# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Samuel Dagorne' _publ_contact_author_email DAGORNE@CHIMIE.U-STRASBG.FR _publ_section_title ; Synthesis and structural characterization of well-defined lithium aluminium alkoxide complexes supported by NON-type diamido ether tridentate ligands and their use for the controlled ROP of lactide ; loop_ _publ_author_name 'Samuel Dagorne' 'Pierre Haquette' 'Frederic Hild' data_fred_al_li_08_2008 _database_code_depnum_ccdc_archive 'CCDC 735904' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 Al Li N2 O2, C H2 CL2' _chemical_formula_sum 'C27 H38 Al Cl2 Li N2 O2' _chemical_formula_weight 527.41 _chemical_absolute_configuration . 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' O O 0.0106 0.0060 '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' Al Al 0.0645 0.0514 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5310(3) _cell_length_b 12.9330(5) _cell_length_c 13.3830(4) _cell_angle_alpha 102.9210(18) _cell_angle_beta 109.0090(17) _cell_angle_gamma 107.7770(16) _cell_volume 1386.31(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4458 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.292 _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 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11345 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8002 _reflns_number_gt 6720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0837P)^2^+0.5970P] 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 8002 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1588 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 Cl1 Cl 0.50838(9) 0.18432(6) 0.32405(6) 0.06062(19) Uani 1 1 d . . . Cl2 Cl 0.69686(8) 0.17265(6) 0.53950(6) 0.06078(18) Uani 1 1 d . . . Al Al 0.36553(5) 0.30094(4) 0.81605(3) 0.01579(11) Uani 1 1 d . . . O1 O 0.69454(12) 0.43709(9) 0.90881(8) 0.0171(2) Uani 1 1 d . . . O2 O 0.77515(16) 0.43022(11) 1.16741(9) 0.0290(3) Uani 1 1 d . . . N1 N 0.42803(14) 0.33164(10) 0.70370(10) 0.0171(2) Uani 1 1 d . . . N2 N 0.49743(14) 0.24511(10) 0.91107(10) 0.0163(2) Uani 1 1 d . . . C1 C 0.68157(17) 0.49586(12) 0.83166(11) 0.0172(3) Uani 1 1 d . . . C2 C 0.80138(19) 0.60488(13) 0.86320(13) 0.0221(3) Uani 1 1 d . . . H2 H 0.8908 0.6393 0.9357 0.027 Uiso 1 1 calc . . . C3 C 0.7897(2) 0.66373(14) 0.78760(14) 0.0259(3) Uani 1 1 d . . . H3 H 0.8701 0.7393 0.8082 0.031 Uiso 1 1 calc . . . C4 C 0.6590(2) 0.61057(14) 0.68188(14) 0.0258(3) Uani 1 1 d . . . H4 H 0.6516 0.6497 0.6294 0.031 Uiso 1 1 calc . . . C5 C 0.5382(2) 0.50075(14) 0.65115(13) 0.0233(3) Uani 1 1 d . . . H5 H 0.4501 0.4665 0.5781 0.028 Uiso 1 1 calc . . . C6 C 0.54399(17) 0.43939(12) 0.72607(12) 0.0175(3) Uani 1 1 d . . . C7 C 0.33137(18) 0.25692(13) 0.58390(12) 0.0194(3) Uani 1 1 d . . . H7 H 0.3969 0.2812 0.5416 0.023 Uiso 1 1 calc . . . C8 C 0.1631(2) 0.25709(15) 0.52405(13) 0.0267(3) Uani 1 1 d . . . H8A H 0.1039 0.2534 0.5726 0.032 Uiso 1 1 calc . . . H8B H 0.1742 0.3278 0.5047 0.032 Uiso 1 1 calc . . . C9 C 0.0748(3) 0.14775(18) 0.41692(16) 0.0405(5) Uani 1 1 d . . . H9A H 0.0820 0.1680 0.3511 0.049 Uiso 1 1 calc . . . H9B H -0.0415 0.1099 0.4008 0.049 Uiso 1 1 calc . . . C10 C 0.1589(2) 0.06621(16) 0.43922(15) 0.0343(4) Uani 1 1 d . . . H10A H 0.2102 0.0536 0.3867 0.041 Uiso 1 1 calc . . . H10B H 0.0795 -0.0100 0.4291 0.041 Uiso 1 1 calc . . . C11 C 0.2884(2) 0.12737(14) 0.56238(14) 0.0252(3) Uani 1 1 d . . . H11A H 0.2443 0.1029 0.6148 0.030 Uiso 1 1 calc . . . H11B H 0.3852 0.1100 0.5717 0.030 Uiso 1 1 calc . . . C12 C 0.72971(16) 0.33925(12) 0.88011(11) 0.0167(3) Uani 1 1 d . . . C13 C 0.86011(18) 0.34481(14) 0.85442(13) 0.0224(3) Uani 1 1 d . . . H13 H 0.9249 0.4141 0.8497 0.027 Uiso 1 1 calc . . . C14 C 0.8955(2) 0.24682(16) 0.83547(14) 0.0265(3) Uani 1 1 d . . . H14 H 0.9830 0.2482 0.8158 0.032 Uiso 1 1 calc . . . C15 C 0.8014(2) 0.14778(15) 0.84568(14) 0.0264(3) Uani 1 1 d . . . H15 H 0.8270 0.0818 0.8349 0.032 Uiso 1 1 calc . . . C16 C 0.66916(19) 0.14327(14) 0.87168(13) 0.0225(3) Uani 1 1 d . . . H16 H 0.6065 0.0745 0.8785 0.027 Uiso 1 1 calc . . . C17 C 0.62845(16) 0.23907(12) 0.88779(11) 0.0169(3) Uani 1 1 d . . . C18 C 0.42070(18) 0.15493(12) 0.94970(12) 0.0187(3) Uani 1 1 d . . . H18 H 0.5087 0.1412 1.0028 0.022 Uiso 1 1 calc . . . C19 C 0.2919(2) 0.03506(14) 0.85747(14) 0.0262(3) Uani 1 1 d . . . H19A H 0.2581 0.0411 0.7815 0.031 Uiso 1 1 calc . . . H19B H 0.3375 -0.0243 0.8572 0.031 Uiso 1 1 calc . . . C20 C 0.1477(3) 0.0022(2) 0.8877(2) 0.0519(7) Uani 1 1 d . . . H20A H 0.1115 -0.0796 0.8837 0.062 Uiso 1 1 calc . . . H20B H 0.0556 0.0110 0.8346 0.062 Uiso 1 1 calc . . . C21 C 0.2062(2) 0.08453(16) 1.00806(16) 0.0329(4) Uani 1 1 d . . . H21A H 0.1151 0.0973 1.0207 0.039 Uiso 1 1 calc . . . H21B H 0.2577 0.0538 1.0645 0.039 Uiso 1 1 calc . . . C22 C 0.32941(19) 0.19596(14) 1.01472(13) 0.0221(3) Uani 1 1 d . . . H22A H 0.4051 0.2457 1.0944 0.026 Uiso 1 1 calc . . . H22B H 0.2742 0.2404 0.9789 0.026 Uiso 1 1 calc . . . C23 C 0.8581(2) 0.52750(16) 1.27336(15) 0.0331(4) Uani 1 1 d . . . H23A H 0.7837 0.5322 1.3097 0.040 Uiso 1 1 calc . . . H23B H 0.9017 0.6015 1.2616 0.040 Uiso 1 1 calc . . . C24 C 0.9957(3) 0.50263(19) 1.34541(16) 0.0388(4) Uani 1 1 d . . . H24A H 1.0900 0.5256 1.3264 0.047 Uiso 1 1 calc . . . H24B H 1.0318 0.5432 1.4272 0.047 Uiso 1 1 calc . . . C25 C 0.9150(3) 0.37245(19) 1.31222(16) 0.0387(4) Uani 1 1 d . . . H25A H 0.8511 0.3514 1.3555 0.046 Uiso 1 1 calc . . . H25B H 0.9964 0.3384 1.3246 0.046 Uiso 1 1 calc . . . C26 C 0.8054(3) 0.33225(17) 1.18741(15) 0.0362(4) Uani 1 1 d . . . H26A H 0.8590 0.3060 1.1410 0.043 Uiso 1 1 calc . . . H26B H 0.7017 0.2667 1.1672 0.043 Uiso 1 1 calc . . . C27 C 0.5826(4) 0.0994(2) 0.3935(2) 0.0564(6) Uani 1 1 d . . . H27A H 0.4896 0.0287 0.3798 0.068 Uiso 1 1 calc . . . H27B H 0.6512 0.0743 0.3606 0.068 Uiso 1 1 calc . . . Li Li 0.6182(3) 0.4299(2) 1.0327(2) 0.0231(5) Uani 1 1 d . . . H1 H 0.183(3) 0.218(2) 0.7632(19) 0.033(6) Uiso 1 1 d . . . H6 H 0.395(3) 0.4201(18) 0.9029(18) 0.028(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 Cl1 0.0699(4) 0.0600(4) 0.0690(4) 0.0397(3) 0.0290(3) 0.0366(3) Cl2 0.0548(4) 0.0622(4) 0.0481(3) 0.0114(3) 0.0097(3) 0.0213(3) Al 0.0149(2) 0.0182(2) 0.01437(19) 0.00612(15) 0.00597(15) 0.00698(16) O1 0.0189(5) 0.0183(5) 0.0148(4) 0.0073(4) 0.0070(4) 0.0077(4) O2 0.0379(7) 0.0290(6) 0.0177(5) 0.0069(4) 0.0049(5) 0.0193(5) N1 0.0164(5) 0.0176(5) 0.0127(5) 0.0051(4) 0.0038(4) 0.0038(4) N2 0.0156(5) 0.0180(5) 0.0188(5) 0.0094(4) 0.0091(4) 0.0075(4) C1 0.0190(6) 0.0180(6) 0.0153(6) 0.0078(5) 0.0078(5) 0.0065(5) C2 0.0221(7) 0.0192(7) 0.0195(6) 0.0055(5) 0.0076(5) 0.0038(5) C3 0.0294(8) 0.0185(7) 0.0261(7) 0.0089(6) 0.0128(6) 0.0036(6) C4 0.0350(8) 0.0228(7) 0.0228(7) 0.0132(6) 0.0141(6) 0.0104(6) C5 0.0266(7) 0.0231(7) 0.0174(6) 0.0096(5) 0.0064(6) 0.0083(6) C6 0.0188(6) 0.0185(6) 0.0158(6) 0.0073(5) 0.0075(5) 0.0072(5) C7 0.0205(6) 0.0195(6) 0.0132(6) 0.0039(5) 0.0047(5) 0.0060(5) C8 0.0249(7) 0.0286(8) 0.0168(7) 0.0048(6) 0.0004(6) 0.0102(6) C9 0.0400(10) 0.0318(9) 0.0215(8) -0.0004(7) -0.0060(7) 0.0069(8) C10 0.0360(9) 0.0264(8) 0.0235(8) -0.0023(6) 0.0071(7) 0.0054(7) C11 0.0300(8) 0.0188(7) 0.0226(7) 0.0048(5) 0.0097(6) 0.0081(6) C12 0.0157(6) 0.0198(6) 0.0148(6) 0.0069(5) 0.0055(5) 0.0080(5) C13 0.0178(6) 0.0290(8) 0.0223(7) 0.0116(6) 0.0096(6) 0.0092(6) C14 0.0227(7) 0.0384(9) 0.0275(7) 0.0142(7) 0.0146(6) 0.0180(7) C15 0.0286(8) 0.0311(8) 0.0289(8) 0.0122(6) 0.0147(6) 0.0202(7) C16 0.0236(7) 0.0228(7) 0.0254(7) 0.0104(6) 0.0119(6) 0.0122(6) C17 0.0159(6) 0.0206(6) 0.0150(6) 0.0067(5) 0.0064(5) 0.0084(5) C18 0.0210(6) 0.0170(6) 0.0199(6) 0.0089(5) 0.0103(5) 0.0069(5) C19 0.0301(8) 0.0183(7) 0.0272(8) 0.0058(6) 0.0147(6) 0.0052(6) C20 0.0352(10) 0.0411(11) 0.0493(12) -0.0116(9) 0.0263(10) -0.0113(9) C21 0.0351(9) 0.0279(8) 0.0340(9) 0.0094(7) 0.0231(8) 0.0032(7) C22 0.0251(7) 0.0231(7) 0.0213(7) 0.0094(5) 0.0139(6) 0.0087(6) C23 0.0414(10) 0.0299(9) 0.0215(7) 0.0047(6) 0.0075(7) 0.0162(8) C24 0.0372(10) 0.0414(11) 0.0267(8) 0.0116(8) 0.0047(7) 0.0123(8) C25 0.0427(11) 0.0416(10) 0.0283(9) 0.0169(8) 0.0063(8) 0.0190(9) C26 0.0423(10) 0.0309(9) 0.0262(8) 0.0079(7) 0.0003(7) 0.0207(8) C27 0.0750(18) 0.0553(14) 0.0443(12) 0.0166(11) 0.0176(12) 0.0425(14) Li 0.0259(13) 0.0254(13) 0.0185(11) 0.0082(10) 0.0083(10) 0.0121(11) _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 Cl1 C27 1.753(3) . ? Cl2 C27 1.748(3) . ? Al N1 1.8652(13) . ? Al N2 1.9085(12) . ? Al H1 1.55(2) . ? Al H6 1.59(2) . ? O1 C1 1.4086(17) . ? O1 C12 1.4095(17) . ? O1 Li 2.025(3) . ? O2 C23 1.443(2) . ? O2 C26 1.444(2) . ? O2 Li 1.930(3) . ? N1 C6 1.3823(18) . ? N1 C7 1.4678(17) . ? N2 C17 1.4017(17) . ? N2 C18 1.4689(18) . ? N2 Li 2.246(3) . ? C1 C2 1.381(2) . ? C1 C6 1.4130(19) . ? C2 C3 1.392(2) . ? C2 H2 0.9500 . ? C3 C4 1.386(2) . ? C3 H3 0.9500 . ? C4 C5 1.394(2) . ? C4 H4 0.9500 . ? C5 C6 1.409(2) . ? C5 H5 0.9500 . ? C7 C11 1.532(2) . ? C7 C8 1.542(2) . ? C7 H7 1.0000 . ? C8 C9 1.531(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.531(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.537(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.3794(19) . ? C12 C17 1.408(2) . ? C13 C14 1.399(2) . ? C13 H13 0.9500 . ? C14 C15 1.386(3) . ? C14 H14 0.9500 . ? C15 C16 1.401(2) . ? C15 H15 0.9500 . ? C16 C17 1.400(2) . ? C16 H16 0.9500 . ? C18 C22 1.538(2) . ? C18 C19 1.558(2) . ? C18 H18 1.0000 . ? C19 C20 1.521(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.525(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.518(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.525(3) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.509(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.515(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? Li H6 2.21(2) . ? 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 Al N2 114.17(5) . . ? N1 Al H1 110.4(9) . . ? N2 Al H1 111.6(9) . . ? N1 Al H6 108.8(8) . . ? N2 Al H6 102.4(8) . . ? H1 Al H6 109.2(11) . . ? C1 O1 C12 115.72(10) . . ? C1 O1 Li 134.76(11) . . ? C12 O1 Li 107.24(11) . . ? C23 O2 C26 108.68(13) . . ? C23 O2 Li 122.70(13) . . ? C26 O2 Li 127.54(13) . . ? C6 N1 C7 116.19(11) . . ? C6 N1 Al 120.26(9) . . ? C7 N1 Al 121.81(9) . . ? C17 N2 C18 116.32(11) . . ? C17 N2 Al 114.69(9) . . ? C18 N2 Al 119.33(9) . . ? C17 N2 Li 98.96(11) . . ? C18 N2 Li 117.08(11) . . ? Al N2 Li 84.21(8) . . ? C2 C1 O1 118.82(13) . . ? C2 C1 C6 123.75(13) . . ? O1 C1 C6 117.42(12) . . ? C1 C2 C3 119.28(14) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 119.04(14) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 121.20(14) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 121.46(14) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? N1 C6 C5 125.33(13) . . ? N1 C6 C1 119.43(13) . . ? C5 C6 C1 115.23(13) . . ? N1 C7 C11 113.67(12) . . ? N1 C7 C8 117.26(12) . . ? C11 C7 C8 102.07(13) . . ? N1 C7 H7 107.8 . . ? C11 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C9 C8 C7 104.28(14) . . ? C9 C8 H8A 110.9 . . ? C7 C8 H8A 110.9 . . ? C9 C8 H8B 110.9 . . ? C7 C8 H8B 110.9 . . ? H8A C8 H8B 108.9 . . ? C8 C9 C10 106.76(14) . . ? C8 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? C8 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C9 C10 C11 105.70(14) . