# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email JOHN.HAGADORN@COLORADO.EDU _publ_contact_author_name 'Prof John Hagadorn' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Colorado 215 UCB Boulder CO 80309-0215 UNITED STATES OF AMERICA ; _publ_section_title ; New dibenzofuran-bridged bis(amidoamine) and bis(ethylenediamine) ligands and their dinuclear zinc and aluminum complexes ; _publ_author_name 'John Hagadorn' data_compound_3 _database_code_CSD 217505 _chemical_name_common LH2Zn2Cl4aCH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Cl6 N4 O Zn2' _chemical_formula_weight 697.93 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 13.9254(6) _cell_length_b 18.4546(7) _cell_length_c 11.2231(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2884.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 158(2) _cell_measurement_reflns_used 6149 _cell_measurement_theta_min 2.207 _cell_measurement_theta_max 31.254 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 2.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; absorption correction applied using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 158(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 ? _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 17210 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4544 _reflns_number_gt 4191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0260P)^2^+1.3926P] 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 0.078(14) _refine_ls_number_reflns 4544 _refine_ls_number_parameters 319 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.42184(3) 0.38922(2) 0.37680(5) 0.03008(13) Uani 1 1 d . . . Zn2 Zn 0.52921(3) 0.11807(2) 0.39040(5) 0.02881(13) Uani 1 1 d . . . Cl1 Cl 0.31221(9) 0.46303(6) 0.45495(12) 0.0418(3) Uani 1 1 d . . . Cl2 Cl 0.52730(8) 0.34070(5) 0.50164(11) 0.0346(2) Uani 1 1 d . . . Cl3 Cl 0.54605(8) 0.20198(6) 0.24870(11) 0.0388(3) Uani 1 1 d . . . Cl4 Cl 0.44837(8) 0.01739(6) 0.35596(12) 0.0422(3) Uani 1 1 d . . . Cl5 Cl 0.81428(9) 0.32499(7) 0.25171(14) 0.0502(3) Uani 1 1 d . . . Cl6 Cl 0.84294(9) 0.28824(7) 0.50240(12) 0.0457(3) Uani 1 1 d . . . O1 O 0.34609(19) 0.22746(15) 0.4315(3) 0.0296(7) Uani 1 1 d . . . N1 N 0.4852(3) 0.43792(19) 0.2292(4) 0.0357(9) Uani 1 1 d . . . N2 N 0.3439(3) 0.32609(19) 0.2509(4) 0.0335(8) Uani 1 1 d . . . N3 N 0.4899(2) 0.16367(18) 0.5587(3) 0.0264(8) Uani 1 1 d . . . N4 N 0.6619(3) 0.09806(18) 0.4705(3) 0.0302(8) Uani 1 1 d . . . C1 C 0.5913(4) 0.4305(3) 0.2306(6) 0.0518(13) Uani 1 1 d . . . H1A H 0.6085 0.3794 0.2401 0.078 Uiso 1 1 calc R . . H1B H 0.6177 0.4586 0.2970 0.078 Uiso 1 1 calc R . . H1C H 0.6177 0.4488 0.1554 0.078 Uiso 1 1 calc R . . C2 C 0.4591(5) 0.5160(3) 0.2238(6) 0.0555(15) Uani 1 1 d . . . H2A H 0.4838 0.5408 0.2947 0.083 Uiso 1 1 calc R . . H2B H 0.3891 0.5209 0.2209 0.083 Uiso 1 1 calc R . . H2C H 0.4873 0.5378 0.1523 0.083 Uiso 1 1 calc R . . C3 C 0.4444(4) 0.3996(3) 0.1232(5) 0.0415(12) Uani 1 1 d . . . H3A H 0.4845 0.3569 0.1041 0.058 Uiso 1 1 calc R . . H3B H 0.4453 0.4325 0.0535 0.058 Uiso 1 1 calc R . . C4 C 0.3425(4) 0.3756(3) 0.1476(5) 0.0412(12) Uani 1 1 d . . . H4A H 0.3015 0.4181 0.1650 0.058 Uiso 1 1 calc R . . H4B H 0.3160 0.3504 0.0770 0.058 Uiso 1 1 calc R . . C5 C 0.2546(3) 0.3001(2) 0.2954(5) 0.0352(10) Uani 1 1 d . . . C6 C 0.1626(4) 0.3206(3) 0.2605(5) 0.0421(12) Uani 1 1 d . . . H6 H 0.1540 0.3534 0.1963 0.051 Uiso 1 1 calc R . . C7 C 0.0823(4) 0.2922(3) 0.3212(6) 0.0473(14) Uani 1 1 d . . . H7 H 0.0202 0.3065 0.2953 0.057 Uiso 1 1 calc R . . C8 C 0.0888(3) 0.2449(3) 0.4159(5) 0.0435(13) Uani 1 1 d . . . H8 H 0.0330 0.2277 0.4556 0.052 Uiso 1 1 calc R . . C9 C 0.1811(3) 0.2231(2) 0.4514(5) 0.0347(10) Uani 1 1 d . . . C10 C 0.2586(3) 0.25120(19) 0.3887(5) 0.0324(9) Uani 1 1 d . . . C11 C 0.3219(3) 0.1833(2) 0.5265(4) 0.0292(9) Uani 1 1 d . . . C12 C 0.2239(3) 0.1783(2) 0.5439(4) 0.0339(10) Uani 1 1 d . . . C13 C 0.1921(3) 0.1361(2) 0.6409(5) 0.0367(11) Uani 1 1 d . . . H13 H 0.1256 0.1304 0.6571 0.044 Uiso 1 1 calc R . . C14 C 0.2611(4) 0.1032(2) 0.7119(5) 0.0377(11) Uani 1 1 d . . . H14 H 0.2403 0.0748 0.7777 0.045 Uiso 1 1 calc R . . C15 C 0.3596(3) 0.1098(2) 0.6911(5) 0.0331(10) Uani 1 1 d . . . H15 H 0.4042 0.0861 0.7420 0.040 Uiso 1 1 calc R . . C16 C 0.3924(3) 0.1510(2) 0.5959(4) 0.0291(9) Uani 1 1 d . . . C17 C 0.5671(3) 0.1425(2) 0.6422(4) 0.0295(9) Uani 1 1 d . . . H17A H 0.5563 0.0925 0.6714 0.041 Uiso 1 1 calc R . . H17B H 0.5681 0.1756 0.7116 0.041 Uiso 1 1 calc R . . C18 C 0.6615(3) 0.1468(2) 0.5753(4) 0.0327(10) Uani 1 1 d . . . H18A H 0.6723 0.1973 0.5486 0.046 Uiso 1 1 calc R . . H18B H 0.7147 0.1333 0.6294 0.046 Uiso 1 1 calc R . . C19 C 0.6720(4) 0.0210(2) 0.5089(5) 0.0453(12) Uani 1 1 d . . . H19A H 0.6725 -0.0105 0.4386 0.068 Uiso 1 1 calc R . . H19B H 0.6179 0.0078 0.5605 0.068 Uiso 1 1 calc R . . H19C H 0.7323 0.0150 0.5529 0.068 Uiso 1 1 calc R . . C20 C 0.7436(3) 0.1160(2) 0.3916(6) 0.0417(11) Uani 1 1 d . . . H20A H 0.7371 0.1660 0.3634 0.063 Uiso 1 1 calc R . . H20B H 0.7439 0.0830 0.3232 0.063 Uiso 1 1 calc R . . H20C H 0.8038 0.1109 0.4359 0.063 Uiso 1 1 calc R . . C21 C 0.7755(4) 0.3395(3) 0.3993(6) 0.0503(13) Uani 1 1 d . . . H21A H 0.7069 0.3261 0.4061 0.070 Uiso 1 1 calc R . . H21B H 0.7816 0.3916 0.4189 0.070 Uiso 1 1 calc R . . H1 H 0.381(3) 0.292(2) 0.232(4) 0.020(11) Uiso 1 1 d . . . H2 H 0.500(3) 0.210(3) 0.545(5) 0.032(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0381(3) 0.0292(2) 0.0230(3) 0.0014(2) -0.0003(2) -0.00177(18) Zn2 0.0306(2) 0.0299(2) 0.0260(3) 0.0009(2) -0.0012(2) -0.00100(17) Cl1 0.0512(7) 0.0373(5) 0.0368(7) -0.0030(5) 0.0120(6) 0.0002(5) Cl2 0.0420(6) 0.0314(5) 0.0304(6) 0.0009(4) -0.0062(5) -0.0031(4) Cl3 0.0424(6) 0.0415(6) 0.0324(6) 0.0094(5) -0.0002(5) -0.0001(5) Cl4 0.0423(6) 0.0345(5) 0.0498(8) -0.0055(5) -0.0055(6) -0.0065(5) Cl5 0.0449(7) 0.0626(8) 0.0433(8) -0.0053(6) -0.0029(6) 0.0010(6) Cl6 0.0375(6) 0.0559(7) 0.0438(8) -0.0031(6) 0.0007(6) -0.0048(5) O1 0.0261(14) 0.0312(14) 0.0315(18) -0.0015(12) -0.0027(12) 0.0038(11) N1 0.044(2) 0.0343(19) 0.029(2) 0.0033(16) 0.0022(18) 0.0030(16) N2 0.038(2) 0.0289(17) 0.034(2) -0.0032(17) -0.0030(19) 0.0095(16) N3 0.0238(18) 0.0238(17) 0.032(2) 0.0027(15) 0.0021(15) -0.0031(13) N4 0.0325(19) 0.0281(16) 0.030(2) 0.0037(15) 0.0047(17) 0.0059(14) C1 0.045(3) 0.070(3) 0.041(3) 0.010(3) 0.003(3) -0.004(3) C2 0.082(4) 0.034(3) 0.050(4) 0.013(2) 0.016(3) 0.006(2) C3 0.056(3) 0.050(3) 0.019(2) 0.004(2) 0.005(2) 0.014(2) C4 0.054(3) 0.046(3) 0.023(3) -0.001(2) -0.013(2) 0.015(2) C5 0.034(2) 0.036(2) 0.035(3) -0.0131(19) -0.006(2) 0.0086(19) C6 0.042(3) 0.041(2) 0.043(3) -0.010(2) -0.014(2) 0.010(2) C7 0.033(3) 0.047(3) 0.062(4) -0.020(3) -0.020(3) 0.011(2) C8 0.024(2) 0.047(3) 0.059(4) -0.024(2) -0.006(2) 0.0052(18) C9 0.029(2) 0.036(2) 0.039(3) -0.015(2) 0.001(2) 0.0015(18) C10 0.026(2) 0.0331(19) 0.038(3) -0.011(2) -0.010(2) 0.0070(15) C11 0.030(2) 0.0269(19) 0.031(3) -0.0033(17) 0.003(2) 0.0011(17) C12 0.031(2) 0.031(2) 0.040(3) -0.0144(19) 0.002(2) -0.0014(17) C13 0.031(3) 0.036(2) 0.043(3) -0.014(2) 0.012(2) -0.0072(19) C14 0.043(3) 0.031(2) 0.039(3) -0.004(2) 0.008(2) -0.0037(19) C15 0.036(2) 0.032(2) 0.032(3) -0.0026(18) 0.007(2) 0.0011(17) C16 0.030(2) 0.026(2) 0.032(3) -0.0062(17) 