Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemsitry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Li, Jian-Feng' 'Liu, Dian-Sheng' 'Wei, Xue-Hong' 'Weng, Linhong' _publ_contact_author_name 'Prof Dian-Sheng Liu' _publ_contact_author_address ; Chemistry Shanxi University, Taiyuan, 030006, Taiyuan shanxi 030006 CHINA ; _publ_contact_author_email 'DSLIU@MAIL.SXU.EDU.CN' _publ_section_title ; Synthesis and structures of a novel chiral lithium amidinate and mono- and di- lithium (1R, 2R)-(-)-1,2-(NHSiMe3)2-cyclohexane ; data_compound3 _database_code_CSD 161938 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 Li4 N4 Si4' _chemical_formula_weight 540.85 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Trigonal' _symmetry_space_group_name_H-M 'P3(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 10.5111(14) _cell_length_b 10.5111(14) _cell_length_c 27.891(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2668.7(7) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 885 _cell_measurement_theta_min 2.672 _cell_measurement_theta_max 24.208 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9383 _exptl_absorpt_correction_T_max 0.9468 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.45 _diffrn_reflns_number 11141 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6280 _reflns_number_gt 5037 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0675P)^2^+1.7060P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ; DIFMAP & GEOM (H atoms of SiMe3 were located by geom and rest were found from difmap ; _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 -0.03(16) _refine_ls_number_reflns 6280 _refine_ls_number_parameters 405 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.4244(8) 0.0414(8) 0.7143(3) 0.0463(18) Uani 1 1 d . . . Li2 Li 0.2730(8) 0.1432(9) 0.6673(3) 0.0474(18) Uani 1 1 d . . . Li3 Li 0.1665(7) -0.0894(8) 0.7041(2) 0.0383(16) Uani 1 1 d . . . Li4 Li 0.3113(8) 0.1626(8) 0.7507(3) 0.0431(17) Uani 1 1 d . . . N1 N 0.4760(4) 0.2547(4) 0.69877(12) 0.0380(8) Uani 1 1 d . . . N2 N 0.3248(4) -0.0189(4) 0.64967(12) 0.0412(8) Uani 1 1 d . . . C1 C 0.5516(5) 0.2275(5) 0.65837(16) 0.0424(10) Uani 1 1 d . . . C2 C 0.6574(6) 0.3655(6) 0.62944(19) 0.0530(12) Uani 1 1 d . . . C3 C 0.7398(7) 0.3333(8) 0.5910(2) 0.0778(18) Uani 1 1 d . . . C4 C 0.6366(7) 0.2090(7) 0.55802(19) 0.0698(16) Uani 1 1 d . . . C5 C 0.5310(7) 0.0751(7) 0.58668(19) 0.0544(13) Uani 1 1 d . . . C6 C 0.4417(5) 0.1078(5) 0.62348(15) 0.0382(9) Uani 1 1 d . . . H1 H 0.620(6) 0.195(6) 0.6697(19) 0.063(15) Uiso 1 1 d . . . H2A H 0.606(5) 0.396(5) 0.6139(17) 0.038(13) Uiso 1 1 d . . . H2B H 0.708(5) 0.456(5) 0.6545(17) 0.050(13) Uiso 1 1 d . . . H3A H 0.805(5) 0.432(5) 0.5730(17) 0.045(12) Uiso 1 1 d . . . H3B H 0.829(5) 0.321(5) 0.6049(17) 0.047(13) Uiso 1 1 d . . . H4A H 0.701(6) 0.170(6) 0.534(2) 0.077(17) Uiso 1 1 d . . . H4B H 0.562(5) 0.242(5) 0.5385(17) 0.056(14) Uiso 1 1 d . . . H5A H 0.577(4) 0.028(4) 0.6038(12) 0.009(8) Uiso 1 1 d . . . H5B H 0.486(5) 0.013(5) 0.5686(16) 0.035(14) Uiso 1 1 d . . . H6 H 0.389(5) 0.154(5) 0.5962(15) 0.042(11) Uiso 1 1 d . . . Si1 Si 0.56683(15) 0.41166(14) 0.73132(5) 0.0480(3) Uani 1 1 d . . . C7 C 0.5900(9) 0.5830(7) 0.7040(3) 0.093(2) Uani 1 1 d . . . H7A H 0.6467 0.6040 0.6751 0.139 Uiso 1 1 calc R . . H7B H 0.6400 0.6629 0.7261 0.139 Uiso 1 1 calc R . . H7C H 0.4953 0.5707 0.6966 0.139 Uiso 1 1 calc R . . C8 C 0.4538(7) 0.3830(7) 0.7879(2) 0.0777(18) Uani 1 1 d . . . H8A H 0.4366 0.2946 0.8036 0.117 Uiso 1 1 calc R . . H8B H 0.3615 0.3749 0.7794 0.117 Uiso 1 1 calc R . . H8C H 0.5065 0.4651 0.8090 0.117 Uiso 1 1 calc R . . C9 C 0.7501(7) 0.4500(7) 0.7534(2) 0.0745(17) Uani 1 1 d . . . H9A H 0.8135 0.4658 0.7265 0.112 Uiso 1 1 calc R . . H9B H 0.7389 0.3677 0.7717 0.112 Uiso 1 1 calc R . . H9C H 0.7922 0.5361 0.7732 0.112 Uiso 1 1 calc R . . Si2 Si 0.22647(16) -0.18239(15) 0.62108(5) 0.0537(4) Uani 1 1 d . . . C10 C 0.3203(10) -0.2920(8) 0.6138(3) 0.101(2) Uani 1 1 d . . . H10A H 0.4059 -0.2388 0.5941 0.151 Uiso 1 1 calc R . . H10B H 0.2544 -0.3842 0.5989 0.151 Uiso 1 1 calc R . . H10C H 0.3489 -0.3094 0.6447 0.151 Uiso 1 1 calc R . . C11 C 0.1503(8) -0.1738(9) 0.5618(3) 0.097(2) Uani 1 1 d . . . H11A H 0.2294 -0.1149 0.5402 0.145 Uiso 1 1 calc R . . H11B H 0.0890 -0.1308 0.5655 0.145 Uiso 1 1 calc R . . H11C H 0.0932 -0.2712 0.5490 0.145 Uiso 1 1 calc R . . C12 C 0.0608(7) -0.3015(7) 0.6608(3) 0.086(2) Uani 1 1 d . . . H12A H 0.0941 -0.3101 0.6921 0.129 Uiso 1 1 calc R . . H12B H 0.0046 -0.3974 0.6468 0.129 Uiso 1 1 calc R . . H12C H 0.0006 -0.2570 0.6635 0.129 Uiso 1 1 calc R . . N3 N 0.1161(4) 0.0748(4) 0.71932(13) 0.0407(8) Uani 1 1 d . . . N4 N 0.2660(4) -0.0474(4) 0.76830(12) 0.0367(8) Uani 1 1 d . . . C13 C 0.0374(5) -0.0312(5) 0.75865(16) 0.0412(10) Uani 1 1 d . . . C14 C -0.0741(7) -0.0077(8) 0.7864(2) 0.0634(15) Uani 1 1 d . . . C15 C -0.1568(7) -0.1269(9) 0.8235(2) 0.0735(19) Uani 1 1 d . . . C16 C -0.0527(7) -0.1433(8) 0.8567(2) 0.0651(16) Uani 1 1 d . . . C17 C 0.0579(6) -0.1656(6) 0.82935(18) 0.0529(12) Uani 1 1 d . . . C18 C 0.1468(5) -0.0418(5) 0.79396(15) 0.0392(10) Uani 1 1 d . . . H13 H -0.020(5) -0.131(5) 0.7473(16) 0.042(12) Uiso 1 1 d . . . H14A H -0.046(8) 0.071(8) 0.801(3) 0.09(2) Uiso 1 1 d . . . H14B H -0.154(7) -0.024(6) 0.759(2) 0.078(17) Uiso 1 1 d . . . H15A H -0.235(6) -0.237(6) 0.8030(19) 0.062(14) Uiso 1 1 d . . . H15B H -0.203(6) -0.115(6) 0.838(2) 0.057(18) Uiso 1 1 d . . . H16A H 0.004(6) -0.055(7) 0.881(2) 0.086(19) Uiso 1 1 d . . . H16B H -0.097(5) -0.203(5) 0.8787(18) 0.041(13) Uiso 1 1 d . . . H17A H 0.130(4) -0.195(4) 0.8546(14) 0.032(10) Uiso 1 1 d . . . H17B H 0.014(4) -0.262(4) 0.8099(14) 0.025(9) Uiso 1 1 d . . . H18 H 0.196(4) 0.057(4) 0.8138(13) 0.022(9) Uiso 1 1 d . . . Si3 Si 0.02530(15) 0.14233(16) 0.68662(5) 0.0513(3) Uani 1 1 d . . . C19 C 0.1441(6) 0.2393(6) 0.6324(2) 0.0647(15) Uani 1 1 d . . . H19A H 0.1641 0.1723 0.6151 0.097 Uiso 1 1 calc R . . H19B H 0.2349 0.3220 0.6429 0.097 Uiso 1 1 calc R . . H19C H 0.0933 0.2726 0.6119 0.097 Uiso 1 1 calc R . . C20 C -0.1544(6) 0.0003(7) 0.6612(2) 0.0771(18) Uani 1 1 d . . . H20A H -0.1424 -0.0744 0.6455 0.116 Uiso 1 1 calc R . . H20B H -0.1881 0.0453 0.6384 0.116 Uiso 1 1 calc R . . H20C H -0.2251 -0.0431 0.6865 0.116 Uiso 1 1 