Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Eva Hevia' 'David R. Armstrong' 'W. Clegg' 'David V. Graham' 'Emma Herd' 'A R Kennedy' 'Luca Russo' _publ_contact_author_name 'Eva Hevia' _publ_contact_author_address ; Pure and Applied Chemistry UNiversity of Strathclyde Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email EVA.HEVIA@STRATH.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Structural Elucidation of Solvent-Free and Solvated Lithium Dimethyl(HMDS) zincates ; data_grem289 _database_code_depnum_ccdc_archive 'CCDC 665388' #--------------------------------------------- #-------------- COMPOUND 4 ------------------- #--------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H24 Li N Si2 Zn' _chemical_formula_weight 262.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.7840(3) _cell_length_b 13.9936(7) _cell_length_c 15.8133(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.650(2) _cell_angle_gamma 90.00 _cell_volume 1487.84(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 3486 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.777 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Lots on non-Bragg diffraction - streaks along c axis. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17703 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3239 _reflns_number_gt 2286 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The Zn and Li sites are treated as being affected by mutual substitution disorder, caused by the similarity in the atomic radii of Zn and Li. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+6.0385P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3239 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.36936(10) 0.33852(6) 0.99497(5) 0.0255(2) Uani 0.799(2) 1 d P . 1 Li2 Li 0.0231(4) 0.3317(2) 0.99108(15) 0.0327(9) Uani 0.799(2) 1 d P . 1 Si1 Si 0.1642(2) 0.15318(11) 0.90847(9) 0.0277(4) Uani 1 1 d . . . Si2 Si 0.1546(2) 0.33901(12) 0.80745(9) 0.0297(4) Uani 1 1 d . . . N1 N 0.1702(6) 0.2756(3) 0.9008(2) 0.0230(9) Uani 1 1 d . . . C1 C 0.2119(11) 0.3964(6) 1.0795(4) 0.0384(15) Uani 1 1 d . . . C2 C 0.6551(10) 0.3285(7) 0.9879(5) 0.040(2) Uani 0.799(2) 1 d P . 1 H2A H 0.7101 0.3924 0.9815 0.061 Uiso 0.799(2) 1 calc PR . 1 H2B H 0.6758 0.2892 0.9385 0.061 Uiso 0.799(2) 1 calc PR . 1 H2C H 0.7221 0.2988 1.0401 0.061 Uiso 0.799(2) 1 calc PR . 1 C3 C 0.1100(12) 0.1230(5) 1.0194(4) 0.0537(19) Uani 1 1 d . . . H3A H 0.2057 0.1558 1.0615 0.081 Uiso 1 1 calc R . . H3B H 0.1212 0.0538 1.0283 0.081 Uiso 1 1 calc R . . H3C H -0.0251 0.1437 1.0260 0.081 Uiso 1 1 calc R . . C4 C 0.4077(8) 0.0942(4) 0.8963(5) 0.0496(18) Uani 1 1 d . . . H4A H 0.4482 0.1120 0.8412 0.074 Uiso 1 1 calc R . . H4B H 0.3925 0.0247 0.8989 0.074 Uiso 1 1 calc R . . H4C H 0.5094 0.1151 0.9424 0.074 Uiso 1 1 calc R . . C5 C -0.0336(8) 0.0975(4) 0.8300(4) 0.0352(14) Uani 1 1 d . . . H5A H -0.1643 0.1209 0.8406 0.053 Uiso 1 1 calc R . . H5B H -0.0287 0.0279 0.8365 0.053 Uiso 1 1 calc R . . H5C H -0.0114 0.1146 0.7720 0.053 Uiso 1 1 calc R . . C6 C 