Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Scherer, W.' ; Anorganisch-chemisches Institut Technische Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen (Germany) ; 'Sirsch, P.' ; Anorganisch-chemisches Institut Technische Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen (Germany) ; 'Grosche, M.' ; Anorganisch-chemisches Institut Technische Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen (Germany) ; 'Spiegler, M.' ; Anorganisch-chemisches Institut Technische Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching bei Munchen (Germany) ; 'Mason, S. A.' ; Institut Laue-Langevin BP156 F-38042 Grenoble Cedex 9 (France) ; 'Gardiner, M.G.' ; School of Chemistry University of Sydney Building F11 Sydney, 2006 (N. S. W. Australia) ; # 0. AUDIT DETAILS _audit_creation_date 'Apr 26 16:56:04 2001' _audit_creation_method 'PLATON option' _audit_update_record ; 27.04.01 updated by author P. Sirsch 30.04.01 updated by author P. Sirsch ; #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondence ; Dr. Wolfgang Scherer ; _publ_contact_author_address # address of author for correspondence ; Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching GERMANY ; _publ_contact_author_email wolfgang.scherer@ch.tum.de _publ_contact_author_fax '49(89)28913473' _publ_contact_author_phone '49(89)28913096' _publ_requested_journal 'Chem. Commun.' # Publication choise FI FM FO CI CM CO _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Regular Structural Paper. ; #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Agostic Deformations based on Electron Delocalization in the Alkyllithium-complex [{2-(Me3Si)2CLiC5H4N}2] ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; # Insert blank lines between paragraphs _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; # Insert blank lines between references _publ_section_references ; Blessing, R.H. (1995), Acta Cryst. A51, 33-37. COLLECT. Data Collection Software. Nonius BV, 1998. Koritsanszky, T., Howard, S.T., Richter, T., Mallinson, P.R., Su, Z., and Hansen, N.K. (1995). XD - a computer program package for multipole refinement and analysis of charge densities from diffraction data. Otwinowski, Z., Minor, W., Processing of X-ray Diffraction Data Collected in Oscillation Mode, Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p. 307-326, 1997, Carter, C.W., Jr., Sweet, R.M., Eds., Academic Press. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. Spek, A.L. (1990). Acta Cryst. A46, C-34. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_acknowledgements ; ? ; _publ_section_figure_captions ; View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. ; #=============================================================================== data_li_xd_115 # compound 1 _database_code_CSD 169890 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 Li2 N2 Si4' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C24 H44 Li2 N2 Si4' _chemical_formula_weight 486.85 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Si Si 0.0817 0.0704 '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' Li Li -0.0003 0.0001 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' 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 11.7233(2) _cell_length_b 9.8814(2) _cell_length_c 12.7702(2) _cell_angle_alpha 90 _cell_angle_beta 93.4810(11) _cell_angle_gamma 90 _cell_volume 1476.60(5) _cell_formula_units_Z 2 _cell_measurement_temperature 115 _cell_measurement_reflns_used 28093 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; ? ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 1.12 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.28 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.215 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SORTAV (R.H. Blessing, 1995)' _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.942 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 115 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD (Nonius)' _diffrn_measurement_method 'rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 80348 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 50.61 _diffrn_reflns_theta_full 50.61 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 15534 # number of observed reflections (> n sig(I)) _reflns_number_gt 8905 _reflns_threshold_expression 'F>3\s(F)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'XD (Koritsanszky et al, 1995)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; The lithium and hydrogen atom positions and their anisotropic thermal parameters were fixed at the values obtained by neutron diffraction (100 K) while the thermal parameters of the neutron study were scaled by the average ratio (U(xray)/U(neutron)) = 1.30 for the heavy atoms to account for the temperature difference. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo)]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 8905 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_gt 0.0314 _refine_ls_R_Fsqd_factor 0.0265 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.21 _refine_diff_density_min -0.20 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Si1 Si Uani 0.36009(1) 0.36447(1) 0.14265(1) 1.000 0.0184(1) Si2 Si Uani 0.30228(1) 0.26310(1) -0.08625(1) 1.000 0.0194(1) N N Uani 0.32170(4) 0.65175(5) 0.01422(4) 1.000 0.0173(1) C1 C Uani 0.34445(3) 0.40747(4) 0.00109(3) 1.000 0.0154(1) C2 C Uani 0.21836(5) 0.35769(7) 0.20396(4) 1.000 0.0363(2) C3 C Uani 0.44800(8) 0.49177(8) 0.22359(5) 1.000 0.0328(2) C4 C Uani 0.43410(5) 0.19839(7) 0.16947(5) 1.000 0.0349(2) C5 C Uani 0.25199(5) 0.31911(7) -0.22208(4) 1.000 0.0343(1) C6 C Uani 0.18768(5) 0.14550(5) -0.04195(5) 1.000 0.0312(1) C7 C Uani 0.43079(6) 0.15207(8) -0.10675(7) 1.000 0.0326(2) C11 C Uani 0.27294(3) 0.53035(4) -0.01261(3) 1.000 0.0150(1) C12 C Uani 0.15600(4) 0.52954(5) -0.04788(4) 1.000 0.0225(1) C13 C Uani 0.09272(4) 0.64778(5) -0.05310(4) 1.000 0.0265(1) C14 C Uani 0.14460(4) 0.77001(5) -0.02328(4) 1.000 0.0240(1) C15 C Uani 0.25923(4) 0.76603(5) 0.00900(3) 1.000 0.0210(1) Li Li Uani 0.51919 0.39297 -0.05280 1.000 0.0284 H2A H Uani 0.22900 0.33521 0.28731 1.000 0.0886 H2B H Uani 0.16371 0.27859 0.16845 1.000 0.0689 H2C H Uani 0.17169 0.45205 0.19426 1.000 0.0742 H3A H Uani 0.45026 0.46178 0.30606 1.000 0.0701 H3B H Uani 0.41136 0.59432 0.22082 1.000 0.0653 H3C H Uani 0.53683 0.49804 0.20281 1.000 0.0657 H4A H Uani 0.44233 0.18219 0.25495 1.000 0.0736 H4B H Uani 0.52035 0.19701 0.14191 1.000 0.0685 H4C H Uani 0.38823 0.11186 0.13530 1.000 0.0686 H5A H Uani 0.23974 0.23074 -0.27289 1.000 0.0829 H5B H Uani 0.31118 0.38333 -0.25812 1.000 0.1003 H5C H Uani 0.17037 0.37072 -0.22631 1.000 0.0962 H6A H Uani 0.17366 0.06305 -0.09905 1.000 0.0671 H6B H Uani 0.10642 0.19677 -0.03671 1.000 0.0693 H6C H Uani 0.21003 0.09903 0.03440 1.000 0.0678 H7A H Uani 0.40248 0.06223 -0.15068 1.000 0.0783 H7B H Uani 0.47515 0.11794 -0.03447 1.000 0.0727 H7C H Uani 0.49471 0.19902 -0.15460 1.000 0.0667 H12 H Uani 0.11450 0.43384 -0.06803 1.000 0.0516 H13 H Uani 0.00191 0.64463 -0.08010 1.000 0.0564 H14 H Uani 0.09735 0.86567 -0.02670 1.000 0.0499 H15 H Uani 0.30452 0.85932 0.03114 1.000 0.0470 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 0.0171(1) 0.0209(1) 0.0171(1) 0.0037(1) -0.0005(1) 0.0004(1) Si2 0.0152(1) 0.0196(1) 0.0232(1) -0.0053(1) 0.0000(1) -0.0006(1) N 