# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1609 data_global #====================================================================== _audit_creation_date 12-03-98 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; Prof. Jean Fischer ; _publ_contact_author_address # Address of author for correspondance ; Universite Louis Pasteur Laboratoire de Cristallochimie et de Chimie Structurale 4, rue Blaise Pascal 67070 Strasbourg cedex France ; _publ_contact_author_phone '+33 (0)3 88 41 60 58' _publ_contact_author_fax '+33 (0)3 88 41 53 63' _publ_contact_author_email fischer@chimie.u-strasbg.fr _publ_requested_journal 'Chem. Comm.' _publ_contact_letter ; ; _publ_requested_category FM #====================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The arched four-rung ladder structure of the unsolvated dilithium salt of N,N'-bis(trimethylsilyl)-2-aminobenzylamine, and its structural deformation on THF co;plexation. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Gauvin Regis M.' ; Universite Louis Pasteur Laboratoire de Chimie des Metaux de Transition et de Catalyse UMR 7513 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Kress Jacky' ; Universite Louis Pasteur Laboratoire de Chimie des Metaux de Transition et de Catalyse UMR 7513 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Gruber Nathalie' ; Universite Louis Pasteur Laboratoire de Cristallochimie et de Chimie Structurale UMR 7513 4, rue Blaise Pascal 67070 Strasbourg cedex France ; 'Fischer Jean' ; Universite Louis Pasteur Laboratoire de Cristallochimie et de Chimie Structurale UMR 7513 4, rue Blaise Pascal 67070 Strasbourg cedex France ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #====================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st109 #====================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H48 N4 Li4 Si4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H48 N4 Li4 Si4' _chemical_formula_weight 556.81 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 Li ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #====================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.7590(2) _cell_length_b 21.3540(4) _cell_length_c 16.7940(6) _cell_angle_alpha 90 _cell_angle_beta 98.073(5) _cell_angle_gamma 90 _cell_volume 3465.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.07 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #====================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 180 frames, 30 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times. Detector to crystal distance 25 mm. ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25648 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7232 _reflns_number_gt 4455 _reflns_threshold_expression 3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #====================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4455 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details ; ? ; _refine_ls_R_factor_all 0.073 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_all 0.292 _refine_ls_wR_factor_ref 0.058 _refine_ls_goodness_of_fit_all 5.653 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_shift/su_max 0.013 _refine_ls_shift/esd_mean 0.003 _refine_diff_density_max 0.208 _refine_diff_density_min -0.358 #====================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol LI1 0.2078(4) 0.3182(2) 0.6479(2) 0.039(2) Uani ? ? Li LI2 0.3417(4) 0.3948(2) 0.8068(2) 0.037(2) Uani ? ? Li LI3 0.5191(4) 0.3159(2) 0.8176(2) 0.039(2) Uani ? ? Li LI4 0.3750(3) 0.4028(2) 0.6689(2) 0.034(2) Uani ? ? Li N1 0.1842(2) 0.39624(8) 0.7144(1) 0.0309(9) Uani ? ? N SI1 0.11053(6) 0.46331(3) 0.67233(4) 0.0336(3) Uani ? ? Si C1 