#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Deacon, G.' 'Forsyth, Craig M.' 'Scott, Natalie M.' _publ_contact_author_name 'Prof G Deacon' _publ_contact_author_address ; Prof G Deacon Centre for Green Chemistry Monash University School of Chemistry PO Box 23 Victoria 3800 AUSTRALIA ; _publ_contact_author_email 'G.DEACON@SCI.MONASH.EDU.AU' data_c_lidme #\mydocu~1\craig'~1\listru~1\lidme\lidme _database_code_CSD 163622 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (1,2-dimethoxyethane)(N-(2-phenoxyphenyl)-N-(trimethylsilyl)amido)lithium(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H28 Li N O3 Si' _chemical_formula_weight 353.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1225(2) _cell_length_b 12.8885(2) _cell_length_c 16.4847(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.395(1) _cell_angle_gamma 90.00 _cell_volume 2052.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.144 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf Nonius Kappa CCD _diffrn_measurement_method 1 deg phi scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27566 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5063 _reflns_number_gt 3500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Povray' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.8202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5063 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.5447(3) 0.5890(2) 0.25499(17) 0.0265(6) Uani 1 1 d . . . Si1 Si 0.23233(4) 0.53438(3) 0.14927(3) 0.02443(12) Uani 1 1 d . . . N1 N 0.34637(12) 0.59838(10) 0.23082(8) 0.0227(3) Uani 1 1 d . . . O1 O 0.55251(10) 0.68899(8) 0.35399(7) 0.0233(2) Uani 1 1 d . . . C1 C 0.31107(15) 0.65380(11) 0.29149(10) 0.0206(3) Uani 1 1 d . . . C2 C 0.41505(15) 0.70326(12) 0.35729(10) 0.0217(3) Uani 1 1 d . . . C3 C 0.38977(18) 0.76430(13) 0.41927(11) 0.0299(4) Uani 1 1 d . . . H3 H 0.4641 0.7980 0.4599 0.036 Uiso 1 1 calc R . . C4 C 0.2548(2) 0.77658(14) 0.42239(12) 0.0362(4) Uani 1 1 d . . . H4 H 0.2359 0.8180 0.4653 0.043 Uiso 1 1 calc R . . C5 C 0.14905(18) 0.72732(13) 0.36186(12) 0.0341(4) Uani 1 1 d . . . H5 H 0.0567 0.7337 0.3641 0.041 Uiso 1 1 calc R . . C6 C 0.17512(16) 0.66876(12) 0.29794(11) 0.0270(4) Uani 1 1 d . . . H6 H 0.0994 0.6373 0.2567 0.032 Uiso 1 1 calc R . . C7 C 0.08855(17) 0.61799(15) 0.08193(11) 0.0351(4) Uani 1 1 d . . . H7A H 0.1282 0.6785 0.0617 0.053 Uiso 1 1 calc R . . H7B H 0.0295 0.6412 0.1159 0.053 Uiso 1 1 calc R . . H7C H 0.0331 0.5778 0.0331 0.053 Uiso 1 1 calc R . . C8 C 0.1488(2) 0.42049(14) 0.18536(12) 0.0406(5) Uani 1 1 d . . . H8A H 0.0941 0.4448 0.2217 0.061 Uiso 1 1 calc R . . H8B H 0.2205 0.3726 0.2175 0.061 Uiso 1 1 calc R . . H8C H 0.0880 0.3847 0.1357 0.061 Uiso 1 1 calc R . . C9 C 0.33381(19) 0.48173(16) 0.08059(12) 0.0393(4) Uani 1 1 d . . . H9A H 0.3793 0.5390 0.0603 0.059 Uiso 1 1 calc R . . H9B H 0.2714 0.4454 0.0319 0.059 Uiso 1 1 calc R . . H9C H 0.4040 0.4333 0.1136 0.059 Uiso 1 1 calc R . . C11 C 0.65130(15) 0.65127(11) 0.42655(10) 0.0216(3) Uani 1 1 d . . . C12 C 0.61684(16) 0.59801(12) 0.49017(10) 0.0265(4) Uani 1 1 d . . . H12 H 0.5227 0.5899 0.4883 0.032 Uiso 1 1 calc R . . C13 C 0.72227(18) 0.55641(14) 0.55696(11) 0.0344(4) Uani 1 1 d . . . H13 H 0.6998 0.5193 0.6009 0.041 Uiso 1 1 calc R . . C14 C 0.85917(18) 0.56858(15) 0.56002(12) 0.0373(4) Uani 1 1 d . . . H14 H 0.9306 0.5396 0.6056 0.045 Uiso 1 1 calc R . . C15 C 0.89175(17) 0.62315(14) 0.49649(12) 0.0357(4) Uani 1 1 d . . . H15 H 0.9860 0.6322 0.4989 0.043 Uiso 1 1 calc R . . C16 C 0.78814(16) 0.66494(13) 0.42906(11) 0.0288(4) Uani 1 1 d . . . H16 H 0.8108 0.7023 0.3854 0.035 Uiso 1 1 calc R . . O2 O 0.62838(11) 0.45070(9) 0.27941(8) 0.0309(3) Uani 1 1 d . . . O3 O 0.70121(11) 0.61441(9) 0.20814(7) 0.0295(3) Uani 1 1 d . . . C20 C 0.6147(2) 0.37949(14) 0.34255(14) 0.0470(5) Uani 1 1 d . . . H20A H 0.5212 0.3847 0.3482 0.071 Uiso 1 1 calc R . . H20B H 0.6829 0.3961 0.3971 0.071 Uiso 1 1 calc R . . H20C H 0.6304 0.3087 0.3257 0.071 Uiso 1 1 calc R . . C21 C 0.76174(17) 0.44802(14) 0.26742(13) 0.0359(4) Uani 1 1 d . . . H21A H 0.7854 0.3762 0.2555 0.043 Uiso 1 1 calc R . . H21B H 0.8327 0.4729 0.3192 0.043 Uiso 1 1 calc R . . C22 C 0.7569(2) 0.51682(14) 0.19401(13) 0.0384(4) Uani 1 1 d . . . H22A H 0.8512 0.5263 0.1890 0.046 Uiso 1 1 calc R . . H22B H 0.6980 0.4854 0.1406 0.046 Uiso 1 1 calc R . . C23 C 0.7073(2) 0.69032(16) 0.14662(13) 0.0458(5) Uani 1 1 d . . . H23A H 0.6681 0.7557 0.1592 0.069 Uiso 1 1 calc R . . H23B H 0.6541 0.6662 0.0899 0.069 Uiso 1 1 calc R . . H23C H 0.8039 0.7013 0.1484 0.069 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 0.0225(13) 0.0280(14) 0.0301(14) -0.0010(11) 0.0095(11) 0.0030(12) Si1 0.0225(2) 0.0254(2) 0.0237(2) 0.00072(18) 0.00436(17) -0.00095(19) N1 0.0184(6) 0.0232(7) 0.0268(7) -0.0020(5) 0.0073(5) 0.0021(6) O1 0.0180(5) 0.0286(6) 0.0238(6) 0.0012(4) 0.0071(4) 0.0004(5) C1 0.0206(7) 0.0164(7) 0.0270(8) 0.0052(6) 0.0104(6) 0.0021(6) C2 0.0195(7) 0.0211(8) 0.0266(8) 0.0024(6) 0.0102(6) 0.0027(6) C3 0.0352(9) 0.0262(8) 0.0304(9) -0.0045(7) 0.0129(7) -0.0005(8) C4 0.0439(10) 0.0311(9) 0.0436(11) -0.0022(8) 0.0283(9) 0.0076(9) C5 0.0306(9) 0.0291(9) 0.0516(11) 0.0066(8) 0.0258(8) 0.0087(8) C6 0.0199(8) 0.0246(8) 0.0391(10) 0.0034(7) 0.0127(7) 0.0025(7) C7 0.0255(8) 0.0485(11) 0.0310(9) 0.0098(8) 0.0080(7) 0.0026(8) C8 0.0470(11) 0.0319(10) 0.0370(10) 0.0012(8) 0.0037(9) -0.0118(9) C9 0.0379(10) 0.0475(11) 0.0299(9) -0.0076(8) 0.0063(8) 0.0073(9) C11 0.0210(7) 0.0193(7) 0.0237(8) -0.0036(6) 0.0054(6) -0.0001(6) C12 0.0241(8) 0.0246(8) 0.0314(9) 0.0010(7) 0.0090(7) -0.0037(7) C13 0.0361(9) 0.0335(9) 0.0325(10) 0.0077(7) 0.0084(8) -0.0005(8) C14 0.0292(9) 0.0423(10) 0.0343(10) 0.0057(8) 0.0000(8) 0.0047(8) C15 0.0205(8) 0.0430(11) 0.0403(11) 0.0001(8) 0.0042(7) -0.0018(8) C16 0.0239(8) 0.0316(9) 0.0317(9) 0.0002(7) 0.0097(7) -0.0043(7) O2 0.0291(6) 0.0282(6) 0.0397(7) 0.0025(5) 0.0166(5) 0.0042(5) O3 0.0310(6) 0.0262(6) 0.0367(7) -0.0002(5) 0.0181(5) 0.0034(5) C20 0.0670(14) 0.0277(9) 0.0565(13) 0.0047(9) 0.0339(11) 0.0032(10) C21 0.0232(8) 0.0314(10) 0.0538(12) -0.0002(8) 0.0128(8) 0.0079(8) C22 0.0370(10) 0.0332(10) 0.0548(12) -0.0042(9) 0.0285(9) 0.0058(8) C23 0.0638(14) 0.0392(11) 0.0440(12) 0.0071(9) 0.0308(10) 0.0061(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N1 1.930(3) . ? Li1 O2 1.963(3) . ? Li1 O3 1.986(3) . ? Li1 O1 2.062(3) . ? Li1 C1 2.739(3) . ? Li1 C22 2.789(3) . ? Si1 N1 1.7006(14) . ? Si1 C9 1.8688(19) . ? Si1 C8 1.8774(19) . ? Si1 C7 1.8830(18) . ? N1 C1 1.3609(19) . ? O1 C11 1.3971(19) . ? O1 C2 1.4205(17) . ? C1 C2 1.417(2) . ? C1 C6 1.425(2) . ? C2 C3 1.373(2) . ? C3 C4 1.391(2) . ? C4 C5 1.381(3) . ? C5 C6 1.384(2) . ? C11 C12 1.383(2) . ? C11 C16 1.385(2) . ? C12 C13 1.391(2) . ? C13 C14 1.381(2) . ? C14 C15 1.381(3) . ? C15 C16 1.389(2) . ? O2 C21 1.4220(19) . ? O2 C20 1.425(2) . ? O3 C23 1.424(2) . ? O3 C22 1.426(2) . ? C21 C22 1.489(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 Li1 O2 117.24(14) . . ? N1 Li1 O3 144.16(16) . . ? O2 Li1 O3 83.35(11) . . ? N1 Li1 O1 85.16(11) . . ? O2 Li1 O1 119.55(14) . . ? O3 Li1 O1 111.00(13) . . ? N1 Li1 C1 27.53(6) . . ? O2 Li1 C1 125.44(13) . . ? O3 Li1 C1 151.22(14) . . ? O1 Li1 C1 57.79(8) . . ? N1 Li1 C22 144.29(14) . . ? O2 Li1 C22 55.91(8) . . ? O3 Li1 C22 28.98(6) . . ? O1 Li1 C22 129.95(13) . . ? C1 Li1 C22 171.59(12) . . ? N1 Si1 C9 106.79(8) . . ? N1 Si1 C8 113.10(8) . . ? C9 Si1 C8 106.82(9) . . ? N1 Si1 C7 114.25(8) . . ? C9 Si1 C7 108.58(8) . . ? C8 Si1 C7 106.99(9) . . ? C1 N1 Si1 124.77(10) . . ? C1 N1 Li1 111.50(13) . . ? Si1 N1 Li1 123.44(11) . . ? C11 O1 C2 118.09(11) . . ? C11 O1 Li1 107.95(11) . . ? C2 O1 Li1 107.76(11) . . ? N1 C1 C2 120.03(13) . . ? N1 C1 C6 126.70(14) . . ? C2 C1 C6 113.27(14) . . ? N1 C1 Li1 40.97(9) . . ? C2 C1 Li1 79.21(10) . . ? C6 C1 Li1 166.98(13) . . ? C3 C2 C1 124.50(14) . . ? C3 C2 O1 120.35(14) . . ? C1 C2 O1 115.11(13) . . ? C2 C3 C4 119.76(16) . . ? C5 C4 C3 118.61(16) . . ? C4 C5 C6 121.18(16) . . ? C5 C6 C1 122.61(16) . . ? C12 C11 C16 121.16(15) . . ? C12 C11 O1 122.95(13) . . ? C16 C11 O1 115.78(14) . . ? C11 C12 C13 118.94(15) . . ? C14 C13 C12 120.61(16) . . ? C13 C14 C15 119.66(16) . . ? C14 C15 C16 120.67(16) . . ? C11 C16 C15 118.95(16) . . ? C21 O2 C20 112.93(14) . . ? C21 O2 Li1 111.28(12) . . ? C20 O2 Li1 127.17(13) . . ? C23 O3 C22 112.73(13) . . ? C23 O3 Li1 126.85(14) . . ? C22 O3 Li1 108.56(12) . . ? O2 C21 C22 107.25(14) . . ? O3 C22 C21 108.12(14) . . ? O3 C22 Li1 42.45(9) . . ? C21 C22 Li1 75.37(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.309 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.048 data_c_liphan #:\mydocu~1\craig'~1\listru~1\lidigl~1\liphan _database_code_CSD 163623 _audit_creation_method SHELXL-97 _chemical_name_systematic ; di[(diethyl ether)(N-(2-phenoxyphenyl)-N-(trimethylsilyl)amido)lithium(I)) (N-(2-(2'-lithiophenyloxy)phenyl)-N-(trimethylsilyl)amido)lithium(I)] (bis(2-methoxyethyl) ether) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H104 Li6 N4 O9 Si4' _chemical_formula_weight 1347.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 40.3040(11) _cell_length_b 10.5611(3) _cell_length_c 18.7238(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.263(2) _cell_angle_gamma 90.00 _cell_volume 7866(3) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 0.129 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf Nonius Kappa CCD _diffrn_measurement_method 1 deg phi scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20642 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0911 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 28.27 _reflns_number_total 9449 _reflns_number_gt 5969 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Povray' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+14.0602P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9449 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1222 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.15951(11) 0.3663(4) 0.3685(2) 0.0226(9) Uani 1 1 d . . . Si1 Si 0.133321(17) 0.58331(7) 0.46783(4) 0.01848(17) Uani 1 1 d . . . O1 O 0.17841(4) 0.22543(17) 0.43201(9) 0.0227(4) Uani 1 1 d . . . N1 N 0.14225(5) 0.4256(2) 0.45765(10) 0.0178(4) Uani 1 1 d . . . C1 C 0.15568(6) 0.3511(2) 0.51633(13) 0.0172(5) Uani 1 1 d . . . C2 C 0.17501(6) 0.2434(2) 0.50516(12) 0.0180(5) Uani 1 1 d . . . C3 C 0.18914(6) 0.1625(3) 0.55943(13) 0.0214(6) Uani 1 1 d . . . H3 H 0.2019 0.0915 0.5487 0.026 Uiso 1 1 calc R . . C4 C 0.18436(6) 0.1865(3) 0.63049(14) 0.0255(6) Uani 1 1 d . . . H4 H 0.1940 0.1321 0.6687 0.031 Uiso 1 1 calc R . . C5 C 0.16557(7) 0.2896(3) 0.64442(14) 0.0269(6) Uani 1 1 d . . . H5 H 0.1621 0.3061 0.6925 0.032 Uiso 1 1 calc R . . C6 C 0.15158(6) 0.3700(3) 0.58885(13) 0.0238(6) Uani 1 1 d . . . H6 H 0.1387 0.4405 0.6002 0.029 Uiso 1 1 calc R . . C7 C 0.09147(7) 0.6101(3) 0.49760(15) 0.0285(6) Uani 1 1 d . . . H7A H 0.0915 0.5704 0.5449 0.043 Uiso 1 1 calc