# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2224 data_rs9904 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H54 Al2 Li2 N2 O5' _chemical_formula_weight 650.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.333(3) _cell_length_b 13.439(3) _cell_length_c 14.021(4) _cell_angle_alpha 109.870(10) _cell_angle_beta 91.58(2) _cell_angle_gamma 114.210(10) _cell_volume 1955.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5103 _exptl_absorpt_correction_T_max 0.8294 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8243 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.01 _diffrn_reflns_theta_max 54.98 _reflns_number_total 4837 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+2.0047P] 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 4837 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1766 _refine_ls_wR_factor_gt 0.1707 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.075 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.26639(9) 0.20043(10) 0.70076(8) 0.0520(3) Uani 1 1 d . . . O1 O 0.49060(18) 0.37132(17) 0.62885(16) 0.0398(5) Uani 1 1 d . . . N1 N 0.4407(3) 0.2549(3) 0.7199(2) 0.0545(8) Uani 1 1 d . . . Li1 Li 0.3494(5) 0.2809(5) 0.5177(4) 0.0427(13) Uani 1 1 d . . . C1 C 0.3326(5) 0.4162(5) 0.8867(5) 0.111(2) Uani 1 1 d . . . H1A H 0.3103 0.4574 0.9493 0.166 Uiso 1 1 calc R . . H1B H 0.3443 0.4586 0.8402 0.166 Uiso 1 1 calc R . . H1C H 0.4081 0.4132 0.9055 0.166 Uiso 1 1 calc R . . Al2 Al 0.26926(8) 0.23800(8) 0.29425(7) 0.0399(3) Uani 1 1 d . . . O2 O 0.37746(16) 0.43110(16) 0.49282(15) 0.0332(5) Uani 1 1 d . . . N2 N 0.1997(2) 0.3317(2) 0.3825(2) 0.0387(6) Uani 1 1 d . . . C2 C 0.1175(5) 0.3034(7) 0.8091(5) 0.113(2) Uani 1 1 d . . . H2A H 0.1018 0.3491 0.8734 0.169 Uiso 1 1 calc R . . H2B H 0.0487 0.2246 0.7774 0.169 Uiso 1 1 calc R . . H2C H 0.1285 0.3441 0.7613 0.169 Uiso 1 1 calc R . . Li2 Li 0.5169(4) 0.5147(4) 0.6071(4) 0.0385(12) Uani 1 1 d . . . C3 C 0.2095(6) 0.2282(6) 0.9086(4) 0.111(2) Uani 1 1 d . . . H3A H 0.1823 0.2697 0.9675 0.167 Uiso 1 1 calc R . . H3B H 0.2846 0.2283 0.9333 0.167 Uiso 1 1 calc R . . H3C H 0.1469 0.1465 0.8734 0.167 Uiso 1 1 calc R . . O3 O 0.3130(2) 0.17845(18) 0.37336(16) 0.0452(6) Uani 1 1 d . . . C4 C 0.2324(4) 0.2914(4) 0.8326(3) 0.0665(11) Uani 1 1 d . . . O4 O 0.22801(18) 0.2315(2) 0.59479(17) 0.0499(6) Uani 1 1 d . . . C5 C 0.1916(4) 0.0271(4) 0.6634(4) 0.0858(15) Uani 1 1 d . . . H5A H 0.2343 0.0091 0.7102 0.129 Uiso 1 1 calc R . . H5B H 0.1974 -0.0122 0.5921 0.129 Uiso 1 1 calc R . . H5C H 0.1062 -0.0011 0.6695 0.129 Uiso 1 1 calc R . . O5 O 0.39938(18) 0.34399(18) 0.27403(15) 0.0413(5) Uani 1 1 d . . . C6 C 0.4831(4) 0.2126(5) 0.7906(4) 0.0918(17) Uani 1 1 d . . . H6A H 0.5602 0.2756 0.8354 0.138 Uiso 1 1 calc R . . H6B H 0.4947 0.1435 0.7502 0.138 Uiso 1 1 calc R . . H6C H 0.4227 0.1908 0.8331 0.138 Uiso 1 1 calc R . . C7 C 0.5210(3) 0.3311(3) 0.6886(2) 0.0409(8) Uani 1 1 d . . . C8 C 0.6546(3) 0.3714(3) 0.7212(3) 0.0446(8) Uani 1 1 d . . . C9 C 0.7067(3) 0.2961(4) 0.6830(3) 0.0614(10) Uani 1 1 d . . . H9A H 0.6577 0.2164 0.6374 0.074 Uiso 1 1 calc R . . C10 C 0.8322(4) 0.3374(5) 0.7118(4) 0.0786(14) Uani 1 1 d . . . H10A H 0.8688 0.2865 0.6850 0.094 Uiso 1 1 calc R . . C11 C 0.9015(4) 0.4524(5) 0.7793(4) 0.0828(15) Uani 1 1 d . . . H11A H 0.9861 0.4802 0.8000 0.099 Uiso 1 1 calc R . . C12 C 0.8506(4) 0.5264(4) 0.8165(4) 0.0757(13) Uani 1 1 d . . . H12A H 0.8997 0.6055 0.8632 0.091 Uiso 1 1 calc R . . C13 C 0.7277(3) 0.4875(3) 0.7869(3) 0.0575(10) Uani 1 1 d . . . H13A H 0.6931 0.5406 0.8117 0.069 Uiso 1 1 calc R . . C14 C 0.1047(3) 0.1756(4) 0.5427(3) 0.0702(12) Uani 1 1 d . . . H14A H 0.0546 0.1200 0.5723 0.105 Uiso 1 1 calc R . . H14B H 0.0987 0.1328 0.4690 0.105 Uiso 1 1 calc R . . H14C H 0.0762 0.2357 0.5509 0.105 Uiso 1 1 calc R . . C15 C 0.4128(6) 0.0821(5) 0.2528(4) 0.0958(16) Uani 1 1 d . . . H15A H 0.4899 0.1541 0.2762 0.144 Uiso 1 1 calc R . . H15B H 0.3637 0.0802 0.1955 0.144 Uiso 1 1 calc R . . H15C H 0.4285 0.0126 0.2296 0.144 Uiso 1 1 calc R . . C16 C 0.4200(6) 0.0915(5) 0.4335(4) 0.0953(17) Uani 1 1 d . . . H16A H 0.3737 0.0882 0.4890 0.143 Uiso 1 1 calc R . . H16B H 0.4935 0.1669 0.4578 0.143 Uiso 1 1 calc R . . H16C H 0.4423 0.0262 0.4134 0.143 Uiso 1 1 calc R . . C17 C 0.3443(4) 0.0811(3) 0.3424(3) 0.0581(10) Uani 1 1 d . . . C18 C 0.2266(6) -0.0331(4) 0.3043(5) 0.108(2) Uani 1 1 d . . . H18A H 0.1827 -0.0369 0.3612 0.161 Uiso 1 1 calc R . . H18B H 0.2450 -0.1009 0.2796 0.161 Uiso 1 1 calc R . . H18C H 0.1764 -0.0350 0.2477 0.161 Uiso 1 1 calc R . . C19 C 0.1478(4) 0.1293(3) 0.1675(3) 0.0643(11) Uani 1 1 d . . . H19A H 0.1217 0.1742 0.1380 0.096 Uiso 1 1 calc R . . H19B H 0.0778 0.0728 0.1835 0.096 Uiso 1 1 calc R . . H19C H 0.1830 0.0864 0.1175 0.096 Uiso 1 1 calc R . . C20 C 0.0729(3) 0.3082(3) 0.3562(3) 0.0519(9) Uani 1 1 d . . . H20A H 0.0505 0.3531 0.4167 0.078 Uiso 1 1 calc R . . H20B H 0.0199 0.2236 0.3353 0.078 Uiso 1 1 calc R . . H20C H 0.0638 0.3324 0.2991 0.078 Uiso 1 1 calc R . . C21 C 0.2697(3) 0.4187(3) 0.4682(2) 0.0347(7) Uani 1 1 d . . . C22 C 0.2363(3) 0.5068(3) 0.5403(2) 0.0411(8) Uani 1 1 d . . . C23 C 0.2387(3) 0.5185(4) 0.6422(3) 0.0575(10) Uani 1 1 d . . . H23A H 0.2550 0.4658 0.6644 0.069 Uiso 1 1 calc R . . C24 C 0.2176(4) 0.6059(5) 0.7115(3) 0.0767(14) Uani 1 1 d . . . H24A H 0.2172 0.6124 0.7811 0.092 Uiso 1 1 calc R . . C25 C 0.1969(4) 0.6847(5) 0.6798(4) 0.0806(15) Uani 1 1 d . . . H25A H 0.1842 0.7464 0.7282 0.097 Uiso 1 1 calc R . . C26 C 0.1946(4) 0.6741(4) 0.5796(4) 0.0769(13) Uani 1 1 d . . . H26A H 0.1812 0.7289 0.5584 0.092 Uiso 1 1 calc R . . C27 C 0.2120(3) 0.5835(3) 0.5084(3) 0.0583(10) Uani 1 1 d . . . H27A H 0.2071 0.5741 0.4379 0.070 Uiso 1 1 calc R . . C28 C 0.4438(4) 0.3254(4) 0.1810(3) 0.0600(10) Uani 1 1 d . . . H28A H 0.4676 0.3957 