# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1601 # The synthesis and molecular structures of the crystalline # 1-aza-2-phospha(V)allyllithium compounds [Li(LL')(OEt2)2] # and [Li(LL')]2 [LL' = CH(SiMe3)P(Ph)2=NSiMe3] and the preparation # and characterisation of the new phosphinimines CH(R1)(R2)P(Ph)2=NSiMe3 # [R1 = R2 = SiMe3; R1 = H, R2 = Si(Me)2NEt2] data_complex6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Li(Et2O)2{Me3SiNP(Ph)2CHSiMe3}]' _chemical_formula_analytical ? _chemical_formula_sum 'C27 H49 Li N O2 P Si2' _chemical_formula_weight 513.76 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.332(3) _cell_length_b 10.682(4) _cell_length_c 17.870(5) _cell_angle_alpha 89.36(3) _cell_angle_beta 79.07(3) _cell_angle_gamma 65.26(3) _cell_volume 1583.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method ? _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5545 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5545 _reflns_number_observed 4413 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The H atom on C1 was freely refined ; all other H atoms were riding. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+1.8322P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5545 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_obs 0.0536 _refine_ls_wR_factor_all 0.1453 _refine_ls_wR_factor_obs 0.1325 _refine_ls_goodness_of_fit_all 1.022 _refine_ls_goodness_of_fit_obs 1.050 _refine_ls_restrained_S_all 1.022 _refine_ls_restrained_S_obs 1.050 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Li Li -0.0255(6) 0.4341(5) 0.7525(3) 0.0344(11) Uani 1 d . . P P 0.10178(8) 0.16617(7) 0.73824(4) 0.0228(2) Uani 1 d . . Si1 Si 0.29870(9) 0.25637(8) 0.61131(4) 0.0285(2) Uani 1 d . . Si2 Si -0.17078(9) 0.20695(8) 0.88395(4) 0.0275(2) Uani 1 d . . O1 O 0.0207(3) 0.5503(2) 0.81879(13) 0.0467(6) Uani 1 d . . O2 O -0.1865(3) 0.5556(2) 0.69517(14) 0.0480(6) Uani 1 d . . N N 0.1558(3) 0.2697(2) 0.68879(12) 0.0266(5) Uani 1 d . . C1 C -0.0840(3) 0.2544(3) 0.7945(2) 0.0258(6) Uani 1 d . . H1 H -0.1569(38) 0.2942(31) 0.7666(18) 0.033(8) Uiso 1 d . . C2 C 0.5078(4) 0.1573(4) 0.6265(2) 0.0473(8) Uani 1 d . . H2C H 0.5241(4) 0.0630(4) 0.6382(2) 0.071 Uiso 1 calc R . H2B H 0.5246(4) 0.2027(4) 0.6692(2) 0.071 Uiso 1 calc R . H2A H 0.5849(4) 0.1539(4) 0.5801(2) 0.071 Uiso 1 calc R . C3 C 0.2760(4) 0.4343(3) 0.5894(2) 0.0415(8) Uani 1 d . . H3C H 0.1669(4) 0.4896(3) 0.5810(2) 0.062 Uiso 1 calc R . H3B H 0.3548(4) 0.4289(3) 0.5432(2) 0.062 Uiso 1 calc R . H3A H 0.2944(4) 0.4777(3) 0.6324(2) 0.062 Uiso 1 calc R . C4 C 0.2794(5) 0.1777(4) 0.5228(2) 0.0451(8) Uani 1 d . . H4C H 0.1701(5) 0.2282(4) 0.5136(2) 0.068 Uiso 1 calc R . H4B H 0.3007(5) 0.0807(4) 0.5294(2) 0.068 Uiso 1 calc R . H4A H 0.3574(5) 0.1829(4) 0.4791(2) 0.068 Uiso 1 calc R . C5 C -0.0720(4) 0.2102(4) 0.9654(2) 0.0430(8) Uani 1 d . . H5C H -0.1252(4) 0.1836(4) 1.0113(2) 0.064 Uiso 1 calc R . H5B H -0.0811(4) 0.3037(4) 0.9749(2) 0.064 Uiso 1 calc R . H5A H 0.0421(4) 0.1451(4) 0.9525(2) 0.064 Uiso 1 calc R . C6 C -0.3863(4) 0.3376(3) 0.9107(2) 0.0475(9) Uani 1 d . . H6C H -0.4381(4) 0.3159(3) 0.9589(2) 0.071 Uiso 1 calc R . H6B H -0.4431(4) 0.3350(3) 