calc R . . C21 C 0.2776(9) -0.3150(7) 0.8029(2) 0.090(2) Uani 1 1 d . . . H21A H 0.1901 -0.3518 0.8219 0.135 Uiso 1 1 calc R . . H21B H 0.3447 -0.3394 0.8180 0.135 Uiso 1 1 calc R . . H21C H 0.2528 -0.3585 0.7715 0.135 Uiso 1 1 calc R . . Si4 Si 0.36637(15) -0.10966(16) 0.79737(5) 0.0520(4) Uani 1 1 d . . . C22 C 0.4429(8) -0.0198(8) 0.8577(2) 0.087(2) Uani 1 1 d . . . H22A H 0.3633 -0.0426 0.8793 0.131 Uiso 1 1 calc R . . H22B H 0.5007 0.0847 0.8536 0.131 Uiso 1 1 calc R . . H22C H 0.5034 -0.0562 0.8705 0.131 Uiso 1 1 calc R . . C23 C 0.5357(7) -0.0562(9) 0.7587(2) 0.086(2) Uani 1 1 d . . . H23A H 0.5053 -0.0982 0.7273 0.129 Uiso 1 1 calc R . . H23B H 0.5943 -0.0924 0.7732 0.129 Uiso 1 1 calc R . . H23C H 0.5925 0.0488 0.7561 0.129 Uiso 1 1 calc R . . C26 C -0.0010(9) 0.2885(8) 0.7168(3) 0.095(2) Uani 1 1 d . . . H26A H -0.0611 0.2480 0.7448 0.142 Uiso 1 1 calc R . . H26B H -0.0481 0.3226 0.6950 0.142 Uiso 1 1 calc R . . H26C H 0.0929 0.3692 0.7260 0.142 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 Li1 0.049(4) 0.046(4) 0.048(4) 0.008(3) 0.003(4) 0.026(4) Li2 0.044(4) 0.053(5) 0.049(4) -0.006(4) -0.002(3) 0.027(4) Li3 0.036(4) 0.037(4) 0.035(4) -0.010(3) -0.002(3) 0.013(3) Li4 0.047(4) 0.040(4) 0.041(4) 0.001(3) 0.003(3) 0.021(3) N1 0.0347(19) 0.0352(19) 0.0358(19) 0.0017(15) 0.0077(15) 0.0113(16) N2 0.045(2) 0.041(2) 0.040(2) -0.0014(16) 0.0018(16) 0.0231(18) C1 0.036(2) 0.050(3) 0.042(2) 0.001(2) 0.0066(19) 0.022(2) C2 0.049(3) 0.055(3) 0.042(3) 0.009(2) 0.006(2) 0.016(3) C3 0.059(4) 0.092(5) 0.061(4) 0.013(3) 0.033(3) 0.023(4) C4 0.084(4) 0.093(5) 0.042(3) 0.011(3) 0.022(3) 0.052(4) C5 0.060(3) 0.066(4) 0.038(3) 0.001(3) 0.007(3) 0.032(3) C6 0.040(2) 0.044(2) 0.033(2) 0.0036(18) 0.0052(18) 0.023(2) Si1 0.0458(7) 0.0362(7) 0.0500(7) -0.0040(6) 0.0022(6) 0.0115(6) C7 0.110(6) 0.061(4) 0.098(5) 0.010(4) -0.002(4) 0.036(4) C8 0.075(4) 0.064(4) 0.084(4) -0.039(3) -0.001(3) 0.026(3) C9 0.066(4) 0.072(4) 0.059(3) -0.007(3) 0.000(3) 0.014(3) Si2 0.0588(9) 0.0496(8) 0.0499(8) -0.0125(6) 0.0000(6) 0.0249(7) C10 0.147(7) 0.072(4) 0.112(6) -0.005(4) 0.011(5) 0.076(5) C11 0.093(5) 0.104(5) 0.084(5) -0.033(4) -0.034(4) 0.041(4) C12 0.062(4) 0.056(4) 0.102(5) -0.017(3) 0.013(3) 0.001(3) N3 0.0351(19) 0.046(2) 0.044(2) 0.0049(17) 0.0028(16) 0.0226(17) N4 0.0329(18) 0.041(2) 0.0355(19) 0.0071(15) 0.0014(15) 0.0182(16) C13 0.033(2) 0.044(3) 0.040(2) -0.003(2) 0.0060(18) 0.014(2) C14 0.051(3) 0.090(5) 0.054(3) 0.002(3) 0.007(3) 0.040(3) C15 0.051(3) 0.110(5) 0.059(4) 0.001(3) 0.025(3) 0.040(4) C16 0.070(4) 0.074(4) 0.048(3) 0.010(3) 0.024(3) 0.033(3) C17 0.048(3) 0.053(3) 0.048(3) 0.011(2) 0.010(2) 0.018(2) C18 0.038(2) 0.037(2) 0.035(2) -0.0011(18) 0.0023(18) 0.0134(19) Si3 0.0456(8) 0.0576(8) 0.0597(8) 0.0074(7) 0.0005(6) 0.0325(7) C19 0.050(3) 0.065(3) 0.075(4) 0.026(3) -0.005(3) 0.026(3) C20 0.049(3) 0.090(5) 0.077(4) 0.023(4) -0.005(3) 0.023(3) C21 0.136(6) 0.074(4) 0.083(5) 0.019(4) 0.005(4) 0.070(5) Si4 0.0505(8) 0.0597(9) 0.0513(8) 0.0155(7) -0.0009(6) 0.0315(7) C22 0.089(5) 0.083(5) 0.060(4) 0.005(3) -0.018(3) 0.021(4) C23 0.076(4) 0.136(6) 0.087(4) 0.030(4) 0.010(3) 0.084(4) C26 0.116(6) 0.093(5) 0.119(6) 0.002(4) -0.002(5) 0.085(5) _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 N2 2.021(9) . ? Li1 N1 2.072(8) . ? Li1 N4 2.087(8) . ? Li1 C23 2.271(9) . ? Li1 C1 2.330(9) . ? Li1 Li4 2.362(11) . ? Li1 Li3 2.365(10) . ? Li1 C6 2.609(8) . ? Li1 Li2 2.664(11) . ? Li1 Si4 2.701(8) . ? Li2 N3 2.039(9) . ? Li2 N1 2.048(8) . ? Li2 N2 2.090(8) . ? Li2 C19 2.273(9) . ? Li2 C6 2.331(8) . ? Li2 Li4 2.354(10) . ? Li2 Li3 2.355(11) . ? Li2 C1 2.613(9) . ? Li2 Si3 2.654(8) . ? Li3 N4 2.009(7) . ? Li3 N3 2.087(8) . ? Li3 N2 2.094(8) . ? Li3 C12 2.277(9) . ? Li3 C13 2.317(8) . ? Li3 C18 2.585(8) . ? Li3 Li4 2.645(10) . ? Li3 Si2 2.706(7) . ? Li4 N3 1.984(8) . ? Li4 N4 2.071(8) . ? Li4 N1 2.087(8) . ? Li4 C8 2.283(9) . ? Li4 C18 2.312(8) . ? Li4 C13 2.574(9) . ? Li4 Si1 2.707(7) . ? N1 C1 1.487(5) . ? N1 Si1 1.698(4) . ? N2 C6 1.477(5) . ? N2 Si2 1.698(4) . ? C1 C2 1.543(7) . ? C1 C6 1.552(6) . ? C2 C3 1.519(8) . ? C3 C4 1.521(10) . ? C4 C5 1.513(8) . ? C5 C6 1.542(7) . ? Si1 C7 1.856(6) . ? Si1 C9 1.865(6) . ? Si1 C8 1.906(6) . ? Si2 C11 1.859(7) . ? Si2 C10 1.865(7) . ? Si2 C12 1.910(6) . ? N3 C13 1.486(6) . ? N3 Si3 1.710(4) . ? N4 C18 1.469(5) . ? N4 Si4 1.700(4) . ? C13 C14 1.524(7) . ? C13 C18 1.560(6) . ? C14 C15 1.520(9) . ? C15 C16 1.508(9) . ? C16 C17 1.504(8) . ? C17 C18 1.525(6) . ? Si3 C20 1.866(6) . ? Si3 C26 1.890(6) . ? Si3 C19 1.900(6) . ? C21 Si4 1.881(6) . ? Si4 C22 1.899(6) . ? Si4 C23 1.910(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 N2 Li1 N1 88.1(3) . . ? N2 Li1 N4 109.3(4) . . ? N1 Li1 N4 110.7(4) . . ? N2 Li1 C23 130.4(4) . . ? N1 Li1 C23 133.5(4) . . ? N4 Li1 C23 83.1(3) . . ? N2 Li1 C1 69.9(3) . . ? N1 Li1 C1 38.94(19) . . ? N4 Li1 C1 148.5(4) . . ? C23 Li1 C1 122.3(4) . . ? N2 Li1 Li4 103.4(4) . . ? N1 Li1 Li4 55.7(3) . . ? N4 Li1 Li4 55.0(3) . . ? C23 Li1 Li4 121.4(4) . . ? C1 Li1 Li4 93.9(3) . . ? N2 Li1 Li3 56.4(3) . . ? N1 Li1 Li3 102.0(4) . . ? N4 Li1 Li3 53.2(3) . . ? C23 Li1 Li3 120.2(4) . . ? C1 Li1 Li3 114.7(4) . . ? Li4 Li1 Li3 68.1(3) . . ? N2 Li1 C6 34.30(18) . . ? N1 Li1 C6 64.0(2) . . ? N4 Li1 C6 138.9(4) . . ? C23 Li1 C6 131.9(4) . . ? C1 Li1 C6 36.08(18) . . ? Li4 Li1 C6 105.1(3) . . ? Li3 Li1 C6 86.8(3) . . ? N2 Li1 Li2 50.7(2) . . ? N1 Li1 Li2 49.3(2) . . ? N4 Li1 Li2 91.8(3) . . ? C23 Li1 Li2 174.9(4) . . ? C1 Li1 Li2 62.7(3) . . ? Li4 Li1 Li2 55.5(3) . . ? Li3 Li1 Li2 55.5(3) . . ? C6 Li1 Li2 52.4(2) . . ? N2 Li1 Si4 130.7(4) . . ? N1 Li1 Si4 132.5(4) . . ? N4 Li1 Si4 39.01(16) . . ? C23 Li1 Si4 44.1(2) . . ? C1 Li1 Si4 159.0(4) . . ? Li4 Li1 Si4 85.5(3) . . ? Li3 Li1 Si4 84.6(3) . . ? C6 Li1 Si4 162.8(3) . . ? Li2 Li1 Si4 130.8(3) . . ? N3 Li2 N1 108.9(4) . . ? N3 Li2 N2 112.0(4) . . ? N1 Li2 N2 86.9(3) . . ? N3 Li2 C19 84.5(3) . . ? N1 Li2 C19 127.6(4) . . ? N2 Li2 C19 135.9(4) . . ? N3 Li2 C6 149.6(4) . . ? N1 Li2 C6 70.0(3) . . ? N2 Li2 C6 38.54(19) . . ? C19 Li2 C6 121.1(4) . . ? N3 Li2 Li4 53.1(3) . . ? N1 Li2 Li4 56.1(3) . . ? N2 Li2 Li4 101.5(4) . . ? C19 Li2 Li4 119.9(4) . . ? C6 Li2 Li4 114.9(4) . . ? N3 Li2 Li3 56.1(3) . . ? N1 Li2 Li3 103.0(4) . . ? N2 Li2 Li3 55.8(3) . . ? C19 Li2 Li3 124.6(4) . . ? C6 