0.0030(19) -0.0015(17) C17 0.028(2) 0.036(2) 0.024(2) 0.0014(18) -0.0020(18) 0.0020(17) C18 0.027(2) 0.039(2) 0.032(3) 0.002(2) -0.0047(19) 0.0034(18) C19 0.049(3) 0.034(2) 0.052(3) 0.011(2) -0.002(3) 0.011(2) C20 0.038(2) 0.051(2) 0.036(3) 0.003(2) 0.007(3) 0.0039(19) C21 0.048(3) 0.051(3) 0.052(4) 0.005(3) 0.016(3) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.080(4) . ? Zn1 N2 2.129(4) . ? Zn1 Cl2 2.2185(12) . ? Zn1 Cl1 2.2261(13) . ? Zn1 Zn2 5.2249(6) . ? Zn2 N4 2.087(4) . ? Zn2 N3 2.139(4) . ? Zn2 Cl4 2.2065(12) . ? Zn2 Cl3 2.2321(12) . ? Cl5 C21 1.763(6) . ? Cl6 C21 1.765(6) . ? O1 C10 1.381(5) . ? O1 C11 1.383(5) . ? N1 C1 1.484(6) . ? N1 C2 1.488(6) . ? N1 C3 1.496(7) . ? N2 C5 1.424(6) . ? N2 C4 1.476(6) . ? N3 C16 1.439(5) . ? N3 C17 1.479(6) . ? N4 C20 1.479(6) . ? N4 C18 1.480(6) . ? N4 C19 1.493(5) . ? C3 C4 1.512(7) . ? C5 C10 1.383(7) . ? C5 C6 1.391(7) . ? C6 C7 1.410(8) . ? C7 C8 1.379(8) . ? C8 C9 1.404(6) . ? C9 C10 1.390(7) . ? C9 C12 1.455(7) . ? C11 C12 1.382(6) . ? C11 C16 1.388(6) . ? C12 C13 1.409(7) . ? C13 C14 1.388(7) . ? C14 C15 1.398(7) . ? C15 C16 1.389(6) . ? C17 C18 1.516(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 N1 Zn1 N2 85.64(16) . . ? N1 Zn1 Cl2 113.36(11) . . ? N2 Zn1 Cl2 122.39(10) . . ? N1 Zn1 Cl1 109.88(11) . . ? N2 Zn1 Cl1 104.29(11) . . ? Cl2 Zn1 Cl1 116.88(5) . . ? N1 Zn1 Zn2 108.40(10) . . ? N2 Zn1 Zn2 68.97(10) . . ? Cl2 Zn1 Zn2 53.53(3) . . ? Cl1 Zn1 Zn2 140.42(3) . . ? N4 Zn2 N3 85.17(14) . . ? N4 Zn2 Cl4 112.21(10) . . ? N3 Zn2 Cl4 110.82(10) . . ? N4 Zn2 Cl3 109.67(11) . . ? N3 Zn2 Cl3 112.53(10) . . ? Cl4 Zn2 Cl3 120.86(5) . . ? N4 Zn2 Zn1 115.80(10) . . ? N3 Zn2 Zn1 64.90(9) . . ? Cl4 Zn2 Zn1 130.94(4) . . ? Cl3 Zn2 Zn1 49.06(3) . . ? C10 O1 C11 103.9(3) . . ? C1 N1 C2 109.4(4) . . ? C1 N1 C3 110.0(4) . . ? C2 N1 C3 109.4(4) . . ? C1 N1 Zn1 112.0(3) . . ? C2 N1 Zn1 110.3(3) . . ? C3 N1 Zn1 105.6(3) . . ? C5 N2 C4 118.2(4) . . ? C5 N2 Zn1 113.4(3) . . ? C4 N2 Zn1 100.9(3) . . ? C16 N3 C17 117.3(4) . . ? C16 N3 Zn2 115.7(3) . . ? C17 N3 Zn2 105.6(3) . . ? C20 N4 C18 110.0(4) . . ? C20 N4 C19 108.3(3) . . ? C18 N4 C19 110.5(4) . . ? C20 N4 Zn2 112.5(3) . . ? C18 N4 Zn2 103.4(2) . . ? C19 N4 Zn2 112.1(3) . . ? N1 C3 C4 110.5(4) . . ? N2 C4 C3 108.1(4) . . ? C10 C5 C6 115.3(5) . . ? C10 C5 N2 116.7(4) . . ? C6 C5 N2 127.9(5) . . ? C5 C6 C7 119.6(5) . . ? C8 C7 C6 123.7(4) . . ? C7 C8 C9 117.4(5) . . ? C10 C9 C8 117.4(5) . . ? C10 C9 C12 104.8(4) . . ? C8 C9 C12 137.8(5) . . ? O1 C10 C5 120.4(4) . . ? O1 C10 C9 113.0(4) . . ? C5 C10 C9 126.5(4) . . ? C12 C11 O1 112.9(4) . . ? C12 C11 C16 126.2(4) . . ? O1 C11 C16 120.9(4) . . ? C11 C12 C13 117.1(4) . . ? C11 C12 C9 105.4(4) . . ? C13 C12 C9 137.4(4) . . ? C14 C13 C12 118.0(4) . . ? C13 C14 C15 123.0(5) . . ? C16 C15 C14 119.9(5) . . ? C11 C16 C15 115.7(4) . . ? C11 C16 N3 115.8(4) . . ? C15 C16 N3 128.5(4) . . ? N3 C17 C18 107.6(4) . . ? N4 C18 C17 111.4(4) . . ? Cl5 C21 Cl6 111.8(3) . . ? 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 N1 Zn1 Zn2 N4 83.73(17) . . . . ? N2 Zn1 Zn2 N4 161.39(17) . . . . ? Cl2 Zn1 Zn2 N4 -22.16(12) . . . . ? Cl1 Zn1 Zn2 N4 -111.48(13) . . . . ? N1 Zn1 Zn2 N3 154.47(16) . . . . ? N2 Zn1 Zn2 N3 -127.86(16) . . . . ? Cl2 Zn1 Zn2 N3 48.58(11) . . . . ? Cl1 Zn1 Zn2 N3 -40.73(12) . . . . ? N1 Zn1 Zn2 Cl4 -109.03(13) . . . . ? N2 Zn1 Zn2 Cl4 -31.37(13) . . . . ? Cl2 Zn1 Zn2 Cl4 145.08(7) . . . . ? Cl1 Zn1 Zn2 Cl4 55.76(8) . . . . ? N1 Zn1 Zn2 Cl3 -10.60(12) . . . . ? N2 Zn1 Zn2 Cl3 67.06(13) . . . . ? Cl2 Zn1 Zn2 Cl3 -116.49(6) . . . . ? Cl1 Zn1 Zn2 Cl3 154.19(8) . . . . ? N2 Zn1 N1 C1 -122.2(3) . . . . ? Cl2 Zn1 N1 C1 1.4(4) . . . . ? Cl1 Zn1 N1 C1 134.2(3) . . . . ? Zn2 Zn1 N1 C1 -56.0(3) . . . . ? N2 Zn1 N1 C2 115.7(4) . . . . ? Cl2 Zn1 N1 C2 -120.8(3) . . . . ? Cl1 Zn1 N1 C2 12.1(4) . . . . ? Zn2 Zn1 N1 C2 -178.2(3) . . . . ? N2 Zn1 N1 C3 -2.5(3) . . . . ? Cl2 Zn1 N1 C3 121.1(3) . . . . ? Cl1 Zn1 N1 C3 -106.1(3) . . . . ? Zn2 Zn1 N1 C3 63.7(3) . . . . ? N1 Zn1 N2 C5 -154.4(3) . . . . ? Cl2 Zn1 N2 C5 90.6(3) . . . . ? Cl1 Zn1 N2 C5 -45.0(3) . . . . ? Zn2 Zn1 N2 C5 94.0(3) . . . . ? N1 Zn1 N2 C4 -27.0(3) . . . . ? Cl2 Zn1 N2 C4 -142.0(2) . . . . ? Cl1 Zn1 N2 C4 82.4(3) . . . . ? Zn2 Zn1 N2 C4 -138.6(3) . . . . ? N4 Zn2 N3 C16 -143.0(3) . . . . ? Cl4 Zn2 N3 C16 -31.1(3) . . . . ? Cl3 Zn2 N3 C16 107.6(3) . . . . ? Zn1 Zn2 N3 C16 95.5(3) . . . . ? N4 Zn2 N3 C17 -11.5(3) . . . . ? Cl4 Zn2 N3 C17 100.4(2) . . . . ? Cl3 Zn2 N3 C17 -120.8(2) . . . . ? Zn1 Zn2 N3 C17 -133.0(3) . . . . ? N3 Zn2 N4 C20 -136.7(3) . . . . ? Cl4 Zn2 N4 C20 112.8(3) . . . . ? Cl3 Zn2 N4 C20 -24.5(3) . . . . ? Zn1 Zn2 N4 C20 -77.6(3) . . . . ? N3 Zn2 N4 C18 -18.0(3) . . . . ? Cl4 Zn2 N4 C18 -128.6(2) . . . . ? Cl3 Zn2 N4 C18 94.2(3) . . . . ? Zn1 Zn2 N4 C18 41.1(3) . . . . ? N3 Zn2 N4 C19 101.0(3) . . . . ? Cl4 Zn2 N4 C19 -9.6(3) . . . . ? Cl3 Zn2 N4 C19 -146.8(3) . . . . ? Zn1 Zn2 N4 C19 160.1(3) . . . . ? C1 N1 C3 C4 153.3(4) . . . . ? C2 N1 C3 C4 -86.5(5) . . . . ? Zn1 N1 C3 C4 32.2(4) . . . . ? C5 N2 C4 C3 175.9(4) . . . . ? Zn1 N2 C4 C3 51.7(4) . . . . ? N1 C3 C4 N2 -59.8(5) . . . . ? C4 N2 C5 C10 177.1(4) . . . . ? Zn1 N2 C5 C10 -65.1(4) . . . . ? C4 N2 C5 C6 -6.5(7) . . . . ? Zn1 N2 C5 C6 111.3(5) . . . . ? C10 C5 C6 C7 0.9(6) . . . . ? N2 C5 C6 C7 -175.6(4) . . . . ? C5 C6 C7 C8 0.7(7) . . . . ? C6 C7 C8 C9 -1.3(7) . . . . ? C7 C8 C9 C10 0.3(6) . . . . ? C7 C8 C9 C12 177.5(5) . . . . ? C11 O1 C10 C5 176.9(4) . . . . ? C11 O1 C10 C9 -0.9(4) . . . . ? C6 C5 C10 O1 -179.5(4) . . . . ? N2 C5 C10 O1 -2.6(6) . . . . ? C6 C5 C10 C9 -2.0(7) . . . . ? N2 C5 C10 C9 174.9(4) . . . . ? C8 C9 C10 O1 179.0(4) . . . . ? C12 C9 C10 O1 1.0(5) . . . . ? C8 C9 C10 C5 1.4(7) . . . . ? C12 C9 C10 C5 -176.6(4) . . . . ? C10 O1 C11 C12 0.4(4) . . . . ? C10 O1 C11 C16 -177.7(4) . . . . ? O1 C11 C12 C13 -178.2(3) . . . . ? C16 C11 C12 C13 -0.2(7) . . . . ? O1 C11 C12 C9 0.2(5) . . . . ? C16 C11 C12 C9 178.1(4) . . . . ? C10 C9 C12 C11 -0.7(5) . . . . ? C8 C9 C12 C11 -178.0(5) . . . . ? C10 C9 C12 C13 177.2(5) . . . . ? C8 C9 C12 C13 -0.2(9) . . . . ? C11 C12 C13 C14 0.3(6) . . . . ? C9 C12 C13 C14 -177.4(5) . . . . ? C12 C13 C14 C15 -0.3(7) . . . . ? C13 C14 C15 C16 0.2(7) . . . . ? C12 C11 C16 C15 0.2(6) . . . . ? O1 C11 C16 C15 178.0(4) . . . . ? C12 C11 C16 N3 179.3(4) . . . . ? O1 C11 C16 N3 -2.9(6) . . . . ? C14 C15 C16 C11 -0.1(6) . . . . ? C14 C15 C16 N3 -179.1(4) . . . . ? C17 N3 C16 C11 168.5(4) . . . . ? Zn2 N3 C16 C11 -65.7(4) . . . . ? C17 N3 C16 C15 -12.5(6) . . . . ? Zn2 N3 C16 C15 113.2(4) . . . . ? C16 N3 C17 C18 168.9(3) . . . . ? Zn2 N3 C17 C18 38.3(4) . . . . ? C20 N4 C18 C17 166.4(4) . . . . ? C19 N4 C18 C17 -74.1(4) . . . . ? Zn2 N4 C18 C17 46.0(4) . . . . ? N3 C17 C18 N4 -59.