0.8703(2) 0.071 Uiso 1 calc R . H6A H -0.3901(4) 0.4301(3) 0.9168(2) 0.071 Uiso 1 calc R . C7 C -0.1736(4) 0.0324(3) 0.8810(2) 0.0392(7) Uani 1 d . . H7C H -0.2224(4) 0.0169(3) 0.9317(2) 0.059 Uiso 1 calc R . H7B H -0.0630(4) -0.0391(3) 0.8659(2) 0.059 Uiso 1 calc R . H7A H -0.2367(4) 0.0284(3) 0.8439(2) 0.059 Uiso 1 calc R . C8 C 0.2376(3) 0.0783(3) 0.80211(15) 0.0257(6) Uani 1 d . . C9 C 0.3125(3) 0.1486(3) 0.8318(2) 0.0327(7) Uani 1 d . . H9 H 0.2987(3) 0.2371(3) 0.8155(2) 0.039 Uiso 1 calc R . C10 C 0.4074(4) 0.0907(4) 0.8853(2) 0.0418(8) Uani 1 d . . H10 H 0.4573(4) 0.1401(4) 0.9057(2) 0.050 Uiso 1 calc R . C11 C 0.4292(4) -0.0381(4) 0.9088(2) 0.0415(8) Uani 1 d . . H11 H 0.4947(4) -0.0777(4) 0.9452(2) 0.050 Uiso 1 calc R . C12 C 0.3562(4) -0.1094(3) 0.8796(2) 0.0373(7) Uani 1 d . . H12 H 0.3708(4) -0.1981(3) 0.8960(2) 0.045 Uiso 1 calc R . C13 C 0.2613(3) -0.0518(3) 0.8264(2) 0.0298(6) Uani 1 d . . H13 H 0.2117(3) -0.1018(3) 0.8062(2) 0.036 Uiso 1 calc R . C14 C 0.1187(3) 0.0245(3) 0.67516(15) 0.0270(6) Uani 1 d . . C15 C 0.2658(4) -0.0851(3) 0.6447(2) 0.0340(7) Uani 1 d . . H15 H 0.3608(4) -0.0918(3) 0.6599(2) 0.041 Uiso 1 calc R . C16 C 0.2752(4) -0.1844(3) 0.5927(2) 0.0440(8) Uani 1 d . . H16 H 0.3759(4) -0.2597(3) 0.5731(2) 0.053 Uiso 1 calc R . C17 C 0.1380(5) -0.1741(4) 0.5690(2) 0.0470(9) Uani 1 d . . H17 H 0.1446(5) -0.2415(4) 0.5327(2) 0.056 Uiso 1 calc R . C18 C -0.0075(5) -0.0662(4) 0.5983(2) 0.0481(9) Uani 1 d . . H18 H -0.1016(5) -0.0583(4) 0.5817(2) 0.058 Uiso 1 calc R . C19 C -0.0179(4) 0.0312(3) 0.6518(2) 0.0358(7) Uani 1 d . . H19 H -0.1199(4) 0.1038(3) 0.6730(2) 0.043 Uiso 1 calc R . C20 C 0.1003(5) 0.6363(4) 0.7912(3) 0.0702(12) Uani 1 d . . H20A H 0.0441(5) 0.7273(4) 0.8209(3) 0.084 Uiso 1 calc R . H20B H 0.0933(5) 0.6518(4) 0.7370(3) 0.084 Uiso 1 calc R . C21 C 0.2693(5) 0.5751(6) 0.7974(3) 0.086(2) Uani 1 d . . H21A H 0.3188(5) 0.6370(6) 0.7780(3) 0.130 Uiso 1 calc R . H21B H 0.3260(5) 0.4858(6) 0.7672(3) 0.130 Uiso 1 calc R . H21C H 0.2768(5) 0.5613(6) 0.8511(3) 0.130 Uiso 1 calc R . C22 C -0.0239(6) 0.5554(6) 0.8988(2) 0.0800(15) Uani 1 d . . H22A H 0.0420(6) 0.5909(6) 0.9216(2) 0.096 Uiso 1 calc R . H22B H 0.0039(6) 0.4598(6) 0.9138(2) 0.096 Uiso 1 calc R . C23 C -0.1877(6) 0.6369(6) 0.9311(3) 0.098(2) Uani 1 d . . H23A H -0.2055(6) 0.6333(6) 0.9867(3) 0.147 Uiso 1 calc R . H23B H -0.2548(6) 0.6013(6) 0.9106(3) 0.147 Uiso 1 calc R . H23C H -0.2166(6) 0.7328(6) 0.9184(3) 0.147 Uiso 1 calc R . C24 C -0.3193(6) 0.6816(5) 0.7257(4) 0.100(2) Uani 1 d . . H24A H -0.3561(6) 0.6737(5) 0.7805(4) 0.120 Uiso 1 calc R . H24B H -0.4087(6) 0.6948(5) 0.6996(4) 0.120 Uiso 1 calc R . C25 C -0.2877(6) 0.8024(4) 0.7187(3) 0.0761(13) Uani 1 d . . H25A H -0.3857(6) 0.8841(4) 0.7411(3) 0.114 Uiso 1 calc R . H25B H -0.2543(6) 0.8132(4) 0.6645(3) 0.114 Uiso 1 calc R . H25C H -0.2016(6) 0.7920(4) 0.7456(3) 0.114 Uiso 1 calc R . C26 C -0.1977(5) 0.5014(5) 0.6230(2) 0.0706(12) Uani 1 d . . H26A H -0.2177(5) 0.5750(5) 0.5870(2) 0.085 Uiso 1 calc R . H26B H -0.0924(5) 0.4244(5) 0.6012(2) 0.085 Uiso 1 calc R . C27 C -0.3213(6) 0.4522(5) 0.6281(3) 0.0752(13) Uani 1 d . . H27A H -0.3198(6) 0.4179(5) 0.5772(3) 0.113 