Li2 Li3 93.8(3) . . ? Li4 Li2 Li3 68.3(3) . . ? N3 Li2 C1 139.3(4) . . ? N1 Li2 C1 34.60(18) . . ? N2 Li2 C1 63.2(2) . . ? C19 Li2 C1 128.7(4) . . ? C6 Li2 C1 36.03(18) . . ? Li4 Li2 C1 87.2(3) . . ? Li3 Li2 C1 105.3(3) . . ? N3 Li2 Si3 40.11(17) . . ? N1 Li2 Si3 130.8(3) . . ? N2 Li2 Si3 134.4(4) . . ? C19 Li2 Si3 44.54(19) . . ? C6 Li2 Si3 158.3(4) . . ? Li4 Li2 Si3 85.7(3) . . ? Li3 Li2 Si3 87.2(3) . . ? C1 Li2 Si3 162.1(3) . . ? N3 Li2 Li1 92.7(3) . . ? N1 Li2 Li1 50.1(3) . . ? N2 Li2 Li1 48.5(3) . . ? C19 Li2 Li1 175.6(4) . . ? C6 Li2 Li1 62.6(3) . . ? Li4 Li2 Li1 55.8(3) . . ? Li3 Li2 Li1 55.8(3) . . ? C1 Li2 Li1 52.4(2) . . ? Si3 Li2 Li1 132.8(4) . . ? N4 Li3 N3 87.5(3) . . ? N4 Li3 N2 109.5(3) . . ? N3 Li3 N2 109.9(4) . . ? N4 Li3 C12 129.3(4) . . ? N3 Li3 C12 135.8(4) . . ? N2 Li3 C12 82.8(3) . . ? N4 Li3 C13 70.4(2) . . ? N3 Li3 C13 39.00(19) . . ? N2 Li3 C13 148.1(4) . . ? C12 Li3 C13 122.9(4) . . ? N4 Li3 Li2 103.6(3) . . ? N3 Li3 Li2 54.2(3) . . ? N2 Li3 Li2 55.7(3) . . ? C12 Li3 Li2 122.1(4) . . ? C13 Li3 Li2 92.8(3) . . ? N4 Li3 Li1 56.3(3) . . ? N3 Li3 Li1 100.7(3) . . ? N2 Li3 Li1 53.5(3) . . ? C12 Li3 Li1 119.3(4) . . ? C13 Li3 Li1 114.8(3) . . ? Li2 Li3 Li1 68.7(3) . . ? N4 Li3 C18 34.50(17) . . ? N3 Li3 C18 64.2(2) . . ? N2 Li3 C18 139.5(3) . . ? C12 Li3 C18 131.0(4) . . ? C13 Li3 C18 36.60(17) . . ? Li2 Li3 C18 105.3(3) . . ? Li1 Li3 C18 87.1(3) . . ? N4 Li3 Li4 50.6(2) . . ? N3 Li3 Li4 47.8(2) . . ? N2 Li3 Li4 92.5(3) . . ? C12 Li3 Li4 175.0(4) . . ? C13 Li3 Li4 62.1(3) . . ? Li2 Li3 Li4 55.8(3) . . ? Li1 Li3 Li4 55.9(3) . . ? C18 Li3 Li4 52.5(2) . . ? N4 Li3 Si2 130.7(3) . . ? N3 Li3 Si2 132.4(3) . . ? N2 Li3 Si2 38.84(15) . . ? C12 Li3 Si2 44.02(19) . . ? C13 Li3 Si2 158.5(3) . . ? Li2 Li3 Si2 85.8(3) . . ? Li1 Li3 Si2 84.7(3) . . ? C18 Li3 Si2 162.7(3) . . ? Li4 Li3 Si2 131.4(3) . . ? N3 Li4 N4 88.6(3) . . ? N3 Li4 N1 109.5(4) . . ? N4 Li4 N1 110.7(4) . . ? N3 Li4 C8 132.4(4) . . ? N4 Li4 C8 131.2(4) . . ? N1 Li4 C8 82.7(3) . . ? N3 Li4 C18 71.3(3) . . ? N4 Li4 C18 38.68(19) . . ? N1 Li4 C18 148.7(4) . . ? C8 Li4 C18 120.8(4) . . ? N3 Li4 Li2 55.3(3) . . ? N4 Li4 Li2 101.7(4) . . ? N1 Li4 Li2 54.5(3) . . ? C8 Li4 Li2 122.3(4) . . ? C18 Li4 Li2 114.8(4) . . ? N3 Li4 Li1 104.0(4) . . ? N4 Li4 Li1 55.7(3) . . ? N1 Li4 Li1 55.1(3) . . ? C8 Li4 Li1 119.4(4) . . ? C18 Li4 Li1 93.9(3) . . ? Li2 Li4 Li1 68.8(3) . . ? N3 Li4 C13 35.12(19) . . ? N4 Li4 C13 64.3(2) . . ? N1 Li4 C13 140.1(4) . . ? C8 Li4 C13 132.1(4) . . ? C18 Li4 C13 36.75(19) . . ? Li2 Li4 C13 86.6(3) . . ? Li1 Li4 C13 106.0(3) . . ? N3 Li4 Li3 51.2(2) . . ? N4 Li4 Li3 48.6(2) . . ? N1 Li4 Li3 92.9(3) . . ? C8 Li4 Li3 175.2(4) . . ? C18 Li4 Li3 62.4(3) . . ? Li2 Li4 Li3 55.9(3) . . ? Li1 Li4 Li3 56.0(3) . . ? C13 Li4 Li3 52.7(2) . . ? N3 Li4 Si1 131.1(3) . . ? N4 Li4 Si1 131.8(3) . . ? N1 Li4 Si1 38.83(16) . . ? C8 Li4 Si1 43.9(2) . . ? C18 Li4 Si1 157.3(3) . . ? Li2 Li4 Si1 86.0(3) . . ? Li1 Li4 Si1 85.0(3) . . ? C13 Li4 Si1 163.5(3) . . ? Li3 Li4 Si1 131.8(3) . . ? C1 N1 Si1 119.8(3) . . ? C1 N1 Li2 94.0(3) . . ? Si1 N1 Li2 134.8(3) . . ? C1 N1 Li1 80.0(3) . . ? Si1 N1 Li1 130.9(3) . . ? Li2 N1 Li1 80.6(3) . . ? C1 N1 Li4 146.7(4) . . ? Si1 N1 Li4 90.7(2) . . ? Li2 N1 Li4 69.4(3) . . ? Li1 N1 Li4 69.2(3) . . ? C6 N2 Si2 119.5(3) . . ? C6 N2 Li1 95.2(3) . . ? Si2 N2 Li1 134.0(3) . . ? C6 N2 Li2 79.6(3) . . ? Si2 N2 Li2 131.4(3) . . ? Li1 N2 Li2 80.8(3) . . ? C6 N2 Li3 146.4(3) . . ? Si2 N2 Li3 90.5(2) . . ? Li1 N2 Li3 70.1(3) . . ? Li2 N2 Li3 68.5(3) . . ? N1 C1 C2 114.7(4) . . ? N1 C1 C6 112.2(3) . . ? C2 C1 C6 109.2(4) . . ? N1 C1 Li1 61.1(3) . . ? C2 C1 Li1 168.8(4) . . ? C6 C1 Li1 81.8(3) . . ? N1 C1 Li2 51.5(3) . . ? C2 C1 Li2 121.8(4) . . ? C6 C1 Li2 62.0(3) . . ? Li1 C1 Li2 64.9(3) . . ? C3 C2 C1 112.5(5) . . ? C2 C3 C4 112.1(5) . . ? C5 C4 C3 110.8(5) . . ? C4 C5 C6 112.9(5) . . ? N2 C6 C5 116.9(4) . . ? N2 C6 C1 111.5(3) . . ? C5 C6 C1 108.0(4) . . ? N2 C6 Li2 61.9(3) . . ? C5 C6 Li2 168.9(4) . . ? C1 C6 Li2 81.9(3) . . ? N2 C6 Li1 50.5(3) . . ? C5 C6 Li1 123.8(4) . . ? C1 C6 Li1 62.1(3) . . ? Li2 C6 Li1 65.0(3) . . ? N1 Si1 C7 117.4(3) . . ? N1 Si1 C9 113.9(2) . . ? C7 Si1 C9 107.8(3) . . ? N1 Si1 C8 106.6(2) . . ? C7 Si1 C8 105.2(3) . . ? C9 Si1 C8 104.8(3) . . ? N1 Si1 Li4 50.44(19) . . ? C7 Si1 Li4 127.3(3) . . ? C9 Si1 Li4 124.1(3) . . ? C8 Si1 Li4 56.2(2) . . ? Si1 C8 Li4 80.0(3) . . ? N2 Si2 C11 115.3(3) . . ? N2 Si2 C10 115.7(3) . . ? C11 Si2 C10 107.9(4) . . ? N2 Si2 C12 106.6(2) . . ? C11 Si2 C12 105.9(4) . . ? C10 Si2 C12 104.4(4) . . ? N2 Si2 Li3 50.69(19) . . ? C11 Si2 Li3 124.0(3) . . ? C10 Si2 Li3 127.3(3) . . ? C12 Si2 Li3 56.0(2) . . ? Si2 C12 Li3 80.0(3) . . ? C13 N3 Si3 119.2(3) . . ? C13 N3 Li4 94.7(3) . . ? Si3 N3 Li4 134.8(3) . . ? C13 N3 Li2 147.1(4) . . ? Si3 N3 Li2 89.7(3) . . ? Li4 N3 Li2 71.6(3) . . ? C13 N3 Li3 78.9(3) . . ? Si3 N3 Li3 131.3(3) . . ? Li4 N3 Li3 81.0(3) . . ? Li2 N3 Li3 69.6(3) . . ? C18 N4 Si4 119.2(3) . . ? C18 N4 Li3 94.7(3) . . ? Si4 N4 Li3 134.1(3) . . ? C18 N4 Li4 79.6(3) . . ? Si4 N4 Li4 131.9(3) . . ? Li3 N4 Li4 80.8(3) . . ? C18 N4 Li1 147.0(3) . . ? Si4 N4 Li1 90.4(3) . . ? Li3 N4 Li1 70.5(3) . . ? Li4 N4 Li1 69.2(3) . . ? N3 C13 C14 116.0(4) . . ? N3 C13 C18 111.4(3) . . ? C14 C13 C18 110.2(4) . . ? N3 C13 Li3 62.1(3) . . ? C14 C13 Li3 167.5(4) . . ? C18 C13 Li3 81.1(3) . . ? N3 C13 Li4 50.2(2) . . ? C14 C13 Li4 124.2(4) . . ? C18 C13 Li4 62.5(3) . . ? Li3 C13 Li4 65.2(3) . . ? C15 C14 C13 112.5(5) . . ? C16 C15 C14 111.4(5) . . ? C17 C16 C15 111.6(5) . . ? C16 C17 C18 112.8(5) . . ? N4 C18 C17 116.9(4) . . ? N4 C18 C13 111.7(3) . . ? C17 C18 C13 108.1(4) . . ? N4 C18 Li4 61.7(3) . . ? C17 C18 Li4 170.1(4) . . ? C13 C18 Li4 80.8(3) . . ? N4 C18 Li3 50.8(2) . . ? C17 C18 Li3 122.5(3) . . ? C13 C18 Li3 62.3(3) . . ? Li4 C18 Li3 65.1(3) . . ? N3 Si3 C20 115.0(2) . . ? N3 Si3 C26 116.0(3) . . ? C20 Si3 C26 108.6(3) . . ? N3 Si3 C19 107.1(2) . . ? C20 Si3 C19 104.9(3) . . ? C26 Si3 C19 104.0(3) . . ? N3 Si3 Li2 50.2(2) . . ? C20 Si3 Li2 121.6(3) . . ? C26 Si3 Li2 129.0(3) . . ? C19 Si3 Li2 57.0(2) . . ? Si3 C19 Li2 78.4(3) . . ? N4 Si4 C21 115.7(3) . . ? N4 Si4 C22 114.9(3) . . ? C21 Si4 C22 110.0(3) . . ? N4 Si4 C23 106.5(2) . . ? C21 Si4 C23 103.8(3) . . ? C22 Si4 C23 104.7(3) . . ? N4 Si4 Li1 50.6(2) . . ? C21 Si4 Li1 125.5(3) . . ? C22 Si4 Li1 123.5(3) . . ? C23 Si4 Li1 55.9(2) . . ? Si4 C23 Li1 80.0(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.222 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.049 # === END data_compound2 _database_code_CSD 161939 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H54 Li2 N4 Si4' _chemical_formula_weight 524.95 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 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.778(3) _cell_length_b 18.113(5) _cell_length_c 10.387(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.643(5) _cell_angle_gamma 90.00 _cell_volume 1787.