0.1643 0.090 Uiso 1 1 calc R . . H28B H 0.3804 0.2570 0.1250 0.090 Uiso 1 1 calc R . . H28C H 0.5144 0.3107 0.1892 0.090 Uiso 1 1 calc R . . C100 C 0.2734(9) 0.9662(6) -0.0796(5) 0.162(4) Uani 1 1 d . . . H10B H 0.1938 0.9591 -0.1022 0.243 Uiso 1 1 calc R . . H10C H 0.3159 0.9590 -0.1377 0.243 Uiso 1 1 calc R . . H10D H 0.3209 1.0433 -0.0234 0.243 Uiso 1 1 calc R . . C101 C 0.2585(8) 0.8765(5) -0.0447(4) 0.114(2) Uani 1 1 d . . . C102 C 0.3517(6) 0.8425(6) -0.0422(4) 0.0985(18) Uani 1 1 d . . . H10E H 0.4238 0.8809 -0.0645 0.118 Uiso 1 1 calc R . . C103 C 0.3413(5) 0.7601(6) -0.0103(4) 0.1012(18) Uani 1 1 d . . . H10F H 0.4066 0.7401 -0.0091 0.121 Uiso 1 1 calc R . . C104 C 0.2347(7) 0.6977(6) 0.0235(4) 0.1052(19) Uani 1 1 d . . . H10G H 0.2273 0.6362 0.0458 0.126 Uiso 1 1 calc R . . C105 C 0.1489(6) 0.7297(7) 0.0220(4) 0.114(2) Uani 1 1 d . . . H10H H 0.0782 0.6911 0.0457 0.137 Uiso 1 1 calc R . . C106 C 0.1540(5) 0.8201(5) -0.0134(4) 0.0830(14) Uani 1 1 d . . . H10J H 0.0883 0.8396 -0.0151 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0367(6) 0.0564(7) 0.0560(7) 0.0343(5) -0.0012(5) 0.0050(5) O1 0.0345(12) 0.0337(11) 0.0465(13) 0.0203(10) -0.0061(9) 0.0077(9) N1 0.0402(16) 0.0645(19) 0.0628(19) 0.0429(17) 0.0007(14) 0.0129(15) Li1 0.039(3) 0.038(3) 0.041(3) 0.020(2) -0.004(2) 0.005(2) C1 0.108(4) 0.078(4) 0.108(4) 0.017(3) 0.029(3) 0.021(3) Al2 0.0368(5) 0.0315(5) 0.0386(5) 0.0108(4) -0.0064(4) 0.0065(4) O2 0.0241(11) 0.0334(11) 0.0389(12) 0.0159(9) -0.0015(9) 0.0088(9) N2 0.0266(13) 0.0388(15) 0.0457(16) 0.0192(13) -0.0024(12) 0.0083(12) C2 0.100(4) 0.168(6) 0.114(4) 0.076(4) 0.047(4) 0.081(4) Li2 0.031(3) 0.035(3) 0.040(3) 0.016(2) -0.003(2) 0.006(2) C3 0.154(6) 0.122(5) 0.076(3) 0.059(3) 0.043(4) 0.060(4) O3 0.0514(13) 0.0300(12) 0.0448(13) 0.0120(10) -0.0045(10) 0.0124(10) C4 0.054(2) 0.077(3) 0.066(3) 0.038(2) 0.0119(19) 0.018(2) O4 0.0304(12) 0.0549(14) 0.0548(14) 0.0311(12) -0.0053(10) 0.0031(10) C5 0.083(3) 0.068(3) 0.089(3) 0.047(3) -0.008(3) 0.006(2) O5 0.0390(12) 0.0383(12) 0.0360(12) 0.0131(10) 0.0022(9) 0.0089(10) C6 0.056(3) 0.138(4) 0.117(4) 0.104(4) 0.011(3) 0.032(3) C7 0.0381(18) 0.0383(18) 0.0408(18) 0.0156(15) -0.0038(14) 0.0122(15) C8 0.0380(18) 0.045(2) 0.055(2) 0.0296(17) -0.0005(15) 0.0141(16) C9 0.052(2) 0.057(2) 0.085(3) 0.041(2) 0.006(2) 0.022(2) C10 0.058(3) 0.094(4) 0.126(4) 0.071(3) 0.023(3) 0.049(3) C11 0.038(2) 0.090(4) 0.133(4) 0.076(3) -0.002(2) 0.015(3) C12 0.047(2) 0.065(3) 0.102(3) 0.043(3) -0.019(2) 0.006(2) C13 0.047(2) 0.053(2) 0.067(2) 0.027(2) -0.0093(18) 0.0148(18) C14 0.036(2) 0.077(3) 0.080(3) 0.046(2) -0.0119(19) -0.0022(19) C15 0.137(5) 0.097(4) 0.079(3) 0.030(3) 0.024(3) 0.078(4) C16 0.149(5) 0.079(3) 0.075(3) 0.017(3) -0.010(3) 0.078(4) C17 0.077(3) 0.037(2) 0.058(2) 0.0159(17) 0.0003(19) 0.0267(19) C18 0.132(5) 0.040(2) 0.117(4) 0.018(3) -0.020(4) 0.020(3) C19 0.058(2) 0.054(2) 0.053(2) 0.0104(18) -0.0134(18) 0.0088(19) C20 0.0269(17) 0.061(2) 0.059(2) 0.0244(18) -0.0045(15) 0.0118(16) C21 0.0287(17) 0.0362(17) 0.0393(18) 0.0210(15) 0.0029(14) 0.0095(14) C22 0.0245(16) 0.0458(19) 0.048(2) 0.0159(16) 0.0047(13) 0.0126(14) C23 0.047(2) 0.073(3) 0.048(2) 0.019(2) 0.0046(17) 0.025(2) C24 0.054(3) 0.107(4) 0.051(2) 0.010(3) 0.0074(19) 0.036(3) C25 0.054(3) 0.089(3) 0.076(3) -0.004(3) 0.006(2) 0.040(2) C26 0.065(3) 0.072(3) 0.107(4) 0.031(3) 0.020(3) 0.046(2) C27 0.056(2) 0.065(2) 0.070(3) 0.032(2) 0.0208(19) 0.036(2) C28 0.064(2) 0.061(2) 0.045(2) 0.0156(18) 0.0117(18) 0.022(2) C100 0.293(11) 0.088(4) 0.071(4) 0.008(3) -0.008(5) 0.076(6) C101 0.170(7) 0.078(4) 0.051(3) 0.011(3) -0.010(3) 0.028(4) C102 0.103(4) 0.129(5) 0.061(3) 0.015(3) -0.003(3) 0.068(4) C103 0.091(4) 0.146(6) 0.065(3) 0.044(4) 0.016(3) 0.048(4) C104 0.134(5) 0.105(4) 0.066(3) 0.023(3) -0.008(3) 0.053(4) C105 0.093(4) 0.128(6) 0.073(4) 0.000(4) -0.016(3) 0.040(4) C106 0.084(4) 0.080(3) 0.060(3) 0.006(3) -0.004(2) 0.032(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O4 1.775(2) . ? Al1 N1 1.943(3) . ? Al1 C5 1.983(5) . ? Al1 C4 2.003(5) . ? Al1 Li1 3.151(5) . ? O1 C7 1.262(4) . ? O1 Li1 1.940(5) . ? O1 Li2 1.950(5) . ? N1 C7 1.312(4) . ? N1 C6 1.475(5) . ? Li1 O4 1.900(6) . ? Li1 O3 1.935(6) . ? Li1 O2 2.056(6) . ? Li1 C21 2.685(6) . ? Li1 Li2 2.750(7) . ? Li1 Al2 3.043(5) . ? C1 C4 1.517(7) . ? Al2 O3 1.757(2) . ? Al2 O5 1.763(2) . ? Al2 N2 1.934(3) . ? Al2 C19 1.957(4) . ? Al2 Li2 3.066(5) 2_666 ? O2 C21 1.291(3) . ? O2 Li2 1.957(5) . ? O2 Li2 2.051(5) 2_666 ? N2 C21 1.310(4) . ? N2 C20 1.471(4) . ? C2 C4 1.529(7) . ? Li2 O5 1.896(5) 2_666 ? Li2 O2 2.051(5) 2_666 ? Li2 C21 2.776(6) 2_666 ? Li2 Li2 2.889(10) 2_666 ? Li2 Al2 3.066(5) 2_666 ? C3 C4 1.540(6) . ? O3 C17 1.444(4) . ? O4 C14 1.428(4) . ? O5 C28 1.412(4) . ? O5 Li2 1.896(5) 2_666 ? C7 C8 1.508(5) . ? C8 C9 1.381(5) . ? C8 C13 1.384(5) . ? C9 C10 1.406(6) . ? C10 C11 1.375(7) . ? C11 C12 1.354(7) . ? C12 C13 1.383(6) . ? C15 C17 1.534(6) . ? C16 C17 1.492(6) . ? C17 C18 1.524(6) . ? C21 C22 1.485(5) . ? C21 Li2 2.776(6) 2_666 ? C22 C23 1.381(5) . ? C22 C27 1.383(5) . ? C23 C24 1.371(6) . ? C24 C25 1.386(7) . ? C25 C26 1.362(7) . ? C26 C27 1.387(6) . ? C100 C101 1.397(8) . ? C101 C106 1.372(8) . ? C101 C102 1.404(9) . ? C102 C103 1.292(8) . ? C103 C104 1.433(8) . ? C104 C105 1.299(8) . ? C105 C106 1.439(9) . ? 