# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1657 data_B003169K-1 _audit_creation_date 1999-10-15T09:48:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{LiN(SiMe3)(SiMe2Ph)}2]' _chemical_formula_moiety 'C22 H40 Li2 N2 Si2' _chemical_formula_structural 'C22 H40 LI2 N2 SI2' _chemical_formula_sum 'C22 H40 Li2 N2 Si4' _chemical_formula_weight 458.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.2980(3) _cell_length_b 13.6936(3) _cell_length_c 15.2530(3) _cell_angle_alpha 90 _cell_angle_beta 98.6350(10) _cell_angle_gamma 90 _cell_volume 2952.55(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13499 _cell_measurement_theta_min 4.431 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.212 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 24486 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 27.85 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6948 _reflns_number_gt 5613 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0491P)^2^+1.1624P] 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_number_reflns 6948 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.103 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.328 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.31003(19) 0.2925(2) 0.03929(18) 0.0356(6) Uani 1 1 d . . . Li2 Li 0.14747(19) 0.2986(2) -0.01365(18) 0.0383(6) Uani 1 1 d . . . Si1 Si 0.26370(3) 0.10371(3) 0.08065(3) 0.03252(12) Uani 1 1 d . . . Si2 Si 0.12852(3) 0.23789(4) 0.15297(3) 0.03568(12) Uani 1 1 d . . . Si3 Si 0.21173(3) 0.36979(4) -0.16347(3) 0.03456(12) Uani 1 1 d . . . Si4 Si 0.29324(3) 0.48935(3) -0.00548(3) 0.03402(12) Uani 1 1 d . . . N1 N 0.20763(9) 0.21288(10) 0.08323(8) 0.0302(3) Uani 1 1 d . . . N2 N 0.24529(9) 0.38508(9) -0.05283(8) 0.0298(3) Uani 1 1 d . . . C1 C 0.19831(15) 0.01061(15) 0.00496(14) 0.0536(5) Uani 1 1 d . . . H1A H 0.1796 0.0394 -0.0539 0.08 Uiso 1 1 calc R . . H1B H 0.1417 -0.0104 0.029 0.08 Uiso 1 1 calc R . . H1C H 0.2394 -0.0458 0.0002 0.08 Uiso 1 1 calc R . . C2 C 0.29734(15) 0.04372(15) 0.19154(12) 0.0485(5) Uani 1 1 d . . . H2A H 0.3317 0.0905 0.2331 0.073 Uiso 1 1 calc R . . H2B H 0.3378 -0.0129 0.1853 0.073 Uiso 1 1 calc R . . H2C H 0.2401 0.0222 0.2141 0.073 Uiso 1 1 calc R . . C3 C 0.38031(11) 0.12978(11) 0.03972(10) 0.0317(3) Uani 1 1 d . . . C4 C 0.39794(14) 0.10581(15) -0.04527(12) 0.0481(5) Uani 1 1 d . . . H4 H 0.3492 0.076 -0.0857 0.058 Uiso 1 1 calc R . . C5 C 0.48443(16) 0.12422(18) -0.07228(14) 0.0598(6) Uani 1 1 d . . . H5 H 0.4943 0.1064 -0.1304 0.072 Uiso 1 1 calc R . . C6 C 0.55618(14) 0.16806(16) -0.01565(13) 0.0506(5) Uani 1 1 d . . . H6 H 0.6154 0.1807 -0.0345 0.061 Uiso 1 1 calc R . . C7 C 0.54137(13) 0.19343(14) 0.06846(12) 0.0445(4) Uani 1 1 d . . . H7 H 0.5904 0.2241 0.1079 0.053 Uiso 1 1 calc R . . C8 C 0.45473(12) 0.17426(13) 0.09573(11) 0.0376(4) Uani 1 1 d . . . H8 H 0.4457 0.1919 0.1541 0.045 Uiso 1 1 calc R . . C9 C 0.06554(14) 0.35554(16) 0.11602(14) 0.0535(5) Uani 1 1 d . . . H9A H 0.0355 0.3493 0.0541 0.08 Uiso 1 1 calc R . . H9B H 0.1113 0.4093 0.1212 0.08 Uiso 1 1 calc R . . H9C H 0.0171 0.369 0.1536 0.08 Uiso 1 1 calc R . . C10 C 0.03508(17) 0.14252(19) 0.15298(19) 0.0755(8) Uani 1 1 d . . . H10A H 0.005 0.13 0.0919 0.113 Uiso 1 1 calc R . . H10B H -0.0126 0.1654 0.1881 0.113 Uiso 1 1 calc R . . H10C H 0.0638 0.0821 0.1789 0.113 Uiso 1 1 calc R . . C11 C 0.18168(16) 0.25766(17) 0.27134(12) 0.0558(5) Uani 1 1 d . . . H11A H 0.2312 0.3076 0.2744 0.084 Uiso 1 1 calc R . . H11B H 0.2092 0.1964 0.2964 0.084 Uiso 1 1 calc R . . H11C H 0.1325 0.2794 0.3052 0.084 Uiso 1 1 calc R . . C12 C 0.30447(16) 0.3174(2) -0.22337(14) 0.0642(6) Uani 1 1 d . . . H12A H 0.3312 0.2588 -0.1924 0.096 Uiso 1 1 calc R . . H12B H 0.3547 0.3658 -0.2253 0.096 Uiso 1 1 calc R . . H12C H 0.2763 0.3003 -0.284 0.096 Uiso 1 1 calc R . . C13 C 0.16354(17) 0.48187(16) -0.22603(14) 0.0610(6) Uani 1 1 d . . . H13A H 0.1142 0.5112 -0.1963 0.091 Uiso 1 1 calc R . . H13B H 0.1366 0.4637 -0.2867 0.091 Uiso 1 1 calc R . . H13C H 0.2147 0.5291 -0.2276 0.091 Uiso 1 1 calc R . . C14 C 0.10908(11) 0.28049(12) -0.17346(10) 0.0327(3) Uani 1 1 d . . . C15 C 0.11462(13) 0.18376(13) -0.20081(11) 0.0410(4) Uani 1 1 d . . . H15 H 0.1712 0.1614 -0.2197 0.049 Uiso 1 1 calc R . . C16 C 0.03963(15) 0.11910(15) -0.20117(13) 0.0529(5) Uani 1 1 d . . . H16 H 0.0448 0.054 -0.2215 0.064 Uiso 1 1 calc R . . C17 C -0.04225(14) 0.14963(16) -0.17198(13) 0.0528(5) Uani 1 1 d . . . H17 H -0.093 0.1051 -0.171 0.063 Uiso 1 1 