Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c1615fin _database_code_depnum_ccdc_archive 'CCDC 276506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H58 Li4 N6 S Si' _chemical_formula_weight 554.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 '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' 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.488(2) _cell_length_b 17.147(3) _cell_length_c 19.450(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.114(4) _cell_angle_gamma 90.00 _cell_volume 3661.6(12) _cell_formula_units_Z 4 _cell_measurement_temperature 206(2) _cell_measurement_reflns_used 952 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.36 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.006 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 206(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23374 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 29.22 _reflns_number_total 8822 _reflns_number_gt 6006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0667P)^2^+3.5363P] 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 8822 _refine_ls_number_parameters 486 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1867 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 S1 S -0.05182(6) 0.18163(4) 0.00914(3) 0.04117(17) Uani 1 1 d . . . Si1 Si -0.14537(7) 0.36630(5) 0.01273(4) 0.0472(2) Uani 1 1 d . . . N1 N -0.1222(2) 0.13842(15) 0.19066(13) 0.0502(6) Uani 1 1 d . . . N2 N 0.03813(18) 0.01431(13) 0.17115(11) 0.0411(5) Uani 1 1 d . . . N3 N 0.2522(2) 0.24051(14) -0.02128(14) 0.0535(6) Uani 1 1 d . . . N4 N 0.3191(2) 0.08949(18) 0.05030(14) 0.0643(8) Uani 1 1 d . . . N5 N 0.4691(2) 0.0108(2) 0.31018(15) 0.0708(8) Uani 1 1 d . . . N6 N 0.4154(3) -0.12100(16) 0.20817(17) 0.0664(7) Uani 1 1 d . . . C1 C -0.0080(2) 0.32468(14) 0.08087(13) 0.0379(5) Uani 1 1 d . . . C2 C 0.0293(2) 0.24589(14) 0.07961(12) 0.0337(5) Uani 1 1 d . . . C3 C 0.1312(2) 0.21304(14) 0.13261(13) 0.0363(5) Uani 1 1 d . . . C4 C 0.1932(2) 0.26520(16) 0.18660(14) 0.0425(6) Uani 1 1 d . . . C5 C 0.1611(3) 0.34264(17) 0.18928(16) 0.0506(7) Uani 1 1 d . . . C6 C 0.0615(3) 0.37161(16) 0.13644(16) 0.0472(6) Uani 1 1 d . . . C7 C -0.2888(3) 0.3170(3) 0.0156(3) 0.0668(9) Uani 1 1 d . . . C8 C -0.1297(4) 0.3628(3) -0.07990(19) 0.0658(9) Uani 1 1 d . . . C9 C -0.1608(4) 0.4712(2) 0.0348(3) 0.0725(10) Uani 1 1 d . . . C10 C -0.2514(3) 0.1336(3) 0.1507(2) 0.0738(10) Uani 1 1 d . . . C11 C -0.0965(4) 0.2130(3) 0.2288(2) 0.0750(11) Uani 1 1 d . . . C12 C -0.0857(3) 0.0727(2) 0.24129(17) 0.0569(8) Uani 1 1 d . . . C13 C -0.0591(3) 0.00077(19) 0.20519(18) 0.0532(7) Uani 1 1 d . . . C14 C 0.0375(3) -0.0504(2) 0.1222(2) 0.0635(9) Uani 1 1 d . . . C15 C 0.1632(2) 0.02064(18) 0.22381(15) 0.0454(6) Uani 1 1 d . . . C16 C 0.2587(5) 0.3195(2) 0.0064(3) 0.0816(12) Uani 1 1 d . . . C17 C 0.1955(5) 0.2405(3) -0.0977(2) 0.1055(16) Uani 1 1 d . . . H17A H 0.1146 0.2628 -0.1082 0.158 Uiso 1 1 calc R . . H17B H 0.1895 0.1873 -0.1155 0.158 Uiso 1 1 calc R . . H17C H 0.2441 0.2712 -0.1209 0.158 Uiso 1 1 calc R . . C18 C 0.3754(4) 0.2064(2) -0.0001(4) 0.116(2) Uani 1 1 d . . . H18A H 0.4145 0.2219 -0.0365 0.139 Uiso 1 1 calc R . . H18B H 0.4213 0.2313 0.0451 0.139 Uiso 1 1 calc R . . C19 C 0.3902(4) 0.1288(3) 0.0091(3) 0.119(2) Uani 1 1 d . . . H19A H 0.4766 0.1187 0.0331 0.143 Uiso 1 1 calc R . . H19B H 0.3702 0.1045 -0.0385 0.143 Uiso 1 1 calc R . . C20 