# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'R. E. Mulvey' _publ_contact_author_address ; Department of Pure & Applied Chemistry University of Strathclyde 295 Cathedral Street Glasgow G1 1XL UNITED KINGDOM ; _publ_contact_author_email R.E.MULVEY@STRATH.AC.UK _publ_section_title ; Lewis base stabilized lithium TMP aluminates: an unexpected fragmentation and capture reaction involving cyclic ether 1,4-dioxane ; _publ_contact_letter ; Dear Sir, The following cif contains the supplementary X-ray data for a ms submitted to Chem. Commun. by Garcia-Alvarez, Hevia, Kennedy, Klett and Mulvey. Please advise me of any problems Yours Alan Kennedy a.r.kennedy@strath.ac.uk ; loop_ _publ_author_name 'R. E. Mulvey' 'Joaquin Garcia-Alvarez' 'Eva Hevia' 'Alan R. Kennedy' 'Jan Klett' ############################################################ ########### COMPOUND 1 ################################### ######################################################### data_grem245 _database_code_depnum_ccdc_archive 'CCDC 634093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H64 Al Li N2' _chemical_formula_weight 486.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5631(2) _cell_length_b 18.6410(5) _cell_length_c 10.6743(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.995(2) _cell_angle_gamma 90.00 _cell_volume 1637.92(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3841 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description chunk _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 _exptl_absorpt_coefficient_mu 0.080 _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 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23836 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7415 _reflns_number_gt 5436 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.4850P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(17) _refine_ls_number_reflns 7415 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0912 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1144 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.26635(8) 0.16306(4) 1.02450(6) 0.03519(16) Uani 1 1 d . . . Li1 Li 0.2748(5) 0.0888(2) 0.7944(4) 0.0413(9) Uani 1 1 d . . . N1 N 0.3017(2) 0.19425(10) 0.85564(18) 0.0350(4) Uani 1 1 d . . . N2 N 0.2616(2) -0.01088(12) 0.6879(2) 0.0421(5) Uani 1 1 d . . . C1 C 0.2067(3) 0.05791(14) 0.9821(3) 0.0421(6) Uani 1 1 d . . . C2 C -0.0485(4) 0.0087(2) 1.0311(5) 0.0857(12) Uani 1 1 d . . . H2A H -0.0779 -0.0198 0.9508 0.129 Uiso 1 1 calc R . . H2B H -0.0970 0.0565 1.0136 0.129 Uiso 1 1 calc R . . H2C H -0.0891 -0.0151 1.0978 0.129 Uiso 1 1 calc R . . C3 C 0.1353(3) 0.01544(15) 1.0792(3) 0.0507(7) Uani 1 1 d . . . H3 H 0.1623 0.0424 1.1635 0.061 Uiso 1 1 calc R . . C4 C 0.2048(4) -0.0592(2) 1.1069(4) 0.0892(12) Uani 1 1 d . . . H4A H 0.1577 -0.0828 1.1700 0.134 Uiso 1 1 calc R . . H4B H 0.3230 -0.0562 1.1427 0.134 Uiso 1 1 calc R . . H4C H 0.1789 -0.0870 1.0258 0.134 Uiso 1 1 calc R . . C5 C 0.4620(3) 0.17548(16) 1.1810(2) 0.0447(6) Uani 1 1 d . . . C6 C 0.5934(4) 0.05524(18) 1.2510(3) 0.0694(9) Uani 1 1 d . . . H6A H 0.5273 0.0338 1.1698 0.104 Uiso 1 1 calc R . . H6B H 0.6144 0.0194 1.3207 0.104 Uiso 1 1 calc R . . H6C H 0.6968 0.0718 1.2387 0.104 Uiso 1 1 calc R . . C7 C 0.5029(4) 0.11856(18) 1.2877(3) 0.0568(7) Uani 1 1 d . . . H7 H 0.3986 0.1003 1.3005 0.068 Uiso 1 1 calc R . . C8 C 0.6044(4) 0.1499(2) 1.4181(3) 0.0701(9) Uani 1 1 d . . . H8A H 0.7070 0.1686 1.4077 0.105 Uiso 1 1 calc R . . H8B H 0.6269 0.1122 1.4847 0.105 Uiso 1 1 calc R . . H8C H 0.5438 0.1889 1.4449 0.105 Uiso 1 1 calc R . . C9 C 0.0748(3) 0.2056(2) 1.0778(3) 0.0532(7) Uani 1 1 d . . . C10 C -0.0550(4) 0.2244(2) 1.2604(3) 0.0792(11) Uani 1 1 d . . . H10A H -0.0324 0.2387 1.3521 0.119 Uiso 1 1 calc R . . H10B H -0.0904 0.1742 1.2510 0.119 Uiso 1 1 calc R . . H10C H -0.1410 0.2549 1.2070 0.119 Uiso 1 1 calc R . . C11 C 0.0984(3) 0.23264(15) 1.2159(3) 0.0475(6) Uani 1 1 d . . . H11 H 0.1851 0.2027 1.2747 0.057 Uiso 1 1 calc R . . C12 C 0.1537(4) 0.30853(18) 1.2315(4) 0.0770(10) Uani 1 1 d . . . H12A H 0.2458 0.3147 1.1947 0.116 Uiso 1 1 calc R . . H12B H 0.1873 0.3209 1.3243 0.116 Uiso 1 1 calc R . . H12C H 0.0645 0.3400 1.1859 0.116 Uiso 1 1 calc R . . C13 C 0.1748(4) 0.24265(15) 0.7737(2) 0.0515(7) Uani 1 1 d . . . C14 C 0.1999(4) 0.25484(18) 0.6370(3) 0.0683(9) Uani 1 1 d . . . H14A H 0.1783 0.2093 0.5875 0.082 Uiso 1 1 calc R . . H14B H 0.1196 0.2906 0.5896 0.082 Uiso 1 1 calc R . . C15 C 0.3673(5) 0.28046(19) 0.6403(3) 0.0775(11) Uani 1 1 d . . . H15A H 0.3880 0.3281 0.6828 0.093 Uiso 1 1 calc R . . H15B H 0.3781 0.2848 0.5506 0.093 Uiso 1 1 calc R . . C16 C 0.4868(4) 0.22604(17) 0.7166(3) 0.0620(8) Uani 1 1 d . . . H16A H 0.5984 0.2426 0.7220 0.074 Uiso 1 1 calc R . . H16B H 0.4697 0.1800 0.6687 0.074 Uiso 1 1 calc R . . C17 C 0.4729(3) 0.21312(13) 0.8554(2) 0.0433(6) Uani 1 1 d . . . C18 C 0.0098(4) 0.2049(2) 0.7519(3) 0.0673(9) Uani 1 1 d . . . H18A H 0.0140 0.1578 0.7120 0.101 Uiso 1 1 calc R . . H18B H -0.0753 0.2341 0.6940 0.101 