calc R . . C18 C -0.05071(13) 0.24422(16) -0.14435(12) 0.0490(5) Uani 1 1 d . . . H18 H -0.1072 0.2651 -0.1242 0.059 Uiso 1 1 calc R . . C19 C 0.02358(12) 0.30923(14) -0.14600(11) 0.0403(4) Uani 1 1 d . . . H19 H 0.0164 0.3749 -0.1281 0.048 Uiso 1 1 calc R . . C20 C 0.35315(13) 0.45799(14) 0.10997(11) 0.0431(4) Uani 1 1 d . . . H20A H 0.3999 0.4063 0.1066 0.065 Uiso 1 1 calc R . . H20B H 0.3057 0.4353 0.1455 0.065 Uiso 1 1 calc R . . H20C H 0.3849 0.5161 0.1377 0.065 Uiso 1 1 calc R . . C21 C 0.38571(15) 0.54401(17) -0.06545(14) 0.0579(5) Uani 1 1 d . . . H21A H 0.4329 0.4942 -0.0735 0.087 Uiso 1 1 calc R . . H21B H 0.4166 0.5984 -0.0307 0.087 Uiso 1 1 calc R . . H21C H 0.356 0.568 -0.1235 0.087 Uiso 1 1 calc R . . C22 C 0.20568(16) 0.58807(16) 0.00760(16) 0.0632(6) Uani 1 1 d . . . H22A H 0.156 0.562 0.0389 0.095 Uiso 1 1 calc R . . H22B H 0.1773 0.6117 -0.051 0.095 Uiso 1 1 calc R . . H22C H 0.2379 0.6421 0.0418 0.095 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 0.0335(13) 0.0346(15) 0.0385(14) 0.0074(12) 0.0043(11) -0.0020(11) Li2 0.0334(14) 0.0482(17) 0.0325(13) 0.0058(12) 0.0029(11) -0.0041(12) Si1 0.0383(2) 0.0284(2) 0.0314(2) 0.00145(17) 0.00689(17) -0.00246(17) Si2 0.0332(2) 0.0425(3) 0.0334(2) 0.00275(19) 0.01143(18) -0.00092(19) Si3 0.0403(3) 0.0376(3) 0.0261(2) 0.00313(17) 0.00574(18) -0.00638(19) Si4 0.0347(2) 0.0298(2) 0.0354(2) 0.00151(18) -0.00185(18) -0.00216(17) N1 0.0320(6) 0.0313(7) 0.0284(6) 0.0037(5) 0.0078(5) -0.0009(5) N2 0.0319(6) 0.0291(7) 0.0280(6) 0.0033(5) 0.0028(5) -0.0032(5) C1 0.0578(12) 0.0418(11) 0.0601(12) -0.0099(9) 0.0055(10) -0.0123(9) C2 0.0594(11) 0.0426(11) 0.0451(10) 0.0165(8) 0.0128(9) 0.0058(9) C3 0.0374(8) 0.0275(8) 0.0303(7) -0.0006(6) 0.0059(6) 0.0042(6) C4 0.0486(10) 0.0592(12) 0.0374(9) -0.0157(8) 0.0094(8) -0.0055(9) C5 0.0612(13) 0.0797(16) 0.0435(11) -0.0157(10) 0.0236(10) -0.0061(11) C6 0.0423(10) 0.0609(13) 0.0520(11) 0.0021(9) 0.0181(9) 0.0008(9) C7 0.0401(9) 0.0490(11) 0.0434(10) 0.0030(8) 0.0028(7) -0.0044(8) C8 0.0442(9) 0.0390(9) 0.0296(8) -0.0007(7) 0.0058(7) -0.0010(7) C9 0.0446(10) 0.0668(14) 0.0507(11) 0.0058(10) 0.0126(9) 0.0214(10) C10 0.0586(13) 0.0782(17) 0.0994(19) -0.0081(14) 0.0437(13) -0.0256(12) C11 0.0685(13) 0.0667(14) 0.0334(9) 0.0000(9) 0.0119(9) 0.0180(11) C12 0.0580(13) 0.0900(18) 0.0505(12) -0.0142(12) 0.0274(10) -0.0154(12) C13 0.0827(15) 0.0495(12) 0.0438(11) 0.0176(9) -0.0131(10) -0.0153(11) C14 0.0373(8) 0.0368(9) 0.0227(7) -0.0002(6) 0.0002(6) -0.0027(7) C15 0.0433(9) 0.0435(10) 0.0363(9) -0.0064(7) 0.0060(7) -0.0021(8) C16 0.0599(12) 0.0463(12) 0.0518(11) -0.0112(9) 0.0062(9) -0.0129(9) C17 0.0467(11) 0.0613(13) 0.0482(11) -0.0021(9) 0.0002(9) -0.0202(10) C18 0.0343(9) 0.0683(14) 0.0435(10) -0.0064(9) 0.0035(8) -0.0046(9) C19 0.0379(9) 0.0460(10) 0.0354(8) -0.0053(7) 0.0000(7) 0.0007(7) C20 0.0440(9) 0.0473(11) 0.0356(9) -0.0015(8) -0.0021(7) -0.0062(8) C21 0.0560(12) 0.0573(13) 0.0572(12) 0.0156(10) -0.0013(9) -0.0239(10) C22 0.0657(14) 0.0436(12) 0.0746(15) -0.0124(11) -0.0077(11) 0.0144(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.012(3) . ? Li1 N1 2.019(3) . ? Li2 N1 1.980(3) . ? Li2 N2 1.992(3) . ? Si1 N1 1.6995(14) . ? Si1 C1 1.8730(19) . ? Si1 C2 1.8769(18) . ? Si1 C3 1.8999(16) . ? Si2 N1 1.6999(13) . ? Si2 C10 1.868(2) . ? Si2 C11 1.870(2) . ? Si2 C9 1.890(2) . ? Si3 N2 1.6967(13) . ? Si3 C12 1.863(2) . ? Si3 C13 1.882(2) . ? Si3 C14 1.8988(16) . ? Si4 N2 1.6975(13) . ? Si4 C21 1.873(2) . ? Si4 C22 1.873(2) . ? Si4 C20 1.8885(17) . ? C3 C4 1.396(2) . ? C3 C8 1.400(2) . ? C4 C5 1.384(3) . ? C5 C6 1.376(3) . ? C6 C7 1.376(3) . ? C7 C8 1.390(2) . ? C14 C15 1.394(2) . ? C14 C19 1.407(2) . ? C15 C16 1.390(3) . ? C16 C17 1.378(3) . ? C17 C18 1.373(3) . ? C18 C19 1.389(3) . ? 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 106.95(13) . . ? N1 Li2 N2 109.30(14) . . ? N1 Si1 C1 114.80(9) . . ? N1 Si1 C2 114.96(8) . . ? C1 Si1 C2 107.11(10) . . ? N1 Si1 C3 106.42(7) . . ? C1 Si1 C3 107.87(8) . . ? C2 Si1 C3 105.04(8) . . ? N1 Si2 C10 113.71(9) . . ? N1 Si2 C11 114.91(8) . . ? C10 Si2 C11 106.74(12) . . ? N1 Si2 C9 108.49(8) . . ? C10 Si2 C9 106.69(12) . . ? C11 Si2 C9 105.72(10) . . ? N2 Si3 C12 114.80(9) . . ? N2 Si3 C13 115.53(9) . . ? C12 Si3 C13 107.36(11) . . ? N2 Si3 C14 105.01(6) . . ? C12 Si3 C14 108.14(9) . . ? C13 Si3 C14 105.35(9) . . ? N2 Si4 C21 113.45(9) . . ? N2 Si4 C22 114.75(9) . . ? C21 Si4 C22 107.19(11) . . ? N2 Si4 C20 107.65(7) . . ? C21 Si4 C20 106.96(9) . . ? C22 