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 O4 Al1 N1 105.38(12) . . ? O4 Al1 C5 109.92(17) . . ? N1 Al1 C5 106.85(19) . . ? O4 Al1 C4 112.59(16) . . ? N1 Al1 C4 107.03(16) . . ? C5 Al1 C4 114.5(2) . . ? O4 Al1 Li1 32.20(12) . . ? N1 Al1 Li1 73.62(13) . . ? C5 Al1 Li1 114.81(18) . . ? C4 Al1 Li1 127.86(17) . . ? C7 O1 Li1 124.5(2) . . ? C7 O1 Li2 144.7(2) . . ? Li1 O1 Li2 90.0(2) . . ? C7 N1 C6 119.0(3) . . ? C7 N1 Al1 128.8(2) . . ? C6 N1 Al1 111.8(2) . . ? O4 Li1 O3 115.6(3) . . ? O4 Li1 O1 99.3(2) . . ? O3 Li1 O1 136.4(3) . . ? O4 Li1 O2 116.5(3) . . ? O3 Li1 O2 96.1(2) . . ? O1 Li1 O2 90.4(2) . . ? O4 Li1 C21 95.3(2) . . ? O3 Li1 C21 90.3(2) . . ? O1 Li1 C21 112.5(2) . . ? O2 Li1 C21 27.78(11) . . ? O4 Li1 Li2 115.1(3) . . ? O3 Li1 Li2 126.5(3) . . ? O1 Li1 Li2 45.14(16) . . ? O2 Li1 Li2 45.25(15) . . ? C21 Li1 Li2 69.06(18) . . ? O4 Li1 Al2 118.3(2) . . ? O3 Li1 Al2 32.62(11) . . ? O1 Li1 Al2 141.3(2) . . ? O2 Li1 Al2 65.55(14) . . ? C21 Li1 Al2 57.98(12) . . ? Li2 Li1 Al2 105.35(19) . . ? O4 Li1 Al1 29.85(11) . . ? O3 Li1 Al1 126.1(2) . . ? O1 Li1 Al1 74.66(16) . . ? O2 Li1 Al1 132.2(3) . . ? C21 Li1 Al1 120.2(2) . . ? Li2 Li1 Al1 106.43(19) . . ? Al2 Li1 Al1 143.95(18) . . ? O3 Al2 O5 109.53(11) . . ? O3 Al2 N2 103.46(11) . . ? O5 Al2 N2 103.58(11) . . ? O3 Al2 C19 118.46(15) . . ? O5 Al2 C19 113.18(15) . . ? N2 Al2 C19 107.04(16) . . ? O3 Al2 Li1 36.42(13) . . ? O5 Al2 Li1 101.06(12) . . ? N2 Al2 Li1 71.14(14) . . ? C19 Al2 Li1 144.74(16) . . ? O3 Al2 Li2 95.88(12) . 2_666 ? O5 Al2 Li2 34.48(12) . 2_666 ? N2 Al2 Li2 76.39(13) . 2_666 ? C19 Al2 Li2 142.52(16) . 2_666 ? Li1 Al2 Li2 72.48(13) . 2_666 ? C21 O2 Li2 142.3(2) . . ? C21 O2 Li2 110.2(2) . 2_666 ? Li2 O2 Li2 92.2(2) . 2_666 ? C21 O2 Li1 104.3(2) . . ? Li2 O2 Li1 86.5(2) . . ? Li2 O2 Li1 123.1(2) 2_666 . ? C21 N2 C20 120.0(3) . . ? C21 N2 Al2 117.6(2) . . ? C20 N2 Al2 122.3(2) . . ? O5 Li2 O1 114.3(3) 2_666 . ? O5 Li2 O2 143.1(3) 2_666 . ? O1 Li2 O2 93.1(2) . . ? O5 Li2 O2 96.8(2) 2_666 2_666 ? O1 Li2 O2 122.4(3) . 2_666 ? O2 Li2 O2 87.8(2) . 2_666 ? O5 Li2 Li1 150.3(3) 2_666 . ? O1 Li2 Li1 44.85(16) . . ? O2 Li2 Li1 48.27(16) . . ? O2 Li2 Li1 112.4(2) 2_666 . ? O5 Li2 C21 86.60(19) 2_666 2_666 ? O1 Li2 C21 106.3(2) . 2_666 ? O2 Li2 C21 109.9(2) . 2_666 ? O2 Li2 C21 25.88(10) 2_666 2_666 ? Li1 Li2 C21 117.2(2) . 2_666 ? O5 Li2 Li2 128.7(3) 2_666 2_666 ? O1 Li2 Li2 114.7(3) . 2_666 ? O2 Li2 Li2 45.19(14) . 2_666 ? O2 Li2 Li2 42.60(14) 2_666 2_666 ? Li1 Li2 Li2 79.6(2) . 2_666 ? C21 Li2 Li2 65.88(19) 2_666 2_666 ? O5 Li2 Al2 31.77(10) 2_666 2_666 ? O1 Li2 Al2 129.0(2) . 2_666 ? O2 Li2 Al2 137.2(2) . 2_666 ? O2 Li2 Al2 65.10(14) 2_666 2_666 ? Li1 Li2 Al2 171.8(2) . 2_666 ? C21 Li2 Al2 56.89(11) 2_666 2_666 ? Li2 Li2 Al2 101.4(2) 2_666 2_666 ? C17 O3 Al2 127.9(2) . . ? C17 O3 Li1 120.0(3) . . ? Al2 O3 Li1 110.95(19) . . ? C1 C4 C2 106.3(5) . . ? C1 C4 C3 109.0(4) . . ? C2 C4 C3 106.7(4) . . ? C1 C4 Al1 112.8(3) . . ? C2 C4 Al1 109.5(3) . . ? C3 C4 Al1 112.2(3) . . ? C14 O4 Al1 119.8(2) . . ? C14 O4 Li1 117.1(3) . . ? Al1 O4 Li1 118.0(2) . . ? C28 O5 Al2 124.4(2) . . ? C28 O5 Li2 121.7(3) . 2_666 ? Al2 O5 Li2 113.76(19) . 2_666 ? O1 C7 N1 122.0(3) . . ? O1 C7 C8 117.4(3) . . ? N1 C7 C8 120.5(3) . . ? C9 C8 C13 119.2(3) . . ? C9 C8 C7 121.2(3) . . ? C13 C8 C7 119.6(3) . . ? C8 C9 C10 119.9(4) . . ? C11 C10 C9 119.4(4) . . ? C12 C11 C10 120.8(4) . . ? C11 C12 C13 120.3(4) . . ? C12 C13 C8 120.4(4) . . ? O3 C17 C16 108.6(3) . . ? O3 C17 C18 107.7(4) . . ? C16 C17 C18 111.2(4) . . ? O3 C17 C15 110.4(3) . . ? C16 C17 C15 110.7(4) . . ? C18 C17 C15 108.1(4) . . ? O2 C21 N2 118.4(3) . . ? O2 C21 C22 116.2(3) . . ? N2 C21 C22 125.4(3) . . ? O2 C21 Li1 47.92(17) . . ? N2 C21 Li1 92.2(2) . . ? C22 C21 Li1 126.1(2) . . ? O2 C21 Li2 43.91(16) . 2_666 ? N2 C21 Li2 97.3(2) . 2_666 ? C22 C21 Li2 122.1(2) . 2_666 ? Li1 C21 Li2 82.80(18) . 2_666 ? C23 C22 C27 119.6(3) . . ? C23 C22 C21 119.8(3) . . ? C27 C22 C21 120.4(3) . . ? C24 C23 C22 120.3(4) . . ? C23 C24 C25 119.8(4) . . ? C26 C25 C24 120.4(4) . . ? C25 C26 C27 120.0(4) . . ? C22 C27 C26 119.9(4) . . ? C106 C101 C100 121.3(8) . . ? C106 C101 C102 119.3(6) . . ? C100 C101 C102 119.4(8) . . ? C103 C102 C101 121.2(7) . . ? C102 C103 C104 122.5(7) . . ? C105 C104 C103 116.3(7) . . ? C104 C105 C106 124.2(7) . . ? C101 C106 C105 116.6(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 54.99 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.691 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.054 data_rs9944 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common rs9944 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H50 Al2 Li2 N2 O2' _chemical_formula_weight 634.64 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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 33.1340(16) _cell_length_b 33.1340(16) _cell_length_c 14.4150(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15825.7(12) _cell_formula_units_Z 16 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 12909 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5440 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9723 _exptl_absorpt_correction_T_max 0.9723 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12299 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6920 _reflns_number_gt 3900 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1388P)^2^+36.4875P] 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 6920 _refine_ls_number_parameters 484 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1574 _refine_ls_R_factor_gt 0.0926 _refine_ls_wR_factor_ref 0.2922 _refine_ls_wR_factor_gt 0.2474 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.040 _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 Al1 Al 0.28120(4) 0.11814(5) 0.65476(9) 0.0548(5) Uani 1 1 d . B . O1 O 0.35766(9) 0.15683(9) 0.58995(19) 0.0480(8) Uani 1 1 d . B . N1 N 0.32542(11) 0.14486(11) 0.7243(2) 0.0439(9) Uani 1 1 d . B . C1 C 0.25517(15) 0.1602(2) 0.5737(4) 0.0702(16) Uani 1 1 d D . . Li1 Li 0.3326(3) 0.1225(3) 0.5019(5) 0.063(2) Uani 1 1 d . . . Al2 Al 0.46613(4) 0.12489(5) 0.40421(10) 0.0552(5) Uani 1 1 d . . . O2 O 0.37527(12) 0.13074(12) 0.4218(2) 0.0735(11) Uani 1 1 d . B . N2 N 0.42121(14) 0.11655(14) 0.3118(3) 0.0648(12) Uani 1 1 d . B . Li2 Li 0.3967(3) 0.1728(2) 0.4996(5) 0.0536(19) Uani 