data_vb34-rs5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H90 Li12 N6' _chemical_formula_sum 'C72 H90 Li12 N6' _chemical_formula_weight 1122.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'trigonal' _symmetry_space_group_name_H-M 'r3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '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' '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' _cell_length_a 25.7286(5) _cell_length_b 25.7286(5) _cell_length_c 8.9644(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5139.06(18) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8657 _cell_measurement_theta_min 3.4328 _cell_measurement_theta_max 66.2894 _exptl_crystal_description needle _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8967 _exptl_absorpt_correction_T_max 0.9402 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies , Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18469 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 66.40 _reflns_number_total 4001 _reflns_number_gt 3909 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-14 (Sheldrick, 2014)' _computing_molecular_graphics 'XSeed' _computing_publication_material 'Cif-Tab' _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. Structure was checked in PLATON for additional symmetry however did not refine well in R-3 suggested space group. The starting molecule is a pure chiral source so its chirality is based upon this rather than structural ; _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^)+(0.0457P)^2^+1.9549P] 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 0.0(3) _refine_ls_number_reflns 4001 _refine_ls_number_parameters 281 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _chemical_absolute_configuration syn 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 N1 N 0.49088(5) 0.21289(5) 0.93107(12) 0.0218(2) Uani 1 1 d . . . N2 N 0.61075(5) 0.15955(5) 1.00191(13) 0.0243(3) Uani 1 1 d . . . C1 C 0.47170(6) 0.11359(7) 0.68997(17) 0.0266(3) Uani 1 1 d . . . H1 H 0.5016 0.1496 0.6447 0.032 Uiso 1 1 calc R . . C2 C 0.46740(7) 0.05928(7) 0.65060(19) 0.0326(3) Uani 1 1 d . . . H2 H 0.4939 0.0584 0.5784 0.039 Uiso 1 1 calc R . . C3 C 0.42415(8) 0.00634(7) 0.7172(2) 0.0363(4) Uani 1 1 d . . . H3 H 0.4207 -0.0309 0.6896 0.044 Uiso 1 1 calc R . . C4 C 0.38626(8) 0.00808(7) 0.8233(2) 0.0372(4) Uani 1 1 d . . . H4 H 0.3572 -0.0279 0.8705 0.045 Uiso 1 1 calc R . . C5 C 0.39063(7) 0.06268(7) 0.86148(17) 0.0308(3) Uani 1 1 d . . . H5 H 0.3642 0.0633 0.9345 0.037 Uiso 1 1 calc R . . C6 C 0.43275(6) 0.11614(6) 0.79519(15) 0.0232(3) Uani 1 1 d . . . C7 C 0.43783(6) 0.17601(6) 0.83802(15) 0.0234(3) Uani 1 1 d . . . H7 H 0.4014 0.1672 0.8974 0.028 Uiso 1 1 calc R . . C8 C 0.43911(6) 0.21117(6) 0.70054(15) 0.0288(3) Uani 1 1 d . . . H8A H 0.4343 0.2451 0.7306 0.043 Uiso 1 1 calc R . . H8B H 0.4063 0.1849 0.6334 0.043 Uiso 1 1 calc R . . H8C H 0.4776 