Si4 C20 106.35(10) . . ? Si1 N1 Si2 123.52(8) . . ? Si1 N1 Li2 131.14(11) . . ? Si2 N1 Li2 95.29(10) . . ? Si1 N1 Li1 95.69(10) . . ? Si2 N1 Li1 133.07(11) . . ? Li2 N1 Li1 71.79(12) . . ? Si3 N2 Si4 124.25(8) . . ? Si3 N2 Li2 96.81(10) . . ? Si4 N2 Li2 129.00(11) . . ? Si3 N2 Li1 130.43(11) . . ? Si4 N2 Li1 96.83(10) . . ? Li2 N2 Li1 71.70(12) . . ? C4 C3 C8 116.24(15) . . ? C4 C3 Si1 123.40(13) . . ? C8 C3 Si1 120.35(12) . . ? C5 C4 C3 121.83(18) . . ? C6 C5 C4 120.53(17) . . ? C5 C6 C7 119.40(18) . . ? C6 C7 C8 120.02(17) . . ? C7 C8 C3 121.97(15) . . ? C15 C14 C19 116.47(15) . . ? C15 C14 Si3 123.90(13) . . ? C19 C14 Si3 119.45(13) . . ? C16 C15 C14 121.86(17) . . ? C17 C16 C15 119.84(19) . . ? C18 C17 C16 120.24(18) . . ? C17 C18 C19 119.74(18) . . ? C18 C19 C14 121.82(17) . . ? #===END data_B003169K-2 _audit_creation_date 1999-11-25T16:03:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[{NaN(SiMe3)(SiMe2Ph)}2]' _chemical_formula_moiety 'C11 H20 N1 Na1 Si2' _chemical_formula_structural 'C11 H20 SI2 N NA' _chemical_formula_sum 'C11 H20 N Na Si2' _chemical_formula_weight 245.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.6414(6) _cell_length_b 14.6700(5) _cell_length_c 11.6899(4) _cell_angle_alpha 90 _cell_angle_beta 93.187(2) _cell_angle_gamma 90 _cell_volume 2849.43(17) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11812 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.251 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 13397 _diffrn_reflns_av_R_equivalents 0.0907 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.71 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 3364 _reflns_number_gt 2958 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0471P)^2^+2.4527P] 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_number_reflns 3364 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.857 _refine_ls_shift/su_mean 0.047 _refine_diff_density_max 0.371 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Na Na 0.0362 0.0249 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0 -0.08244(6) 0.25 0.0281(2) Uani 1 2 d S . . Na2 Na 0 -0.28968(6) 0.25 0.0300(2) Uani 1 2 d S . . Si1 Si -0.07841(2) -0.15801(3) 0.01209(3) 0.02079(12) Uani 1 1 d . . . Si2 Si 0.09317(2) -0.22432(3) 0.03796(3) 0.02398(12) Uani 1 1 d . . . N1 N 0.00682(7) -0.18473(8) 0.08974(10) 0.0229(2) Uani 1 1 d . . . C1 C -0.15064(10) -0.09838(12) 0.10645(14) 0.0322(3) Uani 1 1 d G . . H1A H -0.1286 -0.039 0.1306 0.048 Uiso 1 1 d G . . H1B H -0.1581 -0.1362 0.1741 0.048 Uiso 1 1 d G . . H1C H -0.2026 -0.0896 0.0643 0.048 Uiso 1 1 d G . . C2 C -0.13466(11) -0.25871(12) -0.05164(16) 0.0359(4) Uani 1 1 d G . . H2A H -0.1023 -0.2865 -0.1099 0.054 Uiso 1 1 d G . . H2B H -0.1878 -0.2425 -0.0861 0.054 Uiso 1 1 d G . . H2C H -0.1409 -0.3022 0.0109 0.054 Uiso 1 1 d G . . C3 C -0.06266(9) -0.07614(11) -0.11018(12) 0.0273(3) Uani 1 1 d G . . H3A H -0.0442 -0.0171 -0.0794 0.041 Uiso 1 1 d G . . H3B H -0.1135 -0.0679 -0.1555 0.041 Uiso 1 1 d G . . H3C H -0.0221 -0.1013 -0.159 0.041 Uiso 1 1 d G . . C4 C 0.08825(12) -0.25974(15) -0.11734(14) 0.0422(4) Uani 1 1 d G . . H4A H 0.0438 -0.3025 -0.1332 0.063 Uiso 1 1 d G . . H4B H 0.1392 -0.2892 -0.1335 0.063 Uiso 1 1 d G . . H4C H 0.0804 -0.2058 -0.1661 0.063 Uiso 1 1 d G . . C5 C 0.17989(10) -0.14294(12) 0.05507(15) 0.0339(4) Uani 1 1 d G . . H5A H 0.1879 -0.1235 0.1351 0.051 Uiso 1 1 d G . . H5B H 0.168 -0.0896 0.0065 0.051 Uiso 1 1 d G . . H5C H 0.2289 -0.1727 0.0309 0.051 Uiso 1 1 d G . . C6 C 0.12314(9) -0.33232(10) 0.12079(13) 0.0268(3) Uani 1 1 d . . . C7 C 0.07961(13) -0.41307(13) 0.1011(2) 0.0500(5) Uani 1 1 d G . . H7 H 0.0371 -0.415 0.0435 0.06 Uiso 1 1 d G . . C8 C 0.09442(16) -0.49110(14) 0.1660(3) 0.0673(7) Uani 1 1 d G . . H8 H 0.0645 -0.5455 0.1518 0.081 Uiso 1 1 d G . . C9 C 0.15367(15) -0.49123(15) 0.2519(3) 0.0608(6) Uani 1 1 d G . . H9 H 0.1602 -0.5459 0.2949 0.073 Uiso 1 1 d G . . C10 C 0.19734(12) -0.41332(15) 0.27438(19) 0.0495(5) Uani 1 1 d G . . H10 H 0.2384 -0.411 0.3341 0.059 Uiso 1 1 d G . . C11 C 0.18234(10) -0.33497(12) 0.21005(16) 0.0345(4) Uani 1 1 d G . . H11 H 0.2134 -0.2816 0.2258 0.041 Uiso 1 1 d G . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0410(5) 0.0258(4) 0.0173(4) 0 -0.0002(3) 0 Na2 0.0416(5) 0.0257(4) 0.0230(4) 0 0.0052(3) 0 Si1 0.0240(2) 0.0232(2) 0.01524(19) 0.00061(14) 0.00106(14) 0.00138(15) Si2 0.0276(2) 0.0282(2) 0.01623(19) -0.00033(15) 0.00168(15) 0.00705(16) N1 0.0268(6) 0.0265(6) 0.0153(5) 0.0005(5) 0.0005(4) 0.0055(5) C1 0.0305(8) 0.0411(9) 0.0254(7) 0.0017(7) 0.0057(6) 0.0067(7) C2 0.0396(9) 0.0334(8) 0.0340(8) -0.0035(7) -0.0031(7) -0.0070(7) C3 0.0332(7) 0.0307(7) 0.0179(6) 0.0045(6) 0.0002(5) 0.0030(6) C4 0.0456(10) 0.0606(12) 0.0205(7) -0.0075(8) 0.0023(7) 0.0204(9) C5 0.0320(8) 0.0327(8) 0.0382(9) 0.0040(7) 0.0117(7) 0.0047(7) C6 0.0274(7) 0.0262(7) 0.0268(7) -0.0028(6) 0.0015(6) 0.0066(6) C7 0.0554(12) 0.0295(9) 0.0624(13) -0.0054(9) -0.0205(10) 0.0003(8) C8 0.0729(16) 0.0254(9) 0.101(2) 0.0035(11) -0.0178(14) -0.0019(10) C9 0.0614(13) 0.0356(10) 0.0845(17) 0.0236(11) -0.0027(12) 0.0130(10) C10 0.0458(11) 0.0515(12) 0.0499(12) 0.0177(10) -0.0082(9) 0.0115(9) C11 0.0335(8) 0.0343(8) 0.0351(9) 0.0047(7) -0.0034(7) 0.0026(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 N1 2.4078(13) . ? Na1 N1 2.4078(13) 2 ? Na1 C1 2.9474(17) 2 ? Na1 C1 2.9475(17) . ? Na1 Na2 3.0402(12) . ? Na1 C3 3.0595(16) 5 ? Na1 C3 3.0595(16) 6_556 ? Na1 Si1 3.2035(5) 2 ? Na1 Si1 3.2036(5) . ? Na2 N1 2.4325(13) . ? Na2 N1 2.4325(13) 2 ? Na2 C6 2.6862(15) . ? Na2 C6 2.6863(15) 2 ? Na2 C7 2.884(2) . ? Na2 C7 2.884(2) 2 ? Na2 Si2 3.1455(5) 2 ? Na2 Si2 3.1455(5) . ? Si1 N1 1.6870(12) . ? Si1 C2 1.8804(17) . ? Si1 C1 1.8906(16) . ? Si1 C3 1.8963(15) . ? Si2 N1 1.6927(12) . ? Si2 C5 1.8752(18) . ? Si2 C4 1.8857(17) . ? Si2 C6 1.9086(16) . ? C3 Na1 3.0596(16) 5 ? C6 C11 1.395(2) . ? C6 C7 1.401(2) . ? C7 C8 1.388(3) . ? C8 C9 1.367(4) . ? C9 C10 1.372(3) . ? C10 C11 1.389(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Na1 N1 102.90(7) . 2 ? N1 Na1 C1 108.55(5) . 2 ? N1 Na1 C1 65.35(4) 2 2 ? N1 Na1 C1 65.35(4) . . ? N1 Na1 C1 108.55(5) 2 . ? C1 Na1 C1 170.90(8) 2 . ? N1 Na1 Na2 51.45(3) . . ? N1 Na1 Na2 51.45(3) 2 . ? C1 Na1 Na2 85.45(4) 2 . ? C1 Na1 Na2 85.45(4) . . ? N1 Na1 C3 91.49(4) . 5 ? N1 Na1 C3 157.18(4) 2 5 ? C1 Na1 C3 93.4 2 5 ? C1 Na1 C3 93.5 . 5 ? Na2 Na1 C3 139.50(3) . 5 ? N1 Na1 C3 157.18(4) . 6_556 ? N1 Na1 C3 91.49(4) 2 6_556 ? C1 Na1 C3 93.5 2 6_556 ? C1 Na1 C3 93.4 . 6_556 ? Na2 Na1 C3 139.50(3) . 6_556 ? C3 Na1 C3 81.00(6) 5 6_556 ? N1 Na1 Si1 115.17(4) . 2 ? N1 Na1 Si1 31.07(3) 2 2 ? C1 Na1 Si1 35.49(3) 2 2 ? C1 Na1 Si1 139.40(4) . 2 ? Na2 Na1 Si1 69.754(16) . 2 ? C3 Na1 Si1 126.33(3) 5 2 ? C3 Na1 Si1 86.20(3) 6_556 2 ? N1 Na1 Si1 31.07(3) . . ? N1 Na1 Si1 115.17(4) 2 . ? C1 Na1 Si1 139.40(4) 2 . ? C1 Na1 Si1 35.49(3) . . ? Na2 Na1 Si1 69.753(16) . . ? C3 Na1 Si1 86.20(3) 5 . ? C3 Na1 Si1 126.33(3) 6_556 . ? Si1 Na1 Si1 139.51(3) 2 . ? N1 Na2 N1 101.46(6) . 2 ? N1 Na2 C6 69.18(4) . . ? N1 Na2 C6 130.55(5) 2 . ? N1 Na2 C6 130.55(5) . 2 ? N1 Na2 C6 69.18(4) 2 2 ? C6 Na2 C6 153.07(7) . 2 ? N1 Na2 C7 83.67(5) . . ? N1 Na2 C7 154.79(5) 2 . ? C6 Na2 C7 28.85(5) . . ? C6 Na2 C7 125.70(6) 2 . ? N1 Na2 C7 154.79(5) . 2 ? N1 Na2 C7 83.67(5) 2 2 ? C6 Na2 C7 125.70(6) . 2 ? C6 Na2 C7 28.85(5) 2 2 ? C7 Na2 C7 102.25(9) . 2 ? N1 Na2 Na1 50.73(3) . . ? N1 Na2 Na1 50.73(3) 2 . ? C6 Na2 Na1 103.47(4) . . ? C6 Na2 Na1 103.47(4) 2 . ? C7 Na2 Na1 128.87(5) . . ? C7 Na2 Na1 128.87(5) 2 . ? N1 Na2 Si2 117.39(4) . 2 ? N1 Na2 Si2 32.22(3) 2 2 ? C6 Na2 Si2 159.87(3) . 2 ? C6 Na2 Si2 37.16(3) 2 2 ? C7 Na2 Si2 158.43(5) . 2 ? C7 Na2 Si2 56.81(5) 2 2 ? Na1 Na2 Si2 72.254(17) . 2 ? N1 Na2 Si2 32.22(3) . . ? N1 Na2 Si2 117.39(4) 2 . ? C6 Na2 Si2 37.16(3) . . ? C6 Na2 Si2 159.87(3) 2 . ? C7 Na2 Si2 56.81(5) . . ? C7 Na2 Si2 158.43(5) 2 . ? Na1 Na2 Si2 72.253(17) . . ? Si2 Na2 Si2 144.51(3) 2 . ? N1 Si1 C2 114.57(7) . . ? N1 Si1 C1 109.66(7) . . ? C2 Si1 C1 106.02(8) . . ? N1 Si1 C3 113.91(7) . . ? C2 Si1 C3 106.59(8) . . ? C1 Si1 C3 105.41(7) . . ? N1 Si1 Na1 47.44(4) . . ? C2 Si1 Na1 141.78(6) . . ? C1 Si1 Na1 64.84(5) . . ? C3 Si1 Na1 111.62(5) . . ? N1 Si2 C5 114.02(7) . . ? N1 Si2 C4 116.53(7) . . ? C5 Si2 C4 105.66(9) . . ? N1 Si2 C6 107.85(6) . . ? C5 Si2 C6 107.25(7) . . ? C4 Si2 C6 104.82(8) . . ? N1 Si2 Na2 50.02(4) . . ? C5 Si2 Na2 121.34(6) . . ? C4 Si2 Na2 132.67(7) . . ? C6 Si2 Na2 58.23(5) . . ? Si1 N1 Si2 126.32(7) . . ? Si1 N1 Na1 101.50(6) . . ? Si2 N1 Na1 124.73(6) . . ? Si1 N1 Na2 119.18(6) . . ? Si2 N1 Na2 97.76(5) . . ? Na1 N1 Na2 77.82(4) . . ? Si1 C1 Na1 79.67(5) . . ? Si1 C3 Na1 161.77(8) . 5 ? C11 C6 C7 115.89(16) . . ? C11 C6 Si2 123.80(12) . . ? C7 C6 Si2 120.02(13) . . ? C11 C6 Na2 96.61(11) . . ? C7 C6 Na2 83.44(12) . . ? Si2 C6 Na2 84.60(5) . . ? C8 C7 C6 122.22(18) . . ? C8 C7 Na2 105.15(18) . . ? C6 C7 Na2 67.71(11) . . ? C9 C8 C7 120.1(2) . . ? C8 C9 C10 119.49(19) . . ? C9 C10 C11 120.54(19) . . ? C10 C11 C6 121.76(17) . . ? #===END data_B003169K-4 _audit_creation_date 1999-05-09T13:50:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C9 H14 Li1 N1 Si1' _chemical_formula_structural 'C9 H14 N LI SI' _chemical_formula_sum 'C36 H56 Li4 N4 Si4' _chemical_formula_weight 684.