C 0.3834(3) 0.08483(19) 0.12970(17) 0.0510(7) Uani 1 1 d . . . C21 C 0.2935(4) 0.0096(3) 0.0225(2) 0.0901(14) Uani 1 1 d . . . H21A H 0.2495 0.0114 -0.0284 0.135 Uiso 1 1 calc R . . H21B H 0.2445 -0.0171 0.0482 0.135 Uiso 1 1 calc R . . H21C H 0.3696 -0.0182 0.0293 0.135 Uiso 1 1 calc R . . C22 C 0.4156(4) 0.0156(3) 0.3682(2) 0.1022(15) Uani 1 1 d . . . H22A H 0.3664 -0.0304 0.3680 0.153 Uiso 1 1 calc R . . H22B H 0.3647 0.0617 0.3622 0.153 Uiso 1 1 calc R . . H22C H 0.4796 0.0187 0.4136 0.153 Uiso 1 1 calc R . . C23 C 0.5360(6) 0.0862(4) 0.3115(3) 0.168(3) Uani 1 1 d . . . H23A H 0.5981 0.0917 0.3574 0.252 Uiso 1 1 calc R . . H23B H 0.4792 0.1293 0.3047 0.252 Uiso 1 1 calc R . . H23C H 0.5741 0.0863 0.2731 0.252 Uiso 1 1 calc R . . C24 C 0.5514(5) -0.0497(5) 0.3148(3) 0.157(3) Uani 1 1 d . . . H24A H 0.5974 -0.0576 0.3654 0.189 Uiso 1 1 calc R . . H24B H 0.6095 -0.0345 0.2890 0.189 Uiso 1 1 calc R . . C25 C 0.4944(4) -0.1235(3) 0.2852(3) 0.0998(15) Uani 1 1 d . . . H25A H 0.4446 -0.1418 0.3152 0.120 Uiso 1 1 calc R . . H25B H 0.5588 -0.1622 0.2890 0.120 Uiso 1 1 calc R . . C26 C 0.3210(4) -0.1797(2) 0.1965(3) 0.1129(18) Uani 1 1 d . . . H26A H 0.2709 -0.1780 0.1467 0.169 Uiso 1 1 calc R . . H26B H 0.2709 -0.1695 0.2278 0.169 Uiso 1 1 calc R . . H26C H 0.3581 -0.2308 0.2071 0.169 Uiso 1 1 calc R . . C27 C 0.4927(5) -0.1308(3) 0.1621(3) 0.128(2) Uani 1 1 d . . . H27A H 0.5409 -0.1779 0.1757 0.191 Uiso 1 1 calc R . . H27B H 0.5464 -0.0862 0.1672 0.191 Uiso 1 1 calc R . . H27C H 0.4426 -0.1351 0.1125 0.191 Uiso 1 1 calc R . . Li1 Li -0.0111(4) 0.1215(3) 0.1238(2) 0.0418(9) Uani 1 1 d . . . Li2 Li 0.1657(4) 0.1662(3) 0.0333(2) 0.0436(10) Uani 1 1 d . . . Li3 Li 0.2290(4) 0.1070(3) 0.1661(3) 0.0489(11) Uani 1 1 d . . . Li4 Li 0.3429(4) -0.0051(3) 0.2058(2) 0.0448(10) Uani 1 1 d . . . H4 H 0.262(2) 0.2455(15) 0.2247(14) 0.037(7) Uiso 1 1 d . . . H5 H 0.204(3) 0.3767(18) 0.2255(17) 0.058(9) Uiso 1 1 d . . . H6 H 0.040(2) 0.4238(17) 0.1379(15) 0.047(8) Uiso 1 1 d . . . H7A H -0.297(4) 0.320(2) 0.059(2) 0.093(14) Uiso 1 1 d . . . H7B H -0.289(3) 0.260(2) 0.0047(19) 0.080(11) Uiso 1 1 d . . . H7C H -0.355(4) 0.338(3) -0.017(2) 0.105(15) Uiso 1 1 d . . . H8A H -0.122(5) 0.310(3) -0.096(3) 0.14(2) Uiso 1 1 d . . . H8B H -0.058(4) 0.389(2) -0.083(2) 0.092(13) Uiso 1 1 d . . . H8C H -0.180(5) 0.388(3) -0.109(3) 0.129(19) Uiso 1 1 d . . . H9A H -0.169(3) 0.480(2) 0.083(2) 0.076(11) Uiso 1 1 d . . . H9B H -0.234(4) 0.490(2) 0.006(2) 0.089(13) Uiso 1 1 d . . . H9C H -0.095(5) 0.504(3) 0.034(3) 0.113(17) Uiso 1 1 d . . . H10A H -0.270(3) 0.173(2) 0.112(2) 0.081(12) Uiso 1 1 d . . . H10B H -0.304(4) 0.138(2) 0.185(2) 0.086(12) Uiso 1 1 d . . . H10C H -0.271(4) 0.089(3) 0.123(2) 0.096(15) Uiso 1 1 d . . . H11A H -0.121(3) 0.254(2) 0.194(2) 0.075(12) Uiso 1 1 d . . . H11B H -0.144(3) 0.219(2) 0.262(2) 0.084(11) Uiso 1 1 d . . . H11C H -0.001(5) 0.221(3) 0.252(2) 0.108(15) Uiso 1 1 d . . . H12A H -0.148(3) 0.0611(18) 0.2642(16) 0.058(9) Uiso 1 1 d . . . H12B H -0.017(3) 0.0900(19) 0.2788(18) 0.062(9) Uiso 1 1 d . . . H13A H -0.132(3) -0.0156(18) 0.1676(17) 0.062(9) Uiso 1 1 d . . . H13B H -0.039(3) -0.0442(18) 0.2401(17) 0.056(8) Uiso 1 1 d . . . H14A H 0.107(4) -0.042(2) 0.098(2) 0.082(11) Uiso 1 1 d . . . H14B H -0.037(3) -0.054(2) 0.087(2) 0.076(11) Uiso 1 1 d . . . H14C H 0.056(3) -0.101(2) 0.1483(19) 0.075(11) Uiso 1 1 d . . . H15A H 0.158(3) 0.0633(18) 