Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dian-sheng Liu' _publ_contact_author_address ; Institute of Modern Chemistry Shanxi University Taiyuan 030006 CHINA ; _publ_contact_author_email DSLIU@SXU.EDU.CN _publ_section_title ; A convenient route to silyl linked-bis(amidinate) ligands ; loop_ _publ_author_name 'Dian-sheng Liu' 'Sheng-Di Bai' 'Jian-Ping Guo' # Attachment 'compound1.cif' data_s096p _database_code_depnum_ccdc_archive 'CCDC 288539' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H58 Li2 N4 O4 Si' _chemical_formula_weight 748.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.913(3) _cell_length_b 17.185(4) _cell_length_c 19.212(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.383(3) _cell_angle_gamma 90.00 _cell_volume 4237.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2193 _cell_measurement_theta_min 2.371 _cell_measurement_theta_max 23.815 _exptl_crystal_description Block _exptl_crystal_colour 'Pale Yellow' _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 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.01 _diffrn_reflns_number 8614 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3737 _reflns_number_gt 2917 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0625P)^2^+5.2425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3737 _refine_ls_number_parameters 249 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.0000 1.02179(8) 0.7500 0.0328(4) Uani 1 2 d S . . N1 N -0.1560(2) 0.91335(16) 0.68745(13) 0.0360(7) Uani 1 1 d . . . N2 N 0.0106(2) 0.96374(15) 0.67736(13) 0.0324(7) Uani 1 1 d . . . O1 O 0.26719(19) 0.98115(14) 0.66846(12) 0.0448(6) Uani 1 1 d . . . O2 O 0.1786(2) 0.81385(14) 0.66614(12) 0.0476(7) Uani 1 1 d . . . C1 C -0.2550(3) 0.90641(19) 0.65143(16) 0.0359(8) Uani 1 1 d . . . C2 C -0.3309(3) 0.8618(2) 0.67933(19) 0.0469(10) Uani 1 1 d . . . H2A H -0.3121 0.8325 0.7195 0.056 Uiso 1 1 calc R . . C3 C -0.4327(3) 0.8599(2) 0.6491(2) 0.0540(11) Uani 1 1 d . . . H3A H -0.4813 0.8299 0.6693 0.065 Uiso 1 1 calc R . . C4 C -0.4630(3) 0.9017(3) 0.5896(2) 0.0580(12) Uani 1 1 d . . . H4A H -0.5316 0.8998 0.5689 0.070 Uiso 1 1 calc R . . C5 C -0.3901(3) 0.9464(3) 0.5610(2) 0.0583(11) Uani 1 1 d . . . H5A H -0.4097 0.9749 0.5205 0.070 Uiso 1 1 calc R . . C6 C -0.2884(3) 0.9496(2) 0.59163(18) 0.0420(9) Uani 1 1 d . . . H6A H -0.2410 0.9813 0.5720 0.050 Uiso 1 1 calc R . . C7 C -0.0712(3) 0.92277(18) 0.65274(16) 0.0324(8) Uani 1 1 d . . . C8 C -0.0642(2) 0.88163(18) 0.58382(16) 0.0317(8) Uani 1 1 d . . . C9 C -0.1165(3) 0.8126(2) 0.56568(17) 0.0393(9) Uani 1 1 d . . . H9A H -0.1588 0.7903 0.5964 0.047 Uiso 1 1 calc R . . C10 C -0.1062(3) 0.7769(2) 0.50257(18) 0.0455(9) Uani 1 1 d . . . H10A H -0.1417 0.7308 0.4909 0.055 Uiso 1 1 calc R . . C11 C -0.0435(3) 0.8092(2) 0.45665(19) 0.0492(10) Uani 1 1 d . . . H11A H -0.0377 0.7854 0.4138 0.059 Uiso 1 1 calc R . . C12 C 0.0101(3) 0.8764(2) 0.47430(18) 0.0473(10) Uani 1 1 d . . . H12A H 0.0530 0.8983 0.4437 0.057 Uiso 1 1 calc R . . C13 C -0.0001(3) 0.9114(2) 0.53764(16) 0.0388(9) Uani 1 1 d . . . H13A H 0.0375 0.9566 0.5496 0.047 Uiso 1 1 calc R . . C14 C -0.1143(3) 1.0895(2) 0.73576(19) 0.0482(10) Uani 1 1 d . . . H14A H -0.0943 1.1357 0.7125 0.072 Uiso 1 1 calc R . . H14B H -0.1367 1.1032 0.7801 0.072 Uiso 1 1 calc R . . H14C H -0.1703 1.0642 0.7073 0.072 Uiso 1 1 calc R . . C15 C 0.2407(3) 1.0295(2) 0.60823(19) 0.0590(12) Uani 1 1 d . . . H15A H 0.1672 1.0425 0.6035 0.071 Uiso 1 1 calc R . . H15B H 0.2564 1.0032 0.5660 0.071 Uiso 1 1 calc R . . C16 C 0.3060(4) 1.1017(3) 0.6206(2) 0.0680(13) Uani 1 1 d . . . H16A H 0.3233 1.1236 0.5768 0.082 Uiso 1 1 calc R . . H16B H 0.2703 1.1408 0.6455 0.082 Uiso 1 1 calc R . . C17 C 0.3997(4) 1.0735(3) 0.6635(2) 0.0683(13) Uani 1 1 d . . . H17A H 0.4303 1.1144 0.6941 0.082 Uiso 1 1 calc R . . H17B H 0.4513 1.0556 0.6341 0.082 Uiso 1 1 calc R . . C18 C 0.3629(3) 1.0077(2) 0.70549(19) 0.0496(10) Uani 1 1 d . . . H18A H 0.4139 0.9661 0.7099 0.060 Uiso 1 1 calc R . . H18B H 0.3517 1.0254 0.7520 0.060 Uiso 1 1 calc R . . C19 C 0.1246(4) 0.7458(2) 0.6852(2) 0.0672(13) Uani 1 1 d . . . H19A H 0.0521 0.7580 0.6891 0.081 Uiso 1 1 calc R . . H19B H 0.1559 0.7261 0.7300 0.081 Uiso 1 1 calc R . . C20 C 0.1322(4) 0.6875(3) 0.6302(3) 0.0762(14) Uani 1 1 d . . . H20A H 0.1578 0.6385 0.6506 0.091 Uiso 1 1 calc R . . H20B H 0.0645 0.6787 0.6042 0.091 Uiso 1 1 calc R . . C21 C 0.2044(4) 0.7182(3) 0.5844(3) 0.0848(16) Uani 1 1 d . . . H21A H 0.2631 0.6833 0.5831 0.102 Uiso 1 1 calc R . . H21B H 0.1700 0.7241 0.5372 0.102 Uiso 1 1 calc R . . C22 C 0.2396(4) 0.7932(3) 0.6124(2) 0.0710(14) Uani 1 1 d . . . H22A H 0.3125 0.7903 0.6310 0.085 Uiso 1 1 calc R . . H22B H 0.2323 0.8322 0.5757 0.085 Uiso 1 1 calc R . . Li1 Li 0.1548(5) 0.9169(3) 0.7045(3) 0.0386(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0341(8) 0.0362(8) 0.0279(7) 0.000 0.0025(6) 0.000 N1 0.0345(17) 0.0483(18) 0.0253(14) -0.0010(12) 0.0031(13) -0.0076(13) N2 0.0342(16) 0.0350(16) 0.0272(14) 0.0034(12) -0.0001(12) -0.0044(12) O1 0.0431(15) 0.0491(16) 0.0417(14) 0.0036(12) 0.0033(11) -0.0111(12) O2 0.0587(18) 0.0432(15) 0.0442(14) -0.0011(12) 0.0209(13) -0.0028(12) C1 0.038(2) 0.041(2) 0.0295(18) -0.0117(15) 0.0066(15) -0.0030(16) C2 0.047(2) 0.054(2) 0.041(2) -0.0148(18) 0.0084(18) -0.0076(18) C3 0.046(3) 0.055(3) 0.064(3) -0.026(2) 0.016(2) -0.0158(19) C4 0.034(2) 0.068(3) 0.069(3) -0.023(2) -0.003(2) 0.004(2) C5 0.048(3) 0.068(3) 0.056(2) -0.006(2) -0.006(2) 0.018(2) C6 0.036(2) 0.050(2) 0.039(2) -0.0037(17) 0.0012(16) 0.0047(16) C7 0.039(2) 0.0340(19) 0.0236(16) 0.0075(14) -0.0003(15) 0.0045(15) C8 0.035(2) 0.0323(19) 0.0259(16) 0.0007(14) -0.0040(14) 0.0032(14) C9 0.040(2) 0.039(2) 0.039(2) -0.0030(16) 0.0079(16) -0.0029(16) C10 0.054(3) 0.036(2) 0.045(2) -0.0106(17) -0.0016(19) -0.0040(17) C11 0.063(3) 0.049(2) 0.036(2) -0.0105(18) 0.0073(19) 0.002(2) C12 0.060(3) 0.046(2) 0.038(2) -0.0046(17) 0.0132(18) -0.0045(19) C13 0.051(2) 0.036(2) 0.0286(18) -0.0011(15) 0.0015(16) -0.0090(16) C14 0.047(2) 0.053(2) 0.045(2) 0.0095(18) 0.0051(18) 0.0068(18) C15 0.061(3) 0.073(3) 0.041(2) 0.015(2) -0.001(2) -0.017(2) C16 0.072(3) 0.058(3) 0.076(3) 0.019(2) 0.014(3) -0.016(2) C17 0.063(3) 0.069(3) 0.071(3) 0.002(2) -0.001(2) -0.022(2) C18 0.038(2) 0.058(3) 0.053(2) 0.0041(19) 0.0037(18) -0.0023(18) C19 0.079(3) 0.058(3) 0.069(3) 0.012(2) 0.029(2) -0.009(2) C20 0.077(4) 0.048(3) 0.106(4) -0.003(3) 0.021(3) -0.002(2) C21 0.122(5) 0.057(3) 0.082(3) -0.016(3) 0.044(3) -0.007(3) C22 0.078(3) 0.067(3) 0.075(3) -0.018(2) 0.041(3) -0.011(2) Li1 0.040(3) 0.046(4) 0.030(3) -0.003(3) 0.005(3) 0.001(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 Si1 N2 1.733(3) . ? Si1 N2 1.733(3) 2_556 ? Si1 C14 1.875(4) 2_556 ? Si1 C14 1.875(4) . ? Si1 Li1 2.899(6) . ? Si1 Li1 2.899(6) 2_556 ? N1 C7 1.354(4) . ? N1 C1 1.389(4) . ? N1 Li1 2.076(6) 2_556 ? N2 C7 1.313(4) . ? N2 Li1 2.042(6) . ? O1 C18 1.430(4) . ? O1 C15 1.435(4) . ? O1 Li1 2.007(6) . ? O2 C22 1.411(4) . ? O2 C19 1.431(4) . ? O2 Li1 1.955(6) . ? C1 C6 1.396(5) . ? C1 C2 1.397(5) . ? C2 C3 1.377(5) . ? C3 C4 1.370(6) . ? C4 C5 1.376(6) . ? C5 C6 1.379(5) . ? C7 C8 1.513(4) . ? C8 C13 1.378(4) . ? C8 C9 1.390(5) . ? C9 C10 1.378(5) . ? C10 C11 1.378(5) . ? C11 C12 1.370(5) . ? C12 C13 1.377(5) . ? C15 C16 1.504(6) . ? C16 C17 1.469(6) . ? C17 C18 1.496(5) . ? C19 C20 1.468(6) . ? C20 C21 1.450(6) . ? C21 C22 1.450(6) . ? Li1 N1 2.076(6) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Si1 N2 109.72(18) . 2_556 ? N2 Si1 C14 110.07(14) . 2_556 ? N2 Si1 C14 111.78(15) 2_556 2_556 ? N2 Si1 C14 111.78(15) . . ? N2 Si1 C14 110.07(14) 2_556 . ? C14 Si1 C14 103.3(3) 2_556 . ? N2 Si1 Li1 43.94(14) . . ? N2 Si1 Li1 90.23(15) 2_556 . ? C14 Si1 Li1 82.65(17) 2_556 . ? C14 Si1 Li1 154.14(15) . . ? N2 Si1 Li1 90.23(15) . 2_556 ? N2 Si1 Li1 43.94(14) 2_556 2_556 ? C14 Si1 Li1 154.14(15) 2_556 2_556 ? C14 Si1 Li1 82.65(17) . 2_556 ? Li1 Si1 Li1 103.1(2) . 2_556 ? C7 N1 C1 121.0(3) . . ? C7 N1 Li1 124.9(3) . 2_556 ? C1 N1 Li1 113.9(3) . 2_556 ? C7 N2 Si1 117.8(2) . . ? C7 N2 Li1 123.7(3) . . ? Si1 N2 Li1 100.0(2) . . ? C18 O1 C15 109.3(3) . . ? C18 O1 Li1 128.5(3) . . ? C15 O1 Li1 118.7(3) . . ? C22 O2 C19 108.0(3) . . ? C22 O2 Li1 128.8(3) . . ? C19 O2 Li1 122.8(3) . . ? N1 C1 C6 123.2(3) . . ? N1 C1 C2 120.1(3) . . ? C6 C1 C2 116.2(3) . . ? C3 C2 C1 121.9(4) . . ? C4 C3 C2 120.7(4) . . ? C3 C4 C5 118.8(4) . . ? C4 C5 C6 120.8(4) . . ? C5 C6 C1 121.5(4) . . ? N2 C7 N1 123.3(3) . . ? N2 C7 C8 116.2(3) . . ? N1 C7 C8 120.4(3) . . ? C13 C8 C9 117.8(3) . . ? C13 C8 C7 119.2(3) . . ? C9 C8 C7 122.9(3) . . ? C10 C9 C8 120.6(3) . . ? C9 C10 C11 120.3(3) . . ? C12 C11 C10 119.9(3) . . ? C11 C12 C13 119.5(3) . . ? C12 C13 C8 122.0(3) . . ? O1 C15 C16 105.7(3) . . ? C17 C16 C15 103.2(4) . . ? C16 C17 C18 105.1(3) . . ? O1 C18 C17 106.4(3) . . ? O2 C19 C20 107.4(3) . . ? C21 C20 C19 106.7(4) . . ? C22 C21 C20 107.1(4) . . ? O2 C22 C21 108.5(4) . . ? O2 Li1 O1 102.6(3) . . ? O2 Li1 N2 116.0(3) . . ? O1 Li1 N2 111.6(3) . . ? O2 Li1 N1 111.5(3) . 2_556 ? O1 Li1 N1 115.8(3) . 2_556 ? N2 Li1 N1 99.9(3) . 2_556 ? O2 Li1 Si1 145.1(3) . . ? O1 Li1 Si1 108.1(2) . . ? N2 Li1 Si1 36.08(12) . . ? N1 Li1 Si1 69.20(17) 2_556 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.401 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.048 # Attachment 'compound3.cif' data_p _database_code_depnum_ccdc_archive 'CCDC 288540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H132 Li4 N8 O4 Si2' _chemical_formula_weight 1546.