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.440 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.069 #======END data_compound_4 _database_code_CSD 217506 _chemical_name_common L2Li4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Li4 N8 O2' _chemical_formula_weight 704.66 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' O O 0.0106 0.0060 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6476(3) _cell_length_b 21.3387(6) _cell_length_c 17.4505(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.4100(10) _cell_angle_gamma 90.00 _cell_volume 3953.12(19) _cell_formula_units_Z 4 _cell_measurement_temperature 142(2) _cell_measurement_reflns_used 8279 _cell_measurement_theta_min 2.239 _cell_measurement_theta_max 28.930 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.388 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; semi-empirical absorption correction applied using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 142(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 ? _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 30666 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9055 _reflns_number_gt 5746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0513P)^2^+0.8295P] 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 9055 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 O1 O 0.63629(11) 0.20161(6) 0.84202(7) 0.0320(3) Uani 1 1 d . . . N1 N 0.51258(14) 0.04077(7) 0.65156(9) 0.0315(4) Uani 1 1 d . A . N2 N 0.51934(14) 0.09002(7) 0.80276(9) 0.0318(4) Uani 1 1 d . . . N3 N 0.82935(15) 0.27239(7) 0.78966(10) 0.0365(4) Uani 1 1 d . . . N4 N 1.05085(16) 0.22097(8) 0.73666(10) 0.0404(4) Uani 1 1 d . . . Li1 Li 0.5649(3) 0.12486(15) 0.70114(18) 0.0341(7) Uani 1 1 d . A . Li2 Li 0.8932(3) 0.18509(15) 0.78288(19) 0.0365(7) Uani 1 1 d . A . C1 C 0.58424(19) 0.01008(9) 0.59384(12) 0.0374(5) Uani 1 1 d . . . H1A H 0.5408 -0.0284 0.5761 0.056 Uiso 1 1 calc R . . H1B H 0.6687 -0.0003 0.6166 0.056 Uiso 1 1 calc R . . H1C H 0.5912 0.0384 0.5502 0.056 Uiso 1 1 calc R . . C2 C 0.38659(18) 0.05647(10) 0.61611(12) 0.0417(5) Uani 1 1 d . . . H2A H 0.3947 0.0857 0.5735 0.063 Uiso 1 1 calc R . . H2B H 0.3367 0.0760 0.6546 0.063 Uiso 1 1 calc R . . H2C H 0.3445 0.0182 0.5967 0.063 Uiso 1 1 calc R . . C3 C 0.5059(2) -0.00076(9) 0.71876(11) 0.0383(5) Uani 1 1 d . . . H3A H 0.5917 -0.0159 0.7352 0.054 Uiso 1 1 calc R A . H3B H 0.4534 -0.0377 0.7037 0.054 Uiso 1 1 calc R . . C4 C 0.4514(2) 0.03167(9) 0.78552(11) 0.0387(5) Uani 1 1 d . . . H4A H 0.3611 0.0407 0.7725 0.054 Uiso 1 1 calc R . . H4B H 0.4584 0.0040 0.8312 0.054 Uiso 1 1 calc R . . C5 C 0.47045(17) 0.12568(9) 0.85878(10) 0.0338(4) Uani 1 1 d . A . C6 C 0.36778(19) 0.11370(11) 0.90345(11) 0.0419(5) Uani 1 1 d . . . H6 H 0.3207 0.0762 0.8952 0.050 Uiso 1 1 calc R A . C7 C 0.3338(2) 0.15630(12) 0.96000(12) 0.0497(6) Uani 1 1 d . . . H7 H 0.2635 0.1462 0.9880 0.060 Uiso 1 1 calc R . . C8 C 0.3958(2) 0.21152(11) 0.97710(12) 0.0455(5) Uani 1 1 d . . . H8 H 0.3699 0.2392 1.0155 0.055 Uiso 1 1 calc R A . C9 C 0.50002(19) 0.22501(10) 0.93472(11) 0.0394(5) Uani 1 1 d . A . C10 C 0.52938(17) 0.18301(9) 0.87849(10) 0.0331(4) Uani 1 1 d . A . C11 C 0.67269(18) 0.25869(9) 0.87816(11) 0.0350(4) Uani 1 1 d . A . C12 C 0.59306(19) 0.27487(10) 0.93382(11) 0.0401(5) Uani 1 1 d . . . C13 C 0.6130(2) 0.33356(11) 0.97072(12) 0.0480(6) Uani 1 1 d . . . H13 H 0.5625 0.3469 1.0103 0.058 Uiso 1 1 calc R . . C14 C 0.7081(2) 0.37035(11) 0.94687(14) 0.0506(6) Uani 1 1 d . . . H14 H 0.7227 0.4099 0.9710 0.061 Uiso 1 1 calc R A . C15 C 0.7845(2) 0.35293(10) 0.88918(14) 0.0470(6) Uani 1 1 d . A . H15 H 0.8489 0.3807 0.8755 0.056 Uiso 1 1 calc R . . C16 C 0.76846(18) 0.29498(9) 0.85043(12) 0.0375(5) Uani 1 1 d . A . C17 C 0.92685(19) 0.31423(10) 0.76492(15) 0.0481(6) Uani 1 1 d . A . H17A H 0.9830 0.3273 0.8100 0.067 Uiso 1 1 calc R . . H17B H 0.8874 0.3523 0.7413 0.067 Uiso 1 1 calc R . . C18 C 1.0022(2) 0.28159(11) 0.70789(13) 0.0505(6) Uani 1 1 d . A . H18A H 0.9487 0.2749 0.6597 0.071 Uiso 1 1 calc R . . H18B H 1.0738 0.3086 0.6960 0.071 Uiso 1 1 calc R . . C19 C 1.1398(2) 0.22804(12) 0.80398(14) 0.0534(6) Uani 1 1 d . . . H19A H 1.2064 0.2574 0.7922 0.080 Uiso 1 1 calc R . . H19B H 1.1771 0.1872 0.8179 0.080 Uiso 1 1 calc R . . H19C H 1.0955 0.2442 0.8470 0.080 Uiso 1 1 calc R . . C20 C 1.1104(2) 0.18967(13) 0.67409(16) 0.0690(8) Uani 1 1 d . . . H20A H 1.0473 0.1821 0.6312 0.103 Uiso 1 1 calc R . . H20B H 1.1462 0.1496 0.6925 0.103 Uiso 1 1 calc R . . H20C H 1.1776 0.2163 0.6567 0.103 Uiso 1 1 calc R . . O2 O 0.77728(11) 0.12991(6) 0.68614(7) 0.0280(3) Uani 1 1 d . A 1 N5 N 0.52122(15) 0.31790(7) 0.71365(9) 0.0366(4) Uani 1 1 d . A 1 N6 N 0.57913(14) 0.20520(7) 0.63509(8) 0.0298(3) Uani 1 1 d . A 1 N7 N 0.89044(14) 0.09448(7) 0.82650(8) 0.0312(3) Uani 1 1 d . A 1 N8 N 0.75371(16) 0.07733(9) 0.95876(9) 0.0410(4) Uani 1 1 d . A 1 Li3 Li 0.6615(3) 0.25064(15) 0.72681(19) 0.0368(7) Uani 1 1 d . A 1 Li4 Li 0.7051(3) 0.10094(16) 0.84510(18) 0.0361(7) Uani 1 1 d . A 1 C21 C 0.5798(2) 0.36661(10) 0.66868(14) 0.0532(6) Uani 1 1 d . A 1 H21A H 0.6233 0.3469 0.6274 0.080 Uiso 1 1 calc R A 1 H21B H 0.6406 0.3903 0.7023 0.080 Uiso 1 1 calc R A 1 H21C H 0.5146 0.3950 0.6464 0.080 Uiso 1 1 calc R A 1 C22 C 0.4622(2) 0.34725(10) 0.77804(13) 0.0462(5) Uani 1 1 d . A 1 H22A H 0.3943 0.3751 0.7580 0.069 Uiso 1 1 calc R A 1 H22B H 0.5255 0.3716 0.8091 0.069 Uiso 1 1 calc R A 1 H22C H 0.4277 0.3147 0.8099 0.069 Uiso 1 1 calc R A 1 C23 C 0.42412(18) 0.28236(9) 0.66704(12) 0.0375(5) Uani 1 1 d . A 1 H23A H 0.3599 0.3120 0.6445 0.053 Uiso 1 1 calc R A 1 H23B H 0.3817 0.2534 0.7010 0.053 Uiso 1 1 calc R A 1 C24 C 0.47625(18) 0.24500(9) 0.60289(11) 0.0345(4) Uani 1 1 d . A 1 H24A H 0.4089 0.2187 0.5772 0.048 Uiso 1 1 calc R A 1 H24B H 0.5077 0.2738 0.5642 0.048 Uiso 1 1 calc R A 1 C25 C 0.64535(16) 0.17625(8) 0.58076(10) 0.0289(4) Uani 1 1 d . A 1 C26 C 0.62444(18) 0.17527(9) 0.49991(10) 0.0339(4) Uani 1 1 d . A 1 H26 H 0.5554 0.1981 0.4762 0.041 Uiso 1 1 calc R A 1 C27 C 0.70205(18) 0.14176(9) 0.45361(11) 0.0366(5) Uani 1 1 d . A 1 H27 H 0.6844 0.1435 0.3995 0.044 Uiso 1 1 calc R A 1 C28 C 0.80331(18) 0.10616(9) 0.48258(10) 0.0339(4) Uani 1 1 d . A 1 H28 H 0.8551 0.0841 0.4498 0.041 Uiso 1 1 calc R A 1 C29 C 0.82592(16) 0.10426(8) 0.56304(10) 0.0296(4) Uani 1 1 d . A 1 C30 C 0.74928(16) 0.13913(8) 0.60689(10) 0.0280(4) Uani 1 1 d . A 1 C31 C 0.87805(16) 0.08725(8) 0.68991(11) 0.0287(4) Uani 1 1 d . A 1 C32 C 0.91238(17) 0.07090(8) 0.61801(10) 0.0294(4) Uani 1 1 d . A 1 C33 C 1.01623(17) 0.03096(9) 0.61322(11) 0.0334(4) Uani 1 1 d . A 1 H33 H 1.0434 0.0179 0.5651 0.040 Uiso 1 1 calc R A 1 C34 C 1.07713(18) 0.01146(9) 0.68206(12) 0.0370(5) Uani 1 1 d . A 1 H34 H 1.1474 -0.0158 0.6804 0.044 Uiso 1 1 calc R A 1 C35 C 1.04048(17) 0.02979(9) 0.75388(11) 0.0342(4) Uani 1 1 d . A 1 H35 H 1.0869 0.0149 0.7989 0.041 Uiso 1 1 calc R A 1 C36 C 0.93655(17) 0.06974(8) 0.76162(11) 0.0302(4) Uani 1 1 d . A 1 C37 C 0.95731(19) 0.07396(10) 0.89815(11) 0.0387(5) Uani 1 1 d . A 1 H37A H 1.0436 0.0916 0.9023 0.054 Uiso 1 1 calc R A 1 H37B H 0.9641 0.0277 0.8986 0.054 Uiso 1 1 calc R A 1 C38 C 0.88721(19) 0.09561(11) 0.96575(11) 0.0422(5) Uani 1 1 d . A 1 H38A H 0.9281 0.0775 1.0136 0.059 Uiso 1 1 calc R A 1 H38B H 0.8932 0.1418 0.9698 0.059 Uiso 1 1 calc R A 1 C39 C 0.6894(2) 0.10455(14) 1.02247(12) 0.0613(7) Uani 1 1 d . A 1 H39A H 0.7246 0.0867 1.0712 0.092 Uiso 1 1 calc R A 1 H39B H 0.5992 0.0951 1.0155 0.092 Uiso 1 1 calc R A 1 H39C H 0.7015 0.1501 1.0232 0.092 Uiso 1 1 calc R A 1 C40 C 0.7396(2) 0.00908(12) 0.95904(15) 0.0604(7) Uani 1 1 d . A 1 H40A H 0.7740 -0.0085 0.9132 0.091 Uiso 1 1 calc R A 1 H40B H 0.6502 -0.0017 0.9590 0.091 Uiso 1 1 calc R A 1 H40C H 0.7853 -0.0082 1.0051 0.091 Uiso 1 