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 892 _cell_measurement_theta_min 2.425 _cell_measurement_theta_max 20.075 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9062 _exptl_absorpt_correction_T_max 0.9855 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.97 _diffrn_reflns_number 8423 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.39 _reflns_number_total 6875 _reflns_number_gt 3748 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0804P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0030(13) _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 -0.09(14) _refine_ls_number_reflns 6875 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.7834(7) 0.8663(4) 0.3968(7) 0.0650(18) Uani 1 1 d . . . Li2 Li 0.8471(7) 0.7536(4) 0.3123(6) 0.0654(17) Uani 1 1 d . . . N1 N 0.8677(3) 0.77769(17) 0.5024(3) 0.0542(8) Uani 1 1 d . . . N2 N 0.6986(4) 0.9019(2) 0.5484(4) 0.0631(9) Uani 1 1 d . . . N3 N 0.7523(4) 0.84079(18) 0.2067(3) 0.0619(9) Uani 1 1 d . . . N4 N 0.7706(4) 0.6868(2) 0.1441(4) 0.0668(10) Uani 1 1 d . . . C1 C 0.7796(4) 0.7731(2) 0.5993(4) 0.0556(9) Uani 1 1 d . . . C2 C 0.7230(5) 0.6941(2) 0.6089(4) 0.0688(12) Uani 1 1 d . . . H2A H 0.6639 0.6800 0.5237 0.083 Uiso 1 1 calc R . . H2B H 0.8014 0.6599 0.6301 0.083 Uiso 1 1 calc R . . C3 C 0.6391(5) 0.6886(3) 0.7131(5) 0.0845(14) Uani 1 1 d . . . H3A H 0.6049 0.6385 0.7158 0.101 Uiso 1 1 calc R . . H3B H 0.6996 0.6998 0.7992 0.101 Uiso 1 1 calc R . . C4 C 0.5166(5) 0.7411(3) 0.6849(5) 0.0914(16) Uani 1 1 d . . . H4A H 0.4677 0.7386 0.7558 0.110 Uiso 1 1 calc R . . H4B H 0.4511 0.7269 0.6031 0.110 Uiso 1 1 calc R . . C5 C 0.5672(5) 0.8195(3) 0.6727(5) 0.0783(14) Uani 1 1 d . . . H5A H 0.6259 0.8349 0.7573 0.094 Uiso 1 1 calc R . . H5B H 0.4866 0.8523 0.6511 0.094 Uiso 1 1 calc R . . C6 C 0.6507(4) 0.8261(2) 0.5665(4) 0.0559(10) Uani 1 1 d . . . C7 C 1.1210(6) 0.8571(3) 0.6603(6) 0.0982(17) Uani 1 1 d . . . H7A H 1.1828 0.8433 0.7431 0.147 Uiso 1 1 calc R . . H7B H 1.0466 0.8876 0.6767 0.147 Uiso 1 1 calc R . . H7C H 1.1730 0.8839 0.6080 0.147 Uiso 1 1 calc R . . C8 C 1.0997(5) 0.6957(3) 0.6902(5) 0.0916(16) Uani 1 1 d . . . H8A H 1.1640 0.7144 0.7679 0.137 Uiso 1 1 calc R . . H8B H 1.1453 0.6578 0.6508 0.137 Uiso 1 1 calc R . . H8C H 1.0186 0.6754 0.7144 0.137 Uiso 1 1 calc R . . C9 C 1.1326(4) 0.7577(3) 0.4286(4) 0.0904(15) Uani 1 1 d . . . H9A H 1.2329 0.7589 0.4621 0.136 Uiso 1 1 calc R . . H9B H 1.1049 0.7962 0.3642 0.136 Uiso 1 1 calc R . . H9C H 1.1053 0.7107 0.3879 0.136 Uiso 1 1 calc R . . C10 C 0.5683(8) 1.0257(5) 0.6768(7) 0.163(3) Uani 1 1 d . . . H10A H 0.6587 1.0387 0.7315 0.244 Uiso 1 1 calc R . . H10B H 0.5221 0.9919 0.7238 0.244 Uiso 1 1 calc R . . H10C H 0.5120 1.0694 0.6551 0.244 Uiso 1 1 calc R . . C11 C 0.4148(5) 0.9569(3) 0.4140(5) 0.0961(17) Uani 1 1 d . . . H11A H 0.3700 0.9213 0.4589 0.144 Uiso 1 1 calc R . . H11B H 0.4258 0.9365 0.3318 0.144 Uiso 1 1 calc R . . H11C H 0.3577 1.0006 0.3967 0.144 Uiso 1 1 calc R . . C12 C 0.6881(8) 1.0485(4) 0.4425(11) 0.189(4) Uani 1 1 d . . . H12A H 0.7776 1.0588 0.5012 0.284 Uiso 1 1 calc R . . H12B H 0.6344 1.0933 0.4245 0.284 Uiso 1 1 calc R . . H12C H 0.7023 1.0285 0.3611 0.284 Uiso 1 1 calc R . . C13 C 0.6313(4) 0.8022(2) 0.1227(4) 0.0618(11) Uani 1 1 d . . . C14 C 0.4908(5) 0.8347(3) 0.1374(5) 0.0782(14) Uani 1 1 d . . . H14A H 0.4868 0.8864 0.1129 0.094 Uiso 1 1 calc R . . H14B H 0.4864 0.8316 0.2295 0.094 Uiso 1 1 calc R . . C15 C 0.3630(5) 0.7947(4) 0.0515(6) 0.1046(18) Uani 1 1 d . . . H15A H 0.2772 0.8152 0.0683 0.125 Uiso 1 1 calc R . . H15B H 0.3610 0.8021 -0.0414 0.125 Uiso 1 1 calc R . . C16 C 0.3702(5) 0.7139(4) 0.0823(6) 0.0990(18) Uani 1 1 d . . . H16A H 0.2915 0.6892 0.0236 0.119 Uiso 1 1 calc R . . H16B H 0.3612 0.7067 0.1724 0.119 Uiso 1 1 calc R . . C17 C 0.5062(5) 0.6786(3) 0.0670(4) 0.0768(13) Uani 1 1 d . . . H17A H 0.5116 0.6812 -0.0249 0.092 Uiso 1 1 calc R . . H17B H 0.5075 0.6269 0.0920 0.092 Uiso 1 1 calc R . . C18 C 0.6354(4) 0.7187(2) 0.1557(4) 0.0588(11) Uani 1 1 d . . . C19 C 0.7178(7) 0.9758(4) 0.0370(8) 0.153(3) Uani 1 1 d . . . H19A H 0.7429 0.9845 -0.0457 0.229 Uiso 1 1 calc R . . H19B H 0.7270 1.0208 0.0870 0.229 Uiso 1 1 calc R . . H19C H 0.6222 0.9588 0.0201 0.229 Uiso 1 1 calc R . . C20 C 0.9329(7) 0.8615(4) 0.0141(7) 0.146(3) Uani 1 1 d . . . H20A H 0.9244 0.8933 -0.0612 0.219 Uiso 1 1 calc R . . H20B H 0.8922 0.8143 -0.0146 0.219 Uiso 1 1 calc R . . H20C H 1.0305 0.8553 0.0569 0.219 Uiso 1 1 calc R . . C21 C 0.9730(6) 0.9512(3) 0.2664(6) 0.116(2) Uani 1 1 d . . . H21A H 1.0351 0.9794 0.2263 0.174 Uiso 1 1 calc R . . H21B H 1.0262 0.9150 0.3249 0.174 Uiso 1 1 calc R . . H21C H 0.9267 0.9836 0.3157 0.174 Uiso 1 1 calc R . . C22 C 1.0071(7) 0.5997(4) 0.1283(9) 0.163(3) Uani 1 1 d . . . H22A H 1.0637 0.6350 0.1864 0.244 Uiso 1 1 calc R . . H22B H 1.0003 0.6139 0.0379 0.244 Uiso 1 1 calc R . . H22C H 1.0497 0.5518 0.1438 0.244 Uiso 1 1 calc R . . C23 C 0.7242(7) 0.5274(3) 0.0458(7) 0.136(3) Uani 1 1 d . . . H23A H 0.6321 0.5234 0.0629 0.204 Uiso 1 1 calc R . . H23B H 0.7703 0.4803 0.0598 0.204 Uiso 1 1 calc R . . H23C H 0.7158 0.5427 -0.0442 0.204 Uiso 1 1 calc R . . C24 C 0.8373(8) 0.5704(3) 0.3343(6) 0.138(3) Uani 1 1 d . . . H24A H 0.7435 0.5678 0.3477 0.207 Uiso 1 1 calc R . . H24B H 0.8902 0.6067 0.3929 0.207 Uiso 1 1 calc R . . H24C H 0.8821 0.5232 0.3525 0.207 Uiso 1 1 calc R . . Si1 Si 1.04405(11) 0.77214(6) 0.56911(11) 0.0614(3) Uani 1 1 d . . . Si2 Si 0.59194(15) 0.98114(7) 0.52065(15) 0.0810(4) Uani 1 1 d . . . Si3 Si 0.83780(16) 0.90362(8) 0.13370(14) 0.0833(4) Uani 1 1 d . . . Si4 Si 0.82952(16) 0.59680(8) 0.16034(15) 0.0876(5) Uani 1 1 d . . . H2 H 0.765(5) 