# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 186/1687
 
data_lappert-paper-structure-4 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      [{(Me3SiN(CHN)3)SiMe3)Li}3] 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C29.50 H69 Li3 N12 Si6' 
_chemical_formula_weight          781.33 
_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' 
 'Li'  'Li'  -0.0003   0.0001 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/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                    18.869(7) 
_cell_length_b                    14.603(4) 
_cell_length_c                    19.523(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  112.10(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      4984.2(25) 
_cell_formula_units_Z             4 
_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           0.40 
_exptl_crystal_size_mid           0.40 
_exptl_crystal_size_min           0.40 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.041 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1692 
_exptl_absorpt_coefficient_mu     0.199 
_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        ' 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             9027 
_diffrn_reflns_av_R_equivalents   0.0334 
_diffrn_reflns_av_sigmaI/netI     0.0918 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -23 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.25 
_diffrn_reflns_theta_max          24.97 
_reflns_number_total              8753 
_reflns_number_observed           5240 
_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 
; 
 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^)+(0.0545P)^2^+2.6341P] 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     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8752 
_refine_ls_number_parameters      453 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1186 
_refine_ls_R_factor_obs           0.0610 
_refine_ls_wR_factor_all          0.1608 
_refine_ls_wR_factor_obs          0.1316 
_refine_ls_goodness_of_fit_all    1.020 
_refine_ls_goodness_of_fit_obs    1.095 
_refine_ls_restrained_S_all       1.021 
_refine_ls_restrained_S_obs       1.095 
_refine_ls_shift/esd_max          0.003 
_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 0.7248(4) 0.0496(4) 0.0454(4) 0.044(2) Uani 1 d . . 
Li2 Li 0.7018(4) -0.0958(4) -0.0659(4) 0.041(2) Uani 1 d . . 
Li3 Li 0.6606(4) -0.2453(5) -0.1732(4) 0.044(2) Uani 1 d . . 
Si1 Si 0.57148(6) 0.18934(7) -0.00019(6) 0.0358(3) Uani 1 d . . 
Si2 Si 0.46813(6) -0.31200(9) -0.34484(6) 0.0459(3) Uani 1 d . . 
Si3 Si 0.89644(6) 0.18319(8) 0.10530(6) 0.0378(3) Uani 1 d . . 
Si4 Si 0.76739(7) -0.28357(9) -0.28629(7) 0.0521(4) Uani 1 d . . 
Si5 Si 0.73130(7) 0.05454(9) 0.25872(6) 0.0470(3) Uani 1 d . . 
Si6 Si 0.64179(7) -0.44389(8) -0.09120(7) 0.0475(3) Uani 1 d . . 
N1 N 0.6201(2) 0.1047(2) -0.0284(2) 0.0316(7) Uani 1 d . . 
N2 N 0.6148(2) -0.0124(2) -0.1118(2) 0.0322(7) Uani 1 d . . 
N3 N 0.5862(2) -0.1336(2) -0.1934(2) 0.0344(7) Uani 1 d . . 
N4 N 0.5401(2) -0.2549(2) -0.2738(2) 0.0372(8) Uani 1 d . . 
N5 N 0.8337(2) 0.0987(2) 0.0539(2) 0.0328(7) Uani 1 d . . 
N6 N 0.8037(2) -0.0224(2) -0.0280(2) 0.0307(7) Uani 1 d . . 
N7 N 0.7778(2) -0.1350(2) -0.1146(2) 0.0306(7) Uani 1 d . . 
N8 N 0.7524(2) -0.2386(2) -0.2104(2) 0.0367(8) Uani 1 d . . 
N9 N 0.7234(2) 0.0251(2) 0.1696(2) 0.0378(8) Uani 1 d . . 
N10 N 0.7029(2) -0.0802(2) 0.0763(2) 0.0330(7) Uani 1 d . . 
N11 N 0.6828(2) -0.1966(2) -0.0078(2) 0.0331(7) Uani 1 d . . 
N12 N 0.6599(2) -0.3263(2) -0.0835(2) 0.0358(7) Uani 1 d . . 
C1 C 0.5854(2) 0.0626(3) -0.0895(2) 0.0339(9) Uani 1 d . . 
H1 H 0.5366(2) 0.0846(3) -0.1210(2) 0.041 Uiso 1 calc R . 
C2 C 0.5680(2) -0.0548(3) -0.1719(2) 0.0368(9) Uani 1 d . . 
H2 H 0.5202(2) -0.0275(3) -0.2002(2) 0.044 Uiso 1 calc R . 
C3 C 0.5307(2) -0.1745(3) -0.2531(2) 0.0390(9) Uani 1 d . . 
H3 H 0.4847(2) -0.1424(3) -0.2793(2) 0.047 Uiso 1 calc R . 
C4 C 0.5255(2) 0.1333(3) 0.0578(2) 0.0534(12) Uani 1 d . . 
H4C H 0.4880(2) 0.0884(3) 0.0281(2) 0.080 Uiso 1 calc R . 
H4B H 0.4998(2) 0.1797(3) 0.0765(2) 0.080 Uiso 1 calc R . 
H4A H 0.5646(2) 0.1023(3) 0.0996(2) 0.080 Uiso 1 calc R . 
C5 C 0.6425(3) 0.2743(3) 0.0551(3) 0.0644(13) Uani 1 d . . 
H5C H 0.6665(3) 0.3036(3) 0.0240(3) 0.097 Uiso 1 calc R . 
H5B H 0.6818(3) 0.2436(3) 0.0968(3) 0.097 Uiso 1 calc R . 
H5A H 0.6170(3) 0.3210(3) 0.0737(3) 0.097 Uiso 1 calc R . 
C6 C 0.4974(2) 0.2485(3) -0.0800(2) 0.0575(12) Uani 1 d . . 
H6C H 0.4595(2) 0.2037(3) -0.1095(2) 0.086 Uiso 1 calc R . 
H6B H 0.5219(2) 0.2773(3) -0.1108(2) 0.086 Uiso 1 calc R . 
H6A H 0.4720(2) 0.2954(3) -0.0616(2) 0.086 Uiso 1 calc R . 
C7 C 0.5162(3) -0.3897(3) -0.3897(3) 0.0645(14) Uani 1 d . . 
H7C H 0.5457(3) -0.3532(3) -0.4117(3) 0.097 Uiso 1 calc R . 
H7B H 0.4775(3) -0.4255(3) -0.4283(3) 0.097 Uiso 1 calc R . 
H7A H 0.5506(3) -0.4312(3) -0.3526(3) 0.097 Uiso 1 calc R . 
C8 C 0.4124(3) -0.3821(3) -0.3033(3) 0.0651(14) Uani 1 d . . 
H8C H 0.4469(3) -0.4237(3) -0.2664(3) 0.098 Uiso 1 calc R . 
H8B H 0.3738(3) -0.4177(3) -0.3421(3) 0.098 Uiso 1 calc R . 
H8A H 0.3870(3) -0.3417(3) -0.2795(3) 0.098 Uiso 1 calc R . 
C9 C 0.4026(3) -0.2329(4) -0.4149(3) 0.077(2) Uani 1 d . . 
H9C H 0.4321(3) -0.1960(4) -0.4367(3) 0.115 Uiso 1 calc R . 
H9B H 0.3773(3) -0.1925(4) -0.3911(3) 0.115 Uiso 1 calc R . 
H9A H 0.3641(3) -0.2686(4) -0.4537(3) 0.115 Uiso 1 calc R . 
C10 C 0.8503(2) 0.0469(2) 0.0093(2) 0.0313(8) Uani 1 d . . 
H10 H 0.8966(2) 0.0572(2) 0.0019(2) 0.038 Uiso 1 calc R . 
C11 C 0.8232(2) -0.0688(2) -0.0767(2) 0.0300(8) Uani 1 d . . 
H11 H 0.8689(2) -0.0546(2) -0.0841(2) 0.036 Uiso 1 calc R . 
C12 C 0.7949(2) -0.1760(3) -0.1693(2) 0.0347(9) Uani 1 d . . 
H12 H 0.8396(2) -0.1576(3) -0.1771(2) 0.042 Uiso 1 calc R . 
C13 C 0.9857(3) 0.1847(4) 0.0875(3) 0.095(2) Uani 1 d . . 
H13C H 0.9739(3) 0.1972(4) 0.0350(3) 0.142 Uiso 1 calc R . 
H13B H 1.0112(3) 0.1251(4) 0.1005(3) 0.142 Uiso 1 calc R . 
H13A H 1.0196(3) 0.2327(4) 0.1175(3) 0.142 Uiso 1 calc R . 
C14 C 0.9169(4) 0.1600(4) 0.2031(3) 0.116(3) Uani 1 d . . 
H14C H 0.9404(4) 0.0994(4) 0.2160(3) 0.174 Uiso 1 calc R . 
H14B H 0.8692(4) 0.1618(4) 0.2120(3) 0.174 Uiso 1 calc R . 
H14A H 0.9522(4) 0.2066(4) 0.2335(3) 0.174 Uiso 1 calc R . 
C15 C 0.8524(3) 0.2972(3) 0.0810(3) 0.089(2) Uani 1 d . . 
H15C H 0.8414(3) 0.3096(3) 0.0287(3) 0.133 Uiso 1 calc R . 
H15B H 0.8877(3) 0.3437(3) 0.1115(3) 0.133 Uiso 1 calc R . 
H15A H 0.8047(3) 0.2989(3) 0.0900(3) 0.133 Uiso 1 calc R . 
C16 C 0.7540(3) -0.4090(3) -0.2880(3) 0.074(2) Uani 1 d . . 
H16C H 0.7927(3) -0.4361(3) -0.2438(3) 0.111 Uiso 1 calc R . 
H16B H 0.7594(3) -0.4344(3) -0.3322(3) 0.111 Uiso 1 calc R . 
H16A H 0.7029(3) -0.4229(3) -0.2888(3) 0.111 Uiso 1 calc R . 
C17 C 0.8650(3) -0.2601(4) -0.2850(3) 0.081(2) Uani 1 d . . 
H17C H 0.8734(3) -0.1938(4) -0.2841(3) 0.121 Uiso 1 calc R . 
H17B H 0.8697(3) -0.2863(4) -0.3294(3) 0.121 Uiso 1 calc R . 
H17A H 0.9033(3) -0.2880(4) -0.2409(3) 0.121 Uiso 1 calc R . 
C18 C 0.6952(3) -0.2299(4) -0.3691(3) 0.096(2) Uani 1 d . . 
H18C H 0.7032(3) -0.1635(4) -0.3671(3) 0.143 Uiso 1 calc R . 
H18B H 0.6438(3) -0.2431(4) -0.3702(3) 0.143 Uiso 1 calc R . 
H18A H 0.7003(3) -0.2546(4) -0.4136(3) 0.143 Uiso 1 calc R . 
C19 C 0.7073(2) -0.0562(3) 0.1454(2) 0.0356(9) Uani 1 d . . 
H19 H 0.6981(2) -0.1013(3) 0.1761(2) 0.043 Uiso 1 calc R . 
C20 C 0.6880(2) -0.1667(3) 0.0575(2) 0.0342(9) Uani 1 d . . 
H20 H 0.6809(2) -0.2083(3) 0.0917(2) 0.041 Uiso 1 calc R . 
C21 C 0.6680(2) -0.2874(3) -0.0220(2) 0.0372(9) Uani 1 d . . 
H21 H 0.6632(2) -0.3245(3) 0.0161(2) 0.045 Uiso 1 calc R . 
C22 C 0.6650(3) -0.0151(4) 0.2884(3) 0.084(2) Uani 1 d . . 
H22C H 0.6780(3) -0.0801(4) 0.2886(3) 0.125 Uiso 1 calc R . 
H22B H 0.6122(3) -0.0052(4) 0.2539(3) 0.125 Uiso 1 calc R . 
H22A H 0.6699(3) 0.0034(4) 0.3382(3) 0.125 Uiso 1 calc R . 
C23 C 0.7061(4) 0.1763(4) 0.2587(3) 0.094(2) Uani 1 d . . 
H23C H 0.6539(4) 0.1861(4) 0.2231(3) 0.141 Uiso 1 calc R . 
H23B H 0.7417(4) 0.2136(4) 0.2446(3) 0.141 Uiso 1 calc R . 
H23A H 0.7095(4) 0.1940(4) 0.3082(3) 0.141 Uiso 1 calc R . 
C24 C 0.8301(2) 0.0335(4) 0.3255(2) 0.0684(15) Uani 1 d . . 
H24C H 0.8425(2) -0.0316(4) 0.3248(2) 0.103 Uiso 1 calc R . 
H24B H 0.8338(2) 0.0506(4) 0.3753(2) 0.103 Uiso 1 calc R . 
H24A H 0.8661(2) 0.0702(4) 0.3117(2) 0.103 Uiso 1 calc R . 
C25 C 0.6287(3) -0.4781(3) -0.1862(3) 0.080(2) Uani 1 d . . 
H25C H 0.5847(3) -0.4456(3) -0.2215(3) 0.120 Uiso 1 calc R . 
H25B H 0.6198(3) -0.5442(3) -0.1919(3) 0.120 Uiso 1 calc R . 
H25A H 0.6748(3) -0.4625(3) -0.1956(3) 0.120 Uiso 1 calc R . 
C26 C 0.5550(3) -0.4697(4) -0.0718(3) 0.090(2) Uani 1 d . . 
H26C H 0.5631(3) -0.4511(4) -0.0212(3) 0.135 Uiso 1 calc R . 
H26B H 0.5445(3) -0.5356(4) -0.0773(3) 0.135 Uiso 1 calc R . 
H26A H 0.5113(3) -0.4362(4) -0.1067(3) 0.135 Uiso 1 calc R . 
C27 C 0.7251(3) -0.5053(4) -0.0244(3) 0.088(2) Uani 1 d . . 
H27C H 0.7321(3) -0.4872(4) 0.0260(3) 0.131 Uiso 1 calc R . 
H27B H 0.7712(3) -0.4897(4) -0.0338(3) 0.131 Uiso 1 calc R . 
H27A H 0.7162(3) -0.5715(4) -0.0301(3) 0.131 Uiso 1 calc R . 
C28 C 0.5325(16) -0.0147(19) 0.5104(28) 0.182(12) Uiso 0.50 d P . 
C29 C 0.4418(22) -0.0046(25) 0.3895(21) 0.226(15) Uiso 0.50 d P . 
C30 C 0.4697(13) -0.0247(15) 0.3721(12) 0.144(8) Uiso 0.50 d P . 
C29A C 0.4974(39) -0.0117(28) 0.4599(28) 0.260(17) Uiso 0.50 d P . 
C30A C 0.4253(18) -0.0497(21) 0.4224(19) 0.230(13) Uiso 0.50 d P . 
  
