# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'R. E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; New reactivity and structural insights of alkali-metal-mediated alumination in directed ortho-alumination of a tertiary aromatic amide ; loop_ _publ_author_name 'R. E. Mulvey' 'Joaquin Garcia-Alvarez' 'D. Graham' 'Alan Kennedy' 'Susan Weatherstone' data_grem189 _database_code_depnum_ccdc_archive 'CCDC 606350' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H61 Al N3 Na' _chemical_formula_weight 477.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.3767(2) _cell_length_b 16.9980(4) _cell_length_c 17.8197(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3143.09(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3902 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35650 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.09 _reflns_number_total 6929 _reflns_number_gt 5768 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+1.5263P] 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 0.00(19) _refine_ls_number_reflns 6929 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.005 _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 0.56113(6) 0.87947(4) 0.79599(3) 0.02547(14) Uani 1 1 d . . . Na1 Na 0.84740(8) 0.87419(6) 0.72026(5) 0.0304(2) Uani 1 1 d . . . N1 N 0.73217(17) 0.85477(11) 0.83796(10) 0.0273(4) Uani 1 1 d . . . N2 N 1.02425(19) 0.95588(12) 0.67313(11) 0.0348(5) Uani 1 1 d . . . N3 N 0.9331(2) 0.79903(13) 0.60916(13) 0.0482(6) Uani 1 1 d . . . C1 C 0.6006(2) 0.90463(14) 0.68658(12) 0.0276(5) Uani 1 1 d . . . C2 C 0.4878(2) 0.92928(14) 0.63438(14) 0.0346(5) Uani 1 1 d . . . H2 H 0.4068 0.9058 0.6549 0.042 Uiso 1 1 calc R . . C3 C 0.4702(3) 1.01822(15) 0.63202(15) 0.0444(6) Uani 1 1 d . . . H3A H 0.3970 1.0313 0.5996 0.067 Uiso 1 1 calc R . . H3B H 0.5485 1.0428 0.6121 0.067 Uiso 1 1 calc R . . H3C H 0.4539 1.0379 0.6828 0.067 Uiso 1 1 calc R . . C4 C 0.5045(3) 0.89962(18) 0.55437(15) 0.0509(7) Uani 1 1 d . . . H4A H 0.5847 0.9207 0.5334 0.076 Uiso 1 1 calc R . . H4B H 0.4314 0.9171 0.5237 0.076 Uiso 1 1 calc R . . H4C H 0.5082 0.8420 0.5545 0.076 Uiso 1 1 calc R . . C5 C 0.4179(3) 0.79759(15) 0.80339(17) 0.0389(6) Uani 1 1 d . . . C6 C 0.3992(3) 0.71659(16) 0.76789(16) 0.0422(6) Uani 1 1 d . . . H6 H 0.4725 0.6825 0.7843 0.051 Uiso 1 1 calc R . . C7 C 0.4017(3) 0.72043(16) 0.68296(16) 0.0440(6) Uani 1 1 d . . . H7A H 0.3323 0.7549 0.6653 0.066 Uiso 1 1 calc R . . H7B H 0.3895 0.6675 0.6623 0.066 Uiso 1 1 calc R . . H7C H 0.4849 0.7413 0.6663 0.066 Uiso 1 1 calc R . . C8 C 0.2742(3) 0.67780(18) 0.79448(19) 0.0548(8) Uani 1 1 d . . . H8A H 0.2638 0.6268 0.7695 0.082 Uiso 1 1 calc R . . H8B H 0.2009 0.7118 0.7820 0.082 Uiso 1 1 calc R . . H8C H 0.2777 0.6700 0.8489 0.082 Uiso 1 1 calc R . . C9 C 0.4632(2) 0.97673(15) 0.83031(15) 0.0351(5) Uani 1 1 d . . . C10 C 0.4070(3) 0.99941(16) 0.90579(15) 0.0431(6) Uani 1 1 d . . . H10 H 0.4802 1.0143 0.9394 0.052 Uiso 1 1 calc R . . C11 C 0.3179(3) 1.07130(18) 0.89897(17) 0.0531(7) Uani 1 1 d . . . H11A H 0.2428 1.0576 0.8683 0.080 Uiso 1 1 calc R . . H11B H 0.3649 1.1147 0.8752 0.080 Uiso 1 1 calc R . . H11C H 0.2893 1.0875 0.9491 0.080 Uiso 1 1 calc R . . C12 C 0.3324(3) 0.93235(17) 0.94407(15) 0.0461(7) Uani 1 1 d . . . H12A H 0.3907 0.8880 0.9532 0.069 Uiso 1 1 calc R . . H12B H 0.2616 0.9153 0.9115 0.069 Uiso 1 1 calc R . . H12C H 0.2975 0.9510 0.9920 0.069 Uiso 1 1 calc R . . C13 C 0.7912(2) 0.91169(17) 0.89232(13) 0.0377(6) Uani 1 1 d . . . C14 C 0.9341(2) 0.89464(18) 0.90635(14) 0.0457(7) Uani 1 1 d . . . H14A H 0.9834 0.9076 0.8604 0.055 Uiso 1 1 calc R . . H14B H 0.9652 0.9294 0.9471 0.055 Uiso 1 1 calc R . . C15 C 0.9612(3) 0.8092(2) 0.92782(17) 0.0604(9) Uani 1 1 d . . . H15A H 1.0551 0.8008 0.9333 0.072 Uiso 1 1 calc R . . H15B H 0.9192 0.7966 0.9762 0.072 Uiso 1 1 calc R . . C16 C 0.9085(3) 0.75716(18) 0.86658(18) 0.0530(8) Uani 1 1 d . . . H16A H 0.9227 0.7015 0.8807 0.064 Uiso 1 1 calc R . . H16B H 0.9572 0.7673 0.8198 0.064 Uiso 1 1 calc R . . C17 C 0.7634(3) 0.76962(15) 0.85097(15) 0.0401(6) Uani 1 1 d . . . C18 C 0.7861(3) 0.99401(15) 0.85807(16) 0.0418(6) Uani 1 1 d . . . H18A H 0.6960 1.0106 0.8531 0.063 Uiso 1 1 calc R . . H18B H 0.8268 0.9933 0.8085 0.063 Uiso 1 1 calc R . . H18C H 0.8321 1.0310 0.8907 0.063 Uiso 1 1 calc R . . C19 C 0.7205(3) 0.9152(2) 0.96895(15) 0.0550(8) Uani 1 1 d . . . H19A H 0.6271 0.9152 0.9606 0.083 Uiso 1 1 calc R . . H19B H 0.7453 0.9633 0.9956 0.083 Uiso 1 1 calc R . . H19C H 0.7443 0.8692 0.9991 0.083 Uiso 1 1 calc R . . C20 C 0.7332(3) 0.72468(16) 0.77860(19) 0.0426(6) Uani 1 1 d . . . C21 C 0.6841(3) 0.73161(19) 0.91479(18) 0.0592(8) Uani 1 1 d . . . H21A H 0.5925 0.7432 0.9074 0.089 Uiso 1 1 calc R . . H21B H 0.7124 0.7530 0.9632 0.089 Uiso 1 1 calc R . . H21C H 0.6973 0.6745 0.9143 0.089 Uiso 1 1 calc R . . C22 C 1.1185(3) 0.9829(2) 0.72818(18) 0.0595(8) Uani 1 1 d . . . H22A H 1.0756 1.0161 0.7656 0.089 Uiso 1 1 calc R . . H22B H 1.1858 1.0134 0.7028 0.089 Uiso 1 1 calc R . . H22C H 1.1575 0.9374 0.7532 0.089 Uiso 1 1 calc R . . C23 C 0.9657(3) 1.0240(2) 0.6378(2) 0.0681(10) Uani 1 1 d . . . H23A H 1.0308 1.0520 0.6083 0.102 Uiso 1 1 calc R . . H23B H 0.9312 1.0591 0.6766 0.102 Uiso 1 1 calc R . . H23C H 0.8957 1.0068 0.6048 0.102 Uiso 1 1 calc R . . C24 C 1.0920(3) 0.9066(2) 0.61727(18) 0.0582(8) Uani 1 1 d . . . H24A H 1.1431 0.9417 0.5844 0.070 Uiso 1 1 calc R . . H24B H 1.1534 0.8723 0.6443 0.070 Uiso 1 1 calc R . . C25 C 1.0109(4) 0.8568(2) 0.5694(2) 0.0755(11) Uani 1 1 d . . . H25A H 0.9527 0.8911 0.5400 0.091 Uiso 1 1 calc R . . H25B H 1.0671 0.8287 0.5334 0.091 Uiso 1 1 calc R . . C26 C 1.0031(3) 0.7275(2) 0.63012(19) 0.0604(8) Uani 1 1 d . . . H26A H 1.0676 0.7402 0.6685 0.091 Uiso 1 1 calc R . . H26B H 1.0463 0.7058 0.5858 0.091 Uiso 1 1 calc R . . H26C H 0.9424 0.6887 0.6501 0.091 Uiso 1 1 calc R . . C27 C 0.8297(4) 0.7760(2) 0.55654(19) 0.0706(10) Uani 1 1 d . . . H27A H 0.8681 0.7542 0.5108 0.106 Uiso 1 1 calc R . . H27B H 0.7779 0.8223 0.5438 0.106 Uiso 1 1 calc R . . H27C H 0.7747 0.7362 0.5802 0.106 Uiso 1 1 calc R . . H1A H 0.641(2) 0.8563(15) 0.6641(15) 0.036(7) Uiso 1 1 d . . . H1B H 0.665(3) 0.9417(16) 0.6815(15) 0.039(7) Uiso 1 1 d . . . H5A H 0.336(3) 0.8254(18) 0.7878(18) 0.061(9) Uiso 1 1 d . . . H5B H 0.406(3) 0.7887(17) 0.8529(18) 0.047(8) Uiso 1 1 d . . . H9A H 0.503(3) 1.0251(17) 0.8103(15) 0.042(7) Uiso 1 1 d . . . H9B H 0.384(3) 0.9723(16) 0.7897(16) 0.047(8) Uiso 1 1 d . . . H20A H 0.790(3) 0.7391(18) 0.7398(18) 0.052(9) Uiso 1 1 d . . . H20B H 0.743(3) 0.6714(19) 0.7837(17) 0.049(8) Uiso 1 1 d . . . H20C H 0.650(3) 0.7340(18) 0.7582(17) 0.055(9) 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 Al1 0.0230(3) 0.0266(3) 0.0268(3) -0.0019(3) 0.0022(3) -0.0010(3) Na1 0.0269(4) 0.0360(5) 0.0283(4) -0.0015(4) 0.0040(3) -0.0021(4) N1 0.0263(9) 0.0323(10) 0.0233(9) 0.0038(8) -0.0002(8) 0.0005(8) N2 0.0313(10) 0.0365(11) 0.0367(11) 0.0026(9) 0.0009(9) -0.0024(8) N3 0.0541(14) 0.0411(12) 0.0493(13) -0.0116(10) 0.0217(12) -0.0083(11) C1 0.0225(10) 0.0309(11) 0.0294(11) -0.0009(9) 0.0015(9) -0.0027(9) C2 0.0325(12) 0.0353(12) 0.0362(13) 0.0044(10) -0.0044(10) -0.0003(10) C3 0.0484(15) 0.0436(15) 0.0413(14) 0.0048(12) -0.0053(12) 0.0056(12) C4 0.0641(18) 0.0527(17) 0.0361(14) 0.0021(12) -0.0184(13) 0.0012(14) C5 0.0349(13) 0.0384(14) 0.0434(15) -0.0036(12) 0.0088(12) -0.0052(11) C6 0.0372(13) 0.0385(14) 0.0509(15) 0.0032(12) 0.0016(12) -0.0057(11) C7 0.0431(14) 0.0373(14) 0.0517(16) -0.0080(12) -0.0003(12) -0.0030(11) C8 0.0503(16) 0.0497(17) 0.0645(19) 