Uiso 1 1 calc R . . H18C H -0.0145 0.1987 0.8357 0.101 Uiso 1 1 calc R . . C19 C 0.1632(5) 0.31713(17) 0.8347(3) 0.0748(10) Uani 1 1 d . . . H19A H 0.1699 0.3114 0.9273 0.112 Uiso 1 1 calc R . . H19B H 0.0595 0.3397 0.7898 0.112 Uiso 1 1 calc R . . H19C H 0.2529 0.3475 0.8257 0.112 Uiso 1 1 calc R . . C20 C 0.5796(3) 0.14787(15) 0.9063(3) 0.0460(6) Uani 1 1 d . . . C21 C 0.5441(4) 0.27829(16) 0.9396(3) 0.0641(8) Uani 1 1 d . . . H21A H 0.4903 0.3220 0.8983 0.096 Uiso 1 1 calc R . . H21B H 0.6609 0.2815 0.9483 0.096 Uiso 1 1 calc R . . H21C H 0.5267 0.2730 1.0261 0.096 Uiso 1 1 calc R . . C22 C 0.1319(3) -0.01228(16) 0.5587(3) 0.0524(7) Uani 1 1 d . . . C23 C 0.1105(4) -0.08856(18) 0.5009(3) 0.0693(9) Uani 1 1 d . . . H23A H 0.0594 -0.1192 0.5543 0.083 Uiso 1 1 calc R . . H23B H 0.0360 -0.0866 0.4117 0.083 Uiso 1 1 calc R . . C24 C 0.2686(4) -0.12260(18) 0.4952(3) 0.0714(9) Uani 1 1 d . . . H24A H 0.3184 -0.0941 0.4380 0.086 Uiso 1 1 calc R . . H24B H 0.2485 -0.1717 0.4591 0.086 Uiso 1 1 calc R . . C25 C 0.3822(4) -0.12517(17) 0.6329(3) 0.0679(9) Uani 1 1 d . . . H25A H 0.4863 -0.1472 0.6299 0.082 Uiso 1 1 calc R . . H25B H 0.3335 -0.1563 0.6872 0.082 Uiso 1 1 calc R . . C26 C 0.4164(3) -0.05170(13) 0.6973(3) 0.0428(6) Uani 1 1 d . . . C27 C 0.1662(6) 0.0425(2) 0.4658(3) 0.0875(12) Uani 1 1 d . . . H27A H 0.1985 0.0879 0.5120 0.131 Uiso 1 1 calc R . . H27B H 0.0681 0.0500 0.3938 0.131 Uiso 1 1 calc R . . H27C H 0.2541 0.0252 0.4313 0.131 Uiso 1 1 calc R . . C28 C -0.0244(4) 0.0063(2) 0.5919(4) 0.0874(12) Uani 1 1 d . . . H28A H -0.0409 -0.0272 0.6578 0.131 Uiso 1 1 calc R . . H28B H -0.1159 0.0028 0.5132 0.131 Uiso 1 1 calc R . . H28C H -0.0174 0.0553 0.6261 0.131 Uiso 1 1 calc R . . C29 C 0.5296(4) -0.0090(2) 0.6367(3) 0.0707(9) Uani 1 1 d . . . H29A H 0.4897 -0.0115 0.5415 0.106 Uiso 1 1 calc R . . H29B H 0.6393 -0.0293 0.6652 0.106 Uiso 1 1 calc R . . H29C H 0.5323 0.0412 0.6646 0.106 Uiso 1 1 calc R . . C30 C 0.4996(4) -0.06117(17) 0.8418(3) 0.0597(8) Uani 1 1 d . . . H30A H 0.5291 -0.0141 0.8821 0.090 Uiso 1 1 calc R . . H30B H 0.5978 -0.0902 0.8529 0.090 Uiso 1 1 calc R . . H30C H 0.4254 -0.0853 0.8835 0.090 Uiso 1 1 calc R . . H1N H 0.207(4) -0.0373(17) 0.754(3) 0.069(9) Uiso 1 1 d . . . H1A H 0.300(4) 0.0331(15) 0.973(3) 0.049(7) Uiso 1 1 d . . . H1B H 0.132(4) 0.0490(17) 0.899(3) 0.060(8) Uiso 1 1 d . . . H5A H 0.569(4) 0.1832(15) 1.166(3) 0.056(8) Uiso 1 1 d . . . H5B H 0.438(3) 0.2213(16) 1.214(3) 0.048(7) Uiso 1 1 d . . . H9A H -0.013(4) 0.166(2) 1.062(3) 0.079(9) Uiso 1 1 d . . . H9B H 0.024(5) 0.240(2) 1.020(4) 0.100(14) Uiso 1 1 d . . . H20A H 0.552(3) 0.1043(18) 0.852(3) 0.058(8) Uiso 1 1 d . . . H20B H 0.575(3) 0.1280(14) 0.989(3) 0.047(7) Uiso 1 1 d . . . H20C H 0.685(5) 0.155(2) 0.905(3) 0.092(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0333(3) 0.0404(4) 0.0307(3) -0.0010(3) 0.0069(2) 0.0060(3) Li1 0.043(2) 0.040(2) 0.040(2) -0.0020(18) 0.0106(18) 0.0053(18) N1 0.0399(10) 0.0308(10) 0.0333(10) 0.0019(8) 0.0083(8) 0.0074(8) N2 0.0449(12) 0.0410(12) 0.0391(11) -0.0036(10) 0.0094(9) 0.0008(9) C1 0.0419(14) 0.0480(15) 0.0370(14) -0.0025(12) 0.0121(11) 0.0011(12) C2 0.059(2) 0.072(2) 0.137(4) 0.024(2) 0.044(2) 0.0010(17) C3 0.0559(16) 0.0533(16) 0.0473(15) 0.0014(13) 0.0217(13) -0.0083(13) C4 0.071(2) 0.076(2) 0.124(3) 0.044(2) 0.034(2) 0.0010(19) C5 0.0377(13) 0.0525(18) 0.0399(13) -0.0031(13) 0.0040(10) 0.0044(12) C6 0.070(2) 0.062(2) 0.061(2) 0.0109(16) -0.0066(16) 0.0103(16) C7 0.0490(16) 0.072(2) 0.0464(16) 0.0128(14) 0.0086(13) 0.0001(14) C8 0.081(2) 0.090(3) 0.0326(14) 0.0083(15) 0.0036(13) 0.0018(18) C9 0.0359(14) 0.070(2) 0.0529(17) -0.0170(16) 0.0101(12) 0.0069(15) C10 0.068(2) 0.113(3) 0.066(2) -0.008(2) 0.0348(17) -0.007(2) C11 0.0421(14) 0.0570(17) 0.0448(15) -0.0064(12) 0.0145(11) 0.0032(12) C12 0.071(2) 0.061(2) 0.098(3) -0.0193(19) 0.0210(19) -0.0033(17) C13 0.0664(18) 0.0488(16) 0.0356(14) 0.0045(12) 0.0077(12) 0.0260(13) C14 0.103(3) 0.0577(19) 0.0413(16) 0.0109(14) 0.0144(16) 0.0352(18) C15 0.125(3) 0.057(2) 0.061(2) 0.0204(17) 0.043(2) 0.011(2) C16 0.079(2) 0.0584(19) 0.0587(18) 0.0060(15) 0.0368(16) -0.0061(15) C17 0.0520(15) 0.0359(13) 0.0449(14) -0.0002(11) 0.0182(11) -0.0025(11) C18 0.0518(17) 0.096(2) 0.0449(16) 0.0006(17) -0.0014(13) 0.0317(17) C19 0.112(3) 0.0547(19) 0.0552(19) 0.0046(15) 0.0192(18) 0.0452(19) C20 0.0385(14) 0.0470(18) 0.0553(17) -0.0035(14) 0.0175(12) 0.0014(11) C21 0.079(2) 0.0439(16) 0.068(2) -0.0040(14) 0.0182(16) -0.0173(15) C22 0.0555(16) 0.0501(16) 0.0426(15) -0.0094(13) -0.0016(12) -0.0007(13) C23 0.078(2) 0.064(2) 0.0554(19) -0.0150(16) 0.0000(16) -0.0121(17) C24 0.089(2) 0.0551(19) 0.067(2) -0.0293(16) 0.0158(18) -0.0039(17) C25 0.074(2) 0.0501(18) 0.076(2) -0.0216(16) 0.0156(17) 0.0096(15) C26 0.0451(14) 0.0386(14) 0.0464(15) -0.0071(11) 0.0156(11) 0.0012(11) C27 0.134(3) 0.073(2) 0.0424(18) 0.0086(17) 0.002(2) -0.011(2) C28 0.057(2) 0.114(3) 0.075(2) -0.013(2) -0.0091(17) 0.006(2) C29 0.067(2) 0.080(2) 0.074(2) -0.0151(19) 0.0363(17) -0.0171(17) C30 0.0611(18) 0.0551(17) 0.0573(18) -0.0015(14) 0.0069(14) 0.0141(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.995(2) . ? Al1 C5 2.027(2) . ? Al1 C9 2.039(3) . ? Al1 C1 2.045(3) . ? Al1 Li1 2.837(4) . ? Li1 N1 2.064(5) . ? Li1 N2 2.165(5) . ? Li1 C1 2.309(5) . ? Li1 C20 2.781(5) . ? Li1 H1A 2.13(3) . ? Li1 H1B 2.01(3) . ? Li1 H20A 2.30(3) . ? N1 C13 1.496(3) . ? N1 C17 1.508(3) . ? N2 C26 1.508(3) . ? N2 C22 1.515(3) . ? N2 H1N 1.07(3) . ? C1 C3 1.557(4) . ? C1 H1A 0.96(3) . ? C1 H1B 0.95(3) . ? C2 C3 1.520(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.510(5) . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.525(4) . ? C5 H5A 0.98(3) . ? C5 H5B 0.97(3) . ? C6 C7 1.522(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.539(4) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.518(4) . ? C9 H9A 1.03(4) . ? C9 H9B 0.91(5) . ? C10 C11 1.524(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.486(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.537(5) . ? C13 C19 1.548(4) . ? C13 C14 1.549(4) . ? C14 C15 1.502(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.510(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.537(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C20 1.528(4) . ? C17 C21 1.534(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.99(3) . ? C20 H20B 0.96(3) . ? C20 H20C 0.91(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.507(5) . ? C22 C28 1.515(5) . ? C22 C23 1.541(4) . ? C23 C24 1.511(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.524(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.524(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C30 1.520(4) . ? C26 C29 1.528(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 C5 114.49(10) . . ? N1 Al1 C9 118.22(12) . . ? C5 Al1 C9 105.76(12) . . ? N1 Al1 C1 99.80(9) . . ? C5 Al1 C1 113.05(12) . . ? C9 Al1 C1 105.27(13) . . ? N1 Al1 Li1 46.66(10) . . ? C5 Al1 Li1 123.82(12) . . ? C9 Al1 Li1 130.20(12) . . ? C1 Al1 Li1 53.50(11) . . ? N1 Li1 N2 165.6(2) . . ? N1 Li1 C1 89.75(17) . . ? N2 Li1 C1 104.6(2) . . ? N1 Li1 C20 58.49(13) . . ? N2 Li1 C20 118.19(18) . . ? C1 Li1 C20 99.08(17) . . ? N1 Li1 Al1 44.66(9) . . ? N2 Li1 Al1 149.6(2) . . ? C1 Li1 Al1 45.39(10) . . ? C20 Li1 Al1 71.33(12) . . ? N1 Li1 H1A 101.9(8) . . ? N2 Li1 H1A 91.6(8) . . ? C1 Li1 H1A 24.5(8) . . ? C20 Li1 H1A 87.5(8) . . ? Al1 Li1 H1A 59.0(8) . . ? N1 Li1 H1B 102.0(9) . . ? N2 Li1 H1B 91.3(9) . . ? C1 Li1 H1B 24.3(9) . . ? C20 Li1 H1B 123.3(10) . . ? Al1 Li1 H1B 62.3(9) . . ? H1A Li1 H1B 41.5(11) . . ? N1 Li1 H20A 77.3(9) . . ? N2 Li1 H20A 98.5(9) . . ? C1 Li1 H20A 106.9(7) . . ? C20 Li1 H20A 19.7(8) . . ? Al1 Li1 H20A 88.8(8) . . ? H1A Li1 H20A 88.8(11) . . ? H1B Li1 H20A 129.8(12) . . ? C13 N1 C17 114.1(2) . . ? C13 N1 Al1 115.94(15) . . ? C17 N1 Al1 117.34(14) . . ? C13 N1 Li1 112.91(19) . . ? C17 N1 Li1 104.19(17) . . ? Al1 N1 Li1 88.69(14) . . ? C26 N2 C22 117.6(2) . . ? C26 N2 Li1 118.72(18) . . ? C22 N2 Li1 114.3(2) . . ? C26 N2 H1N 104.9(16) . . ? C22 N2 H1N 104.6(17) . . ? Li1 N2 H1N 91.0(17) . . ? C3 C1 Al1 117.37(18) . . ? C3 C1 Li1 160.8(2) . . ? Al1 C1 Li1 81.11(14) . . ? C3 C1 H1A 108.6(16) . . ? Al1 C1 H1A 108.7(16) . . ? Li1 C1 H1A 67.0(16) . . ? C3 C1 H1B 104.1(18) . . ? Al1 C1 H1B 115.8(19) . . ? Li1 C1 H1B 60.2(18) . . ? H1A C1 H1B 101(2) . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 C2 107.8(3) . . ? C4 C3 C1 113.1(2) . . ? C2 C3 C1 112.1(3) . . ? C4 C3 H3 107.9 . . ? C2 C3 H3 107.9 . . ? C1 C3 H3 107.9 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 Al1 120.2(2) . . ? C7 C5 H5A 101.2(16) . . ? Al1 C5 H5A 118.3(16) . . ? C7 C5 H5B 111.8(16) . . ? Al1 C5 H5B 101.1(16) . . ? H5A C5 H5B 103(2) . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C6 C7 C5 112.1(2) . . ? C6 C7 C8 109.1(3) . . ? C5 C7 C8 111.6(3) . . ? C6 C7 H7 108.0 . . ? C5 C7 H7 108.0 . . ? C8 C7 H7 108.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 Al1 119.84(19) . . ? C11 C9 H9A 107.1(17) . . ? Al1 C9 H9A 106.3(19) . . ? C11 C9 H9B 109(3) . . ? Al1 C9 H9B 111(3) . . ? H9A C9 H9B 102(3) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 112.2(3) . . ? C12 C11 C10 109.7(3) . . ? C9 C11 C10 111.9(2) . . ? C12 C11 H11 107.6 . . ? C9 C11 H11 107.6 . . ? C10 C11 H11 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C18 107.6(2) . . ? N1 C13 C19 114.5(2) . . ? C18 C13 C19 108.2(3) . . ? N1 C13 C14 111.8(2) . . ? C18 C13 C14 106.6(2) . . ? C19 C13 C14 107.8(2) . . ? C15 C14 C13 113.8(3) . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 107.5(3) . . ? C14 C15 H15A 110.2 . . ? C16 C15 H15A 110.2 . . ? C14 C15 H15B 110.2 . . ? C16 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C15 C16 C17 113.8(3) . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16B 108.8 . . ? C17 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N1 C17 C20 107.4(2) . . ? N1 C17 C21 114.4(2) . . ? C20 C17 C21 108.6(2) . . ? N1 C17 C16 111.8(2) . . ? C20 C17 C16 105.7(2) . . ? C21 C17 C16 108.5(2) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 Li1 76.36(17) . . ? C17 C20 H20A 115.0(17) . . ? Li1 C20 H20A 51.8(17) . . ? C17 C20 H20B 117.4(15) . . ? Li1 C20 H20B 88.5(16) . . ? H20A C20 H20B 99(2) . . ? C17 C20 H20C 112(2) . . ? Li1 C20 H20C 150(2) . . ? H20A C20 H20C 100(3) . . ? H20B C20 H20C 110(3) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 N2 111.1(3) . . ? C27 C22 C28 110.1(3) . . ? N2 C22 C28 104.8(2) . . ? C27 C22 C23 112.7(3) . . ? N2 C22 C23 110.9(2) . . ? C28 C22 C23 106.8(3) . . ? C24 C23 C22 113.3(3) . . ? C24 C23 H23A 108.9 . . ? C22 C23 H23A 108.9 . . ? C24 C23 H23B 108.9 . . ? C22 C23 H23B 108.9 . . ? H23A C23 H23B 107.7 . . ? C23 C24 C25 108.3(3) . . ? C23 C24 H24A 110.0 . . ? C25 C24 H24A 110.0 . . ? C23 C24 H24B 110.0 . . ? C25 C24 H24B 110.0 . . ? H24A C24 H24B 108.4 . . ? C24 C25 C26 113.6(3) . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N2 C26 C30 106.5(2) . . ? N2 C26 C25 111.5(2) . . ? C30 C26 C25 109.4(2) . . ? N2 C26 C29 110.9(2) . . ? C30 C26 C29 108.4(2) . . ? C25 C26 C29 110.0(2) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C22 C28 H28A 109.5 . . ? C22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Al1 Li1 N1 -93.07(16) . . . . ? C9 Al1 Li1 N1 93.1(2) . . . . ? C1 Al1 Li1 N1 171.74(19) . . . . ? N1 Al1 Li1 N2 177.9(5) . . . . ? C5 Al1 Li1 N2 84.8(4) . . . . ? C9 Al1 Li1 N2 -89.0(4) . . . . ? C1 Al1 Li1 N2 -10.4(3) . . . . ? N1 Al1 Li1 C1 -171.74(19) . . . . ? C5 Al1 Li1 C1 95.19(16) . . . . ? C9 Al1 Li1 C1 -78.7(2) . . . . ? N1 Al1 Li1 C20 63.70(13) . . . . ? C5 Al1 Li1 C20 -29.37(17) . . . . ? C9 Al1 Li1 C20 156.78(17) . . . . ? C1 Al1 Li1 C20 -124.56(16) . . . . ? C5 Al1 N1 C13 -130.76(19) . . . . ? C9 Al1 N1 C13 -5.1(2) . . . . ? C1 Al1 N1 C13 108.23(19) . . . . ? Li1 Al1 N1 C13 115.0(2) . . . . ? C5 Al1 N1 C17 8.96(19) . . . . ? C9 Al1 N1 C17 134.62(17) . . . . ? C1 Al1 N1 C17 -112.05(17) . . . . ? Li1 Al1 N1 C17 -105.3(2) . . . . ? C5 Al1 N1 Li1 114.28(16) . . . . ? C9 Al1 N1 Li1 -120.06(16) . . . . ? C1 Al1 N1 Li1 -6.73(15) . . . . ? N2 Li1 N1 C13 66.6(10) . . . . ? C1 Li1 N1 C13 -111.86(19) . . . . ? C20 Li1 N1 C13 147.32(19) . . . . ? Al1 Li1 N1 C13 -117.73(19) . . . . ? N2 Li1 N1 C17 -57.8(10) . . . . ? C1 Li1 N1 C17 123.78(17) . . . . ? C20 Li1 N1 C17 22.96(15) . . . . ? Al1 Li1 N1 C17 117.91(16) . . . . ? N2 Li1 N1 Al1 -175.7(9) . . . . ? C1 Li1 N1 Al1 5.87(13) . . . . ? C20 Li1 N1 Al1 -94.95(11) . . . . ? N1 Li1 N2 C26 83.3(10) . . . . ? C1 Li1 N2 C26 -98.3(2) . . . . ? C20 Li1 N2 C26 10.6(3) . . . . ? Al1 Li1 N2 C26 -90.7(4) . . . . ? N1 Li1 N2 C22 -62.5(10) . . . . ? C1 Li1 N2 C22 115.9(2) . . . . ? C20 Li1 N2 C22 -135.2(2) . . . . ? Al1 Li1 N2 C22 123.5(4) . . . . ? N1 Al1 C1 C3 -168.3(2) . . . . ? C5 Al1 C1 C3 69.7(2) . . . . ? C9 Al1 C1 C3 -45.3(2) . . . . ? Li1 Al1 C1 C3 -174.4(3) . . . . ? N1 Al1 C1 Li1 6.09(14) . . . . ? C5 Al1 C1 Li1 -115.96(15) . . . . ? C9 Al1 C1 Li1 129.08(15) . . . . ? N1 Li1 C1 C3 158.9(6) . . . . ? N2 Li1 C1 C3 -20.7(7) . . . . ? C20 Li1 C1 C3 -143.2(6) . . . . ? Al1 Li1 C1 C3 164.7(7) . . . . ? N1 Li1 C1 Al1 -5.80(13) . . . . ? N2 Li1 C1 Al1 174.60(17) . . . . ? C20 Li1 C1 Al1 52.20(14) . . . . ? Al1 C1 C3 C4 -137.1(3) . . . . ? Li1 C1 C3 C4 60.0(8) . . . . ? Al1 C1 C3 C2 100.8(3) . . . . ? Li1 C1 C3 C2 -62.1(8) . . . . ? N1 Al1 C5 C7 -140.7(2) . . . . ? C9 Al1 C5 C7 87.4(3) . . . . ? C1 Al1 C5 C7 -27.3(3) . . . . ? Li1 Al1 C5 C7 -87.7(3) . . . . ? Al1 C5 C7 C6 80.9(3) . . . . ? Al1 C5 C7 C8 -156.4(2) . . . . ? N1 Al1 C9 C11 -134.2(2) . . . . ? C5 Al1 C9 C11 -4.4(3) . . . . ? C1 Al1 C9 C11 115.6(3) . . . . ? Li1 Al1 C9 C11 170.3(2) . . . . ? Al1 C9 C11 C12 86.9(3) . . . . ? Al1 C9 C11 C10 -149.2(3) . . . . ? C17 N1 C13 C18 163.9(2) . . . . ? Al1 N1 C13 C18 -55.1(2) . . . . ? Li1 N1 C13 C18 45.2(3) . . . . ? C17 N1 C13 C19 -75.9(3) . . . . ? Al1 N1 C13 C19 65.2(3) . . . . ? Li1 N1 C13 C19 165.4(3) . . . . ? C17 N1 C13 C14 47.2(3) . . . . ? Al1 N1 C13 C14 -171.8(2) . . . . ? Li1 N1 C13 C14 -71.5(3) . . . . ? N1 C13 C14 C15 -53.3(3) . . . . ? C18 C13 C14 C15 -170.6(3) . . . . ? C19 C13 C14 C15 73.5(3) . . . . ? C13 C14 C15 C16 56.8(3) . . . . ? C14 C15 C16 C17 -57.0(4) . . . . ? C13 N1 C17 C20 -163.0(2) . . . . ? Al1 N1 C17 C20 56.6(2) . . . . ? Li1 N1 C17 C20 -39.4(2) . . . . ? C13 N1 C17 C21 76.4(3) . . . . ? Al1 N1 C17 C21 -64.1(2) . . . . ? Li1 N1 C17 C21 -160.1(2) . . . . ? C13 N1 C17 C16 -47.4(3) . . . . ? Al1 N1 C17 C16 172.12(17) . . . . ? Li1 N1 C17 C16 76.1(2) . . . . ? C15 C16 C17 N1 53.3(3) . . . . ? C15 C16 C17 C20 169.9(3) . . . . ? C15 C16 C17 C21 -73.7(3) . . . . ? N1 C17 C20 Li1 28.02(17) . . . . ? C21 C17 C20 Li1 152.3(2) . . . . ? C16 C17 C20 Li1 -91.5(2) . . . . ? N1 Li1 C20 C17 -22.59(15) . . . . ? N2 Li1 C20 C17 141.3(2) . . . . ? C1 Li1 C20 C17 -106.7(2) . . . . ? Al1 Li1 C20 C17 -70.25(15) . . . . ? C26 N2 C22 C27 -82.5(3) . . . . ? Li1 N2 C22 C27 63.7(3) . . . . ? C26 N2 C22 C28 158.6(3) . . . . ? Li1 N2 C22 C28 -55.2(3) . . . . ? C26 N2 C22 C23 43.7(3) . . . . ? Li1 N2 C22 C23 -170.1(2) . . . . ? C27 C22 C23 C24 74.0(4) . . . . ? N2 C22 C23 C24 -51.3(4) . . . . ? C28 C22 C23 C24 -165.0(3) . . . . ? C22 C23 C24 C25 58.5(4) . . . . ? C23 C24 C25 C26 -58.2(4) . . . . ? C22 N2 C26 C30 -162.7(2) . . . . ? Li1 N2 C26 C30 52.6(3) . . . . ? C22 N2 C26 C25 -43.5(3) . . . . ? Li1 N2 C26 C25 171.8(2) . . . . ? C22 N2 C26 C29 79.5(3) . . . . ? Li1 N2 C26 C29 -65.2(3) . . . . ? C24 C25 C26 N2 50.5(3) . . . . ? C24 C25 C26 C30 168.0(3) . . . . ? C24 C25 C26 C29 -73.