0.2438(2) 0.5018(1) 0.6186(2) 0.042(1) Uani ? ? C C2 0.0614(2) 0.5205(1) 0.7471(2) 0.051(1) Uani ? ? C C3 -0.0495(2) 0.4493(1) 0.5991(2) 0.047(1) Uani ? ? C C4 0.0971(2) 0.3626(1) 0.7670(1) 0.035(1) Uani ? ? C C5 0.1273(2) 0.2934(1) 0.7695(1) 0.033(1) Uani ? ? C C6 0.2493(2) 0.2696(1) 0.8157(1) 0.033(1) Uani ? ? C C7 0.2718(2) 0.2049(1) 0.8120(1) 0.043(1) Uani ? ? C C8 0.1805(3) 0.1654(1) 0.7670(2) 0.052(1) Uani ? ? C C9 0.0629(3) 0.1888(1) 0.7225(2) 0.054(1) Uani ? ? C C10 0.0384(2) 0.2522(1) 0.7231(1) 0.044(1) Uani ? ? C N2 0.3448(2) 0.30967(8) 0.8615(1) 0.0331(9) Uani ? ? N SI2 0.36613(6) 0.30841(3) 0.96399(4) 0.0370(3) Uani ? ? Si C11 0.5507(2) 0.3291(1) 0.9987(2) 0.052(1) Uani ? ? C C12 0.2564(3) 0.3677(1) 1.0072(2) 0.059(2) Uani ? ? C C13 0.3273(3) 0.2319(1) 1.0092(2) 0.055(2) Uani ? ? C N3 0.5308(2) 0.40128(8) 0.7634(1) 0.0317(9) Uani ? ? N SI3 0.60147(6) 0.46606(3) 0.81358(4) 0.0363(3) Uani ? ? Si C14 0.7658(2) 0.4495(1) 0.8833(2) 0.053(1) Uani ? ? C C15 0.6434(2) 0.5304(1) 0.7455(2) 0.052(1) Uani ? ? C C16 0.4680(3) 0.4960(1) 0.8746(2) 0.052(1) Uani ? ? C C17 0.6198(2) 0.3750(1) 0.7056(1) 0.035(1) Uani ? ? C C18 0.5941(2) 0.3059(1) 0.6934(1) 0.034(1) Uani ? ? C C19 0.4771(2) 0.2839(1) 0.6418(1) 0.033(1) Uani ? ? C C20 0.4588(2) 0.2186(1) 0.6365(1) 0.043(1) Uani ? ? C C21 0.5514(3) 0.1774(1) 0.6803(2) 0.053(1) Uani ? ? C C22 0.6639(3) 0.1998(1) 0.7314(2) 0.058(2) Uani ? ? C C23 0.6831(2) 0.2634(1) 0.7378(1) 0.046(1) Uani ? ? C N4 0.3798(2) 0.32533(8) 0.6002(1) 0.0316(9) Uani ? ? N SI4 0.37685(6) 0.33484(3) 0.49869(4) 0.0355(3) Uani ? ? Si C24 0.1993(3) 0.3617(1) 0.4550(2) 0.055(2) Uani ? ? C C25 0.4168(2) 0.2625(1) 0.4439(1) 0.047(1) Uani ? ? C C26 0.5040(3) 0.3955(1) 0.4748(2) 0.058(2) Uani ? ? C H1 0.2070 0.5395 0.5942 0.0556 Uiso calc C1 H H2 0.3236 0.5111 0.6560 0.0556 Uiso calc C1 H H3 0.2683 0.4744 0.5784 0.0556 Uiso calc C1 H H4 0.0213 0.5565 0.7198 0.0656 Uiso calc C2 H H5 -0.0037 0.5018 0.7769 0.0656 Uiso calc C2 H H6 0.1415 0.5325 0.7827 0.0656 Uiso calc C2 H H7 -0.0852 0.4882 0.5781 0.0618 Uiso calc C3 H H8 -0.0277 0.4236 0.5565 0.0618 Uiso calc C3 H H9 -0.1169 0.4290 0.6257 0.0618 Uiso calc C3 H H10 0.0023 0.3689 0.7466 0.0458 Uiso calc C4 H H11 0.1157 0.3791 0.8199 0.0458 Uiso calc C4 H H12 0.3532 0.1878 0.8417 0.0561 Uiso calc C7 H H13 0.1988 0.1218 0.7668 0.0711 Uiso calc C8 H H14 -0.0006 0.1615 0.6916 0.0718 Uiso calc C9 H H15 -0.0415 0.2684 0.6909 0.0588 Uiso calc C10 H H16 0.5671 0.3290 1.0558 0.0725 Uiso calc C11 H H17 0.6094 0.2993 0.9785 0.0725 Uiso calc C11 H H18 0.5695 0.3696 0.9795 0.0725 Uiso calc C11 H H19 0.2720 0.3652 1.0642 0.0765 Uiso calc C12 H H20 0.2799 0.4085 0.9908 0.0765 Uiso calc C12 H H21 0.1616 0.3597 0.9885 0.0765 Uiso calc C12 H H22 0.3417 0.2353 1.0661 0.0739 Uiso calc C13 H H23 0.2336 0.2208 0.9916 0.0739 Uiso calc C13 H H24 0.3866 0.2006 0.9929 0.0739 Uiso calc C13 H H25 0.7994 0.4872 0.9090 0.0700 Uiso calc C14 H H26 0.7478 0.4199 0.9227 0.0700 Uiso calc C14 H H27 0.8333 0.4331 0.8533 0.0700 Uiso calc C14 H H28 0.6820 0.5648 0.7769 0.0683 Uiso calc C15 H H29 0.7081 0.5157 0.7126 0.0683 Uiso calc C15 H H30 0.5612 0.5435 0.7125 0.0683 Uiso calc C15 H H31 0.5027 0.5322 0.9037 0.0677 Uiso calc C16 H H32 0.3859 0.5065 0.8398 0.0677 Uiso calc C16 H H33 0.4480 0.4645 0.9112 0.0677 Uiso calc C16 H H34 0.7144 0.3815 0.7265 0.0465 Uiso calc C17 H H35 0.5990 0.3958 0.6554 0.0465 Uiso calc C17 H H36 0.3815 0.2021 0.6023 0.0554 Uiso calc C20 H H37 0.5369 0.1335 0.6750 0.0722 Uiso calc C21 H H38 0.7268 0.1718 0.7615 0.0767 Uiso calc C22 H H39 0.7594 0.2790 0.7736 0.0615 Uiso calc C23 H H40 0.1955 0.3673 0.3986 0.0742 Uiso calc C24 H H41 0.1332 0.3311 0.4653 0.0742 Uiso calc C24 H H42 0.1793 0.4003 0.4791 