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 20.4738(13) _cell_length_b 11.3967(7) _cell_length_c 21.0692(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.957(2) _cell_angle_gamma 90.00 _cell_volume 4809.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9659 _exptl_absorpt_correction_T_max 0.9827 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25316 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.1189 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8469 _reflns_number_gt 3302 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8469 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1687 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1967 _refine_ls_wR_factor_gt 0.1497 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.7500 0.59512(12) 0.7500 0.0476(4) Uani 1 2 d S . . Si2 Si 0.7500 0.12690(13) 0.7500 0.0530(4) Uani 1 2 d S . . N1 N 0.77853(14) 0.4493(3) 0.59020(13) 0.0504(8) Uani 1 1 d . . . N2 N 0.75697(14) 0.4983(2) 0.68920(12) 0.0470(8) Uani 1 1 d . . . N3 N 0.90784(14) 0.2812(3) 0.71044(14) 0.0531(8) Uani 1 1 d . . . N4 N 0.81057(13) 0.2239(2) 0.73847(14) 0.0504(8) Uani 1 1 d . . . C1 C 0.76866(18) 0.4662(3) 0.52213(17) 0.0509(10) Uani 1 1 d . . . C2 C 0.72194(19) 0.3992(4) 0.48004(18) 0.0581(11) Uani 1 1 d . . . C3 C 0.7141(2) 0.4174(5) 0.4136(2) 0.0811(14) Uani 1 1 d . . . H3A H 0.6826 0.3734 0.3852 0.097 Uiso 1 1 calc R . . C4 C 0.7513(3) 0.4978(5) 0.3892(2) 0.0926(16) Uani 1 1 d . . . H4A H 0.7436 0.5116 0.3447 0.111 Uiso 1 1 calc R . . C5 C 0.8001(3) 0.5586(5) 0.4306(2) 0.0890(15) Uani 1 1 d . . . H5A H 0.8273 0.6099 0.4135 0.107 Uiso 1 1 calc R . . C6 C 0.8101(2) 0.5457(4) 0.4975(2) 0.0661(11) Uani 1 1 d . . . C7 C 0.8650(2) 0.6103(4) 0.5422(2) 0.0904(15) Uani 1 1 d . . . H7A H 0.8510 0.6185 0.5837 0.109 Uiso 1 1 calc R . . C8 C 0.8772(4) 0.7360(6) 0.5192(3) 0.168(3) Uani 1 1 d . . . H8A H 0.8363 0.7799 0.5128 0.251 Uiso 1 1 calc R . . H8B H 0.8925 0.7321 0.4792 0.251 Uiso 1 1 calc R . . H8C H 0.9104 0.7741 0.5515 0.251 Uiso 1 1 calc R . . C9 C 0.9293(3) 0.5398(7) 0.5558(4) 0.185(3) Uani 1 1 d . . . H9A H 0.9207 0.4630 0.5709 0.278 Uiso 1 1 calc R . . H9B H 0.9618 0.5789 0.5883 0.278 Uiso 1 1 calc R . . H9C H 0.9462 0.5328 0.5166 0.278 Uiso 1 1 calc R . . C10 C 0.6832(2) 0.3042(4) 0.5053(2) 0.0729(12) Uani 1 1 d . . . H10A H 0.6837 0.3224 0.5508 0.087 Uiso 1 1 calc R . . C11 C 0.6103(2) 0.2972(5) 0.4704(3) 0.127(2) Uani 1 1 d . . . H11A H 0.5893 0.3719 0.4728 0.191 Uiso 1 1 calc R . . H11B H 0.5879 0.2385 0.4906 0.191 Uiso 1 1 calc R . . H11C H 0.6079 0.2768 0.4257 0.191 Uiso 1 1 calc R . . C12 C 0.7172(3) 0.1862(5) 0.5039(3) 0.126(2) Uani 1 1 d . . . H12A H 0.7628 0.1919 0.5267 0.190 Uiso 1 1 calc R . . H12B H 0.7158 0.1638 0.4597 0.190 Uiso 1 1 calc R . . H12C H 0.6945 0.1283 0.5244 0.190 Uiso 1 1 calc R . . C13 C 0.74697(17) 0.5158(3) 0.62497(17) 0.0430(9) Uani 1 1 d . . . C14 C 0.6976(2) 0.6060(3) 0.59290(16) 0.0520(10) Uani 1 1 d . . . C15 C 0.6317(2) 0.5773(4) 0.5752(2) 0.0787(13) Uani 1 1 d . . . H15A H 0.6179 0.5022 0.5836 0.094 Uiso 1 1 calc R . . C16 C 0.5849(3) 0.6578(7) 0.5450(3) 0.115(2) Uani 1 1 d . . . H16A H 0.5401 0.6365 0.5331 0.138 Uiso 1 1 calc R . . C17 C 0.6040(4) 0.7672(8) 0.5328(3) 0.126(3) Uani 1 1 d . . . H17A H 0.5726 0.8206 0.5116 0.151 Uiso 1 1 calc R . . C18 C 0.6685(4) 0.7998(5) 0.5511(3) 0.117(2) Uani 1 1 d . . . H18A H 0.6811 0.8761 0.5434 0.141 Uiso 1 1 calc R . . C19 C 0.7168(3) 0.7192(4) 0.5817(2) 0.0811(14) Uani 1 1 d . . . H19A H 0.7612 0.7417 0.5944 0.097 Uiso 1 1 calc R . . C20 C 0.6752(2) 0.6921(4) 0.73685(18) 0.0726(13) Uani 1 1 d . . . H20A H 0.6892 0.7726 0.7394 0.109 Uiso 1 1 calc R . . H20B H 0.6500 0.6766 0.7696 0.109 Uiso 1 1 calc R . . H20C H 0.6480 0.6769 0.6948 0.109 Uiso 1 1 calc R . . C21 C 0.97713(18) 0.2790(4) 0.71235(19) 0.0542(10) Uani 1 1 d . . . C22 C 1.01993(19) 0.3514(4) 0.75601(19) 0.0614(11) Uani 1 1 d . . . C23 C 1.0867(2) 0.3592(4) 0.7514(2) 0.0818(14) Uani 1 1 d . . . H23A H 1.1155 0.4070 0.7803 0.098 Uiso 1 1 calc R . . C24 C 1.1108(2) 0.2983(5) 0.7054(3) 0.0933(16) Uani 1 1 d . . . H24A H 1.1554 0.3051 0.7030 0.112 Uiso 1 1 calc R . . C25 C 1.0689(2) 0.2272(4) 0.6628(2) 0.0824(14) Uani 1 1 d . . . H25A H 1.0859 0.1861 0.6316 0.099 Uiso 1 1 calc R . . C26 C 1.0014(2) 0.2147(4) 0.6648(2) 0.0663(12) Uani 1 1 d . . . C27 C 0.9569(2) 0.1384(5) 0.6169(2) 0.0890(14) Uani 1 1 d . . . H27A H 0.9182 0.1186 0.6354 0.107 Uiso 1 1 calc R . . C28 C 0.9307(3) 0.2042(6) 0.5535(3) 0.147(3) Uani 1 1 d . . . H28A H 0.9098 0.2759 0.5626 0.220 Uiso 1 1 calc R . . H28B H 0.8987 0.1562 0.5252 0.220 Uiso 1 1 calc R . . H28C H 0.9671 0.2218 0.5328 0.220 Uiso 1 1 calc R . . C29 C 0.9892(3) 0.0232(6) 0.6032(3) 0.161(3) Uani 1 1 d . . . H29A H 1.0044 -0.0184 0.6431 0.241 Uiso 1 1 calc R . . H29B H 1.0265 0.0392 0.5833 0.241 Uiso 1 1 calc R . . H29C H 0.9571 -0.0239 0.5744 0.241 Uiso 1 1 calc R . . C30 C 0.9955(2) 0.4231(4) 0.8068(2) 0.0707(12) Uani 1 1 d . . . H30A H 0.9484 0.4034 0.8043 0.085 Uiso 1 1 calc R . . C31 C 0.9995(3) 0.5555(5) 0.7931(3) 0.1099(17) Uani 1 1 d . . . H31A H 0.9748 0.5724 0.7502 0.165 Uiso 1 1 calc R . . H31B H 1.0453 0.5777 0.7965 0.165 Uiso 1 1 calc R . . H31C H 0.9809 0.5989 0.8242 0.165 Uiso 1 1 calc R . . C32 C 1.0329(2) 0.3977(5) 0.8754(2) 0.0987(16) Uani 1 1 d . . . H32A H 1.0296 0.3157 0.8845 0.148 Uiso 1 1 calc R . . H32B H 1.0138 0.4427 0.9055 0.148 Uiso 1 1 calc R . . H32C H 1.0790 0.4187 0.8796 0.148 Uiso 1 1 calc R . . C33 C 0.87652(17) 0.2097(3) 0.74291(17) 0.0464(9) Uani 1 1 d . . . C34 C 0.91344(18) 0.1168(3) 0.7863(2) 0.0564(10) Uani 1 1 d . . . C35 C 0.9289(2) 0.0101(4) 0.7621(3) 0.0920(16) Uani 1 1 d . . . H35A H 0.9176 -0.0034 0.7177 0.110 Uiso 1 1 calc R . . C36 C 0.9606(3) -0.0769(5) 0.8025(4) 0.126(3) Uani 1 1 d . . . H36A H 0.9703 -0.1484 0.7854 0.151 Uiso 1 1 calc R . . C37 C 0.9778(3) -0.0576(7) 0.8678(5) 0.137(3) Uani 1 1 d . . . H37A H 1.0001 -0.1155 0.8950 0.164 Uiso 1 1 calc R . . C38 C 0.9622(3) 0.0478(6) 0.8934(3) 0.124(2) Uani 1 1 d . . . H38A H 0.9732 0.0608 0.9379 0.148 Uiso 1 1 calc R . . C39 C 0.9297(2) 0.1344(4) 0.8520(2) 0.0895(15) Uani 1 1 d . . . H39A H 0.9188 0.2052 0.8692 0.107 Uiso 1 1 calc R . . C40 C 0.7307(2) 0.0305(4) 0.6771(2) 0.0820(14) Uani 1 1 d . . . H40A H 0.7345 -0.0502 0.6904 0.123 Uiso 1 1 calc R . . H40B H 0.7616 0.0463 0.6496 0.123 Uiso 1 1 calc R . . H40C H 0.6861 0.0457 0.6537 0.123 Uiso 1 1 calc R . . C41 C 1.1573(3) -0.1821(6) 0.6334(3) 0.139(2) Uani 1 1 d . . . H41A H 1.1932 -0.1964 0.6107 0.167 Uiso 1 1 calc R . . H41B H 1.1384 -0.1055 0.6207 0.167 Uiso 1 1 calc R . . C42 C 1.1055(4) -0.2741(7) 0.6170(3) 0.151(3) Uani 1 1 d . . . H42A H 1.0628 -0.2395 0.5971 0.181 Uiso 1 1 calc R . . H42B H 1.1178 -0.3305 0.5870 0.181 Uiso 1 1 calc R . . C43 C 1.1017(4) -0.3284(8) 0.6756(4) 0.196(4) Uani 1 1 d . . . H43A H 1.0579 -0.3154 0.6852 0.235 Uiso 1 1 calc R . . H43B H 1.1082 -0.4123 0.6722 0.235 Uiso 1 1 calc R . . C44 C 1.1492(5) -0.2836(8) 0.7236(3) 0.196(4) Uani 1 1 d . . . H44A H 1.1819 -0.3438 0.7399 0.235 Uiso 1 1 calc R . . H44B H 1.1290 -0.2584 0.7591 0.235 Uiso 1 1 calc R . . C45 C 1.1449(3) 0.0077(6) 0.8154(3) 0.1164(19) Uani 1 1 d . . . H45A H 1.1328 -0.0702 0.8275 0.140 Uiso 1 1 calc R . . H45B H 1.1151 0.0295 0.7751 0.140 Uiso 1 1 calc R . . C46 C 1.1393(3) 0.0917(6) 0.8663(4) 0.143(2) Uani 1 1 d . . . H46A H 1.1040 0.1478 0.8509 0.172 Uiso 1 1 calc R . . H46B H 1.1300 0.0518 0.9041 0.172 Uiso 1 1 calc R . . C47 C 1.2035(4) 0.1494(7) 0.8815(4) 0.178(3) Uani 1 1 d . . . H47A H 1.1978 0.2329 0.8731 0.214 Uiso 1 1 calc R . . H47B H 1.2232 0.1389 0.9272 0.214 Uiso 1 1 calc R . . C48 C 1.2438(3) 0.1041(7) 0.8453(4) 0.181(4) Uani 1 1 d . . . H48A H 1.2847 0.0766 0.8731 0.217 Uiso 1 1 calc R . . H48B H 1.2552 0.1641 0.8168 0.217 Uiso 1 1 calc R . . Li1 Li 0.8255(3) 0.3634(6) 0.6696(3) 0.0628(18) Uani 1 1 d . . . Li2 Li 0.7500 0.3605(8) 0.7500 0.060(2) Uani 1 2 d S . . Li3 Li 1.2500 -0.0895(13) 0.7500 0.113(4) Uani 1 2 d S . . O1 O 1.18171(19) -0.1862(4) 0.70074(18) 0.1194(13) Uani 1 1 d . . . O2 O 1.21108(19) 0.0085(4) 0.80739(18) 0.1176(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0582(10) 0.0408(9) 0.0434(8) 0.000 0.0098(7) 0.000 Si2 0.0427(9) 0.0394(9) 0.0763(10) 0.000 0.0108(8) 0.000 N1 0.0475(19) 0.059(2) 0.0441(18) -0.0046(15) 0.0071(15) 0.0099(16) N2 0.060(2) 0.0442(18) 0.0348(16) -0.0008(13) 0.0061(15) 0.0048(15) N3 0.0408(19) 0.063(2) 0.0556(19) 0.0128(17) 0.0111(16) 0.0038(16) N4 0.0365(18) 0.0435(19) 0.070(2) 0.0020(15) 0.0085(16) 0.0047(14) C1 0.044(2) 0.063(3) 0.047(2) -0.003(2) 0.012(2) 0.011(2) C2 0.052(3) 0.072(3) 0.050(2) -0.007(2) 0.010(2) 0.009(2) C3 0.082(3) 0.107(4) 0.049(3) -0.012(3) -0.001(2) 0.006(3) C4 0.106(4) 0.121(5) 0.053(3) 0.004(3) 0.023(3) 0.011(4) C5 0.095(4) 0.105(4) 0.079(3) 0.012(3) 0.045(3) -0.002(3) C6 0.069(3) 0.073(3) 0.060(3) -0.001(2) 0.023(2) 0.001(2) C7 0.079(4) 0.097(4) 0.101(4) -0.004(3) 0.032(3) -0.029(3) C8 0.209(8) 0.137(6) 0.157(6) 0.012(5) 0.038(5) -0.096(6) C9 0.071(4) 0.205(8) 0.264(9) -0.035(7) -0.001(5) -0.009(5) C10 0.067(3) 0.084(3) 0.063(3) -0.008(2) 0.004(2) -0.005(3) C11 0.078(4) 0.151(5) 0.139(5) 0.010(4) -0.012(4) -0.031(4) C12 0.140(5) 0.090(4) 0.152(5) 0.005(4) 0.040(4) 0.006(4) C13 0.040(2) 0.037(2) 0.050(2) -0.0019(18) 0.0040(18) -0.0028(17) C14 0.065(3) 0.053(3) 0.038(2) 0.0003(18) 0.009(2) 0.015(2) C15 0.062(3) 0.086(3) 0.081(3) -0.009(3) -0.004(3) 0.020(3) C16 0.093(4) 0.154(6) 0.086(4) -0.010(4) -0.010(3) 