0.0043(15) 0.0009(16) -0.0202(13) C9 0.0318(13) 0.0328(12) 0.0408(13) -0.0036(11) 0.0079(11) 0.0022(10) C10 0.0424(14) 0.0474(15) 0.0396(14) -0.0037(12) 0.0027(12) 0.0063(12) C11 0.0528(17) 0.0568(18) 0.0497(16) -0.0095(14) 0.0080(14) 0.0197(14) C12 0.0466(15) 0.0526(17) 0.0391(14) -0.0062(13) 0.0096(12) -0.0014(13) C13 0.0324(12) 0.0574(16) 0.0234(11) -0.0061(11) -0.0020(10) -0.0014(11) C14 0.0319(12) 0.0718(19) 0.0334(12) -0.0036(12) -0.0096(11) 0.0002(13) C15 0.0381(15) 0.096(2) 0.0468(16) 0.0206(17) -0.0106(13) 0.0103(16) C16 0.0407(15) 0.0548(17) 0.0634(18) 0.0223(15) -0.0023(14) 0.0151(13) C17 0.0383(13) 0.0391(14) 0.0429(15) 0.0172(11) 0.0051(11) 0.0063(11) C18 0.0389(14) 0.0415(14) 0.0449(15) -0.0138(12) -0.0060(12) -0.0059(11) C19 0.0433(15) 0.090(2) 0.0314(14) -0.0104(15) 0.0003(12) 0.0016(16) C20 0.0405(14) 0.0268(13) 0.0606(19) 0.0026(13) 0.0081(15) 0.0032(11) C21 0.0613(19) 0.0603(19) 0.0562(18) 0.0310(16) 0.0087(16) -0.0009(15) C22 0.0408(15) 0.081(2) 0.0567(18) -0.0001(17) -0.0041(14) -0.0205(16) C23 0.058(2) 0.064(2) 0.083(2) 0.0330(19) 0.0118(18) 0.0108(16) C24 0.0433(16) 0.070(2) 0.0613(19) -0.0174(16) 0.0269(14) -0.0164(14) C25 0.089(3) 0.072(2) 0.066(2) -0.0166(18) 0.038(2) -0.018(2) C26 0.0508(17) 0.076(2) 0.0545(18) -0.0154(16) 0.0081(15) 0.0115(16) C27 0.086(3) 0.073(2) 0.0531(19) -0.0199(17) -0.0041(19) 0.021(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 Al1 N1 1.9712(19) . ? Al1 C9 2.034(2) . ? Al1 C1 2.038(2) . ? Al1 C5 2.040(3) . ? Al1 Na1 3.2639(10) . ? Na1 N1 2.4368(19) . ? Na1 N2 2.450(2) . ? Na1 N3 2.518(2) . ? Na1 C1 2.680(2) . ? Na1 C20 2.990(3) . ? Na1 C17 3.057(3) . ? Na1 H1A 2.38(2) . ? Na1 H1B 2.32(3) . ? Na1 H20A 2.40(3) . ? N1 C13 1.500(3) . ? N1 C17 1.501(3) . ? N2 C23 1.450(4) . ? N2 C22 1.460(4) . ? N2 C24 1.479(3) . ? N3 C25 1.455(4) . ? N3 C26 1.465(4) . ? N3 C27 1.478(4) . ? C1 C2 1.553(3) . ? C1 H1A 1.01(3) . ? C1 H1B 0.92(3) . ? C2 C4 1.522(4) . ? C2 C3 1.523(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.528(4) . ? C5 H5A 1.01(3) . ? C5 H5B 0.90(3) . ? C6 C7 1.515(4) . ? C6 C8 1.530(4) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.516(4) . ? C9 H9A 0.99(3) . ? C9 H9B 1.10(3) . ? C10 C11 1.537(4) . ? C10 C12 1.537(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.527(4) . ? C13 C14 1.531(4) . ? C13 C19 1.551(3) . ? C14 C15 1.527(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.508(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.545(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C20 1.531(4) . ? C17 C21 1.545(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.94(3) . ? C20 H20B 0.92(3) . ? C20 H20C 0.95(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.468(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 C9 120.57(10) . . ? N1 Al1 C1 103.10(9) . . ? C9 Al1 C1 102.57(10) . . ? N1 Al1 C5 119.08(10) . . ? C9 Al1 C5 99.85(11) . . ? C1 Al1 C5 110.58(11) . . ? N1 Al1 Na1 48.05(5) . . ? C9 Al1 Na1 126.95(8) . . ? C1 Al1 Na1 55.05(7) . . ? C5 Al1 Na1 132.14(8) . . ? N1 Na1 N2 137.68(8) . . ? N1 Na1 N3 141.37(8) . . ? N2 Na1 N3 75.73(8) . . ? N1 Na1 C1 75.53(7) . . ? N2 Na1 C1 121.97(8) . . ? N3 Na1 C1 105.03(8) . . ? N1 Na1 C20 52.50(8) . . ? N2 Na1 C20 153.85(8) . . ? N3 Na1 C20 88.97(8) . . ? C1 Na1 C20 82.15(8) . . ? N1 Na1 C17 29.01(7) . . ? N2 Na1 C17 143.55(8) . . ? N3 Na1 C17 113.87(8) . . ? C1 Na1 C17 90.60(7) . . ? C20 Na1 C17 29.31(8) . . ? N1 Na1 Al1 36.99(5) . . ? N2 Na1 Al1 143.89(6) . . ? N3 Na1 Al1 131.33(7) . . ? C1 Na1 Al1 38.54(5) . . ? C20 Na1 Al1 61.25(6) . . ? C17 Na1 Al1 56.05(5) . . ? N1 Na1 H1A 84.5(6) . . ? N2 Na1 H1A 127.0(6) . . ? N3 Na1 H1A 85.6(7) . . ? C1 Na1 H1A 21.9(6) . . ? C20 Na1 H1A 71.4(6) . . ? C17 Na1 H1A 89.4(6) . . ? Al1 Na1 H1A 50.2(6) . . ? N1 Na1 H1B 85.6(7) . . ? N2 Na1 H1B 103.2(7) . . ? N3 Na1 H1B 107.8(7) . . ? C1 Na1 H1B 19.6(7) . . ? C20 Na1 H1B 101.6(7) . . ? C17 Na1 H1B 106.4(7) . . ? Al1 Na1 H1B 50.7(7) . . ? H1A Na1 H1B 37.3(8) . . ? N1 Na1 H20A 67.8(8) . . ? N2 Na1 H20A 141.2(8) . . ? N3 Na1 H20A 73.5(8) . . ? C1 Na1 H20A 88.8(7) . . ? C20 Na1 H20A 15.6(8) . . ? C17 Na1 H20A 42.4(8) . . ? Al1 Na1 H20A 74.9(8) . . ? H1A Na1 H20A 73.4(9) . . ? H1B Na1 H20A 108.3(10) . . ? C13 N1 C17 115.72(19) . . ? C13 N1 Al1 118.38(14) . . ? C17 N1 Al1 117.29(15) . . ? C13 N1 Na1 105.55(13) . . ? C17 N1 Na1 99.06(13) . . ? Al1 N1 Na1 94.95(7) . . ? C23 N2 C22 108.7(3) . . ? C23 N2 C24 111.0(2) . . ? C22 N2 C24 108.2(2) . . ? C23 N2 Na1 106.70(17) . . ? C22 N2 Na1 116.75(17) . . ? C24 N2 Na1 105.42(15) . . ? C25 N3 C26 114.1(3) . . ? C25 N3 C27 105.8(3) . . ? C26 N3 C27 107.6(2) . . ? C25 N3 Na1 103.68(17) . . ? C26 N3 Na1 113.32(18) . . ? C27 N3 Na1 112.15(19) . . ? C2 C1 Al1 118.57(16) . . ? C2 C1 Na1 155.01(16) . . ? Al1 C1 Na1 86.41(8) . . ? C2 C1 H1A 107.3(15) . . ? Al1 C1 H1A 107.1(15) . . ? Na1 C1 H1A 62.1(14) . . ? C2 C1 H1B 107.6(17) . . ? Al1 C1 H1B 112.5(17) . . ? Na1 C1 H1B 57.4(17) . . ? H1A C1 H1B 102(2) . . ? C4 C2 C3 108.5(2) . . ? C4 C2 C1 112.7(2) . . ? C3 C2 C1 112.0(2) . . ? C4 C2 H2 107.8 . . ? C3 C2 H2 107.8 . . ? C1 C2 H2 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Al1 132.89(19) . . ? C6 C5 H5A 101.5(18) . . ? Al1 C5 H5A 106.1(18) . . ? C6 C5 H5B 103.7(19) . . ? Al1 C5 H5B 105.9(19) . . ? H5A C5 H5B 104(3) . . ? C7 C6 C5 111.9(2) . . ? C7 C6 C8 110.0(2) . . ? C5 C6 C8 111.6(2) . . ? C7 C6 H6 107.7 . . ? C5 C6 H6 107.7 . . ? C8 C6 H6 107.7 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Al1 131.73(19) . . ? C10 C9 H9A 105.7(16) . . ? Al1 C9 H9A 111.0(16) . . ? C10 C9 H9B 108.2(15) . . ? Al1 C9 H9B 96.9(15) . . ? H9A C9 H9B 98(2) . . ? C9 C10 C11 111.3(2) . . ? C9 C10 C12 113.5(2) . . ? C11 C10 C12 108.8(2) . . ? C9 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C18 108.59(19) . . ? N1 C13 C14 112.3(2) . . ? C18 C13 C14 105.8(2) . . ? N1 C13 C19 113.6(2) . . ? C18 C13 C19 107.5(2) . . ? C14 C13 C19 108.7(2) . . ? C15 C14 C13 113.5(2) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 108.0(2) . . ? C16 C15 H15A 110.1 . . ? C14 C15 H15A 110.1 . . ? C16 C15 H15B 110.1 . . ? C14 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? C15 C16 C17 113.8(3) . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N1 C17 C20 107.9(2) . . ? N1 C17 C16 111.7(2) . . ? C20 C17 C16 106.4(2) . . ? N1 C17 C21 113.7(2) . . ? C20 C17 C21 107.6(2) . . ? C16 C17 C21 109.2(2) . . ? N1 C17 Na1 51.93(10) . . ? C20 C17 Na1 72.94(14) . . ? C16 C17 Na1 86.51(15) . . ? C21 C17 Na1 162.89(19) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 Na1 77.75(14) . . ? C17 C20 H20A 111.3(19) . . ? Na1 C20 H20A 43.6(19) . . ? C17 C20 H20B 112.7(19) . . ? Na1 C20 H20B 146.0(18) . . ? H20A C20 H20B 105(3) . . ? C17 C20 H20C 115.1(19) . . ? Na1 C20 H20C 95.0(19) . . ? H20A C20 H20C 104(3) . . ? H20B C20 H20C 108(3) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 N2 116.5(3) . . ? C25 C24 H24A 108.2 . . ? N2 C24 H24A 108.2 . . ? C25 C24 H24B 108.2 . . ? N2 C24 H24B 108.2 . . ? H24A C24 H24B 107.3 . . ? N3 C25 C24 115.1(3) . . ? N3 C25 H25A 108.5 . . ? C24 C25 H25A 108.5 . . ? N3 C25 H25B 108.5 . . ? C24 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Al1 Na1 N1 100.35(12) . . . . ? C1 Al1 Na1 N1 179.19(12) . . . . ? C5 Al1 Na1 N1 -93.91(14) . . . . ? N1 Al1 Na1 N2 -105.39(13) . . . . ? C9 Al1 Na1 N2 -5.04(15) . . . . ? C1 Al1 Na1 N2 73.80(13) . . . . ? C5 Al1 Na1 N2 160.70(15) . . . . ? N1 Al1 Na1 N3 124.16(12) . . . . ? C9 Al1 Na1 N3 -135.49(13) . . . . ? C1 Al1 Na1 N3 -56.65(12) . . . . ? C5 Al1 Na1 N3 30.25(16) . . . . ? N1 Al1 Na1 C1 -179.19(12) . . . . ? C9 Al1 