Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dominic S. Wright' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UK ; _publ_contact_author_email DSW1000@CUS.CAM.AC.UK _publ_section_title ; Bonding versus Oligomerisation in the Aromatic Anions [C6H4N2E] : Formation of the Cyclic Tetrameric Tetraanion [C6H4N2Sb]44 ; loop_ _publ_author_name 'Dominic S. Wright' 'Felipe Garcia' 'Robert J. Less' 'M. McPartlin' 'Vesal Naseri' 'J. Rawson' data_dw0735 _database_code_depnum_ccdc_archive 'CCDC 662877' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H108 Li4 N20 Sb4' _chemical_formula_weight 1624.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 tetragonal _symmetry_space_group_name_H-M i41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 18.9905(9) _cell_length_b 18.9905(9) _cell_length_c 30.5264(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11009.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 18298 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3296 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.709 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_reflns_number 12239 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4492 _reflns_number_gt 3613 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _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^)+(0.0937P)^2^+24.5678P] 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 4492 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1939 _refine_ls_wR_factor_gt 0.1705 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_restrained_S_all 1.256 _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 Sb1 Sb 0.49820(2) -0.14257(2) 0.589478(12) 0.0571(2) Uani 1 1 d . . . Li1 Li 0.5967(7) 0.0141(6) 0.5945(4) 0.081(3) Uani 1 1 d . . . N1 N 0.5311(3) -0.0524(3) 0.61783(19) 0.0730(14) Uani 1 1 d . . . N2 N 0.4615(3) -0.1674(3) 0.65039(16) 0.0588(11) Uani 1 1 d . . . N3 N 0.5541(5) 0.1175(3) 0.5859(2) 0.096(2) Uani 1 1 d . . . N4 N 0.6432(4) 0.0285(4) 0.5301(2) 0.097(2) Uani 1 1 d . . . N5 N 0.7021(4) 0.0045(4) 0.6165(2) 0.100(2) Uani 1 1 d . . . C1 C 0.5153(4) -0.0547(3) 0.6613(2) 0.0665(16) Uani 1 1 d . . . C2 C 0.4769(3) -0.1136(3) 0.6800(2) 0.0596(13) Uani 1 1 d . . . C3 C 0.4576(4) -0.1131(4) 0.7236(2) 0.0700(16) Uani 1 1 d . . . H3 H 0.4320 -0.1517 0.7353 0.084 Uiso 1 1 calc R . . C4 C 0.4752(4) -0.0565(4) 0.7510(3) 0.086(2) Uani 1 1 d . . . H4 H 0.4613 -0.0568 0.7809 0.103 Uiso 1 1 calc R . . C5 C 0.5128(5) -0.0003(4) 0.7345(3) 0.093(2) Uani 1 1 d . . . H5 H 0.5247 0.0380 0.7531 0.111 Uiso 1 1 calc R . . C6 C 0.5335(5) 0.0006(4) 0.6910(3) 0.089(2) Uani 1 1 d . . . H6 H 0.5605 0.0392 0.6806 0.106 Uiso 1 1 calc R . . C11 C 0.5615(6) 0.1286(5) 0.5389(3) 0.108(3) Uani 1 1 d . . . H11A H 0.5548 0.1792 0.5321 0.130 Uiso 1 1 calc R . . H11B H 0.5246 0.1017 0.5232 