Uiso 1 calc R . H27B H -0.4269(6) 0.5281(5) 0.6482(3) 0.113 Uiso 1 calc R . H27C H -0.3013(6) 0.3772(5) 0.6624(3) 0.113 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li 0.034(3) 0.028(2) 0.038(3) -0.005(2) -0.012(2) -0.008(2) P 0.0224(4) 0.0221(4) 0.0217(3) 0.0004(3) -0.0035(3) -0.0076(3) Si1 0.0311(4) 0.0268(4) 0.0241(4) 0.0021(3) -0.0010(3) -0.0108(3) Si2 0.0251(4) 0.0299(4) 0.0259(4) -0.0020(3) -0.0003(3) -0.0120(3) O1 0.059(2) 0.0537(14) 0.0373(12) -0.0094(10) -0.0031(11) -0.0362(13) O2 0.0421(13) 0.0325(12) 0.0591(15) 0.0069(11) -0.0158(11) -0.0038(10) N 0.0282(12) 0.0228(12) 0.0244(12) 0.0002(9) -0.0015(9) -0.0083(10) C1 0.0213(14) 0.0277(15) 0.0238(14) 0.0001(11) -0.0040(11) -0.0062(12) C2 0.030(2) 0.051(2) 0.048(2) 0.008(2) 0.0004(14) -0.009(2) C3 0.050(2) 0.036(2) 0.037(2) 0.0063(14) -0.0030(15) -0.020(2) C4 0.064(2) 0.045(2) 0.026(2) 0.0009(14) -0.0025(15) -0.025(2) C5 0.054(2) 0.059(2) 0.025(2) 0.0034(14) -0.0043(14) -0.034(2) C6 0.034(2) 0.041(2) 0.054(2) -0.005(2) 0.009(2) -0.011(2) C7 0.034(2) 0.038(2) 0.047(2) 0.0019(14) -0.0021(14) -0.0183(14) C8 0.0210(13) 0.0295(15) 0.0223(13) 0.0000(11) -0.0017(10) -0.0078(11) C9 0.030(2) 0.037(2) 0.0301(15) -0.0009(12) -0.0056(12) -0.0137(13) C10 0.032(2) 0.058(2) 0.036(2) -0.005(2) -0.0084(14) -0.020(2) C11 0.028(2) 0.057(2) 0.029(2) 0.0033(15) -0.0096(13) -0.0066(15) C12 0.034(2) 0.040(2) 0.030(2) 0.0101(13) -0.0050(13) -0.0082(14) C13 0.0241(14) 0.034(2) 0.0305(15) 0.0031(12) -0.0051(11) -0.0114(12) C14 0.0314(15) 0.0251(14) 0.0237(14) 0.0032(11) -0.0035(11) -0.0121(12) C15 0.037(2) 0.0274(15) 0.033(2) -0.0005(12) -0.0045(13) -0.0099(13) C16 0.057(2) 0.028(2) 0.036(2) -0.0036(13) 0.001(2) -0.011(2) C17 0.072(3) 0.040(2) 0.034(2) -0.0073(14) -0.007(2) -0.030(2) C18 0.059(2) 0.055(2) 0.044(2) -0.002(2) -0.018(2) -0.034(2) C19 0.037(2) 0.038(2) 0.033(2) -0.0013(13) -0.0089(13) -0.0149(14) C20 0.065(3) 0.042(2) 0.099(4) -0.005(2) -0.004(2) -0.023(2) C21 0.059(3) 0.114(4) 0.093(4) -0.011(3) -0.008(3) -0.046(3) C22 0.080(3) 0.137(5) 0.037(2) -0.006(2) -0.011(2) -0.059(3) C23 0.070(3) 0.110(4) 0.058(3) 0.019(3) 0.010(2) 0.006(3) C24 0.067(3) 0.050(3) 0.158(6) -0.015(3) -0.026(3) 0.001(2) C25 0.072(3) 0.045(2) 0.093(3) -0.001(2) 0.010(3) -0.017(2) C26 0.057(3) 0.103(4) 0.043(2) 0.007(2) -0.014(2) -0.024(2) C27 0.091(3) 0.076(3) 0.068(3) 0.013(2) -0.040(3) -0.034(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li O1 1.949(5) . ? Li O2 1.978(5) . ? Li N 2.018(5) . ? Li C1 2.289(6) . ? Li P 2.593(5) . ? P N 1.592(2) . ? P C1 1.702(3) . ? P C8 1.822(3) . ? P C14 1.832(3) . ? Si1 N 1.691(2) . ? Si1 C2 1.862(3) . ? Si1 C3 1.868(3) . ? Si1 C4 1.872(3) . ? Si2 C1 1.817(3) . ? Si2 C5 1.873(3) . ? Si2 C6 1.876(3) . ? Si2 C7 1.877(3) . ? O1 C22 1.406(4) . ? O1 C20 1.436(5) . ? O2 C24 1.417(5) . ? O2 C26 1.458(5) . ? C8 C9 1.387(4) . ? C8 C13 1.390(4) . ? C9 C10 1.389(4) . ? C10 C11 1.377(5) . ? C11 C12 1.377(5) . ? C12 C13 1.385(4) . ? C14 C19 1.388(4) . ? C14 C15 1.391(4) . ? C15 C16 1.382(4) . ? C16 C17 1.384(5) . ? C17 C18 1.372(5) . ? C18 C19 1.382(4) . ? C20 C21 1.460(6) . ? C22 C23 1.411(6) . ? C24 C25 1.438(6) . ? C26 C27 1.442(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Li