Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Barbara Gehrhus' 'P. B. Hitchcock' 'Massimo Parruci' _publ_contact_author_name 'Dr Barbara Gehrhus' _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton UK BN1 9QJ UK ; _publ_contact_author_email B.GEHRHUS@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Reaction of the stable silylene Si[(NCH2-t-Bu)2C6H4-1,2] with lithium amides ; _publ_requested_category FM data_(2)-oct2700 _database_code_depnum_ccdc_archive 'CCDC 271590' _audit_creation_date 2000-10-18T10:43:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; [C6H4(NCH2tBu)2Si(SiMe3){N(tBu)(Li(thf)2)}] ; _chemical_formula_moiety 'C31 H60 Li N3 O2 Si2' _chemical_formula_sum 'C31 H60 Li N3 O2 Si2' _chemical_formula_weight 569.94 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2837(8) _cell_length_b 11.1486(6) _cell_length_c 19.2661(7) _cell_angle_alpha 90 _cell_angle_beta 115.341(3) _cell_angle_gamma 90 _cell_volume 3549.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12836 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.128 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 21308 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_unetI/netI 0.0757 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 6248 _reflns_number_gt 4326 _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^)+(0.0541P)^2^+2.1801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6248 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.258 _refine_diff_density_min -0.26 _refine_diff_density_rms 0.047 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 Si1 Si 0.24768(4) 0.48037(6) 0.24467(4) 0.02517(19) Uani 1 1 d . . . Si2 Si 0.20933(5) 0.57908(7) 0.12425(4) 0.0350(2) Uani 1 1 d . . . O1 O 0.32471(13) 0.27704(18) 0.43807(11) 0.0527(6) Uani 1 1 d . . . O2 O 0.20081(14) 0.43729(18) 0.45584(12) 0.0514(6) Uani 1 1 d . . . N1 N 0.17602(12) 0.36682(18) 0.23718(11) 0.0274(5) Uani 1 1 d . . . N2 N 0.31297(12) 0.36592(18) 0.23805(11) 0.0284(5) Uani 1 1 d . . . N3 N 0.27278(12) 0.55064(18) 0.32709(11) 0.0291(5) Uani 1 1 d . . . C1 C 0.19846(15) 0.2533(2) 0.22187(13) 0.0276(6) Uani 1 1 d . . . C2 C 0.27575(15) 0.2536(2) 0.22062(13) 0.0277(6) Uani 1 1 d . . . C3 C 0.30550(16) 0.1476(2) 0.20497(15) 0.0352(6) Uani 1 1 d . . . H3 H 0.3557 0.1474 0.2013 0.042 Uiso 1 1 calc R . . C4 C 0.26195(18) 0.0411(2) 0.19466(17) 0.0434(7) Uani 1 1 d . . . H4 H 0.283 -0.0312 0.1843 0.052 Uiso 1 1 calc R . . C5 C 0.18939(18) 0.0395(2) 0.19925(17) 0.0440(7) Uani 1 1 d . . . H5 H 0.161 -0.0339 0.1936 0.053 Uiso 1 1 calc R . . C6 C 0.15703(17) 0.1464(2) 0.21233(16) 0.0372(7) Uani 1 1 d . . . H6 H 0.1062 0.1454 0.2147 0.045 Uiso 1 1 calc R . . C7 C 0.11103(15) 0.3777(2) 0.26201(15) 0.0333(6) Uani 1 1 d . . . H7A H 0.128 0.4387 0.3033 0.04 Uiso 1 1 calc R . . H7B H 0.1074 0.3002 0.2855 0.04 Uiso 1 1 calc R . . C8 C 0.02512(15) 0.4107(2) 0.20275(16) 0.0371(7) Uani 1 1 d . . . C9 C 0.02656(18) 0.5344(3) 0.1697(2) 0.0529(8) Uani 1 1 d . . . H9A H 0.0483 0.593 0.2115 0.079 Uiso 1 1 calc R . . H9B H -0.0286 0.5575 0.1341 0.079 Uiso 1 1 calc R . . H9C H 0.0608 0.5322 0.1421 0.079 Uiso 1 1 calc R . . C10 C -0.02819(18) 0.4148(3) 0.2459(2) 0.0582(9) Uani 1 1 d . . . H10A H -0.0289 0.3356 0.2676 0.087 Uiso 1 1 calc R . . H10B H -0.0834 0.4375 0.2103 0.087 Uiso 1 1 calc R . . H10C H -0.0065 0.474 0.2874 0.087 Uiso 1 1 calc R . . C11 C -0.00936(18) 0.3189(3) 0.13767(17) 0.0518(8) Uani 1 1 d . . . H11A H -0.0102 0.2395 0.1591 0.078 Uiso 1 1 calc R . . H11B H 0.0246 0.3164 0.1098 0.078 Uiso 1 1 calc R . . H11C H -0.0646 0.3421 0.1024 0.078 Uiso 1 1 calc R . . C12 C 0.39028(15) 0.3863(2) 0.23443(16) 0.0370(7) Uani 1 1 d . . . H12A H 0.3904 0.4699 0.217 0.044 Uiso 1 1 calc R . . H12B H 0.3922 0.333 0.1942 0.044 Uiso 1 1 calc R . . C13 C 0.46918(16) 0.3673(3) 0.30799(17) 0.0418(7) Uani 1 1 d . . . C14 C 0.4728(2) 0.4565(4) 0.3686(2) 0.1009(18) Uani 1 1 d . . . H14A H 0.4277 0.4417 0.3823 0.151 Uiso 1 1 calc R . . H14B H 0.4687 0.5381 0.3485 0.151 Uiso 1 1 calc R . . H14C H 0.5241 0.4473 0.4143 0.151 Uiso 1 1 calc R . . C15 C 0.5391(2) 0.3907(4) 0.2868(3) 0.0875(14) Uani 1 1 d . . . H15A H 0.5369 0.3332 0.2474 0.131 Uiso 1 1 calc R . . H15B H 0.5905 0.3815 0.3325 0.131 Uiso 1 1 calc R . . H15C H 0.535 0.4725 0.2668 0.131 Uiso 1 1 calc R . . C16 C 0.47758(19) 0.2424(3) 0.34048(19) 0.0588(9) Uani 1 1 d . . . H16A H 0.4759 0.184 0.3018 0.088 Uiso 1 1 calc R . . H16B H 0.433 0.2265 0.3547 0.088 Uiso 1 1 calc R . . H16C H 0.5293 0.2354 0.3861 0.088 Uiso 1 1 calc R . . C17 C 0.1449(2) 0.7182(3) 0.10392(17) 0.0488(8) Uani 1 1 d . . . H17A H 0.1735 0.7795 0.1425 0.073 Uiso 1 1 calc R . . H17B H 0.0936 0.6987 0.1059 0.073 Uiso 1 1 calc R . . H17C H 0.1342 0.7487 0.0528 0.073 Uiso 1 1 calc R . . C18 C 0.2966(2) 0.6262(3) 0.10305(19) 0.0626(10) Uani 1 1 d . . . H18A H 0.3338 0.5586 0.1122 0.094 Uiso 1 1 calc R . . H18B H 0.3253 0.6932 0.1366 0.094 Uiso 1 1 calc R . . H18C H 0.2761 0.6515 0.0493 0.094 Uiso 1 1 calc R . . C19 C 0.1533(2) 0.4630(3) 0.04950(16) 0.0597(10) Uani 1 1 d . . . H19A H 0.1862 0.39 0.0595 0.089 Uiso 1 1 calc R . . H19B H 0.1426 0.4941 -0.0015 0.089 Uiso 1 1 calc R . . H19C H 0.1019 0.4443 0.0515 0.089 Uiso 1 1 calc R . . C20 C 0.29283(15) 0.6755(2) 0.34981(14) 0.0306(6) Uani 1 1 d . . . C21 C 0.33906(17) 0.7375(2) 0.30976(16) 0.0417(7) Uani 1 1 d . . . H21A H 0.3884 0.6921 0.3193 0.063 Uiso 1 1 calc R . . H21B H 0.3536 0.8191 0.3299 0.063 Uiso 1 1 calc R . . H21C H 0.3048 0.741 0.2544 0.063 Uiso 1 1 calc R . . C22 C 0.21667(17) 0.7491(3) 0.33296(18) 0.0438(7) Uani 1 1 d . . . H22A H 0.1819 0.7481 0.2776 0.066 Uiso 1 1 calc R . . H22B H 0.2319 0.832 0.3499 0.066 Uiso 1 1 calc R . . H22C H 0.1874 0.7145 0.3605 0.066 Uiso 1 1 calc R . . C23 C 0.34655(18) 0.6791(3) 0.43664(15) 0.0444(7) Uani 1 1 d . . . H23A H 0.3957 0.6321 0.4484 0.067 Uiso 1 1 calc R . . H23B H 0.3169 0.6452 0.464 0.067 Uiso 1 1 calc R . . H23C H 0.3613 0.7624 0.4529 0.067 Uiso 1 1 calc R . . C24 C 0.3084(2) 0.1553(3) 0.41352(19) 0.0586(9) Uani 1 1 d . . . H24A H 0.3038 0.1469 0.3606 0.07 Uiso 1 1 calc R . . H24B H 0.257 0.1288 0.414 0.07 Uiso 1 1 calc R . . C25 C 0.3761(3) 0.0824(4) 0.4671(3) 0.1016(16) Uani 1 1 d . . . H25A H 0.3556 0.0141 0.4864 0.122 Uiso 1 1 calc R . . H25B H 0.4085 0.0506 0.4411 0.122 Uiso 1 1 calc R . . C26 C 0.4244(3) 0.1597(4) 0.5289(3) 0.1097(18) Uani 1 1 d . . . H26A H 0.4805 0.1619 0.5338 0.132 Uiso 1 1 calc R . . H26B H 0.4257 0.1292 0.5777 0.132 Uiso 1 1 calc R . . C27 C 0.3902(3) 0.2777(4) 0.5137(2) 0.0903(14) Uani 1 1 d . . . H27A H 0.4317 0.3369 0.5165 0.108 Uiso 1 1 calc R . . H27B H 0.37 0.2997 0.5522 0.108 Uiso 1 1 calc R . . C28 C 0.1749(2) 0.3333(3) 0.4839(2) 0.0639(10) Uani 1 1 d . . . H28A H 0.2145 0.3141 0.5369 0.077 Uiso 1 1 calc R . . H28B H 0.17 0.2631 0.4507 0.077 Uiso 1 1 calc R . . C29 C 0.0958(3) 0.3625(3) 0.4825(3) 0.0846(13) Uani 1 1 d . . . H29A H 0.0923 0.3313 0.529 0.102 Uiso 1 1 calc R . . H29B H 0.0515 0.3268 0.4367 0.102 Uiso 1 1 calc R . . C30 C 0.0899(2) 0.4973(3) 0.4798(2) 0.0646(10) Uani 1 1 d . . . H30A H 0.0404 0.524 0.4351 0.077 Uiso 1 1 calc R . . H30B H 0.0888 0.5291 0.5273 0.077 Uiso 1 1 calc R . . C31 C 0.1638(3) 0.5385(3) 0.4725(3) 0.0914(15) Uani 1 1 d . . . H31A H 0.1491 0.5984 0.4308 0.11 Uiso 1 1 calc R . . H31B H 0.2018 0.5764 0.5211 0.11 Uiso 1 1 calc R . . Li Li 0.2654(3) 0.4289(4) 0.3967(3) 0.0436(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0237(3) 0.0231(4) 0.0279(4) 0.0000(3) 0.0103(3) -0.0004(3) Si2 0.0450(5) 0.0282(4) 0.0305(4) 0.0025(3) 0.0149(3) 0.0013(3) O1 0.0593(13) 0.0410(13) 0.0488(12) 0.0095(10) 0.0146(11) 0.0035(10) O2 0.0732(15) 0.0424(12) 0.0542(12) 0.0044(10) 0.0420(12) -0.0030(11) N1 0.0249(11) 0.0252(12) 0.0342(11) -0.0015(9) 0.0146(10) -0.0003(9) N2 0.0250(11) 0.0266(12) 0.0362(12) -0.0014(9) 0.0155(10) -0.0015(9) N3 0.0308(12) 0.0241(11) 0.0313(11) -0.0015(9) 0.0123(10) -0.0030(9) C1 0.0285(14) 0.0269(14) 0.0263(13) 0.0000(11) 0.0107(11) 0.0015(11) C2 