1 calc R . . H46C H 0.4645 0.7842 0.4621 0.113 Uiso 1 1 calc R . . C47 C 0.2759(4) 0.7546(4) 0.51672(19) 0.0802(19) Uani 1 1 d . . . H47A H 0.2180 0.7241 0.5275 0.120 Uiso 1 1 calc R . . H47B H 0.2563 0.8027 0.4975 0.120 Uiso 1 1 calc R . . H47C H 0.3126 0.7798 0.5405 0.120 Uiso 1 1 calc R . . C48 C 0.4165(3) 0.2806(3) 0.60033(17) 0.0617(16) Uani 1 1 d . . . H48A H 0.4739 0.3138 0.6096 0.093 Uiso 1 1 calc R . . H48B H 0.4303 0.2164 0.6011 0.093 Uiso 1 1 calc R . . H48C H 0.3619 0.2939 0.6192 0.093 Uiso 1 1 calc R . . C49 C 0.4859(4) 0.2728(4) 0.50860(18) 0.0791(19) Uani 1 1 d . . . H49A H 0.5460 0.3047 0.5153 0.119 Uiso 1 1 calc R . . H49B H 0.4684 0.2834 0.4789 0.119 Uiso 1 1 calc R . . H49C H 0.4954 0.2086 0.5132 0.119 Uiso 1 1 calc R . . C50 C 0.2679(4) 0.2539(3) 0.52952(18) 0.0732(18) Uani 1 1 d . . . H50A H 0.2125 0.2835 0.5430 0.110 Uiso 1 1 calc R . . H50B H 0.2715 0.1918 0.5392 0.110 Uiso 1 1 calc R . . H50C H 0.2597 0.2552 0.4987 0.110 Uiso 1 1 calc R . . Li1 Li 0.2569(5) 0.5225(5) 0.5659(3) 0.049(2) Uiso 1 1 d . . . Li2 Li 0.4406(5) 0.5419(6) 0.5814(3) 0.052(2) Uiso 1 1 d . . . Li3 Li 0.3454(6) 0.4543(5) 0.6385(3) 0.054(2) 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 Si1 0.0394(9) 0.0480(9) 0.0500(11) -0.0018(8) 0.0057(8) -0.0046(8) Si2 0.0527(9) 0.0359(9) 0.0559(11) -0.0061(8) -0.0020(9) -0.0029(8) Si3 0.0382(9) 0.0639(10) 0.0548(11) 0.0037(9) -0.0037(8) -0.0017(9) Si4 0.0469(9) 0.0554(10) 0.0517(11) 0.0136(9) -0.0078(8) -0.0042(8) Si5 0.0557(10) 0.0548(10) 0.0527(11) 0.0166(9) -0.0035(9) -0.0076(9) Si6 0.0552(10) 0.0399(9) 0.0522(11) -0.0097(8) 0.0001(8) 0.0013(8) N1 0.044(3) 0.066(3) 0.050(3) 0.004(3) 0.000(2) -0.002(3) N2 0.032(2) 0.030(2) 0.039(3) -0.002(2) 0.0031(19) -0.001(2) N3 0.035(2) 0.031(2) 0.039(3) 0.001(2) 0.000(2) -0.007(2) N4 0.027(2) 0.052(3) 0.042(3) 0.007(2) -0.005(2) -0.007(2) N5 0.031(2) 0.041(3) 0.048(3) 0.004(2) -0.008(2) -0.002(2) N6 0.041(2) 0.034(2) 0.032(3) 0.004(2) 0.000(2) -0.0021(19) N7 0.045(3) 0.031(2) 0.037(3) 0.006(2) 0.001(2) -0.001(2) C1 0.034(4) 0.067(4) 0.054(4) 0.004(3) -0.002(3) 0.005(3) C2 0.038(4) 0.050(4) 0.049(4) 0.003(3) -0.018(3) -0.006(3) C3 0.076(4) 0.082(5) 0.047(4) -0.002(4) 0.000(4) -0.032(4) C4 0.100(5) 0.078(5) 0.049(4) 0.008(4) -0.029(4) -0.029(4) C5 0.076(5) 0.038(4) 0.073(5) 0.005(4) -0.039(4) -0.009(4) C6 0.053(4) 0.073(4) 0.100(6) -0.019(4) -0.018(4) -0.001(3) C7 0.052(4) 0.081(4) 0.071(5) -0.019(4) -0.020(4) -0.001(4) C8 0.133(5) 0.053(4) 0.111(6) 0.009(4) -0.082(5) -0.024(4) C9 0.044(3) 0.036(3) 0.025(3) 0.002(3) -0.004(3) 0.001(3) C10 0.037(3) 0.036(3) 0.038(3) -0.005(3) 0.005(3) 0.006(3) C11 0.057(4) 0.058(4) 0.036(4) -0.004(3) 0.000(3) 0.021(3) C12 