1 calc R A 1 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 O1 0.0318(7) 0.0311(7) 0.0330(7) -0.0049(6) 0.0017(5) -0.0005(5) N1 0.0333(8) 0.0290(8) 0.0314(8) -0.0008(7) -0.0030(7) -0.0002(7) N2 0.0331(8) 0.0320(8) 0.0302(8) 0.0007(7) 0.0019(6) -0.0049(7) N3 0.0307(8) 0.0296(8) 0.0486(10) -0.0015(8) -0.0014(7) -0.0045(7) N4 0.0383(9) 0.0426(10) 0.0409(9) -0.0116(8) 0.0072(7) -0.0091(8) Li1 0.0385(17) 0.0304(16) 0.0334(16) 0.0021(14) 0.0029(14) -0.0010(13) Li2 0.0379(17) 0.0345(17) 0.0373(17) -0.0020(15) 0.0031(14) 0.0007(14) C1 0.0395(11) 0.0315(10) 0.0404(11) -0.0083(9) -0.0011(9) -0.0005(8) C2 0.0344(11) 0.0458(12) 0.0439(12) -0.0020(10) -0.0043(9) 0.0020(9) C3 0.0458(12) 0.0279(10) 0.0402(11) 0.0012(9) -0.0025(9) -0.0067(8) C4 0.0425(11) 0.0381(11) 0.0352(11) 0.0044(9) 0.0011(9) -0.0105(9) C5 0.0316(10) 0.0412(11) 0.0284(9) 0.0045(9) 0.0002(8) 0.0025(8) C6 0.0349(11) 0.0540(13) 0.0369(11) 0.0062(10) 0.0040(9) -0.0039(9) C7 0.0393(12) 0.0745(17) 0.0364(11) 0.0073(12) 0.0113(9) 0.0074(11) C8 0.0449(12) 0.0593(14) 0.0325(11) -0.0043(10) 0.0053(9) 0.0111(11) C9 0.0400(11) 0.0468(12) 0.0310(10) -0.0027(9) -0.0002(8) 0.0100(9) C10 0.0309(10) 0.0386(11) 0.0296(9) 0.0015(9) 0.0022(8) 0.0022(8) C11 0.0380(11) 0.0302(10) 0.0352(10) -0.0093(8) -0.0075(8) 0.0037(8) C12 0.0409(11) 0.0431(12) 0.0349(11) -0.0073(9) -0.0066(9) 0.0078(9) C13 0.0539(13) 0.0486(13) 0.0394(12) -0.0155(11) -0.0094(10) 0.0162(11) C14 0.0498(13) 0.0409(12) 0.0580(14) -0.0200(11) -0.0165(11) 0.0066(10) C15 0.0394(12) 0.0358(11) 0.0631(15) -0.0137(11) -0.0124(10) 0.0007(9) C16 0.0316(10) 0.0325(10) 0.0463(12) -0.0057(9) -0.0108(9) 0.0023(8) C17 0.0354(11) 0.0328(11) 0.0751(16) 0.0070(11) -0.0029(11) -0.0055(9) C18 0.0459(13) 0.0553(14) 0.0496(13) 0.0107(11) -0.0007(10) -0.0165(11) C19 0.0379(12) 0.0672(16) 0.0544(14) -0.0084(13) -0.0020(10) 0.0023(11) C20 0.0632(16) 0.0751(18) 0.0731(18) -0.0357(15) 0.0344(14) -0.0317(14) O2 0.0283(6) 0.0288(6) 0.0264(6) 0.0013(5) -0.0002(5) 0.0031(5) N5 0.0379(9) 0.0312(8) 0.0399(9) -0.0006(7) -0.0025(7) 0.0016(7) N6 0.0290(8) 0.0283(8) 0.0318(8) 0.0021(7) -0.0003(6) 0.0038(6) N7 0.0314(8) 0.0339(8) 0.0275(8) 0.0035(7) -0.0030(6) 0.0020(7) N8 0.0412(10) 0.0499(11) 0.0317(9) 0.0051(8) 0.0017(7) -0.0002(8) Li3 0.0337(17) 0.0350(18) 0.0410(18) -0.0019(15) -0.0014(14) -0.0013(14) Li4 0.0323(16) 0.0401(18) 0.0356(17) 0.0057(15) 0.0010(13) 0.0014(14) C21 0.0617(15) 0.0380(12) 0.0584(14) 0.0065(11) -0.0046(12) -0.0062(11) C22 0.0465(12) 0.0425(12) 0.0480(13) -0.0090(10) -0.0061(10) 0.0134(10) C23 0.0329(10) 0.0350(10) 0.0432(11) -0.0031(9) -0.0061(9) 0.0083(8) C24 0.0344(10) 0.0312(10) 0.0369(10) 0.0019(9) -0.0047(8) 0.0064(8) C25 0.0295(9) 0.0252(9) 0.0316(9) 0.0013(8) -0.0001(7) -0.0016(7) C26 0.0360(10) 0.0341(10) 0.0305(10) 0.0038(8) -0.0038(8) 0.0011(8) C27 0.0424(11) 0.0407(11) 0.0264(9) 0.0017(8) 0.0003(8) -0.0006(9) C28 0.0369(10) 0.0360(10) 0.0292(9) -0.0031(8) 0.0045(8) 0.0007(8) C29 0.0288(9) 0.0277(9) 0.0323(9) 0.0008(8) 0.0015(8) -0.0010(7) C30 0.0289(9) 0.0284(9) 0.0265(9) 0.0018(8) 0.0000(7) -0.0020(7) C31 0.0252(9) 0.0244(9) 0.0364(10) -0.0013(8) 0.0003(7) 0.0017(7) C32 0.0286(9) 0.0273(9) 0.0320(9) -0.0003(8) 0.0009(7) -0.0020(7) C33 0.0323(10) 0.0317(10) 0.0365(10) -0.0038(8) 0.0034(8) 0.0017(8) C34 0.0329(10) 0.0290(10) 0.0492(12) 0.0009(9) 0.0039(9) 0.0048(8) C35 0.0313(10) 0.0332(10) 0.0375(10) 0.0045(9) -0.0013(8) 0.0035(8) C36 0.0289(9) 0.0281(9) 0.0329(10) 0.0019(8) -0.0014(8) -0.0020(7) C37 0.0346(10) 0.0454(12) 0.0350(10) 0.0059(9) -0.0055(8) 0.0019(9) C38 0.0414(11) 0.0530(13) 0.0308(10) 0.0039(10) -0.0069(9) 0.0001(10) C39 0.0544(14) 0.099(2) 0.0302(11) 0.0041(13) 0.0038(10) 0.0107(14) C40 0.0616(16) 0.0597(16) 0.0593(16) 0.0196(13) 0.0023(12) -0.0116(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 O1 C10 1.404(2) . ? O1 C11 1.412(2) . ? O1 Li4 2.269(4) . ? O1 Li3 2.300(4) . ? N1 C1 1.464(2) . ? N1 C2 1.472(2) . ? N1 C3 1.476(2) . ? N1 Li1 2.050(3) . ? N2 C5 1.373(2) . ? N2 C4 1.460(2) . ? N2 Li1 2.016(3) . ? N2 Li4 2.071(3) . ? N3 C16 1.372(3) . ? N3 C17 1.460(3) . ? N3 Li2 1.990(4) . ? N3 Li3 2.076(4) . ? N4 C19 1.459(3) . ? N4 C20 1.465(3) . ? N4 C18 1.467(3) . ? N4 Li2 2.065(4) . ? Li1 N6 2.078(3) . ? Li1 O2 2.299(3) . ? Li2 N7 2.079(4) . ? Li2 O2 2.332(3) . ? C3 C4 1.509(3) . ? C5 C10 1.405(3) . ? C5 C6 1.414(3) . ? C5 Li4 2.583(4) . ? C6 C7 1.409(3) . ? C7 C8 1.372(3) . ? C8 C9 1.410(3) . ? C9 C10 1.383(3) . ? C9 C12 1.455(3) . ? C10 Li4 2.660(4) . ? C11 C12 1.381(3) . ? C11 C16 1.396(3) . ? C11 Li3 2.640(4) . ? C12 C13 1.417(3) . ? C13 C14 1.371(3) . ? C14 C15 1.393(3) . ? C15 C16 1.413(3) . ? C16 Li3 2.543(4) . ? C17 C18 1.498(3) . ? O2 C31 1.405(2) . ? O2 C30 1.406(2) . ? N5 C22 1.469(3) . ? N5 C21 1.470(3) . ? N5 C23 1.475(2) . ? N5 Li3 2.072(4) . ? N6 C25 1.371(2) . ? N6 C24 1.464(2) . ? N6 Li3 2.014(4) . ? N7 C36 1.374(2) . ? N7 C37 1.458(2) . ? N7 Li4 2.029(3) . ? N8 C40 1.464(3) . ? N8 C39 1.469(3) . ? N8 C38 1.470(3) . ? N8 Li4 2.073(4) . ? C23 C24 1.514(3) . ? C25 C30 1.408(2) . ? C25 C26 1.411(3) . ? C26 C27 1.396(3) . ? C27 C28 1.383(3) . ? C28 C29 1.407(3) . ? C29 C30 1.379(2) . ? C29 C32 1.462(2) . ? C31 C32 1.378(3) . ? C31 C36 1.405(2) . ? C32 C33 1.404(3) . ? C33 C34 1.385(3) . ? C34 C35 1.397(3) . ? C35 C36 1.412(3) . ? C37 C38 1.516(3) . ? 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 C10 O1 C11 104.23(14) . . ? C10 O1 Li4 89.61(13) . . ? C11 O1 Li4 136.81(13) . . ? C10 O1 Li3 132.70(13) . . ? C11 O1 Li3 87.23(13) . . ? Li4 O1 Li3 113.08(13) . . ? C1 N1 C2 108.61(15) . . ? C1 N1 C3 109.72(15) . . ? C2 N1 C3 111.88(16) . . ? C1 N1 Li1 122.87(15) . . ? C2 N1 Li1 100.79(15) . . ? C3 N1 Li1 102.61(14) . . ? C5 N2 C4 114.23(16) . . ? C5 N2 Li1 123.52(15) . . ? C4 N2 Li1 106.39(14) . . ? C5 N2 Li4 95.03(14) . . ? C4 N2 Li4 127.90(16) . . ? Li1 N2 Li4 89.12(14) . . ? C16 N3 C17 113.75(17) . . ? C16 N3 Li2 123.97(16) . . ? C17 N3 Li2 107.52(16) . . ? C16 N3 Li3 92.76(14) . . ? C17 N3 Li3 125.70(17) . . ? Li2 N3 Li3 92.49(14) . . ? C19 N4 C20 110.86(19) . . ? C19 N4 C18 111.98(17) . . ? C20 N4 C18 107.95(19) . . ? C19 N4 Li2 102.75(16) . . ? C20 N4 Li2 122.24(16) . . ? C18 N4 Li2 100.64(16) . . ? N2 Li1 N1 88.43(14) . . ? N2 Li1 N6 145.58(18) . . ? N1 Li1 N6 121.13(16) . . ? N2 Li1 O2 115.00(15) . . ? N1 Li1 O2 103.33(14) . . ? N6 Li1 O2 77.51(11) . . ? N3 Li2 N4 88.16(15) . . ? N3 Li2 N7 146.57(19) . . ? N4 Li2 N7 121.51(17) . . ? N3 Li2 O2 110.58(15) . . ? N4 Li2 O2 107.78(15) . . ? N7 Li2 O2 76.93(12) . . ? N1 C3 C4 112.50(16) . . ? N2 C4 C3 109.64(16) . . ? N2 C5 C10 118.04(17) . . ? N2 C5 C6 130.11(19) . . ? C10 C5 C6 111.84(18) . . ? N2 C5 Li4 53.01(11) . . ? C10 C5 Li4 77.51(13) . . ? C6 C5 Li4 143.96(15) . . ? C7 C6 C5 121.4(2) . . ? C8 C7 C6 124.1(2) . . ? C7 C8 C9 116.5(2) . . ? C10 C9 C8 118.0(2) . . ? C10 C9 C12 105.97(18) . . ? C8 C9 C12 136.0(2) . . ? C9 C10 O1 111.96(17) . . ? C9 C10 C5 128.10(18) . . ? O1 C10 C5 119.85(16) . . ? C9 C10 Li4 141.59(15) . . ? O1 C10 Li4 58.54(11) . . ? C5 C10 Li4 71.44(13) . . ? C12 C11 C16 127.53(19) . . ? C12 C11 O1 111.56(17) . . ? C16 C11 O1 120.42(17) . . ? C12 C11 Li3 137.46(15) . . ? C16 C11 Li3 70.57(13) . . ? O1 C11 Li3 60.49(11) . . ? C11 C12 C13 117.5(2) . . ? C11 C12 C9 106.27(17) . . ? C13 C12 C9 