0.0742 Uiso calc C24 H H43 0.4131 0.2716 0.3882 0.0625 Uiso calc C25 H H44 0.5069 0.2481 0.4646 0.0625 Uiso calc C25 H H45 0.3508 0.2310 0.4508 0.0625 Uiso calc C25 H H46 0.4993 0.3994 0.4182 0.0760 Uiso calc C26 H H47 0.4824 0.4346 0.4970 0.0760 Uiso calc C26 H H48 0.5949 0.3832 0.4973 0.0760 Uiso calc C26 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol LI1 0.038(2) 0.037(2) 0.040(2) -0.003(2) 0.012(1) -0.002(2) Li LI2 0.038(2) 0.038(2) 0.034(2) -0.002(2) 0.008(1) 0.002(2) Li LI3 0.038(2) 0.041(2) 0.039(2) -0.000(2) 0.007(2) 0.005(2) Li LI4 0.033(2) 0.033(2) 0.037(2) 0.002(1) 0.008(1) 0.003(2) Li N1 0.0281(8) 0.0339(9) 0.0311(9) 0.0022(7) 0.0081(7) 0.0042(8) N SI1 0.0325(3) 0.0317(3) 0.0369(3) 0.0048(2) 0.0062(2) 0.0032(3) Si C1 0.046(1) 0.036(1) 0.046(1) 0.000(1) 0.006(1) 0.006(1) C C2 0.051(1) 0.044(1) 0.059(2) 0.007(1) 0.016(1) -0.003(1) C C3 0.041(1) 0.051(1) 0.050(1) 0.008(1) 0.002(1) 0.009(1) C C4 0.0289(9) 0.044(1) 0.034(1) 0.0034(9) 0.0082(8) 0.007(1) C C5 0.033(1) 0.039(1) 0.027(1) -0.0056(9) 0.0075(9) 0.0030(9) C C6 0.035(1) 0.035(1) 0.028(1) -0.0027(9) 0.0103(8) 0.0029(9) C C7 0.052(1) 0.036(1) 0.043(1) 0.002(1) 0.012(1) 0.005(1) C C8 0.082(2) 0.035(1) 0.050(2) -0.010(1) 0.019(1) -0.002(1) C C9 0.075(2) 0.050(1) 0.041(1) -0.029(1) 0.010(1) -0.006(1) C C10 0.042(1) 0.060(1) 0.033(1) -0.016(1) 0.004(1) 0.005(1) C N2 0.0324(8) 0.037(1) 0.030(1) -0.0020(8) 0.0037(7) 0.0043(9) N SI2 0.0337(3) 0.0539(4) 0.0279(3) -0.0067(3) 0.0036(2) 0.0063(3) Si C11 0.047(1) 0.082(2) 0.037(1) -0.014(1) -0.001(1) 0.010(1) C C12 0.061(1) 0.076(2) 0.043(1) -0.010(1) 0.020(1) -0.008(1) C C13 0.053(1) 0.071(2) 0.044(1) -0.011(1) 0.001(1) 0.019(1) C N3 0.0289(8) 0.035(1) 0.0317(9) -0.0024(7) 0.0061(7) -0.0002(8) N SI3 0.0348(3) 0.0360(3) 0.0383(3) -0.0070(3) 0.0046(3) -0.0015(3) Si C14 0.045(1) 0.064(2) 0.050(2) -0.016(1) -0.001(1) 0.001(1) C C15 0.050(1) 0.042(1) 0.066(2) -0.006(1) 0.009(1) 0.006(1) C C16 0.052(1) 0.050(1) 0.054(2) -0.007(1) 0.009(1) -0.015(1) C C17 0.0283(9) 0.046(1) 0.034(1) -0.0012(9) 0.0060(9) -0.001(1) C C18 0.035(1) 0.038(1) 0.031(1) 0.0076(9) 0.0114(8) 0.002(1) C C19 0.037(1) 0.033(1) 0.029(1) 0.0035(9) 0.0130(8) 0.0038(9) C C20 0.057(1) 0.033(1) 0.042(1) 0.001(1) 0.020(1) 0.002(1) C C21 0.089(2) 0.032(1) 0.053(1) 0.014(1) 0.036(1) 0.011(1) C C22 0.080(2) 0.058(2) 0.041(1) 0.034(1) 0.016(1) 0.014(1) C C23 0.049(1) 0.059(2) 0.034(1) 0.020(1) 0.008(1) 0.005(1) C N4 0.0328(8) 0.034(1) 0.0287(9) 0.0029(7) 0.0058(7) 0.0014(8) N SI4 0.0371(3) 0.0424(3) 0.0285(3) 0.0036(3) 0.0052(2) -0.0003(3) Si C24 0.056(1) 0.071(2) 0.043(2) 0.020(1) -0.001(1) -0.005(1) C C25 0.049(1) 0.060(2) 0.035(1) 0.005(1) 0.006(1) -0.007(1) C C26 0.077(2) 0.060(2) 0.042(1) -0.003(1) 0.023(1) 0.007(1) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag LI1 LI4 2.427(5) . . ? LI1 N1 2.038(4) . . ? LI1 C5 2.350(5) . . ? LI1 N4 1.964(4) . . ? LI2 LI3 2.404(5) . . ? LI2 LI4 2.389(6) . . ? LI2 N1 2.025(4) . . ? LI2 C4 2.484(4) . . ? LI2 N2 2.035(4) . . ? LI2 N3 2.080(4) . . ? LI3 N2 1.952(4) . . ? LI3 N3 2.048(4) . . ? LI3 C18 2.314(5) . . ? LI3 C23 2.492(5) . . ? LI4 N1 2.113(4) . . ? LI4 N3 2.039(4) . . ? LI4 C17 2.455(4) . . ? LI4 N4 2.021(4) . . ? N1 SI1 1.710(2) . . ? N1 C4 1.494(3) . . ? SI1 C1 1.873(2) . . ? SI1 C2 1.862(3) . . ? SI1 C3 1.871(3) . . ? C4 C5 1.507(3) . . ? C5 C6 1.421(3) . . ? C5 C10 1.394(3) . . ? C6 C7 1.400(3) . . ? C6 N2 1.411(3) . . ? C7 C8 1.373(4) . . ? C8 C9 1.373(4) . . ? C9 C10 1.374(4) . . ? N2 SI2 1.704(2) . . ? SI2 C11 1.867(3) . . ? SI2 C12 1.870(3) . . ? SI2 C13 1.863(3) . . ? N3 SI3 1.713(2) . . ? N3 C17 1.500(3) . . ? SI3 C14 1.881(3) . . ? SI3 C15 1.869(3) . . ? SI3 C16 1.879(3) . . ? C17 C18 1.506(3) . . ? C18 C19 