# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author 'Dr. Richard A. Layfield' _publ_contact_author_email richard.layfield@manchester.ac.uk _publ_section_title ; Ansa-tris(allyl) complexes of alkali metals: tripodal analogues of cyclopentadienyl and ansa-metallocene ligands ; _publ_contact_author_name 'Dr. Richard A. Layfield' loop_ _publ_author_name 'Richard A. Layfield' 'Felipe Garcia' 'Julian Hannauer' 'Simon M. Humphrey' # Attachment 'new_1_thf.cif' data_lf0702 _database_code_depnum_ccdc_archive 'CCDC 656893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H63 K O Si6 Sn' _chemical_formula_sum 'C31 H63 K O Si6 Sn' _chemical_formula_weight 778.14 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' _cell_length_a 17.4815(9) _cell_length_b 17.4815(9) _cell_length_c 27.596(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7303.5(8) _cell_formula_units_Z 6 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13543 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 20.60 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 7480 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 20.59 _reflns_number_total 1622 _reflns_number_gt 1309 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+16.6017P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 1622 _refine_ls_number_parameters 136 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group K1 K -0.3333 0.3333 0.46703(9) 0.0812(8) Uani 1 3 d S . . Sn1 Sn -0.3333 0.3333 0.334182(16) 0.0558(2) Uani 1 3 d S . . Si1 Si -0.20525(13) 0.24031(14) 0.33099(9) 0.0752(6) Uani 1 1 d . . . Si2 Si -0.04722(17) 0.48292(18) 0.46961(9) 0.1040(8) Uani 1 1 d . . . C1 C -0.2460(4) 0.2895(4) 0.3771(3) 0.066(2) Uani 1 1 d . . . H1 H -0.294(4) 0.238(4) 0.404(2) 0.079 Uiso 1 1 d . . . C2 C -0.1711(5) 0.3686(5) 0.4009(3) 0.0722(19) Uani 1 1 d . . . H2 H -0.140(5) 0.415(4) 0.373(3) 0.087 Uiso 1 1 d . . . C3 C -0.1424(5) 0.3802(5) 0.4466(3) 0.083(2) Uani 1 1 d . . . H3 H -0.179(4) 0.324(5) 0.477(3) 0.099 Uiso 1 1 d . . . C4 C -0.2992(6) 0.1480(6) 0.2968(4) 0.109(3) Uani 1 1 d . . . H4A H -0.3387 0.1023 0.3196 0.163 Uiso 1 1 calc R . . H4B H -0.2757 0.1225 0.2736 0.163 Uiso 1 1 calc R . . H4C H -0.3321 0.1712 0.2793 0.163 Uiso 1 1 calc R . . C5 C -0.1435(7) 0.1938(7) 0.3621(4) 0.122(4) Uani 1 1 d . . . H5A H -0.1833 0.1465 0.3841 0.183 Uiso 1 1 calc R . . H5B H -0.0947 0.2404 0.3807 0.183 Uiso 1 1 calc R . . H5C H -0.1199 0.1699 0.3380 0.183 Uiso 1 1 calc R . . C6 C -0.1298(6) 0.3283(6) 0.2880(3) 0.108(3) Uani 1 1 d . . . H6A H -0.1080 0.3029 0.2639 0.163 Uiso 1 1 calc R . . H6B H -0.0798 0.3749 0.3060 0.163 Uiso 1 1 calc R . . H6C H -0.1621 0.3535 0.2717 0.163 Uiso 1 1 calc R . . C7 C 0.0057(7) 0.5648(7) 0.4215(4) 0.146(4) Uani 1 1 d . . . H7A H 0.0276 0.5411 0.3964 0.219 Uiso 1 1 calc R . . H7B H 0.0552 0.6187 0.4351 0.219 Uiso 1 1 calc R . . H7C H -0.0374 0.5787 