# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1872 data_(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Li2 N6' _chemical_formula_weight 514.52 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.104(3) _cell_length_b 11.5602(16) _cell_length_c 14.2505(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2982.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 6745 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 24.45 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12310 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.61 _reflns_number_total 4291 _reflns_number_gt 3767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0700P)^2^+1.4354P] 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 SHELXL _refine_ls_extinction_coef 0.0060(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -1(3) _refine_ls_number_reflns 4291 _refine_ls_number_parameters 368 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1514 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 Li1 Li 0.0844(3) -0.0547(5) 0.2525(4) 0.0528(14) Uani 1 1 d . . . Li2 Li 0.1980(3) 0.0013(5) 0.1614(4) 0.0476(13) Uani 1 1 d . . . N1 N 0.1154(2) -0.1056(3) 0.1229(2) 0.0714(10) Uani 1 1 d D . . H1N H 0.085(2) -0.070(4) 0.082(3) 0.086 Uiso 1 1 d D . . C1 C 0.1165(2) -0.2125(3) 0.0791(3) 0.0570(10) Uani 1 1 d . . . C2 C 0.0761(2) -0.2348(3) 0.0005(3) 0.0600(10) Uani 1 1 d . . . H2 H 0.0463 -0.1745 -0.0243 0.072 Uiso 1 1 calc R . . C3 C 0.0761(2) -0.3391(4) -0.0445(3) 0.0648(11) Uani 1 1 d . . . H3 H 0.0474 -0.3482 -0.0998 0.078 Uiso 1 1 calc R . . C4 C 0.1167(3) -0.4316(4) -0.0118(4) 0.0695(13) Uani 1 1 d . . . H4 H 0.1159 -0.5047 -0.0422 0.083 Uiso 1 1 calc R . . C5 C 0.1594(2) -0.4121(4) 0.0689(4) 0.0725(14) Uani 1 1 d . . . H5 H 0.1892 -0.4722 0.0940 0.087 Uiso 1 1 calc R . . C6 C 0.1579(2) -0.3035(5) 0.1121(3) 0.0693(13) Uani 1 1 d . . . H6 H 0.1870 -0.2921 0.1669 0.083 Uiso 1 1 calc R . . N2 N 0.16217(17) 0.0604(2) 0.28889(19) 0.0511(7) Uani 1 1 d D . . H2N H 0.1912(17) 0.029(3) 0.3333(19) 0.061 Uiso 1 1 d D . . C7 C 0.16102(18) 0.1779(3) 0.2995(3) 0.0470(8) Uani 1 1 d . . . C8 C 0.11967(19) 0.2459(4) 0.2375(4) 0.0718(13) Uani 1 1 d . . . H8 H 0.0912 0.2089 0.1903 0.086 Uiso 1 1 calc R . . C9 C 0.1191(3) 0.3653(5) 0.2428(7) 0.117(3) Uani 1 1 d . . . H9 H 0.0908 0.4086 0.1989 0.140 Uiso 1 1 calc R . . C10 C 0.1588(5) 0.4218(5) 0.3107(8) 0.134(4) Uani 1 1 d . . . H10 H 0.1575 0.5038 0.3150 0.161 Uiso 1 1 calc R . . C11 C 0.2005(4) 0.3579(5) 0.3726(5) 0.111(2) Uani 1 1 d . . . H11 H 0.2289 0.3965 0.4191 0.134 Uiso 1 1 calc R . . C12 C 0.2018(3) 0.2383(4) 0.3683(3) 0.0668(11) Uani 1 1 d . . . H12 H 0.2306 0.1962 0.4123 0.080 Uiso 1 1 calc R . . N3 N 0.06217(17) -0.1683(3) 0.3609(2) 0.0530(8) Uani 1 1 d . . . C13 C 0.0627(2) -0.2840(3) 0.3554(3) 0.0647(11) Uani 1 1 d . . . H13 H 0.0769 -0.3190 0.2978 0.078 Uiso 1 1 calc R . . C14 C 0.0438(3) -0.3542(4) 0.4293(4) 0.0830(14) Uani 1 1 d . . . H14 H 0.0465 -0.4360 0.4236 0.100 Uiso 1 1 calc R . . C15 C 0.0210(4) -0.3045(5) 0.5106(4) 0.1018(19) Uani 1 1 d . . . H15 H 0.0061 -0.3511 0.5621 0.122 Uiso 1 1 calc R . . C16 C 0.0199(3) -0.1859(4) 0.5176(3) 0.0920(17) Uani 1 1 d . . . H16 H 0.0045 -0.1491 0.5738 0.110 Uiso 1 1 calc R . . C17 C 0.0414(3) -0.1231(4) 0.4425(3) 0.0698(12) Uani 1 1 d . . . H17 H 0.0416 -0.0413 0.4484 0.084 Uiso 1 1 calc R . . N4 N 0.20943(16) 0.1136(3) 0.0461(2) 0.0557(8) Uani 1 1 d . . . C18 C 0.1753(3) 0.1026(4) -0.0331(3) 0.0754(13) Uani 1 1 d . . . H18 H 0.1432 0.0384 -0.0409 0.091 Uiso 1 1 calc R . . C19 C 0.1831(4) 0.1792(6) -0.1074(4) 0.112(2) Uani 1 1 d . . . H19 H 0.1572 0.1662 -0.1644 0.135 Uiso 1 1 calc R . . C20 C 0.2275(3) 0.2726(4) -0.0984(4) 0.0818(14) Uani 1 1 d . . . H20 H 0.2334 0.3266 -0.1480 0.098 Uiso 1 1 calc R . . C21 C 0.2621(3) 0.2854(5) -0.0185(4) 0.0924(17) Uani 1 1 d . . . H21 H 0.2934 0.3503 -0.0088 0.111 Uiso 1 1 calc R . . C22 C 0.2529(3) 0.2044(5) 0.0516(4) 0.0967(18) Uani 1 1 d . . . H22 H 0.2800 0.2151 0.1080 0.116 Uiso 1 1 calc R . . N5 N 0.30651(16) -0.0537(3) 0.1770(2) 0.0528(8) Uani 1 1 d . . . C23 C 0.3317(2) -0.1252(3) 0.1118(3) 0.0597(10) Uani 1 1 d . . . H23 H 0.2968 -0.1674 0.0758 0.072 Uiso 1 1 calc R . . C24 C 0.4058(2) -0.1419(3) 0.0932(3) 0.0560(10) Uani 1 1 d . . . H24 H 0.4211 -0.1909 0.0434 0.067 Uiso 1 1 calc R . . C25 C 0.4564(2) -0.0871(4) 0.1474(3) 0.0592(10) Uani 1 1 d . . . H25 H 0.5078 -0.0982 0.1377 0.071 Uiso 1 1 calc R . . C26 C 0.4308(2) -0.0145(4) 0.2172(3) 0.0621(10) Uani 1 1 d . . . H26 H 0.4646 