0.2261 0.6490 0.043 Uiso 1 1 calc R . . C9 C 0.48133(6) 0.18669(6) 1.07974(15) 0.0234(3) Uani 1 1 d . . . H9A H 0.4800 0.1476 1.0734 0.028 Uiso 1 1 calc R . . H9B H 0.4421 0.1792 1.1184 0.028 Uiso 1 1 calc R . . C10 C 0.53065(6) 0.22738(6) 1.18775(15) 0.0236(3) Uani 1 1 d . . . C11 C 0.52168(7) 0.20107(8) 1.34192(17) 0.0345(3) Uani 1 1 d . . . H11A H 0.5554 0.2282 1.4057 0.052 Uiso 1 1 calc R . . H11B H 0.5196 0.1620 1.3366 0.052 Uiso 1 1 calc R . . H11C H 0.4842 0.1959 1.3839 0.052 Uiso 1 1 calc R . . C12 C 0.57550(6) 0.28163(6) 1.14397(16) 0.0236(3) Uani 1 1 d D . . H12 H 0.6016(7) 0.3015(7) 1.2299(14) 0.028 Uiso 1 1 d D . . C13 C 0.69266(7) 0.14018(6) 1.24650(18) 0.0317(3) Uani 1 1 d . . . H13 H 0.6872 0.1692 1.2992 0.038 Uiso 1 1 calc R . . C14 C 0.74336(8) 0.13531(8) 1.2750(2) 0.0450(4) Uani 1 1 d . . . H14 H 0.7720 0.1606 1.3469 0.054 Uiso 1 1 calc R . . C15 C 0.75183(8) 0.09379(10) 1.1989(2) 0.0511(5) Uani 1 1 d . . . H15 H 0.7861 0.0901 1.2185 0.061 Uiso 1 1 calc R . . C16 C 0.71054(9) 0.05774(9) 1.0947(2) 0.0479(5) Uani 1 1 d . . . H16 H 0.7166 0.0293 1.0415 0.057 Uiso 1 1 calc R . . C17 C 0.65988(8) 0.06219(7) 1.06559(18) 0.0364(4) Uani 1 1 d . . . H17 H 0.6318 0.0369 0.9927 0.044 Uiso 1 1 calc R . . C18 C 0.64992(7) 0.10341(6) 1.14235(17) 0.0264(3) Uani 1 1 d . . . C19 C 0.59601(7) 0.11203(6) 1.11264(17) 0.0293(3) Uani 1 1 d . . . H19 H 0.5886 0.1273 1.2082 0.035 Uiso 1 1 calc R . . C20 C 0.53863(7) 0.05269(7) 1.0809(2) 0.0471(4) Uani 1 1 d . . . H20A H 0.5047 0.0598 1.0721 0.071 Uiso 1 1 calc R . . H20B H 0.5311 0.0246 1.1628 0.071 Uiso 1 1 calc R . . H20C H 0.5432 0.0357 0.9874 0.071 Uiso 1 1 calc R . . C21 C 0.62134(6) 0.14420(6) 0.85246(16) 0.0253(3) Uani 1 1 d . . . H21A H 0.5869 0.1051 0.8221 0.030 Uiso 1 1 calc R . . H21B H 0.6577 0.1402 0.8535 0.030 Uiso 1 1 calc R . . C22 C 0.62963(6) 0.19197(6) 0.74047(15) 0.0235(3) Uani 1 1 d . . . C23 C 0.63779(6) 0.17678(7) 0.58179(17) 0.0293(3) Uani 1 1 d . . . H23A H 0.5988 0.1467 0.5411 0.044 Uiso 1 1 calc R . . H23B H 0.6652 0.1607 0.5814 0.044 Uiso 1 1 calc R . . H23C H 0.6547 0.2131 0.5203 0.044 Uiso 1 1 calc R . . C24 C 0.62652(6) 0.24086(6) 0.78205(16) 0.0234(3) Uani 1 1 d D . . H24 H 0.6326(8) 0.2650(6) 0.6938(14) 0.028 Uiso 1 1 d D . . Li1 Li 0.54377(11) 0.17095(11) 0.9005(3) 0.0281(5) Uani 1 1 d . . . Li2 Li 0.50495(11) 0.29326(11) 1.0306(3) 0.0274(5) Uani 1 1 d . . . Li3 Li 0.57557(10) 0.27909(10) 0.8755(3) 0.0259(5) Uani 1 1 d . . . Li4 Li 0.63058(11) 0.24383(11) 1.0455(3) 0.0273(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0209(6) 0.0210(6) 0.0227(6) 0.0000(4) -0.0009(4) 0.0098(5) N2 0.0253(6) 0.0209(6) 0.0278(7) 0.0027(5) 0.0028(5) 0.0124(5) C1 0.0205(7) 0.0230(7) 0.0313(8) -0.0006(5) -0.0021(5) 0.0072(6) C2 0.0277(8) 0.0320(8) 0.0411(9) -0.0062(7) -0.0038(6) 0.0171(6) C3 0.0400(8) 0.0251(7) 0.0462(10) -0.0038(6) -0.0090(7) 0.0180(7) C4 0.0397(9) 0.0228(7) 0.0421(9) 