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.302 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.036 ############################################################ ########### COMPOUND 2 ################################### ######################################################### data_grem253 _database_code_depnum_ccdc_archive 'CCDC 634094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H60 Al Li N2' _chemical_formula_weight 446.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5683(7) _cell_length_b 11.0648(7) _cell_length_c 14.9605(7) _cell_angle_alpha 96.822(4) _cell_angle_beta 105.870(3) _cell_angle_gamma 113.030(3) _cell_volume 1497.42(15) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 5202 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.02 _exptl_crystal_description 'cut needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10472 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.1020 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5850 _reflns_number_gt 3535 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SHELXS _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^)+(0.0318P)^2^+0.6125P] 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 5850 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1211 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.07713(8) 0.16497(7) 0.77266(4) 0.02075(18) Uani 1 1 d . . . Li1 Li 0.3269(4) 0.2650(4) 0.7263(3) 0.0288(9) Uani 1 1 d . . . N1 N 0.16400(19) 0.32196(17) 0.71847(11) 0.0180(4) Uani 1 1 d . . . N2 N 0.51694(19) 0.28958(18) 0.69580(12) 0.0239(5) Uani 1 1 d . . . C1 C 0.2378(3) 0.1007(3) 0.7962(2) 0.0301(6) Uani 1 1 d . . . C2 C 0.2056(3) -0.0281(2) 0.83424(17) 0.0317(6) Uani 1 1 d . . . H2 H 0.1385 -0.0317 0.8709 0.038 Uiso 1 1 calc R . . C3 C 0.3431(3) -0.0268(3) 0.9027(2) 0.0646(10) Uani 1 1 d . . . H3A H 0.3161 -0.1097 0.9253 0.097 Uiso 1 1 calc R . . H3B H 0.3898 0.0526 0.9577 0.097 Uiso 1 1 calc R . . H3C H 0.4117 -0.0223 0.8690 0.097 Uiso 1 1 calc R . . C4 C 0.1270(3) -0.1559(3) 0.75257(19) 0.0479(8) Uani 1 1 d . . . H4A H 0.1931 -0.1590 0.7184 0.072 Uiso 1 1 calc R . . H4B H 0.0399 -0.1555 0.7080 0.072 Uiso 1 1 calc R . . H4C H 0.0973 -0.2357 0.7785 0.072 Uiso 1 1 calc R . . C5 C -0.1134(3) 0.0055(3) 0.68367(17) 0.0286(6) Uani 1 1 d . . . C6 C -0.2047(3) -0.0981(2) 0.72981(16) 0.0272(6) Uani 1 1 d . . . H6 H -0.1357 -0.0982 0.7908 0.033 Uiso 1 1 calc R . . C7 C -0.2856(3) -0.2428(2) 0.66454(18) 0.0444(7) Uani 1 1 d . . . H7A H -0.3388 -0.3051 0.6974 0.067 Uiso 1 1 calc R . . H7B H -0.2145 -0.2703 0.6498 0.067 Uiso 1 1 calc R . . H7C H -0.3554 -0.2455 0.6047 0.067 Uiso 1 1 calc R . . C8 C -0.3171(3) -0.0605(3) 0.75432(18) 0.0374(7) Uani 1 1 d . . . H8A H -0.3898 -0.0659 0.6950 0.056 Uiso 1 1 calc R . . H8B H -0.2676 0.0323 0.7955 0.056 Uiso 1 1 calc R . . H8C H -0.3664 -0.1237 0.7882 0.056 Uiso 1 1 calc R . . C9 C 0.0329(3) 0.2028(3) 0.89299(15) 0.0233(5) Uani 1 1 d . . . C10 C 0.1310(3) 0.2861(2) 0.99650(15) 0.0283(6) Uani 1 1 d . . . H10 H 0.1905 0.3811 0.9948 0.034 Uiso 1 1 calc R . . C11 C 0.2367(3) 0.2289(3) 1.04053(16) 0.0389(7) Uani 1 1 d . . . H11A H 0.2971 0.2826 1.1068 0.058 Uiso 1 1 calc R . . H11B H 0.3001 0.2330 1.0028 0.058 Uiso 1 1 calc R . . H11C H 0.1806 0.1342 1.0403 0.058 Uiso 1 1 calc R . . C12 C 0.0391(3) 0.2908(3) 1.05881(17) 0.0435(7) Uani 1 1 d . . . H12A H -0.0254 0.1981 1.0576 0.065 Uiso 1 1 calc R . . H12B H -0.0204 0.3367 1.0337 0.065 Uiso 1 1 calc R . . H12C H 0.1043 0.3407 1.1250 0.065 Uiso 1 1 calc R . . C13 C 0.0799(2) 0.3144(2) 0.61690(15) 0.0217(5) Uani 1 1 d . . . C14 C 0.1662(3) 0.4321(2) 0.57920(15) 0.0267(6) Uani 1 1 d . . . H14A H 0.2488 0.4186 0.5686 0.032 Uiso 1 1 calc R . . H14B H 0.1010 0.4287 0.5163 0.032 Uiso 1 1 calc R . . C15 C 0.2269(3) 0.5716(2) 0.64595(16) 0.0293(6) Uani 1 1 d . . . H15A H 0.1454 0.5907 0.6526 0.035 Uiso 1 1 calc R . . H15B H 0.2860 0.6421 0.6197 0.035 Uiso 1 1 calc R . . C16 C 0.3219(3) 0.5729(2) 0.74312(15) 0.0268(6) Uani 1 1 d . . . H16A H 0.3603 0.6627 0.7880 0.032 Uiso 1 1 calc R . . H16B H 0.4069 0.5608 0.7359 0.032 Uiso 1 1 calc R . . C17 C 0.2395(2) 0.4615(2) 0.78713(15) 0.0230(5) Uani 1 1 d . . . C18 C 0.0557(3) 0.1839(2) 0.55138(15) 0.0262(6) Uani 1 1 d . . . H18A H 0.1508 0.1848 0.5575 0.039 Uiso 1 1 calc R . . H18B H 0.0046 0.1785 0.4845 0.039 Uiso 1 1 calc R . . H18C H -0.0037 0.1051 0.5702 0.039 Uiso 1 1 calc R . . C19 C -0.0713(2) 0.3111(2) 0.60391(16) 0.0288(6) Uani 1 1 d . . . H19A H -0.1212 0.2480 0.6376 0.043 Uiso 1 1 calc R . . H19B H -0.1307 0.2810 0.5353 0.043 Uiso 1 1 calc R . . H19C H -0.0582 0.4023 0.6306 0.043 Uiso 1 1 