0.0249 0.2570 0.074 Uiso 1 1 calc R . . C27 C 0.35635(19) 0.0004(3) 0.2287(3) 0.0553(9) Uani 1 1 d . . . H27 H 0.3397 0.0519 0.2761 0.066 Uiso 1 1 calc R . . N6 N -0.02217(16) 0.0058(3) 0.2262(2) 0.0575(8) Uani 1 1 d . . . C28 C -0.0525(2) 0.0969(4) 0.2695(3) 0.0616(10) Uani 1 1 d . . . H28 H -0.0221 0.1426 0.3093 0.074 Uiso 1 1 calc R . . C29 C -0.1254(2) 0.1278(4) 0.2594(3) 0.0690(11) Uani 1 1 d . . . H29 H -0.1450 0.1935 0.2908 0.083 Uiso 1 1 calc R . . C30 C -0.1691(2) 0.0608(5) 0.2023(3) 0.0749(13) Uani 1 1 d . . . H30 H -0.2198 0.0793 0.1946 0.090 Uiso 1 1 calc R . . C31 C -0.1397(2) -0.0326(4) 0.1567(4) 0.0744(13) Uani 1 1 d . . . H31 H -0.1692 -0.0790 0.1164 0.089 Uiso 1 1 calc R . . C32 C -0.0662(2) -0.0572(4) 0.1708(3) 0.0673(11) Uani 1 1 d . . . H32 H -0.0457 -0.1223 0.1396 0.081 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 Li1 0.057(3) 0.056(4) 0.045(3) 0.000(3) 0.002(3) -0.006(3) Li2 0.053(3) 0.051(3) 0.039(3) -0.001(3) 0.006(2) -0.007(2) N1 0.076(2) 0.073(3) 0.065(2) -0.011(2) 0.0073(19) -0.0114(18) C1 0.057(2) 0.054(2) 0.060(3) -0.007(2) 0.0215(19) -0.0146(18) C2 0.074(3) 0.049(2) 0.057(3) 0.004(2) 0.018(2) -0.0060(18) C3 0.082(3) 0.073(3) 0.039(2) 0.002(2) 0.0049(19) -0.021(2) C4 0.093(3) 0.043(2) 0.072(3) -0.012(2) 0.035(2) -0.013(2) C5 0.053(2) 0.078(3) 0.086(3) 0.035(3) 0.023(2) 0.012(2) C6 0.051(2) 0.112(4) 0.044(2) -0.008(2) 0.0059(18) -0.034(2) N2 0.0631(19) 0.0393(17) 0.051(2) -0.0031(15) -0.0106(14) 0.0018(13) C7 0.0423(17) 0.047(2) 0.052(2) -0.0015(18) 0.0130(15) -0.0011(14) C8 0.0422(19) 0.068(3) 0.106(4) 0.028(3) 0.003(2) 0.0046(17) C9 0.066(3) 0.067(4) 0.217(9) 0.064(5) 0.051(4) 0.022(2) C10 0.152(6) 0.040(3) 0.210(9) 0.000(4) 0.120(7) -0.003(4) C11 0.163(6) 0.073(4) 0.098(4) -0.041(4) 0.070(4) -0.061(4) C12 0.087(3) 0.062(3) 0.051(2) -0.008(2) 0.020(2) -0.021(2) N3 0.0669(19) 0.0502(18) 0.0419(18) -0.0001(15) 0.0020(14) -0.0057(14) C13 0.086(3) 0.051(2) 0.058(3) -0.009(2) 0.007(2) -0.0065(19) C14 0.133(4) 0.044(2) 0.072(3) 0.002(2) 0.019(3) -0.011(2) C15 0.170(6) 0.071(3) 0.065(3) 0.016(3) 0.032(3) -0.010(3) C16 0.158(5) 0.072(3) 0.045(3) -0.006(2) 0.026(3) -0.009(3) C17 0.105(3) 0.048(2) 0.056(3) -0.004(2) 0.006(2) -0.005(2) N4 0.0560(17) 0.065(2) 0.0463(18) 0.0031(16) 0.0013(15) -0.0055(15) C18 0.097(3) 0.062(3) 0.067(3) -0.002(2) -0.016(3) -0.009(2) C19 0.176(6) 0.101(4) 0.060(3) 0.018(3) -0.043(4) -0.012(4) C20 0.117(4) 0.068(3) 0.060(3) 0.019(2) 0.009(3) 0.012(3) C21 0.096(4) 0.101(4) 0.081(4) 0.035(3) 0.004(3) -0.027(3) C22 0.102(4) 0.109(4) 0.079(3) 0.036(3) -0.029(3) -0.054(3) N5 0.0534(17) 0.059(2) 0.0464(18) -0.0044(16) 0.0076(14) 0.0020(14) C23 0.059(2) 0.061(2) 0.058(2) -0.002(2) 0.0048(19) -0.0048(18) C24 0.064(2) 0.053(2) 0.051(2) -0.0024(18) 0.0096(18) 0.0052(18) C25 0.052(2) 0.075(3) 0.051(2) 0.004(2) 0.0066(17) 0.0138(18) C26 0.054(2) 0.083(3) 0.049(2) -0.009(2) -0.0017(19) -0.0012(19) C27 0.056(2) 0.063(2) 0.047(2) -0.0052(19) 0.0027(19) 0.0035(18) N6 0.0546(17) 0.064(2) 0.0542(19) 0.0068(17) 0.0046(16) -0.0097(15) C28 0.061(2) 0.076(3) 0.048(2) -0.004(2) 0.0051(18) -0.0048(19) C29 0.061(2) 0.083(3) 0.063(3) -0.012(2) 0.012(2) -0.004(2) C30 0.047(2) 0.100(4) 0.078(3) -0.001(3) 0.004(2) -0.006(2) C31 0.055(2) 0.080(3) 0.088(4) -0.011(3) -0.003(2) -0.018(2) C32 0.062(2) 0.060(3) 0.080(3) -0.007(2) 0.014(2) -0.0115(18) _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 Li1 N2 2.005(6) . ? Li1 N1 2.018(7) . ? Li1 N3 2.067(7) . ? Li1 N6 2.087(7) . ? Li2 N1 2.016(7) . ? Li2 N2 2.046(7) . ? Li2 N5 2.076(7) . ? Li2 N4 2.105(7) . ? N1 C1 1.385(5) . ? C1 C2 1.362(6) . ? C1 C6 1.375(6) . ? C2 C3 1.366(6) . ? C3 C4 1.379(6) . ? C4 C5 1.404(7) . ? C5 C6 1.398(7) . ? N2 C7 1.367(4) . ? C7 C8 1.400(5) . ? C7 C12 1.412(6) . ? C8 C9 1.382(8) . ? C9 C10 1.371(11) . ? C10 C11 1.377(11) . ? C11 C12 1.384(7) . ? N3 C17 1.330(5) . ? N3 C13 1.340(5) . ? C13 C14 1.373(6) . ? C14 C15 1.357(7) . ? C15 C16 1.375(7) . ? C16 C17 1.350(6) . ? N4 C18 1.293(5) . ? N4 C22 1.314(5) . ? C18 C19 1.387(7) . ? C19 C20 1.352(8) . ? C20 C21 1.307(7) . ? C21 C22 1.379(7) . ? N5 C27 1.322(5) . ? N5 C23 1.324(5) . ? C23 C24 1.381(5) . ? C24 C25 1.355(6) . ? C25 C26 1.382(6) . ? C26 C27 1.369(5) . ? N6 C32 1.337(5) . ? N6 C28 1.339(5) . ? C28 C29 1.376(6) . ? C29 C30 1.373(6) . ? C30 C31 1.367(7) . ? C31 C32 1.376(6) . ? 