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.103(4) _cell_length_b 10.873(5) _cell_length_c 20.223(7) _cell_angle_alpha 99.82(3) _cell_angle_beta 91.76(3) _cell_angle_gamma 113.16(3) _cell_volume 2000.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.6 _cell_measurement_theta_max 10 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_T_min 0.9487 _exptl_absorpt_correction_T_max 0.9653 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 0.37083E-1 _diffrn_orient_matrix_ub_12 -0.45033E-1 _diffrn_orient_matrix_ub_13 -0.37876E-1 _diffrn_orient_matrix_ub_21 -0.36436E-1 _diffrn_orient_matrix_ub_22 0.42772E-1 _diffrn_orient_matrix_ub_23 -0.32282E-1 _diffrn_orient_matrix_ub_31 0.95027E-1 _diffrn_orient_matrix_ub_32 0.81098E-1 _diffrn_orient_matrix_ub_33 0.8641E-2 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_standards_decay_corr_max 1.244 _diffrn_standards_decay_corr_min 0.972 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 3 -5 -1 4 -2 _diffrn_reflns_number 7003 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.1182 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7003 _reflns_number_gt 4136 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 _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_number_reflns 7003 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1398 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1944 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.404 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.5513(9) 0.2813(8) 0.3182(4) 0.0288(19) Uani 1 1 d . . . Li2 Li 0.5611(9) 0.2604(8) 0.1886(4) 0.0266(18) Uani 1 1 d . . . Li3 Li 0.3578(10) 0.4188(9) 0.3866(5) 0.036(2) Uani 1 1 d . . . Li4 Li 0.3488(10) -0.0128(9) 0.0967(4) 0.035(2) Uani 1 1 d . . . M1 C 0.3677 0.5054 0.2958 0 Uiso 0 1 d P A 1 M2 C 0.3263 -0.1044 0.1851 0 Uiso 0 1 d P B 1 Si1 Si 0.76745(15) 0.55403(14) 0.25169(7) 0.0247(3) Uani 1 1 d . A 2 Si2 Si 0.72885(14) 0.11455(13) 0.27829(6) 0.0209(3) Uani 1 1 d . B 2 Si3 Si 0.29957(15) 0.13192(14) 0.41577(7) 0.0239(3) Uani 1 1 d . A 2 Si4 Si 0.32716(15) 0.24146(14) 0.06059(7) 0.0250(3) Uani 1 1 d . B 2 N1 N 0.5987(4) 0.4336(4) 0.25958(19) 0.0230(9) Uani 1 1 d . A 2 N2 N 0.5711(4) 0.1264(4) 0.25035(18) 0.0205(9) Uani 1 1 d . B 2 N3 N 0.4344(4) 0.2829(4) 0.40603(18) 0.0218(9) Uani 1 1 d . A 2 N4 N 0.4489(4) 0.1795(4) 0.08660(18) 0.0228(9) Uani 1 1 d . B 2 C1 C 0.4892(5) 0.4719(5) 0.2783(2) 0.0212(10) Uani 1 1 d . A 2 C2 C 0.5065(5) 0.5973(5) 0.3191(2) 0.0261(11) Uani 1 1 d . A 2 H2 H 0.6016 0.6618 0.3363 0.031 Uiso 1 1 calc R A 2 C3 C 0.3907(6) 0.6300(5) 0.3348(3) 0.0339(13) Uani 1 1 d . A 2 H3 H 0.408 0.7167 0.3616 0.041 Uiso 1 1 calc R A 2 C4 C 0.2507(6) 0.5389(6) 0.3124(3) 0.0393(14) Uani 1 1 d . A 2 H4 H 0.1715 0.5617 0.3236 0.047 Uiso 1 1 calc R A 2 C5 C 0.2273(6) 0.4134(6) 0.2731(3) 0.0323(12) Uani 1 1 d . A 2 H5 H 0.1313 0.3498 0.2569 0.039 Uiso 1 1 calc R A 2 C6 C 0.3420(5) 0.3803(5) 0.2575(2) 0.0256(11) Uani 1 1 d . A 2 H6 H 0.3224 0.2923 0.2316 0.031 Uiso 1 1 calc R A 2 C7 C 0.8679(6) 0.4629(6) 0.2035(3) 0.0360(13) Uani 1 1 d . A 2 H7A H 0.8776 0.3962 0.2282 0.054 Uiso 1 1 calc R A 2 H7B H 0.9643 0.529 0.198 0.054 Uiso 1 1 calc R A 2 H7C H 0.8145 0.4155 0.159 0.054 Uiso 1 1 calc R A 2 C8 C 0.8860(6) 0.6564(5) 0.3326(3) 0.0370(13) Uani 1 1 d . A 2 H8A H 0.8372 0.7063 0.3596 0.055 Uiso 1 1 calc R A 2 H8B H 0.9783 0.7213 0.322 0.055 Uiso 1 1 calc R A 2 H8C H 0.904 0.5947 0.3582 0.055 Uiso 1 1 calc R A 2 C9 C 0.7530(6) 0.6795(5) 0.2021(3) 0.0399(14) Uani 1 1 d . A 2 H9A H 0.7003 0.7291 0.226 0.06 Uiso 1 1 calc R A 2 H9B H 0.7008 0.6308 0.1575 0.06 Uiso 1 1 calc R A 2 H9C H 0.8502 0.7442 0.1968 0.06 Uiso 1 1 calc R A 2 C10 C 0.4539(5) 0.0114(5) 0.2179(2) 0.0214(10) Uani 1 1 d . B 2 C11 C 0.4609(6) -0.1075(5) 0.1809(3) 0.0306(12) Uani 1 1 d . B 2 H11 H 0.5528 -0.1112 0.177 0.037 Uiso 1 1 calc R B 2 C12 C 0.3379(6) -0.2191(5) 0.1500(3) 0.0412(14) Uani 1 1 d . B 2 H12 H 0.3469 -0.2976 0.1255 0.049 Uiso 1 1 calc R B 2 C13 C 0.2020(6) -0.2178(6) 0.1543(3) 0.0470(16) Uani 1 1 d . B 2 H13 H 0.1178 -0.2955 0.1339 0.056 Uiso 1 1 calc R B 2 C14 C 0.1906(6) -0.1017(6) 0.1888(3) 0.0366(13) Uani 1 1 d . B 2 H14 H 0.0982 -0.0986 0.1915 0.044 Uiso 