0.0299(14) 0.0245(14) 0.0265(13) 0.0004(11) 0.0101(11) 0.0022(11) C3 0.0333(15) 0.0333(16) 0.0403(15) -0.0019(12) 0.0171(13) 0.0052(12) C4 0.0464(18) 0.0273(16) 0.0548(18) -0.0048(13) 0.0201(15) 0.0043(13) C5 0.0436(18) 0.0250(16) 0.0612(19) -0.0021(13) 0.0203(15) -0.0042(13) C6 0.0335(15) 0.0281(15) 0.0489(16) 0.0009(13) 0.0166(13) -0.0022(12) C7 0.0288(14) 0.0336(15) 0.0395(15) -0.0057(12) 0.0165(12) -0.0026(12) C8 0.0227(13) 0.0337(16) 0.0513(17) -0.0065(13) 0.0123(13) -0.0024(12) C9 0.0358(16) 0.0407(18) 0.072(2) 0.0030(16) 0.0131(16) 0.0030(14) C10 0.0338(17) 0.062(2) 0.083(2) -0.0133(19) 0.0289(17) -0.0044(16) C11 0.0362(16) 0.0476(19) 0.0536(18) -0.0120(15) 0.0021(14) 0.0003(14) C12 0.0341(15) 0.0340(16) 0.0497(17) 0.0023(13) 0.0244(14) 0.0011(12) C13 0.0239(14) 0.0373(16) 0.0629(19) -0.0042(14) 0.0175(14) 0.0008(12) C14 0.049(2) 0.105(4) 0.097(3) -0.056(3) -0.018(2) 0.026(2) C15 0.038(2) 0.090(3) 0.136(4) 0.043(3) 0.039(2) 0.0050(19) C16 0.0398(18) 0.062(2) 0.060(2) 0.0141(17) 0.0072(16) -0.0013(16) C17 0.064(2) 0.0337(17) 0.0448(17) 0.0083(14) 0.0196(16) 0.0058(15) C18 0.072(2) 0.070(2) 0.057(2) 0.0167(18) 0.0387(19) 0.0027(19) C19 0.090(3) 0.0419(19) 0.0334(16) -0.0021(14) 0.0137(17) 0.0020(18) C20 0.0327(14) 0.0243(14) 0.0325(14) -0.0041(11) 0.0116(12) -0.0025(11) C21 0.0445(17) 0.0312(16) 0.0524(18) -0.0052(13) 0.0237(15) -0.0093(13) C22 0.0412(16) 0.0348(17) 0.0566(18) -0.0024(14) 0.0220(15) 0.0040(13) C23 0.0492(18) 0.0384(17) 0.0388(15) -0.0090(13) 0.0123(14) -0.0031(14) C24 0.069(2) 0.050(2) 0.056(2) -0.0038(17) 0.0255(18) -0.0043(18) C25 0.148(4) 0.053(3) 0.077(3) 0.022(2) 0.023(3) 0.024(3) C26 0.103(4) 0.089(4) 0.090(3) 0.022(3) -0.004(3) 0.015(3) C27 0.094(3) 0.074(3) 0.060(2) -0.011(2) -0.008(2) 0.004(2) C28 0.090(3) 0.048(2) 0.067(2) 0.0135(17) 0.046(2) -0.0075(19) C29 0.104(3) 0.058(3) 0.131(4) -0.003(2) 0.088(3) -0.011(2) C30 0.079(3) 0.058(2) 0.075(2) 0.0022(19) 0.049(2) -0.0024(19) C31 0.137(4) 0.043(2) 0.153(4) -0.013(2) 0.119(4) -0.008(2) Li 0.050(3) 0.037(3) 0.050(3) 0.008(2) 0.027(2) 0.003(2) #----------------------------------------------------------------------------# # 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 Si1 N3 1.650(2) . ? Si1 N1 1.783(2) . ? Si1 N2 1.789(2) . ? Si1 Si2 2.3859(10) . ? Si2 C19 1.880(3) . ? Si2 C18 1.883(3) . ? Si2 C17 1.884(3) . ? O1 C24 1.426(4) . ? O1 C27 1.437(4) . ? O1 Li 1.985(5) . ? O2 C31 1.422(4) . ? O2 C28 1.442(4) . ? O2 Li 1.962(5) . ? N1 C1 1.401(3) . ? N1 C7 1.463(3) . ? N2 C2 1.396(3) . ? N2 C12 1.463(3) . ? N3 C20 1.458(3) . ? N3 Li 1.953(5) . ? C1 C6 1.381(4) . ? C1 C2 1.424(4) . ? C2 C3 1.387(3) . ? C3 C4 1.395(4) . ? C4 C5 1.367(4) . ? C5 C6 1.400(4) . ? C7 C8 1.540(4) . ? C8 C9 1.525(4) . ? C8 C10 1.528(4) . ? C8 C11 1.530(4) . ? C12 C13 1.544(4) . ? C13 C16 1.507(4) . ? C13 C14 1.514(4) . ? C13 C15 1.523(4) . ? C20 C22 1.527(4) . ? C20 C21 1.532(4) . ? C20 C23 1.536(4) . ? C24 C25 1.471(5) . ? C25 C26 1.428(6) . ? C26 C27 1.432(6) . ? C28 C29 1.470(5) . ? C29 C30 1.507(5) . ? C30 C31 1.489(5) . ? 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 Si1 N1 107.88(10) . . ? N3 Si1 N2 119.22(10) . . ? N1 Si1 N2 88.71(9) . . ? N3 Si1 Si2 124.18(8) . . ? N1 Si1 Si2 110.42(7) . . ? N2 Si1 Si2 100.78(7) . . ? C19 Si2 C18 105.10(17) . . ? C19 Si2 C17 108.66(15) . . ? C18 Si2 C17 103.74(15) . . ? C19 Si2 Si1 105.32(10) . . ? C18 Si2 Si1 114.58(11) . . ? C17 Si2 Si1 118.63(10) . . ? C24 O1 C27 107.8(3) . . ? C24 O1 Li 132.7(2) . . ? C27 O1 Li 118.6(3) . . ? C31 O2 C28 106.8(2) . . ? C31 O2 Li 129.2(2) . . ? C28 O2 Li 123.7(2) . . ? C1 N1 C7 119.7(2) . . ? C1 N1 Si1 112.80(16) . . ? C7 N1 Si1 125.89(16) . . ? C2 N2 C12 120.6(2) . . ? C2 N2 Si1 112.68(16) . . ? C12 N2 Si1 125.49(17) . . ? C20 N3 Si1 132.29(17) . . ? C20 N3 Li 122.7(2) . . ? Si1 N3 Li 104.98(18) . . ? C6 C1 N1 127.9(2) . . ? C6 C1 C2 119.5(2) . . ? N1 C1 C2 112.6(2) . . ? C3 C2 N2 128.4(2) . . ? C3 C2 C1 119.1(2) . . ? N2 C2 C1 112.6(2) . . ? C2 C3 C4 120.2(3) . . ? C5 C4 C3 120.8(3) . . ? C4 C5 C6 119.8(3) . . ? C1 C6 C5 120.5(3) . . ? N1 C7 C8 119.4(2) . . ? C9 C8 C10 109.2(3) . . ? C9 C8 C11 109.7(3) . . ? C10 C8 C11 109.3(2) . . ? C9 C8 C7 109.4(2) . . ? C10 C8 C7 106.8(2) . . ? C11 C8 C7 112.3(2) . . ? N2 C12 C13 118.5(2) . . ? C16 C13 C14 108.9(3) . . ? C16 C13 C15 108.8(3) . . ? C14 C13 C15 109.3(3) . . ? C16 C13 C12 113.4(2) . . ? C14 C13 C12 109.4(2) . . ? C15 C13 C12 107.0(3) . . ? N3 C20 C22 111.1(2) . . ? N3 C20 C21 113.7(2) . . ? C22 C20 C21 107.4(2) . . ? N3 C20 C23 108.3(2) . . ? C22 C20 C23 108.5(2) . . ? C21 C20 C23 107.7(2) . . ? O1 C24 C25 107.4(3) . . ? C26 C25 C24 106.6(3) . . ? C25 C26 C27 108.9(4) . . ? C26 C27 O1 107.7(3) . . ? O2 C28 C29 107.0(3) . . ? C28 C29 C30 106.1(3) . . ? C31 C30 C29 104.8(3) . . ? O2 C31 C30 108.4(3) . . ? N3 Li O2 127.0(3) . . ? N3 Li O1 133.0(3) . . ? O2 Li O1 99.7(2) . . ? N3 Li Si1 33.81(10) . . ? O2 Li Si1 138.7(2) . . ? O1 Li Si1 112.6(2) . . ? #===END data_(3)-oct2400 _database_code_depnum_ccdc_archive 'CCDC 271591' _audit_creation_date 2000-10-17T09:52:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[C6H4(NCH2tBu)2Si(Li(thf)2}{N(SiMe3)(C6H3Me2)}]' ; _chemical_formula_moiety 'C35 H60 Li N3 O2 Si2' _chemical_formula_sum 'C35 H60 Li N3 O2 Si2' _chemical_formula_weight 617.98 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2629(10) _cell_length_b 19.5814(7) _cell_length_c 21.4761(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7680.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14679 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _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 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 20489 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_unetI/netI 0.059 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 22.98 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 5293 _reflns_number_gt 3844 _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^)+(0.0922P)^2^+7.2912P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5293 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.062 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.631 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 Li Li 0.4185(5) 0.0344(3) 0.7265(3) 0.066(2) Uani 1 1 d . . . Si1 Si 0.42786(5) 0.14762(4) 0.66142(4) 0.0320(3) Uani 1 1 d . . . Si2 Si 0.56527(6) 0.20109(5) 0.57872(4) 0.0393(3) Uani 1 1 d . . . O1 O 0.38639(17) -0.05544(13) 0.70448(17) 0.0752(10) Uani 1 1 d . . . O2 O 0.4434(2) 0.02194(16) 0.81429(15) 0.0816(10) Uani 1 1 d . . . N1 N 0.41076(15) 0.22811(13) 0.69931(12) 0.0333(7) Uani 1 1 d . . . N2 N 0.37531(15) 0.18175(13) 0.59778(12) 0.0350(7) Uani 1 1 d . . . N3 N 0.52173(15) 0.14792(13) 0.63214(12) 0.0346(7) Uani 1 1 d . . . C1 C 0.38819(18) 0.27948(16) 0.65884(16) 0.0354(8) Uani 1 1 d . . . C2 C 0.36711(18) 0.25275(17) 0.60002(15) 0.0357(8) Uani 1 1 d . . . C3 C 0.3430(2) 0.2971(2) 0.55381(17) 0.0476(10) Uani 1 1 d . . . H3 H 0.3277 0.2796 0.5146 0.057 Uiso 1 1 calc R . . C4 C 0.3411(2) 0.3673(2) 0.5649(2) 0.0591(12) Uani 1 1 d . . . H4 H 0.3252 0.3975 0.533 0.071 Uiso 1 1 calc R . . C5 C 0.3620(2) 0.3931(2) 0.6214(2) 0.0556(11) Uani 1 1 d . . . H5 H 0.3604 0.4409 0.6285 0.067 Uiso 1 1 calc R . . C6 C 0.3858(2) 0.34949(18) 0.66869(18) 0.0451(9) Uani 1 1 d . . . H6 H 0.4003 0.3678 0.7077 0.054 Uiso 1 1 calc R . . C7 C 0.42224(19) 0.24185(18) 0.76492(15) 0.0379(8) Uani 1 1 d . . . H7A H 0.4425 0.2886 0.769 0.045 Uiso 1 1 calc R . . H7B H 0.4598 0.2097 0.7806 0.045 Uiso 1 1 calc R . . C8 C 0.3545(2) 0.23631(18) 0.80735(15) 0.0405(9) Uani 1 1 d . . . C9 C 0.3220(2) 0.16475(19) 0.80285(18) 0.0517(10) Uani 1 1 d . . . H9A H 0.305 0.1565 0.7602 0.078 Uiso 1 1 calc R . . H9B H 0.2807 0.1607 0.8317 0.078 Uiso 1 1 calc R . . H9C H 0.3595 0.131 0.8137 0.078 Uiso 1 1 calc R . . C10 C 0.3806(3) 0.2492(3) 0.87406(18) 0.0743(14) Uani 1 1 d . . . H10A H 0.4016 0.2952 0.877 0.111 Uiso 1 1 calc R . . H10B H 0.4178 0.2154 0.8852 0.111 Uiso 1 1 