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 N2 Li1 N1 103.6(3) . . ? N2 Li1 N3 111.4(3) . . ? N1 Li1 N3 123.6(3) . . ? N2 Li1 N6 118.2(3) . . ? N1 Li1 N6 101.0(3) . . ? N3 Li1 N6 99.6(3) . . ? N1 Li2 N2 102.2(3) . . ? N1 Li2 N5 122.9(3) . . ? N2 Li2 N5 107.9(3) . . ? N1 Li2 N4 103.8(3) . . ? N2 Li2 N4 121.2(3) . . ? N5 Li2 N4 100.3(3) . . ? C1 N1 Li2 131.3(3) . . ? C1 N1 Li1 132.5(4) . . ? Li2 N1 Li1 77.2(3) . . ? C2 C1 C6 115.4(4) . . ? C2 C1 N1 122.1(4) . . ? C6 C1 N1 122.4(4) . . ? C1 C2 C3 123.6(4) . . ? C2 C3 C4 121.7(4) . . ? C3 C4 C5 116.4(4) . . ? C6 C5 C4 119.7(4) . . ? C1 C6 C5 123.1(4) . . ? C7 N2 Li1 132.7(3) . . ? C7 N2 Li2 115.8(3) . . ? Li1 N2 Li2 76.8(3) . . ? N2 C7 C8 119.7(4) . . ? N2 C7 C12 124.1(4) . . ? C8 C7 C12 116.1(4) . . ? C9 C8 C7 122.0(6) . . ? C10 C9 C8 120.7(6) . . ? C9 C10 C11 119.0(5) . . ? C10 C11 C12 121.1(7) . . ? C11 C12 C7 121.1(5) . . ? C17 N3 C13 116.4(4) . . ? C17 N3 Li1 117.4(3) . . ? C13 N3 Li1 126.1(3) . . ? N3 C13 C14 122.9(4) . . ? C15 C14 C13 118.7(4) . . ? C14 C15 C16 119.2(5) . . ? C17 C16 C15 118.3(4) . . ? N3 C17 C16 124.3(4) . . ? C18 N4 C22 114.6(4) . . ? C18 N4 Li2 125.0(3) . . ? C22 N4 Li2 120.3(3) . . ? N4 C18 C19 123.7(5) . . ? C20 C19 C18 119.8(5) . . ? C21 C20 C19 117.3(5) . . ? C20 C21 C22 119.7(5) . . ? N4 C22 C21 124.8(5) . . ? C27 N5 C23 116.8(3) . . ? C27 N5 Li2 124.1(3) . . ? C23 N5 Li2 116.2(3) . . ? N5 C23 C24 123.8(4) . . ? C25 C24 C23 118.8(4) . . ? C24 C25 C26 117.9(3) . . ? C27 C26 C25 119.5(4) . . ? N5 C27 C26 123.1(4) . . ? C32 N6 C28 117.1(3) . . ? C32 N6 Li1 118.3(3) . . ? C28 N6 Li1 124.1(3) . . ? N6 C28 C29 123.3(4) . . ? C30 C29 C28 117.9(4) . . ? C31 C30 C29 120.3(4) . . ? C30 C31 C32 118.0(4) . . ? N6 C32 C31 123.4(4) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 25.61 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.715 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.036 #===END data_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44.50 H44 Li2 N6' _chemical_formula_weight 676.74 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.3971(6) _cell_length_b 9.614(2) _cell_length_c 18.024(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.287(6) _cell_angle_gamma 90.00 _cell_volume 7270(3) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 7902 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 28.41 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7850 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20565 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6394 _reflns_number_gt 4016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0775P)^2^+17.1150P] 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 6394 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2258 _refine_ls_wR_factor_gt 0.2038 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 Li1 Li 0.09797(15) -0.1192(7) -0.3301(4) 0.0402(15) Uani 1 1 d . . . Li2 Li 0.13615(14) -0.2866(7) -0.2524(3) 0.0343(14) Uani 1 1 d . . . N1 N 0.07177(8) -0.0777(4) -0.43567(18) 0.0409(8) Uani 1 1 d . . . C1 C 0.04644(9) -0.1468(4) -0.4707(2) 0.0387(9) Uani 1 1 d . . . H1 H 0.0405 -0.2312 -0.4490 0.046 Uiso 1 1 calc R . . C2 C 0.02869(9) -0.1028(4) -0.5358(2) 0.0392(10) Uani 1 1 d . . . H2 H 0.0109 -0.1566 -0.5574 0.047 Uiso 1 1 calc R . . C3 C 0.03598(9) 0.0166(4) -0.5705(2) 0.0407(10) Uani 1 1 d . . . C4 C 0.06262(11) 0.0910(5) -0.5343(2) 0.0528(12) Uani 1 1 d . . . H4 H 0.0691 0.1754 -0.5550 0.063 Uiso 1 1 calc R . . C5 C 0.07891(11) 0.0391(5) -0.4687(2) 0.0536(12) Uani 1 1 d . . . H5 H 0.0967 0.0909 -0.4451 0.064 Uiso 1 1 calc R . . C6 C 0.01808(11) 0.0673(5) -0.6435(2) 0.0595(13) Uani 1 1 d . . . H6A H -0.0030 0.0235 -0.6521 0.089 Uiso 1 1 calc R . . H6B H 0.0299 0.0429 -0.6845 0.089 Uiso 1 1 calc R . . H6C H 0.0156 0.1685 -0.6416 0.089 Uiso 1 1 calc R . . N2 N 0.08423(7) 0.0489(3) -0.26542(18) 0.0381(8) Uani 1 1 d . . . C7 C 0.06622(9) 0.1587(4) -0.2874(2) 0.0437(10) Uani 1 1 d . . . H7 H 0.0562 0.1625 -0.3380 0.052 Uiso 1 1 calc R . . C8 C 0.06133(9) 0.2679(4) -0.2402(2) 0.0430(10) Uani 1 1 d . . . H8 H 0.0480 0.3435 -0.2586 0.052 Uiso 1 1 calc R . . C9 C 0.07587(8) 0.2670(4) -0.1659(2) 0.0368(9) Uani 1 1 d . . . C10 C 0.09458(9) 0.1540(4) -0.1438(2) 0.0374(9) Uani 1 1 d . . . H10 H 0.1051 0.1477 -0.0936 0.045 Uiso 1 1 calc R . . C11 C 0.09816(9) 0.0494(4) -0.1942(2) 0.0404(10) Uani 1 1 d . . . H11 H 0.1114 -0.0273 -0.1771 0.049 Uiso 1 1 calc R . . C12 C 0.07134(10) 0.3841(4) -0.1139(3) 0.0504(11) Uani 1 1 d . . . H12A H 0.0515 0.3700 -0.0929 0.076 Uiso 1 1 calc R . . H12B H 0.0702 0.4722 -0.1415 0.076 Uiso 1 1 calc R . . H12C H 0.0894 0.3868 -0.0732 0.076 Uiso 1 1 calc R . . N3 N 0.14790(7) -0.2434(3) -0.13620(16) 