0.0066(6) -0.0028(7) 0.0104(7) C5 0.0303(8) 0.0263(7) 0.0298(8) 0.0035(6) 0.0012(6) 0.0095(6) C6 0.0216(7) 0.0220(7) 0.0251(7) -0.0017(5) -0.0050(5) 0.0101(6) C7 0.0186(6) 0.0228(6) 0.0271(7) -0.0009(5) -0.0015(5) 0.0091(5) C8 0.0305(7) 0.0256(7) 0.0312(7) -0.0007(5) -0.0057(5) 0.0148(6) C9 0.0219(7) 0.0215(7) 0.0255(7) 0.0015(5) 0.0037(5) 0.0098(5) C10 0.0251(7) 0.0263(7) 0.0239(7) -0.0008(5) 0.0008(5) 0.0163(6) C11 0.0345(8) 0.0367(8) 0.0275(8) 0.0036(6) 0.0017(6) 0.0141(7) C12 0.0206(7) 0.0255(7) 0.0266(7) -0.0015(5) -0.0006(5) 0.0130(6) C13 0.0339(8) 0.0245(8) 0.0335(8) 0.0040(6) 0.0001(6) 0.0122(6) C14 0.0318(8) 0.0364(9) 0.0544(11) 0.0098(8) -0.0095(8) 0.0077(7) C15 0.0317(9) 0.0585(12) 0.0709(13) 0.0173(10) 0.0064(9) 0.0283(9) C16 0.0593(12) 0.0587(11) 0.0477(11) 0.0046(9) 0.0104(9) 0.0460(10) C17 0.0470(9) 0.0383(9) 0.0321(9) -0.0027(6) -0.0020(7) 0.0275(8) C18 0.0280(7) 0.0213(7) 0.0295(7) 0.0066(5) 0.0053(6) 0.0119(6) C19 0.0255(7) 0.0262(7) 0.0369(8) 0.0073(6) 0.0053(6) 0.0134(6) C20 0.0282(8) 0.0333(8) 0.0706(12) 0.0214(8) 0.0014(7) 0.0084(7) C21 0.0214(6) 0.0225(7) 0.0331(8) -0.0018(5) 0.0004(5) 0.0118(5) C22 0.0168(6) 0.0235(7) 0.0272(7) -0.0036(5) -0.0011(5) 0.0078(5) C23 0.0287(7) 0.0322(8) 0.0285(7) -0.0036(6) -0.0007(6) 0.0164(6) C24 0.0186(6) 0.0230(7) 0.0265(7) 0.0015(5) -0.0007(5) 0.0089(6) Li1 0.0239(12) 0.0254(12) 0.0350(14) 0.0024(10) 0.0021(10) 0.0124(10) Li2 0.0250(12) 0.0236(11) 0.0323(13) -0.0018(9) 0.0011(10) 0.0112(10) Li3 0.0231(11) 0.0228(11) 0.0307(13) 0.0003(9) 0.0021(9) 0.0107(9) Li4 0.0226(11) 0.0297(12) 0.0313(13) -0.0023(10) -0.0017(9) 0.0144(10) _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 N1 C9 1.4579(18) . ? N1 C7 1.4711(17) . ? N1 Li3 2.046(3) . ? N1 Li2 2.111(3) . ? N1 Li1 2.135(3) . ? N2 C21 1.4604(19) . ? N2 C19 1.4699(18) . ? N2 Li4 2.002(3) . ? N2 Li1 2.094(3) . ? N2 Li2 2.157(3) 2_655 ? C1 C2 1.391(2) . ? C1 C6 1.401(2) . ? C1 Li1 2.538(3) . ? C2 C3 1.391(2) . ? C3 C4 1.379(3) . ? C4 C5 1.395(2) . ? C5 C6 1.389(2) . ? C6 C7 1.5285(19) . ? C6 Li1 2.648(3) . ? C7 C8 1.5193(19) . ? C9 C10 1.5216(19) . ? C9 Li1 2.445(3) . ? C9 Li2 2.533(3) . ? C10 C12 1.350(2) . ? C10 C11 1.505(2) . ? C10 Li2 2.533(3) . ? C10 Li4 2.706(3) . ? C12 Li4 2.152(3) 3_665 ? C12 Li2 2.227(3) . ? C12 Li4 2.261(3) . ? C12 Li3 2.408(3) . ? C13 C18 1.391(2) . ? C13 C14 1.395(2) . ? C13 Li2 2.568(3) 2_655 ? C14 C15 1.373(3) . ? C15 C16 1.370(3) . ? C16 C17 1.389(3) . ? C17 C18 1.391(2) . ? C18 C19 1.534(2) . ? C18 Li2 2.613(3) 2_655 ? C19 C20 1.529(2) . ? C21 C22 1.517(2) . ? C21 Li1 2.453(3) . ? C21 Li2 2.565(3) 2_655 ? C22 C24 1.352(2) . ? C22 C23 1.517(2) . ? C22 Li1 2.457(3) . ? C24 Li3 2.163(3) . ? C24 Li1 2.251(3) . ? C24 Li3 2.274(3) 2_655 ? C24 Li4 2.364(3) . ? Li1 Li4 2.451(3) . ? Li1 Li3 2.487(3) . ? Li2 N2 2.157(3) 3_665 ? Li2 Li3 2.456(3) . ? Li2 Li4 2.482(3) 3_665 ? Li2 C21 2.565(3) 3_665 ? Li2 C13 2.568(3) 3_665 ? Li2 C18 2.613(3) 3_665 ? Li3 C24 2.274(3) 3_665 ? Li3 Li4 2.532(3) 3_665 ? Li3 Li4 2.537(3) . ? Li3 Li3 3.537(4) 3_665 ? Li3 Li3 3.537(4) 2_655 ? Li4 C12 2.152(3) 2_655 ? Li4 Li2 2.482(3) 2_655 ? Li4 Li3 2.532(3) 2_655 ? Li4 Li4 3.476(4) 2_655 ? Li4 Li4 3.476(4) 3_665 ? 