calc R . . H10C H 0.339 0.2454 0.9027 0.111 Uiso 1 1 calc R . . C11 C 0.2957(2) 0.2887(2) 0.7909(2) 0.0548(11) Uani 1 1 d . . . H11A H 0.278 0.2802 0.7486 0.082 Uiso 1 1 calc R . . H11B H 0.3165 0.3348 0.7934 0.082 Uiso 1 1 calc R . . H11C H 0.2549 0.2848 0.8203 0.082 Uiso 1 1 calc R . . C12 C 0.3514(2) 0.14368(19) 0.54286(16) 0.0445(9) Uani 1 1 d . . . H12A H 0.3852 0.1047 0.5367 0.053 Uiso 1 1 calc R . . H12B H 0.3561 0.1738 0.5061 0.053 Uiso 1 1 calc R . . C13 C 0.2721(2) 0.1157(2) 0.54474(19) 0.0575(11) Uani 1 1 d . . . C14 C 0.2167(3) 0.1712(3) 0.5562(4) 0.118(2) Uani 1 1 d . . . H14A H 0.2204 0.2056 0.5232 0.177 Uiso 1 1 calc R . . H14B H 0.2263 0.1925 0.5966 0.177 Uiso 1 1 calc R . . H14C H 0.1674 0.1514 0.5561 0.177 Uiso 1 1 calc R . . C15 C 0.2668(3) 0.0622(3) 0.5941(3) 0.105(2) Uani 1 1 d . . . H15A H 0.3028 0.0262 0.5859 0.158 Uiso 1 1 calc R . . H15B H 0.2175 0.0424 0.5939 0.158 Uiso 1 1 calc R . . H15C H 0.2766 0.0828 0.6348 0.158 Uiso 1 1 calc R . . C16 C 0.2588(4) 0.0831(5) 0.4816(3) 0.150(3) Uani 1 1 d . . . H16A H 0.2613 0.1181 0.4491 0.225 Uiso 1 1 calc R . . H16B H 0.2103 0.0617 0.4811 0.225 Uiso 1 1 calc R . . H16C H 0.2963 0.0483 0.4738 0.225 Uiso 1 1 calc R . . C17 C 0.6588(2) 0.1667(2) 0.5621(2) 0.0583(11) Uani 1 1 d . . . H17A H 0.6863 0.1628 0.6011 0.087 Uiso 1 1 calc R . . H17B H 0.6845 0.1978 0.5338 0.087 Uiso 1 1 calc R . . H17C H 0.6545 0.1216 0.5427 0.087 Uiso 1 1 calc R . . C18 C 0.5175(2) 0.2066(2) 0.50240(17) 0.0563(11) Uani 1 1 d . . . H18A H 0.5112 0.1606 0.4853 0.084 Uiso 1 1 calc R . . H18B H 0.5468 0.2342 0.4736 0.084 Uiso 1 1 calc R . . H18C H 0.4695 0.228 0.5082 0.084 Uiso 1 1 calc R . . C19 C 0.5743(3) 0.29088(19) 0.6069(2) 0.0614(12) Uani 1 1 d . . . H19A H 0.5992 0.2912 0.6473 0.092 Uiso 1 1 calc R . . H19B H 0.5256 0.3112 0.6112 0.092 Uiso 1 1 calc R . . H19C H 0.603 0.3174 0.5768 0.092 Uiso 1 1 calc R . . C20 C 0.56658(19) 0.09514(18) 0.65973(15) 0.0383(8) Uani 1 1 d . . . C21 C 0.5665(2) 0.02891(19) 0.63460(18) 0.0494(10) Uani 1 1 d . . . C22 C 0.6101(3) -0.0211(2) 0.6611(2) 0.0642(12) Uani 1 1 d . . . H22 H 0.6095 -0.0659 0.644 0.077 Uiso 1 1 calc R . . C23 C 0.6538(3) -0.0079(2) 0.7111(2) 0.0689(13) Uani 1 1 d . . . H23 H 0.6837 -0.0427 0.7284 0.083 Uiso 1 1 calc R . . C24 C 0.6540(2) 0.0564(2) 0.7359(2) 0.0598(11) Uani 1 1 d . . . H24 H 0.6843 0.0658 0.7708 0.072 Uiso 1 1 calc R . . C25 C 0.6107(2) 0.10885(19) 0.71130(16) 0.0441(9) Uani 1 1 d . . . C26 C 0.5218(3) 0.0124(2) 0.5779(2) 0.0648(12) Uani 1 1 d . . . H26A H 0.5324 -0.0344 0.5645 0.097 Uiso 1 1 calc R . . H26B H 0.5341 0.0443 0.5444 0.097 Uiso 1 1 calc R . . H26C H 0.4696 0.0164 0.588 0.097 Uiso 1 1 calc R . . C27 C 0.6143(2) 0.1788(2) 0.73967(18) 0.0511(10) Uani 1 1 d . . . H27A H 0.6531 0.2052 0.7194 0.077 Uiso 1 1 calc R . . H27B H 0.6249 0.1748 0.7843 0.077 Uiso 1 1 calc R . . H27C H 0.5672 0.202 0.7339 0.077 Uiso 1 1 calc R . . C28 C 0.3186(3) -0.0832(3) 0.6848(4) 0.109(2) Uani 1 1 d . . . H28A H 0.2899 -0.0488 0.6615 0.131 Uiso 1 1 calc R . . H28B H 0.2896 -0.0989 0.721 0.131 Uiso 1 1 calc R . . C29 C 0.3379(3) -0.1418(3) 0.6437(3) 0.1015(19) Uani 1 1 d . . . H29A H 0.303 -0.18 0.6495 0.122 Uiso 1 1 calc R . . H29B H 0.3376 -0.1279 0.5994 0.122 Uiso 1 1 calc R . . C30 C 0.4114(4) -0.1616(3) 0.6634(3) 0.102(2) Uani 1 1 d . . . H30A H 0.4103 -0.2071 0.6835 0.122 Uiso 1 1 calc R . . H30B H 0.4446 -0.1638 0.627 0.122 Uiso 1 1 calc R . . C31 C 0.4361(3) -0.1118(2) 0.7061(3) 0.097(2) Uani 1 1 d . . . H31A H 0.4859 -0.0964 0.6946 0.117 Uiso 1 1 calc R . . H31B H 0.438 -0.1313 0.7486 0.117 Uiso 1 1 calc R . . C32 C 0.4011(5) -0.0165(3) 0.8577(3) 0.137(3) Uani 1 1 d . . . H32A H 0.4024 -0.0658 0.8476 0.165 Uiso 1 1 calc R . . H32B H 0.3496 -0.0008 0.8582 0.165 Uiso 1 1 calc R . . C33 C 0.4378(8) -0.0026(6) 0.9186(4) 0.227(7) Uani 1 1 d . . . H33A H 0.4004 0.0111 0.9496 0.273 Uiso 1 1 calc R . . H33B H 0.4614 -0.045 0.9337 0.273 Uiso 1 1 calc R . . C34 C 0.4922(5) 0.0504(5) 0.9139(3) 0.138(3) Uani 1 1 d . . . H34A H 0.5374 0.0375 0.9366 0.165 Uiso 1 1 calc R . . H34B H 0.4735 0.094 0.9312 0.165 Uiso 1 1 calc R . . C35 C 0.5062(4) 0.0566(4) 0.8481(3) 0.127(3) Uani 1 1 d . . . H35A H 0.5532 0.0344 0.8373 0.152 Uiso 1 1 calc R . . H35B H 0.509 0.1054 0.8361 0.152 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 Li 0.096(6) 0.045(4) 0.058(4) 0.011(3) 0.003(4) -0.003(4) Si1 0.0388(6) 0.0314(5) 0.0257(5) 0.0016(4) -0.0010(4) -0.0005(4) Si2 0.0394(6) 0.0455(6) 0.0332(6) 0.0051(4) 0.0027(4) 0.0003(4) O1 0.063(2) 0.0390(15) 0.123(3) 0.0095(17) -0.0090(19) -0.0015(14) O2 0.117(3) 0.069(2) 0.058(2) 0.0271(17) 0.005(2) 0.012(2) N1 0.0399(17) 0.0361(15) 0.0238(14) 0.0008(12) 0.0009(12) 0.0012(12) N2 0.0412(17) 0.0363(16) 0.0276(14) -0.0022(12) -0.0014(13) 0.0010(13) N3 0.0388(17) 0.0351(15) 0.0299(15) 0.0022(12) -0.0018(13) 0.0038(12) C1 0.035(2) 0.0352(19) 0.0363(19) 0.0032(16) 0.0062(16) 0.0009(15) C2 0.038(2) 0.038(2) 0.0304(18) 0.0050(16) 0.0051(16) 0.0018(16) C3 0.051(2) 0.057(2) 0.0344(19) 0.0118(19) 0.0005(18) 0.0062(18) C4 0.063(3) 0.050(3) 0.065(3) 0.022(2) 0.010(2) 0.016(2) C5 0.060(3) 0.038(2) 0.069(3) 0.011(2) 0.014(2) 0.0060(19) C6 0.048(2) 0.039(2) 0.049(2) 0.0002(18) 0.0082(19) 0.0007(17) C7 0.040(2) 0.0401(19) 0.0338(19) -0.0063(16) -0.0029(16) -0.0050(16) C8 0.046(2) 0.046(2) 0.0296(18) -0.0031(16) 0.0029(16) -0.0039(17) C9 0.055(2) 0.051(2) 0.049(2) 0.0046(19) 0.016(2) -0.0054(19) C10 0.085(3) 0.107(4) 0.031(2) -0.012(2) 0.004(2) -0.003(3) C11 0.050(3) 0.055(2) 0.060(3) -0.001(2) 0.019(2) 0.0006(19) C12 0.048(2) 0.055(2) 0.0314(19) -0.0034(17) -0.0069(17) -0.0017(18) C13 0.054(3) 0.072(3) 0.047(2) 0.004(2) -0.012(2) -0.019(2) C14 0.040(3) 0.100(4) 0.213(8) 0.022(5) -0.008(4) -0.012(3) C15 0.094(4) 0.106(4) 0.116(5) 0.041(4) -0.019(4) -0.053(4) C16 0.117(6) 0.234(9) 0.099(5) -0.067(5) -0.015(4) -0.087(6) C17 0.048(3) 0.073(3) 0.054(2) 0.015(2) 0.005(2) 0.007(2) C18 0.053(3) 0.078(3) 0.038(2) 0.019(2) 0.0034(19) 0.001(2) C19 0.073(3) 0.044(2) 0.067(3) 0.005(2) 0.011(2) -0.012(2) C20 0.038(2) 0.042(2) 0.0348(19) 0.0051(16) 0.0018(16) 0.0016(16) C21 0.055(2) 0.044(2) 0.049(2) -0.0018(19) -0.0039(19) 0.0058(19) C22 0.071(3) 0.045(2) 0.077(3) 0.003(2) -0.005(3) 0.012(2) C23 0.069(3) 0.053(3) 0.085(3) 0.022(3) -0.015(3) 0.011(2) C24 0.051(3) 0.073(3) 0.056(3) 0.021(2) -0.013(2) 0.002(2) C25 0.041(2) 0.053(2) 0.038(2) 0.0069(18) -0.0016(17) -0.0049(17) C26 0.083(3) 0.047(2) 0.064(3) -0.017(2) -0.010(2) 0.011(2) C27 0.048(2) 0.062(3) 0.043(2) -0.0023(19) -0.0070(19) -0.0090(19) C28 0.060(3) 0.068(3) 0.198(7) 0.000(4) -0.011(4) 0.005(3) C29 0.096(4) 0.103(4) 0.106(4) -0.018(4) -0.033(4) 0.011(3) C30 0.114(5) 0.098(4) 0.092(4) -0.030(3) -0.026(4) 0.040(4) C31 0.071(3) 0.057(3) 0.164(6) -0.003(4) -0.030(4) 0.016(3) C32 0.240(9) 0.100(5) 0.072(4) 0.037(4) 0.000(5) -0.060(5) C33 0.332(16) 0.265(13) 0.086(6) 0.020(7) 0.011(7) -0.173(12) C34 0.141(7) 0.163(7) 0.108(6) 0.003(5) -0.015(5) -0.004(6) C35 0.080(4) 0.203(8) 0.098(5) 0.085(5) 0.021(4) 0.026(5) #----------------------------------------------------------------------------# # 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 Li O1 1.914(8) . ? Li O2 1.954(8) . ? Li Si1 2.626(7) . ? Si1 N2 1.799(3) . ? Si1 N1 1.801(3) . ? Si1 N3 1.826(3) . ? Si2 N3 1.741(3) . ? Si2 C18 1.860(4) . ? Si2 C19 1.867(4) . ? Si2 C17 1.870(4) . ? O1 C28 1.417(6) . ? O1 C31 1.429(5) . ? O2 C32 1.425(7) . ? O2 C35 1.518(8) . ? N1 C1 1.392(4) . ? N1 C7 1.450(4) . ? N2 C2 1.399(4) . ? N2 C12 1.462(4) . ? N3 C20 1.446(4) . ? C1 C6 1.388(5) . ? C1 C2 1.421(5) . ? C2 C3 1.391(5) . ? C3 C4 1.396(6) . ? C4 C5 1.368(6) . ? C5 C6 1.396(5) . ? C7 C8 1.540(5) . ? C8 C9 1.524(5) . ? C8 C10 1.531(5) . ? C8 C11 1.526(5) . ? C12 C13 1.549(5) . ? C13 C15 1.493(6) . ? C13 C14 1.505(7) . ? C13 C16 1.519(7) . ? C20 C25 1.396(5) . ? C20 C21 1.405(5) . ? C21 C22 1.385(6) . ? C21 C26 1.501(6) . ? C22 C23 1.362(6) . ? C23 C24 1.367(6) . ? C24 C25 1.399(5) . ? C25 C27 1.500(5) . ? C28 C29 1.488(8) . ? C29 C30 1.460(8) . ? C30 C31 1.412(7) . ? C32 C33 1.495(10) . ? C33 C34 1.440(11) . ? C34 C35 1.442(9) . ? 