0.071(4) 0.063(4) 0.036(4) -0.006(3) -0.002(3) 0.029(4) C13 0.042(3) 0.055(4) 0.056(4) -0.017(3) 0.011(3) 0.016(3) C14 0.046(3) 0.062(4) 0.041(4) -0.008(3) -0.007(3) 0.024(3) C15 0.053(4) 0.050(3) 0.039(4) -0.003(3) 0.000(3) 0.016(3) C16 0.072(4) 0.089(5) 0.078(5) -0.026(4) 0.008(4) 0.026(4) C17 0.038(3) 0.024(3) 0.055(4) 0.001(3) -0.014(3) 0.005(3) C18 0.030(3) 0.046(3) 0.040(3) 0.006(3) -0.005(3) -0.004(3) C19 0.044(3) 0.050(4) 0.054(4) 0.003(3) -0.008(3) 0.005(3) C20 0.034(3) 0.064(4) 0.052(4) 0.017(3) -0.002(3) 0.009(3) C21 0.028(3) 0.087(5) 0.043(4) -0.004(4) -0.001(3) -0.003(4) C22 0.044(4) 0.063(4) 0.066(5) -0.012(3) -0.005(3) -0.012(3) C23 0.047(3) 0.052(4) 0.058(4) 0.001(3) -0.012(3) -0.006(3) C24 0.041(3) 0.136(5) 0.051(4) 0.005(4) -0.010(3) -0.007(3) C25 0.025(3) 0.043(4) 0.040(3) -0.009(3) 0.002(3) -0.007(3) C26 0.038(3) 0.052(3) 0.038(3) -0.007(3) 0.001(3) 0.002(3) C27 0.044(3) 0.103(5) 0.054(4) -0.011(4) 0.012(3) -0.004(3) C28 0.079(5) 0.149(7) 0.035(4) -0.005(4) 0.024(4) 0.029(5) C29 0.074(5) 0.127(6) 0.044(4) -0.027(4) 0.000(4) 0.024(5) C30 0.076(4) 0.075(4) 0.053(4) -0.026(4) -0.016(4) 0.012(4) C31 0.061(4) 0.061(4) 0.043(4) -0.004(3) 0.005(3) -0.004(3) C32 0.133(6) 0.190(7) 0.043(4) -0.051(5) -0.009(4) 0.033(5) C33 0.059(3) 0.049(3) 0.090(5) -0.011(3) -0.008(3) -0.004(3) C34 0.080(4) 0.060(4) 0.072(4) -0.014(3) -0.024(3) -0.006(3) C35 0.079(4) 0.043(3) 0.072(5) -0.001(3) 0.010(4) 0.010(3) C36 0.075(4) 0.060(4) 0.115(6) 0.019(4) 0.015(4) -0.011(3) C37 0.058(3) 0.098(5) 0.067(5) 0.003(4) -0.007(3) -0.033(3) C38 0.056(4) 0.087(4) 0.072(5) -0.001(4) 0.018(3) -0.011(3) C39 0.067(4) 0.104(5) 0.076(5) -0.006(4) 0.001(3) 0.024(4) C40 0.056(3) 0.102(5) 0.069(5) 0.001(4) 0.010(3) -0.013(3) C41 0.051(3) 0.103(4) 0.058(4) 0.024(4) 0.003(3) -0.008(3) C42 0.069(4) 0.082(4) 0.045(4) 0.006(3) 0.000(3) -0.011(3) C43 0.099(4) 0.078(4) 0.076(5) 0.038(4) -0.030(4) -0.020(4) C44 0.055(4) 0.099(5) 0.077(5) 0.033(4) 0.010(3) -0.003(3) C45 0.083(4) 0.081(4) 0.068(5) 0.030(4) -0.019(4) -0.017(3) C46 0.083(4) 0.073(4) 0.070(5) 0.035(4) -0.007(4) -0.020(3) C47 0.096(4) 0.061(4) 0.085(5) 0.019(4) -0.002(4) 0.011(3) C48 0.080(4) 0.037(3) 0.068(4) 0.005(3) -0.013(3) 0.005(3) C49 0.095(4) 0.072(4) 0.070(5) -0.020(4) 0.012(4) 0.020(3) C50 0.095(4) 0.051(4) 0.073(5) -0.008(3) -0.017(4) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N2 1.724(4) . ? Si1 C36 1.847(5) . ? Si1 C37 1.850(5) . ? Si1 C38 1.854(5) . ? Si2 N3 1.740(4) . ? Si2 C33 1.851(5) . ? Si2 C35 1.865(4) . ? Si2 C34 1.871(5) . ? Si3 N5 1.705(4) . ? Si3 C40 1.861(5) . ? Si3 C39 1.859(5) . ? Si3 C41 1.869(5) . ? Si3 Li2 3.028(8) . ? Si4 N4 1.707(4) . ? Si4 C42 1.847(5) . ? Si4 C44 