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10B 110.6 . . ? C11 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? C7 C11 C10 104.04(13) . . ? C7 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? C7 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 109.0 . . ? C13 C12 C17 123.31(13) . . ? C13 C12 O1 122.07(13) . . ? C17 C12 O1 114.47(12) . . ? C12 C13 C14 118.99(14) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 119.29(14) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 121.10(14) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 120.66(14) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 N2 126.48(13) . . ? C16 C17 C12 116.59(13) . . ? N2 C17 C12 116.92(12) . . ? N2 C18 C22 110.62(12) . . ? N2 C18 C19 117.42(12) . . ? C22 C18 C19 104.40(12) . . ? N2 C18 H18 108.0 . . ? C22 C18 H18 108.0 . . ? C19 C18 H18 108.0 . . ? C20 C19 C18 106.38(13) . . ? C20 C19 H19A 110.5 . . ? C18 C19 H19A 110.5 . . ? C20 C19 H19B 110.5 . . ? C18 C19 H19B 110.5 . . ? H19A C19 H19B 108.6 . . ? C19 C20 C21 106.43(15) . . ? C19 C20 H20A 110.4 . . ? C21 C20 H20A 110.4 . . ? C19 C20 H20B 110.4 . . ? C21 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? C22 C21 C20 103.31(14) . . ? C22 C21 H21A 111.1 . . ? C20 C21 H21A 111.1 . . ? C22 C21 H21B 111.1 . . ? C20 C21 H21B 111.1 . . ? H21A C21 H21B 109.1 . . ? C21 C22 C18 104.51(13) . . ? C21 C22 H22A 110.8 . . ? C18 C22 H22A 110.8 . . ? C21 C22 H22B 110.8 . . ? C18 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? O2 C23 C24 104.46(14) . . ? O2 C23 H23A 110.9 . . ? C24 C23 H23A 110.9 . . ? O2 C23 H23B 110.9 . . ? C24 C23 H23B 110.9 . . ? H23A C23 H23B 108.9 . . ? C25 C24 C23 101.69(16) . . ? C25 C24 H24A 111.4 . . ? C23 C24 H24A 111.4 . . ? C25 C24 H24B 111.4 . . ? C23 C24 H24B 111.4 . . ? H24A C24 H24B 109.3 . . ? C24 C25 C26 102.93(16) . . ? C24 C25 H25A 111.2 . . ? C26 C25 H25A 111.2 . . ? C24 C25 H25B 111.2 . . ? C26 C25 H25B 111.2 . . ? H25A C25 H25B 109.1 . . ? O2 C26 C25 107.08(15) . . ? O2 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O2 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? Cl2 C27 Cl1 113.25(14) . . ? Cl2 C27 H27A 108.9 . . ? Cl1 C27 H27A 108.9 . . ? Cl2 C27 H27B 108.9 . . ? Cl1 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? O2 Li O1 114.15(14) . . ? O2 Li N2 105.24(13) . . ? O1 Li N2 75.82(9) . . ? O2 Li H6 164.3(6) . . ? O1 Li H6 81.5(6) . . ? N2 Li H6 75.7(6) . . ? 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 Al N1 C6 -87.56(12) . . . . ? N2 Al N1 C7 108.05(11) . . . . ? N1 Al N2 C17 2.67(12) . . . . ? N1 Al N2 C18 -142.21(10) . . . . ? N1 Al N2 Li 99.89(9) . . . . ? C12 O1 C1 C2 -109.87(15) . . . . ? Li O1 C1 C2 89.93(19) . . . . ? C12 O1 C1 C6 70.90(16) . . . . ? Li O1 C1 C6 -89.30(19) . . . . ? O1 C1 C2 C3 -179.96(13) . . . . ? C6 C1 C2 C3 -0.8(2) . . . . ? C1 C2 C3 C4 -0.9(2) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C7 N1 C6 C5 25.6(2) . . . . ? Al N1 C6 C5 -139.58(13) . . . . ? C7 N1 C6 C1 -154.38(13) . . . . ? Al N1 C6 C1 40.39(17) . . . . ? C4 C5 C6 N1 178.45(15) . . . . ? C4 C5 C6 C1 -1.5(2) . . . . ? C2 C1 C6 N1 -178.03(13) . . . . ? O1 C1 C6 N1 1.16(19) . . . . ? C2 C1 C6 C5 2.0(2) . . . . ? O1 C1 C6 C5 -178.86(12) . . . . ? C6 N1 C7 C11 144.31(13) . . . . ? Al N1 C7 C11 -50.70(16) . . . . ? C6 N1 C7 C8 -96.83(16) . . . . ? Al N1 C7 C8 68.16(16) . . . . ? N1 C7 C8 C9 -163.28(14) . . . . ? C11 C7 C8 C9 -38.39(17) . . . . ? C7 C8 C9 C10 21.8(2) . . . . ? C8 C9 C10 C11 3.4(2) . . . . ? N1 C7 C11 C10 167.81(13) . . . . ? C8 C7 C11 C10 40.57(16) . . . . ? C9 C10 C11 C7 -27.44(19) . . . . ? C1 O1 C12 C13 52.77(17) . . . . ? Li O1 C12 C13 -141.81(14) . . . . ? C1 O1 C12 C17 -131.49(12) . . . . ? Li O1 C12 C17 33.93(15) . . . . ? C17 C12 C13 C14 -0.4(2) . . . . ? O1 C12 C13 C14 174.97(13) . . . . ? C12 C13 C14 C15 -1.6(2) . . . . ? C13 C14 C15 C16 1.7(3) . . . . ? C14 C15 C16 C17 0.2(2) . . . . ? C15 C16 C17 N2 178.19(14) . . . . ? C15 C16 C17 C12 -2.0(2) . . . . ? C18 N2 C17 C16 16.1(2) . . . . ? Al N2 C17 C16 -129.84(13) . . . . ? Li N2 C17 C16 142.45(15) . . . . ? C18 N2 C17 C12 -163.66(12) . . . . ? Al N2 C17 C12 50.36(15) . . . . ? Li N2 C17 C12 -37.36(15) . . . . ? C13 C12 C17 C16 2.2(2) . . . . ? O1 C12 C17 C16 -173.53(12) . . . . ? C13 C12 C17 N2 -178.03(13) . . . . ? O1 C12 C17 N2 6.30(18) . . . . ? C17 N2 C18 C22 157.93(12) . . . . ? Al N2 C18 C22 -57.73(14) . . . . ? Li N2 C18 C22 41.32(16) . . . . ? C17 N2 C18 C19 -82.44(16) . . . . ? Al N2 C18 C19 61.90(15) . . . . ? Li N2 C18 C19 160.95(13) . . . . ? N2 C18 C19 C20 -133.81(18) . . . . ? C22 C18 C19 C20 -10.9(2) . . . . ? C18 C19 C20 C21 -13.1(2) . . . . ? C19 C20 C21 C22 32.4(2) . . . . ? C20 C21 C22 C18 -39.3(2) . . . . ? N2 C18 C22 C21 158.25(13) . . . . ? C19 C18 C22 C21 31.06(16) . . . . ? C26 O2 C23 C24 24.2(2) . . . . ? Li O2 C23 C24 -166.93(16) . . . . ? O2 C23 C24 C25 -37.6(2) . . . . ? C23 C24 C25 C26 36.2(2) . . . . ? C23 O2 C26 C25 -0.9(2) . . . . ? Li O2 C26 C25 -169.14(16) . . . . ? C24 C25 C26 O2 -22.8(2) . . . . ? C23 O2 Li O1 110.53(17) . . . . ? C26 O2 Li O1 -82.8(2) . . . . ? C23 O2 Li N2 -168.45(14) . . . . ? C26 O2 Li N2 -1.7(2) . . . . ? C1 O1 Li O2 -139.37(15) . . . . ? C12 O1 Li O2 59.26(17) . . . . ? C1 O1 Li N2 120.04(14) . . . . ? C12 O1 Li N2 -41.33(11) . . . . ? C17 N2 Li O2 -69.54(14) . . . . ? C18 N2 Li O2 56.24(16) . . . . ? Al N2 Li O2 176.31(12) . . . . ? C17 N2 Li O1 42.09(11) . . . . ? C18 N2 Li O1 167.87(10) . . . . ? Al N2 Li O1 -72.06(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.927 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.124 data_2b _database_code_depnum_ccdc_archive 'CCDC 735905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 Al Li N2 O2, C H2 Cl2' _chemical_formula_sum 'C29 H42 Al Cl2 Li N2 O2' _chemical_formula_weight 555.47 _chemical_absolute_configuration . 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4620(2) _cell_length_b 12.1940(3) _cell_length_c 14.0420(3) _cell_angle_alpha 107.8950(9) _cell_angle_beta 106.3370(9) _cell_angle_gamma 91.0310(9) _cell_volume 1469.82(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11473 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.279 _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 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 19301 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 30.02 _reflns_number_total 8573 _reflns_number_gt 6143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0800P)^2^+0.6000P] 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 8573 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _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 Cl1 Cl 0.05222(9) 0.47089(6) 0.23162(5) 0.0677(2) Uani 1 1 d . . . Cl2 Cl 0.07916(12) 0.59694(7) 0.44902(7) 0.0967(3) Uani 1 1 d . . . Al Al 0.55474(5) 0.18825(4) 0.18332(4) 0.02044(12) Uani 1 1 d . . . O2 O 0.68866(16) 0.17049(10) -0.07927(10) 0.0344(3) Uani 1 1 d . . . O1 O 0.28046(13) 0.09136(9) 0.05803(9) 0.0223(2) Uani 1 1 d . . . N1 N 0.44501(15) 0.30274(11) 0.14746(11) 0.0220(3) Uani 1 1 d . . . N2 N 0.46123(15) 0.09612(11) 0.24148(11) 0.0211(3) Uani 1 1 d . . . C26 C 0.7778(2) 0.30453(17) -0.14657(17) 0.0386(4) Uani 1 1 d . . . H26A H 0.6962 0.3495 -0.1687 0.046 Uiso 1 1 calc . . . H26B H 0.8542 0.3112 -0.1810 0.046 Uiso 1 1 calc . . . C25 C 0.7213(3) 0.17923(17) -0.17141(16) 0.0433(5) Uani 1 1 d . . . H25A H 0.6308 0.1558 -0.2326 0.052 Uiso 1 1 calc . . . H25B H 0.7974 0.1282 -0.1878 0.052 Uiso 1 1 calc . . . C27 C 0.8433(2) 0.34485(16) -0.02834(16) 0.0374(4) Uani 1 1 d . . . H27A H 0.8469 0.4300 0.0022 0.045 Uiso 1 1 calc . . . H27B H 0.9442 0.3219 -0.0069 0.045 Uiso 1 1 calc . . . C22 C 0.8151(2) 0.05917(19) 0.50165(17) 0.0406(5) Uani 1 1 d . . . H22A H 0.8601 0.0312 0.5613 0.049 Uiso 1 1 calc . . . H22B H 0.8939 0.1060 0.4927 0.049 Uiso 1 1 calc . . . C9 C 0.01518(19) 0.15863(15) 0.21152(16) 0.0316(4) Uani 1 1 d . . . H9 H -0.0840 0.1760 0.2043 0.038 Uiso 1 1 calc . . . C17 C 0.4877(3) 0.56156(16) 0.39344(17) 0.0455(6) Uani 1 1 d . . . H17A H 0.4050 0.6006 0.3623 0.055 Uiso 1 1 calc . . . H17B H 0.4843 0.5664 0.4644 0.055 Uiso 1 1 calc . . . C18 C 0.4690(2) 0.43424(15) 0.32539(15) 0.0350(4) Uani 1 1 d . . . H18A H 0.5495 0.3942 0.3578 0.042 Uiso 1 1 calc . . . H18B H 0.3733 0.3957 0.3209 0.042 Uiso 1 1 calc . . . C16 C 0.6338(3) 0.62279(18) 0.40196(16) 0.0486(6) Uani 1 1 d . . . H16A H 0.7166 0.5871 0.4376 0.058 Uiso 1 1 calc . . . H16B H 0.6425 0.7053 0.4450 0.058 Uiso 1 1 calc . . . C13 C 0.47330(19) 0.42555(13) 0.21563(13) 0.0236(3) Uani 1 1 d . . . H13 H 0.3905 0.4665 0.1854 0.028 Uiso 1 1 calc . . . C19 C 0.54810(18) 0.06682(13) 0.33410(13) 0.0226(3) Uani 1 1 d . . . H19 H 0.4789 0.0183 0.3513 0.027 Uiso 1 1 calc . . . C10 C 0.1034(2) 0.15083(15) 0.30491(15) 0.0308(4) Uani 1 1 d . . . H10 H 0.0630 0.1606 0.3613 0.037 Uiso 1 1 calc . . . C1 C 0.34360(18) 0.27888(13) 0.04914(13) 0.0227(3) Uani 1 1 d . . . C7 C 0.21877(18) 0.11918(13) 0.14197(13) 0.0211(3) Uani 1 1 d . . . C20 C 0.6158(2) 0.17208(14) 0.43267(13) 0.0282(4) Uani 1 1 d . . . H20A H 0.6866 0.2214 0.4188 0.034 Uiso 1 1 calc . . . H20B H 0.5363 0.2188 0.4497 0.034 Uiso 1 1 calc . . . C6 C 0.26043(18) 0.16895(13) -0.00034(13) 0.0231(3) Uani 1 1 d . . . C8 C 0.07304(19) 0.14068(14) 0.12736(14) 0.0268(3) Uani 1 1 d . . . H8 H 0.0131 0.1432 0.0614 0.032 Uiso 1 1 calc . . . C24 C 0.6695(2) -0.00654(15) 0.30847(14) 0.0293(4) Uani 1 1 d . . . H24A H 0.7406 0.0390 0.2913 0.035 Uiso 1 1 calc . . . H24B H 0.6250 -0.0758 0.2463 0.035 Uiso 1 1 calc . . . C12 C 0.31450(17) 0.11511(12) 0.23733(13) 0.0211(3) Uani 1 1 d . . . C11 C 0.2504(2) 0.12904(14) 0.31892(14) 0.0267(3) Uani 1 1 d . . . H11 H 0.3082 0.1235 0.3843 0.032 Uiso 1 1 calc . . . C5 C 0.1606(2) 0.13448(15) -0.09952(14) 0.0285(4) Uani 1 1 d . . . H5 H 0.1098 0.0582 -0.1297 0.034 Uiso 1 1 calc . . . C2 C 0.3127(2) 0.35660(15) -0.00896(14) 0.0293(4) Uani 1 1 d . . . H2 H 0.3635 0.4329 0.0204 0.035 Uiso 1 1 calc . . . C3 C 0.2096(2) 0.32374(16) -0.10805(15) 0.0318(4) Uani 1 1 d . . . H3 H 0.1899 0.3786 -0.1444 0.038 Uiso 1 1 calc . . . C4 C 0.1350(2) 0.21287(16) -0.15520(14) 0.0322(4) Uani 1 1 d . . . H4 H 0.0676 0.1906 -0.2241 0.039 Uiso 1 1 calc . . . C14 C 0.6182(2) 0.48830(15) 0.22102(15) 0.0323(4) Uani 1 1 d . . . H14A H 0.6154 0.4868 0.1496 0.039 Uiso 1 1 calc . . . H14B H 0.7019 0.4467 0.2467 0.039 Uiso 1 1 calc . . . C21 C 0.6959(2) 0.13446(17) 0.52602(15) 0.0352(4) Uani 1 1 d . . . H21A H 0.7415 0.2040 0.5877 0.042 Uiso 1 1 calc . . . H21B H 0.6235 0.0907 0.5437 0.042 Uiso 1 1 calc . . . C15 C 0.6446(3) 0.61482(16) 0.29379(16) 0.0404(5) Uani 1 1 d . . . H15A H 0.7441 0.6495 0.3011 0.049 Uiso 1 1 calc . . . H15B H 0.5702 0.6597 0.2622 0.049 Uiso 1 1 calc . . . C23 C 0.7518(2) -0.04487(17) 0.40183(17) 0.0381(4) Uani 1 1 d . . . H23A H 0.6826 -0.0972 0.4141 0.046 Uiso 1 1 calc . . . H23B H 0.8335 -0.0887 0.3850 0.046 Uiso 1 1 calc . . . C28 C 0.7341(2) 0.28112(16) 0.00335(15) 0.0365(4) Uani 1 1 d . . . H28A H 0.7821 0.2703 0.0717 0.044 Uiso 1 1 calc . . . H28B H 0.6478 0.3247 0.0088 0.044 Uiso 1 1 calc . . . C29 C 0.0533(3) 0.4608(2) 0.3533(2) 0.0539(6) Uani 1 1 d . . . H29A H 0.1338 0.4152 0.3763 0.065 Uiso 1 1 calc . . . H29B H -0.0419 0.4189 0.3457 0.065 Uiso 1 1 calc . . . Li Li 0.4089(4) -0.0361(2) 0.0698(3) 0.0305(6) Uani 1 1 d . . . H1AL H 0.711(2) 0.2431(17) 0.2591(16) 0.030(5) Uiso 1 1 d . . . H2AL H 0.572(2) 0.0957(17) 0.0811(16) 0.031(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 Cl1 0.0791(5) 0.0672(4) 0.0514(4) 0.0283(3) 0.0023(3) -0.0080(3) Cl2 0.1259(8) 0.0596(4) 0.0842(6) -0.0111(4) 0.0412(6) -0.0389(5) Al 0.0201(2) 0.0189(2) 0.0220(2) 0.00443(17) 0.00817(19) 0.00264(17) O2 0.0494(8) 0.0238(6) 0.0304(7) 0.0040(5) 0.0184(6) -0.0024(5) O1 0.0267(6) 0.0196(5) 0.0219(6) 0.0061(4) 0.0097(5) 0.0042(4) N1 0.0240(7) 0.0172(6) 0.0218(7) 0.0038(5) 0.0052(5) 0.0010(5) N2 0.0203(6) 0.0215(6) 