0.2985(10) 0.2846(5) 0.7263(4) 0.0526(18) Uani 1 1 d . . . H6A H 0.4388 0.2789 0.7504 0.079 Uiso 1 1 calc R . . H6B H 0.2871 0.3253 0.6755 0.079 Uiso 1 1 calc R . . H6C H 0.2450 0.2210 0.7105 0.079 Uiso 1 1 calc R . . C7 C -0.1076(9) 0.3557(5) 0.7564(4) 0.0515(18) Uani 1 1 d . . . H7A H -0.1714 0.2932 0.7464 0.077 Uiso 1 1 calc R . . H7B H -0.1084 0.3891 0.7019 0.077 Uiso 1 1 calc R . . H7C H -0.1805 0.3936 0.7941 0.077 Uiso 1 1 calc R . . C8 C 0.2576(9) 0.4624(4) 0.8325(4) 0.0423(15) Uani 1 1 d . . . H8A H 0.1881 0.4918 0.8764 0.063 Uiso 1 1 calc R . . H8B H 0.2382 0.5017 0.7807 0.063 Uiso 1 1 calc R . . H8C H 0.3999 0.4580 0.8533 0.063 Uiso 1 1 calc R . . Li1 Li 0.36936(10) 0.33852(6) 0.99497(5) 0.0255(2) Uani 0.201(2) 1 d P . 2 Zn2 Zn 0.0231(4) 0.3317(2) 0.99108(15) 0.0327(9) Uani 0.201(2) 1 d P . 2 C2A C 0.726(5) 0.337(3) 0.969(2) 0.039 Uiso 0.201(2) 1 d P . 2 H1A H 0.306(10) 0.438(5) 1.116(4) 0.07(2) Uiso 1 1 d . . . H1B H 0.171(13) 0.354(7) 1.110(6) 0.11(3) Uiso 1 1 d . . . H1C H 0.127(13) 0.433(7) 1.058(6) 0.10(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0181(3) 0.0328(4) 0.0248(4) -0.0015(4) -0.0003(3) -0.0037(3) Li2 0.0297(14) 0.0406(17) 0.0295(14) 0.0011(12) 0.0101(10) 0.0037(12) Si1 0.0277(7) 0.0283(8) 0.0259(8) -0.0018(7) -0.0012(6) -0.0037(7) Si2 0.0284(7) 0.0377(9) 0.0221(7) 0.0018(7) 0.0005(6) -0.0060(7) N1 0.018(2) 0.029(2) 0.022(2) -0.0011(18) 0.0008(17) -0.0031(18) C1 0.039(4) 0.044(4) 0.032(4) -0.009(3) 0.001(3) -0.010(3) C2 0.024(4) 0.060(6) 0.036(5) -0.005(4) 0.001(3) -0.015(4) C3 0.097(6) 0.035(4) 0.028(3) 0.002(3) 0.002(3) -0.013(4) C4 0.034(3) 0.035(4) 0.076(5) -0.009(3) -0.007(3) 0.003(3) C5 0.031(3) 0.042(4) 0.032(3) -0.007(3) 0.002(2) -0.008(3) C6 0.070(5) 0.057(4) 0.035(4) -0.005(3) 0.024(3) -0.011(4) C7 0.041(4) 0.066(5) 0.043(4) 0.015(3) -0.012(3) -0.008(3) C8 0.047(4) 0.038(4) 0.039(3) 0.011(3) -0.002(3) -0.007(3) Li1 0.0181(3) 0.0328(4) 0.0248(4) -0.0015(4) -0.0003(3) -0.0037(3) Zn2 0.0297(14) 0.0406(17) 0.0295(14) 0.0011(12) 0.0101(10) 0.0037(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C2 1.962(7) . ? Zn1 C1 1.991(7) . ? Zn1 N1 2.070(4) . ? Zn1 Li2 2.344(2) . ? Li2 C1 1.985(7) . ? Li2 N1 2.008(5) . ? Li2 C2 2.491(7) 1_455 ? Li2 Si1 3.033(3) . ? Li2 Si2 3.151(3) . ? Li2 H1B 2.04(9) . ? Li2 H1C 1.84(9) . ? Si1 N1 1.718(4) . ? Si1 C5 1.872(5) . ? Si1 C4 1.879(6) . ? Si1 C3 1.887(6) . ? Si2 N1 1.714(4) . ? Si2 C7 1.867(6) . ? Si2 C6 1.875(6) . ? Si2 C8 1.885(6) . ? C1 H1A 0.99(8) . ? C1 H1B 0.84(9) . ? C1 H1C 0.81(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C2A Zn2 2.00(3) 1_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Zn1 C1 133.6(3) . . ? C2 Zn1 N1 118.9(3) . . ? C1 Zn1 N1 107.4(2) . . ? C2 Zn1 Li2 172.0(3) . . ? C1 Zn1 Li2 53.8(2) . . ? N1 Zn1 Li2 53.68(12) . . ? C1 Li2 N1 110.1(3) . . ? C1 Li2 Zn1 54.0(2) . . ? N1 Li2 Zn1 56.17(13) . . ? C1 Li2 C2 125.0(3) . 1_455 ? N1 Li2 C2 124.7(2) . 1_455 ? Zn1 Li2 C2 178.7(3) . 