R . . H7B H 0.0736 0.5725 0.4621 0.043 Uiso 1 1 calc R . . H7C H 0.0875 0.7012 0.5012 0.043 Uiso 1 1 calc R . . C8 C 0.16670(7) 0.6673(3) 0.53323(15) 0.0291(6) Uani 1 1 d . . . H8A H 0.1682 0.6288 0.5813 0.044 Uiso 1 1 calc R . . H8B H 0.1608 0.7570 0.5359 0.044 Uiso 1 1 calc R . . H8C H 0.1884 0.6596 0.5164 0.044 Uiso 1 1 calc R . . C9 C 0.13127(7) 0.6609(2) 0.37746(13) 0.0230(6) Uani 1 1 d . . . H9A H 0.1527 0.6485 0.3598 0.034 Uiso 1 1 calc R . . H9B H 0.1271 0.7517 0.3820 0.034 Uiso 1 1 calc R . . H9C H 0.1130 0.6230 0.3432 0.034 Uiso 1 1 calc R . . C11 C 0.19812(6) 0.1247(2) 0.41413(13) 0.0199(5) Uani 1 1 d . . . C12 C 0.18259(7) 0.0155(3) 0.38714(15) 0.0274(6) Uani 1 1 d . . . H12 H 0.1589 0.0065 0.3829 0.033 Uiso 1 1 calc R . . C13 C 0.20209(7) -0.0818(3) 0.36599(17) 0.0350(7) Uani 1 1 d . . . H13 H 0.1918 -0.1581 0.3470 0.042 Uiso 1 1 calc R . . C14 C 0.23669(7) -0.0674(3) 0.37271(16) 0.0336(7) Uani 1 1 d . . . H14 H 0.2500 -0.1347 0.3590 0.040 Uiso 1 1 calc R . . C15 C 0.25192(7) 0.0440(3) 0.39910(15) 0.0297(7) Uani 1 1 d . . . H15 H 0.2756 0.0537 0.4029 0.036 Uiso 1 1 calc R . . C16 C 0.23264(6) 0.1415(3) 0.42002(14) 0.0241(6) Uani 1 1 d . . . H16 H 0.2428 0.2186 0.4381 0.029 Uiso 1 1 calc R . . O3 O 0.19433(4) 0.41150(19) 0.30957(10) 0.0280(4) Uani 1 1 d . . . C31 C 0.22597(8) 0.5333(3) 0.40436(18) 0.0454(9) Uani 1 1 d . . . H31A H 0.2477 0.5743 0.4200 0.068 Uiso 1 1 calc R . . H31B H 0.2222 0.4689 0.4399 0.068 Uiso 1 1 calc R . . H31C H 0.2080 0.5968 0.4005 0.068 Uiso 1 1 calc R . . C32 C 0.22584(8) 0.4729(4) 0.33328(18) 0.0472(9) Uani 1 1 d . . . H32A H 0.2298 0.5379 0.2974 0.057 Uiso 1 1 calc R . . H32B H 0.2442 0.4100 0.3369 0.057 Uiso 1 1 calc R . . C33 C 0.19229(7) 0.3610(3) 0.23726(14) 0.0303(7) Uani 1 1 d . . . H33A H 0.2020 0.4233 0.2070 0.036 Uiso 1 1 calc R . . H33B H 0.1683 0.3494 0.2162 0.036 Uiso 1 1 calc R . . C34 C 0.21025(8) 0.2369(3) 0.23452(16) 0.0367(7) Uani 1 1 d . . . H34A H 0.2078 0.2075 0.1843 0.055 Uiso 1 1 calc R . . H34B H 0.2005 0.1741 0.2637 0.055 Uiso 1 1 calc R . . H34C H 0.2342 0.2480 0.2538 0.055 Uiso 1 1 calc R . . Li21 Li 0.09981(11) 0.3304(4) 0.4079(2) 0.0217(9) Uani 1 1 d . . . Si21 Si 0.075519(18) 0.06452(7) 0.46943(4) 0.02072(18) Uani 1 1 d . . . O21 O 0.11624(4) 0.30442(16) 0.30741(8) 0.0165(4) Uani 1 1 d . . . N21 N 0.08156(5) 0.1521(2) 0.39543(11) 0.0199(5) Uani 1 1 d . A . C21 C 0.09268(6) 0.1008(2) 0.33520(12) 0.0168(5) Uani 1 1 d . . . C22 C 0.10837(6) 0.1771(2) 0.28792(13) 0.0172(5) Uani 1 1 d . . . C23 C 0.11879(6) 0.1305(3) 0.22609(13) 0.0205(6) Uani 1 1 d . . . H23 H 0.1287 0.1861 0.1957 0.025 Uiso 1 1 calc R . . C24 C 0.11490(7) 0.0036(3) 0.20812(14) 0.0241(6) Uani 1 1 d . . . H24 H 0.1221 -0.0285 0.1658 0.029 Uiso 1 1 calc R . . C25 C 0.10029(6) -0.0756(3) 0.25324(13) 0.0231(6) Uani 1 1 d . . . H25 H 0.0978 -0.1632 0.2421 0.028 Uiso 1 1 calc R . . C26 C 0.08932(6) -0.0282(2) 0.31435(13) 0.0203(5) Uani 1 1 d . . . H26 H 0.0791 -0.0848 0.3437 0.024 Uiso 1 1 calc R . . C27 C 0.06752(8) 0.1814(3) 0.53948(15) 0.0367(7) Uani 1 1 d . . . H27A H 0.0478 0.2327 0.5206 0.055 Uiso 1 1 calc R . . H27B H 0.0871 0.2366 0.5517 0.055 Uiso 1 1 calc R . . H27C H 0.0634 0.1362 0.5829 0.055 Uiso 1 1 calc R . . C28 C 0.03858(7) -0.0475(3) 0.45593(16) 0.0324(7) Uani 1 1 d . . . H28A H 0.0418 -0.1111 0.4195 0.049 Uiso 1 1 calc R . . H28B H 0.0179 0.0001 0.4395 0.049 Uiso 1 1 calc R . . H28C H 0.0369 -0.0898 0.5018 0.049 Uiso 1 1 calc R . . C29 C 0.11317(7) -0.0324(3) 0.50665(14) 0.0254(6) Uani 1 1 d . . . H29A H 0.1175 -0.0944 0.4704 0.038 Uiso 1 1 calc R . . H29B H 0.1090 -0.0767 0.5503 0.038 Uiso 1 1 calc R . . H29C H 0.1327 0.0232 0.5188 0.038 Uiso 1 1 calc R . . C211 C 0.09188(6) 0.4002(2) 0.27810(13) 0.0163(5) Uani 1 1 d . . . C212 C 0.06513(6) 0.4208(3) 0.31534(13) 0.0210(5) Uani 1 1 d . A . C213 C 0.04491(6) 0.5238(3) 0.28668(14) 0.0248(6) Uani 1 1 d . . . H213 H 0.0260 0.5451 0.3087 0.030 Uiso 1 1 calc R . . C214 C 0.05106(7) 0.5959(3) 0.22808(14) 0.0257(6) Uani 1 1 d . . . H214 H 0.0366 0.6646 0.2115 0.031 Uiso 1 1 calc R . . C215 C 0.07810(7) 0.5680(3) 0.19390(14) 0.0251(6) Uani 1 1 d . . . H215 H 0.0822 0.6164 0.1535 0.030 Uiso 1 1 calc R . . C216 C 0.09912(6) 0.4682(2) 0.21940(14) 0.0218(6) Uani 1 1 d . . . H216 H 0.1180 0.4471 0.1971 0.026 Uiso 1 1 calc R . . Li3 Li 0.04061(12) 0.2597(5) 0.3518(3) 0.0314(11) Uani 1 1 d . . . O51 O 0.00154(10) 0.2904(4) 0.4059(2) 0.0299(9) Uiso 0.50 1 d P A 1 O52 O -0.00235(11) 0.2307(4) 0.3685(2) 0.0403(11) Uiso 0.50 1 d P A 2 O53 O -0.00080(12) 0.1794(5) 0.2761(2) 0.0494(13) Uiso 0.50 1 d P . 1 C51 C -0.02506(9) 0.1450(4) 0.32339(18) 0.0476(9) Uiso 1 1 d . . . H51A H -0.0464 0.1165 0.2941 0.057 Uiso 1 1 calc R A 1 H51B H -0.0160 0.0752 0.3562 0.057 Uiso 1 1 calc R A 1 C54 C -0.00190(17) 0.3975(7) 0.4465(4) 0.0447(16) Uiso 0.50 1 d P A 1 H54A H 0.0200 0.4204 0.4744 0.067 Uiso 0.50 1 calc PR A 1 H54B H -0.0178 0.3805 0.4798 0.067 Uiso 0.50 1 calc PR A 1 H54C H -0.0103 0.4675 0.4143 0.067 Uiso 0.50 1 calc PR A 1 C52 C -0.03069(16) 0.2561(6) 0.3647(3) 0.0355(14) Uiso 0.50 1 d P A 1 H52A H -0.0470 0.2375 0.3975 0.043 Uiso 0.50 1 calc PR A 1 H52B H -0.0396 0.3261 0.3320 0.043 Uiso 0.50 1 calc PR A 1 C50 C -0.0064(2) 0.0796(8) 0.2730(4) 0.055(2) Uiso 0.50 1 d P . 2 H50A H 0.0114 0.0401 0.3088 0.066 Uiso 0.50 1 calc PR . 2 H50B H -0.0224 0.0095 0.2583 0.066 Uiso 0.50 1 calc PR . 2 C53 C -0.0191(2) 0.3252(9) 0.4023(5) 0.070(2) Uiso 0.50 1 d P A 2 H53A H -0.0025 0.3795 0.4317 0.106 Uiso 0.50 1 calc PR A 2 H53B H -0.0335 0.2853 0.4333 0.106 Uiso 0.50 1 calc PR A 2 H53C H -0.0329 0.3765 0.3653 0.106 Uiso 0.50 1 calc PR A 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 0.021(2) 0.025(2) 0.023(2) 0.0015(19) 0.0048(17) 0.0019(19) Si1 0.0183(3) 0.0185(4) 0.0182(4) -0.0017(3) 0.0017(3) 0.0032(3) O1 0.0274(10) 0.0245(10) 0.0167(9) 0.0014(7) 0.0045(7) 0.0121(8) N1 0.0171(10) 0.0191(11) 0.0170(11) 0.0010(9) 0.0017(8) 0.0034(9) C1 0.0152(12) 0.0185(13) 0.0177(13) 0.0008(10) 0.0014(9) -0.0003(10) C2 0.0161(12) 0.0249(14) 0.0133(12) -0.0004(10) 0.0031(9) 0.0003(10) C3 0.0169(12) 0.0246(14) 0.0229(14) 0.0026(11) 0.0035(10) 0.0034(11) C4 0.0211(13) 0.0342(16) 0.0199(14) 0.0102(12) -0.0002(10) 0.0006(12) C5 0.0251(14) 0.0400(18) 0.0165(13) 0.0034(12) 0.0057(11) 0.0024(13) C6 0.0232(14) 0.0297(15) 0.0193(14) -0.0016(11) 0.0053(10) 0.0049(12) C7 0.0279(15) 0.0279(16) 0.0312(16) 0.0001(12) 0.0095(12) 0.0053(12) C8 0.0305(15) 0.0271(16) 0.0272(15) -0.0046(12) -0.0030(12) 0.0031(12) C9 0.0250(14) 0.0185(14) 0.0245(14) 0.0003(11) 0.0011(11) 0.0016(11) C11 0.0223(13) 0.0215(14) 0.0168(13) 0.0025(10) 0.0060(10) 0.0071(11) C12 0.0204(14) 0.0270(15) 0.0363(16) 0.0036(13) 0.0090(12) 0.0021(12) C13 0.0313(16) 0.0243(16) 0.0513(19) -0.0065(14) 0.0123(14) -0.0007(13) C14 0.0314(16) 0.0298(17) 0.0430(18) -0.0003(14) 0.0159(13) 0.0113(13) C15 0.0177(13) 0.0376(18) 0.0347(16) 0.0038(13) 0.0068(12) 0.0043(12) C16 0.0212(14) 0.0258(15) 0.0242(14) -0.0006(11) 0.0007(11) 0.0021(11) O3 0.0173(9) 0.0395(12) 0.0274(10) 0.0014(9) 0.0042(7) -0.0015(8) C31 0.0318(17) 0.049(2) 0.052(2) -0.0032(17) -0.0043(15) 0.0039(16) C32 0.0297(17) 0.064(3) 0.048(2) -0.0075(18) 0.0072(15) -0.0121(16) C33 0.0255(15) 0.0446(19) 0.0222(15) 0.0070(13) 0.0084(11) 0.0015(13) C34 0.0413(18) 0.043(2) 0.0271(16) 0.0064(14) 0.0101(13) 0.0039(15) Li21 0.024(2) 0.021(2) 0.019(2) -0.0003(18) 0.0028(17) 0.0024(18) Si21 0.0247(4) 0.0197(4) 0.0196(4) 0.0021(3) 0.0091(3) 0.0024(3) O21 0.0152(8) 0.0174(9) 0.0164(9) 0.0005(7) 0.0012(6) 0.0021(7) N21 0.0236(11) 0.0171(11) 0.0206(11) 0.0000(9) 0.0082(9) 0.0020(9) C21 0.0133(11) 0.0196(13) 0.0167(12) 0.0018(10) -0.0004(9) 0.0028(10) C22 0.0142(12) 0.0170(13) 0.0195(13) -0.0016(10) -0.0001(9) 0.0032(10) C23 0.0199(13) 0.0255(14) 0.0164(13) 0.0025(11) 0.0041(10) 0.0030(11) C24 0.0276(15) 0.0277(15) 0.0175(13) -0.0042(11) 0.0048(11) 0.0061(12) C25 0.0272(14) 0.0192(14) 0.0218(14) -0.0040(11) 0.0010(11) 0.0016(11) C26 0.0222(13) 0.0184(13) 0.0206(13) 0.0030(10) 0.0040(10) -0.0001(11) C27 0.052(2) 0.0345(18) 0.0279(16) -0.0010(13) 0.0191(14) 0.0099(15) C28 0.0247(15) 0.0393(18) 0.0348(17) 0.0119(13) 0.0099(12) -0.0018(13) C29 0.0278(15) 0.0227(15) 0.0262(15) -0.0009(11) 0.0056(11) -0.0021(12) C211 0.0153(12) 0.0143(12) 0.0178(12) 0.0014(10) -0.0019(9) 0.0003(9) C212 0.0177(12) 0.0225(14) 0.0230(13) 0.0005(11) 0.0035(10) 0.0020(11) C213 0.0184(13) 0.0240(15) 0.0313(15) -0.0002(12) 0.0021(11) 0.0024(11) C214 0.0212(13) 0.0216(15) 0.0316(15) 0.0046(12) -0.0039(11) 0.0029(11) C215 0.0313(15) 0.0216(14) 0.0207(14) 0.0064(11) -0.0010(11) -0.0021(12) C216 0.0207(13) 0.0225(14) 0.0224(14) -0.0001(11) 0.0043(10) -0.0016(11) Li3 0.026(2) 0.031(3) 0.038(3) 0.001(2) 0.009(2) -0.002(2) _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 O3 1.978(5) . ? Li1 O1 1.979(5) . ? Li1 N1 2.009(5) . ? Li1 O21 2.033(5) . ? Si1 N1 1.722(2) . ? Si1 C9 1.870(3) . ? Si1 C7 1.881(3) . ? Si1 C8 1.888(3) . ? O1 C11 1.400(3) . ? O1 C2 1.411(3) . ? N1 C1 1.388(3) . ? N1 Li21 2.072(5) . ? C1 C6 1.408(3) . ? C1 C2 1.413(3) . ? C2 C3 1.379(3) . ? C3 C4 1.398(4) . ? C4 C5 1.376(4) . ? C5 C6 1.390(4) . ? C11 C12 1.369(4) . ? C11 C16 1.389(4) . ? C12 C13 1.390(4) . ? C13 C14 1.388(4) . ? C14 C15 1.381(4) . ? C15 C16 1.384(4) . ? O3 C32 1.432(3) . ? O3 C33 1.445(3) . ? C31 C32 1.475(5) . ? C33 C34 1.502(4) . ? Li21 N21 2.021(5) . ? Li21 O21 2.110(4) . ? Li21 C212 2.256(5) . ? Li21 C211 2.510(5) . ? Si21 N21 1.716(2) . ? Si21 C27 1.866(3) . ? Si21 C29 1.869(3) . ? Si21 C28 1.887(3) . ? O21 C22 1.416(3) . ? O21 C211 1.455(3) . ? N21 C21 1.389(3) . ? N21 Li3 2.061(5) . ? C21 C26 1.418(3) . ? C21 C22 1.418(3) . ? C22 C23 1.384(3) . ? C23 C24 1.385(4) . ? C24 C25 1.386(4) . ? C25 C26 1.385(3) . ? C211 C216 1.382(3) . ? C211 C212 1.392(3) . ? C212 C213 1.412(4) . ? C212 Li3 2.134(6) . ? C213 C214 1.390(4) . ? C214 C215 1.382(4) . ? C215 C216 1.388(4) . ? Li3 O52 1.835(6) . ? Li3 O51 2.031(6) . ? Li3 O53 2.180(7) . ? O51 C54 1.382(8) . ? O51 C52 1.446(7) . ? O52 C53 1.410(10) . ? O52 C51 1.457(6) . ? O53 O53 0.989(8) 2 ? O53 C51 1.467(5) . ? C51 C52 1.444(7) . ? C51 C50 1.470(7) . ? C50 C50 1.074(13) 2 ? 