1.863(5) . ? Si4 C43 1.869(5) . ? Si4 Li3 3.180(9) . ? Si5 N7 1.725(4) . ? Si5 C46 1.850(5) . ? Si5 C47 1.861(5) . ? Si5 C45 1.876(5) . ? Si6 N6 1.733(4) . ? Si6 C48 1.850(5) . ? Si6 C50 1.864(5) . ? Si6 C49 1.867(5) . ? N1 C1 1.152(6) . ? N1 Li1 2.047(9) . ? N2 C9 1.331(5) . ? N2 Li3 2.065(8) . ? N2 Li1 2.291(9) . ? N3 C9 1.352(5) . ? N3 Li3 2.120(9) . ? N3 Li1 2.185(9) . ? N3 Li2 2.481(9) . ? N4 C17 1.327(5) . ? N4 Li3 1.950(9) . ? N5 C17 1.374(6) . ? N5 Li2 2.072(9) . ? N6 C25 1.332(5) . ? N6 Li1 2.114(8) . ? N6 Li2 2.177(9) . ? N7 C25 1.339(5) . ? N7 Li2 2.176(9) . ? N7 Li1 2.224(9) . ? C1 C2 1.430(7) . ? C2 C7 1.352(6) . ? C2 C3 1.402(7) . ? C3 C4 1.380(7) . ? C3 H3 0.9300 . ? C4 C5 1.349(7) . ? C4 H4 0.9300 . ? C5 C6 1.379(8) . ? C5 C8 1.520(7) . ? C6 C7 1.377(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.506(6) . ? C9 Li3 2.329(9) . ? C9 Li1 2.343(10) . ? C10 C11 1.375(6) . ? C10 C15 1.391(6) . ? C11 C12 1.376(6) . ? C11 H11 0.9300 . ? C12 C13 1.368(6) . ? C12 H12 0.9300 . ? C13 C14 1.392(7) . ? C13 C16 1.509(6) . ? C14 C15 1.364(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.505(6) . ? C17 Li3 2.694(9) . ? C18 C19 1.383(6) . ? C18 C23 1.389(6) . ? C19 C20 1.394(6) . ? C19 H19 0.9300 . ? C20 C21 1.375(7) . ? C20 H20 0.9300 . ? C21 C22 1.389(7) . ? C21 C24 1.514(6) . ? C22 C23 1.387(7) . ? C22 H22 0.9300 . ? C23 H23 0.9299 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.515(6) . ? C25 Li1 2.333(9) . ? C25 Li2 2.445(10) . ? C26 C31 1.375(6) . ? C26 C27 1.399(6) . ? C27 C28 1.404(8) . ? C27 H27 0.9300 . ? C28 C29 1.359(8) . ? C28 H28 0.9300 . ? C29 C30 1.357(7) . ? C29 C32 1.529(7) . ? C30 C31 1.397(7) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9591 . ? C34 H34B 0.9607 . ? C34 H34C 0.9597 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 Li2 2.788(9) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? Li1 Li2 2.544(10) . ? Li1 Li3 2.734(12) . ? Li2 Li3 2.534(12) . ? 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 N2 Si1 C36 106.2(2) . . ? N2 Si1 C37 112.0(2) . . ? C36 Si1 C37 108.4(3) . . ? N2 Si1 C38 117.2(2) . . ? C36 Si1 C38 106.3(3) . . ? C37 Si1 C38 106.4(2) . . ? N3 Si2 C33 107.1(2) . . ? N3 Si2 C35 117.0(2) . . ? C33 Si2 C35 107.2(2) . . ? N3 Si2 C34 110.2(2) . . ? C33 Si2 C34 106.7(2) . . ? C35 Si2 C34 108.2(2) . . ? N5 Si3 C40 118.2(2) . . ? N5 Si3 C39 113.2(2) . . ? C40 Si3 C39 107.3(2) . . ? N5 Si3 C41 105.4(2) . . ? C40 Si3 C41 105.6(2) . . ? C39 Si3 C41 106.3(3) . . ? N5 Si3 Li2 41.1(2) . . ? C40 Si3 Li2 125.7(2) . . ? C39 Si3 Li2 127.0(2) . . ? C41 Si3 Li2 64.4(2) . . ? N4 Si4 C42 119.3(2) . . ? N4 Si4 C44 106.3(2) . . ? C42 Si4 C44 103.9(2) . . ? N4 Si4 C43 108.7(2) . . ? C42 