0.0220(7) 0.0071(5) 0.0070(5) 0.0042(5) C26 0.0449(11) 0.0323(9) 0.0402(11) 0.0169(8) 0.0098(9) -0.0001(8) C25 0.0648(14) 0.0332(10) 0.0313(10) 0.0040(8) 0.0217(10) -0.0107(9) C27 0.0411(11) 0.0281(9) 0.0385(11) 0.0081(8) 0.0085(9) -0.0015(8) C22 0.0348(10) 0.0471(11) 0.0364(11) 0.0201(9) -0.0017(8) 0.0030(9) C9 0.0231(8) 0.0305(9) 0.0444(11) 0.0110(8) 0.0164(8) 0.0049(7) C17 0.0863(17) 0.0253(9) 0.0321(10) 0.0060(7) 0.0324(11) 0.0125(10) C18 0.0584(13) 0.0230(8) 0.0305(9) 0.0077(7) 0.0250(9) 0.0091(8) C16 0.0787(17) 0.0297(10) 0.0249(10) -0.0018(7) 0.0084(10) 0.0003(10) C13 0.0295(8) 0.0177(7) 0.0229(8) 0.0046(6) 0.0089(7) 0.0035(6) C19 0.0235(8) 0.0208(7) 0.0227(8) 0.0065(6) 0.0064(6) 0.0025(6) C10 0.0318(9) 0.0289(8) 0.0371(10) 0.0082(7) 0.0212(8) 0.0048(7) C1 0.0234(8) 0.0219(7) 0.0233(8) 0.0060(6) 0.0090(6) 0.0029(6) C7 0.0229(7) 0.0172(6) 0.0236(8) 0.0050(5) 0.0092(6) 0.0009(5) C20 0.0322(9) 0.0251(8) 0.0227(8) 0.0050(6) 0.0045(7) 0.0012(7) C6 0.0256(8) 0.0224(7) 0.0225(8) 0.0076(6) 0.0085(6) 0.0043(6) C8 0.0218(8) 0.0248(8) 0.0341(9) 0.0101(7) 0.0083(7) 0.0029(6) C24 0.0279(9) 0.0295(8) 0.0297(9) 0.0096(7) 0.0073(7) 0.0082(7) C12 0.0222(7) 0.0163(6) 0.0247(8) 0.0041(5) 0.0095(6) 0.0022(5) C11 0.0289(8) 0.0262(8) 0.0256(8) 0.0060(6) 0.0121(7) 0.0030(6) C5 0.0303(9) 0.0262(8) 0.0243(8) 0.0041(6) 0.0058(7) 0.0012(7) C2 0.0335(9) 0.0268(8) 0.0290(9) 0.0118(7) 0.0087(7) 0.0018(7) C3 0.0373(10) 0.0343(9) 0.0276(9) 0.0159(7) 0.0091(8) 0.0065(7) C4 0.0349(10) 0.0374(9) 0.0216(8) 0.0093(7) 0.0046(7) 0.0045(8) C14 0.0392(10) 0.0245(8) 0.0284(9) 0.0001(7) 0.0127(8) -0.0051(7) C21 0.0398(10) 0.0375(10) 0.0235(9) 0.0101(7) 0.0025(8) -0.0018(8) C15 0.0541(13) 0.0244(8) 0.0323(10) -0.0028(7) 0.0111(9) -0.0118(8) C23 0.0375(10) 0.0375(10) 0.0403(11) 0.0184(8) 0.0063(9) 0.0133(8) C28 0.0460(11) 0.0282(9) 0.0311(10) 0.0015(7) 0.0146(9) 0.0013(8) C29 0.0564(15) 0.0472(12) 0.0507(14) 0.0152(10) 0.0061(12) -0.0016(11) Li 0.0347(16) 0.0243(13) 0.0353(17) 0.0102(12) 0.0140(13) 0.0050(12) _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 Cl1 C29 1.747(3) . ? Cl2 C29 1.747(3) . ? Al N1 1.8630(14) . ? Al N2 1.9096(14) . ? Al Li 2.807(3) . ? Al H1AL 1.55(2) . ? Al H2AL 1.58(2) . ? O2 C28 1.445(2) . ? O2 C25 1.445(2) . ? O2 Li 1.925(3) 2_655 ? O1 C7 1.4118(18) . ? O1 C6 1.4136(19) . ? O1 Li 2.009(3) . ? N1 C1 1.382(2) . ? N1 C13 1.4802(19) . ? N2 C12 1.400(2) . ? N2 C19 1.480(2) . ? N2 Li 2.360(3) . ? C26 C25 1.510(3) . ? C26 C27 1.513(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 C28 1.521(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C22 C21 1.514(3) . ? C22 C23 1.530(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C9 C10 1.375(3) . ? C9 C8 1.398(2) . ? C9 H9 0.9500 . ? C17 C16 1.515(4) . ? C17 C18 1.529(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C13 1.524(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C16 C15 1.525(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C13 C14 1.530(2) . ? C13 H13 1.0000 . ? C19 C24 1.523(2) . ? C19 C20 1.534(2) . ? C19 H19 1.0000 . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? C1 C6 1.408(2) . ? C1 C2 1.414(2) . ? C7 C8 1.378(2) . ? C7 C12 1.406(2) . ? C20 C21 1.525(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C6 C5 1.376(2) . ? C8 H8 0.9500 . ? C24 C23 1.536(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C12 C11 1.408(2) . ? C11 H11 0.9500 . ? C5 C4 1.395(3) . ? C5 H5 0.9500 . ? C2 C3 1.388(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C14 C15 1.536(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? Li O2 1.925(3) 2_655 ? Li H2AL 2.15(2) . ? 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 Al N2 114.42(6) . . ? N1 Al Li 112.50(8) . . ? N2 Al Li 56.25(7) . . ? N1 Al H1AL 110.1(8) . . ? N2 Al H1AL 110.2(7) . . ? Li Al H1AL 136.9(7) . . ? N1 Al H2AL 109.9(8) . . ? N2 Al H2AL 102.8(7) . . ? Li Al H2AL 49.4(7) . . ? H1AL Al H2AL 109.1(10) . . ? C28 O2 C25 108.98(13) . . ? C28 O2 Li 125.21(14) . 2_655 ? C25 O2 Li 125.74(14) . 2_655 ? C7 O1 C6 115.28(12) . . ? C7 O1 Li 108.43(13) . . ? C6 O1 Li 135.14(13) . . ? C1 N1 C13 116.22(13) . . ? C1 N1 Al 120.64(10) . . ? C13 N1 Al 122.72(11) . . ? C12 N2 C19 115.43(12) . . ? C12 N2 Al 114.84(10) . . ? C19 N2 Al 120.19(10) . . ? C12 N2 Li 96.80(12) . . ? C19 N2 Li 121.56(12) . . ? Al N2 Li 81.46(9) . . ? C25 C26 C27 102.57(16) . . ? C25 C26 H26A 111.3 . . ? C27 C26 H26A 111.3 . . ? C25 C26 H26B 111.3 . . ? C27 C26 H26B 111.3 . . ? H26A C26 H26B 109.2 . . ? O2 C25 C26 106.71(15) . . ? O2 C25 H25A 110.4 . . ? C26 C25 H25A 110.4 . . ? O2 C25 H25B 110.4 . . ? C26 C25 H25B 110.4 . . ? H25A C25 H25B 108.6 . . ? C26 C27 C28 101.74(16) . . ? C26 C27 H27A 111.4 . . ? C28 C27 H27A 111.4 . . ? C26 C27 H27B 111.4 . . ? C28 C27 H27B 111.4 . . ? H27A C27 H27B 109.3 . . ? C21 C22 C23 111.35(17) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C10 C9 C8 119.24(16) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? C16 C17 C18 110.82(18) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C13 C18 C17 110.03(14) . . ? C13 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? C13 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? C17 C16 C15 110.99(18) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N1 C13 C18 110.17(13) . . ? N1 C13 C14 113.70(13) . . ? C18 C13 C14 110.55(15) . . ? N1 C13 H13 107.4 . . ? C18 C13 H13 107.4 . . ? C14 C13 H13 107.4 . . ? N2 C19 C24 110.71(13) . . ? N2 C19 C20 114.40(13) . . ? C24 C19 C20 109.67(14) . . ? N2 C19 H19 107.2 . . ? C24 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? C9 C10 C11 121.67(16) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? N1 C1 C6 119.35(14) . . ? N1 C1 C2 125.74(14) . . ? C6 C1 C2 114.91(15) . . ? C8 C7 C12 123.93(15) . . ? C8 C7 O1 121.38(15) . . ? C12 C7 O1 114.55(13) . . ? C21 C20 C19 111.18(14) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? C5 C6 C1 124.22(15) . . ? C5 C6 O1 119.04(14) . . ? C1 C6 O1 116.73(14) . . ? C7 C8 C9 118.65(17) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C19 C24 C23 110.68(15) . . ? C19 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N2 C12 C7 117.56(13) . . ? N2 C12 C11 126.77(15) . . ? C7 C12 C11 115.66(15) . . ? C10 C11 C12 120.74(17) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C6 C5 C4 119.19(16) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C3 C2 C1 121.36(16) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C4 C3 C2 121.53(16) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 118.72(16) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C13 C14 C15 112.07(15) . . ? C13 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? C13 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C22 C21 C20 111.01(16) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C16 C15 C14 111.30(16) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C22 C23 C24 111.49(16) . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? O2 C28 C27 105.01(15) . . ? O2 C28 H28A 110.7 . . ? C27 C28 H28A 110.7 . . ? O2 C28 H28B 110.7 . . ? C27 C28 H28B 110.7 . . ? H28A C28 H28B 108.8 . . ? Cl1 C29 Cl2 112.18(14) . . ? Cl1 C29 H29A 109.2 . . ? Cl2 C29 H29A 109.2 . . ? Cl1 C29 H29B 109.2 . . ? Cl2 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? O2 Li O1 114.46(16) 2_655 . ? O2 Li N2 102.47(14) 2_655 . ? O1 Li N2 74.00(10) . . ? O2 Li Al 144.64(16) 2_655 . ? O1 Li Al 65.69(9) . . ? N2 Li Al 42.28(6) . . ? O2 Li H2AL 163.8(6) 2_655 . ? O1 Li H2AL 80.4(6) . . ? N2 Li H2AL 74.6(5) . . ? Al Li H2AL 34.1(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.593 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.091 data_fred2 _database_code_depnum_ccdc_archive 'CCDC 735906' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H54 Al Li N2 O4' _chemical_formula_sum 'C39 H54 Al Li N2 O4' _chemical_formula_weight 648.76 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' 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.5757(14) _cell_length_b 22.3191(16) _cell_length_c 17.1128(7) _cell_angle_alpha 90.00 _cell_angle_beta 124.518(3) _cell_angle_gamma 90.00 _cell_volume 7419.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28899 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.095 _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 173(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 KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21934 _diffrn_reflns_av_R_equivalents 0.0889 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8428 _reflns_number_gt 4825 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1493P)^2^+9.8790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0020(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8428 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1556 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2899 _refine_ls_wR_factor_gt 0.2436 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C1 C 0.83560(17) 0.21929(15) 0.2552(2) 0.0353(8) Uani 1 1 d . B . H1 H 0.8625 0.2509 0.3041 0.042 Uiso 1 1 calc R . . C2 C 0.77384(18) 0.25001(15) 0.1690(2) 0.0402(8) Uani 1 1 d . . . H2A H 0.7441 0.2677 0.1868 0.048 Uiso 1 1 calc R . . H2B H 0.7464 0.2201 0.1184 0.048 Uiso 1 1 calc R . . C3 C 0.7981(2) 0.29935(19) 0.1320(3) 0.0597(12) Uani 1 1 d . . . H3A H 0.7575 0.3178 0.0749 0.072 Uiso 1 1 calc R . . H3B H 0.8221 0.3309 0.1810 0.072 Uiso 1 1 calc R . . C4 C 0.8458(2) 0.2752(2) 0.1076(3) 0.0657(13) Uani 1 1 d . . . H4A H 0.8630 0.3088 0.0887 0.079 Uiso 1 1 calc R . . H4B H 0.8200 0.2476 0.0529 0.079 Uiso 1 1 calc R . . C5 C 0.9065(2) 0.2421(2) 0.1909(3) 0.0609(12) Uani 1 1 d . . . H5A H 0.9361 0.2710 0.2424 0.073 Uiso 1 1 calc R . . H5B H 0.9344 0.2237 0.1706 0.073 Uiso 1 1 calc R . . C6 C 0.88222(18) 0.19361(18) 0.2282(2) 0.0463(9) Uani 1 1 d . . . H6A H 0.9227 0.1744 0.2844 0.056 Uiso 1 1 calc R . . H6B H 0.8569 0.1625 0.1789 0.056 Uiso 1 1 calc R . . C7 C 0.85785(17) 0.16789(15) 0.3935(2) 0.0356(8) Uani 1 1 d . B . C8 C 0.92581(18) 0.18885(17) 0.4541(2) 0.0432(8) Uani 1 1 d . . . H8 H 0.9452 0.2117 0.4279 0.052 Uiso 1 1 calc R . . C9 C 0.9656(2) 0.17735(18) 0.5509(3) 0.0496(9) Uani 1 1 d . . . H9 H 1.0113 0.1923 0.5891 0.059 Uiso 1 1 calc R . . C10 C 0.9401(2) 0.14487(19) 0.5922(2) 0.0513(10) Uani 1 1 d . . . H10 H 0.9679 0.1371 0.6585 0.062 Uiso 1 1 calc R . . C11 C 0.87273(19) 0.12330(16) 0.5359(2) 0.0426(9) Uani 1 1 d . . . H11 H 0.8540 0.1005 0.5631 0.051 Uiso 1 1 calc R . . C12 C 0.83412(17) 0.13562(15) 0.4406(2) 0.0350(7) Uani 1 1 d . . . C13 C 0.71235(17) 0.15047(14) 0.3675(2) 0.0340(7) Uani 1 1 d . . . C14 C 0.71586(19) 0.17637(16) 0.4428(2) 0.0415(8) Uani 1 1 d . . . H14 H 0.7563 0.1729 0.5053 0.050 Uiso 1 1 calc R . . C15 C 0.6586(2) 0.20796(17) 0.4255(3) 0.0469(9) Uani 1 1 d . . . H15 H 0.6597 0.2269 0.4761 0.056 Uiso 1 1 calc R . . C16 C 0.6010(2) 0.21130(17) 0.3349(3) 0.0450(9) Uani 1 1 d . . . H16 H 0.5615 0.2316 0.3234 0.054 Uiso 1 1 calc R . . C17 C 0.59888(18) 0.18587(15) 0.2597(2) 0.0404(8) Uani 1 1 d . . . H17 H 0.5583 0.1899 0.1975 0.048 Uiso 1 1 calc R . . C18 C 0.65541(17) 0.15407(14) 0.2727(2) 0.0340(7) Uani 1 1 d . B . C19 C 0.59500(17) 0.12535(14) 0.1078(2) 0.0354(7) Uani 1 1 d . B . H19 H 0.5566 0.1241 0.1166 0.042 Uiso 1 1 calc R . . C20 C 0.58404(18) 0.18163(15) 0.0495(2) 0.0378(8) Uani 1 1 d . . . H20A H 0.5841 0.2173 0.0839 0.045 Uiso 1 1 calc R . . H20B H 0.6227 0.1858 0.0423 0.045 Uiso 1 1 calc R . . C21 C 0.5166(2) 0.17924(17) -0.0481(3) 0.0507(10) Uani 1 1 d . . . H21A H 0.4780 0.1825 -0.0408 0.061 Uiso 1 1 calc R . . H21B H 0.5143 0.2142 -0.0855 0.061 Uiso 1 1 calc R . . C22 C 0.5080(2) 0.12295(19) -0.1019(3) 