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 Li1 O1 106.1(2) . . ? O3 Li1 N1 139.4(3) . . ? O1 Li1 N1 83.47(18) . . ? O3 Li1 O21 112.6(2) . . ? O1 Li1 O21 108.0(2) . . ? N1 Li1 O21 100.8(2) . . ? N1 Si1 C9 107.66(11) . . ? N1 Si1 C7 113.06(12) . . ? C9 Si1 C7 106.93(12) . . ? N1 Si1 C8 112.73(11) . . ? C9 Si1 C8 107.72(13) . . ? C7 Si1 C8 108.46(13) . . ? C11 O1 C2 118.80(18) . . ? C11 O1 Li1 127.30(19) . . ? C2 O1 Li1 113.20(19) . . ? C1 N1 Si1 121.49(16) . . ? C1 N1 Li1 109.8(2) . . ? Si1 N1 Li1 120.01(17) . . ? C1 N1 Li21 105.6(2) . . ? Si1 N1 Li21 110.31(16) . . ? Li1 N1 Li21 81.16(18) . . ? N1 C1 C6 126.3(2) . . ? N1 C1 C2 119.5(2) . . ? C6 C1 C2 114.2(2) . . ? C3 C2 O1 122.6(2) . . ? C3 C2 C1 124.2(2) . . ? O1 C2 C1 113.2(2) . . ? C2 C3 C4 119.1(2) . . ? C5 C4 C3 119.2(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 C1 122.6(3) . . ? C12 C11 C16 122.0(2) . . ? C12 C11 O1 119.0(2) . . ? C16 C11 O1 118.9(2) . . ? C11 C12 C13 118.8(3) . . ? C14 C13 C12 119.9(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C16 119.8(3) . . ? C15 C16 C11 118.9(3) . . ? C32 O3 C33 111.8(2) . . ? C32 O3 Li1 127.6(2) . . ? C33 O3 Li1 119.7(2) . . ? O3 C32 C31 110.5(3) . . ? O3 C33 C34 113.5(2) . . ? N21 Li21 N1 139.7(2) . . ? N21 Li21 O21 86.37(18) . . ? N1 Li21 O21 96.28(19) . . ? N21 Li21 C212 97.86(19) . . ? N1 Li21 C212 120.3(2) . . ? O21 Li21 C212 67.35(14) . . ? N21 Li21 C211 100.07(18) . . ? N1 Li21 C211 105.08(19) . . ? O21 Li21 C211 35.37(9) . . ? C212 Li21 C211 33.43(10) . . ? N21 Si21 C27 105.90(12) . . ? N21 Si21 C29 112.59(11) . . ? C27 Si21 C29 108.76(14) . . ? N21 Si21 C28 116.20(12) . . ? C27 Si21 C28 106.68(14) . . ? C29 Si21 C28 106.39(13) . . ? C22 O21 C211 117.01(17) . . ? C22 O21 Li1 125.89(19) . . ? C211 O21 Li1 117.03(19) . . ? C22 O21 Li21 105.29(18) . . ? C211 O21 Li21 87.50(17) . . ? Li1 O21 Li21 79.66(18) . . ? C21 N21 Si21 123.49(17) . . ? C21 N21 Li21 107.32(19) . . ? Si21 N21 Li21 120.36(16) . . ? C21 N21 Li3 103.6(2) . . ? Si21 N21 Li3 114.14(17) . . ? Li21 N21 Li3 77.6(2) . . ? N21 C21 C26 124.7(2) . . ? N21 C21 C22 121.3(2) . . ? C26 C21 C22 114.0(2) . . ? C23 C22 O21 117.9(2) . . ? C23 C22 C21 123.1(2) . . ? O21 C22 C21 118.8(2) . . ? C22 C23 C24 120.6(2) . . ? C23 C24 C25 118.6(2) . . ? C26 C25 C24 120.6(2) . . ? C25 C26 C21 123.1(2) . . ? C216 C211 C212 126.7(2) . . ? C216 C211 O21 116.4(2) . . ? C212 C211 O21 116.7(2) . . ? C216 C211 Li21 155.8(2) . . ? C212 C211 Li21 63.21(17) . . ? O21 C211 Li21 57.12(14) . . ? C211 C212 C213 112.1(2) . . ? C211 C212 Li3 118.1(2) . . ? C213 C212 Li3 117.8(2) . . ? C211 C212 Li21 83.37(18) . . ? C213 C212 Li21 150.0(2) . . ? Li3 C212 Li21 71.24(19) . . ? C214 C213 C212 123.8(2) . . ? C215 C214 C213 120.2(2) . . ? C214 C215 C216 119.1(2) . . ? C211 C216 C215 118.2(2) . . ? O52 Li3 O51 27.42(17) . . ? O52 Li3 N21 123.9(3) . . ? O51 Li3 N21 121.7(3) . . ? O52 Li3 C212 133.3(3) . . ? O51 Li3 C212 117.9(3) . . ? N21 Li3 C212 100.6(2) . . ? O52 Li3 O53 53.2(2) . . ? O51 Li3 O53 79.2(2) . . ? N21 Li3 O53 121.6(3) . . ? C212 Li3 O53 116.6(3) . . ? C54 O51 C52 109.7(5) . . ? C54 O51 Li3 124.1(4) . . ? C52 O51 Li3 113.3(4) . . ? C53 O52 C51 113.5(5) . . ? C53 O52 Li3 119.5(5) . . ? C51 O52 Li3 121.7(4) . . ? O53 O53 C51 138.8(7) 2 . ? O53 O53 Li3 118.5(6) 2 . ? C51 O53 Li3 102.6(3) . . ? C52 C51 O52 47.3(3) . . ? C52 C51 O53 107.5(4) . . ? O52 C51 O53 77.2(3) . . ? C52 C51 C50 150.1(5) . . ? O52 C51 C50 109.1(4) . . ? O53 C51 C50 43.1(3) . . ? C51 C52 O51 106.5(5) . . ? C50 C50 C51 151.3(4) 2 . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.205 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.069 data_c_li2phbu #:\mydocu~1\craig'~1\listru~1\li2phbu\li2phbu _database_code_CSD 163624 _audit_creation_method SHELXL-97 _chemical_name_systematic ; di[(diethyl ether)(N-(2-(2'-lithiophenyloxy)phenyl)-N-(trimethylsilyl)amido) lithium(I).(n-butyl)lithium(I)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H68 Li6 N2 O4 Si2' _chemical_formula_weight 810.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9117(2) _cell_length_b 11.517(2) _cell_length_c 16.967(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.24(3) _cell_angle_gamma 90.00 _cell_volume 2482.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf Nonius Kappa CCD _diffrn_measurement_method 1 deg phi scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37344 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5851 _reflns_number_gt 3955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Povray' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+1.2241P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5851 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.2598(3) 0.4191(3) 0.0250(2) 0.0232(7) Uani 1 1 d . . . Si1 Si 0.25809(4) 0.13217(5) 0.01417(3) 0.02196(16) Uani 1 1 d . . . O1 O 0.17663(10) 0.46013(11) 0.10613(8) 0.0197(3) Uani 1 1 d . . . N1 N 0.19707(12) 0.25722(14) 0.03708(9) 0.0187(4) Uani 1 1 d . . . C11 C 0.13354(14) 0.26122(16) 0.09483(11) 0.0178(4) Uani 1 1 d . . . C12 C 0.11739(14) 0.37010(16) 0.13077(11) 0.0172(4) Uani 1 1 d . . . C13 C 0.05380(15) 0.38521(17) 0.18721(11) 0.0204(4) Uani 1 1 d . . . H13 H 0.0472 0.4596 0.2101 0.024 Uiso 1 1 calc R . . C14 C -0.00102(16) 0.28973(19) 0.21057(12) 0.0254(5) Uani 1 1 d . . . H14 H -0.0459 0.2985 0.2488 0.031 Uiso 1 1 calc R . . C15 C 0.01157(16) 0.18283(18) 0.17691(12) 0.0259(5) Uani 1 1 d . . . H15 H -0.0256 0.1177 0.1921 0.031 Uiso 1 1 calc R . . C16 C 0.07727(15) 0.16839(18) 0.12131(12) 0.0228(4) Uani 1 1 d . . . H16 H 0.0847 0.0930 0.1002 0.027 Uiso 1 1 calc R . . C17 C 0.35458(18) 0.1747(2) -0.05068(16) 0.0373(6) Uani 1 1 d . . . H17A H 0.4038 0.2321 -0.0226 0.056 Uiso 1 1 calc R . . H17B H 0.3169 0.2083 -0.1007 0.056 Uiso 1 1 calc R . . H17C H 0.3937 0.1059 -0.0627 0.056 Uiso 1 1 calc R . . C18 C 0.33200(18) 0.0580(2) 0.10515(14) 0.0352(5) Uani 1 1 d . . . H18A H 0.3794 0.1136 0.1370 0.053 Uiso 1 1 calc R . . H18B H 0.3732 -0.0063 0.0887 0.053 Uiso 1 1 calc R . . H18C H 0.2821 0.0277 0.1374 0.053 Uiso 1 1 calc R . . C19 C 0.16795(18) 0.02357(19) -0.04567(14) 0.0321(5) Uani 1 1 d . . . H19A H 0.1154 -0.0025 -0.0144 0.048 Uiso 1 1 calc R . . H19B H 0.2091 -0.0432 -0.0584 0.048 Uiso 1 1 calc R . . H19C H 0.1324 0.0598 -0.0955 0.048 Uiso 1 1 calc R . . C111 C 0.14994(14) 0.57750(16) 0.12044(11) 0.0163(4) Uani 1 1 d . . . C112 C 0.07237(14) 0.63036(17) 0.06425(11) 0.0183(4) Uani 1 1 d . . . C113 C 0.06554(15) 0.75082(17) 0.07932(12) 0.0200(4) Uani 1 1 d . . . H113 H 0.0168 0.7953 0.0429 0.024 Uiso 1 1 calc R . . C114 C 0.12555(15) 0.80839(17) 0.14396(12) 0.0223(4) Uani 1 1 d . . . H114 H 0.1166 0.8894 0.1508 0.027 Uiso 1 1 calc R . . C115 C 0.19816(16) 0.74740(18) 0.19801(12) 0.0252(5) Uani 1 1 d . . . H115 H 0.2385 0.7856 0.2428 0.030 Uiso 1 1 calc R . . C116 C 0.21127(15) 0.62987(17) 0.18603(11) 0.0212(4) Uani 1 1 d . . . H116 H 0.2612 0.5861 0.2220 0.025 Uiso 1 1 calc R . . Li2 Li 0.0595(3) 0.5488(3) -0.0536(2) 0.0304(8) Uani 1 1 d . . . O2 O 0.38258(10) 0.52312(12) 0.05052(8) 0.0234(3) Uani 1 1 d . . . C21 C 0.35869(18) 0.73603(19) 0.03877(14) 0.0324(5) Uani 1 1 d . . . H21A H 0.3695 0.8018 0.0045 0.049 Uiso 1 1 calc R . . H21B H 0.3991 0.7484 0.0927 0.049 Uiso 1 1 calc R . . H21C H 0.2837 0.7295 0.0415 0.049 Uiso 1 1 calc R . . C22 C 0.39524(17) 0.62603(19) 0.00439(12) 0.0270(5) Uani 1 1 d . . . H22A H 0.3554 0.6156 -0.0506 0.032 Uiso 1 1 calc R . . H22B H 0.4705 0.6344 0.0007 0.032 Uiso 1 1 calc R . . C23 C 0.45467(17) 0.5201(2) 0.12528(13) 0.0293(5) Uani 1 1 d . . . H23A H 0.4378 0.5831 0.1606 0.035 Uiso 1 1 calc R . . H23B H 0.5275 0.5319 0.1159 0.035 Uiso 1 1 calc R . . C24 C 0.44602(18) 0.4050(2) 0.16430(13) 0.0357(6) Uani 1 1 d . . . H24A H 0.4952 0.4022 0.2154 0.054 Uiso 1 1 calc R . . H24B H 0.4632 0.3430 0.1292 0.054 Uiso 1 1 calc R . . H24C H 0.3740 0.3942 0.1739 0.054 Uiso 1 1 calc R . . Li3 Li 0.0996(3) 0.3318(3) -0.0550(2) 0.0244(7) Uani 1 1 d . . . C1 C 0.18378(16) 0.46209(17) -0.10811(12) 0.0235(4) Uani 1 1 d . . . C2 C 0.15358(16) 0.37832(18) -0.18075(12) 0.0244(4) Uani 1 1 d . . . H2A H 0.1529 0.2980 -0.1601 0.029 Uiso 1 1 calc R . . H2B H 0.0811 0.3970 -0.2078 0.029 Uiso 1 1 calc R . . C3 C 0.22585(19) 0.3819(2) -0.24313(13) 0.0340(5) Uani 1 1 d . . . H3A H 0.2240 0.4610 -0.2662 0.041 Uiso 1 1 calc R . . H3B H 0.2990 0.3662 -0.2161 0.041 Uiso 1 1 calc R . . C4 C 0.1957(2) 0.2946(2) -0.31100(15) 0.0464(7) Uani 1 1 d . . . H4A H 0.2446 0.3015 -0.3488 0.070 Uiso 1 1 calc R . . H4B H 0.1239 0.3105 -0.3388 0.070 Uiso 1 1 calc R . . H4C H 0.1993 0.2158 -0.2889 0.070 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 0.0212(17) 0.0222(18) 0.0260(18) -0.0009(14) 0.0041(14) -0.0007(13) Si1 0.0208(3) 0.0165(3) 0.0273(3) -0.0044(2) 0.0010(2) 0.0007(2) O1 0.0207(7) 0.0127(7) 0.0270(7) -0.0021(6) 0.0078(6) -0.0011(5) N1 0.0196(8) 0.0148(8) 0.0212(8) -0.0020(6) 0.0022(7) 0.0003(6) C11 0.0170(10) 0.0171(10) 0.0164(9) 0.0022(7) -0.0047(7) 0.0005(7) C12 0.0153(9) 0.0165(9) 0.0178(9) 0.0035(8) -0.0028(7) -0.0011(7) C13 0.0210(10) 0.0221(11) 0.0165(9) 0.0015(8) -0.0005(8) 0.0016(8) C14 0.0254(11) 0.0317(12) 0.0197(10) 0.0060(9) 0.0053(8) -0.0009(8) C15 0.0293(11) 0.0232(11) 0.0238(11) 0.0079(9) 0.0009(9) -0.0067(9) C16 0.0262(11) 0.0180(10) 0.0221(10) 0.0028(8) -0.0015(8) -0.0018(8) C17 0.0319(13) 0.0302(13) 0.0531(15) -0.0069(11) 0.0163(11) 0.0010(10) C18 0.0361(13) 0.0272(13) 0.0392(13) -0.0035(10) -0.0015(10) 0.0096(9) C19 0.0341(12) 0.0237(12) 0.0375(13) -0.0104(10) 0.0038(10) -0.0018(9) C111 0.0185(10) 0.0130(9) 0.0183(9) -0.0015(8) 0.0059(7) -0.0013(7) C112 0.0175(10) 0.0197(10) 0.0174(9) -0.0005(8) 0.0022(7) -0.0020(7) C113 0.0187(10) 0.0197(10) 0.0212(10) 0.0025(8) 0.0026(8) 0.0015(7) C114 0.0258(11) 0.0135(10) 0.0279(11) -0.0048(8) 0.0055(8) -0.0013(8) C115 0.0237(11) 0.0274(12) 0.0224(10) -0.0098(9) -0.0016(8) -0.0030(8) C116 0.0197(10) 0.0240(11) 0.0185(10) -0.0012(8) -0.0007(8) 0.0020(8) Li2 0.0269(19) 0.037(2) 0.0243(18) -0.0061(16) -0.0034(14) 0.0063(15) O2 0.0221(7) 0.0270(8) 0.0203(7) -0.0005(6) 0.0017(6) -0.0056(6) C21 0.0347(12) 0.0278(12) 0.0375(13) 0.0013(10) 0.0141(10) -0.0003(9) C22 0.0298(12) 0.0275(12) 0.0246(11) -0.0012(9) 0.0074(9) -0.0101(9) C23 0.0243(11) 0.0367(13) 0.0247(11) -0.0077(9) -0.0013(9) 0.0016(9) C24 0.0298(13) 0.0483(15) 0.0279(12) 0.0062(11) 0.0022(10) 0.0050(10) Li3 0.0208(17) 0.0247(18) 0.0265(18) -0.0006(15) 0.0009(14) -0.0017(13) C1 0.0255(11) 0.0217(11) 0.0220(10) -0.0042(8) 0.0010(8) -0.0031(8) C2 0.0237(11) 0.0270(11) 0.0221(10) -0.0030(9) 0.0033(8) -0.0023(8) C3 0.0389(13) 0.0382(14) 0.0264(12) -0.0065(10) 0.0101(10) -0.0086(10) C4 0.0518(16) 0.0576(18) 0.0335(14) -0.0166(13) 0.0179(12) -0.0117(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O1 1.948(4) . ? Li1 O2 1.973(4) . ? Li1 N1 2.057(4) . ? Li1 C1 2.350(4) . ? Li1 Li3 2.476(5) . ? Li1 Li2 3.078(5) . ? Si1 N1 1.7189(17) . ? Si1 C17 1.868(2) . ? Si1 C18 1.871(2) . ? Si1 C19 1.879(2) . ? Si1 Li3 3.161(4) . ? O1 C12 1.396(2) . ? O1 C111 1.426(2) . ? N1 C11 1.386(3) . ? N1 Li3 2.016(4) . ? C11 C16 1.410(3) . ? C11 C12 1.426(3) . ? C11 Li3 2.631(4) . ? C12 C13 1.379(3) . ? C12 Li2 2.596(4) 3_565 ? C13 C14 1.402(3) . ? C13 Li2 2.583(4) 3_565 ? C14 C15 1.379(3) . ? C15 C16 1.386(3) . ? C111 C116 1.384(3) . ? C111 C112 1.394(3) . ? C112 C113 1.416(3) . ? C112 Li2 2.189(4) . ? C112 Li3 2.241(4) 3_565 ? C112 Li2 2.660(4) 3_565 ? C113 C114 1.393(3) . ? C113 Li3 2.304(4) 3_565 ? C114 C115 1.381(3) . ? C115 C116 1.383(3) . ? Li2 C1 2.226(4) . ? Li2 Li3 2.554(5) . ? Li2 C13 2.583(4) 3_565 ? Li2 C12 2.596(4) 3_565 ? Li2 C112 2.660(4) 3_565 ? Li2 Li2 2.816(8) 3_565 ? Li2 Li3 3.296(5) 3_565 ? O2 C23 1.434(2) . ? O2 C22 1.445(2) . ? C21 C22 1.505(3) . ? C23 C24 1.495(3) . ? Li3 C1 2.143(4) . ? Li3 C112 2.241(4) 3_565 ? Li3 C113 2.304(4) 3_565 ? Li3 C2 2.419(4) . ? Li3 Li2 3.296(5) 3_565 ? C1 C2 1.559(3) . ? C2 C3 1.531(3) . ? C3 C4 1.526(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 O1 Li1 O2 102.71(16) . . ? O1 Li1 N1 82.75(14) . . ? O2 Li1 N1 147.54(19) . . ? O1 Li1 C1 116.07(16) . . ? O2 Li1 C1 105.32(16) . . ? N1 Li1 C1 100.50(15) . . ? O1 Li1 Li3 88.56(15) . . ? O2 Li1 Li3 157.94(19) . . ? N1 Li1 Li3 51.80(12) . . ? C1 Li1 Li3 52.64(12) . . ? O1 Li1 Li2 70.27(12) . . ? O2 Li1 Li2 112.37(16) . . ? N1 Li1 Li2 99.66(14) . . ? C1 Li1 Li2 46.04(10) . . ? Li3 Li1 Li2 53.42(12) . . ? N1 Si1 C17 107.12(9) . . ? N1 Si1 C18 112.53(9) . . ? C17 Si1 C18 108.05(11) . . ? N1 Si1 C19 114.53(9) . . ? C17 Si1 C19 105.67(11) . . ? C18 Si1 C19 108.53(11) . . ? N1 Si1 Li3 35.16(8) . . ? C17 Si1 Li3 92.65(10) . . ? C18 Si1 Li3 147.15(10) . . ? C19 Si1 Li3 89.17(10) . . ? C12 O1 C111 119.41(14) . . ? C12 O1 Li1 115.54(15) . . ? C111 O1 Li1 122.05(15) . . ? C11 N1 Si1 122.72(13) . . ? C11 N1 Li3 99.66(15) . . ? Si1 N1 Li3 115.43(13) . . ? C11 N1 Li1 109.45(15) . . ? Si1 N1 Li1 122.17(13) . . ? Li3 N1 Li1 74.89(14) . . ? N1 C11 C16 127.11(18) . . ? N1 C11 C12 118.79(16) . . ? C16 C11 C12 114.05(18) . . ? N1 C11 Li3 49.05(11) . . ? C16 C11 Li3 122.38(15) . . ? C12 C11 Li3 97.47(14) . . ? C13 C12 O1 122.68(17) . . ? C13 C12 C11 123.95(17) . . ? O1 C12 C11 113.30(16) . . ? C13 C12 Li2 74.07(13) . 