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 C9 N1 C7 109.43(10) . . ? C9 N1 Li3 118.08(11) . . ? C7 N1 Li3 131.10(11) . . ? C9 N1 Li2 88.47(10) . . ? C7 N1 Li2 121.40(11) . . ? Li3 N1 Li2 72.41(10) . . ? C9 N1 Li1 83.46(10) . . ? C7 N1 Li1 102.80(11) . . ? Li3 N1 Li1 72.96(10) . . ? Li2 N1 Li1 135.14(10) . . ? C21 N2 C19 113.57(11) . . ? C21 N2 Li4 119.42(11) . . ? C19 N2 Li4 126.09(12) . . ? C21 N2 Li1 85.28(10) . . ? C19 N2 Li1 121.42(11) . . ? Li4 N2 Li1 73.45(11) . . ? C21 N2 Li2 88.12(10) . 2_655 ? C19 N2 Li2 100.12(11) . 2_655 ? Li4 N2 Li2 73.19(10) . 2_655 ? Li1 N2 Li2 136.98(9) . 2_655 ? C2 C1 C6 121.21(14) . . ? C2 C1 Li1 116.16(12) . . ? C6 C1 Li1 78.69(10) . . ? C3 C2 C1 119.87(15) . . ? C4 C3 C2 119.77(15) . . ? C3 C4 C5 119.98(15) . . ? C6 C5 C4 121.50(15) . . ? C5 C6 C1 117.64(13) . . ? C5 C6 C7 121.45(13) . . ? C1 C6 C7 120.89(12) . . ? C5 C6 Li1 118.34(11) . . ? C1 C6 Li1 70.04(9) . . ? C7 C6 Li1 81.24(9) . . ? N1 C7 C8 109.81(11) . . ? N1 C7 C6 112.13(11) . . ? C8 C7 C6 111.21(11) . . ? N1 C9 C10 111.95(11) . . ? N1 C9 Li1 60.21(9) . . ? C10 C9 Li1 98.11(10) . . ? N1 C9 Li2 56.41(9) . . ? C10 C9 Li2 72.52(9) . . ? Li1 C9 Li2 104.08(9) . . ? C12 C10 C11 126.26(13) . . ? C12 C10 C9 120.92(13) . . ? C11 C10 C9 112.79(12) . . ? C12 C10 Li2 61.36(9) . . ? C11 C10 Li2 141.16(11) . . ? C9 C10 Li2 72.52(9) . . ? C12 C10 Li4 56.46(9) . . ? C11 C10 Li4 115.02(11) . . ? C9 C10 Li4 102.01(9) . . ? Li2 C10 Li4 100.30(9) . . ? C10 C12 Li4 155.27(12) . 3_665 ? C10 C12 Li2 86.50(11) . . ? Li4 C12 Li2 69.05(10) 3_665 . ? C10 C12 Li4 93.68(11) . . ? Li4 C12 Li4 103.92(14) 3_665 . ? Li2 C12 Li4 127.45(11) . . ? C10 C12 Li3 105.92(11) . . ? Li4 C12 Li3 67.20(10) 3_665 . ? Li2 C12 Li3 63.85(9) . . ? Li4 C12 Li3 65.74(10) . . ? C18 C13 C14 121.23(16) . . ? C18 C13 Li2 76.22(10) . 2_655 ? C14 C13 Li2 113.53(12) . 2_655 ? C15 C14 C13 119.86(18) . . ? C16 C15 C14 119.65(16) . . ? C15 C16 C17 120.93(17) . . ? C16 C17 C18 120.54(16) . . ? C13 C18 C17 117.78(14) . . ? C13 C18 C19 118.87(13) . . ? C17 C18 C19 123.29(14) . . ? C13 C18 Li2 72.64(10) . 2_655 ? C17 C18 Li2 113.89(12) . 2_655 ? C19 C18 Li2 81.01(9) . 2_655 ? N2 C19 C20 115.07(13) . . ? N2 C19 C18 111.21(11) . . ? C20 C19 C18 112.31(12) . . ? N2 C21 C22 110.95(11) . . ? N2 C21 Li1 58.32(9) . . ? C22 C21 Li1 72.15(9) . . ? N2 C21 Li2 57.20(9) . 2_655 ? C22 C21 Li2 97.92(10) . 2_655 ? Li1 C21 Li2 104.03(9) . 2_655 ? C24 C22 C21 121.43(12) . . ? C24 C22 C23 125.33(13) . . ? C21 C22 C23 113.15(12) . . ? C24 C22 Li1 65.09(10) . . ? C21 C22 Li1 71.85(9) . . ? C23 C22 Li1 135.71(11) . . ? C22 C24 Li3 149.45(12) . . ? C22 C24 Li1 81.89(10) . . ? Li3 C24 Li1 68.56(10) . . ? C22 C24 Li3 98.37(11) . 