0.914(3) 0.605(4) 0.073(16) Uiso 1 1 d . . . H4 H 0.802(5) 0.707(3) 0.090(5) 0.079(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.072(5) 0.049(4) 0.075(5) 0.005(3) 0.018(4) 0.007(3) Li2 0.068(4) 0.062(4) 0.066(4) -0.001(4) 0.016(3) 0.011(4) N1 0.0531(18) 0.0510(19) 0.0588(18) 0.0061(15) 0.0139(15) 0.0030(16) N2 0.055(2) 0.056(2) 0.076(2) -0.0073(19) 0.011(2) 0.0031(19) N3 0.062(2) 0.058(2) 0.064(2) 0.0060(16) 0.0104(18) 0.0045(18) N4 0.067(2) 0.067(2) 0.070(3) -0.006(2) 0.023(2) 0.000(2) C1 0.054(2) 0.050(2) 0.063(2) 0.0075(19) 0.0143(18) 0.000(2) C2 0.076(3) 0.062(3) 0.066(3) 0.009(2) 0.012(2) -0.007(2) C3 0.084(3) 0.084(3) 0.081(3) 0.021(3) 0.011(3) -0.014(3) C4 0.070(3) 0.117(4) 0.093(4) 0.024(3) 0.029(3) -0.007(3) C5 0.064(3) 0.099(4) 0.076(3) 0.010(3) 0.023(3) 0.010(3) C6 0.049(2) 0.058(3) 0.062(3) 0.0005(19) 0.018(2) 0.0005(19) C7 0.082(4) 0.088(4) 0.118(4) -0.022(3) 0.009(3) -0.013(3) C8 0.069(3) 0.103(4) 0.094(4) 0.021(3) 0.002(3) 0.021(3) C9 0.066(3) 0.116(4) 0.090(3) 0.003(3) 0.019(2) 0.016(3) C10 0.157(7) 0.160(7) 0.151(6) -0.054(5) -0.004(5) 0.079(6) C11 0.082(3) 0.083(4) 0.113(4) -0.005(3) 0.001(3) 0.026(3) C12 0.125(6) 0.070(4) 0.383(13) 0.077(6) 0.080(7) 0.032(4) C13 0.057(3) 0.063(3) 0.065(3) 0.007(2) 0.012(2) 0.005(2) C14 0.077(3) 0.083(3) 0.072(3) 0.008(2) 0.012(3) 0.026(3) C15 0.059(3) 0.138(6) 0.107(4) 0.016(4) 0.001(3) 0.013(3) C16 0.063(3) 0.123(5) 0.108(4) 0.007(4) 0.014(3) -0.007(3) C17 0.067(3) 0.088(3) 0.073(3) 0.018(3) 0.012(2) -0.011(3) C18 0.048(2) 0.063(3) 0.066(3) 0.005(2) 0.015(2) 0.003(2) C19 0.140(6) 0.132(6) 0.177(7) 0.101(5) 0.019(5) -0.012(5) C20 0.129(6) 0.193(8) 0.138(6) -0.006(5) 0.077(5) -0.049(5) C21 0.116(5) 0.096(4) 0.129(5) 0.002(4) 0.015(4) -0.033(4) C22 0.086(4) 0.163(7) 0.246(8) -0.090(6) 0.053(5) 0.018(4) C23 0.136(6) 0.090(5) 0.168(6) -0.054(4) 0.009(5) 0.004(4) C24 0.213(8) 0.071(4) 0.126(5) 0.018(3) 0.032(5) 0.021(4) Si1 0.0532(7) 0.0605(8) 0.0669(7) -0.0004(6) 0.0073(5) 0.0057(6) Si2 0.0694(8) 0.0619(8) 0.1092(11) -0.0086(8) 0.0164(8) 0.0150(7) Si3 0.0818(10) 0.0871(10) 0.0798(9) 0.0225(7) 0.0165(7) -0.0108(8) Si4 0.0861(10) 0.0704(10) 0.1050(11) -0.0221(8) 0.0197(8) 0.0089(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N3 1.980(8) . ? Li1 N1 2.008(7) . ? Li1 N2 2.050(8) . ? Li1 Li2 2.363(10) . ? Li1 C6 2.530(8) . ? Li1 C1 2.705(8) . ? Li1 Si3 2.982(7) . ? Li2 N1 1.985(7) . ? Li2 N3 2.019(8) . ? Li2 N4 2.112(8) . ? Li2 C18 2.397(8) . ? Li2 C13 2.673(7) . ? Li2 C9 2.769(8) . ? Li2 Si1 2.918(6) . ? N1 C1 1.474(4) . ? N1 Si1 1.703(3) . ? N2 C6 1.477(5) . ? N2 Si2 1.757(4) . ? N3 C13 1.470(5) . ? N3 Si3 1.694(4) . ? N4 C18 1.474(5) . ? N4 Si4 1.724(4) . ? C1 C2 1.545(6) . ? C1 C6 1.556(5) . ? C2 C3 1.508(6) . ? C3 C4 1.503(7) . ? C4 C5 1.519(7) . ? C5 C6 1.525(6) . ? C7 Si1 1.869(5) . ? C8 Si1 1.864(5) . ? C9 Si1 1.883(5) . ? C10 Si2 1.874(7) . ? C11 Si2 1.875(5) . ? C12 Si2 1.841(7) . ? C13 C14 1.534(6) . ? C13 C18 1.550(6) . ? C14 C15 1.535(7) . ? C15 C16 1.496(7) . ? C16 C17 1.517(7) . ? C17 C18 1.556(6) . ? C19 Si3 1.881(6) . ? C20 Si3 1.880(7) . ? C21 Si3 1.879(6) . ? C22 Si4 1.844(6) . ? C23 Si4 1.865(6) . ? C24 Si4 1.853(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 N3 Li1 N1 107.7(3) . . ? N3 Li1 N2 147.6(4) . . ? N1 Li1 N2 91.2(3) . . ? N3 Li1 Li2 54.5(2) . . ? N1 Li1 Li2 53.3(2) . . ? N2 Li1 Li2 138.3(4) . . ? N3 Li1 C6 130.1(4) . . ? N1 Li1 C6 66.5(2) . . ? N2 Li1 C6 35.72(18) . . ? Li2 Li1 C6 103.5(3) . . ? N3 Li1 C1 127.0(3) . . ? N1 Li1 C1 32.37(15) . . ? N2 Li1 C1 61.1(2) . . ? Li2 Li1 C1 78.6(3) . . ? C6 Li1 C1 34.39(15) . . ? N3 Li1 Si3 32.64(15) . . ? N1 Li1 Si3 122.9(3) . . ? N2 Li1 Si3 145.6(3) . . ? Li2 Li1 Si3 74.7(3) . . ? C6 Li1 Si3 159.3(3) . . ? C1 Li1 Si3 153.2(3) . . ? N1 Li2 N3 107.1(3) . . ? N1 Li2 N4 151.9(4) . . ? N3 Li2 N4 88.3(3) . . ? N1 Li2 Li1 54.2(3) . . ? N3 Li2 Li1 53.0(3) . . ? N4 Li2 Li1 136.8(4) . . ? N1 Li2 C18 127.0(3) . . ? N3 Li2 C18 68.0(2) . . ? N4 Li2 C18 37.49(18) . . ? Li1 Li2 C18 102.7(3) . . ? N1 Li2 C13 122.5(3) . . ? N3 Li2 C13 32.91(17) . . ? N4 Li2 C13 61.0(2) . . ? Li1 Li2 C13 76.0(3) . . ? C18 Li2 C13 35.08(15) . . ? N1 Li2 C9 72.8(2) . . ? N3 Li2 C9 120.2(4) . . ? N4 Li2 C9 120.0(3) . . ? Li1 Li2 C9 98.1(3) . . ? C18 Li2 C9 157.5(3) . . ? C13 Li2 C9 148.4(3) . . ? N1 Li2 Si1 34.43(14) . . ? N3 Li2 Si1 121.8(3) . . ? N4 Li2 Si1 148.3(3) . . ? Li1 Li2 Si1 74.7(3) . . ? C18 Li2 Si1 158.3(3) . . ? C13 Li2 Si1 150.7(3) . . ? C9 Li2 Si1 38.55(13) . . ? C1 N1 Si1 114.7(2) . . ? C1 N1 Li2 136.7(3) . . ? Si1 N1 Li2 104.3(2) . . ? C1 N1 Li1 100.8(3) . . ? Si1 N1 Li1 121.0(3) . . ? Li2 N1 Li1 72.5(3) . . ? C6 N2 Si2 125.9(3) . . ? C6 N2 Li1 90.2(3) . . ? Si2 N2 Li1 117.6(3) . . ? C13 N3 Si3 117.8(3) . . ? C13 N3 Li1 128.0(3) . . ? Si3 N3 Li1 108.3(3) . . ? C13 N3 Li2 98.8(3) . . ? Si3 N3 Li2 123.8(3) . . ? Li1 N3 Li2 72.4(3) . . ? C18 N4 Si4 130.4(3) . . ? C18 N4 Li2 81.8(3) . . ? Si4 N4 Li2 114.6(3) . . ? N1 C1 C2 111.9(3) . . ? N1 C1 C6 112.9(3) . . ? C2 C1 C6 107.5(3) . . ? N1 C1 Li1 46.8(2) . . ? C2 C1 Li1 134.4(3) . . ? C6 C1 Li1 66.6(2) . . ? C3 C2 C1 111.8(4) . . ? C4 C3 C2 111.2(4) . . ? C3 C4 C5 110.3(4) . . ? C4 C5 C6 111.9(4) . . ? N2 C6 C5 113.8(3) . . ? N2 C6 C1 109.7(3) . . ? C5 C6 C1 109.7(3) . . ? N2 C6 Li1 54.1(2) . . ? C5 C6 Li1 167.7(3) . . ? C1 C6 Li1 79.0(2) . . ? Si1 C9 Li2 74.99(19) . . ? N3 C13 C14 111.9(4) . . ? N3 C13 C18 110.9(3) . . ? C14 C13 C18 109.2(4) . . ? N3 C13 Li2 48.3(2) . . ? C14 C13 Li2 128.5(3) . . ? C18 C13 Li2 62.7(3) . . ? C13 C14 C15 112.8(4) . . ? C16 C15 C14 110.3(5) . . ? C15 C16 C17 112.9(5) . . ? C16 C17 C18 110.5(4) . . ? N4 C18 C13 109.9(3) . . ? N4 C18 C17 112.8(4) . . ? C13 C18 C17 110.5(4) . . ? N4 C18 Li2 60.7(3) . . ? C13 C18 Li2 82.3(3) . . ? C17 C18 Li2 167.3(4) . . ? N1 Si1 C8 115.16(19) . . ? N1 Si1 C7 113.9(2) . . ? C8 Si1 C7 104.5(2) . . ? N1 Si1 C9 107.43(17) . . ? C8 Si1 C9 107.8(2) . . ? C7 Si1 C9 107.7(3) . . ? N1 Si1 Li2 41.24(16) . . ? C8 Si1 Li2 123.8(2) . . ? C7 Si1 Li2 131.1(2) . . ? C9 Si1 Li2 66.46(19) . . ? N2 Si2 C12 105.6(2) . . ? N2 Si2 C10 113.5(3) . . ? C12 Si2 C10 106.0(5) . . ? N2 Si2 C11 109.6(2) . . ? C12 Si2 C11 113.0(4) . . ? C10 Si2 C11 109.1(3) . . ? N3 Si3 C21 108.4(2) . . ? N3 Si3 C20 113.3(3) . . ? C21 Si3 C20 107.4(3) . . ? N3 Si3 C19 113.2(2) . . ? C21 Si3 C19 108.4(3) . . ? C20 Si3 C19 105.8(4) . . ? N3 Si3 Li1 39.10(18) . . ? C21 Si3 Li1 71.2(2) . . ? C20 Si3 Li1 137.4(3) . . ? C19 Si3 Li1 115.0(3) . . ? N4 Si4 C22 105.2(3) . . ? N4 Si4 C24 106.0(3) . . ? C22 Si4 C24 111.1(4) . . ? N4 Si4 C23 117.0(3) . . ? C22 Si4 C23 107.8(3) . . ? C24 Si4 C23 109.7(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.305 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.038 #===END data_compound4 _database_code_CSD 161940 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H34 Li N3 Si2' _chemical_formula_weight 367.61 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 'Monoclinic' _symmetry_space_group_name_H-M 'P 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.9459(4) _cell_length_b 20.6507(9) _cell_length_c 11.0775(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.703(1) _cell_angle_gamma 90.00 _cell_volume 2259.