0.130 Uiso 1 1 calc R . . C12 C 0.6323(6) 0.1056(5) 0.5235(3) 0.109(3) Uani 1 1 d . . . H12A H 0.6691 0.1319 0.5396 0.131 Uiso 1 1 calc R . . H12B H 0.6373 0.1168 0.4919 0.131 Uiso 1 1 calc R . . C13 C 0.7163(5) 0.0085(6) 0.5344(3) 0.112(3) Uani 1 1 d . . . H13A H 0.7440 0.0310 0.5108 0.134 Uiso 1 1 calc R . . H13B H 0.7206 -0.0431 0.5310 0.134 Uiso 1 1 calc R . . C14 C 0.7468(6) 0.0306(6) 0.5793(3) 0.117(3) Uani 1 1 d . . . H14A H 0.7950 0.0115 0.5824 0.140 Uiso 1 1 calc R . . H14B H 0.7498 0.0826 0.5807 0.140 Uiso 1 1 calc R . . C15 C 0.5893(8) 0.1719(5) 0.6117(4) 0.145(5) Uani 1 1 d . . . H15A H 0.6393 0.1737 0.6038 0.218 Uiso 1 1 calc R . . H15B H 0.5848 0.1608 0.6430 0.218 Uiso 1 1 calc R . . H15C H 0.5675 0.2177 0.6058 0.218 Uiso 1 1 calc R . . C16 C 0.4809(7) 0.1148(5) 0.5975(4) 0.120(3) Uani 1 1 d . . . H16A H 0.4764 0.1074 0.6292 0.181 Uiso 1 1 calc R . . H16B H 0.4581 0.0758 0.5819 0.181 Uiso 1 1 calc R . . H16C H 0.4581 0.1592 0.5895 0.181 Uiso 1 1 calc R . . C17 C 0.6138(5) -0.0128(5) 0.4940(3) 0.107(3) Uani 1 1 d . . . H17A H 0.5640 -0.0006 0.4900 0.160 Uiso 1 1 calc R . . H17B H 0.6179 -0.0631 0.5007 0.160 Uiso 1 1 calc R . . H17C H 0.6397 -0.0024 0.4670 0.160 Uiso 1 1 calc R . . C18 C 0.7246(6) 0.0386(6) 0.6576(3) 0.124(4) Uani 1 1 d . . . H18A H 0.7190 0.0897 0.6550 0.185 Uiso 1 1 calc R . . H18B H 0.7741 0.0273 0.6633 0.185 Uiso 1 1 calc R . . H18C H 0.6955 0.0213 0.6819 0.185 Uiso 1 1 calc R . . C19 C 0.7107(5) -0.0728(5) 0.6208(3) 0.110(3) Uani 1 1 d . . . H19A H 0.6960 -0.0958 0.5936 0.165 Uiso 1 1 calc R . . H19B H 0.6817 -0.0899 0.6451 0.165 Uiso 1 1 calc R . . H19C H 0.7603 -0.0838 0.6267 0.165 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 Sb1 0.0608(3) 0.0544(3) 0.0560(3) 0.00692(15) -0.00177(16) 0.00105(16) Li1 0.099(9) 0.058(6) 0.086(7) 0.008(5) -0.010(6) -0.009(6) N1 0.084(4) 0.052(3) 0.083(4) 0.007(3) -0.001(3) -0.005(2) N2 0.061(3) 0.061(3) 0.054(2) 0.002(2) 0.002(2) 0.002(2) N3 0.132(6) 0.058(3) 0.097(5) 0.009(3) -0.018(4) -0.013(4) N4 0.106(5) 0.094(5) 0.090(4) 0.032(4) -0.018(4) -0.030(4) N5 0.106(5) 0.112(5) 0.083(4) 0.021(4) -0.024(4) -0.044(4) C1 0.077(4) 0.046(3) 0.076(4) 0.000(3) -0.008(3) 0.007(3) C2 0.061(3) 0.054(3) 0.064(3) -0.004(3) -0.001(3) 0.008(3) C3 0.068(4) 0.071(4) 0.071(4) -0.006(3) 0.001(3) 0.009(3) C4 0.090(5) 0.088(5) 0.079(4) -0.018(4) 0.006(4) 0.019(4) C5 0.110(6) 0.079(5) 0.090(5) -0.025(4) -0.014(5) 0.016(4) C6 0.111(6) 0.050(4) 0.104(6) -0.003(4) -0.010(5) 0.001(4) C11 0.139(9) 0.074(5) 0.111(7) 0.033(5) -0.022(6) -0.018(5) C12 0.149(9) 0.091(6) 0.089(5) 0.042(5) -0.023(6) -0.044(6) C13 0.111(7) 0.137(8) 0.086(6) 0.027(5) 0.004(5) -0.030(6) C14 0.112(7) 0.129(8) 0.109(7) 0.037(6) -0.012(5) -0.043(6) C15 0.225(13) 0.057(5) 0.153(9) 0.004(5) -0.059(9) -0.019(6) C16 0.156(10) 0.072(5) 