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 0.041(4) 0.039(4) 0.051(4) 0.000(3) 0.015(3) -0.001(3) 
Li2 0.038(4) 0.030(4) 0.060(4) -0.001(3) 0.024(3) 0.000(3) 
Li3 0.052(4) 0.039(4) 0.049(4) 0.003(3) 0.026(4) 0.007(3) 
Si1 0.0375(6) 0.0329(6) 0.0396(6) -0.0014(5) 0.0174(5) -0.0007(5) 
Si2 0.0377(6) 0.0524(7) 0.0459(7) -0.0148(6) 0.0137(5) -0.0072(6) 
Si3 0.0345(6) 0.0407(6) 0.0363(6) -0.0092(5) 0.0113(5) -0.0032(5) 
Si4 0.0519(8) 0.0640(9) 0.0473(7) -0.0246(6) 0.0267(6) -0.0207(7) 
Si5 0.0456(7) 0.0621(8) 0.0305(6) -0.0087(6) 0.0110(5) 0.0083(6) 
Si6 0.0624(8) 0.0334(6) 0.0485(7) 0.0005(6) 0.0229(6) -0.0003(6) 
N1 0.029(2) 0.034(2) 0.031(2) -0.0007(14) 0.0107(14) -0.0029(14) 
N2 0.032(2) 0.034(2) 0.031(2) -0.0014(14) 0.0119(14) -0.0004(15) 
N3 0.033(2) 0.039(2) 0.032(2) -0.0041(15) 0.0127(14) -0.0027(15) 
N4 0.036(2) 0.042(2) 0.037(2) -0.006(2) 0.0167(15) -0.002(2) 
N5 0.032(2) 0.034(2) 0.032(2) -0.0037(14) 0.0128(14) 0.0006(14) 
N6 0.032(2) 0.030(2) 0.030(2) -0.0016(14) 0.0121(14) -0.0014(14) 
N7 0.029(2) 0.031(2) 0.032(2) -0.0038(14) 0.0117(14) 0.0003(14) 
N8 0.033(2) 0.038(2) 0.037(2) -0.008(2) 0.0112(15) -0.0034(15) 
N9 0.038(2) 0.041(2) 0.032(2) -0.004(2) 0.0117(15) 0.002(2) 
N10 0.034(2) 0.038(2) 0.026(2) 0.0003(14) 0.0101(13) 0.0015(15) 
N11 0.036(2) 0.034(2) 0.028(2) -0.0016(14) 0.0118(14) -0.0005(14) 
N12 0.040(2) 0.035(2) 0.032(2) -0.0019(14) 0.0133(15) 0.0034(15) 
C1 0.028(2) 0.036(2) 0.038(2) 0.008(2) 0.012(2) 0.001(2) 
C2 0.034(2) 0.045(2) 0.030(2) 0.000(2) 0.010(2) -0.002(2) 
C3 0.030(2) 0.049(3) 0.034(2) -0.001(2) 0.008(2) -0.001(2) 
C4 0.053(3) 0.061(3) 0.054(3) 0.006(2) 0.030(2) 0.007(2) 
C5 0.062(3) 0.055(3) 0.077(3) -0.019(3) 0.027(3) -0.011(3) 
C6 0.057(3) 0.056(3) 0.059(3) 0.014(2) 0.022(2) 0.023(2) 
C7 0.051(3) 0.082(4) 0.062(3) -0.036(3) 0.023(2) -0.018(3) 
C8 0.054(3) 0.067(3) 0.082(4) -0.016(3) 0.034(3) -0.015(3) 
C9 0.066(3) 0.083(4) 0.059(3) -0.008(3) -0.001(3) -0.005(3) 
C10 0.026(2) 0.035(2) 0.030(2) 0.003(2) 0.007(2) 0.000(2) 
C11 0.026(2) 0.035(2) 0.027(2) 0.002(2) 0.008(2) -0.002(2) 
C12 0.030(2) 0.041(2) 0.035(2) 0.000(2) 0.014(2) 0.001(2) 
C13 0.049(3) 0.111(5) 0.133(5) -0.077(4) 0.044(3) -0.037(3) 
C14 0.161(6) 0.132(6) 0.033(3) -0.010(3) 0.011(3) -0.083(5) 
C15 0.081(4) 0.050(3) 0.112(5) -0.019(3) 0.010(3) 0.004(3) 
C16 0.078(4) 0.068(3) 0.087(4) -0.041(3) 0.043(3) -0.021(3) 
C17 0.081(4) 0.093(4) 0.097(4) -0.055(3) 0.067(3) -0.040(3) 
C18 0.103(5) 0.130(5) 0.046(3) -0.004(3) 0.020(3) -0.023(4) 
C19 0.035(2) 0.045(2) 0.025(2) 0.008(2) 0.008(2) 0.007(2) 
C20 0.031(2) 0.041(2) 0.031(2) 0.003(2) 0.012(2) 0.002(2) 
C21 0.035(2) 0.040(2) 0.037(2) 0.010(2) 0.014(2) 0.006(2) 
C22 0.065(3) 0.144(6) 0.050(3) -0.012(3) 0.031(3) -0.010(4) 
C23 0.133(5) 0.079(4) 0.060(3) -0.022(3) 0.024(3) 0.028(4) 
C24 0.051(3) 0.115(5) 0.034(2) 0.002(3) 0.010(2) 0.005(3) 
C25 0.136(5) 0.042(3) 0.065(3) -0.012(3) 0.041(3) -0.001(3) 
C26 0.095(4) 0.070(4) 0.121(5) -0.027(3) 0.061(4) -0.037(3) 
C27 0.103(5) 0.063(4) 0.090(4) 0.018(3) 0.029(4) 0.029(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 N10 2.077(7) . ? 
Li1 N1 2.117(7) . ? 
Li1 N5 2.123(7) . ? 
Li1 N9 2.461(7) . ? 
Li2 N2 1.968(7) . ? 
Li2 N11 1.972(7) . ? 
Li2 N7 2.077(7) . ? 
Li2 N6 2.079(7) . ? 
Li2 C11 2.410(7) . ? 
Li3 N3 2.090(7) . ? 
Li3 N12 2.116(7) . ? 
Li3 N8 2.119(7) . ? 
Li3 N4 2.385(8) . ? 
Si1 N1 1.747(3) . ? 
Si1 C5 1.848(4) . ? 
Si1 C4 1.856(4) . ? 
Si1 C6 1.868(4) . ? 
Si2 N4 1.745(3) . ? 
Si2 C8 1.858(5) . ? 
Si2 C9 1.859(5) . ? 
Si2 C7 1.864(4) . ? 
Si3 N5 1.742(3) . ? 
Si3 C14 1.831(5) . ? 
Si3 C15 1.841(5) . ? 
Si3 C13 1.844(5) . ? 
Si4 N8 1.738(3) . ? 
Si4 C16 1.847(5) . ? 
Si4 C18 1.851(5) . ? 
Si4 C17 1.864(5) . ? 
Si5 N9 1.743(3) . ? 
Si5 C23 1.840(5) . ? 
Si5 C24 1.854(4) . ? 
Si5 C22 1.866(5) . ? 
Si6 N12 1.747(3) . ? 
Si6 C25 1.846(5) . ? 
Si6 C27 1.853(5) . ? 
Si6 C26 1.854(5) . ? 
N1 C1 1.281(4) . ? 
N2 C2 1.327(4) . ? 
N2 C1 1.371(4) . ? 
N3 C2 1.313(5) . ? 
N3 C3 1.377(4) . ? 
N4 C3 1.274(5) . ? 
N5 C10 1.280(4) . ? 
N6 C11 1.328(4) . ? 
N6 C10 1.358(4) . ? 
N7 C11 1.317(4) . ? 
N7 C12 1.365(4) . ? 
N8 C12 1.281(4) . ? 
N9 C19 1.272(5) . ? 
N10 C20 1.315(5) . ? 
N10 C19 1.367(4) . ? 
N11 C20 1.316(4) . ? 
N11 C21 1.363(5) . ? 
N12 C21 1.285(4) . ? 
C28 C29A 0.96(4) . ? 
C28 C29A 1.02(3) 3_656 ? 
C28 C28 1.22(5) 3_656 ? 
C28 C30A 1.57(5) 3_656 ? 
C28 C29 1.85(7) 3_656 ? 
C29 C30 0.78(4) . ? 
C29 C30A 1.05(4) . ? 
C29 C29A 1.38(6) . ? 
C29 C28 1.85(7) 3_656 ? 
C30 C30A 1.56(4) . ? 
C30 C29A 1.60(5) . ? 
C29A C28 1.02(3) 3_656 ? 
C29A C30A 1.39(6) . ? 
C29A C29A 1.57(8) 3_656 ? 
C30A C28 1.57(5) 3_656 ? 
  