0.064(5) C17 0.162(7) 0.143(7) 0.068(4) 0.017(4) 0.013(4) 0.102(7) C18 0.201(7) 0.081(4) 0.077(4) 0.020(3) 0.045(5) 0.063(5) C19 0.108(4) 0.063(3) 0.076(3) 0.009(3) 0.029(3) 0.016(3) C20 0.092(3) 0.068(3) 0.060(2) -0.003(2) 0.022(2) 0.022(3) C21 0.038(2) 0.068(3) 0.058(2) 0.016(2) 0.014(2) 0.005(2) C22 0.044(2) 0.075(3) 0.065(3) 0.017(2) 0.012(2) 0.006(2) C23 0.048(3) 0.107(4) 0.089(3) 0.014(3) 0.012(3) -0.007(3) C24 0.052(3) 0.128(5) 0.106(4) 0.023(4) 0.031(3) 0.006(3) C25 0.069(3) 0.101(4) 0.085(3) 0.014(3) 0.035(3) 0.015(3) C26 0.057(3) 0.083(3) 0.062(3) 0.012(2) 0.019(2) 0.006(2) C27 0.089(4) 0.103(4) 0.080(3) -0.009(3) 0.029(3) 0.012(3) C28 0.138(6) 0.208(7) 0.083(4) -0.001(4) -0.002(4) -0.013(5) C29 0.152(6) 0.134(6) 0.202(7) -0.067(5) 0.052(5) 0.021(5) C30 0.052(3) 0.084(3) 0.075(3) -0.002(3) 0.011(2) -0.006(2) C31 0.109(4) 0.093(4) 0.129(4) 0.010(4) 0.029(4) 0.019(3) C32 0.107(4) 0.111(4) 0.073(3) -0.008(3) 0.007(3) -0.001(3) C33 0.039(2) 0.041(2) 0.058(2) -0.0012(19) 0.0074(19) -0.0004(18) C34 0.039(2) 0.048(3) 0.082(3) 0.016(2) 0.012(2) -0.0003(19) C35 0.090(4) 0.066(3) 0.133(4) 0.025(3) 0.051(3) 0.027(3) C36 0.101(5) 0.073(4) 0.220(8) 0.064(5) 0.072(6) 0.033(4) C37 0.058(4) 0.120(6) 0.226(9) 0.109(7) 0.019(5) 0.019(4) C38 0.089(4) 0.130(5) 0.130(5) 0.062(5) -0.028(4) -0.019(4) C39 0.090(4) 0.080(3) 0.084(3) 0.031(3) -0.015(3) -0.005(3) C40 0.069(3) 0.060(3) 0.119(4) -0.023(3) 0.022(3) -0.003(2) C41 0.134(6) 0.170(7) 0.108(5) 0.031(5) 0.014(4) -0.032(5) C42 0.160(7) 0.177(7) 0.102(5) 0.011(5) -0.004(5) -0.038(6) C43 0.217(9) 0.251(10) 0.106(5) 0.015(6) 0.000(6) -0.114(8) C44 0.246(10) 0.223(9) 0.102(5) 0.036(6) -0.002(6) -0.122(8) C45 0.077(4) 0.138(5) 0.139(5) -0.009(4) 0.034(4) -0.015(4) C46 0.122(6) 0.125(5) 0.205(7) -0.026(5) 0.087(5) -0.006(4) C47 0.152(7) 0.202(8) 0.198(8) -0.086(6) 0.076(6) -0.060(7) C48 0.110(5) 0.200(8) 0.250(9) -0.105(7) 0.075(6) -0.069(6) Li1 0.048(4) 0.080(5) 0.058(4) 0.003(4) 0.003(3) 0.015(4) Li2 0.064(6) 0.058(6) 0.060(5) 0.000 0.016(5) 0.000 Li3 0.096(9) 0.146(12) 0.100(9) 0.000 0.029(8) 0.000 O1 0.129(3) 0.149(4) 0.076(2) 0.005(2) 0.010(2) -0.037(3) O2 0.081(3) 0.137(3) 0.144(3) -0.039(3) 0.044(2) -0.016(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 Si1 N2 1.719(3) 2_656 ? Si1 N2 1.719(3) . ? Si1 C20 1.861(4) . ? Si1 C20 1.861(4) 2_656 ? Si1 Li2 2.673(10) . ? Si2 N4 1.716(3) . ? Si2 N4 1.716(3) 2_656 ? Si2 C40 1.863(4) 2_656 ? Si2 C40 1.863(4) . ? Si2 Li2 2.663(10) . ? N1 C13 1.313(4) . ? N1 C1 1.419(4) . ? N1 Li1 2.004(7) . ? N2 C13 1.341(4) . ? N2 Li2 2.050(8) . ? N2 Li1 2.178(7) . ? N3 C33 1.313(4) . ? N3 C21 1.411(4) . ? N3 Li1 1.965(7) . ? N4 C33 1.344(4) . ? N4 Li2 2.036(8) . ? N4 Li1 2.215(7) . ? C1 C2 1.391(5) . ? C1 C6 1.412(5) . ? C2 C3 1.390(5) . ? C2 C10 1.503(5) . ? C3 C4 1.360(6) . ? C4 C5 1.372(6) . ? C5 C6 1.388(6) . ? C6 C7 1.501(6) . ? C7 C9 1.518(7) . ? C7 C8 1.549(7) . ? C10 C12 1.517(6) . ? C10 C11 1.523(6) . ? C13 C14 1.501(5) . ? C13 Li1 2.421(7) . ? C14 C15 1.364(5) . ? C14 C19 1.382(5) . ? C15 C16 1.383(7) . ? C16 C17 1.348(9) . ? C17 C18 1.349(8) . ? C18 C19 1.405(7) . ? C21 C22 1.400(5) . ? C21 C26 1.412(5) . ? C22 C23 1.394(5) . ? C22 C30 1.511(5) . ? C23 C24 1.363(6) . ? C24 C25 1.371(6) . ? C25 C26 1.399(6) . ? C26 C27 1.493(6) . ? C27 C29 1.525(7) . ? C27 C28 1.529(7) . ? C30 C32 1.518(5) . ? C30 C31 1.542(6) . ? C33 C34 1.496(5) . ? C33 Li1 2.424(7) . ? C34 C39 1.371(5) . ? C34 C35 1.380(6) . ? C35 C36 1.379(7) . ? C36 C37 1.364(9) . ? C37 C38 1.382(9) . ? C38 C39 1.391(7) . ? C41 O1 1.405(6) . ? C41 C42 1.481(8) . ? C42 C43 1.398(8) . ? C43 C44 1.351(8) . ? C44 O1 1.428(7) . ? C45 O2 1.399(5) . ? C45 C46 1.459(7) . ? C46 C47 1.444(8) . ? C47 C48 1.339(8) . ? C48 O2 1.431(7) . ? Li1 Li2 2.519(6) . ? Li2 N4 2.036(8) 2_656 ? Li2 N2 2.050(8) 2_656 ? Li2 Li1 2.519(6) 2_656 ? Li3 O1 1.909(10) . ? Li3 O1 1.909(10) 2_756 ? Li3 O2 1.935(10) . ? Li3 O2 1.935(10) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Si1 N2 100.1(2) 2_656 . ? N2 Si1 C20 107.42(16) 2_656 . ? N2 Si1 C20 117.57(15) . . ? N2 Si1 C20 117.57(15) 2_656 2_656 ? N2 Si1 C20 107.42(16) . 2_656 ? C20 Si1 C20 107.2(3) . 2_656 ? N2 Si1 Li2 50.06(10) 2_656 . ? N2 Si1 Li2 50.06(10) . . ? C20 Si1 Li2 126.41(14) . . ? C20 Si1 Li2 126.41(14) 2_656 . ? N4 Si2 N4 99.7(2) . 2_656 ? N4 Si2 C40 117.44(16) . 2_656 ? N4 Si2 C40 107.41(16) 2_656 2_656 ? N4 Si2 C40 107.41(16) . . ? N4 Si2 C40 117.44(16) 2_656 . ? C40 Si2 C40 107.7(3) 2_656 . ? N4 Si2 Li2 49.87(10) . . ? N4 Si2 Li2 49.87(10) 2_656 . ? C40 Si2 Li2 126.14(15) 2_656 . ? C40 Si2 Li2 126.14(15) . . ? C13 N1 C1 120.1(3) . . ? C13 N1 Li1 91.3(3) . . ? C1 N1 Li1 148.5(3) . . ? C13 N2 Si1 129.6(2) . . ? C13 N2 Li2 136.8(3) . . ? Si1 N2 Li2 89.9(2) . . ? C13 N2 Li1 83.3(3) . . ? Si1 N2 Li1 138.7(2) . . ? Li2 N2 Li1 73.1(2) . . ? C33 N3 C21 124.8(3) . . ? C33 N3 Li1 93.2(3) . . ? C21 N3 Li1 141.9(3) . . ? C33 N4 Si2 131.1(2) . . ? C33 N4 Li2 135.4(3) . . ? Si2 N4 Li2 90.0(2) . . ? C33 N4 Li1 81.9(3) . . ? Si2 N4 Li1 139.2(2) . . ? Li2 N4 Li1 72.5(2) . . ? C2 C1 C6 120.3(3) . . ? C2 C1 N1 120.3(3) . . ? C6 C1 N1 119.2(3) . . ? C3 C2 C1 118.7(4) . . ? C3 C2 C10 120.3(4) . . ? C1 C2 C10 120.9(3) . . ? C4 C3 C2 121.7(5) . . ? C3 C4 C5 119.4(4) . . ? C4 C5 C6 121.8(5) . . ? C5 C6 C1 117.9(4) . . ? C5 C6 C7 121.2(4) . . ? C1 C6 C7 120.9(4) . . ? C6 C7 C9 111.5(5) . . ? C6 C7 C8 114.0(5) . . ? C9 C7 C8 111.1(5) . . ? C2 C10 C12 110.7(4) . . ? C2 C10 C11 113.7(4) . . ? C12 C10 C11 110.6(4) . . ? N1 C13 N2 119.2(3) . . ? N1 C13 C14 120.5(3) . . ? N2 C13 C14 120.3(3) . . ? N1 C13 Li1 55.9(2) . . ? N2 C13 Li1 63.3(2) . . ? C14 C13 Li1 176.1(3) . . ? C15 C14 C19 118.5(4) . . ? C15 C14 C13 119.7(4) . . ? C19 C14 C13 121.8(4) . . ? C14 C15 C16 121.3(5) . . ? C17 C16 C15 120.0(6) . . ? C16 C17 C18 120.5(7) . . ? C17 C18 C19 120.3(7) . . ? C14 C19 C18 119.4(5) . . ? C22 C21 N3 119.8(4) . . ? C22 C21 C26 120.5(4) . . ? N3 C21 C26 119.2(4) . . ? C23 C22 C21 118.8(4) . . ? C23 C22 C30 119.2(4) . . ? C21 C22 C30 122.0(3) . . ? C24 C23 C22 121.4(5) . . ? C23 C24 C25 119.9(4) . . ? C24 C25 C26 121.7(5) . . ? C25 C26 C21 117.7(4) . . ? C25 C26 C27 120.4(4) . . ? C21 C26 C27 121.8(4) . . ? C26 C27 C29 113.7(4) . . ? C26 C27 C28 111.1(4) . . ? C29 C27 C28 110.2(5) . . ? C22 C30 C32 113.3(4) . . ? C22 C30 C31 111.1(4) . . ? C32 C30 C31 109.1(4) . . ? N3 C33 N4 118.7(3) . . ? N3 C33 C34 121.1(3) . . ? N4 C33 C34 120.1(3) . . ? N3 C33 Li1 54.0(2) . . ? N4 C33 Li1 64.8(2) . . ? C34 C33 Li1 175.1(3) . . ? C39 C34 C35 118.4(4) . . ? C39 C34 C33 120.0(4) . . ? C35 C34 C33 121.6(4) . . ? C36 C35 C34 121.4(6) . . ? C37 C36 C35 119.8(7) . . ? C36 C37 C38 120.1(7) . . ? C37 C38 C39 119.5(6) . . ? C34 C39 C38 120.9(5) . . ? O1 C41 C42 107.4(5) . . ? C43 C42 C41 106.0(6) . . ? C44 C43 C42 109.4(7) . . ? C43 C44 O1 110.7(6) . . ? O2 C45 C46 108.0(5) . . ? C47 C46 C45 104.8(5) . . ? C48 C47 C46 109.6(6) . . ? C47 C48 O2 109.9(6) . . ? N3 Li1 N1 144.9(4) . . ? N3 Li1 N2 141.4(3) . . ? N1 Li1 N2 66.2(2) . . ? N3 Li1 N4 66.0(2) . . ? N1 Li1 N4 142.2(3) . . ? N2 Li1 N4 101.6(3) . . ? N3 Li1 C13 162.4(4) . . ? N1 Li1 C13 32.84(14) . . ? N2 Li1 C13 33.38(13) . . ? N4 Li1 C13 126.8(3) . . ? N3 Li1 C33 32.74(15) . . ? N1 Li1 C33 162.5(4) . . ? N2 Li1 C33 126.8(3) . . ? N4 Li1 C33 33.29(14) . . ? C13 Li1 C33 158.4(3) . . ? N3 Li1 Li2 106.9(3) . . ? N1 Li1 Li2 108.2(3) . . ? N2 Li1 Li2 51.1(2) . . ? N4 Li1 Li2 50.5(2) . . ? C13 Li1 Li2 79.6(3) . . ? C33 Li1 Li2 78.8(3) . . ? N4 Li2 N4 80.2(4) 2_656 . ? N4 Li2 N2 112.84(11) 2_656 2_656 ? N4 Li2 N2 141.55(11) . 2_656 ? N4 Li2 N2 141.55(11) 2_656 . ? N4 Li2 N2 112.84(11) . . ? N2 Li2 N2 80.0(4) 2_656 . ? N4 Li2 Li1 57.03(19) 2_656 2_656 ? N4 Li2 Li1 124.3(4) . 2_656 ? N2 Li2 Li1 55.81(18) 2_656 2_656 ? N2 Li2 Li1 122.8(4) . 2_656 ? N4 Li2 Li1 124.3(4) 2_656 . ? N4 Li2 Li1 57.03(19) . . ? N2 Li2 Li1 122.8(4) 2_656 . ? N2 Li2 Li1 55.81(18) . . ? Li1 Li2 Li1 178.5(5) 2_656 . ? N4 Li2 Si2 40.12(19) 2_656 . ? N4 Li2 Si2 40.12(19) . . ? N2 Li2 Si2 139.99(18) 2_656 . ? N2 Li2 Si2 139.99(18) . . ? Li1 Li2 Si2 90.7(3) 2_656 . ? Li1 Li2 Si2 90.7(3) . . ? N4 Li2 Si1 139.88(19) 2_656 . ? N4 Li2 Si1 139.88(19) . . ? N2 Li2 Si1 40.01(18) 2_656 . ? N2 Li2 Si1 40.01(18) . . ? Li1 Li2 Si1 89.3(3) 2_656 . ? Li1 Li2 Si1 89.3(3) . . ? Si2 Li2 Si1 180.0 . . ? O1 Li3 O1 109.5(8) . 2_756 ? O1 Li3 O2 108.83(17) . . ? O1 Li3 O2 110.09(17) 2_756 . ? O1 Li3 O2 110.09(17) . 2_756 ? O1 Li3 O2 108.83(17) 2_756 2_756 ? O2 Li3 O2 109.5(8) . 2_756 ? C41 O1 C44 105.9(5) . . ? C41 O1 Li3 126.7(5) . . ? C44 O1 Li3 127.2(5) . . ? C45 O2 C48 106.9(4) . . ? C45 O2 Li3 127.3(4) . . ? C48 O2 Li3 125.6(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.267 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.038 # Attachment 'compound4.cif' data_s094p _database_code_depnum_ccdc_archive 'CCDC 288541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H68 Li4 N8 Si2' _chemical_formula_weight 841.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.050(2) _cell_length_b 16.884(3) _cell_length_c 21.878(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5189.