1.414(3) . . ? C18 C23 1.396(3) . . ? C19 C20 1.407(3) . . ? C19 N4 1.410(3) . . ? C20 C21 1.394(4) . . ? C21 C22 1.380(4) . . ? C22 C23 1.373(4) . . ? N4 SI4 1.713(2) . . ? SI4 C24 1.874(3) . . ? SI4 C25 1.868(3) . . ? SI4 C26 1.876(3) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag LI4 LI1 N1 55.7(1) . . . ? LI4 LI1 C5 110.0(2) . . . ? LI4 LI1 N4 53.6(1) . . . ? N1 LI1 C5 68.3(1) . . . ? N1 LI1 N4 109.2(2) . . . ? C5 LI1 N4 141.4(2) . . . ? LI3 LI2 LI4 85.9(2) . . . ? LI3 LI2 N1 122.0(2) . . . ? LI3 LI2 C4 118.8(2) . . . ? LI3 LI2 N2 51.4(1) . . . ? LI3 LI2 N3 53.8(1) . . . ? LI4 LI2 N1 56.5(1) . . . ? LI4 LI2 C4 90.9(2) . . . ? LI4 LI2 N2 120.5(2) . . . ? LI4 LI2 N3 53.7(1) . . . ? N1 LI2 C4 36.95(9) . . . ? N1 LI2 N2 108.8(2) . . . ? N1 LI2 N3 110.2(2) . . . ? C4 LI2 N2 80.1(1) . . . ? C4 LI2 N3 142.2(2) . . . ? N2 LI2 N3 105.1(2) . . . ? LI2 LI3 N2 54.5(1) . . . ? LI2 LI3 N3 55.0(1) . . . ? LI2 LI3 C18 108.2(2) . . . ? LI2 LI3 C23 141.7(2) . . . ? N2 LI3 N3 109.5(2) . . . ? N2 LI3 C18 137.5(2) . . . ? N2 LI3 C23 146.3(2) . . . ? N3 LI3 C18 68.8(1) . . . ? N3 LI3 C23 94.7(2) . . . ? C18 LI3 C23 33.5(1) . . . ? LI1 LI4 LI2 84.7(2) . . . ? LI1 LI4 N1 52.8(1) . . . ? LI1 LI4 N3 120.9(2) . . . ? LI1 LI4 C17 117.8(2) . . . ? LI1 LI4 N4 51.4(1) . . . ? LI2 LI4 N1 53.0(1) . . . ? LI2 LI4 N3 55.4(1) . . . ? LI2 LI4 C17 89.9(2) . . . ? LI2 LI4 N4 120.7(2) . . . ? N1 LI4 N3 108.4(2) . . . ? N1 LI4 C17 140.2(2) . . . ? N1 LI4 N4 104.1(2) . . . ? N3 LI4 C17 37.57(9) . . . ? N3 LI4 N4 110.9(2) . . . ? C17 LI4 N4 81.1(1) . . . ? SI1 N1 C4 113.9(1) . . . ? N1 SI1 C1 106.62(9) . . . ? N1 SI1 C2 113.9(1) . . . ? N1 SI1 C3 113.7(1) . . . ? C1 SI1 C2 107.4(1) . . . ? C1 SI1 C3 109.0(1) . . . ? C2 SI1 C3 106.1(1) . . . ? N1 C4 C5 111.3(2) . . . ? C4 C5 C6 120.8(2) . . . ? C4 C5 C10 120.0(2) . . . ? C6 C5 C10 119.2(2) . . . ? C5 C6 C7 116.9(2) . . . ? C5 C6 N2 121.3(2) . . . ? C7 C6 N2 121.8(2) . . . ? C6 C7 C8 122.4(2) . . . ? C7 C8 C9 120.3(3) . . . ? C8 C9 C10 119.1(2) . . . ? C5 C10 C9 122.0(2) . . . ? C6 N2 SI2 121.2(1) . . . ? N2 SI2 C11 106.7(1) . . . ? N2 SI2 C12 112.7(1) . . . ? N2 SI2 C13 115.0(1) . . . ? C11 SI2 C12 107.4(1) . . . ? C11 SI2 C13 108.9(1) . . . ? C12 SI2 C13 106.0(1) . . . ? SI3 N3 C17 113.0(1) . . . ? N3 SI3 C14 113.8(1) . . . ? N3 SI3 C15 113.6(1) . . . ? N3 SI3 C16 106.3(1) . . . ? C14 SI3 C15 106.1(1) . . . ? C14 SI3 C16 108.7(1) . . . ? C15 SI3 C16 108.1(1) . . . ? N3 C17 C18 110.8(2) . . . ? C17 C18 C19 120.9(2) . . . ? C17 C18 C23 119.0(2) . . . ? C19 C18 C23 119.9(2) . . . ? C18 C19 C20 116.9(2) . . . ? C18 C19 N4 121.7(2) . . . ? C20 C19 N4 121.4(2) . . . ? C19 C20 C21 121.6(2) . . . ? C20 C21 C22 120.6(2) . . . ? C21 C22 C23 118.6(2) . . . ? C18 C23 C22 122.2(3) . . . ? C19 N4 SI4 118.9(1) . . . ? N4 SI4 C24 108.1(1) . . . ? N4 SI4 C25 114.7(1) . . . ? N4 SI4 C26 112.0(1) . . . ? C24 SI4 C25 107.8(1) . . . ? C24 SI4 C26 108.0(1) . . . ? C25 SI4 C26 106.0(1) . . . ? #====================================================================== data_st416 #====================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C34 H64 Li4 N4 O2 Si4' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H64 Li4 N4 O2 Si4' _chemical_formula_weight 701.02 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Li ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Si ? 0.072 0.071 International_Tables_Vol_IV_Table_2.3.1 #====================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 19.9167(9) _cell_length_b 9.8818(2) _cell_length_c 22.1151(9) _cell_angle_alpha 90 _cell_angle_beta 99.750(2) _cell_angle_gamma 90 _cell_volume 4289.