Na1 C1 -78.84(13) . . . . ? C5 Al1 Na1 C1 86.90(15) . . . . ? N1 Al1 Na1 C20 64.80(10) . . . . ? C9 Al1 Na1 C20 165.15(12) . . . . ? C1 Al1 Na1 C20 -116.01(12) . . . . ? C5 Al1 Na1 C20 -29.11(14) . . . . ? N1 Al1 Na1 C17 30.86(10) . . . . ? C9 Al1 Na1 C17 131.21(12) . . . . ? C1 Al1 Na1 C17 -149.95(11) . . . . ? C5 Al1 Na1 C17 -63.05(14) . . . . ? C9 Al1 N1 C13 -3.4(2) . . . . ? C1 Al1 N1 C13 109.97(17) . . . . ? C5 Al1 N1 C13 -127.18(17) . . . . ? Na1 Al1 N1 C13 110.66(17) . . . . ? C9 Al1 N1 C17 143.07(17) . . . . ? C1 Al1 N1 C17 -103.55(17) . . . . ? C5 Al1 N1 C17 19.3(2) . . . . ? Na1 Al1 N1 C17 -102.87(17) . . . . ? C9 Al1 N1 Na1 -114.07(10) . . . . ? C1 Al1 N1 Na1 -0.68(10) . . . . ? C5 Al1 N1 Na1 122.16(10) . . . . ? N2 Na1 N1 C13 1.16(19) . . . . ? N3 Na1 N1 C13 143.15(16) . . . . ? C1 Na1 N1 C13 -120.77(15) . . . . ? C20 Na1 N1 C13 148.07(17) . . . . ? C17 Na1 N1 C13 120.0(2) . . . . ? Al1 Na1 N1 C13 -121.29(16) . . . . ? N2 Na1 N1 C17 -118.88(16) . . . . ? N3 Na1 N1 C17 23.1(2) . . . . ? C1 Na1 N1 C17 119.20(15) . . . . ? C20 Na1 N1 C17 28.04(14) . . . . ? Al1 Na1 N1 C17 118.68(16) . . . . ? N2 Na1 N1 Al1 122.45(10) . . . . ? N3 Na1 N1 Al1 -95.56(14) . . . . ? C1 Na1 N1 Al1 0.52(7) . . . . ? C20 Na1 N1 Al1 -90.64(10) . . . . ? C17 Na1 N1 Al1 -118.68(16) . . . . ? N1 Na1 N2 C23 -95.6(2) . . . . ? N3 Na1 N2 C23 107.7(2) . . . . ? C1 Na1 N2 C23 8.7(2) . . . . ? C20 Na1 N2 C23 163.7(2) . . . . ? C17 Na1 N2 C23 -141.3(2) . . . . ? Al1 Na1 N2 C23 -36.1(2) . . . . ? N1 Na1 N2 C22 26.1(2) . . . . ? N3 Na1 N2 C22 -130.5(2) . . . . ? C1 Na1 N2 C22 130.5(2) . . . . ? C20 Na1 N2 C22 -74.6(3) . . . . ? C17 Na1 N2 C22 -19.5(3) . . . . ? Al1 Na1 N2 C22 85.6(2) . . . . ? N1 Na1 N2 C24 146.23(18) . . . . ? N3 Na1 N2 C24 -10.40(19) . . . . ? C1 Na1 N2 C24 -109.41(19) . . . . ? C20 Na1 N2 C24 45.5(3) . . . . ? C17 Na1 N2 C24 100.6(2) . . . . ? Al1 Na1 N2 C24 -154.27(17) . . . . ? N1 Na1 N3 C25 -170.4(2) . . . . ? N2 Na1 N3 C25 -15.7(2) . . . . ? C1 Na1 N3 C25 104.1(2) . . . . ? C20 Na1 N3 C25 -174.3(2) . . . . ? C17 Na1 N3 C25 -158.3(2) . . . . ? Al1 Na1 N3 C25 136.8(2) . . . . ? N1 Na1 N3 C26 -46.1(3) . . . . ? N2 Na1 N3 C26 108.6(2) . . . . ? C1 Na1 N3 C26 -131.6(2) . . . . ? C20 Na1 N3 C26 -50.0(2) . . . . ? C17 Na1 N3 C26 -34.1(2) . . . . ? Al1 Na1 N3 C26 -99.0(2) . . . . ? N1 Na1 N3 C27 75.9(3) . . . . ? N2 Na1 N3 C27 -129.4(2) . . . . ? C1 Na1 N3 C27 -9.5(2) . . . . ? C20 Na1 N3 C27 72.0(2) . . . . ? C17 Na1 N3 C27 88.0(2) . . . . ? Al1 Na1 N3 C27 23.1(2) . . . . ? N1 Al1 C1 C2 -178.62(17) . . . . ? C9 Al1 C1 C2 -52.7(2) . . . . ? C5 Al1 C1 C2 53.0(2) . . . . ? Na1 Al1 C1 C2 -179.2(2) . . . . ? N1 Al1 C1 Na1 0.62(9) . . . . ? C9 Al1 C1 Na1 126.55(9) . . . . ? C5 Al1 C1 Na1 -127.73(10) . . . . ? N1 Na1 C1 C2 177.9(4) . . . . ? N2 Na1 C1 C2 40.3(4) . . . . ? N3 Na1 C1 C2 -42.1(4) . . . . ? C20 Na1 C1 C2 -128.9(4) . . . . ? C17 Na1 C1 C2 -157.0(4) . . . . ? Al1 Na1 C1 C2 178.4(5) . . . . ? N1 Na1 C1 Al1 -0.50(7) . . . . ? N2 Na1 C1 Al1 -138.16(8) . . . . ? N3 Na1 C1 Al1 139.50(8) . . . . ? C20 Na1 C1 Al1 52.70(9) . . . . ? C17 Na1 C1 Al1 24.54(9) . . . . ? Al1 C1 C2 C4 -145.17(19) . . . . ? Na1 C1 C2 C4 36.6(5) . . . . ? Al1 C1 C2 C3 92.2(2) . . . . ? Na1 C1 C2 C3 -86.0(4) . . . . ? N1 Al1 C5 C6 -66.9(3) . . . . ? C9 Al1 C5 C6 159.7(3) . . . . ? C1 Al1 C5 C6 52.2(3) . . . . ? Na1 Al1 C5 C6 -8.8(4) . . . . ? Al1 C5 C6 C7 -58.0(4) . . . . ? Al1 C5 C6 C8 178.2(2) . . . . ? N1 Al1 C9 C10 -64.7(3) . . . . ? C1 Al1 C9 C10 -178.4(2) . . . . ? C5 Al1 C9 C10 67.8(3) . . . . ? Na1 Al1 C9 C10 -122.9(2) . . . . ? Al1 C9 C10 C11 -168.2(2) . . . . ? Al1 C9 C10 C12 -45.0(4) . . . . ? C17 N1 C13 C18 162.42(19) . . . . ? Al1 N1 C13 C18 -50.6(2) . . . . ? Na1 N1 C13 C18 54.0(2) . . . . ? C17 N1 C13 C14 45.8(3) . . . . ? Al1 N1 C13 C14 -167.20(17) . . . . ? Na1 N1 C13 C14 -62.6(2) . . . . ? C17 N1 C13 C19 -78.1(3) . . . . ? Al1 N1 C13 C19 68.9(3) . . . . ? Na1 N1 C13 C19 173.53(19) . . . . ? N1 C13 C14 C15 -51.6(3) . . . . ? C18 C13 C14 C15 -169.9(2) . . . . ? C19 C13 C14 C15 75.0(3) . . . . ? C13 C14 C15 C16 56.4(3) . . . . ? C14 C15 C16 C17 -56.5(3) . . . . ? C13 N1 C17 C20 -162.1(2) . . . . ? Al1 N1 C17 C20 50.5(2) . . . . ? Na1 N1 C17 C20 -49.9(2) . . . . ? C13 N1 C17 C16 -45.5(3) . . . . ? Al1 N1 C17 C16 167.11(18) . . . . ? Na1 N1 C17 C16 66.7(2) . . . . ? C13 N1 C17 C21 78.6(3) . . . . ? Al1 N1 C17 C21 -68.7(3) . . . . ? Na1 N1 C17 C21 -169.1(2) . . . . ? C13 N1 C17 Na1 -112.22(18) . . . . ? Al1 N1 C17 Na1 100.41(13) . . . . ? C15 C16 C17 N1 51.9(3) . . . . ? C15 C16 C17 C20 169.3(2) . . . . ? C15 C16 C17 C21 -74.8(3) . . . . ? C15 C16 C17 Na1 98.3(2) . . . . ? N2 Na1 C17 N1 97.18(17) . . . . ? N3 Na1 C17 N1 -164.46(14) . . . . ? C1 Na1 C17 N1 -57.70(14) . . . . ? C20 Na1 C17 N1 -130.4(2) . . . . ? Al1 Na1 C17 N1 -39.52(11) . . . . ? N1 Na1 C17 C20 130.4(2) . . . . ? N2 Na1 C17 C20 -132.44(17) . . . . ? N3 Na1 C17 C20 -34.08(17) . . . . ? C1 Na1 C17 C20 72.68(15) . . . . ? Al1 Na1 C17 C20 90.86(15) . . . . ? N1 Na1 C17 C16 -121.3(2) . . . . ? N2 Na1 C17 C16 -24.1(2) . . . . ? N3 Na1 C17 C16 74.27(19) . . . . ? C1 Na1 C17 C16 -178.98(18) . . . . ? C20 Na1 C17 C16 108.3(2) . . . . ? Al1 Na1 C17 C16 -160.80(19) . . . . ? N1 Na1 C17 C21 35.9(7) . . . . ? N2 Na1 C17 C21 133.1(7) . . . . ? N3 Na1 C17 C21 -128.6(7) . . . . ? C1 Na1 C17 C21 -21.8(7) . . . . ? C20 Na1 C17 C21 -94.5(7) . . . . ? Al1 Na1 C17 C21 -3.6(7) . . . . ? N1 C17 C20 Na1 39.05(16) . . . . ? C16 C17 C20 Na1 -80.99(18) . . . . ? C21 C17 C20 Na1 162.1(2) . . . . ? N1 Na1 C20 C17 -27.75(13) . . . . ? N2 Na1 C20 C17 95.8(2) . . . . ? N3 Na1 C20 C17 149.17(16) . . . . ? C1 Na1 C20 C17 -105.50(15) . . . . ? Al1 Na1 C20 C17 -71.08(14) . . . . ? C23 N2 C24 C25 -76.8(4) . . . . ? C22 N2 C24 C25 164.0(3) . . . . ? Na1 N2 C24 C25 38.4(3) . . . . ? C26 N3 C25 C24 -81.2(4) . . . . ? C27 N3 C25 C24 160.8(3) . . . . ? Na1 N3 C25 C24 42.6(4) . . . . ? N2 C24 C25 N3 -60.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.624 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.041 #===END data_grem222 _database_code_depnum_ccdc_archive 'CCDC 606351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H64 Al N4 Na' _chemical_formula_weight 554.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.4085(4) _cell_length_b 9.7578(4) _cell_length_c 10.5611(4) _cell_angle_alpha 102.489(2) _cell_angle_beta 102.940(2) _cell_angle_gamma 91.186(2) _cell_volume 920.16(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4897 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 29.13 _exptl_crystal_description lump _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 308 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23628 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 29.26 _reflns_number_total 9674 _reflns_number_gt 7563 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SIR _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.4036P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(14) _refine_ls_number_reflns 9674 _refine_ls_number_parameters 382 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al -0.03699(6) -0.02099(6) 0.47655(6) 0.02803(14) Uani 1 1 d . . . Na1 Na 0.29440(9) 0.14756(9) 0.77270(8) 0.0335(2) Uani 1 1 d . . . N1 N 0.2356(2) 0.0190(2) 0.9417(2) 0.0390(5) Uani 1 1 d . . . N2 N 0.51253(19) -0.02400(19) 0.83111(18) 0.0328(4) Uani 1 1 d . . . N3 N 0.3884(2) 0.4016(2) 0.9162(2) 0.0456(5) Uani 1 1 d . . . N4 N 0.3993(2) 0.2784(2) 0.6286(2) 0.0393(5) Uani 1 1 d . . . C1 C -0.0218(2) 0.1456(2) 0.6314(2) 0.0307(4) Uani 1 1 d . . . C2 C -0.0442(2) 0.2529(2) 