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 
N10 Li1 N1 107.9(3) . . ? 
N10 Li1 N5 125.3(3) . . ? 
N1 Li1 N5 123.5(3) . . ? 
N10 Li1 N9 60.3(2) . . ? 
N1 Li1 N9 111.9(3) . . ? 
N5 Li1 N9 109.9(3) . . ? 
N2 Li2 N11 115.0(3) . . ? 
N2 Li2 N7 124.4(4) . . ? 
N11 Li2 N7 111.3(3) . . ? 
N2 Li2 N6 110.2(3) . . ? 
N11 Li2 N6 121.5(4) . . ? 
N7 Li2 N6 66.4(2) . . ? 
N2 Li2 C11 121.1(3) . . ? 
N11 Li2 C11 123.8(3) . . ? 
N7 Li2 C11 33.10(14) . . ? 
N6 Li2 C11 33.40(14) . . ? 
N3 Li3 N12 112.3(3) . . ? 
N3 Li3 N8 118.5(3) . . ? 
N12 Li3 N8 124.7(3) . . ? 
N3 Li3 N4 61.7(2) . . ? 
N12 Li3 N4 110.4(3) . . ? 
N8 Li3 N4 111.7(3) . . ? 
N1 Si1 C5 107.9(2) . . ? 
N1 Si1 C4 107.6(2) . . ? 
C5 Si1 C4 110.0(2) . . ? 
N1 Si1 C6 112.4(2) . . ? 
C5 Si1 C6 109.1(2) . . ? 
C4 Si1 C6 109.8(2) . . ? 
N4 Si2 C8 108.4(2) . . ? 
N4 Si2 C9 113.0(2) . . ? 
C8 Si2 C9 109.5(2) . . ? 
N4 Si2 C7 107.1(2) . . ? 
C8 Si2 C7 109.0(2) . . ? 
C9 Si2 C7 109.8(2) . . ? 
N5 Si3 C14 107.5(2) . . ? 
N5 Si3 C15 110.4(2) . . ? 
C14 Si3 C15 109.5(3) . . ? 
N5 Si3 C13 111.8(2) . . ? 
C14 Si3 C13 110.4(3) . . ? 
C15 Si3 C13 107.2(3) . . ? 
N8 Si4 C16 109.0(2) . . ? 
N8 Si4 C18 106.3(2) . . ? 
C16 Si4 C18 110.7(3) . . ? 
N8 Si4 C17 113.3(2) . . ? 
C16 Si4 C17 108.0(2) . . ? 
C18 Si4 C17 109.4(3) . . ? 
N9 Si5 C23 108.2(2) . . ? 
N9 Si5 C24 110.3(2) . . ? 
C23 Si5 C24 110.6(3) . . ? 
N9 Si5 C22 111.1(2) . . ? 
C23 Si5 C22 108.9(3) . . ? 
C24 Si5 C22 107.8(2) . . ? 
N12 Si6 C25 107.4(2) . . ? 
N12 Si6 C27 109.2(2) . . ? 
C25 Si6 C27 109.5(3) . . ? 
N12 Si6 C26 110.0(2) . . ? 
C25 Si6 C26 110.9(3) . . ? 
C27 Si6 C26 109.8(3) . . ? 
C1 N1 Si1 119.1(3) . . ? 
C1 N1 Li1 118.1(3) . . ? 
Si1 N1 Li1 121.4(2) . . ? 
C2 N2 C1 116.1(3) . . ? 
C2 N2 Li2 106.1(3) . . ? 
C1 N2 Li2 135.9(3) . . ? 
C2 N3 C3 116.3(3) . . ? 
C2 N3 Li3 149.4(3) . . ? 
C3 N3 Li3 93.7(3) . . ? 
C3 N4 Si2 122.2(3) . . ? 
C3 N4 Li3 83.6(3) . . ? 
Si2 N4 Li3 153.9(2) . . ? 
C10 N5 Si3 121.6(3) . . ? 
C10 N5 Li1 102.9(3) . . ? 
Si3 N5 Li1 135.5(2) . . ? 
C11 N6 C10 117.7(3) . . ? 
C11 N6 Li2 87.1(3) . . ? 
C10 N6 Li2 154.2(3) . . ? 
C11 N7 C12 117.8(3) . . ? 
C11 N7 Li2 87.5(3) . . ? 
C12 N7 Li2 152.4(3) . . ? 
C12 N8 Si4 122.7(3) . . ? 
C12 N8 Li3 102.6(3) . . ? 
Si4 N8 Li3 133.8(2) . . ? 
C19 N9 Si5 121.3(3) . . ? 
C19 N9 Li1 81.9(3) . . ? 
Si5 N9 Li1 156.8(2) . . ? 
C20 N10 C19 116.7(3) . . ? 
C20 N10 Li1 147.1(3) . . ? 
C19 N10 Li1 96.1(3) . . ? 
C20 N11 C21 117.0(3) . . ? 
C20 N11 Li2 110.3(3) . . ? 
C21 N11 Li2 132.7(3) . . ? 
C21 N12 Si6 117.7(3) . . ? 
C21 N12 Li3 119.5(3) . . ? 
Si6 N12 Li3 122.7(2) . . ? 
N1 C1 N2 123.5(3) . . ? 
N3 C2 N2 121.6(3) . . ? 
N4 C3 N3 121.1(4) . . ? 
N5 C10 N6 122.0(3) . . ? 
N7 C11 N6 118.7(3) . . ? 
N7 C11 Li2 59.4(2) . . ? 
N6 C11 Li2 59.5(2) . . ? 
N8 C12 N7 121.9(3) . . ? 
N9 C19 N10 121.6(3) . . ? 
N10 C20 N11 121.2(3) . . ? 
N12 C21 N11 124.2(3) . . ? 
C29A C28 C29A 104.5(48) . 3_656 ? 
C29A C28 C28 54.6(31) . 3_656 ? 
C29A C28 C28 49.9(27) 3_656 3_656 ? 
C29A C28 C30A 140.3(42) . 3_656 ? 
C29A C28 C30A 61.0(49) 3_656 3_656 ? 
C28 C28 C30A 101.5(48) 3_656 3_656 ? 
C29A C28 C29 152.1(60) . 3_656 ? 
C29A C28 C29 47.7(54) 3_656 3_656 ? 
C28 C28 C29 97.6(51) 3_656 3_656 ? 
C30A C28 C29 34.4(18) 3_656 3_656 ? 
C30 C29 C30A 115.8(53) . . ? 
C30 C29 C29A 91.2(43) . . ? 
C30A C29 C29A 68.4(32) . . ? 
C30 C29 C28 124.3(45) . 3_656 ? 
C30A C29 C28 57.8(27) . 3_656 ? 
C29A C29 C28 33.1(24) . 3_656 ? 
C29 C30 C30A 37.2(35) . . ? 
C29 C30 C29A 59.6(37) . . ? 
C30A C30 C29A 52.3(21) . . ? 
C28 C29A C28 75.5(48) . 3_656 ? 
C28 C29A C29 174.7(80) . . ? 
C28 C29A C29 99.2(73) 3_656 . ? 
C28 C29A C30A 132.9(53) . . ? 
C28 C29A C30A 79.0(51) 3_656 . ? 
C29 C29A C30A 44.2(25) . . ? 
C28 C29A C29A 39.2(26) . 3_656 ? 
C28 C29A C29A 36.3(25) 3_656 3_656 ? 
C29 C29A C29A 135.5(76) . 3_656 ? 
C30A C29A C29A 107.0(53) . 3_656 ? 
C28 C29A C30 156.1(79) . . ? 
C28 C29A C30 128.4(78) 3_656 . ? 
C29 C29A C30 29.2(20) . . ? 
C30A C29A C30 62.0(30) . . ? 
C29A C29A C30 164.7(78) 3_656 . ? 
C29 C30A C29A 67.4(29) . . ? 
C29 C30A C30 26.9(24) . . ? 
C29A C30A C30 65.6(23) . . ? 
C29 C30A C28 87.8(36) . 3_656 ? 
C29A C30A C28 39.9(17) . 3_656 ? 
C30 C30A C28 99.3(21) . 3_656 ? 
  