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 29787 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.5 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.09 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #====================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 29787 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 35. mm. Scan angle = 2.1 deg 1 scans of 100 sec per frame. Data collection was divided into 2 sets with the following starting angles and number of frames : Set 1 Theta = 8.09 Omega = 180.00 Kappa = 0.00 87 frames Set 2 Theta = -8.08 Kappa = 173.50 Phi = 0.00 32 frames Friedel pairs were not averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29787 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 27.53 _reflns_number_total 10292 _reflns_number_gt 4972 _reflns_threshold_expression 3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #====================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4972 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.102 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_all 0.097 _refine_ls_wR_factor_ref 0.064 _refine_ls_goodness_of_fit_all 1.580 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_shift/su_max 0.004 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.483 _refine_diff_density_min -0.173 #====================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol LI1 0.3144(3) -0.0519(4) 0.0843(2) 0.030(3) 1.000 Uani ? ? Li LI2 0.2361(3) -0.1876(4) 0.2036(2) 0.026(2) 1.000 Uani ? ? Li LI3 0.1648(3) -0.3698(5) 0.1503(2) 0.032(3) 1.000 Uani ? ? Li LI4 0.3327(3) -0.2339(4) 0.1616(2) 0.025(2) 1.000 Uani ? ? Li N1 0.2980(1) -0.0419(2) 0.1762(1) 0.021(1) 1.000 Uani ? ? N SI1 0.36389(4) 0.01622(8) 0.23053(4) 0.0264(4) 1.000 Uani ? ? Si C1 0.4258(2) -0.1280(3) 0.2497(2) 0.039(2) 1.000 Uani ? ? C C2 0.3372(2) 0.0761(3) 0.3036(2) 0.041(2) 1.000 Uani ? ? C C3 0.4131(2) 0.1595(3) 0.2043(2) 0.041(2) 1.000 Uani ? ? C C4 0.2387(1) 0.0534(3) 0.1632(1) 0.024(1) 1.000 Uani ? ? C C5 0.1863(1) 0.0128(2) 0.1078(1) 0.022(1) 1.000 Uani ? ? C C6 0.1392(1) -0.0953(2) 0.1107(1) 0.022(1) 1.000 Uani ? ? C C7 0.0932(2) -0.1229(3) 0.0568(1) 0.031(2) 1.000 Uani ? ? C C8 0.0918(2) -0.0514(3) 0.0027(1) 0.037(2) 1.000 Uani ? ? C C9 0.1373(2) 0.0529(3) 0.0004(1) 0.036(2) 1.000 Uani ? ? C C10 0.1837(1) 0.0840(3) 0.0529(1) 0.028(1) 1.000 Uani ? ? C N2 0.1396(1) -0.1735(2) 0.1646(1) 0.023(1) 1.000 Uani ? ? N SI2 0.07789(4) -0.14818(7) 0.20896(4) 0.0284(4) 1.000 Uani ? ? Si C11 0.0757(2) -0.2990(3) 0.2600(1) 0.043(2) 1.000 Uani ? ? C C12 0.0962(2) 0.0030(3) 0.2614(2) 0.045(2) 1.000 Uani ? ? C C13 -0.0107(2) -0.1233(3) 0.1646(2) 0.044(2) 1.000 Uani ? ? C O1 0.0949(1) -0.5174(2) 0.13689(9) 0.033(1) 1.000 Uani ? ? O C14 0.2273(2) -0.5780(3) 0.2785(1) 0.040(2) 1.000 Uani ? ? C C15 0.3753(2) -0.5021(3) 0.2889(2) 0.042(2) 1.000 Uani ? ? C C16 0.2717(2) -0.2936(3) 0.3154(1) 0.039(2) 1.000 Uani ? ? C C17 0.2905(1) -0.4743(2) 0.1428(1) 0.026(1) 1.000 Uani ? ? C N3 0.2699(1) -0.3786(2) 0.1893(1) 0.022(1) 1.000 Uani ? ? N SI3 0.28585(4) -0.43796(8) 0.26321(4) 0.0272(4) 1.000 Uani ? ? Si C18 0.2604(1) -0.4377(2) 0.0771(1) 0.024(1) 1.000 Uani ? ? C C19 0.2868(1) -0.3285(2) 0.0460(1) 0.022(1) 1.000 Uani ? ? C C20 0.2545(2) -0.3040(3) -0.0147(1) 0.032(2) 1.000 Uani ? ? C C21 0.2013(2) -0.3809(3) -0.0443(1) 0.037(2) 1.000 Uani ? ? C C22 0.1767(2) -0.4877(3) -0.0143(1) 0.037(2) 1.000 Uani ? ? C C23 0.2065(2) -0.5145(3) 0.0458(1) 0.032(2) 1.000 Uani ? ? C C24 0.4753(2) -0.1194(3) 0.0798(2) 0.047(2) 1.000 Uani ? ? C C25 0.4194(2) -0.2867(3) -0.0313(2) 0.047(2) 1.000 Uani ? ? C C26 0.4658(2) -0.4221(3) 0.0904(2) 0.048(2) 1.000 Uani ? ? C C27 0.0346(2) -0.4958(3) 0.0913(2) 0.045(2) 1.000 Uani ? ? C C28 0.0203(4) -0.6387(6) 0.0606(3) 0.046(4) 0.500 Uani ? ? C N4 