calc R . . C20 C 0.3571(3) 0.4606(3) 0.87313(17) 0.0264(6) Uani 1 1 d . . . C21 C 0.1372(3) 0.5035(2) 0.82489(16) 0.0270(6) Uani 1 1 d . . . H21A H 0.0704 0.5183 0.7724 0.040 Uiso 1 1 calc R . . H21B H 0.1960 0.5875 0.8764 0.040 Uiso 1 1 calc R . . H21C H 0.0801 0.4313 0.8500 0.040 Uiso 1 1 calc R . . C22 C 0.5186(3) 0.1576(2) 0.66584(16) 0.0277(6) Uani 1 1 d . . . H22A H 0.5182 0.1131 0.7195 0.033 Uiso 1 1 calc R . . H22B H 0.6112 0.1753 0.6541 0.033 Uiso 1 1 calc R . . C23 C 0.3908(3) 0.0603(2) 0.57643(16) 0.0347(6) Uani 1 1 d . . . H23A H 0.2982 0.0484 0.5849 0.052 Uiso 1 1 calc R . . H23B H 0.3934 -0.0277 0.5660 0.052 Uiso 1 1 calc R . . H23C H 0.3982 0.0973 0.5207 0.052 Uiso 1 1 calc R . . C24 C 0.6533(3) 0.3787(3) 0.77913(16) 0.0336(6) Uani 1 1 d . . . H24A H 0.6560 0.4693 0.7951 0.040 Uiso 1 1 calc R . . H24B H 0.7390 0.3904 0.7598 0.040 Uiso 1 1 calc R . . C25 C 0.6689(3) 0.3264(3) 0.86877(17) 0.0397(7) Uani 1 1 d . . . H25A H 0.5815 0.3082 0.8862 0.060 Uiso 1 1 calc R . . H25B H 0.7559 0.3948 0.9217 0.060 Uiso 1 1 calc R . . H25C H 0.6793 0.2424 0.8564 0.060 Uiso 1 1 calc R . . C26 C 0.5070(3) 0.3594(2) 0.61681(16) 0.0284(6) Uani 1 1 d . . . H26A H 0.5066 0.4462 0.6418 0.034 Uiso 1 1 calc R . . H26B H 0.4110 0.3027 0.5650 0.034 Uiso 1 1 calc R . . C27 C 0.6257(3) 0.3906(3) 0.57212(18) 0.0389(7) Uani 1 1 d . . . H27A H 0.7215 0.4507 0.6215 0.058 Uiso 1 1 calc R . . H27B H 0.6056 0.4352 0.5209 0.058 Uiso 1 1 calc R . . H27C H 0.6265 0.3057 0.5453 0.058 Uiso 1 1 calc R . . H1A H 0.264(3) 0.083(3) 0.7397(18) 0.050(8) Uiso 1 1 d . . . H1B H 0.328(3) 0.174(2) 0.8453(16) 0.034(7) Uiso 1 1 d . . . H5A H -0.181(3) 0.032(2) 0.6421(17) 0.039(7) Uiso 1 1 d . . . H5B H -0.086(3) -0.044(2) 0.6400(16) 0.035(7) Uiso 1 1 d . . . H9A H -0.050(2) 0.230(2) 0.8721(15) 0.028(6) Uiso 1 1 d . . . H9B H -0.021(2) 0.111(2) 0.8984(14) 0.026(6) Uiso 1 1 d . . . H20A H 0.406(2) 0.548(2) 0.9236(16) 0.033(7) Uiso 1 1 d . . . H20B H 0.437(2) 0.451(2) 0.8533(14) 0.022(6) Uiso 1 1 d . . . H20C H 0.317(2) 0.392(2) 0.9057(14) 0.024(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0245(4) 0.0187(4) 0.0201(3) 0.0066(3) 0.0088(3) 0.0095(3) Li1 0.028(2) 0.029(2) 0.033(2) 0.0113(18) 0.0149(18) 0.0126(19) N1 0.0225(10) 0.0150(10) 0.0174(9) 0.0043(7) 0.0074(8) 0.0089(8) N2 0.0210(10) 0.0212(11) 0.0284(10) 0.0043(8) 0.0074(9) 0.0097(9) C1 0.0391(16) 0.0270(15) 0.0365(15) 0.0158(13) 0.0192(14) 0.0207(14) C2 0.0376(15) 0.0297(15) 0.0409(15) 0.0205(12) 0.0200(13) 0.0204(13) C3 0.057(2) 0.057(2) 0.092(2) 0.0438(19) 0.0179(19) 0.0364(18) C4 0.073(2) 0.0330(17) 0.0570(18) 0.0209(14) 0.0340(17) 0.0328(16) C5 0.0344(15) 0.0216(14) 0.0245(13) 0.0072(11) 0.0089(12) 0.0077(12) C6 0.0298(14) 0.0209(14) 0.0256(12) 0.0073(10) 0.0070(11) 0.0073(12) C7 0.0529(18) 0.0238(15) 0.0408(15) 0.0049(12) 0.0178(14) 0.0017(14) C8 0.0296(15) 0.0325(16) 0.0451(16) 0.0140(12) 0.0101(13) 0.0096(13) C9 0.0243(14) 0.0190(14) 0.0241(13) 0.0051(10) 0.0110(11) 0.0057(12) C10 0.0316(14) 0.0226(14) 0.0234(12) 0.0044(10) 0.0122(11) 0.0035(12) C11 0.0402(16) 0.0364(16) 0.0239(13) 0.0055(11) 0.0038(12) 0.0067(14) C12 0.0465(17) 0.0406(17) 0.0300(14) 0.0009(12) 0.0201(13) 0.0040(14) C13 0.0220(13) 0.0243(13) 0.0231(12) 0.0095(10) 0.0106(10) 0.0116(11) C14 0.0296(14) 0.0301(15) 0.0298(13) 0.0158(11) 0.0150(11) 0.0172(12) C15 0.0399(15) 0.0231(14) 0.0380(14) 0.0180(11) 0.0245(12) 0.0166(12) C16 0.0315(14) 0.0186(13) 0.0322(13) 0.0065(10) 0.0173(12) 0.0089(11) C17 0.0272(13) 0.0206(13) 0.0243(12) 0.0073(10) 0.0122(11) 0.0109(11) C18 0.0289(14) 0.0314(15) 0.0206(12) 0.0089(10) 0.0103(11) 0.0138(12) C19 0.0264(14) 0.0344(15) 0.0309(13) 0.0128(11) 0.0108(11) 0.0170(12) C20 0.0272(15) 0.0240(15) 0.0244(13) 0.0030(12) 0.0101(12) 0.0081(12) C21 0.0360(15) 0.0197(14) 0.0306(13) 0.0081(10) 0.0178(12) 0.0130(12) C22 0.0266(14) 0.0278(15) 0.0304(13) 0.0050(11) 0.0109(11) 0.0137(12) C23 0.0366(15) 0.0285(15) 0.0365(14) 0.0028(12) 0.0105(12) 0.0151(13) C24 0.0231(14) 0.0315(15) 0.0381(14) 0.0002(12) 0.0071(12) 0.0088(12) C25 0.0325(15) 0.0395(17) 0.0354(15) -0.0012(12) -0.0003(12) 0.0157(14) C26 0.0261(14) 0.0268(14) 0.0360(14) 0.0114(11) 0.0139(11) 0.0125(12) C27 0.0335(15) 0.0438(18) 0.0510(16) 0.0205(13) 0.0247(13) 0.0197(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 2.0028(18) . ? Al1 C9 2.017(2) . ? Al1 C5 2.034(2) . ? Al1 C1 2.047(3) . ? Al1 Li1 2.751(4) . ? Li1 N1 2.032(4) . ? Li1 N2 2.102(4) . ? Li1 C1 2.221(5) . ? Li1 C20 2.749(5) . ? Li1 H1A 1.92(3) . ? Li1 H1B 2.15(2) . ? Li1 H20B 2.28(2) . ? N1 C13 1.510(3) . ? N1 C17 1.512(3) . ? N2 C22 1.484(3) . ? N2 C24 1.489(3) . ? N2 C26 1.489(3) . ? C1 C2 1.546(3) . ? C1 H1A 0.98(3) . ? C1 H1B 0.99(2) . ? C2 C4 1.515(3) . ? C2 C3 1.524(3) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.552(3) . ? C5 H5A 0.98(2) . ? C5 H5B 0.97(2) . ? C6 C8 1.519(3) . ? C6 C7 1.532(3) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.535(3) . ? C9 H9A 1.02(2) . ? C9 H9B 0.98(2) . ? C10 C11 1.527(3) . ? C10 C12 1.529(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.533(3) . ? C13 