0.4073 0.219 Uiso 1 1 calc R . . C8 C 0.0368(8) 0.4571(8) 0.4918(6) 0.189(6) Uani 1 1 d . . . H8A H 0.0115 0.4131 0.5178 0.283 Uiso 1 1 calc R . . H8B H 0.0877 0.5110 0.5043 0.283 Uiso 1 1 calc R . . H8C H 0.0558 0.4335 0.4652 0.283 Uiso 1 1 calc R . . C9 C -0.0837(11) 0.5337(10) 0.5153(6) 0.241(10) Uani 1 1 d . . . H9A H -0.1116 0.4926 0.5423 0.362 Uiso 1 1 calc R . . H9B H -0.1264 0.5478 0.5008 0.362 Uiso 1 1 calc R . . H9C H -0.0326 0.5881 0.5273 0.362 Uiso 1 1 calc R . . O1 O -0.3333 0.3333 0.5673(4) 0.134(4) Uani 1 3 d S . . C10 C -0.2637(18) 0.343(4) 0.5969(7) 0.279(17) Uani 0.67 1 d P . . C11 C -0.290(3) 0.328(4) 0.6465(8) 0.23(2) Uani 0.67 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0904(12) 0.0904(12) 0.0627(17) 0.000 0.000 0.0452(6) Sn1 0.0600(3) 0.0600(3) 0.0476(4) 0.000 0.000 0.02999(14) Si1 0.0800(14) 0.0820(14) 0.0784(14) -0.0055(13) 0.0035(13) 0.0516(13) Si2 0.1007(18) 0.0954(18) 0.0963(18) -0.0234(17) -0.0358(13) 0.0344(16) C1 0.067(5) 0.071(5) 0.063(5) -0.004(4) -0.007(3) 0.037(5) C2 0.067(5) 0.075(5) 0.074(6) -0.001(5) -0.002(5) 0.035(4) C3 0.073(5) 0.100(6) 0.070(6) -0.005(5) -0.028(4) 0.040(5) C4 0.108(7) 0.105(7) 0.122(8) -0.046(6) -0.013(6) 0.060(6) C5 0.126(8) 0.145(8) 0.150(9) 0.000(7) -0.006(6) 0.109(8) C6 0.119(8) 0.117(7) 0.106(8) 0.007(6) 0.027(6) 0.071(6) C7 0.142(10) 0.107(7) 0.146(10) 0.005(7) -0.028(8) 0.029(7) C8 0.143(10) 0.158(10) 0.238(15) 0.023(11) -0.092(11) 0.054(9) C9 0.226(17) 0.199(15) 0.196(17) -0.104(13) 0.025(13) 0.029(13) O1 0.158(6) 0.158(6) 0.086(10) 0.000 0.000 0.079(3) C10 0.16(2) 0.55(5) 0.12(2) 0.02(3) -0.003(16) 0.17(3) C11 0.37(7) 0.30(3) 0.114(11) -0.09(3) -0.12(3) 0.23(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O1 2.767(11) . ? K1 C3 3.065(8) . ? K1 C3 3.065(8) 3_455 ? K1 C3 3.065(8) 2_565 ? K1 C2 3.164(8) . ? K1 C2 3.164(8) 3_455 ? K1 C2 3.164(8) 2_565 ? K1 C1 3.201(7) . ? K1 C1 3.201(7) 3_455 ? K1 C1 3.201(7) 2_565 ? K1 Sn1 3.666(3) . ? K1 H1 2.73(6) . ? K1 H3 2.80(7) . ? Sn1 C1 2.344(7) . ? Sn1 C1 2.344(7) 3_455 ? Sn1 C1 2.344(7) 2_565 ? Si1 C5 1.856(8) . ? Si1 C1 1.865(7) . ? Si1 C6 1.866(8) . ? Si1 C4 1.882(9) . ? Si2 C7 1.828(10) . ? Si2 C9 1.831(14) . ? Si2 C8 1.844(11) . ? Si2 C3 1.846(8) . ? C1 C2 1.499(9) . ? C1 H1 1.14(6) . ? C2 C3 1.337(10) . ? C2 H2 1.04(7) . ? C3 H3 1.20(7) . ? 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 . ? O1 C10 1.40(2) . ? O1 C10 1.40(2) 3_455 ? O1 C10 1.40(2) 2_565 ? C10 C11 1.43(4) . ? C10 C10 1.97(4) 3_455 ? C10 C10 1.97(4) 2_565 ? C11 C11 1.39(4) 2_565 ? C11 C11 1.39(4) 3_455 ? 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 O1 K1 C3 100.58(17) . . ? O1 K1 C3 100.58(17) . 3_455 ? C3 K1 C3 116.71(10) . 3_455 ? O1 K1 C3 100.58(17) . 2_565 ? C3 K1 C3 116.71(10) . 2_565 ? C3 K1 C3 116.71(10) 3_455 2_565 ? O1 K1 C2 125.25(16) . . ? C3 K1 C2 24.72(19) . . ? C3 K1 C2 105.9(2) 3_455 . ? C3 K1 C2 108.4(2) 2_565 . ? O1 K1 C2 125.25(16) . 