0.2559(16) 0.053(8) Uiso 1 1 d . . . H15B H 0.171(3) -0.0282(19) 0.2538(17) 0.065(9) Uiso 1 1 d . . . H16A H 0.311(3) 0.353(2) -0.015(2) 0.078(11) Uiso 1 1 d . . . H16B H 0.173(5) 0.343(3) -0.007(3) 0.14(2) Uiso 1 1 d . . . H16C H 0.291(4) 0.319(2) 0.057(3) 0.101(15) Uiso 1 1 d . . . H20A H 0.403(3) 0.138(2) 0.1471(17) 0.063(9) Uiso 1 1 d . . . H20B H 0.466(3) 0.0574(18) 0.1359(16) 0.063(9) 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 S1 0.0420(3) 0.0455(3) 0.0333(3) -0.0074(3) 0.0068(2) -0.0003(3) Si1 0.0427(4) 0.0503(4) 0.0491(4) 0.0096(3) 0.0141(3) 0.0110(3) N1 0.0436(12) 0.0631(15) 0.0504(13) -0.0013(11) 0.0241(10) 0.0030(11) N2 0.0357(11) 0.0466(12) 0.0426(11) -0.0013(9) 0.0141(9) -0.0032(9) N3 0.0562(14) 0.0460(13) 0.0668(16) 0.0030(12) 0.0314(12) 0.0011(11) N4 0.0529(15) 0.089(2) 0.0600(15) 0.0314(15) 0.0311(12) 0.0316(14) N5 0.0440(14) 0.107(2) 0.0543(16) 0.0025(15) 0.0026(12) 0.0017(15) N6 0.0626(17) 0.0546(16) 0.087(2) 0.0139(14) 0.0305(15) 0.0156(13) C1 0.0372(12) 0.0405(13) 0.0376(12) -0.0010(10) 0.0136(10) 0.0044(10) C2 0.0345(11) 0.0376(12) 0.0310(11) -0.0041(9) 0.0129(9) -0.0015(9) C3 0.0334(12) 0.0400(13) 0.0375(12) -0.0016(10) 0.0138(10) 0.0008(10) C4 0.0328(12) 0.0517(15) 0.0403(13) -0.0050(11) 0.0068(10) -0.0001(11) C5 0.0454(15) 0.0517(16) 0.0509(16) -0.0206(13) 0.0084(13) -0.0035(12) C6 0.0484(15) 0.0383(14) 0.0560(16) -0.0108(12) 0.0171(13) 0.0038(12) C7 0.0454(18) 0.077(3) 0.078(3) 0.017(2) 0.0180(17) 0.0106(17) C8 0.064(2) 0.084(3) 0.0474(18) 0.0194(18) 0.0125(16) 0.010(2) C9 0.072(3) 0.055(2) 0.092(3) 0.009(2) 0.026(2) 0.0230(19) C10 0.0452(18) 0.098(3) 0.080(3) 0.012(3) 0.0210(18) 0.0086(19) C11 0.093(3) 0.073(2) 0.076(3) -0.015(2) 0.053(2) 0.005(2) C12 0.0499(17) 0.083(2) 0.0467(16) 0.0069(15) 0.0276(14) 0.0027(16) C13 0.0438(15) 0.0615(19) 0.0576(17) 0.0097(15) 0.0196(14) -0.0064(14) C14 0.0525(19) 0.062(2) 0.072(2) -0.0220(18) 0.0121(17) -0.0028(16) C15 0.0378(13) 0.0491(16) 0.0475(15) 0.0004(13) 0.0098(11) -0.0008(12) C16 0.116(4) 0.050(2) 0.094(3) 0.003(2) 0.054(3) -0.013(2) C17 0.140(4) 0.125(4) 0.062(2) 0.001(2) 0.045(3) -0.041(3) C18 0.071(3) 0.072(3) 0.237(6) 0.032(3) 0.096(4) 0.003(2) C19 0.089(3) 0.168(5) 0.132(4) 0.097(4) 0.083(3) 0.073(3) C20 0.0438(15) 0.0540(18) 0.0587(17) 0.0080(14) 0.0205(13) 0.0078(13) C21 0.090(3) 0.115(3) 0.059(2) -0.016(2) 0.0121(19) 0.045(3) C22 0.082(3) 0.166(5) 0.053(2) -0.018(3) 0.0109(19) 0.009(3) C23 0.135(5) 0.244(8) 0.099(4) -0.016(4) -0.005(3) -0.120(5) C24 0.119(4) 0.243(8) 0.077(3) -0.022(4) -0.022(3) 0.100(5) C25 0.080(3) 0.084(3) 0.122(4) 0.048(3) 0.010(3) 0.027(2) C26 0.096(3) 0.044(2) 0.187(6) 0.001(3) 0.023(3) 0.000(2) C27 0.162(5) 0.115(4) 0.139(5) 0.036(3) 0.095(4) 0.076(4) Li1 0.036(2) 0.051(3) 0.040(2) -0.0029(19) 0.0126(17) -0.0007(18) Li2 0.041(2) 0.052(3) 0.041(2) 0.0010(19) 0.0179(18) 0.0040(19) Li3 0.042(2) 0.050(3) 0.055(3) 0.006(2) 0.014(2) 0.008(2) Li4 0.036(2) 0.044(2) 0.051(3) 0.0049(19) 0.0077(19) 0.0028(18) _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 S1 C2 1.791(2) . ? S1 Li1 2.375(4) . ? S1 Li2 2.417(4) . ? Si1 C8 1.863(4) . ? Si1 C7 1.868(4) . ? Si1 C9 1.870(4) . ? Si1 C1 1.878(3) . ? N1 C10 1.461(4) . ? N1 C11 1.464(5) . ? N1 C12 1.474(4) . ? N1 Li1 2.094(5) . ? N2 C14 1.460(4) . ? N2 C13 1.474(3) . ? N2 C15 1.503(3) . ? N2 Li1 2.059(5) . ? N3 C17 1.437(5) . ? N3 C16 1.451(5) . ? N3 C18 1.473(5) . ? N3 Li2 2.088(5) . ? N4 C19 