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16443 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8828 _exptl_absorpt_correction_T_max 1.1638 _exptl_special_details ; ABSCOR by T.Higashi 8 March, 1995 ; _diffrn_ambient_temperature 173(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 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method 'Oscilation' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_reflns_number 16443 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5212 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Molecular Structure Corporation (1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_cell_refinement ; Molecular Structure Corporation (1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381 USA. ; _computing_data_reduction ; Sheldrick, G. M. (1997) SHELXS97, Program for the Solution of Crystal Structure, University of Gottingen, Germany. ; _computing_structure_solution ; Sheldrick, G. M. (1997) SHELXS97, Program for the Solution of Crystal Structure, University of Gottingen, Germany. ; _computing_structure_refinement ; Sheldrick, G. M. (1997) SHELXL97, Program for the Refinement of Crystal Structure, University of Gottingen, Germany. ; _computing_molecular_graphics ; Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _computing_publication_material ; Sheldrick, G. M. (1997) SHELXL97, Program for the refinement of Crystal Structure, University of Gottingen, Germany. ; _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 w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'hydrogen atoms are generated by HFIX instructions' _refine_ls_hydrogen_treatment ; hydrogen coordinates ride on the coordinates of the previous atom, the isotropic U values are 1.2 OR 1.5 time over the U values of the previous atom. ; _refine_ls_extinction_method SHELXL97 _refine_ls_extinction_coef 0.0017(6) _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 0.11(9) _refine_ls_number_reflns 5212 _refine_ls_number_parameters 470 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si11 Si 0.97970(8) -0.29611(4) 0.77430(7) 0.03024(18) Uani 1 d . . . Si12 Si 1.52088(9) -0.54519(4) 1.00308(8) 0.0361(2) Uani 1 d . . . Si21 Si 1.06625(8) -0.55083(4) 0.75476(7) 0.03175(18) Uani 1 d . . . Si22 Si 1.41389(8) -0.22269(4) 0.55131(7) 0.03064(18) Uani 1 d . . . N11 N 1.1497(2) -0.31243(11) 0.7989(2) 0.0299(5) Uani 1 d . . . N12 N 1.3531(2) -0.34799(11) 0.8940(2) 0.0269(5) Uani 1 d . . . N13 N 1.4643(2) -0.46480(11) 1.0029(2) 0.0302(5) Uani 1 d . . . N21 N 1.1851(2) -0.49273(11) 0.7343(2) 0.0293(5) Uani 1 d . . . N22 N 1.3367(2) -0.43239(10) 0.64124(19) 0.0245(5) Uani 1 d . . . N23 N 1.3753(2) -0.30563(10) 0.5444(2) 0.0272(5) Uani 1 d . . . Li1 Li 1.2993(5) -0.3409(2) 0.7024(4) 0.0295(10) Uani 1 d . . . Li2 Li 1.3364(5) -0.4433(2) 0.8343(4) 0.0311(10) Uani 1 d . . . C11 C 1.2317(3) -0.32093(12) 0.9001(2) 0.0262(5) Uani 1 d . . . C12 C 1.1927(2) -0.30117(13) 1.0225(2) 0.0278(5) Uani 1 d . . . C13 C 1.2016(3) -0.23769(14) 1.0613(3) 0.0368(7) Uani 1 d . . . H13 H 1.2323 -0.2061 1.0113 0.044 Uiso 1 calc R . . C14 C 1.1654(3) -0.22056(19) 1.1737(3) 0.0487(9) Uani 1 d . . . H14 H 1.1716 -0.1775 1.1985 0.058 Uiso 1 calc R . . C15 C 1.1204(3) -0.2663(2) 1.2487(3) 0.0538(10) Uani 1 d . . . H15 H 1.0965 -0.2547 1.3244 0.065 Uiso 1 calc R . . C16 C 1.1108(3) -0.3297(2) 1.2110(3) 0.0481(9) Uani 1 d . . . H16 H 1.0799 -0.3610 1.2616 0.058 Uiso 1 calc R . . C17 C 1.1466(3) -0.34749(15) 1.0986(3) 0.0367(7) Uani 1 d . . . H17 H 1.1399 -0.3906 1.0741 0.044 Uiso 1 calc R . . C18 C 1.4565(3) -0.34598(13) 0.9993(2) 0.0256(5) Uani 1 d . . . H18 H 1.4108 -0.3466 1.0730 0.031 Uiso 1 calc R . . C19 C 1.5404(3) -0.28411(14) 0.9999(3) 0.0348(7) Uani 1 d . . . H19A H 1.4807 -0.2469 0.9995 0.042 Uiso 1 calc R . . H19B H 1.5851 -0.2824 0.9267 0.042 Uiso 1 calc R . . C20 C 1.6468(3) -0.28027(15) 1.1110(3) 0.0447(8) Uani 1 d . . . H20A H 1.6996 -0.2410 1.1071 0.054 Uiso 1 calc R . . H20B H 1.6023 -0.2787 1.1843 0.054 Uiso 1 calc R . . C21 C 1.7394(3) -0.33835(16) 1.1156(3) 0.0439(8) Uani 1 d . . . H21A H 1.8008 -0.3372 1.1903 0.053 Uiso 1 calc R . . H21B H 1.7932 -0.3364 1.0481 0.053 Uiso 1 calc R . . C22 C 1.6603(3) -0.40165(16) 1.1095(3) 0.0393(7) Uani 1 d . . . H22A H 1.6192 -0.4068 1.1841 0.047 Uiso 1 calc R . . H22B H 1.7228 -0.4373 1.1043 0.047 Uiso 1 calc R . . C23 C 1.5489(3) -0.40565(14) 1.0013(3) 0.0286(6) Uani 1 d . . . H23 H 1.5923 -0.4059 0.9263 0.034 Uiso 1 calc R . . C24 C 0.8784(3) -0.36967(16) 0.7999(3) 0.0464(8) Uani 1 d . . . H24A H 0.9016 -0.4038 0.7472 0.070 Uiso 1 calc R . . H24B H 0.7838 -0.3599 0.7827 0.070 Uiso 1 calc R . . H24C H 0.8977 -0.3832 0.8830 0.070 Uiso 1 calc R . . C25 C 0.9415(3) -0.27434(17) 0.6091(3) 0.0451(8) Uani 1 d . . . H25A H 0.9750 -0.2316 0.5959 0.068 Uiso 1 calc R . . H25B H 0.8454 -0.2754 0.5862 0.068 Uiso 1 calc R . . H25C H 0.9846 -0.3049 0.5607 0.068 Uiso 1 calc R . . C26 C 0.9186(3) -0.22830(16) 0.8670(3) 0.0403(7) Uani 1 d . . . H26A H 0.9270 -0.2407 0.9510 0.061 Uiso 1 calc R . . H26B H 0.8254 -0.2192 0.8393 0.061 Uiso 1 calc R . . H26C H 0.9721 -0.1903 0.8579 0.061 Uiso 1 calc R . . C27 C 1.3747(4) -0.59294(17) 1.0444(4) 0.0611(10) Uani 1 d . . . H27A H 1.3496 -0.5777 1.1205 0.092 Uiso 1 calc R . . H27B H 1.3993 -0.6378 1.0515 0.092 Uiso 1 calc R . . H27C H 1.2995 -0.5879 0.9824 0.092 Uiso 1 calc R . . C28 C 1.6709(4) -0.56619(18) 1.1136(3) 