3_455 ? C3 K1 C2 108.4(2) . 3_455 ? C3 K1 C2 24.72(19) 3_455 3_455 ? C3 K1 C2 105.9(2) 2_565 3_455 ? C2 K1 C2 90.0(2) . 3_455 ? O1 K1 C2 125.25(16) . 2_565 ? C3 K1 C2 105.9(2) . 2_565 ? C3 K1 C2 108.4(2) 3_455 2_565 ? C3 K1 C2 24.72(19) 2_565 2_565 ? C2 K1 C2 90.0(2) . 2_565 ? C2 K1 C2 90.0(2) 3_455 2_565 ? O1 K1 C1 140.81(13) . . ? C3 K1 C1 48.36(19) . . ? C3 K1 C1 80.1(2) 3_455 . ? C3 K1 C1 114.2(2) 2_565 . ? C2 K1 C1 27.24(18) . . ? C2 K1 C1 62.78(19) 3_455 . ? C2 K1 C1 90.3(2) 2_565 . ? O1 K1 C1 140.81(13) . 3_455 ? C3 K1 C1 114.2(2) . 3_455 ? C3 K1 C1 48.36(19) 3_455 3_455 ? C3 K1 C1 80.1(2) 2_565 3_455 ? C2 K1 C1 90.3(2) . 3_455 ? C2 K1 C1 27.24(18) 3_455 3_455 ? C2 K1 C1 62.78(19) 2_565 3_455 ? C1 K1 C1 66.3(2) . 3_455 ? O1 K1 C1 140.81(13) . 2_565 ? C3 K1 C1 80.1(2) . 2_565 ? C3 K1 C1 114.2(2) 3_455 2_565 ? C3 K1 C1 48.36(19) 2_565 2_565 ? C2 K1 C1 62.78(19) . 2_565 ? C2 K1 C1 90.3(2) 3_455 2_565 ? C2 K1 C1 27.24(18) 2_565 2_565 ? C1 K1 C1 66.3(2) . 2_565 ? C1 K1 C1 66.3(2) 3_455 2_565 ? O1 K1 Sn1 180.000(1) . . ? C3 K1 Sn1 79.42(17) . . ? C3 K1 Sn1 79.42(17) 3_455 . ? C3 K1 Sn1 79.42(17) 2_565 . ? C2 K1 Sn1 54.75(16) . . ? C2 K1 Sn1 54.75(16) 3_455 . ? C2 K1 Sn1 54.75(16) 2_565 . ? C1 K1 Sn1 39.19(13) . . ? C1 K1 Sn1 39.19(13) 3_455 . ? C1 K1 Sn1 39.19(13) 2_565 . ? O1 K1 H1 129.9(14) . . ? C3 K1 H1 58.2(12) . . ? C3 K1 H1 62.5(13) 3_455 . ? C3 K1 H1 129.5(14) 2_565 . ? C2 K1 H1 43.5(13) . . ? C2 K1 H1 50.2(12) 3_455 . ? C2 K1 H1 104.8(14) 2_565 . ? C1 K1 H1 20.2(13) . . ? C1 K1 H1 63.3(13) 3_455 . ? C1 K1 H1 84.1(14) 2_565 . ? Sn1 K1 H1 50.1(14) . . ? O1 K1 H3 84.3(14) . . ? C3 K1 H3 23.1(14) . . ? C3 K1 H3 104.3(14) 3_455 . ? C3 K1 H3 136.7(14) 2_565 . ? C2 K1 H3 43.2(15) . . ? C2 K1 H3 105.6(14) 3_455 . ? C2 K1 H3 129.1(15) 2_565 . ? C1 K1 H3 58.2(14) . . ? C1 K1 H3 122.1(14) 3_455 . ? C1 K1 H3 103.1(15) 2_565 . ? Sn1 K1 H3 95.7(14) . . ? H1 K1 H3 58.9(19) . . ? C1 Sn1 C1 96.7(2) . 3_455 ? C1 Sn1 C1 96.7(2) . 2_565 ? C1 Sn1 C1 96.7(2) 3_455 2_565 ? C1 Sn1 K1 59.64(17) . . ? C1 Sn1 K1 59.64(17) 3_455 . ? C1 Sn1 K1 59.64(17) 2_565 . ? C5 Si1 C1 109.0(4) . . ? C5 Si1 C6 109.2(5) . . ? C1 Si1 C6 109.2(4) . . ? C5 Si1 C4 107.9(5) . . ? C1 Si1 C4 111.5(4) . . ? C6 Si1 C4 110.0(5) . . ? C7 Si2 C9 106.4(7) . . ? C7 Si2 C8 106.3(6) . . ? C9 Si2 C8 113.7(9) . . ? C7 Si2 C3 111.7(5) . . ? C9 Si2 C3 110.2(6) . . ? C8 Si2 C3 108.5(5) . . ? C2 C1 Si1 111.4(5) . . ? C2 C1 Sn1 109.3(5) . . ? Si1 C1 Sn1 105.5(3) . . ? C2 C1 K1 75.0(4) . . ? Si1 C1 K1 167.8(4) . . ? Sn1 C1 K1 81.18(19) . . ? C2 C1 H1 114(3) . . ? Si1 C1 H1 112(3) . . ? Sn1 C1 H1 104(3) . . ? K1 C1 H1 56(3) . . ? C3 C2 C1 129.9(8) . . ? C3 C2 K1 73.5(5) . . ? C1 C2 K1 77.8(4) . . ? C3 C2 H2 124(4) . . ? C1 C2 H2 106(4) . . ? K1 C2 H2 130(4) . . ? C2 C3 Si2 124.0(7) . . ? C2 C3 K1 81.8(5) . . ? Si2 C3 K1 121.9(4) . . ? C2 C3 H3 122(3) . . ? Si2 C3 H3 114(3) . . ? K1 C3 H3 66(3) . . ? 