0.0363(8) Uani 1 1 d . . . C13 C 0.16366(9) -0.1398(4) -0.0971(2) 0.0389(9) Uani 1 1 d . . . H13 H 0.1728 -0.0694 -0.1242 0.047 Uiso 1 1 calc R . . C14 C 0.16732(10) -0.1293(4) -0.0209(2) 0.0437(10) Uani 1 1 d . . . H14 H 0.1783 -0.0518 0.0032 0.052 Uiso 1 1 calc R . . C15 C 0.15521(10) -0.2306(4) 0.0214(2) 0.0430(10) Uani 1 1 d . . . C16 C 0.13905(11) -0.3365(5) -0.0178(2) 0.0485(11) Uani 1 1 d . . . H16 H 0.1300 -0.4089 0.0082 0.058 Uiso 1 1 calc R . . C17 C 0.13586(10) -0.3384(4) -0.0952(2) 0.0471(11) Uani 1 1 d . . . H17 H 0.1242 -0.4129 -0.1207 0.057 Uiso 1 1 calc R . . C18 C 0.15949(13) -0.2250(5) 0.1059(2) 0.0643(14) Uani 1 1 d . . . H18A H 0.1472 -0.3002 0.1249 0.096 Uiso 1 1 calc R . . H18B H 0.1519 -0.1352 0.1220 0.096 Uiso 1 1 calc R . . H18C H 0.1821 -0.2361 0.1258 0.096 Uiso 1 1 calc R . . N4 N 0.16125(7) -0.4726(3) -0.25504(17) 0.0378(8) Uani 1 1 d . . . C19 C 0.19220(9) -0.4731(4) -0.2607(2) 0.0442(10) Uani 1 1 d . . . H19 H 0.2011 -0.3923 -0.2798 0.053 Uiso 1 1 calc R . . C20 C 0.21209(9) -0.5851(4) -0.2401(2) 0.0440(10) Uani 1 1 d . . . H20 H 0.2341 -0.5793 -0.2450 0.053 Uiso 1 1 calc R . . C21 C 0.20016(9) -0.7046(4) -0.2127(2) 0.0382(9) Uani 1 1 d . . . C22 C 0.16780(10) -0.7043(4) -0.2072(2) 0.0416(10) Uani 1 1 d . . . H22 H 0.1582 -0.7842 -0.1889 0.050 Uiso 1 1 calc R . . C23 C 0.14971(9) -0.5891(5) -0.2280(2) 0.0426(10) Uani 1 1 d . . . H23 H 0.1277 -0.5919 -0.2231 0.051 Uiso 1 1 calc R . . C24 C 0.22016(11) -0.8298(5) -0.1925(3) 0.0582(12) Uani 1 1 d . . . H24A H 0.2147 -0.9019 -0.2306 0.087 Uiso 1 1 calc R . . H24B H 0.2162 -0.8648 -0.1436 0.087 Uiso 1 1 calc R . . H24C H 0.2427 -0.8050 -0.1899 0.087 Uiso 1 1 calc R . . N5 N 0.14655(8) -0.1249(4) -0.31883(17) 0.0366(8) Uani 1 1 d . . . H5N H 0.1593(9) -0.068(4) -0.291(2) 0.044 Uiso 1 1 d . . . C25 C 0.16478(8) -0.1612(4) -0.3722(2) 0.0318(9) Uani 1 1 d . . . C26 C 0.19698(9) -0.1226(4) -0.3711(2) 0.0417(10) Uani 1 1 d . . . H26 H 0.2070 -0.0673 -0.3308 0.050 Uiso 1 1 calc R . . C27 C 0.21427(10) -0.1628(5) -0.4267(3) 0.0508(12) Uani 1 1 d . . . H27 H 0.2359 -0.1347 -0.4239 0.061 Uiso 1 1 calc R . . C28 C 0.20069(12) -0.2431(5) -0.4863(3) 0.0596(13) Uani 1 1 d . . . H28 H 0.2126 -0.2696 -0.5248 0.072 Uiso 1 1 calc R . . C29 C 0.16938(11) -0.2838(5) -0.4885(2) 0.0541(12) Uani 1 1 d . . . H29 H 0.1598 -0.3403 -0.5288 0.065 Uiso 1 1 calc R . . C30 C 0.15187(9) -0.2449(4) -0.4342(2) 0.0408(10) Uani 1 1 d . . . H30 H 0.1303 -0.2746 -0.4380 0.049 Uiso 1 1 calc R . . N6 N 0.08863(7) -0.2974(3) -0.26861(18) 0.0388(8) Uani 1 1 d . . . H6N H 0.0781(10) -0.267(4) -0.235(2) 0.047 Uiso 1 1 d . . . C31 C 0.06831(8) -0.3794(4) -0.3144(2) 0.0326(9) Uani 1 1 d . . . C32 C 0.08016(9) -0.4608(4) -0.3706(2) 0.0360(9) Uani 1 1 d . . . H32 H 0.1023 -0.4592 -0.3739 0.043 Uiso 1 1 calc R . . C33 C 0.06029(12) -0.5413(4) -0.4198(2) 0.0545(12) Uani 1 1 d . . . H33 H 0.0689 -0.5945 -0.4565 0.065 Uiso 1 1 calc R . . C34 C 0.02742(13) -0.5459(5) -0.4166(3) 0.0689(16) Uani 1 1 d . . . H34 H 0.0135 -0.6005 -0.4509 0.083 Uiso 1 1 calc R . . C35 C 0.01602(11) -0.4679(5) -0.3613(3) 0.0619(14) Uani 1 1 d . . . H35 H -0.0062 -0.4696 -0.3582 0.074 Uiso 1 1 calc R . . C36 C 0.03523(9) -0.3900(4) -0.3119(2) 0.0444(10) Uani 1 1 d . . . H36 H 0.0263 -0.3406 -0.2743 0.053 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 Li1 0.043(4) 0.038(4) 0.039(4) -0.006(3) 0.005(3) 0.005(3) Li2 0.035(3) 0.041(4) 0.026(3) -0.001(3) 0.004(2) -0.003(3) N1 0.046(2) 0.044(2) 0.0340(18) 0.0030(16) 0.0100(15) -0.0022(16) C1 0.041(2) 0.031(2) 0.043(2) 0.0050(18) 0.0050(18) 0.0026(18) C2 0.034(2) 0.043(2) 0.041(2) 0.002(2) 0.0035(17) 0.0001(18) C3 0.044(2) 0.044(3) 0.036(2) -0.0022(19) 0.0118(18) 0.009(2) C4 0.080(3) 0.041(3) 0.041(3) 0.007(2) 0.019(2) -0.007(2) C5 0.059(3) 0.067(3) 0.036(2) -0.008(2) 0.008(2) -0.022(2) C6 0.061(3) 0.067(3) 0.049(3) 0.019(2) 0.001(2) 0.019(2) N2 0.0409(18) 0.0338(19) 0.041(2) 0.0031(15) 0.0091(15) -0.0003(15) C7 0.046(2) 0.048(3) 0.037(2) 0.009(2) 0.0058(18) 0.000(2) C8 0.044(2) 0.031(2) 0.054(3) 0.010(2) 0.007(2) 0.0079(18) C9 0.0313(19) 0.032(2) 0.050(2) 0.0045(19) 0.0156(17) -0.0053(17) C10 0.036(2) 0.042(2) 0.034(2) 0.0024(19) 0.0027(16) -0.0002(18) C11 0.041(2) 0.039(2) 0.040(2) 0.005(2) 0.0034(18) 0.0093(19) C12 0.052(3) 0.035(2) 0.068(3) -0.005(2) 0.021(2) -0.001(2) N3 0.0416(18) 0.0387(19) 0.0286(17) -0.0024(15) 0.0048(14) -0.0032(15) C13 0.044(2) 0.036(2) 0.036(2) 0.0041(19) 0.0013(17) -0.0017(18) C14 0.055(3) 0.038(2) 0.035(2) -0.004(2) -0.0027(19) -0.003(2) C15 