0.0561(10) Uani 1 d . . . H28A H 1.7508 -0.5474 1.0872 0.084 Uiso 1 calc R . . H28B H 1.6808 -0.6124 1.1179 0.084 Uiso 1 calc R . . H28C H 1.6582 -0.5496 1.1924 0.084 Uiso 1 calc R . . C29 C 1.5607(5) -0.56394(19) 0.8490(3) 0.0633(11) Uani 1 d . . . H29A H 1.4824 -0.5562 0.7916 0.095 Uiso 1 calc R . . H29B H 1.5869 -0.6086 0.8451 0.095 Uiso 1 calc R . . H29C H 1.6337 -0.5368 0.8298 0.095 Uiso 1 calc R . . C31 C 1.2348(2) -0.47491(12) 0.6334(2) 0.0251(5) Uani 1 d . . . C32 C 1.1733(3) -0.50093(12) 0.5117(2) 0.0276(6) Uani 1 d . . . C33 C 1.0712(3) -0.46573(14) 0.4442(3) 0.0369(7) Uani 1 d . . . H33 H 1.0457 -0.4257 0.4725 0.044 Uiso 1 calc R . . C34 C 1.0070(4) -0.48967(16) 0.3356(3) 0.0483(8) Uani 1 d . . . H34 H 0.9389 -0.4658 0.2914 0.058 Uiso 1 calc R . . C35 C 1.0441(4) -0.54867(19) 0.2935(3) 0.0533(9) Uani 1 d . . . H35 H 1.0014 -0.5646 0.2205 0.064 Uiso 1 calc R . . C36 C 1.1449(4) -0.58459(17) 0.3593(3) 0.0520(9) Uani 1 d . . . H36 H 1.1703 -0.6245 0.3303 0.062 Uiso 1 calc R . . C37 C 1.2076(3) -0.56087(14) 0.4681(3) 0.0375(7) Uani 1 d . . . H37 H 1.2740 -0.5855 0.5129 0.045 Uiso 1 calc R . . C38 C 1.4138(3) -0.42382(12) 0.5384(2) 0.0265(6) Uani 1 d . . . H38 H 1.3523 -0.4272 0.4628 0.032 Uiso 1 calc R . . C39 C 1.5234(3) -0.47607(14) 0.5391(3) 0.0320(6) Uani 1 d . . . H39A H 1.5800 -0.4748 0.6165 0.038 Uiso 1 calc R . . H39B H 1.4804 -0.5183 0.5315 0.038 Uiso 1 calc R . . C40 C 1.6123(3) -0.46778(15) 0.4372(3) 0.0376(7) Uani 1 d . . . H40A H 1.6817 -0.5010 0.4436 0.045 Uiso 1 calc R . . H40B H 1.5578 -0.4725 0.3592 0.045 Uiso 1 calc R . . C41 C 1.6783(3) -0.40130(15) 0.4454(3) 0.0368(7) Uani 1 d . . . H41A H 1.7398 -0.3982 0.5198 0.044 Uiso 1 calc R . . H41B H 1.7303 -0.3953 0.3774 0.044 Uiso 1 calc R . . C42 C 1.5717(3) -0.34857(14) 0.4436(3) 0.0315(6) Uani 1 d . . . H42A H 1.5162 -0.3491 0.3656 0.038 Uiso 1 calc R . . H42B H 1.6163 -0.3068 0.4524 0.038 Uiso 1 calc R . . C43 C 1.4807(3) -0.35664(12) 0.5447(2) 0.0260(5) Uani 1 d . . . H43 H 1.5385 -0.3538 0.6224 0.031 Uiso 1 calc R . . C44 C 1.0159(3) -0.53802(17) 0.9106(3) 0.0481(8) Uani 1 d . . . H44A H 1.0951 -0.5295 0.9666 0.072 Uiso 1 calc R . . H44B H 0.9714 -0.5762 0.9357 0.072 Uiso 1 calc R . . H44C H 0.9552 -0.5018 0.9095 0.072 Uiso 1 calc R . . C45 C 0.9063(3) -0.54928(16) 0.6470(3) 0.0416(7) Uani 1 d . . . H45A H 0.8704 -0.5061 0.6422 0.062 Uiso 1 calc R . . H45B H 0.8413 -0.5781 0.6756 0.062 Uiso 1 calc R . . H45C H 0.9254 -0.5629 0.5678 0.062 Uiso 1 calc R . . C46 C 1.1409(3) -0.63378(15) 0.7458(4) 0.0512(9) Uani 1 d . . . H46A H 1.1312 -0.6479 0.6627 0.077 Uiso 1 calc R . . H46B H 1.0945 -0.6633 0.7935 0.077 Uiso 1 calc R . . H46C H 1.2351 -0.6325 0.7766 0.077 Uiso 1 calc R . . C47 C 1.2584(4) -0.18027(15) 0.5854(4) 0.0506(9) Uani 1 d . . . H47A H 1.1876 -0.1870 0.5199 0.076 Uiso 1 calc R . . H47B H 1.2765 -0.1348 0.5945 0.076 Uiso 1 calc R . . H47C H 1.2306 -0.1971 0.6593 0.076 Uiso 1 calc R . . C48 C 1.4663(4) -0.18807(16) 0.4082(3) 0.0486(9) Uani 1 d . . . H48A H 1.5595 -0.1984 0.4029 0.073 Uiso 1 calc R . . H48B H 1.4553 -0.1419 0.4085 0.073 Uiso 1 calc R . . H48C H 1.4110 -0.2061 0.3395 0.073 Uiso 1 calc R . . C49 C 1.5516(4) -0.21088(16) 0.6765(3) 0.0490(8) Uani 1 d . . . H49A H 1.5221 -0.2253 0.7514 0.073 Uiso 1 calc R . . H49B H 1.5749 -0.1658 0.6827 0.073 Uiso 1 calc R . . H49C H 1.6295 -0.2354 0.6602 0.073 Uiso 1 calc R . . H51 H 1.310(4) -0.312(2) 0.490(4) 0.080 Uiso 1 d . . . H52 H 1.411(5) -0.464(2) 1.054(4) 0.080 Uiso 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 Si11 0.0278(4) 0.0306(4) 0.0316(4) -0.0004(3) 0.0006(3) 0.0034(3) Si12 0.0457(5) 0.0286(4) 0.0320(4) 0.0007(3) -0.0033(4) 0.0093(4) Si21 0.0301(4) 0.0254(4) 0.0393(4) 0.0062(3) 0.0024(3) -0.0042(3) Si22 0.0359(4) 0.0217(4) 0.0334(4) 0.0026(3) 0.0004(3) -0.0033(3) N11 0.0293(12) 0.0312(13) 0.0295(12) 0.0012(10) 0.0042(9) 0.0037(9) N12 0.0263(11) 0.0255(11) 0.0285(12) -0.0031(10) 0.0017(9) 0.0016(9) N13 0.0298(13) 0.0276(12) 0.0334(13) 0.0034(10) 0.0039(10) 0.0027(10) N21 0.0310(12) 0.0265(12) 0.0298(12) 0.0025(9) 0.0013(10) -0.0046(9) N22 0.0278(11) 0.0206(10) 0.0255(11) 0.0006(9) 0.0046(9) -0.0044(9) N23 0.0249(11) 0.0227(12) 0.0335(13) 0.0025(10) 0.0008(9) 0.0001(9) Li1 0.036(2) 0.024(2) 0.028(2) 0.0001(19) 0.0013(19) -0.0011(18) Li2 0.040(3) 0.027(2) 0.025(2) -0.0014(18) -0.003(2) 0.0016(19) C11 0.0291(14) 0.0178(11) 0.0321(14) -0.0020(11) 0.0047(11) -0.0029(10) C12 0.0224(12) 0.0303(14) 0.0307(13) -0.0035(12) 0.0024(10) 0.0032(11) C13 0.0349(16) 0.0334(16) 0.0416(17) -0.0080(13) 0.0016(13) 0.0035(12) C14 0.0411(18) 0.051(2) 0.053(2) -0.0240(18) 0.0016(16) 0.0086(16) C15 0.0369(18) 0.090(3) 0.0354(18) -0.016(2) 0.0065(14) 0.0108(19) C16 0.0400(18) 0.073(3) 0.0323(17) 0.0120(17) 0.0084(14) 0.0058(17) C17 0.0331(15) 0.0382(16) 0.0396(17) 0.0038(14) 0.0071(13) -0.0021(13) C18 0.0246(13) 0.0279(13) 0.0241(13) -0.0027(11) 0.0022(10) -0.0013(10) C19 0.0368(16) 0.0309(16) 0.0350(15) -0.0015(12) -0.0032(13) -0.0084(12) C20 0.0435(18) 0.0440(19) 0.0457(19) -0.0054(14) 0.0011(14) -0.0170(14) C21 0.0310(15) 0.058(2) 0.0409(17) 0.0034(15) -0.0037(13) -0.0124(14) C22 0.0315(16) 0.0457(18) 0.0375(17) 0.0041(14) -0.0095(13) -0.0029(13) C23 0.0263(14) 0.0321(15) 0.0268(14) 0.0003(11) 0.0005(11) 0.0009(11) C24 0.0436(19) 0.0429(19) 0.053(2) -0.0010(16) 0.0068(16) -0.0006(15) C25 0.0357(16) 0.059(2) 0.0382(17) 0.0016(15) -0.0055(13) 0.0024(15) C26 0.0334(16) 0.0402(17) 0.0467(18) -0.0041(15) 0.0015(13) 0.0114(14) C27 0.073(3) 0.0338(18) 0.075(3) 0.0175(18) 0.002(2) 0.0042(17) C28 0.064(2) 0.051(2) 0.049(2) -0.0029(17) -0.0117(18) 0.0250(17) C29 0.090(3) 0.056(2) 0.0426(19) -0.0071(17) 0.003(2) 0.030(2) C31 0.0261(13) 0.0179(12) 0.0305(14) 0.0012(11) 0.0005(11) 0.0014(10) C32 0.0309(15) 0.0240(13) 0.0278(14) -0.0005(11) 0.0036(11) -0.0047(10) C33 0.0425(17) 0.0278(14) 0.0380(17) 0.0026(13) -0.0049(13) 0.0010(13) C34 0.050(2) 0.046(2) 0.0437(19) 0.0014(15) -0.0193(15) 0.0001(15) C35 0.057(2) 0.056(2) 0.0426(17) -0.0194(18) -0.0122(16) -0.0079(19) C36 0.051(2) 0.0430(19) 0.059(2) -0.0256(17) -0.0060(17) 0.0006(16) C37 0.0359(15) 0.0319(16) 0.0426(17) -0.0058(13) -0.0042(13) 0.0036(12) C38 0.0287(14) 0.0258(13) 0.0251(13) -0.0005(11) 0.0035(11) -0.0020(10) C39 0.0350(15) 0.0260(13) 0.0358(16) -0.0005(13) 0.0075(12) 0.0045(12) C40 