2_655 ? Li3 C24 Li3 105.70(13) . 2_655 ? Li1 C24 Li3 127.93(11) . 2_655 ? C22 C24 Li4 106.46(11) . . ? Li3 C24 Li4 67.99(10) . . ? Li1 C24 Li4 64.10(10) . . ? Li3 C24 Li4 66.15(10) 2_655 . ? N2 Li1 N1 142.37(14) . . ? N2 Li1 C24 78.52(9) . . ? N1 Li1 C24 104.11(11) . . ? N2 Li1 C9 113.13(12) . . ? N1 Li1 C9 36.34(6) . . ? C24 Li1 C9 127.96(12) . . ? N2 Li1 Li4 51.55(9) . . ? N1 Li1 Li4 96.46(11) . . ? C24 Li1 Li4 60.19(9) . . ? C9 Li1 Li4 87.00(10) . . ? N2 Li1 C21 36.40(6) . . ? N1 Li1 C21 167.93(13) . . ? C24 Li1 C21 64.16(8) . . ? C9 Li1 C21 148.89(12) . . ? Li4 Li1 C21 75.51(10) . . ? N2 Li1 C22 64.66(8) . . ? N1 Li1 C22 133.92(12) . . ? C24 Li1 C22 33.01(6) . . ? C9 Li1 C22 160.11(12) . . ? Li4 Li1 C22 76.48(10) . . ? C21 Li1 C22 36.00(6) . . ? N2 Li1 Li3 111.25(12) . . ? N1 Li1 Li3 51.86(8) . . ? C24 Li1 Li3 54.04(8) . . ? C9 Li1 Li3 75.51(9) . . ? Li4 Li1 Li3 61.82(9) . . ? C21 Li1 Li3 116.07(11) . . ? C22 Li1 Li3 86.82(10) . . ? N2 Li1 C1 130.86(12) . . ? N1 Li1 C1 85.66(9) . . ? C24 Li1 C1 103.76(11) . . ? C9 Li1 C1 103.62(10) . . ? Li4 Li1 C1 163.88(13) . . ? C21 Li1 C1 99.59(10) . . ? C22 Li1 C1 90.50(9) . . ? Li3 Li1 C1 108.63(11) . . ? N2 Li1 C6 145.50(12) . . ? N1 Li1 C6 61.61(7) . . ? C24 Li1 C6 126.50(12) . . ? C9 Li1 C6 72.50(8) . . ? Li4 Li1 C6 157.57(12) . . ? C21 Li1 C6 126.89(11) . . ? C22 Li1 C6 121.38(11) . . ? Li3 Li1 C6 103.15(10) . . ? C1 Li1 C6 31.26(5) . . ? N1 Li2 N2 143.76(14) . 3_665 ? N1 Li2 C12 79.24(9) . . ? N2 Li2 C12 102.32(11) 3_665 . ? N1 Li2 Li3 52.57(8) . . ? N2 Li2 Li3 95.74(11) 3_665 . ? C12 Li2 Li3 61.65(9) . . ? N1 Li2 Li4 111.78(12) . 3_665 ? N2 Li2 Li4 50.54(8) 3_665 3_665 ? C12 Li2 Li4 54.04(9) . 3_665 ? Li3 Li2 Li4 61.70(9) . 3_665 ? N1 Li2 C9 35.13(6) . . ? N2 Li2 C9 164.86(12) 3_665 . ? C12 Li2 C9 62.98(8) . . ? Li3 Li2 C9 74.49(9) . . ? Li4 Li2 C9 114.34(11) 3_665 . ? N1 Li2 C10 63.50(8) . . ? N2 Li2 C10 132.10(12) 3_665 . ? C12 Li2 C10 32.15(6) . . ? Li3 Li2 C10 75.84(9) . . ? Li4 Li2 C10 86.14(10) 3_665 . ? C9 Li2 C10 34.96(5) . . ? N1 Li2 C21 116.44(12) . 3_665 ? N2 Li2 C21 34.69(6) 3_665 3_665 ? C12 Li2 C21 126.14(11) . 3_665 ? Li3 Li2 C21 86.86(10) . 3_665 ? Li4 Li2 C21 72.98(9) 3_665 3_665 ? C9 Li2 C21 151.49(12) . 3_665 ? C10 Li2 C21 157.57(11) . 3_665 ? N1 Li2 C13 128.89(12) . 3_665 ? N2 Li2 C13 86.39(9) 3_665 3_665 ? C12 Li2 C13 103.90(11) . 3_665 ? Li3 Li2 C13 165.53(13) . 3_665 ? Li4 Li2 C13 110.24(12) 3_665 3_665 ? C9 Li2 C13 100.26(10) . 3_665 ? C10 Li2 C13 92.09(10) . 3_665 ? C21 Li2 C13 102.60(10) 3_665 3_665 ? N1 Li2 C18 145.43(12) . 3_665 ? N2 Li2 C18 61.74(7) 3_665 3_665 ? C12 Li2 C18 125.12(12) . 3_665 ? Li3 Li2 C18 156.86(13) . 3_665 ? Li4 Li2 C18 102.74(11) 3_665 3_665 ? C9 Li2 C18 128.65(11) . 3_665 ? C10 Li2 C18 122.42(11) . 3_665 ? C21 Li2 C18 71.56(8) 3_665 3_665 ? C13 Li2 C18 31.14(6) 3_665 3_665 ? N1 Li3 C24 110.55(12) . . ? N1 Li3 C24 134.00(12) . 