Si4 C43 110.2(2) . . ? C44 Si4 C43 107.7(3) . . ? N4 Si4 Li3 31.83(19) . . ? C42 Si4 Li3 145.7(2) . . ? C44 Si4 Li3 80.3(2) . . ? C43 Si4 Li3 100.4(2) . . ? N7 Si5 C46 110.6(2) . . ? N7 Si5 C47 106.6(2) . . ? C46 Si5 C47 107.6(3) . . ? N7 Si5 C45 116.6(2) . . ? C46 Si5 C45 109.1(2) . . ? C47 Si5 C45 106.0(3) . . ? N6 Si6 C48 105.8(2) . . ? N6 Si6 C50 112.6(2) . . ? C48 Si6 C50 107.5(2) . . ? N6 Si6 C49 115.1(2) . . ? C48 Si6 C49 107.0(2) . . ? C50 Si6 C49 108.4(2) . . ? C1 N1 Li1 164.7(5) . . ? C9 N2 Si1 131.2(3) . . ? C9 N2 Li3 83.6(3) . . ? Si1 N2 Li3 136.2(3) . . ? C9 N2 Li1 75.4(3) . . ? Si1 N2 Li1 130.2(3) . . ? Li3 N2 Li1 77.5(3) . . ? C9 N3 Si2 124.9(3) . . ? C9 N3 Li3 81.0(3) . . ? Si2 N3 Li3 131.3(3) . . ? C9 N3 Li1 79.1(3) . . ? Si2 N3 Li1 140.1(3) . . ? Li3 N3 Li1 78.9(3) . . ? C9 N3 Li2 135.3(3) . . ? Si2 N3 Li2 99.8(3) . . ? Li3 N3 Li2 66.3(3) . . ? Li1 N3 Li2 65.7(3) . . ? C17 N4 Si4 130.1(3) . . ? C17 N4 Li3 109.1(4) . . ? Si4 N4 Li3 120.7(3) . . ? C17 N5 Si3 124.6(3) . . ? C17 N5 Li2 129.3(4) . . ? Si3 N5 Li2 106.1(3) . . ? C25 N6 Si6 127.2(3) . . ? C25 N6 Li1 81.8(3) . . ? Si6 N6 Li1 135.5(3) . . ? C25 N6 Li2 84.7(4) . . ? Si6 N6 Li2 134.3(3) . . ? Li1 N6 Li2 72.7(3) . . ? C25 N7 Si5 131.4(4) . . ? C25 N7 Li2 84.6(3) . . ? Si5 N7 Li2 140.2(3) . . ? C25 N7 Li1 77.4(3) . . ? Si5 N7 Li1 126.3(3) . . ? Li2 N7 Li1 70.6(3) . . ? N1 C1 C2 178.5(6) . . ? C7 C2 C3 120.8(5) . . ? C7 C2 C1 120.4(5) . . ? C3 C2 C1 118.9(5) . . ? C4 C3 C2 117.6(5) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C5 C4 C3 122.7(6) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C4 C5 C6 118.0(6) . . ? C4 C5 C8 121.9(7) . . ? C6 C5 C8 120.2(6) . . ? C7 C6 C5 121.6(6) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C2 C7 C6 119.3(6) . . ? C2 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 N3 118.6(4) . . ? N2 C9 C10 120.2(4) . . ? N3 C9 C10 121.0(4) . . ? N2 C9 Li3 61.8(3) . . ? N3 C9 Li3 64.0(3) . . ? C10 C9 Li3 157.0(4) . . ? N2 C9 Li1 71.2(3) . . ? N3 C9 Li1 66.3(3) . . ? C10 C9 Li1 131.4(4) . . ? Li3 C9 Li1 71.6(3) . . ? C11 C10 C15 117.4(4) . . ? C11 C10 C9 123.8(4) . . ? C15 C10 C9 118.8(4) . . ? C10 C11 C12 121.7(4) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 121.0(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 117.6(4) . . ? C12 C13 C16 122.8(5) . . ? C14 C13 C16 119.5(5) . . ? C15 C14 C13 121.5(5) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C10 120.8(5) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 N5 122.7(4) . . ? N4 C17 C18 119.7(5) . . ? N5 C17 C18 117.6(4) . . ? N4 C17 Li3 43.2(3) . . ? N5 C17 Li3 79.5(3) . . ? C18 C17 Li3 162.8(4) . . ? C19 C18 C23 117.1(4) . . ? C19 C18 C17 