136.0(2) . . ? C14 C13 C12 117.2(2) . . ? C13 C14 C15 123.6(2) . . ? C14 C15 C16 121.6(2) . . ? N3 C16 C11 118.29(17) . . ? N3 C16 C15 129.1(2) . . ? C11 C16 C15 112.58(19) . . ? N3 C16 Li3 54.62(12) . . ? C11 C16 Li3 78.24(13) . . ? C15 C16 Li3 139.55(16) . . ? N3 C17 C18 109.99(18) . . ? N4 C18 C17 112.06(18) . . ? C31 O2 C30 103.90(13) . . ? C31 O2 Li1 135.95(13) . . ? C30 O2 Li1 89.00(12) . . ? C31 O2 Li2 86.19(12) . . ? C30 O2 Li2 134.57(13) . . ? Li1 O2 Li2 114.31(12) . . ? C22 N5 C21 109.31(17) . . ? C22 N5 C23 108.56(16) . . ? C21 N5 C23 112.16(16) . . ? C22 N5 Li3 123.90(16) . . ? C21 N5 Li3 102.55(16) . . ? C23 N5 Li3 100.01(14) . . ? C25 N6 C24 113.92(14) . . ? C25 N6 Li3 123.41(15) . . ? C24 N6 Li3 107.05(14) . . ? C25 N6 Li1 94.31(14) . . ? C24 N6 Li1 127.39(15) . . ? Li3 N6 Li1 90.13(14) . . ? C36 N7 C37 114.18(15) . . ? C36 N7 Li4 124.86(15) . . ? C37 N7 Li4 107.46(15) . . ? C36 N7 Li2 92.27(14) . . ? C37 N7 Li2 125.01(16) . . ? Li4 N7 Li2 92.10(14) . . ? C40 N8 C39 109.69(19) . . ? C40 N8 C38 111.24(18) . . ? C39 N8 C38 109.64(17) . . ? C40 N8 Li4 103.11(17) . . ? C39 N8 Li4 122.09(16) . . ? C38 N8 Li4 100.58(14) . . ? N6 Li3 N5 88.80(14) . . ? N6 Li3 N3 146.32(19) . . ? N5 Li3 N3 119.19(17) . . ? N6 Li3 O1 113.75(16) . . ? N5 Li3 O1 106.28(15) . . ? N3 Li3 O1 78.09(12) . . ? N7 Li4 N2 148.14(19) . . ? N7 Li4 N8 87.83(14) . . ? N2 Li4 N8 118.38(16) . . ? N7 Li4 O1 112.14(16) . . ? N2 Li4 O1 78.48(12) . . ? N8 Li4 O1 108.00(16) . . ? N5 C23 C24 113.40(16) . . ? N6 C24 C23 109.14(15) . . ? N6 C25 C30 117.56(15) . . ? N6 C25 C26 130.37(17) . . ? C30 C25 C26 112.03(16) . . ? N6 C25 Li1 53.60(11) . . ? C30 C25 Li1 78.39(12) . . ? C26 C25 Li1 140.59(15) . . ? C27 C26 C25 122.08(17) . . ? C28 C27 C26 123.32(17) . . ? C27 C28 C29 116.72(17) . . ? C30 C29 C28 118.37(17) . . ? C30 C29 C32 105.56(15) . . ? C28 C29 C32 136.01(17) . . ? C29 C30 O2 112.37(15) . . ? C29 C30 C25 127.43(16) . . ? O2 C30 C25 119.95(15) . . ? C32 C31 O2 112.12(15) . . ? C32 C31 C36 127.81(16) . . ? O2 C31 C36 119.92(16) . . ? C32 C31 Li2 138.69(15) . . ? O2 C31 Li2 61.76(11) . . ? C36 C31 Li2 70.19(13) . . ? C31 C32 C33 118.24(17) . . ? C31 C32 C29 106.04(15) . . ? C33 C32 C29 135.68(17) . . ? C34 C33 C32 116.69(18) . . ? C33 C34 C35 123.36(18) . . ? C34 C35 C36 122.01(18) . . ? N7 C36 C31 118.03(16) . . ? N7 C36 C35 130.05(17) . . ? C31 C36 C35 111.87(17) . . ? N7 C36 Li2 54.97(12) . . ? C31 C36 Li2 78.41(13) . . ? C35 C36 Li2 138.83(15) . . ? N7 C37 C38 109.80(16) . . ? N8 C38 C37 112.67(16) . . ? 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 C5 N2 Li1 N1 -146.53(16) . . . . ? C4 N2 Li1 N1 -11.46(17) . . . . ? Li4 N2 Li1 N1 118.02(14) . . . . ? C5 N2 Li1 N6 4.5(4) . . . . ? C4 N2 Li1 N6 139.6(3) . . . . ? Li4 N2 Li1 N6 -90.9(3) . . . . ? C5 N2 Li1 O2 109.48(19) . . . . ? C4 N2 Li1 O2 -115.45(17) . . . . ? Li4 N2 Li1 O2 14.03(17) . . . . ? C1 N1 Li1 N2 -138.45(16) . . . . ? C2 N1 Li1 N2 100.90(15) . . . . ? C3 N1 Li1 N2 -14.66(16) . . . . ? C1 N1 Li1 N6 60.2(2) . . . . ? C2 N1 Li1 N6 -60.5(2) . . . . ? C3 N1 Li1 N6 -176.01(17) . . . . ? C1 N1 Li1 O2 -23.1(2) . . . . ? C2 N1 Li1 O2 -143.76(14) . . . . ? C3 N1 Li1 O2 100.68(15) . . . . ? C16 N3 Li2 N4 -140.13(16) . . . . ? C17 N3 Li2 N4 -3.92(18) . . . . ? Li3 N3 Li2 N4 124.85(14) . . . . ? C16 N3 Li2 N7 14.1(4) . . . . ? C17 N3 Li2 N7 150.3(3) . . . . ? Li3 N3 Li2 N7 -81.0(3) . . . . ? C16 N3 Li2 O2 111.56(18) . . . . ? C17 N3 Li2 O2 -112.23(17) . . . . ? Li3 N3 Li2 O2 16.54(17) . . . . ? C19 N4 Li2 N3 93.88(17) . . . . ? C20 N4 Li2 N3 -141.1(2) . . . . ? C18 N4 Li2 N3 -21.77(17) . . . . ? C19 N4 Li2 N7 -69.8(2) . . . . ? C20 N4 Li2 N7 55.3(3) . . . . ? C18 N4 Li2 N7 174.56(18) . . . . ? C19 N4 Li2 O2 -155.08(16) . . . . ? C20 N4 Li2 O2 -30.0(3) . . . . ? C18 N4 Li2 O2 89.27(17) . . . . ? C1 N1 C3 C4 170.96(16) . . . . ? C2 N1 C3 C4 -68.4(2) . . . . ? Li1 N1 C3 C4 38.8(2) . . . . ? C5 N2 C4 C3 175.06(16) . . . . ? Li1 N2 C4 C3 35.3(2) . . . . ? Li4 N2 C4 C3 -66.8(2) . . . . ? N1 C3 C4 N2 -52.4(2) . . . . ? C4 N2 C5 C10 -179.38(16) . . . . ? Li1 N2 C5 C10 -47.4(2) . . . . ? Li4 N2 C5 C10 44.91(19) . . . . ? C4 N2 C5 C6 2.2(3) . . . . ? Li1 N2 C5 C6 134.2(2) . . . . ? Li4 N2 C5 C6 -133.6(2) . . . . ? C4 N2 C5 Li4 135.71(19) . . . . ? Li1 N2 C5 Li4 -92.28(18) . . . . ? N2 C5 C6 C7 178.59(19) . . . . ? C10 C5 C6 C7 0.0(3) . . . . ? Li4 C5 C6 C7 98.9(3) . . . . ? C5 C6 C7 C8 -0.6(3) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C7 C8 C9 C10 1.7(3) . . . . ? C7 C8 C9 C12 -178.1(2) . . . . ? C8 C9 C10 O1 -178.84(17) . . . . ? C12 C9 C10 O1 1.0(2) . . . . ? C8 C9 C10 C5 -2.5(3) . . . . ? C12 C9 C10 C5 177.33(19) . . . . ? C8 C9 C10 Li4 -112.2(3) . . . . ? C12 C9 C10 Li4 67.6(3) . . . . ? C11 O1 C10 C9 -0.57(19) . . . . ? Li4 O1 C10 C9 138.05(17) . . . . ? Li3 O1 C10 C9 -100.1(2) . . . . ? C11 O1 C10 C5 -177.25(16) . . . . ? Li4 O1 C10 C5 -38.62(18) . . . . ? Li3 O1 C10 C5 83.2(2) . . . . ? C11 O1 C10 Li4 -138.63(14) . . . . ? Li3 O1 C10 Li4 121.81(19) . . . . ? N2 C5 C10 C9 -177.19(18) . . . . ? C6 C5 C10 C9 1.5(3) . . . . ? Li4 C5 C10 C9 -141.9(2) . . . . ? N2 C5 C10 O1 -1.1(3) . . . . ? C6 C5 C10 O1 177.63(16) . . . . ? Li4 C5 C10 O1 34.17(16) . . . . ? N2 C5 C10 Li4 -35.28(16) . . . . ? C6 C5 C10 Li4 143.46(17) . . . . ? C10 O1 C11 C12 -0.1(2) . . . . ? Li4 O1 C11 C12 -105.2(2) . . . . ? Li3 O1 C11 C12 133.37(17) . . . . ? C10 O1 C11 C16 -172.62(17) . . . . ? Li4 O1 C11 C16 82.3(3) . . . . ? Li3 O1 C11 C16 -39.14(19) . . . . ? C10 O1 C11 Li3 -133.48(14) . . . . ? Li4 O1 C11 Li3 121.5(2) . . . . ? C16 C11 C12 C13 -3.5(3) . . . . ? O1 C11 C12 C13 -175.34(16) . . . . ? Li3 C11 C12 C13 -106.0(2) . . . . ? C16 C11 C12 C9 172.56(19) . . . . ? O1 C11 C12 C9 0.7(2) . . . . ? Li3 C11 C12 C9 70.0(3) . . . . ? C10 C9 C12 C11 -1.0(2) . . . . ? C8 C9 C12 C11 178.8(2) . . . . ? C10 C9 C12 C13 173.9(2) . . . . ? C8 C9 C12 C13 -6.3(4) . . . . ? C11 C12 C13 C14 1.5(3) . . . . ? C9 C12 C13 C14 -173.0(2) . . . . ? C12 C13 C14 C15 0.0(3) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C17 N3 C16 C11 179.51(17) . . . . ? Li2 N3 C16 C11 -46.6(3) . . . . ? Li3 N3 C16 C11 48.2(2) . . . . ? C17 N3 C16 C15 2.5(3) . . . . ? Li2 N3 C16 C15 136.4(2) . . . . ? Li3 N3 C16 C15 -128.7(2) . . . . ? C17 N3 C16 Li3 131.26(19) . . . . ? Li2 N3 C16 Li3 -94.87(19) . . . . ? C12 C11 C16 N3 -173.99(19) . . . . ? O1 C11 C16 N3 -2.8(3) . . . . ? Li3 C11 C16 N3 -38.41(16) . . . . ? C12 C11 C16 C15 3.5(3) . . . . ? O1 C11 C16 C15 174.68(16) . . . . ? Li3 C11 C16 C15 139.05(18) . . . . ? C12 C11 C16 Li3 -135.6(2) . . . . ? O1 C11 C16 Li3 35.62(17) . . . . ? C14 C15 C16 N3 175.5(2) . . . . ? C14 C15 C16 C11 -1.7(3) . . . . ? C14 C15 C16 Li3 96.8(3) . . . . ? C16 N3 C17 C18 170.54(17) . . . . ? Li2 N3 C17 C18 29.4(2) . . . . ? Li3 N3 C17 C18 -77.1(2) . . . . ? C19 N4 C18 C17 -64.1(2) . . . . ? C20 N4 C18 C17 173.63(18) . . . . ? Li2 N4 C18 C17 44.5(2) . . . . ? N3 C17 C18 N4 -52.6(2) . . . . ? N2 Li1 O2 C31 56.3(3) . . . . ? N1 Li1 O2 C31 -38.2(2) . . . . ? N6 Li1 O2 C31 -157.68(16) . . . . ? N2 Li1 O2 C30 165.43(17) . . . . ? N1 Li1 O2 C30 70.88(15) . . . . ? N6 Li1 O2 C30 -48.58(12) . . . . ? N2 Li1 O2 Li2 -54.91(19) . . . . ? N1 Li1 O2 Li2 -149.46(13) . . . . ? N6 Li1 O2 Li2 91.08(13) . . . . ? N3 Li2 O2 C31 