3_565 ? O1 C12 Li2 93.52(13) . 3_565 ? C11 C12 Li2 106.46(14) . 3_565 ? C12 C13 C14 119.34(19) . . ? C12 C13 Li2 75.05(13) . 3_565 ? C14 C13 Li2 104.07(15) . 3_565 ? C15 C14 C13 118.72(19) . . ? C14 C15 C16 121.36(19) . . ? C15 C16 C11 122.56(19) . . ? C116 C111 C112 126.75(18) . . ? C116 C111 O1 115.40(16) . . ? C112 C111 O1 117.61(16) . . ? C111 C112 C113 111.38(16) . . ? C111 C112 Li2 111.48(16) . . ? C113 C112 Li2 126.03(17) . . ? C111 C112 Li3 135.67(16) . 3_565 ? C113 C112 Li3 74.29(14) . 3_565 ? Li2 C112 Li3 96.10(15) . 3_565 ? C111 C112 Li2 94.64(14) . 3_565 ? C113 C112 Li2 135.42(15) . 3_565 ? Li2 C112 Li2 70.22(16) . 3_565 ? Li3 C112 Li2 62.10(13) 3_565 3_565 ? C114 C113 C112 124.37(18) . . ? C114 C113 Li3 134.81(17) . 3_565 ? C112 C113 Li3 69.44(14) . 3_565 ? C115 C114 C113 119.83(18) . . ? C114 C115 C116 119.10(18) . . ? C115 C116 C111 118.49(18) . . ? C112 Li2 C1 128.94(17) . . ? C112 Li2 Li3 116.48(18) . . ? C1 Li2 Li3 52.74(12) . . ? C112 Li2 C13 127.91(17) . 3_565 ? C1 Li2 C13 96.05(14) . 3_565 ? Li3 Li2 C13 111.36(16) . 3_565 ? C112 Li2 C12 102.90(15) . 3_565 ? C1 Li2 C12 125.94(16) . 3_565 ? Li3 Li2 C12 120.64(16) . 3_565 ? C13 Li2 C12 30.88(7) 3_565 3_565 ? C112 Li2 C112 109.78(16) . 3_565 ? C1 Li2 C112 97.13(15) . 3_565 ? Li3 Li2 C112 50.87(11) . 3_565 ? C13 Li2 C112 85.02(12) 3_565 3_565 ? C12 Li2 C112 75.52(11) 3_565 3_565 ? C112 Li2 Li2 62.75(14) . 3_565 ? C1 Li2 Li2 127.3(2) . 3_565 ? Li3 Li2 Li2 75.55(18) . 3_565 ? C13 Li2 Li2 113.31(19) 3_565 3_565 ? C12 Li2 Li2 86.41(16) 3_565 3_565 ? C112 Li2 Li2 47.03(12) 3_565 3_565 ? C112 Li2 Li1 83.71(13) . . ? C1 Li2 Li1 49.46(11) . . ? Li3 Li2 Li1 51.14(12) . . ? C13 Li2 Li1 145.51(16) 3_565 . ? C12 Li2 Li1 171.64(17) 3_565 . ? C112 Li2 Li1 97.53(14) 3_565 . ? Li2 Li2 Li1 92.22(17) 3_565 . ? C112 Li2 Li3 42.55(10) . 3_565 ? C1 Li2 Li3 170.69(16) . 3_565 ? Li3 Li2 Li3 124.17(15) . 3_565 ? C13 Li2 Li3 93.21(13) 3_565 3_565 ? C12 Li2 Li3 63.36(11) 3_565 3_565 ? C112 Li2 Li3 84.64(12) 3_565 3_565 ? Li2 Li2 Li3 48.62(13) 3_565 3_565 ? Li1 Li2 Li3 121.28(14) . 3_565 ? C23 O2 C22 112.38(15) . . ? C23 O2 Li1 123.29(16) . . ? C22 O2 Li1 122.90(15) . . ? O2 C22 C21 114.01(17) . . ? O2 C23 C24 108.99(17) . . ? N1 Li3 C1 109.33(16) . . ? N1 Li3 C112 127.67(18) . 3_565 ? C1 Li3 C112 113.85(17) . 3_565 ? N1 Li3 C113 113.15(17) . 3_565 ? C1 Li3 C113 137.40(18) . 3_565 ? C112 Li3 C113 36.27(8) 3_565 3_565 ? N1 Li3 C2 122.71(17) . . ? C1 Li3 C2 39.39(9) . . ? C112 Li3 C2 109.41(15) 3_565 . ? C113 Li3 C2 109.65(15) 3_565 . ? N1 Li3 Li1 53.31(12) . . ? C1 Li3 Li1 60.66(13) . . ? C112 Li3 Li1 132.81(18) 3_565 . ? C113 Li3 Li1 157.15(19) 3_565 . ? C2 Li3 Li1 92.90(15) . . ? N1 Li3 Li2 120.63(17) . . ? C1 Li3 Li2 55.76(13) . . ? C112 Li3 Li2 67.03(13) 3_565 . ? C113 Li3 Li2 102.85(15) 3_565 . ? C2 Li3 Li2 83.22(15) . . ? Li1 Li3 Li2 75.45(15) . . ? N1 Li3 C11 31.29(8) . . ? C1 Li3 C11 127.79(16) . . ? C112 Li3 C11 96.90(14) 3_565 . ? C113 Li3 C11 92.01(13) 3_565 . ? C2 Li3 C11 153.67(16) . . ? Li1 Li3 C11 67.42(12) . . ? Li2 Li3 C11 107.01(15) . . ? N1 Li3 Si1 29.41(7) . . ? C1 Li3 Si1 108.81(13) . . ? C112 Li3 Si1 137.33(15) 3_565 . ? C113 Li3 Si1 106.48(13) 3_565 . ? C2 Li3 Si1 102.70(12) . . ? Li1 Li3 Si1 70.70(11) . . ? Li2 Li3 Si1 145.83(15) . . ? C11 Li3 Si1 55.32(8) . . ? N1 Li3 Li2 96.27(14) . 3_565 ? C1 Li3 Li2 110.84(16) . 3_565 ? C112 Li3 Li2 41.35(10) 3_565 3_565 ? C113 Li3 Li2 67.86(12) 3_565 3_565 ? C2 Li3 Li2 134.97(16) . 3_565 ? Li1 Li3 Li2 93.80(14) . 3_565 ? Li2 Li3 Li2 55.83(15) . 3_565 ? C11 Li3 Li2 66.50(11) . 3_565 ? Si1 Li3 Li2 121.50(13) . 3_565 ? C2 C1 Li3 79.90(14) . . ? C2 C1 Li2 120.55(16) . . ? Li3 C1 Li2 71.51(15) . . ? C2 C1 Li1 129.22(16) . . ? Li3 C1 Li1 66.70(13) . . ? Li2 C1 Li1 84.50(14) . . ? C3 C2 C1 115.61(17) . . ? C3 C2 Li3 157.24(17) . . ? C1 C2 Li3 60.72(13) . . ? C4 C3 C2 113.51(19) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.768 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.058 data_c_linew #:\mydocu~1\craig'~1\listru~1\li2phdme\linew _database_code_CSD 163625 _audit_creation_method SHELXL-97 _chemical_name_systematic ; di[(1,2-dimethoxyethane)(N-(2-(2'-lithiophenyloxy)phenyl)- N-(trimethylsilyl)amido)lithium(I)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H54 Li4 N2 O6 Si2' _chemical_formula_weight 718.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.1749(10) _cell_length_b 14.3421(6) _cell_length_c 34.5285(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.890(3) _cell_angle_gamma 90.00 _cell_volume 10562(4) _cell_formula_units_Z 10 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf Nonius Kappa CCD _diffrn_measurement_method 1 deg phi scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14985 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1453 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.30 _reflns_number_total 14985 _reflns_number_gt 6567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Povray' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1721P)^2^+1.0222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14985 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2276 _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.3433 _refine_ls_wR_factor_gt 0.2734 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li -0.1809(7) 0.3987(7) 0.2282(3) 0.033(4) Uani 1 1 d . . . O31 O -0.2121(3) 0.3358(3) 0.26922(15) 0.058(2) Uani 1 1 d . . . O32 O -0.2639(3) 0.4605(4) 0.21439(17) 0.066(2) Uani 1 1 d . . . C31 C -0.1767(5) 0.2971(6) 0.3029(2) 0.083(3) Uiso 1 1 d . . . H31A H -0.1356 0.2812 0.2994 0.124 Uiso 1 1 calc R . . H31B H -0.1971 0.2404 0.3089 0.124 Uiso 1 1 calc R . . H31C H -0.1714 0.3413 0.3253 0.124 Uiso 1 1 calc R . . C32 C -0.2709(6) 0.3640(6) 0.2673(3) 0.080(3) Uiso 1 1 d . . . H32A H -0.2705 0.3895 0.2940 0.096 Uiso 1 1 calc R . . H32B H -0.2981 0.3080 0.2629 0.096 Uiso 1 1 calc R . . C33 C -0.2984(8) 0.4282(9) 0.2392(4) 0.164(6) Uiso 1 1 d . . . H33A H -0.3102 0.4824 0.2533 0.197 Uiso 1 1 calc R . . H33B H -0.3377 0.4009 0.2221 0.197 Uiso 1 1 calc R . . C34 C -0.2812(6) 0.5490(6) 0.1965(3) 0.096(3) Uiso 1 1 d . . . H34A H -0.2542 0.5649 0.1793 0.144 Uiso 1 1 calc R . . H34B H -0.2765 0.5962 0.2177 0.144 Uiso 1 1 calc R . . H34C H -0.3250 0.5472 0.1803 0.144 Uiso 1 1 calc R . . Li2 Li -0.0928(6) 0.4318(6) 0.1963(2) 0.023(3) Uani 1 1 d . . . Si1 Si -0.19248(12) 0.27297(11) 0.15208(5) 0.0404(8) Uani 1 1 d . . . O1 O -0.0329(2) 0.3841(2) 0.24742(9) 0.0198(13) Uani 1 1 d . . . N1 N -0.1408(3) 0.3134(3) 0.19526(12) 0.0268(18) Uani 1 1 d . . . C11 C -0.1007(3) 0.2529(3) 0.22185(15) 0.0210(12) Uiso 1 1 d . . . C12 C -0.0473(3) 0.2881(3) 0.24967(15) 0.0214(12) Uiso 1 1 d . . . C13 C -0.0030(3) 0.2322(3) 0.27633(15) 0.0226(13) Uiso 1 1 d . . . H13 H 0.0330 0.2597 0.2942 0.027 Uiso 1 1 calc R . . C14 C -0.0120(4) 0.1361(3) 0.27656(16) 0.0267(14) Uiso 1 1 d . . . H14 H 0.0174 0.0970 0.2945 0.032 Uiso 1 1 calc R . . C15 C -0.0646(4) 0.0992(3) 0.25011(15) 0.0261(13) Uiso 1 1 d . . . H15 H -0.0714 0.0338 0.2500 0.031 Uiso 1 1 calc R . . C16 C -0.1083(4) 0.1555(3) 0.22338(15) 0.0248(13) Uiso 1 1 d . . . H16 H -0.1442 0.1273 0.2057 0.030 Uiso 1 1 calc R . . C17 C -0.2556(5) 0.1936(5) 0.1609(2) 0.077(3) Uiso 1 1 d . . . H17A H -0.2775 0.2251 0.1782 0.115 Uiso 1 1 calc R . . H17B H -0.2364 0.1361 0.1739 0.115 Uiso 1 1 calc R . . H17C H -0.2855 0.1784 0.1350 0.115 Uiso 1 1 calc R . . C18 C -0.1514(4) 0.2118(4) 0.11905(19) 0.053(2) Uiso 1 1 d . . . H18A H -0.1292 0.1573 0.1332 0.079 Uiso 1 1 calc R . . H18B H -0.1212 0.2543 0.1123 0.079 Uiso 1 1 calc R . . H18C H -0.1821 0.1917 0.0943 0.079 Uiso 1 1 calc R . . C19 C -0.2349(4) 0.3757(4) 0.12313(18) 0.0441(18) Uiso 1 1 d . . . H19A H -0.2570 0.4095 0.1398 0.066 Uiso 1 1 calc R . . H19B H -0.2652 0.3537 0.0985 0.066 Uiso 1 1 calc R . . H19C H -0.2046 0.4174 0.1160 0.066 Uiso 1 1 calc R . . C111 C -0.0580(3) 0.4435(3) 0.27305(14) 0.0170(11) Uiso 1 1 d . . . C112 C -0.1057(4) 0.5049(3) 0.25251(15) 0.0258(13) Uiso 1 1 d . . . C113 C -0.1238(4) 0.5657(4) 0.27897(16) 0.0299(14) Uiso 1 1 d . . . H113 H -0.1551 0.6106 0.2675 0.036 Uiso 1 1 calc R . . C114 C -0.1000(4) 0.5660(4) 0.32045(16) 0.0305(14) Uiso 1 1 d . . . H114 H -0.1154 0.6084 0.3367 0.037 Uiso 1 1 calc R . . C115 C -0.0527(4) 0.5023(3) 0.33777(17) 0.0292(14) Uiso 1 1 d . . . H115 H -0.0347 0.5024 0.3661 0.035 Uiso 1 1 calc R . . C116 C -0.0320(4) 0.4392(3) 0.31415(15) 0.0264(13) Uiso 1 1 d . . . H116 H -0.0009 0.3942 0.3258 0.032 Uiso 1 1 calc R . . Li3 Li -0.1001(6) 0.6010(5) 0.2048(2) 0.024(4) Uani 1 1 d . . . Si2 Si 0.00401(11) 0.75394(10) 0.24398(4) 0.0294(7) Uani 1 1 d . . . O2 O -0.1666(2) 0.6498(2) 0.15711(9) 0.0202(13) Uani 1 1 d . . . N2 N -0.0556(3) 0.7225(3) 0.20337(12) 0.0201(16) Uani 1 1 d . . . C21 C -0.1003(3) 0.7830(3) 0.18152(15) 0.0215(12) Uiso 1 1 d . . . C22 C -0.1573(3) 0.7479(3) 0.15615(14) 0.0183(12) Uiso 1 1 d . . . C23 C -0.0961(3) 0.8818(3) 0.18097(15) 0.0236(13) Uiso 1 1 d . . . H23 H -0.0594 0.9112 0.1971 0.028 Uiso 1 1 calc R . . C24 C -0.1980(4) 0.8990(4) 0.13335(16) 0.0299(14) Uiso 1 1 d . . . H24 H -0.2297 0.9375 0.1170 0.036 Uiso 1 1 calc R . . C25 C -0.1439(3) 0.9367(3) 0.15768(14) 0.0227(12) Uiso 1 1 d . . . H25 H -0.1391 1.0025 0.1586 0.027 Uiso 1 1 calc R . . C26 C -0.2051(4) 0.8010(3) 0.13336(15) 0.0255(13) Uiso 1 1 d . . . H26 H -0.2426 0.7726 0.1177 0.031 Uiso 1 1 calc R . . C27 C 0.0655(4) 0.8270(5) 0.2313(2) 0.061(2) Uiso 1 1 d . . . H27A H 0.0467 0.8851 0.2187 0.091 Uiso 1 1 calc R . . H27B H 0.0837 0.7928 0.2127 0.091 Uiso 1 1 calc R . . H27C H 0.0985 0.8413 0.2560 0.091 Uiso 1 1 