0.134(8) 0.011(5) -0.012(7) 0.016(6) C17 0.135(8) 0.105(6) 0.080(5) 0.017(5) -0.010(5) -0.034(6) C18 0.148(9) 0.125(8) 0.098(6) 0.005(5) -0.025(6) -0.044(7) C19 0.114(7) 0.098(6) 0.119(7) 0.035(5) -0.030(6) -0.028(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 Sb1 N1 2.017(5) . ? Sb1 N2 2.040(5) . ? Sb1 N2 2.094(5) 15_656 ? Li1 N1 1.912(13) . ? Li1 N5 2.118(15) . ? Li1 N3 2.140(14) . ? Li1 N4 2.173(15) . ? N1 C1 1.360(8) . ? N2 C2 1.394(8) . ? N2 Sb1 2.094(5) 16_546 ? N3 C16 1.437(13) . ? N3 C11 1.456(11) . ? N3 C15 1.462(11) . ? N4 C13 1.444(12) . ? N4 C17 1.465(10) . ? N4 C12 1.492(11) . ? N5 C18 1.475(11) . ? N5 C19 1.483(11) . ? N5 C14 1.502(11) . ? C1 C6 1.430(9) . ? C1 C2 1.454(9) . ? C2 C3 1.380(9) . ? C3 C4 1.402(10) . ? C3 H3 0.9500 . ? C4 C5 1.378(12) . ? C4 H4 0.9500 . ? C5 C6 1.385(11) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C11 C12 1.491(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.545(12) . ? 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 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 N1 Sb1 N2 84.9(2) . . ? N1 Sb1 N2 103.3(2) . 15_656 ? N2 Sb1 N2 89.0(2) . 15_656 ? N1 Li1 N5 116.1(6) . . ? N1 Li1 N3 114.0(8) . . ? N5 Li1 N3 118.4(6) . . ? N1 Li1 N4 133.2(7) . . ? N5 Li1 N4 85.0(6) . . ? N3 Li1 N4 85.8(5) . . ? C1 N1 Li1 121.8(6) . . ? C1 N1 Sb1 108.9(4) . . ? Li1 N1 Sb1 127.1(5) . . ? C2 N2 Sb1 110.6(4) . . ? C2 N2 Sb1 126.5(4) . 16_546 ? Sb1 N2 Sb1 121.6(2) . 16_546 ? C16 N3 C11 110.0(8) . . ? C16 N3 C15 109.6(9) . . ? C11 N3 C15 112.7(8) . . ? C16 N3 Li1 107.6(6) . . ? C11 N3 Li1 102.6(7) . . ? C15 N3 Li1 114.1(7) . . ? C13 N4 C17 107.1(8) . . ? C13 N4 C12 113.8(7) . . ? C17 N4 C12 111.7(7) . . ? C13 N4 Li1 106.0(6) . . ? C17 N4 Li1 117.3(6) . . ? C12 N4 Li1 100.9(7) . . ? C18 N5 C19 109.0(7) . . ? C18 N5 C14 109.6(7) . . ? C19 N5 C14 109.4(8) . . ? C18 N5 Li1 120.4(8) . . ? C19 N5 Li1 102.6(6) . . ? C14 N5 Li1 105.4(6) . . ? N1 C1 C6 122.9(6) . . ? N1 C1 C2 121.2(5) . . ? C6 C1 C2 115.9(6) . . ? C3 C2 N2 125.2(6) . . ? C3 C2 C1 120.4(6) . . ? N2 C2 C1 114.4(5) . . ? C2 C3 C4 121.2(7) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.9(7) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.5(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 122.1(7) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? N3 C11 C12 110.8(8) . . ? N3 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C11 C12 N4 111.7(7) . . ? C11 C12 H12A 109.3 . . ? N4 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? N4 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N4 C13 C14 111.7(9) . . ? N4 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N4 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N5 C14 C13 111.7(7) . . ? N5 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? N5 