1 1 calc R B 2 C15 C 0.3125(5) 0.0086(5) 0.2188(2) 0.0273(11) Uani 1 1 d . B 2 H15 H 0.3019 0.0877 0.2415 0.033 Uiso 1 1 calc R B 2 C16 C 0.6896(6) -0.0266(5) 0.3258(3) 0.0326(12) Uani 1 1 d . B 2 H16A H 0.6313 -0.114 0.2957 0.049 Uiso 1 1 calc R B 2 H16B H 0.636 -0.0121 0.3638 0.049 Uiso 1 1 calc R B 2 H16C H 0.7808 -0.0279 0.3428 0.049 Uiso 1 1 calc R B 2 C17 C 0.8475(5) 0.0905(5) 0.2115(2) 0.0306(12) Uani 1 1 d . B 2 H17A H 0.8707 0.1637 0.1857 0.046 Uiso 1 1 calc R B 2 H17B H 0.7962 0.0021 0.181 0.046 Uiso 1 1 calc R B 2 H17C H 0.9372 0.0934 0.233 0.046 Uiso 1 1 calc R B 2 C18 C 0.8395(5) 0.2774(5) 0.3395(2) 0.0311(12) Uani 1 1 d . B 2 H18A H 0.8633 0.3546 0.3165 0.047 Uiso 1 1 calc R B 2 H18B H 0.9291 0.2733 0.3568 0.047 Uiso 1 1 calc R B 2 H18C H 0.7839 0.2891 0.3771 0.047 Uiso 1 1 calc R B 2 C19 C 0.5640(5) 0.3393(5) 0.4489(2) 0.0236(11) Uani 1 1 d . A 2 C20 C 0.6509(5) 0.4801(5) 0.4620(3) 0.0308(12) Uani 1 1 d . A 2 H20 H 0.6171 0.5381 0.4432 0.037 Uiso 1 1 calc R A 2 C21 C 0.7838(6) 0.5384(6) 0.5013(3) 0.0372(13) Uani 1 1 d . . 2 H21 H 0.8385 0.6342 0.5086 0.045 Uiso 1 1 calc R . 2 C22 C 0.8368(6) 0.4578(6) 0.5298(3) 0.0416(15) Uani 1 1 d . A 2 H22 H 0.9276 0.4971 0.5566 0.05 Uiso 1 1 calc R A 2 C23 C 0.7553(6) 0.3201(6) 0.5184(3) 0.0428(15) Uani 1 1 d . A 2 H23 H 0.7908 0.2636 0.5375 0.051 Uiso 1 1 calc R A 2 C24 C 0.6224(6) 0.2614(6) 0.4797(3) 0.0333(13) Uani 1 1 d . A 2 H24 H 0.5685 0.1656 0.4737 0.04 Uiso 1 1 calc R A 2 C25 C 0.1304(5) 0.1140(5) 0.3668(3) 0.0337(12) Uani 1 1 d . A 2 H25A H 0.1112 0.1955 0.3816 0.05 Uiso 1 1 calc R A 2 H25B H 0.0488 0.0333 0.3746 0.05 Uiso 1 1 calc R A 2 H25C H 0.1427 0.1037 0.3186 0.05 Uiso 1 1 calc R A 2 C26 C 0.3301(6) -0.0269(5) 0.3855(3) 0.0335(12) Uani 1 1 d . A 2 H26A H 0.4181 -0.0207 0.4103 0.05 Uiso 1 1 calc R A 2 H26B H 0.3409 -0.0366 0.3372 0.05 Uiso 1 1 calc R A 2 H26C H 0.2471 -0.1065 0.3933 0.05 Uiso 1 1 calc R A 2 C27 C 0.2607(6) 0.1298(6) 0.5059(3) 0.0390(14) Uani 1 1 d . A 2 H27A H 0.3469 0.1384 0.5332 0.059 Uiso 1 1 calc R A 2 H27B H 0.1801 0.0437 0.5083 0.059 Uiso 1 1 calc R A 2 H27C H 0.2347 0.2062 0.5233 0.059 Uiso 1 1 calc R A 2 C28 C 0.5817(5) 0.2140(5) 0.0601(2) 0.0252(11) Uani 1 1 d . B 2 C29 C 0.6567(6) 0.3363(6) 0.0373(3) 0.0370(13) Uani 1 1 d . B 2 H29 H 0.6117 0.3981 0.0365 0.044 Uiso 1 1 calc R B 2 C30 C 0.7929(6) 0.3698(7) 0.0161(3) 0.0485(16) Uani 1 1 d . B 2 H30 H 0.8405 0.4543 0.0023 0.058 Uiso 1 1 calc R B 2 C31 C 0.8608(6) 0.2806(7) 0.0149(3) 0.0467(16) Uani 1 1 d . B 2 H31 H 0.954 0.3029 -0.0001 0.056 Uiso 1 1 calc R B 2 C32 C 0.7915(5) 0.1600(6) 0.0358(3) 0.0374(14) Uani 1 1 d . . 2 H32 H 0.8377 0.099 0.0358 0.045 Uiso 1 1 calc R . 2 C33 C 0.6545(5) 0.1260(5) 0.0570(2) 0.0276(11) Uani 1 1 d . B 2 H33 H 0.6079 0.0404 0.0698 0.033 Uiso 1 1 calc R B 2 C34 C 0.1499(5) 0.1400(6) 0.0900(3) 0.0361(13) Uani 1 1 d . B 2 H34A H 0.1617 0.1508 0.1393 0.054 Uiso 1 1 calc R B 2 H34B H 0.1182 0.0434 0.0692 0.054 Uiso 1 1 calc R B 2 H34C H 0.0772 0.1727 0.0771 0.054 Uiso 1 1 calc R B 2 C35 C 0.3698(6) 0.4269(5) 0.0937(3) 0.0358(13) Uani 1 1 d . B 2 H35A H 0.3853 0.446 0.1432 0.054 Uiso 1 1 calc R B 2 H35B H 0.2887 0.4477 0.0794 0.054 Uiso 1 1 calc R B 2 H35C H 0.4575 0.4835 0.0759 0.054 Uiso 1 1 calc R B 2 C36 C 0.2983(6) 0.2173(6) -0.0338(3) 0.0368(13) Uani 1 1 d . B 2 H36A H 0.3894 0.2694 -0.0507 0.055 Uiso 1 1 calc R B 2 H36B H 0.2246 0.2496 -0.046 0.055 Uiso 1 1 calc R B 2 H36C H 0.2657 0.1202 -0.054 0.055 Uiso 1 1 calc R B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.039(5) 0.026(5) 0.021(4) 0.002(4) 0.000(4) 0.014(4) Li2 0.037(5) 0.026(5) 0.021(4) 0.008(3) 0.007(4) 0.017(4) Li3 0.039(5) 0.032(5) 0.047(6) 0.019(4) 0.011(4) 0.019(4) Li4 0.042(5) 0.039(5) 0.027(5) 0.013(4) 0.003(4) 0.018(4) Si1 0.0267(8) 0.0217(7) 0.0269(7) 0.0084(6) 0.0055(6) 0.0095(6) Si2 0.0234(7) 0.0223(7) 0.0196(7) 0.0057(6) 0.0025(5) 0.0112(6) Si3 0.0252(8) 0.0258(8) 0.0230(7) 0.0085(6) 0.0032(6) 0.0111(6) Si4 0.0288(8) 0.0282(8) 0.0226(7) 0.0082(6) -0.0005(6) 0.0153(6) N1 0.025(2) 0.018(2) 0.028(2) 0.0063(17) 0.0035(17) 0.0106(18) N2 0.028(2) 0.020(2) 0.019(2) 0.0076(17) 0.0038(17) 0.0131(18) N3 0.027(2) 0.024(2) 0.0157(19) 0.0069(17) 0.0026(16) 0.0102(18) N4 0.027(2) 0.026(2) 0.020(2) 0.0075(17) 0.0026(17) 0.0150(19) C1 0.028(3) 0.024(3) 0.015(2) 0.007(2) 0.0008(19) 0.012(2) C2 0.028(3) 0.020(3) 0.028(3) 0.005(2) 0.004(2) 0.008(2) C3 0.037(3) 0.026(3) 0.040(3) 0.004(2) 0.009(3) 0.016(3) C4 0.038(3) 0.047(4) 0.043(3) 0.011(3) 0.011(3) 