_refine_diff_density_max    0.287 
_refine_diff_density_min   -0.238 
_refine_diff_density_rms    0.053 

#===END

 
data_lappert-paper-structure-5
 
_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             '[Li2(thf){Me3SiNCHNCHNCH(SiMe3)2}2]'
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'C30 H68 Li2 N6 O Si6'
_chemical_formula_weight          711.32
_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'
 '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            monoclinic
_symmetry_space_group_name_H-M    P2/n
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x+1/2, -y, z+1/2'
 '-x, -y, -z'
 '-x-1/2, y, -z-1/2'
 
_cell_length_a                    13.022(3)
_cell_length_b                    8.134(4)
_cell_length_c                    22.607(6)
_cell_angle_alpha                 90.00
_cell_angle_beta                  106.43(2)
_cell_angle_gamma                 90.00
_cell_volume                      2296.8(14)
_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           0.30
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.029
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              776
_exptl_absorpt_coefficient_mu     0.209
_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             4220
_diffrn_reflns_av_R_equivalents   0.0347
_diffrn_reflns_av_sigmaI/netI     0.0900
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        0
_diffrn_reflns_limit_k_max        9
_diffrn_reflns_limit_l_min        -26
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          2.10
_diffrn_reflns_theta_max          24.97
_reflns_number_total              4041
_reflns_number_observed           2570
_reflns_observed_criterion        >2sigma(I)
 
_computing_data_collection        'Enraf-Nonius CAD4'
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 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^)+(0.0581P)^2^+0.7646P] 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          4041
_refine_ls_number_parameters      204
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1112
_refine_ls_R_factor_obs           0.0621
_refine_ls_wR_factor_all          0.1615
_refine_ls_wR_factor_obs          0.1361
_refine_ls_goodness_of_fit_all    1.044
_refine_ls_goodness_of_fit_obs    1.114
_refine_ls_restrained_S_all       1.044
_refine_ls_restrained_S_obs       1.114
_refine_ls_shift/esd_max          0.000
_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 0.2106(5) 0.3672(8) 0.2984(3) 0.037(2) Uani 1 d . .
Si1 Si 0.30770(9) 0.31759(15) 0.57226(5) 0.0395(3) Uani 1 d . .
Si2 Si 0.22372(10) 0.59723(15) 0.46477(5) 0.0399(3) Uani 1 d . .
Si3 Si 0.51613(9) 0.1418(2) 0.18686(5) 0.0416(3) Uani 1 d . .
O O 0.2500 0.5719(4) 0.2500 0.0381(9) Uani 1 d S .
N1 N 0.3163(2) 0.3379(4) 0.39262(12) 0.0322(7) Uani 1 d . .
N2 N 0.3651(2) 0.2789(4) 0.30607(12) 0.0292(7) Uani 1 d . .
N3 N 0.4265(2) 0.2269(4) 0.22244(12) 0.0307(7) Uani 1 d . .
C1 C 0.2867(3) 0.3949(5) 0.4925(2) 0.0321(9) Uani 1 d . .
C2 C 0.3289(3) 0.3037(5) 0.4552(2) 0.0336(9) Uani 1 d . .
H2 H 0.3699(3) 0.2099(5) 0.4725(2) 0.040 Uiso 1 calc R .
C3 C 0.3793(3) 0.2584(5) 0.3670(2) 0.0305(8) Uani 1 d . .
H3 H 0.4338(3) 0.1880(5) 0.3906(2) 0.037 Uiso 1 calc R .
C4 C 0.4366(3) 0.2102(4) 0.2806(2) 0.0305(8) Uani 1 d . .
H4 H 0.4949(3) 0.1490(4) 0.3057(2) 0.037 Uiso 1 calc R .
C5 C 0.3935(4) 0.1310(6) 0.5868(2) 0.0609(14) Uani 1 d . .
H5A H 0.4031(4) 0.0932(6) 0.6292(2) 0.091 Uiso 1 calc R .
H5B H 0.4635(4) 0.1573(6) 0.5810(2) 0.091 Uiso 1 calc R .
H5C H 0.3593(4) 0.0441(6) 0.5579(2) 0.091 Uiso 1 calc R .
C6 C 0.1771(4) 0.2634(7) 0.5853(2) 0.074(2) Uani 1 d . .
H6A H 0.1892(4) 0.2227(7) 0.6276(2) 0.111 Uiso 1 calc R .
H6B H 0.1421(4) 0.1777(7) 0.5561(2) 0.111 Uiso 1 calc R .
H6C H 0.1313(4) 0.3611(7) 0.5793(2) 0.111 Uiso 1 calc R .
C7 C 0.3749(4) 0.4735(6) 0.6304(2) 0.0645(14) Uani 1 d . .
H7A H 0.3848(4) 0.4290(6) 0.6719(2) 0.097 Uiso 1 calc R .
H7B H 0.3306(4) 0.5727(6) 0.6252(2) 0.097 Uiso 1 calc R .
H7C H 0.4448(4) 0.5011(6) 0.6248(2) 0.097 Uiso 1 calc R .
C8 C 0.1494(5) 0.6834(8) 0.5172(2) 0.093(2) Uani 1 d . .
H8A H 0.1972(5) 0.6888(8) 0.5593(2) 0.140 Uiso 1 calc R .
H8B H 0.0882(5) 0.6125(8) 0.5165(2) 0.140 Uiso 1 calc R .
H8C H 0.1238(5) 0.7941(8) 0.5034(2) 0.140 Uiso 1 calc R .
C9 C 0.3342(4) 0.7425(6) 0.4637(2) 0.0692(15) Uani 1 d . .
H9A H 0.3862(4) 0.7457(6) 0.5046(2) 0.104 Uiso 1 calc R .
H9B H 0.3046(4) 0.8527(6) 0.4526(2) 0.104 Uiso 1 calc R .
H9C H 0.3698(4) 0.7053(6) 0.4333(2) 0.104 Uiso 1 calc R .
C10 C 0.1261(3) 0.5928(5) 0.3869(2) 0.0528(12) Uani 1 d . .
H10A H 0.0971(3) 0.7034(5) 0.3760(2) 0.079 Uiso 1 calc R .
H10B H 0.0677(3) 0.5170(5) 0.3870(2) 0.079 Uiso 1 calc R .
H10C H 0.1622(3) 0.5557(5) 0.3567(2) 0.079 Uiso 1 calc R .
C11 C 0.5837(4) -0.0424(7) 0.2296(2) 0.071(2) Uani 1 d . .
H11A H 0.5298(4) -0.1255(7) 0.2309(2) 0.107 Uiso 1 calc R .
H11B H 0.6230(4) -0.0108(7) 0.2717(2) 0.107 Uiso 1 calc R .
H11C H 0.6337(4) -0.0879(7) 0.2086(2) 0.107 Uiso 1 calc R .
C12 C 0.4386(4) 0.0840(6) 0.1075(2) 0.0551(13) Uani 1 d . .
H12A H 0.3848(4) 0.0015(6) 0.1093(2) 0.083 Uiso 1 calc R .
H12B H 0.4872(4) 0.0383(6) 0.0855(2) 0.083 Uiso 1 calc R .
H12C H 0.4030(4) 0.1816(6) 0.0856(2) 0.083 Uiso 1 calc R .
C13 C 0.6186(4) 0.2978(7) 0.1847(2) 0.070(2) Uani 1 d . .
H13A H 0.6589(4) 0.3271(7) 0.2270(2) 0.104 Uiso 1 calc R .
H13B H 0.5834(4) 0.3960(7) 0.1631(2) 0.104 Uiso 1 calc R .
H13C H 0.6676(4) 0.2527(7) 0.1630(2) 0.104 Uiso 1 calc R .
C14 C 0.1652(4) 0.6746(6) 0.2142(2) 0.0580(13) Uani 1 d . .
H14A H 0.1029(4) 0.6723(6) 0.2311(2) 0.070 Uiso 1 calc R .
H14B H 0.1418(4) 0.6376(6) 0.1707(2) 0.070 Uiso 1 calc R .
C15 C 0.2125(6) 0.8445(6) 0.2189(2) 0.101(2) Uani 1 d . .
H15A H 0.2502(6) 0.8626(6) 0.1871(2) 0.122 Uiso 1 calc R .
H15B H 0.1566(6) 0.9298(6) 0.2147(2) 0.122 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 0.039(4) 0.035(4) 0.041(3) 0.003(3) 0.017(3) 0.006(3)
Si1 0.0494(7) 0.0479(7) 0.0262(5) -0.0006(5) 0.0186(5) -0.0035(6)
Si2 0.0525(7) 0.0395(7) 0.0317(6) -0.0046(5) 0.0184(5) 0.0064(6)
Si3 0.0428(7) 0.0607(8) 0.0266(5) 0.0044(5) 0.0183(5) 0.0113(6)
O 0.046(2) 0.028(2) 0.040(2) 0.000 0.011(2) 0.000
N1 0.039(2) 0.033(2) 0.028(2) -0.0018(14) 0.0162(14) 0.002(2)
N2 0.036(2) 0.030(2) 0.025(2) 0.0009(13) 0.0137(13) 0.0029(15)
N3 0.039(2) 0.033(2) 0.024(2) 0.0014(13) 0.0159(13) 0.0011(15)
C1 0.037(2) 0.036(2) 0.027(2) -0.004(2) 0.015(2) -0.001(2)
C2 0.037(2) 0.036(2) 0.028(2) 0.002(2) 0.012(2) -0.001(2)
C3 0.037(2) 0.029(2) 0.028(2) 0.001(2) 0.012(2) 0.001(2)
C4 0.035(2) 0.028(2) 0.030(2) 0.002(2) 0.012(2) 0.000(2)
C5 0.087(4) 0.061(3) 0.036(2) 0.013(2) 0.021(2) 0.011(3)
C6 0.068(3) 0.108(5) 0.054(3) 0.012(3) 0.031(3) -0.016(3)
C7 0.069(3) 0.072(4) 0.044(3) -0.018(3) 0.004(2) 0.006(3)
C8 0.129(5) 0.110(5) 0.057(3) 0.012(3) 0.053(3) 0.061(4)
C9 0.081(4) 0.042(3) 0.075(3) -0.006(3) 0.007(3) -0.011(3)
C10 0.062(3) 0.040(3) 0.053(3) -0.002(2) 0.011(2) 0.011(2)
C11 0.087(4) 0.091(4) 0.047(3) 0.017(3) 0.036(3) 0.049(3)
C12 0.065(3) 0.069(3) 0.034(2) -0.008(2) 0.019(2) 0.016(3)
C13 0.044(3) 0.114(5) 0.055(3) 0.013(3) 0.020(2) -0.008(3)
C14 0.079(3) 0.050(3) 0.050(3) 0.013(2) 0.026(2) 0.027(3)
C15 0.200(8) 0.035(3) 0.087(4) 0.015(3) 0.070(5) 0.024(4)
 