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 O1 Li O2 101.2(3) . . ? O1 Li Si1 131.6(4) . . ? O2 Li Si1 127.2(4) . . ? N2 Si1 N1 85.73(12) . . ? N2 Si1 N3 103.77(13) . . ? N1 Si1 N3 108.39(13) . . ? N2 Si1 Li 133.1(2) . . ? N1 Si1 Li 119.13(19) . . ? N3 Si1 Li 104.3(2) . . ? N3 Si2 C18 113.68(17) . . ? N3 Si2 C19 112.97(17) . . ? C18 Si2 C19 105.8(2) . . ? N3 Si2 C17 109.14(16) . . ? C18 Si2 C17 106.30(19) . . ? C19 Si2 C17 108.6(2) . . ? C28 O1 C31 105.4(4) . . ? C28 O1 Li 134.0(4) . . ? C31 O1 Li 120.6(4) . . ? C32 O2 C35 109.4(4) . . ? C32 O2 Li 124.8(5) . . ? C35 O2 Li 125.5(4) . . ? C1 N1 C7 121.0(3) . . ? C1 N1 Si1 113.7(2) . . ? C7 N1 Si1 125.2(2) . . ? C2 N2 C12 120.1(3) . . ? C2 N2 Si1 113.6(2) . . ? C12 N2 Si1 125.7(2) . . ? C20 N3 Si2 116.0(2) . . ? C20 N3 Si1 112.9(2) . . ? Si2 N3 Si1 131.11(16) . . ? C6 C1 N1 128.9(3) . . ? C6 C1 C2 119.4(3) . . ? N1 C1 C2 111.7(3) . . ? C3 C2 N2 129.1(3) . . ? C3 C2 C1 119.4(3) . . ? N2 C2 C1 111.6(3) . . ? C2 C3 C4 120.1(4) . . ? C5 C4 C3 120.5(4) . . ? C4 C5 C6 120.5(4) . . ? C5 C6 C1 120.2(4) . . ? N1 C7 C8 116.5(3) . . ? C9 C8 C10 109.4(3) . . ? C9 C8 C11 109.3(3) . . ? C10 C8 C11 108.9(3) . . ? C9 C8 C7 109.9(3) . . ? C10 C8 C7 107.0(3) . . ? C11 C8 C7 112.4(3) . . ? N2 C12 C13 116.1(3) . . ? C15 C13 C14 110.3(5) . . ? C15 C13 C16 109.2(5) . . ? C14 C13 C16 110.0(5) . . ? C15 C13 C12 109.1(4) . . ? C14 C13 C12 112.1(4) . . ? C16 C13 C12 105.9(4) . . ? C25 C20 C21 118.9(3) . . ? C25 C20 N3 121.0(3) . . ? C21 C20 N3 120.1(3) . . ? C22 C21 C20 119.7(4) . . ? C22 C21 C26 119.6(4) . . ? C20 C21 C26 120.7(3) . . ? C23 C22 C21 121.7(4) . . ? C22 C23 C24 119.0(4) . . ? C23 C24 C25 121.8(4) . . ? C24 C25 C20 119.0(4) . . ? C24 C25 C27 119.5(3) . . ? C20 C25 C27 121.5(3) . . ? O1 C28 C29 105.5(5) . . ? C30 C29 C28 104.5(5) . . ? C31 C30 C29 107.3(5) . . ? C30 C31 O1 108.4(5) . . ? O2 C32 C33 103.5(6) . . ? C34 C33 C32 112.3(7) . . ? C33 C34 C35 104.5(7) . . ? C34 C35 O2 107.3(6) . . ? #===END data_(4)-jul1600 _database_code_depnum_ccdc_archive 'CCDC 271592' _audit_creation_date 2000-07-13T15:10:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[C6H4(NCH2tBu)Si(SNMe2)Li(thf)3]' _chemical_formula_moiety 'C30 H56 Li N2 O3 Si' _chemical_formula_sum 'C30 H56 Li N3 O3 Si' _chemical_formula_weight 541.81 _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 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8302(5) _cell_length_b 23.0640(14) _cell_length_c 13.7482(9) _cell_angle_alpha 90 _cell_angle_beta 90.062(4) _cell_angle_gamma 90 _cell_volume 3434.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14330 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _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 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 16263 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_unetI/netI 0.0633 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 5918 _reflns_number_gt 3908 _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^)+(0.0987P)^2^+2.4399P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5918 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1171 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2229 _refine_ls_wR_factor_gt 0.1972 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.403 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.044 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 Li Li 0.2974(6) 0.1235(3) 0.3215(5) 0.0699(17) Uani 1 1 d . . . Si Si 0.52809(8) 0.15353(4) 0.27957(7) 0.0486(3) Uani 1 1 d . . . O1 O 0.3058(2) 0.10061(12) 0.45910(19) 0.0727(7) Uani 1 1 d . . . O2 O 0.1731(3) 0.18421(15) 0.3094(4) 0.1280(15) Uani 1 1 d . . . O3 O 0.2289(3) 0.05324(13) 0.2642(2) 0.0845(9) Uani 1 1 d . . . N1 N 0.6403(2) 0.09595(10) 0.29361(18) 0.0451(6) Uani 1 1 d . . . N2 N 0.6093(2) 0.19013(10) 0.37798(19) 0.0450(6) Uani 1 1 d . . . N3 N 0.5737(3) 0.19008(12) 0.1742(2) 0.0593(8) Uani 1 1 d . . . C1 C 0.7261(3) 0.10500(13) 0.3672(2) 0.0436(7) Uani 1 1 d . . . C2 C 0.7073(3) 0.15860(13) 0.4163(2) 0.0436(7) Uani 1 1 d . . . C3 C 0.7822(3) 0.17211(15) 0.4953(2) 0.0549(8) Uani 1 1 d . . . H3 H 0.7711 0.2079 0.5283 0.066 Uiso 1 1 calc R . . C4 C 0.8733(3) 0.13369(16) 0.5267(3) 0.0628(10) Uani 1 1 d . . . H4 H 0.9228 0.1432 0.5815 0.075 Uiso 1 1 calc R . . C5 C 0.8919(3) 0.08239(17) 0.4791(3) 0.0632(10) Uani 1 1 d . . . H5 H 0.9548 0.0567 0.5005 0.076 Uiso 1 1 calc R . . C6 C 0.8187(3) 0.06754(15) 0.3990(2) 0.0549(8) Uani 1 1 d . . . H6 H 0.8321 0.0318 0.3662 0.066 Uiso 1 1 calc R . . C7 C 0.6198(4) 0.03785(14) 0.2556(2) 0.0597(9) Uani 1 1 d . . . H7A H 0.5296 0.0312 0.2526 0.072 Uiso 1 1 calc R . . H7B H 0.6542 0.0098 0.303 0.072 Uiso 1 1 calc R . . C8 C 0.6742(5) 0.0237(2) 0.1552(3) 0.0938(16) Uani 1 1 d . . . C9 C 0.6075(5) 0.05721(19) 0.0756(3) 0.0843(13) Uani 1 1 d . . . H9A H 0.5188 0.0488 0.0787 0.126 Uiso 1 1 calc R . . H9B H 0.6396 0.0455 0.0119 0.126 Uiso 1 1 calc R . . H9C H 0.6209 0.0989 0.0849 0.126 Uiso 1 1 calc R . . C10 C 0.6479(9) -0.0412(2) 0.1380(4) 0.184(4) Uani 1 1 d . . . H10A H 0.5619 -0.0497 0.1548 0.277 Uiso 1 1 calc R . . H10B H 0.7031 -0.0645 0.1788 0.277 Uiso 1 1 calc R . . H10C H 0.6621 -0.0506 0.0694 0.277 Uiso 1 1 calc R . . C11 C 0.8119(6) 0.0383(4) 0.1521(4) 0.159(3) Uani 1 1 d . . . H11A H 0.8426 0.0337 0.0855 0.238 Uiso 1 1 calc R . . H11B H 0.8571 0.012 0.1955 0.238 Uiso 1 1 calc R . . H11C H 0.8244 0.0784 0.1734 0.238 Uiso 1 1 calc R . . C12 C 0.5542(3) 0.23716(13) 0.4339(3) 0.0556(9) Uani 1 1 d . . . H12A H 0.5766 0.2314 0.503 0.067 Uiso 1 1 calc R . . H12B H 0.4634 0.2334 0.429 0.067 Uiso 1 1 calc R . . C13 C 0.5888(4) 0.30001(14) 0.4057(3) 0.0654(10) Uani 1 1 d . . . C14 C 0.5393(4) 0.31549(16) 0.3056(3) 0.0864(14) Uani 1 1 d . . . H14A H 0.449 0.3125 0.3057 0.13 Uiso 1 1 calc R . . H14B H 0.5734 0.2887 0.2572 0.13 Uiso 1 1 calc R . . H14C H 0.5634 0.3553 0.2892 0.13 Uiso 1 1 calc R . . C15 C 0.5301(7) 0.34044(19) 0.4808(4) 0.131(2) Uani 1 1 d . . . H15A H 0.5464 0.3808 0.4628 0.196 Uiso 1 1 calc R . . H15B H 0.5654 0.3326 0.5451 0.196 Uiso 1 1 calc R . . H15C H 0.4407 0.3338 0.4827 0.196 Uiso 1 1 calc R . . C16 C 0.7289(4) 0.30692(19) 0.4032(4) 0.1023(17) Uani 1 1 d . . . H16A H 0.7498 0.3451 0.3767 0.153 Uiso 1 1 calc R . . H16B H 0.7647 0.2766 0.362 0.153 Uiso 1 1 calc R . . H16C H 0.762 0.3035 0.4693 0.153 Uiso 1 1 calc R . . C17 C 0.6991(4) 0.20559(19) 0.1508(3) 0.0814(12) Uani 1 1 d . . . H17A H 0.7215 0.1888 0.0877 0.122 Uiso 1 1 calc R . . H17B H 0.7547 0.1906 0.2011 0.122 Uiso 1 1 calc R . . H17C H 0.7064 0.2479 0.1477 0.122 Uiso 1 1 calc R . . C18 C 0.4868(5) 0.2058(2) 0.0980(4) 0.0984(16) Uani 1 1 d . . . H18A H 0.4924 0.2475 0.0852 0.148 Uiso 1 1 calc R . . H18B H 0.4028 0.1961 0.1189 0.148 Uiso 1 1 calc R . . H18C H 0.5066 0.1843 0.0385 0.148 Uiso 1 1 calc R . . C19 C 0.2536(4) 0.1285(3) 0.5419(4) 0.118(2) Uani 1 1 d . . . H19A H 0.2226 0.1674 0.5237 0.142 Uiso 1 1 calc R . . H19B H 0.1835 0.1055 0.5671 0.142 Uiso 1 1 calc R . . C20 C 0.3464(6) 0.1336(2) 0.6142(4) 0.1069(17) Uani 1 1 d . . . H20A H 0.3156 0.1185 0.6771 0.128 Uiso 1 1 calc R . . H20B H 0.3695 0.1748 0.623 0.128 Uiso 1 1 calc R . . C21 C 0.4549(4) 0.09970(19) 0.5820(3) 0.0818(12) Uani 1 1 d . . . H21A H 0.4827 0.0727 0.6335 0.098 Uiso 1 1 calc R . . H21B H 0.5243 0.1255 0.5642 0.098 Uiso 1 1 calc R . . C22 C 0.4082(4) 0.06719(19) 0.4949(3) 0.0764(12) Uani 1 1 d . . . H22A H 0.4734 0.064 0.4448 0.092 Uiso 1 1 calc R . . H22B H 0.3812 0.0277 0.5135 0.092 Uiso 1 1 calc R . . C23 C 0.2016(6) 0.2443(3) 0.3039(12) 0.292(9) Uani 1 1 d . . . H23A H 0.242 0.2561 0.3655 0.351 Uiso 1 1 calc R . . H23B H 0.262 0.2502 0.2508 0.351 Uiso 1 1 calc R . . C24 C 0.1076(7) 0.2783(3) 0.2888(6) 0.141(2) Uani 1 1 d . . . H24A H 0.1221 0.3044 0.2329 0.169 Uiso 1 1 calc R . . H24B H 0.0885 0.3018 0.3472 0.169 Uiso 1 1 calc R . . C25 C 0.0146(8) 0.2390(4) 