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5701 _cell_measurement_theta_min 2.413 _cell_measurement_theta_max 21.254 _exptl_crystal_description Block _exptl_crystal_colour Colorless _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 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7133 _exptl_absorpt_correction_T_max 0.9587 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.72 _diffrn_reflns_number 20639 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6917 _reflns_number_gt 6319 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+3.8535P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(18) _refine_ls_number_reflns 6917 _refine_ls_number_parameters 559 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.1757 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.34461(9) 0.66348(7) 0.82958(7) 0.0314(3) Uani 1 1 d . . . N1 N 0.2784(3) 0.6154(2) 0.6613(2) 0.0369(10) Uani 1 1 d . . . N2 N 0.2906(3) 0.6341(2) 0.76305(19) 0.0312(9) Uani 1 1 d . . . N3 N 0.3248(2) 0.5760(2) 0.86924(19) 0.0296(9) Uani 1 1 d . . . N4 N 0.3434(3) 0.4639(2) 0.9244(2) 0.0346(10) Uani 1 1 d . . . C1 C 0.2601(4) 0.6347(3) 0.5962(3) 0.0414(13) Uani 1 1 d . . . C2 C 0.2608(6) 0.5535(4) 0.5648(3) 0.072(2) Uani 1 1 d . . . H2A H 0.2130 0.5203 0.5829 0.108 Uiso 1 1 calc R . . H2B H 0.3222 0.5294 0.5698 0.108 Uiso 1 1 calc R . . H2C H 0.2477 0.5601 0.5220 0.108 Uiso 1 1 calc R . . C3 C 0.3363(5) 0.6860(5) 0.5659(3) 0.073(2) Uani 1 1 d . . . H3A H 0.3371 0.7374 0.5847 0.109 Uiso 1 1 calc R . . H3B H 0.3223 0.6915 0.5232 0.109 Uiso 1 1 calc R . . H3C H 0.3975 0.6614 0.5708 0.109 Uiso 1 1 calc R . . C4 C 0.1632(4) 0.6715(3) 0.5887(3) 0.0513(15) Uani 1 1 d . . . H4A H 0.1621 0.7222 0.6085 0.077 Uiso 1 1 calc R . . H4B H 0.1161 0.6377 0.6069 0.077 Uiso 1 1 calc R . . H4C H 0.1496 0.6780 0.5460 0.077 Uiso 1 1 calc R . . C5 C 0.2876(3) 0.6652(3) 0.7063(2) 0.0308(11) Uani 1 1 d . . . C6 C 0.2955(4) 0.7544(3) 0.7001(2) 0.0408(13) Uani 1 1 d . . . C7 C 0.3803(5) 0.7899(4) 0.6864(3) 0.0603(17) Uani 1 1 d . . . H7A H 0.4338 0.7589 0.6789 0.072 Uiso 1 1 calc R . . C8 C 0.3872(9) 0.8712(5) 0.6837(4) 0.099(3) Uani 1 1 d . . . H8A H 0.4461 0.8948 0.6772 0.119 Uiso 1 1 calc R . . C9 C 0.3094(11) 0.9167(5) 0.6903(5) 0.112(4) Uani 1 1 d . . . H9A H 0.3140 0.9713 0.6856 0.134 Uiso 1 1 calc R . . C10 C 0.2234(8) 0.8828(5) 0.7039(4) 0.099(3) Uani 1 1 d . . . H10A H 0.1699 0.9144 0.7093 0.119 Uiso 1 1 calc R . . C11 C 0.2162(5) 0.8006(4) 0.7097(3) 0.0677(19) Uani 1 1 d . . . H11A H 0.1583 0.7774 0.7200 0.081 Uiso 1 1 calc R . . C12 C 0.4731(4) 0.6901(4) 0.8199(3) 0.064(2) Uani 1 1 d . . . H12A H 0.4853 0.7401 0.8392 0.096 Uiso 1 1 calc R . . H12B H 0.4878 0.6939 0.7771 0.096 Uiso 1 1 calc R . . H12C H 0.5122 0.6500 0.8383 0.096 Uiso 1 1 calc R . . C13 C 0.2837(5) 0.7470(3) 0.8687(3) 0.0607(17) Uani 1 1 d . . . H13A H 0.3293 0.7874 0.8784 0.091 Uiso 1 1 calc R . . H13B H 0.2545 0.7283 0.9056 0.091 Uiso 1 1 calc R . . H13C H 0.2357 0.7686 0.8422 0.091 Uiso 1 1 calc R . . C14 C 0.3734(3) 0.5373(3) 0.9129(2) 0.0280(11) Uani 1 1 d . . . C15 C 0.4565(3) 0.5770(3) 0.9427(2) 0.0333(11) Uani 1 1 d . . . C16 C 0.4419(4) 0.6380(3) 0.9831(3) 0.0447(13) Uani 1 1 d . . . H16A H 0.3799 0.6528 0.9927 0.054 Uiso 1 1 calc R . . C17 C 0.5162(5) 0.6777(4) 1.0098(3) 0.0637(19) Uani 1 1 d . . . H17A H 0.5050 0.7188 1.0373 0.076 Uiso 1 1 calc R . . C18 C 0.6090(6) 0.6554(4) 0.9950(4) 0.077(2) Uani 1 1 d . . . H18A H 0.6602 0.6808 1.0134 0.092 Uiso 1 1 calc R . . C19 C 0.6249(4) 0.5966(4) 0.9537(3) 0.0575(18) Uani 1 1 d . . . H19A H 0.6868 0.5836 0.9426 0.069 Uiso 1 1 calc R . . C20 C 0.5497(4) 0.5564(3) 0.9284(3) 0.0457(14) Uani 1 1 d . . . H20A H 0.5612 0.5149 0.9015 0.055 Uiso 1 1 calc R . . C21 C 0.3760(4) 0.4099(3) 0.9728(3) 0.0457(14) Uani 1 1 d . . . C22 C 0.2900(5) 0.3569(4) 0.9844(4) 0.085(3) Uani 1 1 d . . . H22A H 0.2711 0.3321 0.9469 0.127 Uiso 1 1 calc R . . H22B H 0.2384 0.3884 0.9999 0.127 Uiso 1 1 calc R . . H22C H 0.3065 0.3170 1.0139 0.127 Uiso 1 1 calc R . . C23 C 0.4042(5) 0.4492(4) 1.0333(3) 0.0624(18) Uani 1 1 d . . . H23A H 0.4584 0.4828 1.0268 0.094 Uiso 1 1 calc R . . H23B H 0.4199 0.4091 1.0627 0.094 Uiso 1 1 calc R . . H23C H 0.3519 0.4803 1.0482 0.094 Uiso 1 1 calc R . . C24 C 0.4580(5) 0.3594(4) 0.9503(4) 0.074(2) Uani 1 1 d . . . H24A H 0.5127 0.3923 0.9436 0.111 Uiso 1 1 calc R . . H24B H 0.4403 0.3340 0.9128 0.111 Uiso 1 1 calc R . . H24C H 0.4728 0.3199 0.9804 0.111 Uiso 1 1 calc R . . Si2 Si 0.11555(8) 0.41278(8) 0.79451(7) 0.0314(3) Uani 1 1 d . . . N5 N 0.3827(3) 0.4285(2) 0.74341(19) 0.0296(9) Uani 1 1 d . . . N6 N 0.2286(2) 0.4382(2) 0.76733(19) 0.0280(9) Uani 1 1 d . . . N7 N 0.1069(2) 0.4869(2) 0.84691(19) 0.0312(9) Uani 1 1 d . . . N8 N 0.0798(3) 0.5330(2) 0.9428(2) 0.0374(10) Uani 1 1 d . . . C25 C 0.4724(3) 0.4009(3) 0.7150(2) 0.0319(11) Uani 1 1 d . . . C26 C 0.5468(5) 0.4435(10) 0.7470(8) 0.256(12) Uani 1 1 d . . . H26A H 0.5517 0.4239 0.7881 0.384 Uiso 1 1 calc R . . H26B H 0.5316 0.4990 0.7479 0.384 Uiso 1 1 calc R . . H26C H 0.6063 0.4359 0.7263 0.384 Uiso 1 1 calc R . . C27 C 0.4934(7) 0.3193(6) 0.7176(11) 0.270(13) Uani 1 1 d . . . H27A H 0.4869 0.3009 0.7589 0.405 Uiso 1 1 calc R . . H27B H 0.5575 0.3106 0.7039 0.405 Uiso 1 1 calc R . . H27C H 0.4501 0.2908 0.6917 0.405 Uiso 1 1 calc R . . C28 C 0.4774(7) 0.4297(13) 0.6540(5) 0.277(13) Uani 1 1 d . . . H28A H 0.5358 0.4125 0.6355 0.415 Uiso 1 1 calc R . . H28B H 0.4753 0.4866 0.6543 0.415 Uiso 1 1 calc R . . H28C H 0.4245 0.4096 0.6310 0.415 Uiso 1 1 calc R . . C29 C 0.2966(3) 0.3960(2) 0.7402(2) 0.0255(10) Uani 1 1 d . . . C30 C 0.2740(3) 0.3207(3) 0.7077(2) 0.0298(11) Uani 1 1 d . . . C31 C 0.2917(3) 0.2465(3) 0.7332(3) 0.0369(12) Uani 1 1 d . . . H31A H 0.3167 0.2430 0.7725 0.044 Uiso 1 1 calc R . . C32 C 0.2723(4) 0.1775(3) 0.7004(4) 0.0508(17) Uani 1 1 d . . . H32A H 0.2848 0.1282 0.7176 0.061 Uiso 1 1 calc R . . C33 C 0.2350(4) 0.1825(3) 0.6432(3) 0.0520(17) Uani 1 1 d . . . H33A H 0.2230 0.1365 0.6212 0.062 Uiso 1 1 calc R . . C34 C 0.2151(4) 0.2541(4) 0.6178(3) 0.0526(16) Uani 1 1 d . . . H34A H 0.1886 0.2568 0.5789 0.063 Uiso 1 1 calc R . . C35 C 0.2342(4) 0.3229(3) 0.6496(3) 0.0433(14) Uani 1 1 d . . . H35A H 0.2202 0.3716 0.6318 0.052 Uiso 1 1 calc R . . C36 C 0.1145(4) 0.3128(3) 0.8309(3) 0.0552(16) Uani 1 1 d . . . H36A H 0.0697 0.2794 0.8100 0.083 Uiso 1 1 calc R . . H36B H 0.0963 0.3178 0.8730 0.083 Uiso 1 1 calc R . . H36C H 0.1769 0.2899 0.8284 0.083 Uiso 1 1 calc R . . C37 C 0.0248(4) 0.4139(4) 0.7328(3) 0.0608(19) Uani 1 1 d . . . H37A H -0.0047 0.3627 0.7300 0.091 Uiso 1 1 calc R . . H37B H 0.0548 0.4264 0.6946 0.091 Uiso 1 1 calc R . . H37C H -0.0227 0.4530 0.7419 0.091 Uiso 1 1 calc R . . C38 C 0.0457(3) 0.4982(3) 0.8947(2) 0.0305(11) Uani 1 1 d . . . C39 C -0.0546(3) 0.4685(3) 0.8862(2) 0.0312(11) Uani 1 1 d . . . C40 C -0.0829(4) 0.3971(3) 0.9101(3) 0.0424(13) Uani 1 1 d . . . H40A H -0.0407 0.3679 0.9339 0.051 Uiso 1 1 calc R . . C41 C -0.1738(4) 0.3679(4) 0.8991(3) 0.0545(17) Uani 1 1 d . . . H41A H -0.1919 0.3190 0.9149 0.065 Uiso 1 1 calc R . . C42 C -0.2366(4) 0.4113(5) 0.8651(3) 0.0616(19) Uani 1 1 d . . . H42A H -0.2980 0.3924 0.8587 0.074 Uiso 1 1 calc R . . C43 C -0.2098(4) 0.4819(4) 0.8406(3) 0.0603(17) Uani 1 1 d . . . H43A H -0.2526 0.5109 0.8172 0.072 Uiso 1 1 calc R . . C44 C -0.1195(3) 0.5105(4) 0.8505(3) 0.0450(14) Uani 1 1 d . . . H44A H -0.1014 0.5585 0.8331 0.054 Uiso 1 1 calc R . . C45 C 0.0286(4) 0.5575(4) 0.9982(3) 0.0458(14) Uani 1 1 d . . . C46 C 0.0983(5) 0.6111(4) 1.0316(3) 0.069(2) Uani 1 1 d . . . H46A H 0.1105 0.6574 1.0074 0.103 Uiso 1 1 calc R . . H46B H 0.1568 0.5832 1.0385 0.103 Uiso 1 1 calc R . . H46C H 0.0715 0.6267 1.0702 0.103 Uiso 1 1 calc R . . C47 C 0.0120(6) 0.4857(4) 1.0400(3) 0.072(2) Uani 1 1 d . . . H47A H -0.0324 0.4501 1.0210 0.108 Uiso 1 1 calc R . . H47B H -0.0132 0.5033 1.0785 0.108 Uiso 1 1 calc R . . H47C H 0.0713 0.4587 1.0467 0.108 Uiso 1 1 calc R . . C48 C -0.0621(5) 0.6025(5) 0.9862(4) 0.072(2) Uani 1 1 d . . . H48A H -0.0488 0.6470 0.9602 0.109 Uiso 1 1 calc R . . H48B H -0.0881 0.6209 1.0242 0.109 Uiso 1 1 calc R . . H48C H -0.1072 0.5683 0.9664 0.109 Uiso 1 1 calc R . . Li1 Li 0.3121(6) 0.5290(5) 0.7177(4) 0.041(2) Uani 1 1 d . . . Li2 Li 0.2088(6) 0.5113(6) 0.9131(4) 0.044(2) Uani 1 1 d . . . Li3 Li 0.2047(6) 0.5555(5) 0.8057(4) 0.037(2) Uani 1 1 d . . . Li4 Li 0.3387(6) 0.4607(5) 0.8299(4) 0.0372(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0349(7) 0.0307(6) 0.0287(7) 0.0011(6) -0.0030(6) -0.0075(5) N1 0.046(3) 0.036(2) 0.029(3) 0.002(2) -0.003(2) 0.0090(19) N2 0.036(2) 0.0309(19) 0.026(2) 0.0012(18) -0.0076(18) -0.0046(17) N3 0.0250(19) 0.036(2) 0.028(2) 0.0003(19) -0.0053(18) -0.0047(16) N4 0.037(2) 0.037(2) 0.030(2) 0.002(2) 0.0003(19) -0.0030(19) C1 0.055(3) 0.041(3) 0.029(3) 0.002(2) -0.004(3) 0.010(3) C2 0.118(6) 0.069(4) 0.029(4) -0.011(3) -0.020(4) 0.032(4) C3 0.068(4) 0.114(6) 0.037(4) 0.013(4) 0.002(3) 0.007(4) C4 0.063(4) 0.047(3) 0.044(4) 0.014(3) -0.014(3) -0.002(3) C5 0.028(2) 0.033(3) 0.031(3) 0.006(2) 0.002(2) 0.0031(19) C6 0.061(3) 0.039(3) 0.023(3) 0.009(2) 0.001(3) 0.004(3) C7 0.081(4) 0.056(4) 0.044(4) 0.008(3) 0.009(3) -0.020(3) C8 0.172(10) 0.061(5) 0.065(6) 0.014(4) -0.004(6) -0.057(6) C9 0.225(13) 0.038(4) 0.073(7) 0.005(4) -0.003(8) -0.013(6) C10 0.166(9) 0.054(5) 0.078(6) -0.007(4) -0.023(6) 0.044(5) C11 0.098(5) 0.056(4) 0.049(4) -0.004(3) -0.019(4) 0.018(4) C12 0.041(3) 0.083(4) 0.068(5) 0.033(4) -0.006(3) -0.032(3) C13 0.093(5) 0.041(3) 0.048(4) -0.010(3) -0.022(4) 0.010(3) C14 0.023(2) 0.039(3) 0.021(3) -0.004(2) 0.004(2) 0.001(2) C15 0.039(3) 0.038(3) 0.023(3) 0.003(2) -0.005(2) -0.001(2) C16 0.056(3) 0.046(3) 0.033(3) -0.008(3) -0.013(3) 0.000(3) C17 0.080(5) 0.054(4) 0.057(5) -0.010(3) -0.028(4) -0.013(4) C18 0.089(6) 0.062(4) 0.080(6) 0.013(4) -0.048(5) -0.032(4) C19 0.035(3) 0.064(4) 0.074(5) 