1.465(4) . ? N4 C21 1.470(5) . ? N4 C20 1.505(4) . ? N4 Li2 2.146(5) . ? N5 C24 1.389(6) . ? N5 C22 1.437(5) . ? N5 C23 1.501(6) . ? N5 Li4 2.137(5) . ? N6 C27 1.444(5) . ? N6 C26 1.447(5) . ? N6 C25 1.506(5) . ? N6 Li4 2.150(5) . ? C1 C6 1.395(4) . ? C1 C2 1.420(3) . ? C2 C3 1.428(3) . ? C2 Li1 2.395(5) . ? C2 Li2 2.442(5) . ? C3 C4 1.404(3) . ? C3 Li3 2.137(5) . ? C3 Li2 2.233(5) . ? C3 Li1 2.236(5) . ? C4 C5 1.383(4) . ? C5 C6 1.386(4) . ? C12 C13 1.494(5) . ? C13 Li1 2.759(5) . ? C15 Li3 2.127(6) . ? C15 Li4 2.237(5) . ? C18 C19 1.347(6) . ? C18 Li2 2.761(6) . ? C20 Li3 2.127(5) . ? C20 Li4 2.278(5) . ? C24 C25 1.463(8) . ? Li1 Li3 2.648(6) . ? Li1 Li2 3.149(6) . ? Li2 Li3 2.669(6) . ? Li3 Li4 2.325(6) . ? 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 C2 S1 Li1 68.53(13) . . ? C2 S1 Li2 69.11(13) . . ? Li1 S1 Li2 82.14(14) . . ? C8 Si1 C7 110.5(2) . . ? C8 Si1 C9 107.2(2) . . ? C7 Si1 C9 106.5(2) . . ? C8 Si1 C1 111.72(15) . . ? C7 Si1 C1 111.90(15) . . ? C9 Si1 C1 108.69(17) . . ? C10 N1 C11 110.0(3) . . ? C10 N1 C12 110.9(3) . . ? C11 N1 C12 110.7(3) . . ? C10 N1 Li1 111.8(3) . . ? C11 N1 Li1 111.5(2) . . ? C12 N1 Li1 101.7(2) . . ? C14 N2 C13 108.3(2) . . ? C14 N2 C15 108.6(2) . . ? C13 N2 C15 113.8(2) . . ? C14 N2 Li1 116.0(2) . . ? C13 N2 Li1 101.4(2) . . ? C15 N2 Li1 108.8(2) . . ? C17 N3 C16 110.0(3) . . ? C17 N3 C18 113.3(4) . . ? C16 N3 C18 109.1(4) . . ? C17 N3 Li2 112.8(3) . . ? C16 N3 Li2 111.1(3) . . ? C18 N3 Li2 100.2(2) . . ? C19 N4 C21 108.1(4) . . ? C19 N4 C20 113.7(3) . . ? C21 N4 C20 108.2(3) . . ? C19 N4 Li2 101.4(2) . . ? C21 N4 Li2 116.6(3) . . ? C20 N4 Li2 108.9(2) . . ? C24 N5 C22 115.6(4) . . ? C24 N5 C23 107.8(5) . . ? C22 N5 C23 105.8(4) . . ? C24 N5 Li4 103.0(3) . . ? C22 N5 Li4 115.2(3) . . ? C23 N5 Li4 109.1(3) . . ? C27 N6 C26 113.0(4) . . ? C27 N6 C25 108.3(4) . . ? C26 N6 C25 109.9(3) . . ? C27 N6 Li4 113.6(3) . . ? C26 N6 Li4 111.8(2) . . ? C25 N6 Li4 99.5(3) . . ? C6 C1 C2 117.1(2) . . ? C6 C1 Si1 119.9(2) . . ? C2 C1 Si1 122.99(18) . . ? C1 C2 C3 123.4(2) . . ? C1 C2 S1 120.47(18) . . ? C3 C2 S1 116.16(18) . . ? C1 C2 Li1 138.62(19) . . ? C3 C2 Li1 66.04(16) . . ? S1 C2 Li1 67.35(13) . . ? C1 C2 Li2 140.2(2) . . ? C3 C2 Li2 64.34(16) . . ? S1 C2 Li2 67.63(13) . . ? Li1 C2 Li2 81.22(16) . . ? C4 C3 C2 114.6(2) . . ? C4 C3 Li3 102.0(2) . . ? C2 C3 Li3 143.3(2) . . ? C4 C3 Li2 134.1(2) . . ? C2 C3 Li2 80.44(18) . . ? Li3 C3 Li2 75.29(19) . . ? C4 C3 Li1 134.7(2) . . ? C2 C3 Li1 78.23(18) . . ? Li3 C3 Li1 74.51(19) . . ? Li2 C3 Li1 89.61(18) . . ? C5 C4 C3 123.9(2) . . ? C4 C5 C6 119.2(2) . . ? C5 C6 C1 121.8(3) . . ? N1 C12 C13 112.0(2) . . ? N2 C13 C12 111.6(2) . . ? N2 C13 Li1 47.04(15) . . ? C12 C13 Li1 75.74(19) . . ? N2 C15 Li3 96.2(2) . . ? N2 C15 Li4 128.3(2) . . ? Li3 C15 Li4 64.32(18) . . ? C19 C18 N3 120.1(4) . . ? C19 C18 Li2 78.8(2) . . ? N3 C18 Li2 48.09(17) . . ? C18 C19 N4 117.3(4) . . ? N4 C20 Li3 97.3(2) . . ? N4 C20 Li4 124.8(2) . . ? Li3 C20 Li4 63.60(18) . . ? N5 C24 C25 113.8(5) . . ? C24 C25 N6 115.8(4) . . ? N2 Li1 N1 89.03(19) . . ? N2 Li1 C3 119.6(2) . . ? N1 Li1 C3 114.9(2) . . ? N2 Li1 S1 139.4(2) . . ? N1 Li1 S1 122.4(2) . . ? C3 Li1 S1 72.84(14) . . ? N2 Li1 C2 154.0(2) . . ? N1 Li1 C2 108.5(2) . . ? C3 Li1 C2 35.72(11) . . ? S1 Li1 C2 44.12(10) . . ? N2 Li1 Li3 69.71(17) . . ? N1 Li1 Li3 126.2(2) . . ? C3 Li1 Li3 51.04(15) . . ? S1 Li1 Li3 103.41(18) . . ? C2 Li1 Li3 