0.2693(10) 0.230(6) Uani 1 1 d . . . H25A H -0.0052 0.2405 0.199 0.276 Uiso 1 1 calc R . . H25B H -0.0604 0.2506 0.3055 0.276 Uiso 1 1 calc R . . C26 C 0.0459(4) 0.1802(3) 0.2950(4) 0.1074(18) Uani 1 1 d . . . H26A H 0.003 0.1678 0.3551 0.129 Uiso 1 1 calc R . . H26B H 0.0257 0.1529 0.2418 0.129 Uiso 1 1 calc R . . C27 C 0.2188(7) 0.0400(3) 0.1643(4) 0.131(2) Uani 1 1 d . . . H27A H 0.3005 0.0427 0.1325 0.158 Uiso 1 1 calc R . . H27B H 0.1617 0.0674 0.1319 0.158 Uiso 1 1 calc R . . C28 C 0.1719(10) -0.0181(4) 0.1578(5) 0.206(5) Uani 1 1 d . . . H28A H 0.0968 -0.0187 0.1167 0.247 Uiso 1 1 calc R . . H28B H 0.2345 -0.0437 0.1277 0.247 Uiso 1 1 calc R . . C29 C 0.1438(9) -0.0377(3) 0.2514(5) 0.163(3) Uani 1 1 d . . . H29A H 0.188 -0.0744 0.2651 0.195 Uiso 1 1 calc R . . H29B H 0.054 -0.0448 0.2575 0.195 Uiso 1 1 calc R . . C30 C 0.1817(7) 0.0060(2) 0.3179(4) 0.131(2) Uani 1 1 d . . . H30A H 0.1106 0.0187 0.3577 0.157 Uiso 1 1 calc R . . H30B H 0.246 -0.0095 0.362 0.157 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 Li 0.058(3) 0.063(4) 0.088(5) 0.003(3) -0.015(3) -0.003(3) Si 0.0461(5) 0.0396(5) 0.0600(6) 0.0015(4) -0.0085(4) -0.0035(4) O1 0.0680(15) 0.0792(18) 0.0711(17) -0.0147(14) 0.0032(13) 0.0167(13) O2 0.0507(16) 0.088(2) 0.245(5) 0.041(3) -0.033(2) 0.0012(16) O3 0.104(2) 0.090(2) 0.0596(17) 0.0024(14) -0.0012(15) -0.0439(17) N1 0.0543(15) 0.0386(14) 0.0422(14) 0.0026(11) -0.0007(12) 0.0005(11) N2 0.0449(14) 0.0349(13) 0.0553(16) -0.0019(11) -0.0019(12) -0.0006(11) N3 0.0676(18) 0.0530(16) 0.0572(18) 0.0134(14) -0.0192(14) -0.0034(14) C1 0.0485(17) 0.0428(17) 0.0396(17) 0.0097(13) 0.0051(13) -0.0006(13) C2 0.0446(16) 0.0400(16) 0.0463(17) 0.0097(14) -0.0009(13) -0.0063(13) C3 0.061(2) 0.0502(19) 0.053(2) 0.0063(15) -0.0082(16) -0.0097(16) C4 0.069(2) 0.064(2) 0.055(2) 0.0156(18) -0.0180(17) -0.0073(18) C5 0.062(2) 0.066(2) 0.062(2) 0.0248(19) -0.0105(17) 0.0072(18) C6 0.061(2) 0.0513(19) 0.053(2) 0.0115(16) 0.0066(16) 0.0097(16) C7 0.092(3) 0.0414(18) 0.0456(19) -0.0031(15) -0.0053(17) 0.0076(17) C8 0.153(5) 0.084(3) 0.044(2) -0.010(2) -0.004(2) 0.048(3) C9 0.131(4) 0.072(3) 0.049(2) -0.0077(19) -0.006(2) 0.015(3) C10 0.415(13) 0.071(3) 0.067(3) -0.025(3) -0.031(5) 0.089(5) C11 0.131(5) 0.282(10) 0.063(3) -0.001(4) 0.022(3) 0.108(6) C12 0.058(2) 0.0400(18) 0.069(2) -0.0010(16) 0.0021(17) -0.0006(14) C13 0.082(3) 0.0400(18) 0.074(3) -0.0015(17) -0.006(2) -0.0010(17) C14 0.110(3) 0.043(2) 0.106(3) 0.016(2) -0.027(3) 0.003(2) C15 0.225(7) 0.044(2) 0.123(5) -0.017(3) 0.043(4) 0.016(3) C16 0.097(3) 0.058(2) 0.151(5) 0.032(3) -0.042(3) -0.033(2) C17 0.095(3) 0.075(3) 0.074(3) 0.027(2) -0.005(2) -0.019(2) C18 0.119(4) 0.089(3) 0.087(3) 0.020(3) -0.048(3) 0.016(3) C19 0.071(3) 0.156(5) 0.127(5) -0.076(4) 0.008(3) 0.019(3) C20 0.144(5) 0.111(4) 0.065(3) -0.005(3) -0.002(3) 0.044(4) C21 0.082(3) 0.080(3) 0.084(3) 0.022(2) -0.003(2) -0.014(2) C22 0.079(3) 0.084(3) 0.066(3) 0.012(2) 0.018(2) 0.025(2) C23 0.088(5) 0.082(5) 0.71(3) 0.058(9) -0.078(9) 0.013(4) C24 0.132(5) 0.104(4) 0.188(7) -0.018(5) -0.018(5) 0.015(4) C25 0.126(6) 0.111(6) 0.453(18) 0.001(8) -0.092(9) 0.032(5) C26 0.054(2) 0.143(5) 0.126(4) 0.047(4) -0.005(2) -0.018(3) C27 0.190(6) 0.140(5) 0.064(3) 0.003(3) -0.007(3) -0.067(5) C28 0.321(12) 0.201(9) 0.096(5) -0.060(5) 0.069(6) -0.133(8) C29 0.280(9) 0.116(5) 0.092(4) -0.013(4) -0.001(5) -0.095(6) C30 0.205(6) 0.107(4) 0.080(3) 0.000(3) 0.011(4) -0.089(4) #----------------------------------------------------------------------------# # 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 Li O3 1.948(7) . ? Li O2 1.950(7) . ? Li O1 1.966(8) . ? Si N3 1.748(3) . ? Si N1 1.811(3) . ? Si N2 1.821(3) . ? O1 C19 1.425(5) . ? O1 C22 1.438(4) . ? O2 C26 1.394(5) . ? O2 C23 1.422(7) . ? O3 C27 1.411(6) . ? O3 C30 1.413(5) . ? N1 C1 1.389(4) . ? N1 C7 1.455(4) . ? N2 C2 1.390(4) . ? N2 C12 1.457(4) . ? N3 C17 1.441(5) . ? N3 C18 1.453(4) . ? C1 C6 1.393(4) . ? C1 C2 1.423(4) . ? C2 C3 1.391(4) . ? C3 C4 1.394(5) . ? C4 C5 1.367(5) . ? C5 C6 1.399(5) . ? C7 C8 1.537(5) . ? C8 C9 1.521(6) . ? C8 C11 1.529(8) . ? C8 C10 1.542(8) . ? C12 C13 1.546(5) . ? C13 C14 1.520(6) . ? C13 C16 1.526(6) . ? C13 C15 1.531(6) . ? C19 C20 1.418(7) . ? C20 C21 1.480(6) . ? C21 C22 1.500(6) . ? C23 C24 1.301(8) . ? C24 C25 1.381(9) . ? C25 C26 1.442(9) . ? C27 C28 1.435(9) . ? C28 C29 1.399(9) . ? C29 C30 1.420(7) . ? 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 O3 Li O2 107.5(3) . . ? O3 Li O1 100.6(3) . . ? O2 Li O1 107.8(4) . . ? O3 Li Si 119.1(3) . . ? O2 Li Si 116.3(3) . . ? O1 Li Si 103.7(3) . . ? N3 Si N1 104.59(13) . . ? N3 Si N2 104.82(13) . . ? N1 Si N2 86.39(11) . . ? N3 Si Li 124.91(17) . . ? N1 Si Li 114.64(16) . . ? N2 Si Li 114.41(18) . . ? C19 O1 C22 106.0(3) . . ? C19 O1 Li 129.0(4) . . ? C22 O1 Li 120.5(3) . . ? C26 O2 C23 105.8(4) . . ? C26 O2 Li 130.3(4) . . ? C23 O2 Li 123.7(4) . . ? C27 O3 C30 108.3(4) . . ? C27 O3 Li 127.1(4) . . ? C30 O3 Li 124.7(3) . . ? C1 N1 C7 120.1(2) . . ? C1 N1 Si 114.58(19) . . ? C7 N1 Si 122.4(2) . . ? C2 N2 C12 120.2(3) . . ? C2 N2 Si 114.02(19) . . ? C12 N2 Si 122.6(2) . . ? C17 N3 C18 112.8(3) . . ? C17 N3 Si 124.9(2) . . ? C18 N3 Si 122.3(3) . . ? N1 C1 C6 128.0(3) . . ? N1 C1 C2 112.3(2) . . ? C6 C1 C2 119.6(3) . . ? N2 C2 C3 128.6(3) . . ? N2 C2 C1 112.6(3) . . ? C3 C2 C1 118.8(3) . . ? C2 C3 C4 120.7(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 120.3(3) . . ? C1 C6 C5 120.1(3) . . ? N1 C7 C8 117.3(3) . . ? C9 C8 C11 109.4(5) . . ? C9 C8 C7 110.9(4) . . ? C11 C8 C7 110.7(4) . . ? C9 C8 C10 107.2(4) . . ? C11 C8 C10 112.9(6) . . ? C7 C8 C10 105.8(4) . . ? N2 C12 C13 117.8(3) . . ? C14 C13 C16 107.8(4) . . ? C14 C13 C15 108.8(4) . . ? C16 C13 C15 111.5(4) . . ? C14 C13 C12 111.2(3) . . ? C16 C13 C12 110.2(3) . . ? C15 C13 C12 107.5(3) . . ? C20 C19 O1 108.4(4) . . ? C19 C20 C21 108.0(4) . . ? C20 C21 C22 103.7(4) . . ? O1 C22 C21 105.4(3) . . ? C24 C23 O2 115.2(6) . . ? C23 C24 C25 101.9(6) . . ? C24 C25 C26 113.4(6) . . ? O2 C26 C25 101.8(5) . . ? O3 C27 C28 106.8(5) . . ? C29 C28 C27 108.8(5) . . ? C28 C29 C30 107.4(5) . . ? O3 C30 C29 108.5(4) . . ? #===END data_(5)-jun3300 _database_code_depnum_ccdc_archive 'CCDC 271593' _audit_creation_date 2000-07-03T19:05:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common jun3300 _chemical_formula_moiety 'C34 H64 Li N3 O3 Si' _chemical_formula_sum 'C34 H64 Li N3 O3 Si' _chemical_formula_weight 597.91 _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 10.5648(2) _cell_length_b 18.4630(4) _cell_length_c 20.1835(3) _cell_angle_alpha 108.811(1) _cell_angle_beta 90.650(1) _cell_angle_gamma 92.189(1) _cell_volume 3722.78(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23192 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _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 0.2 _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # 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 42756 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 25.12 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 13009 _reflns_number_gt 10237 _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^)+(0.0817P)^2^+2.7712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13009 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.567 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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 Li Li 0.3929(4) 0.1839(2) 0.2303(2) 0.0361(9) Uani 1 1 d . A 1 Si Si 0.28673(5) 0.26275(3) 0.35199(3) 0.02379(15) Uani 1 1 d . A 1 O1 O 0.53110(17) 0.11017(10) 0.22514(9) 0.0425(4) Uani 1 1 d . A 1 O2 O 0.47478(16) 0.23647(11) 0.17003(10) 0.0449(5) Uani 1 1 d . A 1 O3 O 0.25531(17) 0.11267(11) 0.17578(9) 0.0446(4) Uani 1 1 d . A 1 N1 N 0.23123(16) 0.19533(10) 0.39519(9) 0.0246(4) Uani 1 1 d . A 1 N2 N 0.11992(17) 0.28474(11) 0.34774(10) 0.0290(4) Uani 1 1 d . A 1 N3 N 0.34955(18) 0.34598(11) 0.41782(10) 0.0303(4) Uani 1 1 d . A 1 C1 C 0.1022(2) 0.19566(12) 0.40734(11) 