O2 108.4(3) . . ? O1 Li N 120.4(3) . . ? O2 Li N 114.1(3) . . ? O1 Li C1 123.1(3) . . ? O2 Li C1 110.7(2) . . ? N Li C1 77.4(2) . . ? O1 Li P 126.9(2) . . ? O2 Li P 124.7(2) . . ? N Li P 37.86(11) . . ? C1 Li P 40.21(11) . . ? N P C1 110.18(13) . . ? N P C8 112.30(13) . . ? C1 P C8 106.58(13) . . ? N P C14 109.57(12) . . ? C1 P C14 114.65(14) . . ? C8 P C14 103.41(13) . . ? N P Li 51.08(14) . . ? C1 P Li 60.2(2) . . ? C8 P Li 116.10(14) . . ? C14 P Li 140.10(14) . . ? N Si1 C2 113.25(14) . . ? N Si1 C3 108.27(13) . . ? C2 Si1 C3 107.2(2) . . ? N Si1 C4 113.72(14) . . ? C2 Si1 C4 108.0(2) . . ? C3 Si1 C4 106.0(2) . . ? C1 Si2 C5 114.35(14) . . ? C1 Si2 C6 106.67(15) . . ? C5 Si2 C6 107.4(2) . . ? C1 Si2 C7 115.83(14) . . ? C5 Si2 C7 105.4(2) . . ? C6 Si2 C7 106.7(2) . . ? C22 O1 C20 115.0(3) . . ? C22 O1 Li 121.2(3) . . ? C20 O1 Li 123.9(3) . . ? C24 O2 C26 114.0(4) . . ? C24 O2 Li 125.0(3) . . ? C26 O2 Li 119.3(3) . . ? P N Si1 136.51(15) . . ? P N Li 91.1(2) . . ? Si1 N Li 132.4(2) . . ? P C1 Si2 128.2(2) . . ? P C1 Li 79.6(2) . . ? Si2 C1 Li 137.4(2) . . ? C9 C8 C13 118.5(3) . . ? C9 C8 P 118.2(2) . . ? C13 C8 P 123.2(2) . . ? C8 C9 C10 120.6(3) . . ? C11 C10 C9 120.1(3) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C13 120.0(3) . . ? C12 C13 C8 120.8(3) . . ? C19 C14 C15 118.2(3) . . ? C19 C14 P 119.1(2) . . ? C15 C14 P 122.5(2) . . ? C16 C15 C14 120.8(3) . . ? C15 C16 C17 120.1(3) . . ? C18 C17 C16 119.7(3) . . ? C17 C18 C19 120.3(3) . . ? C18 C19 C14 120.9(3) . . ? O1 C20 C21 112.2(4) . . ? O1 C22 C23 116.2(4) . . ? O2 C24 C25 115.1(4) . . ? C27 C26 O2 115.2(4) . . ? _refine_diff_density_max 0.880 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.057 #===END data_complex7 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{Li(Me3SiNPPh2CHSiMe3)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C38 H58 Li2 N2 P2 Si4' _chemical_formula_weight 731.04 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.988(2) _cell_length_b 11.478(2) _cell_length_c 18.753(3) _cell_angle_alpha 100.750(10) _cell_angle_beta 94.930(10) _cell_angle_gamma 108.830(10) _cell_volume 2171.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method ? _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7615 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 24.98 _reflns_number_total 7615 _reflns_number_observed 4860 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; H atoms on C1 and C20 were freely refined isotropic; others in riding mode. Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+0.1748P] 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 7614 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_obs 0.0638 _refine_ls_wR_factor_all 0.1762 _refine_ls_wR_factor_obs 0.1434 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.074 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Li1 Li 0.0490(9) 0.6052(8) 0.2593(6) 0.062(3) Uani 1 d . . Li2 Li 0.1796(8) 0.4533(9) 0.2288(5) 0.048(2) Uani 1 d . . P1 P 0.32404(10) 0.74519(10) 0.23893(6) 0.0260(3) Uani 1 d . . P2 P -0.04144(11) 0.30387(10) 0.24953(6) 0.0272(3) Uani 1 d . . Si1 Si 0.16227(14) 0.86994(13) 0.32872(8) 0.0417(4) Uani 1 d . . Si2 Si 0.41863(12) 0.53414(11) 0.15370(7) 0.0307(3) Uani 1 d . . Si3 Si -0.10852(12) 0.42493(12) 0.12892(7) 0.0317(3) Uani 1 d . . Si4 Si 0.16316(12) 0.38620(12) 0.39394(7) 0.0338(3) Uani 1 d . . N1 N 0.2034(3) 0.7495(3) 0.2806(2) 0.0338(9) Uani 1 d . . N2 N -0.0271(3) 0.4211(3) 0.2107(2) 0.0273(8) Uani 1 d . . C1 C 0.2993(4) 0.6008(4) 0.1858(3) 0.0294(10) Uani 1 d . . H1 H 0.2387(45) 0.5921(43) 0.1480(25) 0.043(14) Uiso 1 d . . C2 C 0.2882(7) 0.9793(8) 0.4058(4) 0.118(3) Uani 1 d . . H2C H 0.3162(7) 0.9305(8) 0.4372(4) 0.177 Uiso 1 calc R . H2B H 0.2519(7) 1.0367(8) 0.4347(4) 0.177 Uiso 1 calc R . H2A H 0.3631(7) 1.0285(8) 0.3862(4) 0.177 Uiso 1 calc R . C3 C 0.1104(6) 0.9639(5) 0.2697(4) 0.068(2) Uani 1 d . . H3C H 0.0437(6) 0.9068(5) 0.2288(4) 0.102 Uiso 1 calc R . H3B H 0.1856(6) 1.0131(5) 0.2504(4) 0.102 Uiso 1 calc R . H3A H 0.0744(6) 1.0213(5) 0.2989(4) 0.102 Uiso 1 calc R . C4 C 0.0128(7) 0.7904(7) 0.3667(4) 0.091(3) Uani 1 d . . H4C H -0.0545(7) 0.7323(7) 0.3263(4) 0.137 Uiso 1 calc R . H4B H -0.0195(7) 0.8543(7) 0.3922(4) 0.137 Uiso 1 calc R . H4A H 0.0342(7) 0.7430(7) 0.4012(4) 0.137 Uiso 1 calc R . C5 C 0.3590(4) 0.8695(4) 0.1880(2) 0.0274(9) Uani 1 d . . C6 C 0.4218(4) 0.9964(4) 0.2236(2) 0.0351(11) Uani 1 d . . H6 H 0.4532(4) 1.0180(4) 0.2748(2) 0.042 Uiso 1 calc R . C7 C 0.4387(5) 1.0912(4) 0.1852(3) 0.0450(12) Uani 1 d . . H7 H 0.4822(5) 1.1771(4) 0.2100(3) 0.054 Uiso 1 calc R . C8 C 0.3924(6) 1.0604(5) 0.1116(3) 0.058(2) Uani 1 d . . H8 H 0.4029(6) 1.1253(5) 0.0853(3) 0.069 Uiso 1 calc R . C9 C 0.3313(6) 0.9373(6) 0.0757(3) 0.065(2) Uani 1 d . . H9 H 0.2989(6) 0.9165(6) 0.0247(3) 0.077 Uiso 1 calc R . C10 C 0.3166(5) 0.8430(5) 0.1137(3) 0.0471(13) Uani 1 d . . H10 H 0.2761(5) 0.7574(5) 0.0878(3) 0.056 Uiso 1 calc R . C11 C 0.4738(4) 0.7877(4) 0.3029(2) 0.0291(10) Uani 1 d . . C12 C 0.5959(4) 0.8385(4) 0.2828(2) 0.0317(10) Uani 1 d . . H12 H 0.6019(4) 0.8597(4) 0.2363(2) 0.038 Uiso 1 calc R . C13 C 0.7075(4) 0.8582(4) 0.3296(3) 0.0411(12) Uani 1 d . . H13 H 0.7901(4) 0.8920(4) 0.3151(3) 0.049 Uiso 1 calc R . C14 C 0.7001(5) 0.8291(5) 0.3975(3) 0.0532(14) Uani 1 d . . H14 H 0.7775(5) 0.8432(5) 0.4298(3) 0.064 Uiso 1 calc R . C15 C 0.5792(5) 0.7791(6) 0.4186(3) 0.0550(15) Uani 1 d . . H15 H 0.5737(5) 0.7590(6) 0.4654(3) 0.066 Uiso 1 calc R . C16 C 0.4675(5) 0.7589(5) 0.3712(2) 0.0413(12) Uani 1 d . . H16 H 0.3849(5) 0.7246(5) 0.3857(2) 0.050 Uiso 1 calc R . C17 C 0.3272(5) 0.3759(4) 0.0901(3) 0.0534(14) Uani 1 d . . H17C H 0.3893(5) 0.3371(4) 0.0717(3) 0.080 Uiso 1 calc R . H17B H 0.2749(5) 0.3871(4) 0.0487(3) 0.080 Uiso 1 calc R . H17A H 0.2700(5) 0.3210(4) 0.1169(3) 0.080 Uiso 1 calc R . C18 C 0.5157(6) 0.5051(5) 0.2308(3) 0.0549(15) Uani 1 d . . H18C H 0.5791(6) 0.4691(5) 0.2115(3) 0.082 Uiso 1 calc R . H18B H 0.4573(6) 0.4458(5) 0.2549(3) 0.082 Uiso 1 calc R . H18A H 0.5617(6) 0.5851(5) 0.2665(3) 0.082 Uiso 1 calc R . C19 C 0.5340(5) 0.6225(4) 0.0994(3) 0.0454(12) Uani 1 d . . H19C H 0.5933(5) 0.5773(4) 0.0853(3) 0.068 Uiso 1 calc R . H19B H 0.5843(5) 0.7072(4) 0.1292(3) 0.068 Uiso 1 calc R . H19A H 0.4852(5) 0.6295(4) 0.0551(3) 0.068 Uiso 1 calc R . C20 C 0.1052(4) 0.3177(5) 0.2965(2) 0.0312(10) Uani 