84.35(17) . . ? N2 Li1 C13 31.60(11) . . ? N1 Li1 C13 59.07(14) . . ? C3 Li1 C13 138.4(2) . . ? S1 Li1 C13 147.9(2) . . ? C2 Li1 C13 165.2(2) . . ? Li3 Li1 C13 96.71(18) . . ? N2 Li1 Li2 109.28(19) . . ? N1 Li1 Li2 157.7(2) . . ? C3 Li1 Li2 45.16(13) . . ? S1 Li1 Li2 49.51(11) . . ? C2 Li1 Li2 50.05(13) . . ? Li3 Li1 Li2 54.01(15) . . ? C13 Li1 Li2 140.74(19) . . ? N3 Li2 N4 87.72(18) . . ? N3 Li2 C3 116.9(2) . . ? N4 Li2 C3 115.7(2) . . ? N3 Li2 S1 117.0(2) . . ? N4 Li2 S1 148.4(2) . . ? C3 Li2 S1 72.07(14) . . ? N3 Li2 C2 107.4(2) . . ? N4 Li2 C2 150.8(2) . . ? C3 Li2 C2 35.22(10) . . ? S1 Li2 C2 43.26(9) . . ? N3 Li2 Li3 133.6(2) . . ? N4 Li2 Li3 68.88(17) . . ? C3 Li2 Li3 50.73(15) . . ? S1 Li2 Li3 101.62(18) . . ? C2 Li2 Li3 82.98(17) . . ? N3 Li2 C18 31.68(13) . . ? N4 Li2 C18 57.00(15) . . ? C3 Li2 C18 120.2(2) . . ? S1 Li2 C18 148.3(2) . . ? C2 Li2 C18 130.3(2) . . ? Li3 Li2 C18 108.3(2) . . ? N3 Li2 Li1 156.2(2) . . ? N4 Li2 Li1 113.6(2) . . ? C3 Li2 Li1 45.23(13) . . ? S1 Li2 Li1 48.35(11) . . ? C2 Li2 Li1 48.74(12) . . ? Li3 Li2 Li1 53.37(15) . . ? C18 Li2 Li1 160.6(2) . . ? C15 Li3 C20 120.8(2) . . ? C15 Li3 C3 121.1(2) . . ? C20 Li3 C3 117.8(2) . . ? C15 Li3 Li4 60.13(18) . . ? C20 Li3 Li4 61.35(18) . . ? C3 Li3 Li4 177.4(3) . . ? C15 Li3 Li1 74.33(18) . . ? C20 Li3 Li1 143.8(3) . . ? C3 Li3 Li1 54.45(15) . . ? Li4 Li3 Li1 127.9(2) . . ? C15 Li3 Li2 137.5(3) . . ? C20 Li3 Li2 76.27(19) . . ? C3 Li3 Li2 53.99(15) . . ? Li4 Li3 Li2 127.1(2) . . ? Li1 Li3 Li2 72.62(17) . . ? N5 Li4 N6 87.0(2) . . ? N5 Li4 C15 103.0(2) . . ? N6 Li4 C15 123.3(2) . . ? N5 Li4 C20 108.7(2) . . ? N6 Li4 C20 119.2(2) . . ? C15 Li4 C20 110.0(2) . . ? N5 Li4 Li3 111.6(2) . . ? N6 Li4 Li3 161.4(3) . . ? C15 Li4 Li3 55.54(17) . . ? C20 Li4 Li3 55.05(17) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 29.22 _diffrn_measured_fraction_theta_full 0.886 _refine_diff_density_max 0.581 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.050 data_c1681fin _database_code_depnum_ccdc_archive 'CCDC 276507' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H70 Li6 N8 S2' _chemical_formula_weight 720.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 '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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6446(12) _cell_length_b 17.4654(17) _cell_length_c 11.6050(11) _cell_angle_alpha 90.00 _cell_angle_beta 114.957(2) _cell_angle_gamma 90.00 _cell_volume 2323.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 3532 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.22 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.030 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12910 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.0878 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4748 _reflns_number_gt 2955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _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^)+(0.0792P)^2^+3.5834P] 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 4748 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1656 _refine_ls_R_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.2592 _refine_ls_wR_factor_gt 0.2288 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 S1 S -0.23914(10) 0.04679(7) 1.49826(12) 0.0473(4) Uani 1 1 d . . . N1 N 0.0064(3) 0.1828(2) 1.4071(3) 0.0437(9) Uani 1 1 d . . . N2 N -0.2434(4) 0.1867(2) 1.2509(4) 0.0591(12) Uani 1 1 d . . . N3 N -0.2225(4) -0.0315(3) 1.7942(4) 0.0641(12) Uani 1 1 d . . . N4 N -0.3650(4) -0.1433(3) 1.6055(6) 0.0761(15) Uani 1 1 d . . . C1 C -0.2397(4) -0.0045(3) 1.3638(4) 0.0420(10) Uani 1 1 d . . . C2 C -0.1336(4) -0.0084(3) 1.3497(4) 0.0418(10) Uani 1 1 d . . . C3 C -0.1430(5) -0.0504(3) 1.2421(5) 0.0553(13) Uani 1 1 d . . . H3 H -0.0758 -0.0551 1.2270 0.066 Uiso 1 1 calc R . . C4 C -0.2442(6) -0.0852(3) 1.1569(5) 0.0707(16) Uani 1 1 d . . . H4 H -0.2439 -0.1133 1.0881 0.085 Uiso 1 1 calc R . . C5 C -0.3448(5) -0.0784(4) 1.1735(5) 0.0732(17) Uani 1 1 d . . . H5 H -0.4142 -0.1013 1.1155 0.088 Uiso 1 1 calc R . . C6 C -0.3433(4) -0.0377(3) 1.2763(5) 0.0609(14) Uani 1 1 d . . . H6 H -0.4123 -0.0322 1.2875 0.073 Uiso 1 1 calc R . . C7 C 0.0572(4) 0.1343(3) 1.3368(5) 0.0434(11) Uani 1 1 d . . . C8 C 0.0993(5) 0.2073(3) 1.5287(5) 0.0583(14) Uani 1 1 d . . . C9 C -0.0524(5) 0.2521(3) 1.3365(5) 0.0520(12) Uani 1 1 d . . . C10 C -0.1622(5) 0.2339(3) 1.2201(5) 0.0566(14) Uani 1 1 d . . . C11 C -0.3057(7) 0.2345(4) 1.3063(9) 0.081(2) Uani 1 1 d . . . C12 C -0.3278(8) 0.1483(5) 1.1378(8) 0.094(3) Uani 1 1 d . . . C13 C -0.2188(9) 0.0513(4) 1.8060(7) 0.135(4) Uani 1 1 d . . . H13A H -0.2868 0.0732 1.7374 0.202 Uiso 1 1 calc R . . H13B H -0.1486 0.0705 1.8017 0.202 Uiso 1 1 calc R . . H13C H -0.2187 0.0655 1.8869 0.202 Uiso 1 1 calc R . . C14 C -0.1241(5) -0.0648(4) 1.9019(5) 0.0752(17) Uani 1 1 d . . . H14A H -0.1304 -0.0520 1.9802 0.113 Uiso 1 1 calc R . . H14B H -0.0517 -0.0444 1.9047 0.113 Uiso 1 1 calc R . . H14C H -0.1249 -0.1200 1.8924 0.113 Uiso 1 1 calc R . . C15 C -0.3307(6) -0.0614(8) 1.7879(8) 0.148(5) Uani 1 1 d . . . H15A H -0.3208 -0.0693 1.8755 0.177 Uiso 1 1 calc R . . H15B H -0.3896 -0.0213 1.7514 0.177 Uiso 1 1 calc R . . C16 C -0.3743(10) -0.1239(8) 1.7261(12) 0.178(6) Uani 1 1 d . . . H16A H -0.4576 -0.1238 1.7070 0.214 Uiso 1 1 calc R . . H16B H -0.3391 -0.1664 1.7850 0.214 Uiso 1 1 calc R . . C17 C -0.4694(5) -0.1183(4) 1.4988(7) 0.098(2) Uani 1 1 d . . . H17A H -0.4599 -0.1255 1.4208 0.147 Uiso 1 1 calc R . . H17B H -0.4829 -0.0645 1.5087 0.147 Uiso 1 1 calc R . . H17C H -0.5354 -0.1481 1.4953 0.147 Uiso 1 1 calc R . . C18 C -0.3537(6) -0.2235(4) 1.6003(13) 0.181(6) Uani 1 1 d . . . H18A H -0.4156 -0.2483 1.6149 0.271 Uiso 1 1 calc R . . H18B H -0.2787 -0.2393 1.6652 0.271 Uiso 1 1 calc R . . H18C H -0.3591 -0.2379 1.5173 0.271 Uiso 1 1 calc R . . Li1 Li -0.1313(7) 0.1143(4) 1.3948(7) 0.0462(18) Uani 1 1 d . . . Li2 Li -0.2197(6) -0.0725(4) 1.6214(8) 0.0484(19) Uani 1 1 d . . . Li3 Li 0.0528(7) 0.0249(4) 1.4333(7) 0.0463(18) Uani 1 1 d . . . H7A H -0.010(4) 0.116(3) 1.257(5) 0.063(15) Uiso 1 1 d . . . H7B H 0.101(4) 0.172(3) 1.303(4) 0.058(14) Uiso 1 1 d . . . H8A H 0.069(5) 0.241(3) 1.579(5) 0.072(17) Uiso 1 1 d . . . H8B H 0.145(5) 0.164(3) 1.585(5) 0.073(17) Uiso 1 1 d . . . H8C H 0.174(5) 0.243(3) 1.517(5) 0.072(16) Uiso 1 1 d . . . H9A H -0.076(4) 0.289(3) 1.394(4) 0.045(12) Uiso 1 1 d . . . H9B H 0.001(4) 0.289(3) 1.312(5) 0.070(16) Uiso 1 1 d . . . H10A H -0.205(4) 0.288(3) 1.173(5) 0.067(15) Uiso 1 1 d . . . H10B H -0.145(4) 0.207(3) 1.165(5) 0.057(15) Uiso 1 1 d . . . H11A H -0.359(7) 0.202(4) 1.333(7) 0.13(3) Uiso 1 1 d . . . H11B H -0.363(5) 0.281(4) 1.234(6) 0.093(19) Uiso 1 1 d . . . H11C H -0.253(6) 0.261(4) 1.371(6) 0.09(3) Uiso 1 1 d . . . H12A H -0.371(5) 0.112(4) 1.162(6) 0.09(2) Uiso 1 1 d . . . H12B H -0.290(6) 0.119(4) 