0.0267(5) Uani 1 1 d . A 1 C2 C 0.0390(2) 0.24864(13) 0.38191(11) 0.0292(5) Uani 1 1 d . A 1 C3 C -0.0899(2) 0.25778(16) 0.39283(13) 0.0388(6) Uani 1 1 d . A 1 H3 H -0.1319 0.2949 0.3784 0.047 Uiso 1 1 calc R A 1 C4 C -0.1579(2) 0.21258(18) 0.42499(14) 0.0468(7) Uani 1 1 d . A 1 H4 H -0.2459 0.2194 0.4324 0.056 Uiso 1 1 calc R A 1 C5 C -0.0991(2) 0.15832(17) 0.44597(14) 0.0438(6) Uani 1 1 d . A 1 H5 H -0.147 0.1263 0.4659 0.053 Uiso 1 1 calc R A 1 C6 C 0.0316(2) 0.15025(14) 0.43804(12) 0.0348(5) Uani 1 1 d . A 1 H6 H 0.0725 0.1136 0.4537 0.042 Uiso 1 1 calc R A 1 C7 C 0.3028(2) 0.13061(12) 0.39896(11) 0.0279(5) Uani 1 1 d . A 1 H7A H 0.3606 0.1166 0.359 0.033 Uiso 1 1 calc R A 1 H7B H 0.2422 0.0865 0.3925 0.033 Uiso 1 1 calc R A 1 C8 C 0.3823(2) 0.14166(13) 0.46650(12) 0.0322(5) Uani 1 1 d . A 1 C9 C 0.3075(3) 0.17662(17) 0.53182(13) 0.0446(6) Uani 1 1 d . A 1 H9A H 0.2326 0.1434 0.5315 0.067 Uiso 1 1 calc R A 1 H9B H 0.2807 0.2272 0.533 0.067 Uiso 1 1 calc R A 1 H9C H 0.3607 0.1818 0.5733 0.067 Uiso 1 1 calc R A 1 C10 C 0.4989(2) 0.19316(18) 0.46758(14) 0.0480(7) Uani 1 1 d . A 1 H10A H 0.5477 0.1706 0.4254 0.072 Uiso 1 1 calc R A 1 H10B H 0.5517 0.1981 0.5092 0.072 Uiso 1 1 calc R A 1 H10C H 0.4724 0.2439 0.4688 0.072 Uiso 1 1 calc R A 1 C11 C 0.4248(4) 0.06301(17) 0.46536(17) 0.0654(10) Uani 1 1 d . A 1 H11A H 0.4736 0.0403 0.4233 0.098 Uiso 1 1 calc R A 1 H11B H 0.3503 0.0297 0.4651 0.098 Uiso 1 1 calc R A 1 H11C H 0.4779 0.0687 0.507 0.098 Uiso 1 1 calc R A 1 C12 C 0.0752(2) 0.34693(14) 0.32518(13) 0.0357(5) Uani 1 1 d . A 1 H12A H 0.1447 0.3866 0.3337 0.043 Uiso 1 1 calc R A 1 H12B H 0.0047 0.3703 0.3555 0.043 Uiso 1 1 calc R A 1 C13 C 0.0291(2) 0.32664(16) 0.24807(14) 0.0397(6) Uani 1 1 d . A 1 C14 C -0.0696(3) 0.25995(18) 0.22811(15) 0.0497(7) Uani 1 1 d . A 1 H14A H -0.1419 0.2733 0.259 0.074 Uiso 1 1 calc R A 1 H14B H -0.0317 0.2143 0.2331 0.074 Uiso 1 1 calc R A 1 H14C H -0.0983 0.2495 0.1795 0.074 Uiso 1 1 calc R A 1 C15 C 0.1403(3) 0.3051(2) 0.19978(15) 0.0528(7) Uani 1 1 d . A 1 H15A H 0.2042 0.3475 0.2122 0.079 Uiso 1 1 calc R A 1 H15B H 0.111 0.2946 0.1512 0.079 Uiso 1 1 calc R A 1 H15C H 0.1777 0.2593 0.2048 0.079 Uiso 1 1 calc R A 1 C16 C -0.0289(3) 0.3982(2) 0.24003(19) 0.0631(9) Uani 1 1 d . A 1 H16A H -0.1011 0.4122 0.271 0.095 Uiso 1 1 calc R A 1 H16B H -0.0577 0.3877 0.1914 0.095 Uiso 1 1 calc R A 1 H16C H 0.0349 0.4406 0.2526 0.095 Uiso 1 1 calc R A 1 C17 C 0.4574(2) 0.39272(14) 0.40463(13) 0.0361(5) Uani 1 1 d . A 1 H17 H 0.4654 0.4406 0.4459 0.043 Uiso 1 1 calc R A 1 C18 C 0.4350(3) 0.41718(16) 0.34018(15) 0.0461(7) Uani 1 1 d . A 1 H18A H 0.3543 0.4425 0.3442 0.069 Uiso 1 1 calc R A 1 H18B H 0.4322 0.3719 0.2981 0.069 Uiso 1 1 calc R A 1 H18C H 0.504 0.4528 0.3369 0.069 Uiso 1 1 calc R A 1 C19 C 0.5828(2) 0.35344(17) 0.39989(16) 0.0481(7) Uani 1 1 d . A 1 H19A H 0.5958 0.3383 0.4417 0.072 Uiso 1 1 calc R A 1 H19B H 0.6522 0.3889 0.3969 0.072 Uiso 1 1 calc R A 1 H19C H 0.581 0.3079 0.3581 0.072 Uiso 1 1 calc R A 1 C20 C 0.2863(2) 0.37898(14) 0.48440(12) 0.0377(6) Uani 1 1 d . A 1 H20 H 0.2188 0.3405 0.4868 0.045 Uiso 1 1 calc R A 1 C21 C 0.2200(3) 0.45282(17) 0.49051(16) 0.0543(7) Uani 1 1 d . A 1 H21A H 0.1637 0.4446 0.4496 0.081 Uiso 1 1 calc R A 1 H21B H 0.2835 0.4937 0.4928 0.081 Uiso 1 1 calc R A 1 H21C H 0.1701 0.4675 0.5331 0.081 Uiso 1 1 calc R A 1 C22 C 0.3737(3) 0.39251(16) 0.54893(13) 0.0510(7) Uani 1 1 d . A 1 H22A H 0.416 0.3452 0.5457 0.077 Uiso 1 1 calc R A 1 H22B H 0.3235 0.4078 0.5913 0.077 Uiso 1 1 calc R A 1 H22C H 0.4376 0.4331 0.5509 0.077 Uiso 1 1 calc R A 1 C23 C 0.5600(3) 0.05896(17) 0.15704(15) 0.0545(8) Uani 1 1 d . A 1 H23A H 0.5685 0.0875 0.1233 0.065 Uiso 1 1 calc R A 1 H23B H 0.4914 0.0189 0.1399 0.065 Uiso 1 1 calc R A 1 C24 C 0.6800(4) 0.0238(3) 0.1639(2) 0.0917(14) Uani 1 1 d . A 1 H24A H 0.6643 -0.0286 0.166 0.11 Uiso 1 1 calc R A 1 H24B H 0.7352 0.0213 0.124 0.11 Uiso 1 1 calc R A 1 C25 C 0.7380(3) 0.0741(3) 0.2295(3) 0.1063(18) Uani 1 1 d . A 1 H25A H 0.7968 0.1128 0.2206 0.128 Uiso 1 1 calc R A 1 H25B H 0.7858 0.0441 0.2533 0.128 Uiso 1 1 calc R A 1 C26 C 0.6321(3) 0.1119(2) 0.27326(16) 0.0566(8) Uani 1 1 d . A 1 H26A H 0.6062 0.0838 0.3056 0.068 Uiso 1 1 calc R A 1 H26B H 0.6574 0.1653 0.3011 0.068 Uiso 1 1 calc R A 1 C27 C 0.6032(2) 0.26546(17) 0.18629(15) 0.0450(6) Uani 1 1 d . A 1 H27A H 0.663 0.2251 0.1644 0.054 Uiso 1 1 calc R A 1 H27B H 0.6193 0.2837 0.2376 0.054 Uiso 1 1 calc R A 1 C28 C 0.6189(3) 0.3304(2) 0.1574(2) 0.0691(10) Uani 1 1 d . A 1 H28A H 0.6199 0.3802 0.1955 0.083 Uiso 1 1 calc R A 1 H28B H 0.6989 0.327 0.1317 0.083 Uiso 1 1 calc R A 1 C29 C 0.5104(5) 0.3226(4) 0.1104(4) 0.143(3) Uani 1 1 d . A 1 H29A H 0.5393 0.3162 0.0624 0.172 Uiso 1 1 calc R A 1 H29B H 0.4603 0.369 0.1261 0.172 Uiso 1 1 calc R A 1 C30 C 0.4327(3) 0.2557(2) 0.11055(15) 0.0522(8) Uani 1 1 d . A 1 H30A H 0.342 0.2677 0.1143 0.063 Uiso 1 1 calc R A 1 H30B H 0.4439 0.2126 0.0669 0.063 Uiso 1 1 calc R A 1 C31 C 0.2173(3) 0.0865(2) 0.10322(15) 0.0657(9) Uani 1 1 d . A 1 H31A H 0.2811 0.0529 0.0748 0.079 Uiso 1 1 calc R A 1 H31B H 0.2074 0.1304 0.0859 0.079 Uiso 1 1 calc R A 1 C32 C 0.0922(3) 0.0426(2) 0.09880(18) 0.0690(10) Uani 1 1 d . A 1 H32A H 0.0203 0.0768 0.105 0.083 Uiso 1 1 calc R A 1 H32B H 0.0811 0.0009 0.0534 0.083 Uiso 1 1 calc R A 1 C33 C 0.1035(3) 0.0113(2) 0.15824(17) 0.0632(8) Uani 1 1 d . A 1 H33A H 0.1516 -0.0361 0.1448 0.076 Uiso 1 1 calc R A 1 H33B H 0.0191 0.0004 0.1746 0.076 Uiso 1 1 calc R A 1 C34 C 0.1747(3) 0.07545(16) 0.21348(15) 0.0455(6) Uani 1 1 d . A 1 H34A H 0.1152 0.1119 0.2426 0.055 Uiso 1 1 calc R A 1 H34B H 0.2261 0.055 0.2442 0.055 Uiso 1 1 calc R A 1 Li1B Li 0.0384(4) -0.2906(3) 0.2633(2) 0.0392(9) Uani 1 1 d . B 2 Si1B Si 0.17927(6) -0.29482(3) 0.14932(3) 0.02692(16) Uani 1 1 d . B 2 O1B O 0.00110(19) -0.18111(11) 0.30770(9) 0.0483(5) Uani 1 1 d . B 2 O2B O -0.13254(16) -0.34693(10) 0.25441(9) 0.0420(4) Uani 1 1 d . B 2 O3B O 0.09977(19) -0.32349(12) 0.34330(10) 0.0506(5) Uani 1 1 d . B 2 N1B N 0.30447(17) -0.22264(10) 0.15242(9) 0.0290(4) Uani 1 1 d . B 2 N2B N 0.10557(18) -0.26219(11) 0.08202(10) 0.0300(4) Uani 1 1 d . B 2 N3B N 0.24596(19) -0.38354(11) 0.10524(11) 0.0358(5) Uani 1 1 d . B 2 C1B C 0.2982(2) -0.19164(13) 0.09843(11) 0.0301(5) Uani 1 1 d . B 2 C2B C 0.1833(2) -0.21414(13) 0.05789(12) 0.0306(5) Uani 1 1 d . B 2 C3B C 0.1630(3) -0.18879(15) 0.00107(13) 0.0405(6) Uani 1 1 d . B 2 H3B H 0.0873 -0.2045 -0.0266 0.049 Uiso 1 1 calc R B 2 C4B C 0.2532(3) -0.14024(16) -0.01570(14) 0.0469(7) Uani 1 1 d . B 2 H4B H 0.2374 -0.1219 -0.0538 0.056 Uiso 1 1 calc R B 2 C5B C 0.3642(3) -0.11915(16) 0.02274(14) 0.0469(7) Uani 1 1 d . B 2 H5B H 0.4253 -0.0866 0.0108 0.056 Uiso 1 1 calc R B 2 C6B C 0.3883(3) -0.14520(14) 0.07959(13) 0.0394(6) Uani 1 1 d . B 2 H6B H 0.4663 -0.1311 0.1053 0.047 Uiso 1 1 calc R B 2 C7B C 0.4214(2) -0.21221(13) 0.19411(12) 0.0330(5) Uani 1 1 d . B 2 H7B1 H 0.4927 -0.2062 0.1646 0.04 Uiso 1 1 calc R B 2 H7B2 H 0.4337 -0.2596 0.2058 0.04 Uiso 1 1 calc R B 2 C8B C 0.4298(2) -0.14370(13) 0.26306(12) 0.0339(5) Uani 1 1 d . B 2 C9B C 0.3519(3) -0.16385(17) 0.31854(14) 0.0505(7) Uani 1 1 d . B 2 H9B1 H 0.3829 -0.2105 0.325 0.076 Uiso 1 1 calc R B 2 H9B2 H 0.2626 -0.1723 0.3033 0.076 Uiso 1 1 calc R B 2 H9B3 H 0.3602 -0.1216 0.3629 0.076 Uiso 1 1 calc R B 2 C10B C 0.3814(3) -0.07101(14) 0.25339(13) 0.0413(6) Uani 1 1 d . B 2 H10D H 0.4308 -0.058 0.2177 0.062 Uiso 1 1 calc R B 2 H10E H 0.3903 -0.0289 0.2978 0.062 Uiso 1 1 calc R B 2 H10F H 0.2919 -0.0794 0.2385 0.062 Uiso 1 1 calc R B 2 C11B C 0.5687(3) -0.12970(17) 0.28827(16) 0.0524(7) Uani 1 1 d . B 2 H11D H 0.6196 -0.1166 0.2532 0.079 Uiso 1 1 calc R B 2 H11E H 0.5998 -0.1762 0.2951 0.079 Uiso 1 1 calc R B 2 H11F H 0.5755 -0.0874 0.3327 0.079 Uiso 1 1 calc R B 2 C12B C -0.0066(2) -0.30029(15) 0.04081(13) 0.0357(5) Uani 1 1 d . B 2 H12C H -0.015 -0.3527 0.0438 0.043 Uiso 1 1 calc R B 2 H12D H 0.0085 -0.3053 -0.0088 0.043 Uiso 1 1 calc R B 2 