0.026(3) C5 0.028(3) 0.041(3) 0.032(3) 0.014(3) 0.004(2) 0.015(3) C6 0.026(3) 0.022(3) 0.027(3) 0.002(2) -0.002(2) 0.009(2) C7 0.035(3) 0.039(3) 0.037(3) 0.013(3) 0.013(2) 0.014(3) C8 0.031(3) 0.034(3) 0.037(3) -0.002(3) -0.002(2) 0.008(3) C9 0.042(3) 0.031(3) 0.049(4) 0.018(3) 0.009(3) 0.013(3) C10 0.031(3) 0.020(3) 0.014(2) 0.008(2) 0.0013(19) 0.010(2) C11 0.034(3) 0.027(3) 0.030(3) 0.005(2) -0.004(2) 0.013(2) C12 0.048(4) 0.024(3) 0.046(4) -0.004(3) -0.004(3) 0.013(3) C13 0.039(4) 0.035(4) 0.046(4) 0.010(3) -0.008(3) -0.006(3) C14 0.028(3) 0.041(4) 0.039(3) 0.019(3) 0.005(2) 0.007(3) C15 0.027(3) 0.032(3) 0.025(3) 0.010(2) 0.005(2) 0.012(2) C16 0.034(3) 0.033(3) 0.036(3) 0.015(2) 0.003(2) 0.016(3) C17 0.036(3) 0.033(3) 0.027(3) 0.005(2) 0.003(2) 0.019(3) C18 0.028(3) 0.033(3) 0.028(3) 0.003(2) -0.002(2) 0.010(2) C19 0.025(3) 0.032(3) 0.017(2) 0.008(2) 0.007(2) 0.014(2) C20 0.033(3) 0.025(3) 0.033(3) 0.003(2) 0.003(2) 0.011(2) C21 0.034(3) 0.032(3) 0.035(3) 0.002(3) 0.007(2) 0.004(3) C22 0.028(3) 0.063(4) 0.028(3) 0.014(3) -0.003(2) 0.012(3) C23 0.037(3) 0.054(4) 0.037(3) 0.022(3) 0.000(3) 0.013(3) C24 0.034(3) 0.034(3) 0.033(3) 0.014(2) -0.001(2) 0.012(3) C25 0.029(3) 0.035(3) 0.035(3) 0.009(2) 0.001(2) 0.010(2) C26 0.040(3) 0.028(3) 0.034(3) 0.011(2) 0.002(2) 0.013(3) C27 0.046(4) 0.043(4) 0.032(3) 0.019(3) 0.011(3) 0.016(3) C28 0.025(3) 0.028(3) 0.020(2) 0.003(2) -0.003(2) 0.008(2) C29 0.043(3) 0.035(3) 0.039(3) 0.018(3) 0.009(3) 0.018(3) C30 0.045(4) 0.060(4) 0.046(4) 0.034(3) 0.014(3) 0.017(3) C31 0.024(3) 0.075(5) 0.044(4) 0.020(3) 0.009(3) 0.020(3) C32 0.025(3) 0.052(4) 0.039(3) 0.009(3) 0.001(2) 0.020(3) C33 0.020(3) 0.037(3) 0.028(3) 0.011(2) 0.002(2) 0.011(2) C34 0.026(3) 0.044(3) 0.042(3) 0.007(3) -0.003(2) 0.019(3) C35 0.047(4) 0.035(3) 0.032(3) 0.008(2) 0.004(2) 0.023(3) C36 0.045(3) 0.039(3) 0.030(3) 0.011(3) -0.003(2) 0.020(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.062(9) . ? Li1 N1 2.112(9) . ? Li1 N3 2.164(9) . ? Li2 N1 2.057(9) . ? Li2 N2 2.103(8) . ? Li2 N4 2.183(9) . ? Li3 N3 2.004(9) . ? Li3 M1 2.189(9) . ? Li3 C6 2.563(10) . ? Li3 C2 2.573(10) . ? Li3 C5 2.591(10) . ? Li3 C3 2.592(10) . ? Li3 C4 2.609(10) . ? Li3 C1 2.626(10) . ? Li4 N4 1.983(10) . ? Li4 M2 2.164(8) . ? Li4 C15 2.492(10) . ? Li4 C14 2.556(10) . ? Li4 C10 2.569(9) . ? Li4 C11 2.575(9) . ? Li4 C12 2.615(10) . ? Li4 C13 2.629(11) . ? Si1 N1 1.726(4) . ? Si1 C7 1.867(5) . ? Si1 C9 1.871(5) . ? Si1 C8 1.887(5) . ? Si2 N2 1.734(4) . ? Si2 C16 1.866(5) . ? Si2 C18 1.878(5) . ? Si2 C17 1.886(5) . ? Si3 N3 1.720(4) . ? Si3 C25 1.873(5) . ? Si3 C26 1.877(5) . ? Si3 C27 1.879(5) . ? Si4 N4 1.725(4) . ? Si4 C34 1.875(5) . ? Si4 C36 1.880(5) . ? Si4 C35 1.881(5) . ? N1 C1 1.369(6) . ? N2 C10 1.379(6) . ? N3 C19 1.400(6) . ? N4 C28 1.395(6) . ? C1 C2 1.410(6) . ? C1 C6 1.427(6) . ? C2 C3 1.382(7) . ? C3 C4 1.376(7) . ? C4 C5 1.382(7) . ? C5 C6 1.373(7) . ? C10 C11 1.408(7) . ? C10 C15 1.418(7) . ? C11 C12 1.384(7) . ? C12 C13 1.384(8) . ? C13 C14 1.383(8) . ? C14 C15 1.367(7) . ? C19 C20 1.405(7) . ? C19 C24 1.416(7) . ? C20 C21 1.388(7) . ? C21 C22 1.381(8) . ? C21 Li3 2.787(10) 2_666 ? C22 C23 1.369(8) . ? C23 C24 1.382(7) . ? C28 C29 1.411(7) . ? C28 C33 1.413(7) . ? C29 C30 1.380(8) . ? C30 C31 1.388(8) . ? C31 C32 1.367(8) . ? C32 C33 1.387(7) . ? C32 Li4 2.876(10) 2_655 ? 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 100.6(4) . . ? N2 Li1 N3 132.8(4) . . ? N1 Li1 N3 122.3(4) . . ? N1 Li2 N2 101.1(4) . . ? N1 Li2 N4 134.1(4) . . ? N2 Li2 N4 120.0(4) . . ? N3 Li3 M1 128.8(5) . . ? N3 Li3 C6 101.9(4) . . ? M1 Li3 C6 32.24(17) . . ? N3 Li3 C2 118.0(4) . . ? M1 Li3 C2 32.22(17) . . ? C6 Li3 C2 55.2(2) . . ? N3 Li3 C5 126.5(5) . . ? M1 Li3 C5 32.25(17) . . ? C6 Li3 C5 30.90(18) . . ? C2 Li3 C5 64.5(3) . . ? N3 Li3 C3 148.9(5) . . ? M1 Li3 C3 32.02(17) . . ? C6 Li3 C3 64.3(3) . . ? C2 Li3 C3 31.03(18) . . ? C5 Li3 C3 54.6(2) . . ? N3 Li3 C4 156.6(5) . . ? M1 Li3 C4 32.48(17) . . ? C6 Li3 C4 55.1(2) . . ? C2 Li3 C4 55.2(2) . . ? C5 Li3 C4 30.83(19) . . ? C3 Li3 C4 30.69(19) . . ? N3 Li3 C1 97.0(4) . . ? M1 Li3 C1 33.49(16) . . ? C6 Li3 C1 31.89(18) . . ? C2 Li3 C1 31.45(18) . . ? C5 Li3 C1 56.3(2) . . ? C3 Li3 C1 56.0(2) . . ? C4 Li3 C1 66.0(3) . . ? N4 Li4 M2 131.1(5) . . ? N4 Li4 C15 103.2(4) . . ? M2 Li4 C15 33.01(17) . . ? N4 Li4 C14 127.5(4) . . ? M2 Li4 C14 32.85(17) . . ? C15 Li4 C14 31.40(19) . . ? N4 Li4 C10 98.9(4) . . ? M2 Li4 C10 34.09(16) . . ? C15 Li4 C10 32.48(18) . . ? C14 Li4 C10 