_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 N3 2.058(7) 4_656 ?
Li N2 2.096(7) . ?
Li O 2.133(7) . ?
Li N1 2.197(7) . ?
Li N2 2.398(7) 4_656 ?
Li C3 2.467(7) . ?
Li C4 2.561(8) 4_656 ?
Li Li 2.668(12) 4_656 ?
Si1 C1 1.854(4) . ?
Si1 C7 1.858(4) . ?
Si1 C5 1.858(5) . ?
Si1 C6 1.859(5) . ?
Si2 C10 1.857(4) . ?
Si2 C1 1.867(4) . ?
Si2 C9 1.867(5) . ?
Si2 C8 1.866(4) . ?
Si3 N3 1.738(3) . ?
Si3 C13 1.851(5) . ?
Si3 C12 1.854(4) . ?
Si3 C11 1.863(5) . ?
O C14 1.438(5) . ?
O C14 1.438(5) 4_656 ?
O Li 2.133(7) 4_656 ?
N1 C3 1.303(4) . ?
N1 C2 1.406(4) . ?
N2 C3 1.346(4) . ?
N2 C4 1.346(4) . ?
N2 Li 2.398(7) 4_656 ?
N3 C4 1.292(4) . ?
N3 Li 2.058(7) 4_656 ?
C1 C2 1.351(5) . ?
C4 Li 2.561(8) 4_656 ?
C14 C15 1.504(7) . ?
C15 C15 1.469(11) 4_656 ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N3 Li N2 125.4(3) 4_656 . ?
N3 Li O 129.4(3) 4_656 . ?
N2 Li O 86.9(2) . . ?
N3 Li N1 115.3(3) 4_656 . ?
N2 Li N1 63.9(2) . . ?
O Li N1 114.0(3) . . ?
N3 Li N2 61.3(2) 4_656 4_656 ?
N2 Li N2 95.5(3) . 4_656 ?
O Li N2 79.6(2) . 4_656 ?
N1 Li N2 153.2(3) . 4_656 ?
N3 Li C3 120.4(3) 4_656 . ?
N2 Li C3 33.07(14) . . ?
O Li C3 107.5(3) . . ?
N1 Li C3 31.79(13) . . ?
N2 Li C3 123.8(3) 4_656 . ?
N3 Li C4 30.03(13) 4_656 4_656 ?
N2 Li C4 113.4(3) . 4_656 ?
O Li C4 105.8(3) . 4_656 ?
N1 Li C4 139.6(3) . 4_656 ?
N2 Li C4 31.28(12) 4_656 4_656 ?
C3 Li C4 128.1(3) . 4_656 ?
N3 Li Li 108.8(3) 4_656 4_656 ?
N2 Li Li 59.0(2) . 4_656 ?
O Li Li 51.3(2) . 4_656 ?
N1 Li Li 121.0(4) . 4_656 ?
N2 Li Li 48.5(2) 4_656 4_656 ?
C3 Li Li 92.0(3) . 4_656 ?
C4 Li Li 79.2(3) 4_656 4_656 ?
C1 Si1 C7 111.5(2) . . ?
C1 Si1 C5 111.4(2) . . ?
C7 Si1 C5 107.0(2) . . ?
C1 Si1 C6 110.2(2) . . ?
C7 Si1 C6 108.6(2) . . ?
C5 Si1 C6 108.0(2) . . ?
C10 Si2 C1 114.8(2) . . ?
C10 Si2 C9 108.9(2) . . ?
C1 Si2 C9 107.2(2) . . ?
C10 Si2 C8 105.7(2) . . ?
C1 Si2 C8 112.0(2) . . ?
C9 Si2 C8 108.1(3) . . ?
N3 Si3 C13 108.8(2) . . ?
N3 Si3 C12 107.2(2) . . ?
C13 Si3 C12 110.3(2) . . ?
N3 Si3 C11 111.1(2) . . ?
C13 Si3 C11 109.1(2) . . ?
C12 Si3 C11 110.2(2) . . ?
C14 O C14 108.9(5) . 4_656 ?
C14 O Li 119.0(3) . . ?
C14 O Li 115.0(3) 4_656 . ?
C14 O Li 115.0(3) . 4_656 ?
C14 O Li 119.0(3) 4_656 4_656 ?
Li O Li 77.4(4) . 4_656 ?
C3 N1 C2 116.2(3) . . ?
C3 N1 Li 85.6(3) . . ?
C2 N1 Li 149.3(3) . . ?
C3 N2 C4 118.3(3) . . ?
C3 N2 Li 88.8(3) . . ?
C4 N2 Li 150.5(3) . . ?
C3 N2 Li 160.7(3) . 4_656 ?
C4 N2 Li 81.1(2) . 4_656 ?
Li N2 Li 72.5(3) . 4_656 ?
C4 N3 Si3 122.8(3) . . ?
C4 N3 Li 97.1(3) . 4_656 ?
Si3 N3 Li 140.1(2) . 4_656 ?
C2 C1 Si1 116.5(3) . . ?
C2 C1 Si2 119.4(3) . . ?
Si1 C1 Si2 123.8(2) . . ?
C1 C2 N1 124.6(4) . . ?
N1 C3 N2 118.2(3) . . ?
N1 C3 Li 62.6(2) . . ?
N2 C3 Li 58.2(2) . . ?
N3 C4 N2 120.5(3) . . ?
N3 C4 Li 52.9(2) . 4_656 ?
N2 C4 Li 67.7(2) . 4_656 ?
O C14 C15 105.1(4) . . ?
C15 C15 C14 102.5(3) 4_656 . ?
 
_refine_diff_density_max    0.303
_refine_diff_density_min   -0.270
_refine_diff_density_rms    0.058

#===END


data_lappert-paper-structure-6
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C22 H53 Li N6 Si3' 
_chemical_formula_weight          492.91 
_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' 
 'Li'  'Li'  -0.0003   0.0001 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            orthorhombic 
_symmetry_space_group_name_H-M    Pnma 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x+1/2, -y+1/2, -z+1/2' 
 '-x, y+1/2, -z' 
 '-x+1/2, -y, z+1/2' 
 '-x, -y, -z' 
 '-x-1/2, y-1/2, z-1/2' 
 'x, -y-1/2, z' 
 'x-1/2, y, -z-1/2' 
  
_cell_length_a                    28.389(5) 
_cell_length_b                    11.343(2) 
_cell_length_c                    10.290(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3313.5(10) 
_cell_formula_units_Z             4 
_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           0.30 
_exptl_crystal_size_min           0.20 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     0.988 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1088 
_exptl_absorpt_coefficient_mu     0.161 
_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        ' 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             4037 
_diffrn_reflns_av_R_equivalents   0.0907 
_diffrn_reflns_av_sigmaI/netI     0.1032 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        29 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          2.11 
_diffrn_reflns_theta_max          22.04 
_reflns_number_total              2149 
_reflns_number_observed           1400 
_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 
; 
 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^)+(0.0680P)^2^+1.5806P] 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     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2148 
_refine_ls_number_parameters      169 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1059 
_refine_ls_R_factor_obs           0.0605 
_refine_ls_wR_factor_all          0.1575 
_refine_ls_wR_factor_obs          0.1362 
_refine_ls_goodness_of_fit_all    1.025 
_refine_ls_goodness_of_fit_obs    1.122 
_refine_ls_restrained_S_all       1.028 
_refine_ls_restrained_S_obs       1.122 
_refine_ls_shift/esd_max          0.000 
_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 0.3066(3) 0.2500 -0.2381(9) 0.034(2) Uani 1 d S . 
Si1 Si 0.40273(6) 0.2500 0.0066(2) 0.0373(5) Uani 1 d S . 
Si2 Si 0.06046(6) 0.2500 0.1694(2) 0.0448(6) Uani 1 d S . 
Si3 Si 0.08512(6) 0.2500 -0.1426(2) 0.0454(6) Uani 1 d S . 
N1 N 0.3474(2) 0.2500 -0.0637(4) 0.0312(12) Uani 1 d S . 
N2 N 0.2666(2) 0.2500 -0.0611(4) 0.0261(11) Uani 1 d S . 
N3 N 0.1854(2) 0.2500 -0.0316(4) 0.0305(12) Uani 1 d S . 
N4 N 0.2836(2) 0.0851(3) -0.3095(4) 0.0578(12) Uani 1 d . . 
N5 N 0.3484(2) 0.2500 -0.4203(5) 0.0425(14) Uani 1 d S . 
C1 C 0.3084(2) 0.2500 0.0004(6) 0.0303(14) Uani 1 d S . 
H1 H 0.3092(2) 0.2500 0.0927(6) 0.036 Uiso 1 calc SR . 
C2 C 0.2281(2) 0.2500 0.0133(6) 0.0262(14) Uani 1 d S . 
H2 H 0.2322(2) 0.2500 0.1050(6) 0.031 Uiso 1 calc SR . 
C3 C 0.1491(2) 0.2500 0.0589(6) 0.034(2) Uani 1 d S . 
H3 H 0.1578(2) 0.2500 0.1480(6) 0.041 Uiso 1 calc SR . 
C4 C 0.1025(2) 0.2500 0.0321(6) 0.037(2) Uani 1 d S . 
C5 C 0.4348(2) 0.1164(5) -0.0465(5) 0.0557(14) Uani 1 d . . 
H5C H 0.4176(2) 0.0461(5) -0.0181(5) 0.084 Uiso 1 calc R . 
H5B H 0.4664(2) 0.1162(5) -0.0081(5) 0.084 Uiso 1 calc R . 
H5A H 0.4374(2) 0.1162(5) -0.1415(5) 0.084 Uiso 1 calc R . 
C6 C 0.3992(2) 0.2500 0.1874(6) 0.052(2) Uani 1 d S . 
H6C H 0.3823(2) 0.1796 0.2167(6) 0.077 Uiso 0.50 calc PR . 
H6B H 0.3824(2) 0.3207 0.2167(6) 0.077 Uiso 0.50 calc PR . 
H6A H 0.4311(2) 0.2498 0.2239(6) 0.077 Uiso 1 calc SR . 
C7 C 0.0908(2) 0.2500 0.3298(7) 0.067(2) Uani 1 d S . 
H7C H 0.0673(2) 0.2500 0.3995(7) 0.101 Uiso 1 calc SR . 
H7B H 0.1106(2) 0.3205 0.3372(7) 0.101 Uiso 0.50 calc PR . 
H7A H 0.1106(2) 0.1795 0.3372(7) 0.101 Uiso 0.50 calc PR . 
C8 C 0.0223(2) 0.1157(4) 0.1648(5) 0.063(2) Uani 1 d . . 
H8C H 0.0004(2) 0.1174(4) 0.2383(5) 0.095 Uiso 1 calc R . 
H8B H 0.0421(2) 0.0451(4) 0.1707(5) 0.095 Uiso 1 calc R . 
H8A H 0.0046(2) 0.1143(4) 0.0832(5) 0.095 Uiso 1 calc R . 
C9 C 0.0196(2) 0.2500 -0.1620(7) 0.068(2) Uani 1 d S . 
H9C H 0.0064(2) 0.3199 -0.1196(7) 0.102 Uiso 0.50 calc PR . 
H9B H 0.0065(2) 0.1789 -0.1218(7) 0.102 Uiso 0.50 calc PR . 
H9A H 0.0117(2) 0.2512 -0.2546(7) 0.102 Uiso 1 calc SR . 
C10 C 0.1064(2) 0.1148(5) -0.2257(6) 0.093(2) Uani 1 d . . 
H10C H 0.0946(2) 0.0451(5) -0.1798(6) 0.139 Uiso 1 calc R . 
H10B H 0.1409(2) 0.1140(5) -0.2258(6) 0.139 Uiso 1 calc R . 
H10A H 0.0949(2) 0.1140(5) -0.3155(6) 0.139 Uiso 1 calc R . 
C11 C 0.3324(3) 0.1467(6) -0.4868(6) 0.125(3) Uani 1 d . . 
H11B H 0.3153(3) 0.1748(6) -0.5646(6) 0.149 Uiso 1 calc R . 
H11A H 0.3611(3) 0.1063(6) -0.5190(6) 0.149 Uiso 1 calc R . 
C12 C 0.3061(3) 0.0648(6) -0.4348(6) 0.111(3) Uani 1 d . . 
H12B H 0.3258(3) -0.0069(6) -0.4262(6) 0.133 Uiso 1 calc R . 
H12A H 0.2809(3) 0.0461(6) -0.4979(6) 0.133 Uiso 1 calc R . 
C13 C 0.3985(3) 0.2500 -0.4079(9) 0.133(5) Uani 1 d S . 
H13C H 0.4085(3) 0.3215 -0.3622(9) 0.199 Uiso 0.50 calc PR . 
H13B H 0.4129(3) 0.2481 -0.4944(9) 0.199 Uiso 1 calc SR . 
H13A H 0.4084(3) 0.1805 -0.3584(9) 0.199 Uiso 0.50 calc PR . 
C14 C 0.2348(2) 0.0771(6) -0.3192(6) 0.106(3) Uani 1 d . . 
H14C H 0.2206(2) 0.0910(6) -0.2338(6) 0.158 Uiso 1 calc R . 
H14B H 0.2261(2) -0.0018(6) -0.3499(6) 0.158 Uiso 1 calc R . 
H14A H 0.2233(2) 0.1363(6) -0.3809(6) 0.158 Uiso 1 calc R . 
C15 C 0.3012(3) 0.0001(5) -0.2122(6) 0.108(2) Uani 1 d . . 
H15C H 0.3356(3) 0.0064(5) -0.2061(6) 0.162 Uiso 1 calc R . 
H15B H 0.2926(3) -0.0800(5) -0.2386(6) 0.162 Uiso 1 calc R . 
H15A H 0.2871(3) 0.0177(5) -0.1274(6) 0.162 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 0.038(6) 0.033(6) 0.029(6) 0.000 0.005(5) 0.000 
Si1 0.0289(10) 0.0532(12) 0.0297(10) 0.000 0.0014(8) 0.000 
Si2 0.0312(10) 0.0427(12) 0.0603(14) 0.000 0.0092(9) 0.000 
Si3 0.0340(10) 0.0507(12) 0.0515(13) 0.000 -0.0070(9) 0.000 
N1 0.032(3) 0.039(3) 0.022(3) 0.000 0.002(2) 0.000 
N2 0.024(3) 0.027(3) 0.027(3) 0.000 0.004(2) 0.000 
N3 0.028(3) 0.032(3) 0.032(3) 0.000 0.002(2) 0.000 
N4 0.089(3) 0.042(3) 0.042(3) -0.014(2) 0.028(2) -0.019(2) 
N5 0.041(3) 0.053(4) 0.033(3) 0.000 0.007(3) 0.000 
C1 0.035(4) 0.032(4) 0.024(3) 0.000 0.000(3) 0.000 
C2 0.031(4) 0.022(3) 0.026(3) 0.000 0.001(3) 0.000 
C3 0.040(4) 0.026(4) 0.036(4) 0.000 0.004(3) 0.000 
C4 0.022(3) 0.031(4) 0.056(5) 0.000 -0.002(3) 0.000 
C5 0.046(3) 0.070(4) 0.051(3) 0.003(3) 0.006(2) 0.013(3) 
C6 0.040(4) 0.082(5) 0.033(4) 0.000 -0.001(3) 0.000 
C7 0.052(4) 0.089(6) 0.061(5) 0.000 0.019(4) 0.000 
C8 0.049(3) 0.049(3) 0.092(4) 0.009(3) 0.018(3) -0.002(3) 
C9 0.040(4) 0.094(6) 0.070(6) 0.000 -0.019(4) 0.000 
C10 0.074(4) 0.116(5) 0.088(5) -0.052(4) -0.031(4) 0.034(4) 
C11 0.206(8) 0.103(6) 0.065(4) -0.043(4) 0.078(5) -0.070(6) 
C12 0.190(8) 0.064(4) 0.078(4) -0.039(4) 0.077(5) -0.051(5) 
C13 0.042(5) 0.293(16) 0.063(6) 0.000 0.012(5) 0.000 
C14 0.099(5) 0.111(6) 0.106(6) -0.056(5) 0.007(4) -0.047(4) 
C15 0.186(8) 0.047(4) 0.091(5) -0.019(4) -0.003(5) 0.020(5) 
  