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 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 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 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 O1 C10 89.5(13) . 3_455 ? C10 O1 C10 89.5(13) . 2_565 ? C10 O1 C10 89.5(13) 3_455 2_565 ? C10 O1 K1 125.6(9) . . ? C10 O1 K1 125.6(9) 3_455 . ? C10 O1 K1 125.6(9) 2_565 . ? O1 C10 C11 111(2) . . ? O1 C10 C10 45.3(6) . 3_455 ? C11 C10 C10 74(2) . 3_455 ? O1 C10 C10 45.3(6) . 2_565 ? C11 C10 C10 81.3(13) . 2_565 ? C10 C10 C10 60.000(12) 3_455 2_565 ? C11 C11 C11 60.00(2) 2_565 3_455 ? C11 C11 C10 95(3) 2_565 . ? C11 C11 C10 106.2(17) 3_455 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 20.59 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.209 _refine_diff_density_min -0.147 _refine_diff_density_rms 0.038 # Attachment 'new_3tmeda3.cif' data_lf0703 _database_code_depnum_ccdc_archive 'CCDC 656894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H87 Li3 N6 Si4' _chemical_formula_sum 'C37 H87 Li3 N6 Si4' _chemical_formula_weight 749.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/nmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 33.6787(3) _cell_length_b 33.6787(3) _cell_length_c 11.17300(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12673.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 93908 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'square rod' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 0.116 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 54441 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5735 _reflns_number_gt 4518 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+12.4581P] 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 5735 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2419 _refine_ls_wR_factor_gt 0.2287 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.2500 0.48954(4) -0.17485(10) 0.0376(3) Uani 1 2 d S . . Si2 Si 0.10211(3) 0.51514(3) 0.08048(9) 0.0485(3) Uani 1 1 d . . . Si3 Si 0.2500 0.34304(5) -0.30468(19) 0.0788(6) Uani 1 2 d S . . Li1 Li 0.18354(16) 0.46715(19) -0.2887(5) 0.0537(14) Uani 1 1 d . A . Li2 Li 0.2500 0.4720(3) 0.0545(7) 0.062(2) Uani 1 2 d S . . N1 N 0.13837(10) 0.42801(12) -0.3383(4) 0.0835(11) Uani 1 1 d . . . N2 N 0.14619(9) 0.51303(11) -0.3658(3) 0.0714(10) Uani 1 1 d . . . N3 N 0.2500 0.5120(2) 0.2067(4) 0.0940(19) Uani 1 2 d S . . N4 N 0.2500 0.4264(2) 0.1714(6) 0.106(2) Uani 1 2 d S . . C1 C 0.2500 0.54557(15) -0.1819(5) 0.0606(13) Uani 1 2 d S . . H1A H 0.2704 0.5544 -0.1477 0.091 Uiso 0.50 1 calc PR A . H1B H 0.2500 0.5538 -0.2642 0.091 Uiso 1 2 d SR . . C2 C 0.20488(9) 0.47280(10) -0.0950(3) 0.0390(7) Uani 1 1 d . A . H2 H 0.2021(10) 0.4456(11) -0.092(3) 0.048(9) Uiso 1 1 d . . . C3 C 0.17441(8) 