1.101(6) 0.08(2) Uiso 1 1 d . . . H12C H -0.379(6) 0.183(4) 1.065(7) 0.10(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 S1 0.0490(7) 0.0484(7) 0.0524(7) 0.0107(6) 0.0291(6) 0.0116(6) N1 0.049(2) 0.037(2) 0.046(2) 0.0013(17) 0.0207(18) 0.0053(17) N2 0.053(2) 0.055(3) 0.062(3) 0.016(2) 0.017(2) 0.005(2) N3 0.072(3) 0.079(3) 0.048(2) 0.011(2) 0.032(2) 0.014(2) N4 0.044(2) 0.057(3) 0.129(5) 0.010(3) 0.038(3) -0.005(2) C1 0.039(2) 0.045(3) 0.041(2) 0.008(2) 0.015(2) 0.003(2) C2 0.048(3) 0.044(2) 0.036(2) 0.005(2) 0.021(2) -0.001(2) C3 0.066(3) 0.056(3) 0.051(3) 0.002(2) 0.032(3) -0.008(3) C4 0.099(5) 0.063(4) 0.048(3) -0.010(3) 0.029(3) -0.025(3) C5 0.069(4) 0.078(4) 0.053(3) -0.003(3) 0.006(3) -0.028(3) C6 0.043(3) 0.070(4) 0.064(3) 0.012(3) 0.016(3) -0.005(3) C7 0.039(2) 0.047(3) 0.047(3) 0.005(2) 0.020(2) 0.002(2) C8 0.063(3) 0.047(3) 0.053(3) -0.008(3) 0.013(3) -0.001(3) C9 0.060(3) 0.033(2) 0.068(3) 0.009(2) 0.032(3) 0.008(2) C10 0.064(3) 0.052(3) 0.059(3) 0.019(3) 0.031(3) 0.017(3) C11 0.069(4) 0.072(5) 0.120(7) 0.029(5) 0.055(5) 0.020(4) C12 0.079(5) 0.080(5) 0.084(6) 0.020(5) -0.004(4) -0.002(4) C13 0.264(12) 0.075(5) 0.086(5) 0.004(4) 0.094(7) 0.052(6) C14 0.071(4) 0.100(5) 0.054(3) 0.002(3) 0.026(3) 0.006(3) C15 0.063(4) 0.318(16) 0.079(5) -0.009(8) 0.048(4) -0.006(7) C16 0.146(9) 0.245(15) 0.182(12) -0.018(10) 0.107(9) -0.109(10) C17 0.060(4) 0.086(5) 0.140(6) 0.040(5) 0.034(4) 0.009(3) C18 0.054(4) 0.057(5) 0.371(16) 0.054(7) 0.031(7) -0.006(4) Li1 0.054(4) 0.045(4) 0.044(4) 0.008(3) 0.025(4) 0.006(4) Li2 0.043(4) 0.046(4) 0.062(5) 0.008(4) 0.027(4) 0.001(3) Li3 0.049(4) 0.045(4) 0.051(4) 0.003(3) 0.028(4) 0.000(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 S1 C1 1.797(5) . ? S1 Li1 2.465(7) . ? S1 Li2 2.479(8) . ? S1 Li3 2.484(8) 3_558 ? N1 C8 1.468(6) . ? N1 C9 1.476(6) . ? N1 C7 1.496(6) . ? N1 Li1 2.067(9) . ? N2 C12 1.459(9) . ? N2 C11 1.468(8) . ? N2 C10 1.473(7) . ? N2 Li1 2.098(8) . ? N3 C15 1.437(9) . ? N3 C13 1.452(8) . ? N3 C14 1.461(7) . ? N3 Li2 2.143(9) . ? N4 C18 1.412(9) . ? N4 C17 1.444(8) . ? N4 C16 1.492(12) . ? N4 Li2 2.156(9) . ? C1 C6 1.400(6) . ? C1 C2 1.420(6) . ? C1 Li1 2.429(9) . ? C1 Li3 2.561(9) 3_558 ? C2 C3 1.409(6) . ? C2 Li1 2.204(9) . ? C2 Li3 2.215(9) . ? C2 Li3 2.301(9) 3_558 ? C3 C4 1.384(7) . ? C4 C5 1.369(8) . ? C5 C6 1.382(8) . ? C7 Li2 2.187(9) 3_558 ? C7 Li3 2.227(9) . ? C7 Li1 2.758(9) . ? C9 C10 1.507(8) . ? C15 C16 1.294(14) . ? Li1 Li3 2.680(10) . ? Li1 Li3 3.034(11) 3_558 ? Li2 C7 2.187(9) 3_558 ? Li2 Li3 2.584(10) 3_558 ? Li3 C2 2.301(9) 3_558 ? Li3 S1 2.484(8) 3_558 ? Li3 C1 2.561(9) 3_558 ? Li3 Li3 2.584(14) 3_558 ? Li3 Li2 2.584(10) 3_558 ? Li3 Li1 3.034(11) 3_558 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 Li1 67.4(2) . . ? C1 S1 Li2 92.6(2) . . ? Li1 S1 Li2 137.9(2) . . ? C1 S1 Li3 71.4(2) . 3_558 ? Li1 S1 Li3 75.6(2) . 3_558 ? Li2 S1 Li3 62.8(2) . 3_558 ? C8 N1 C9 107.8(4) . . ? C8 N1 C7 109.6(4) . . ? C9 N1 C7 113.2(4) . . ? C8 N1 Li1 123.0(4) . . ? C9 N1 Li1 102.9(3) . . ? C7 N1 Li1 100.2(3) . . ? C12 N2 C11 109.4(7) . . ? C12 N2 C10 111.0(6) . . ? C11 N2 C10 110.2(5) . . ? C12 N2 Li1 115.5(5) . . ? C11 N2 Li1 107.5(5) . . ? C10 N2 Li1 102.9(4) . . ? C15 N3 C13 111.0(7) . . ? C15 N3 C14 110.3(6) . . ? C13 N3 C14 109.5(6) . . ? C15 N3 Li2 102.8(5) . . ? C13 N3 Li2 114.1(4) . . ? C14 N3 Li2 108.9(4) . . ? C18 N4 C17 109.6(6) . . ? C18 N4 C16 108.3(8) . . ? C17 N4 C16 109.3(7) . . ? C18 N4 Li2 118.4(5) . . ? C17 N4 Li2 109.7(4) . . ? C16 N4 Li2 101.0(5) . . ? C6 C1 C2 122.5(4) . . ? C6 C1 S1 119.7(4) . . ? C2 C1 S1 117.8(3) . . ? C6 C1 Li1 139.3(4) . . ? C2 C1 Li1 63.7(3) . . ? S1 C1 Li1 69.5(2) . . ? C6 C1 Li3 145.8(4) . 