1_455 ? C1 Li2 Si1 117.9(2) . . ? N1 Li2 Si1 32.43(13) . . ? Zn1 Li2 Si1 70.84(7) . . ? C2 Li2 Si1 110.4(2) 1_455 . ? C1 Li2 Si2 113.5(2) . . ? N1 Li2 Si2 29.41(13) . . ? Zn1 Li2 Si2 67.48(6) . . ? C2 Li2 Si2 112.8(2) 1_455 . ? Si1 Li2 Si2 59.03(6) . . ? C1 Li2 H1B 24(3) . . ? N1 Li2 H1B 119(3) . . ? Zn1 Li2 H1B 67(3) . . ? C2 Li2 H1B 113(3) 1_455 . ? Si1 Li2 H1B 112(3) . . ? Si2 Li2 H1B 133(3) . . ? C1 Li2 H1C 24(3) . . ? N1 Li2 H1C 121(3) . . ? Zn1 Li2 H1C 70(3) . . ? C2 Li2 H1C 109(3) 1_455 . ? Si1 Li2 H1C 139(3) . . ? Si2 Li2 H1C 112(3) . . ? H1B Li2 H1C 42(3) . . ? N1 Si1 C5 112.9(2) . . ? N1 Si1 C4 113.7(3) . . ? C5 Si1 C4 108.2(3) . . ? N1 Si1 C3 107.3(2) . . ? C5 Si1 C3 108.1(3) . . ? C4 Si1 C3 106.2(3) . . ? N1 Si1 Li2 38.81(14) . . ? C5 Si1 Li2 112.9(2) . . ? C4 Si1 Li2 137.6(2) . . ? C3 Si1 Li2 70.9(2) . . ? N1 Si2 C7 112.5(2) . . ? N1 Si2 C6 113.7(3) . . ? C7 Si2 C6 107.9(3) . . ? N1 Si2 C8 108.4(2) . . ? C7 Si2 C8 106.3(3) . . ? C6 Si2 C8 107.7(3) . . ? N1 Si2 Li2 35.12(15) . . ? C7 Si2 Li2 91.8(2) . . ? C6 Si2 Li2 148.8(2) . . ? C8 Si2 Li2 88.8(2) . . ? Si2 N1 Si1 125.3(2) . . ? Si2 N1 Li2 115.5(2) . . ? Si1 N1 Li2 108.8(2) . . ? Si2 N1 Zn1 111.0(2) . . ? Si1 N1 Zn1 113.1(2) . . ? Li2 N1 Zn1 70.14(15) . . ? Li2 C1 Zn1 72.2(2) . . ? Li2 C1 H1A 169(4) . . ? Zn1 C1 H1A 106(4) . . ? Li2 C1 H1B 81(6) . . ? Zn1 C1 H1B 110(6) . . ? H1A C1 H1B 109(7) . . ? Li2 C1 H1C 68(7) . . ? Zn1 C1 H1C 113(6) . . ? H1A C1 H1C 104(7) . . ? H1B C1 H1C 115(8) . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 Zn1 Li2 C1 158.8(19) . . . . ? N1 Zn1 Li2 C1 -177.6(3) . . . . ? C2 Zn1 Li2 N1 -23.6(19) . . . . ? C1 Zn1 Li2 N1 177.6(3) . . . . ? C2 Zn1 Li2 C2 -158(11) . . . 1_455 ? C1 Zn1 Li2 C2 43(10) . . . 1_455 ? N1 Zn1 Li2 C2 -135(10) . . . 1_455 ? C2 Zn1 Li2 Si1 9.0(19) . . . . ? C1 Zn1 Li2 Si1 -149.8(3) . . . . ? N1 Zn1 Li2 Si1 32.56(15) . . . . ? C2 Zn1 Li2 Si2 -54.6(19) . . . . ? C1 Zn1 Li2 Si2 146.6(3) . . . . ? N1 Zn1 Li2 Si2 -30.97(15) . . . . ? C1 Li2 Si1 N1 -83.9(4) . . . . ? Zn1 Li2 Si1 N1 -56.5(2) . . . . ? C2 Li2 Si1 N1 123.2(3) 1_455 . . . ? Si2 Li2 Si1 N1 18.2(2) . . . . ? C1 Li2 Si1 C5 177.5(3) . . . . ? N1 Li2 Si1 C5 -98.6(3) . . . . ? Zn1 Li2 Si1 C5 -155.1(2) . . . . ? C2 Li2 Si1 C5 24.6(3) 1_455 . . . ? Si2 Li2 Si1 C5 -80.4(2) . . . . ? C1 Li2 Si1 C4 -18.1(5) . . . . ? N1 Li2 Si1 C4 65.7(4) . . . . ? Zn1 Li2 Si1 C4 9.3(4) . . . . ? C2 Li2 Si1 C4 -171.0(4) 1_455 . . . ? Si2 Li2 Si1 C4 83.9(3) . . . . ? C1 Li2 Si1 C3 75.3(4) . . . . ? N1 Li2 Si1 C3 159.2(3) . . . . ? Zn1 Li2 Si1 C3 102.7(2) . . . . ? C2 Li2 Si1 C3 -77.6(3) 1_455 . . . ? Si2 Li2 Si1 C3 177.4(3) . . . . ? C1 Li2 Si2 N1 89.6(4) . . . . ? Zn1 Li2 Si2 N1 60.5(2) . . . . ? C2 Li2 Si2 N1 -120.8(4) 1_455 . . . ? Si1 Li2 Si2 N1 -19.9(2) . . . . ? C1 Li2 Si2 C7 -142.1(4) . . . . ? N1 Li2 Si2 C7 128.3(3) . . . . ? Zn1 Li2 Si2 C7 -171.1(2) . . . . ? C2 Li2 Si2 C7 7.5(3) 1_455 . . . ? Si1 Li2 Si2 C7 108.4(2) . . . . ? C1 Li2 Si2 C6 87.6(5) . . . . ? N1 Li2 Si2 C6 -2.0(5) . . . . ? Zn1 Li2 Si2 C6 58.6(5) . . . . ? C2 Li2 Si2 C6 -122.8(5) 1_455 . . . ? Si1 Li2 Si2 C6 -21.9(4) . . . . ? C1 Li2 Si2 C8 -35.8(3) . . . . ? N1 