0.015(4) -0.014(3) -0.008(3) C20 0.048(3) 0.046(3) 0.043(4) -0.002(3) -0.010(3) 0.002(3) C21 0.057(3) 0.039(3) 0.042(4) 0.008(3) -0.020(3) -0.008(3) C22 0.082(5) 0.078(5) 0.095(6) 0.061(5) -0.023(5) -0.021(4) C23 0.092(5) 0.061(4) 0.034(4) 0.007(3) -0.012(4) -0.004(4) C24 0.086(5) 0.061(4) 0.075(5) 0.015(4) -0.015(4) 0.034(4) Si2 0.0246(6) 0.0352(7) 0.0344(8) -0.0053(6) 0.0027(6) -0.0041(5) N5 0.030(2) 0.0262(19) 0.033(2) -0.0001(18) 0.0026(18) -0.0005(16) N6 0.0249(19) 0.0296(19) 0.030(2) -0.0033(18) 0.0028(18) -0.0001(16) N7 0.0243(19) 0.036(2) 0.034(3) -0.0031(18) 0.0084(17) -0.0038(16) N8 0.034(2) 0.045(2) 0.033(3) -0.009(2) 0.005(2) -0.0026(19) C25 0.028(2) 0.035(3) 0.033(3) 0.002(2) 0.004(2) 0.000(2) C26 0.028(4) 0.38(2) 0.36(2) -0.294(19) 0.056(8) -0.051(7) C27 0.087(7) 0.095(7) 0.63(4) 0.114(14) 0.183(14) 0.052(6) C28 0.091(8) 0.67(4) 0.065(7) 0.101(14) 0.056(6) 0.175(15) C29 0.030(2) 0.024(2) 0.022(2) 0.0081(19) -0.004(2) -0.0016(19) C30 0.022(2) 0.040(3) 0.028(3) 0.000(2) 0.005(2) 0.0000(19) C31 0.033(2) 0.037(3) 0.041(3) -0.002(2) 0.007(2) 0.001(2) C32 0.034(3) 0.031(3) 0.087(5) -0.003(3) 0.019(3) 0.001(2) C33 0.044(3) 0.045(3) 0.066(5) -0.026(3) 0.020(3) -0.014(3) C34 0.049(3) 0.067(4) 0.042(4) -0.015(3) -0.003(3) -0.022(3) C35 0.040(3) 0.046(3) 0.043(4) -0.002(3) 0.000(3) -0.012(2) C36 0.060(4) 0.041(3) 0.064(4) -0.001(3) 0.019(4) -0.007(3) C37 0.033(3) 0.079(4) 0.070(5) -0.032(4) -0.008(3) 0.000(3) C38 0.026(2) 0.032(2) 0.033(3) 0.002(2) 0.009(2) 0.0022(19) C39 0.025(2) 0.035(3) 0.033(3) -0.006(2) 0.004(2) 0.000(2) C40 0.040(3) 0.053(3) 0.034(3) -0.007(3) 0.004(3) 0.001(2) C41 0.056(4) 0.061(4) 0.047(4) -0.014(3) 0.017(3) -0.031(3) C42 0.034(3) 0.097(5) 0.054(4) -0.022(4) 0.000(3) -0.017(3) C43 0.036(3) 0.090(5) 0.055(4) -0.011(4) -0.012(3) -0.001(3) C44 0.036(3) 0.063(4) 0.037(3) 0.002(3) 0.001(2) 0.004(3) C45 0.041(3) 0.056(3) 0.041(4) -0.010(3) 0.006(3) -0.001(3) C46 0.072(4) 0.079(5) 0.056(5) -0.032(4) 0.005(4) 0.002(4) C47 0.099(5) 0.074(5) 0.042(4) 0.002(4) 0.017(4) -0.012(4) C48 0.057(4) 0.098(5) 0.063(5) -0.036(4) 0.006(4) 0.011(4) Li1 0.047(5) 0.036(4) 0.041(6) 0.016(4) -0.009(4) 0.002(4) Li2 0.035(5) 0.063(6) 0.034(5) 0.005(5) 0.003(4) -0.008(4) Li3 0.036(4) 0.032(4) 0.042(6) -0.002(4) 0.002(4) -0.013(3) Li4 0.038(4) 0.044(4) 0.030(5) 0.003(4) -0.009(4) 0.003(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 Si1 N2 1.715(4) . ? Si1 N3 1.735(4) . ? Si1 C13 1.859(6) . ? Si1 C12 1.873(5) . ? Si1 Li3 2.731(8) . ? N1 C5 1.300(6) . ? N1 C1 1.483(7) . ? N1 Li1 1.969(9) . ? N2 C5 1.350(6) . ? N2 Li3 2.022(9) . ? N2 Li1 2.056(10) . ? N3 C14 1.344(6) . ? N3 Li4 2.137(9) . ? N3 Li2 2.184(10) . ? N3 Li3 2.213(9) . ? N4 C14 1.333(6) . ? N4 C21 1.469(7) . ? N4 Li2 2.070(10) . ? N4 Li4 2.071(11) . ? C1 C4 1.506(8) . ? C1 C3 1.528(9) . ? C1 C2 1.534(8) . ? C5 C6 1.516(7) . ? C5 Li1 2.339(9) . ? C6 C7 1.367(8) . ? C6 C11 1.376(8) . ? C7 C8 1.378(10) . ? C8 C9 1.343(14) . ? C9 C10 1.370(14) . ? C10 C11 1.397(10) . ? C14 C15 1.497(7) . ? C14 Li4 2.282(10) . ? C14 Li2 2.354(9) . ? C15 C16 1.373(7) . ? C15 C20 1.389(7) . ? C16 C17 1.372(8) . ? C17 C18 1.395(10) . ? C18 C19 1.361(10) . ? C19 C20 1.372(8) . ? C21 C24 1.515(9) . ? C21 C22 1.525(8) . ? C21 C23 1.533(8) . ? Si2 N7 1.702(4) . ? Si2 N6 1.749(4) . ? Si2 C37 1.857(6) . ? Si2 C36 1.866(6) . ? Si2 Li3 2.727(8) . ? N5 C29 1.329(6) . ? N5 C25 1.480(6) . ? N5 Li1 2.044(9) . ? N5 Li4 2.063(10) . ? N6 C29 1.331(6) . ? N6 Li4 2.100(9) . ? N6 Li3 2.177(9) . ? N6 Li1 2.215(9) . ? N7 C38 1.367(6) . ? N7 Li3 2.011(9) . ? N7 Li2 2.077(10) . ? N8 C38 1.297(6) . ? N8 C45 1.469(7) . ? N8 Li2 1.959(10) . ? C25 C27 1.411(10) . ? C25 C28 1.423(12) . ? C25 C26 1.449(10) . ? C29 C30 1.491(6) . ? C29 Li1 2.308(9) . ? C29 Li4 2.322(10) . ? C30 C35 1.390(7) . ? C30 C31 1.393(7) . ? C31 C32 1.396(8) . ? C32 C33 1.360(9) . ? C33 C34 1.360(9) . ? C34 C35 1.380(8) . ? C38 C39 1.508(6) . ? C38 Li2 2.337(10) . ? C39 C40 1.373(7) . ? C39 C44 1.394(7) . ? C40 C41 1.390(8) . ? C41 C42 1.366(9) . ? C42 C43 1.361(10) . ? C43 C44 1.375(8) . ? C45 C48 1.507(8) . ? C45 C46 1.522(9) . ? C45 C47 1.537(9) . ? Li1 Li3 2.487(13) . ? Li1 Li4 2.737(13) . ? Li2 Li3 2.466(13) . ? Li2 Li4 2.715(13) . ? Li3 Li4 2.526(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Si1 N3 96.15(19) . . ? N2 Si1 C13 114.0(2) . . ? N3 Si1 C13 110.0(3) . . ? N2 Si1 C12 113.6(3) . . ? N3 Si1 C12 114.6(2) . . ? C13 Si1 C12 108.3(3) . . ? N2 Si1 Li3 47.6(2) . . ? N3 Si1 Li3 54.0(2) . . ? C13 Si1 Li3 105.3(3) . . ? C12 Si1 Li3 146.3(3) . . ? C5 N1 C1 127.0(4) . . ? C5 N1 Li1 88.9(4) . . ? C1 N1 Li1 143.7(4) . . ? C5 N2 Si1 133.1(3) . . ? C5 N2 Li3 131.4(4) . . ? Si1 N2 Li3 93.6(3) . . ? C5 N2 Li1 84.0(4) . . ? Si1 N2 Li1 126.5(3) . . ? Li3 N2 Li1 75.2(4) . . ? C14 N3 Si1 133.5(3) . . ? C14 N3 Li4 78.3(4) . . ? Si1 N3 Li4 124.0(3) . . ? C14 N3 Li2 79.9(4) . . ? Si1 N3 Li2 139.9(3) . . ? Li4 N3 Li2 77.9(4) . . ? C14 N3 Li3 139.2(4) . . ? Si1 N3 Li3 86.6(3) . . ? Li4 N3 Li3 71.0(3) . . ? Li2 N3 Li3 68.2(3) . . ? C14 N4 C21 127.9(4) . . ? C14 N4 Li2 84.6(4) . . ? C21 N4 Li2 127.7(4) . . ? C14 N4 Li4 81.1(4) . . ? C21 N4 Li4 135.5(4) . . ? Li2 N4 Li4 82.0(4) . . ? N1 C1 C4 110.6(5) . . ? N1 C1 C3 114.8(5) . . ? C4 C1 C3 110.7(5) . . ? N1 C1 C2 103.5(4) . . ? C4 C1 C2 109.0(5) . . ? C3 C1 C2 107.9(6) . . ? N1 C5 N2 116.6(4) . . ? N1 C5 C6 125.6(5) . . ? N2 C5 C6 117.8(5) . . ? N1 C5 Li1 57.3(3) . . ? N2 C5 Li1 60.9(3) . . ? C6 C5 Li1 167.3(4) . . ? C7 C6 C11 119.4(6) . . ? C7 C6 C5 121.2(5) . . ? C11 C6 C5 119.4(5) . . ? C6 C7 C8 120.5(8) . . ? C9 C8 C7 120.6(9) . . ? C8 C9 C10 120.1(8) . . ? C9 C10 C11 120.0(8) . . ? C6 C11 C10 119.3(8) . . ? N4 C14 N3 115.3(4) . . ? N4 C14 C15 125.4(4) . . ? N3 C14 C15 119.3(4) . . ? N4 C14 Li4 63.7(3) . . ? N3 C14 Li4 66.5(3) . . ? C15 C14 Li4 140.1(4) . . ? N4 C14 Li2 61.1(3) . . ? N3 C14 Li2 66.0(3) . . ? C15 C14 Li2 148.2(4) . . ? Li4 C14 Li2 71.7(4) . . ? C16 C15 C20 118.2(5) . . ? C16 C15 C14 120.0(4) . . ? C20 C15 C14 121.7(4) . . ? C17 C16 C15 121.8(6) . . ? C16 C17 C18 118.7(6) . . ? C19 C18 C17 120.3(6) . . ? C18 C19 C20 120.2(6) . . ? C19 C20 C15 120.7(6) . . ? N4 C21 C24 110.7(5) . . ? N4 C21 C22 103.7(4) . . ? C24 C21 C22 109.0(6) . . ? N4 C21 C23 115.7(5) . . ? C24 C21 C23 109.1(5) . . ? C22 C21 C23 108.3(6) . . ? N7 Si2 N6 96.52(18) . . ? N7 Si2 C37 115.7(2) . . ? N6 Si2 C37 112.0(3) . . ? N7 Si2 C36 112.2(3) . . ? N6 Si2 C36 111.9(2) . . ? C37 Si2 C36 108.3(3) . . ? N7 Si2 Li3 47.3(2) . . ? N6 Si2 Li3 52.9(2) . . ? C37 Si2 Li3 111.8(3) . . ? C36 Si2 Li3 139.9(3) . . ? C29 N5 C25 128.5(4) . . ? C29 N5 Li1 83.5(3) . . ? C25 N5 Li1 123.9(4) . . ? C29 N5 Li4 83.4(4) . . ? C25 N5 Li4 136.3(4) . . ? Li1 N5 Li4 83.6(4) . . ? C29 N6 Si2 132.3(3) . . ? C29 N6 Li4 81.9(4) . . ? Si2 N6 Li4 119.4(3) . . ? C29 N6 Li3 140.2(4) . . ? Si2 N6 Li3 87.2(3) . . ? Li4 N6 Li3 72.4(3) . . ? C29 N6 Li1 76.8(3) . . ? Si2 N6 Li1 144.8(3) . . ? Li4 N6 Li1 78.7(4) . . ? Li3 N6 Li1 68.9(4) . . ? C38 N7 Si2 131.5(3) . . ? C38 N7 Li3 133.8(4) . . ? Si2 N7 Li3 94.2(3) . . ? C38 N7 Li2 82.7(4) . . ? Si2 N7 Li2 124.5(3) . . ? Li3 N7 Li2 74.2(4) . . ? C38 N8 C45 128.0(4) . . ? C38 N8 Li2 89.3(4) . . ? C45 N8 Li2 141.2(5) . . ? C27 C25 C28 111.1(12) . . ? C27 C25 C26 108.4(11) . . ? C28 C25 C26 104.4(11) . . ? C27 C25 N5 118.0(5) . . ? C28 C25 N5 109.2(5) . . ? C26 C25 N5 104.8(5) . . ? N5 C29 N6 114.1(4) . . ? N5 C29 C30 124.8(4) . . ? N6 C29 C30 121.0(4) . . ? N5 C29 Li1 61.6(3) . . ? N6 C29 Li1 69.1(3) . . ? C30 C29 Li1 138.4(4) . . ? N5 C29 Li4 62.0(3) . . ? N6 C29 Li4 63.5(3) . . ? C30 C29 Li4 149.1(4) . . ? Li1 C29 Li4 72.5(3) . . ? C35 C30 C31 117.5(5) . . ? C35 C30 C29 119.9(4) . . ? C31 C30 C29 122.6(5) . . ? C30 C31 C32 120.7(6) . . ? C33 C32 C31 119.8(6) . . ? C32 C33 C34 120.7(5) . . ? C33 C34 C35 120.2(6) . . ? C34 C35 C30 121.1(6) . . ? N8 C38 N7 116.8(4) . . ? N8 C38 C39 126.6(4) . . ? N7 C38 C39 116.6(4) . . ? N8 C38 Li2 56.9(3) . . ? N7 C38 Li2 61.8(3) . . ? C39 C38 Li2 165.7(4) . . ? C40 C39 C44 118.2(5) . . ? C40 C39 C38 121.1(5) . . ? C44 C39 C38 120.6(4) . . ? C39 C40 C41 120.7(6) . . ? C42 C41 C40 119.8(6) . . ? C43 C42 C41 120.4(5) . . ? C42 C43 C44 120.1(6) . . ? C43 C44 C39 120.8(6) . . ? N8 C45 C48 114.3(5) . . ? N8 C45 C46 104.4(5) . . ? C48 C45 C46 109.1(5) . . ? N8 C45 C47 110.1(5) . . ? C48 C45 C47 112.0(5) . . ? C46 C45 C47 106.3(6) . . ? N1 Li1 N5 154.8(6) . . ? N1 Li1 N2 68.1(3) . . ? N5 Li1 N2 130.9(5) . . ? N1 Li1 N6 133.9(5) . . ? N5 Li1 N6 63.1(3) . . ? N2 Li1 N6 106.4(5) . . ? N1 Li1 C29 146.3(5) . . ? N5 Li1 C29 34.9(2) . . ? N2 Li1 C29 136.3(5) . . ? N6 Li1 C29 34.14(19) . . ? N1 Li1 C5 33.8(2) . . ? N5 Li1 C5 156.5(5) . . ? N2 Li1 C5 35.0(2) . . ? N6 Li1 C5 130.9(4) . . ? C29 Li1 C5 164.8(5) . . ? N1 Li1 Li3 101.9(4) . . ? N5 Li1 Li3 103.3(4) . . ? N2 Li1 Li3 51.8(3) . . ? N6 Li1 Li3 54.8(3) . . ? C29 Li1 Li3 87.3(4) . . ? C5 Li1 Li3 79.4(4) . . ? N1 Li1 Li4 155.1(5) . . ? N5 Li1 Li4 48.5(3) . . ? N2 Li1 Li4 87.2(4) . . ? N6 Li1 Li4 48.8(3) . . ? C29 Li1 Li4 54.0(3) . . ? C5 Li1 Li4 122.0(5) . . ? Li3 Li1 Li4 57.6(3) . . ? N8 Li2 N4 151.4(5) . . ? N8 Li2 N7 68.3(3) . . ? N4 Li2 N7 129.5(5) . . ? N8 Li2 N3 137.9(5) . . ? N4 Li2 N3 64.2(3) . . ? N7 Li2 N3 107.9(4) . . ? N8 Li2 C38 33.7(2) . . ? N4 Li2 C38 151.7(5) . . ? N7 Li2 C38 35.5(2) . . ? N3 Li2 C38 134.7(5) . . ? N8 Li2 C14 151.0(5) . . ? N4 Li2 C14 34.3(2) . . ? N7 Li2 C14 135.4(5) . . ? N3 Li2 C14 34.2(2) . . ? C38 Li2 C14 168.7(5) . . ? N8 Li2 Li3 103.8(4) . . ? N4 Li2 Li3 104.6(4) . . ? N7 