1 1 d . B . C5 C 0.24430(17) 0.0948(2) 0.7467(4) 0.0801(18) Uani 1 1 d . . . H5A H 0.2303 0.1166 0.7796 0.120 Uiso 1 1 calc R B . H5B H 0.2597 0.0786 0.7912 0.120 Uiso 1 1 calc R . . H5C H 0.2245 0.0777 0.7152 0.120 Uiso 1 1 calc R . . C6 C 0.3065(2) 0.07211(18) 0.5819(4) 0.0824(18) Uani 1 1 d . . . H6A H 0.3059 0.0474 0.6193 0.124 Uiso 1 1 calc R B . H6B H 0.3346 0.0789 0.5670 0.124 Uiso 1 1 calc R . . H6C H 0.2914 0.0679 0.5244 0.124 Uiso 1 1 calc R . . C7 C 0.32260(13) 0.15268(14) 0.8229(3) 0.0443(11) Uani 1 1 d . . . C8 C 0.31804(17) 0.19157(15) 0.8551(3) 0.0621(14) Uani 1 1 d . . . H8A H 0.3173 0.2136 0.8130 0.075 Uiso 1 1 calc R . . C9 C 0.31450(19) 0.19819(18) 0.9501(4) 0.0754(17) Uani 1 1 d . . . H9A H 0.3122 0.2250 0.9728 0.090 Uiso 1 1 calc R . . C10 C 0.31426(19) 0.16680(19) 1.0105(4) 0.0748(17) Uani 1 1 d . . . H10A H 0.3111 0.1718 1.0750 0.090 Uiso 1 1 calc R . . C11 C 0.31853(17) 0.12791(18) 0.9792(3) 0.0652(15) Uani 1 1 d . . . H11A H 0.3190 0.1061 1.0219 0.078 Uiso 1 1 calc R . . C12 C 0.32223(14) 0.12072(15) 0.8846(3) 0.0511(12) Uani 1 1 d . . . H12A H 0.3245 0.0938 0.8622 0.061 Uiso 1 1 calc R . . C13 C 0.35683(13) 0.15892(12) 0.6779(3) 0.0414(10) Uani 1 1 d . . . C14 C 0.39369(13) 0.17579(12) 0.7222(3) 0.0397(10) Uani 1 1 d . B . C15 C 0.41694(15) 0.15258(14) 0.7824(3) 0.0528(12) Uani 1 1 d . . . H15A H 0.4071 0.1272 0.8032 0.063 Uiso 1 1 calc R B . C16 C 0.45410(15) 0.16610(16) 0.8121(3) 0.0569(13) Uani 1 1 d . B . H16A H 0.4700 0.1499 0.8523 0.068 Uiso 1 1 calc R . . C17 C 0.46794(16) 0.20283(17) 0.7836(3) 0.0596(14) Uani 1 1 d . . . H17A H 0.4938 0.2119 0.8031 0.071 Uiso 1 1 calc R B . C18 C 0.44474(17) 0.22691(16) 0.7267(3) 0.0626(14) Uani 1 1 d . B . H18A H 0.4542 0.2528 0.7088 0.075 Uiso 1 1 calc R . . C19 C 0.40781(15) 0.21324(13) 0.6959(3) 0.0506(12) Uani 1 1 d . . . H19A H 0.3919 0.2297 0.6562 0.061 Uiso 1 1 calc R B . C20 C 0.46643(16) 0.07803(18) 0.4901(4) 0.0702(16) Uani 1 1 d D A . C24 C 0.4670(2) 0.1772(2) 0.4719(5) 0.100(2) Uani 1 1 d . B . H24A H 0.4945 0.1828 0.4935 0.150 Uiso 1 1 calc R . . H24B H 0.4488 0.1758 0.5253 0.150 Uiso 1 1 calc R . . H24C H 0.4582 0.1989 0.4303 0.150 Uiso 1 1 calc R . . C25 C 0.51288(16) 0.12661(19) 0.3195(3) 0.0695(15) Uani 1 1 d . B . H25A H 0.5140 0.1016 0.2834 0.104 Uiso 1 1 calc R . . H25B H 0.5378 0.1294 0.3558 0.104 Uiso 1 1 calc R . . H25C H 0.5101 0.1496 0.2774 0.104 Uiso 1 1 calc R . . C26 C 0.42708(18) 0.1085(2) 0.2147(4) 0.0716(16) Uani 1 1 d . . . C27 C 0.4475(2) 0.0736(2) 0.1862(4) 0.0815(18) Uani 1 1 d . B . H27A H 0.4567 0.0544 0.2305 0.098 Uiso 1 1 calc R . . C28 C 0.4540(2) 0.0677(3) 0.0929(5) 0.098(2) Uani 1 1 d . . . H28A H 0.4669 0.0437 0.0722 0.117 Uiso 1 1 calc R B . C29 C 0.4421(2) 0.0960(3) 0.0300(5) 0.102(3) Uani 1 1 d . B . H29A H 0.4468 0.0917 -0.0342 0.123 Uiso 1 1 calc R . . C30 C 0.42379(19) 0.1296(3) 0.0583(4) 0.085(2) Uani 1 1 d . . . H30A H 0.4159 0.1489 0.0130 0.102 Uiso 1 1 calc R B . C31 C 0.41570(17) 0.1378(2) 0.1519(4) 0.0833(19) Uani 1 1 d . B . H31A H 0.4031 0.1622 0.1709 0.100 Uiso 1 1 calc R . . C32 C 0.38433(15) 0.11712(13) 0.3407(3) 0.0473(12) Uani 1 1 d . . . C33 C 0.34778(18) 0.09800(17) 0.2904(3) 0.0656(15) Uani 1 1 d . B . C34 C 0.31381(19) 0.1201(2) 0.2699(4) 0.0734(16) Uani 1 1 d . . . H34A H 0.3127 0.1479 0.2855 0.088 Uiso 1 1 calc R B . C35 C 0.2814(2) 0.1021(3) 0.2269(5) 0.094(2) Uani 1 1 d . B . H35A H 0.2585 0.1181 0.2124 0.113 Uiso 1 1 calc R . . C36 C 0.2811(2) 0.0614(3) 0.2039(4) 0.089(2) Uani 1 1 d . . . H36A H 0.2586 0.0493 0.1741 0.107 Uiso 1 1 calc R B . C37 C 0.3146(2) 0.0394(2) 0.2260(4) 0.090(2) Uani 1 1 d . B . H37A H 0.3148 0.0112 0.2140 0.108 Uiso 1 1 calc R . . C38 C 0.3492(2) 0.0575(2) 0.2662(4) 0.089(2) Uani 1 1 d . . . H38A H 0.3729 0.0421 0.2764 0.107 Uiso 1 1 calc R B . C21' C 0.5118(5) 0.0706(12) 0.5079(13) 0.105(8) Uani 0.50 1 d PDU A 1 H21A H 0.5150 0.0477 0.5502 0.158 Uiso 0.50 1 calc PR A 1 H21B H 0.5238 0.0948 0.5357 0.158 Uiso 0.50 1 calc PR A 1 H21C H 0.5253 0.0646 0.4489 0.158 Uiso 0.50 1 calc PR A 1 C22' C 0.4495(6) 0.0928(5) 0.5856(8) 0.106(6) Uani 0.50 1 d PDU A 1 H22A H 0.4532 0.0716 0.6322 0.158 Uiso 0.50 1 calc PR A 1 H22B H 0.4207 0.0989 0.5794 0.158 Uiso 0.50 1 calc PR A 1 H22C H 0.4640 0.1172 0.6050 0.158 Uiso 0.50 1 calc PR A 1 C23' C 0.4442(6) 0.0417(5) 0.451(2) 0.117(9) Uani 0.50 1 d PDU A 1 H23A H 0.4501 0.0179 0.4894 0.176 Uiso 0.50 1 calc PR A 1 H23B H 0.4529 0.0368 0.3874 0.176 Uiso 0.50 1 calc PR A 1 H23C H 0.4150 0.0470 0.4523 0.176 Uiso 0.50 1 calc PR A 1 C21 C 0.5057(5) 0.0742(13) 0.5462(14) 0.120(9) Uani 0.50 1 d PDU A 2 H21D H 0.5045 0.0500 0.5850 0.180 Uiso 0.50 1 calc PR A 2 H21E H 0.5089 0.0981 0.5857 0.180 Uiso 0.50 1 calc PR A 2 H21F H 0.5286 0.0722 0.5036 0.180 Uiso 0.50 1 calc PR A 2 C22 C 0.4266(5) 0.0716(5) 0.5464(12) 0.106(6) Uani 0.50 1 d PDU A 2 H22D H 0.4280 0.0459 0.5797 0.159 Uiso 0.50 1 calc PR A 2 H22E H 0.4036 0.0713 0.5038 0.159 Uiso 0.50 1 calc PR A 2 H22F H 0.4233 0.0937 0.5911 0.159 Uiso 0.50 1 calc PR A 2 C23 C 0.4638(5) 0.0381(5) 0.4369(18) 0.095(7) Uani 0.50 1 d PDU A 2 H23D H 0.4565 0.0163 0.4798 0.143 Uiso 0.50 1 calc PR A 2 H23E H 0.4901 0.0321 0.4086 0.143 Uiso 0.50 1 calc PR A 2 H23F H 0.4433 0.0403 0.3883 0.143 Uiso 0.50 1 calc PR A 2 C2' C 0.2097(6) 0.151(2) 0.571(4) 0.109(11) Uani 0.50 1 d PDU B 2 H2'A H 0.1950 0.1741 0.5467 0.163 Uiso 0.50 1 calc PR B 2 H2'B H 0.2002 0.1444 0.6336 0.163 Uiso 0.50 1 calc PR B 2 H2'C H 0.2050 0.1274 0.5303 0.163 Uiso 0.50 1 calc PR B 2 C3' C 0.2578(13) 0.2028(8) 0.615(3) 0.117(11) Uani 0.50 1 d PDU B 2 H3'A H 0.2442 0.2220 0.5739 0.175 Uiso 0.50 1 calc PR B 2 H3'B H 0.2862 0.2106 0.6220 0.175 Uiso 0.50 1 calc PR B 2 H3'C H 0.2447 0.2031 0.6761 0.175 Uiso 0.50 1 calc PR B 2 C4' C 0.2740(18) 0.160(2) 0.476(2) 0.104(13) Uani 0.50 1 d PDU B 2 H4'A H 