0.0554(10) Uani 1 1 d . . . H22A H 0.5420 0.1224 -0.1185 0.067 Uiso 1 1 calc R . . H22B H 0.4613 0.1220 -0.1616 0.067 Uiso 1 1 calc R . . C23 C 0.5182(2) 0.06786(17) -0.0422(3) 0.0514(10) Uani 1 1 d . . . H23A H 0.4815 0.0665 -0.0307 0.062 Uiso 1 1 calc R . . H23B H 0.5144 0.0312 -0.0775 0.062 Uiso 1 1 calc R . . C24 C 0.58841(19) 0.06911(16) 0.0527(3) 0.0462(9) Uani 1 1 d . . . H24A H 0.5937 0.0331 0.0901 0.055 Uiso 1 1 calc R . . H24B H 0.6253 0.0685 0.0416 0.055 Uiso 1 1 calc R . . C25 C 0.8209(2) 0.01363(16) 0.2432(3) 0.0488(9) Uani 1 1 d . . . H25A H 0.8702 0.0189 0.2946 0.059 Uiso 1 1 calc R . . H25B H 0.8125 0.0325 0.1852 0.059 Uiso 1 1 calc R . . C26 C 0.8051(3) -0.0522(2) 0.2255(3) 0.0692(6) Uani 1 1 d . . . C27 C 0.7403(3) -0.07434(19) 0.1877(3) 0.0692(6) Uani 1 1 d . . . H27 H 0.7042 -0.0478 0.1741 0.083 Uiso 1 1 calc R . . C28 C 0.7265(3) -0.1355(2) 0.1688(3) 0.0692(6) Uani 1 1 d . . . H28 H 0.6816 -0.1510 0.1426 0.083 Uiso 1 1 calc R . . C29 C 0.7803(3) -0.1727(2) 0.1896(3) 0.0692(6) Uani 1 1 d . . . H29 H 0.7719 -0.2145 0.1781 0.083 Uiso 1 1 calc R . . C30 C 0.8436(3) -0.1519(2) 0.2254(3) 0.0692(6) Uani 1 1 d . . . H30 H 0.8794 -0.1783 0.2375 0.083 Uiso 1 1 calc R . . C31 C 0.8562(3) -0.0926(2) 0.2442(3) 0.0692(6) Uani 1 1 d . . . H31 H 0.9016 -0.0782 0.2711 0.083 Uiso 1 1 calc R . . C32 C 0.9277(8) -0.0244(6) 0.5125(11) 0.0819(8) Uani 0.50 1 d P A 1 H32A H 0.9483 0.0069 0.5623 0.098 Uiso 0.50 1 calc PR A 1 H32B H 0.9375 -0.0141 0.4650 0.098 Uiso 0.50 1 calc PR A 1 C33 C 0.9572(6) -0.0809(5) 0.5537(9) 0.0819(8) Uani 0.50 1 d P A 1 H33A H 0.9937 -0.0911 0.5439 0.098 Uiso 0.50 1 calc PR A 1 H33B H 0.9778 -0.0802 0.6226 0.098 Uiso 0.50 1 calc PR A 1 C34 C 0.9045(5) -0.1222(5) 0.5090(9) 0.0819(8) Uani 0.50 1 d P A 1 H34A H 0.9085 -0.1505 0.5564 0.098 Uiso 0.50 1 calc PR A 1 H34B H 0.9081 -0.1454 0.4626 0.098 Uiso 0.50 1 calc PR A 1 C35 C 0.8408(6) -0.0932(5) 0.4623(9) 0.0819(8) Uani 0.50 1 d P A 1 H35A H 0.8169 -0.1024 0.4933 0.098 Uiso 0.50 1 calc PR A 1 H35B H 0.8113 -0.1060 0.3951 0.098 Uiso 0.50 1 calc PR A 1 C32B C 0.9280(8) -0.0144(6) 0.4947(11) 0.0819(8) Uani 0.50 1 d PD A 2 H32C H 0.9394 0.0288 0.5069 0.098 Uiso 0.50 1 calc PR A 2 H32D H 0.9330 -0.0278 0.4437 0.098 Uiso 0.50 1 calc PR A 2 C33B C 0.9730(6) -0.0512(5) 0.5842(8) 0.0819(8) Uani 0.50 1 d P A 2 H33C H 1.0117 -0.0694 0.5852 0.098 Uiso 0.50 1 calc PR A 2 H33D H 0.9921 -0.0256 0.6412 0.098 Uiso 0.50 1 calc PR A 2 C34B C 0.9271(5) -0.0991(5) 0.5822(8) 0.0819(8) Uani 0.50 1 d PD A 2 H34C H 0.9355 -0.1380 0.5626 0.098 Uiso 0.50 1 calc PR A 2 H34D H 0.9359 -0.1039 0.6457 0.098 Uiso 0.50 1 calc PR A 2 C35B C 0.8552(6) -0.0788(5) 0.5123(9) 0.0819(8) Uani 0.50 1 d P A 2 H35C H 0.8291 -0.1102 0.4638 0.098 Uiso 0.50 1 calc PR A 2 H35D H 0.8320 -0.0711 0.5447 0.098 Uiso 0.50 1 calc PR A 2 C36 C 0.6425(7) -0.0132(9) 0.2904(9) 0.0800(14) Uani 0.50 1 d P B 1 H36A H 0.6413 0.0153 0.2451 0.096 Uiso 0.50 1 calc PR B 1 H36B H 0.6362 -0.0542 0.2648 0.096 Uiso 0.50 1 calc PR B 1 C37 C 0.5918(7) 0.0002(7) 0.3033(7) 0.0800(14) Uani 0.50 1 d P B 1 H37A H 0.5694 -0.0371 0.3039 0.096 Uiso 0.50 1 calc PR B 1 H37B H 0.5564 0.0256 0.2505 0.096 Uiso 0.50 1 calc PR B 1 C38 C 0.6232(6) 0.0332(7) 0.3971(7) 0.0800(14) Uani 0.50 1 d P B 1 H38A H 0.5971 0.0242 0.4249 0.096 Uiso 0.50 1 calc PR B 1 H38B H 0.6220 0.0770 0.3871 0.096 Uiso 0.50 1 calc PR B 1 C39 C 0.6993(10) 0.0113(8) 0.4648(14) 0.0800(14) Uani 0.50 1 d P B 1 H39A H 0.7041 -0.0226 0.5054 0.096 Uiso 0.50 1 calc PR B 1 H39B H 0.7313 0.0440 0.5042 0.096 Uiso 0.50 1 calc PR B 1 C36B C 0.6366(8) -0.0175(9) 0.3101(9) 0.0800(14) Uani 0.50 1 d P B 2 H36C H 0.6272 -0.0610 0.2992 0.096 Uiso 0.50 1 calc PR B 2 H36D H 0.6253 0.0008 0.2502 0.096 Uiso 0.50 1 calc PR B 2 C37B C 0.5928(7) 0.0087(7) 0.3360(8) 0.0800(14) Uani 0.50 1 d P B 2 H37C H 0.5615 -0.0218 0.3341 0.096 Uiso 0.50 1 calc PR B 2 H37D H 0.5648 0.0419 0.2926 0.096 Uiso 0.50 1 calc PR B 2 C38B C 0.6419(7) 0.0313(7) 0.4345(7) 0.0800(14) Uani 0.50 1 d P B 2 H38C H 0.6281 0.0200 0.4774 0.096 Uiso 0.50 1 calc PR B 2 H38D H 0.6487 0.0752 0.4366 0.096 Uiso 0.50 1 calc PR B 2 C39B C 0.7042(10) -0.0032(8) 0.4552(14) 0.0800(14) Uani 0.50 1 d P B 2 H39C H 0.7464 0.0174 0.5062 0.096 Uiso 0.50 1 calc PR B 2 H39D H 0.7037 -0.0437 0.4786 0.096 Uiso 0.50 1 calc PR B 2 Li1 Li 0.7789(4) 0.0209(3) 0.3733(5) 0.0548(17) Uani 1 1 d . . . N1 N 0.81394(14) 0.17512(12) 0.29704(18) 0.0333(6) Uani 1 1 d . . . N2 N 0.65963(13) 0.12724(12) 0.20340(17) 0.0321(6) Uani 1 1 d . . . O1 O 0.76645(11) 0.11317(10) 0.38108(15) 0.0357(5) Uani 1 1 d . B . O2 O 0.78069(13) 0.04301(10) 0.26887(16) 0.0412(6) Uani 1 1 d . B . O3 O 0.85692(18) -0.02643(15) 0.4692(3) 0.0819(8) Uani 1 1 d . A . O4 O 0.70649(16) -0.00870(15) 0.3805(2) 0.0652(8) Uani 1 1 d . B . Al1 Al 0.74627(5) 0.11613(4) 0.22404(7) 0.0326(3) Uani 1 1 d . B . H1A H 0.7338(16) 0.1156(14) 0.131(2) 0.035(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 C1 0.0392(18) 0.0385(18) 0.0301(16) -0.0050(14) 0.0207(15) -0.0085(14) C2 0.043(2) 0.0338(18) 0.0372(18) 0.0021(14) 0.0190(16) -0.0040(15) C3 0.068(3) 0.052(2) 0.044(2) 0.0060(18) 0.022(2) -0.019(2) C4 0.070(3) 0.085(3) 0.042(2) 0.002(2) 0.032(2) -0.033(3) C5 0.053(2) 0.093(3) 0.041(2) -0.014(2) 0.0291(19) -0.030(2) C6 0.038(2) 0.063(2) 0.0350(18) -0.0044(17) 0.0192(16) -0.0038(17) C7 0.0394(19) 0.0364(18) 0.0290(16) -0.0025(14) 0.0182(15) -0.0013(14) C8 0.042(2) 0.049(2) 0.0328(17) -0.0015(16) 0.0182(16) -0.0074(16) C9 0.042(2) 0.058(2) 0.0355(19) -0.0040(17) 0.0143(16) -0.0048(18) C10 0.049(2) 0.061(2) 0.0278(17) 0.0020(17) 0.0125(16) 0.0036(19) C11 0.051(2) 0.044(2) 0.0307(17) 0.0043(15) 0.0222(16) 0.0038(16) C12 0.0400(18) 0.0319(16) 0.0307(16) -0.0014(13) 0.0186(15) -0.0017(14) C13 0.0412(19) 0.0285(16) 0.0346(17) 0.0003(14) 0.0230(15) -0.0031(14) C14 0.049(2) 0.043(2) 0.0352(18) -0.0068(15) 0.0253(16) -0.0086(16) C15 0.055(2) 0.051(2) 0.046(2) -0.0108(17) 0.0356(19) -0.0060(18) C16 0.046(2) 0.046(2) 0.047(2) -0.0064(17) 0.0295(18) -0.0035(17) C17 0.0418(19) 0.0368(18) 0.0406(19) -0.0021(15) 0.0222(16) -0.0035(15) C18 0.0424(19) 0.0291(16) 0.0311(16) -0.0027(13) 0.0212(15) -0.0073(14) C19 0.0355(18) 0.0332(17) 0.0325(16) -0.0016(14) 0.0163(14) -0.0002(14) C20 0.0442(19) 0.0322(17) 0.0359(17) 0.0008(14) 0.0221(15) 0.0002(15) C21 0.049(2) 0.046(2) 0.042(2) 0.0089(17) 0.0169(18) 0.0043(18) C22 0.053(2) 0.064(3) 0.037(2) 0.0010(18) 0.0176(18) -0.002(2) C23 0.048(2) 0.048(2) 0.040(2) -0.0097(17) 0.0142(17) -0.0051(18) C24 0.048(2) 0.0379(19) 0.0413(19) -0.0012(16) 0.0185(17) -0.0038(16) C25 0.056(2) 0.042(2) 0.054(2) 0.0022(17) 0.034(2) 0.0074(18) C26 0.1121(17) 0.0466(10) 0.0557(11) 0.0010(8) 0.0517(12) 0.0141(10) C27 0.1121(17) 0.0466(10) 0.0557(11) 0.0010(8) 0.0517(12) 0.0141(10) C28 0.1121(17) 0.0466(10) 0.0557(11) 0.0010(8) 0.0517(12) 0.0141(10) C29 0.1121(17) 0.0466(10) 0.0557(11) 0.0010(8) 0.0517(12) 0.0141(10) C30 0.1121(17) 0.0466(10) 0.0557(11) 0.0010(8) 0.0517(12) 0.0141(10) C31 0.1121(17) 0.0466(10) 0.0557(11) 0.0010(8) 0.0517(12) 0.0141(10) C32 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C33 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C34 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C35 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C32B 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C33B 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C34B 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C35B 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) C36 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C37 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C38 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C39 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C36B 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C37B 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C38B 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) C39B 0.073(2) 0.115(3) 0.052(3) -0.005(3) 0.035(2) -0.028(2) Li1 0.069(4) 0.048(4) 0.050(4) 0.016(3) 0.035(3) 0.006(3) N1 0.0394(15) 0.0341(15) 0.0258(13) 0.0010(11) 0.0181(12) -0.0032(12) N2 0.0356(15) 0.0316(14) 0.0265(13) -0.0010(11) 0.0160(12) -0.0019(11) O1 0.0405(13) 0.0340(12) 0.0311(11) -0.0013(9) 0.0194(10) -0.0019(10) O2 0.0546(15) 0.0314(12) 0.0418(13) 0.0014(10) 0.0299(12) 0.0049(11) O3 0.0720(15) 0.0606(16) 0.093(2) 0.0274(14) 0.0344(15) 0.0024(12) O4 0.0662(19) 0.077(2) 0.0508(16) 0.0077(15) 0.0320(15) -0.0161(16) Al1 0.0385(6) 0.0290(5) 0.0289(5) -0.0016(4) 0.0183(4) -0.0023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.470(4) . ? C1 C6 1.525(5) . ? C1 C2 1.527(5) . ? C1 H1 1.0000 . ? C2 C3 1.532(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.505(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.522(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.524(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N1 1.373(4) . ? C7 C8 1.407(5) . ? C7 C12 1.412(5) . ? C8 C9 1.389(5) . ? C8 H8 0.9500 . ? C9 C10 1.367(6) . ? C9 H9 0.9500 . ? C10 C11 1.395(5) . ? C10 H10 0.9500 . ? C11 C12 1.372(5) . ? C11 H11 0.9500 . ? C12 O1 1.411(4) . ? C13 C14 1.371(5) . ? C13 C18 1.405(5) . ? C13 O1 1.428(4) . ? C14 C15 1.398(5) . ? C14 H14 0.9500 . ? C15 C16 1.366(5) . ? C15 H15 0.9500 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C17 C18 1.412(5) . ? C17 H17 0.9500 . ? C18 N2 1.381(4) . ? C19 N2 1.475(4) . ? C19 C24 1.524(5) . ? C19 C20 1.532(4) . ? C19 H19 1.0000 . ? C20 C21 1.520(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.502(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.528(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.527(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O2 1.412(4) . ? C25 C26 1.503(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.371(7) . ? C26 C31 1.391(7) . ? C27 C28 1.398(6) . ? C27 H27 0.9500 . ? C28 C29 1.382(7) . ? C28 H28 0.9500 . ? C29 C30 1.337(7) . ? C29 H29 0.9500 . ? C30 C31 1.354(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 O3 1.391(16) . ? C32 C33 1.419(16) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.379(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.397(15) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 O3 1.526(11) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C32B O3 1.497(15) . ? C32B C33B 1.518(15) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.509(14) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B C35B 1.488(14) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35B O3 1.395(10) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36 C37 1.37(2) . ? C36 O4 1.423(15) . ? C36 Li1 2.786(15) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.523(16) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.56(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O4 1.610(16) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C36B O4 1.397(15) . ? C36B C37B 1.459(19) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B C38B 1.492(15) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38B C39B 1.51(2) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B O4 1.316(17) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? Li1 O2 1.877(7) . ? Li1 O4 1.899(8) . ? Li1 O3 1.942(8) . ? Li1 O1 2.096(7) . ? Li1 Al1 3.067(6) . ? N1 Al1 1.892(3) . ? N2 Al1 1.882(3) . ? O2 Al1 1.790(2) . ? Al1 H1A 1.44(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 N1 C1 C6 113.9(3) . . ? N1 C1 C2 111.6(3) . . ? C6 C1 C2 109.4(3) . . ? N1 C1 H1 107.2 . . ? C6 C1 H1 107.2 . . ? C2 C1 H1 107.2 . . ? C1 C2 C3 110.3(3) . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.7(4) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 111.6(3) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.1(3) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 111.5(3) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N1 C7 C8 128.0(3) . . ? N1 C7 C12 118.3(3) . . ? C8 C7 C12 113.8(3) . . ? C9 C8 C7 122.4(3) . . ? C9 C8 H8 118.8 . . ? C7 C8 H8 118.8 . . ? C10 C9 C8 121.1(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.2(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 118.7(3) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 O1 120.3(3) . . ? C11 C12 C7 124.8(3) . . ? O1 C12 C7 114.9(3) . . ? C14 C13 C18 124.8(3) . . ? C14 C13 O1 121.4(3) . . ? C18 C13 O1 113.7(3) . . ? C13 C14 C15 118.5(3) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 119.2(3) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 121.5(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C18 121.8(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? N2 C18 C13 118.7(3) . . ? N2 C18 C17 127.1(3) . . ? C13 C18 C17 114.2(3) . . ? N2 C19 C24 112.9(3) . . ? N2 C19 C20 112.7(3) . . ? C24 C19 C20 110.6(3) . . ? N2 C19 H19 106.7 . . ? C24 C19 H19 106.7 . . ? C20 C19 H19 106.7 . . ? C21 C20 C19 111.9(3) . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 113.4(3) . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C21 C22 C23 110.4(3) . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 111.2(3) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C19 C24 C23 110.0(3) . . ? C19 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? C19 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? O2 C25 C26 112.5(3) . . ? O2 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? O2 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C31 117.6(4) . . ? C27 C26 C25 122.0(4) . . ? C31 C26 C25 120.3(5) . . ? C26 C27 C28 120.8(5) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 117.9(5) . . ? C29 C28 H28 121.0 . . ? C27 C28 H28 121.0 . . ? C30 C29 C28 122.2(5) . . ? C30 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C29 C30 C31 119.1(5) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C30 C31 C26 122.3(6) . . ? C30 C31 H31 118.8 . . ? C26 C31 H31 118.8 . . ? O3 C32 C33 109.8(10) . . ? O3 C32 H32A 109.7 . . ? C33 C32 H32A 109.7 . . ? O3 C32 H32B 109.7 . . ? C33 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C34 C33 C32 106.5(10) . . ? C34 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? C34 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? C33 C34 C35 110.3(10) . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34B 109.6 . . ? C35 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 O3 105.6(8) . . ? C34 C35 H35A 110.6 . . ? O3 C35 H35A 110.6 . . ? C34 C35 H35B 110.6 . . ? O3 C35 H35B 110.6 . . ? H35A C35 H35B 108.8 . . ? O3 C32B C33B 103.0(8) . . ? O3 C32B H32C 111.2 . . ? C33B C32B H32C 111.2 . . ? O3 C32B H32D 111.2 . . ? C33B C32B H32D 111.2 . . ? H32C C32B H32D 109.1 . . ? C34B C33B C32B 106.1(9) . . ? C34B C33B H33C 110.5 . . ? C32B C33B H33C 110.5 . . ? C34B C33B H33D 110.5 . . ? C32B C33B H33D 110.5 . . ? H33C C33B H33D 108.7 . . ? C35B C34B C33B 106.1(8) . . ? C35B C34B H34C 110.5 . . ? C33B C34B H34C 110.5 . . ? C35B C34B H34D 110.5 . . ? C33B C34B H34D 110.5 . . ? H34C C34B H34D 108.7 . . ? O3 C35B C34B 108.6(8) . . ? O3 C35B H35C 110.0 . . ? C34B C35B H35C 110.0 . . ? O3 C35B H35D 110.0 . . ? C34B C35B H35D 110.0 . . ? H35C C35B H35D 108.3 . . ? C37 C36 O4 107.3(10) . . ? C37 C36 Li1 136.2(11) . . ? C37 C36 H36A 110.3 . . ? O4 C36 H36A 110.3 . . ? Li1 C36 H36A 74.8 . . ? C37 C36 H36B 110.3 . . ? O4 C36 H36B 110.3 . . ? Li1 C36 H36B 108.7 . . ? H36A C36 H36B 108.5 . . ? C36 C37 C38 109.1(11) . . ? C36 C37 H37A 109.9 . . ? C38 C37 H37A 109.9 . . ? C36 C37 H37B 109.9 . . ? C38 C37 H37B 109.9 . . ? H37A C37 H37B 108.3 . . ? C37 C38 C39 107.5(13) . . ? C37 C38 H38A 110.2 . . ? C39 C38 H38A 110.2 . . ? C37 C38 H38B 110.2 . . ? C39 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? C38 C39 O4 94.7(13) . . ? C38 C39 H39A 112.8 . . ? O4 C39 H39A 112.8 . . ? C38 C39 H39B 112.8 . . ? O4 C39 H39B 112.8 . . ? H39A C39 H39B 110.3 . . ? O4 C36B C37B 112.0(11) . . ? O4 C36B H36C 109.2 . . ? C37B C36B H36C 109.2 . . ? O4 C36B H36D 109.2 . . ? C37B C36B H36D 109.2 . . ? H36C C36B H36D 107.9 . . ? C36B C37B C38B 104.4(11) . . ? C36B C37B H37C 110.9 . . ? C38B C37B H37C 110.9 . . ? C36B C37B H37D 110.9 . . ? C38B C37B H37D 110.9 . . ? H37C C37B H37D 108.9 . . ? C37B C38B C39B 97.0(13) . . ? C37B C38B H38C 112.4 . . ? C39B C38B H38C 112.4 . . ? C37B C38B H38D 112.4 . . ? C39B C38B H38D 112.4 . . ? H38C C38B H38D 109.9 . . ? O4 C39B C38B 112.9(15) . . ? O4 C39B H39C 109.0 . . ? C38B C39B H39C 109.0 . . ? O4 C39B H39D 109.0 . . ? C38B C39B H39D 109.0 . . ? H39C C39B H39D 107.8 . . ? O2 Li1 O4 131.2(4) . . ? O2 Li1 O3 115.3(4) . . ? O4 Li1 O3 102.2(3) . . ? O2 Li1 O1 83.2(3) . . ? O4 Li1 O1 100.0(3) . . ? O3 Li1 O1 125.5(4) . . ? O2 Li1 C36 103.2(4) . . ? O4 Li1 C36 28.0(3) . . ? O3 Li1 C36 123.3(5) . . ? O1 Li1 C36 97.9(5) . . ? O2 Li1 Al1 32.36(14) . . ? O4 Li1 Al1 119.0(3) . . ? O3 Li1 Al1 138.7(3) . . ? O1 Li1 Al1 52.67(15) . . ? C36 Li1 Al1 95.3(4) . . ? C7 N1 C1 115.5(3) . . ? C7 N1 Al1 119.4(2) . . ? C1 N1 Al1 122.73(19) . . ? C18 N2 C19 115.7(3) . . ? C18 N2 Al1 119.6(2) . . ? C19 N2 Al1 122.2(2) . . ? C12 O1 C13 116.8(2) . . ? C12 O1 Li1 104.6(3) . . ? C13 O1 Li1 135.0(3) . . ? C25 O2 Al1 120.8(2) . . ? C25 O2 Li1 123.7(3) . . ? Al1 O2 Li1 113.5(2) . . ? C32 O3 C35B 97.5(7) . . ? C35B O3 C32B 111.1(7) . . ? C32 O3 C35 104.1(7) . . ? C32B O3 C35 112.7(8) . . ? C32 O3 Li1 135.1(5) . . ? C35B O3 Li1 127.2(6) . . ? C32B O3 Li1 121.1(5) . . ? C35 O3 Li1 113.0(5) . . ? C39B O4 C36B 100.0(10) . . ? C39B O4 C36 117.2(10) . . ? C36B O4 C39 98.0(9) . . ? C36 O4 C39 113.9(9) . . ? C39B O4 Li1 124.4(9) . . ? C36B O4 Li1 131.1(5) . . ? C36 O4 Li1 113.2(5) . . ? C39 O4 Li1 121.2(7) . . ? O2 Al1 N2 112.38(12) . . ? O2 Al1 N1 110.09(12) . . ? N2 Al1 N1 116.85(12) . . ? O2 Al1 Li1 34.14(15) . . ? N2 Al1 Li1 88.93(16) . . ? N1 Al1 Li1 102.28(16) . . ? O2 Al1 H1A 103.0(13) . . ? N2 Al1 H1A 105.8(13) . . ? N1 Al1 H1A 107.6(13) . . ? Li1 Al1 H1A 135.2(13) . . ? 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 C1 C2 C3 175.3(3) . . . . ? C6 C1 C2 C3 -57.8(4) . . . . ? C1 C2 C3 C4 57.0(4) . . . . ? C2 C3 C4 C5 -54.7(5) . . . . ? C3 C4 C5 C6 53.8(5) . . . . ? C4 C5 C6 C1 -55.8(4) . . . . ? N1 C1 C6 C5 -176.5(3) . . . . ? C2 C1 C6 C5 57.9(4) . . . . ? N1 C7 C8 C9 -178.6(3) . . . . ? C12 C7 C8 C9 1.3(5) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C8 C9 C10 C11 -0.4(6) . . . . ? C9 C10 C11 C12 -0.2(6) . . . . ? C10 C11 C12 O1 178.3(3) . . . . ? C10 C11 C12 C7 1.4(6) . . . . ? N1 C7 C12 C11 177.9(3) . . . . ? C8 C7 C12 C11 -1.9(5) . . . . ? N1 C7 C12 O1 0.9(4) . . . . ? C8 C7 C12 O1 -178.9(3) . . . . ? C18 C13 C14 C15 1.2(5) . . . . ? O1 C13 C14 C15 -174.4(3) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C14 C15 C16 C17 -2.2(6) . . . . ? C15 C16 C17 C18 1.4(6) . . . . ? C14 C13 C18 N2 178.1(3) . . . . ? O1 C13 C18 N2 -6.0(4) . . . . ? C14 C13 C18 C17 -1.9(5) . . . . ? O1 C13 C18 C17 174.0(3) . . . . ? C16 C17 C18 N2 -179.5(3) . . . . ? C16 C17 C18 C13 0.6(5) . . . . ? N2 C19 C20 C21 -179.0(3) . . . . ? C24 C19 C20 C21 53.5(4) . . . . ? C19 C20 C21 C22 -52.3(4) . . . . ? C20 C21 C22 C23 53.2(5) . . . . ? C21 C22 C23 C24 -56.5(5) . . . . ? N2 C19 C24 C23 175.7(3) . . . . ? C20 C19 C24 C23 -57.0(4) . . . . ? C22 C23 C24 C19 59.0(4) . . . . ? O2 C25 C26 C27 33.3(6) . . . . ? O2 C25 C26 C31 -149.1(4) . . . . ? C31 C26 C27 C28 0.0(6) . . . . ? C25 C26 C27 C28 177.8(4) . . . . ? C26 C27 C28 C29 0.1(6) . . . . ? C27 C28 C29 C30 -0.9(7) . . . . ? C28 C29 C30 C31 1.6(7) . . . . ? C29 C30 C31 C26 -1.5(7) . . . . ? C27 C26 C31 C30 0.7(7) . . . . ? C25 C26 C31 C30 -177.1(4) . . . . ? O3 C32 C33 C34 20.4(17) . . . . ? C32 C33 C34 C35 -17.1(17) . . . . ? C33 C34 C35 O3 7.8(15) . . . . ? O3 C32B C33B C34B 22.3(15) . . . . ? C32B C33B C34B C35B -17.4(16) . . . . ? C33B C34B C35B O3 5.1(15) . . . . ? O4 C36 C37 C38 18.2(16) . . . . ? Li1 C36 C37 C38 -13.0(19) . . . . ? C36 C37 C38 C39 -29.0(15) . . . . ? C37 C38 C39 O4 24.1(13) . . . . ? O4 C36B C37B C38B -4.4(15) . . . . ? C36B C37B C38B C39B -15.8(13) . . . . ? C37B C38B C39B O4 35.6(15) . . . . ? C37 C36 Li1 O2 -129.1(14) . . . . ? O4 C36 Li1 O2 178.7(9) . . . . ? C37 C36 Li1 O4 52.2(12) . . . . ? C37 C36 Li1 O3 98.2(16) . . . . ? O4 C36 Li1 O3 45.9(10) . . . . ? C37 C36 Li1 O1 -44.2(15) . . . . ? O4 C36 Li1 O1 -96.5(9) . . . . ? C37 C36 Li1 Al1 -97.2(15) . . . . ? O4 C36 Li1 Al1 -149.5(9) . . . . ? C8 C7 N1 C1 -12.6(5) . . . . ? C12 C7 N1 C1 167.5(3) . . . . ? C8 C7 N1 Al1 150.6(3) . . . . ? C12 C7 N1 Al1 -29.3(4) . . . . ? C6 C1 N1 C7 87.5(3) . . . . ? C2 C1 N1 C7 -148.1(3) . . . . ? C6 C1 N1 Al1 -75.1(3) . . . . ? C2 C1 N1 Al1 49.4(4) . . . . ? C13 C18 N2 C19 171.7(3) . . . . ? C17 C18 N2 C19 -8.3(5) . . . . ? C13 C18 N2 Al1 -25.7(4) . . . . ? C17 C18 N2 Al1 154.3(3) . . . . ? C24 C19 N2 C18 -145.9(3) . . . . ? C20 C19 N2 C18 87.8(3) . . . . ? C24 C19 N2 Al1 51.9(4) . . . . ? C20 C19 N2 Al1 -74.3(3) . . . . ? C11 C12 O1 C13 90.9(4) . . . . ? C7 C12 O1 C13 -91.9(3) . . . . ? C11 C12 O1 Li1 -71.1(4) . . . . ? C7 C12 O1 Li1 106.1(3) . . . . ? C14 C13 O1 C12 -48.6(4) . . . . ? C18 C13 O1 C12 135.4(3) . . . . ? C14 C13 O1 Li1 106.4(4) . . . . ? C18 C13 O1 Li1 -69.7(4) . . . . ? O2 Li1 O1 C12 -89.9(3) . . . . ? O4 Li1 O1 C12 139.4(3) . . . . ? O3 Li1 O1 C12 26.4(5) . . . . ? C36 Li1 O1 C12 167.6(3) . . . . ? Al1 Li1 O1 C12 -101.71(19) . . . . ? O2 Li1 O1 C13 113.1(3) . . . . ? O4 Li1 O1 C13 -17.7(5) . . . . ? O3 Li1 O1 C13 -130.6(4) . . . . ? C36 Li1 O1 C13 10.6(5) . . . . ? Al1 Li1 O1 C13 101.3(3) . . . . ? C26 C25 O2 Al1 -140.0(3) . . . . ? C26 C25 O2 Li1 57.4(5) . . . . ? O4 Li1 O2 C25 -116.6(5) . . . . ? O3 Li1 O2 C25 19.9(6) . . . . ? O1 Li1 O2 C25 146.0(3) . . . . ? C36 Li1 O2 C25 -117.4(5) . . . . ? Al1 Li1 O2 C25 163.8(4) . . . . ? O4 Li1 O2 Al1 79.6(5) . . . . ? O3 Li1 O2 Al1 -143.9(3) . . . . ? O1 Li1 O2 Al1 -17.7(3) . . . . ? C36 Li1 O2 Al1 78.8(5) . . . . ? C33 C32 O3 C35B 15.7(15) . . . . ? C33 C32 O3 C32B -143(6) . . . . ? C33 C32 O3 C35 -15.1(15) . . . . ? C33 C32 O3 Li1 -160.4(8) . . . . ? C34B C35B O3 C32 4.1(13) . . . . ? C34B C35B O3 C32B 9.7(14) . . . . ? C34B C35B O3 C35 109(2) . . . . ? C34B C35B O3 Li1 -179.3(7) . . . . ? C33B C32B O3 C32 3(5) . . . . ? C33B C32B O3 C35B -20.1(14) . . . . ? C33B C32B O3 C35 -53.5(14) . . . . ? C33B C32B O3 Li1 168.2(8) . . . . ? C34 C35 O3 C32 4.6(13) . . . . ? C34 C35 O3 C35B -76.5(15) . . . . ? C34 C35 O3 C32B 17.0(13) . . . . ? C34 C35 O3 Li1 158.7(8) . . . . ? O2 Li1 O3 C32 42.5(13) . . . . ? O4 Li1 O3 C32 -169.5(12) . . . . ? O1 Li1 O3 C32 -57.6(13) . . . . ? C36 Li1 O3 C32 170.3(12) . . . . ? Al1 Li1 O3 C32 13.9(14) . . . . ? O2 Li1 O3 C35B -132.7(8) . . . . ? O4 Li1 O3 C35B 15.3(9) . . . . ? O1 Li1 O3 C35B 127.2(8) . . . . ? C36 Li1 O3 C35B -4.9(10) . . . . ? Al1 Li1 O3 C35B -161.3(8) . . . . ? O2 Li1 O3 C32B 37.4(10) . . . . ? O4 Li1 O3 C32B -174.6(9) . . . . ? O1 Li1 O3 C32B -62.7(10) . . . . ? C36 Li1 O3 C32B 165.2(10) . . . . ? Al1 Li1 O3 C32B 8.9(11) . . . . ? O2 Li1 O3 C35 -100.7(7) . . . . ? O4 Li1 O3 C35 47.3(7) . . . . ? O1 Li1 O3 C35 159.2(7) . . . . ? C36 Li1 O3 C35 27.1(9) . . . . ? Al1 Li1 O3 C35 -129.3(7) . . . . ? C38B C39B O4 C36B -38.4(16) . . . . ? C38B C39B O4 C36 -32.9(18) . . . . ? C38B C39B O4 C39 43(7) . . . . ? C38B C39B O4 Li1 119.8(12) . . . . ? C37B C36B O4 C39B 25.6(15) . . . . ? C37B C36B O4 