0.49568(10) -0.0413(3) 0.0395(7) Uani 1 1 d . . . H3 H 0.1776(9) 0.5265(10) -0.049(3) 0.046(9) Uiso 1 1 d . . . C4 C 0.14080(9) 0.48353(10) 0.0198(3) 0.0445(7) Uani 1 1 d . A . H4 H 0.1367(10) 0.4582(10) 0.031(3) 0.048(10) Uiso 1 1 d . . . C5 C 0.05385(11) 0.50956(13) -0.0014(4) 0.0697(11) Uani 1 1 d . . . H5A H 0.0578 0.5159 -0.0862 0.105 Uiso 1 1 calc R . . H5B H 0.0342 0.5277 0.0330 0.105 Uiso 1 1 calc R . . H5C H 0.0444 0.4822 0.0063 0.105 Uiso 1 1 calc R . . C6 C 0.11588(13) 0.56897(12) 0.0731(4) 0.0769(12) Uani 1 1 d . . . H6A H 0.1410 0.5732 0.1155 0.115 Uiso 1 1 calc R . . H6B H 0.0950 0.5849 0.1107 0.115 Uiso 1 1 calc R . . H6C H 0.1189 0.5770 -0.0108 0.115 Uiso 1 1 calc R . . C7 C 0.09176(13) 0.50261(14) 0.2413(4) 0.0751(12) Uani 1 1 d . . . H7A H 0.1163 0.5052 0.2880 0.113 Uiso 1 1 calc R . . H7B H 0.0820 0.4753 0.2468 0.113 Uiso 1 1 calc R . . H7C H 0.0717 0.5208 0.2730 0.113 Uiso 1 1 calc R . . C8 C 0.2500 0.46865(15) -0.3287(4) 0.0435(11) Uani 1 2 d S . . H8 H 0.2500 0.4812(16) -0.392(5) 0.059(16) Uiso 1 2 d S . . C9 C 0.2500 0.42778(16) -0.3519(4) 0.0469(12) Uani 1 2 d S . . H9 H 0.2500 0.4215(13) -0.423(4) 0.041(13) Uiso 1 2 d S . . C10 C 0.2500 0.39593(15) -0.2738(5) 0.0502(12) Uani 1 2 d S . . H10 H 0.2500 0.4013(12) -0.200(4) 0.032(11) Uiso 1 2 d S . . C11 C 0.2066(2) 0.31791(17) -0.2341(8) 0.152(3) Uani 1 1 d . . . H11A H 0.2071 0.3225 -0.1475 0.228 Uiso 1 1 calc R A . H11B H 0.2080 0.2893 -0.2499 0.228 Uiso 1 1 calc R . . H11C H 0.1820 0.3287 -0.2676 0.228 Uiso 1 1 calc R . . C12 C 0.2500 0.3341(3) -0.4711(9) 0.156(4) Uani 1 2 d S . . H12A H 0.2703 0.3444 -0.5016 0.234 Uiso 0.50 1 calc PR A . H12B H 0.2500 0.3061 -0.4874 0.234 Uiso 1 2 d SR . . C13 C 0.10599(18) 0.4540(2) -0.3736(10) 0.187(4) Uani 1 1 d . . . H13A H 0.0908 0.4402 -0.4369 0.281 Uiso 1 1 calc R . . H13B H 0.0881 0.4567 -0.3037 0.281 Uiso 1 1 calc R . . C14 C 0.11330(19) 0.4888(2) -0.4112(8) 0.151(3) Uani 1 1 d . . . H14A H 0.0888 0.5045 -0.3989 0.227 Uiso 1 1 calc R . . H14B H 0.1171 0.4866 -0.4988 0.227 Uiso 1 1 calc R . . C15 C 0.12693(15) 0.40538(16) -0.2336(5) 0.0954(16) Uani 1 1 d . . . H15A H 0.1059 0.3866 -0.2552 0.143 Uiso 1 1 calc R . . H15B H 0.1171 0.4235 -0.1716 0.143 Uiso 1 1 calc R . . H15C H 0.1500 0.3908 -0.2032 0.143 Uiso 1 1 calc R . . C16 C 0.14924(18) 0.3997(2) -0.4334(5) 0.117(2) Uani 1 1 d . . . H16A H 0.1265 0.3825 -0.4509 0.176 Uiso 1 1 calc R . . H16B H 0.1717 0.3835 -0.4067 0.176 Uiso 1 1 calc R . . H16C H 0.1567 0.4143 -0.5058 0.176 Uiso 1 1 calc R . . C17 C 0.16622(17) 0.5329(2) -0.4650(5) 0.127(3) Uani 1 1 d . . . H17A H 0.1487 0.5532 -0.4988 0.191 Uiso 1 1 calc R . . H17B H 0.1728 0.5133 -0.5268 0.191 Uiso 1 1 calc R . . H17C H 0.1906 0.5454 -0.4359 0.191 Uiso 1 1 calc R . . C18 C 0.13303(15) 0.54375(16) -0.2825(4) 0.0937(17) Uani 1 1 d . . . H18A H 0.1164 0.5630 -0.3250 0.141 Uiso 1 1 calc R . . H18B