0.0158(1) 0.0158(2) 0.0203(2) -0.0018(1) -0.0002(1) 0.0005(1) C1 0.0139(1) 0.0161(1) 0.0161(1) -0.0001(1) 0.0000(1) 0.0013(1) C2 0.0262(2) 0.0590(4) 0.0244(2) 0.0090(2) 0.0080(2) 0.0003(2) C3 0.0428(3) 0.0346(3) 0.0200(2) -0.0005(2) -0.0073(2) -0.0082(3) C4 0.0370(3) 0.0277(2) 0.0389(3) 0.0106(2) -0.0079(2) 0.0071(2) C5 0.0315(2) 0.0485(3) 0.0220(2) -0.0059(2) -0.0056(2) -0.0046(2) C6 0.0262(2) 0.0222(2) 0.0453(3) -0.0046(2) 0.0033(2) -0.0072(2) C7 0.0243(2) 0.0278(3) 0.0458(3) -0.0152(3) 0.0023(2) 0.0046(2) C11 0.0123(1) 0.0162(1) 0.0166(1) 0.0012(1) 0.0008(1) 0.0004(1) C12 0.0126(1) 0.0197(2) 0.0349(2) 0.0022(1) -0.0021(1) 0.0001(1) C13 0.0145(1) 0.0239(2) 0.0407(2) 0.0050(2) -0.0015(1) 0.0035(1) C14 0.0199(2) 0.0199(2) 0.0325(2) 0.0035(1) 0.0030(1) 0.0055(1) C15 0.0210(2) 0.0168(2) 0.0252(2) -0.0010(1) 0.0015(1) 0.0022(1) Li 0.0153 0.0408 0.0290 -0.0020 0.0010 0.0020 H2A 0.0671 0.1648 0.0348 0.0213 0.0097 -0.0034 H2B 0.0470 0.0813 0.0792 0.0035 0.0104 -0.0164 H2C 0.0557 0.0811 0.0879 -0.0007 0.0220 0.0216 H3A 0.0950 0.0813 0.0315 0.0079 -0.0155 -0.0168 H3B 0.0962 0.0444 0.0547 -0.0112 -0.0012 -0.0003 H3C 0.0445 0.0863 0.0652 0.0013 -0.0050 -0.0206 H4A 0.0991 0.0695 0.0501 0.0234 -0.0138 0.0130 H4B 0.0458 0.0704 0.0888 0.0085 0.0004 0.0204 H4C 0.0822 0.0351 0.0858 0.0011 -0.0168 0.0006 H5A 0.1170 0.0799 0.0504 -0.0276 -0.0074 -0.0074 H5B 0.1060 0.1347 0.0573 0.0358 -0.0198 -0.0664 H5C 0.0836 0.1469 0.0555 -0.0006 -0.0175 0.0551 H6A 0.0737 0.0506 0.0773 -0.0261 0.0062 -0.0229 H6B 0.0367 0.0547 0.1184 0.0028 0.0193 0.0010 H6C 0.0741 0.0627 0.0662 0.0164 0.0000 -0.0176 H7A 0.0579 0.0547 0.1220 -0.0519 0.0030 -0.0007 H7B 0.0666 0.0796 0.0704 0.0019 -0.0071 0.0358 H7C 0.0505 0.0635 0.0890 -0.0110 0.0274 0.0030 H12 0.0312 0.0320 0.0900 -0.0050 -0.0107 -0.0055 H13 0.0245 0.0514 0.0915 0.0040 -0.0116 0.0046 H14 0.0425 0.0331 0.0740 0.0039 0.0031 0.0154 H15 0.0411 0.0290 0.0697 -0.0085 -0.0064 -0.0034 #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Si1 C1 1.8552(4) . . yes Si1 C2 1.8804(6) . . yes Si1 C3 1.8930(8) . . yes Si1 C4 1.8781(7) . . yes Si2 C1 1.8592(4) . . yes Si2 C5 1.8811(5) . . yes Si2 C6 1.8888(6) . . yes Si2 C7 1.8947(7) . . yes Si2 Li 2.8572 . . yes N C11 1.3636(6) . . yes N C15 1.3454(7) . . yes N Li 1.9508 . 3_665 yes C1 C11 1.4798(5) . . no C1 Li 2.2049 . . yes C11 C12 1.4168(6) . . no C12 C13 1.3834(7) . . no C13 C14 1.3948(7) . . no C14 C15 1.3821(7) . . no C2 H2A 1.0871 . . no C2 H2B 1.0917 . . no C2 H2C 1.0844 . . no C3 H3A 1.0928 . . no C3 H3B 1.1003 . . no C3 H3C 1.0919 . . no C4 H4A 1.1017 . . no C4 H4B 1.0907 . . no C4 H4C 1.0873 . . no C5 H5A 1.0922 . . no C5 H5B 1.0653 . . no C5 H5C 1.0827 . . no C6 H6A 1.0991 . . no C6 H6B 1.0846 . . no C6 H6C 1.0950 . . no C7 H7A 1.0910 . . no C7 H7B 1.0853 . . no C7 H7C 1.0981 . . no C12 H12 1.0872 . . no C13 H13 1.0994 . . no C14 H14 1.0951 . . no C15 H15 1.0924 . . no 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 C1 Si1 C2 112.11(2) . . . yes C1 Si1 C3 113.46(2) . . . yes C1 Si1 C4 113.27(2) . . . yes C2 Si1 C3 105.18(3) . . . yes C2 Si1 C4 107.64(3) . . . yes C3 Si1 C4 104.53(3) . . . yes C1 Si2 C5 112.61(2) . . . yes C1 Si2 C6 117.42(2) . . . yes C1 Si2 C7 110.03(3) . . . yes C1 Si2 Li 50.50 . . . yes C5 Si2 C6 105.57(3) . . . yes C5 Si2 C7 104.50(3) . . . yes C5 Si2 Li 103.41 . . . yes C6 Si2 C7 105.73(3) . . . yes C6 Si2 Li 150.96 . . . yes C7 Si2 Li 64.71 . . . yes C11 N C15 120.49(4) . . . yes C11 N Li 104.12 . . 3_665 yes C15 N Li 135.39 . . 3_665 yes Si1 C1 Si2 114.57(2) . . . yes Si1 C1 C11 108.96(3) . . . yes Si1 C1 Li 104.51 . . . yes Si2 C1 C11 115.50(3) . . . yes Si2 C1 Li 88.92 . . . yes C11 C1 Li 123.15 . . . yes N C11 C1 117.79(3) . . . yes N C11 C12 117.88(4) . . . yes C1 C11 C12 124.28(4) . . . no C11 C12 C13 121.08(4) . . . no C12 C13 C14 119.64(4) . . . no C13 C14 C15 117.18(4) . . . no N C15 C14 123.72(5) . . . yes H2A C2 H2C 108.34 . . . no H2B C2 H2C 106.79 . . . no Si1 C2 H2C 111.98 . . . no Si1 C2 H2A 111.30 . . . no Si1 C2 H2B 111.32 . . . no H2A C2 H2B 106.86 . . . no Si1 C3 H3A 109.06 . . . no H3B C3 H3C 108.43 . . . no Si1 C3 H3C 113.62 . . . no H3A C3 H3B 105.50 . . . no Si1 C3 H3B 113.32 . . . no H3A C3 H3C 106.37 . . . no Si1 C4 H4B 112.28 . . . no Si1 C4 H4C 113.72 . . . no Si1 C4 H4A 108.62 . . . no H4A C4 H4B 106.90 . . . no H4A C4 H4C 107.15 . . . no H4B C4 H4C 107.83 . . . no Si2 C5 H5B 113.44 . . . no Si2 C5 H5C 114.28 . . . no H5A C5 H5B 106.57 . . . no Si2 C5 H5A 109.58 . . . no H5A C5 H5C 105.25 . . . no H5B C5 H5C 107.14 . . . no Si2 C6 H6A 109.74 . . . no H6A C6 H6C 107.33 . . . no H6B C6 H6C 107.73 . . . no H6A C6 H6B 106.90 . . . no Si2 C6 H6B 111.99 . . . no Si2 C6 H6C 112.87 . . . no Si2 C7 H7A 108.82 . . . no H7B C7 H7C 107.25 . . . no Si2 C7 H7C 114.05 . . . no H7A C7 H7B 107.43 . . . no Si2 C7 H7B 113.98 . . . no H7A C7 H7C 104.73 . . . no C11 C12 H12 119.38 . . . no C13 C12 H12 119.49 . . . no C12 C13 H13 119.83 . . . no C14 C13 H13 120.53 . . . no C13 C14 H14 121.70 . . . no C15 C14 H14 121.12 . . . no N C15 H15 116.16 . . . no C14 C15 H15 120.11 . . . no N Li C1 145.90 3_665 . . yes Si2 Li N 139.88 . . 3_665 yes Si2 Li C1 40.59 . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Si1 C1 Si2 -80.20(3) . . . . no C2 Si1 C1 C11 50.92(4) . . . . no C2 Si1 C1 Li -175.75 . . . . no C3 Si1 C1 Si2 160.83(3) . . . . no C3 Si1 C1 C11 -68.05(4) . . . . no C3 Si1 C1 Li 65.27 . . . . no C4 Si1 C1 Si2 41.86(3) . . . . no C4 Si1 C1 C11 172.98(3) . . . . no C4 Si1 C1 Li -53.70 . . . . no C5 Si2 C1 Si1 165.53(2) . . . . no C5 Si2 C1 C11 37.66(4) . . . . no C5 Si2 C1 Li -88.99 . . . . no C6 Si2 C1 Si1 42.61(3) . . . . no C6 Si2 C1 C11 -85.26(3) . . . . no C6 Si2 C1 Li 148.09 . . . . no C7 Si2 C1 Si1 -78.34(3) . . . . no C7 Si2 C1 C11 153.79(4) . . . . no C7 Si2 C1 Li 27.14 . . . . no Li Si2 C1 Si1 -105.48 . . . . no Li Si2 C1 C11 126.65 . . . . no C1 Si2 Li N 126.16 . . . 3_665 no C5 Si2 Li C1 108.40 . . . . no C5 Si2 Li N -125.44 . . . 3_665 no C6 Si2 Li C1 -75.19 . . . . no C6 Si2 Li N 50.97 . . . 3_665 no C7 Si2 Li C1 -151.70 . . . . no C7 Si2 Li N -25.54 . . . 3_665 no C15 N C11 C1 -176.30(4) . . . . no C15 N C11 C12 1.29(7) . . . . no Li N C11 C1 4.19 3_665 . . . no Li N C11 C12 -178.21 3_665 . . . no C11 N C15 C14 -0.29(7) . . . . no Li N C15 C14 179.02 3_665 . . . no C11 N Li Si2 164.36 . . 3_665 3_665 no C11 N Li C1 94.81 . . 3_665 3_665 no C15 N Li Si2 -15.03 . . 3_665 3_665 no C15 N Li C1 -84.58 . . 3_665 3_665 no C11 N C15 H15 -179.51 . . . . no Li N C15 H15 -0.20 3_665 . . . no Si1 C1 C11 N 75.47(4) . . . . no Si2 C1 C11 C12 28.65(5) . . . . no Li C1 C11 N -47.27 . . . . no Li C1 C11 C12 135.31 . . . . no Si1 C1 Li Si2 115.13 . . . . no Si1 C1 Li N 3.27 . . . 3_665 no Si2 C1 Li N -111.86 . . . 3_665 no C11 C1 Li Si2 -120.13 . . . . no C11 C1 Li N 128.01 . . . 3_665 no Si2 C1 C11 N -153.92(3) . . . . no Si1 C1 C11 C12 -101.96(4) . . . . no C1 C11 C12 C13 176.25(4) . . . . no N C11 C12 C13 -1.17(7) . . . . no C11 C12 C13 C14 0.04(9) . . . . no C12 C13 C14 C15 0.95(7) . . . . no C13 C14 C15 N -0.86(7) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Si1 Li 3.0433 . 3_665 no Si2 Li 4.3165 . 3_665 no Si1 H6C 3.4044 . . no Si2 H4C 3.3026 . . no Si2 H12 2.7945 . . no Si2 H3C 3.4183 . 3_665 no N C3 3.3704(9) . . no N H3B 2.8374 . . no C3 N 3.3704(9) . . no C3 Li 2.5107 . 