162.43(17) . . . . ? N4 Li2 O2 C31 67.59(16) . . . . ? N7 Li2 O2 C31 -51.68(12) . . . . ? N3 Li2 O2 C30 56.6(2) . . . . ? N4 Li2 O2 C30 -38.2(2) . . . . ? N7 Li2 O2 C30 -157.48(15) . . . . ? N3 Li2 O2 Li1 -58.08(19) . . . . ? N4 Li2 O2 Li1 -152.91(14) . . . . ? N7 Li2 O2 Li1 87.81(13) . . . . ? N2 Li1 N6 C25 167.9(3) . . . . ? N1 Li1 N6 C25 -46.5(2) . . . . ? O2 Li1 N6 C25 51.66(12) . . . . ? N2 Li1 N6 C24 -67.4(4) . . . . ? N1 Li1 N6 C24 78.2(2) . . . . ? O2 Li1 N6 C24 176.37(15) . . . . ? N2 Li1 N6 Li3 44.4(3) . . . . ? N1 Li1 N6 Li3 -170.04(19) . . . . ? O2 Li1 N6 Li3 -71.87(12) . . . . ? N3 Li2 N7 C36 161.2(3) . . . . ? N4 Li2 N7 C36 -49.5(2) . . . . ? O2 Li2 N7 C36 53.51(12) . . . . ? N3 Li2 N7 C37 -76.9(4) . . . . ? N4 Li2 N7 C37 72.4(2) . . . . ? O2 Li2 N7 C37 175.39(15) . . . . ? N3 Li2 N7 Li4 36.1(3) . . . . ? N4 Li2 N7 Li4 -174.54(19) . . . . ? O2 Li2 N7 Li4 -71.51(12) . . . . ? C25 N6 Li3 N5 141.35(15) . . . . ? C24 N6 Li3 N5 6.08(17) . . . . ? Li1 N6 Li3 N5 -123.40(14) . . . . ? C25 N6 Li3 N3 -6.7(4) . . . . ? C24 N6 Li3 N3 -141.9(3) . . . . ? Li1 N6 Li3 N3 88.6(3) . . . . ? C25 N6 Li3 O1 -111.37(18) . . . . ? C24 N6 Li3 O1 113.37(17) . . . . ? Li1 N6 Li3 O1 -16.12(17) . . . . ? C22 N5 Li3 N6 140.38(17) . . . . ? C21 N5 Li3 N6 -95.73(16) . . . . ? C23 N5 Li3 N6 19.85(16) . . . . ? C22 N5 Li3 N3 -59.3(3) . . . . ? C21 N5 Li3 N3 64.6(2) . . . . ? C23 N5 Li3 N3 -179.81(18) . . . . ? C22 N5 Li3 O1 26.0(2) . . . . ? C21 N5 Li3 O1 149.85(15) . . . . ? C23 N5 Li3 O1 -94.58(16) . . . . ? C16 N3 Li3 N6 -167.3(3) . . . . ? C17 N3 Li3 N6 70.6(4) . . . . ? Li2 N3 Li3 N6 -43.2(4) . . . . ? C16 N3 Li3 N5 50.0(2) . . . . ? C17 N3 Li3 N5 -72.1(3) . . . . ? Li2 N3 Li3 N5 174.18(19) . . . . ? C16 N3 Li3 O1 -52.16(13) . . . . ? C17 N3 Li3 O1 -174.24(17) . . . . ? Li2 N3 Li3 O1 72.04(13) . . . . ? C10 O1 Li3 N6 -56.8(2) . . . . ? C11 O1 Li3 N6 -163.71(17) . . . . ? Li4 O1 Li3 N6 55.68(19) . . . . ? C10 O1 Li3 N5 39.2(2) . . . . ? C11 O1 Li3 N5 -67.71(15) . . . . ? Li4 O1 Li3 N5 151.69(14) . . . . ? C10 O1 Li3 N3 156.40(16) . . . . ? C11 O1 Li3 N3 49.53(12) . . . . ? Li4 O1 Li3 N3 -91.07(14) . . . . ? C36 N7 Li4 N2 -6.1(4) . . . . ? C37 N7 Li4 N2 -144.0(3) . . . . ? Li2 N7 Li4 N2 88.1(4) . . . . ? C36 N7 Li4 N8 141.09(16) . . . . ? C37 N7 Li4 N8 3.15(18) . . . . ? Li2 N7 Li4 N8 -124.68(14) . . . . ? C36 N7 Li4 O1 -110.34(19) . . . . ? C37 N7 Li4 O1 111.73(17) . . . . ? Li2 N7 Li4 O1 -16.10(17) . . . . ? C5 N2 Li4 N7 -163.4(3) . . . . ? C4 N2 Li4 N7 70.4(4) . . . . ? Li1 N2 Li4 N7 -39.8(4) . . . . ? C5 N2 Li4 N8 54.6(2) . . . . ? C4 N2 Li4 N8 -71.6(3) . . . . ? Li1 N2 Li4 N8 178.15(19) . . . . ? C5 N2 Li4 O1 -49.81(13) . . . . ? C4 N2 Li4 O1 -176.01(16) . . . . ? Li1 N2 Li4 O1 73.77(12) . . . . ? C40 N8 Li4 N7 -92.51(17) . . . . ? C39 N8 Li4 N7 143.83(19) . . . . ? C38 N8 Li4 N7 22.44(17) . . . . ? C40 N8 Li4 N2 68.5(2) . . . . ? C39 N8 Li4 N2 -55.1(3) . . . . ? C38 N8 Li4 N2 -176.53(18) . . . . ? C40 N8 Li4 O1 154.90(16) . . . . ? C39 N8 Li4 O1 31.2(2) . . . . ? C38 N8 Li4 O1 -90.15(17) . . . . ? C10 O1 Li4 N7 -163.60(16) . . . . ? C11 O1 Li4 N7 -53.0(3) . . . . ? Li3 O1 Li4 N7 59.15(19) . . . . ? C10 O1 Li4 N2 47.87(12) . . . . ? C11 O1 Li4 N2 158.48(18) . . . . ? Li3 O1 Li4 N2 -89.37(13) . . . . ? C10 O1 Li4 N8 -68.48(16) . . . . ? C11 O1 Li4 N8 42.1(3) . . . . ? Li3 O1 Li4 N8 154.27(14) . . . . ? C22 N5 C23 C24 -174.68(16) . . . . ? C21 N5 C23 C24 64.4(2) . . . . ? Li3 N5 C23 C24 -43.6(2) . . . . ? C25 N6 C24 C23 -170.89(16) . . . . ? Li3 N6 C24 C23 -30.9(2) . . . . ? Li1 N6 C24 C23 72.9(2) . . . . ? N5 C23 C24 N6 53.5(2) . . . . ? C24 N6 C25 C30 177.42(15) . . . . ? Li3 N6 C25 C30 44.8(2) . . . . ? Li1 N6 C25 C30 -48.19(18) . . . . ? C24 N6 C25 C26 -5.1(3) . . . . ? Li3 N6 C25 C26 -137.7(2) . . . . ? Li1 N6 C25 C26 129.3(2) . . . . ? C24 N6 C25 Li1 -134.40(18) . . . . ? Li3 N6 C25 Li1 93.01(18) . . . . ? N2 Li1 C25 N6 -75.7(14) . . . . ? N1 Li1 C25 N6 141.25(18) . . . . ? O2 Li1 C25 N6 -117.47(14) . . . . ? N2 Li1 C25 C30 61.9(14) . . . . ? N1 Li1 C25 C30 -81.17(14) . . . . ? N6 Li1 C25 C30 137.58(17) . . . . ? O2 Li1 C25 C30 20.11(10) . . . . ? N2 Li1 C25 C26 172.5(13) . . . . ? N1 Li1 C25 C26 29.5(3) . . . . ? N6 Li1 C25 C26 -111.7(3) . . . . ? O2 Li1 C25 C26 130.8(2) . . . . ? N6 C25 C26 C27 -178.85(18) . . . . ? C30 C25 C26 C27 -1.3(3) . . . . ? Li1 C25 C26 C27 -99.9(3) . . . . ? C25 C26 C27 C28 1.2(3) . . . . ? C26 C27 C28 C29 0.5(3) . . . . ? C27 C28 C29 C30 -2.1(3) . . . . ? C27 C28 C29 C32 174.8(2) . . . . ? C28 C29 C30 O2 176.32(16) . . . . ? C32 C29 C30 O2 -1.4(2) . . . . ? C28 C29 C30 C25 2.1(3) . . . . ? C32 C29 C30 C25 -175.59(17) . . . . ? C31 O2 C30 C29 0.63(19) . . . . ? Li1 O2 C30 C29 -136.78(16) . . . . ? Li2 O2 C30 C29 99.1(2) . . . . ? C31 O2 C30 C25 175.31(15) . . . . ? Li1 O2 C30 C25 37.90(17) . . . . ? Li2 O2 C30 C25 -86.2(2) . . . . ? N6 C25 C30 C29 177.51(17) . . . . ? C26 C25 C30 C29 -0.4(3) . . . . ? Li1 C25 C30 C29 139.7(2) . . . . ? N6 C25 C30 O2 3.7(2) . . . . ? C26 C25 C30 O2 -174.21(15) . . . . ? Li1 C25 C30 O2 -34.06(16) . . . . ? C30 O2 C31 C32 0.48(18) . . . . ? Li1 O2 C31 C32 103.8(2) . . . . ? Li2 O2 C31 C32 -134.60(16) . . . . ? C30 O2 C31 C36 176.24(16) . . . . ? Li1 O2 C31 C36 -80.5(2) . . . . ? Li2 O2 C31 C36 41.16(17) . . . . ? C30 O2 C31 Li2 135.07(14) . . . . ? Li1 O2 C31 Li2 -121.64(19) . . . . ? N3 Li2 C31 C32 65.7(4) . . . . ? N4 Li2 C31 C32 -26.0(3) . . . . ? N7 Li2 C31 C32 -150.8(2) . . . . ? O2 Li2 C31 C32 92.1(2) . . . . ? N3 Li2 C31 O2 -26.4(2) . . . . ? N4 Li2 C31 O2 -118.08(15) . . . . ? N7 Li2 C31 O2 117.15(14) . . . . ? N3 Li2 C31 C36 -169.0(3) . . . . ? N4 Li2 C31 C36 99.25(15) . . . . ? N7 Li2 C31 C36 -25.52(11) . . . . ? O2 Li2 C31 C36 -142.67(17) . . . . ? O2 C31 C32 C33 176.81(15) . . . . ? C36 C31 C32 C33 1.5(3) . . . . ? Li2 C31 C32 C33 104.9(2) . . . . ? O2 C31 C32 C29 -1.3(2) . . . . ? C36 C31 C32 C29 -176.65(18) . . . . ? Li2 C31 C32 C29 -73.2(2) . . . . ? C30 C29 C32 C31 1.6(2) . . . . ? C28 C29 C32 C31 -175.5(2) . . . . ? C30 C29 C32 C33 -176.0(2) . . . . ? C28 C29 C32 C33 6.9(4) . . . . ? C31 C32 C33 C34 -0.6(3) . . . . ? C29 C32 C33 C34 176.8(2) . . . . ? C32 C33 C34 C35 -0.3(3) . . . . ? C33 C34 C35 C36 0.5(3) . . . . ? C37 N7 C36 C31 -179.70(16) . . . . ? Li4 N7 C36 C31 44.8(2) . . . . ? Li2 N7 C36 C31 -49.37(19) . . . . ? C37 N7 C36 C35 -2.6(3) . . . . ? Li4 N7 C36 C35 -138.1(2) . . . . ? Li2 N7 C36 C35 127.7(2) . . . . ? C37 N7 C36 Li2 -130.33(19) . . . . ? Li4 N7 C36 Li2 94.14(19) . . . . ? C32 C31 C36 N7 176.36(17) . . . . ? O2 C31 C36 N7 1.3(3) . . . . ? Li2 C31 C36 N7 39.38(16) . . . . ? C32 C31 C36 C35 -1.2(3) . . . . ? O2 C31 C36 C35 -176.27(15) . . . . ? Li2 C31 C36 C35 -138.22(17) . . . . ? C32 C31 C36 Li2 137.0(2) . . . . ? O2 C31 C36 Li2 -38.05(16) . . . . ? C34 C35 C36 N7 -177.00(18) . . . . ? C34 C35 C36 C31 0.2(3) . . . . ? C34 C35 C36 Li2 -97.2(3) . . . . ? N3 Li2 C36 N7 -94.2(10) . . . . ? N4 Li2 C36 N7 139.09(18) . . . . ? O2 Li2 C36 N7 -114.98(14) . . . . ? N3 Li2 C36 C31 42.7(10) . . . . ? N4 Li2 C36 C31 -84.06(15) . . . . ? N7 Li2 C36 C31 136.85(17) . . . . ? O2 Li2 C36 C31 21.87(10) . . . . ? N3 Li2 C36 C35 152.7(9) . . . . ? N4 Li2 C36 C35 26.0(3) . . . . ? N7 Li2 C36 C35 -113.1(3) . . . . ? O2 Li2 C36 C35 131.9(2) . . . . ? C36 