0.0401(17) 0.0376(16) 0.0350(16) -0.0024(14) 0.0037(13) 0.0090(13) C41 0.0318(16) 0.0438(17) 0.0353(16) -0.0022(13) 0.0059(13) 0.0015(13) C42 0.0310(14) 0.0333(14) 0.0313(15) 0.0009(12) 0.0077(12) -0.0032(12) C43 0.0272(13) 0.0232(13) 0.0278(13) -0.0002(11) 0.0044(11) -0.0020(10) C44 0.0442(18) 0.051(2) 0.0497(19) 0.0134(16) 0.0099(15) -0.0040(16) C45 0.0385(16) 0.0359(16) 0.0494(18) 0.0030(15) 0.0004(14) -0.0070(14) C46 0.0468(19) 0.0298(17) 0.077(3) 0.0104(17) 0.0079(18) -0.0036(14) C47 0.056(2) 0.0279(16) 0.068(2) -0.0001(15) 0.0087(19) 0.0048(15) C48 0.065(2) 0.0353(17) 0.045(2) 0.0110(15) 0.0028(17) -0.0138(16) C49 0.057(2) 0.0415(19) 0.0453(19) -0.0010(15) -0.0065(16) -0.0084(15) _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 Si11 N11 1.715(2) . ? Si11 C24 1.863(3) . ? Si11 C26 1.879(3) . ? Si11 C25 1.880(3) . ? Si12 N13 1.753(2) . ? Si12 C29 1.838(4) . ? Si12 C27 1.858(4) . ? Si12 C28 1.867(3) . ? Si21 N21 1.718(2) . ? Si21 C44 1.872(3) . ? Si21 C46 1.874(3) . ? Si21 C45 1.875(3) . ? Si22 N23 1.755(2) . ? Si22 C49 1.848(3) . ? Si22 C47 1.854(3) . ? Si22 C48 1.868(3) . ? N11 C11 1.319(3) . ? N11 Li1 2.018(5) . ? N12 C11 1.340(3) . ? N12 C18 1.463(3) . ? N12 Li2 2.076(5) . ? N12 Li1 2.133(5) . ? N13 C23 1.485(4) . ? N13 Li2 2.180(5) . ? N21 C31 1.326(3) . ? N21 Li2 2.036(5) . ? N22 C31 1.336(3) . ? N22 C38 1.457(3) . ? N22 Li1 2.056(5) . ? N22 Li2 2.151(5) . ? N23 C43 1.486(3) . ? N23 Li1 2.115(5) . ? Li1 C11 2.400(5) . ? Li1 Li2 2.572(6) . ? Li1 C43 2.674(5) . ? Li2 C31 2.424(5) . ? Li2 C23 2.753(6) . ? C11 C12 1.509(4) . ? C12 C13 1.379(4) . ? C12 C17 1.388(4) . ? C13 C14 1.382(4) . ? C14 C15 1.368(5) . ? C15 C16 1.374(5) . ? C16 C17 1.384(4) . ? C18 C19 1.525(4) . ? C18 C23 1.536(4) . ? C19 C20 1.529(4) . ? C20 C21 1.509(5) . ? C21 C22 1.523(4) . ? C22 C23 1.536(4) . ? C31 C32 1.513(4) . ? C32 C37 1.386(4) . ? C32 C33 1.394(4) . ? C33 C34 1.386(4) . ? C34 C35 1.370(5) . ? C35 C36 1.384(5) . ? C36 C37 1.380(4) . ? C38 C39 1.534(4) . ? C38 C43 1.537(4) . ? C39 C40 1.522(4) . ? C40 C41 1.520(4) . ? C41 C42 1.518(4) . ? C42 C43 1.529(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 N11 Si11 C24 110.87(14) . . ? N11 Si11 C26 115.82(13) . . ? C24 Si11 C26 108.03(15) . . ? N11 Si11 C25 106.58(13) . . ? C24 Si11 C25 106.98(16) . . ? C26 Si11 C25 108.19(15) . . ? N13 Si12 C29 107.62(15) . . ? N13 Si12 C27 104.02(15) . . ? C29 Si12 C27 112.1(2) . . ? N13 Si12 C28 116.91(14) . . ? C29 Si12 C28 108.50(18) . . ? C27 Si12 C28 107.70(18) . . ? N21 Si21 C44 106.59(14) . . ? N21 Si21 C46 110.40(13) . . ? C44 Si21 C46 109.16(17) . . ? N21 Si21 C45 116.74(13) . . ? C44 Si21 C45 106.66(15) . . ? C46 Si21 C45 107.08(16) . . ? N23 Si22 C49 107.50(13) . . ? N23 Si22 C47 106.64(13) . . ? C49 Si22 C47 110.35(17) . . ? N23 Si22 C48 114.71(13) . . ? C49 Si22 C48 109.30(16) . . ? C47 Si22 C48 108.30(17) . . ? C11 N11 Si11 131.44(19) . . ? C11 N11 Li1 89.5(2) . . ? Si11 N11 Li1 138.36(18) . . ? C11 N12 C18 120.2(2) . . ? C11 N12 Li2 111.8(2) . . ? C18 N12 Li2 107.7(2) . . ? C11 N12 Li1 84.1(2) . . ? C18 N12 Li1 149.7(2) . . ? Li2 N12 Li1 75.31(19) . . ? C23 N13 Si12 126.62(18) . . ? C23 N13 Li2 95.6(2) . . ? Si12 N13 Li2 110.45(17) . . ? C31 N21 Si21 129.42(19) . . ? C31 N21 Li2 89.7(2) . . ? Si21 N21 Li2 139.02(19) . . ? C31 N22 C38 119.6(2) . . ? C31 N22 Li1 117.4(2) . . ? C38 N22 Li1 106.16(19) . . ? C31 N22 Li2 84.7(2) . . ? C38 N22 Li2 148.5(2) . . ? Li1 N22 Li2 75.34(19) . . ? C43 N23 Si22 122.74(17) . . ? C43 N23 Li1 94.28(19) . . ? Si22 N23 Li1 113.43(17) . . ? N11 Li1 N22 128.0(2) . . ? N11 Li1 N23 134.0(2) . . ? N22 Li1 N23 87.00(19) . . ? N11 Li1 N12 66.92(16) . . ? N22 Li1 N12 103.3(2) . . ? N23 Li1 N12 140.8(2) . . ? N11 Li1 C11 33.32(11) . . ? N22 Li1 C11 122.6(2) . . ? N23 Li1 C11 149.4(2) . . ? N12 Li1 C11 33.73(11) . . ? N11 Li1 Li2 90.3(2) . . ? N22 Li1 Li2 54.00(16) . . ? N23 Li1 Li2 135.4(2) . . ? N12 Li1 Li2 51.34(15) . . ? C11 Li1 Li2 70.11(17) . . ? N11 Li1 C43 167.7(2) . . ? N22 Li1 C43 60.72(14) . . ? N23 Li1 C43 33.65(11) . . ? N12 Li1 C43 122.1(2) . . ? C11 Li1 C43 154.1(2) . . ? Li2 Li1 C43 102.0(2) . . ? N21 Li2 N12 132.5(3) . . ? N21 Li2 N22 66.30(16) . . ? N12 Li2 N22 102.0(2) . . ? N21 Li2 N13 133.2(2) . . ? N12 Li2 N13 84.44(18) . . ? N22 Li2 N13 143.6(3) . . ? N21 Li2 C31 33.17(11) . . ? N12 Li2 C31 123.9(2) . . ? N22 Li2 C31 33.27(10) . . ? N13 Li2 C31 150.6(2) . . ? N21 Li2 Li1 93.2(2) . . ? N12 Li2 Li1 53.34(16) . . ? N22 Li2 Li1 50.66(15) . . ? N13 Li2 Li1 133.3(2) . . ? C31 Li2 Li1 71.53(17) . . ? N21 Li2 C23 165.4(2) . . ? N12 Li2 C23 59.46(14) . . ? N22 Li2 C23 123.3(2) . . ? N13 Li2 C23 32.46(11) . . ? C31 Li2 C23 153.9(2) . . ? Li1 Li2 C23 101.4(2) . . ? N11 C11 N12 119.0(2) . . ? N11 C11 C12 122.0(2) . . ? N12 C11 C12 119.1(2) . . ? N11 C11 Li1 57.21(17) . . ? N12 C11 Li1 62.13(18) . . ? C12 C11 Li1 174.1(2) . . ? C13 C12 C17 118.6(3) . . ? C13 C12 C11 121.6(3) . . ? C17 C12 C11 119.8(2) . . ? C12 C13 C14 120.7(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C16 119.4(3) . . ? C15 C16 C17 120.6(3) . . ? C16 C17 C12 120.1(3) . . ? N12 C18 C19 111.2(2) . . ? N12 C18 C23 110.7(2) . . ? C19 C18 C23 110.3(2) . . ? C18 C19 C20 112.0(2) . . ? C21 C20 C19 110.4(3) . . ? C20 C21 C22 111.7(2) . . ? C21 C22 C23 113.8(3) . . ? N13 C23 C22 113.2(2) . . ? N13 C23 C18 108.8(2) . . ? C22 C23 C18 110.1(2) . . ? N13 C23 Li2 51.99(16) . . ? C22 C23 Li2 165.1(2) . . ? C18 C23 Li2 78.79(16) . . ? N21 C31 N22 118.8(2) . . ? N21 C31 C32 120.1(2) . . ? N22 C31 C32 121.1(2) . . ? N21 C31 Li2 57.13(17) . . ? N22 C31 Li2 62.04(18) . . ? C32 C31 Li2 174.8(2) . . ? C37 C32 C33 118.2(3) . . ? C37 C32 C31 122.5(2) . . ? C33 C32 C31 119.1(2) . . ? C34 C33 C32 120.8(3) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.3(3) . . ? C37 C36 C35 119.7(3) . . ? C36 C37 C32 121.1(3) . . ? N22 C38 C39 110.5(2) . . ? N22 C38 C43 109.8(2) . . ? C39 C38 C43 109.3(2) . . ? C40 C39 C38 113.0(2) . . ? C41 C40 C39 110.0(2) . . ? C42 C41 C40 110.6(2) . . ? C41 C42 C43 112.6(2) . . ? N23 C43 C42 113.5(2) . . ? N23 C43 C38 109.8(2) . . ? C42 C43 C38 110.8(2) . . ? N23 C43 Li1 52.07(15) . . ? C42 C43 Li1 165.4(2) . . ? C38 C43 Li1 79.51(16) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.277 _refine_diff_density_min -0.195 _refine_diff_density_rms 0.041 #===END