0.058(3) 0.041(3) 0.029(2) -0.0001(19) 0.0048(18) 0.019(2) C16 0.076(3) 0.042(3) 0.031(2) 0.002(2) 0.021(2) -0.003(2) C17 0.064(3) 0.042(3) 0.039(2) -0.005(2) 0.018(2) -0.015(2) C18 0.106(4) 0.054(3) 0.031(2) 0.004(2) 0.002(2) 0.017(3) N4 0.0373(18) 0.040(2) 0.0370(19) -0.0035(16) 0.0085(14) -0.0021(15) C19 0.038(2) 0.040(2) 0.055(3) -0.003(2) 0.0094(19) -0.0061(19) C20 0.030(2) 0.043(3) 0.059(3) -0.003(2) 0.0046(18) -0.0050(19) C21 0.042(2) 0.039(2) 0.032(2) -0.0070(18) -0.0017(17) 0.0007(18) C22 0.052(2) 0.040(2) 0.035(2) -0.0027(19) 0.0126(18) -0.010(2) C23 0.034(2) 0.055(3) 0.042(2) 0.000(2) 0.0148(18) -0.001(2) C24 0.063(3) 0.046(3) 0.062(3) -0.010(2) -0.003(2) 0.007(2) N5 0.0399(18) 0.043(2) 0.0286(18) -0.0040(15) 0.0086(14) -0.0082(15) C25 0.0320(19) 0.032(2) 0.032(2) 0.0055(17) 0.0064(16) -0.0006(16) C26 0.035(2) 0.048(3) 0.042(2) 0.005(2) 0.0040(17) -0.0040(19) C27 0.032(2) 0.062(3) 0.061(3) 0.016(3) 0.016(2) 0.005(2) C28 0.068(3) 0.059(3) 0.060(3) 0.009(3) 0.035(3) 0.016(3) C29 0.071(3) 0.054(3) 0.041(2) -0.008(2) 0.018(2) -0.007(2) C30 0.045(2) 0.041(2) 0.040(2) -0.0017(19) 0.0158(18) -0.0074(19) N6 0.0365(18) 0.042(2) 0.039(2) -0.0104(16) 0.0122(15) -0.0078(15) C31 0.035(2) 0.027(2) 0.035(2) 0.0094(17) 0.0011(16) -0.0013(17) C32 0.045(2) 0.030(2) 0.033(2) 0.0059(18) 0.0010(17) -0.0040(18) C33 0.088(4) 0.033(3) 0.040(3) 0.004(2) 0.001(2) -0.009(2) C34 0.073(4) 0.050(3) 0.070(4) 0.022(3) -0.039(3) -0.028(3) C35 0.041(3) 0.049(3) 0.090(4) 0.022(3) -0.013(3) -0.009(2) C36 0.033(2) 0.035(2) 0.063(3) 0.011(2) 0.0020(19) 0.0006(18) _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 Li1 N5 2.041(7) . ? Li1 N1 2.099(7) . ? Li1 N6 2.108(8) . ? Li1 N2 2.123(7) . ? Li2 N6 1.997(7) . ? Li2 N5 2.049(7) . ? Li2 N4 2.085(7) . ? Li2 N3 2.122(6) . ? N1 C5 1.325(5) . ? N1 C1 1.341(5) . ? C1 C2 1.367(5) . ? C2 C3 1.364(6) . ? C3 C4 1.414(6) . ? C3 C6 1.502(6) . ? C4 C5 1.375(6) . ? N2 C7 1.329(5) . ? N2 C11 1.334(5) . ? C7 C8 1.386(6) . ? C8 C9 1.390(6) . ? C9 C10 1.371(5) . ? C9 C12 1.495(6) . ? C10 C11 1.378(5) . ? N3 C17 1.323(5) . ? N3 C13 1.341(5) . ? C13 C14 1.363(5) . ? C14 C15 1.380(6) . ? C15 C16 1.365(6) . ? C15 C18 1.510(6) . ? C16 C17 1.382(5) . ? N4 C19 1.331(5) . ? N4 C23 1.342(5) . ? C19 C20 1.385(6) . ? C20 C21 1.376(6) . ? C21 C22 1.390(5) . ? C21 C24 1.487(6) . ? C22 C23 1.368(6) . ? N5 C25 1.363(5) . ? C25 C26 1.412(5) . ? C25 C30 1.421(5) . ? C26 C27 1.380(6) . ? C27 C28 1.380(7) . ? C28 C29 1.379(6) . ? C29 C30 1.363(5) . ? N6 C31 1.356(5) . ? C31 C36 1.413(5) . ? C31 C32 1.428(5) . ? C32 C33 1.371(6) . ? C33 C34 1.404(7) . ? C34 C35 1.389(8) . ? C35 C36 1.344(6) . ? 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 N5 Li1 N1 119.3(3) . . ? N5 Li1 N6 100.9(3) . . ? N1 Li1 N6 121.1(3) . . ? N5 Li1 N2 108.6(3) . . ? N1 Li1 N2 101.6(3) . . ? N6 Li1 N2 104.1(3) . . ? N6 Li2 N5 104.6(3) . . ? N6 Li2 N4 117.4(3) . . ? N5 Li2 N4 118.9(3) . . ? N6 Li2 N3 104.1(3) . . ? N5 Li2 N3 112.9(3) . . ? N4 Li2 N3 98.2(3) . . ? C5 N1 C1 115.3(4) . . ? C5 N1 Li1 116.3(3) . . ? C1 N1 Li1 128.0(3) . . ? N1 C1 C2 123.7(4) . . ? C3 C2 C1 121.4(4) . . ? C2 C3 C4 115.7(4) . . ? C2 C3 C6 123.7(4) . . ? C4 C3 C6 120.6(4) . . ? C5 C4 C3 118.8(4) . . ? N1 C5 C4 125.1(4) . . ? C7 N2 C11 116.1(3) . . ? C7 N2 Li1 129.3(3) . . ? C11 N2 Li1 114.3(3) . . ? N2 C7 C8 123.3(4) . . ? C7 C8 C9 120.1(4) . . ? C10 C9 C8 116.3(4) . . ? C10 C9 C12 122.4(4) . . ? C8 C9 C12 121.3(4) . . ? C9 C10 C11 120.0(4) . . ? N2 C11 C10 124.1(4) . . ? C17 N3 C13 115.0(3) . . ? C17 N3 Li2 111.2(3) . . ? C13 N3 Li2 133.8(3) . . ? N3 C13 C14 124.0(4) . . ? C13 C14 C15 120.4(4) . . ? C16 C15 C14 116.1(4) . . ? C16 C15 C18 121.7(4) . . ? C14 C15 C18 122.2(4) . . ? C15 C16 C17 120.0(4) . . ? N3 C17 C16 124.4(4) . . ? C19 N4 C23 116.1(3) . . ? C19 N4 Li2 121.1(3) . . ? C23 N4 Li2 119.6(3) . . ? N4 C19 C20 123.5(4) . . ? C21 C20 C19 120.3(4) . . ? C20 C21 C22 116.3(4) . . ? C20 C21 C24 122.5(4) . . ? C22 C21 C24 121.2(4) . . ? C23 C22 C21 120.1(4) . . ? N4 C23 C22 123.8(4) . . ? C25 N5 Li1 127.1(3) . . ? C25 N5 Li2 114.2(3) . . ? Li1 N5 Li2 77.2(3) . . ? N5 C25 C26 124.6(4) . . ? N5 C25 C30 120.5(3) . . ? C26 C25 C30 114.9(3) . . ? C27 C26 C25 122.0(4) . . ? C28 C27 C26 121.1(4) . . ? C29 C28 C27 118.3(4) . . ? C30 C29 C28 121.5(4) . . ? C29 C30 C25 122.2(4) . . ? C31 N6 Li2 131.2(3) . . ? C31 N6 Li1 107.7(3) . . ? Li2 N6 Li1 76.9(3) . . ? N6 C31 C36 124.7(4) . . ? N6 C31 C32 119.5(3) . . ? C36 C31 C32 115.8(4) . . ? C33 C32 C31 121.5(4) . . ? C32 C33 C34 120.8(5) . . ? C35 C34 C33 117.6(4) . . ? C36 C35 C34 122.4(5) . . ? C35 C36 C31 121.9(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.228 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.053 #===END data_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H102 Li4 N10' _chemical_formula_weight 1207.46 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0898(18) _cell_length_b 12.1766(18) _cell_length_c 13.717(2) _cell_angle_alpha 106.324(3) _cell_angle_beta 101.859(3) _cell_angle_gamma 98.673(4) _cell_volume 1849.