0.7045(2) 0.0291(4) Uani 1 1 d . . . C3 C -0.0794(2) 0.3841(2) 0.78026(19) 0.0260(4) Uani 1 1 d . . . C4 C -0.0898(2) 0.4007(2) 0.9122(2) 0.0294(4) Uani 1 1 d . . . H4 H -0.0747 0.3234 0.9539 0.035 Uiso 1 1 calc R . . C5 C -0.1216(2) 0.5280(2) 0.9832(2) 0.0343(5) Uani 1 1 d . . . H5 H -0.1264 0.5380 1.0736 0.041 Uiso 1 1 calc R . . C6 C -0.1465(3) 0.6409(2) 0.9236(2) 0.0395(5) Uani 1 1 d . . . H6 H -0.1686 0.7282 0.9727 0.047 Uiso 1 1 calc R . . C7 C -0.1391(3) 0.6261(2) 0.7922(2) 0.0410(6) Uani 1 1 d . . . H7 H -0.1578 0.7030 0.7504 0.049 Uiso 1 1 calc R . . C8 C -0.1045(3) 0.4994(2) 0.7211(2) 0.0340(5) Uani 1 1 d . . . H8 H -0.0978 0.4907 0.6313 0.041 Uiso 1 1 calc R . . C9 C 0.1551(3) -0.1095(3) 0.5194(2) 0.0370(5) Uani 1 1 d . . . C10 C 0.1819(3) -0.2524(3) 0.4374(3) 0.0466(6) Uani 1 1 d . . . H10 H 0.2880 -0.2677 0.4659 0.056 Uiso 1 1 calc R . . C11 C 0.1483(4) -0.2544(4) 0.2905(3) 0.0798(11) Uani 1 1 d . . . H11A H 0.0445 -0.2403 0.2598 0.120 Uiso 1 1 calc R . . H11B H 0.1703 -0.3454 0.2409 0.120 Uiso 1 1 calc R . . H11C H 0.2081 -0.1789 0.2752 0.120 Uiso 1 1 calc R . . C12 C 0.0945(4) -0.3692(3) 0.4675(5) 0.0841(12) Uani 1 1 d . . . H12A H 0.1087 -0.4598 0.4118 0.126 Uiso 1 1 calc R . . H12B H -0.0095 -0.3517 0.4482 0.126 Uiso 1 1 calc R . . H12C H 0.1279 -0.3713 0.5618 0.126 Uiso 1 1 calc R . . C13 C -0.0491(3) 0.0647(3) 0.3173(2) 0.0356(5) Uani 1 1 d . . . C14 C -0.1065(3) 0.2110(2) 0.3250(2) 0.0357(5) Uani 1 1 d . . . H14 H -0.0529 0.2725 0.4120 0.043 Uiso 1 1 calc R . . C15 C -0.2677(3) 0.2068(3) 0.3243(3) 0.0522(7) Uani 1 1 d . . . H15A H -0.3240 0.1517 0.2380 0.078 Uiso 1 1 calc R . . H15B H -0.2993 0.3029 0.3389 0.078 Uiso 1 1 calc R . . H15C H -0.2841 0.1631 0.3956 0.078 Uiso 1 1 calc R . . C16 C -0.0798(3) 0.2794(3) 0.2143(3) 0.0524(7) Uani 1 1 d . . . H16A H -0.1215 0.3712 0.2228 0.079 Uiso 1 1 calc R . . H16B H -0.1263 0.2188 0.1272 0.079 Uiso 1 1 calc R . . H16C H 0.0256 0.2920 0.2218 0.079 Uiso 1 1 calc R . . C17 C -0.2107(3) -0.1396(2) 0.4836(2) 0.0343(5) Uani 1 1 d . B . C18 C -0.2956(3) -0.2529(2) 0.3632(2) 0.0386(5) Uani 1 1 d . . . H18 H -0.2166 -0.3065 0.3303 0.046 Uiso 1 1 calc R A 1 C19 C -0.3836(3) -0.3630(3) 0.4010(3) 0.0519(7) Uani 1 1 d . B . H19A H -0.4297 -0.4346 0.3207 0.078 Uiso 1 1 calc R . . H19B H -0.4594 -0.3182 0.4424 0.078 Uiso 1 1 calc R . . H19C H -0.3187 -0.4075 0.4641 0.078 Uiso 1 1 calc R . . C21 C 0.0804(3) -0.0313(3) 0.9026(3) 0.0588(8) Uani 1 1 d . . . H21A H 0.0200 0.0495 0.9066 0.088 Uiso 1 1 calc R . . H21B H 0.0599 -0.0876 0.9637 0.088 Uiso 1 1 calc R . . H21C H 0.0578 -0.0893 0.8115 0.088 Uiso 1 1 calc R . . C22 C 0.2642(4) 0.1089(3) 1.0750(3) 0.0629(8) Uani 1 1 d . . . H22A H 0.2441 0.0543 1.1375 0.094 Uiso 1 1 calc R . . H22B H 0.2010 0.1875 1.0751 0.094 Uiso 1 1 calc R . . H22C H 0.3669 0.1456 1.1022 0.094 Uiso 1 1 calc R . . C23 C 0.3256(3) -0.1037(3) 0.9389(3) 0.0407(6) Uani 1 1 d . . . H23A H 0.2856 -0.1748 0.8551 0.049 Uiso 1 1 calc R . . H23B H 0.3179 -0.1466 1.0142 0.049 Uiso 1 1 calc R . . C24 C 0.4851(3) -0.0673(3) 0.9480(2) 0.0407(6) Uani 1 1 d . . . H24A H 0.5226 0.0097 1.0277 0.049 Uiso 1 1 calc R . . H24B H 0.5406 -0.1503 0.9608 0.049 Uiso 1 1 calc R . . C25 C 0.4992(3) -0.1455(3) 0.7197(2) 0.0410(5) Uani 1 1 d . . . H25A H 0.3992 -0.1891 0.6948 0.061 Uiso 1 1 calc R . . H25B H 0.5679 -0.2141 0.7462 0.061 Uiso 1 1 calc R . . H25C H 0.5218 -0.1150 0.6434 0.061 Uiso 1 1 calc R . . C26 C 0.6644(3) 0.0374(3) 0.8634(3) 0.0487(7) Uani 1 1 d . . . H26A H 0.6859 0.0622 0.7842 0.073 Uiso 1 1 calc R . . H26B H 0.7316 -0.0313 0.8921 0.073 Uiso 1 1 calc R . . H26C H 0.6766 0.1222 0.9354 0.073 Uiso 1 1 calc R . . C27 C 0.5240(3) 0.3894(3) 1.0103(3) 0.0550(7) Uani 1 1 d . . . H27A H 0.5707 0.4835 1.0546 0.082 Uiso 1 1 calc R . . H27B H 0.5900 0.3349 0.9625 0.082 Uiso 1 1 calc R . . H27C H 0.5028 0.3415 1.0772 0.082 Uiso 1 1 calc R . . C28 C 0.2908(3) 0.4789(3) 0.9915(4) 0.0637(9) Uani 1 1 d . . . H28A H 0.3397 0.5702 1.0428 0.096 Uiso 1 1 calc R . . H28B H 0.2664 0.4246 1.0527 0.096 Uiso 1 1 calc R . . H28C H 0.2010 0.4937 0.9296 0.096 Uiso 1 1 calc R . . C29 C 0.4124(4) 0.4819(3) 0.8200(3) 0.0685(9) Uani 1 1 d . . . H29A H 0.3171 0.5127 0.7782 0.082 Uiso 1 1 calc R . . H29B H 0.4760 0.5676 0.8692 0.082 Uiso 1 1 calc R . . C30 C 0.4777(4) 0.4087(3) 0.7151(4) 0.0709(9) Uani 1 1 d . . . H30A H 0.5768 0.3861 0.7569 0.085 Uiso 1 1 calc R . . H30B H 0.4895 0.4743 0.6580 0.085 Uiso 1 1 calc R . . C31 C 0.5001(4) 0.2048(4) 0.5567(4) 0.0798(11) Uani 1 1 d . . . H31A H 0.5305 0.2633 0.5014 0.120 Uiso 1 1 calc R . . H31B H 0.4516 0.1158 0.4996 0.120 Uiso 1 1 calc R . . H31C H 0.5861 0.1857 0.6204 0.120 Uiso 1 1 calc R . . C32 C 0.2725(3) 0.3070(4) 0.5347(4) 0.0685(9) Uani 1 1 d . . . H32A H 0.2248 0.2183 0.4764 0.103 Uiso 1 1 calc R . . H32B H 0.3029 0.3670 0.4806 0.103 Uiso 1 1 calc R . . H32C H 0.2038 0.3554 0.5834 0.103 Uiso 1 1 calc R . . C20B C -0.3711(7) -0.1972(6) 0.2463(6) 0.0478(13) Uiso 0.50 1 d P B 1 H20A H -0.4394 -0.1288 0.2738 0.072 Uiso 0.50 1 calc PR B 1 H20B H -0.4250 -0.2750 0.1756 0.072 Uiso 0.50 1 calc PR B 1 H20C H -0.2983 -0.1512 0.2127 0.072 Uiso 0.50 1 calc PR B 1 C20A C -0.4184(7) -0.1750(6) 0.2832(6) 0.0458(13) Uiso 0.50 1 d P B 2 H20D H -0.4763 -0.2426 0.2051 0.069 Uiso 0.50 1 calc PR B 2 H20E H -0.3726 -0.1000 0.2540 0.069 Uiso 0.50 1 calc PR B 2 H20F H -0.4823 -0.1342 0.3409 0.069 Uiso 0.50 1 calc PR B 2 H13B H 0.051(3) 0.068(3) 0.293(3) 0.043(7) Uiso 1 1 d . . . H9B H 0.172(3) -0.112(3) 0.610(3) 0.047(7) Uiso 1 1 d . . . H17B H -0.178(3) -0.179(3) 0.562(3) 0.050(8) Uiso 1 1 d . . . H7A H -0.282(3) -0.078(3) 0.518(3) 0.059(8) Uiso 1 1 d . . . H9A H 0.240(3) -0.033(3) 0.521(3) 0.058(8) Uiso 1 1 d . . . H13A H -0.108(3) 0.006(3) 0.248(3) 0.051(8) 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 Al1 0.0322(3) 0.0300(3) 0.0223(3) 0.0069(3) 0.0059(3) 0.0058(3) Na1 0.0379(5) 0.0278(4) 0.0354(5) 0.0089(4) 0.0088(4) -0.0019(4) N1 0.0355(11) 0.0414(11) 0.0487(12) 0.0199(10) 0.0179(9) 0.0057(9) N2 0.0294(9) 0.0330(9) 0.0339(10) 0.0065(8) 0.0044(8) 0.0036(7) N3 0.0498(13) 0.0311(10) 0.0509(12) 0.0024(9) 0.0093(10) -0.0097(9) N4 0.0383(11) 0.0376(11) 0.0471(11) 0.0156(9) 0.0147(9) 0.0042(9) C1 0.0355(12) 0.0332(11) 0.0245(10) 0.0090(9) 0.0067(9) 0.0038(9) C2 0.0288(11) 0.0358(11) 0.0232(10) 0.0097(9) 0.0044(8) -0.0001(9) C3 0.0254(10) 0.0267(10) 0.0246(9) 0.0047(8) 0.0045(8) -0.0006(8) C4 0.0324(11) 0.0283(10) 0.0282(10) 0.0083(8) 0.0071(8) -0.0006(8) C5 0.0388(13) 0.0359(12) 0.0283(11) 0.0038(9) 0.0118(9) -0.0003(9) C6 0.0457(14) 0.0277(11) 0.0447(13) 0.0032(10) 0.0147(11) 0.0058(10) C7 0.0495(15) 0.0321(12) 0.0457(14) 0.0158(10) 0.0131(11) 0.0071(11) C8 0.0404(13) 0.0338(11) 0.0297(11) 0.0105(9) 0.0088(9) 0.0017(9) C9 0.0377(13) 0.0388(13) 0.0322(12) 0.0061(10) 0.0048(10) 0.0093(10) C10 0.0352(13) 0.0425(14) 0.0514(15) -0.0030(11) 0.0004(11) 0.0107(11) C11 0.086(2) 0.086(2) 0.0459(17) -0.0191(16) 0.0007(16) 0.042(2) C12 0.064(2) 0.0396(16) 0.144(4) 0.019(2) 0.015(2) 0.0128(15) C13 0.0426(14) 0.0392(13) 0.0257(11) 0.0077(10) 0.0087(10) 0.0052(11) C14 0.0472(14) 0.0359(12) 0.0243(10) 0.0101(9) 0.0059(10) 0.0027(10) C15 0.0531(17) 0.0522(16) 0.0599(17) 0.0275(14) 0.0155(14) 0.0161(13) C16 0.074(2) 0.0486(16) 0.0390(13) 0.0196(12) 0.0137(13) 0.0004(14) C17 0.0371(12) 0.0387(12) 0.0272(11) 0.0066(9) 0.0084(9) 0.0019(10) C18 0.0406(13) 0.0372(12) 0.0355(12) 0.0067(10) 0.0050(10) 0.0007(10) C19 0.0596(18) 0.0446(15) 0.0474(15) 0.0063(12) 0.0091(13) -0.0083(13) C21 0.0413(15) 0.075(2) 0.073(2) 0.0416(17) 0.0174(14) -0.0024(14) C22 0.071(2) 0.0541(17) 0.071(2) 