3_665 no C4 C7 3.5548(11) . . no C5 C12 3.2928(8) . . no C5 C14 3.5718(7) . 2_544 no C7 C4 3.5548(11) . . no C12 C5 3.2928(8) . . no C14 C5 3.5718(7) . 2_554 no C2 H13 2.9453 . 3_565 no C3 H5B 3.0882 . 3_665 no C4 H5C 3.0761 . 4_555 no C4 H7B 2.7926 . . no C5 H12 2.8528 . . no C5 H3C 3.0627 . 3_665 no C6 H2B 3.0198 . . no C6 H12 2.9883 . . no C6 H14 2.9716 . 1_545 no C11 H2C 3.0606 . . no C12 H5C 2.7803 . . no C12 H13 3.0704 . 3_565 no C13 H12 3.0661 . 3_565 no C13 H6B 3.0741 . 3_565 no C14 H6A 3.0785 . 1_565 no C14 H5A 3.0320 . 2_554 no C14 H5B 3.0808 . 2_554 no C15 H2A 2.6849 . 2_555 no C15 H5A 3.0360 . 2_554 no Li Si2 4.3165 . 3_665 no Li C3 2.5107 . 3_665 no Li Si1 3.0433 . 3_665 no Li Li 2.5630 . 3_665 no Li H3C 3.4196 . . no Li H4B 3.1509 . . no Li H3B 2.3441 . 3_665 no Li H3C 2.2601 . 3_665 no H2A C15 2.6849 . 2_545 no H2A H15 2.3868 . 2_545 no H2B C6 3.0198 . . no H2B H6C 2.5468 . . no H2B H3B 2.4981 . 2_545 no H2B H13 2.3135 . 3_565 no H2C C11 3.0606 . . no H3B N 2.8374 . . no H3B H2B 2.4981 . 2_555 no H3B Li 2.3441 . 3_665 no H3B H7C 2.4922 . 3_665 no H3C Li 3.4196 . . no H3C Si2 3.4183 . 3_665 no H3C C5 3.0627 . 3_665 no H3C Li 2.2601 . 3_665 no H3C H5B 2.2125 . 3_665 no H4B Li 3.1509 . . no H4B H7B 2.4124 . . no H4B H5C 2.4523 . 4_555 no H4C Si2 3.3026 . . no H4C H6C 2.3903 . . no H4C H7B 2.4516 . . no H5A C14 3.0320 . 2_544 no H5A C15 3.0360 . 2_544 no H5B C14 3.0808 . 2_544 no H5B H6A 2.5596 . 2_554 no H5B C3 3.0882 . 3_665 no H5B H3C 2.2125 . 3_665 no H5C C12 2.7803 . . no H5C H12 2.2504 . . no H5C H7A 2.5720 . 2_554 no H5C C4 3.0761 . 4_454 no H5C H4B 2.4523 . 4_454 no H6A C14 3.0785 . 1_545 no H6A H14 2.3576 . 1_545 no H6A H5B 2.5596 . 2_544 no H6B H12 2.3793 . . no H6B C13 3.0741 . 3_565 no H6B H13 2.5542 . 3_565 no H6C Si1 3.4044 . . no H6C H2B 2.5468 . . no H6C H4C 2.3903 . . no H7A H5C 2.5720 . 2_544 no H7B C4 2.7926 . . no H7B H4B 2.4124 . . no H7B H4C 2.4516 . . no H7B H7B 2.5466 . 3_655 no H7B H15 2.5905 . 3_665 no H7C H3B 2.4922 . 3_665 no H12 Si2 2.7945 . . no H12 C5 2.8528 . . no H12 C6 2.9883 . . no H12 H5C 2.2504 . . no H12 H6B 2.3793 . . no H12 C13 3.0661 . 3_565 no H12 H13 2.5210 . 3_565 no H13 C2 2.9453 . 3_565 no H13 C12 3.0704 . 3_565 no H13 H2B 2.3135 . 3_565 no H13 H6B 2.5542 . 3_565 no H13 H12 2.5210 . 3_565 no H14 C6 2.9716 . 1_565 no H14 H6A 2.3576 . 1_565 no H15 H2A 2.3868 . 2_555 no H15 H7B 2.5905 . 3_665 no loop_ _atom_rho_multipole_label _atom_rho_multipole_coeff_Pv _atom_rho_multipole_coeff_P00 _atom_rho_multipole_coeff_P11 _atom_rho_multipole_coeff_P1-1 _atom_rho_multipole_coeff_P10 _atom_rho_multipole_coeff_P20 _atom_rho_multipole_coeff_P21 _atom_rho_multipole_coeff_P2-1 _atom_rho_multipole_coeff_P22 _atom_rho_multipole_coeff_P2-2 _atom_rho_multipole_coeff_P30 _atom_rho_multipole_coeff_P31 _atom_rho_multipole_coeff_P3-1 _atom_rho_multipole_coeff_P32 _atom_rho_multipole_coeff_P3-2 _atom_rho_multipole_coeff_P33 _atom_rho_multipole_coeff_P3-3 _atom_rho_multipole_coeff_P40 _atom_rho_multipole_coeff_P41 _atom_rho_multipole_coeff_P4-1 _atom_rho_multipole_coeff_P42 _atom_rho_multipole_coeff_P4-2 _atom_rho_multipole_coeff_P43 _atom_rho_multipole_coeff_P4-3 _atom_rho_multipole_coeff_P44 _atom_rho_multipole_coeff_P4-4 _atom_rho_multipole_kappa_prime _atom_rho_multipole_kappa_dprime0 _atom_rho_multipole_kappa_dprime1 _atom_rho_multipole_kappa_dprime2 _atom_rho_multipole_kappa_dprime3 _atom_rho_multipole_kappa_dprime4 SI(2) 3.26(10) 0.00 -0.05(2) 0.13(2) 0.06(2) -0.02(2) 0.00(2) -0.01(2) -0.03(2) -0.11(2) -0.01(3) -0.22(3) -0.30(3) 0.06(3) 0.01(2) 0.36(3) -0.01(2) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.051(7) 1.00 1.00 1.00 1.00 1.00 SI(1) 3.23(11) 0.00 0.07(2) -0.01(2) 0.02(2) -0.07(2) 0.171(19) -0.03(2) -0.045(19) 0.02(2) -0.09(3) -0.21(3) -0.43(3) 0.13(2) -0.09(3) 0.28(3) 0.04(3) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.031(7) 1.00 1.00 1.00 1.00 1.00 N 5.33(5) 0.00 -0.009(13) -0.064(12) 0.004(11) -0.119(13) 0.018(11) 0.006(11) 0.022(12) 0.019(12) 0.002(11) -0.013(11) -0.018(11) -0.004(10) 0.015(10) 0.137(11) 0.014(11) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.983(2) 1.00 1.00 1.00 1.00 1.00 C(1) 4.52(4) 0.00 0.024(13) -0.024(13) -0.019(13) -0.029(13) -0.014(12) -0.021(12) -0.002(13) -0.045(12) -0.035(14) -0.054(13) -0.097(13) -0.015(13) 0.091(13) 0.107(13) 0.000(13) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.97 1.00 1.00 1.00 1.00 1.00 C(2) 4.44(6) 0.00 0.00 0.00 0.018(12) 0.043(12) 0.00 0.00 0.00 0.00 0.175(13) 0.00 0.00 0.00 0.00 0.004(11) 0.127(12) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.986(3) 1.00 1.00 1.00 1.00 1.00 C(3) 4.46(4) 0.00 0.06(2) 0.025(16) 0.029(17) 0.052(16) -0.042(19) 0.005(14) 0.012(16) 0.077(19) 0.176(16) -0.039(17) 0.003(14) -0.007(15) 0.006(17) -0.017(16) 0.225(16) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.98 1.00 1.00 1.00 1.00 1.00 C(4) 4.44 0.00 0.00 0.00 0.02 0.04 0.00 0.00 0.00 0.00 0.17 0.00 0.00 0.00 0.00 0.00 0.13 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.986(3) 1.00 1.00 1.00 1.00 1.00 C(5) 4.59(7) 0.00 0.00 0.00 0.014(12) 0.049(11) 0.00 0.00 0.00 0.00 0.236(12) 0.00 0.00 0.00 0.00 0.020(11) 0.144(11) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.984(3) 1.00 1.00 1.00 1.00 1.00 C(6) 4.59 0.00 0.00 0.00 0.01 0.05 0.00 0.00 0.00 0.00 0.24 0.00 0.00 0.00 0.00 0.02 0.14 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.984(3) 1.00 1.00 1.00 1.00 1.00 C(7) 4.54(10) 0.00 0.10(2) 0.006(17) 0.024(17) 0.019(16) -0.007(19) 0.049(15) 0.014(18) 0.053(19) 0.179(19) -0.065(16) 0.007(15) 0.005(17) -0.033(17) -0.047(16) 0.163(17) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.985(5) 1.00 1.00 1.00 1.00 1.00 C(11) 3.79(5) 0.00 0.000(11) 0.028(13) -0.040(14) 0.044(15) -0.006(12) 0.016(13) -0.143(12) 0.011(11) 0.184(16) 0.013(14) -0.004(15) 0.180(14) -0.022(13) 0.032(12) -0.013(12) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.030(4) 1.00 1.00 1.00 1.00 1.00 C(12) 4.13(3) 0.00 0.005(11) -0.019(10) 0.00 -0.193(9) 0.00 0.00 0.007(10) 0.002(8) 0.00 0.032(10) 0.030(9) 0.00 0.00 0.249(8) -0.018(11) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.009(2) 1.00 1.00 1.00 1.00 1.00 C(13) 4.13 0.00 0.01 -0.02 0.00 -0.19 0.00 0.00 0.01 0.00 0.00 0.03 0.03 0.00 0.00 0.25 -0.02 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.009(2) 1.00 1.00 1.00 1.00 1.00 C(14) 4.13 0.00 0.01 -0.02 0.00 -0.19 0.00 0.00 0.01 0.00 0.00 0.03 0.03 0.00 0.00 0.25 -0.02 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.009(2) 1.00 1.00 1.00 1.00 1.00 C(15) 4.02(4) 0.00 0.036(15) 0.040(15) 0.00 -0.182(15) 0.00 0.00 -0.021(14) 0.021(15) 0.00 0.009(14) 0.021(14) 0.00 0.00 0.300(15) -0.005(15) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.009(2) 1.00 1.00 1.00 1.00 1.00 LI 0.90(11) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(2A) 0.888(10) 0.00 0.00 0.00 0.099(6) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(2B) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(2C) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(3A) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(3B) 0.83(3) 0.00 0.00 0.00 0.06(2) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(3C) 0.91(3) 0.00 0.00 0.00 