0.3420(1) -0.2473(2) 0.0742(1) 0.024(1) 1.000 Uani ? ? N SI4 0.42042(4) -0.26914(8) 0.05330(4) 0.0294(4) 1.000 Uani ? ? Si C29 0.0449(2) -0.7336(3) 0.1100(2) 0.045(2) 1.000 Uani ? ? C C30 0.0978(2) -0.6585(3) 0.1553(1) 0.038(2) 1.000 Uani ? ? C O2 0.3377(1) 0.0935(2) 0.02991(9) 0.036(1) 1.000 Uani ? ? O C31 0.3162(2) 0.0831(3) -0.0354(1) 0.049(2) 1.000 Uani ? ? C C32 0.2985(2) 0.2254(3) -0.0571(2) 0.050(2) 1.000 Uani ? ? C C33 0.3507(2) 0.3092(3) -0.0154(2) 0.044(2) 1.000 Uani ? ? C C34 0.3618(2) 0.2307(3) 0.0446(2) 0.042(2) 1.000 Uani ? ? C C28A -0.0085(3) -0.6267(5) 0.0924(3) 0.032(3) 0.500 Uani ? ? C H1 0.4630 -0.0992 0.2797 0.0531 1.000 Uiso calc C1 H H2 0.4035 -0.2018 0.2654 0.0531 1.000 Uiso calc C1 H H3 0.4422 -0.1556 0.2137 0.0531 1.000 Uiso calc C1 H H4 0.3760 0.1066 0.3312 0.0562 1.000 Uiso calc C2 H H5 0.3056 0.1485 0.2947 0.0562 1.000 Uiso calc C2 H H6 0.3163 0.0037 0.3218 0.0562 1.000 Uiso calc C2 H H7 0.4484 0.1858 0.2366 0.0562 1.000 Uiso calc C3 H H8 0.4325 0.1316 0.1699 0.0562 1.000 Uiso calc C3 H H9 0.3835 0.2340 0.1930 0.0562 1.000 Uiso calc C3 H H10 0.2554 0.1409 0.1560 0.0312 1.000 Uiso calc C4 H H11 0.2168 0.0560 0.1982 0.0312 1.000 Uiso calc C4 H H12 0.0614 -0.1943 0.0574 0.0412 1.000 Uiso calc C7 H H13 0.0596 -0.0742 -0.0326 0.0509 1.000 Uiso calc C8 H H14 0.1370 0.1026 -0.0364 0.0480 1.000 Uiso calc C9 H H15 0.2147 0.1564 0.0514 0.0371 1.000 Uiso calc C10 H H16 0.0416 -0.2862 0.2848 0.0543 1.000 Uiso calc C11 H H17 0.0654 -0.3778 0.2355 0.0543 1.000 Uiso calc C11 H H18 0.1188 -0.3095 0.2855 0.0543 1.000 Uiso calc C11 H H19 0.0608 0.0129 0.2849 0.0566 1.000 Uiso calc C12 H H20 0.1384 -0.0101 0.2881 0.0566 1.000 Uiso calc C12 H H21 0.0987 0.0822 0.2375 0.0566 1.000 Uiso calc C12 H H22 -0.0416 -0.1101 0.1924 0.0584 1.000 Uiso calc C13 H H23 -0.0113 -0.0463 0.1388 0.0584 1.000 Uiso calc C13 H H24 -0.0238 -0.2011 0.1402 0.0584 1.000 Uiso calc C13 H H25 0.2388 -0.6060 0.3200 0.0542 1.000 Uiso calc C14 H H26 0.1816 -0.5465 0.2709 0.0542 1.000 Uiso calc C14 H H27 0.2318 -0.6523 0.2522 0.0542 1.000 Uiso calc C14 H H28 0.3800 -0.5331 0.3301 0.0569 1.000 Uiso calc C15 H H29 0.3841 -0.5747 0.2632 0.0569 1.000 Uiso calc C15 H H30 0.4068 -0.4310 0.2865 0.0569 1.000 Uiso calc C15 H H31 0.2802 -0.3237 0.3568 0.0523 1.000 Uiso calc C16 H H32 0.3019 -0.2215 0.3105 0.0523 1.000 Uiso calc C16 H H33 0.2260 -0.2630 0.3053 0.0523 1.000 Uiso calc C16 H H34 0.2757 -0.5628 0.1511 0.0338 1.000 Uiso calc C17 H H35 0.3388 -0.4734 0.1469 0.0338 1.000 Uiso calc C17 H H36 0.2701 -0.2307 -0.0364 0.0419 1.000 Uiso calc C20 H H37 0.1814 -0.3605 -0.0854 0.0509 1.000 Uiso calc C21 H H38 0.1401 -0.5417 -0.0343 0.0509 1.000 Uiso calc C22 H H39 0.1897 -0.5880 0.0665 0.0407 1.000 Uiso calc C23 H H40 0.5188 -0.1309 0.0684 0.0621 1.000 Uiso calc C24 H H41 0.4546 -0.0396 0.0614 0.0621 1.000 Uiso calc C24 H H42 0.4803 -0.1120 0.1232 0.0621 1.000 Uiso calc C24 H H43 0.4647 -0.2984 -0.0387 0.0601 1.000 Uiso calc C25 H H44 0.3928 -0.3632 -0.0463 0.0601 1.000 Uiso calc C25 H H45 0.4003 -0.2076 -0.0517 0.0601 1.000 Uiso calc C25 H H46 0.5089 -0.4306 0.0777 0.0652 1.000 Uiso calc C26 H H47 0.4723 -0.4126 0.1338 0.0652 1.000 Uiso calc C26 H H48 0.4394 -0.5007 0.0786 0.0652 1.000 Uiso calc C26 H H49 0.2774 0.0259 -0.0446 0.0654 1.000 Uiso calc C31 H H50 0.3520 0.0483 -0.0544 0.0654 1.000 Uiso calc C31 H H51 0.2535 0.2485 -0.0521 0.0708 1.000 Uiso calc C32 H H52 0.3030 0.2364 -0.0989 0.0708 1.000 Uiso calc C32 H H53 0.3336 0.3974 -0.0098 0.0568 1.000 Uiso calc C33 H H54 0.3918 0.3161 -0.0315 0.0568 1.000 Uiso calc C33 H H55 0.4088 0.2297 0.0620 0.0551 1.000 Uiso calc C34 H H56 0.3366 0.2709 0.0728 0.0551 1.000 Uiso calc C34 H H57 0.0878 -0.6670 0.1956 0.0503 1.000 Uiso calc C30 H