3_665 ? C24 Li3 C24 107.51(12) . 3_665 ? N1 Li3 C12 76.37(9) . . ? C24 Li3 C12 114.10(11) . . ? C24 Li3 C12 110.19(11) 3_665 . ? N1 Li3 Li2 55.02(9) . . ? C24 Li3 Li2 161.55(13) . . ? C24 Li3 Li2 90.70(10) 3_665 . ? C12 Li3 Li2 54.50(9) . . ? N1 Li3 Li1 55.18(8) . . ? C24 Li3 Li1 57.40(9) . . ? C24 Li3 Li1 162.03(14) 3_665 . ? C12 Li3 Li1 86.32(10) . . ? Li2 Li3 Li1 105.14(13) . . ? N1 Li3 Li4 112.16(11) . 3_665 ? C24 Li3 Li4 127.56(13) . 3_665 ? C24 Li3 Li4 58.63(10) 3_665 3_665 ? C12 Li3 Li4 51.57(7) . 3_665 ? Li2 Li3 Li4 59.67(9) . 3_665 ? Li1 Li3 Li4 137.17(12) . 3_665 ? N1 Li3 Li4 96.22(10) . . ? C24 Li3 Li4 59.78(10) . . ? C24 Li3 Li4 125.31(13) 3_665 . ? C12 Li3 Li4 54.34(7) . . ? Li2 Li3 Li4 107.42(11) . . ? Li1 Li3 Li4 58.39(9) . . ? Li4 Li3 Li4 86.58(13) 3_665 . ? N1 Li3 Li3 157.08(12) . 3_665 ? C24 Li3 Li3 91.45(7) . 3_665 ? C24 Li3 Li3 36.06(8) 3_665 3_665 ? C12 Li3 Li3 89.09(7) . 3_665 ? Li2 Li3 Li3 102.10(11) . 3_665 ? Li1 Li3 Li3 142.60(11) . 3_665 ? Li4 Li3 Li3 45.80(9) 3_665 3_665 ? Li4 Li3 Li3 89.27(9) . 3_665 ? N1 Li3 Li3 136.37(13) . 2_655 ? C24 Li3 Li3 38.24(8) . 2_655 ? C24 Li3 Li3 89.62(7) 3_665 2_655 ? C12 Li3 Li3 90.66(6) . 2_655 ? Li2 Li3 Li3 142.67(8) . 2_655 ? Li1 Li3 Li3 82.94(11) . 2_655 ? Li4 Li3 Li3 89.34(9) 3_665 2_655 ? Li4 Li3 Li3 45.70(9) . 2_655 ? Li3 Li3 Li3 60.000(1) 3_665 2_655 ? N2 Li4 C12 110.54(12) . 2_655 ? N2 Li4 C12 131.84(13) . . ? C12 Li4 C12 106.19(12) 2_655 . ? N2 Li4 C24 77.67(10) . . ? C12 Li4 C24 116.44(12) 2_655 . ? C12 Li4 C24 112.14(11) . . ? N2 Li4 Li1 55.00(9) . . ? C12 Li4 Li1 163.28(13) 2_655 . ? C12 Li4 Li1 90.50(10) . . ? C24 Li4 Li1 55.71(9) . . ? N2 Li4 Li2 56.27(9) . 2_655 ? C12 Li4 Li2 56.91(9) 2_655 2_655 ? C12 Li4 Li2 158.97(14) . 2_655 ? C24 Li4 Li2 87.98(11) . 2_655 ? Li1 Li4 Li2 106.60(13) . 2_655 ? N2 Li4 Li3 97.49(11) . 2_655 ? C12 Li4 Li3 61.23(10) 2_655 2_655 ? C12 Li4 Li3 127.59(14) . 2_655 ? C24 Li4 Li3 55.22(7) . 2_655 ? Li1 Li4 Li3 109.36(11) . 2_655 ? Li2 Li4 Li3 58.63(9) 2_655 2_655 ? N2 Li4 Li3 112.60(11) . . ? C12 Li4 Li3 129.72(14) 2_655 . ? C12 Li4 Li3 59.92(9) . . ? C24 Li4 Li3 52.23(7) . . ? Li1 Li4 Li3 59.79(8) . . ? Li2 Li4 Li3 139.58(13) 2_655 . ? Li3 Li4 Li3 88.51(13) 2_655 . ? N2 Li4 C10 102.41(11) . . ? C12 Li4 C10 122.09(12) 2_655 . ? C12 Li4 C10 29.86(6) . . ? C24 Li4 C10 116.26(10) . . ? Li1 Li4 C10 72.49(9) . . ? Li2 Li4 C10 145.04(13) 2_655 . ? Li3 Li4 C10 155.96(13) 2_655 . ? Li3 Li4 C10 71.51(9) . . ? N2 Li4 Li4 138.11(14) . 2_655 ? C12 Li4 Li4 39.15(9) 2_655 2_655 ? C12 Li4 Li4 89.77(7) . 2_655 ? C24 Li4 Li4 92.11(7) . 2_655 ? Li1 Li4 Li4 144.98(8) . 2_655 ? Li2 Li4 Li4 83.18(12) 2_655 2_655 ? Li3 Li4 Li4 46.76(9) 2_655 2_655 ? Li3 Li4 Li4 90.66(9) . 2_655 ? C10 Li4 Li4 118.26(8) . 2_655 ? N2 Li4 Li4 157.69(13) . 3_665 ? C12 Li4 Li4 91.60(7) 2_655 3_665 ? C12 Li4 Li4 36.94(8) . 3_665 ? C24 Li4 Li4 90.34(7) . 3_665 ? Li1 Li4 Li4 102.71(11) . 