Li2 Si2 C8 -125.4(3) . . . . ? Zn1 Li2 Si2 C8 -64.8(2) . . . . ? C2 Li2 Si2 C8 113.8(3) 1_455 . . . ? Si1 Li2 Si2 C8 -145.3(2) . . . . ? C7 Si2 N1 Si1 82.7(4) . . . . ? C6 Si2 N1 Si1 -40.4(4) . . . . ? C8 Si2 N1 Si1 -160.0(3) . . . . ? Li2 Si2 N1 Si1 140.7(4) . . . . ? C7 Si2 N1 Li2 -58.1(4) . . . . ? C6 Si2 N1 Li2 178.9(3) . . . . ? C8 Si2 N1 Li2 59.2(3) . . . . ? C7 Si2 N1 Zn1 -135.4(3) . . . . ? C6 Si2 N1 Zn1 101.6(3) . . . . ? C8 Si2 N1 Zn1 -18.1(3) . . . . ? Li2 Si2 N1 Zn1 -77.3(2) . . . . ? C5 Si1 N1 Si2 -44.4(4) . . . . ? C4 Si1 N1 Si2 79.3(4) . . . . ? C3 Si1 N1 Si2 -163.5(3) . . . . ? Li2 Si1 N1 Si2 -142.9(4) . . . . ? C5 Si1 N1 Li2 98.5(3) . . . . ? C4 Si1 N1 Li2 -137.8(3) . . . . ? C3 Si1 N1 Li2 -20.6(3) . . . . ? C5 Si1 N1 Zn1 174.3(2) . . . . ? C4 Si1 N1 Zn1 -62.0(3) . . . . ? C3 Si1 N1 Zn1 55.2(3) . . . . ? Li2 Si1 N1 Zn1 75.8(2) . . . . ? C1 Li2 N1 Si2 -102.4(3) . . . . ? Zn1 Li2 N1 Si2 -104.5(2) . . . . ? C2 Li2 N1 Si2 74.4(4) 1_455 . . . ? Si1 Li2 N1 Si2 147.0(4) . . . . ? C1 Li2 N1 Si1 110.6(3) . . . . ? Zn1 Li2 N1 Si1 108.6(2) . . . . ? C2 Li2 N1 Si1 -72.6(4) 1_455 . . . ? Si2 Li2 N1 Si1 -147.0(4) . . . . ? C1 Li2 N1 Zn1 2.1(3) . . . . ? C2 Li2 N1 Zn1 178.9(3) 1_455 . . . ? Si1 Li2 N1 Zn1 -108.6(2) . . . . ? Si2 Li2 N1 Zn1 104.5(2) . . . . ? C2 Zn1 N1 Si2 -73.1(4) . . . . ? C1 Zn1 N1 Si2 108.5(3) . . . . ? Li2 Zn1 N1 Si2 110.6(3) . . . . ? C2 Zn1 N1 Si1 73.8(4) . . . . ? C1 Zn1 N1 Si1 -104.6(3) . . . . ? Li2 Zn1 N1 Si1 -102.6(2) . . . . ? C2 Zn1 N1 Li2 176.4(3) . . . . ? C1 Zn1 N1 Li2 -2.0(3) . . . . ? N1 Li2 C1 Zn1 -2.1(3) . . . . ? C2 Li2 C1 Zn1 -178.9(3) 1_455 . . . ? Si1 Li2 C1 Zn1 32.5(3) . . . . ? Si2 Li2 C1 Zn1 -33.6(3) . . . . ? C2 Zn1 C1 Li2 -176.0(4) . . . . ? N1 Zn1 C1 Li2 2.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.772 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.096 #===END #--------------------------------------------- #-------------- COMPOUND 5 ------------------- #--------------------------------------------- data_rem388 _database_code_depnum_ccdc_archive 'CCDC 665389' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H47 Li N4 Si2 Zn' _chemical_formula_weight 436.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.616(3) _cell_length_b 13.522(4) _cell_length_c 20.444(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.676(4) _cell_angle_gamma 90.00 _cell_volume 2612.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.039 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6246 _exptl_absorpt_correction_T_max 0.8597 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22855 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.67 _diffrn_reflns_theta_max 28.36 _reflns_number_total 6301 _reflns_number_gt 5588 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Mercury 1.5' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+0.7214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6301 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0642 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.249484(15) 