H58 0.1419 -0.6942 0.1542 0.0503 1.000 Uiso calc C30 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol LI1 0.034(3) 0.024(2) 0.033(3) 0.001(2) 0.006(2) -0.001(2) Li LI2 0.026(3) 0.028(2) 0.025(2) 0.003(2) 0.003(2) 0.003(2) Li LI3 0.034(3) 0.025(2) 0.039(3) -0.004(2) 0.008(2) -0.000(2) Li LI4 0.031(3) 0.019(2) 0.028(2) 0.001(2) 0.004(2) -0.004(2) Li N1 0.020(1) 0.018(1) 0.025(1) 0.0022(9) 0.001(1) -0.0043(9) N SI1 0.0237(4) 0.0253(4) 0.0307(4) 0.0025(3) -0.0033(4) -0.0088(3) Si C1 0.031(2) 0.041(2) 0.047(2) 0.006(1) -0.004(2) -0.010(2) C C2 0.049(2) 0.035(2) 0.041(2) 0.009(1) -0.006(2) -0.014(1) C C3 0.033(2) 0.039(2) 0.054(2) -0.006(1) -0.004(2) -0.010(2) C C4 0.021(1) 0.021(1) 0.030(1) 0.000(1) 0.005(1) 0.001(1) C C5 0.020(1) 0.022(1) 0.024(1) 0.004(1) 0.003(1) -0.000(1) C C6 0.019(1) 0.021(1) 0.028(1) 0.004(1) 0.006(1) 0.000(1) C C7 0.029(2) 0.030(1) 0.034(2) -0.007(1) -0.003(1) 0.001(1) C C8 0.040(2) 0.044(2) 0.028(2) -0.007(2) -0.009(2) 0.003(1) C C9 0.038(2) 0.044(2) 0.027(2) 0.000(1) 0.000(1) 0.013(1) C C10 0.023(2) 0.029(1) 0.034(2) -0.001(1) 0.004(1) 0.007(1) C N2 0.021(1) 0.021(1) 0.028(1) 0.0029(9) 0.005(1) 0.005(1) N SI2 0.0247(4) 0.0271(4) 0.0344(4) 0.0041(3) 0.0083(4) 0.0051(4) Si C11 0.038(2) 0.041(2) 0.050(2) 0.003(1) 0.019(2) 0.009(2) C C12 0.042(2) 0.046(2) 0.045(2) 0.006(2) 0.016(2) -0.005(2) C C13 0.032(2) 0.048(2) 0.058(2) 0.006(2) 0.016(2) 0.003(2) C O1 0.030(1) 0.030(1) 0.039(1) -0.0051(9) 0.003(1) 0.0000(9) O C14 0.047(2) 0.041(2) 0.034(2) 0.003(2) -0.002(2) 0.011(1) C C15 0.046(2) 0.044(2) 0.036(2) 0.016(2) -0.007(2) 0.003(2) C C16 0.043(2) 0.049(2) 0.028(2) 0.003(2) 0.004(2) -0.002(2) C C17 0.031(2) 0.019(1) 0.030(1) 0.003(1) 0.008(1) -0.002(1) C N3 0.026(1) 0.023(1) 0.019(1) 0.005(1) 0.002(1) -0.002(1) N SI3 0.0330(5) 0.0268(4) 0.0228(4) 0.0069(3) -0.0011(4) 0.0022(3) Si C18 0.023(1) 0.024(1) 0.024(1) 0.003(1) 0.006(1) -0.007(1) C C19 0.021(1) 0.022(1) 0.023(1) 0.004(1) 0.004(1) -0.004(1) C C20 0.034(2) 0.038(1) 0.025(2) -0.005(1) 0.007(1) 0.002(1) C C21 0.039(2) 0.052(2) 0.024(2) -0.007(2) -0.002(2) -0.000(1) C C22 0.027(2) 0.054(2) 0.034(2) -0.014(1) -0.003(1) -0.012(2) C C23 0.032(2) 0.032(1) 0.032(2) -0.006(1) 0.011(1) -0.005(1) C C24 0.030(2) 0.052(2) 0.064(2) -0.009(2) 0.016(2) -0.019(2) C C25 0.036(2) 0.058(2) 0.048(2) -0.001(2) 0.018(1) -0.013(2) C C26 0.032(2) 0.047(2) 0.072(2) 0.009(2) 0.009(2) -0.004(2) C C27 0.040(2) 0.038(2) 0.060(2) -0.005(2) -0.022(2) 0.005(2) C C28 0.086(6) 0.027(3) 0.043(4) -0.011(3) -0.010(4) 0.006(3) C N4 0.022(1) 0.023(1) 0.028(1) -0.0020(9) 0.006(1) -0.007(1) N SI4 0.0245(4) 0.0286(4) 0.0362(4) -0.0009(3) 0.0088(4) -0.0095(4) Si C29 0.045(2) 0.038(2) 0.053(2) -0.003(2) -0.014(2) -0.002(2) C C30 0.044(2) 0.029(1) 0.041(2) -0.001(1) 0.002(2) 0.008(1) C O2 0.044(1) 0.0273(9) 0.038(1) -0.0034(9) 0.014(1) 0.0014(9) O C31 0.078(2) 0.037(2) 0.041(2) -0.016(2) 0.026(2) -0.008(2) C C32 0.087(3) 0.042(2) 0.035(2) -0.017(2) 0.011(2) 0.002(2) C C33 0.056(2) 0.034(2) 0.044(2) -0.010(2) 0.018(2) -0.000(1) C C34 0.043(2) 0.036(2) 0.048(2) -0.010(1) 0.007(2) -0.004(2) C C28A 0.031(3) 0.029(3) 0.036(3) 0.003(3) 0.003(3) -0.002(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag LI1 LI4 2.467(7) . . ? LI1 N1 2.116(6) . . ? LI1 N4 2.030(5) . . ? LI1 O2 1.979(5) . . ? LI2 LI3 2.466(7) . . ? LI2 LI4 2.318(7) . . ? LI2 N1 2.051(5) . . ? LI2 C4 2.546(5) . . ? LI2 N2 1.974(6) . . ? LI2 N3 2.046(5) . . ? LI3 N2 2.042(5) . . ? LI3 O1 2.003(5) . . ? LI3 N3 2.127(6) . . ? LI4 N1 2.063(5) . . ? LI4 C17 2.531(5) . . ? LI4 N3 2.059(5) . . ? LI4 N4 1.978(5) . . ? N1 SI1 1.720(2) . . ? N1 C4 1.500(3) . . ? SI1 C1 1.886(3) . . ? SI1 C2 1.881(4) . . ? SI1 C3 1.870(3) . . ? C4 C5 1.522(4) . . ? C5 C6 