H 0.1562 0.5574 -0.2490 0.141 Uiso 1 1 calc R . . H18C H 0.1177 0.5315 -0.2177 0.141 Uiso 1 1 calc R . . C19 C 0.2328(4) 0.4471(5) 0.2830(9) 0.138(6) Uani 0.50 1 d P A -1 C20 C 0.2500 0.4824(5) 0.3031(8) 0.177(6) Uani 1 2 d S . . C21 C 0.2844(3) 0.4018(3) 0.1600(10) 0.233(6) Uani 1 1 d . . . H21A H 0.2829 0.3800 0.2178 0.350 Uiso 1 1 calc R A . H21B H 0.3082 0.4177 0.1755 0.350 Uiso 1 1 calc R . . H21C H 0.2856 0.3910 0.0787 0.350 Uiso 1 1 calc R . . C22 C 0.28518(16) 0.5375(2) 0.2115(6) 0.130(3) Uani 1 1 d . . . H22A H 0.2833 0.5552 0.2809 0.195 Uiso 1 1 calc R A . H22B H 0.2868 0.5534 0.1382 0.195 Uiso 1 1 calc R . . H22C H 0.3090 0.5210 0.2186 0.195 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0298(6) 0.0483(7) 0.0347(6) 0.0065(5) 0.000 0.000 Si2 0.0375(5) 0.0539(6) 0.0543(6) 0.0011(4) 0.0059(4) 0.0103(4) Si3 0.0752(11) 0.0568(10) 0.1043(14) -0.0108(9) 0.000 0.000 Li1 0.035(3) 0.076(4) 0.050(3) 0.009(3) -0.006(2) -0.001(3) Li2 0.051(5) 0.092(7) 0.043(4) 0.018(4) 0.000 0.000 N1 0.052(2) 0.097(3) 0.102(3) 0.010(2) -0.0316(19) -0.0111(19) N2 0.0529(19) 0.100(3) 0.062(2) 0.0200(19) -0.0054(16) 0.0217(18) N3 0.062(3) 0.166(6) 0.054(3) -0.027(3) 0.000 0.000 N4 0.074(4) 0.140(6) 0.104(5) 0.070(4) 0.000 0.000 C1 0.058(3) 0.050(3) 0.074(3) 0.017(3) 0.000 0.000 C2 0.0318(15) 0.0476(18) 0.0376(16) 0.0052(14) -0.0011(12) 0.0021(13) C3 0.0338(16) 0.0495(18) 0.0351(15) 0.0038(13) -0.0027(12) 0.0043(13) C4 0.0358(16) 0.0462(19) 0.0516(19) 0.0016(15) 0.0048(14) 0.0054(13) C5 0.043(2) 0.081(3) 0.085(3) -0.001(2) -0.0027(19) 0.0159(18) C6 0.068(3) 0.059(2) 0.104(3) -0.004(2) 0.009(2) 0.014(2) C7 0.077(3) 0.089(3) 0.059(2) -0.001(2) 0.022(2) 0.024(2) C8 0.040(2) 0.065(3) 0.026(2) 0.011(2) 0.000 0.000 C9 0.037(2) 0.074(4) 0.029(3) -0.006(2) 0.000 0.000 C10 0.053(3) 0.060(3) 0.037(3) -0.002(2) 0.000 0.000 C11 0.123(5) 0.073(4) 0.259(9) 0.028(5) 0.026(6) -0.024(3) C12 0.214(12) 0.125(8) 0.130(8) -0.074(7) 0.000 0.000 C13 0.069(4) 0.138(6) 0.355(13) 0.083(7) -0.103(6) -0.020(4) C14 0.087(4) 0.127(6) 0.240(9) 0.011(6) -0.105(5) 0.019(4) C15 0.075(3) 0.102(4) 0.109(4) -0.016(3) -0.001(3) -0.026(3) C16 0.096(4) 0.176(6) 0.079(3) -0.008(4) -0.024(3) -0.046(4) C17 0.111(4) 0.195(7) 0.076(3) 0.068(4) 0.025(3) 0.071(4) C18 0.091(3) 0.125(4) 0.066(3) 0.018(3) 0.000(2) 0.052(3) C19 0.160(13) 0.211(14) 0.044(5) 0.020(7) 0.015(5) -0.103(11) C20 0.251(17) 0.227(16) 0.053(5) 0.019(7) 0.000 0.000 C21 0.147(7) 0.248(11) 0.304(12) 0.211(10) 0.035(7) 0.084(7) C22 0.071(3) 0.208(7) 0.112(4) -0.075(5) 0.003(3) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C2 1.851(3) 14_655 ? Si1 C2 1.851(3) . ? Si1 C8 1.858(5) . ? Si1 C1 1.888(5) . ? Si1 Li2 2.630(8) . ? Si1 Li1 2.682(5) . ? Si1 Li1 2.682(5) 14_655 ? Si2 C4 1.814(3) . ? Si2 C6 1.873(4) . ? Si2 C5 1.875(4) . ? Si2 C7 1.878(4) . ? Si3 C10 1.815(5) . ? Si3 C11 1.863(6) 14_655 ? Si3 C11 