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 H17A 109.5 . . ? N4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 H18A 109.5 . . ? N5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 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 N5 Li1 N1 C1 63.9(10) . . . . ? N3 Li1 N1 C1 -79.0(8) . . . . ? N4 Li1 N1 C1 173.1(8) . . . . ? N5 Li1 N1 Sb1 -97.2(7) . . . . ? N3 Li1 N1 Sb1 119.9(6) . . . . ? N4 Li1 N1 Sb1 12.0(13) . . . . ? N2 Sb1 N1 C1 2.1(4) . . . . ? N2 Sb1 N1 C1 -85.7(5) 15_656 . . . ? N2 Sb1 N1 Li1 165.1(6) . . . . ? N2 Sb1 N1 Li1 77.4(6) 15_656 . . . ? N1 Sb1 N2 C2 -0.6(4) . . . . ? N2 Sb1 N2 C2 102.9(5) 15_656 . . . ? N1 Sb1 N2 Sb1 167.4(3) . . . 16_546 ? N2 Sb1 N2 Sb1 -89.16(12) 15_656 . . 16_546 ? N1 Li1 N3 C16 -3.3(9) . . . . ? N5 Li1 N3 C16 -145.3(8) . . . . ? N4 Li1 N3 C16 132.7(7) . . . . ? N1 Li1 N3 C11 -119.3(8) . . . . ? N5 Li1 N3 C11 98.7(8) . . . . ? N4 Li1 N3 C11 16.7(7) . . . . ? N1 Li1 N3 C15 118.5(10) . . . . ? N5 Li1 N3 C15 -23.5(11) . . . . ? N4 Li1 N3 C15 -105.5(9) . . . . ? N1 Li1 N4 C13 -109.1(11) . . . . ? N5 Li1 N4 C13 12.5(7) . . . . ? N3 Li1 N4 C13 131.5(7) . . . . ? N1 Li1 N4 C17 10.4(13) . . . . ? N5 Li1 N4 C17 132.0(7) . . . . ? N3 Li1 N4 C17 -109.0(7) . . . . ? N1 Li1 N4 C12 132.0(10) . . . . ? N5 Li1 N4 C12 -106.3(6) . . . . ? N3 Li1 N4 C12 12.7(7) . . . . ? N1 Li1 N5 C18 -85.5(9) . . . . ? N3 Li1 N5 C18 55.7(10) . . . . ? N4 Li1 N5 C18 138.2(7) . . . . ? N1 Li1 N5 C19 35.7(9) . . . . ? N3 Li1 N5 C19 176.9(7) . . . . ? N4 Li1 N5 C19 -100.6(6) . . . . ? N1 Li1 N5 C14 150.2(8) . . . . ? N3 Li1 N5 C14 -68.6(9) . . . . ? N4 Li1 N5 C14 13.9(7) . . . . ? Li1 N1 C1 C6 14.1(11) . . . . ? Sb1 N1 C1 C6 178.3(6) . . . . ? Li1 N1 C1 C2 -167.5(7) . . . . ? Sb1 N1 C1 C2 -3.4(8) . . . . ? Sb1 N2 C2 C3 178.1(5) . . . . ? Sb1 N2 C2 C3 10.9(9) 16_546 . . . ? Sb1 N2 C2 C1 -1.0(6) . . . . ? Sb1 N2 C2 C1 -168.2(4) 16_546 . . . ? N1 C1 C2 C3 -176.1(6) . . . . ? C6 C1 C2 C3 2.4(9) . . . . ? N1 C1 C2 N2 3.0(9) . . . . ? C6 C1 C2 N2 -178.5(6) . . . . ? N2 C2 C3 C4 -179.8(6) . . . . ? C1 C2 C3 C4 -0.8(10) . . . . ? C2 C3 C4 C5 -0.4(11) . . . . ? C3 C4 C5 C6 -0.1(12) . . . . ? C4 C5 C6 C1 1.9(13) . . . . ? N1 C1 C6 C5 175.5(7) . . . . ? C2 C1 C6 C5 -2.9(11) . . . . ? C16 N3 C11 C12 -158.9(7) . . . . ? C15 N3 C11 C12 78.5(11) . . . . ? Li1 N3 C11 C12 -44.7(9) . . . . ? N3 C11 C12 N4 63.0(10) . . . . ? C13 N4 C12 C11 -154.3(8) . . . . ? C17 N4 C12 C11 84.2(9) . . . . ? Li1 N4 C12 C11 -41.2(9) . . . . ? C17 N4 C13 C14 -162.6(7) . . . . ? C12 N4 C13 C14 73.4(9) . . . . ? Li1 N4 C13 C14 -36.6(9) . . . . ? C18 N5 C14 C13 -168.5(10) . . . . ? C19 N5 C14 C13 72.1(11) . . . . ? Li1 N5 C14 C13 -37.7(11) . . . . ? N4 C13 C14 N5 52.7(12) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.696 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.096