122.7(5) . . ? C23 C18 C17 120.1(4) . . ? C18 C19 C20 121.7(5) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 118.4(5) . . ? C20 C21 C24 121.8(6) . . ? C22 C21 C24 119.7(6) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 121.6(5) . . ? C22 C23 H23 119.2 . . ? C18 C23 H23 119.2 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N6 C25 N7 118.0(4) . . ? N6 C25 C26 122.2(4) . . ? N7 C25 C26 119.8(5) . . ? N6 C25 Li1 63.7(3) . . ? N7 C25 Li1 68.5(3) . . ? C26 C25 Li1 139.1(4) . . ? N6 C25 Li2 62.5(3) . . ? N7 C25 Li2 62.4(3) . . ? C26 C25 Li2 156.6(4) . . ? Li1 C25 Li2 64.3(3) . . ? C31 C26 C27 118.0(5) . . ? C31 C26 C25 120.6(4) . . ? C27 C26 C25 121.3(5) . . ? C26 C27 C28 119.6(5) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 121.5(6) . . ? C29 C28 H28 119.2 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 118.7(6) . . ? C28 C29 C32 120.8(6) . . ? C30 C29 C32 120.5(6) . . ? C29 C30 C31 121.5(5) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C26 C31 C30 120.6(5) . . ? C26 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.4 . . ? Si2 C34 H34B 109.3 . . ? H34A C34 H34B 109.4 . . ? Si2 C34 H34C 109.8 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si1 C36 H36A 109.5 . . ? Si1 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si1 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si1 C37 H37A 109.5 . . ? Si1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si1 C38 H38A 109.5 . . ? Si1 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si1 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si3 C39 H39A 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si3 C40 H40A 109.5 . . ? Si3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si3 C41 Li2 78.4(2) . . ? Si3 C41 H41A 109.5 . . ? Li2 C41 H41A 66.1 . . ? Si3 C41 H41B 109.5 . . ? Li2 C41 H41B 172.1 . . ? H41A C41 H41B 109.5 . . ? Si3 C41 H41C 109.5 . . ? Li2 C41 H41C 67.4 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si4 C44 H44A 109.5 . . ? Si4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si5 C45 H45A 109.5 . . ? Si5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si5 C46 H46A 109.5 . . ? Si5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si5 C47 H47A 109.5 . . ? Si5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si6 C48 H48A 109.5 . . ? Si6 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si6 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si6 C49 H49A 109.5 . . ? Si6 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si6 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si6 C50 H50A 109.5 . . ? Si6 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si6 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N1 