C36 -139(6) . . . . ? C37B C36B O4 C39 14.3(12) . . . . ? C37B C36B O4 Li1 -130.4(8) . . . . ? C37 C36 O4 C39B 10.6(17) . . . . ? Li1 C36 O4 C39B 155.7(12) . . . . ? C37 C36 O4 C36B 28(4) . . . . ? Li1 C36 O4 C36B 173(5) . . . . ? C37 C36 O4 C39 -1.3(17) . . . . ? Li1 C36 O4 C39 143.7(12) . . . . ? C37 C36 O4 Li1 -145.0(9) . . . . ? C38 C39 O4 C39B -124(8) . . . . ? C38 C39 O4 C36B -23.7(12) . . . . ? C38 C39 O4 C36 -14.8(15) . . . . ? C38 C39 O4 Li1 125.7(9) . . . . ? O2 Li1 O4 C39B -155.3(11) . . . . ? O3 Li1 O4 C39B 64.3(11) . . . . ? O1 Li1 O4 C39B -65.6(11) . . . . ? C36 Li1 O4 C39B -153.6(14) . . . . ? Al1 Li1 O4 C39B -118.3(11) . . . . ? O2 Li1 O4 C36B -4.4(13) . . . . ? O3 Li1 O4 C36B -144.8(12) . . . . ? O1 Li1 O4 C36B 85.3(12) . . . . ? C36 Li1 O4 C36B -2.7(19) . . . . ? Al1 Li1 O4 C36B 32.6(12) . . . . ? O2 Li1 O4 C36 -1.7(11) . . . . ? O3 Li1 O4 C36 -142.1(9) . . . . ? O1 Li1 O4 C36 88.0(10) . . . . ? Al1 Li1 O4 C36 35.3(10) . . . . ? O2 Li1 O4 C39 -142.4(10) . . . . ? O3 Li1 O4 C39 77.2(9) . . . . ? O1 Li1 O4 C39 -52.7(9) . . . . ? C36 Li1 O4 C39 -140.8(14) . . . . ? Al1 Li1 O4 C39 -105.4(9) . . . . ? C25 O2 Al1 N2 145.8(3) . . . . ? Li1 O2 Al1 N2 -49.9(3) . . . . ? C25 O2 Al1 N1 -82.1(3) . . . . ? Li1 O2 Al1 N1 82.2(3) . . . . ? C25 O2 Al1 Li1 -164.3(4) . . . . ? C18 N2 Al1 O2 95.3(2) . . . . ? C19 N2 Al1 O2 -103.2(2) . . . . ? C18 N2 Al1 N1 -33.3(3) . . . . ? C19 N2 Al1 N1 128.1(2) . . . . ? C18 N2 Al1 Li1 69.9(3) . . . . ? C19 N2 Al1 Li1 -128.6(3) . . . . ? C7 N1 Al1 O2 -38.4(3) . . . . ? C1 N1 Al1 O2 123.5(2) . . . . ? C7 N1 Al1 N2 91.3(3) . . . . ? C1 N1 Al1 N2 -106.7(3) . . . . ? C7 N1 Al1 Li1 -3.8(3) . . . . ? C1 N1 Al1 Li1 158.2(3) . . . . ? O4 Li1 Al1 O2 -122.3(5) . . . . ? O3 Li1 Al1 O2 53.9(5) . . . . ? O1 Li1 Al1 O2 157.7(4) . . . . ? C36 Li1 Al1 O2 -106.4(5) . . . . ? O2 Li1 Al1 N2 134.9(3) . . . . ? O4 Li1 Al1 N2 12.7(3) . . . . ? O3 Li1 Al1 N2 -171.2(5) . . . . ? O1 Li1 Al1 N2 -67.40(19) . . . . ? C36 Li1 Al1 N2 28.5(4) . . . . ? O2 Li1 Al1 N1 -107.8(3) . . . . ? O4 Li1 Al1 N1 130.0(3) . . . . ? O3 Li1 Al1 N1 -53.9(5) . . . . ? O1 Li1 Al1 N1 49.9(2) . . . . ? C36 Li1 Al1 N1 145.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.138 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.133 # Attachment 'compound_5a_CCDC-735907__cif_revised_final_.cif' data_welt7 _database_code_depnum_ccdc_archive 'CCDC 735907' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H56 Al Li N2 O5' _chemical_formula_sum 'C44 H56 Al Li N2 O5' _chemical_formula_weight 726.83 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 0.0000 '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' Al Al 0.0645 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 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 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7739(4) _cell_length_b 20.3007(11) _cell_length_c 11.7890(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.960(3) _cell_angle_gamma 90.00 _cell_volume 1997.49(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6969 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.098 _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 173(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 KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10906 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4707 _reflns_number_gt 2780 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The structure contains disorder. Restraints are used to fix C-C bond distances according to standard values reported in the International Tables for Crystallography (Vol. C). ; _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^)+(0.1391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.061(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 4707 _refine_ls_number_parameters 467 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1554 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2392 _refine_ls_wR_factor_gt 0.2010 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.031 _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 C1 C -1.5755(7) 0.1399(3) -1.6082(5) 0.0457(15) Uani 1 1 d . D . H1 H -1.5843 0.1801 -1.5616 0.055 Uiso 1 1 calc R . . C2 C -1.6126(8) 0.1631(4) -1.7377(6) 0.061(2) Uani 1 1 d . . . H2A H -1.5642 0.2068 -1.7415 0.073 Uiso 1 1 calc R . . H2B H -1.5719 0.1312 -1.7850 0.073 Uiso 1 1 calc R . . C3 C -1.7938(9) 0.1669(6) -1.7828(8) 0.092(2) Uani 1 1 d . . . H3A H -1.8323 0.2085 -1.7576 0.111 Uiso 1 1 calc R . . H3B H -1.8334 0.1640 -1.8709 0.111 Uiso 1 1 calc R . . C4 C -1.8490(10) 0.1083(6) -1.7267(8) 0.092(2) Uani 1 1 d . . . H4A H -1.9532 0.1178 -1.7140 0.111 Uiso 1 1 calc R . . H4B H -1.8617 0.0692 -1.7790 0.111 Uiso 1 1 calc R . . C5 C -1.7222(8) 0.0959(5) -1.6093(6) 0.064(2) Uani 1 1 d . . . H5A H -1.6913 0.0489 -1.6017 0.077 Uiso 1 1 calc R . . H5B H -1.7625 0.1079 -1.5423 0.077 Uiso 1 1 calc R . . C6 C -1.3690(8) 0.0582(3) -1.5956(6) 0.0480(16) Uani 1 1 d . B . C7 C -1.4568(11) 0.0196(4) -1.6938(7) 0.067(2) Uani 1 1 d . . . H7 H -1.5638 0.0322 -1.7353 0.081 Uiso 1 1 calc R . . C8 C -1.3947(13) -0.0352(4) -1.7322(8) 0.075(2) Uani 1 1 d . . . H8 H -1.4594 -0.0602 -1.7975 0.090 Uiso 1 1 calc R . . C9 C -1.2399(15) -0.0537(4) -1.6763(8) 0.081(3) Uani 1 1 d . . . H9 H -1.1981 -0.0920 -1.7024 0.097 Uiso 1 1 calc R . . C10 C -1.1420(12) -0.0166(4) -1.5806(7) 0.070(2) Uani 1 1 d . . . H10 H -1.0334 -0.0286 -1.5430 0.084 Uiso 1 1 calc R . . C11 C -1.2085(9) 0.0381(3) -1.5427(6) 0.0502(16) Uani 1 1 d . B . C12 C -1.0115(7) 0.0563(3) -1.3487(7) 0.0510(17) Uani 1 1 d . B . C13 C -0.8643(8) 0.0331(4) -1.3459(8) 0.063(2) Uani 1 1 d . . . H13 H -0.8335 0.0320 -1.4164 0.076 Uiso 1 1 calc R . . C14 C -0.7588(9) 0.0109(4) -1.2361(10) 0.081(3) Uani 1 1 d . . . H14 H -0.6578 -0.0077 -1.2320 0.098 Uiso 1 1 calc R . . C15 C -0.8051(9) 0.0166(4) -1.1364(9) 0.073(2) Uani 1 1 d . . . H15 H -0.7338 0.0020 -1.0625 0.087 Uiso 1 1 calc R . . C16 C -0.9524(7) 0.0429(4) -1.1379(7) 0.0564(18) Uani 1 1 d . . . H16 H -0.9794 0.0463 -1.0660 0.068 Uiso 1 1 calc R . . C17 C -1.0608(7) 0.0644(3) -1.2459(6) 0.0474(16) Uani 1 1 d . B . C18 C -1.2822(7) 0.0933(3) -1.1691(5) 0.0448(15) Uani 1 1 d . B . H18 H -1.3952 0.1084 -1.2058 0.054 Uiso 1 1 calc R . . C19 C -1.2933(9) 0.0248(4) -1.1133(6) 0.064(2) Uani 1 1 d D . . H19A H -1.2243 -0.0078 -1.1363 0.077 Uiso 1 1 calc R A 1 H19B H -1.4051 0.0084 -1.1387 0.077 Uiso 1 1 calc R A 1 C20 C -1.232(3) 0.0383(11) -0.9726(13) 0.096(4) Uani 0.50 1 d PD B 1 H20A H -1.2883 0.0101 -0.9301 0.115 Uiso 0.50 1 calc PR B 1 H20B H -1.1148 0.0306 -0.9392 0.115 Uiso 0.50 1 calc PR B 1 C21 C -1.273(4) 0.1115(11) -0.965(3) 0.096(4) Uani 0.50 1 d PD B 1 H21A H -1.3900 0.1185 -0.9836 0.115 Uiso 0.50 1 calc PR B 1 H21B H -1.2166 0.1306 -0.8860 0.115 Uiso 0.50 1 calc PR B 1 C20B C -1.322(3) 0.0361(13) -0.9967(14) 0.096(4) Uani 0.50 1 d PD B 2 H20C H -1.2723 0.0009 -0.9390 0.115 Uiso 0.50 1 calc PR B 2 H20D H -1.4376 0.0383 -1.0062 0.115 Uiso 0.50 1 calc PR B 2 C21B C -1.241(4) 0.1020(12) -0.957(2) 0.096(4) Uani 0.50 1 d PD B 2 H21C H -1.1377 0.0948 -0.8934 0.115 Uiso 0.50 1 calc PR B 2 H21D H -1.3098 0.1294 -0.9231 0.115 Uiso 0.50 1 calc PR B 2 C22 C -1.2104(9) 0.1383(4) -1.0618(6) 0.068(2) Uani 1 1 d D . . H22A H -1.0919 0.1367 -1.0365 0.081 Uiso 1 1 calc R B 1 H22B H -1.2455 0.1844 -1.0811 0.081 Uiso 1 1 calc R B 1 C23 C -1.5672(6) 0.2007(3) -1.3466(5) 0.0428(14) Uani 1 1 d . . . H23A H -1.6011 0.1540 -1.3556 0.051 Uiso 1 1 calc R . . H23B H -1.6439 0.2261 -1.4109 0.051 Uiso 1 1 calc R . . C24 C -1.5730(7) 0.2258(3) -1.2275(5) 0.0414(14) Uani 1 1 d . . . C25 C -1.6501(8) 0.1890(4) -1.1624(6) 0.0568(18) Uani 1 1 d . . . H25 H -1.6971 0.1479 -1.1927 0.068 Uiso 1 1 calc R . . C26 C -1.6590(10) 0.2113(5) -1.0544(7) 0.075(2) Uani 1 1 d . . . H26 H -1.7128 0.1857 -1.0111 0.090 Uiso 1 1 calc R . . C27 C -1.5915(11) 0.2697(5) -1.0094(7) 0.075(2) Uani 1 1 d . . . H27 H -1.5966 0.2844 -0.9341 0.090 Uiso 1 1 calc R . . C28 C -1.5153(11) 0.3077(5) -1.0729(7) 0.076(2) Uani 1 1 d . . . H28 H -1.4677 0.3485 -1.0415 0.091 Uiso 1 1 calc R . . C29 C -1.5089(9) 0.2857(4) -1.1834(6) 0.0573(18) Uani 1 1 d . . . H29 H -1.4598 0.3123 -1.2285 0.069 Uiso 1 1 calc R . . C30 C -1.0184(7) 0.2221(3) -1.4452(6) 0.0457(15) Uani 1 1 d . . . H30A H -0.9726 0.1785 -1.4536 0.055 Uiso 1 1 calc R . . H30B H -0.9370 0.2469 -1.3828 0.055 Uiso 1 1 calc R . . C31 C -1.0549(7) 0.2583(3) -1.5604(6) 0.0439(15) Uani 1 1 d . . . C32 C -0.9914(12) 0.3192(4) -1.5692(8) 0.074(2) Uani 1 1 d . . . H32 H -0.9201 0.3385 -1.4996 0.089 Uiso 1 1 calc R . . C33 C -1.0274(15) 0.3532(5) -1.6753(11) 0.101(3) Uani 1 1 d . . . H33 H -0.9802 0.3949 -1.6790 0.121 Uiso 1 1 calc R . . C34 C -1.1348(15) 0.3252(6) -1.7778(10) 0.097(3) Uani 1 1 d . . . H34 H -1.1624 0.3482 -1.8515 0.117 Uiso 1 1 calc R . . C35 C -1.2002(12) 0.2639(5) -1.7708(8) 0.084(3) Uani 1 1 d . . . H35 H -1.2736 0.2447 -1.8394 0.100 Uiso 1 1 calc R . . C36 C -1.1581(10) 0.2314(4) -1.6640(7) 0.069(2) Uani 1 1 d . . . H36 H -1.2011 0.1887 -1.6605 0.082 Uiso 1 1 calc R . . C37 C -1.0118(13) 0.3004(6) -1.1652(8) 0.104(3) Uani 1 1 d D . . H37A H -0.9083 0.3119 -1.1775 0.125 Uiso 1 1 calc R C 1 H37B H -1.0276 0.2522 -1.1762 0.125 Uiso 1 1 calc R C 1 C38 C -1.008(5) 0.3186(14) -1.043(2) 0.128(6) Uani 0.50 1 d PD D 1 H38A H -0.9052 0.3078 -0.9818 0.154 Uiso 0.50 1 calc PR D 1 H38B H -1.0997 0.3013 -1.0203 0.154 Uiso 0.50 1 calc PR D 1 C39 C -1.025(3) 0.394(2) -1.0793(18) 0.128(6) Uani 0.50 1 d PD D 1 H39A H -1.0656 0.4193 -1.0229 0.154 Uiso 0.50 1 calc PR D 1 H39B H -0.9187 0.4123 -1.0762 0.154 Uiso 0.50 1 calc PR D 1 C38B C -0.975(5) 0.3486(18) -1.059(3) 0.128(6) Uani 0.50 1 d PD D 2 H38C H -0.9612 0.3239 -0.9845 0.154 Uiso 0.50 1 calc PR D 2 H38D H -0.8747 0.3727 -1.0525 0.154 Uiso 0.50 1 calc PR D 2 C39B C -1.103(3) 0.3938(17) -1.0774(17) 0.128(6) Uani 0.50 1 d PD D 2 H39C H -1.0679 0.4361 -1.0356 0.154 Uiso 0.50 1 calc PR D 2 H39D H -1.1930 0.3754 -1.0535 0.154 Uiso 0.50 1 calc PR D 2 C40 C -1.1434(13) 0.4006(5) -1.2087(11) 0.117(4) Uani 1 1 d D . . H40A H -1.2520 0.4134 -1.2080 0.140 Uiso 1 1 calc R D 1 H40B H -1.1047 0.4328 -1.2565 0.140 Uiso 1 1 calc R D 1 C41 C -1.392(3) 0.4123(11) -1.478(2) 0.099(3) Uani 0.50 1 d P D 1 H41A H -1.2768 0.4237 -1.4520 0.119 Uiso 0.50 1 calc PR D 1 H41B H -1.4431 0.4310 -1.4216 0.119 Uiso 0.50 1 calc PR D 1 C42 C -1.481(3) 0.4386(13) -1.615(2) 0.099(3) Uani 0.50 1 d P D 1 H42A H -1.4937 0.4870 -1.6199 0.119 Uiso 0.50 1 calc PR D 1 H42B H -1.4272 0.4231 -1.6729 0.119 Uiso 0.50 1 calc PR D 1 C43 C -1.629(3) 0.4046(11) -1.627(2) 0.099(3) Uani 0.50 1 d P D 1 H43A H -1.6778 0.3897 -1.7105 0.119 Uiso 0.50 1 calc PR D 1 H43B H -1.7054 0.4344 -1.6060 0.119 Uiso 0.50 1 calc PR D 1 C44 C -1.590(3) 0.3415(11) -1.538(2) 0.099(3) Uani 0.50 1 d P D 1 H44A H -1.6409 0.3458 -1.4742 0.119 Uiso 0.50 1 calc PR D 1 H44B H -1.6250 0.2998 -1.5817 0.119 Uiso 0.50 1 calc PR D 1 C41B C -1.354(2) 0.4076(9) -1.5278(19) 0.099(3) Uani 0.50 1 d PD D 2 H41C H -1.2991 0.4008 -1.5885 0.119 Uiso 0.50 1 calc PR D 2 H41D H -1.2873 0.4342 -1.4605 0.119 Uiso 0.50 1 calc PR D 2 C42B C -1.533(3) 0.4351(13) -1.582(2) 0.099(3) Uani 0.50 1 d PD D 2 H42C H -1.5381 0.4799 -1.6164 0.119 Uiso 0.50 1 calc PR D 2 H42D H -1.5973 0.4322 -1.5267 0.119 Uiso 0.50 1 calc PR D 2 C43B C -1.570(3) 0.3738(10) -1.6856(18) 0.099(3) Uani 0.50 1 d PD D 2 H43C H -1.6858 0.3699 -1.7296 0.119 Uiso 0.50 1 calc PR D 2 H43D H -1.5089 0.3796 -1.7427 0.119 Uiso 0.50 1 calc PR D 2 C44B C -1.510(3) 0.3167(9) -1.6038(19) 0.099(3) Uani 0.50 1 d PD D 2 H44C H -1.6013 0.2911 -1.5937 0.119 Uiso 0.50 1 calc PR D 2 H44D H -1.4441 0.2873 -1.6363 0.119 Uiso 0.50 1 calc PR D 2 Al1 Al -1.28455(18) 0.14706(8) -1.40214(15) 0.0361(4) Uani 1 1 d . B . Li1 Li -1.2878(13) 0.2808(5) -1.3777(12) 0.056(3) Uani 1 1 d . . . N1 N -1.4183(6) 0.1125(3) -1.5479(4) 0.0429(12) Uani 1 1 d . . . N2 N -1.2104(5) 0.0934(3) -1.2647(4) 0.0400(11) Uani 1 1 d . . . O1 O -1.1212(5) 0.0809(2) -1.4526(4) 0.0486(11) Uani 1 1 d . . . O2 O -1.4116(4) 0.2060(2) -1.3596(3) 0.0389(9) Uani 1 1 d . B . O3 O -1.1567(4) 0.2133(2) -1.4090(4) 0.0443(10) Uani 1 1 d . B . O4 O -1.1413(7) 0.3349(3) -1.2522(5) 0.0739(16) Uani 1 1 d . D . O5 O -1.4140(6) 0.3448(3) -1.4891(6) 0.0683(15) Uani 1 1 d . 