calc R . . C28 C -0.0243(4) 0.8175(4) 0.28266(17) 0.0437(18) Uiso 1 1 d . . . H28A H -0.0443 0.8760 0.2712 0.066 Uiso 1 1 calc R . . H28B H 0.0113 0.8313 0.3059 0.066 Uiso 1 1 calc R . . H28C H -0.0547 0.7788 0.2912 0.066 Uiso 1 1 calc R . . C29 C 0.0425(4) 0.6449(4) 0.26787(18) 0.0417(17) Uiso 1 1 d . . . H29A H 0.0578 0.6095 0.2482 0.063 Uiso 1 1 calc R . . H29B H 0.0121 0.6072 0.2769 0.063 Uiso 1 1 calc R . . H29C H 0.0778 0.6608 0.2910 0.063 Uiso 1 1 calc R . . C211 C -0.1408(3) 0.5962(3) 0.12997(15) 0.0203(12) Uiso 1 1 d . . . C212 C -0.0949(3) 0.5310(3) 0.14826(15) 0.0214(12) Uiso 1 1 d . . . C213 C -0.0742(4) 0.4789(4) 0.12003(16) 0.0295(14) Uiso 1 1 d . . . H213 H -0.0429 0.4330 0.1298 0.035 Uiso 1 1 calc R . . C214 C -0.0964(4) 0.4901(4) 0.07942(18) 0.0380(16) Uiso 1 1 d . . . H214 H -0.0805 0.4518 0.0620 0.046 Uiso 1 1 calc R . . C215 C -0.1415(4) 0.5561(4) 0.06305(19) 0.0406(17) Uiso 1 1 d . . . H215 H -0.1566 0.5635 0.0347 0.049 Uiso 1 1 calc R . . C216 C -0.1644(4) 0.6120(4) 0.08935(16) 0.0304(14) Uiso 1 1 d . . . H216 H -0.1950 0.6588 0.0794 0.036 Uiso 1 1 calc R . . Li4 Li -0.0276(8) 0.6592(8) 0.1577(3) 0.045(5) Uani 1 1 d . . . O41 O 0.0571(4) 0.6203(4) 0.1532(2) 0.109(4) Uani 1 1 d . . . O42 O -0.0232(5) 0.7494(5) 0.11329(17) 0.087(3) Uani 1 1 d . . . C41 C 0.0917(6) 0.5588(7) 0.1751(3) 0.105(4) Uiso 1 1 d . . . H41A H 0.0684 0.5280 0.1919 0.158 Uiso 1 1 calc R . . H41B H 0.1292 0.5887 0.1925 0.158 Uiso 1 1 calc R . . H41C H 0.1041 0.5125 0.1579 0.158 Uiso 1 1 calc R . . C42 C 0.0750(6) 0.6801(7) 0.1248(3) 0.093(3) Uiso 1 1 d . . . H42A H 0.1065 0.7256 0.1396 0.112 Uiso 1 1 calc R . . H42B H 0.0948 0.6419 0.1077 0.112 Uiso 1 1 calc R . . C43 C 0.0250(9) 0.7274(10) 0.1005(4) 0.155(6) Uiso 1 1 d . . . H43A H 0.0415 0.7861 0.0923 0.186 Uiso 1 1 calc R . . H43B H 0.0091 0.6897 0.0757 0.186 Uiso 1 1 calc R . . C44 C -0.0670(5) 0.8087(5) 0.0881(2) 0.078(3) Uiso 1 1 d . . . H44A H -0.1011 0.8216 0.1004 0.117 Uiso 1 1 calc R . . H44B H -0.0840 0.7788 0.0619 0.117 Uiso 1 1 calc R . . H44C H -0.0465 0.8674 0.0845 0.117 Uiso 1 1 calc R . . Li5 Li 0.1307(9) 1.1482(8) 0.1465(3) 0.050(5) Uani 1 1 d . . . O71 O 0.0468(4) 1.1099(4) 0.1517(2) 0.107(3) Uani 1 1 d . . . O72 O 0.1305(5) 1.2378(6) 0.19241(18) 0.096(3) Uani 1 1 d . . . C71 C 0.1692(6) 1.3078(6) 0.2133(2) 0.081(3) Uiso 1 1 d . . . H71A H 0.2071 1.3115 0.2040 0.121 Uiso 1 1 calc R . . H71B H 0.1810 1.2937 0.2422 0.121 Uiso 1 1 calc R . . H71C H 0.1470 1.3675 0.2085 0.121 Uiso 1 1 calc R . . C72 C 0.0782(10) 1.2242(11) 0.2005(4) 0.157(7) Uiso 1 1 d . . . H72A H 0.0575 1.2859 0.1975 0.188 Uiso 1 1 calc R . . H72B H 0.0894 1.2095 0.2296 0.188 Uiso 1 1 calc R . . C73 C 0.0339(8) 1.1647(9) 0.1835(4) 0.126(5) Uiso 1 1 d . . . H73A H -0.0056 1.1996 0.1724 0.151 Uiso 1 1 calc R . . H73B H 0.0272 1.1220 0.2045 0.151 Uiso 1 1 calc R . . C74 C 0.0176(6) 1.0410(7) 0.1337(3) 0.106(4) Uiso 1 1 d . . . H74A H 0.0380 1.0186 0.1137 0.159 Uiso 1 1 calc R . . H74B H -0.0257 1.0591 0.1202 0.159 Uiso 1 1 calc R . . H74C H 0.0174 0.9912 0.1531 0.159 Uiso 1 1 calc R . . Li6 Li 0.1990(6) 1.0946(5) 0.0960(3) 0.024(3) Uani 1 1 d . . . Si5 Si 0.09158(11) 1.24539(10) 0.06121(4) 0.0263(6) Uani 1 1 d . . . O5 O 0.2675(2) 1.1436(2) 0.14338(10) 0.0195(13) Uani 1 1 d . . . N5 N 0.1542(3) 1.2151(3) 0.10027(12) 0.0248(18) Uani 1 1 d . . . C51 C 0.2005(3) 1.2758(3) 0.12080(15) 0.0212(12) Uiso 1 1 d . . . C52 C 0.2586(3) 1.2415(3) 0.14448(15) 0.0210(12) Uiso 1 1 d . . . C53 C 0.3071(4) 1.2962(3) 0.16559(15) 0.0277(14) Uiso 1 1 d . . . H53 H 0.3454 1.2687 0.1804 0.033 Uiso 1 1 calc R . . C54 C 0.2995(4) 1.3945(4) 0.16511(16) 0.0333(15) Uiso 1 1 d . . . H54 H 0.3318 1.4340 0.1802 0.040 Uiso 1 1 calc R . . C55 C 0.2437(4) 1.4309(4) 0.14211(15) 0.0287(14) Uiso 1 1 d . . . H55 H 0.2380 1.4966 0.1412 0.034 Uiso 1 1 calc R . . C56 C 0.1958(4) 1.3747(3) 0.12029(15) 0.0253(13) Uiso 1 1 d . . . H56 H 0.1584 1.4031 0.1044 0.030 Uiso 1 1 calc R . . C57 C 0.0306(4) 1.3150(5) 0.0767(2) 0.057(2) Uiso 1 1 d . . . H57A H 0.0490 1.3735 0.0891 0.086 Uiso 1 1 calc R . . H57B H 0.0150 1.2791 0.0961 0.086 Uiso 1 1 calc R . . H57C H -0.0042 1.3287 0.0530 0.086 Uiso 1 1 calc R . . C58 C 0.1155(4) 1.3124(4) 0.02115(17) 0.0407(17) Uiso 1 1 d . . . H58A H 0.1356 1.3709 0.0325 0.061 Uiso 1 1 calc R . . H58B H 0.0783 1.3262 -0.0011 0.061 Uiso 1 1 calc R . . H58C H 0.1450 1.2752 0.0111 0.061 Uiso 1 1 calc R . . C59 C 0.0535(4) 1.1357(4) 0.03776(18) 0.0413(17) Uiso 1 1 d . . . H59A H 0.0408 1.0986 0.0580 0.062 Uiso 1 1 calc R . . H59B H 0.0833 1.0999 0.0272 0.062 Uiso 1 1 calc R . . H59C H 0.0165 1.1509 0.0157 0.062 Uiso 1 1 calc R . . C511 C 0.2442(3) 1.0901(3) 0.17128(14) 0.0196(12) Uiso 1 1 d . . . C512 C 0.2000(4) 1.0215(3) 0.15369(15) 0.0227(13) Uiso 1 1 d . . . C513 C 0.1811(4) 0.9680(3) 0.18267(15) 0.0279(14) Uiso 1 1 d . . . H513 H 0.1505 0.9210 0.1732 0.033 Uiso 1 1 calc R . . C514 C 0.2040(4) 0.9792(4) 0.22376(17) 0.0323(15) Uiso 1 1 d . . . H514 H 0.1903 0.9396 0.2417 0.039 Uiso 1 1 calc R . . C515 C 0.2476(4) 1.0497(4) 0.23853(18) 0.0351(15) Uiso 1 1 d . . . H515 H 0.2637 1.0587 0.2667 0.042 Uiso 1 1 calc R . . C516 C 0.2675(4) 1.1066(3) 0.21198(15) 0.0258(13) Uiso 1 1 d . . . H516 H 0.2964 1.1557 0.2216 0.031 Uiso 1 1 calc R . . Li7 Li 0.1945(6) 0.9273(5) 0.1035(2) 0.024(4) Uani 1 1 d . . . Si6 Si 0.30431(11) 0.77609(10) 0.14117(5) 0.0270(6) Uani 1 1 d . . . O6 O 0.1338(2) 0.8770(2) 0.05215(10) 0.0202(13) Uani 1 1 d . . . N6 N 0.2461(3) 0.8120(3) 0.10020(12) 0.0231(17) Uani 1 1 d . . . C61 C 0.2036(3) 0.7489(3) 0.07640(14) 0.0198(12) Uiso 1 1 d . . . C62 C 0.1480(4) 0.7805(3) 0.05051(15) 0.0231(13) Uiso 1 1 d . . . C63 C 0.1021(4) 0.7227(3) 0.02633(16) 0.0297(14) Uiso 1 1 d . . . H63 H 0.0643 0.7483 0.0098 0.036 Uiso 1 1 calc R . . C64 C 0.1130(4) 0.6262(4) 0.02692(16) 0.0313(15) Uiso 1 1 d . . . H64 H 0.0828 0.5853 0.0106 0.038 Uiso 1 1 calc R . . C65 C 0.1676(4) 0.5924(4) 0.05136(16) 0.0307(14) Uiso 1 1 d . . . H65 H 0.1753 0.5272 0.0518 0.037 Uiso 1 1 calc R . . C66 C 0.2122(4) 0.6505(3) 0.07563(16) 0.0269(13) Uiso 1 1 d . . . H66 H 0.2496 0.6240 0.0922 0.032 Uiso 1 1 calc R . . C67 C 0.3660(4) 0.7040(5) 0.1286(2) 0.055(2) Uiso 1 1 d . . . H67A H 0.3836 0.7380 0.1096 0.082 Uiso 1 1 calc R . . H67B H 0.3476 0.6453 0.1163 0.082 Uiso 1 1 calc R . . H67C H 0.3993 0.6907 0.1532 0.082 Uiso 1 1 calc R . . C68 C 0.2725(4) 0.7080(4) 0.17757(17) 0.0397(16) Uiso 1 1 d . . . H68A H 0.2398 0.7444 0.1848 0.060 Uiso 1 1 calc R . . H68B H 0.3064 0.6948 0.2019 0.060 Uiso 1 1 calc R . . H68C H 0.2547 0.6492 0.1651 0.060 Uiso 1 1 calc R . . C69 C 0.3436(4) 0.8808(4) 0.16823(17) 0.0323(15) Uiso 1 1 d . . . H69A H 0.3609 0.9183 0.1501 0.049 Uiso 1 1 calc R . . H69B H 0.3775 0.8614 0.1915 0.049 Uiso 1 1 calc R . . H69C H 0.3130 0.9181 0.1774 0.049 Uiso 1 1 calc R . . C611 C 0.1580(3) 0.9363(3) 0.02605(15) 0.0206(12) Uiso 1 1 d . . . C612 C 0.1978(3) 1.0062(3) 0.04560(15) 0.0211(12) Uiso 1 1 d . . . C613 C 0.2171(3) 1.0657(3) 0.01858(15) 0.0233(13) Uiso 1 1 d . . . H613 H 0.2447 1.1154 0.0295 0.028 Uiso 1 1 calc R . . C614 C 0.1979(4) 1.0556(4) -0.02299(16) 0.0315(14) Uiso 1 1 d . . . H614 H 0.2126 1.0973 -0.0398 0.038 Uiso 1 1 calc R . . C615 C 0.1568(4) 0.9834(4) -0.03990(18) 0.0334(15) Uiso 1 1 d . . . H615 H 0.1427 0.9763 -0.0683 0.040 Uiso 1 1 calc R . . C616 C 0.1364(4) 0.9217(3) -0.01494(16) 0.0273(14) Uiso 1 1 d . . . H616 H 0.1088 0.8717 -0.0257 0.033 Uiso 1 1 calc R . . Li8 Li 0.2786(7) 0.8995(6) 0.0627(3) 0.038(4) Uani 1 1 d . . . O81 O 0.3593(3) 0.9630(2) 0.07313(12) 0.0408(18) Uani 1 1 d . . . O82 O 0.3012(3) 0.8404(2) 0.01769(12) 0.0423(18) Uani 1 1 d . . . C81 C 0.3749(4) 1.0550(4) 0.09075(19) 0.0476(19) Uiso 1 1 d . . . H81A H 0.3578 1.0620 0.1139 0.071 Uiso 1 1 calc R . . H81B H 0.3569 1.1028 0.0706 0.071 Uiso 1 1 calc R . . H81C H 0.4206 1.0623 0.0996 0.071 Uiso 1 1 calc R . . C82 C 0.3819(5) 0.9496(4) 0.0392(2) 0.052(2) Uiso 1 1 d . . . H82A H 0.4278 0.9598 0.0466 0.063 Uiso 1 1 calc R . . H82B H 0.3619 0.9949 0.0179 0.063 Uiso 1 1 calc R . . C83 C 0.3671(5) 0.8527(4) 0.0239(2) 0.050(2) Uiso 1 1 d . . . H83A H 0.3784 0.8439 -0.0017 0.060 Uiso 1 1 calc R . . H83B H 0.3908 0.8070 0.0438 0.060 Uiso 1 1 calc R . . C84 C 0.2762(5) 0.7549(4) -0.0021(2) 0.060(2) Uiso 1 1 d . . . H84A H 0.2310 0.7522 -0.0050 0.089 Uiso 1 1 calc R . . H84B H 0.2969 0.7018 0.0140 0.089 Uiso 1 1 calc R . . H84C H 0.2837 0.7526 -0.0287 0.089 Uiso 1 1 calc R . . Li9 Li 0.5843(7) 0.6249(7) -0.0237(3) 0.035(4) Uani 1 1 d . . . Si9 Si 0.58635(11) 0.74952(10) 0.05216(4) 0.0292(7) Uani 1 1 d . . . O9 O 0.4311(2) 0.6311(2) -0.04460(9) 0.0194(13) Uani 1 1 d . . . N9 N 0.5373(3) 0.7078(3) 0.00845(12) 0.0212(17) Uani 1 1 d . . . C91 C 0.4957(3) 0.7658(3) -0.01843(14) 0.0185(12) Uiso 1 1 d . . . C92 C 0.4421(3) 0.7277(3) -0.04664(14) 0.0185(12) Uiso 1 1 d . . . C93 C 0.3976(3) 0.7812(3) -0.07311(15) 0.0221(12) Uiso 1 1 d . . . H93 H 0.3621 0.7521 -0.0908 0.027 Uiso 1 1 calc R . . C94 C 0.4043(3) 0.8775(3) -0.07409(15) 0.0233(13) Uiso 1 1 d . . . H94 H 0.3739 0.9149 -0.0922 0.028 Uiso 1 1 calc R . . C95 C 0.4567(3) 0.9172(3) -0.04784(14) 0.0218(12) Uiso 1 1 d . . . H95 H 0.4626 0.9827 -0.0484 0.026 Uiso 1 1 calc R . . C96 C 0.5005(3) 0.8635(3) -0.02095(15) 0.0210(12) Uiso 1 1 d . . . H96 H 0.5354 0.8938 -0.0033 0.025 Uiso 1 1 calc R . . C97 C 0.6482(4) 0.8347(4) 0.0456(2) 0.054(2) Uiso 1 1 d . . . H97A H 0.6278 0.8894 0.0307 0.081 Uiso 1 1 calc R . . H97B H 0.6746 0.8045 0.0307 0.081 Uiso 1 1 calc R . . H97C H 0.6743 0.8541 0.0722 0.081 Uiso 1 1 calc R . . C98 C 0.5431(4) 0.8054(4) 0.08486(17) 0.0404(17) Uiso 1 1 d . . . H98A H 0.5194 0.8589 0.0708 0.061 Uiso 1 1 calc R . . H98B H 0.5729 0.8265 0.1098 0.061 Uiso 1 1 calc R . . H98C H 0.5140 0.7602 0.0912 0.061 Uiso 1 1 calc R . . C99 C 0.6308(4) 0.6498(3) 0.08039(16) 0.0336(15) Uiso 1 1 d . . . H99A H 0.6543 0.6189 0.0638 0.050 Uiso 1 1 calc R . . H99B H 0.6015 0.6054 0.0870 0.050 Uiso 1 1 calc R . . H99C H 0.6600 0.6725 0.1053 0.050 Uiso 1 1 calc R . . C911 C 0.4587(3) 0.5765(3) -0.07046(15) 0.0198(12) Uiso 1 1 d . . . C912 C 0.5098(4) 0.5198(3) -0.05072(15) 0.0232(13) Uiso 1 1 d . . . C913 C 0.5314(4) 0.4634(3) -0.07765(16) 0.0290(14) Uiso 1 1 d . . . H913 H 0.5658 0.4229 -0.0668 0.035 Uiso 1 1 calc R . . C914 C 0.5056(4) 0.4637(3) -0.11880(16) 0.0303(14) Uiso 1 1 d . . . H914 H 0.5225 0.4246 -0.1355 0.036 Uiso 1 1 calc R . . C915 C 0.4549(4) 0.5214(4) -0.13567(18) 0.0338(15) Uiso 1 1 d . . . H915 H 0.4365 0.5211 -0.1640 0.041 Uiso 1 1 calc R . . C916 C 0.4311(4) 0.5795(3) -0.11122(16) 0.0273(14) Uiso 1 1 d . . . H916 H 0.3968 0.6200 -0.1223 0.033 Uiso 1 1 calc R . . Li10 Li 0.4932(6) 0.5857(5) 0.0056(3) 0.024(4) Uani 1 1 d . . . O101 O 0.6674(3) 0.5659(3) -0.00855(14) 0.058(2) Uani 1 1 d . . . O102 O 0.6166(3) 0.6951(3) -0.06339(12) 0.0438(19) Uani 1 1 d . . . C101 C 0.6926(6) 0.4903(6) 0.0154(2) 0.093(3) Uiso 1 1 d . . . H10A H 0.6604 0.4627 0.0265 0.140 Uiso 1 1 calc R . . H10B H 0.7280 0.5110 0.0375 