Li1 N6 117.5(4) . . ? N1 Li1 N3 131.7(4) . . ? N6 Li1 N3 110.7(4) . . ? N1 Li1 N7 96.9(4) . . ? N6 Li1 N7 63.6(3) . . ? N3 Li1 N7 101.5(3) . . ? N1 Li1 N2 105.4(3) . . ? N6 Li1 N2 106.3(4) . . ? N3 Li1 N2 62.0(3) . . ? N7 Li1 N2 157.7(4) . . ? N1 Li1 C25 97.3(4) . . ? N6 Li1 C25 34.42(18) . . ? N3 Li1 C25 122.1(4) . . ? N7 Li1 C25 34.06(18) . . ? N2 Li1 C25 140.7(4) . . ? N1 Li1 C9 109.5(4) . . ? N6 Li1 C9 126.2(4) . . ? N3 Li1 C9 34.53(18) . . ? N7 Li1 C9 135.3(4) . . ? N2 Li1 C9 33.36(18) . . ? C25 Li1 C9 153.1(4) . . ? N1 Li1 Li2 150.6(5) . . ? N6 Li1 Li2 54.8(3) . . ? N3 Li1 Li2 62.8(3) . . ? N7 Li1 Li2 53.8(3) . . ? N2 Li1 Li2 103.9(4) . . ? C25 Li1 Li2 60.0(3) . . ? C9 Li1 Li2 93.8(4) . . ? N1 Li1 Li3 151.9(4) . . ? N6 Li1 Li3 72.3(3) . . ? N3 Li1 Li3 49.5(3) . . ? N7 Li1 Li3 110.6(3) . . ? N2 Li1 Li3 47.5(2) . . ? C25 Li1 Li3 102.2(3) . . ? C9 Li1 Li3 53.9(3) . . ? Li2 Li1 Li3 57.3(3) . . ? N5 Li2 N7 160.4(4) . . ? N5 Li2 N6 111.8(4) . . ? N7 Li2 N6 63.5(3) . . ? N5 Li2 C25 135.0(4) . . ? N7 Li2 C25 33.04(18) . . ? N6 Li2 C25 32.87(17) . . ? N5 Li2 N3 105.5(4) . . ? N7 Li2 N3 94.0(3) . . ? N6 Li2 N3 98.6(3) . . ? C25 Li2 N3 106.8(3) . . ? N5 Li2 Li3 73.9(3) . . ? N7 Li2 Li3 120.2(4) . . ? N6 Li2 Li3 75.7(3) . . ? C25 Li2 Li3 105.0(4) . . ? N3 Li2 Li3 50.0(2) . . ? N5 Li2 Li1 138.5(4) . . ? N7 Li2 Li1 55.6(3) . . ? N6 Li2 Li1 52.5(3) . . ? C25 Li2 Li1 55.7(3) . . ? N3 Li2 Li1 51.5(3) . . ? Li3 Li2 Li1 65.2(3) . . ? N5 Li2 C41 69.9(3) . . ? N7 Li2 C41 91.5(3) . . ? N6 Li2 C41 97.6(3) . . ? C25 Li2 C41 86.0(3) . . ? N3 Li2 C41 163.7(4) . . ? Li3 Li2 C41 137.4(4) . . ? Li1 Li2 C41 141.6(4) . . ? N5 Li2 Si3 32.76(16) . . ? N7 Li2 Si3 128.6(3) . . ? N6 Li2 Si3 110.0(3) . . ? C25 Li2 Si3 115.7(3) . . ? N3 Li2 Si3 135.7(4) . . ? Li3 Li2 Si3 104.9(3) . . ? Li1 Li2 Si3 160.6(4) . . ? C41 Li2 Si3 37.20(14) . . ? N4 Li3 N2 142.9(5) . . ? N4 Li3 N3 114.7(4) . . ? N2 Li3 N3 66.9(3) . . ? N4 Li3 C9 127.9(4) . . ? N2 Li3 C9 34.60(18) . . ? N3 Li3 C9 34.98(17) . . ? N4 Li3 Li2 100.5(4) . . ? N2 Li3 Li2 111.5(4) . . ? N3 Li3 Li2 63.7(3) . . ? C9 Li3 Li2 94.4(4) . . ? N4 Li3 C17 27.75(18) . . ? N2 Li3 C17 166.7(4) . . ? N3 Li3 C17 106.5(3) . . ? C9 Li3 C17 135.1(4) . . ? Li2 Li3 C17 73.4(3) . . ? N4 Li3 Li1 156.9(4) . . ? N2 Li3 Li1 54.9(3) . . ? N3 Li3 Li1 51.6(3) . . ? C9 Li3 Li1 54.4(3) . . ? Li2 Li3 Li1 57.6(3) . . ? C17 Li3 Li1 131.0(4) . . ? N4 Li3 Si4 27.50(18) . . ? N2 Li3 Si4 116.6(3) . . ? N3 Li3 Si4 118.7(3) . . ? C9 Li3 Si4 113.6(3) . . ? Li2 Li3 Si4 127.6(3) . . ? C17 Li3 Si4 55.2(2) . . ? Li1 Li3 Si4 168.0(4) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.047 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.049