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 C1 0.047(3) 0.053(4) 0.037(3) -0.001(3) 0.013(3) -0.006(3) C2 0.058(4) 0.085(6) 0.036(3) 0.012(3) 0.010(3) -0.009(4) C3 0.056(3) 0.140(7) 0.069(4) 0.012(4) 0.002(3) -0.012(4) C4 0.056(3) 0.140(7) 0.069(4) 0.012(4) 0.002(3) -0.012(4) C5 0.067(5) 0.077(5) 0.058(4) -0.016(4) 0.032(4) -0.019(4) C6 0.067(4) 0.043(4) 0.045(4) -0.002(3) 0.033(3) -0.010(3) C7 0.105(6) 0.050(4) 0.055(4) -0.007(4) 0.036(4) -0.016(4) C8 0.114(7) 0.053(5) 0.069(5) -0.017(4) 0.041(5) -0.017(5) C9 0.153(10) 0.040(4) 0.073(6) -0.020(4) 0.067(6) -0.009(5) C10 0.104(6) 0.056(5) 0.071(5) 0.008(4) 0.055(5) 0.005(4) C11 0.076(5) 0.036(3) 0.054(4) -0.003(3) 0.042(4) -0.004(3) C12 0.044(3) 0.037(3) 0.075(5) 0.006(3) 0.023(3) 0.004(3) C13 0.051(4) 0.050(4) 0.096(6) 0.005(4) 0.033(4) 0.002(3) C14 0.048(4) 0.070(6) 0.130(9) 0.005(6) 0.033(5) 0.009(4) C15 0.050(4) 0.054(5) 0.102(7) 0.018(4) 0.004(4) 0.004(4) C16 0.037(3) 0.053(4) 0.070(5) 0.014(4) 0.003(3) 0.005(3) C17 0.041(3) 0.036(3) 0.062(4) 0.011(3) 0.011(3) 0.004(3) C18 0.030(3) 0.055(4) 0.044(3) 0.002(3) 0.004(2) 0.005(3) C19 0.060(4) 0.072(5) 0.063(5) 0.012(4) 0.026(4) -0.009(4) C20 0.099(10) 0.143(8) 0.045(5) 0.007(5) 0.019(6) 0.031(8) C21 0.099(10) 0.143(8) 0.045(5) 0.007(5) 0.019(6) 0.031(8) C20B 0.099(10) 0.143(8) 0.045(5) 0.007(5) 0.019(6) 0.031(8) C21B 0.099(10) 0.143(8) 0.045(5) 0.007(5) 0.019(6) 0.031(8) C22 0.069(4) 0.062(5) 0.056(4) -0.008(4) -0.004(3) 0.016(4) C23 0.036(3) 0.054(4) 0.036(3) 0.000(3) 0.007(2) 0.006(3) C24 0.044(3) 0.045(3) 0.034(3) 0.005(3) 0.010(3) 0.015(3) C25 0.060(4) 0.056(4) 0.054(4) 0.012(3) 0.018(3) 0.005(4) C26 0.090(6) 0.085(6) 0.056(5) 0.013(5) 0.032(4) 0.002(5) C27 0.084(5) 0.100(7) 0.045(4) 0.006(5) 0.026(4) 0.020(5) C28 0.089(6) 0.080(6) 0.054(5) -0.012(4) 0.016(4) 0.002(5) C29 0.064(4) 0.059(4) 0.049(4) -0.008(3) 0.018(3) -0.002(4) C30 0.040(3) 0.042(4) 0.053(4) -0.002(3) 0.011(3) -0.001(3) C31 0.047(3) 0.037(3) 0.051(4) 0.000(3) 0.020(3) 0.001(3) C32 0.115(7) 0.043(4) 0.077(6) -0.007(4) 0.049(5) -0.007(4) C33 0.143(10) 0.059(6) 0.112(9) 0.031(6) 0.057(8) 0.002(6) C34 0.129(9) 0.098(8) 0.071(6) 0.031(6) 0.041(6) 0.031(7) C35 0.094(6) 0.094(7) 0.050(5) 0.004(5) 0.004(4) 0.002(6) C36 0.080(5) 0.066(5) 0.049(4) -0.003(4) 0.005(4) -0.009(4) C37 0.106(8) 0.108(8) 0.080(7) -0.026(6) 0.002(6) -0.004(7) C38 0.132(14) 0.125(13) 0.143(9) -0.076(10) 0.067(9) -0.039(13) C39 0.132(14) 0.125(13) 0.143(9) -0.076(10) 0.067(9) -0.039(13) C38B 0.132(14) 0.125(13) 0.143(9) -0.076(10) 0.067(9) -0.039(13) C39B 0.132(14) 0.125(13) 0.143(9) -0.076(10) 0.067(9) -0.039(13) C40 0.107(7) 0.073(7) 0.181(12) -0.066(8) 0.061(8) -0.035(6) C41 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C42 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C43 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C44 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C41B 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C42B 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C43B 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) C44B 0.128(7) 0.075(4) 0.094(7) 0.020(4) 0.034(5) 0.006(4) Al1 0.0354(8) 0.0359(9) 0.0353(9) 0.0027(8) 0.0085(7) 0.0019(8) Li1 0.053(6) 0.035(6) 0.085(8) -0.004(5) 0.026(6) 0.007(5) N1 0.045(3) 0.043(3) 0.040(3) -0.002(2) 0.011(2) -0.006(2) N2 0.034(2) 0.043(3) 0.041(3) 0.011(2) 0.007(2) 0.010(2) O1 0.051(2) 0.035(2) 0.062(3) 0.004(2) 0.022(2) 0.0057(19) O2 0.0311(18) 0.042(2) 0.040(2) 0.0012(19) 0.0061(15) 0.0035(18) O3 0.038(2) 0.035(2) 0.061(3) 0.002(2) 0.0163(19) 0.0007(19) O4 0.071(3) 0.052(3) 0.088(4) -0.018(3) 0.009(3) -0.004(3) O5 0.059(3) 0.048(3) 0.100(4) 0.014(3) 0.027(3) 0.008(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 C1 N1 1.453(8) . ? C1 C2 1.533(8) . ? C1 C5 1.563(9) . ? C1 H1 1.0000 . ? C2 C3 1.515(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.512(15) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.505(11) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.366(9) . ? C6 C7 1.413(10) . ? C6 C11 1.414(10) . ? C7 C8 1.376(12) . ? C7 H7 0.9500 . ? C8 C9 1.367(14) . ? C8 H8 0.9500 . ? C9 C10 1.407(13) . ? C9 H9 0.9500 . ? C10 C11 1.391(10) . ? C10 H10 0.9500 . ? C11 O1 1.403(8) . ? C12 C13 1.365(9) . ? C12 O1 1.396(8) . ? C12 C17 1.417(10) . ? C13 C14 1.413(13) . ? C13 H13 0.9500 . ? C14 C15 1.362(13) . ? C14 H14 0.9500 . ? C15 C16 1.393(11) . ? C15 H15 0.9500 . ? C16 C17 1.403(9) . ? C16 H16 0.9500 . ? C17 N2 1.392(8) . ? C18 N2 1.450(8) . ? C18 C22 1.531(10) . ? C18 C19 1.554(10) . ? C18 H18 1.0000 . ? C19 C20B 1.488(15) . ? C19 C20 1.601(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.539(19) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.513(18) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20B C21B 1.519(19) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B C22 1.533(17) . ? C21B H21C 0.9900 . ? C21B H21D 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.423(6) . ? C23 C24 1.509(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C29 1.372(10) . ? C24 C25 1.388(9) . ? C25 C26 1.376(11) . ? C25 H25 0.9500 . ? C26 C27 1.358(13) . ? C26 H26 0.9500 . ? C27 C28 1.383(12) . ? C27 H27 0.9500 . ? C28 C29 1.394(10) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 O3 1.416(7) . ? C30 C31 1.489(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.372(10) . ? C31 C36 1.389(10) . ? C32 C33 1.378(13) . ? C32 H32 0.9500 . ? C33 C34 1.403(16) . ? C33 H33 0.9500 . ? C34 C35 1.382(16) . ? C34 H34 0.9500 . ? C35 C36 1.368(12) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 O4 1.454(12) . ? C37 C38 1.476(17) . ? C37 C38B 1.540(17) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.59(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.565(18) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C38B C39B 1.41(5) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B C40 1.484(18) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? C40 O4 1.431(11) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 O5 1.38(2) . ? C41 C42 1.65(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.44(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.63(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 O5 1.47(2) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C41B O5 1.50(2) . ? C41B C42B 1.597(19) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42B C43B 1.70(4) . ? C42B H42C 0.9900 . ? C42B H42D 0.9900 . ? C43B C44B 1.50(3) . ? C43B H43C 0.9900 . ? C43B H43D 0.9900 . ? C44B O5 1.47(2) . ? C44B H44C 0.9900 . ? C44B H44D 0.9900 . ? Al1 O3 1.769(4) . ? Al1 O2 1.808(4) . ? Al1 N1 1.892(5) . ? Al1 N2 1.893(5) . ? Al1 O1 2.177(4) . ? Al1 Li1 2.731(11) . ? Li1 O3 1.897(11) . ? Li1 O2 1.918(12) . ? Li1 O5 1.935(13) . ? Li1 O4 1.968(13) . ? 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 C1 C2 118.9(5) . . ? N1 C1 C5 116.1(6) . . ? C2 C1 C5 104.2(5) . . ? N1 C1 H1 105.5 . . ? C2 C1 H1 105.5 . . ? C5 C1 H1 105.5 . . ? C3 C2 C1 104.1(6) . . ? C3 C2 H2A 110.9 . . ? C1 C2 H2A 110.9 . . ? C3 C2 H2B 110.9 . . ? C1 C2 H2B 110.9 . . ? H2A C2 H2B 109.0 . . ? C4 C3 C2 104.5(7) . . ? C4 C3 H3A 110.9 . . ? C2 C3 H3A 110.9 . . ? C4 C3 H3B 110.9 . . ? C2 C3 H3B 110.9 . . ? H3A C3 H3B 108.9 . . ? C5 C4 C3 106.7(7) . . ? C5 C4 H4A 110.4 . . ? C3 C4 H4A 110.4 . . ? C5 C4 H4B 110.4 . . ? C3 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? C4 C5 C1 106.6(7) . . ? C4 C5 H5A 110.4 . . ? C1 C5 H5A 110.4 . . ? C4 C5 H5B 110.4 . . ? C1 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? N1 C6 C7 128.5(7) . . ? N1 C6 C11 116.8(6) . . ? C7 C6 C11 114.7(6) . . ? C8 C7 C6 123.2(9) . . ? C8 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? C9 C8 C7 120.0(8) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.6(8) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 118.1(9) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 O1 123.6(7) . . ? C10 C11 C6 123.3(7) . . ? O1 C11 C6 113.1(5) . . ? C13 C12 O1 122.4(7) . . ? C13 C12 C17 123.8(7) . . ? O1 C12 C17 113.5(5) . . ? C12 C13 C14 118.7(8) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C15 C14 C13 118.5(7) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C14 C15 C16 123.0(8) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 119.8(8) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? N2 C17 C16 128.2(6) . . ? N2 C17 C12 115.8(6) . . ? C16 C17 C12 116.1(6) . . ? N2 C18 C22 118.3(5) . . ? N2 C18 C19 115.5(5) . . ? C22 C18 C19 104.3(5) . . ? N2 C18 H18 105.9 . . ? C22 C18 H18 105.9 . . ? C19 C18 H18 105.9 . . ? C20B C19 C18 107.7(12) . . ? C18 C19 C20 103.9(10) . . ? C20B C19 H19A 130.3 . . ? C18 C19 H19A 111.0 . . ? C20 C19 H19A 111.0 . . ? C20B C19 H19B 84.3 . . ? C18 C19 H19B 111.0 . . ? C20 C19 H19B 111.0 . . ? H19A C19 H19B 109.0 . . ? C21 C20 C19 102.4(18) . . ? C21 C20 H20A 111.3 . . ? C19 C20 H20A 111.3 . . ? C21 C20 H20B 111.3 . . ? C19 C20 H20B 111.3 . . ? H20A C20 H20B 109.2 . . ? C22 C21 C20 99.0(16) . . ? C22 C21 H21A 112.0 . . ? C20 C21 H21A 112.0 . . ? C22 C21 H21B 112.0 . . ? C20 C21 H21B 112.0 . . ? H21A C21 H21B 109.7 . . ? C19 C20B C21B 103.2(18) . . ? C19 C20B H20C 111.1 . . ? C21B C20B H20C 111.1 . . ? C19 C20B H20D 111.1 . . ? C21B C20B H20D 111.1 . . ? H20C C20B H20D 109.1 . . ? C20B C21B C22 111(2) . . ? C20B C21B H21C 109.5 . . ? C22 C21B H21C 109.5 . . ? C20B C21B H21D 109.5 . . ? C22 C21B H21D 109.5 . . ? H21C C21B H21D 108.1 . . ? C21 C22 C18 104.8(14) . . ? C18 C22 C21B 104.5(13) . . ? C21 C22 H22A 110.8 . . ? C18 C22 H22A 110.8 . . ? C21B C22 H22A 99.8 . . ? C21 C22 H22B 110.8 . . ? C18 C22 H22B 110.8 . . ? C21B C22 H22B 121.4 . . ? H22A C22 H22B 108.9 . . ? O2 C23 C24 112.5(5) . . ? O2 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O2 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C29 C24 C25 118.7(6) . . ? C29 C24 C23 121.6(6) . . ? C25 C24 C23 119.6(6) . . ? C26 C25 C24 120.7(8) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 120.5(8) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 120.0(8) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 119.5(9) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C24 C29 C28 120.5(7) . . ? C24 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? O3 C30 C31 111.9(5) . . ? O3 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? O3 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C32 C31 C36 117.3(7) . . ? C32 C31 C30 122.3(7) . . ? C36 C31 C30 120.4(6) . . ? C31 C32 C33 122.3(9) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C32 C33 C34 119.0(9) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C35 C34 C33 119.6(9) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C36 C35 C34 119.4(9) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C31 122.4(8) . . ? C35 C36 H36 118.8 . . ? C31 C36 H36 118.8 . . ? O4 C37 C38 110.2(18) . . ? O4 C37 C38B 100.8(19) . . ? O4 C37 H37A 109.6 . . ? C38 C37 H37A 109.6 . . ? C38B C37 H37A 89.8 . . ? O4 C37 H37B 109.6 . . ? C38 C37 