0.10(2) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(4A) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(4B) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(4C) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(5A) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(5B) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(5C) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(6A) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(6B) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(6C) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(7A) 0.89 0.00 0.00 0.00 0.10 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(7B) 0.82(3) 0.00 0.00 0.00 0.11(2) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(7C) 0.94(3) 0.00 0.00 0.00 0.17(2) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(12) 0.888(12) 0.00 0.00 0.00 0.125(9) 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(13) 0.89 0.00 0.00 0.00 0.12 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(14) 0.89 0.00 0.00 0.00 0.12 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 H(15) 0.89 0.00 0.00 0.00 0.12 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 1.20 1.20 1.20 1.20 1.20 1.20 loop_ _atom_local_axes_label _atom_local_axes_atom0 _atom_local_axes_ax1 _atom_local_axes_atom1 _atom_local_axes_atom2 _atom_local_axes_ax2 SI(2) C(7) X SI(2) C(1) Y SI(1) C(3) X SI(1) C(1) Y N C(11) X N C(15) Y C(1) SI(2) X C(1) SI(1) Y C(2) SI(1) Z C(2) C(1) Y C(3) SI(1) Z C(3) C(1) Y C(4) SI(1) Z C(4) C(1) Y C(5) SI(2) Z C(5) C(1) Y C(6) SI(2) Z C(6) C(1) Y C(7) SI(2) Z C(7) C(1) Y C(11) N Z C(11) C(12) Y C(12) C(11) X C(12) C(13) Y C(13) C(12) X C(13) C(14) Y C(14) C(13) X C(14) C(15) Y C(15) C(14) X C(15) N Y LI C(1) X LI SI(2) Y H(2A) C(2) Z H(2A) SI(1) Y H(2B) C(2) Z H(2B) SI(1) Y H(2C) C(2) Z H(2C) SI(1) Y H(3A) C(3) Z H(3A) SI(1) Y H(3B) C(3) Z H(3B) SI(1) Y H(3C) C(3) Z H(3C) SI(1) Y H(4A) C(4) Z H(4A) SI(1) Y H(4B) C(4) Z H(4B) SI(1) Y H(4C) C(4) Z H(4C) SI(1) Y H(5A) C(5) Z H(5A) SI(2) Y H(5B) C(5) Z H(5B) SI(2) Y H(5C) C(5) Z H(5C) SI(2) Y H(6A) C(6) Z H(6A) SI(2) Y H(6B) C(6) Z H(6B) SI(2) Y H(6C) C(6) Z H(6C) SI(2) Y H(7A) C(7) Z H(7A) SI(2) Y H(7B) C(7) Z H(7B) SI(2) Y H(7C) C(7) Z H(7C) SI(2) Y H(12) C(12) Z H(12) C(13) Y H(13) C(13) Z H(13) C(12) Y H(14) C(14) Z H(14) C(15) Y H(15) C(15) Z H(15) N Y # End of Crystallographic Information File # CIF-file generated for li_n_100 / compound 1 / 100 K neutron measurement #============================================================================== data_li_n_100 # compound 1 /100 K neutron measurement _database_code_CSD 169891 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 Li2 N2 Si4' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C24 H44 Li2 N2 Si4' _chemical_formula_weight 486.85 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Si Si 4.1491 'Sears, V. F. (1992) Neutron News 3, 26-37.' N N 9.36 'Sears, V. F. (1992) Neutron News 3, 26-37.' Li Li -1.90 'Sears, V. F. (1992) Neutron News 3, 26-37.' H H -3.7390 'Sears, V. F. (1992) Neutron News 3, 26-37.' C C 6.6460 'Sears, V. F. (1992) Neutron News 3, 26-37.' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' 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 11.7220(13) _cell_length_b 9.8640(12) _cell_length_c 12.7517(15) _cell_angle_alpha 90 _cell_angle_beta 93.479(4) _cell_angle_gamma 90 _cell_volume 1471.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 4132 _cell_measurement_theta_min 3.93 _cell_measurement_theta_max 39.97 _cell_special_details ; ? ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 4.5 _exptl_crystal_size_mid 2.2 _exptl_crystal_size_min 1.7 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.231 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # cylinder 'cylindrical' # empirical 'empirical from intensities' # gaussian 'Gaussian from crystal shape' # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # refdelf 'refined from delta-F' # sphere 'spherical' _exptl_absorpt_correction_type none # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.694 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.82306 _diffrn_radiation_type neutron _diffrn_radiation_monochromator 'Cu 220' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_details ; hot neutron four-circle diffractometer D9 at the ILL (Grenoble, France) ; _diffrn_measurement_method 'profile data from coupled \wx\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 9 0 3 -1 8 2 -2 0 8 # number of measured reflections (redundant set) _diffrn_reflns_number 4132 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 39.97 _diffrn_reflns_theta_full 39.97 _diffrn_measured_fraction_theta_max 0.62 _diffrn_measured_fraction_theta_full 0.62 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 3811 # number of observed reflections (> n sig(I)) _reflns_number_gt 3145 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'MAD, HKLGEN (ILL)' _computing_cell_refinement 'RAFD9 (ILL)' _computing_data_reduction 'RACER (ILL)' _computing_structure_solution 'SIR-92 (C. Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2, conventional R-factors R are based on F, with F set to zero for negative F^2. The observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. Density synthesis with coefficients Fo-Fc Highest peak 0.57 at 0.2620 0.6585 0.0383 [ 0.78 A from N ] Deepest hole -0.64 at 0.3720 0.6397 0.0462 [ 0.71 A from N ] All hydrogen atoms could be located with difference Fourier maps and were refined anisotropically. Unit cell contains no residual solvent accessible area. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+3.057P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'shelxl' _refine_ls_extinction_coef 0.0285(8) _refine_ls_extinction_expression 'FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^' _refine_ls_abs_structure_details none _refine_ls_number_reflns 3811 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.575 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.135 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Si1 Si Uani 0.35970(11) 0.36448(15) 0.14255(11) 1.000 0.0147(3) Si2 Si Uani 0.30233(11) 0.26314(15) -0.08654(12) 1.000 0.0150(3) N N Uani 0.32145(5) 0.65239(7) 0.01388(5) 1.000 0.0144(1) C1 C Uani 0.34450(7) 0.40762(9) 0.00074(7) 1.000 0.0123(2) C2 C Uani 0.21789(9) 0.35774(15) 0.20407(9) 1.000 0.0279(3) C3 C Uani 0.44730(10) 0.49276(12) 0.22394(9) 1.000 0.0257(3) C4 C Uani 0.43425(10) 0.19848(12) 0.16972(10) 1.000 0.0270(3) C5 C Uani 0.25182(10) 0.31850(13) -0.22274(9) 1.000 0.0266(3) C6 C Uani 0.18767(9) 0.14504(11) -0.04199(9) 1.000 0.0242(3) C7 C Uani 0.43098(8) 0.15144(12) -0.10682(10) 1.000 0.0253(3) C11 C Uani 0.27249(7) 0.53084(9) -0.01296(7) 1.000 0.0122(2) C12 C Uani 0.15549(7) 0.52956(10) -0.04801(8) 1.000 0.0176(2) C13 C Uani 0.09198(7) 0.64811(11) -0.05324(9) 1.000 0.0206(2) C14 C Uani 0.14394(8) 0.77074(10) -0.02332(8) 1.000 0.0190(3) C15 C Uani 0.25900(8) 0.76697(10) 0.00859(8) 1.000 0.0164(2) Li Li Uani 0.5192(3) 0.3930(4) -0.0528(3) 1.000 0.0218(9) H2A H Uani 0.2290(3) 0.3352(5) 0.2873(2) 1.000 0.0683(15) H2B H Uani 0.1637(3) 0.2786(4) 0.1684(3) 1.000 0.0530(10) H2C H Uani 0.1717(3) 0.4520(4) 0.1943(3) 1.000 0.0571(11) H3A H Uani 0.4503(3) 0.4618(4) 0.3061(2) 1.000 0.0539(10) H3B H Uani 0.4114(3) 0.5943(3) 0.2208(2) 1.000 0.0503(9) H3C H Uani 0.5368(2) 0.4980(4) 0.2028(3) 1.000 0.0505(9) H4A H Uani 0.4423(3) 0.1822(4) 0.2550(3) 1.000 0.0565(10) H4B H Uani 0.5204(2) 0.1970(4) 0.1419(3) 1.000 0.0525(10) H4C