0.0057(15) 0.0396(17) -0.0010(15) C23 0.0496(15) 0.0371(13) 0.0415(13) 0.0192(11) 0.0128(11) 0.0055(11) C24 0.0436(14) 0.0450(13) 0.0330(12) 0.0125(10) 0.0035(10) 0.0129(11) C25 0.0369(13) 0.0434(13) 0.0395(13) 0.0035(10) 0.0078(10) 0.0076(10) C26 0.0316(13) 0.0407(14) 0.0686(18) 0.0088(13) 0.0041(12) 0.0022(11) C27 0.0425(15) 0.0477(15) 0.0732(19) 0.0107(14) 0.0134(14) 0.0027(12) C28 0.0364(15) 0.0505(17) 0.096(2) 0.0002(16) 0.0140(15) -0.0004(12) C29 0.101(3) 0.0360(15) 0.067(2) 0.0093(14) 0.0197(18) -0.0167(16) C30 0.084(2) 0.0574(19) 0.080(2) 0.0226(17) 0.0320(19) -0.0200(17) C31 0.090(3) 0.088(3) 0.096(3) 0.048(2) 0.064(2) 0.038(2) C32 0.0508(18) 0.078(2) 0.084(2) 0.0469(19) 0.0035(16) 0.0007(15) _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 C17 2.007(2) . ? Al1 C13 2.017(2) . ? Al1 C1 2.018(2) . ? Al1 C9 2.021(2) . ? Na1 N4 2.526(2) . ? Na1 N1 2.539(2) . ? Na1 N3 2.628(2) . ? Na1 N2 2.723(2) . ? Na1 C1 3.013(2) . ? N1 C22 1.452(4) . ? N1 C21 1.468(3) . ? N1 C23 1.480(3) . ? N2 C25 1.460(3) . ? N2 C24 1.461(3) . ? N2 C26 1.475(3) . ? N3 C27 1.456(4) . ? N3 C29 1.462(4) . ? N3 C28 1.464(4) . ? N4 C32 1.445(4) . ? N4 C31 1.451(4) . ? N4 C30 1.466(4) . ? C1 C2 1.212(3) . ? C2 C3 1.443(3) . ? C3 C4 1.393(3) . ? C3 C8 1.400(3) . ? C4 C5 1.382(3) . ? C4 H4 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 C7 1.382(3) . ? C6 H6 0.9500 . ? C7 C8 1.387(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.532(3) . ? C9 H9B 0.95(3) . ? C9 H9A 1.07(3) . ? C10 C11 1.508(4) . ? C10 C12 1.520(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.529(3) . ? C13 H13B 1.03(3) . ? C13 H13A 0.90(3) . ? C14 C15 1.514(4) . ? C14 C16 1.529(3) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.542(3) . ? C17 H17B 0.98(3) . ? C17 H7A 0.99(3) . ? C18 C20B 1.496(6) . ? C18 C19 1.515(4) . ? C18 C20A 1.582(6) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.512(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.448(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C20B H20A 0.9800 . ? C20B H20B 0.9800 . ? C20B H20C 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Al1 C13 118.44(10) . . ? C17 Al1 C1 103.65(9) . . ? C13 Al1 C1 104.45(9) . . ? C17 Al1 C9 113.91(11) . . ? C13 Al1 C9 110.47(11) . . ? C1 Al1 C9 104.12(9) . . ? N4 Na1 N1 169.79(8) . . ? N4 Na1 N3 72.28(7) . . ? N1 Na1 N3 103.46(7) . . ? N4 Na1 N2 100.29(7) . . ? N1 Na1 N2 71.73(6) . . ? N3 Na1 N2 106.85(7) . . ? N4 Na1 C1 96.71(7) . . ? N1 Na1 C1 93.47(7) . . ? N3 Na1 C1 109.76(7) . . ? N2 Na1 C1 142.83(6) . . ? C22 N1 C21 108.1(2) . . ? C22 N1 C23 110.9(2) . . ? C21 N1 C23 108.9(2) . . ? C22 N1 Na1 112.16(16) . . ? C21 N1 Na1 109.65(15) . . ? C23 N1 Na1 107.02(14) . . ? C25 N2 C24 110.62(19) . . ? C25 N2 C26 106.97(19) . . ? C24 N2 C26 108.67(19) . . ? C25 N2 Na1 109.69(13) . . ? C24 N2 Na1 103.36(13) . . ? C26 N2 Na1 117.47(14) . . ? C27 N3 C29 111.8(2) . . ? C27 N3 C28 108.0(2) . . ? C29 N3 C28 107.2(2) . . ? C27 N3 Na1 107.53(16) . . ? C29 N3 Na1 104.93(16) . . ? C28 N3 Na1 117.53(16) . . ? C32 N4 C31 109.6(3) . . ? C32 N4 C30 111.5(2) . . ? C31 N4 C30 107.5(3) . . ? C32 N4 Na1 104.14(17) . . ? C31 N4 Na1 116.39(17) . . ? C30 N4 Na1 107.77(16) . . ? C2 C1 Al1 163.85(19) . . ? C2 C1 Na1 94.75(15) . . ? Al1 C1 Na1 100.69(8) . . ? C1 C2 C3 174.4(2) . . ? C4 C3 C8 118.11(19) . . ? C4 C3 C2 121.97(18) . . ? C8 C3 C2 119.91(18) . . ? C5 C4 C3 120.88(19) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.5(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.6(2) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 120.2(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 120.7(2) . . ? C7 C8 H8 119.7 . . ? C3 C8 H8 119.7 . . ? C10 C9 Al1 121.66(17) . . ? C10 C9 H9B 109.7(17) . . ? Al1 C9 H9B 106.1(17) . . ? C10 C9 H9A 108.9(16) . . ? Al1 C9 H9A 106.9(16) . . ? H9B C9 H9A 102(2) . . ? C11 C10 C12 112.1(3) . . ? C11 C10 C9 111.2(2) . . ? C12 C10 C9 109.9(2) . . ? C11 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C9 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 Al1 117.71(16) . . ? C14 C13 H13B 107.7(14) . . ? Al1 C13 H13B 110.7(14) . . ? C14 C13 H13A 107.6(18) . . ? Al1 C13 H13A 106.8(18) . . ? H13B C13 H13A 106(2) . . ? C15 C14 C16 109.8(2) . . ? C15 C14 C13 111.1(2) . . ? C16 C14 C13 113.3(2) . . ? C15 C14 H14 107.4 . . ? C16 C14 H14 107.4 . . ? C13 C14 H14 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Al1 122.94(16) . . ? C18 C17 H17B 111.0(17) . . ? Al1 C17 H17B 105.3(16) . . ? C18 C17 H7A 108.1(18) . . ? Al1 C17 H7A 109.0(17) . . ? H17B C17 H7A 98(2) . . ? C20B C18 C19 116.0(3) . . ? C20B C18 C17 114.6(3) . . ? C19 C18 C17 113.8(2) . . ? C20B C18 C20A 24.7(3) . . ? C19 C18 C20A 102.7(3) . . ? C17 C18 C20A 105.9(3) . . ? C20B C18 H18 103.4 . . ? C19 C18 H18 103.4 . . ? C17 C18 H18 103.4 . . ? C20A C18 H18 128.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 C24 113.5(2) . . ? N1 C23 H23A 108.9 . . ? C24 C23 H23A 108.9 . . ? N1 C23 H23B 108.9 . . ? C24 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? N2 C24 C23 114.01(19) . . ? N2 C24 H24A 108.7 . . ? C23 C24 H24A 108.7 . . ? N2 C24 H24B 108.7 . . ? C23 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? N2 C25 H25A 109.5 . . ? N2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 H28A 109.5 . . ? N3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N3 115.9(3) . . ? C30 C29 H29A 108.3 . . ? N3 C29 H29A 108.3 . . ? C30 C29 H29B 108.3 . . ? N3 C29 H29B 108.3 . . ? H29A C29 H29B 107.4 . . ? C29 C30 N4 117.2(3) . . ? C29 C30 H30A 108.0 . . ? N4 C30 H30A 108.0 . . ? C29 C30 H30B 108.0 . . ? N4 C30 H30B 108.0 . . ? H30A C30 H30B 107.2 . . ? N4 C31 H31A 109.5 . . ? N4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 H32A 109.5 . . ? N4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C18 C20B H20A 109.5 . . ? C18 C20B H20B 109.5 . . ? C18 C20B H20C 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Na1 N1 C22 64.4(5) . . . . ? N3 Na1 N1 C22 0.3(2) . . . . ? N2 Na1 N1 C22 103.86(19) . . . . ? C1 Na1 N1 C22 -110.99(19) . . . . ? N4 Na1 N1 C21 -175.5(4) . . . . ? N3 Na1 N1 C21 120.41(19) . . . . ? N2 Na1 N1 C21 -136.00(19) . . . . ? C1 Na1 N1 C21 9.14(19) . . . . ? N4 Na1 N1 C23 -57.5(5) . . . . ? N3 Na1 N1 C23 -121.59(16) . . . . ? N2 Na1 N1 C23 -18.00(14) . . . . ? C1 Na1 N1 C23 127.14(15) . . . . ? N4 Na1 N2 C25 -80.67(15) . . . . ? N1 Na1 N2 C25 105.91(15) . . . . ? N3 Na1 N2 C25 -155.11(15) . . . . ? C1 Na1 N2 C25 35.16(19) . . . . ? N4 Na1 N2 C24 161.33(14) . . . . ? N1 Na1 N2 C24 -12.08(14) . . . . ? N3 Na1 N2 C24 86.89(14) . . . . ? C1 Na1 N2 C24 -82.83(17) . . . . ? N4 Na1 N2 C26 41.71(18) . . . . ? N1 Na1 N2 C26 -131.71(18) . . . . ? N3 Na1 N2 C26 -32.73(18) . . . . ? C1 Na1 N2 C26 157.54(16) . . . . ? N4 Na1 N3 C27 -105.13(18) . . . . ? N1 Na1 N3 C27 65.23(18) . . . . ? N2 Na1 N3 C27 -9.45(18) . . . . ? C1 Na1 N3 C27 163.98(16) . . . . ? N4 Na1 N3 C29 14.00(19) . . . . ? N1 Na1 N3 C29 -175.6(2) . . . . ? N2 Na1 N3 C29 109.7(2) . . . . ? C1 Na1 N3 C29 -76.9(2) . . . . ? N4 Na1 N3 C28 132.9(2) . . . . ? N1 Na1 N3 C28 -56.7(2) . . . . ? N2 Na1 N3 C28 -131.4(2) . . . . ? C1 Na1 N3 C28 42.0(2) . . . . ? N1 Na1 N4 C32 -174.1(4) . . . . ? N3 Na1 N4 C32 -107.4(2) . . . . ? N2 Na1 N4 C32 148.02(19) . . . . ? C1 Na1 N4 C32 1.2(2) . . . . ? N1 Na1 N4 C31 65.2(5) . . . . ? N3 Na1 N4 C31 131.9(2) . . . . ? N2 Na1 N4 C31 27.3(2) . . . . ? C1 Na1 N4 C31 -119.5(2) . . . . ? N1 Na1 N4 C30 -55.5(5) . . . . ? N3 Na1 N4 C30 11.1(2) . . . . ? N2 Na1 N4 C30 -93.4(2) . . . . ? C1 Na1 N4 C30 119.8(2) . . . . ? C17 Al1 C1 C2 -69.2(7) . . . . ? C13 Al1 C1 C2 