N7 C37 C38 -171.28(16) . . . . ? Li4 N7 C37 C38 -28.3(2) . . . . ? Li2 N7 C37 C38 77.2(2) . . . . ? C40 N8 C38 C37 63.5(2) . . . . ? C39 N8 C38 C37 -174.99(18) . . . . ? Li4 N8 C38 C37 -45.2(2) . . . . ? N7 C37 C38 N8 52.6(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.234 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.043 #======END data_compound_5 _database_code_CSD 217507 _chemical_name_common LAl2Me4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H38 Al2 N4 O' _chemical_formula_weight 452.54 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 '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 13.3634(4) _cell_length_b 10.6542(3) _cell_length_c 18.4122(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.5860(10) _cell_angle_gamma 90.00 _cell_volume 2584.86(14) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 7680 _cell_measurement_theta_min 2.217 _cell_measurement_theta_max 31.509 _exptl_crystal_description tablet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.134 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.385 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; semi-empirical absorption correction applied using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 ? _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 19632 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5916 _reflns_number_gt 4508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0567P)^2^+0.7562P] 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 5916 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.36403(4) 0.38113(5) 0.34152(3) 0.02263(14) Uani 1 1 d . . . Al2 Al -0.12318(4) 0.48837(5) 0.35584(3) 0.02453(14) Uani 1 1 d . . . O1 O 0.23695(9) 0.60691(11) 0.37879(7) 0.0233(3) Uani 1 1 d . . . N1 N 0.49601(12) 0.28971(14) 0.33314(8) 0.0256(3) Uani 1 1 d . . . N2 N 0.44543(12) 0.51150(14) 0.38734(8) 0.0245(3) Uani 1 1 d . . . N3 N 0.00948(12) 0.53836(14) 0.35164(8) 0.0256(3) Uani 1 1 d . . . N4 N -0.07491(12) 0.31066(14) 0.34669(8) 0.0268(3) Uani 1 1 d . . . C1 C 0.49063(17) 0.15079(18) 0.33642(14) 0.0410(5) Uani 1 1 d . . . H1A H 0.4396 0.1202 0.2958 0.061 Uiso 1 1 calc R . . H1B H 0.4717 0.1253 0.3834 0.061 Uiso 1 1 calc R . . H1C H 0.5570 0.1151 0.3322 0.061 Uiso 1 1 calc R . . C2 C 0.53581(17) 0.3263(2) 0.26572(11) 0.0378(5) Uani 1 1 d . . . H2A H 0.5343 0.4179 0.2609 0.057 Uiso 1 1 calc R . . H2B H 0.4936 0.2887 0.2226 0.057 Uiso 1 1 calc R . . H2C H 0.6058 0.2965 0.2691 0.057 Uiso 1 1 calc R . . C3 C 0.56370(15) 0.33755(17) 0.39987(10) 0.0276(4) Uani 1 1 d . . . H3A H 0.6350 0.3152 0.3975 0.039 Uiso 1 1 calc R . . H3B H 0.5451 0.2982 0.4445 0.039 Uiso 1 1 calc R . . C4 C 0.55349(15) 0.47918(17) 0.40444(10) 0.0279(4) Uani 1 1 d . . . H4A H 0.5823 0.5087 0.4545 0.039 Uiso 1 1 calc R . . H4B H 0.5909 0.5202 0.3688 0.039 Uiso 1 1 calc R . . C5 C 0.42345(14) 0.63585(16) 0.39970(9) 0.0233(4) Uani 1 1 d . . . C6 C 0.49811(15) 0.72953(17) 0.41900(10) 0.0259(4) Uani 1 1 d . . . H6 H 0.5675 0.7071 0.4222 0.031 Uiso 1 1 calc R . . C7 C 0.47409(15) 0.85409(17) 0.43361(10) 0.0284(4) Uani 1 1 d . . . H7 H 0.5276 0.9130 0.4459 0.034 Uiso 1 1 calc R . . C8 C 0.37560(15) 0.89373(17) 0.43065(10) 0.0289(4) Uani 1 1 d . . . H8 H 0.3601 0.9782 0.4410 0.035 Uiso 1 1 calc R . . C9 C 0.29895(15) 0.80383(16) 0.41168(10) 0.0254(4) Uani 1 1 d . . . C10 C 0.32334(14) 0.68071(16) 0.39596(9) 0.0229(4) Uani 1 1 d . . . C11 C 0.15483(14) 0.68692(16) 0.38432(9) 0.0239(4) Uani 1 1 d . . . C12 C 0.19001(15) 0.80814(16) 0.40494(10) 0.0253(4) Uani 1 1 d . . . C13 C 0.12230(16) 0.90418(17) 0.41542(11) 0.0299(4) Uani 1 1 d . . . H13 H 0.1454 0.9866 0.4288 0.036 Uiso 1 1 calc R . . C14 C 0.02092(16) 0.87402(17) 0.40547(11) 0.0303(4) Uani 1 1 d . . . H14 H -0.0269 0.9366 0.4131 0.036 Uiso 1 1 calc R . . C15 C -0.01337(15) 0.75391(17) 0.38439(10) 0.0277(4) Uani 1 1 d . . . H15 H -0.0843 0.7384 0.3775 0.033 Uiso 1 1 calc R . . C16 C 0.05197(14) 0.65311(16) 0.37263(9) 0.0240(4) Uani 1 1 d . . . C17 C 0.07401(15) 0.43828(17) 0.33037(12) 0.0310(4) Uani 1 1 d . . . H17A H 0.1225 0.4093 0.3737 0.043 Uiso 1 1 calc R . . H17B H 0.1130 0.4692 0.2927 0.043 Uiso 1 1 calc R . . C18 C 0.00428(15) 0.33109(18) 0.29930(11) 0.0304(4) Uani 1 1 d . . . H18A H -0.0287 0.3516 0.2485 0.043 Uiso 1 1 calc R . . H18B H 0.0445 0.2534 0.2976 0.043 Uiso 1 1 calc R . . C19 C -0.02840(18) 0.25934(19) 0.41963(11) 0.0371(5) Uani 1 1 d . . . H19A H -0.0818 0.2417 0.4488 0.056 Uiso 1 1 calc R . . H19B H 0.0191 0.3209 0.4455 0.056 Uiso 1 1 calc R . . H19C H 0.0080 0.1816 0.4126 0.056 Uiso 1 1 calc R . . C20 C -0.15188(17) 0.22071(19) 0.31029(12) 0.0361(5) Uani 1 1 d . . . H20A H -0.1193 0.1400 0.3038 0.054 Uiso 1 1 calc R . . H20B H -0.1828 0.2537 0.2621 0.054 Uiso 1 1 calc R . . H20C H -0.2045 0.2089 0.3409 0.054 Uiso 1 1 calc R . . C21 C 0.29558(16) 0.41383(19) 0.23987(11) 0.0317(4) Uani 1 1 d . . . H21A H 0.2763 0.5025 0.2348 0.048 Uiso 1 1 calc R . . H21B H 0.2347 0.3614 0.2289 0.048 Uiso 1 1 calc R . . H21C H 0.3418 0.3938 0.2054 0.048 Uiso 1 1 calc R . . C22 C 0.29969(15) 0.27343(18) 0.40736(11) 0.0296(4) Uani 1 1 d . . . H22A H 0.3523 0.2294 0.4414 0.044 Uiso 1 1 calc R . . H22B H 0.2557 0.2120 0.3780 0.044 Uiso 1 1 calc R . . H22C H 0.2591 0.3253 0.4354 0.044 Uiso 1 1 calc R . . C23 C -0.22165(17) 0.5301(2) 0.26752(12) 0.0372(5) Uani 1 1 d . . . H23A H -0.2373 0.6200 0.2676 0.056 Uiso 1 1 calc R . . H23B H -0.2840 0.4816 0.2675 0.056 Uiso 1 1 calc R . . H23C H -0.1928 0.5096 0.2234 0.056 Uiso 1 1 calc R . . C24 C -0.16778(16) 0.50736(19) 0.45131(11) 0.0335(4) Uani 1 1 d . . . H24A H -0.1089 0.5020 0.4908 0.050 Uiso 1 1 calc R . . H24B H -0.2160 0.4405 0.4575 0.050 Uiso 1 1 calc R . . H24C H -0.2007 0.5891 0.4534 0.050 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 Al1 0.0223(3) 0.0203(3) 0.0257(3) -0.00106(19) 0.0052(2) -0.0009(2) Al2 0.0222(3) 0.0253(3) 0.0265(3) -0.0009(2) 0.0052(2) -0.0004(2) O1 0.0213(7) 0.0201(6) 0.0291(6) -0.0012(5) 0.0057(5) -0.0008(5) N1 0.0265(8) 0.0226(7) 0.0285(8) -0.0024(6) 0.0071(6) 0.0002(6) N2 0.0228(8) 0.0229(7) 0.0287(7) -0.0022(6) 0.0065(6) -0.0003(6) N3 0.0249(8) 0.0225(7) 0.0307(8) -0.0026(6) 0.0082(6) 0.0003(6) N4 0.0265(9) 0.0246(8) 0.0291(8) -0.0012(6) 0.0043(7) -0.0036(6) C1 0.0328(12) 0.0217(9) 0.0674(15) -0.0071(9) 0.0053(11) 0.0028(8) C2 0.0332(12) 0.0529(13) 0.0297(10) -0.0017(9) 0.0124(9) 0.0060(10) C3 0.0240(10) 0.0285(9) 0.0300(9) -0.0004(7) 0.0038(8) 0.0034(7) C4 0.0241(10) 0.0269(9) 0.0328(9) -0.0040(7) 0.0048(8) -0.0011(7) C5 0.0285(10) 0.0211(8) 0.0212(8) 0.0001(6) 0.0069(7) -0.0029(7) C6 0.0246(10) 0.0273(9) 0.0260(8) -0.0003(7) 0.0050(7) -0.0047(7) C7 0.0323(11) 0.0234(9) 0.0288(9) 0.0002(7) 0.0026(8) -0.0093(8) C8 0.0349(11) 0.0196(8) 0.0324(9) -0.0003(7) 0.0066(8) -0.0041(7) C9 0.0308(10) 0.0201(8) 0.0260(8) 0.0017(6) 0.0064(7) 0.0000(7) C10 0.0247(9) 0.0204(8) 0.0241(8) -0.0008(6) 0.0053(7) -0.0048(7) C11 0.0273(10) 0.0196(8) 0.0258(8) 0.0010(6) 0.0074(7) 0.0021(7) C12 0.0286(10) 0.0220(8) 0.0264(8) 0.0006(7) 0.0073(7) -0.0008(7) C13 0.0347(11) 0.0192(8) 0.0368(10) 0.0009(7) 0.0090(9) 0.0021(7) C14 0.0343(11) 0.0236(9) 0.0350(10) 0.0019(7) 0.0117(8) 0.0062(8) C15 0.0269(10) 0.0257(9) 0.0315(9) 0.0021(7) 0.0081(8) 0.0023(7) C16 0.0282(10) 0.0207(8) 0.0239(8) 0.0008(6) 0.0070(7) 