3_558 ? C2 C1 Li3 63.2(3) . 3_558 ? S1 C1 Li3 66.8(2) . 3_558 ? Li1 C1 Li3 74.8(3) . 3_558 ? C3 C2 C1 113.4(4) . . ? C3 C2 Li1 134.7(4) . . ? C1 C2 Li1 81.1(3) . . ? C3 C2 Li3 101.6(4) . . ? C1 C2 Li3 145.0(4) . . ? Li1 C2 Li3 74.7(3) . . ? C3 C2 Li3 137.5(4) . 3_558 ? C1 C2 Li3 83.4(3) . 3_558 ? Li1 C2 Li3 84.6(3) . 3_558 ? Li3 C2 Li3 69.8(3) . 3_558 ? C4 C3 C2 124.6(5) . . ? C5 C4 C3 119.7(5) . . ? C4 C5 C6 119.4(5) . . ? C5 C6 C1 120.4(5) . . ? N1 C7 Li2 137.6(4) . 3_558 ? N1 C7 Li3 96.0(3) . . ? Li2 C7 Li3 71.7(3) 3_558 . ? N1 C7 Li1 47.5(3) . . ? Li2 C7 Li1 135.4(3) 3_558 . ? Li3 C7 Li1 64.0(3) . . ? N1 C9 C10 112.5(4) . . ? N2 C10 C9 111.9(4) . . ? C16 C15 N3 120.6(9) . . ? C15 C16 N4 121.8(8) . . ? N1 Li1 N2 88.5(3) . . ? N1 Li1 C2 120.3(4) . . ? N2 Li1 C2 117.4(4) . . ? N1 Li1 C1 155.6(4) . . ? N2 Li1 C1 104.3(4) . . ? C2 Li1 C1 35.26(19) . . ? N1 Li1 S1 150.0(4) . . ? N2 Li1 S1 110.5(3) . . ? C2 Li1 S1 72.3(2) . . ? C1 Li1 S1 43.08(17) . . ? N1 Li1 Li3 71.2(3) . . ? N2 Li1 Li3 137.1(4) . . ? C2 Li1 Li3 52.8(3) . . ? C1 Li1 Li3 85.6(3) . . ? S1 Li1 Li3 105.1(3) . . ? N1 Li1 C7 32.25(18) . . ? N2 Li1 C7 95.3(3) . . ? C2 Li1 C7 89.5(3) . . ? C1 Li1 C7 124.3(3) . . ? S1 Li1 C7 153.1(3) . . ? Li3 Li1 C7 48.3(2) . . ? N1 Li1 Li3 112.7(3) . 3_558 ? N2 Li1 Li3 158.5(4) . 3_558 ? C2 Li1 Li3 49.0(2) . 3_558 ? C1 Li1 Li3 54.6(2) . 3_558 ? S1 Li1 Li3 52.5(2) . 3_558 ? Li3 Li1 Li3 53.3(3) . 3_558 ? C7 Li1 Li3 100.6(3) . 3_558 ? N3 Li2 N4 85.5(3) . . ? N3 Li2 C7 110.0(4) . 3_558 ? N4 Li2 C7 115.0(4) . 3_558 ? N3 Li2 S1 102.8(3) . . ? N4 Li2 S1 124.0(4) . . ? C7 Li2 S1 113.4(3) 3_558 . ? N3 Li2 Li3 117.4(4) . 3_558 ? N4 Li2 Li3 156.6(5) . 3_558 ? C7 Li2 Li3 54.9(3) 3_558 3_558 ? S1 Li2 Li3 58.7(2) . 3_558 ? C2 Li3 C7 104.6(4) . . ? C2 Li3 C2 110.2(3) . 3_558 ? C7 Li3 C2 124.3(4) . 3_558 ? C2 Li3 S1 134.3(4) . 3_558 ? C7 Li3 S1 111.8(3) . 3_558 ? C2 Li3 S1 70.4(2) 3_558 3_558 ? C2 Li3 C1 139.9(4) . 3_558 ? C7 Li3 C1 111.9(3) . 3_558 ? C2 Li3 C1 33.41(18) 3_558 3_558 ? S1 Li3 C1 41.71(16) 3_558 3_558 ? C2 Li3 Li3 56.7(3) . 3_558 ? C7 Li3 Li3 135.9(5) . 3_558 ? C2 Li3 Li3 53.5(3) 3_558 3_558 ? S1 Li3 Li3 107.4(4) 3_558 3_558 ? C1 Li3 Li3 85.0(4) 3_558 3_558 ? C2 Li3 Li2 143.6(4) . 3_558 ? C7 Li3 Li2 53.4(3) . 3_558 ? C2 Li3 Li2 106.1(4) 3_558 3_558 ? S1 Li3 Li2 58.5(2) 3_558 3_558 ? C1 Li3 Li2 74.8(3) 3_558 3_558 ? Li3 Li3 Li2 159.6(5) 3_558 3_558 ? C2 Li3 Li1 52.5(3) . . ? C7 Li3 Li1 67.7(3) . . ? C2 Li3 Li1 102.0(3) 3_558 . ? S1 Li3 Li1 170.8(4) 3_558 . ? C1 Li3 Li1 129.3(4) 3_558 . ? Li3 Li3 Li1 70.4(4) 3_558 . ? Li2 Li3 Li1 120.9(4) 3_558 . ? C2 Li3 Li1 94.0(3) . 3_558 ? C7 Li3 Li1 161.3(4) . 3_558 ? C2 Li3 Li1 46.3(2) 3_558 3_558 ? S1 Li3 Li1 51.9(2) 3_558 3_558 ? C1 Li3 Li1 50.6(2) 3_558 3_558 ? Li3 Li3 Li1 56.3(3) 3_558 3_558 ? Li2 Li3 Li1 110.2(3) 3_558 3_558 ? Li1 Li3 Li1 126.7(3) . 3_558 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.478 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.079 #------------------------------------------------------------------------------# # END OF DATA BLOCK # #------------------------------------------------------------------------------#