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5740 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.53 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.72 _exptl_crystal_size_min 0.52 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4571 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11139 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6298 _reflns_number_gt 3595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1000P)^2^+0.0000P] 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 6298 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _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 Li1 Li 0.5951(4) 0.5732(4) 0.3114(3) 0.0366(11) Uani 1 1 d . . . Li2 Li 0.5300(4) 0.4958(4) 0.0920(3) 0.0399(12) Uani 1 1 d . . . N1 N 0.7304(2) 0.5921(2) 0.43919(17) 0.0390(6) Uani 1 1 d . . . C1 C 0.7253(3) 0.4988(3) 0.4703(2) 0.0491(8) Uani 1 1 d . . . H1A H 0.6642 0.4323 0.4310 0.059 Uiso 1 1 calc R . . C2 C 0.8030(3) 0.4916(3) 0.5563(2) 0.0463(8) Uani 1 1 d . . . H2A H 0.7934 0.4219 0.5750 0.056 Uiso 1 1 calc R . . C3 C 0.8941(2) 0.5846(2) 0.61494(19) 0.0297(6) Uani 1 1 d . . . C4 C 0.9000(3) 0.6815(3) 0.5818(2) 0.0475(8) Uani 1 1 d . . . H4A H 0.9612 0.7486 0.6184 0.057 Uiso 1 1 calc R . . C5 C 0.8175(3) 0.6819(3) 0.4958(2) 0.0506(8) Uani 1 1 d . . . H5A H 0.8238 0.7509 0.4760 0.061 Uiso 1 1 calc R . . C6 C 0.9793(2) 0.5838(2) 0.7137(2) 0.0351(7) Uani 1 1 d . . . C7 C 0.9422(3) 0.6538(3) 0.8080(2) 0.0653(10) Uani 1 1 d . . . H7A H 0.8639 0.6154 0.8056 0.098 Uiso 1 1 calc R . . H7B H 0.9426 0.7336 0.8057 0.098 Uiso 1 1 calc R . . H7C H 0.9962 0.6573 0.8733 0.098 Uiso 1 1 calc R . . C8 C 1.1025(3) 0.6432(3) 0.7210(3) 0.0694(11) Uani 1 1 d . . . H8A H 1.1268 0.6006 0.6600 0.104 Uiso 1 1 calc R . . H8B H 1.1549 0.6428 0.7857 0.104 Uiso 1 1 calc R . . H8C H 1.1049 0.7244 0.7222 0.104 Uiso 1 1 calc R . . C9 C 0.9790(3) 0.4617(3) 0.7191(3) 0.0619(10) Uani 1 1 d . . . H9A H 0.9961 0.4139 0.6559 0.093 Uiso 1 1 calc R . . H9B H 0.9026 0.4261 0.7233 0.093 Uiso 1 1 calc R . . H9C H 1.0380 0.4659 0.7816 0.093 Uiso 1 1 calc R . . N2 N 0.47306(18) 0.6492(2) 0.37316(16) 0.0375(6) Uani 1 1 d . . . C10 C 0.3881(2) 0.6736(3) 0.3087(2) 0.0394(7) Uani 1 1 d . . . H10A H 0.3731 0.6348 0.2353 0.047 Uiso 1 1 calc R . . C11 C 0.3210(2) 0.7511(2) 0.3416(2) 0.0374(7) Uani 1 1 d . . . H11A H 0.2635 0.7656 0.2911 0.045 Uiso 1 1 calc R . . C12 C 0.3367(2) 0.8081(2) 0.4481(2) 0.0342(7) Uani 1 1 d . . . C13 C 0.4231(2) 0.7810(2) 0.5153(2) 0.0346(7) Uani 1 1 d . . . H13A H 0.4378 0.8161 0.5892 0.041 Uiso 1 1 calc R . . C14 C 0.4876(2) 0.7039(2) 0.4759(2) 0.0361(7) Uani 1 1 d . . . H14A H 0.5462 0.6883 0.5247 0.043 Uiso 1 1 calc R . . C15 C 0.2682(2) 0.8971(3) 0.4912(2) 0.0431(7) Uani 1 1 d . . . C16 C 0.3501(3) 1.0171(3) 0.5428(3) 0.0797(12) Uani 1 1 d . . . H16A H 0.3837 1.0399 0.4903 0.120 Uiso 1 1 calc R . . H16B H 0.4122 1.0138 0.5997 0.120 Uiso 1 1 calc R . . H16C H 0.3071 1.0750 0.5716 0.120 Uiso 1 1 calc R . . C17 C 0.1715(3) 0.9065(4) 0.4058(3) 0.0793(12) Uani 1 1 d . . . H17A H 0.2050 0.9370 0.3568 0.119 Uiso 1 1 calc R . . H17B H 0.1263 0.9600 0.4379 0.119 Uiso 1 1 calc R . . H17C H 0.1209 0.8288 0.3676 0.119 Uiso 1 1 calc R . . C18 C 0.2151(3) 0.8618(3) 0.5737(3) 0.0744(11) Uani 1 1 d . . . H18A H 0.1728 0.9202 0.6026 0.112 Uiso 1 1 calc R . . H18B H 0.2771 0.8580 0.6304 0.112 Uiso 1 1 calc R . . H18C H 0.1618 0.7848 0.5405 0.112 Uiso 1 1 calc R . . N3 N 0.65979(18) 0.6878(2) 0.23773(17) 0.0363(6) Uani 1 1 d . . . C19 C 0.7678(2) 0.6831(3) 0.2289(2) 0.0437(8) Uani 1 1 d . . . H19A H 0.8016 0.6247 0.2493 0.052 Uiso 1 1 calc R . . C20 C 0.8324(2) 0.7576(2) 0.1921(2) 0.0373(7) Uani 1 1 d . . . H20A H 0.9091 0.7511 0.1894 0.045 Uiso 1 1 calc R . . C21 C 0.7856(2) 0.8421(2) 0.15882(19) 0.0295(6) Uani 1 1 d . . . C22 C 0.6740(2) 0.8458(2) 0.1664(2) 0.0356(7) Uani 1 1 d . . . H22A H 0.6369 0.9010 0.1437 0.043 Uiso 1 1 calc R . . C23 C 0.6160(2) 0.7700(2) 0.2066(2) 0.0380(7) Uani 1 1 d . . . H23A H 0.5402 