H Uani 0.3882(3) 0.1119(3) 0.1353(3) 1.000 0.0527(10) H5A H Uani 0.2397(4) 0.2307(4) -0.2729(3) 1.000 0.0637(13) H5B H Uani 0.3112(4) 0.3833(5) -0.2581(3) 1.000 0.0775(15) H5C H Uani 0.1704(3) 0.3707(5) -0.2263(3) 1.000 0.0739(13) H6A H Uani 0.1737(3) 0.0630(3) -0.0990(3) 1.000 0.0516(9) H6B H Uani 0.1064(2) 0.1968(3) -0.0367(3) 1.000 0.0533(9) H6C H Uani 0.2100(3) 0.0990(3) 0.0344(3) 1.000 0.0522(10) H7A H Uani 0.4025(3) 0.0622(3) -0.1507(3) 1.000 0.0603(12) H7B H Uani 0.4751(3) 0.1179(4) -0.0345(3) 1.000 0.0558(10) H7C H Uani 0.4947(3) 0.1990(3) -0.1546(3) 1.000 0.0512(9) H12 H Uani 0.1145(2) 0.4338(2) -0.0680(3) 1.000 0.0397(7) H13 H Uani 0.00191(18) 0.6446(3) -0.0801(3) 1.000 0.0434(8) H14 H Uani 0.0973(2) 0.8657(2) -0.0267(2) 1.000 0.0384(7) H15 H Uani 0.3045(2) 0.8593(2) 0.0311(2) 1.000 0.0361(6) 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 0.0125(5) 0.0183(6) 0.0131(6) 0.0031(5) -0.0006(4) 0.0005(5) Si2 0.0120(5) 0.0159(6) 0.0170(7) -0.0030(5) 0.0004(5) -0.0001(4) N 0.0122(2) 0.0143(2) 0.0164(3) -0.0012(2) -0.0010(2) 0.0007(2) C1 0.0110(3) 0.0133(3) 0.0124(4) 0.0000(3) 0.0000(3) 0.0003(3) C2 0.0193(4) 0.0456(7) 0.0195(5) 0.0068(5) 0.0061(3) 0.0012(5) C3 0.0313(5) 0.0282(5) 0.0167(5) -0.0008(4) -0.0056(4) -0.0064(4) C4 0.0280(5) 0.0228(5) 0.0293(6) 0.0087(4) -0.0059(4) 0.0054(4) C5 0.0241(5) 0.0372(6) 0.0177(5) -0.0036(4) -0.0046(4) -0.0036(4) C6 0.0193(4) 0.0180(4) 0.0354(6) -0.0034(4) 0.0028(4) -0.0054(4) C7 0.0175(4) 0.0222(4) 0.0362(6) -0.0105(4) 0.0019(4) 0.0035(4) C11 0.0099(3) 0.0136(3) 0.0131(4) 0.0003(3) -0.0001(3) 0.0001(3) C12 0.0105(3) 0.0159(4) 0.0260(5) 0.0010(3) -0.0022(3) 0.0001(3) C13 0.0112(3) 0.0180(4) 0.0322(5) 0.0030(4) -0.0019(3) 0.0022(3) C14 0.0148(4) 0.0165(4) 0.0259(5) 0.0029(3) 0.0018(3) 0.0039(3) C15 0.0150(3) 0.0143(4) 0.0197(4) -0.0014(3) 0.0004(3) 0.0010(3) Li 0.0118(12) 0.0314(17) 0.0223(17) -0.0015(14) 0.0008(11) 0.0015(12) H2A 0.0516(17) 0.127(4) 0.0268(14) 0.0164(18) 0.0074(12) -0.003(2) H2B 0.0362(13) 0.0625(19) 0.0609(19) 0.0027(15) 0.0080(12) -0.0127(13) H2C 0.0428(15) 0.062(2) 0.068(2) -0.0005(16) 0.0169(14) 0.0166(14) H3A 0.073(2) 0.0625(19) 0.0243(13) 0.0061(12) -0.0119(12) -0.0129(16) H3B 0.074(2) 0.0341(13) 0.0421(15) -0.0086(11) -0.0010(13) -0.0002(13) H3C 0.0342(12) 0.0664(19) 0.0501(16) 0.0010(14) -0.0039(11) -0.0158(13) H4A 0.076(2) 0.0534(18) 0.0385(16) 0.0180(13) -0.0106(14) 0.0100(15) H4B 0.0352(13) 0.0541(17) 0.068(2) 0.0066(15) 0.0003(12) 0.0157(12) H4C 0.0632(18) 0.0270(12) 0.0660(19) 0.0009(12) -0.0129(15) 0.0005(12) H5A 0.090(3) 0.061(2) 0.0388(17) -0.0213(15) -0.0057(16) -0.0057(19) H5B 0.082(3) 0.104(3) 0.0441(17) 0.0275(19) -0.0153(17) -0.051(2) H5C 0.064(2) 0.113(3) 0.0427(17) -0.0005(19) -0.0134(15) 0.042(2) H6A 0.0567(17) 0.0389(14) 0.0595(18) -0.0201(13) 0.0048(14) -0.0176(12) H6B 0.0282(11) 0.0421(14) 0.091(2) 0.0021(15) 0.0149(13) 0.0008(10) H6C 0.0570(17) 0.0482(16) 0.0509(17) 0.0126(13) 0.0000(13) -0.0135(13) H7A 0.0445(15) 0.0421(15) 0.094(3) -0.0399(16) 0.0023(16) -0.0006(12) H7B 0.0512(16) 0.0612(19) 0.0541(17) 0.0014(15) -0.0054(13) 0.0275(14) H7C 0.0389(13) 0.0488(15) 0.068(2) -0.0085(14) 0.0211(13) 0.0023(12) H12 0.0240(9) 0.0246(10) 0.0692(18) -0.0038(10) -0.0082(10) -0.0042(8) H13 0.0188(9) 0.0395(12) 0.0704(18) 0.0031(12) -0.0089(10) 0.0035(9) H14 0.0327(10) 0.0255(10) 0.0569(15) 0.0030(10) 0.0024(10) 0.0119(8) H15 0.0316(10) 0.0223(9) 0.0536(14) -0.0065(9) -0.0049(9) -0.0026(8) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Si1 C1 1.8557(17) . . yes Si1 C2 1.8818(17) . . yes Si1 C3 1.8982(18) . . yes Si1 C4 1.8783(19) . . yes Si2 C1 1.8567(17) . . yes Si2 C5 1.8816(19) . . yes Si2 C6 1.8918(18) . . yes Si2 C7 1.8980(17) . . yes Si2 Li 2.856(4) . . yes N C11 1.3639(11) . . yes N C15 1.3460(12) . . yes N Li 1.955(4) . 3_665 yes C1 C11 1.4841(12) . . no C1 Li 2.202(4) . . yes C11 C12 1.4165(12) . . no C12 C13 1.3857(14) . . no C13 C14 1.3970(14) . . no C14 C15 1.3854(13) . . no C2 H2A 1.084(3) . . no C2 H2B 1.088(4) . . no C2 H2C 1.079(4) . . no C3 H3A 1.090(3) . . no C3 H3B 1.086(3) . . no C3 H3C 1.100(3) . . no C4 H4A 1.098(4) . . no C4 H4B 1.091(3) . . no C4 H4C 1.088(3) . . no C5 H5A 1.081(4) . . no C5 H5B 1.065(5) . . no C5 H5C 1.083(4) . . no C6 H6A 1.093(4) . . no C6 H6B 1.087(3) . . no C6 H6C 1.092(4) . . no C7 H7A 1.085(3) . . no C7 H7B 1.081(4) . . no C7 H7C 1.097(4) . . no C12 H12 1.083(2) . . no C13 H13 1.091(2) . . no C14 H14 1.084(2) . . no C15 H15 1.085(2) . . no 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 C1 Si1 C2 112.29(8) . . . yes C1 Si1 C3 113.37(9) . . . yes C1 Si1 C4 113.31(9) . . . yes C2 Si1 C3 104.94(9) . . . yes C2 Si1 C4 107.77(9) . . . yes C3 Si1 C4 104.48(8) . . . yes C1 Si2 C5 112.83(9) . . . yes C1 Si2 C6 117.44(9) . . . yes C1 Si2 C7 110.02(8) . . . yes C1 Si2 Li 50.45(9) . . . yes C5 Si2 C6 105.45(8) . . . yes C5 Si2 C7 104.53(9) . . . yes C5 Si2 Li 103.67(10) . . . yes C6 Si2 C7 105.56(9) . . . yes C6 Si2 Li 150.82(11) . . . yes C7 Si2 Li 64.76(9) . . . yes C11 N C15 120.42(7) . . . yes C11 N Li 104.08(13) . . 3_665 yes C15 N Li 135.50(13) . . 3_665 yes Si1 C1 Si2 114.48(8) . . . yes Si1 C1 C11 108.83(7) . . . yes Si1 C1 Li 104.53(11) . . . yes Si2 C1 C11 115.42(7) . . . yes Si2 C1 Li 89.01(11) . . . yes C11 C1 Li 123.37(12) . . . yes N C11 C1 117.57(7) . . . yes N C11 C12 118.14(8) . . . yes C1 C11 C12 124.25(8) . . . no C11 C12 C13 120.98(9) . . . no C12 C13 C14 119.57(8) . . . no C13 C14 C15 117.23(9) . . . no N C15 C14 123.64(9) . . . yes H2A C2 H2C 108.6(3) . . . no H2B C2 H2C 107.1(3) . . . no Si1 C2 H2C 111.8(2) . . . no Si1 C2 H2A 111.0(2) . . . no Si1 C2 H2B 111.0(2) . . . no H2A C2 H2B 107.1(3) . . . no Si1 C3 H3A 108.9(2) . . . no H3B C3 H3C 108.7(3) . . . no Si1 C3 H3C 112.9(2) . . . no H3A C3 H3B 106.5(3) . . . no Si1 C3 H3B 113.52(19) . . . no H3A C3 H3C 105.8(3) . . . no Si1 C4 H4B 112.4(2) . . . no Si1 C4 H4C 113.3(2) . . . no Si1 C4 H4A 108.7(2) . . . no H4A C4 H4B 107.1(3) . . . no H4A C4 H4C 107.2(3) . . . no H4B C4 H4C 107.7(3) . . . no Si2 C5 H5B 112.8(2) . . . no Si2 C5 H5C 113.8(2) . . . no H5A C5 H5B 107.2(3) . . . no Si2 C5 H5A 109.7(2) . . . no H5A C5 H5C 105.8(4) . . . no H5B C5 H5C 107.1(4) . . . no Si2 C6 H6A 109.7(2) . . . no H6A C6 H6C 107.7(3) . . . no H6B C6 H6C 107.7(3) . . . no H6A C6 H6B 107.0(3) . . . no Si2 C6 H6B 111.77(18) . . . no Si2 C6 H6C 112.8(2) . . . no Si2 C7 H7A 108.6(2) . . . no H7B C7 H7C 107.3(3) . . . no Si2 C7 H7C 113.62(19) . . . no H7A C7 H7B 107.9(3) . . . no Si2 C7 H7B 113.8(2) . . . no H7A C7 H7C 105.0(3) . . . no C11 C12 H12 119.29(15) . . . no C13 C12 H12 119.69(15) . . . no C12 C13 H13 119.70(18) . . . no C14 C13 H13 120.73(18) . . . no C13 C14 H14 121.79(15) . . . no C15 C14 H14 120.96(15) . . . no N C15 H15 115.74(14) . . . no C14 C15 H15 120.61(15) . . . no N Li C1 145.9(2) 3_665 . . yes Si2 Li N 139.77(19) . . 3_665 yes Si2 Li C1 40.55(7) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Si1 C1 Si2 -80.14(11) . . . . no C3 Si1 C1 Si2 161.13(8) . . . . no C4 Si1 C1 Si2 42.26(11) . . . . no C2 Si1 C1 C11 50.68(11) . . . . no C3 Si1 C1 C11 -68.06(10) . . . . no C4 Si1 C1 C11 173.07(8) . . . . no C2 Si1 C1 Li -175.78(13) . . . . no C3 Si1 C1 Li 65.48(14) . . . . no C4 Si1 C1 Li -53.39(14) . . . . no C5 Si2 C1 Si1 165.33(8) . . . . no C6 Si2 C1 Si1 42.36(11) . . . . no C7 Si2 C1 Si1 -78.37(10) . . . . no Li Si2 C1 Si1 -105.54(12) . . . . no C5 Si2 C1 C11 37.80(11) . . . . no C6 Si2 C1 C11 -85.17(11) . . . . no C7 Si2 C1 C11 154.10(8) . . . . no Li Si2 C1 C11 126.93(13) . . . . no C5 Si2 C1 Li -89.13(13) . . . . no C6 Si2 C1 Li 147.90(13) . . . . no C7 Si2 C1 Li 27.17(13) . . . . no C6 Si2 Li N 50.9(4) . . . 