Li2 Li3 51.7(3) . . ? N3 Li2 Li3 56.5(3) . . ? C38 Li2 Li3 80.9(4) . . ? C14 Li2 Li3 88.0(4) . . ? N8 Li2 Li4 154.5(5) . . ? N4 Li2 Li4 49.0(3) . . ? N7 Li2 Li4 86.2(4) . . ? N3 Li2 Li4 50.3(3) . . ? C38 Li2 Li4 120.9(4) . . ? C14 Li2 Li4 52.9(3) . . ? Li3 Li2 Li4 58.1(3) . . ? N7 Li3 N2 173.2(5) . . ? N7 Li3 N6 75.8(3) . . ? N2 Li3 N6 109.1(4) . . ? N7 Li3 N3 109.2(4) . . ? N2 Li3 N3 74.5(3) . . ? N6 Li3 N3 105.5(4) . . ? N7 Li3 Li2 54.1(3) . . ? N2 Li3 Li2 128.6(4) . . ? N6 Li3 Li2 95.1(4) . . ? N3 Li3 Li2 55.3(3) . . ? N7 Li3 Li1 131.2(4) . . ? N2 Li3 Li1 53.0(3) . . ? N6 Li3 Li1 56.3(3) . . ? N3 Li3 Li1 93.0(4) . . ? Li2 Li3 Li1 132.0(5) . . ? N7 Li3 Li4 92.9(4) . . ? N2 Li3 Li4 93.9(4) . . ? N6 Li3 Li4 52.4(3) . . ? N3 Li3 Li4 53.1(3) . . ? Li2 Li3 Li4 65.9(4) . . ? Li1 Li3 Li4 66.2(4) . . ? N7 Li3 Si2 38.50(17) . . ? N2 Li3 Si2 144.4(4) . . ? N6 Li3 Si2 39.86(16) . . ? N3 Li3 Si2 123.0(4) . . ? Li2 Li3 Si2 80.1(3) . . ? Li1 Li3 Si2 92.9(3) . . ? Li4 Li3 Si2 78.6(3) . . ? N7 Li3 Si1 142.2(4) . . ? N2 Li3 Si1 38.80(18) . . ? N6 Li3 Si1 124.8(4) . . ? N3 Li3 Si1 39.36(16) . . ? Li2 Li3 Si1 90.2(3) . . ? Li1 Li3 Si1 80.3(3) . . ? Li4 Li3 Si1 81.2(3) . . ? Si2 Li3 Si1 159.7(4) . . ? N5 Li4 N4 155.9(5) . . ? N5 Li4 N6 64.9(3) . . ? N4 Li4 N6 132.8(5) . . ? N5 Li4 N3 129.6(4) . . ? N4 Li4 N3 65.0(3) . . ? N6 Li4 N3 111.1(4) . . ? N5 Li4 C14 144.6(4) . . ? N4 Li4 C14 35.3(2) . . ? N6 Li4 C14 141.2(4) . . ? N3 Li4 C14 35.2(2) . . ? N5 Li4 C29 34.6(2) . . ? N4 Li4 C29 149.8(4) . . ? N6 Li4 C29 34.6(2) . . ? N3 Li4 C29 138.2(4) . . ? C14 Li4 C29 173.4(4) . . ? N5 Li4 Li3 101.4(4) . . ? N4 Li4 Li3 102.6(4) . . ? N6 Li4 Li3 55.2(3) . . ? N3 Li4 Li3 55.9(3) . . ? C14 Li4 Li3 88.1(4) . . ? C29 Li4 Li3 86.1(4) . . ? N5 Li4 Li2 154.0(4) . . ? N4 Li4 Li2 49.0(3) . . ? N6 Li4 Li2 90.0(4) . . ? N3 Li4 Li2 51.8(3) . . ? C14 Li4 Li2 55.4(3) . . ? C29 Li4 Li2 122.9(4) . . ? Li3 Li4 Li2 56.0(3) . . ? N5 Li4 Li1 47.9(3) . . ? N4 Li4 Li1 152.8(4) . . ? N6 Li4 Li1 52.5(3) . . ? N3 Li4 Li1 88.0(3) . . ? C14 Li4 Li1 120.3(4) . . ? C29 Li4 Li1 53.5(3) . . ? Li3 Li4 Li1 56.2(3) . . ? Li2 Li4 Li1 112.2(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.534 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.056 # Attachment 'compound5.cif' data_s143p _database_code_depnum_ccdc_archive 'CCDC 288542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H54 Li2 N4 O2 Si2' _chemical_formula_weight 644.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 10.7863(17) _cell_length_b 10.3647(16) _cell_length_c 16.405(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.373(2) _cell_angle_gamma 90.00 _cell_volume 1833.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 4254 _cell_measurement_theta_min 2.325 _cell_measurement_theta_max 27.758 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7403 _exptl_absorpt_correction_T_max 0.9367 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.58 _diffrn_reflns_number 8663 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3220 _reflns_number_gt 2819 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+1.2315P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3220 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.54789(6) 0.59723(6) 0.15033(4) 0.0292(2) Uani 1 1 d . . . N1 N 0.57909(16) 0.61176(17) 0.04982(11) 0.0274(4) Uani 1 1 d . . . N2 N 0.39339(17) 0.53946(19) 0.14931(12) 0.0356(5) Uani 1 1 d . . . H2A H 0.3863 0.4603 0.1321 0.043 Uiso 1 1 calc R . . C1 C 0.66872(19) 0.6947(2) 0.01949(13) 0.0267(5) Uani 1 1 d . . . C2 C 0.7772(2) 0.7314(2) 0.06286(15) 0.0338(5) Uani 1 1 d . . . H2B H 0.7914 0.6988 0.1157 0.041 Uiso 1 1 calc R . . C3 C 0.8635(2) 0.8140(2) 0.02994(16) 0.0392(6) Uani 1 1 d . . . H3A H 0.9345 0.8368 0.0609 0.047 Uiso 1 1 calc R . . C4 C 0.8468(2) 0.8633(2) -0.04764(17) 0.0420(6) Uani 1 1 d . . . H4A H 0.9062 0.9187 -0.0699 0.050 Uiso 1 1 calc R . . C5 C 0.7414(2) 0.8297(2) -0.09187(15) 0.0375(6) Uani 1 1 d . . . H5A H 0.7285 0.8625 -0.1448 0.045 Uiso 1 1 calc R . . C6 C 0.6548(2) 0.7483(2) -0.05885(14) 0.0306(5) Uani 1 1 d . . . H6A H 0.5833 0.7277 -0.0901 0.037 Uiso 1 1 calc R . . C7 C 0.5624(2) 0.7473(3) 0.21257(16) 0.0437(6) Uani 1 1 d . . . H7A H 0.5195 0.7359 0.2634 0.066 Uiso 1 1 calc R . . H7B H 0.5257 0.8190 0.1826 0.066 Uiso 1 1 calc R . . H7C H 0.6493 0.7651 0.2241 0.066 Uiso 1 1 calc R . . C8 C 0.6377(2) 0.4694(3) 0.20593(16) 0.0424(6) Uani 1 1 d . . . H8A H 0.6425 0.4902 0.2636 0.064 Uiso 1 1 calc R . . H8B H 0.7208 0.4647 0.1847 0.064 Uiso 1 1 calc R . . H8C H 0.5966 0.3869 0.1984 0.064 Uiso 1 1 calc R . . C9 C 0.2799(2) 0.5950(2) 0.17048(13) 0.0294(5) Uani 1 1 d . . . C10 C 0.2616(2) 0.7276(2) 0.17204(14) 0.0345(5) Uani 1 1 d . . . H10A H 0.3274 0.7834 0.1602 0.041 Uiso 1 1 calc R . . C11 C 0.1471(2) 0.7781(2) 0.19095(15) 0.0392(6) Uani 1 1 d . . . H11A H 0.1359 0.8680 0.1917 0.047 Uiso 1 1 calc R . . C12 C 0.0493(2) 0.6986(3) 0.20872(15) 0.0411(6) Uani 1 1 d . . . H12A H -0.0281 0.7336 0.2219 0.049 Uiso 1 1 calc R . . C13 C 0.0663(2) 0.5668(2) 0.20689(15) 0.0377(6) Uani 1 1 d . . . H13A H -0.0001 0.5116 0.2187 0.045 Uiso 1 1 calc R . . C14 C 0.1797(2) 0.5152(2) 0.18797(14) 0.0333(5) Uani 1 1 d . . . H14A H 0.1898 0.4252 0.1868 0.040 Uiso 1 1 calc R . . O1 O 0.69260(14) 0.27390(15) 0.02635(10) 0.0323(4) Uani 1 1 d . . . C15 C 0.6410(2) 0.1477(2) 0.01416(15) 0.0369(6) Uani 1 1 d . . . H15A H 0.6920 0.1005 -0.0245 0.044 Uiso 1 1 calc R . . H15B H 0.5576 0.1563 -0.0103 0.044 Uiso 1 1 calc R . . C16 C 0.6331(3) 0.0701(3) 0.09159(18) 0.0528(7) Uani 1 1 d . . . H16A H 0.5977 -0.0139 0.0793 0.079 Uiso 1 1 calc R . . H16B H 0.5810 0.1150 0.1298 0.079 Uiso 1 1 calc R . . H16C H 0.7155 0.0593 0.1156 0.079 Uiso 1 1 calc R . . C17 C 0.8220(2) 0.2691(3) 0.04627(18) 0.0465(7) Uani 1 1 d . . . H17A H 0.8628 0.2078 0.0102 0.056 Uiso 1 1 calc R . . H17B H 0.8342 0.2389 0.1025 0.056 Uiso 1 1 calc R . . C18 C 0.8783(2) 0.3978(3) 0.03740(19) 0.0510(7) Uani 1 1 d . . . H18A H 0.9662 0.3930 0.0509 0.077 Uiso 1 1 calc R . . H18B H 0.8388 0.4580 0.0739 0.077 Uiso 1 1 calc R . . H18C H 0.8669 0.4271 -0.0184 0.077 Uiso 1 1 calc R . . Li1 Li 0.5976(3) 0.4296(3) -0.0084(2) 0.0299(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0301(4) 0.0291(4) 0.0284(3) -0.0022(3) 0.0018(3) -0.0030(3) N1 0.0267(9) 0.0267(10) 0.0288(10) -0.0012(8) 0.0009(8) -0.0025(7) N2 0.0334(11) 0.0279(10) 0.0462(12) -0.0090(9) 0.0117(9) -0.0020(8) C1 0.0241(11) 0.0231(11) 0.0332(12) -0.0027(9) 0.0028(9) 0.0036(8) C2 0.0300(12) 0.0355(13) 0.0360(13) 0.0024(10) -0.0009(10) 0.0014(10) C3 0.0266(12) 0.0415(14) 0.0493(15) 0.0018(12) -0.0008(11) -0.0037(10) C4 0.0350(13) 0.0369(14) 0.0548(16) 0.0063(12) 0.0137(12) -0.0043(11) C5 0.0450(14) 0.0325(13) 0.0354(13) 0.0045(10) 0.0091(11) 0.0042(11) C6 0.0325(12) 0.0262(12) 0.0329(12) -0.0032(9) -0.0006(10) 0.0032(9) C7 0.0489(16) 0.0433(15) 0.0390(14) -0.0114(11) 0.0024(12) -0.0093(12) C8 0.0418(14) 0.0468(15) 0.0384(14) 0.0086(12) -0.0021(11) -0.0023(12) C9 0.0321(12) 0.0320(12) 0.0243(11) -0.0019(9) 0.0044(9) -0.0013(9) C10 0.0391(13) 0.0339(13) 0.0307(12) -0.0003(10) 0.0030(10) -0.0035(10) C11 0.0473(15) 0.0337(13) 0.0363(13) -0.0041(10) -0.0037(11) 0.0093(11) C12 0.0348(13) 0.0513(16) 0.0371(13) -0.0041(12) -0.0001(11) 0.0103(11) C13 0.0302(13) 0.0450(15) 0.0378(13) 0.0018(11) 0.0023(10) -0.0019(10) C14 0.0357(13) 0.0308(12) 0.0333(12) 0.0008(10) 0.0022(10) 0.0011(10) O1 0.0279(8) 0.0302(8) 0.0387(9) 0.0002(7) -0.0006(7) 0.0035(6) C15 0.0378(13) 0.0290(12) 0.0438(14) -0.0023(11) 0.0018(11) 0.0020(10) C16 0.0568(18) 0.0417(16) 0.0600(18) 0.0132(14) 0.0035(14) 0.0000(13) C17 0.0332(14) 0.0484(16) 0.0574(17) 0.0015(13) -0.0083(12) 0.0061(11) C18 0.0379(15) 0.0561(18) 0.0590(18) -0.0001(14) -0.0032(13) -0.0067(12) Li1 0.0288(19) 0.0280(19) 0.0326(19) -0.0037(15) -0.0002(15) 0.0005(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.6975(19) . ? Si1 N2 1.770(2) . ? Si1 C7 1.865(2) . ? Si1 C8 1.867(3) . ? Si1 Li1 2.790(4) 3_665 ? Si1 Li1 3.187(4) . ? N1 C1 1.395(3) . ? N1 Li1 2.053(4) 3_665 ? N1 Li1 2.127(4) . ? N2 C9 1.404(3) . ? N2 Li1 2.338(4) 3_665 ? C1 C6 1.405(3) . ? C1 C2 1.407(3) . ? C2 C3 1.383(3) . ? C3 C4 1.379(4) . ? C4 C5 1.379(4) . ? C5 C6 1.380(3) . ? C9 C10 1.389(3) . ? C9 C14 1.397(3) . ? C10 C11 1.384(3) . ? C11 C12 1.375(4) . ? C12 C13 1.379(4) . ? C13 C14 1.377(3) . ? O1 C17 1.427(3) . ? O1 C15 1.434(3) . ? O1 Li1 1.988(4) . ? C15 C16 1.508(4) . ? C17 C18 1.475(4) . ? Li1 N1 2.053(4) 3_665 ? Li1 N2 2.338(4) 3_665 ? Li1 Li1 2.581(7) 3_665 ? Li1 Si1 2.790(4) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 N2 103.26(9) . . ? N1 Si1 C7 116.22(11) . . ? N2 Si1 C7 110.71(11) . . ? N1 Si1 C8 115.15(11) . . ? N2 Si1 C8 104.01(11) . . ? C7 Si1 C8 106.79(13) . . ? N1 Si1 Li1 47.06(10) . 3_665 ? N2 Si1 Li1 56.50(10) . 3_665 ? C7 Si1 Li1 125.30(12) . 3_665 ? C8 Si1 Li1 127.73(11) . 3_665 ? N1 Si1 Li1 38.13(9) . . ? N2 Si1 Li1 89.12(9) . . ? C7 Si1 Li1 152.70(11) . . ? C8 Si1 Li1 85.23(11) . . ? Li1 Si1 Li1 50.65(12) 3_665 . ? C1 N1 Si1 123.82(14) . . ? C1 N1 Li1 131.04(17) . 3_665 ? Si1 N1 Li1 95.68(13) . 3_665 ? C1 N1 Li1 108.30(17) . . ? Si1 N1 Li1 112.35(14) . . ? Li1 N1 Li1 76.25(16) 3_665 . ? C9 N2 Si1 133.23(16) . . ? C9 N2 Li1 104.22(16) . 3_665 ? Si1 N2 Li1 84.34(12) . 