C13B C -0.1345(2) -0.26208(17) 0.06087(14) 0.0426(6) Uani 1 1 d . B 2 C14B C -0.1293(3) -0.1792(2) 0.0629(2) 0.0771(11) Uani 1 1 d . B 2 H14D H -0.104 -0.1764 0.0173 0.116 Uiso 1 1 calc R B 2 H14E H -0.0675 -0.1497 0.099 0.116 Uiso 1 1 calc R B 2 H14F H -0.2131 -0.1581 0.0739 0.116 Uiso 1 1 calc R B 2 C15B C -0.1738(3) -0.2689(2) 0.13079(16) 0.0623(9) Uani 1 1 d . B 2 H15D H -0.177 -0.3229 0.128 0.093 Uiso 1 1 calc R B 2 H15E H -0.2577 -0.248 0.1422 0.093 Uiso 1 1 calc R B 2 H15F H -0.1121 -0.2401 0.1673 0.093 Uiso 1 1 calc R B 2 C16B C -0.2338(3) -0.3083(2) 0.00635(18) 0.0699(10) Uani 1 1 d . B 2 H16D H -0.212 -0.3053 -0.0398 0.105 Uiso 1 1 calc R B 2 H16E H -0.3173 -0.2873 0.019 0.105 Uiso 1 1 calc R B 2 H16F H -0.2359 -0.3619 0.0049 0.105 Uiso 1 1 calc R B 2 C17B C 0.2160(4) -0.44936(19) 0.1288(2) 0.0784(12) Uani 1 1 d . B 2 H17B H 0.2672 -0.4828 0.0904 0.094 Uiso 1 1 calc R B 2 C18B C 0.1013(3) -0.4950(2) 0.09851(19) 0.0664(9) Uani 1 1 d . B 2 H18D H 0.0635 -0.4751 0.0637 0.1 Uiso 1 1 calc R B 2 H18E H 0.0406 -0.4922 0.1356 0.1 Uiso 1 1 calc R B 2 H18F H 0.1225 -0.5484 0.0759 0.1 Uiso 1 1 calc R B 2 C19B C 0.2952(5) -0.4626(3) 0.1789(3) 0.122(2) Uani 1 1 d . B 2 H19D H 0.3675 -0.4255 0.1895 0.183 Uiso 1 1 calc R B 2 H19E H 0.3259 -0.5146 0.1608 0.183 Uiso 1 1 calc R B 2 H19F H 0.2481 -0.4571 0.2216 0.183 Uiso 1 1 calc R B 2 C20B C 0.3237(3) -0.4003(2) 0.04309(15) 0.0674(10) Uani 1 1 d . B 2 H20B H 0.3206 -0.3461 0.0437 0.081 Uiso 1 1 calc R B 2 C21B C 0.2616(4) -0.4268(3) -0.02411(18) 0.1034(18) Uani 1 1 d . B 2 H21D H 0.1696 -0.4259 -0.0184 0.155 Uiso 1 1 calc R B 2 H21E H 0.2853 -0.4793 -0.0489 0.155 Uiso 1 1 calc R B 2 H21F H 0.2873 -0.3934 -0.0512 0.155 Uiso 1 1 calc R B 2 C22B C 0.4585(3) -0.3923(3) 0.05377(18) 0.0800(12) Uani 1 1 d . B 2 H22D H 0.4788 -0.3713 0.104 0.12 Uiso 1 1 calc R B 2 H22E H 0.4936 -0.3576 0.0301 0.12 Uiso 1 1 calc R B 2 H22F H 0.4952 -0.4426 0.0345 0.12 Uiso 1 1 calc R B 2 C23B C 0.0050(4) -0.14652(19) 0.38234(16) 0.0699(10) Uani 1 1 d . B 2 H23C H 0.089 -0.1522 0.4019 0.084 Uiso 1 1 calc R B 2 H23D H -0.0606 -0.1708 0.4039 0.084 Uiso 1 1 calc R B 2 C24B C -0.0191(6) -0.0652(2) 0.3959(2) 0.113(2) Uani 1 1 d . B 2 H24C H 0.03 -0.0325 0.4376 0.136 Uiso 1 1 calc R B 2 H24D H -0.1103 -0.0558 0.4033 0.136 Uiso 1 1 calc R B 2 C25B C 0.0239(5) -0.0499(2) 0.3308(2) 0.0910(14) Uani 1 1 d . B 2 H25C H -0.0238 -0.0084 0.3225 0.109 Uiso 1 1 calc R B 2 H25D H 0.1156 -0.0356 0.3341 0.109 Uiso 1 1 calc R B 2 C26B C -0.0033(4) -0.12271(18) 0.27544(18) 0.0646(9) Uani 1 1 d . B 2 H26C H -0.0881 -0.1232 0.2539 0.078 Uiso 1 1 calc R B 2 H26D H 0.0606 -0.1309 0.2385 0.078 Uiso 1 1 calc R B 2 C27B C -0.1689(4) -0.42558(18) 0.2170(2) 0.0686(9) Uani 1 1 d . B 2 H27C H -0.1114 -0.4603 0.2298 0.082 Uiso 1 1 calc R B 2 H27D H -0.1652 -0.4354 0.1658 0.082 Uiso 1 1 calc R B 2 C28B C -0.3010(4) -0.4384(2) 0.2372(2) 0.0849(12) Uani 1 1 d . B 2 H28C H -0.3015 -0.46 0.2762 0.102 Uiso 1 1 calc R B 2 H28D H -0.3505 -0.4736 0.197 0.102 Uiso 1 1 calc R B 2 C29B C -0.3532(3) -0.3605(2) 0.25944(19) 0.0647(9) Uani 1 1 d . B 2 H29C H -0.3906 -0.3489 0.219 0.078 Uiso 1 1 calc R B 2 H29D H -0.4186 -0.3558 0.2952 0.078 Uiso 1 1 calc R B 2 C30B C -0.2409(3) -0.30937(17) 0.28901(17) 0.0523(7) Uani 1 1 d . B 2 H30C H -0.2489 -0.2596 0.281 0.063 Uiso 1 1 calc R B 2 H30D H -0.2328 -0.2999 0.34 0.063 Uiso 1 1 calc R B 2 C31B C 0.1009(4) -0.3987(2) 0.41822(19) 0.0712(10) Uani 1 1 d . B 2 H31C H 0.0982 -0.3852 0.4698 0.085 Uiso 1 1 calc R B 2 H31D H 0.0693 -0.4525 0.3966 0.085 Uiso 1 1 calc R B 2 C32B C 0.0240(3) -0.3460(2) 0.39333(18) 0.0662(9) Uani 1 1 d . B 2 H32C H -0.0563 -0.3724 0.3709 0.079 Uiso 1 1 calc R B 2 H32D H 0.0038 -0.3004 0.4331 0.079 Uiso 1 1 calc R B 2 C33B C 0.2303(4) -0.3877(3) 0.3959(3) 0.1010(16) Uani 1 1 d . B 2 H33C H 0.2572 -0.4352 0.3605 0.121 Uiso 1 1 calc R B 2 H33D H 0.2905 -0.3741 0.4364 0.121 Uiso 1 1 calc R B 2 C34B C 0.2263(3) -0.3248(2) 0.3657(2) 0.0762(11) Uani 1 1 d . B 2 H34C H 0.2526 -0.2753 0.4014 0.091 Uiso 1 1 calc R B 2 H34D H 0.2838 -0.3341 0.3257 0.091 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 Li 0.036(2) 0.038(2) 0.036(2) 0.0133(18) 0.0003(17) 0.0001(17) Si 0.0239(3) 0.0216(3) 0.0259(3) 0.0081(2) -0.0016(2) -0.0015(2) O1 0.0489(11) 0.0441(11) 0.0351(9) 0.0125(8) 0.0018(8) 0.0110(8) O2 0.0352(9) 0.0638(13) 0.0489(11) 0.0371(10) -0.0013(8) -0.0022(9) O3 0.0480(10) 0.0447(11) 0.0361(9) 0.0075(8) -0.0078(8) -0.0099(8) N1 0.0232(9) 0.0221(9) 0.0286(9) 0.0082(7) 0.0000(7) 0.0004(7) N2 0.0264(9) 0.0289(10) 0.0340(10) 0.0135(8) -0.0022(8) 0.0021(8) N3 0.0341(10) 0.0253(10) 0.0298(10) 0.0074(8) -0.0001(8) -0.0074(8) C1 0.0273(11) 0.0254(11) 0.0239(11) 0.0035(9) 0.0000(9) -0.0031(9) C2 0.0273(11) 0.0325(12) 0.0255(11) 0.0066(9) -0.0019(9) -0.0009(9) C3 0.0267(12) 0.0503(16) 0.0393(13) 0.0140(12) -0.0001(10) 0.0061(11) C4 0.0238(12) 0.074(2) 0.0408(14) 0.0169(14) 0.0026(11) -0.0045(13) C5 0.0354(14) 0.0558(17) 0.0394(14) 0.0159(12) 0.0036(11) -0.0151(12) C6 0.0352(13) 0.0352(13) 0.0346(13) 0.0131(10) 0.0009(10) -0.0069(10) C7 0.0321(12) 0.0217(11) 0.0300(11) 0.0084(9) 0.0010(9) 0.0019(9) C8 0.0374(13) 0.0278(12) 0.0338(12) 0.0130(10) -0.0024(10) 0.0045(10) C9 0.0467(15) 0.0563(18) 0.0329(13) 0.0174(12) -0.0005(11) 0.0013(13) C10 0.0367(14) 0.0632(19) 0.0411(15) 0.0139(13) -0.0061(11) -0.0049(13) C11 0.095(3) 0.0406(17) 0.0605(19) 0.0157(14) -0.0274(18) 0.0219(17) C12 0.0317(12) 0.0311(13) 0.0477(14) 0.0172(11) -0.0042(10) 0.0054(10) C13 0.0356(13) 0.0456(15) 0.0456(14) 0.0254(12) -0.0056(11) 0.0051(11) C14 0.0446(15) 0.0613(19) 0.0445(15) 0.0205(14) -0.0126(12) -0.0061(13) C15 0.0455(16) 0.075(2) 0.0477(16) 0.0336(15) -0.0001(13) 0.0062(15) C16 0.067(2) 0.064(2) 0.074(2) 0.0413(18) -0.0085(17) 0.0175(17) C17 0.0416(14) 0.0272(12) 0.0373(13) 0.0094(10) -0.0036(10) -0.0139(10) C18 0.0540(16) 0.0380(15) 0.0508(16) 0.0224(12) -0.0021(13) -0.0137(12) C19 0.0368(14) 0.0522(17) 0.0570(17) 0.0219(14) -0.0040(12) -0.0148(12) C20 0.0468(15) 0.0281(13) 0.0331(12) 0.0039(10) 0.0030(11) -0.0072(11) C21 0.0656(19) 0.0407(16) 0.0478(16) 0.0013(13) 0.0023(14) 0.0084(14) C22 0.079(2) 0.0377(15) 0.0318(14) 0.0058(11) -0.0051(13) -0.0100(14) C23 0.080(2) 0.0410(16) 0.0413(15) 0.0106(13) 0.0130(14) 0.0079(15) C24 0.104(3) 0.095(3) 0.085(3) 0.035(3) 0.039(3) 0.055(3) C25 0.043(2) 0.070(3) 0.176(5) -0.001(3) -0.009(2) 0.0081(18) C26 0.0502(17) 0.067(2) 0.0533(17) 0.0199(15) -0.0081(14) 0.0108(15) C27 0.0360(14) 0.0563(17) 0.0469(15) 0.0234(13) -0.0050(11) -0.0037(12) C28 0.063(2) 0.068(2) 0.089(3) 0.047(2) -0.0115(18) -0.0182(17) C29 0.099(3) 0.173(5) 0.229(6) 0.177(5) -0.089(4) -0.076(3) C30 0.0385(15) 0.084(2) 0.0485(16) 0.0411(16) 0.0001(12) 0.0022(14) C31 0.083(2) 0.070(2) 0.0369(16) 0.0095(15) -0.0166(15) -0.0187(18) C32 0.067(2) 0.067(2) 0.060(2) 0.0046(17) -0.0276(17) -0.0052(17) C33 0.0595(19) 0.057(2) 0.063(2) 0.0088(16) -0.0110(16) -0.0154(16) C34 0.0500(16) 0.0384(15) 0.0471(15) 0.0140(12) -0.0058(12) -0.0077(12) Li1B 0.043(2) 0.042(2) 0.036(2) 0.0158(18) 0.0036(18) 0.0062(19) Si1B 0.0277(3) 0.0260(3) 0.0261(3) 0.0072(2) 0.0001(2) 0.0010(2) O1B 0.0648(13) 0.0376(10) 0.0417(10) 0.0106(8) 0.0117(9) 0.0077(9) O2B 0.0413(10) 0.0382(10) 0.0438(10) 0.0083(8) 0.0069(8) 0.0087(8) O3B 0.0562(12) 0.0582(13) 0.0456(11) 0.0279(10) -0.0038(9) 0.0048(10) N1B 0.0314(10) 0.0237(10) 0.0296(10) 0.0057(8) -0.0025(8) -0.0006(8) N2B 0.0303(10) 0.0304(10) 0.0291(10) 0.0100(8) -0.0015(8) -0.0023(8) N3B 0.0403(11) 0.0232(10) 0.0414(11) 0.0073(9) -0.0019(9) 0.0005(8) C1B 0.0360(12) 0.0233(11) 0.0279(11) 0.0040(9) 0.0040(9) 0.0010(9) C2B 0.0358(12) 0.0245(12) 0.0293(12) 0.0055(9) 0.0035(9) 0.0023(10) C3B 0.0493(15) 0.0410(15) 0.0331(13) 0.0149(11) -0.0003(11) 0.0008(12) C4B 0.0654(19) 0.0419(16) 0.0374(14) 0.0185(12) 0.0078(13) 0.0011(13) C5B 0.0600(18) 0.0377(15) 0.0431(15) 0.0142(12) 0.0118(13) -0.0101(13) C6B 0.0463(15) 0.0304(13) 0.0369(13) 0.0051(10) 0.0038(11) -0.0057(11) C7B 0.0308(12) 0.0254(12) 