0.140 Uiso 1 1 calc R . . H10C H 0.7070 0.4438 -0.0008 0.140 Uiso 1 1 calc R . . C102 C 0.7054(6) 0.6132(7) -0.0276(3) 0.103(4) Uiso 1 1 d . . . H10D H 0.7392 0.5711 -0.0306 0.124 Uiso 1 1 calc R . . H10E H 0.7253 0.6666 -0.0106 0.124 Uiso 1 1 calc R . . C103 C 0.6710(6) 0.6468(6) -0.0663(2) 0.070(3) Uiso 1 1 d . . . H10F H 0.6977 0.6891 -0.0771 0.084 Uiso 1 1 calc R . . H10G H 0.6587 0.5936 -0.0851 0.084 Uiso 1 1 calc R . . C104 C 0.5752(4) 0.7152(4) -0.10180(17) 0.0446(18) Uiso 1 1 d . . . H10H H 0.5383 0.7483 -0.0984 0.067 Uiso 1 1 calc R . . H10I H 0.5619 0.6568 -0.1164 0.067 Uiso 1 1 calc R . . H10J H 0.5967 0.7543 -0.1171 0.067 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 0.010(13) 0.045(6) 0.049(6) 0.017(5) 0.015(6) 0.006(5) O31 0.039(7) 0.085(4) 0.062(3) 0.042(3) 0.036(3) 0.023(3) O32 0.032(7) 0.080(4) 0.097(4) 0.058(3) 0.040(4) 0.031(3) Li2 0.029(11) 0.028(5) 0.014(4) 0.005(3) 0.010(5) 0.006(4) Si1 0.041(2) 0.0324(9) 0.0339(10) 0.0106(7) -0.0135(11) -0.0152(9) O1 0.025(4) 0.0174(17) 0.0186(19) 0.0008(13) 0.008(2) -0.0005(16) N1 0.028(6) 0.020(2) 0.026(3) 0.0058(18) -0.003(3) -0.003(2) Li3 0.039(12) 0.019(4) 0.019(5) 0.002(3) 0.014(5) 0.002(4) Si2 0.034(2) 0.0240(7) 0.0240(8) 0.0024(6) -0.0023(9) -0.0085(8) O2 0.022(4) 0.0176(17) 0.0198(19) 0.0012(13) 0.004(2) 0.0000(16) N2 0.014(5) 0.022(2) 0.026(2) 0.0012(17) 0.010(3) 0.002(2) Li4 0.024(15) 0.060(7) 0.054(7) -0.023(6) 0.014(7) -0.006(6) O41 0.110(10) 0.071(4) 0.121(5) -0.009(4) -0.010(6) -0.006(4) O42 0.050(9) 0.158(7) 0.070(4) -0.014(4) 0.046(4) -0.002(5) Li5 0.055(17) 0.077(8) 0.025(6) 0.026(5) 0.023(7) 0.024(8) O71 0.068(9) 0.086(5) 0.145(6) 0.013(4) -0.006(6) 0.021(4) O72 0.033(10) 0.204(9) 0.066(4) 0.031(4) 0.037(4) 0.025(6) Li6 0.025(11) 0.021(4) 0.028(5) 0.003(4) 0.010(5) 0.001(4) Si5 0.027(2) 0.0270(8) 0.0240(8) 0.0019(6) 0.0051(9) 0.0084(8) O5 0.020(4) 0.0195(17) 0.0234(19) -0.0004(14) 0.014(2) 0.0006(16) N5 0.030(6) 0.022(2) 0.025(2) 0.0013(18) 0.011(3) 0.003(2) Li7 0.024(11) 0.023(4) 0.022(5) -0.003(3) 0.002(5) 0.012(4) Si6 0.028(2) 0.0245(7) 0.0253(9) 0.0017(6) 0.0018(9) 0.0067(7) O6 0.021(4) 0.0194(17) 0.0223(19) 0.0005(14) 0.010(2) 0.0015(16) N6 0.029(5) 0.016(2) 0.025(2) 0.0025(17) 0.008(3) -0.002(2) Li8 0.065(14) 0.020(5) 0.034(6) -0.004(4) 0.022(6) 0.007(5) O81 0.052(6) 0.029(2) 0.044(3) -0.0060(18) 0.017(3) -0.005(2) O82 0.053(6) 0.031(2) 0.049(3) -0.0069(19) 0.025(3) -0.003(2) Li9 0.035(14) 0.037(5) 0.037(6) -0.002(4) 0.015(6) -0.007(5) Si9 0.035(2) 0.0216(7) 0.0243(8) 0.0032(6) -0.0043(9) -0.0053(7) O9 0.027(4) 0.0136(16) 0.0188(18) -0.0006(13) 0.008(2) -0.0021(16) N9 0.019(5) 0.019(2) 0.021(2) -0.0001(17) 0.000(2) 0.003(2) Li10 0.032(12) 0.018(4) 0.027(5) 0.009(3) 0.017(5) -0.003(4) O101 0.042(7) 0.069(3) 0.070(3) 0.031(3) 0.027(3) 0.012(3) O102 0.056(6) 0.041(2) 0.041(3) 0.0067(19) 0.025(3) 0.003(2) _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 O31 1.958(14) . ? Li1 O32 1.981(15) . ? Li1 N1 2.033(14) . ? Li1 C112 2.243(14) . ? Li1 Li2 2.54(2) . ? Li1 C32 2.74(2) . ? Li1 C33 2.77(2) . ? Li1 Si1 3.140(12) . ? O31 C31 1.334(8) . ? O31 C32 1.349(12) . ? O32 C33 1.375(15) . ? O32 C34 1.418(9) . ? C32 C33 1.356(14) . ? Li2 N1 2.000(11) . ? Li2 O1 2.016(9) . ? Li2 C212 2.176(10) . ? Li2 C112 2.292(11) . ? Li2 Li3 2.454(11) . ? Li2 C111 2.555(9) . ? Li2 C11 2.734(9) . ? Li2 C12 2.765(9) . ? Si1 N1 1.714(5) . ? Si1 C18 1.863(8) . ? Si1 C19 1.882(6) . ? Si1 C17 1.892(10) . ? O1 C12 1.421(6) . ? O1 C111 1.445(6) . ? N1 C11 1.392(7) . ? C11 C12 1.400(8) . ? C11 C16 1.410(6) . ? C12 C13 1.399(8) . ? C13 C14 1.394(7) . ? C14 C15 1.375(9) . ? C15 C16 1.398(8) . ? C111 C116 1.379(7) . ? C111 C112 1.410(8) . ? C112 C113 1.399(8) . ? C112 Li3 2.178(10) . ? C113 C114 1.384(7) . ? C114 C115 1.396(9) . ? C115 C116 1.378(8) . ? Li3 N2 2.010(11) . ? Li3 O2 2.013(10) . ? Li3 C212 2.225(10) . ? Li3 C211 2.493(10) . ? Li3 Li4 2.71(2) . ? Li3 C21 2.732(9) . ? Li3 C22 2.776(9) . ? Si2 N2 1.704(5) . ? Si2 C28 1.862(7) . ? Si2 C29 1.862(6) . ? Si2 C27 1.864(9) . ? Si2 Li4 3.172(11) . ? O2 C22 1.424(5) . ? O2 C211 1.447(7) . ? N2 C21 1.377(7) . ? N2 Li4 2.057(14) . ? C21 C22 1.418(9) . ? C21 C23 1.420(6) . ? C21 Li4 2.675(17) . ? C22 C26 1.367(8) . ? C23 C25 1.387(8) . ? C24 C25 1.373(9) . ? C24 C26 1.413(7) . ? C211 C216 1.375(7) . ? C211 C212 1.398(8) . ? C211 Li4 2.592(17) . ? C212 C213 1.402(8) . ? C212 Li4 2.334(15) . ? C213 C214 1.362(7) . ? C214 C215 1.380(10) . ? C215 C216 1.406(9) . ? Li4 O41 2.005(18) . ? Li4 O42 2.030(14) . ? Li4 C43 2.74(2) . ? O41 C41 1.273(11) . ? O41 C42 1.439(12) . ? O42 C43 1.302(17) . ? O42 C44 1.400(10) . ? C42 C43 1.373(16) . ? Li5 O71 1.994(19) . ? Li5 O72 2.041(14) . ? Li5 N5 2.049(14) . ? Li5 C512 2.349(15) . ? Li5 C511 2.566(18) . ? Li5 C72 2.68(2) . ? Li5 C51 2.700(18) . ? Li5 Li6 2.71(2) . ? Li5 Si5 3.157(9) . ? O71 C74 1.250(10) . ? O71 C73 1.442(13) . ? O72 C72 1.279(19) . ? O72 C71 1.389(11) . ? C72 C73 1.313(17) . ? Li6 N5 2.018(11) . ? Li6 O5 2.029(10) . ? Li6 C612 2.149(10) . ? Li6 C512 2.244(10) . ? Li6 Li7 2.419(12) . ? Li6 C511 2.516(10) . ? Li6 C51 2.733(9) . ? Li6 C52 2.788(10) . ? Si5 N5 1.705(5) . ? Si5 C59 1.862(6) . ? Si5 C57 1.873(9) . ? Si5 C58 1.876(7) . ? O5 C52 1.420(5) . ? O5 C511 1.435(7) . ? N5 C51 1.385(8) . ? C51 C52 1.412(9) . ? C51 C56 1.423(6) . ? C52 C53 1.368(8) . ? C53 C54 1.420(7) . ? C54 C55 1.376(9) . ? C55 C56 1.381(9) . ? C511 C516 1.378(7) . ? C511 C512 1.404(8) . ? C512 C513 1.412(8) . ? C512 Li7 2.175(10) . ? C513 C514 1.379(7) . ? C514 C515 1.396(9) . ? C515 C516 1.386(8) . ? Li7 N6 2.031(11) . ? Li7 O6 2.041(10) . ? Li7 C612 2.315(11) . ? Li7 C611 2.576(9) . ? Li7 Li8 2.66(2) . ? Li7 C61 2.750(9) . ? Si6 N6 1.713(5) . ? Si6 C69 1.855(5) . ? Si6 C67 1.859(9) . ? Si6 C68 1.875(7) . ? Si6 Li8 3.155(10) . ? O6 C62 1.424(6) . ? O6 C611 1.444(7) . ? N6 C61 1.399(7) . ? N6 Li8 2.070(13) . ? C61 C62 1.386(9) . ? C61 C66 1.425(7) . ? C62 C63 1.397(8) . ? C63 C64 1.404(7) . ? C64 C65 1.362(9) . ? C65 C66 1.386(8) . ? C611 C616 1.380(7) . ? C611 C612 1.382(8) . ? C611 Li8 2.680(16) . ? C612 C613 1.414(8) . ? C612 Li8 2.307(14) . ? C613 C614 1.389(7) . ? C614 C615 1.398(9) . ? C615 C616 1.393(8) . ? Li8 O82 1.952(12) . ? Li8 O81 1.953(16) . ? Li8 C82 2.728(19) . ? Li8 C83 2.745(18) . ? O81 C82 1.408(9) . ? O81 C81 1.455(7) . ? O82 C83 1.429(11) . ? O82 C84 1.437(7) . ? C82 C83 1.491(8) . ? Li9 O101 1.964(15) . ? Li9 O102 1.984(13) . ? Li9 N9 2.090(14) . ? Li9 C912 2.243(13) . ? Li9 Li10 2.56(2) . ? Li9 C102 2.73(2) . ? Li9 C103 2.738(19) . ? Li9 Si9 3.162(11) . ? Si9 N9 1.709(4) . ? Si9 C98 1.852(7) . ? Si9 C99 1.854(5) . ? Si9 C97 1.896(8) . ? O9 C92 1.411(5) . ? O9 C911 1.443(7) . ? O9 Li10 2.003(10) . ? N9 C91 1.391(7) . ? N9 Li10 1.995(10) . ? C91 C96 1.410(6) . ? C91 C92 1.424(8) . ? C91 Li10 2.717(9) . ? C92 C93 1.380(8) . ? C92 Li10 2.750(9) . ? C93 C94 1.390(6) . ? C94 C95 1.385(8) . ? C95 C96 1.380(8) . ? C911 C916 1.373(7) . ? C911 C912 1.410(9) . ? C911 Li10 2.528(10) . ? C912 C913 1.411(8) . ? C912 Li10 2.187(9) 3_665 ? C912 Li10 2.280(12) . ? C913 C914 1.379(7) . ? C913 Li10 2.781(11) 3_665 ? C914 C915 1.389(10) . ? C915 C916 1.390(8) . ? Li10 C912 2.187(9) 3_665 ? Li10 Li10 2.519(16) 3_665 ? Li10 C913 2.781(11) 3_665 ? O101 C102 1.380(12) . ? O101 C101 1.385(9) . ? O102 C103 1.419(11) . ? O102 C104 1.421(7) . ? C102 C103 1.430(11) . ? 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 O31 Li1 O32 83.7(6) . . ? O31 Li1 N1 115.0(5) . . ? O32 Li1 N1 130.8(6) . . ? O31 Li1 C112 114.6(5) . . ? O32 Li1 C112 109.4(5) . . ? N1 Li1 C112 103.0(7) . . ? O31 Li1 Li2 150.1(6) . . ? O32 Li1 Li2 126.0(5) . . ? N1 Li1 Li2 50.4(4) . . ? C112 Li1 Li2 56.9(4) . . ? O31 Li1 C32 27.4(3) . . ? O32 Li1 C32 56.4(5) . . ? N1 Li1 C32 130.9(5) . . ? C112 Li1 C32 120.3(6) . . ? Li2 Li1 C32 176.5(6) . . ? O31 Li1 C33 55.8(5) . . ? O32 Li1 C33 27.9(4) . . ? N1 Li1 C33 137.8(6) . . ? C112 Li1 C33 118.4(6) . . ? Li2 Li1 C33 153.8(5) . . ? C32 Li1 C33 28.5(3) . . ? O31 Li1 Si1 112.1(5) . . ? O32 Li1 Si1 101.4(5) . . ? N1 Li1 Si1 30.0(2) . . ? C112 Li1 Si1 125.8(6) . . ? Li2 Li1 Si1 68.9(4) . . ? C32 Li1 Si1 113.8(5) . . ? C33 Li1 Si1 109.8(5) . . ? C31 O31 C32 119.8(8) . . ? C31 O31 Li1 125.6(8) . . ? C32 O31 Li1 110.8(6) . . ? C33 O32 C34 116.2(10) . . ? C33 O32 Li1 109.7(8) . . ? C34 O32 Li1 129.0(7) . . ? O31 C32 C33 118.5(12) . . ? O31 C32 Li1 41.8(5) . . ? C33 C32 Li1 76.7(10) . . ? C32 C33 O32 117.2(14) . . ? C32 C33 Li1 74.8(10) . . ? O32 C33 Li1 42.4(6) . . ? N1 Li2 O1 87.0(4) . . ? N1 Li2 C212 129.9(5) . . ? O1 Li2 C212 139.6(7) . . ? N1 Li2 C112 102.3(5) . . ? O1 Li2 C112 67.6(3) . . ? C212 Li2 C112 111.4(4) . . ? N1 Li2 Li3 142.1(8) . . ? O1 Li2 Li3 106.3(4) . . ? C212 Li2 Li3 57.1(3) . . ? C112 Li2 Li3 54.5(3) . . ? N1 Li2 Li1 51.6(4) . . ? O1 Li2 Li1 87.5(4) . . ? C212 Li2 Li1 126.5(6) . . ? C112 Li2 Li1 55.1(4) . . ? Li3 Li2 Li1 92.8(5) . . ? N1 Li2 C111 94.7(4) . . ? O1 Li2 C111 34.4(2) . . ? C212 Li2 C111 133.2(4) . . ? C112 Li2 C111 33.3(2) . . ? Li3 Li2 C111 79.8(3) . . ? Li1 Li2 C111 67.1(4) . . ? N1 Li2 C11 29.3(2) . . ? O1 Li2 C11 59.0(3) . . ? C212 Li2 C11 150.4(4) . . ? C112 Li2 C11 97.0(4) . . ? Li3 Li2 C11 151.2(5) . . ? Li1 Li2 C11 63.8(4) . . ? C111 Li2 C11 75.8(3) . . ? N1 Li2 C12 58.3(3) . . ? O1 Li2 C12 29.62(18) . . ? C212 Li2 C12 157.4(7) . . ? C112 Li2 C12 83.3(3) . . ? Li3 Li2 C12 133.0(4) . . ? Li1 Li2 C12 75.8(4) . . ? C111 Li2 C12 53.6(2) . . ? C11 Li2 C12 29.48(19) . . ? N1 Si1 C18 111.7(3) . . ? N1 Si1 C19 108.4(2) . . ? C18 Si1 C19 107.5(3) . . ? N1 Si1 C17 114.3(3) . . ? C18 Si1 C17 108.8(4) . . ? C19 Si1 C17 105.8(4) . . ? N1 Si1 Li1 36.4(3) . . ? C18 Si1 Li1 147.3(4) . . ? C19 Si1 Li1 84.8(3) . . ? C17 Si1 Li1 96.1(4) . . ? C12 O1 C111 114.1(5) . . ? C12 O1 Li2 105.8(4) . . ? C111 O1 Li2 93.7(4) . . ? C11 N1 Si1 121.1(3) . . ? C11 N1 Li2 106.0(5) . . ? Si1 N1 Li2 121.9(3) . . ? C11 N1 Li1 107.7(4) . . ? Si1 N1 Li1 113.6(5) . . ? Li2 N1 Li1 78.0(5) . . ? N1 C11 C12 119.8(4) . . ? N1 C11 C16 125.5(5) . . ? C12 C11 C16 114.7(5) . . ? N1 C11 Li2 44.7(4) . . ? C12 C11 Li2 76.5(4) . . ? C16 C11 Li2 163.9(4) . . ? C13 C12 C11 123.8(5) . . ? C13 C12 O1 117.6(5) . . ? C11 C12 O1 118.2(4) . . ? C13 C12 Li2 158.1(6) . . ? C11 C12 Li2 74.0(4) . . ? O1 C12 Li2 44.5(3) . . ? C14 C13 C12 119.6(6) . . ? C15 C14 C13 118.3(5) . . ? C14 C15 C16 121.7(5) . . ? C15 C16 C11 122.0(6) . . ? C116 C111 C112 126.2(6) . . ? C116 C111 O1 118.8(5) . . ? C112 C111 O1 115.0(4) . . ? C116 C111 Li2 170.7(6) . . ? C112 C111 Li2 63.1(4) . . ? O1 C111 Li2 52.0(3) . . ? C113 C112 C111 111.7(5) . . ? C113 C112 Li3 100.7(4) . . ? C111 C112 Li3 125.7(7) . . ? C113 C112 Li1 110.6(7) . . ? C111 C112 Li1 98.2(5) . . ? Li3 C112 Li1 109.7(4) . . ? C113 C112 Li2 164.4(5) . . ? C111 C112 Li2 83.7(4) . . ? Li3 C112 Li2 66.5(3) . . ? Li1 C112 Li2 68.0(5) . . ? C114 C113 C112 125.6(6) . . ? C113 C114 C115 118.1(6) . . ? C116 C115 C114 120.6(5) . . ? C115 C116 C111 117.8(6) . . ? N2 Li3 O2 86.1(3) . . ? N2 