0.7769 0.2126 0.046 Uiso 1 1 calc R . . C24 C 0.8554(2) 0.9234(2) 0.1151(2) 0.0348(7) Uani 1 1 d . . . C25 C 0.9719(2) 0.9850(3) 0.1952(2) 0.0446(8) Uani 1 1 d . . . H25A H 0.9587 1.0316 0.2610 0.067 Uiso 1 1 calc R . . H25B H 1.0171 1.0367 0.1672 0.067 Uiso 1 1 calc R . . H25C H 1.0146 0.9262 0.2087 0.067 Uiso 1 1 calc R . . C26 C 0.7910(3) 1.0153(3) 0.0910(3) 0.0548(9) Uani 1 1 d . . . H26A H 0.7720 1.0597 0.1545 0.082 Uiso 1 1 calc R . . H26B H 0.7195 0.9762 0.0351 0.082 Uiso 1 1 calc R . . H26C H 0.8403 1.0689 0.0678 0.082 Uiso 1 1 calc R . . C27 C 0.8756(3) 0.8469(3) 0.0129(2) 0.0502(8) Uani 1 1 d . . . H27A H 0.9171 0.7879 0.0280 0.075 Uiso 1 1 calc R . . H27B H 0.9217 0.8965 -0.0162 0.075 Uiso 1 1 calc R . . H27C H 0.8007 0.8075 -0.0383 0.075 Uiso 1 1 calc R . . N4 N 0.56860(19) 0.4182(2) 0.20243(17) 0.0345(6) Uani 1 1 d . . . H4N H 0.628(2) 0.395(2) 0.183(2) 0.041 Uiso 1 1 d . . . C28 C 0.5057(2) 0.3166(2) 0.20735(18) 0.0305(6) Uani 1 1 d . . . C29 C 0.5353(2) 0.2078(2) 0.1811(2) 0.0393(7) Uani 1 1 d . . . H29A H 0.6039 0.2019 0.1583 0.047 Uiso 1 1 calc R . . C30 C 0.4690(3) 0.1081(3) 0.1870(2) 0.0439(7) Uani 1 1 d . . . H30A H 0.4918 0.0353 0.1673 0.053 Uiso 1 1 calc R . . C31 C 0.3692(3) 0.1141(3) 0.2217(2) 0.0439(8) Uani 1 1 d . . . H31A H 0.3232 0.0462 0.2263 0.053 Uiso 1 1 calc R . . C32 C 0.3386(2) 0.2197(3) 0.2491(2) 0.0429(7) Uani 1 1 d . . . H32A H 0.2711 0.2247 0.2738 0.051 Uiso 1 1 calc R . . C33 C 0.4030(2) 0.3196(3) 0.2419(2) 0.0368(7) Uani 1 1 d . . . H33A H 0.3782 0.3913 0.2603 0.044 Uiso 1 1 calc R . . N5 N 0.3730(2) 0.5012(2) 0.01274(18) 0.0372(6) Uani 1 1 d . . . H5N H 0.336(2) 0.432(2) 0.010(2) 0.045 Uiso 1 1 d . . . C34 C 0.3058(2) 0.5816(2) 0.02751(18) 0.0294(6) Uani 1 1 d . . . C35 C 0.1933(2) 0.5592(3) 0.04389(19) 0.0365(7) Uani 1 1 d . . . H35A H 0.1594 0.4821 0.0405 0.044 Uiso 1 1 calc R . . C36 C 0.1324(2) 0.6458(3) 0.0645(2) 0.0451(8) Uani 1 1 d . . . H36A H 0.0575 0.6271 0.0752 0.054 Uiso 1 1 calc R . . C37 C 0.1770(3) 0.7592(3) 0.0702(2) 0.0439(8) Uani 1 1 d . . . H37A H 0.1352 0.8191 0.0862 0.053 Uiso 1 1 calc R . . C38 C 0.2859(2) 0.7827(3) 0.0517(2) 0.0406(7) Uani 1 1 d . . . H38A H 0.3184 0.8597 0.0540 0.049 Uiso 1 1 calc R . . C39 C 0.3467(2) 0.6965(2) 0.03009(19) 0.0315(6) Uani 1 1 d . . . H39A H 0.4199 0.7155 0.0163 0.038 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 Li1 0.032(3) 0.054(3) 0.023(2) 0.017(2) 0.003(2) 0.006(2) Li2 0.039(3) 0.058(3) 0.031(3) 0.023(2) 0.009(2) 0.019(2) N1 0.0342(14) 0.0524(15) 0.0327(13) 0.0199(13) 0.0061(11) 0.0081(12) C1 0.0395(18) 0.060(2) 0.0401(18) 0.0263(16) -0.0043(14) -0.0103(15) C2 0.0444(19) 0.0550(19) 0.0371(17) 0.0272(16) -0.0010(15) -0.0037(16) C3 0.0218(14) 0.0454(17) 0.0245(14) 0.0128(13) 0.0094(12) 0.0074(13) C4 0.0448(19) 0.0486(19) 0.0360(17) 0.0167(15) -0.0082(15) -0.0079(15) C5 0.062(2) 0.0439(18) 0.0431(19) 0.0236(16) 0.0003(17) 0.0027(17) C6 0.0213(15) 0.0569(19) 0.0288(15) 0.0183(14) 0.0043(12) 0.0088(13) C7 0.067(2) 0.109(3) 0.0290(17) 0.0255(19) 0.0108(17) 0.041(2) C8 0.0259(18) 0.115(3) 0.069(2) 0.048(2) 0.0014(17) 0.0032(19) C9 0.047(2) 0.072(2) 0.065(2) 0.032(2) -0.0045(17) 0.0171(18) N2 0.0265(13) 0.0573(15) 0.0263(13) 0.0144(12) 0.0060(10) 0.0019(11) C10 0.0295(16) 0.064(2) 0.0223(15) 0.0152(14) 0.0051(13) 0.0036(15) C11 0.0285(16) 0.0598(19) 0.0264(15) 0.0225(14) 0.0044(12) 0.0047(14) C12 0.0252(15) 0.0454(17) 0.0335(16) 0.0187(14) 0.0077(12) 0.0004(13) C13 0.0296(16) 0.0497(17) 0.0210(14) 0.0118(13) 0.0033(12) 0.0029(13) C14 0.0279(15) 0.0562(19) 0.0245(15) 0.0181(14) 0.0042(12) 0.0044(14) C15 0.0375(18) 0.0496(19) 0.0426(18) 0.0159(15) 0.0100(14) 0.0095(15) C16 0.074(3) 0.055(2) 0.104(3) 0.008(2) 0.034(3) 0.015(2) C17 0.065(3) 0.105(3) 0.076(3) 0.030(2) 0.012(2) 0.047(2) C18 0.073(3) 0.099(3) 0.083(3) 0.043(2) 0.054(2) 0.039(2) N3 0.0242(13) 0.0534(15) 0.0386(14) 0.0219(12) 0.0106(11) 0.0132(11) C19 0.0367(18) 0.059(2) 0.0516(19) 0.0343(17) 0.0156(15) 0.0219(15) C20 0.0264(15) 0.0544(18) 0.0430(17) 0.0268(15) 0.0136(13) 0.0170(14) C21 0.0279(15) 0.0410(16) 0.0211(13) 0.0119(12) 0.0050(11) 0.0102(12) C22 0.0295(16) 0.0486(18) 0.0382(16) 0.0251(14) 0.0085(13) 0.0163(13) C23 0.0248(15) 0.0538(18) 0.0418(17) 0.0216(15) 0.0099(13) 0.0146(14) C24 0.0294(16) 0.0483(17) 0.0318(16) 0.0203(14) 0.0089(13) 0.0077(13) C25 0.0371(18) 0.0557(19) 0.0415(18) 0.0207(16) 0.0113(15) 0.0003(15) C26 0.050(2) 0.066(2) 0.065(2) 0.0449(19) 0.0164(17) 0.0157(17) C27 0.049(2) 0.073(2) 0.0329(17) 0.0233(16) 0.0157(15) 0.0095(17) N4 