3_665 ? N1 C1 C6 120.66(19) . . ? N1 C1 C2 124.1(2) . . ? C6 C1 C2 115.2(2) . . ? C3 C2 C1 121.9(2) . . ? C4 C3 C2 121.1(2) . . ? C5 C4 C3 118.6(2) . . ? C4 C5 C6 120.4(2) . . ? C5 C6 C1 122.8(2) . . ? C10 C9 C14 118.1(2) . . ? C10 C9 N2 122.4(2) . . ? C14 C9 N2 119.5(2) . . ? C11 C10 C9 120.5(2) . . ? C12 C11 C10 120.9(2) . . ? C11 C12 C13 119.1(2) . . ? C14 C13 C12 120.6(2) . . ? C13 C14 C9 120.8(2) . . ? C17 O1 C15 111.97(18) . . ? C17 O1 Li1 126.10(18) . . ? C15 O1 Li1 120.32(17) . . ? O1 C15 C16 113.5(2) . . ? O1 C17 C18 110.4(2) . . ? O1 Li1 N1 113.17(18) . 3_665 ? O1 Li1 N1 130.15(19) . . ? N1 Li1 N1 103.76(16) 3_665 . ? O1 Li1 N2 111.19(17) . 3_665 ? N1 Li1 N2 76.22(13) 3_665 3_665 ? N1 Li1 N2 109.19(17) . 3_665 ? O1 Li1 Li1 147.6(3) . 3_665 ? N1 Li1 Li1 53.18(13) 3_665 3_665 ? N1 Li1 Li1 50.57(13) . 3_665 ? N2 Li1 Li1 94.7(2) 3_665 3_665 ? O1 Li1 Si1 115.74(16) . 3_665 ? N1 Li1 Si1 37.26(8) 3_665 3_665 ? N1 Li1 Si1 113.97(15) . 3_665 ? N2 Li1 Si1 39.16(7) 3_665 3_665 ? Li1 Li1 Si1 72.66(15) 3_665 3_665 ? O1 Li1 Si1 107.69(15) . . ? N1 Li1 Si1 102.21(14) 3_665 . ? N1 Li1 Si1 29.52(7) . . ? N2 Li1 Si1 138.16(15) 3_665 . ? Li1 Li1 Si1 56.70(14) 3_665 . ? Si1 Li1 Si1 129.36(12) 3_665 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.388 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.048 # Attachment 'compound2.cif' data_s155p _database_code_depnum_ccdc_archive 'CCDC 289605' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H66 N4 Na2 O4 Si' _chemical_formula_weight 837.12 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 22.975(9) _cell_length_b 21.168(8) _cell_length_c 10.860(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.372(5) _cell_angle_gamma 90.00 _cell_volume 4884(3) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2495 _cell_measurement_theta_min 2.717 _cell_measurement_theta_max 21.904 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7300 _exptl_absorpt_correction_T_max 0.9783 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.32 _diffrn_reflns_number 9983 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6047 _reflns_number_gt 4486 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+0.6220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.1(2) _refine_ls_number_reflns 6047 _refine_ls_number_parameters 532 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1981 _refine_ls_wR_factor_gt 0.1824 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.66753(7) 0.31614(7) 0.55887(14) 0.0573(4) Uani 1 1 d . . . Na1 Na 0.63120(9) 0.26950(10) 0.7898(2) 0.0670(6) Uani 1 1 d . . . Na2 Na 0.38618(9) 0.34094(10) 0.3593(2) 0.0669(6) Uani 1 1 d . . . N1 N 0.78984(19) 0.2038(2) 0.8333(4) 0.0582(11) Uani 1 1 d . . . N2 N 0.71022(19) 0.2713(2) 0.6936(4) 0.0568(11) Uani 1 1 d . . . N3 N 0.59701(19) 0.3192(2) 0.5763(4) 0.0549(10) Uani 1 1 d . . . N4 N 0.48709(18) 0.31265(19) 0.5064(4) 0.0561(11) Uani 1 1 d . . . C1 C 0.7558(3) 0.1969(3) 0.9189(6) 0.0645(15) Uani 1 1 d . . . C2 C 0.7040(3) 0.1566(3) 0.8845(7) 0.0808(18) Uani 1 1 d . . . C3 C 0.6726(4) 0.1499(4) 0.9728(10) 0.097(2) Uani 1 1 d . . . H3A H 0.6377 0.1228 0.9510 0.117 Uiso 1 1 calc R . . C4 C 0.6929(5) 0.1826(6) 1.0900(10) 0.123(3) Uani 1 1 d . . . H4A H 0.6718 0.1780 1.1485 0.147 Uiso 1 1 calc R . . C5 C 0.7432(4) 0.2217(5) 1.1226(7) 0.101(2) Uani 1 1 d . . . H5A H 0.7568 0.2433 1.2042 0.121 Uiso 1 1 calc R . . C6 C 0.7750(3) 0.2305(3) 1.0391(6) 0.0749(17) Uani 1 1 d . . . C7 C 0.6822(4) 0.1216(4) 0.7542(10) 0.117(3) Uani 1 1 d . . . H7A H 0.7024 0.0806 0.7673 0.175 Uiso 1 1 calc R . . H7B H 0.6932 0.1456 0.6900 0.175 Uiso 1 1 calc R . . H7C H 0.6369 0.1161 0.7211 0.175 Uiso 1 1 calc R . . C8 C 0.8298(3) 0.2751(5) 1.0748(7) 0.103(2) Uani 1 1 d . . . H8A H 0.8369 0.2945 1.1603 0.155 Uiso 1 1 calc R . . H8B H 0.8207 0.3077 1.0072 0.155 Uiso 1 1 calc R . . H8C H 0.8671 0.2520 1.0801 0.155 Uiso 1 1 calc R . . C9 C 0.7641(2) 0.2409(2) 0.7292(5) 0.0535(12) Uani 1 1 d . . . C10 C 0.8040(2) 0.2470(3) 0.6464(5) 0.0601(14) Uani 1 1 d . . . C11 C 0.8454(3) 0.2974(4) 0.6668(7) 0.0833(18) Uani 1 1 d . . . H11A H 0.8488 0.3269 0.7340 0.100 Uiso 1 1 calc R . . C12 C 0.8803(4) 0.3052(6) 0.5946(13) 0.125(3) Uani 1 1 d . . . H12A H 0.9079 0.3398 0.6111 0.150 Uiso 1 1 calc R . . C13 C 0.8762(5) 0.2639(8) 0.4982(13) 0.138(5) Uani 1 1 d . . . H13A H 0.9007 0.2701 0.4469 0.165 Uiso 1 1 calc R . . C14 C 0.8381(5) 0.2143(6) 0.4741(7) 0.105(3) Uani 1 1 d . . . H14A H 0.8358 0.1857 0.4062 0.127 Uiso 1 1 calc R . . C15 C 0.8011(3) 0.2046(4) 0.5504(6) 0.086(2) Uani 1 1 d . . . H15A H 0.7746 0.1692 0.5350 0.103 Uiso 1 1 calc R . . C16 C 0.7061(3) 0.3953(3) 0.5694(8) 0.094(2) Uani 1 1 d . . . H16A H 0.7143 0.4025 0.4892 0.141 Uiso 1 1 calc R . . H16B H 0.7456 0.3961 0.6462 0.141 Uiso 1 1 calc R . . H16C H 0.6785 0.4281 0.5783 0.141 Uiso 1 1 calc R . . C17 C 0.6582(3) 0.2793(4) 0.3953(6) 0.093(2) Uani 1 1 d . . . H17A H 0.6750 0.3076 0.3467 0.140 Uiso 1 1 calc R . . H17B H 0.6139 0.2718 0.3436 0.140 Uiso 1 1 calc R . . H17C H 0.6809 0.2396 0.4111 0.140 Uiso 1 1 calc R . . C18 C 0.5389(2) 0.3317(2) 0.4920(5) 0.0505(12) Uani 1 1 d . . . C19 C 0.5267(2) 0.3717(2) 0.3689(5) 0.0509(12) Uani 1 1 d . . . C20 C 0.5530(2) 0.4305(3) 0.3799(6) 0.0665(15) Uani 1 1 d . . . H20A H 0.5770 0.4467 0.4647 0.080 Uiso 1 1 calc R . . C21 C 0.5444(3) 0.4670(3) 0.2659(8) 0.090(2) Uani 1 1 d . . . H21A H 0.5635 0.5069 0.2745 0.109 Uiso 1 1 calc R . . C22 C 0.5081(3) 0.4440(4) 0.1420(7) 0.0860(19) Uani 1 1 d . . . H22A H 0.5014 0.4684 0.0654 0.103 Uiso 1 1 calc R . . C23 C 0.4820(3) 0.3858(4) 0.1313(6) 0.0838(19) Uani 1 1 d . . . H23A H 0.4576 0.3697 0.0467 0.101 Uiso 1 1 calc R . . C24 C 0.4908(3) 0.3498(3) 0.2440(6) 0.0656(14) Uani 1 1 d . . . H24A H 0.4718 0.3098 0.2345 0.079 Uiso 1 1 calc R . . C25 C 0.4953(2) 0.2733(2) 0.6155(6) 0.0568(13) Uani 1 1 d . . . C26 C 0.4936(3) 0.2989(3) 0.7336(6) 0.0670(15) Uani 1 1 d . . . C27 C 0.5003(3) 0.2601(3) 0.8386(7) 0.0792(18) Uani 1 1 d . . . H27A H 0.5000 0.2775 0.9180 0.095 Uiso 1 1 calc R . . C28 C 0.5073(3) 0.1968(4) 0.8301(9) 0.092(2) Uani 1 1 d . . . H28A H 0.5115 0.1707 0.9032 0.111 Uiso 1 1 calc R . . C29 C 0.5083(3) 0.1707(3) 0.7156(9) 0.086(2) Uani 1 1 d . . . H29A H 0.5120 0.1267 0.7099 0.103 Uiso 1 1 calc R . . C30 C 0.5038(3) 0.2082(3) 0.6081(7) 0.0708(16) Uani 1 1 d . . . C31 C 0.4862(4) 0.3697(4) 0.7415(8) 0.097(2) Uani 1 1 d . . . H31A H 0.4425 0.3797 0.7236 0.146 Uiso 1 1 calc R . . H31B H 0.4990 0.3904 0.6761 0.146 Uiso 1 1 calc R . . H31C H 0.5124 0.3845 0.8299 0.146 Uiso 1 1 calc R . . C32 C 0.5070(4) 0.1799(3) 0.4859(8) 0.096(2) Uani 1 1 d . . . H32A H 0.5128 0.1346 0.4976 0.144 Uiso 1 1 calc R . . H32B H 0.5421 0.1981 0.4694 0.144 Uiso 1 1 calc R . . H32C H 0.4682 0.1886 0.4108 0.144 Uiso 1 1 calc R . . O1 O 0.6483(2) 0.3525(3) 0.9395(5) 0.0984(15) Uani 1 1 d . . . C33 C 0.6382(5) 0.3613(5) 1.0581(9) 0.125(3) Uani 1 1 d . . . H33A H 0.6474 0.3221 1.1101 0.150 Uiso 1 1 calc R . . H33B H 0.5942 0.3726 1.0378 0.150 Uiso 1 1 calc R . . C34 C 0.6796(7) 0.4118(7) 1.1344(11) 0.171(5) Uani 1 1 d . . . H34A H 0.6554 0.4503 1.1314 0.206 Uiso 1 1 calc R . . H34B H 0.7013 0.3991 1.2276 0.206 Uiso 1 1 calc R . . C35 C 0.7230(6) 0.4221(5) 1.0746(12) 0.138(4) Uani 1 1 d . . . H35A H 0.7621 0.3991 1.1222 0.165 Uiso 1 1 calc R . . H35B H 0.7326 0.4672 1.0747 0.165 Uiso 1 1 calc R . . C36 C 0.6914(4) 0.3976(4) 0.9326(8) 0.103(2) Uani 1 1 d . . . H36A H 0.6699 0.4319 0.8716 0.124 Uiso 1 1 calc R . . H36B H 0.7224 0.3784 0.9021 0.124 Uiso 1 1 calc R . . O2 O 0.3599(3) 0.4454(3) 0.3084(8) 0.123(2) Uani 1 1 d D . . C37 C 0.3758(11) 0.4896(8) 0.234(3) 0.37(2) Uani 1 1 d D . . H37A H 0.3741 0.4710 0.1504 0.444 Uiso 1 1 calc R . . H37B H 0.4186 0.5052 0.2835 0.444 Uiso 1 1 calc R . . C38 C 0.3285(10) 0.5433(7) 0.207(2) 0.293(14) Uani 1 1 d D . . H38A H 0.2977 0.5417 0.1154 0.351 Uiso 1 1 calc R . . H38B H 0.3498 0.5844 0.2230 0.351 Uiso 1 1 calc R . . C39 C 0.2968(10) 0.5321(8) 0.306(3) 0.41(3) Uani 1 1 d D . . H39A H 0.2526 0.5198 0.2595 0.491 Uiso 1 1 calc R . . H39B H 0.2988 0.5699 0.3592 0.491 Uiso 1 1 calc R . . C40 C 0.3354(10) 0.4781(7) 0.3923(14) 0.287(14) Uani 1 1 d D . . H40A H 0.3695 0.4946 0.4714 0.345 Uiso 1 1 calc R . . H40B H 0.3088 0.4503 0.4206 0.345 Uiso 1 1 calc R . . O3 O 0.6237(12) 0.9653(9) 0.9174(16) 0.321(12) Uani 1 1 d . . . C41 C 0.6360(12) 0.9215(12) 0.827(3) 0.298(17) Uani 1 1 d . . . H41A H 0.6492 0.8804 0.8696 0.357 Uiso 1 1 calc R . . H41B H 0.6695 0.9379 0.8005 0.357 Uiso 1 1 calc R . . C42 C 0.5771(13) 0.9151(14) 0.709(3) 0.304(16) Uani 1 1 d . . . H42A H 0.5840 0.9202 0.6260 0.365 Uiso 1 1 calc R . . H42B H 0.5565 0.8745 0.7083 0.365 Uiso 1 1 calc R . . C43 C 0.5436(13) 0.9644(18) 0.730(2) 0.335(19) Uani 1 1 d . . . H43A H 0.5316 0.9919 0.6520 0.402 Uiso 1 1 calc R . . H43B H 0.5046 0.9470 0.7333 0.402 Uiso 1 1 calc R . . C44 C 0.5692(8) 0.9999(8) 0.835(3) 0.197(6) Uani 1 1 d . . . H44A H 0.5403 1.0063 0.8813 0.237 Uiso 1 1 calc R . . H44B H 0.5810 1.0412 0.8112 0.237 Uiso 1 1 calc R . . O4 O 0.9101(13) 0.5311(7) 0.348(3) 0.396(17) Uani 1 1 d D . . C45 C 0.8719(9) 0.5485(6) 0.415(2) 0.277(14) Uani 1 1 d D . . H45A H 0.8409 0.5798 0.3630 0.332 Uiso 1 1 calc R . . H45B H 0.8974 0.5673 0.5012 0.332 Uiso 1 1 calc R . . C46 C 0.8387(8) 0.4901(11) 0.436(3) 0.315(14) Uani 1 1 d D . . H46A H 0.7959 0.4871 0.3685 0.378 Uiso 1 1 calc R . . H46B H 0.8371 0.4898 0.5246 0.378 Uiso 1 1 calc R . . C47 C 0.8799(14) 0.4368(6) 0.420(3) 0.37(2) Uani 1 1 d D . . H47A H 0.9094 0.4223 0.5076 0.446 Uiso 1 1 calc R . . H47B H 0.8541 0.4010 0.3727 0.446 Uiso 1 1 calc R . . C48 C 0.9143(12) 0.4656(8) 0.342(2) 0.290(14) Uani 1 1 d D . . H48A H 0.9585 0.4525 0.3788 0.348 Uiso 1 1 calc R . . H48B H 0.8956 0.4514 0.2491 0.348 