0.2564 0.1747 0.4334 0.156 Uiso 0.50 1 calc PR B 2 H4'B H 0.2773 0.1322 0.4549 0.156 Uiso 0.50 1 calc PR B 2 H4'C H 0.3005 0.1733 0.4786 0.156 Uiso 0.50 1 calc PR B 2 C2 C 0.2108(7) 0.148(2) 0.558(4) 0.104(9) Uani 0.50 1 d PDU B 1 H2A H 0.1965 0.1701 0.5273 0.156 Uiso 0.50 1 calc PR B 1 H2B H 0.1981 0.1422 0.6179 0.156 Uiso 0.50 1 calc PR B 1 H2C H 0.2098 0.1238 0.5189 0.156 Uiso 0.50 1 calc PR B 1 C3 C 0.2573(9) 0.2005(7) 0.627(3) 0.095(9) Uani 0.50 1 d PDU B 1 H3A H 0.2391 0.2201 0.5975 0.143 Uiso 0.50 1 calc PR B 1 H3B H 0.2850 0.2109 0.6248 0.143 Uiso 0.50 1 calc PR B 1 H3C H 0.2492 0.1963 0.6913 0.143 Uiso 0.50 1 calc PR B 1 C4 C 0.2697(16) 0.1713(19) 0.4754(19) 0.086(9) Uani 0.50 1 d PDU B 1 H4A H 0.2549 0.1950 0.4534 0.129 Uiso 0.50 1 calc PR B 1 H4B H 0.2649 0.1486 0.4334 0.129 Uiso 0.50 1 calc PR B 1 H4C H 0.2987 0.1775 0.4771 0.129 Uiso 0.50 1 calc PR B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0469(9) 0.0744(11) 0.0431(8) 0.0005(7) 0.0036(6) -0.0101(7) O1 0.0493(18) 0.060(2) 0.0350(17) 0.0029(14) 0.0005(13) -0.0065(15) N1 0.045(2) 0.047(2) 0.0399(19) 0.0015(16) 0.0025(17) 0.0019(17) C1 0.046(3) 0.110(5) 0.055(3) 0.012(3) -0.003(2) 0.000(3) Li1 0.062(5) 0.088(6) 0.040(4) -0.009(4) 0.007(4) -0.019(5) Al2 0.0454(8) 0.0663(10) 0.0540(9) 0.0042(7) 0.0069(7) 0.0060(7) O2 0.079(3) 0.084(3) 0.058(2) -0.0070(19) 0.0119(19) -0.003(2) N2 0.065(3) 0.079(3) 0.050(2) -0.002(2) 0.006(2) 0.000(2) Li2 0.064(5) 0.056(5) 0.042(4) -0.006(3) 0.007(4) -0.002(4) C5 0.059(3) 0.117(5) 0.064(3) 0.007(3) 0.009(3) -0.028(3) C6 0.105(5) 0.070(4) 0.071(4) -0.013(3) 0.022(3) -0.020(3) C7 0.044(3) 0.054(3) 0.034(2) -0.002(2) 0.0017(19) 0.002(2) C8 0.084(4) 0.050(3) 0.053(3) 0.002(2) 0.008(3) 0.012(3) C9 0.106(5) 0.065(4) 0.055(3) -0.015(3) 0.006(3) 0.013(3) C10 0.100(5) 0.084(4) 0.040(3) -0.007(3) 0.005(3) 0.009(3) C11 0.082(4) 0.073(4) 0.041(3) 0.012(3) -0.002(3) 0.001(3) C12 0.062(3) 0.051(3) 0.041(2) 0.002(2) 0.000(2) 0.006(2) C13 0.049(3) 0.037(2) 0.039(2) 0.0035(19) -0.002(2) 0.007(2) C14 0.049(3) 0.038(2) 0.032(2) -0.0020(18) 0.0020(19) 0.002(2) C15 0.060(3) 0.044(3) 0.055(3) 0.008(2) -0.003(2) -0.004(2) C16 0.056(3) 0.065(3) 0.050(3) 0.006(2) -0.010(2) -0.006(3) C17 0.060(3) 0.077(4) 0.042(3) -0.005(3) -0.005(2) -0.017(3) C18 0.084(4) 0.056(3) 0.048(3) 0.002(2) -0.008(3) -0.025(3) C19 0.073(3) 0.040(3) 0.039(2) 0.001(2) -0.006(2) -0.004(2) C20 0.067(4) 0.083(4) 0.061(3) 0.015(3) 0.010(3) 0.026(3) C24 0.082(5) 0.087(5) 0.131(6) -0.037(4) 0.028(4) -0.001(4) C25 0.064(3) 0.097(4) 0.047(3) -0.007(3) 0.007(3) -0.012(3) C26 0.080(4) 0.093(4) 0.042(3) 0.004(3) -0.005(3) -0.012(3) C27 0.098(5) 0.082(4) 0.065(4) -0.016(3) 0.011(3) -0.001(4) C28 0.095(5) 0.139(7) 0.059(4) -0.035(4) 0.000(4) -0.016(5) C29 0.074(5) 0.180(8) 0.053(4) -0.007(5) -0.001(3) -0.031(5) C30 0.068(4) 0.147(7) 0.040(3) 0.013(4) 0.009(3) -0.006(4) C31 0.058(4) 0.108(5) 0.083(4) 0.022(4) -0.011(3) -0.008(3) C32 0.068(3) 0.049(3) 0.025(2) -0.0045(19) -0.005(2) 0.010(2) C33 0.090(4) 0.067(4) 0.041(3) -0.006(2) 0.006(3) 0.014(3) C34 0.065(4) 0.089(4) 0.066(4) 0.001(3) 0.016(3) -0.004(3) C35 0.075(5) 0.106(6) 0.100(5) 0.026(4) 0.023(4) 0.022(4) C36 0.071(4) 0.129(7) 0.068(4) -0.015(4) 0.018(3) -0.009(4) C37 0.115(6) 0.081(5) 0.075(4) -0.026(3) 0.001(4) -0.004(4) C38 0.111(5) 0.086(5) 0.071(4) -0.020(3) -0.013(4) 0.010(4) C21' 0.108(12) 0.141(16) 0.066(15) 0.046(16) -0.040(10) 0.015(11) C22' 0.173(18) 0.102(13) 0.041(7) 0.017(7) 0.037(9) 0.040(11) C23' 0.093(16) 0.091(12) 0.168(17) 0.083(11) -0.053(17) -0.031(11) C21 0.144(16) 0.152(16) 0.065(16) 0.034(17) -0.064(12) -0.028(14) C22 0.138(15) 0.101(13) 0.079(10) 0.037(9) 0.045(10) 0.033(10) C23 0.072(13) 0.095(11) 0.119(13) 0.041(9) -0.056(13) -0.012(10) C2' 0.053(14) 0.19(2) 0.087(19) 0.029(18) -0.021(14) 0.015(15) C3' 0.13(2) 0.13(2) 0.091(14) 0.045(14) 0.021(14) 0.044(17) C4' 0.059(13) 0.17(3) 0.084(13) 0.063(14) -0.018(10) 0.032(16) C2 0.061(15) 0.18(2) 0.071(14) 0.012(14) 0.022(11) -0.010(15) C3 0.051(11) 0.096(14) 0.14(2) 0.043(13) -0.020(13) 0.025(10) C4 0.049(15) 0.15(3) 0.062(10) 0.045(11) 0.006(10) 0.014(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C5 1.961(5) . ? Al1 N1 1.984(4) . ? Al1 C1 2.012(6) . ? Al1 C6 2.033(6) . ? Al1 Li1 2.788(8) . ? O1 C13 1.270(5) . ? O1 Li1 1.896(8) . ? O1 Li2 1.911(8) . ? N1 C13 1.322(5) . ? N1 C7 1.448(5) . ? C1 C4' 1.536(14) . ? C1 C3' 1.538(14) . ? C1 C2' 1.539(13) . ? C1 C2 1.540(13) . ? C1 C4 1.541(13) . ? C1 C3 1.543(13) . ? Li1 O2 1.846(9) . ? Li1 Li2 2.701(12) . ? Al2 C25 1.973(5) . ? Al2 C20 1.986(6) . ? Al2 C24 1.990(6) . ? Al2 N2 2.016(5) . ? Al2 Li2 3.114(8) . ? O2 C32 1.289(5) . ? O2 Li2 1.924(9) . ? N2 C32 1.291(6) . ? N2 C26 1.438(7) . ? Li2 C25 2.446(10) 11_666 ? C7 C8 1.378(7) . ? C7 C12 1.383(6) . ? C8 C9 1.391(7) . ? C9 C10 1.357(8) . ? C10 C11 1.373(8) . ? C11 C12 1.391(7) . ? C13 C14 1.488(6) . ? C14 C19 1.379(6) . ? C14 C15 1.392(6) . ? C15 C16 1.378(7) . ? C16 C17 1.364(7) . ? C17 C18 1.379(7) . ? C18 C19 1.378(7) . ? C20 C23' 1.518(13) . ? C20 C23 1.532(13) . ? C20 C21 1.537(13) . ? C20 C21' 1.545(13) . ? C20 C22 1.564(11) . ? C20 C22' 1.565(10) . ? C26 C31 1.381(8) . ? C26 C27 1.402(8) . ? C27 C28 1.377(8) . ? C28 C29 1.363(10) . ? C29 C30 1.332(10) . ? C30 C31 1.402(9) . ? C32 C33 1.548(7) . ? C33 C34 1.375(8) . ? C33 C38 1.388(8) . ? C34 C35 1.375(9) . ? C35 C36 1.390(10) . ? C36 C37 1.365(9) . ? C37 C38 1.415(9) . ? 