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
  
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Li N4 2.113(6) . ? 
Li N4 2.113(6) 7_565 ? 
Li N1 2.135(11) . ? 
Li N2 2.147(10) . ? 
Li N5 2.219(11) . ? 
Li C1 2.454(11) . ? 
Si1 N1 1.730(5) . ? 
Si1 C5 1.850(5) 7_565 ? 
Si1 C5 1.850(5) . ? 
Si1 C6 1.863(6) . ? 
Si2 C4 1.849(6) . ? 
Si2 C7 1.862(7) . ? 
Si2 C8 1.869(5) . ? 
Si2 C8 1.869(5) 7_565 ? 
Si3 C10 1.857(5) . ? 
Si3 C10 1.857(5) 7_565 ? 
Si3 C4 1.864(6) . ? 
Si3 C9 1.870(6) . ? 
N1 C1 1.287(7) . ? 
N2 C2 1.335(7) . ? 
N2 C1 1.346(7) . ? 
N3 C2 1.296(7) . ? 
N3 C3 1.390(7) . ? 
N4 C14 1.395(7) . ? 
N4 C12 1.457(6) . ? 
N4 C15 1.476(7) . ? 
N5 C13 1.427(9) . ? 
N5 C11 1.431(6) . ? 
N5 C11 1.431(6) 7_565 ? 
C3 C4 1.351(8) . ? 
C11 C12 1.307(7) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N4 Li N4 124.6(5) . 7_565 ? 
N4 Li N1 117.3(3) . . ? 
N4 Li N1 117.3(3) 7_565 . ? 
N4 Li N2 97.6(3) . . ? 
N4 Li N2 97.6(3) 7_565 . ? 
N1 Li N2 64.8(3) . . ? 
N4 Li N5 82.6(3) . . ? 
N4 Li N5 82.6(3) 7_565 . ? 
N1 Li N5 114.9(5) . . ? 
N2 Li N5 179.6(5) . . ? 
N4 Li C1 110.7(3) . . ? 
N4 Li C1 110.7(3) 7_565 . ? 
N1 Li C1 31.6(2) . . ? 
N2 Li C1 33.2(2) . . ? 
N5 Li C1 146.5(5) . . ? 
N1 Si1 C5 108.9(2) . 7_565 ? 
N1 Si1 C5 108.9(2) . . ? 
C5 Si1 C5 109.9(3) 7_565 . ? 
N1 Si1 C6 111.6(3) . . ? 
C5 Si1 C6 108.7(2) 7_565 . ? 
C5 Si1 C6 108.7(2) . . ? 
C4 Si2 C7 112.3(3) . . ? 
C4 Si2 C8 110.8(2) . . ? 
C7 Si2 C8 106.9(2) . . ? 
C4 Si2 C8 110.8(2) . 7_565 ? 
C7 Si2 C8 106.9(2) . 7_565 ? 
C8 Si2 C8 109.1(3) . 7_565 ? 
C10 Si3 C10 111.3(4) . 7_565 ? 
C10 Si3 C4 111.0(2) . . ? 
C10 Si3 C4 111.0(2) 7_565 . ? 
C10 Si3 C9 105.9(2) . . ? 
C10 Si3 C9 105.9(2) 7_565 . ? 
C4 Si3 C9 111.5(3) . . ? 
C1 N1 Si1 124.5(4) . . ? 
C1 N1 Li 88.0(4) . . ? 
Si1 N1 Li 147.5(4) . . ? 
C2 N2 C1 117.0(5) . . ? 
C2 N2 Li 157.0(5) . . ? 
C1 N2 Li 86.1(4) . . ? 
C2 N3 C3 117.0(5) . . ? 
C14 N4 C12 111.2(5) . . ? 
C14 N4 C15 110.1(5) . . ? 
C12 N4 C15 110.4(5) . . ? 
C14 N4 Li 112.9(4) . . ? 
C12 N4 Li 108.2(4) . . ? 
C15 N4 Li 103.8(4) . . ? 
C13 N5 C11 111.0(5) . . ? 
C13 N5 C11 111.0(5) . 7_565 ? 
C11 N5 C11 110.0(8) . 7_565 ? 
C13 N5 Li 117.2(5) . . ? 
C11 N5 Li 103.5(4) . . ? 
C11 N5 Li 103.5(4) 7_565 . ? 
N1 C1 N2 121.1(5) . . ? 
N1 C1 Li 60.4(4) . . ? 
N2 C1 Li 60.8(4) . . ? 
N3 C2 N2 124.1(5) . . ? 
C4 C3 N3 126.2(6) . . ? 
C3 C4 Si2 118.4(5) . . ? 
C3 C4 Si3 117.1(5) . . ? 
Si2 C4 Si3 124.5(3) . . ? 
C12 C11 N5 124.6(5) . . ? 
C11 C12 N4 120.1(5) . . ? 
  
_refine_diff_density_max    0.369 
_refine_diff_density_min   -0.386 
_refine_diff_density_rms    0.088 