H37B 109.6 . . ? C38B C37 H37B 136.1 . . ? H37A C37 H37B 108.1 . . ? C37 C38 C39 90.4(19) . . ? C37 C38 H38A 113.6 . . ? C39 C38 H38A 113.6 . . ? C37 C38 H38B 113.6 . . ? C39 C38 H38B 113.6 . . ? H38A C38 H38B 110.8 . . ? C40 C39 C38 109(2) . . ? C40 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? C40 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C39B C38B C37 110(3) . . ? C39B C38B H38C 109.8 . . ? C37 C38B H38C 109.8 . . ? C39B C38B H38D 109.8 . . ? C37 C38B H38D 109.8 . . ? H38C C38B H38D 108.2 . . ? C38B C39B C40 98(2) . . ? C38B C39B H39C 112.2 . . ? C40 C39B H39C 112.2 . . ? C38B C39B H39D 112.2 . . ? C40 C39B H39D 112.2 . . ? H39C C39B H39D 109.8 . . ? O4 C40 C39B 105.3(16) . . ? O4 C40 C39 101.2(16) . . ? O4 C40 H40A 111.5 . . ? C39B C40 H40A 86.4 . . ? C39 C40 H40A 111.5 . . ? O4 C40 H40B 111.5 . . ? C39B C40 H40B 129.9 . . ? C39 C40 H40B 111.5 . . ? H40A C40 H40B 109.4 . . ? O5 C41 C42 102.8(18) . . ? O5 C41 H41A 111.2 . . ? C42 C41 H41A 111.2 . . ? O5 C41 H41B 111.2 . . ? C42 C41 H41B 111.2 . . ? H41A C41 H41B 109.1 . . ? C43 C42 C41 94.6(18) . . ? C43 C42 H42A 112.8 . . ? C41 C42 H42A 112.8 . . ? C43 C42 H42B 112.8 . . ? C41 C42 H42B 112.8 . . ? H42A C42 H42B 110.3 . . ? C42 C43 C44 108.1(19) . . ? C42 C43 H43A 110.1 . . ? C44 C43 H43A 110.1 . . ? C42 C43 H43B 110.1 . . ? C44 C43 H43B 110.1 . . ? H43A C43 H43B 108.4 . . ? O5 C44 C43 101.8(16) . . ? O5 C44 H44A 111.4 . . ? C43 C44 H44A 111.4 . . ? O5 C44 H44B 111.4 . . ? C43 C44 H44B 111.4 . . ? H44A C44 H44B 109.3 . . ? O5 C41B C42B 91.7(14) . . ? O5 C41B H41C 113.3 . . ? C42B C41B H41C 113.3 . . ? O5 C41B H41D 113.3 . . ? C42B C41B H41D 113.3 . . ? H41C C41B H41D 110.7 . . ? C41B C42B C43B 88.9(14) . . ? C41B C42B H42C 113.8 . . ? C43B C42B H42C 113.8 . . ? C41B C42B H42D 113.8 . . ? C43B C42B H42D 113.8 . . ? H42C C42B H42D 111.1 . . ? C44B C43B C42B 98.8(14) . . ? C44B C43B H43C 112.0 . . ? C42B C43B H43C 112.0 . . ? C44B C43B H43D 112.0 . . ? C42B C43B H43D 112.0 . . ? H43C C43B H43D 109.7 . . ? O5 C44B C43B 106.2(13) . . ? O5 C44B H44C 110.5 . . ? C43B C44B H44C 110.5 . . ? O5 C44B H44D 110.5 . . ? C43B C44B H44D 110.5 . . ? H44C C44B H44D 108.7 . . ? O3 Al1 O2 87.9(2) . . ? O3 Al1 N1 117.7(2) . . ? O2 Al1 N1 103.6(2) . . ? O3 Al1 N2 114.9(2) . . ? O2 Al1 N2 102.8(2) . . ? N1 Al1 N2 121.1(2) . . ? O3 Al1 O1 88.64(18) . . ? O2 Al1 O1 176.56(19) . . ? N1 Al1 O1 78.4(2) . . ? N2 Al1 O1 78.3(2) . . ? O3 Al1 Li1 43.7(3) . . ? O2 Al1 Li1 44.4(3) . . ? N1 Al1 Li1 116.2(3) . . ? N2 Al1 Li1 119.6(3) . . ? O1 Al1 Li1 132.2(3) . . ? O3 Li1 O2 81.2(5) . . ? O3 Li1 O5 127.4(7) . . ? O2 Li1 O5 112.5(6) . . ? O3 Li1 O4 104.7(6) . . ? O2 Li1 O4 128.3(7) . . ? O5 Li1 O4 103.9(6) . . ? O3 Li1 Al1 40.1(2) . . ? O2 Li1 Al1 41.3(2) . . ? O5 Li1 Al1 128.2(6) . . ? O4 Li1 Al1 127.5(6) . . ? C6 N1 C1 118.7(5) . . ? C6 N1 Al1 119.1(4) . . ? C1 N1 Al1 122.1(4) . . ? C17 N2 C18 119.3(5) . . ? C17 N2 Al1 116.0(4) . . ? C18 N2 Al1 123.3(4) . . ? C12 O1 C11 120.7(5) . . ? C12 O1 Al1 108.4(4) . . ? C11 O1 Al1 109.7(4) . . ? C23 O2 Al1 132.4(4) . . ? C23 O2 Li1 131.8(5) . . ? Al1 O2 Li1 94.3(4) . . ? C30 O3 Al1 136.4(4) . . ? C30 O3 Li1 126.5(5) . . ? Al1 O3 Li1 96.3(4) . . ? C40 O4 C37 106.8(7) . . ? C40 O4 Li1 135.3(7) . . ? C37 O4 Li1 116.7(6) . . ? C41 O5 C44B 119.4(13) . . ? C41 O5 C44 100.4(14) . . ? C44B O5 C44 52.2(12) . . ? C44B O5 C41B 101.8(10) . . ? C44 O5 C41B 110.0(11) . . ? C41 O5 Li1 124.7(11) . . ? C44B O5 Li1 114.2(9) . . ? C44 O5 Li1 123.0(9) . . ? C41B O5 Li1 126.6(8) . . ? 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 C1 C2 C3 162.1(7) . . . . ? C5 C1 C2 C3 31.0(9) . . . . ? C1 C2 C3 C4 -38.1(10) . . . . ? C2 C3 C4 C5 30.3(11) . . . . ? C3 C4 C5 C1 -10.6(11) . . . . ? N1 C1 C5 C4 -145.4(7) . . . . ? C2 C1 C5 C4 -12.6(9) . . . . ? N1 C6 C7 C8 -178.4(7) . . . . ? C11 C6 C7 C8 3.0(10) . . . . ? C6 C7 C8 C9 -1.6(13) . . . . ? C7 C8 C9 C10 -0.9(13) . . . . ? C8 C9 C10 C11 1.7(11) . . . . ? C9 C10 C11 O1 -176.6(6) . . . . ? C9 C10 C11 C6 -0.1(10) . . . . ? N1 C6 C11 C10 179.1(6) . . . . ? C7 C6 C11 C10 -2.1(9) . . . . ? N1 C6 C11 O1 -4.0(8) . . . . ? C7 C6 C11 O1 174.7(5) . . . . ? O1 C12 C13 C14 178.2(6) . . . . ? C17 C12 C13 C14 5.3(11) . . . . ? C12 C13 C14 C15 -3.3(12) . . . . ? C13 C14 C15 C16 0.6(13) . . . . ? C14 C15 C16 C17 0.5(12) . . . . ? C15 C16 C17 N2 -178.1(7) . . . . ? C15 C16 C17 C12 1.2(10) . . . . ? C13 C12 C17 N2 175.2(7) . . . . ? O1 C12 C17 N2 1.8(8) . . . . ? C13 C12 C17 C16 -4.2(10) . . . . ? O1 C12 C17 C16 -177.6(6) . . . . ? N2 C18 C19 C20B 163.0(10) . . . . ? C22 C18 C19 C20B 31.4(11) . . . . ? N2 C18 C19 C20 134.2(10) . . . . ? C22 C18 C19 C20 2.6(11) . . . . ? C20B C19 C20 C21 -74(3) . . . . ? C18 C19 C20 C21 27.2(19) . . . . ? C19 C20 C21 C22 -46(2) . . . . ? C18 C19 C20B C21B -29(2) . . . . ? C20 C19 C20B C21B 57(3) . . . . ? C19 C20B C21B C22 17(3) . . . . ? C20 C21 C22 C18 49(2) . . . . ? C20 C21 C22 C21B -41(9) . . . . ? N2 C18 C22 C21 -162.5(12) . . . . ? C19 C18 C22 C21 -32.5(13) . . . . ? N2 C18 C22 C21B -149.6(14) . . . . ? C19 C18 C22 C21B -19.6(14) . . . . ? C20B C21B C22 C21 95(12) . . . . ? C20B C21B C22 C18 2(3) . . . . ? O2 C23 C24 C29 48.6(8) . . . . ? O2 C23 C24 C25 -134.0(6) . . . . ? C29 C24 C25 C26 -1.5(10) . . . . ? C23 C24 C25 C26 -179.0(6) . . . . ? C24 C25 C26 C27 -0.4(12) . . . . ? C25 C26 C27 C28 1.1(13) . . . . ? C26 C27 C28 C29 0.2(12) . . . . ? C25 C24 C29 C28 2.7(10) . . . . ? C23 C24 C29 C28 -179.8(6) . . . . ? C27 C28 C29 C24 -2.1(12) . . . . ? O3 C30 C31 C32 115.9(7) . . . . ? O3 C30 C31 C36 -63.2(8) . . . . ? C36 C31 C32 C33 0.3(12) . . . . ? C30 C31 C32 C33 -178.8(8) . . . . ? C31 C32 C33 C34 1.1(15) . . . . ? C32 C33 C34 C35 -1.0(16) . . . . ? C33 C34 C35 C36 -0.5(16) . . . . ? C34 C35 C36 C31 1.9(15) . . . . ? C32 C31 C36 C35 -1.8(12) . . . . ? C30 C31 C36 C35 177.3(8) . . . . ? O4 C37 C38 C39 -47(2) . . . . ? C38B C37 C38 C39 28(5) . . . . ? C37 C38 C39 C40 39(3) . . . . ? O4 C37 C38B C39B 16(3) . . . . ? C38 C37 C38B C39B -98(6) . . . . ? C37 C38B C39B C40 -36(3) . . . . ? C38B C39B C40 O4 44(2) . . . . ? C38B C39B C40 C39 -40(4) . . . . ? C38 C39 C40 O4 -19(3) . . . . ? C38 C39 C40 C39B 83(6) . . . . ? O5 C41 C42 C43 52(2) . . . . ? C41 C42 C43 C44 -26(3) . . . . ? C42 C43 C44 O5 -4(3) . . . . ? O5 C41B C42B C43B -65.7(14) . . . . ? C41B C42B C43B C44B 50.2(19) . . . . ? C42B C43B C44B O5 -15(2) . . . . ? O2 Al1 Li1 O3 173.7(6) . . . . ? N1 Al1 Li1 O3 -103.6(4) . . . . ? N2 Al1 Li1 O3 96.1(4) . . . . ? O1 Al1 Li1 O3 -5.4(6) . . . . ? O3 Al1 Li1 O2 -173.7(6) . . . . ? N1 Al1 Li1 O2 82.7(4) . . . . ? N2 Al1 Li1 O2 -77.6(4) . . . . ? O1 Al1 Li1 O2 -179.1(3) . . . . ? O3 Al1 Li1 O5 105.4(8) . . . . ? O2 Al1 Li1 O5 -80.9(7) . . . . ? N1 Al1 Li1 O5 1.8(8) . . . . ? N2 Al1 Li1 O5 -158.5(6) . . . . ? O1 Al1 Li1 O5 100.0(7) . . . . ? O3 Al1 Li1 O4 -65.6(6) . . . . ? O2 Al1 Li1 O4 108.1(9) . . . . ? N1 Al1 Li1 O4 -169.3(6) . . . . ? N2 Al1 Li1 O4 30.5(8) . . . . ? O1 Al1 Li1 O4 -71.0(9) . . . . ? C7 C6 N1 C1 -6.1(9) . . . . ? C11 C6 N1 C1 172.4(5) . . . . ? C7 C6 N1 Al1 171.1(5) . . . . ? C11 C6 N1 Al1 -10.3(7) . . . . ? C2 C1 N1 C6 -58.8(8) . . . . ? C5 C1 N1 C6 66.8(7) . . . . ? C2 C1 N1 Al1 124.1(6) . . . . ? C5 C1 N1 Al1 -110.4(6) . . . . ? O3 Al1 N1 C6 96.0(5) . . . . ? O2 Al1 N1 C6 -169.1(4) . . . . ? N2 Al1 N1 C6 -54.8(5) . . . . ? O1 Al1 N1 C6 13.8(4) . . . . ? Li1 Al1 N1 C6 145.3(5) . . . . ? O3 Al1 N1 C1 -86.8(5) . . . . ? O2 Al1 N1 C1 8.0(5) . . . . ? N2 Al1 N1 C1 122.4(5) . . . . ? O1 Al1 N1 C1 -169.1(5) . . . . ? Li1 Al1 N1 C1 -37.6(6) . . . . ? C16 C17 N2 C18 -11.3(10) . . . . ? C12 C17 N2 C18 169.4(6) . . . . ? C16 C17 N2 Al1 155.4(6) . . . . ? C12 C17 N2 Al1 -23.9(7) . . . . ? C22 C18 N2 C17 71.9(8) . . . . ? C19 C18 N2 C17 -52.7(8) . . . . ? C22 C18 N2 Al1 -93.8(6) . . . . ? C19 C18 N2 Al1 141.6(5) . . . . ? O3 Al1 N2 C17 -57.7(5) . . . . ? O2 Al1 N2 C17 -151.4(5) . . . . ? N1 Al1 N2 C17 93.8(5) . . . . ? O1 Al1 N2 C17 25.2(5) . . . . ? Li1 Al1 N2 C17 -106.9(5) . . . . ? O3 Al1 N2 C18 108.4(5) . . . . ? O2 Al1 N2 C18 14.7(5) . . . . ? N1 Al1 N2 C18 -100.0(5) . . . . ? O1 Al1 N2 C18 -168.6(5) . . . . ? Li1 Al1 N2 C18 59.2(6) . . . . ? C13 C12 O1 C11 75.8(8) . . . . ? C17 C12 O1 C11 -110.6(6) . . . . ? C13 C12 O1 Al1 -156.5(6) . . . . ? C17 C12 O1 Al1 17.1(6) . . . . ? C10 C11 O1 C12 -42.2(8) . . . . ? C6 C11 O1 C12 140.9(6) . . . . ? C10 C11 O1 Al1 -169.3(5) . . . . ? C6 C11 O1 Al1 13.9(6) . . . . ? O3 Al1 O1 C12 92.7(4) . . . . ? N1 Al1 O1 C12 -148.7(4) . . . . ? N2 Al1 O1 C12 -23.1(4) . . . . ? Li1 Al1 O1 C12 96.4(5) . . . . ? O3 Al1 O1 C11 -133.6(4) . . . . ? N1 Al1 O1 C11 -15.0(4) . . . . ? N2 Al1 O1 C11 110.6(4) . . . . ? Li1 Al1 O1 C11 -129.9(5) . . . . ? C24 C23 O2 Al1 128.4(5) . . . . ? C24 C23 O2 Li1 -69.9(8) . . . . ? O3 Al1 O2 C23 170.7(5) . . . . ? N1 Al1 O2 C23 52.7(5) . . . . ? N2 Al1 O2 C23 -74.2(5) . . . . ? Li1 Al1 O2 C23 166.4(6) . . . . ? O3 Al1 O2 Li1 4.3(4) . . . . ? N1 Al1 O2 Li1 -113.7(4) . . . . ? N2 Al1 O2 Li1 119.4(4) . . . . ? O3 Li1 O2 C23 -170.6(4) . . . . ? O5 Li1 O2 C23 -43.6(10) . . . . ? O4 Li1 O2 C23 87.5(9) . . . . ? Al1 Li1 O2 C23 -166.5(6) . . . . ? O3 Li1 O2 Al1 -4.1(4) . . . . ? O5 Li1 O2 Al1 122.9(6) . . . . ? O4 Li1 O2 Al1 -106.0(7) . . . . ? C31 C30 O3 Al1 106.8(6) . . . . ? C31 C30 O3 Li1 -59.9(8) . . . . ? O2 Al1 O3 C30 -173.7(5) . . . . ? N1 Al1 O3 C30 -69.5(6) . . . . ? N2 Al1 O3 C30 83.1(6) . . . . ? O1 Al1 O3 C30 6.7(5) . . . . ? Li1 Al1 O3 C30 -169.3(8) . . . . ? O2 Al1 O3 Li1 -4.4(4) . . . . ? N1 Al1 O3 Li1 99.9(5) . . . . ? N2 Al1 O3 Li1 -107.5(5) . . . . ? O1 Al1 O3 Li1 176.0(5) . . . . ? O2 Li1 O3 C30 175.1(5) . . . . ? O5 Li1 O3 C30 63.4(10) . . . . ? O4 Li1 O3 C30 -57.5(9) . . . . ? Al1 Li1 O3 C30 170.9(6) . . . . ? O2 Li1 O3 Al1 4.2(4) . . . . ? O5 Li1 O3 Al1 -107.5(7) . . . . ? O4 Li1 O3 Al1 131.6(5) . . . . ? C39B C40 O4 C37 -36.8(16) . . . . ? C39 C40 O4 C37 -10.2(16) . . . . ? C39B C40 O4 Li1 130.0(14) . . . . ? C39 C40 O4 Li1 156.6(14) . . . . ? C38 C37 O4 C40 40.4(16) . . . . ? C38B C37 O4 C40 13.3(17) . . . . ? C38 C37 O4 Li1 -129.3(14) . . . . ? C38B C37 O4 Li1 -156.3(15) . . . . ? O3 Li1 O4 C40 159.8(9) . . . . ? O2 Li1 O4 C40 -109.8(11) . . . . ? O5 Li1 O4 C40 24.4(13) . . . . ? Al1 Li1 O4 C40 -162.9(9) . . . . ? O3 Li1 O4 C37 -34.4(10) . . . . ? O2 Li1 O4 C37 56.0(10) . . . . ? O5 Li1 O4 C37 -169.8(7) . . . . ? Al1 Li1 O4 C37 3.0(11) . . . . ? C42 C41 O5 C44B -4(3) . . . . ? C42 C41 O5 C44 -56(2) . . . . ? C42 C41 O5 C41B 56(2) . . . . ? C42 C41 O5 Li1 160.2(13) . . . . ? C43B C44B O5 C41 -2(3) . . . . ? C43B C44B O5 C44 78(2) . . . . ? C43B C44B O5 C41B -29(2) . . . . ? C43B C44B O5 Li1 -168.2(14) . . . . ? C43 C44 O5 C41 38(2) . . . . ? C43 C44 O5 C44B -81.7(18) . . . . ? C43 C44 O5 C41B 8(2) . . . . ? C43 C44 O5 Li1 -178.2(12) . . . . ? C42B C41B O5 C41 -67(3) . . . . ? C42B C41B O5 C44B 62.4(17) . . . . ? C42B C41B O5 C44 9(2) . . . . ? C42B C41B O5 Li1 -164.9(12) . . . . ? O3 Li1 O5 C41 -118.4(15) . . . . ? O2 Li1 O5 C41 145.3(14) . . . . ? O4 Li1 O5 C41 2.8(16) . . . . ? Al1 Li1 O5 C41 -169.8(14) . . . . ? O3 Li1 O5 C44B 46.7(14) . . . . ? O2 Li1 O5 C44B -49.6(13) . . . . ? O4 Li1 O5 C44B 168.0(11) . . . . ? Al1 Li1 O5 C44B -4.7(13) . . . . ? O3 Li1 O5 C44 106.0(14) . . . . ? O2 Li1 O5 C44 9.8(15) . . . . ? O4 Li1 O5 C44 -132.7(13) . . . . ? Al1 Li1 O5 C44 54.6(15) . . . . ? O3 Li1 O5 C41B -81.2(14) . . . . ? O2 Li1 O5 C41B -177.4(12) . . . . ? O4 Li1 O5 C41B 40.1(14) . . . . ? Al1 Li1 O5 C41B -132.6(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.675 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.121