1.863(6) . ? Si3 C12 1.884(9) . ? Li1 N1 2.088(7) . ? Li1 N2 2.171(7) . ? Li1 C8 2.283(5) . ? Li1 C2 2.289(6) . ? Li1 C9 2.696(6) . ? Li2 N4 2.017(10) . ? Li2 N3 2.169(11) . ? Li2 C2 2.258(7) . ? Li2 C2 2.258(7) 14_655 ? Li2 C19 2.749(12) 14_655 ? Li2 C19 2.749(12) . ? N1 C15 1.448(6) . ? N1 C13 1.453(7) . ? N1 C16 1.474(7) . ? N2 C17 1.459(6) . ? N2 C18 1.460(6) . ? N2 C14 1.466(7) . ? N3 C22 1.464(7) . ? N3 C22 1.464(7) 14_655 ? N3 C20 1.468(13) . ? N4 C21 1.428(9) 14_655 ? N4 C21 1.428(9) . ? N4 C19 1.542(15) . ? N4 C19 1.542(15) 14_655 ? C1 H1A 0.8400 . ? C1 H1B 0.9600 . ? C2 C3 1.416(4) . ? C2 H2 0.92(3) . ? C3 C4 1.384(4) . ? C3 H3 1.05(3) . ? C4 H4 0.87(3) . ? 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 C9 1.401(7) . ? C8 Li1 2.283(5) 14_655 ? C8 H8 0.82(6) . ? C9 C10 1.383(7) . ? C9 Li1 2.696(6) 14_655 ? C9 H9 0.83(5) . ? C10 H10 0.84(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.8400 . ? C12 H12B 0.9583 . ? C13 C14 1.268(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.340(16) . ? C20 C19 1.340(16) 14_655 ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 Si1 C2 110.42(19) 14_655 . ? C2 Si1 C8 109.33(13) 14_655 . ? C2 Si1 C8 109.33(13) . . ? C2 Si1 C1 108.95(14) 14_655 . ? C2 Si1 C1 108.95(14) . . ? C8 Si1 C1 109.8(2) . . ? C2 Si1 Li2 57.42(11) 14_655 . ? C2 Si1 Li2 57.42(11) . . ? C8 Si1 Li2 144.8(3) . . ? C1 Si1 Li2 105.4(3) . . ? C2 Si1 Li1 145.92(18) 14_655 . ? C2 Si1 Li1 57.17(15) . . ? C8 Si1 Li1 56.96(13) . . ? C1 Si1 Li1 105.13(17) . . ? Li2 Si1 Li1 113.50(16) . . ? C2 Si1 Li1 57.17(15) 14_655 14_655 ? C2 Si1 Li1 145.92(18) . 14_655 ? C8 Si1 Li1 56.96(13) . 14_655 ? C1 Si1 Li1 105.13(17) . 14_655 ? Li2 Si1 Li1 113.50(16) . 14_655 ? Li1 Si1 Li1 113.1(3) . 14_655 ? C4 Si2 C6 111.94(18) . . ? C4 Si2 C5 112.45(17) . . ? C6 Si2 C5 106.9(2) . . ? C4 Si2 C7 111.03(17) . . ? C6 Si2 C7 107.8(2) . . ? C5 Si2 C7 106.5(2) . . ? C10 Si3 C11 111.4(2) . 14_655 ? C10 Si3 C11 111.4(2) . . ? C11 Si3 C11 103.2(5) 14_655 . ? C10 Si3 C12 110.2(4) . . ? C11 Si3 C12 110.2(3) 14_655 . ? C11 Si3 C12 110.2(3) . . ? N1 Li1 N2 85.5(2) . . ? N1 Li1 C8 132.6(4) . . ? N2 Li1 C8 118.3(3) . . ? N1 Li1 C2 122.2(3) . . ? N2 Li1 C2 119.9(3) . . ? C8 Li1 C2 82.9(2) . . ? N1 Li1 Si1 155.7(3) . . ? N2 Li1 Si1 118.1(3) . . ? C8 Li1 Si1 43.01(15) . . ? C2 Li1 Si1 42.80(12) . . ? N1 Li1 C9 103.0(3) . . ? N2 Li1 C9 136.6(3) . . ? C8 Li1 C9 31.31(17) . . ? C2 Li1 C9 91.6(2) . . ? Si1 Li1 C9 64.53(15) . . ? N4 Li2 N3 88.0(4) . . ? N4 Li2 C2 119.2(4) . . ? N3 Li2 C2 124.9(4) . . ? N4 Li2 C2 119.2(4) . 14_655 ? N3 Li2 C2 124.9(4) . 14_655 ? C2 Li2 C2 84.6(3) . 14_655 ? N4 Li2 Si1 143.4(5) . . ? N3 Li2 Si1 128.7(5) . . ? C2 Li2 Si1 43.67(16) . . ? C2 Li2 Si1 43.67(16) 14_655 . ? N4 Li2 C19 33.5(4) . 14_655 ? N3 Li2 C19 57.4(4) . 14_655 ? C2 Li2 C19 146.3(4) . 14_655 ? C2 Li2 C19 123.3(3) 14_655 14_655 ? Si1 Li2 C19 166.8(3) . 