55.5(7) . . . . ? C9 Al1 C1 C2 171.4(7) . . . . ? C17 Al1 C1 Na1 128.16(9) . . . . ? C13 Al1 C1 Na1 -107.18(9) . . . . ? C9 Al1 C1 Na1 8.75(11) . . . . ? N4 Na1 C1 C2 -92.72(15) . . . . ? N1 Na1 C1 C2 86.45(15) . . . . ? N3 Na1 C1 C2 -19.19(16) . . . . ? N2 Na1 C1 C2 150.36(14) . . . . ? N4 Na1 C1 Al1 82.51(9) . . . . ? N1 Na1 C1 Al1 -98.32(9) . . . . ? N3 Na1 C1 Al1 156.04(8) . . . . ? N2 Na1 C1 Al1 -34.41(14) . . . . ? Al1 C1 C2 C3 -22(3) . . . . ? Na1 C1 C2 C3 141(2) . . . . ? C1 C2 C3 C4 149(2) . . . . ? C1 C2 C3 C8 -31(2) . . . . ? C8 C3 C4 C5 -1.0(3) . . . . ? C2 C3 C4 C5 179.1(2) . . . . ? C3 C4 C5 C6 1.2(3) . . . . ? C4 C5 C6 C7 -0.1(4) . . . . ? C5 C6 C7 C8 -1.0(4) . . . . ? C6 C7 C8 C3 1.2(4) . . . . ? C4 C3 C8 C7 -0.2(3) . . . . ? C2 C3 C8 C7 179.7(2) . . . . ? C17 Al1 C9 C10 59.0(2) . . . . ? C13 Al1 C9 C10 -77.2(2) . . . . ? C1 Al1 C9 C10 171.1(2) . . . . ? Al1 C9 C10 C11 52.6(3) . . . . ? Al1 C9 C10 C12 -72.1(3) . . . . ? C17 Al1 C13 C14 90.3(2) . . . . ? C1 Al1 C13 C14 -24.3(2) . . . . ? C9 Al1 C13 C14 -135.74(19) . . . . ? Al1 C13 C14 C15 -68.6(2) . . . . ? Al1 C13 C14 C16 167.18(18) . . . . ? C13 Al1 C17 C18 45.3(2) . . . . ? C1 Al1 C17 C18 160.31(18) . . . . ? C9 Al1 C17 C18 -87.2(2) . . . . ? Al1 C17 C18 C20B -64.2(4) . . . . ? Al1 C17 C18 C19 158.96(19) . . . . ? Al1 C17 C18 C20A -89.0(3) . . . . ? C22 N1 C23 C24 -73.6(3) . . . . ? C21 N1 C23 C24 167.5(2) . . . . ? Na1 N1 C23 C24 49.0(2) . . . . ? C25 N2 C24 C23 -75.0(2) . . . . ? C26 N2 C24 C23 167.9(2) . . . . ? Na1 N2 C24 C23 42.4(2) . . . . ? N1 C23 C24 N2 -67.8(3) . . . . ? C27 N3 C29 C30 75.7(3) . . . . ? C28 N3 C29 C30 -166.2(3) . . . . ? Na1 N3 C29 C30 -40.5(3) . . . . ? N3 C29 C30 N4 58.7(4) . . . . ? C32 N4 C30 C29 74.9(4) . . . . ? C31 N4 C30 C29 -165.0(3) . . . . ? Na1 N4 C30 C29 -38.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.491 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.039 #===END data_dvgrem317 _database_code_depnum_ccdc_archive 'CCDC 606352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H70 Al Li N4 O2' _chemical_formula_weight 672.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 11.3307(3) _cell_length_b 20.5770(5) _cell_length_c 18.5945(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.5393(14) _cell_angle_gamma 90.00 _cell_volume 4262.20(19) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9333 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 'Nonius Kappa CCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17709 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.57 _reflns_number_total 9680 _reflns_number_gt 6609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+1.7480P] 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 9958 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Li1 Li 0.7476(2) 0.13374(13) 0.91914(14) 0.0235(6) Uani 1 1 d . . . Al1 Al 0.92358(4) 0.13241(2) 0.76226(3) 0.02087(11) Uani 1 1 d . . . C1 C 0.97138(15) 0.11815(8) 0.87190(9) 0.0231(3) Uani 1 1 d . . . C2 C 0.95553(15) 0.23008(8) 0.90919(10) 0.0308(4) Uani 1 1 d . . . H2A H 0.9272 0.2588 0.9445 0.046 Uiso 1 1 calc R . . H2B H 0.9153 0.2415 0.8596 0.046 Uiso 1 1 calc R . . H2C H 1.0425 0.2351 0.9131 0.046 Uiso 1 1 calc R . . C3 C 0.98436(14) 0.14816(9) 1.00082(9) 0.0281(4) Uani 1 1 d . . . H3A H 0.9662 0.1837 1.0329 0.034 Uiso 1 1 calc R . . H3B H 1.0726 0.1462 1.0045 0.034 Uiso 1 1 calc R . . C4 C 0.94070(15) 0.08479(9) 1.02695(9) 0.0290(4) Uani 1 1 d . . . H4A H 0.9646 0.0487 0.9974 0.035 Uiso 1 1 calc R . . H4B H 0.9791 0.0775 1.0786 0.035 Uiso 1 1 calc R . . C5 C 0.76470(19) 0.01826(9) 1.02322(11) 0.0414(5) Uani 1 1 d . . . H5A H 0.8009 -0.0020 1.0697 0.062 Uiso 1 1 calc R . . H5B H 0.7863 -0.0067 0.9826 0.062 Uiso 1 1 calc R . . H5C H 0.6772 0.0189 1.0188 0.062 Uiso 1 1 calc R . . C6 C 0.77394(16) 0.12269(9) 1.08020(9) 0.0330(4) Uani 1 1 d . . . H6A H 0.6863 0.1225 1.0751 0.049 Uiso 1 1 calc R . . H6B H 0.8022 0.1675 1.0777 0.049 Uiso 1 1 calc R . . H6C H 0.8100 0.1036 1.1274 0.049 Uiso 1 1 calc R . . C7 C 1.04646(14) 0.19437(8) 0.73572(9) 0.0271(4) Uani 1 1 d . . . H7A H 1.0384 0.2348 0.7632 0.032 Uiso 1 1 calc R . . H7B H 1.1257 0.1758 0.7572 0.032 Uiso 1 1 calc R . . C8 C 1.05644(14) 0.21587(9) 0.65802(10) 0.0306(4) Uani 1 1 d . . . H8 H 0.9782 0.2361 0.6353 0.037 Uiso 1 1 calc R . . C9 C 1.15490(17) 0.26720(10) 0.65941(11) 0.0424(5) Uani 1 1 d . . . H9A H 1.2316 0.2498 0.6851 0.064 Uiso 1 1 calc R . . H9B H 1.1342 0.3061 0.6848 0.064 Uiso 1 1 calc R . . H9C H 1.1619 0.2786 0.6092 0.064 Uiso 1 1 calc R . . C10 C 1.07944(18) 0.15902(10) 0.61028(11) 0.0429(5) Uani 1 1 d . . . H10A H 1.1587 0.1405 0.6293 0.064 Uiso 1 1 calc R . . H10B H 1.0768 0.1742 0.5600 0.064 Uiso 1 1 calc R . . H10C H 1.0177 0.1258 0.6107 0.064 Uiso 1 1 calc R . . C11 C 0.91498(14) 0.04270(8) 0.71759(9) 0.0243(4) Uani 1 1 d . . . H11A H 0.8361 0.0239 0.7217 0.029 Uiso 1 1 calc R . . H11B H 0.9160 0.0478 0.6648 0.029 Uiso 1 1 calc R . . C12 C 1.01206(15) -0.00758(8) 0.74830(9) 0.0264(4) Uani 1 1 d . . . H12 H 1.0147 -0.0106 0.8023 0.032 Uiso 1 1 calc R . . C13 C 1.13606(15) 0.01301(9) 0.73655(12) 0.0410(5) Uani 1 1 d . . . H13A H 1.1950 -0.0201 0.7568 0.062 Uiso 1 1 calc R . . H13B H 1.1576 0.0546 0.7612 0.062 Uiso 1 1 calc R . . H13C H 1.1355 0.0178 0.6841 0.062 Uiso 1 1 calc R . . C14 C 0.98538(16) -0.07549(9) 0.71622(12) 0.0395(5) Uani 1 1 d . . . H14A H 0.9803 -0.0739 0.6631 0.059 Uiso 1 1 calc R . . H14B H 0.9089 -0.0909 0.7274 0.059 Uiso 1 1 calc R . . H14C H 1.0498 -0.1052 0.7376 0.059 Uiso 1 1 calc R . . C15 C 0.75791(14) 0.17589(8) 0.73778(8) 0.0207(3) Uani 1 1 d . . . C16 C 0.75108(14) 0.24068(8) 0.71280(9) 0.0239(4) Uani 1 1 d . . . H16 H 0.8234 0.2617 0.7071 0.029 Uiso 1 1 calc R . . C17 C 0.64450(15) 0.27558(8) 0.69600(9) 0.0264(4) Uani 1 1 d . . . H17 H 0.6457 0.3194 0.6801 0.032 Uiso 1 1 calc R . . C18 C 0.53649(15) 0.24655(8) 0.70247(9) 0.0263(4) Uani 1 1 d . . . H18 H 0.4633 0.2700 0.6909 0.032 Uiso 1 1 calc R . . C19 C 0.53740(14) 0.18272(8) 0.72609(9) 0.0237(3) Uani 1 1 d . . . H19 H 0.4641 0.1621 0.7306 0.028 Uiso 1 1 calc R . . C20 C 0.64573(13) 0.14837(7) 0.74337(8) 0.0190(3) Uani 1 1 d . . . C21 C 0.64078(13) 0.08174(7) 0.77669(8) 0.0192(3) Uani 1 1 d . . . C22 C 0.56116(15) -0.02975(8) 0.77182(9) 0.0252(4) Uani 1 1 d . . . H22 H 0.5124 -0.0572 0.7330 0.030 Uiso 1 1 calc R . . C23 C 0.48626(16) -0.02105(9) 0.83140(10) 0.0316(4) Uani 1 1 d . . . H23A H 0.5331 0.0027 0.8727 0.047 Uiso 1 1 calc R . . H23B H 0.4641 -0.0638 0.8481 0.047 Uiso 1 1 calc R . . H23C H 0.4134 0.0035 0.8118 0.047 Uiso 1 1 calc R . . C24 C 0.67724(16) -0.06700(8) 0.79886(10) 0.0317(4) Uani 1 1 d . . . H24A H 0.7209 -0.0727 0.7584 0.048 Uiso 1 1 calc R . . H24B H 0.6582 -0.1097 0.8171 0.048 Uiso 1 1 calc R . . H24C H 0.7271 -0.0426 0.8384 0.048 Uiso 1 1 calc R . . C25 C 0.53679(15) 0.03882(8) 0.65650(9) 0.0266(4) Uani 1 1 d . . . H25 H 0.5633 0.0820 0.6406 0.032 Uiso 1 1 calc R . . C26 C 0.59161(17) -0.01338(9) 0.61424(10) 0.0353(4) Uani 1 1 d . . . H26A H 0.6792 -0.0126 0.6288 0.053 Uiso 1 1 calc R . . H26B H 0.5695 -0.0048 0.5617 0.053 Uiso 1 1 calc R . . H26C H 0.5612 -0.0562 0.6252 0.053 Uiso 1 1 calc R . . C27 C 0.39997(16) 0.03727(9) 0.63811(11) 0.0376(5) Uani 1 1 d . . . H27A H 0.3711 -0.0046 0.6532 0.056 Uiso 1 1 calc R . . H27B H 0.3736 0.0429 0.5853 0.056 Uiso 1 1 calc R . . H27C H 0.3674 0.0725 0.6641 0.056 Uiso 1 1 calc R . . C28 C 0.68063(15) 0.31872(9) 0.89075(10) 0.0320(4) Uani 1 1 d . . . H28 H 0.6569 0.2992 0.8441 0.038 Uiso 1 1 calc R . . C29 C 0.75665(17) 0.37206(10) 0.89919(13) 0.0443(5) Uani 1 1 d . . . H29 H 