1.431(4) . . ? C5 C10 1.396(4) . . ? C6 C7 1.402(4) . . ? C6 N2 1.420(4) . . ? C7 C8 1.385(4) . . ? C8 C9 1.379(4) . . ? C9 C10 1.390(4) . . ? N2 SI2 1.716(2) . . ? SI2 C11 1.874(3) . . ? SI2 C12 1.888(3) . . ? SI2 C13 1.884(4) . . ? O1 C27 1.447(4) . . ? O1 C30 1.451(3) . . ? C14 SI3 1.877(3) . . ? C15 SI3 1.886(4) . . ? C16 SI3 1.886(3) . . ? C17 N3 1.503(3) . . ? C17 C18 1.520(4) . . ? N3 SI3 1.716(2) . . ? C18 C19 1.427(4) . . ? C18 C23 1.398(4) . . ? C19 C20 1.408(4) . . ? C19 N4 1.417(4) . . ? C20 C21 1.376(4) . . ? C21 C22 1.380(4) . . ? C22 C23 1.385(4) . . ? C24 SI4 1.874(3) . . ? C25 SI4 1.875(4) . . ? C26 SI4 1.878(4) . . ? C27 C28 1.572(8) . . ? C28 C29 1.461(8) . . ? N4 SI4 1.717(2) . . ? C29 C30 1.518(5) . . ? O2 C31 1.440(4) . . ? O2 C34 1.456(4) . . ? C31 C32 1.508(5) . . ? C32 C33 1.514(5) . . ? C33 C34 1.521(5) . . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag LI4 LI1 N1 52.8(2) . . . ? LI4 LI1 N4 51.1(2) . . . ? LI4 LI1 O2 158.2(3) . . . ? N1 LI1 N4 103.8(2) . . . ? N1 LI1 O2 129.8(3) . . . ? N4 LI1 O2 121.9(3) . . . ? LI3 LI2 LI4 96.6(2) . . . ? LI3 LI2 N1 134.3(3) . . . ? LI3 LI2 C4 124.0(3) . . . ? LI3 LI2 N2 53.4(2) . . . ? LI3 LI2 N3 55.3(2) . . . ? LI4 LI2 N1 55.9(2) . . . ? LI4 LI2 C4 88.7(2) . . . ? LI4 LI2 N2 130.7(3) . . . ? LI4 LI2 N3 55.9(2) . . . ? N1 LI2 C4 36.1(1) . . . ? N1 LI2 N2 114.3(2) . . . ? N1 LI2 N3 111.8(2) . . . ? C4 LI2 N2 81.8(2) . . . ? C4 LI2 N3 141.4(2) . . . ? N2 LI2 N3 108.6(3) . . . ? LI2 LI3 N2 50.9(2) . . . ? LI2 LI3 O1 158.7(3) . . . ? LI2 LI3 N3 52.3(2) . . . ? N2 LI3 O1 122.2(3) . . . ? N2 LI3 N3 103.1(2) . . . ? O1 LI3 N3 129.9(3) . . . ? LI1 LI4 LI2 95.6(2) . . . ? LI1 LI4 N1 54.8(2) . . . ? LI1 LI4 C17 124.4(3) . . . ? LI1 LI4 N3 133.3(3) . . . ? LI1 LI4 N4 53.0(2) . . . ? LI2 LI4 N1 55.5(2) . . . ? LI2 LI4 C17 88.6(2) . . . ? LI2 LI4 N3 55.4(2) . . . ? LI2 LI4 N4 128.7(3) . . . ? N1 LI4 C17 141.1(3) . . . ? N1 LI4 N3 110.8(2) . . . ? N1 LI4 N4 107.7(2) . . . ? C17 LI4 N3 36.4(1) . . . ? C17 LI4 N4 82.0(2) . . . ? N3 LI4 N4 113.9(2) . . . ? SI1 N1 C4 114.0(2) . . . ? N1 SI1 C1 107.3(1) . . . ? N1 SI1 C2 114.3(1) . . . ? N1 SI1 C3 114.5(1) . . . ? C1 SI1 C2 108.3(2) . . . ? C1 SI1 C3 106.5(2) . . . ? C2 SI1 C3 105.5(2) . . . ? N1 C4 C5 113.5(2) . . . ? C4 C5 C6 121.7(2) . . . ? C4 C5 C10 119.2(3) . . . ? C6 C5 C10 119.1(3) . . . ? C5 C6 C7 116.5(3) . . . ? C5 C6 N2 122.2(3) . . . ? C7 C6 N2 121.3(3) . . . ? C6 C7 C8 123.4(3) . . . ? C7 C8 C9 119.7(3) . . . ? C8 C9 C10 118.8(3) . . . ? C5 C10 C9 122.5(3) . . . ? C6 N2 SI2 119.8(2) . . . ? N2 SI2 C11 108.7(1) . . . ? N2 SI2 C12 112.5(1) . . . ? N2 SI2 C13 114.8(1) . . . ? C11 SI2 C12 106.3(2) . . . ? C11 SI2 C13 107.5(2) . . . ? C12 SI2 C13 106.4(2) . . . ? C27 O1 C30 109.0(2) . . . ? N3 C17 C18 113.2(2) . . . ? C17 N3 SI3 114.1(2) . . . ? C14 SI3 C15 106.4(2) . . . ? C14 SI3 C16 106.6(2) . . . ? C14 SI3 N3 113.8(1) . . . ? C15 SI3 C16 107.5(2) . . . ? C15 SI3 N3 114.5(1) . . . ? C16 SI3 N3 107.6(1) . . . ? C17 C18 C19 121.5(3) . . . ? C17 C18 C23 119.3(3) . . . ? C19 C18 C23 119.1(3) . . . ? C18 C19 C20 116.3(3) . . . ? C18 C19 N4 122.5(3) . . . ? C20 C19 N4 121.2(3) . . . ? C19 C20 C21 123.3(3) . . . ? C20 C21 C22 120.1(3) . . . ? C21 C22 C23 118.5(3) . . . ? C18 C23 C22 122.7(3) . . . ? O1 C27 C28 103.7(4) . . . ? C27 C28 C29 103.9(5) . . . ? C19 N4 SI4 118.9(2) . . . ? C24 SI4 C25 107.0(2) . . . ? C24 SI4 C26 106.6(2) . . . ? C24 SI4 N4 109.0(1) . . . ? C25 SI4 C26 106.5(2) . . . ? C25 SI4 N4 115.1(1) . . . ? C26 SI4 N4 112.1(1) . . . ? C28 C29 C30 106.6(4) . . . ? O1 C30 C29 107.2(3) . . . ? C31 O2 C34 108.8(2) . . . ? O2 C31 C32 105.4(3) . . . ? C31 C32 C33 102.6(3) . . . ? C32 C33 C34 103.6(3) . . . ? O2 C34 C33 106.6(3) . . . ?