1 d . . H20 H 0.1215(51) 0.2546(50) 0.2834(28) 0.061(18) Uiso 1 d . . C21 C -0.0370(5) 0.3667(5) 0.0494(2) 0.0439(12) Uani 1 d . . H21C H 0.0571(5) 0.4122(5) 0.0578(2) 0.066 Uiso 1 calc R . H21B H -0.0766(5) 0.3812(5) 0.0046(2) 0.066 Uiso 1 calc R . H21A H -0.0539(5) 0.2761(5) 0.0439(2) 0.066 Uiso 1 calc R . C22 C -0.0890(5) 0.5954(4) 0.1340(3) 0.0444(12) Uani 1 d . . H22C H 0.0038(5) 0.6469(4) 0.1445(3) 0.067 Uiso 1 calc R . H22B H -0.1332(5) 0.6243(4) 0.1733(3) 0.067 Uiso 1 calc R . H22A H -0.1275(5) 0.6039(4) 0.0870(3) 0.067 Uiso 1 calc R . C23 C -0.2862(4) 0.3347(5) 0.1090(3) 0.0438(12) Uani 1 d . . H23C H -0.3278(4) 0.3626(5) 0.1498(3) 0.066 Uiso 1 calc R . H23B H -0.3009(4) 0.2443(5) 0.1030(3) 0.066 Uiso 1 calc R . H23A H -0.3237(4) 0.3494(5) 0.0636(3) 0.066 Uiso 1 calc R . C24 C -0.1006(4) 0.1547(4) 0.1815(2) 0.0316(10) Uani 1 d . . C25 C -0.0141(5) 0.1111(5) 0.1443(2) 0.0422(12) Uani 1 d . . H25 H 0.0763(5) 0.1593(5) 0.1552(2) 0.051 Uiso 1 calc R . C26 C -0.0572(6) -0.0006(5) 0.0920(3) 0.0543(14) Uani 1 d . . H26 H 0.0038(6) -0.0291(5) 0.0677(3) 0.065 Uiso 1 calc R . C27 C -0.1882(6) -0.0718(5) 0.0744(3) 0.056(2) Uani 1 d . . H27 H -0.2176(6) -0.1489(5) 0.0382(3) 0.067 Uiso 1 calc R . C28 C -0.2758(6) -0.0295(5) 0.1102(3) 0.0521(14) Uani 1 d . . H28 H -0.3662(6) -0.0773(5) 0.0982(3) 0.063 Uiso 1 calc R . C29 C -0.2327(5) 0.0817(4) 0.1634(2) 0.0390(11) Uani 1 d . . H29 H -0.2940(5) 0.1091(4) 0.1881(2) 0.047 Uiso 1 calc R . C30 C -0.1698(4) 0.2925(4) 0.3066(2) 0.0286(10) Uani 1 d . . C31 C -0.2312(4) 0.3802(5) 0.3165(2) 0.0368(11) Uani 1 d . . H31 H -0.2086(4) 0.4476(5) 0.2919(2) 0.044 Uiso 1 calc R . C32 C -0.3254(5) 0.3718(5) 0.3618(3) 0.0481(13) Uani 1 d . . H32 H -0.3659(5) 0.4339(5) 0.3688(3) 0.058 Uiso 1 calc R . C33 C -0.3603(5) 0.2722(6) 0.3967(3) 0.0519(14) Uani 1 d . . H33 H -0.4254(5) 0.2658(6) 0.4274(3) 0.062 Uiso 1 calc R . C34 C -0.3015(5) 0.1831(5) 0.3871(3) 0.0451(12) Uani 1 d . . H34 H -0.3259(5) 0.1150(5) 0.4111(3) 0.054 Uiso 1 calc R . C35 C -0.2065(4) 0.1924(4) 0.3423(2) 0.0386(11) Uani 1 d . . H35 H -0.1658(4) 0.1304(4) 0.3358(2) 0.046 Uiso 1 calc R . C36 C 0.1236(5) 0.5325(5) 0.4239(3) 0.0529(14) Uani 1 d . . H36C H 0.1558(5) 0.5676(5) 0.4765(3) 0.079 Uiso 1 calc R . H36B H 0.0291(5) 0.5119(5) 0.4148(3) 0.079 Uiso 1 calc R . H36A H 0.1653(5) 0.5949(5) 0.3962(3) 0.079 Uiso 1 calc R . C37 C 0.3440(5) 0.4253(6) 0.4116(3) 0.0558(15) Uani 1 d . . H37C H 0.3763(5) 0.4624(6) 0.4640(3) 0.084 Uiso 1 calc R . H37B H 0.3857(5) 0.4860(6) 0.3829(3) 0.084 Uiso 1 calc R . H37A H 0.3644(5) 0.3481(6) 0.3971(3) 0.084 Uiso 1 calc R . C38 C 0.0977(6) 0.2801(6) 0.4564(3) 0.059(2) Uani 1 d . . H38C H 0.1342(6) 0.3248(6) 0.5075(3) 0.088 Uiso 1 calc R . H38B H 0.1220(6) 0.2045(6) 0.4446(3) 0.088 Uiso 1 calc R . H38A H 0.0026(6) 0.2551(6) 0.4498(3) 0.088 Uiso 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 0.057(6) 0.033(5) 0.080(7) 0.003(5) 0.020(5) -0.003(4) Li2 0.034(5) 0.060(6) 0.047(5) 0.022(4) 0.010(4) 0.004(4) P1 0.0231(6) 0.0205(6) 0.0320(6) 0.0072(5) 0.0065(5) 0.0034(5) P2 0.0262(6) 0.0218(6) 0.0287(6) 0.0085(5) 0.0058(5) 0.0001(5) Si1 0.0418(8) 0.0402(8) 0.0483(8) 0.0082(6) 0.0146(6) 0.0201(7) Si2 