C14 1.540(3) . ? C13 C19 1.541(3) . ? C14 C15 1.517(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.519(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.541(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C20 1.530(3) . ? C17 C21 1.538(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.99(2) . ? C20 H20B 1.00(2) . ? C20 H20C 0.97(2) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.518(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.516(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.522(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 C9 117.74(9) . . ? N1 Al1 C5 116.85(9) . . ? C9 Al1 C5 103.00(11) . . ? N1 Al1 C1 100.01(9) . . ? C9 Al1 C1 111.64(11) . . ? C5 Al1 C1 107.43(12) . . ? N1 Al1 Li1 47.47(10) . . ? C9 Al1 Li1 133.77(11) . . ? C5 Al1 Li1 122.91(12) . . ? C1 Al1 Li1 52.69(11) . . ? N1 Li1 N2 148.9(2) . . ? N1 Li1 C1 93.59(18) . . ? N2 Li1 C1 117.5(2) . . ? N1 Li1 C20 59.37(12) . . ? N2 Li1 C20 117.03(18) . . ? C1 Li1 C20 92.20(16) . . ? N1 Li1 Al1 46.56(10) . . ? N2 Li1 Al1 164.04(19) . . ? C1 Li1 Al1 47.15(10) . . ? C20 Li1 Al1 72.34(11) . . ? N1 Li1 H1A 109.7(8) . . ? N2 Li1 H1A 99.0(8) . . ? C1 Li1 H1A 26.1(8) . . ? C20 Li1 H1A 117.9(8) . . ? Al1 Li1 H1A 65.1(8) . . ? N1 Li1 H1B 101.3(6) . . ? N2 Li1 H1B 107.5(6) . . ? C1 Li1 H1B 26.1(6) . . ? C20 Li1 H1B 75.3(6) . . ? Al1 Li1 H1B 60.8(6) . . ? H1A Li1 H1B 45.2(9) . . ? N1 Li1 H20B 77.5(6) . . ? N2 Li1 H20B 96.8(6) . . ? C1 Li1 H20B 100.9(5) . . ? C20 Li1 H20B 20.3(6) . . ? Al1 Li1 H20B 91.5(6) . . ? H1A Li1 H20B 123.5(9) . . ? H1B Li1 H20B 78.3(8) . . ? C13 N1 C17 115.01(16) . . ? C13 N1 Al1 117.47(13) . . ? C17 N1 Al1 116.28(13) . . ? C13 N1 Li1 112.76(16) . . ? C17 N1 Li1 104.66(17) . . ? Al1 N1 Li1 85.97(13) . . ? C22 N2 C24 108.94(17) . . ? C22 N2 C26 112.27(17) . . ? C24 N2 C26 109.30(18) . . ? C22 N2 Li1 112.04(18) . . ? C24 N2 Li1 112.05(18) . . ? C26 N2 Li1 102.12(16) . . ? C2 C1 Al1 115.52(18) . . ? C2 C1 Li1 162.9(2) . . ? Al1 C1 Li1 80.15(13) . . ? C2 C1 H1A 105.9(15) . . ? Al1 C1 H1A 114.2(15) . . ? Li1 C1 H1A 59.3(15) . . ? C2 C1 H1B 106.6(13) . . ? Al1 C1 H1B 107.8(13) . . ? Li1 C1 H1B 72.6(13) . . ? H1A C1 H1B 106(2) . . ? C4 C2 C3 109.7(2) . . ? C4 C2 C1 111.4(2) . . ? C3 C2 C1 113.0(2) . . ? C4 C2 H2 107.5 . . ? C3 C2 H2 107.5 . . ? C1 C2 H2 107.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Al1 117.76(16) . . ? C6 C5 H5A 106.2(14) . . ? Al1 C5 H5A 113.8(14) . . ? C6 C5 H5B 107.3(14) . . ? Al1 C5 H5B 105.9(14) . . ? H5A C5 H5B 104.9(18) . . ? C8 C6 C7 108.2(2) . . ? C8 C6 C5 112.0(2) . . ? C7 C6 C5 112.3(2) . . ? C8 C6 H6 108.1 . . ? C7 C6 H6 108.1 . . ? C5 C6 H6 108.1 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Al1 132.71(17) . . ? C10 C9 H9A 108.0(12) . . ? Al1 C9 H9A 104.5(12) . . ? C10 C9 H9B 105.0(12) . . ? Al1 C9 H9B 101.7(12) . . ? H9A C9 H9B 100.6(17) . . ? C11 C10 C12 110.3(2) . . ? C11 C10 C9 110.8(2) . . ? C12 C10 C9 111.2(2) . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C9 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C18 107.92(17) . . ? N1 C13 C14 112.54(17) . . ? C18 C13 C14 106.08(18) . . ? N1 C13 C19 113.67(18) . . ? C18 C13 C19 108.12(18) . . ? C14 C13 C19 108.15(18) . . ? C15 C14 C13 114.04(19) . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C14 C15 C16 107.95(19) . . ? C14 C15 H15A 110.1 . . ? C16 C15 H15A 110.1 . . ? C14 C15 H15B 110.1 . . ? C16 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? C15 C16 C17 113.41(19) . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? N1 C17 C20 107.21(18) . . ? N1 C17 C21 114.46(18) . . ? C20 C17 C21 108.16(18) . . ? N1 C17 C16 112.17(17) . . ? C20 C17 C16 105.86(19) . . ? C21 C17 C16 108.55(18) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 Li1 76.77(15) . . ? C17 C20 H20A 111.4(13) . . ? Li1 C20 H20A 157.6(14) . . ? C17 C20 H20B 110.6(11) . . ? Li1 C20 H20B 52.3(12) . . ? H20A C20 H20B 105.9(18) . . ? C17 C20 H20C 112.8(12) . . ? Li1 C20 H20C 90.7(13) . . ? H20A C20 H20C 104.2(18) . . ? H20B C20 H20C 111.7(18) . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 C23 114.56(18) . . ? N2 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? N2 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C25 114.8(2) . . ? N2 C24 H24A 108.6 . . ? C25 C24 H24A 108.6 . . ? N2 C24 H24B 108.6 . . ? C25 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C27 117.7(2) . . ? N2 C26 H26A 107.9 . . ? C27 C26 H26A 107.9 . . ? N2 C26 H26B 107.9 . . ? C27 C26 H26B 107.9 . . ? H26A C26 H26B 107.