0.647702(10) 0.387805(7) 0.02601(5) Uani 1 1 d . . . Si1 Si 0.05833(3) 0.73028(2) 0.484756(16) 0.02328(7) Uani 1 1 d . . . Si2 Si 0.33117(3) 0.83541(2) 0.473922(16) 0.02343(7) Uani 1 1 d . . . Li1 Li 0.2758(2) 0.47644(15) 0.31501(10) 0.0268(4) Uani 1 1 d . . . C1 C 0.27364(16) 0.70333(11) 0.29956(7) 0.0374(3) Uani 1 1 d . . . H1A H 0.1839 0.7320 0.2770 0.056 Uiso 1 1 calc R . . H1B H 0.3021 0.6504 0.2721 0.056 Uiso 1 1 calc R . . H1C H 0.3467 0.7548 0.3066 0.056 Uiso 1 1 calc R . . C2 C 0.27047(17) 0.50873(10) 0.42673(7) 0.0384(3) Uani 1 1 d . . . H2A H 0.2764 0.5122 0.4750 0.058 Uiso 1 1 calc R . . H2B H 0.3568 0.4783 0.4169 0.058 Uiso 1 1 calc R . . H2C H 0.1883 0.4688 0.4070 0.058 Uiso 1 1 calc R . . C3 C -0.07155(15) 0.64882(11) 0.42913(7) 0.0367(3) Uani 1 1 d . . . H3A H -0.0942 0.6781 0.3846 0.055 Uiso 1 1 calc R . . H3B H -0.1583 0.6427 0.4476 0.055 Uiso 1 1 calc R . . H3C H -0.0299 0.5832 0.4263 0.055 Uiso 1 1 calc R . . C4 C -0.03901(15) 0.84850(10) 0.49477(7) 0.0333(3) Uani 1 1 d . . . H4A H 0.0224 0.8926 0.5255 0.050 Uiso 1 1 calc R . . H4B H -0.1244 0.8336 0.5127 0.050 Uiso 1 1 calc R . . H4C H -0.0657 0.8809 0.4514 0.050 Uiso 1 1 calc R . . C5 C 0.09341(15) 0.66845(11) 0.56876(7) 0.0372(3) Uani 1 1 d . . . H5A H 0.1520 0.6095 0.5669 0.056 Uiso 1 1 calc R . . H5B H 0.0034 0.6491 0.5810 0.056 Uiso 1 1 calc R . . H5C H 0.1432 0.7145 0.6021 0.056 Uiso 1 1 calc R . . C6 C 0.50771(14) 0.79234(13) 0.45766(7) 0.0414(3) Uani 1 1 d . . . H6A H 0.5306 0.7279 0.4789 0.062 Uiso 1 1 calc R . . H6B H 0.5808 0.8404 0.4761 0.062 Uiso 1 1 calc R . . H6C H 0.5036 0.7863 0.4096 0.062 Uiso 1 1 calc R . . C7 C 0.29080(17) 0.95386(11) 0.42652(8) 0.0420(3) Uani 1 1 d . . . H7A H 0.2776 0.9404 0.3787 0.063 Uiso 1 1 calc R . . H7B H 0.3696 1.0002 0.4392 0.063 Uiso 1 1 calc R . . H7C H 0.2041 0.9829 0.4369 0.063 Uiso 1 1 calc R . . C8 C 0.35493(15) 0.87123(12) 0.56436(7) 0.0373(3) Uani 1 1 d . . . H8A H 0.2675 0.9014 0.5731 0.056 Uiso 1 1 calc R . . H8B H 0.4328 0.9188 0.5749 0.056 Uiso 1 1 calc R . . H8C H 0.3769 0.8122 0.5921 0.056 Uiso 1 1 calc R . . C9 C 0.08274(16) 0.53835(11) 0.18155(7) 0.0397(3) Uani 1 1 d . . . H9A H -0.0023 0.5234 0.1486 0.060 Uiso 1 1 calc R . . H9B H 0.1662 0.5341 0.1605 0.060 Uiso 1 1 calc R . . H9C H 0.0754 0.6053 0.1989 0.060 Uiso 1 1 calc R . . C10 C -0.02735(15) 0.47717(12) 0.26884(7) 0.0395(3) Uani 1 1 d . . . H10A H -0.0317 0.5450 0.2852 0.059 Uiso 1 1 calc R . . H10B H -0.0191 0.4309 0.3063 0.059 Uiso 1 1 calc R . . H10C H -0.1137 0.4626 0.2366 0.059 Uiso 1 1 calc R . . C11 C 0.10271(15) 0.36610(10) 0.20897(6) 0.0329(3) Uani 1 1 d . . . H11A H 0.1732 0.3652 0.1793 0.040 Uiso 1 1 calc R . . H11B H 0.0094 0.3492 0.1819 0.040 Uiso 1 1 calc R . . C12 C 0.14237(15) 0.28874(10) 0.26285(7) 0.0355(3) Uani 1 1 d . . . H12A H 0.0640 0.2817 0.2878 0.043 Uiso 1 1 calc R . . H12B H 0.1551 0.2242 0.2419 0.043 Uiso 1 1 calc R . . C13 C 0.28169(17) 0.25531(11) 0.37046(7) 0.0403(3) Uani 1 1 d . . . H13A H 0.2000 0.2701 0.3912 0.060 Uiso 1 1 calc R . . H13B H 0.3691 0.2717 0.4015 