3_665 no C7 Si2 Li N -25.5(2) . . . 3_665 no C5 Si2 Li C1 108.48(11) . . . . no C6 Si2 Li C1 -75.3(2) . . . . no C7 Si2 Li C1 -151.69(13) . . . . no C1 Si2 Li N 126.2(3) . . . 3_665 no C5 Si2 Li N -125.3(3) . . . 3_665 no C11 N Li C1 -95.1(4) 3_665 3_665 . . no C15 N Li C1 84.4(4) 3_665 3_665 . . no Li N C11 C12 -178.49(13) 3_665 . . . no Li N C15 C14 179.50(17) 3_665 . . . no C11 N Li Si2 -164.4(2) 3_665 3_665 . . no C11 N C15 C14 0.05(15) . . . . no Li N C11 C1 3.96(14) 3_665 . . . no C15 N C11 C12 1.10(12) . . . . no C15 N C11 C1 -176.45(8) . . . . no C15 N Li Si2 15.1(4) 3_665 3_665 . . no C11 N C15 H15 -179.84(18) . . . . no Li N C15 H15 -0.4(3) 3_665 . . . no C11 C1 Li Si2 -120.17(12) . . . . no Si1 C1 Li N 3.5(4) . . . 3_665 no Si2 C1 Li N -111.6(4) . . . 3_665 no Li C1 C11 N -47.07(16) . . . . no Si2 C1 C11 N -153.93(8) . . . . no Si2 C1 C11 C12 28.68(13) . . . . no Si1 C1 C11 C12 -101.62(10) . . . . no Li C1 C11 C12 135.54(14) . . . . no Si1 C1 Li Si2 115.07(9) . . . . no C11 C1 Li N 128.2(3) . . . 3_665 no Si1 C1 C11 N 75.76(9) . . . . no C1 C11 C12 C13 176.31(9) . . . . no N C11 C12 C13 -1.06(14) . . . . no C11 C12 C13 C14 -0.13(16) . . . . no C12 C13 C14 C15 1.25(15) . . . . no C13 C14 C15 N -1.26(15) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Si1 Li 3.041(4) . 3_665 no Si2 Li 4.311(4) . 3_665 no Si1 H6C 3.398(4) . . no Si2 H4C 3.301(4) . . no Si2 H12 2.793(3) . . no Si2 H3C 3.412(4) . 3_665 no N C3 3.3691(14) . . no N H3B 2.840(3) . . no C3 N 3.3691(14) . . no C3 Li 2.508(4) . 3_665 no C4 C7 3.5547(18) . . no C5 C12 3.2984(16) . . no C5 C14 3.5610(16) . 2_544 no C7 C4 3.5547(18) . . no C12 C5 3.2984(16) . . no C14 C5 3.5610(16) . 2_554 no C2 H13 2.940(3) . 3_565 no C3 H5B 3.090(5) . 3_665 no C4 H5C 3.073(4) . 4_555 no C4 H7B 2.792(4) . . no C5 H12 2.857(3) . . no C5 H3C 3.067(3) . 3_665 no C6 H2B 3.017(4) . . no C6 H12 2.987(2) . . no C6 H14 2.963(2) . 1_545 no C11 H2C 3.060(4) . . no C12 H5C 2.775(4) . . no C12 H13 3.064(3) . 3_565 no C13 H12 3.059(3) . 3_565 no C13 H6B 3.064(3) . 3_565 no C14 H6A 3.067(3) . 1_565 no C14 H5A 3.033(4) . 2_554 no C14 H5B 3.075(4) . 2_554 no C14 H6B 3.094(3) . 3_565 no C15 H2A 2.684(3) . 2_555 no C15 H5A 3.028(4) . 2_554 no Li Si2 4.311(4) . 3_665 no Li C3 2.508(4) . 3_665 no Li Si1 3.041(4) . 3_665 no Li Li 2.558(6) . 3_665 no Li H3C 3.414(5) . . no Li H4B 3.146(5) . . no Li H3B 2.341(5) . 3_665 no Li H3C 2.257(5) . 3_665 no H2A C15 2.684(3) . 2_545 no H2A H15 2.384(4) . 2_545 no H2B C6 3.017(4) . . no H2B H6C 2.543(5) . . no H2B H3B 2.495(5) . 2_545 no H2B H13 2.312(5) . 3_565 no H2C C11 3.060(4) . . no H3B N 2.840(3) . . no H3B H2B 2.495(5) . 2_555 no H3B Li 2.341(5) . 3_665 no H3B H7C 2.489(4) . 3_665 no H3C Li 3.414(5) . . no H3C Si2 3.412(4) . 3_665 no H3C C5 3.067(3) . 3_665 no H3C Li 2.257(5) . 3_665 no H3C H5B 2.211(6) . 3_665 no H4B Li 3.146(5) . . no H4B H7B 2.409(5) . . no H4B H5C 2.450(5) . 4_555 no H4C Si2 3.301(4) . . no H4C H6C 2.389(5) . . no H4C H7B 2.449(5) . . no H5A C14 3.033(4) . 2_544 no H5A C15 3.028(4) . 2_544 no H5B C14 3.075(4) . 2_544 no H5B H6A 2.556(6) . 2_554 no H5B C3 3.090(5) . 3_665 no H5B H3C 2.211(6) . 3_665 no H5C C12 2.775(4) . . no H5C H12 2.248(5) . . no H5C H7A 2.568(6) . 2_554 no H5C C4 3.073(4) . 4_454 no H5C H4B 2.450(5) . 4_454 no H6A C14 3.067(3) . 1_545 no H6A H14 2.354(4) . 1_545 no H6A H5B 2.556(6) . 2_544 no H6B H12 2.374(4) . . no H6B C13 3.064(3) . 3_565 no H6B C14 3.094(3) . 3_565 no H6B H13 2.551(4) . 3_565 no H6C Si1 3.398(4) . . no H6C H2B 2.543(5) . . no H6C H4C 2.389(5) . . no H7A H5C 2.568(6) . 2_544 no H7B C4 2.792(4) . . no H7B H4B 2.409(5) . . no H7B H4C 2.449(5) . . no H7B H7B 2.542(6) . 3_655 no H7B H15 2.591(4) . 3_665 no H7C H3B 2.489(4) . 3_665 no H12 Si2 2.793(3) . . no H12 C5 2.857(3) . . no H12 C6 2.987(2) . . no H12 H5C 2.248(5) . . no H12 H6B 2.374(4) . . no H12 C13 3.059(3) . 3_565 no H12 H13 2.518(5) . 3_565 no H13 C2 2.940(3) . 3_565 no H13 C12 3.064(3) . 3_565 no H13 H2B 2.312(5) . 3_565 no H13 H6B 2.551(4) . 3_565 no H13 H12 2.518(5) . 3_565 no H14 C6 2.963(2) . 1_565 no H14 H6A 2.354(4) . 1_565 no H15 H2A 2.384(4) . 2_555 no H15 H7B 2.591(4) . 3_665 no # End of Crystallographic Information File # CIF-file generated for li_n_20 / compound 1 /20 K neutron measurement #============================================================================== data_li_n_20 # compound 1 / 20 K neutron measurement _database_code_CSD 169892 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 Li2 N2 Si4' _chemical_formula_structural ? # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_sum 'C24 H44 Li2 N2 Si4' _chemical_formula_weight 486.85 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_length_neutron _atom_type_scat_source Si Si 4.1491 'Sears, V. F. (1992) Neutron News 3, 26-37.' N N 9.36 'Sears, V. F. (1992) Neutron News 3, 26-37.' Li Li -1.90 'Sears, V. F. (1992) Neutron News 3, 26-37.' H H -3.7390 'Sears, V. F. (1992) Neutron News 3, 26-37.' C C 6.6460 'Sears, V. F. (1992) Neutron News 3, 26-37.' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' 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 11.6982(5) _cell_length_b 9.8218(5) _cell_length_c 12.6895(6) _cell_angle_alpha 90 _cell_angle_beta 93.5114(19) _cell_angle_gamma 90 _cell_volume 1455.25(12) _cell_formula_units_Z 2 _cell_measurement_temperature 20(1) _cell_measurement_reflns_used 4077 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 33.78 _cell_special_details ; ? ; _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 4.5 _exptl_crystal_size_mid 2.2 _exptl_crystal_size_min 1.7 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.231 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # cylinder 'cylindrical' # empirical 'empirical from intensities' # gaussian 'Gaussian from crystal shape' # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # refdelf 'refined from delta-F' # sphere 'spherical' _exptl_absorpt_correction_type none # Example: '(North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.694 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; _diffrn_ambient_temperature 20(1) _diffrn_radiation_wavelength 0.95070 _diffrn_radiation_type neutron _diffrn_radiation_monochromator 'Cu 220' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_details ; thermal neutron four-circle diffractometer D19 at the ILL (Grenoble, France) ; _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 9 0 3 -1 8 2 -2 0 8 # number of measured reflections (redundant set) _diffrn_reflns_number 4077 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 33.78 _diffrn_reflns_theta_full 33.78 _diffrn_measured_fraction_theta_max 0.83 _diffrn_measured_fraction_theta_full 0.83 _diffrn_reflns_reduction_process ; ? ; # number of unique reflections _reflns_number_total 2161 # number of observed reflections (> n sig(I)) _reflns_number_gt 1844 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'MAD, HKLGEN (ILL)' _computing_cell_refinement 'RAFD19 (ILL)' _computing_data_reduction 'RETREAT (ILL)' _computing_structure_solution 'SIR-92 (C. Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2 for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2, conventional R-factors R are based on F, with F set to zero for negative F^2. The observed criterion of F^2 > 2sigma(F^2) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2 are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. Density synthesis with coefficients Fo-Fc Highest peak 0.40 at 0.0434 0.0170 0.4231 [ 0.98 A from LI ] Deepest hole -0.38 at 0.1651 0.0371 0.5636 [ 1.00 A from C11 ] All hydrogen atoms could be located with difference Fourier maps and were refined anisotropically. Unit cell contains no residual solvent accessible area. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+1.3674P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method shelxl _refine_ls_extinction_coef 0.0203(7) _refine_ls_extinction_expression 'FC^*^=KFC[1+0.001XFC^2^\L^3^/SIN(2\Q)]^-1/4^' _refine_ls_abs_structure_details none _refine_ls_number_reflns 2161 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.403 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.096 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Si1 Si Uani 0.35926(15) 0.36443(19) 0.14273(14) 1.000 0.0049(5) Si2 Si Uani 0.30227(15) 0.26266(19) -0.08745(14) 1.000 0.0054(5) N N Uani 0.32122(7) 0.65396(9) 0.01344(6) 1.000 0.0063(2) C1 C Uani 0.34450(10) 0.40827(12) 0.00011(9) 1.000 0.0053(3) C2 C Uani 0.21661(11) 0.35694(14) 0.20372(10) 1.000 0.0097(4) C3 C Uani 0.44635(11) 0.49360(14) 0.22454(10) 1.000 0.0100(4) C4 C Uani 0.43409(11) 0.19746(13) 0.17012(11) 1.000 0.0098(4) C5 C Uani 0.25123(11) 0.31810(14) -0.22433(10) 1.000 0.0102(4) C6 C Uani 0.18755(10) 0.14406(13) -0.04250(10) 1.000 0.0086(4) C7 C Uani 0.43153(11) 0.15108(14) -0.10778(11) 1.000 0.0098(4) C11 C Uani 0.27203(10) 0.53179(12) -0.01337(9) 1.000 0.0046(3) C12 C Uani 0.15487(10) 0.53024(13) -0.04835(9) 1.000 0.0068(4) C13 C Uani 0.09083(10) 0.64931(13) -0.05307(9) 1.000 0.0082(4) C14 C Uani 0.14303(10) 0.77224(13) -0.02320(10) 1.000 0.0076(4) C15 C Uani 0.25822(10) 0.76880(13) 0.00838(9) 1.000 0.0064(4) Li Li Uani 0.5193(4) 0.3925(5) -0.0535(3) 1.000 0.0113(12) H2A H Uani 0.2276(3) 0.3342(4) 0.2874(2) 1.000 0.0372(10) H2B H Uani 0.1634(2) 0.2774(3) 0.1672(3) 1.000 0.0323(9) H2C H Uani 0.1707(3) 0.4535(3) 0.1949(3) 1.000 0.0348(10) H3A H Uani 0.4487(3) 0.4632(3) 0.3080(2) 1.000 0.0328(10) H3B H Uani 0.4100(3) 0.5952(3) 0.2209(2) 1.000 0.0296(9) H3C H Uani 0.5358(3) 0.4982(3) 0.2035(2) 1.000 0.0319(10) H4A H Uani 0.4422(3) 0.1814(3) 0.2550(2) 1.000 0.0329(10) H4B H Uani 0.5206(2) 0.1970(3) 0.1419(2) 1.000 0.0313(10) H4C H Uani 0.3882(3) 0.1100(3) 0.1355(3) 1.000 0.0312(9) H5A H Uani 0.2399(3) 0.2290(3) -0.2748(2) 1.000 0.0349(10) H5B H Uani 0.3128(3) 0.3820(4) -0.2606(3) 1.000 0.0405(10) H5C H Uani 0.1712(3) 0.3722(4) -0.2273(2) 1.000 0.0407(11) H6A H Uani 0.1735(3) 0.0620(3) -0.0997(3) 1.000 0.0321(9) H6B H Uani 0.1060(3) 0.1966(3) -0.0371(3) 1.000 0.0329(10) H6C H Uani 0.2096(3) 0.0981(3) 0.0346(2) 1.000 0.0318(9) H7A H Uani 0.4026(3) 0.0606(3) -0.1513(3) 1.000 0.0355(10) H7B H Uani 0.4757(3) 0.1167(3) -0.0348(3) 1.000 0.0352(10) H7C H Uani 0.4945(3) 0.1978(3) -0.1559(3) 1.000 0.0326(9) H12 H Uani 0.1137(2) 0.4341(3) -0.0687(2) 1.000 0.0217(8) H13 H Uani 0.0010(2) 0.6457(3) -0.0800(2) 1.000 0.0257(9) H14 H Uani 0.0962(2) 0.8680(3) -0.0260(2) 1.000 0.0230(8) H15 H Uani 0.3042(2) 0.8619(3) 0.0302(2) 1.000 0.0223(8) 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 0.0074(9) 0.0038(9) 0.0036(9) 0.0017(7) 0.0012(7) -0.0015(7) Si2 0.0071(9) 0.0036(9) 0.0054(9) 0.0005(7) -0.0004(7) -0.0015(7) N 0.0070(4) 0.0038(4) 0.0079(4) -0.0004(3) -0.0001(3) 0.0004(3) C1 0.0065(5) 0.0040(6) 0.0052(6) 0.0006(4) -0.0002(4) 0.0010(4) C2 0.0085(6) 0.0134(8) 0.0076(8) 0.0024(6) 0.0026(5) 0.0001(6) C3 0.0140(8) 0.0096(8) 0.0062(7) -0.0004(5) -0.0013(5) -0.0031(6) C4 0.0124(7) 0.0063(7) 0.0106(8) 0.0016(5) -0.0008(5) 0.0015(6) C5 0.0130(7) 0.0121(7) 0.0052(6) 0.0004(6) -0.0015(5) -0.0015(7) C6 0.0093(7) 0.0058(6) 0.0109(7) -0.0008(6) 0.0021(5) -0.0025(5) C7 0.0093(6) 0.0082(7) 0.0122(7) -0.0026(6) 0.0028(6) 0.0025(5) C11 0.0059(6) 0.0033(6) 0.0047(6) -0.0001(5) 0.0002(4) 0.0004(5) C12 0.0052(6) 0.0044(7) 0.0106(6) 0.0007(5) -0.0003(4) -0.0001(5) C13 0.0078(7) 0.0057(6) 0.0109(6) 0.0001(5) -0.0005(5) 0.0015(5) C14 0.0073(6) 0.0050(7) 0.0106(6) 0.0003(5) 0.0012(5) 0.0008(5) C15 0.0071(6) 0.0039(7) 0.0082(6) 0.0007(5) 0.0005(4) 0.0005(5) Li 0.010(2) 0.011(2) 0.013(2) -0.0017(19) 0.0009(17) -0.0005(18) H2A 0.0353(16) 0.065(2) 0.0118(16) 0.0082(14) 0.0054(11) -0.0014(15) H2B 0.0248(14) 0.0324(17) 0.0396(17) -0.0057(14) 0.0011(13) -0.0102(14) H2C 0.0317(16) 0.0257(17) 0.0482(19) 0.0025(14) 0.0128(13) 0.0103(14) H3A 0.0478(18) 0.0362(17) 0.0138(16) 0.0051(13) -0.0023(12) -0.0087(14) H3B 0.0381(16) 0.0179(16) 0.0323(16) -0.0035(12) -0.0012(12) 0.0042(13) H3C 0.0213(17) 0.0388(18) 0.0353(17) -0.0011(14) 0.0005(13) -0.0071(13) H4A 0.0465(18) 0.0321(16) 0.0198(18) 0.0067(13) -0.0010(12) 0.0071(14) H4B 0.0235(16) 0.0331(17) 0.0380(17) 0.0028(13) 0.0085(13) 0.0056(12) H4C 0.0361(16) 0.0150(14) 0.0414(17) -0.0031(13) -0.0066(13) -0.0066(13) H5A 0.055(2) 0.0270(18) 0.0219(16) -0.0096(14) -0.0050(14) -0.0010(14) H5B 0.0421(18) 0.051(2) 0.0279(16) 0.0169(16) -0.0021(14) -0.0234(17) H5C 0.0379(19) 0.059(2) 0.0247(16) 0.0015(15) -0.0026(13) 0.0249(18) H6A 0.0401(17) 0.0229(16) 0.0336(16) -0.0121(15) 0.0052(13) -0.0097(13) H6B 0.0204(15) 0.0273(15) 0.052(2) 0.0046(14) 0.0112(13) 0.0057(13) H6C 0.0379(16) 0.0341(16) 0.0231(17) 0.0136(14) -0.0006(12) -0.0047(13) H7A 0.0346(16) 0.0231(16) 0.0485(19) -0.0194(15) 0.0009(14) -0.0007(13) H7B 0.0379(16) 0.0404(18) 0.0264(17) 0.0023(14) -0.0043(14) 0.0174(14) H7C 0.0291(15) 0.0306(16) 0.0403(18) 0.0020(14) 0.0192(15) 0.0003(14) H12 0.0196(12) 0.0104(14) 0.0348(15) -0.0041(11) -0.0014(11) -0.0033(11) H13 0.0160(15) 0.0232(14) 0.0370(16) -0.0031(12) -0.0051(12) 0.0016(11) H14 0.0218(13) 0.0119(14) 0.0353(15) 0.0007(11) 0.0010(11) 0.0062(12) H15 0.0226(13) 0.0122(14) 0.0317(15) -0.0053(11) -0.0005(11) -0.0025(12) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Si1 C1 1.858(2) . . yes Si1 C2 1.883(2) . . yes Si1 C3 1.896(2) . . yes Si1 C4 1.881(2) . . yes Si2 C1 1.859(2) . . yes Si2 C5 1.882(2) . . yes Si2 C6 1.891(2) . . yes Si2 C7 1.898(2) . . yes Si2 Li 2.850(5) . . yes N C11 1.3648(15) . . yes N C15 1.3467(15) . . yes N Li 1.957(5) . 3_665 yes C1 C11 1.4839(17) . . no C1 Li 2.200(5) . . yes C11 C12 1.4146(17) . . no C12 C13 1.3882(18) . . no C13 C14 1.3950(18) . . no C14 C15 1.3825(17) . . no C2 H2A 1.085(3) . . no C2 H2B 1.085(3) . . no C2 H2C 1.092(3) . . no C3 H3A 1.099(3) . . no C3 H3B 1.085(3) . . no C3 H3C 1.097(4) . . no C4 H4A 1.087(3) . . no C4 H4B 1.094(3) . . no C4 H4C 1.091(3) . . no C5 H5A 1.088(3) . . no C5 H5B 1.079(4) . . no C5 H5C 1.075(4) . . no C6 H6A 1.090(4) . . no C6 H6B 1.090(4) . . no C6 H6C 1.094(3) . . no C7 H7A 1.089(4) . . no C7 H7B 1.086(4) . . no C7 H7C 1.087(4) . . no C12 H12 1.084(3) . . no C13 H13 1.086(3) . . no C14 H14 1.088(3) . . no C15 H15 1.088(3) . . no 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 C1 Si1 C2 112.18(10) . . . yes C1 Si1 C3 113.14(11) . . . yes C1 Si1 C4 113.35(11) . . . yes C2 Si1 C3 105.13(10) . . . yes C2 Si1 C4 107.70(11) . . . yes C3 Si1 C4 104.70(10) . . . yes C1 Si2 C5 112.74(11) . . . yes C1 Si2 C6 117.45(11) . . . yes C1 Si2 C7 109.92(10) . . . yes C1 Si2 Li 50.50(10) . . . yes C5 Si2 C6 105.40(10) . . . yes C5 Si2 C7 104.59(10) . . . yes C5 Si2 Li 103.85(12) . . . yes C6 Si2 C7 105.74(11) . . . yes C6 Si2 Li 150.68(13) . . . yes C7 Si2 Li 64.48(12) . . . yes C11 N C15 120.22(9) . . . yes C11 N Li 103.91(16) . . 