Li3 C112 134.2(5) . . ? O2 Li3 C112 131.1(7) . . ? N2 Li3 C212 103.1(5) . . ? O2 Li3 C212 69.0(3) . . ? C112 Li3 C212 113.9(4) . . ? N2 Li3 Li2 143.7(7) . . ? O2 Li3 Li2 107.7(4) . . ? C112 Li3 Li2 59.0(3) . . ? C212 Li3 Li2 55.2(3) . . ? N2 Li3 C211 92.3(4) . . ? O2 Li3 C211 35.5(2) . . ? C112 Li3 C211 133.4(5) . . ? C212 Li3 C211 33.9(2) . . ? Li2 Li3 C211 82.3(3) . . ? N2 Li3 Li4 48.9(4) . . ? O2 Li3 Li4 79.9(4) . . ? C112 Li3 Li4 144.6(7) . . ? C212 Li3 Li4 55.4(4) . . ? Li2 Li3 Li4 99.4(5) . . ? C211 Li3 Li4 59.6(4) . . ? N2 Li3 C21 29.0(2) . . ? O2 Li3 C21 59.0(2) . . ? C112 Li3 C21 146.3(4) . . ? C212 Li3 C21 99.8(4) . . ? Li2 Li3 C21 154.8(5) . . ? C211 Li3 C21 75.6(3) . . ? Li4 Li3 C21 58.9(4) . . ? N2 Li3 C22 58.2(3) . . ? O2 Li3 C22 29.46(18) . . ? C112 Li3 C22 145.7(6) . . ? C212 Li3 C22 86.4(3) . . ? Li2 Li3 C22 135.4(4) . . ? C211 Li3 C22 54.4(2) . . ? Li4 Li3 C22 69.6(4) . . ? C21 Li3 C22 29.83(19) . . ? N2 Si2 C28 112.5(3) . . ? N2 Si2 C29 107.5(3) . . ? C28 Si2 C29 107.3(3) . . ? N2 Si2 C27 114.1(3) . . ? C28 Si2 C27 107.7(3) . . ? C29 Si2 C27 107.4(4) . . ? N2 Si2 Li4 36.1(4) . . ? C28 Si2 Li4 148.4(4) . . ? C29 Si2 Li4 90.7(3) . . ? C27 Si2 Li4 90.5(4) . . ? C22 O2 C211 115.1(4) . . ? C22 O2 Li3 106.5(4) . . ? C211 O2 Li3 90.7(4) . . ? C21 N2 Si2 124.3(3) . . ? C21 N2 Li3 106.0(6) . . ? Si2 N2 Li3 119.0(3) . . ? C21 N2 Li4 100.5(5) . . ? Si2 N2 Li4 114.7(5) . . ? Li3 N2 Li4 83.6(5) . . ? N2 C21 C22 120.0(4) . . ? N2 C21 C23 126.6(6) . . ? C22 C21 C23 113.4(5) . . ? N2 C21 Li4 49.1(4) . . ? C22 C21 Li4 94.9(4) . . ? C23 C21 Li4 127.7(6) . . ? N2 C21 Li3 45.0(4) . . ? C22 C21 Li3 76.8(4) . . ? C23 C21 Li3 164.3(4) . . ? Li4 C21 Li3 60.2(4) . . ? C26 C22 C21 125.3(5) . . ? C26 C22 O2 118.0(5) . . ? C21 C22 O2 116.6(4) . . ? C26 C22 Li3 157.8(6) . . ? C21 C22 Li3 73.4(4) . . ? O2 C22 Li3 44.0(3) . . ? C25 C23 C21 122.1(6) . . ? C25 C24 C26 118.1(6) . . ? C24 C25 C23 122.1(5) . . ? C22 C26 C24 119.0(6) . . ? C216 C211 C212 126.7(6) . . ? C216 C211 O2 117.7(5) . . ? C212 C211 O2 115.5(4) . . ? C216 C211 Li3 168.9(4) . . ? C212 C211 Li3 62.5(4) . . ? O2 C211 Li3 53.8(3) . . ? C216 C211 Li4 112.3(6) . . ? C212 C211 Li4 63.6(5) . . ? O2 C211 Li4 95.2(4) . . ? Li3 C211 Li4 64.4(4) . . ? C211 C212 C213 112.2(5) . . ? C211 C212 Li2 130.0(7) . . ? C213 C212 Li2 103.8(4) . . ? C211 C212 Li3 83.6(4) . . ? C213 C212 Li3 162.9(6) . . ? Li2 C212 Li3 67.8(3) . . ? C211 C212 Li4 84.0(5) . . ? C213 C212 Li4 101.5(6) . . ? Li2 C212 Li4 121.9(5) . . ? Li3 C212 Li4 72.9(5) . . ? C214 C213 C212 123.9(6) . . ? C213 C214 C215 121.3(7) . . ? C214 C215 C216 118.4(6) . . ? C211 C216 C215 117.4(6) . . ? O41 Li4 O42 83.0(7) . . ? O41 Li4 N2 131.9(7) . . ? O42 Li4 N2 112.6(6) . . ? O41 Li4 C212 110.3(6) . . ? O42 Li4 C212 123.9(6) . . ? N2 Li4 C212 98.0(7) . . ? O41 Li4 C211 135.0(5) . . ? O42 Li4 C211 100.6(6) . . ? N2 Li4 C211 88.4(6) . . ? C212 Li4 C211 32.4(3) . . ? O41 Li4 C21 149.8(6) . . ? O42 Li4 C21 88.1(5) . . ? N2 Li4 C21 30.4(3) . . ? C212 Li4 C21 98.6(7) . . ? C211 Li4 C21 75.0(5) . . ? O41 Li4 Li3 133.0(6) . . ? O42 Li4 Li3 143.9(8) . . ? N2 Li4 Li3 47.4(4) . . ? C212 Li4 Li3 51.7(4) . . ? C211 Li4 Li3 56.0(4) . . ? C21 Li4 Li3 61.0(4) . . ? O41 Li4 C43 56.6(6) . . ? O42 Li4 C43 26.8(4) . . ? N2 Li4 C43 132.3(6) . . ? C212 Li4 C43 124.3(5) . . ? C211 Li4 C43 114.7(5) . . ? C21 Li4 C43 113.3(6) . . ? Li3 Li4 C43 169.4(7) . . ? O41 Li4 Si2 102.8(5) . . ? O42 Li4 Si2 113.1(4) . . ? N2 Li4 Si2 29.2(2) . . ? C212 Li4 Si2 115.9(6) . . ? C211 Li4 Si2 116.1(6) . . ? C21 Li4 Si2 54.8(2) . . ? Li3 Li4 Si2 65.4(3) . . ? C43 Li4 Si2 119.8(5) . . ? C41 O41 C42 125.8(12) . . ? C41 O41 Li4 124.8(10) . . ? C42 O41 Li4 109.1(7) . . ? C43 O42 C44 115.5(10) . . ? C43 O42 Li4 108.4(10) . . ? C44 O42 Li4 133.5(10) . . ? C43 C42 O41 112.6(14) . . ? O42 C43 C42 120.9(13) . . ? O42 C43 Li4 44.8(7) . . ? C42 C43 Li4 79.3(9) . . ? O71 Li5 O72 84.4(7) . . ? O71 Li5 N5 129.9(7) . . ? O72 Li5 N5 111.4(7) . . ? O71 Li5 C512 112.1(6) . . ? O72 Li5 C512 123.0(6) . . ? N5 Li5 C512 98.4(7) . . ? O71 Li5 C511 137.2(5) . . ? O72 Li5 C511 99.0(6) . . ? N5 Li5 C511 88.6(7) . . ? C512 Li5 C511 32.8(3) . . ? O71 Li5 C72 57.1(6) . . ? O72 Li5 C72 27.3(5) . . ? N5 Li5 C72 127.0(6) . . ? C512 Li5 C72 129.5(5) . . ? C511 Li5 C72 118.2(6) . . ? O71 Li5 C51 148.2(6) . . ? O72 Li5 C51 87.3(6) . . ? N5 Li5 C51 30.1(3) . . ? C512 Li5 C51 98.1(7) . . ? C511 Li5 C51 74.4(5) . . ? C72 Li5 C51 110.5(6) . . ? O71 Li5 Li6 132.7(7) . . ? O72 Li5 Li6 142.9(9) . . ? N5 Li5 Li6 47.7(4) . . ? C512 Li5 Li6 52.0(4) . . ? C511 Li5 Li6 56.8(4) . . ? C72 Li5 Li6 170.1(8) . . ? C51 Li5 Li6 60.6(4) . . ? O71 Li5 Si5 100.4(5) . . ? O72 Li5 Si5 112.8(5) . . ? N5 Li5 Si5 29.5(2) . . ? C512 Li5 Si5 116.4(5) . . ? C511 Li5 Si5 116.6(6) . . ? C72 Li5 Si5 114.1(5) . . ? C51 Li5 Si5 55.2(2) . . ? Li6 Li5 Si5 65.5(3) . . ? C74 O71 C73 128.7(13) . . ? C74 O71 Li5 122.9(10) . . ? C73 O71 Li5 107.6(8) . . ? C72 O72 C71 117.8(12) . . ? C72 O72 Li5 105.6(11) . . ? C71 O72 Li5 136.5(10) . . ? O72 C72 C73 127.9(17) . . ? O72 C72 Li5 47.1(8) . . ? C73 C72 Li5 80.8(12) . . ? C72 C73 O71 114.4(16) . . ? N5 Li6 O5 85.4(4) . . ? N5 Li6 C612 131.8(5) . . ? O5 Li6 C612 134.2(7) . . ? N5 Li6 C512 102.8(5) . . ? O5 Li6 C512 67.9(3) . . ? C612 Li6 C512 116.0(4) . . ? N5 Li6 Li7 143.8(8) . . ? O5 Li6 Li7 107.5(4) . . ? C612 Li6 Li7 60.6(3) . . ? C512 Li6 Li7 55.5(3) . . ? N5 Li6 C511 90.7(4) . . ? O5 Li6 C511 34.8(2) . . ? C612 Li6 C511 137.3(5) . . ? C512 Li6 C511 33.7(2) . . ? Li7 Li6 C511 83.2(3) . . ? N5 Li6 Li5 48.6(4) . . ? O5 Li6 Li5 79.2(5) . . ? C612 Li6 Li5 143.4(7) . . ? C512 Li6 Li5 55.6(4) . . ? Li7 Li6 Li5 99.6(6) . . ? C511 Li6 Li5 58.6(4) . . ? N5 Li6 C51 29.3(3) . . ? O5 Li6 C51 58.4(3) . . ? C612 Li6 C51 144.2(4) . . ? C512 Li6 C51 99.8(4) . . ? Li7 Li6 C51 155.2(5) . . ? C511 Li6 C51 74.6(3) . . ? Li5 Li6 C51 59.4(4) . . ? N5 Li6 C52 58.1(3) . . ? O5 Li6 C52 29.22(18) . . ? C612 Li6 C52 146.2(6) . . ? C512 Li6 C52 86.2(3) . . ? Li7 Li6 C52 135.4(4) . . ? C511 Li6 C52 53.9(2) . . ? Li5 Li6 C52 70.0(4) . . ? C51 Li6 C52 29.6(2) . . ? N5 Si5 C59 107.6(3) . . ? N5 Si5 C57 113.9(3) . . ? C59 Si5 C57 107.3(4) . . ? N5 Si5 C58 112.4(3) . . ? C59 Si5 C58 107.3(3) . . ? C57 Si5 C58 108.0(3) . . ? N5 Si5 Li5 36.3(4) . . ? C59 Si5 Li5 90.5(3) . . ? C57 Si5 Li5 90.2(4) . . ? C58 Si5 Li5 148.6(4) . . ? C52 O5 C511 115.6(4) . . ? C52 O5 Li6 106.5(4) . . ? C511 O5 Li6 91.5(4) . . ? C51 N5 Si5 125.1(3) . . ? C51 N5 Li6 105.3(6) . . ? Si5 N5 Li6 118.1(3) . . ? C51 N5 Li5 101.9(5) . . ? Si5 N5 Li5 114.2(6) . . ? Li6 N5 Li5 83.7(5) . . ? N5 C51 C52 120.6(5) . . ? N5 C51 C56 125.3(6) . . ? C52 C51 C56 114.0(5) . . ? N5 C51 Li5 47.9(4) . . ? C52 C51 Li5 95.1(5) . . ? C56 C51 Li5 129.3(6) . . ? N5 C51 Li6 45.4(4) . . ? C52 C51 Li6 77.4(4) . . ? C56 C51 Li6 161.8(4) . . ? Li5 C51 Li6 59.9(4) . . ? C53 C52 C51 124.6(5) . . ? C53 C52 O5 119.1(6) . . ? C51 C52 O5 116.1(5) . . ? C53 C52 Li6 158.0(6) . . ? C51 C52 Li6 73.0(4) . . ? O5 C52 Li6 44.2(3) . . ? C52 C53 C54 119.3(6) . . ? C55 C54 C53 118.0(6) . . ? C54 C55 C56 121.9(5) . . ? C55 C56 C51 122.2(6) . . ? C516 C511 C512 125.7(6) . . ? C516 C511 O5 119.3(5) . . ? C512 C511 O5 115.0(4) . . ? C516 C511 Li6 168.6(4) . . ? C512 C511 Li6 62.5(4) . . ? O5 C511 Li6 53.7(3) . . ? C516 C511 Li5 110.1(6) . . ? C512 C511 Li5 65.0(5) . . ? O5 C511 Li5 96.0(4) . . ? Li6 C511 Li5 64.5(4) . . ? C511 C512 C513 112.4(5) . . ? C511 C512 Li7 131.3(7) . . ? C513 C512 Li7 105.3(4) . . ? C511 C512 Li6 83.8(4) . . ? C513 C512 Li6 161.7(6) . . ? Li7 C512 Li6 66.3(3) . . ? C511 C512 Li5 82.1(5) . . ? C513 C512 Li5 100.6(6) . . ? Li7 C512 Li5 120.3(5) . . ? Li6 C512 Li5 72.4(4) . . ? C514 C513 C512 124.7(6) . . ? C513 C514 C515 118.9(6) . . ? C516 C515 C514 119.9(5) . . ? C511 C516 C515 118.4(6) . . ? N6 Li7 O6 84.9(3) . . ? N6 Li7 C512 129.9(5) . . ? O6 Li7 C512 142.3(7) . . ? N6 Li7 C612 101.5(5) . . ? O6 Li7 C612 65.9(3) . . ? C512 Li7 C612 112.1(4) . . ? N6 Li7 Li6 139.6(8) . . ? O6 Li7 Li6 107.1(4) . . ? C512 Li7 Li6 58.2(3) . . ? C612 Li7 Li6 54.0(3) . . ? N6 Li7 C611 90.3(4) . . ? O6 Li7 C611 34.0(2) . . ? C512 Li7 C611 136.8(4) . . ? C612 Li7 C611 32.3(2) . . ? Li6 Li7 C611 81.4(4) . . ? N6 Li7 Li8 50.3(4) . . ? O6 Li7 Li8 83.0(4) . . ? C512 Li7 Li8 128.4(6) . . ? C612 Li7 Li8 54.8(4) . . ? Li6 Li7 Li8 92.2(5) . . ? C611 Li7 Li8 61.6(4) . . ? N6 Li7 C61 29.4(2) . . ? O6 Li7 C61 57.9(2) . . ? C512 Li7 C61 148.8(4) . . ? C612 Li7 C61 98.0(4) . . ? Li6 Li7 C61 151.4(6) . . ? C611 Li7 C61 74.1(3) . . ? Li8 Li7 C61 63.4(3) . . ? N6 Si6 C69 108.5(2) . . ? N6 Si6 C67 114.2(3) . . ? C69 Si6 C67 107.1(4) . . ? N6 Si6 C68 111.9(3) . . ? C69 Si6 C68 107.1(3) . . ? C67 Si6 C68 107.6(3) . . ? N6 Si6 Li8 37.2(3) . . ? C69 Si6 Li8 85.9(3) . . ? C67 Si6 Li8 94.7(3) . . ? C68 Si6 Li8 148.8(4) . . ? C62 O6 C611 115.1(5) . . ? C62 O6 Li7 106.1(4) . . ? C611 O6 Li7 93.7(4) . . ? C61 N6 Si6 121.7(3) . . ? C61 N6 Li7 105.1(6) . . ? Si6 N6 Li7 120.5(3) . . ? C61 N6 Li8 108.6(4) . . ? Si6 N6 Li8 112.7(5) . . ? Li7 N6 Li8 80.7(5) . . ? C62 C61 N6 120.3(4) . . ? C62 C61 C66 114.3(5) . . ? N6 C61 C66 125.4(5) . . ? C62 C61 Li7 77.3(4) . . ? N6 C61 Li7 45.5(4) . . ? C66 C61 Li7 161.8(4) . . ? C61 C62 C63 124.4(5) . . ? C61 C62 O6 117.3(5) . . ? C63 C62 O6 117.9(6) . . ? C62 C63 C64 118.9(6) . . ? C65 C64 C63 118.6(6) . . ? C64 C65 C66 121.8(5) . . ? C65 C66 C61 122.0(6) . . ? C616 C611 C612 127.3(6) . . ? C616 C611 O6 117.9(5) . . ? C612 C611 O6 114.7(4) . . ? C616 C611 Li7 168.2(4) . . ? C612 C611 Li7 63.4(4) . . ? O6 C611 Li7 52.2(3) . . ? C616 C611 Li8 118.4(6) . . ? C612 C611 Li8 59.4(4) . . ? O6 C611 Li8 94.7(4) . . ? Li7 C611 Li8 60.7(4) . . ? C611 C612 C613 112.5(5) . . ? C611 C612 Li6 133.5(7) . . ? C613 C612 Li6 103.9(4) . . ? C611 C612 Li8 89.5(5) . . ? C613 C612 Li8 102.4(6) . . ? Li6 C612 Li8 110.4(4) . . ? C611 C612 Li7 84.3(4) . . ? C613 C612 Li7 162.0(5) . . ? Li6 C612 Li7 65.5(3) . . ? Li8 C612 Li7 70.2(5) . . ? C614 C613 C612 123.8(5) . . ? C613 C614 C615 119.3(6) . . ? C616 C615 C614 119.8(5) . . ? C611 C616 C615 117.3(5) . . ? O82 Li8 O81 85.8(7) . . ? O82 Li8 N6 116.3(4) . . ? O81 Li8 N6 128.8(6) . . ? O82 Li8 C612 115.8(5) . . ? O81 Li8 C612 110.3(4) . . ? N6 Li8 C612 100.5(7) . . ? O82 Li8 Li7 149.0(7) . . ? O81 Li8 Li7 125.0(5) . . ? N6 Li8 Li7 49.0(4) . . ? C612 Li8 Li7 55.1(4) . . ? O82 Li8 C611 98.6(4) . . ? O81 Li8 C611 137.9(4) . . ? N6 Li8 C611 86.6(6) . . ? C612 Li8 C611 31.1(3) . . ? Li7 Li8 C611 57.7(4) . . ? O82 Li8 C82 57.2(4) . . ? O81 Li8 C82 29.5(3) . . ? N6 Li8 C82 144.2(6) . . ? C612 Li8 C82 114.0(4) . . ? Li7 Li8 C82 152.5(4) . . ? C611 Li8 C82 128.2(4) . . ? O82 Li8 C83 29.8(3) . . ? O81 Li8 C83 57.4(4) . . ? N6 Li8 C83 125.1(5) . . ? C612 Li8 C83 130.3(5) . . ? Li7 Li8 C83 174.1(4) . . ? C611 Li8 C83 124.9(4) . . ? C82 Li8 C83 31.6(3) . . ? O82 Li8 Si6 114.5(4) . . ? O81 Li8 Si6 99.3(4) . . ? N6 Li8 Si6 30.0(2) . . ? C612 Li8 Si6 122.5(6) . . ? Li7 Li8 Si6 67.5(3) . . ? C611 