14_655 ? N4 Li2 C19 33.5(4) . . ? N3 Li2 C19 57.4(4) . . ? C2 Li2 C19 123.3(3) . . ? C2 Li2 C19 146.3(4) 14_655 . ? Si1 Li2 C19 166.8(3) . . ? C19 Li2 C19 24.3(6) 14_655 . ? C15 N1 C13 109.7(5) . . ? C15 N1 C16 107.9(4) . . ? C13 N1 C16 112.4(6) . . ? C15 N1 Li1 108.1(3) . . ? C13 N1 Li1 103.8(4) . . ? C16 N1 Li1 114.8(3) . . ? C17 N2 C18 107.5(4) . . ? C17 N2 C14 110.0(5) . . ? C18 N2 C14 112.7(5) . . ? C17 N2 Li1 111.1(3) . . ? C18 N2 Li1 115.3(3) . . ? C14 N2 Li1 100.3(4) . . ? C22 N3 C22 108.0(8) . 14_655 ? C22 N3 C20 111.8(5) . . ? C22 N3 C20 111.8(5) 14_655 . ? C22 N3 Li2 113.1(3) . . ? C22 N3 Li2 113.1(3) 14_655 . ? C20 N3 Li2 98.8(7) . . ? C21 N4 C21 108.3(11) 14_655 . ? C21 N4 C19 91.7(7) 14_655 . ? C21 N4 C19 129.7(8) . . ? C21 N4 C19 129.7(8) 14_655 14_655 ? C21 N4 C19 91.7(7) . 14_655 ? C19 N4 C19 44.1(10) . 14_655 ? C21 N4 Li2 112.5(4) 14_655 . ? C21 N4 Li2 112.5(4) . . ? C19 N4 Li2 100.3(7) . . ? C19 N4 Li2 100.3(7) 14_655 . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.1 . . ? H1A C1 H1B 109.6 . . ? C3 C2 Si1 129.3(3) . . ? C3 C2 Li2 100.4(3) . . ? Si1 C2 Li2 78.91(18) . . ? C3 C2 Li1 102.6(2) . . ? Si1 C2 Li1 80.03(18) . . ? Li2 C2 Li1 155.5(3) . . ? C3 C2 H2 117(2) . . ? Si1 C2 H2 114(2) . . ? Li2 C2 H2 92(2) . . ? Li1 C2 H2 86(2) . . ? C4 C3 C2 129.8(3) . . ? C4 C3 H3 114.8(17) . . ? C2 C3 H3 115.4(17) . . ? C3 C4 Si2 126.8(3) . . ? C3 C4 H4 119(2) . . ? Si2 C4 H4 114(2) . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 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 . . ? C9 C8 Si1 122.9(4) . . ? C9 C8 Li1 90.8(2) . 14_655 ? Si1 C8 Li1 80.04(19) . 14_655 ? C9 C8 Li1 90.8(2) . . ? Si1 C8 Li1 80.04(19) . . ? Li1 C8 Li1 157.2(4) 14_655 . ? C9 C8 H8 110(4) . . ? Si1 C8 H8 127(4) . . ? Li1 C8 H8 100.3(4) 14_655 . ? Li1 C8 H8 100.3(4) . . ? C10 C9 C8 130.2(5) . . ? C10 C9 Li1 102.5(2) . 14_655 ? C8 C9 Li1 57.87(17) . 14_655 ? C10 C9 Li1 102.5(2) . . ? C8 C9 Li1 57.87(17) . . ? Li1 C9 Li1 112.2(3) 14_655 . ? C10 C9 H9 114(3) . . ? C8 C9 H9 115(3) . . ? Li1 C9 H9 112.2(14) 14_655 . ? Li1 C9 H9 112.2(14) . . ? C9 C10 Si3 129.9(4) . . ? C9 C10 H10 117(3) . . ? Si3 C10 H10 113(3) . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 110.1 . . ? H12A C12 H12B 109.3 . . ? C14 C13 N1 120.1(6) . . ? C14 C13 H13A 107.3 . . ? N1 C13 H13A 107.3 . . ? C14 C13 H13B 107.3 . . ? N1 C13 H13B 107.3 . . ? H13A C13 H13B 106.9 . . ? C13 C14 N2 123.1(5) . . ? C13 C14 H14A 106.6 . . ? N2 C14 H14A 106.6 . . ? C13 C14 H14B 106.6 . . ? N2 C14 H14B 106.6 . . ? H14A C14 H14B 106.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 N4 112.0(8) . . ? C20 C19 Li2 78.1(7) . . ? N4 C19 Li2 46.2(4) . . ? C19 C20 C19 51.2(15) 14_655 . ? C19 C20 N3 118.6(9) 14_655 . ? C19 C20 N3 118.6(9) . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.516 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.058