0.0310(7) 0.0230(7) 0.0390(7) 0.0089(5) 0.0120(5) 0.0081(5) Si3 0.0283(7) 0.0278(7) 0.0356(7) 0.0111(5) 0.0047(5) 0.0030(5) Si4 0.0330(7) 0.0376(8) 0.0328(7) 0.0131(6) 0.0031(5) 0.0125(6) N1 0.027(2) 0.031(2) 0.045(2) 0.011(2) 0.011(2) 0.009(2) N2 0.024(2) 0.020(2) 0.033(2) 0.010(2) 0.005(2) -0.001(2) C1 0.025(2) 0.020(2) 0.042(3) 0.008(2) 0.013(2) 0.003(2) C2 0.104(6) 0.152(8) 0.077(5) -0.065(5) -0.007(4) 0.072(6) C3 0.074(4) 0.047(4) 0.106(5) 0.035(3) 0.039(4) 0.036(3) C4 0.093(5) 0.119(6) 0.130(6) 0.087(5) 0.082(5) 0.079(5) C5 0.022(2) 0.027(2) 0.032(2) 0.008(2) 0.004(2) 0.006(2) C6 0.035(3) 0.028(3) 0.038(3) 0.009(2) 0.001(2) 0.006(2) C7 0.048(3) 0.025(3) 0.058(3) 0.015(2) 0.005(3) 0.005(2) C8 0.069(4) 0.041(3) 0.069(4) 0.032(3) 0.007(3) 0.017(3) C9 0.091(5) 0.055(4) 0.040(3) 0.019(3) -0.017(3) 0.017(3) C10 0.054(3) 0.037(3) 0.043(3) 0.009(2) -0.005(2) 0.009(3) C11 0.031(2) 0.027(2) 0.030(2) 0.006(2) 0.006(2) 0.010(2) C12 0.030(2) 0.028(2) 0.036(2) 0.012(2) 0.006(2) 0.006(2) C13 0.025(2) 0.042(3) 0.054(3) 0.015(2) 0.005(2) 0.006(2) C14 0.039(3) 0.071(4) 0.049(3) 0.016(3) -0.004(3) 0.021(3) C15 0.052(3) 0.085(4) 0.040(3) 0.030(3) 0.011(3) 0.029(3) C16 0.035(3) 0.057(3) 0.038(3) 0.021(2) 0.012(2) 0.017(2) C17 0.054(3) 0.030(3) 0.072(4) 0.001(3) 0.020(3) 0.011(3) C18 0.074(4) 0.060(4) 0.051(3) 0.019(3) 0.018(3) 0.046(3) C19 0.050(3) 0.034(3) 0.049(3) 0.009(2) 0.022(2) 0.007(2) C20 0.028(2) 0.028(3) 0.037(3) 0.012(2) 0.010(2) 0.005(2) C21 0.040(3) 0.049(3) 0.039(3) 0.015(2) 0.006(2) 0.007(2) C22 0.046(3) 0.038(3) 0.049(3) 0.021(2) -0.001(2) 0.010(2) C23 0.033(3) 0.041(3) 0.053(3) 0.013(2) 0.006(2) 0.007(2) C24 0.038(3) 0.025(2) 0.024(2) 0.009(2) 0.003(2) 0.000(2) C25 0.048(3) 0.039(3) 0.039(3) 0.010(2) 0.010(2) 0.011(2) C26 0.080(4) 0.044(3) 0.043(3) 0.008(3) 0.012(3) 0.027(3) C27 0.090(5) 0.028(3) 0.039(3) 0.003(2) -0.001(3) 0.013(3) C28 0.061(4) 0.034(3) 0.042(3) 0.010(2) -0.001(3) -0.006(3) C29 0.042(3) 0.027(3) 0.039(3) 0.009(2) 0.005(2) -0.001(2) C30 0.023(2) 0.027(2) 0.027(2) 0.004(2) 0.001(2) -0.002(2) C31 0.028(2) 0.046(3) 0.031(2) 0.009(2) 0.003(2) 0.005(2) C32 0.036(3) 0.069(4) 0.041(3) 0.009(3) 0.008(2) 0.021(3) C33 0.030(3) 0.078(4) 0.038(3) 0.010(3) 0.012(2) 0.006(3) C34 0.039(3) 0.046(3) 0.040(3) 0.013(2) 0.010(2) -0.001(2) C35 0.038(3) 0.037(3) 0.033(2) 0.011(2) 0.006(2) 0.000(2) C36 0.042(3) 0.047(3) 0.059(3) -0.008(3) -0.009(3) 0.017(3) C37 0.041(3) 0.072(4) 0.055(3) 0.016(3) 0.001(3) 0.020(3) C38 0.063(4) 0.074(4) 0.045(3) 0.033(3) 0.010(3) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N1 1.898(10) . ? Li1 N2 2.000(9) . ? Li1 Li2 2.610(13) . ? Li2 C1 2.122(9) . ? Li2 N2 2.166(9) . ? Li2 C20 2.190(9) . ? Li2 P2 2.591(8) . ? P1 N1 1.606(4) . ? P1 C1 1.692(4) . ? P1 C11 1.820(4) . ? P1 C5 1.820(4) . ? P2 N2 1.617(3) . ? P2 C20 1.714(5) . ? P2 C24 1.819(4) . ? P2 C30 1.829(4) . ? Si1 N1 1.714(4) . ? Si1 C2 1.854(7) . ? Si1 C3 1.856(6) . ? Si1 C4 1.874(6) . ? Si2 C1 1.810(4) . ? Si2 C19 1.857(5) . ? Si2 C18 1.866(5) . ? Si2 C17 1.881(5) . ? Si3 N2 1.723(3) . ? Si3 C23 1.857(5) . ? Si3 C21 1.859(5) . ? Si3 C22 1.881(5) . ? Si4 C20 1.817(5) . ? Si4 C38 1.867(5) . ? Si4 C36 1.867(5) . ? Si4 C37 