3_665 ? Li2 Li4 Li4 143.06(12) 2_655 3_665 ? Li3 Li4 Li4 90.73(9) 2_655 3_665 ? Li3 Li4 Li4 46.66(9) . 3_665 ? C10 Li4 Li4 65.93(9) . 3_665 ? Li4 Li4 Li4 60.0 2_655 3_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.135 _refine_diff_density_min -0.128 _refine_diff_density_rms 0.027 #===END data_vb224mf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 N2 Na2' _chemical_formula_sum 'C24 H32 N2 Na2' _chemical_formula_weight 394.50 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4543(6) _cell_length_b 11.3694(7) _cell_length_c 8.8489(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.044(4) _cell_angle_gamma 90.00 _cell_volume 1122.64(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5260 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6858 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details 'SADABS (SHeldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10457 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 29.79 _reflns_number_total 3178 _reflns_number_gt 2829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_molecular_graphics 'XSEED' _computing_publication_material 'Cif Tab' _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^)+(0.0593P)^2^+0.3904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'constr' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3178 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Na1 Na 0.52048(4) -0.07713(4) -0.13851(5) 0.02258(13) Uani 1 1 d . . . N1 N 0.45171(7) -0.13081(7) 0.10023(10) 0.01801(18) Uani 1 1 d . . . C1 C 0.11547(10) -0.15029(12) -0.05265(16) 0.0332(3) Uani 1 1 d . . . H1A H 0.1009 -0.2241 -0.0028 0.050 Uiso 1 1 calc R . . H1B H 0.1212 -0.1661 -0.1596 0.050 Uiso 1 1 calc R . . H1C H 0.0492 -0.0957 -0.0530 0.050 Uiso 1 1 calc R . . C2 C 0.23194(9) -0.09607(10) 0.03639(13) 0.0237(2) Uani 1 1 d . . . H2 H 0.2490 -0.0245 -0.0206 0.028 Uiso 1 1 calc R . . C3 C 0.22033(10) -0.05923(11) 0.19740(15) 0.0301(3) Uani 1 1 d . . . H3A H 0.1665 0.0086 0.1891 0.045 Uiso 1 1 calc R . . H3B H 0.2994 -0.0379 0.2601 0.045 Uiso 1 1 calc R . . H3C H 0.1876 -0.1247 0.2469 0.045 Uiso 1 1 calc R . . C4 C 0.33431(9) -0.18292(9) 0.04482(13) 0.0211(2) Uani 1 1 d . . . H4A H 0.3245 -0.2484 0.1146 0.025 Uiso 1 1 calc R . . H4B H 0.3296 -0.2163 -0.0597 0.025 Uiso 1 1 calc R . . C5 C 0.53942(9) -0.21183(8) 0.12652(11) 0.01730(19) Uani 1 1 d . . . C6 C 0.52939(10) -0.33134(9) 0.09764(12) 0.0217(2) Uani 1 1 d . . . H6A H 0.4533 -0.3649 0.0540 0.026 Uiso 1 1 calc R . . H6B H 0.5986 -0.3799 0.1215 0.026 Uiso 1 1 calc R . . C7 C 0.66251(9) -0.16451(9) 0.19419(11) 0.01832(19) Uani 1 1 d . . . C8 C 0.76289(10) -0.20671(10) 0.14713(14) 0.0255(2) Uani 1 1 d . . . H8 H 0.7537 -0.2661 0.0698 0.031 Uiso 1 1 calc R . . C9 C 0.87631(10) -0.16271(12) 0.21223(16) 0.0329(3) Uani 1 1 d . . . H9 H 0.9441 -0.1924 0.1794 0.039 Uiso 1 1 calc R . . C10 C 0.89105(11) -0.07641(12) 0.32404(16) 