0.7843 0.3894 0.8579 0.053 Uiso 1 1 calc R . . C30 C 0.79235(17) 0.40011(10) 0.96675(14) 0.0497(6) Uani 1 1 d . . . H30 H 0.8447 0.4365 0.9720 0.060 Uiso 1 1 calc R . . C31 C 0.75239(18) 0.37550(10) 1.02668(12) 0.0467(5) Uani 1 1 d . . . H31 H 0.7775 0.3948 1.0734 0.056 Uiso 1 1 calc R . . C32 C 0.67578(16) 0.32274(9) 1.01919(10) 0.0338(4) Uani 1 1 d . . . H32 H 0.6479 0.3060 1.0607 0.041 Uiso 1 1 calc R . . C33 C 0.63952(13) 0.29417(8) 0.95104(8) 0.0212(3) Uani 1 1 d . . . C34 C 0.56272(14) 0.23428(8) 0.94349(8) 0.0208(3) Uani 1 1 d . . . C35 C 0.32564(18) 0.31616(9) 1.00527(12) 0.0427(5) Uani 1 1 d . . . H35A H 0.2621 0.2839 1.0057 0.064 Uiso 1 1 calc R . . H35B H 0.2909 0.3599 1.0026 0.064 Uiso 1 1 calc R . . H35C H 0.3858 0.3121 1.0501 0.064 Uiso 1 1 calc R . . C36 C 0.38459(14) 0.30471(8) 0.93938(9) 0.0255(4) Uani 1 1 d . . . H36 H 0.4481 0.3386 0.9404 0.031 Uiso 1 1 calc R . . C37 C 0.29679(16) 0.31196(9) 0.86701(11) 0.0382(5) Uani 1 1 d . . . H37A H 0.3399 0.3065 0.8263 0.057 Uiso 1 1 calc R . . H37B H 0.2602 0.3552 0.8645 0.057 Uiso 1 1 calc R . . H37C H 0.2340 0.2788 0.8639 0.057 Uiso 1 1 calc R . . C38 C 0.40288(17) 0.14259(9) 1.01236(10) 0.0375(5) Uani 1 1 d . . . H38A H 0.4794 0.1206 1.0116 0.056 Uiso 1 1 calc R . . H38B H 0.3407 0.1101 1.0155 0.056 Uiso 1 1 calc R . . H38C H 0.4116 0.1715 1.0549 0.056 Uiso 1 1 calc R . . C39 C 0.36712(14) 0.18225(8) 0.94263(9) 0.0245(4) Uani 1 1 d . . . H39 H 0.2840 0.1986 0.9426 0.029 Uiso 1 1 calc R . . C40 C 0.36054(15) 0.14154(9) 0.87370(10) 0.0323(4) Uani 1 1 d . . . H40A H 0.3352 0.1690 0.8306 0.048 Uiso 1 1 calc R . . H40B H 0.3024 0.1063 0.8739 0.048 Uiso 1 1 calc R . . H40C H 0.4398 0.1231 0.8722 0.048 Uiso 1 1 calc R . . N1 N 0.80892(12) 0.08457(6) 1.02099(7) 0.0253(3) Uani 1 1 d . . . N2 N 0.92804(11) 0.16266(6) 0.92464(7) 0.0223(3) Uani 1 1 d . . . N3 N 0.58144(11) 0.03323(6) 0.73649(7) 0.0210(3) Uani 1 1 d . . . N4 N 0.44463(11) 0.24054(6) 0.94327(7) 0.0207(3) Uani 1 1 d . . . O1 O 0.68775(9) 0.07360(5) 0.84216(6) 0.0227(2) Uani 1 1 d . . . O2 O 0.61121(10) 0.18058(5) 0.93939(6) 0.0277(3) Uani 1 1 d . . . H1A H 1.0608(17) 0.1155(8) 0.8857(9) 0.033(5) Uiso 1 1 d . . . H1B H 0.9424(15) 0.0737(9) 0.8826(9) 0.027(5) 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 Li1 0.0213(13) 0.0234(14) 0.0255(14) -0.0022(12) 0.0032(11) 0.0026(11) Al1 0.0180(2) 0.0238(3) 0.0211(2) 0.0021(2) 0.00434(18) -0.0001(2) C1 0.0216(8) 0.0257(9) 0.0226(8) -0.0005(7) 0.0056(7) 0.0038(7) C2 0.0303(9) 0.0260(9) 0.0369(10) -0.0042(8) 0.0086(8) -0.0043(8) C3 0.0211(8) 0.0411(11) 0.0212(8) -0.0044(7) 0.0014(6) 0.0026(8) C4 0.0301(9) 0.0367(10) 0.0198(8) 0.0032(7) 0.0036(7) 0.0128(8) C5 0.0547(13) 0.0293(10) 0.0400(11) 0.0054(9) 0.0077(9) -0.0039(9) C6 0.0326(9) 0.0444(11) 0.0226(9) -0.0022(8) 0.0071(7) 0.0056(8) C7 0.0212(8) 0.0321(10) 0.0276(9) 0.0051(7) 0.0039(7) -0.0017(7) C8 0.0184(8) 0.0400(11) 0.0333(10) 0.0115(8) 0.0047(7) 0.0005(8) C9 0.0346(10) 0.0508(12) 0.0428(12) 0.0152(10) 0.0090(9) -0.0104(10) C10 0.0410(11) 0.0563(13) 0.0346(11) 0.0059(10) 0.0149(9) -0.0071(10) C11 0.0197(8) 0.0297(9) 0.0239(8) 0.0003(7) 0.0047(6) 0.0004(7) C12 0.0272(9) 0.0277(9) 0.0243(8) -0.0004(7) 0.0044(7) 0.0046(7) C13 0.0237(9) 0.0349(11) 0.0617(14) -0.0019(10) 0.0006(9) 0.0060(8) C14 0.0293(10) 0.0312(10) 0.0586(13) -0.0043(9) 0.0098(9) 0.0041(8) C15 0.0227(8) 0.0222(8) 0.0174(8) -0.0012(6) 0.0045(6) -0.0007(7) C16 0.0246(8) 0.0255(9) 0.0235(8) 0.0021(7) 0.0095(7) -0.0022(7) C17 0.0350(9) 0.0211(9) 0.0247(9) 0.0049(7) 0.0097(7) 0.0020(7) C18 0.0263(8) 0.0270(9) 0.0258(9) 0.0027(7) 0.0053(7) 0.0077(7) C19 0.0203(8) 0.0265(9) 0.0244(8) 0.0005(7) 0.0047(6) 0.0000(7) C20 0.0209(8) 0.0203(8) 0.0159(7) -0.0010(6) 0.0034(6) -0.0007(6) C21 0.0151(7) 0.0220(8) 0.0210(8) -0.0005(6) 0.0051(6) 0.0017(6) C22 0.0279(9) 0.0171(8) 0.0297(9) 0.0005(7) 0.0032(7) -0.0040(7) C23 0.0291(9) 0.0271(9) 0.0407(11) 0.0054(8) 0.0124(8) -0.0037(8) C24 0.0388(10) 0.0219(9) 0.0357(10) 0.0031(8) 0.0107(8) 0.0050(8) C25 0.0308(9) 0.0259(9) 0.0205(8) -0.0003(7) -0.0023(7) -0.0010(7) C26 0.0420(11) 0.0366(11) 0.0253(9) -0.0066(8) 0.0013(8) -0.0008(9) C27 0.0322(10) 0.0350(11) 0.0396(11) -0.0015(9) -0.0093(8) -0.0017(8) C28 0.0323(9) 0.0332(10) 0.0329(10) 0.0035(8) 0.0126(8) 0.0004(8) C29 0.0371(11) 0.0357(11) 0.0660(15) 0.0167(11) 0.0251(10) 0.0018(9) C30 0.0278(10) 0.0300(11) 0.0896(18) -0.0011(11) 0.0065(11) -0.0075(9) C31 0.0373(11) 0.0442(12) 0.0536(13) -0.0110(11) -0.0052(10) -0.0081(10) C32 0.0316(9) 0.0383(11) 0.0290(9) -0.0023(8) -0.0008(7) -0.0047(8) C33 0.0160(7) 0.0228(8) 0.0249(8) 0.0015(7) 0.0036(6) 0.0024(6) C34 0.0215(8) 0.0229(8) 0.0178(8) 0.0006(6) 0.0033(6) 0.0019(7) C35 0.0419(11) 0.0356(11) 0.0559(13) -0.0099(10) 0.0226(10) 0.0063(9) C36 0.0213(8) 0.0197(8) 0.0361(10) 0.0004(7) 0.0065(7) 0.0021(7) C37 0.0294(10) 0.0314(10) 0.0494(12) 0.0100(9) -0.0041(8) 0.0037(8) C38 0.0412(11) 0.0323(10) 0.0394(11) 0.0089(8) 0.0081(9) -0.0092(9) C39 0.0208(8) 0.0207(8) 0.0328(9) 0.0008(7) 0.0069(7) -0.0029(7) C40 0.0265(9) 0.0304(10) 0.0394(10) -0.0059(8) 0.0047(8) -0.0039(8) N1 0.0316(8) 0.0231(7) 0.0220(7) -0.0003(6) 0.0065(6) 0.0025(6) N2 0.0212(7) 0.0240(7) 0.0213(7) -0.0023(6) 0.0030(5) 0.0004(6) N3 0.0218(7) 0.0199(7) 0.0206(7) 0.0009(6) 0.0024(5) -0.0021(6) N4 0.0184(6) 0.0181(7) 0.0259(7) 0.0010(6) 0.0052(5) 0.0006(5) O1 0.0250(6) 0.0223(6) 0.0198(6) 0.0002(5) 0.0020(4) -0.0009(5) O2 0.0234(6) 0.0233(6) 0.0364(7) -0.0015(5) 0.0057(5) 0.0042(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O2 1.916(3) . ? Li1 O1 1.920(3) . ? Li1 N2 2.114(3) . ? Li1 N1 2.148(3) . ? Al1 C7 2.0147(16) . ? Al1 C11 2.0192(17) . ? Al1 C1 2.0327(17) . ? Al1 C15 2.0540(16) . ? C1 N2 1.489(2) . ? C1 H1A 1.001(18) . ? C1 H1B 1.004(17) . ? C2 N2 1.462(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N2 1.474(2) . ? C3 C4 1.506(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N1 1.477(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.457(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 N1 1.464(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.535(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C10 1.520(3) . ? C8 C9 1.533(2) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.542(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.521(2) . ? C12 C14 1.528(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.409(2) . ? C15 C20 1.413(2) . ? C16 C17 1.391(2) . ? C16 H16 0.9500 . ? C17 C18 1.387(2) . ? C17 H17 0.9500 . ? C18 C19 1.384(2) . ? C18 H18 0.9500 . ? C19 C20 1.402(2) . ? C19 H19 0.9500 . ? C20 C21 1.510(2) . ? C21 O1 1.2475(18) . ? C21 N3 1.3503(19) . ? C22 N3 1.490(2) . ? C22 C23 1.524(2) . ? C22 C24 1.526(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N3 1.485(2) . ? C25 C27 1.526(2) . ? C25 C26 1.528(2) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.386(2) . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C29 C30 1.375(3) . ? C29 H29 0.9500 . ? C30 C31 1.374(3) . ? C30 H30 0.9500 . ? C31 C32 1.381(3) . ? C31 H31 0.9500 . ? C32 C33 1.389(2) . ? C32 H32 0.9500 . ? C33 C34 1.500(2) . ? C34 O2 1.2426(18) . ? C34 N4 1.3436(19) . ? C35 C36 1.517(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 N4 1.481(2) . ? C36 C37 1.527(2) . ? C36 H36 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.523(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 N4 1.4853(19) . ? C39 C40 1.522(2) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Li1 O1 106.44(13) . . ? O2 Li1 N2 131.04(15) . . ? O1 Li1 N2 115.11(13) . . ? O2 Li1 N1 101.89(13) . . ? O1 Li1 N1 111.53(14) . . ? N2 Li1 N1 86.33(11) . . ? C7 Al1 C11 117.47(7) . . ? C7 Al1 C1 105.53(7) . . ? C11 Al1 C1 105.34(7) . . ? C7 Al1 C15 108.34(7) . . ? C11 Al1 C15 109.49(7) . . ? C1 Al1 C15 110.50(6) . . ? N2 C1 Al1 120.81(11) . . ? N2 C1 H1A 107.7(10) . . ? Al1 C1 H1A 109.7(10) . . ? N2 C1 H1B 105.7(9) . . ? Al1 C1 H1B 107.0(10) . . ? H1A C1 H1B 104.6(14) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 112.03(13) . . ? N2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N1 C4 C3 111.44(13) . . ? N1 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? N1 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 Al1 125.89(12) . . ? C8 C7 H7A 105.8 . . ? Al1 C7 H7A 105.8 . . ? C8 C7 H7B 105.8 . . ? Al1 C7 H7B 105.8 . . ? H7A C7 H7B 106.2 . . ? C10 C8 C9 109.77(15) . . ? C10 C8 C7 112.21(15) . . ? C9 C8 C7 111.18(15) . . ? C10 C8 H8 107.8 . . ? C9 C8 H8 107.8 . . ? C7 C8 H8 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 Al1 118.92(11) . . ? C12 C11 H11A 107.6 . . ? Al1 C11 H11A 107.6 . . ? C12 C11 H11B 107.6 . . ? Al1 C11 H11B 107.6 . . ? H11A C11 H11B 107.0 . . ? C13 C12 C14 108.70(14) . . ? C13 C12 C11 112.04(14) . . ? C14 C12 C11 113.10(14) . . ? C13 C12 H12 107.6 . . ? C14 C12 H12 107.6 . . ? C11 C12 H12 107.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 114.05(14) . . ? C16 C15 Al1 118.56(11) . . ? C20 C15 Al1 127.39(11) . . ? C17 C16 C15 123.76(15) . . ? C17 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? C18 C17 C16 120.13(15) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 118.73(15) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 120.44(15) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 122.88(14) . . ? C19 C20 C21 117.09(13) . . ? C15 C20 C21 119.71(13) . . ? O1 C21 N3 121.43(14) . . ? O1 C21 C20 118.75(13) . . ? N3 C21 C20 119.75(13) . . ? N3 C22 C23 111.70(13) . . ? N3 C22 C24 112.90(13) . . ? C23 C22 C24 112.36(14) . . ? N3 C22 H22 106.4 . . ? C23 C22 H22 106.4 . . ? C24 C22 H22 106.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 C27 111.64(14) . . ? N3 C25 C26 111.37(13) . . ? C27 C25 C26 111.22(14) . . ? N3 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 119.41(18) . . ? C33 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 120.58(19) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 120.07(18) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.1(2) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 120.02(18) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 119.78(16) . . ? C28 C33 C34 119.92(15) . . ? C32 C33 C34 120.18(15) . . ? O2 C34 N4 122.44(14) . . ? O2 C34 C33 118.73(13) . . ? N4 C34 C33 118.81(14) . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C36 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 C35 111.42(14) . . ? N4 C36 C37 110.46(14) . . ? C35 C36 C37 112.59(15) . . ? N4 C36 H36 107.4 . . ? C35 C36 H36 107.4 . . ? C37 C36 H36 107.4 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C39 C40 112.90(13) . . ? N4 C39 C38 111.17(13) . . ? C40 C39 C38 112.74(14) . . ? N4 C39 H39 106.5 . . ? C40 C39 H39 106.5 . . ? C38 C39 H39 106.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C5 N1 C6 109.79(14) . . ? C5 N1 C4 110.42(14) . . ? C6 N1 C4 110.55(13) . . ? C5 N1 Li1 114.14(13) . . ? C6 N1 Li1 108.80(12) . . ? C4 N1 Li1 102.95(12) . . ? C2 N2 C3 108.10(13) . . ? C2 N2 C1 110.27(13) . . ? C3 N2 C1 111.80(12) . . ? C2 N2 Li1 119.78(13) . . ? C3 N2 Li1 103.56(12) . . ? C1 N2 Li1 103.15(12) . . ? C21 N3 C25 122.75(13) . . ? C21 N3 C22 120.02(13) . . ? C25 N3 C22 117.21(12) . . ? C34 N4 C36 122.27(13) . . ? C34 N4 C39 120.64(13) . . ? C36 N4 C39 116.99(12) . . ? C21 O1 Li1 132.12(13) . . ? C34 O2 Li1 147.23(14) . . ? 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 C7 Al1 C1 N2 87.29(13) . . . . ? C11 Al1 C1 N2 -147.77(12) . . . . ? C15 Al1 C1 N2 -29.61(15) . . . . ? N2 C3 C4 N1 -57.57(18) . . . . ? C11 Al1 C7 C8 57.36(16) . . . . ? C1 Al1 C7 C8 174.35(14) . . . . ? C15 Al1 C7 C8 -67.29(16) . . . . ? Al1 C7 C8 C10 -60.83(19) . . . . ? Al1 C7 C8 C9 175.80(13) . . . . ? C7 Al1 C11 C12 76.14(14) . . . . ? C1 Al1 C11 C12 -40.95(14) . . . . ? C15 Al1 C11 C12 -159.79(12) . . . . ? Al1 C11 C12 C13 -64.18(17) . . . . ? Al1 C11 C12 C14 172.54(12) . . . . ? C7 Al1 C15 C16 -4.64(14) . . . . ? C11 Al1 C15 C16 -133.90(12) . . . . ? C1 Al1 C15 C16 110.51(13) . . . . ? C7 Al1 C15 C20 175.80(13) . . . . ? C11 Al1 C15 C20 46.54(15) . . . . ? C1 Al1 C15 C20 -69.05(15) . . . . ? C20 C15 C16 C17 1.0(2) . . . . ? Al1 C15 C16 C17 -178.62(13) . . . . ? C15 C16 C17 C18 -0.9(2) . . . . ? C16 C17 C18 C19 0.2(2) . . . . ? C17 C18 C19 C20 0.3(2) . . . . ? C18 C19 C20 C15 -0.2(2) . . . . ? C18 C19 C20 C21 173.32(14) . . . . ? C16 C15 C20 C19 -0.4(2) . . . . ? Al1 C15 C20 C19 179.13(12) . . . . ? C16 C15 C20 C21 -173.76(13) . . . . ? Al1 C15 C20 C21 5.8(2) . . . . ? C19 C20 C21 O1 -110.37(16) . . . . ? C15 C20 C21 O1 63.32(19) . . . . ? C19 C20 C21 N3 66.63(19) . . . . ? C15 C20 C21 N3 -119.67(16) . . . . ? C33 C28 C29 C30 0.7(3) . . . . ? C28 C29 C30 C31 -0.2(3) . . . . ? C29 C30 C31 C32 -0.3(3) . . . . ? C30 C31 C32 C33 0.4(3) . . . . ? C29 C28 C33 C32 -0.7(3) . . . . ? C29 C28 C33 C34 -176.64(15) . . . . ? C31 C32 C33 C28 0.1(3) . . . . ? C31 C32 C33 C34 176.08(16) . . . . ? C28 C33 C34 O2 76.1(2) . . . . ? C32 C33 C34 O2 -99.90(19) . . . . ? C28 C33 C34 N4 -105.60(18) . . . . ? C32 C33 C34 N4 78.44(19) . . . . ? C3 C4 N1 C5 161.54(14) . . . . ? C3 C4 N1 C6 -76.76(17) . . . . ? C3 C4 N1 Li1 39.31(16) . . . . ? O2 Li1 N1 C5 95.61(16) . . . . ? O1 Li1 N1 C5 -17.60(19) . . . . ? N2 Li1 N1 C5 -133.18(13) . . . . ? O2 Li1 N1 C6 -27.39(16) . . . . ? O1 Li1 N1 C6 -140.59(14) . . . . ? N2 Li1 N1 C6 103.83(13) . . . . ? O2 Li1 N1 C4 -144.69(13) . . . . ? O1 Li1 N1 C4 102.10(15) . . . . ? N2 Li1 N1 C4 -13.48(13) . . . . ? C4 C3 N2 C2 168.29(13) . . . . ? C4 C3 N2 C1 -70.16(17) . . . . ? C4 C3 N2 Li1 40.24(16) . . . . ? Al1 C1 N2 C2 -53.05(16) . . . . ? Al1 C1 N2 C3 -173.34(11) . . . . ? Al1 C1 N2 Li1 76.00(14) . . . . ? O2 Li1 N2 C2 -31.8(2) . . . . ? O1 Li1 N2 C2 113.50(16) . . . . ? N1 Li1 N2 C2 -134.41(13) . . . . ? O2 Li1 N2 C3 88.6(2) . . . . ? O1 Li1 N2 C3 -126.08(15) . . . . ? N1 Li1 N2 C3 -13.99(13) . . . . ? O2 Li1 N2 C1 -154.75(18) . . . . ? O1 Li1 N2 C1 -9.43(18) . . . . ? N1 Li1 N2 C1 102.66(12) . . . . ? O1 C21 N3 C25 -172.73(14) . . . . ? C20 C21 N3 C25 10.3(2) . . . . ? O1 C21 N3 C22 5.7(2) . . . . ? C20 C21 N3 C22 -171.27(13) . . . . ? C27 C25 N3 C21 -114.38(16) . . . . ? C26 C25 N3 C21 120.62(16) . . . . ? C27 C25 N3 C22 67.19(18) . . . . ? C26 C25 N3 C22 -57.80(18) . . . . ? C23 C22 N3 C21 61.25(18) . . . . ? C24 C22 N3 C21 -66.53(18) . . . . ? C23 C22 N3 C25 -120.28(15) . . . . ? C24 C22 N3 C25 111.94(16) . . . . ? O2 C34 N4 C36 -172.65(14) . . . . ? C33 C34 N4 C36 9.1(2) . . . . ? O2 C34 N4 C39 3.8(2) . . . . ? C33 C34 N4 C39 -174.49(13) . . . . ? C35 C36 N4 C34 -120.78(17) . . . . ? C37 C36 N4 C34 113.29(16) . . . . ? C35 C36 N4 C39 62.67(18) . . . . ? C37 C36 N4 C39 -63.26(18) . . . . ? C40 C39 N4 C34 -63.53(19) . . . . ? C38 C39 N4 C34 64.31(19) . . . . ? C40 C39 N4 C36 113.08(16) . . . . ? C38 C39 N4 C36 -119.08(15) . . . . ? N3 C21 O1 Li1 -165.17(15) . . . . ? C20 C21 O1 Li1 11.8(2) . . . . ? O2 Li1 O1 C21 66.7(2) . . . . ? N2 Li1 O1 C21 -86.69(19) . . . . ? N1 Li1 O1 C21 177.06(13) . . . . ? N4 C34 O2 Li1 162.3(2) . . . . ? C33 C34 O2 Li1 -19.4(3) . . . . ? O1 Li1 O2 C34 -122.8(2) . . . . ? N2 Li1 O2 C34 24.7(4) . . . . ? N1 Li1 O2 C34 120.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.292 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.043 #===END