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0336(6) 0.0812(9) 0.0603(8) 0.0156(7) 0.0214(6) 0.0076(6) Na1 0.0473(11) 0.0930(15) 0.0658(12) 0.0114(11) 0.0274(9) 0.0010(10) Na2 0.0365(10) 0.0827(13) 0.0758(13) 0.0049(11) 0.0148(9) -0.0048(9) N1 0.037(2) 0.082(3) 0.056(2) 0.015(2) 0.0169(18) 0.007(2) N2 0.039(2) 0.075(3) 0.057(2) 0.007(2) 0.0195(19) 0.002(2) N3 0.032(2) 0.070(2) 0.062(2) 0.000(2) 0.0174(18) 0.0020(18) N4 0.033(2) 0.068(2) 0.062(3) 0.004(2) 0.0122(19) -0.0029(18) C1 0.047(3) 0.082(4) 0.066(4) 0.028(3) 0.024(3) 0.019(3) C2 0.067(4) 0.086(4) 0.090(4) 0.025(4) 0.030(3) 0.006(3) C3 0.081(5) 0.117(6) 0.106(6) 0.044(5) 0.049(4) 0.007(4) C4 0.101(7) 0.185(9) 0.105(7) 0.067(7) 0.065(6) 0.033(6) C5 0.073(5) 0.172(7) 0.063(4) 0.033(4) 0.032(4) 0.040(5) C6 0.053(3) 0.116(5) 0.054(3) 0.022(3) 0.019(3) 0.026(3) C7 0.092(6) 0.102(5) 0.153(8) -0.012(5) 0.042(5) -0.032(5) C8 0.056(4) 0.162(7) 0.081(4) -0.023(4) 0.015(3) 0.014(4) C9 0.037(3) 0.068(3) 0.055(3) 0.001(2) 0.016(2) 0.002(2) C10 0.036(3) 0.088(4) 0.054(3) 0.016(3) 0.015(2) 0.019(3) C11 0.052(4) 0.100(5) 0.104(5) 0.014(4) 0.037(3) 0.006(3) C12 0.088(6) 0.147(8) 0.177(10) 0.052(7) 0.092(7) 0.025(5) C13 0.082(6) 0.229(13) 0.134(9) 0.107(9) 0.078(6) 0.076(8) C14 0.095(6) 0.171(8) 0.057(4) 0.014(5) 0.036(4) 0.062(6) C15 0.061(4) 0.125(5) 0.066(4) -0.012(4) 0.019(3) 0.035(4) C16 0.043(3) 0.111(5) 0.129(6) 0.056(4) 0.032(3) 0.001(3) C17 0.068(4) 0.155(7) 0.061(4) 0.012(4) 0.030(3) 0.036(4) C18 0.036(3) 0.055(3) 0.058(3) -0.010(2) 0.014(2) -0.005(2) C19 0.032(2) 0.057(3) 0.063(3) -0.003(2) 0.018(2) 0.005(2) C20 0.045(3) 0.063(3) 0.083(4) 0.010(3) 0.014(3) 0.009(2) C21 0.065(4) 0.073(4) 0.127(6) 0.023(4) 0.029(4) 0.005(3) C22 0.078(4) 0.098(5) 0.086(5) 0.035(4) 0.035(4) 0.017(4) C23 0.070(4) 0.121(6) 0.062(4) 0.002(4) 0.026(3) 0.006(4) C24 0.049(3) 0.085(4) 0.063(3) 0.001(3) 0.022(3) 0.000(3) C25 0.028(2) 0.065(3) 0.077(4) 0.006(3) 0.019(2) -0.005(2) C26 0.046(3) 0.082(4) 0.077(4) 0.005(3) 0.027(3) 0.001(3) C27 0.056(4) 0.099(5) 0.088(4) 0.014(4) 0.034(3) -0.008(3) C28 0.069(4) 0.097(6) 0.117(6) 0.034(5) 0.043(4) -0.007(3) C29 0.068(4) 0.073(4) 0.117(6) 0.012(4) 0.035(4) -0.007(3) C30 0.050(3) 0.067(4) 0.095(4) 0.002(3) 0.028(3) -0.007(3) C31 0.105(6) 0.102(5) 0.100(5) -0.015(4) 0.055(4) 0.008(4) C32 0.110(6) 0.074(4) 0.103(5) -0.012(4) 0.040(4) 0.001(4) O1 0.089(3) 0.133(4) 0.084(3) -0.013(3) 0.045(3) -0.024(3) C33 0.120(7) 0.172(8) 0.098(6) -0.035(6) 0.059(5) -0.020(6) C34 0.176(12) 0.235(14) 0.123(8) -0.068(8) 0.080(8) -0.090(11) C35 0.133(9) 0.118(6) 0.165(10) -0.022(6) 0.058(8) -0.021(6) C36 0.096(6) 0.105(5) 0.115(6) 0.016(5) 0.048(5) 0.005(5) O2 0.088(4) 0.098(3) 0.187(6) 0.010(4) 0.055(4) 0.016(3) C37 0.45(4) 0.188(15) 0.67(6) 0.20(3) 0.44(5) 0.17(2) C38 0.27(2) 0.149(12) 0.54(4) 0.175(18) 0.24(3) 0.114(14) C39 0.24(2) 0.141(13) 0.90(9) 0.13(3) 0.28(4) 0.065(14) C40 0.45(4) 0.193(15) 0.194(15) -0.065(13) 0.09(2) 0.02(2) O3 0.42(3) 0.240(14) 0.212(13) 0.034(12) 0.019(16) -0.049(17) C41 0.22(2) 0.30(2) 0.27(2) -0.13(2) -0.027(18) 0.107(19) C42 0.29(3) 0.34(3) 0.27(3) -0.12(2) 0.09(2) 0.11(2) C43 0.27(3) 0.43(4) 0.205(19) -0.13(2) -0.015(19) 0.06(3) C44 0.155(12) 0.185(13) 0.25(2) -0.010(15) 0.074(13) 0.030(11) O4 0.57(4) 0.180(12) 0.65(4) -0.072(17) 0.48(4) -0.034(17) C45 0.181(18) 0.135(11) 0.45(4) -0.037(17) 0.04(2) 0.047(11) C46 0.143(15) 0.39(4) 0.41(4) -0.06(3) 0.095(18) -0.07(2) C47 0.49(6) 0.154(16) 0.43(5) 0.08(2) 0.13(4) 0.00(2) C48 0.45(4) 0.156(15) 0.32(3) -0.019(16) 0.21(3) 0.09(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 Si1 N3 1.702(4) . ? Si1 N2 1.706(4) . ? Si1 C17 1.875(7) . ? Si1 C16 1.879(7) . ? Si1 Na1 3.091(3) . ? Na1 O1 2.324(6) . ? Na1 N3 2.390(5) . ? Na1 N2 2.416(5) . ? Na1 C2 2.873(7) . ? Na1 C25 2.973(5) . ? Na1 C26 3.047(6) . ? Na1 C1 3.076(5) . ? Na1 C30 3.123(6) . ? Na2 O2 2.303(6) . ? Na2 N1 2.324(5) 4_454 ? Na2 N4 2.338(4) . ? Na2 C10 3.009(5) 4_454 ? Na2 C24 3.110(6) . ? N1 C9 1.317(6) . ? N1 C1 1.433(7) . ? N1 Na2 2.324(5) 4 ? N2 C9 1.315(6) . ? N3 C18 1.327(6) . ? N4 C18 1.321(7) . ? N4 C25 1.401(7) . ? C1 C2 1.394(9) . ? C1 C6 1.402(9) . ? C2 C3 1.408(11) . ? C2 C7 1.505(11) . ? C3 C4 1.366(13) . ? C4 C5 1.354(13) . ? C5 C6 1.377(10) . ? C6 C8 1.502(11) . ? C9 C10 1.515(8) . ? C10 C15 1.356(9) . ? C10 C11 1.389(9) . ? C10 Na2 3.009(5) 4 ? C11 C12 1.329(12) . ? C12 C13 1.340(15) . ? C13 C14 1.327(16) . ? C14 C15 1.411(12) . ? C18 C19 1.516(7) . ? C19 C20 1.368(8) . ? C19 C24 1.372(7) . ? C20 C21 1.409(9) . ? C21 C22 1.374(10) . ? C22 C23 1.356(10) . ? C23 C24 1.390(9) . ? C25 C30 1.398(8) . ? C25 C26 1.407(8) . ? C26 C27 1.366(9) . ? C26 C31 1.514(10) . ? C27 C28 1.358(11) . ? C28 C29 1.368(11) . ? C29 C30 1.384(10) . ? C30 C32 1.483(10) . ? O1 C36 1.399(9) . ? O1 C33 1.404(10) . ? C33 C34 1.461(14) . ? C34 C35 1.397(16) . ? C35 C36 1.524(13) . ? O2 C37 1.370(8) . ? O2 C40 1.420(8) . ? C37 C38 1.522(9) . ? C38 C39 1.523(9) . ? C39 C40 1.530(9) . ? O3 C44 1.43(2) . ? O3 C41 1.46(3) . ? C41 C42 1.47(3) . ? C42 C43 1.36(3) . ? C43 C44 1.31(2) . ? O4 C45 1.388(9) . ? O4 C48 1.393(8) . ? C45 C46 1.513(9) . ? C46 C47 1.520(9) . ? C47 C48 1.497(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Si1 N2 100.8(2) . . ? N3 Si1 C17 110.5(3) . . ? N2 Si1 C17 113.7(3) . . ? N3 Si1 C16 114.0(3) . . ? N2 Si1 C16 109.9(3) . . ? C17 Si1 C16 108.0(4) . . ? N3 Si1 Na1 50.17(15) . . ? N2 Si1 Na1 51.05(16) . . ? C17 Si1 Na1 131.8(3) . . ? C16 Si1 Na1 120.2(3) . . ? O1 Na1 N3 104.57(19) . . ? O1 Na1 N2 109.66(18) . . ? N3 Na1 N2 66.22(14) . . ? O1 Na1 C2 117.3(2) . . ? N3 Na1 C2 130.1(2) . . ? N2 Na1 C2 74.77(18) . . ? O1 Na1 C25 106.35(19) . . ? N3 Na1 C25 59.50(15) . . ? N2 Na1 C25 120.27(17) . . ? C2 Na1 C25 125.28(19) . . ? O1 Na1 C26 82.61(19) . . ? N3 Na1 C26 77.47(16) . . ? N2 Na1 C26 143.46(16) . . ? C2 Na1 C26 131.27(19) . . ? C25 Na1 C26 27.00(16) . . ? O1 Na1 C1 100.33(19) . . ? N3 Na1 C1 124.55(17) . . ? N2 Na1 C1 58.88(15) . . ? C2 Na1 C1 26.82(17) . . ? C25 Na1 C1 150.81(18) . . ? C26 Na1 C1 155.17(17) . . ? O1 Na1 Si1 107.48(15) . . ? N3 Na1 Si1 33.17(10) . . ? N2 Na1 Si1 33.31(10) . . ? C2 Na1 Si1 104.83(16) . . ? C25 Na1 Si1 90.97(13) . . ? C26 Na1 Si1 110.62(13) . . ? C1 Na1 Si1 92.16(13) . . ? O1 Na1 C30 128.6(2) . . ? N3 Na1 C30 71.74(17) . . ? N2 Na1 C30 114.29(18) . . ? C2 Na1 C30 99.13(19) . . ? C25 Na1 C30 26.37(16) . . ? C26 Na1 C30 46.11(17) . . ? C1 Na1 C30 124.49(18) . . ? Si1 Na1 C30 95.60(15) . . ? O2 Na2 N1 102.2(2) . 4_454 ? O2 Na2 N4 120.7(2) . . ? N1 Na2 N4 129.02(18) 4_454 . ? O2 Na2 C10 112.3(2) . 4_454 ? N1 Na2 C10 50.53(15) 4_454 4_454 ? N4 Na2 C10 122.38(17) . 4_454 ? O2 Na2 C24 91.0(2) . . ? N1 Na2 C24 145.27(17) 4_454 . ? N4 Na2 C24 64.73(16) . . ? C10 Na2 C24 94.75(17) 4_454 . ? C9 N1 C1 116.1(4) . . ? C9 N1 Na2 116.3(3) . 4 ? C1 N1 Na2 127.5(3) . 4 ? C9 N2 Si1 133.9(4) . . ? C9 N2 Na1 130.0(3) . . ? Si1 N2 Na1 95.64(19) . . ? C18 N3 Si1 132.9(4) . . ? C18 N3 Na1 129.1(4) . . ? Si1 N3 Na1 96.66(18) . . ? C18 N4 C25 116.3(4) . . ? C18 N4 Na2 123.0(3) . . ? C25 N4 Na2 120.6(3) . . ? C2 C1 C6 119.7(6) . . ? C2 C1 N1 120.7(6) . . ? C6 C1 N1 119.6(5) . . ? C2 C1 Na1 68.4(3) . . ? C6 C1 Na1 94.6(3) . . ? N1 C1 Na1 107.2(3) . . ? C1 C2 C3 119.0(7) . . ? C1 C2 C7 119.8(7) . . ? C3 C2 C7 121.1(7) . . ? C1 C2 Na1 84.8(3) . . ? C3 C2 Na1 87.1(4) . . ? C7 C2 Na1 97.7(4) . . ? C4 C3 C2 120.1(8) . . ? C5 C4 C3 120.5(8) . . ? C4 C5 C6 121.7(8) . . ? C5 C6 C1 119.0(7) . . ? C5 C6 C8 121.2(7) . . ? C1 C6 C8 119.8(6) . . ? N2 C9 N1 127.5(5) . . ? N2 C9 C10 119.9(4) . . ? N1 C9 C10 112.6(4) . . ? C15 C10 C11 117.5(6) . . ? C15 C10 C9 122.4(6) . . ? C11 C10 C9 120.1(6) . . ? C15 C10 Na2 90.9(4) . 4 ? C11 C10 Na2 99.3(4) . 4 ? C9 C10 Na2 80.6(3) . 4 ? C12 C11 C10 122.1(9) . . ? C11 C12 C13 120.1(10) . . ? C14 C13 C12 121.0(8) . . ? C13 C14 C15 119.9(9) . . ? C10 C15 C14 119.3(8) . . ? N4 C18 N3 124.9(5) . . ? N4 C18 C19 113.7(4) . . ? N3 C18 C19 121.3(5) . . ? C20 C19 C24 118.2(5) . . ? C20 C19 C18 120.2(4) . . ? C24 C19 C18 121.6(5) . . ? C19 C20 C21 120.9(6) . . ? C22 C21 C20 119.7(6) . . ? C23 C22 C21 119.3(6) . . ? C22 C23 C24 120.8(6) . . ? C19 C24 C23 121.1(6) . . ? C19 C24 Na2 83.6(3) . . ? C23 C24 Na2 120.8(4) . . ? C30 C25 N4 120.9(5) . . ? C30 C25 C26 119.0(5) . . ? N4 C25 C26 120.1(5) . . ? C30 C25 Na1 82.8(3) . . ? N4 C25 Na1 109.0(3) . . ? C26 C25 Na1 79.5(3) . . ? C27 C26 C25 119.8(6) . . ? C27 C26 C31 121.8(6) . . ? C25 C26 C31 118.4(5) . . ? C27 C26 Na1 86.1(4) . . ? C25 C26 Na1 73.5(3) . . ? C31 C26 Na1 108.8(4) . . ? C28 C27 C26 121.0(7) . . ? C27 C28 C29 120.3(7) . . ? C28 C29 C30 120.9(6) . . ? C29 C30 C25 119.0(6) . . ? C29 C30 C32 120.7(6) . . ? C25 C30 C32 120.3(6) . . ? C29 C30 Na1 87.4(4) . . ? C25 C30 Na1 70.8(3) . . ? C32 C30 Na1 112.3(5) . . ? C36 O1 C33 109.1(7) . . ? C36 O1 Na1 114.4(5) . . ? C33 O1 Na1 134.3(6) . . ? O1 C33 C34 108.5(9) . . ? C35 C34 C33 106.0(9) . . ? C34 C35 C36 105.6(9) . . ? O1 C36 C35 104.5(7) . . ? C37 O2 C40 107.6(7) . . ? C37 O2 Na2 133.9(6) . . ? C40 O2 Na2 116.4(7) . . ? O2 C37 C38 107.1(7) . . ? C37 C38 C39 104.2(5) . . ? C38 C39 C40 103.1(6) . . ? O2 C40 C39 104.4(6) . . ? C44 O3 C41 104.7(15) . . ? O3 C41 C42 107.1(19) . . ? C43 C42 C41 100.1(19) . . ? C44 C43 C42 119(2) . . ? C43 C44 O3 104.1(18) . . ? C45 O4 C48 110.9(6) . . ? O4 C45 C46 108.4(6) . . ? C45 C46 C47 102.8(6) . . ? C48 C47 C46 104.2(7) . . ? O4 C48 C47 108.6(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.358 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.057