0.060 Uiso 1 1 calc R . . H13C H 0.2817 0.1848 0.3593 0.060 Uiso 1 1 calc R . . C14 C 0.40113(15) 0.29656(9) 0.28066(7) 0.0329(3) Uani 1 1 d . . . H14A H 0.3787 0.3080 0.2320 0.039 Uiso 1 1 calc R . . H14B H 0.4314 0.2269 0.2883 0.039 Uiso 1 1 calc R . . C15 C 0.52083(14) 0.36449(10) 0.31164(7) 0.0326(3) Uani 1 1 d . . . H15A H 0.5411 0.3545 0.3605 0.039 Uiso 1 1 calc R . . H15B H 0.6073 0.3473 0.2943 0.039 Uiso 1 1 calc R . . C16 C 0.58535(15) 0.53338(11) 0.34093(8) 0.0393(3) Uani 1 1 d . . . H16A H 0.6816 0.5205 0.3336 0.059 Uiso 1 1 calc R . . H16B H 0.5801 0.5192 0.3874 0.059 Uiso 1 1 calc R . . H16C H 0.5613 0.6029 0.3311 0.059 Uiso 1 1 calc R . . C17 C 0.49383(16) 0.49311(11) 0.22757(7) 0.0378(3) Uani 1 1 d . . . H17A H 0.4677 0.5625 0.2184 0.057 Uiso 1 1 calc R . . H17B H 0.4289 0.4503 0.1975 0.057 Uiso 1 1 calc R . . H17C H 0.5908 0.4822 0.2207 0.057 Uiso 1 1 calc R . . N1 N 0.20607(11) 0.74752(7) 0.45233(5) 0.0257(2) Uani 1 1 d . . . N2 N 0.27317(11) 0.31424(8) 0.30953(5) 0.0277(2) Uani 1 1 d . . . N3 N 0.09624(11) 0.46663(8) 0.23657(5) 0.0269(2) Uani 1 1 d . . . N4 N 0.48490(11) 0.46962(8) 0.29685(5) 0.0269(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02982(8) 0.02370(8) 0.02689(8) -0.00654(5) 0.01141(6) -0.00343(5) Si1 0.02438(16) 0.02315(16) 0.02406(15) -0.00185(12) 0.00902(12) -0.00315(12) Si2 0.02215(15) 0.02561(16) 0.02330(15) -0.00438(12) 0.00622(12) -0.00403(12) Li1 0.0274(10) 0.0280(10) 0.0257(9) -0.0024(8) 0.0066(8) 0.0018(8) C1 0.0445(8) 0.0407(8) 0.0290(6) -0.0022(5) 0.0124(6) -0.0006(6) C2 0.0564(9) 0.0300(7) 0.0333(7) -0.0022(5) 0.0203(6) 0.0009(6) C3 0.0341(7) 0.0367(7) 0.0403(7) -0.0063(6) 0.0091(6) -0.0123(5) C4 0.0318(7) 0.0330(7) 0.0373(7) -0.0024(5) 0.0125(5) 0.0029(5) C5 0.0355(7) 0.0439(8) 0.0346(7) 0.0099(6) 0.0125(6) -0.0011(6) C6 0.0257(6) 0.0605(10) 0.0386(7) -0.0133(7) 0.0079(5) -0.0014(6) C7 0.0429(8) 0.0323(7) 0.0501(9) 0.0066(6) 0.0062(7) -0.0106(6) C8 0.0340(7) 0.0481(8) 0.0300(6) -0.0130(6) 0.0068(5) -0.0069(6) C9 0.0431(8) 0.0422(8) 0.0314(7) 0.0105(6) 0.0005(6) -0.0050(6) C10 0.0334(7) 0.0521(9) 0.0339(7) 0.0027(6) 0.0084(6) 0.0045(6) C11 0.0353(7) 0.0343(7) 0.0279(6) -0.0057(5) 0.0021(5) -0.0067(5) C12 0.0391(7) 0.0255(6) 0.0408(7) -0.0028(5) 0.0046(6) -0.0079(5) C13 0.0497(8) 0.0312(7) 0.0417(8) 0.0118(6) 0.0131(6) 0.0058(6) C14 0.0399(7) 0.0233(6) 0.0376(7) -0.0038(5) 0.0129(6) 0.0050(5) C15 0.0288(6) 0.0320(7) 0.0381(7) -0.0009(5) 0.0094(5) 0.0085(5) C16 0.0287(7) 0.0423(8) 0.0459(8) -0.0080(6) 0.0042(6) -0.0058(6) C17 0.0408(7) 0.0406(8) 0.0356(7) 0.0012(6) 0.0163(6) -0.0037(6) N1 0.0285(5) 0.0241(5) 0.0278(5) -0.0076(4) 0.0133(4) -0.0065(4) N2 0.0324(5) 0.0219(5) 0.0293(5) 0.0014(4) 0.0069(4) 0.0008(4) N3 0.0285(5) 0.0283(5) 0.0233(5) 0.0018(4) 0.0036(4) -0.0014(4) N4 0.0256(5) 0.0271(5) 0.0289(5) -0.0016(4) 0.0072(4) -0.0003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 Li1 2.790(2) . ? Zn1 C1 2.0074(14) . ? Zn1 C2 2.0361(15) . ? Zn1 N1 1.9851(10) . ? Si1 C3 1.8816(14) . ? Si1 C4 1.8827(14) . ? Si1 C5 1.8835(15) . ? Si1 