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 C5 Al1 N1 107.1(2) . . ? C5 Al1 C1 113.4(3) . . ? N1 Al1 C1 107.5(2) . . ? C5 Al1 C6 108.1(3) . . ? N1 Al1 C6 106.9(2) . . ? C1 Al1 C6 113.3(3) . . ? C5 Al1 Li1 159.2(3) . . ? N1 Al1 Li1 85.7(2) . . ? C1 Al1 Li1 76.5(3) . . ? C6 Al1 Li1 51.6(3) . . ? C13 O1 Li1 133.7(4) . . ? C13 O1 Li2 132.8(4) . . ? Li1 O1 Li2 90.4(4) . . ? C13 N1 C7 119.0(4) . . ? C13 N1 Al1 118.9(3) . . ? C7 N1 Al1 121.9(3) . . ? C4' C1 C3' 110(3) . . ? C4' C1 C2' 112(3) . . ? C3' C1 C2' 105(3) . . ? C4' C1 C2 105(3) . . ? C3' C1 C2 111(3) . . ? C2' C1 C2 8(5) . . ? C4' C1 C4 15(4) . . ? C3' C1 C4 97(3) . . ? C2' C1 C4 109(3) . . ? C2 C1 C4 103(3) . . ? C4' C1 C3 116(3) . . ? C3' C1 C3 7(4) . . ? C2' C1 C3 104(3) . . ? C2 C1 C3 110(3) . . ? C4 C1 C3 103(3) . . ? C4' C1 Al1 110.8(19) . . ? C3' C1 Al1 112.7(18) . . ? C2' C1 Al1 107(2) . . ? C2 C1 Al1 108(2) . . ? C4 C1 Al1 124.5(19) . . ? C3 C1 Al1 107.0(16) . . ? O2 Li1 O1 89.6(4) . . ? O2 Li1 Li2 45.4(3) . . ? O1 Li1 Li2 45.0(3) . . ? O2 Li1 Al1 165.9(4) . . ? O1 Li1 Al1 76.7(3) . . ? Li2 Li1 Al1 121.5(3) . . ? C25 Al2 C20 113.8(2) . . ? C25 Al2 C24 105.5(3) . . ? C20 Al2 C24 112.0(3) . . ? C25 Al2 N2 100.1(2) . . ? C20 Al2 N2 108.0(2) . . ? C24 Al2 N2 117.0(3) . . ? C25 Al2 Li2 147.0(2) . . ? C20 Al2 Li2 97.3(2) . . ? C24 Al2 Li2 49.5(2) . . ? N2 Al2 Li2 79.4(2) . . ? C32 O2 Li1 133.9(4) . . ? C32 O2 Li2 134.1(4) . . ? Li1 O2 Li2 91.5(4) . . ? C32 N2 C26 116.4(4) . . ? C32 N2 Al2 118.9(3) . . ? C26 N2 Al2 124.6(4) . . ? O1 Li2 O2 86.9(4) . . ? O1 Li2 C25 109.5(4) . 11_666 ? O2 Li2 C25 107.0(4) . 11_666 ? O1 Li2 Li1 44.6(3) . . ? O2 Li2 Li1 43.1(3) . . ? C25 Li2 Li1 109.2(4) 11_666 . ? O1 Li2 Al2 131.3(4) . . ? O2 Li2 Al2 69.3(3) . . ? C25 Li2 Al2 117.7(3) 11_666 . ? Li1 Li2 Al2 105.8(3) . . ? C8 C7 C12 119.9(4) . . ? C8 C7 N1 120.3(4) . . ? C12 C7 N1 119.6(4) . . ? C7 C8 C9 119.2(5) . . ? C10 C9 C8 120.8(5) . . ? C9 C10 C11 120.5(5) . . ? C10 C11 C12 119.5(5) . . ? C7 C12 C11 120.0(5) . . ? O1 C13 N1 120.2(4) . . ? O1 C13 C14 115.6(4) . . ? N1 C13 C14 124.2(4) . . ? C19 C14 C15 118.7(4) . . ? C19 C14 C13 119.9(4) . . ? C15 C14 C13 121.0(4) . . ? C16 C15 C14 120.5(4) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C18 120.5(5) . . ? C19 C18 C17 119.8(5) . . ? C18 C19 C14 120.5(4) . . ? C23' C20 C23 26.4(11) . . ? C23' C20 C21 122.7(18) . . ? C23 C20 C21 103.9(17) . . ? C23' C20 C21' 114.1(18) . . ? C23 C20 C21' 90.0(16) . . ? C21 C20 C21' 22.5(14) . . ? C23' C20 C22 70.9(12) . . ? C23 C20 C22 95.5(12) . . ? C21 C20 C22 115.5(12) . . ? C21' C20 C22 135.6(11) . . ? C23' C20 C22' 113.4(14) . . ? C23 C20 C22' 133.7(14) . . ? C21 C20 C22' 82.3(13) . . ? C21' C20 C22' 104.6(12) . . ? C22 C20 C22' 44.3(8) . . ? C23' C20 Al2 112.8(11) . . ? C23 C20 Al2 111.3(11) . . ? C21 C20 Al2 113.3(14) . . ? C21' C20 Al2 103.5(13) . . ? C22 C20 Al2 115.2(6) . . ? C22' C20 Al2 107.6(6) . . ? C31 C26 C27 121.3(6) . . ? C31 C26 N2 118.2(6) . . ? C27 C26 N2 120.2(5) . . ? C28 C27 C26 118.7(7) . . ? C29 C28 C27 120.4(7) . . ? C30 C29 C28 120.3(7) . . ? C29 C30 C31 123.0(7) . . ? C26 C31 C30 116.2(7) . . ? O2 C32 N2 121.2(4) . . ? O2 C32 C33 112.8(4) . . ? N2 C32 C33 125.7(4) . . ? C34 C33 C38 119.2(6) . . ? C34 C33 C32 121.5(5) . . ? C38 C33 C32 119.2(5) . . ? C33 C34 C35 120.3(6) . . ? C34 C35 C36 122.3(6) . . ? C37 C36 C35 117.1(7) . . ? C36 C37 C38 121.9(7) . . ? C33 C38 C37 119.0(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.325 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.061 data_rs9934 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H66 Al2 Li2 N2 O4' _chemical_formula_weight 850.91 _chemical_melting_point ? _chemical_compound_source ? 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' 'Al' 'Al' 0.0645 0.0514 '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' '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.787(5) _cell_length_b 11.779(5) _cell_length_c 14.112(3) _cell_angle_alpha 108.20(3) _cell_angle_beta 101.91(3) _cell_angle_gamma 108.08(3) _cell_volume 1383.8(10) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10374 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.022 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.021 _exptl_crystal_density_method ? _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8491 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0989 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 26.10 _reflns_number_total 5395 _reflns_number_observed 2530 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1860P)^2^+0.3539P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5395 _refine_ls_number_parameters 285 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.1940 _refine_ls_R_factor_obs 0.1029 _refine_ls_wR_factor_all 0.3447 _refine_ls_wR_factor_obs 0.2837 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.267 _refine_ls_restrained_S_all 1.062 _refine_ls_restrained_S_obs 1.279 _refine_ls_shift/esd_max 0.013 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.10457(19) -0.16909(13) 0.16506(11) 0.0807(6) Uani 1 d D . O1 O 0.0801(4) 0.0495(3) 0.1035(2) 0.0692(9) Uani 1 d . . N1 N 0.1651(4) 0.0172(3) 0.2493(2) 0.0555(9) Uani 1 d . . Li1 Li -0.0499(11) -0.1207(7) -0.0029(6) 0.081(3) Uani 1 d . . O2 O -0.0766(4) -0.2213(3) 0.0734(2) 0.0741(10) Uani 1 d D . C1 C 0.1466(5) 0.0956(4) 0.2026(3) 0.0538(10) Uani 1 d . . C2 C 0.2012(5) 0.2407(4) 0.2601(3) 0.0507(10) Uani 1 d . . C3 C 0.0998(5) 0.2970(4) 0.2465(4) 0.0701(13) Uani 1 d . . H3 H -0.0047 0.2434 0.2062 0.084 Uiso 1 calc R . C4 C 0.1483(7) 0.4319(5) 0.2909(5) 0.0860(16) Uani 1 d . . H4 H 0.0769 0.4703 0.2823 0.103 Uiso 1 calc R . C5 C 0.2992(7) 0.5090(5) 0.3472(4) 0.0851(16) Uani 1 d . . H5 H 0.3332 0.6014 0.3771 0.102 Uiso 1 calc R . C6 C 0.4004(6) 0.4534(5) 0.3603(4) 0.0784(15) Uani 1 d . . H6 H 0.5051 0.5077 0.3991 0.094 Uiso 1 calc R . C7 C 0.3533(5) 0.3191(4) 0.3180(3) 0.0631(12) Uani 1 d . . H7 H 0.4248 0.2812 0.3286 0.076 Uiso 1 calc R . C8 C 0.2262(5) 0.0711(4) 0.3625(3) 0.0538(11) Uani 1 d . . C9 C 0.1380(6) 0.1087(5) 0.4225(3) 0.0697(13) Uani 1 d . . H9 H 0.0387 0.1006 0.3888 0.084 Uiso 1 calc R . C10 C 0.1991(7) 0.1585(6) 0.5327(4) 0.0880(17) Uani 1 d . . H10 H 0.1410 0.1852 