0.0335(3) Uani 1 1 d . . . H10 H 0.9688 -0.0467 0.3683 0.040 Uiso 1 1 calc R . . C11 C 0.79181(10) -0.03282(11) 0.37209(13) 0.0273(2) Uani 1 1 d . . . H11 H 0.8014 0.0271 0.4487 0.033 Uiso 1 1 calc R . . C12 C 0.67913(9) -0.07713(9) 0.30781(12) 0.0213(2) Uani 1 1 d . . . H12 H 0.6118 -0.0475 0.3416 0.026 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 Na1 0.0357(3) 0.0156(2) 0.0185(2) -0.00091(14) 0.01038(17) -0.00007(16) N1 0.0168(4) 0.0156(4) 0.0211(4) 0.0017(3) 0.0034(3) -0.0006(3) C1 0.0196(5) 0.0359(6) 0.0408(7) -0.0022(5) 0.0003(5) -0.0045(4) C2 0.0180(4) 0.0214(5) 0.0304(5) 0.0018(4) 0.0024(4) -0.0015(4) C3 0.0232(5) 0.0301(6) 0.0385(6) -0.0066(5) 0.0098(4) -0.0004(4) C4 0.0189(4) 0.0170(4) 0.0278(5) 0.0003(4) 0.0060(4) -0.0024(3) C5 0.0219(4) 0.0164(4) 0.0147(4) 0.0028(3) 0.0064(3) 0.0004(3) C6 0.0288(5) 0.0157(4) 0.0223(5) 0.0019(3) 0.0092(4) 0.0017(4) C7 0.0190(4) 0.0169(4) 0.0185(4) 0.0053(3) 0.0032(3) 0.0032(3) C8 0.0224(5) 0.0252(5) 0.0297(5) 0.0009(4) 0.0072(4) 0.0062(4) C9 0.0184(5) 0.0400(7) 0.0395(6) 0.0027(5) 0.0054(4) 0.0087(4) C10 0.0195(5) 0.0420(7) 0.0348(6) 0.0039(5) -0.0025(4) -0.0004(5) C11 0.0264(5) 0.0300(6) 0.0222(5) -0.0003(4) -0.0013(4) -0.0019(4) C12 0.0207(5) 0.0237(5) 0.0191(4) 0.0024(4) 0.0038(3) 0.0022(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 Na1 N1 2.3994(9) 3_655 ? Na1 N1 2.4914(9) . ? Na1 C6 2.5792(11) 4 ? Na1 C12 3.0003(11) 3_655 ? Na1 Na1 3.1344(8) 3_655 ? N1 C5 1.3440(13) . ? N1 C4 1.4499(12) . ? N1 Na1 2.3994(9) 3_655 ? C1 C2 1.5186(15) . ? C2 C3 1.5195(17) . ? C2 C4 1.5219(15) . ? C5 C6 1.3825(14) . ? C5 C7 1.5015(14) . ? C6 Na1 2.5792(11) 4_556 ? C7 C8 1.3935(14) . ? C7 C12 1.3956(15) . ? C8 C9 1.3899(16) . ? C9 C10 1.3766(19) . ? C10 C11 1.3916(18) . ? C11 C12 1.3827(15) . ? C12 Na1 3.0003(11) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Na1 N1 100.31(3) 3_655 . ? N1 Na1 C6 119.62(3) 3_655 4 ? N1 Na1 C6 138.89(3) . 4 ? N1 Na1 C12 63.67(3) 3_655 3_655 ? N1 Na1 C12 102.44(3) . 3_655 ? C6 Na1 C12 88.01(3) 4 3_655 ? N1 Na1 Na1 51.45(2) 3_655 3_655 ? N1 Na1 Na1 48.86(2) . 3_655 ? C6 Na1 Na1 167.75(3) 4 3_655 ? C12 Na1 Na1 80.31(3) 3_655 3_655 ? C5 N1 C4 112.24(8) . . ? C5 N1 Na1 125.49(7) . 3_655 ? C4 N1 Na1 122.26(6) . 3_655 ? C5 N1 Na1 87.00(6) . . ? C4 N1 Na1 105.07(6) . . ? Na1 N1 Na1 79.69(3) 3_655 . ? C1 C2 C3 110.23(10) . . ? C1 C2 C4 109.81(9) . . ? C3 C2 C4 111.25(9) . . ? N1 C4 C2 113.39(8) . . ? N1 C5 C6 127.87(10) . . ? N1 C5 C7 114.92(8) . . ? C6 C5 C7 117.21(9) . . ? C5 C6 Na1 104.35(7) . 4_556 ? C8 C7 C12 118.22(10) . . ? C8 C7 C5 121.42(9) . . ? C12 C7 C5 120.36(9) . . ? C9 C8 C7 120.61(11) . . ? C10 C9 C8 120.40(11) . . ? C9 C10 C11 119.82(11) . . ? C12 C11 C10 119.71(11) . . ? C11 C12 C7 121.24(10) . . ? C11 C12 Na1 121.86(8) . 3_655 ? C7 C12 Na1 95.26(6) . 3_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.522 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.048