1.875(5) . ? C5 C10 1.375(6) . ? C5 C6 1.397(6) . ? C6 C7 1.386(6) . ? C7 C8 1.369(7) . ? C8 C9 1.362(7) . ? C9 C10 1.378(7) . ? C11 C16 1.383(6) . ? C11 C12 1.395(6) . ? C12 C13 1.374(6) . ? C13 C14 1.377(7) . ? C14 C15 1.391(7) . ? C15 C16 1.380(7) . ? C24 C25 1.390(6) . ? C24 C29 1.396(6) . ? C25 C26 1.374(7) . ? C26 C27 1.381(8) . ? C27 C28 1.380(8) . ? C28 C29 1.379(6) . ? C30 C31 1.375(6) . ? C30 C35 1.402(6) . ? C31 C32 1.385(6) . ? C32 C33 1.386(7) . ? C33 C34 1.368(7) . ? C34 C35 1.385(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Li1 N2 144.2(6) . . ? N1 Li1 Li2 91.8(4) . . ? N2 Li1 Li2 54.1(3) . . ? C1 Li2 N2 115.9(4) . . ? C1 Li2 C20 163.8(5) . . ? N2 Li2 C20 78.1(3) . . ? C1 Li2 P2 154.2(4) . . ? N2 Li2 P2 38.4(2) . . ? C20 Li2 P2 40.9(2) . . ? C1 Li2 Li1 84.1(4) . . ? N2 Li2 Li1 48.4(3) . . ? C20 Li2 Li1 101.3(4) . . ? P2 Li2 Li1 77.1(3) . . ? N1 P1 C1 112.7(2) . . ? N1 P1 C11 112.0(2) . . ? C1 P1 C11 107.0(2) . . ? N1 P1 C5 108.3(2) . . ? C1 P1 C5 113.1(2) . . ? C11 P1 C5 103.5(2) . . ? N2 P2 C20 111.0(2) . . ? N2 P2 C24 110.8(2) . . ? C20 P2 C24 108.2(2) . . ? N2 P2 C30 108.7(2) . . ? C20 P2 C30 113.7(2) . . ? C24 P2 C30 104.2(2) . . ? N2 P2 Li2 56.4(2) . . ? C20 P2 Li2 56.9(2) . . ? C24 P2 Li2 112.3(2) . . ? C30 P2 Li2 143.4(2) . . ? N1 Si1 C2 115.0(2) . . ? N1 Si1 C3 113.5(2) . . ? C2 Si1 C3 108.9(4) . . ? N1 Si1 C4 105.3(3) . . ? C2 Si1 C4 108.8(4) . . ? C3 Si1 C4 104.7(3) . . ? C1 Si2 C19 117.1(2) . . ? C1 Si2 C18 111.7(2) . . ? C19 Si2 C18 108.0(3) . . ? C1 Si2 C17 107.4(2) . . ? C19 Si2 C17 105.0(2) . . ? C18 Si2 C17 106.9(3) . . ? N2 Si3 C23 116.4(2) . . ? N2 Si3 C21 111.3(2) . . ? C23 Si3 C21 106.9(2) . . ? N2 Si3 C22 106.2(2) . . ? C23 Si3 C22 106.6(2) . . ? C21 Si3 C22 109.3(2) . . ? C20 Si4 C38 115.3(2) . . ? C20 Si4 C36 111.1(2) . . ? C38 Si4 C36 107.0(3) . . ? C20 Si4 C37 108.8(2) . . ? C38 Si4 C37 105.0(3) . . ? C36 Si4 C37 109.5(3) . . ? P1 N1 Si1 133.5(2) . . ? P1 N1 Li1 119.2(4) . . ? Si1 N1 Li1 105.6(3) . . ? P2 N2 Si3 129.6(2) . . ? P2 N2 Li1 126.9(4) . . ? Si3 N2 Li1 101.3(3) . . ? P2 N2 Li2 85.2(3) . . ? Si3 N2 Li2 123.0(3) . . ? Li1 N2 Li2 77.5(4) . . ? P1 C1 Si2 128.7(3) . . ? P1 C1 Li2 112.1(3) . . ? Si2 C1 Li2 101.3(3) . . ? C10 C5 C6 117.3(4) . . ? C10 C5 P1 121.2(3) . . ? C6 C5 P1 121.4(3) . . ? C7 C6 C5 121.0(4) . . ? C8 C7 C6 119.6(5) . . ? C9 C8 C7 120.4(5) . . ? C8 C9 C10 119.9(5) . . ? C5 C10 C9 121.8(5) . . ? C16 C11 C12 118.7(4) . . ? C16 C11 P1 119.3(3) . . ? C12 C11 P1 121.8(3) . . ? C13 C12 C11 120.6(4) . . ? C12 C13 C14 120.3(4) . . ? C13 C14 C15 119.9(5) . . ? C16 C15 C14 119.6(5) . . ? C15 C16 C11 121.0(4) . . ? P2 C20 Si4 126.1(3) . . ? P2 C20 Li2 82.2(3) . . ? Si4 C20 Li2 112.3(3) . . ? C25 C24 C29 117.7(4) . . ? C25 C24 P2 120.2(3) . . ? C29 C24 P2 122.0(4) . . ? C26 C25 C24 121.0(5) . . ? C25 C26 C27 120.7(5) . . ? C28 C27 C26 119.1(5) . . ? C29 C28 C27 120.4(5) . . ? C28 C29 C24 121.0(5) . . ? C31 C30 C35 118.6(4) . . ? C31 C30 P2 122.1(3) . . ? C35 C30 P2 119.4(3) . . ? C30 C31 C32 121.1(5) . . ? C31 C32 C33 119.6(5) . . ? C34 C33 C32 120.4(5) . . ? C33 C34 C35 119.9(5) . . ? C34 C35 C30 120.5(5) . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.076