3_665 yes C15 N Li 135.87(16) . . 3_665 yes Si1 C1 Si2 114.16(10) . . . yes Si1 C1 C11 108.67(10) . . . yes Si1 C1 Li 104.61(13) . . . yes Si2 C1 C11 115.53(10) . . . yes Si2 C1 Li 88.80(14) . . . yes C11 C1 Li 123.87(15) . . . yes N C11 C1 117.44(10) . . . yes N C11 C12 118.25(10) . . . yes C1 C11 C12 124.27(11) . . . no C11 C12 C13 120.96(11) . . . no C12 C13 C14 119.43(11) . . . no C13 C14 C15 117.40(11) . . . no N C15 C14 123.72(11) . . . yes H2A C2 H2C 107.9(3) . . . no H2B C2 H2C 108.4(3) . . . no Si1 C2 H2C 111.5(2) . . . no Si1 C2 H2A 110.8(2) . . . no Si1 C2 H2B 110.62(19) . . . no H2A C2 H2B 107.5(3) . . . no Si1 C3 H3A 109.07(19) . . . no H3B C3 H3C 109.2(3) . . . no Si1 C3 H3C 112.52(18) . . . no H3A C3 H3B 106.1(2) . . . no Si1 C3 H3B 113.3(2) . . . no H3A C3 H3C 106.1(3) . . . no Si1 C4 H4B 111.87(18) . . . no Si1 C4 H4C 113.6(2) . . . no Si1 C4 H4A 108.72(19) . . . no H4A C4 H4B 107.3(3) . . . no H4A C4 H4C 107.2(3) . . . no H4B C4 H4C 107.9(3) . . . no Si2 C5 H5B 112.3(2) . . . no Si2 C5 H5C 113.68(17) . . . no H5A C5 H5B 106.1(3) . . . no Si2 C5 H5A 109.32(18) . . . no H5A C5 H5C 107.6(3) . . . no H5B C5 H5C 107.5(3) . . . no Si2 C6 H6A 109.6(2) . . . no H6A C6 H6C 107.9(3) . . . no H6B C6 H6C 107.4(3) . . . no H6A C6 H6B 107.1(3) . . . no Si2 C6 H6B 111.5(2) . . . no Si2 C6 H6C 113.0(2) . . . no Si2 C7 H7A 108.3(2) . . . no H7B C7 H7C 107.9(3) . . . no Si2 C7 H7C 113.9(2) . . . no H7A C7 H7B 107.2(3) . . . no Si2 C7 H7B 113.9(2) . . . no H7A C7 H7C 105.1(3) . . . no C11 C12 H12 119.47(17) . . . no C13 C12 H12 119.53(17) . . . no C12 C13 H13 119.71(19) . . . no C14 C13 H13 120.87(19) . . . no C13 C14 H14 121.88(17) . . . no C15 C14 H14 120.70(18) . . . no N C15 H15 115.54(17) . . . no C14 C15 H15 120.74(18) . . . no N Li C1 145.6(2) 3_665 . . yes Si2 Li N 139.6(2) . . 3_665 yes Si2 Li C1 40.70(9) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Si1 C1 Si2 -79.87(13) . . . . no C3 Si1 C1 Si2 161.40(10) . . . . no C4 Si1 C1 Si2 42.38(14) . . . . no C2 Si1 C1 C11 50.69(14) . . . . no C3 Si1 C1 C11 -68.05(13) . . . . no C4 Si1 C1 C11 172.93(10) . . . . no C2 Si1 C1 Li -175.21(16) . . . . no C3 Si1 C1 Li 66.05(17) . . . . no C4 Si1 C1 Li -52.97(17) . . . . no C5 Si2 C1 Si1 165.04(10) . . . . no C6 Si2 C1 Si1 42.20(15) . . . . no C7 Si2 C1 Si1 -78.70(13) . . . . no Li Si2 C1 Si1 -105.49(15) . . . . no C5 Si2 C1 C11 37.95(14) . . . . no C6 Si2 C1 C11 -84.89(14) . . . . no C7 Si2 C1 C11 154.22(10) . . . . no Li Si2 C1 C11 127.42(15) . . . . no C5 Si2 C1 Li -89.47(15) . . . . no C6 Si2 C1 Li 147.69(15) . . . . no C7 Si2 C1 Li 26.79(15) . . . . no C6 Si2 Li N 50.3(5) . . . 3_665 no C7 Si2 Li N -26.0(3) . . . 3_665 no C5 Si2 Li C1 108.23(13) . . . . no C6 Si2 Li C1 -75.6(3) . . . . no C7 Si2 Li C1 -151.99(15) . . . . no C1 Si2 Li N 126.0(3) . . . 3_665 no C5 Si2 Li N -125.8(3) . . . 3_665 no C11 N Li C1 -95.1(4) 3_665 3_665 . . no C15 N Li C1 85.3(5) 3_665 3_665 . . no Li N C11 C12 -179.00(15) 3_665 . . . no Li N C15 C14 -179.57(19) 3_665 . . . no C11 N Li Si2 -164.3(2) 3_665 3_665 . . no C11 N C15 C14 -0.03(16) . . . . no Li N C11 C1 3.25(16) 3_665 . . . no C15 N C11 C12 1.33(15) . . . . no C15 N C11 C1 -176.42(10) . . . . no C15 N Li Si2 16.1(4) 3_665 3_665 . . no C11 N C15 H15 -179.31(17) . . . . no Li N C15 H15 1.1(3) 3_665 . . . no C11 C1 Li Si2 -120.34(14) . . . . no Si1 C1 Li N 3.1(5) . . . 3_665 no Si2 C1 Li N -111.6(4) . . . 3_665 no Li C1 C11 N -46.89(18) . . . . no Si2 C1 C11 N -153.90(10) . . . . no Si2 C1 C11 C12 28.51(16) . . . . no Si1 C1 C11 C12 -101.30(13) . . . . no Li C1 C11 C12 135.52(16) . . . . no Si1 C1 Li Si2 114.68(11) . . . . no C11 C1 Li N 128.1(4) . . . 3_665 no Si1 C1 C11 N 76.30(12) . . . . no C1 C11 C12 C13 176.15(11) . . . . no N C11 C12 C13 -1.43(17) . . . . no C11 C12 C13 C14 0.23(17) . . . . no C12 C13 C14 C15 1.04(17) . . . . no C13 C14 C15 N -1.19(18) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Si1 Li 3.033(5) . 3_665 no Si2 Li 4.309(5) . 3_665 no Si1 H6C 3.391(4) . . no Si2 H4C 3.304(4) . . no Si2 H12 2.797(3) . . no Si2 H3C 3.408(4) . 3_665 no N C3 3.3643(15) . . no N H3B 2.830(3) . . no C3 N 3.3643(15) . . no C3 Li 2.496(4) . 3_665 no C4 C7 3.554(2) . . no C5 C12 3.3026(18) . . no C5 C14 3.5330(18) . 2_544 no C7 C4 3.554(2) . . no C12 C5 3.3026(18) . . no C14 C5 3.5330(18) . 2_554 no C2 H13 2.908(3) . 3_565 no C3 H5B 3.079(4) . 3_665 no C4 H5C 3.068(4) . 4_555 no C4 H7B 2.790(4) . . no C5 H12 2.859(3) . . no C5 H3C 3.074(4) . 3_665 no C6 H2B 2.995(4) . . no C6 H12 2.989(3) . . no C6 H14 2.927(3) . 1_545 no C11 H2C 3.060(4) . . no C12 H5C 2.767(3) . . no C12 H13 3.054(3) . 3_565 no C13 H12 3.039(3) . 3_565 no C13 H6B 3.037(4) . 3_565 no C14 H6A 3.035(3) . 1_565 no C14 H5A 3.009(3) . 2_554 no C14 H5B 3.021(4) . 2_554 no C14 H6B 3.072(4) . 3_565 no C15 H2A 2.665(3) . 2_555 no C15 H5A 2.991(3) . 2_554 no Li Si2 4.309(5) . 3_665 no Li C3 2.496(4) . 3_665 no Li Si1 3.033(5) . 3_665 no Li Li 2.565(7) . 3_665 no Li H3C 3.417(5) . . no Li H4B 3.135(5) . . no Li H3B 2.329(5) . 3_665 no Li H3C 2.245(5) . 3_665 no H2A C15 2.665(3) . 2_545 no H2A H15 2.382(4) . 2_545 no H2B C6 2.995(4) . . no H2B H6C 2.517(4) . . no H2B H3B 2.471(4) . 2_545 no H2B H13 2.288(4) . 3_565 no H2C C11 3.060(4) . . no H2C H13 2.598(4) . 3_565 no H3B N 2.830(3) . . no H3B H2B 2.471(4) . 2_555 no H3B Li 2.329(5) . 3_665 no H3B H7C 2.485(4) . 3_665 no H3C Li 3.417(5) . . no H3C Si2 3.408(4) . 3_665 no H3C C5 3.074(4) . 3_665 no H3C Li 2.245(5) . 3_665 no H3C H5B 2.211(5) . 3_665 no H4B Li 3.135(5) . . no H4B H7B 2.404(5) . . no H4B H5C 2.442(4) . 4_555 no H4C Si2 3.304(4) . . no H4C H6C 2.385(5) . . no H4C H7B 2.448(5) . . no H5A C14 3.009(3) . 2_544 no H5A C15 2.991(3) . 2_544 no H5B C14 3.021(4) . 2_544 no H5B H6A 2.516(5) . 2_554 no H5B C3 3.079(4) . 3_665 no H5B H3C 2.211(5) . 3_665 no H5C C12 2.767(3) . . no H5C H12 2.245(4) . . no H5C H7A 2.526(5) . 2_554 no H5C C4 3.068(4) . 4_454 no H5C H4B 2.442(4) . 4_454 no H6A C14 3.035(3) . 1_545 no H6A H14 2.330(4) . 1_545 no H6A H5B 2.516(5) . 2_544 no H6B H12 2.370(4) . . no H6B C13 3.037(4) . 3_565 no H6B C14 3.072(4) . 3_565 no H6B H13 2.530(4) . 3_565 no H6C Si1 3.391(4) . . no H6C H2B 2.517(4) . . no H6C H4C 2.385(5) . . no H6C H15 2.572(4) . 1_545 no H7A H5C 2.526(5) . 2_544 no H7B C4 2.790(4) . . no H7B H4B 2.404(5) . . no H7B H4C 2.448(5) . . no H7B H7B 2.509(4) . 3_655 no H7B H15 2.580(4) . 3_665 no H7C H3B 2.485(4) . 3_665 no H12 Si2 2.797(3) . . no H12 C5 2.859(3) . . no H12 C6 2.989(3) . . no H12 H5C 2.245(4) . . no H12 H6B 2.370(4) . . no H12 C13 3.039(3) . 3_565 no H12 H13 2.507(4) . 3_565 no H13 C2 2.908(3) . 3_565 no H13 C12 3.054(3) . 3_565 no H13 H2B 2.288(4) . 3_565 no H13 H2C 2.598(4) . 3_565 no H13 H6B 2.530(4) . 3_565 no H13 H12 2.507(4) . 3_565 no H14 C6 2.927(3) . 1_565 no H14 H6A 2.330(4) . 1_565 no H15 H6C 2.572(4) . 1_565 no H15 H2A 2.382(4) . 2_555 no H15 H7B 2.580(4) . 3_665 no # End of Crystallographic Information File