#===END


data_lappert-paper-structure-7 
  
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C40 H88 Li4 N12 Si8' 
_chemical_formula_weight          989.70 
_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' 
 '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                    10.047(3) 
_cell_length_b                    12.148(4) 
_cell_length_c                    13.646(3) 
_cell_angle_alpha                 82.42(2) 
_cell_angle_beta                  76.68(2) 
_cell_angle_gamma                 76.74(2) 
_cell_volume                      1572.0(8) 
_cell_formula_units_Z             1 
_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           0.20 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.045 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              536 
_exptl_absorpt_coefficient_mu     0.206 
_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        ' 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             5516 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0663 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.13 
_diffrn_reflns_theta_max          24.97 
_reflns_number_total              5516 
_reflns_number_observed           4010 
_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 
; 
 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^)+(0.0561P)^2^+0.2181P] 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     riding 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5516 
_refine_ls_number_parameters      289 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0769 
_refine_ls_R_factor_obs           0.0481 
_refine_ls_wR_factor_all          0.1242 
_refine_ls_wR_factor_obs          0.1088 
_refine_ls_goodness_of_fit_all    1.030 
_refine_ls_goodness_of_fit_obs    1.067 
_refine_ls_restrained_S_all       1.030 
_refine_ls_restrained_S_obs       1.067 
_refine_ls_shift/esd_max          0.000 
_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 0.0702(5) 0.0311(4) -0.0957(3) 0.0370(11) Uani 1 d . . 
Li2 Li 0.1056(5) 0.1433(4) 0.0829(3) 0.0319(10) Uani 1 d . . 
Si1 Si 0.20063(8) 0.09924(7) -0.35363(5) 0.0274(2) Uani 1 d . . 
Si2 Si 0.27017(9) 0.51099(7) 0.21807(6) 0.0346(2) Uani 1 d . . 
Si3 Si -0.34719(8) 0.00234(7) -0.20992(5) 0.0285(2) Uani 1 d . . 
Si4 Si -0.19820(8) 0.35631(7) 0.35889(6) 0.0320(2) Uani 1 d . . 
N1 N 0.1673(2) 0.1074(2) -0.22400(15) 0.0260(5) Uani 1 d . . 
N2 N 0.1728(2) 0.1885(2) -0.08120(15) 0.0261(5) Uani 1 d . . 
N3 N 0.1910(2) 0.2829(2) 0.0477(2) 0.0301(5) Uani 1 d . . 
N4 N -0.2238(2) 0.0017(2) -0.13723(15) 0.0263(5) Uani 1 d . . 
N5 N -0.1419(2) 0.0845(2) -0.02444(15) 0.0253(5) Uani 1 d . . 
N6 N -0.1110(2) 0.1671(2) 0.10927(15) 0.0254(5) Uani 1 d . . 
C1 C 0.1991(3) 0.1850(2) -0.1828(2) 0.0264(6) Uani 1 d . . 
H1 H 0.2423(3) 0.2413(2) -0.2250(2) 0.032 Uiso 1 calc R . 
C2 C 0.2133(3) 0.2729(2) -0.0485(2) 0.0297(6) Uani 1 d . . 
H2 H 0.2580(3) 0.3248(2) -0.0956(2) 0.036 Uiso 1 calc R . 
C3 C 0.2357(3) 0.3717(2) 0.0778(2) 0.0321(6) Uani 1 d . . 
H3 H 0.2861(3) 0.4165(2) 0.0267(2) 0.039 Uiso 1 calc R . 
C4 C 0.2130(3) 0.3975(2) 0.1717(2) 0.0362(7) Uani 1 d . . 
H4 H 0.1610(3) 0.3524(2) 0.2213(2) 0.043 Uiso 1 calc R . 
C5 C 0.0375(3) 0.0797(3) -0.3848(2) 0.0422(8) Uani 1 d . . 
H5A H -0.0372(3) 0.1460(3) -0.3674(2) 0.063 Uiso 1 calc R . 
H5B H 0.0102(3) 0.0115(3) -0.3462(2) 0.063 Uiso 1 calc R . 
H5C H 0.0535(3) 0.0711(3) -0.4573(2) 0.063 Uiso 1 calc R . 
C6 C 0.2540(3) 0.2289(3) -0.4273(2) 0.0378(7) Uani 1 d . . 
H6A H 0.3400(3) 0.2389(3) -0.4105(2) 0.057 Uiso 1 calc R . 
H6B H 0.1795(3) 0.2955(3) -0.4101(2) 0.057 Uiso 1 calc R . 
H6C H 0.2704(3) 0.2203(3) -0.4997(2) 0.057 Uiso 1 calc R . 
C7 C 0.3434(3) -0.0259(3) -0.3862(2) 0.0398(7) Uani 1 d . . 
H7A H 0.4290(3) -0.0149(3) -0.3695(2) 0.060 Uiso 1 calc R . 
H7B H 0.3599(3) -0.0347(3) -0.4586(2) 0.060 Uiso 1 calc R . 
H7C H 0.3166(3) -0.0942(3) -0.3476(2) 0.060 Uiso 1 calc R . 
C8 C 0.1236(4) 0.6358(3) 0.2435(3) 0.0713(12) Uani 1 d . . 
H8A H 0.1563(4) 0.6950(3) 0.2681(3) 0.107 Uiso 1 calc R . 
H8B H 0.0469(4) 0.6128(3) 0.2948(3) 0.107 Uiso 1 calc R . 
H8C H 0.0905(4) 0.6653(3) 0.1811(3) 0.107 Uiso 1 calc R . 
C9 C 0.3323(4) 0.4542(4) 0.3369(3) 0.0650(11) Uani 1 d . . 
H9A H 0.3631(4) 0.5136(4) 0.3627(3) 0.097 Uiso 1 calc R . 
H9B H 0.4106(4) 0.3894(4) 0.3232(3) 0.097 Uiso 1 calc R . 
H9C H 0.2558(4) 0.4297(4) 0.3874(3) 0.097 Uiso 1 calc R . 
C10 C 0.4163(4) 0.5588(3) 0.1239(2) 0.0504(9) Uani 1 d . . 
H10A H 0.4448(4) 0.6191(3) 0.1502(2) 0.076 Uiso 1 calc R . 
H10B H 0.3854(4) 0.5878(3) 0.0606(2) 0.076 Uiso 1 calc R . 
H10C H 0.4958(4) 0.4946(3) 0.1113(2) 0.076 Uiso 1 calc R . 
C11 C -0.2325(3) 0.0850(2) -0.0858(2) 0.0262(6) Uani 1 d . . 
H11 H -0.3050(3) 0.1500(2) -0.0905(2) 0.031 Uiso 1 calc R . 
C12 C -0.1810(3) 0.1665(2) 0.0399(2) 0.0260(6) Uani 1 d . . 
H12 H -0.2608(3) 0.2248(2) 0.0348(2) 0.031 Uiso 1 calc R . 
C13 C -0.1673(3) 0.2504(2) 0.1784(2) 0.0289(6) Uani 1 d . . 
H13 H -0.2408(3) 0.3104(2) 0.1633(2) 0.035 Uiso 1 calc R . 
C14 C -0.1241(3) 0.2506(2) 0.2635(2) 0.0307(6) Uani 1 d . . 
H14 H -0.0487(3) 0.1914(2) 0.2767(2) 0.037 Uiso 1 calc R . 
C15 C -0.4910(3) -0.0618(3) -0.1303(2) 0.0431(8) Uani 1 d . . 
H15A H -0.5377(3) -0.0157(3) -0.0736(2) 0.065 Uiso 1 calc R . 
H15B H -0.4526(3) -0.1389(3) -0.1044(2) 0.065 Uiso 1 calc R . 
H15C H -0.5586(3) -0.0647(3) -0.1710(2) 0.065 Uiso 1 calc R . 
C16 C -0.4176(3) 0.1497(3) -0.2587(2) 0.0472(8) Uani 1 d . . 
H16A H -0.4642(3) 0.1956(3) -0.2017(2) 0.071 Uiso 1 calc R . 
H16B H -0.4850(3) 0.1481(3) -0.3000(2) 0.071 Uiso 1 calc R . 
H16C H -0.3407(3) 0.1830(3) -0.3000(2) 0.071 Uiso 1 calc R . 
C17 C -0.2593(3) -0.0848(3) -0.3173(2) 0.0448(8) Uani 1 d . . 
H17A H -0.1834(3) -0.0510(3) -0.3594(2) 0.067 Uiso 1 calc R . 
H17B H -0.3271(3) -0.0877(3) -0.3578(2) 0.067 Uiso 1 calc R . 
H17C H -0.2210(3) -0.1619(3) -0.2914(2) 0.067 Uiso 1 calc R . 
C18 C -0.0592(3) 0.3739(3) 0.4218(2) 0.0538(9) Uani 1 d . . 
H18A H -0.0212(3) 0.3009(3) 0.4554(2) 0.081 Uiso 1 calc R . 
H18B H -0.0990(3) 0.4297(3) 0.4719(2) 0.081 Uiso 1 calc R . 
H18C H 0.0157(3) 0.4003(3) 0.3710(2) 0.081 Uiso 1 calc R . 
C19 C -0.2701(4) 0.4944(3) 0.2949(3) 0.0563(9) Uani 1 d . . 
H19A H -0.3093(4) 0.5505(3) 0.3448(3) 0.084 Uiso 1 calc R . 
H19B H -0.3437(4) 0.4851(3) 0.2623(3) 0.084 Uiso 1 calc R . 
H19C H -0.1953(4) 0.5203(3) 0.2438(3) 0.084 Uiso 1 calc R . 
C20 C -0.3390(4) 0.3084(3) 0.4586(2) 0.0537(9) Uani 1 d . . 
H20A H -0.3007(4) 0.2355(3) 0.4922(2) 0.081 Uiso 1 calc R . 
H20B H -0.4144(4) 0.2996(3) 0.4276(2) 0.081 Uiso 1 calc R . 
H20C H -0.3759(4) 0.3649(3) 0.5084(2) 0.081 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 0.035(3) 0.046(3) 0.029(3) 0.009(2) -0.006(2) -0.014(2) 
Li2 0.036(3) 0.036(3) 0.030(2) 0.000(2) -0.011(2) -0.017(2) 
Si1 0.0331(4) 0.0334(4) 0.0188(4) -0.0014(3) -0.0036(3) -0.0154(3) 
Si2 0.0382(5) 0.0386(5) 0.0310(4) -0.0109(4) -0.0054(3) -0.0129(4) 