0.5744 0.106 Uiso 1 calc R . C11 C 0.3405(7) 0.1692(5) 0.5813(4) 0.0834(16) Uani 1 d . . H11 H 0.3809 0.2041 0.6564 0.100 Uiso 1 calc R . C12 C 0.4247(6) 0.1299(5) 0.5223(4) 0.0771(15) Uani 1 d . . H12 H 0.5231 0.1366 0.5565 0.093 Uiso 1 calc R . C13 C 0.3669(5) 0.0802(4) 0.4128(3) 0.0634(12) Uani 1 d . . H13 H 0.4257 0.0521 0.3723 0.076 Uiso 1 calc R . C14_a C 0.2348(14) -0.1620(15) 0.0701(9) 0.102(4) Uiso 0.517(4) d PDU 1 H14A_a H 0.2068 -0.1181 0.0254 0.153 Uiso 0.517(4) calc PR 1 H14B_a H 0.2176 -0.2510 0.0252 0.153 Uiso 0.517(4) calc PR 1 H14C_a H 0.3428 -0.1135 0.1140 0.153 Uiso 0.517(4) calc PR 1 C18_a C 0.1574(15) -0.2583(11) 0.2553(8) 0.090(3) Uiso 0.517(4) d PDU 1 H18A_a H 0.2650 -0.2101 0.3001 0.135 Uiso 0.517(4) calc PR 1 H18B_a H 0.1405 -0.3472 0.2104 0.135 Uiso 0.517(4) calc PR 1 H18C_a H 0.0931 -0.2618 0.3000 0.135 Uiso 0.517(4) calc PR 1 C19_b C -0.2122(10) -0.3206(8) 0.0536(6) 0.073(3) Uiso 0.480(5) d PDU 2 C20_b C -0.2112(13) -0.4565(9) 0.0135(7) 0.083(3) Uiso 0.480(5) d PDU 2 H20A_b H -0.1839 -0.4725 -0.0510 0.125 Uiso 0.480(5) calc PR 2 H20B_b H -0.3128 -0.5221 -0.0022 0.125 Uiso 0.480(5) calc PR 2 H20C_b H -0.1364 -0.4621 0.0679 0.125 Uiso 0.480(5) calc PR 2 C21_b C -0.3309(12) -0.3149(10) -0.0324(7) 0.078(3) Uiso 0.480(5) d PDU 2 H21A_b H -0.2977 -0.3215 -0.0941 0.117 Uiso 0.480(5) calc PR 2 H21B_b H -0.3417 -0.2319 -0.0049 0.117 Uiso 0.480(5) calc PR 2 H21C_b H -0.4293 -0.3875 -0.0533 0.117 Uiso 0.480(5) calc PR 2 C22_b C -0.2570(15) -0.3000(12) 0.1531(7) 0.086(4) Uiso 0.480(5) d PDU 2 H22A_b H -0.1786 -0.3002 0.2088 0.129 Uiso 0.480(5) calc PR 2 H22B_b H -0.3551 -0.3706 0.1370 0.129 Uiso 0.480(5) calc PR 2 H22C_b H -0.2662 -0.2160 0.1774 0.129 Uiso 0.480(5) calc PR 2 C19'_d C -0.2384(11) -0.2773(11) 0.0644(8) 0.083(3) Uiso 0.208(6) d PDU 4 C20'_d C -0.2770(37) -0.4239(16) 0.0062(17) 0.119(10) Uiso 0.208(6) d PDU 4 H20D_d H -0.2106 -0.4498 0.0492 0.179 Uiso 0.208(6) calc PR 4 H20E_d H -0.2612 -0.4400 -0.0623 0.179 Uiso 0.208(6) calc PR 4 H20F_d H -0.3839 -0.4749 -0.0051 0.179 Uiso 0.208(6) calc PR 4 C21'_d C -0.3440(26) -0.2413(23) -0.0056(14) 0.079(7) Uiso 0.208(6) d PDU 4 H21D_d H -0.3204 -0.2508 -0.0711 0.119 Uiso 0.208(6) calc PR 4 H21E_d H -0.3290 -0.1507 0.0322 0.119 Uiso 0.208(6) calc PR 4 H21F_d H -0.4503 -0.2994 -0.0228 0.119 Uiso 0.208(6) calc PR 4 C22'_d C -0.2727(34) -0.2570(27) 0.1676(13) 0.093(8) Uiso 0.208(6) d PDU 4 H22D_d H -0.2011 -0.2743 0.2151 0.139 Uiso 0.208(6) calc PR 4 H22E_d H -0.3773 -0.3170 0.1526 0.139 Uiso 0.208(6) calc PR 4 H22F_d H -0.2615 -0.1667 0.2015 0.139 Uiso 0.208(6) calc PR 4 C19"_c C -0.2384(11) -0.2773(11) 0.0644(8) 0.083(3) Uiso 0.312(3) d P 3 H19D_c H -0.3030 -0.2888 -0.0039 0.125 Uiso 0.312(3) calc PR 3 H19E_c H -0.2567 -0.2181 0.1219 0.125 Uiso 0.312(3) calc PR 3 H19F_c H -0.2631 -0.3621 0.0691 0.125 Uiso 0.312(3) calc PR 3 C14"_e C 0.2408(10) -0.2032(9) 0.0905(7) 0.079(3) Uiso 0.171(5) d P 5 H14D_e H 0.3422 -0.1737 0.1416 0.118 Uiso 0.171(5) calc PR 5 H14E_e H 0.2476 -0.1561 0.0442 0.118 Uiso 0.171(5) calc PR 5 H14F_e H 0.2019 -0.2971 0.0477 0.118 Uiso 0.171(5) calc PR 5 C14'_c C 0.2408(10) -0.2032(9) 0.0905(7) 0.079(3) Uiso 0.312(3) d PDU 3 C15'_c C 0.3710(15) -0.2074(13) 0.1664(10) 0.078(4) Uiso 0.312(3) d PD 3 H15A_c H 0.3305 -0.2736 0.1931 0.116 Uiso 0.312(3) calc PR 3 H15B_c H 0.4273 -0.1217 0.2259 0.116 Uiso 0.312(3) calc PR 3 H15C_c H 0.4398 -0.2295 0.1295 0.116 Uiso 0.312(3) calc PR 3 C16'_c C 0.1492(16) -0.3357(11) -0.0022(10) 0.083(5) Uiso 0.312(3) d PD 3 H16A_c H 0.1106 -0.4022 0.0245 0.125 Uiso 0.312(3) calc PR 3 H16B_c H 0.2149 -0.3583 -0.0420 0.125 Uiso 0.312(3) calc PR 3 H16C_c H 0.0631 -0.3317 -0.0489 0.125 Uiso 0.312(3) calc PR 3 C17'_c C 0.2994(16) -0.1001(11) 0.0491(10) 0.069(4) Uiso 0.312(3) d PD 3 H17A_c H 0.3573 -0.0148 0.1087 0.103 Uiso 0.312(3) calc PR 3 H17B_c H 0.2129 -0.0970 0.0021 0.103 Uiso 0.312(3) calc PR 3 H17C_c H 0.3658 -0.1219 0.0098 0.103 Uiso 0.312(3) calc PR 3 C18'_b C 0.0922(12) -0.2453(9) 0.2748(6) 0.059(2) Uiso 0.483(4) d PDU 2 H18D_b H 0.0209 -0.2233 0.3090 0.089 Uiso 0.483(4) calc PR 2 H18E_b H 0.1935 -0.2090 0.3281 0.089 Uiso 0.483(4) calc PR 2 H18F_b H 0.0562 -0.3404 0.2403 0.089 Uiso 0.483(4) calc PR 2 C50_a C -0.2771(21) 0.4222(16) 0.2520(12) 0.147(6) Uiso 0.50 d PD 1 H50A_a H -0.2383 0.5101 0.3079 0.221 Uiso 0.50 calc PR 1 H50B_a H -0.3841 0.3960 0.2115 0.221 Uiso 0.50 calc PR 1 H50C_a H -0.2167 0.4222 0.2046 0.221 Uiso 0.50 calc PR 1 C51_a C -0.2662(21) 0.3332(12) 0.2980(8) 0.109(5) Uiso 0.50 d PD 1 C52_a C -0.3205(22) 0.2029(13) 0.2355(9) 0.129(5) Uiso 0.50 d PD 1 H52_a H -0.3686 0.1701 0.1611 0.155 Uiso 0.50 calc PR 1 C53_a C -0.3031(28) 0.1210(12) 0.2838(12) 0.151(7) Uiso 0.50 d PD 1 H53_a H -0.3433 0.0307 0.2391 0.181 Uiso 0.50 calc PR 1 C54_a C -0.2344(18) 0.1552(11) 0.3892(10) 0.108(4) Uiso 0.50 d PD 1 H54_a H -0.2196 0.0963 0.4193 0.129 Uiso 0.50 calc PR 1 C55_a C -0.1900(17) 0.2860(11) 0.4454(8) 0.104(4) Uiso 0.50 d PD 1 H55_a H -0.1462 0.3179 0.5201 0.125 Uiso 0.50 calc PR 1 C56_a C -0.2018(15) 0.3766(9) 0.4051(7) 0.083(3) Uiso 0.50 d PD 1 H56_a H -0.1663 0.4663 0.4504 0.099 Uiso 0.50 calc PR 1 C50'_b C -0.2195(27) 0.4918(16) 0.3434(16) 0.202(9) Uiso 0.50 d PD 2 H50D_b H -0.1700 0.5522 0.4182 0.303 Uiso 0.50 calc PR 2 H50E_b H -0.3205 0.4914 0.3169 0.303 Uiso 0.50 calc PR 2 H50F_b H -0.1570 0.5198 0.3024 0.303 Uiso 0.50 calc PR 2 C51'_b C -0.2354(29) 0.3647(12) 0.3331(11) 0.152(7) Uiso 0.50 d PD 2 C52'_b C -0.3060(20) 0.2617(13) 0.2357(9) 0.128(5) Uiso 0.50 d PD 2 H52'_b H -0.3401 0.2743 0.1732 0.153 Uiso 0.50 calc PR 2 C53'_b C -0.3253(19) 0.1397(11) 0.2321(9) 0.114(4) Uiso 0.50 d PD 2 H53'_b H -0.3753 0.0696 0.1641 0.137 Uiso 0.50 calc PR 2 C54'_b C -0.2813(23) 0.1067(14) 0.3147(11) 0.123(5) Uiso 0.50 d PD 2 H54'_b H -0.2924 0.0213 0.3080 0.148 Uiso 0.50 calc