N1 1.6914(11) . ? Si2 C6 1.8816(15) . ? Si2 C7 1.8750(15) . ? Si2 C8 1.8838(14) . ? Si2 N1 1.6904(11) . ? Li1 N2 2.196(2) . ? Li1 N3 2.132(2) . ? Li1 N4 2.113(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C9 N3 1.4726(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 N3 1.4691(17) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.5156(19) . ? C11 N3 1.4775(17) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 N2 1.4720(17) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 N2 1.4683(17) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.5164(19) . ? C14 N2 1.4793(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 N4 1.4809(17) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 N4 1.4717(17) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 N4 1.4694(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Li1 Zn1 C1 78.14(6) . . ? Li1 Zn1 C2 55.26(6) . . ? Li1 Zn1 N1 165.95(5) . . ? C1 Zn1 C2 132.64(6) . . ? C1 Zn1 N1 114.59(6) . . ? C2 Zn1 N1 112.68(5) . . ? C3 Si1 C4 105.97(7) . . ? C3 Si1 C5 106.14(7) . . ? C3 Si1 N1 110.82(6) . . ? C4 Si1 C5 106.65(7) . . ? C4 Si1 N1 113.34(6) . . ? C5 Si1 N1 113.39(6) . . ? C6 Si2 C7 106.28(8) . . ? C6 Si2 C8 107.68(7) . . ? C6 Si2 N1 110.97(6) . . ? C7 Si2 C8 105.28(8) . . ? C7 Si2 N1 113.36(6) . . ? C8 Si2 N1 112.84(6) . . ? Zn1 Li1 N2 148.76(10) . . ? Zn1 Li1 N3 108.19(8) . . ? Zn1 Li1 N4 108.26(9) . . ? N2 Li1 N3 84.22(8) . . ? N2 Li1 N4 87.12(8) . . ? N3 Li1 N4 121.97(10) . . ? Zn1 C1 H1A 109.5 . . ? Zn1 C1 H1B 109.5 . . ? Zn1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Zn1 C2 H2A 109.5 . . ? Zn1 C2 H2B 109.5 . . ? Zn1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9A C9 N3 109.5 . . ? H9B C9 H9C 109.5 . . ? H9B C9 N3 109.5 . . ? H9C C9 N3 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10A C10 N3 109.5 . . ? H10B C10 H10C 109.5 . . ? H10B C10 N3 109.5 . . ? H10C C10 N3 109.5 . . ? H11A C11 H11B 107.9 . . ? H11A C11 C12 109.1 . . ? H11A C11 N3 109.1 . . ? H11B C11 C12 109.1 . . ? H11B C11 N3 109.1 . . ? C12 C11 N3 112.35(11) . . ? C11 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C11 C12 N2 112.29(11) . . ? H12A C12 H12B 107.9 . . ? H12A C12 N2 109.1 . . ? H12B C12 N2 109.1 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13A C13 N2 109.5 . . ? H13B C13 H13C 109.5 . . ? H13B C13 N2 109.5 . . ? H13C C13 N2 109.5 . . ? H14A C14 H14B 108.0 . . ? H14A C14 C15 109.4 . . ? H14A C14 N2 109.4 . . ? H14B C14 C15 109.4 . . ? H14B C14 N2 109.4 . . ? C15 C14 N2 111.01(10) . . ? C14 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? C14 C15 N4 111.46(11) . . ? H15A C15 H15B 108.0 . . ? H15A C15 N4 109.3 . . ? H15B C15 N4 109.3 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16A C16 N4 109.5 . . ? H16B C16 H16C 109.5 . . ? H16B C16 N4 109.5 . . ? H16C C16 N4 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17A C17 N4 109.5 . . ? H17B C17 H17C 109.5 . . ? H17B C17 N4 109.5 . . ? H17C C17 N4 109.5 . . ? Zn1 N1 Si1 117.52(5) . . ? Zn1 N1 Si2 115.12(5) . . ? Si1 N1 Si2 127.11(6) . . ? Li1 