0.0003(7) C17 0.0249(10) 0.0256(9) 0.0442(11) -0.0068(8) 0.0110(8) -0.0014(8) C18 0.0285(10) 0.0279(9) 0.0368(10) -0.0076(8) 0.0116(8) -0.0022(8) C19 0.0448(13) 0.0280(10) 0.0361(11) 0.0044(8) -0.0002(9) -0.0004(9) C20 0.0336(11) 0.0307(10) 0.0438(11) -0.0100(8) 0.0064(9) -0.0092(9) C21 0.0294(11) 0.0340(10) 0.0318(9) 0.0014(8) 0.0054(8) 0.0008(8) C22 0.0283(10) 0.0282(9) 0.0331(10) 0.0029(7) 0.0073(8) -0.0008(8) C23 0.0319(12) 0.0396(11) 0.0381(11) 0.0044(9) 0.0001(9) 0.0002(9) C24 0.0303(11) 0.0380(11) 0.0341(10) -0.0046(8) 0.0107(9) -0.0021(8) _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 Al1 N2 1.8759(16) . ? Al1 C22 1.9678(19) . ? Al1 C21 1.973(2) . ? Al1 N1 2.0430(17) . ? Al1 Al2 6.6586(8) . ? Al2 N3 1.8649(17) . ? Al2 C24 1.958(2) . ? Al2 C23 1.965(2) . ? Al2 N4 2.0164(16) . ? O1 C10 1.389(2) . ? O1 C11 1.407(2) . ? N1 C2 1.482(2) . ? N1 C1 1.483(2) . ? N1 C3 1.489(2) . ? N2 C5 1.384(2) . ? N2 C4 1.467(2) . ? N3 C16 1.376(2) . ? N3 C17 1.465(2) . ? N4 C20 1.482(2) . ? N4 C19 1.487(2) . ? N4 C18 1.495(2) . ? C3 C4 1.519(3) . ? C5 C10 1.411(3) . ? C5 C6 1.414(2) . ? C6 C7 1.402(3) . ? C7 C8 1.375(3) . ? C8 C9 1.403(3) . ? C9 C10 1.394(2) . ? C9 C12 1.441(3) . ? C11 C16 1.402(3) . ? C11 C12 1.405(2) . ? C12 C13 1.400(3) . ? C13 C14 1.375(3) . ? C14 C15 1.392(3) . ? C15 C16 1.423(3) . ? C17 C18 1.524(3) . ? 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 Al1 C22 115.78(8) . . ? N2 Al1 C21 116.01(8) . . ? C22 Al1 C21 120.42(9) . . ? N2 Al1 N1 86.77(7) . . ? C22 Al1 N1 103.87(8) . . ? C21 Al1 N1 106.40(8) . . ? N2 Al1 Al2 110.66(5) . . ? C22 Al1 Al2 62.95(6) . . ? C21 Al1 Al2 72.86(6) . . ? N1 Al1 Al2 161.25(5) . . ? N3 Al2 C24 116.17(8) . . ? N3 Al2 C23 114.28(9) . . ? C24 Al2 C23 117.23(10) . . ? N3 Al2 N4 86.85(7) . . ? C24 Al2 N4 108.75(8) . . ? C23 Al2 N4 108.84(8) . . ? N3 Al2 Al1 26.47(5) . . ? C24 Al2 Al1 119.93(7) . . ? C23 Al2 Al1 122.04(7) . . ? N4 Al2 Al1 60.46(5) . . ? C10 O1 C11 105.63(13) . . ? C2 N1 C1 108.85(16) . . ? C2 N1 C3 110.35(15) . . ? C1 N1 C3 109.57(15) . . ? C2 N1 Al1 111.88(12) . . ? C1 N1 Al1 115.10(13) . . ? C3 N1 Al1 100.83(10) . . ? C5 N2 C4 114.70(15) . . ? C5 N2 Al1 131.27(13) . . ? C4 N2 Al1 113.52(11) . . ? C16 N3 C17 119.20(16) . . ? C16 N3 Al2 126.36(13) . . ? C17 N3 Al2 114.16(12) . . ? C20 N4 C19 108.96(15) . . ? C20 N4 C18 109.61(15) . . ? C19 N4 C18 110.52(16) . . ? C20 N4 Al2 115.94(13) . . ? C19 N4 Al2 111.17(12) . . ? C18 N4 Al2 100.34(11) . . ? N1 C3 C4 109.75(15) . . ? N2 C4 C3 108.40(15) . . ? N2 C5 C10 122.79(16) . . ? N2 C5 C6 123.83(17) . . ? C10 C5 C6 113.37(16) . . ? C7 C6 C5 122.81(18) . . ? C8 C7 C6 122.11(17) . . ? C7 C8 C9 117.03(17) . . ? C10 C9 C8 120.52(18) . . ? C10 C9 C12 106.25(16) . . ? C8 C9 C12 133.21(17) . . ? O1 C10 C9 111.46(16) . . ? O1 C10 C5 124.37(15) . . ? C9 C10 C5 124.13(16) . . ? C16 C11 C12 123.57(16) . . ? C16 C11 O1 126.14(15) . . ? C12 C11 O1 110.28(15) . . ? C13 C12 C11 120.93(18) . . ? C13 C12 C9 132.69(17) . . ? C11 C12 C9 106.37(15) . . ? C14 C13 C12 117.13(17) . . ? C13 C14 C15 121.55(18) . . ? C14 C15 C16 123.65(18) . . ? N3 C16 C11 128.27(17) . . ? N3 C16 C15 118.57(17) . . ? C11 C16 C15 113.16(16) . . ? N3 C17 C18 107.18(16) . . ? N4 C18 C17 109.76(15) . . ? 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 N2 Al1 Al2 N3 30.03(12) . . . . ? C22 Al1 Al2 N3 139.26(13) . . . . ? C21 Al1 Al2 N3 -81.94(13) . . . . ? N1 Al1 Al2 N3 -172.54(18) . . . . ? N2 Al1 Al2 C24 -59.15(9) . . . . ? C22 Al1 Al2 C24 50.08(10) . . . . ? C21 Al1 Al2 C24 -171.12(10) . . . . ? N1 Al1 Al2 C24 98.28(16) . . . . ? N2 Al1 Al2 C23 110.34(9) . . . . ? C22 Al1 Al2 C23 -140.44(10) . . . . ? C21 Al1 Al2 C23 -1.64(10) . . . . ? N1 Al1 Al2 C23 -92.24(16) . . . . ? N2 Al1 Al2 N4 -154.89(7) . . . . ? C22 Al1 Al2 N4 -45.66(8) . . . . ? C21 Al1 Al2 N4 93.14(8) . . . . ? N1 Al1 Al2 N4 2.54(15) . . . . ? N2 Al1 N1 C2 -86.34(13) . . . . ? C22 Al1 N1 C2 157.89(13) . . . . ? C21 Al1 N1 C2 29.84(15) . . . . ? Al2 Al1 N1 C2 114.74(16) . . . . ? N2 Al1 N1 C1 148.73(15) . . . . ? C22 Al1 N1 C1 32.96(16) . . . . ? C21 Al1 N1 C1 -95.09(15) . . . . ? Al2 Al1 N1 C1 -10.2(2) . . . . ? N2 Al1 N1 C3 30.95(11) . . . . ? C22 Al1 N1 C3 -84.82(12) . . . . ? C21 Al1 N1 C3 147.13(12) . . . . ? Al2 Al1 N1 C3 -127.97(13) . . . . ? C22 Al1 N2 C5 -93.69(17) . . . . ? C21 Al1 N2 C5 55.77(18) . . . . ? N1 Al1 N2 C5 162.45(16) . . . . ? Al2 Al1 N2 C5 -24.64(17) . . . . ? C22 Al1 N2 C4 95.06(14) . . . . ? C21 Al1 N2 C4 -115.47(14) . . . . ? N1 Al1 N2 C4 -8.79(13) . . . . ? Al2 Al1 N2 C4 164.11(11) . . . . ? C24 Al2 N3 C16 -53.27(18) . . . . ? C23 Al2 N3 C16 88.09(17) . . . . ? N4 Al2 N3 C16 -162.64(15) . . . . ? Al1 Al2 N3 C16 -158.3(2) . . . . ? C24 Al2 N3 C17 120.48(14) . . . . ? C23 Al2 N3 C17 -98.16(15) . . . . ? N4 Al2 N3 C17 11.11(14) . . . . ? Al1 Al2 N3 C17 15.40(10) . . . . ? N3 Al2 N4 C20 -150.69(14) . . . . ? C24 Al2 N4 C20 92.70(15) . . . . ? C23 Al2 N4 C20 -36.08(16) . . . . ? Al1 Al2 N4 C20 -152.89(15) . . . . ? N3 Al2 N4 C19 84.14(14) . . . . ? C24 Al2 N4 C19 -32.46(16) . . . . ? C23 Al2 N4 C19 -161.25(14) . . . . ? Al1 Al2 N4 C19 81.95(13) . . . . ? N3 Al2 N4 C18 -32.78(11) . . . . ? C24 Al2 N4 C18 -149.39(12) . . . . ? C23 Al2 N4 C18 81.83(13) . . . . ? Al1 Al2 N4 C18 -34.98(9) . . . . ? C2 N1 C3 C4 71.20(19) . . . . ? C1 N1 C3 C4 -168.97(16) . . . . ? Al1 N1 C3 C4 -47.21(16) . . . . ? C5 N2 C4 C3 171.13(14) . . . . ? Al1 N2 C4 C3 -16.10(18) . . . . ? N1 C3 C4 N2 43.8(2) . . . . ? C4 N2 C5 C10 -171.27(16) . . . . ? Al1 N2 C5 C10 17.6(3) . . . . ? C4 N2 C5 C6 7.1(2) . . . . ? Al1 N2 C5 C6 -164.10(14) . . . . ? N2 C5 C6 C7 -177.85(17) . . . . ? C10 C5 C6 C7 0.6(2) . . . . ? C5 C6 C7 C8 0.5(3) . . . . ? C6 C7 C8 C9 -0.5(3) . . . . ? C7 C8 C9 C10 -0.7(3) . . . . ? C7 C8 C9 C12 178.06(19) . . . . ? C11 O1 C10 C9 -0.30(18) . . . . ? C11 O1 C10 C5 177.53(16) . . . . ? C8 C9 C10 O1 179.79(15) . . . . ? C12 C9 C10 O1 0.7(2) . . . . ? C8 C9 C10 C5 2.0(3) . . . . ? C12 C9 C10 C5 -177.10(16) . . . . ? N2 C5 C10 O1 -0.9(3) . . . . ? C6 C5 C10 O1 -179.39(15) . . . . ? N2 C5 C10 C9 176.66(16) . . . . ? C6 C5 C10 C9 -1.8(2) . . . . ? C10 O1 C11 C16 -179.20(16) . . . . ? C10 O1 C11 C12 -0.28(18) . . . . ? C16 C11 C12 C13 0.2(3) . . . . ? O1 C11 C12 C13 -178.75(16) . . . . ? C16 C11 C12 C9 179.68(16) . . . . ? O1 C11 C12 C9 0.72(19) . . . . ? C10 C9 C12 C13 178.51(19) . . . . ? C8 C9 C12 C13 -0.4(4) . . . . ? C10 C9 C12 C11 -0.87(19) . . . . ? C8 C9 C12 C11 -179.75(19) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? C9 C12 C13 C14 -178.60(19) . . . . ? C12 C13 C14 C15 -1.3(3) . . . . ? C13 C14 C15 C16 1.0(3) . . . . ? C17 N3 C16 C11 -7.3(3) . . . . ? Al2 N3 C16 C11 166.17(14) . . . . ? C17 N3 C16 C15 172.38(16) . . . . ? Al2 N3 C16 C15 -14.2(2) . . . . ? C12 C11 C16 N3 179.17(17) . . . . ? O1 C11 C16 N3 -2.0(3) . . . . ? C12 C11 C16 C15 -0.5(2) . . . . ? O1 C11 C16 C15 178.28(16) . . . . ? C14 C15 C16 N3 -179.80(17) . . . . ? C14 C15 C16 C11 -0.1(3) . . . . ? C16 N3 C17 C18 -171.65(16) . . . . ? Al2 N3 C17 C18 14.1(2) . . . . ? C20 N4 C18 C17 171.14(17) . . . . ? C19 N4 C18 C17 -68.75(19) . . . . ? Al2 N4 C18 C17 48.66(17) . . . . ? N3 C17 C18 N4 -43.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.436 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.057