0.0398(13) 0.0064(10) -0.0043(10) 0.0010(9) C8B 0.0347(13) 0.0281(12) 0.0358(13) 0.0065(10) -0.0067(10) -0.0009(10) C9B 0.0666(19) 0.0434(16) 0.0386(15) 0.0103(12) -0.0015(13) -0.0058(14) C10B 0.0535(16) 0.0281(13) 0.0378(13) 0.0043(11) -0.0046(12) 0.0047(11) C11B 0.0452(16) 0.0434(16) 0.0588(18) 0.0034(13) -0.0197(13) 0.0014(13) C12B 0.0345(13) 0.0385(14) 0.0349(13) 0.0139(11) -0.0069(10) -0.0047(10) C13B 0.0330(13) 0.0579(17) 0.0434(14) 0.0257(13) -0.0057(11) 0.0015(12) C14B 0.0517(19) 0.065(2) 0.128(3) 0.047(2) 0.017(2) 0.0236(17) C15B 0.0442(16) 0.100(3) 0.0521(18) 0.0360(18) 0.0050(14) 0.0166(17) C16B 0.0384(16) 0.111(3) 0.067(2) 0.041(2) -0.0164(15) -0.0084(17) C17B 0.084(2) 0.0372(17) 0.124(3) 0.046(2) -0.056(2) -0.0271(16) C18B 0.062(2) 0.063(2) 0.075(2) 0.0252(18) 0.0110(17) -0.0220(17) C19B 0.131(4) 0.146(5) 0.134(4) 0.116(4) -0.059(3) -0.057(4) C20B 0.0496(17) 0.090(3) 0.0395(16) -0.0146(16) 0.0004(13) 0.0303(17) C21B 0.083(3) 0.183(5) 0.0411(19) 0.041(2) -0.0114(18) -0.069(3) C22B 0.0505(19) 0.128(4) 0.0518(19) 0.019(2) 0.0071(15) -0.034(2) C23B 0.108(3) 0.0532(19) 0.0405(16) 0.0047(14) 0.0298(17) -0.0101(19) C24B 0.218(6) 0.041(2) 0.073(3) 0.0050(18) 0.064(3) 0.002(3) C25B 0.159(4) 0.0407(19) 0.070(2) 0.0133(17) 0.029(3) -0.002(2) C26B 0.093(3) 0.0450(18) 0.0599(19) 0.0208(15) 0.0034(17) 0.0156(17) C27B 0.088(3) 0.0362(17) 0.073(2) 0.0048(15) 0.0116(19) 0.0122(16) C28B 0.097(3) 0.061(2) 0.078(3) 0.0006(19) 0.008(2) -0.028(2) C29B 0.0487(18) 0.075(2) 0.068(2) 0.0206(18) -0.0019(15) -0.0013(16) C30B 0.0438(16) 0.0454(17) 0.0639(18) 0.0111(14) 0.0141(13) 0.0108(13) C31B 0.103(3) 0.058(2) 0.062(2) 0.0327(17) -0.0020(19) 0.0030(19) C32B 0.074(2) 0.084(3) 0.0563(19) 0.0443(19) 0.0068(16) 0.0056(19) C33B 0.086(3) 0.115(4) 0.139(4) 0.090(3) -0.009(3) 0.022(3) C34B 0.063(2) 0.087(3) 0.093(3) 0.053(2) -0.0270(19) -0.0139(19) #----------------------------------------------------------------------------# # 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 Li O2 1.972(4) . ? Li O3 1.985(4) . ? Li O1 2.016(4) . ? Li Si 2.700(4) . ? Si N3 1.7755(19) . ? Si N1 1.8192(18) . ? Si N2 1.8308(18) . ? O1 C26 1.427(3) . ? O1 C23 1.439(3) . ? O2 C30 1.429(3) . ? O2 C27 1.434(3) . ? O3 C31 1.434(3) . ? O3 C34 1.443(3) . ? N1 C1 1.388(3) . ? N1 C7 1.460(3) . ? N2 C2 1.384(3) . ? N2 C12 1.457(3) . ? N3 C20 1.465(3) . ? N3 C17 1.481(3) . ? C1 C6 1.393(3) . ? C1 C2 1.425(3) . ? C2 C3 1.391(3) . ? C3 C4 1.395(4) . ? C4 C5 1.373(4) . ? C5 C6 1.400(4) . ? C7 C8 1.545(3) . ? C8 C9 1.515(3) . ? C8 C10 1.523(4) . ? C8 C11 1.530(3) . ? C12 C13 1.547(3) . ? C13 C15 1.517(4) . ? C13 C14 1.528(4) . ? C13 C16 1.532(4) . ? C17 C19 1.524(4) . ? C17 C18 1.527(4) . ? C20 C21 1.527(4) . ? C20 C22 1.535(4) . ? C23 C24 1.471(5) . ? C24 C25 1.462(6) . ? C25 C26 1.484(5) . ? C27 C28 1.498(4) . ? C28 C29 1.453(5) . ? C29 C30 1.457(5) . ? C31 C32 1.510(5) . ? C32 C33 1.496(5) . ? C33 C34 1.508(4) . ? Li1B O1B 1.986(5) . ? Li1B O3B 2.009(4) . ? Li1B O2B 2.026(5) . ? Li1B Si1B 2.736(4) . ? Si1B N3B 1.770(2) . ? Si1B N1B 1.8273(19) . ? Si1B N2B 1.8314(19) . ? O1B C26B 1.430(4) . ? O1B C23B 1.434(3) . ? O2B C30B 1.430(3) . ? O2B C27B 1.439(4) . ? O3B C34B 1.410(4) . ? O3B C32B 1.448(4) . ? N1B C1B 1.387(3) . ? N1B C7B 1.458(3) . ? N2B C2B 1.389(3) . ? N2B C12B 1.458(3) . ? N3B C20B 1.462(4) . ? N3B C17B 1.466(4) . ? C1B C6B 1.394(3) . ? C1B C2B 1.427(3) . ? C2B C3B 1.389(3) . ? C3B C4B 1.402(4) . ? C4B C5B 1.371(4) . ? C5B C6B 1.404(4) . ? C7B C8B 1.549(3) . ? C8B C10B 1.523(3) . ? C8B C9B 1.528(4) . ? C8B C11B 1.532(3) . ? C12B C13B 1.546(4) . ? C13B C14B 1.515(4) . ? C13B C15B 1.518(4) . ? C13B C16B 1.529(4) . ? C17B C19B 1.392(5) . ? C17B C18B 1.458(4) . ? C20B C21B 1.427(4) . ? C20B C22B 1.432(4) . ? C23B C24B 1.469(5) . ? C24B C25B 1.502(5) . ? C25B C26B 1.461(5) . ? C27B C28B 1.490(5) . ? C28B C29B 1.491(5) . ? C29B C30B 1.480(4) . ? C31B C33B 1.471(6) . ? C31B C32B 1.492(5) . ? C33B C34B 1.478(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li O3 109.1(2) . . ? O2 Li O1 96.06(19) . . ? O3 Li O1 100.5(2) . . ? O2 Li Si 121.61(19) . . ? O3 Li Si 104.91(17) . . ? O1 Li Si 122.57(18) . . ? N3 Si N1 107.55(9) . . ? N3 Si N2 101.91(9) . . ? N1 Si N2 85.75(8) . . ? N3 Si Li 127.86(11) . . ? N1 Si Li 108.66(11) . . ? N2 Si Li 116.92(11) . . ? C26 O1 C23 109.3(2) . . ? C26 O1 Li 130.8(2) . . ? C23 O1 Li 117.4(2) . . ? C30 O2 C27 107.83(19) . . ? C30 O2 Li 133.7(2) . . ? C27 O2 Li 118.49(18) . . ? C31 O3 C34 109.3(2) . . ? C31 O3 Li 133.6(2) . . ? C34 O3 Li 117.08(19) . . ? C1 N1 C7 119.19(18) . . ? C1 N1 Si 114.64(14) . . ? C7 N1 Si 123.85(14) . . ? C2 N2 C12 119.84(18) . . ? C2 N2 Si 114.46(14) . . ? C12 N2 Si 124.33(15) . . ? C20 N3 C17 115.62(18) . . ? C20 N3 Si 121.92(15) . . ? C17 N3 Si 121.83(15) . . ? N1 C1 C6 128.2(2) . . ? N1 C1 C2 112.54(19) . . ? C6 C1 C2 119.2(2) . . ? N2 C2 C3 128.5(2) . . ? N2 C2 C1 112.29(19) . . ? C3 C2 C1 119.2(2) . . ? C2 C3 C4 120.3(2) . . ? C5 C4 C3 120.8(2) . . ? C4 C5 C6 119.9(2) . . ? C1 C6 C5 120.4(2) . . ? N1 C7 C8 117.32(18) . . ? C9 C8 C10 109.2(2) . . ? C9 C8 C11 109.2(2) . . ? C10 C8 C11 109.0(2) . . ? C9 C8 C7 112.07(19) . . ? C10 C8 C7 109.36(19) . . ? C11 C8 C7 107.9(2) . . ? N2 C12 C13 117.3(2) . . ? C15 C13 C14 108.8(2) . . ? C15 C13 C16 109.2(2) . . ? C14 C13 C16 109.9(2) . . ? C15 C13 C12 109.9(2) . . ? C14 C13 C12 111.6(2) . . ? C16 C13 C12 107.3(2) . . ? N3 C17 C19 112.6(2) . . ? N3 C17 C18 112.6(2) . . ? C19 C17 C18 110.6(2) . . ? N3 C20 C21 114.1(2) . . ? N3 C20 C22 113.7(2) . . ? C21 C20 C22 108.9(2) . . ? O1 C23 C24 107.5(3) . . ? C25 C24 C23 104.6(3) . . ? C24 C25 C26 106.1(3) . . ? O1 C26 C25 105.5(3) . . ? O2 C27 C28 106.0(2) . . ? C29 C28 C27 105.4(3) . . ? C28 C29 C30 108.5(3) . . ? O2 C30 C29 106.1(3) . . ? O3 C31 C32 106.0(3) . . ? C33 C32 C31 102.6(3) . . ? C32 C33 C34 102.6(3) . . ? O3 C34 C33 105.7(2) . . ? O1B Li1B O3B 104.1(2) . . ? O1B Li1B O2B 104.3(2) . . ? O3B Li1B O2B 94.27(19) . . ? O1B Li1B Si1B 105.23(18) . . ? O3B Li1B Si1B 124.14(19) . . ? O2B Li1B Si1B 122.29(19) . . ? N3B Si1B N1B 104.90(9) . . ? N3B Si1B N2B 106.74(9) . . ? N1B Si1B N2B 85.03(9) . . ? N3B Si1B Li1B 115.90(11) . . ? N1B Si1B Li1B 122.32(11) . . ? N2B Si1B Li1B 117.28(11) . . ? C26B O1B C23B 109.5(2) . . ? C26B O1B Li1B 127.9(2) . . ? C23B O1B Li1B 121.1(2) . . ? C30B O2B C27B 108.7(2) . . ? C30B O2B Li1B 121.4(2) . . ? C27B O2B Li1B 129.9(2) . . ? C34B O3B C32B 104.9(2) . . ? C34B O3B Li1B 127.3(2) . . ? C32B O3B Li1B 127.7(2) . . ? C1B N1B C7B 119.23(19) . . ? C1B N1B Si1B 114.58(15) . . ? C7B N1B Si1B 124.05(15) . . ? C2B N2B C12B 119.59(19) . . ? C2B N2B Si1B 114.52(15) . . ? C12B N2B Si1B 123.21(15) . . ? C20B N3B C17B 114.8(3) . . ? C20B N3B Si1B 126.2(2) . . ? C17B N3B Si1B 118.9(2) . . ? N1B C1B C6B 128.6(2) . . ? N1B C1B C2B 112.3(2) . . ? C6B C1B C2B 119.1(2) . . ? C3B C2B N2B 128.5(2) . . ? C3B C2B C1B 119.5(2) . . ? N2B C2B C1B 112.00(19) . . ? C2B C3B C4B 120.5(2) . . ? C5B C4B C3B 120.1(2) . . ? C4B C5B C6B 120.6(2) . . ? C1B C6B C5B 120.2(2) . . ? N1B C7B C8B 116.69(19) . . ? C10B C8B C9B 109.2(2) . . ? C10B C8B C11B 109.3(2) . . ? C9B C8B C11B 108.7(2) . . ? C10B C8B C7B 112.08(19) . . ? C9B C8B C7B 109.2(2) . . ? C11B C8B C7B 108.3(2) . . ? N2B C12B C13B 117.4(2) . . ? C14B C13B C15B 111.0(3) . . ? C14B C13B C16B 109.9(3) . . ? C15B C13B C16B 106.9(2) . . ? C14B C13B C12B 112.3(2) . . ? C15B C13B C12B 109.1(2) . . ? C16B C13B C12B 107.4(2) . . ? C19B C17B C18B 125.0(3) . . ? C19B C17B N3B 118.7(3) . . ? C18B C17B N3B 116.2(3) . . ? C21B C20B C22B 124.1(3) . . ? C21B C20B N3B 118.4(3) . . ? C22B C20B N3B 117.4(3) . . ? O1B C23B C24B 106.1(3) . . ? C23B C24B C25B 104.0(3) . . ? C26B C25B C24B 103.7(3) . . ? O1B C26B C25B 106.6(3) . . ? O2B C27B C28B 106.6(3) . . ? C27B C28B C29B 104.0(3) . . ? C30B C29B C28B 103.4(3) . . ? O2B C30B C29B 107.2(2) . . ? C33B C31B C32B 104.6(3) . . ? O3B C32B C31B 106.8(3) . . ? C31B C33B C34B 106.3(3) . . ? O3B C34B C33B 106.2(3) . . ? #===END