N2 C12 105.51(9) . . ? Li1 N2 C13 120.03(10) . . ? Li1 N2 C14 100.32(9) . . ? C12 N2 C13 109.25(11) . . ? C12 N2 C14 112.17(11) . . ? C13 N2 C14 109.33(11) . . ? Li1 N3 C9 118.57(10) . . ? Li1 N3 C10 105.42(10) . . ? Li1 N3 C11 105.01(9) . . ? C9 N3 C10 108.36(11) . . ? C9 N3 C11 108.55(10) . . ? C10 N3 C11 110.83(11) . . ? Li1 N4 C15 101.51(9) . . ? Li1 N4 C16 113.88(10) . . ? Li1 N4 C17 112.79(10) . . ? C15 N4 C16 109.60(11) . . ? C15 N4 C17 110.56(11) . . ? C16 N4 C17 108.34(11) . . ? 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 C1 Zn1 Li1 N2 -175.9(2) . . . . ? C1 Zn1 Li1 N3 -66.13(9) . . . . ? C1 Zn1 Li1 N4 67.91(9) . . . . ? C2 Zn1 Li1 N2 13.03(17) . . . . ? C2 Zn1 Li1 N3 122.74(11) . . . . ? C2 Zn1 Li1 N4 -103.21(11) . . . . ? N1 Zn1 Li1 N2 -20.0(4) . . . . ? N1 Zn1 Li1 N3 89.7(2) . . . . ? N1 Zn1 Li1 N4 -136.26(19) . . . . ? N3 C11 C12 N2 -52.92(16) . . . . ? N2 C14 C15 N4 -63.73(14) . . . . ? C6 Si2 N1 Zn1 -21.34(9) . . . . ? C6 Si2 N1 Si1 152.64(8) . . . . ? C7 Si2 N1 Zn1 98.16(8) . . . . ? C7 Si2 N1 Si1 -87.86(10) . . . . ? C8 Si2 N1 Zn1 -142.29(7) . . . . ? C8 Si2 N1 Si1 31.69(11) . . . . ? C3 Si1 N1 Zn1 -22.43(9) . . . . ? C3 Si1 N1 Si2 163.72(8) . . . . ? C4 Si1 N1 Zn1 -141.42(7) . . . . ? C4 Si1 N1 Si2 44.73(10) . . . . ? C5 Si1 N1 Zn1 96.81(8) . . . . ? C5 Si1 N1 Si2 -77.05(10) . . . . ? Li1 Zn1 N1 Si1 -29.3(3) . . . . ? Li1 Zn1 N1 Si2 145.3(2) . . . . ? C1 Zn1 N1 Si1 124.52(7) . . . . ? C1 Zn1 N1 Si2 -60.89(8) . . . . ? C2 Zn1 N1 Si1 -58.38(8) . . . . ? C2 Zn1 N1 Si2 116.20(7) . . . . ? C11 C12 N2 Li1 32.18(14) . . . . ? C11 C12 N2 C13 162.49(11) . . . . ? C11 C12 N2 C14 -76.12(14) . . . . ? C15 C14 N2 Li1 41.19(13) . . . . ? C15 C14 N2 C12 152.77(11) . . . . ? C15 C14 N2 C13 -85.89(13) . . . . ? Zn1 Li1 N2 C12 108.75(19) . . . . ? Zn1 Li1 N2 C13 -15.0(2) . . . . ? Zn1 Li1 N2 C14 -134.60(18) . . . . ? N3 Li1 N2 C12 -7.23(10) . . . . ? N3 Li1 N2 C13 -130.99(11) . . . . ? N3 Li1 N2 C14 109.42(9) . . . . ? N4 Li1 N2 C12 -129.78(10) . . . . ? N4 Li1 N2 C13 106.47(12) . . . . ? N4 Li1 N2 C14 -13.13(10) . . . . ? C12 C11 N3 Li1 42.19(13) . . . . ? C12 C11 N3 C9 169.94(11) . . . . ? C12 C11 N3 C10 -71.18(14) . . . . ? Zn1 Li1 N3 C9 69.50(13) . . . . ? Zn1 Li1 N3 C10 -51.98(11) . . . . ? Zn1 Li1 N3 C11 -169.10(8) . . . . ? N2 Li1 N3 C9 -139.89(11) . . . . ? N2 Li1 N3 C10 98.63(10) . . . . ? N2 Li1 N3 C11 -18.48(10) . . . . ? N4 Li1 N3 C9 -56.93(16) . . . . ? N4 Li1 N3 C10 -178.41(12) . . . . ? N4 Li1 N3 C11 64.48(14) . . . . ? C14 C15 N4 Li1 44.86(13) . . . . ? C14 C15 N4 C16 165.59(11) . . . . ? C14 C15 N4 C17 -75.04(13) . . . . ? Zn1 Li1 N4 C15 135.72(9) . . . . ? Zn1 Li1 N4 C16 18.04(13) . . . . ? Zn1 Li1 N4 C17 -105.96(11) . . . . ? N2 Li1 N4 C15 -16.52(10) . . . . ? N2 Li1 N4 C16 -134.20(10) . . . . ? N2 Li1 N4 C17 101.80(10) . . . . ? N3 Li1 N4 C15 -97.88(13) . . . . ? N3 Li1 N4 C16 144.43(12) . . . . ? N3 Li1 N4 C17 20.43(16) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.344 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.040 #===END