Li8 Si6 116.0(5) . . ? C82 Li8 Si6 115.7(5) . . ? C83 Li8 Si6 107.2(4) . . ? C82 O81 C81 112.0(5) . . ? C82 O81 Li8 107.4(5) . . ? C81 O81 Li8 126.9(6) . . ? C83 O82 C84 115.0(6) . . ? C83 O82 Li8 107.5(6) . . ? C84 O82 Li8 126.8(7) . . ? O81 C82 C83 109.1(7) . . ? O81 C82 Li8 43.1(4) . . ? C83 C82 Li8 74.8(6) . . ? O82 C83 C82 106.6(7) . . ? O82 C83 Li8 42.7(4) . . ? C82 C83 Li8 73.6(6) . . ? O101 Li9 O102 85.1(6) . . ? O101 Li9 N9 132.1(5) . . ? O102 Li9 N9 113.9(5) . . ? O101 Li9 C912 110.6(5) . . ? O102 Li9 C912 114.7(5) . . ? N9 Li9 C912 100.7(7) . . ? O101 Li9 Li10 125.8(5) . . ? O102 Li9 Li10 149.0(7) . . ? N9 Li9 Li10 49.6(4) . . ? C912 Li9 Li10 56.2(4) . . ? O101 Li9 C102 28.7(3) . . ? O102 Li9 C102 56.8(4) . . ? N9 Li9 C102 134.5(5) . . ? C912 Li9 C102 124.2(6) . . ? Li10 Li9 C102 154.1(5) . . ? O101 Li9 C103 56.5(5) . . ? O102 Li9 C103 29.9(3) . . ? N9 Li9 C103 138.2(5) . . ? C912 Li9 C103 113.6(5) . . ? Li10 Li9 C103 169.7(5) . . ? C102 Li9 C103 30.3(3) . . ? O101 Li9 Si9 102.9(4) . . ? O102 Li9 Si9 111.0(4) . . ? N9 Li9 Si9 29.99(19) . . ? C912 Li9 Si9 124.5(6) . . ? Li10 Li9 Si9 68.3(4) . . ? C102 Li9 Si9 106.5(4) . . ? C103 Li9 Si9 121.8(4) . . ? N9 Si9 C98 112.3(3) . . ? N9 Si9 C99 108.2(2) . . ? C98 Si9 C99 107.6(3) . . ? N9 Si9 C97 115.3(3) . . ? C98 Si9 C97 107.9(3) . . ? C99 Si9 C97 105.2(4) . . ? N9 Si9 Li9 37.7(3) . . ? C98 Si9 Li9 149.0(4) . . ? C99 Si9 Li9 83.4(3) . . ? C97 Si9 Li9 96.4(3) . . ? C92 O9 C911 113.2(4) . . ? C92 O9 Li10 106.0(4) . . ? C911 O9 Li10 93.0(4) . . ? C91 N9 Si9 121.7(3) . . ? C91 N9 Li10 105.3(5) . . ? Si9 N9 Li10 122.5(3) . . ? C91 N9 Li9 108.7(4) . . ? Si9 N9 Li9 112.3(4) . . ? Li10 N9 Li9 77.5(5) . . ? N9 C91 C96 126.0(5) . . ? N9 C91 C92 120.3(4) . . ? C96 C91 C92 113.7(5) . . ? N9 C91 Li10 45.1(4) . . ? C96 C91 Li10 166.3(4) . . ? C92 C91 Li10 76.2(3) . . ? C93 C92 O9 118.5(5) . . ? C93 C92 C91 123.5(4) . . ? O9 C92 C91 117.7(4) . . ? C93 C92 Li10 159.7(6) . . ? O9 C92 Li10 44.4(3) . . ? C91 C92 Li10 73.6(3) . . ? C92 C93 C94 120.4(6) . . ? C95 C94 C93 117.9(5) . . ? C96 C95 C94 121.4(5) . . ? C95 C96 C91 123.0(5) . . ? C916 C911 C912 126.0(6) . . ? C916 C911 O9 118.1(6) . . ? C912 C911 O9 115.8(4) . . ? C916 C911 Li10 170.2(6) . . ? C912 C911 Li10 63.5(4) . . ? O9 C911 Li10 52.3(3) . . ? C911 C912 C913 112.6(5) . . ? C911 C912 Li10 124.6(7) . 3_665 ? C913 C912 Li10 98.9(4) . 3_665 ? C911 C912 Li9 102.5(5) . . ? C913 C912 Li9 108.3(6) . . ? Li10 C912 Li9 109.4(4) 3_665 . ? C911 C912 Li10 82.9(5) . . ? C913 C912 Li10 164.2(5) . . ? Li10 C912 Li10 68.6(4) 3_665 . ? Li9 C912 Li10 68.9(5) . . ? C914 C913 C912 123.9(6) . . ? C914 C913 Li10 142.7(6) . 3_665 ? C912 C913 Li10 51.0(3) . 3_665 ? C913 C914 C915 119.5(7) . . ? C914 C915 C916 120.1(5) . . ? C911 C916 C915 117.8(6) . . ? N9 Li10 O9 88.2(3) . . ? N9 Li10 C912 133.0(5) . 3_665 ? O9 Li10 C912 134.0(6) . 3_665 ? N9 Li10 C912 102.4(5) . . ? O9 Li10 C912 68.3(3) . . ? C912 Li10 C912 111.4(4) 3_665 . ? N9 Li10 Li10 141.8(10) . 3_665 ? O9 Li10 Li10 105.6(5) . 3_665 ? C912 Li10 Li10 57.4(3) 3_665 3_665 ? C912 Li10 Li10 53.9(4) . 3_665 ? N9 Li10 C911 95.9(4) . . ? O9 Li10 C911 34.8(2) . . ? C912 Li10 C911 130.2(4) 3_665 . ? C912 Li10 C911 33.6(2) . . ? Li10 Li10 C911 78.8(4) 3_665 . ? N9 Li10 Li9 52.9(4) . . ? O9 Li10 Li9 90.9(4) . . ? C912 Li10 Li9 128.0(6) 3_665 . ? C912 Li10 Li9 54.9(4) . . ? Li10 Li10 Li9 90.7(7) 3_665 . ? C911 Li10 Li9 69.4(4) . . ? N9 Li10 C91 29.6(2) . . ? O9 Li10 C91 59.6(2) . . ? C912 Li10 C91 151.9(5) 3_665 . ? C912 Li10 C91 96.5(4) . . ? Li10 Li10 C91 150.2(7) 3_665 . ? C911 Li10 C91 76.0(3) . . ? Li9 Li10 C91 65.5(4) . . ? N9 Li10 C92 59.4(3) . . ? O9 Li10 C92 29.55(18) . . ? C912 Li10 C92 153.2(7) 3_665 . ? C912 Li10 C92 83.2(3) . . ? Li10 Li10 C92 131.9(5) 3_665 . ? C911 Li10 C92 53.5(2) . . ? Li9 Li10 C92 78.8(4) . . ? C91 Li10 C92 30.19(19) . . ? N9 Li10 C913 113.0(4) . 3_665 ? O9 Li10 C913 126.9(6) . 3_665 ? C912 Li10 C913 30.1(2) 3_665 3_665 ? C912 Li10 C913 140.8(4) . 3_665 ? Li10 Li10 C913 87.2(4) 3_665 3_665 ? C911 Li10 C913 147.0(5) . 3_665 ? Li9 Li10 C913 141.2(5) . 3_665 ? C91 Li10 C913 122.6(4) . 3_665 ? C92 Li10 C913 128.9(5) . 3_665 ? C102 O101 C101 118.1(9) . . ? C102 O101 Li9 108.2(7) . . ? C101 O101 Li9 133.8(8) . . ? C103 O102 C104 112.2(6) . . ? C103 O102 Li9 106.0(6) . . ? C104 O102 Li9 119.0(6) . . ? O101 C102 C103 111.8(11) . . ? O101 C102 Li9 43.1(5) . . ? C103 C102 Li9 75.2(8) . . ? O102 C103 C102 110.2(9) . . ? O102 C103 Li9 44.1(4) . . ? C102 C103 Li9 74.5(8) . . ? _diffrn_measured_fraction_theta_max 0.571 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.571 _refine_diff_density_max 0.847 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.078 data_c_phanish #:\mydocu~1\craig'~1\listru~1\phanis\phanish _database_code_CSD 163626 _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-(2-phenoxyphenyl)-N-(trimethylsilyl)amine ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H19 N O Si' _chemical_formula_weight 257.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 21.4777(4) _cell_length_b 7.9215(2) _cell_length_c 16.9555(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2884.7(10) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description acicular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.152 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf Nonius Kappa CCD _diffrn_measurement_method 1 deg phi scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number N/A _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37638 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.86 _reflns_number_total 3414 _reflns_number_gt 2851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius BV, 1994)' _computing_cell_refinement 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_data_reduction 'DENZO-SMN (Otwinoski and Minor, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Povray' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+1.6442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3414 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.367147(19) 0.12907(5) 0.25441(2) 0.01763(12) Uani 1 1 d . . . O1 O 0.45046(5) -0.32989(13) 0.14292(6) 0.0187(2) Uani 1 1 d . . . N1 N 0.39269(6) -0.04690(17) 0.20165(7) 0.0204(3) Uani 1 1 d . . . C1 C 0.36669(7) -0.13048(18) 0.13759(8) 0.0174(3) Uani 1 1 d . . . H1 H 0.4226(9) -0.096(2) 0.2201(11) 0.024(5) Uiso 1 1 d . . . C2 C 0.39648(7) -0.27208(18) 0.10510(8) 0.0170(3) Uani 1 1 d . . . C3 C 0.37317(7) -0.3578(2) 0.04076(9) 0.0213(3) Uani 1 1 d . . . H3 H 0.3959(9) -0.456(2) 0.0211(10) 0.027(5) Uiso 1 1 d . . . C4 C 0.31842(8) -0.3023(2) 0.00539(9) 0.0243(3) Uani 1 1 d . . . H4 H 0.3023(9) -0.358(3) -0.0404(11) 0.035(5) Uiso 1 1 d . . . C5 C 0.28784(7) -0.1632(2) 0.03622(9) 0.0238(3) Uani 1 1 d . . . H5 H 0.2490(9) -0.124(2) 0.0132(10) 0.028(5) Uiso 1 1 d . . . C6 C 0.31123(7) -0.0788(2) 0.10150(9) 0.0209(3) Uani 1 1 d . . . H6 H 0.2907(8) 0.015(2) 0.1211(10) 0.020(4) Uiso 1 1 d . . . C7 C 0.28906(8) 0.0897(3) 0.29901(11) 0.0309(4) Uani 1 1 d . . . C8 C 0.36255(9) 0.3180(2) 0.18953(10) 0.0274(4) Uani 1 1 d . . . C9 C 0.42682(8) 0.1607(2) 0.33230(10) 0.0239(3) Uani 1 1 d . . . C11 C 0.50757(6) -0.29493(18) 0.10829(8) 0.0162(3) Uani 1 1 d . . . C12 C 0.55930(7) -0.34630(19) 0.15114(9) 0.0209(3) Uani 1 1 d . . . H12 H 0.5531(8) -0.405(2) 0.2005(10) 0.022(4) Uiso 1 1 d . . . C13 C 0.61831(7) -0.3115(2) 0.12228(10) 0.0261(4) Uani 1 1 d . . . H13 H 0.6535(9) -0.347(2) 0.1529(10) 0.028(5) Uiso 1 1 d . . . C14 C 0.62580(8) -0.2264(2) 0.05133(10) 0.0269(4) Uani 1 1 d . . . H14 H 0.6670(9) -0.201(2) 0.0324(11) 0.033(5) Uiso 1 1 d . . . C15 C 0.57382(8) -0.1789(2) 0.00845(10) 0.0244(4) Uani 1 1 d . . . H15 H 0.5797(9) -0.118(2) -0.0410(11) 0.030(5) Uiso 1 1 d . . . C16 C 0.51408(7) -0.21278(19) 0.03644(9) 0.0194(3) Uani 1 1 d . . . H16 H 0.4792(9) -0.179(2) 0.0055(10) 0.023(4) Uiso 1 1 d . . . H7A H 0.2583(13) 0.064(3) 0.2616(14) 0.067(8) Uiso 1 1 d . . . H8A H 0.3352(11) 0.305(3) 0.1463(13) 0.048(6) Uiso 1 1 d . . . H9A H 0.4150(9) 0.254(3) 0.3674(12) 0.039(5) Uiso 1 1 d . . . H7B H 0.2759(11) 0.184(3) 0.3282(14) 0.059(7) Uiso 1 1 d . . . H8B H 0.3518(10) 0.415(3) 0.2215(12) 0.042(6) Uiso 1 1 d . . . H9B H 0.4667(11) 0.184(3) 0.3101(13) 0.049(6) Uiso 1 1 d . . . H7C H 0.2913(12) 0.002(4) 0.3370(16) 0.074(8) Uiso 1 1 d . . . H8C H 0.4025(11) 0.345(3) 0.1671(12) 0.046(6) Uiso 1 1 d . . . H9C H 0.4307(10) 0.064(3) 0.3639(13) 0.047(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0174(2) 0.0170(2) 0.0185(2) 0.00000(16) 0.00061(15) -0.00047(16) O1 0.0166(5) 0.0209(5) 0.0187(5) 0.0049(4) 0.0004(4) 0.0015(4) N1 0.0195(7) 0.0209(7) 0.0209(6) -0.0025(5) -0.0056(5) 0.0039(5) C1 0.0174(7) 0.0175(7) 0.0173(7) 0.0024(6) 0.0005(5) -0.0035(6) C2 0.0168(7) 0.0165(7) 0.0176(7) 0.0048(6) -0.0004(5) -0.0018(6) C3 0.0252(8) 0.0181(7) 0.0207(7) 0.0012(6) 0.0010(6) -0.0026(6) C4 0.0265(8) 0.0245(8) 0.0218(8) 0.0011(7) -0.0054(6) -0.0086(7) C5 0.0184(8) 0.0266(8) 0.0263(8) 0.0047(7) -0.0048(6) -0.0046(6) C6 0.0176(7) 0.0197(8) 0.0253(8) 0.0013(6) -0.0003(6) 0.0005(6) C7 0.0230(9) 0.0372(11) 0.0327(10) -0.0027(8) 0.0061(7) -0.0029(8) C8 0.0334(10) 0.0219(8) 0.0270(9) 0.0035(7) -0.0040(7) 0.0011(7) C9 0.0256(9) 0.0236(9) 0.0224(8) -0.0008(7) -0.0021(6) -0.0013(7) C11 0.0172(7) 0.0131(6) 0.0182(7) -0.0039(6) 0.0022(5) 0.0004(5) C12 0.0230(8) 0.0192(8) 0.0207(8) -0.0023(6) -0.0023(6) 0.0034(6) C13 0.0197(8) 0.0251(8) 0.0336(9) -0.0056(7) -0.0045(7) 0.0050(6) C14 0.0199(8) 0.0237(8) 0.0372(9) -0.0078(7) 0.0079(7) 0.0006(6) C15 0.0287(9) 0.0189(8) 0.0254(8) -0.0006(7) 0.0090(6) 0.0002(7) C16 0.0216(8) 0.0170(7) 0.0197(7) 0.0003(6) 0.0006(6) 0.0016(6) _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 N1 1.7448(14) . ? Si1 C9 1.8573(17) . ? Si1 C8 1.8601(18) . ? Si1 C7 1.8660(18) . ? O1 C11 1.3878(17) . ? O1 C2 1.4018(17) . ? N1 C1 1.3892(19) . ? C1 C6 1.400(2) . ? C1 C2 1.404(2) . ? C2 C3 1.379(2) . ? C3 C4 1.391(2) . ? C4 C5 1.385(2) . ? C5 C6 1.388(2) . ? C11 C16 1.388(2) . ? C11 C12 1.389(2) . ? C12 C13 1.386(2) . ? C13 C14 1.389(2) . ? C14 C15 1.384(2) . ? C15 C16 1.394(2) . ? 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 Si1 C9 104.79(7) . . ? N1 Si1 C8 110.87(8) . . ? C9 Si1 C8 110.41(8) . . ? N1 Si1 C7 110.91(8) . . ? C9 Si1 C7 110.76(8) . . ? C8 Si1 C7 109.06(9) . . ? C11 O1 C2 118.18(11) . . ? C1 N1 Si1 130.94(11) . . ? N1 C1 C6 122.96(14) . . ? N1 C1 C2 120.29(13) . . ? C6 C1 C2 116.74(13) . . ? C3 C2 O1 120.07(13) . . ? C3 C2 C1 122.58(14) . . ? O1 C2 C1 117.29(12) . . ? C2 C3 C4 119.47(15) . . ? C5 C4 C3 119.31(15) . . ? C4 C5 C6 120.87(15) . . ? C5 C6 C1 121.02(15) . . ? O1 C11 C16 123.62(13) . . ? O1 C11 C12 115.30(13) . . ? C16 C11 C12 121.07(14) . . ? C13 C12 C11 119.25(15) . . ? C12 C13 C14 120.55(15) . . ? C15 C14 C13 119.58(15) . . ? C14 C15 C16 120.74(15) . . ? C11 C16 C15 118.79(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.328 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.045