57.2(2) . . ? N4 Li4 C11 120.1(4) . . ? M2 Li4 C11 32.38(17) . . ? C15 Li4 C11 56.0(2) . . ? C14 Li4 C11 65.2(3) . . ? C10 Li4 C11 31.77(18) . . ? N4 Li4 C12 151.0(5) . . ? M2 Li4 C12 31.70(17) . . ? C15 Li4 C12 64.7(3) . . ? C14 Li4 C12 54.9(3) . . ? C10 Li4 C12 56.2(2) . . ? C11 Li4 C12 30.91(19) . . ? N4 Li4 C13 157.9(5) . . ? M2 Li4 C13 32.10(18) . . ? C15 Li4 C13 55.3(3) . . ? C14 Li4 C13 30.9(2) . . ? C10 Li4 C13 66.2(3) . . ? C11 Li4 C13 55.1(2) . . ? C12 Li4 C13 30.6(2) . . ? N1 Si1 C7 107.6(2) . . ? N1 Si1 C9 111.2(2) . . ? C7 Si1 C9 107.3(3) . . ? N1 Si1 C8 116.6(2) . . ? C7 Si1 C8 106.7(3) . . ? C9 Si1 C8 106.8(3) . . ? N1 Si1 Li2 39.8(2) . . ? C7 Si1 Li2 69.7(2) . . ? C9 Si1 Li2 112.1(2) . . ? C8 Si1 Li2 140.2(2) . . ? N2 Si2 C16 111.4(2) . . ? N2 Si2 C18 107.5(2) . . ? C16 Si2 C18 106.7(2) . . ? N2 Si2 C17 116.2(2) . . ? C16 Si2 C17 107.4(2) . . ? C18 Si2 C17 107.3(2) . . ? N2 Si2 Li1 40.4(2) . . ? C16 Si2 Li1 111.8(2) . . ? C18 Si2 Li1 68.8(2) . . ? C17 Si2 Li1 140.0(2) . . ? N3 Si3 C25 107.0(2) . . ? N3 Si3 C26 116.3(2) . . ? C25 Si3 C26 107.5(2) . . ? N3 Si3 C27 112.9(2) . . ? C25 Si3 C27 107.1(2) . . ? C26 Si3 C27 105.6(2) . . ? N3 Si3 Li3 36.6(2) . . ? C25 Si3 Li3 74.0(2) . . ? C26 Si3 Li3 143.1(2) . . ? C27 Si3 Li3 109.0(3) . . ? N3 Si3 Li1 34.87(19) . . ? C25 Si3 Li1 101.5(2) . . ? C26 Si3 Li1 86.6(2) . . ? C27 Si3 Li1 143.4(2) . . ? Li3 Si3 Li1 57.8(2) . . ? N4 Si4 C34 106.4(2) . . ? N4 Si4 C36 112.8(2) . . ? C34 Si4 C36 107.6(3) . . ? N4 Si4 C35 117.0(2) . . ? C34 Si4 C35 107.1(3) . . ? C36 Si4 C35 105.5(2) . . ? N4 Si4 Li4 37.1(2) . . ? C34 Si4 Li4 72.8(2) . . ? C36 Si4 Li4 109.0(2) . . ? C35 Si4 Li4 143.7(2) . . ? C1 N1 Si1 120.8(3) . . ? C1 N1 Li2 121.9(4) . . ? Si1 N1 Li2 107.8(3) . . ? C1 N1 Li1 95.6(4) . . ? Si1 N1 Li1 127.0(3) . . ? Li2 N1 Li1 77.2(3) . . ? C10 N2 Si2 120.5(3) . . ? C10 N2 Li1 123.2(4) . . ? Si2 N2 Li1 106.6(3) . . ? C10 N2 Li2 98.0(3) . . ? Si2 N2 Li2 124.7(3) . . ? Li1 N2 Li2 77.3(3) . . ? C19 N3 Si3 119.8(3) . . ? C19 N3 Li3 114.5(4) . . ? Si3 N3 Li3 112.7(3) . . ? C19 N3 Li1 91.0(3) . . ? Si3 N3 Li1 118.1(3) . . ? Li3 N3 Li1 96.8(4) . . ? C28 N4 Si4 119.7(3) . . ? C28 N4 Li4 116.4(4) . . ? Si4 N4 Li4 111.2(3) . . ? C28 N4 Li2 90.1(3) . . ? Si4 N4 Li2 118.9(3) . . ? Li4 N4 Li2 96.9(4) . . ? N1 C1 C2 125.8(4) . . ? N1 C1 C6 120.0(4) . . ? C2 C1 C6 114.1(4) . . ? N1 C1 Li3 123.7(3) . . ? C2 C1 Li3 72.2(3) . . ? C6 C1 Li3 71.6(3) . . ? N1 C1 Li1 53.1(3) . . ? C2 C1 Li1 125.7(4) . . ? C6 C1 Li1 92.2(3) . . ? Li3 C1 Li1 72.9(3) . . ? C3 C2 C1 122.6(5) . . ? C3 C2 Li3 75.2(4) . . ? C1 C2 Li3 76.3(3) . . ? C4 C3 C2 120.9(5) . . ? C4 C3 Li3 75.3(4) . . ? C2 C3 Li3 73.7(4) . . ? C3 C4 C5 118.9(5) . . ? C3 C4 Li3 74.0(4) . . ? C5 C4 Li3 73.9(4) . . ? C6 C5 C4 120.4(5) . . ? C6 C5 Li3 73.4(3) . . ? C4 C5 Li3 75.3(4) . . ? C5 C6 C1 123.0(5) . . ? C5 C6 Li3 75.7(3) . . ? C1 C6 Li3 76.5(3) . . ? N2 C10 C11 125.5(4) . . ? N2 C10 C15 119.8(4) . . ? C11 C10 C15 114.7(4) . . ? N2 C10 Li4 122.2(3) . . ? C11 C10 Li4 74.3(3) . . ? C15 C10 Li4 70.7(3) . . ? N2 C10 Li2 51.2(3) . . ? C11 C10 Li2 127.0(4) . . ? C15 C10 Li2 92.2(3) . . ? Li4 C10 Li2 73.1(3) . . ? C12 C11 C10 121.9(5) . . ? C12 C11 Li4 76.1(4) . . ? C10 C11 Li4 73.9(3) . . ? C11 C12 C13 120.9(5) . . ? C11 C12 Li4 73.0(4) . . ? C13 C12 Li4 75.3(4) . . ? C14 C13 C12 119.0(5) . . ? C14 C13 Li4 71.6(4) . . ? C12 C13 Li4 74.1(4) . . ? C15 C14 C13 119.8(5) . . ? C15 C14 Li4 71.7(4) . . ? C13 C14 Li4 77.5(4) . . ? C14 C15 C10 123.6(5) . . ? C14 C15 Li4 76.9(4) . . ? C10 C15 Li4 76.8(3) . . ? Si2 C18 Li1 74.7(2) . . ? N3 C19 C20 121.6(4) . . ? N3 C19 C24 124.0(4) . . ? C20 C19 C24 114.4(5) . . ? N3 C19 Li1 56.4(3) . . ? C20 C19 Li1 101.0(4) . . ? C24 C19 Li1 111.5(4) . . ? N3 C19 Li3 39.3(3) . . ? C20 C19 Li3 83.5(3) . . ? C24 C19 Li3 160.8(4) . . ? Li1 C19 Li3 69.2(3) . . ? C21 C20 C19 123.1(5) . . ? C22 C21 C20 120.4(5) . . ? C22 C21 Li3 92.6(4) . 2_666 ? C20 C21 Li3 88.8(4) . 2_666 ? C23 C22 C21 118.4(5) . . ? C22 C23 C24 121.6(5) . . ? C23 C24 C19 122.2(5) . . ? N4 C28 C29 125.1(4) . . ? N4 C28 C33 120.1(4) . . ? C29 C28 C33 114.7(5) . . ? N4 C28 Li2 57.4(3) . . ? C29 C28 Li2 111.4(4) . . ? C33 C28 Li2 100.3(3) . . ? N4 C28 Li4 38.0(3) . . ? C29 C28 Li4 160.9(4) . . ? C33 C28 Li4 83.2(3) . . ? Li2 C28 Li4 69.2(3) . . ? C30 C29 C28 122.6(5) . . ? C29 C30 C31 120.4(6) . . ? C32 C31 C30 119.1(5) . . ? C31 C32 C33 120.7(5) . . ? C31 C32 Li4 93.9(4) . 2_655 ? C33 C32 Li4 87.4(4) . 2_655 ? C32 C33 C28 122.4(5) . . ? #===END