PR 2 C55'_b C -0.2189(29) 0.2151(16) 0.4084(12) 0.170(8) Uiso 0.50 d PD 2 H55'_b H -0.1941 0.2012 0.4714 0.203 Uiso 0.50 calc PR 2 C56'_b C -0.1887(29) 0.3416(14) 0.4205(10) 0.175(8) Uiso 0.50 d PD 2 H56'_b H -0.1363 0.4116 0.4885 0.210 Uiso 0.50 calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0983(13) 0.0494(8) 0.0633(9) 0.0156(7) -0.0161(8) 0.0260(8) O1 0.088(2) 0.0468(16) 0.0426(15) 0.0163(12) -0.0111(14) 0.0118(15) N1 0.065(2) 0.0470(18) 0.0424(17) 0.0180(15) -0.0010(15) 0.0190(17) Li1 0.098(6) 0.052(4) 0.050(4) 0.021(3) -0.015(4) 0.000(4) O2 0.083(2) 0.0521(17) 0.0587(18) 0.0232(14) -0.0049(16) 0.0091(16) C1 0.052(3) 0.050(2) 0.044(2) 0.0188(19) 0.0021(18) 0.011(2) C2 0.058(3) 0.048(2) 0.0393(19) 0.0213(17) 0.0067(18) 0.016(2) C3 0.059(3) 0.062(3) 0.080(3) 0.033(2) 0.006(2) 0.019(2) C4 0.088(4) 0.061(3) 0.113(4) 0.040(3) 0.029(4) 0.035(3) C5 0.108(5) 0.045(3) 0.086(4) 0.019(3) 0.027(3) 0.021(3) C6 0.078(4) 0.054(3) 0.062(3) 0.014(2) 0.000(2) -0.001(3) C7 0.060(3) 0.054(3) 0.054(2) 0.017(2) 0.000(2) 0.013(2) C8 0.061(3) 0.044(2) 0.044(2) 0.0204(17) 0.002(2) 0.014(2) C9 0.065(3) 0.078(3) 0.060(3) 0.033(2) 0.010(2) 0.023(3) C10 0.113(5) 0.101(4) 0.054(3) 0.033(3) 0.034(3) 0.044(4) C11 0.104(5) 0.071(3) 0.049(3) 0.023(2) 0.001(3) 0.022(3) C12 0.085(4) 0.067(3) 0.054(3) 0.019(2) -0.012(3) 0.026(3) C13 0.065(3) 0.059(3) 0.053(2) 0.020(2) -0.001(2) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O2 1.7535(36) . ? Al1 C14"_e 1.9217(80) . ? Al1 N1 1.9631(35) . ? Al1 C18_a 1.9727(77) . ? Al1 C18'_b 2.0236(70) . ? Al1 C14_a 2.0332(86) . ? Al1 Li1 2.8511(75) . ? O1 C1 1.2673(44) . ? O1 Li1 1.8785(78) 2 ? O1 Li1 1.9075(76) . ? N1 C1 1.3235(50) . ? N1 C8 1.4314(48) . ? Li1 O2 1.8309(82) . ? Li1 O1 1.8786(78) 2 ? Li1 Li1 2.6721(149) 2 ? Li1 C19'_d 2.7225(134) . ? O2 C19_b 1.3739(92) . ? O2 C19"_c 1.4754(97) . ? O2 C19'_d 1.4754(97) . ? C1 C2 1.5013(54) . ? C2 C3 1.3685(59) . ? C2 C7 1.3817(58) . ? C3 C4 1.3885(66) . ? C4 C5 1.3673(76) . ? C5 C6 1.3589(73) . ? C6 C7 1.3846(63) . ? C8 C13 1.3675(60) . ? C8 C9 1.4011(63) . ? C9 C10 1.3969(65) . ? C10 C11 1.3591(76) . ? C11 C12 1.3654(74) . ? C12 C13 1.3853(61) . ? C19_b C22_b 1.5256(77) . ? C19_b C20_b 1.5261(78) . ? C19_b C21_b 1.5314(76) . ? C19'_d C22'_d 1.5251(85) . ? C19'_d C21'_d 1.5274(84) . ? C19'_d C20'_d 1.5426(85) . ? C14'_c C15'_c 1.5114(79) . ? C14'_c C17'_c 1.5138(79) . ? C14'_c C16'_c 1.5241(78) . ? C50_a C51_a 1.4146(140) . ? C51_a C56_a 1.3661(78) . ? C51_a C52_a 1.3679(78) . ? C52_a C53_a 1.3739(81) . ? C53_a C54_a 1.3688(82) . ? C54_a C55_a 1.3675(83) . ? C55_a C56_a 1.3796(79) . ? C50'_b C51'_b 1.4125(142) . ? C51'_b C56'_b 1.3637(78) . ? C51'_b C52'_b 1.3737(79) . ? C52'_b C53'_b 1.3735(80) . ? C53'_b C54'_b 1.3680(83) . ? C54'_b C55'_b 1.3708(83) . ? C55'_b C56'_b 1.3717(81) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al1 C14"_e 109.3(3) . . ? O2 Al1 N1 105.31(15) . . ? C14"_e Al1 N1 113.5(3) . . ? O2 Al1 C18_a 124.8(4) . . ? N1 Al1 C18_a 111.4(4) . . ? O2 Al1 C18'_b 111.2(3) . . ? N1 Al1 C18'_b 102.2(3) . . ? O2 Al1 C14_a 100.7(4) . . ? N1 Al1 C14_a 101.5(4) . . ? C18_a Al1 C14_a 110.3(5) . . ? O2 Al1 Li1 38.3(2) . . ? C14"_e Al1 Li1 89.6(4) . . ? N1 Al1 Li1 84.49(18) . . ? C18_a Al1 Li1 161.6(4) . . ? C18'_b Al1 Li1 148.4(4) . . ? C14_a Al1 Li1 73.8(5) . . ? C1 O1 Li1 135.3(3) . 2 ? C1 O1 Li1 134.6(3) . . ? Li1 O1 Li1 89.8(3) 2 . ? C1 N1 C8 118.4(3) . . ? C1 N1 Al1 120.6(3) . . ? C8 N1 Al1 121.0(3) . . ? O2 Li1 O1 163.8(5) . 2 ? O2 Li1 O1 102.9(4) . . ? O1 Li1 O1 90.2(3) 2 . ? O2 Li1 Li1 146.6(5) . 2 ? O1 Li1 Li1 45.5(2) 2 2 ? O1 Li1 Li1 44.7(2) . 2 ? O2 Li1 C19'_d 30.5(3) . . ? O1 Li1 C19'_d 134.5(5) 2 . ? O1 Li1 C19'_d 114.5(4) . . ? Li1 Li1 C19'_d 142.1(7) 2 . ? O2 Li1 Al1 36.37(18) . . ? O1 Li1 Al1 159.6(5) 2 . ? O1 Li1 Al1 76.0(2) . . ? Li1 Li1 Al1 119.1(4) 2 . ? C19'_d Li1 Al1 65.7(3) . . ? C19_b O2 Al1 130.2(4) . . ? C19"_c O2 Al1 139.0(4) . . ? C19'_d O2 Al1 139.0(4) . . ? C19_b O2 Li1 124.3(5) . . ? C19"_c O2 Li1 110.4(5) . . ? C19'_d O2 Li1 110.4(5) . . ? Al1 O2 Li1 105.4(3) . . ? O1 C1 N1 120.3(3) . . ? O1 C1 C2 115.8(3) . . ? N1 C1 C2 123.9(3) . . ? C3 C2 C7 119.5(4) . . ? C3 C2 C1 118.7(4) . . ? C7 C2 C1 121.5(4) . . ? C2 C3 C4 120.6(5) . . ? C5 C4 C3 119.7(5) . . ? C6 C5 C4 119.9(5) . . ? C5 C6 C7 121.1(5) . . ? C2 C7 C6 119.2(5) . . ? C13 C8 C9 119.4(4) . . ? C13 C8 N1 120.7(4) . . ? C9 C8 N1 119.8(4) . . ? C10 C9 C8 118.6(5) . . ? C11 C10 C9 121.0(5) . . ? C10 C11 C12 120.1(5) . . ? C11 C12 C13 120.1(5) . . ? C8 C13 C12 120.7(5) . . ? O2 C19_b C22_b 110.7(7) . . ? O2 C19_b C20_b 114.2(7) . . ? C22_b C19_b C20_b 107.9(6) . . ? O2 C19_b C21_b 105.8(7) . . ? C22_b C19_b C21_b 109.8(6) . . ? C20_b C19_b C21_b 108.4(6) . . ? O2 C19'_d C22'_d 116.8(13) . . ? O2 C19'_d C21'_d 114.7(12) . . ? C22'_d C19'_d C21'_d 108.7(7) . . ? O2 C19'_d C20'_d 100.1(14) . . ? C22'_d C19'_d C20'_d 108.0(7) . . ? C21'_d C19'_d C20'_d 107.5(7) . . ? O2 C19'_d Li1 39.1(3) . . ? C22'_d C19'_d Li1 134.2(12) . . ? C21'_d C19'_d Li1 75.7(10) . . ? C20'_d C19'_d Li1 113.9(12) . . ? C15'_c C14'_c C17'_c 110.9(6) . . ? C15'_c C14'_c C16'_c 110.9(6) . . ? C17'_c C14'_c C16'_c 109.5(6) . . ? C56_a C51_a C52_a 119.6(10) . . ? C56_a C51_a C50_a 120.3(7) . . ? C52_a C51_a C50_a 120.1(7) . . ? C51_a C52_a C53_a 117.8(9) . . ? C54_a C53_a C52_a 127.2(10) . . ? C55_a C54_a C53_a 110.5(11) . . ? C54_a C55_a C56_a 127.0(9) . . ? C51_a C56_a C55_a 117.8(8) . . ? C56'_b C51'_b C52'_b 119.1(10) . . ? C56'_b C51'_b C50'_b 120.4(7) . . ? C52'_b C51'_b C50'_b 120.4(7) . . ? C53'_b C52'_b C51'_b 117.3(9) . . ? C54'_b C53'_b C52'_b 127.9(10) . . ? C53'_b C54'_b C55'_b 110.0(11) . . ? C54'_b C55'_b C56'_b 126.7(11) . . ? C51'_b C56'_b C55'_b 118.6(9) . . ? _refine_diff_density_max 0.641 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.062