0.0293(13) 0.0486(15) 0.0318(13) 0.0195(12) 0.0081(11) 0.0138(11) C28 0.0295(15) 0.0440(17) 0.0188(13) 0.0145(13) 0.0004(11) 0.0103(13) C29 0.0310(16) 0.0545(19) 0.0353(16) 0.0190(15) 0.0063(13) 0.0127(14) C30 0.0470(19) 0.0451(18) 0.0391(17) 0.0163(15) 0.0035(15) 0.0135(15) C31 0.0432(19) 0.0469(19) 0.0367(17) 0.0182(15) 0.0007(15) -0.0005(15) C32 0.0318(17) 0.065(2) 0.0322(16) 0.0195(16) 0.0070(13) 0.0061(15) C33 0.0306(16) 0.0487(17) 0.0330(16) 0.0157(14) 0.0057(13) 0.0134(14) N5 0.0374(14) 0.0463(15) 0.0355(13) 0.0216(13) 0.0116(11) 0.0132(12) C34 0.0231(14) 0.0484(17) 0.0161(13) 0.0127(12) 0.0005(11) 0.0081(13) C35 0.0238(15) 0.0581(19) 0.0280(15) 0.0203(14) 0.0021(12) 0.0040(14) C36 0.0214(15) 0.089(3) 0.0307(16) 0.0266(17) 0.0066(13) 0.0153(16) C37 0.0385(18) 0.065(2) 0.0307(16) 0.0151(16) 0.0041(14) 0.0264(16) C38 0.0389(18) 0.0514(18) 0.0299(16) 0.0164(14) 0.0014(13) 0.0098(15) C39 0.0206(14) 0.0495(17) 0.0242(14) 0.0160(13) 0.0014(11) 0.0053(13) _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 Li1 N4 1.983(5) . ? Li1 N2 2.058(5) . ? Li1 N1 2.069(5) . ? Li1 N3 2.091(5) . ? Li2 N5 2.005(5) . ? Li2 N4 2.013(4) . ? Li2 N5 2.036(5) 2_665 ? Li2 N3 2.627(5) . ? N1 C1 1.317(3) . ? N1 C5 1.322(4) . ? C1 C2 1.382(4) . ? C2 C3 1.375(4) . ? C3 C4 1.375(4) . ? C3 C6 1.528(3) . ? C4 C5 1.381(4) . ? C6 C9 1.509(4) . ? C6 C8 1.524(4) . ? C6 C7 1.529(4) . ? N2 C10 1.339(3) . ? N2 C14 1.340(3) . ? C10 C11 1.376(4) . ? C11 C12 1.388(4) . ? C12 C13 1.390(3) . ? C12 C15 1.523(4) . ? C13 C14 1.374(4) . ? C15 C17 1.518(4) . ? C15 C16 1.521(4) . ? C15 C18 1.537(4) . ? N3 C23 1.331(3) . ? N3 C19 1.344(3) . ? C19 C20 1.376(4) . ? C20 C21 1.386(3) . ? C21 C22 1.380(4) . ? C21 C24 1.530(3) . ? C22 C23 1.378(4) . ? C24 C26 1.527(4) . ? C24 C25 1.528(4) . ? C24 C27 1.539(4) . ? N4 C28 1.378(3) . ? C28 C29 1.394(4) . ? C28 C33 1.418(4) . ? C29 C30 1.382(4) . ? C30 C31 1.391(4) . ? C31 C32 1.363(4) . ? C32 C33 1.382(4) . ? N5 C34 1.363(3) . ? N5 Li2 2.036(5) 2_665 ? C34 C39 1.400(4) . ? C34 C35 1.422(4) . ? C35 C36 1.374(4) . ? C36 C37 1.379(4) . ? C37 C38 1.394(4) . ? C38 C39 1.370(4) . ? 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 N4 Li1 N2 127.3(2) . . ? N4 Li1 N1 110.8(2) . . ? N2 Li1 N1 105.8(2) . . ? N4 Li1 N3 101.9(2) . . ? N2 Li1 N3 103.8(2) . . ? N1 Li1 N3 104.8(2) . . ? N5 Li2 N4 128.1(3) . . ? N5 Li2 N5 103.1(2) . 2_665 ? N4 Li2 N5 121.2(2) . 2_665 ? N5 Li2 N3 118.8(2) . . ? N4 Li2 N3 84.93(17) . . ? N5 Li2 N3 95.0(2) 2_665 . ? C1 N1 C5 115.5(2) . . ? C1 N1 Li1 113.3(2) . . ? C5 N1 Li1 131.1(2) . . ? N1 C1 C2 124.3(3) . . ? C3 C2 C1 120.3(3) . . ? C4 C3 C2 115.4(2) . . ? C4 C3 C6 121.9(2) . . ? C2 C3 C6 122.6(2) . . ? C3 C4 C5 120.5(3) . . ? N1 C5 C4 124.0(3) . . ? C9 C6 C8 108.7(2) . . ? C9 C6 C3 112.8(2) . . ? C8 C6 C3 111.2(2) . . ? C9 C6 C7 108.7(2) . . ? C8 C6 C7 108.5(3) . . ? C3 C6 C7 106.9(2) . . ? C10 N2 C14 114.9(2) . . ? C10 N2 Li1 118.7(2) . . ? C14 N2 Li1 124.1(2) . . ? N2 C10 C11 124.4(2) . . ? C10 C11 C12 120.5(2) . . ? C11 C12 C13 115.2(2) . . ? C11 C12 C15 123.9(2) . . ? C13 C12 C15 120.9(2) . . ? C14 C13 C12 120.7(2) . . ? N2 C14 C13 124.2(2) . . ? C17 C15 C16 107.9(3) . . ? C17 C15 C12 112.5(3) . . ? C16 C15 C12 108.7(2) . . ? C17 C15 C18 108.8(3) . . ? C16 C15 C18 109.3(3) . . ? C12 C15 C18 109.6(2) . . ? C23 N3 C19 115.5(2) . . ? C23 N3 Li1 130.8(2) . . ? C19 N3 Li1 113.4(2) . . ? C23 N3 Li2 101.22(19) . . ? C19 N3 Li2 103.8(2) . . ? Li1 N3 Li2 71.46(17) . . ? N3 C19 C20 124.0(2) . . ? C19 C20 C21 120.1(2) . . ? C22 C21 C20 115.9(2) . . ? C22 C21 C24 123.5(2) . . ? C20 C21 C24 120.6(2) . . ? C23 C22 C21 120.6(2) . . ? N3 C23 C22 123.9(2) . . ? C26 C24 C25 109.4(2) . . ? C26 C24 C21 111.7(2) . . ? C25 C24 C21 109.2(2) . . ? C26 C24 C27 109.2(2) . . ? C25 C24 C27 109.7(2) . . ? C21 C24 C27 107.6(2) . . ? C28 N4 Li1 123.0(2) . . ? C28 N4 Li2 127.0(2) . . ? Li1 N4 Li2 88.5(2) . . ? N4 C28 C29 124.8(2) . . ? N4 C28 C33 119.4(2) . . ? C29 C28 C33 115.8(2) . . ? C30 C29 C28 122.7(3) . . ? C29 C30 C31 120.1(3) . . ? C32 C31 C30 118.6(3) . . ? C31 C32 C33 121.9(3) . . ? C32 C33 C28 121.0(3) . . ? C34 N5 Li2 133.2(2) . . ? C34 N5 Li2 117.3(2) . 2_665 ? Li2 N5 Li2 76.9(2) . 2_665 ? N5 C34 C39 120.5(2) . . ? N5 C34 C35 124.6(2) . . ? C39 C34 C35 114.9(2) . . ? C36 C35 C34 121.9(3) . . ? C35 C36 C37 121.7(3) . . ? C36 C37 C38 117.5(3) . . ? C39 C38 C37 121.1(3) . . ? C38 C39 C34 122.8(2) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.287 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.059 #===END