Si3 0.0281(4) 0.0387(5) 0.0227(4) -0.0030(3) -0.0072(3) -0.0129(3) 
Si4 0.0381(5) 0.0356(5) 0.0258(4) -0.0045(3) -0.0063(3) -0.0139(4) 
N1 0.0278(12) 0.0330(13) 0.0201(11) -0.0015(9) -0.0046(9) -0.0131(10) 
N2 0.0313(12) 0.0305(13) 0.0192(11) -0.0011(9) -0.0048(9) -0.0128(10) 
N3 0.0379(13) 0.0318(13) 0.0245(12) -0.0038(10) -0.0044(10) -0.0161(11) 
N4 0.0284(12) 0.0344(13) 0.0191(11) -0.0015(10) -0.0044(9) -0.0134(10) 
N5 0.0271(12) 0.0324(13) 0.0206(11) -0.0013(9) -0.0066(9) -0.0133(10) 
N6 0.0280(12) 0.0314(13) 0.0193(11) -0.0009(9) -0.0046(9) -0.0120(10) 
C1 0.0276(14) 0.032(2) 0.0194(13) 0.0022(11) -0.0031(11) -0.0107(12) 
C2 0.035(2) 0.031(2) 0.0250(14) 0.0013(11) -0.0062(12) -0.0129(13) 
C3 0.040(2) 0.032(2) 0.0285(15) 0.0010(12) -0.0083(12) -0.0187(13) 
C4 0.052(2) 0.036(2) 0.0251(15) -0.0011(12) -0.0052(13) -0.0221(15) 
C5 0.045(2) 0.058(2) 0.032(2) -0.0029(14) -0.0105(13) -0.024(2) 
C6 0.051(2) 0.043(2) 0.0224(14) 0.0031(13) -0.0060(13) -0.021(2) 
C7 0.045(2) 0.041(2) 0.032(2) -0.0080(13) 0.0005(13) -0.0119(15) 
C8 0.053(2) 0.051(2) 0.106(3) -0.028(2) -0.001(2) -0.008(2) 
C9 0.066(2) 0.100(3) 0.042(2) -0.005(2) -0.017(2) -0.037(2) 
C10 0.057(2) 0.053(2) 0.047(2) -0.011(2) -0.001(2) -0.028(2) 
C11 0.0217(13) 0.034(2) 0.0230(13) 0.0021(11) -0.0038(10) -0.0097(12) 
C12 0.0259(14) 0.0286(15) 0.0247(13) 0.0021(11) -0.0055(11) -0.0104(12) 
C13 0.0313(15) 0.029(2) 0.0266(14) -0.0006(12) -0.0067(11) -0.0081(12) 
C14 0.0320(15) 0.035(2) 0.0251(14) -0.0025(12) -0.0061(11) -0.0068(13) 
C15 0.037(2) 0.065(2) 0.034(2) 0.0005(15) -0.0087(13) -0.025(2) 
C16 0.050(2) 0.052(2) 0.050(2) 0.006(2) -0.029(2) -0.018(2) 
C17 0.036(2) 0.070(2) 0.036(2) -0.019(2) -0.0078(13) -0.016(2) 
C18 0.053(2) 0.081(3) 0.037(2) -0.021(2) -0.010(2) -0.022(2) 
C19 0.074(3) 0.037(2) 0.062(2) -0.005(2) -0.020(2) -0.013(2) 
C20 0.064(2) 0.058(2) 0.040(2) -0.017(2) 0.008(2) -0.025(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 N1 2.019(5) . ? 
Li1 N5 2.118(5) . ? 
Li1 N5 2.157(5) 2 ? 
Li1 N6 2.373(6) 2 ? 
Li1 N2 2.420(5) . ? 
Li1 C12 2.503(6) 2 ? 
Li1 C1 2.530(5) . ? 
Li1 Li1 2.766(9) 2 ? 
Li1 Li2 3.020(7) 2 ? 
Li1 Li2 3.069(7) . ? 
Li2 N3 2.026(5) . ? 
Li2 N4 2.041(5) 2 ? 
Li2 N6 2.080(5) . ? 
Li2 N2 2.218(5) . ? 
Li2 C2 2.451(5) . ? 
Li2 C11 2.773(6) 2 ? 
Li2 Li1 3.020(7) 2 ? 
Si1 N1 1.735(2) . ? 
Si1 C5 1.857(3) . ? 
Si1 C7 1.858(3) . ? 
Si1 C6 1.871(3) . ? 
Si2 C4 1.841(3) . ? 
Si2 C10 1.863(3) . ? 
Si2 C9 1.863(3) . ? 
Si2 C8 1.862(4) . ? 
Si3 N4 1.756(2) . ? 
Si3 C17 1.852(3) . ? 
Si3 C15 1.856(3) . ? 
Si3 C16 1.863(3) . ? 
Si4 C19 1.856(3) . ? 
Si4 C14 1.858(3) . ? 
Si4 C20 1.863(3) . ? 
Si4 C18 1.862(3) . ? 
N1 C1 1.292(3) . ? 
N2 C2 1.345(3) . ? 
N2 C1 1.355(3) . ? 
N3 C2 1.297(3) . ? 
N3 C3 1.399(3) . ? 
N4 C11 1.281(3) . ? 
N4 Li2 2.041(5) 2 ? 
N5 C12 1.345(3) . ? 
N5 C11 1.370(3) . ? 
N5 Li1 2.157(5) 2 ? 
N6 C12 1.305(3) . ? 
N6 C13 1.406(3) . ? 
N6 Li1 2.373(6) 2 ? 
C3 C4 1.316(4) . ? 
C11 Li2 2.773(6) 2 ? 
C12 Li1 2.503(6) 2 ? 
C13 C14 1.331(4) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Li1 N5 124.8(3) . . ? 
N1 Li1 N5 134.0(3) . 2 ? 
N5 Li1 N5 99.4(2) . 2 ? 
N1 Li1 N6 109.9(2) . 2 ? 
N5 Li1 N6 107.6(2) . 2 ? 
N5 Li1 N6 60.99(15) 2 2 ? 
N1 Li1 N2 62.1(2) . . ? 
N5 Li1 N2 103.0(2) . . ? 
N5 Li1 N2 99.2(2) 2 . ? 
N6 Li1 N2 145.7(2) 2 . ? 
N1 Li1 C12 118.4(2) . 2 ? 
N5 Li1 C12 114.7(2) . 2 ? 
N5 Li1 C12 32.48(11) 2 2 ? 
N6 Li1 C12 30.89(10) 2 2 ? 
N2 Li1 C12 119.8(2) . 2 ? 
N1 Li1 C1 30.44(10) . . ? 
N5 Li1 C1 116.8(2) . . ? 
N5 Li1 C1 121.3(2) 2 . ? 
N6 Li1 C1 133.4(2) 2 . ? 
N2 Li1 C1 31.67(10) . . ? 
C12 Li1 C1 125.7(2) 2 . ? 
N1 Li1 Li1 168.3(4) . 2 ? 
N5 Li1 Li1 50.3(2) . 2 ? 
N5 Li1 Li1 49.1(2) 2 2 ? 
N6 Li1 Li1 81.6(2) 2 2 ? 
N2 Li1 Li1 107.3(3) . 2 ? 
C12 Li1 Li1 70.3(2) 2 2 ? 
C1 Li1 Li1 138.6(3) . 2 ? 
N1 Li1 Li2 125.9(2) . 2 ? 
N5 Li1 Li2 66.1(2) . 2 ? 
N5 Li1 Li2 80.5(2) 2 2 ? 
N6 Li1 Li2 43.35(13) 2 2 ? 
N2 Li1 Li2 168.6(2) . 2 ? 
C12 Li1 Li2 65.4(2) 2 2 ? 
C1 Li1 Li2 155.2(2) . 2 ? 
Li1 Li1 Li2 63.9(2) 2 2 ? 
N1 Li1 Li2 107.8(2) . . ? 
N5 Li1 Li2 79.8(2) . . ? 
N5 Li1 Li2 64.7(2) 2 . ? 
N6 Li1 Li2 125.7(2) 2 . ? 
N2 Li1 Li2 45.80(13) . . ? 
C12 Li1 Li2 96.1(2) 2 . ? 
C1 Li1 Li2 77.5(2) . . ? 
Li1 Li1 Li2 62.1(2) 2 . ? 
Li2 Li1 Li2 126.0(2) 2 . ? 
N3 Li2 N4 117.6(2) . 2 ? 
N3 Li2 N6 117.8(3) . . ? 
N4 Li2 N6 121.2(2) 2 . ? 
N3 Li2 N2 64.9(2) . . ? 
N4 Li2 N2 114.4(2) 2 . ? 
N6 Li2 N2 105.4(2) . . ? 
N3 Li2 C2 31.92(11) . . ? 
N4 Li2 C2 120.8(2) 2 . ? 
N6 Li2 C2 116.4(2) . . ? 
N2 Li2 C2 33.02(10) . . ? 
N3 Li2 C11 130.2(2) . 2 ? 
N4 Li2 C11 25.52(10) 2 2 ? 
N6 Li2 C11 111.7(2) . 2 ? 
N2 Li2 C11 98.0(2) . 2 ? 
C2 Li2 C11 117.5(2) . 2 ? 
N3 Li2 Li1 164.4(2) . 2 ? 
N4 Li2 Li1 76.9(2) 2 2 ? 
N6 Li2 Li1 51.54(15) . 2 ? 
N2 Li2 Li1 104.9(2) . 2 ? 
C2 Li2 Li1 137.0(2) . 2 ? 
C11 Li2 Li1 60.71(14) 2 2 ? 
N3 Li2 Li1 116.3(2) . . ? 
N4 Li2 Li1 93.2(2) 2 . ? 
N6 Li2 Li1 79.2(2) . . ? 
N2 Li2 Li1 51.45(13) . . ? 
C2 Li2 Li1 84.4(2) . . ? 
C11 Li2 Li1 67.77(15) 2 . ? 
Li1 Li2 Li1 54.0(2) 2 . ? 
N1 Si1 C5 107.01(12) . . ? 
N1 Si1 C7 108.24(13) . . ? 
C5 Si1 C7 110.00(15) . . ? 
N1 Si1 C6 112.84(12) . . ? 
C5 Si1 C6 109.80(14) . . ? 
C7 Si1 C6 108.92(14) . . ? 
C4 Si2 C10 111.01(14) . . ? 
C4 Si2 C9 108.4(2) . . ? 
C10 Si2 C9 108.7(2) . . ? 
C4 Si2 C8 110.8(2) . . ? 
C10 Si2 C8 108.3(2) . . ? 
C9 Si2 C8 109.5(2) . . ? 
N4 Si3 C17 108.04(13) . . ? 
N4 Si3 C15 108.82(12) . . ? 
C17 Si3 C15 109.38(15) . . ? 
N4 Si3 C16 110.72(12) . . ? 
C17 Si3 C16 109.7(2) . . ? 
C15 Si3 C16 110.2(2) . . ? 
C19 Si4 C14 109.09(14) . . ? 
C19 Si4 C20 109.7(2) . . ? 
C14 Si4 C20 110.84(14) . . ? 
C19 Si4 C18 109.6(2) . . ? 
C14 Si4 C18 109.94(14) . . ? 
C20 Si4 C18 107.7(2) . . ? 
C1 N1 Si1 123.3(2) . . ? 
C1 N1 Li1 97.3(2) . . ? 
Si1 N1 Li1 139.3(2) . . ? 
C2 N2 C1 115.7(2) . . ? 
C2 N2 Li2 83.0(2) . . ? 
C1 N2 Li2 161.3(2) . . ? 
C2 N2 Li1 165.5(2) . . ? 
C1 N2 Li1 78.7(2) . . ? 
Li2 N2 Li1 82.7(2) . . ? 
C2 N3 C3 117.4(2) . . ? 
C2 N3 Li2 92.4(2) . . ? 
C3 N3 Li2 150.2(2) . . ? 
C11 N4 Si3 121.6(2) . . ? 
C11 N4 Li2 111.1(2) . 2 ? 
Si3 N4 Li2 123.3(2) . 2 ? 
C12 N5 C11 115.7(2) . . ? 
C12 N5 Li1 121.2(2) . . ? 
C11 N5 Li1 112.8(2) . . ? 
C12 N5 Li1 88.0(2) . 2 ? 
C11 N5 Li1 134.5(2) . 2 ? 
Li1 N5 Li1 80.6(2) . 2 ? 
C12 N6 C13 116.6(2) . . ? 
C12 N6 Li2 124.2(2) . . ? 
C13 N6 Li2 107.6(2) . . ? 
C12 N6 Li1 80.1(2) . 2 ? 
C13 N6 Li1 142.5(2) . 2 ? 
Li2 N6 Li1 85.1(2) . 2 ? 
N1 C1 N2 121.9(2) . . ? 
N1 C1 Li1 52.3(2) . . ? 
N2 C1 Li1 69.7(2) . . ? 
N3 C2 N2 119.6(2) . . ? 
N3 C2 Li2 55.7(2) . . ? 
N2 C2 Li2 64.0(2) . . ? 
C4 C3 N3 124.7(3) . . ? 
C3 C4 Si2 127.6(2) . . ? 
N4 C11 N5 122.9(2) . . ? 
N4 C11 Li2 43.3(2) . 2 ? 
N5 C11 Li2 81.3(2) . 2 ? 
N6 C12 N5 121.0(2) . . ? 
N6 C12 Li1 69.0(2) . 2 ? 
N5 C12 Li1 59.5(2) . 2 ? 
C14 C13 N6 124.2(3) . . ? 
C13 C14 Si4 125.8(2) . . ? 
  
_refine_diff_density_max    0.306 
_refine_diff_density_min   -0.250 
_refine_diff_density_rms    0.054 

#===END