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 Al1 Li1 N1 -89.77(17) . . . . ? C5 Al1 Li1 N1 97.84(14) . . . . ? C1 Al1 Li1 N1 -174.72(18) . . . . ? N1 Al1 Li1 N2 -167.4(7) . . . . ? C9 Al1 Li1 N2 102.8(7) . . . . ? C5 Al1 Li1 N2 -69.5(7) . . . . ? C1 Al1 Li1 N2 17.9(6) . . . . ? N1 Al1 Li1 C1 174.72(19) . . . . ? C9 Al1 Li1 C1 84.95(18) . . . . ? C5 Al1 Li1 C1 -87.44(16) . . . . ? N1 Al1 Li1 C20 64.22(11) . . . . ? C9 Al1 Li1 C20 -25.55(18) . . . . ? C5 Al1 Li1 C20 162.06(11) . . . . ? C1 Al1 Li1 C20 -110.50(15) . . . . ? C9 Al1 N1 C13 -121.07(15) . . . . ? C5 Al1 N1 C13 2.38(19) . . . . ? C1 Al1 N1 C13 117.87(16) . . . . ? Li1 Al1 N1 C13 113.61(19) . . . . ? C9 Al1 N1 C17 20.96(18) . . . . ? C5 Al1 N1 C17 144.41(16) . . . . ? C1 Al1 N1 C17 -100.10(16) . . . . ? Li1 Al1 N1 C17 -104.37(19) . . . . ? C9 Al1 N1 Li1 125.32(14) . . . . ? C5 Al1 N1 Li1 -111.23(16) . . . . ? C1 Al1 N1 Li1 4.26(15) . . . . ? N2 Li1 N1 C13 55.2(5) . . . . ? C1 Li1 N1 C13 -122.04(17) . . . . ? C20 Li1 N1 C13 147.53(17) . . . . ? Al1 Li1 N1 C13 -118.16(16) . . . . ? N2 Li1 N1 C17 -70.5(4) . . . . ? C1 Li1 N1 C17 112.25(17) . . . . ? C20 Li1 N1 C17 21.82(13) . . . . ? Al1 Li1 N1 C17 116.13(14) . . . . ? N2 Li1 N1 Al1 173.3(4) . . . . ? C1 Li1 N1 Al1 -3.88(14) . . . . ? C20 Li1 N1 Al1 -94.31(9) . . . . ? N1 Li1 N2 C22 -140.4(4) . . . . ? C1 Li1 N2 C22 36.4(3) . . . . ? C20 Li1 N2 C22 144.76(17) . . . . ? Al1 Li1 N2 C22 21.7(7) . . . . ? N1 Li1 N2 C24 96.8(4) . . . . ? C1 Li1 N2 C24 -86.4(2) . . . . ? C20 Li1 N2 C24 22.0(2) . . . . ? Al1 Li1 N2 C24 -101.1(7) . . . . ? N1 Li1 N2 C26 -20.1(5) . . . . ? C1 Li1 N2 C26 156.8(2) . . . . ? C20 Li1 N2 C26 -94.9(2) . . . . ? Al1 Li1 N2 C26 142.1(6) . . . . ? N1 Al1 C1 C2 -176.87(18) . . . . ? C9 Al1 C1 C2 57.8(2) . . . . ? C5 Al1 C1 C2 -54.4(2) . . . . ? Li1 Al1 C1 C2 -172.9(3) . . . . ? N1 Al1 C1 Li1 -3.95(14) . . . . ? C9 Al1 C1 Li1 -129.30(14) . . . . ? C5 Al1 C1 Li1 118.48(14) . . . . ? N1 Li1 C1 C2 161.6(7) . . . . ? N2 Li1 C1 C2 -16.8(9) . . . . ? C20 Li1 C1 C2 -139.0(7) . . . . ? Al1 Li1 C1 C2 157.7(8) . . . . ? N1 Li1 C1 Al1 3.84(14) . . . . ? N2 Li1 C1 Al1 -174.5(2) . . . . ? C20 Li1 C1 Al1 63.28(12) . . . . ? Al1 C1 C2 C4 89.7(2) . . . . ? Li1 C1 C2 C4 -65.8(8) . . . . ? Al1 C1 C2 C3 -146.3(2) . . . . ? Li1 C1 C2 C3 58.2(8) . . . . ? N1 Al1 C5 C6 -163.71(17) . . . . ? C9 Al1 C5 C6 -33.0(2) . . . . ? C1 Al1 C5 C6 85.0(2) . . . . ? Li1 Al1 C5 C6 141.38(19) . . . . ? Al1 C5 C6 C8 91.1(2) . . . . ? Al1 C5 C6 C7 -146.95(19) . . . . ? N1 Al1 C9 C10 -65.1(3) . . . . ? C5 Al1 C9 C10 164.7(2) . . . . ? C1 Al1 C9 C10 49.8(3) . . . . ? Li1 Al1 C9 C10 -8.7(3) . . . . ? Al1 C9 C10 C11 -61.6(3) . . . . ? Al1 C9 C10 C12 175.3(2) . . . . ? C17 N1 C13 C18 161.23(18) . . . . ? Al1 N1 C13 C18 -56.3(2) . . . . ? Li1 N1 C13 C18 41.3(2) . . . . ? C17 N1 C13 C14 44.5(2) . . . . ? Al1 N1 C13 C14 -172.98(14) . . . . ? Li1 N1 C13 C14 -75.4(2) . . . . ? C17 N1 C13 C19 -78.9(2) . . . . ? Al1 N1 C13 C19 63.6(2) . . . . ? Li1 N1 C13 C19 161.23(19) . . . . ? N1 C13 C14 C15 -50.9(3) . . . . ? C18 C13 C14 C15 -168.70(19) . . . . ? C19 C13 C14 C15 75.5(2) . . . . ? C13 C14 C15 C16 56.3(3) . . . . ? C14 C15 C16 C17 -57.2(3) . . . . ? C13 N1 C17 C20 -161.29(18) . . . . ? Al1 N1 C17 C20 55.8(2) . . . . ? Li1 N1 C17 C20 -37.0(2) . . . . ? C13 N1 C17 C21 78.8(2) . . . . ? Al1 N1 C17 C21 -64.2(2) . . . . ? Li1 N1 C17 C21 -156.97(18) . . . . ? C13 N1 C17 C16 -45.5(2) . . . . ? Al1 N1 C17 C16 171.55(14) . . . . ? Li1 N1 C17 C16 78.8(2) . . . . ? C15 C16 C17 N1 52.7(3) . . . . ? C15 C16 C17 C20 169.4(2) . . . . ? C15 C16 C17 C21 -74.7(2) . . . . ? N1 C17 C20 Li1 26.24(16) . . . . ? C21 C17 C20 Li1 150.15(18) . . . . ? C16 C17 C20 Li1 -93.67(17) . . . . ? N1 Li1 C20 C17 -21.43(14) . . . . ? N2 Li1 C20 C17 123.1(2) . . . . ? C1 Li1 C20 C17 -114.29(18) . . . . ? Al1 Li1 C20 C17 -70.88(14) . . . . ? C24 N2 C22 C23 -175.6(2) . . . . ? C26 N2 C22 C23 -54.4(3) . . . . ? Li1 N2 C22 C23 59.8(2) . . . . ? C22 N2 C24 C25 -63.4(3) . . . . ? C26 N2 C24 C25 173.6(2) . . . . ? Li1 N2 C24 C25 61.1(3) . . . . ? C22 N2 C26 C27 -57.6(3) . . . . ? C24 N2 C26 C27 63.4(3) . . . . ? Li1 N2 C26 C27 -177.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.242 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.047 ############################################################ ########### COMPOUND 3 ################################### ######################################################### data_grem255 _database_code_depnum_ccdc_archive 'CCDC 634095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H64 Al Li N2 O' _chemical_formula_weight 550.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.9601(5) _cell_length_b 16.2475(4) _cell_length_c 11.5036(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3543.73(16) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7772 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4255 _reflns_number_gt 3189 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo and Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.6090P] 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 4255 _refine_ls_number_parameters 390 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.20413(4) 0.01491(4) 0.20004(6) 0.02019(17) Uani 1 1 d . . . Li1 Li 0.1434(2) -0.1398(2) 0.2085(5) 0.0323(10) Uani 1 1 d . . . O1 O 0.09833(8) -0.24146(9) 0.22729(17) 0.0302(4) Uani 1 1 d . . . N1 N 0.15210(10) -0.05197(12) 0.08528(18) 0.0203(4) Uani 1 1 d . . . N2 N 0.07363(10) -0.37774(12) 0.23874(19) 0.0253(5) Uani 1 1 d . . . C1 C 0.07816(12) -0.02746(14) 0.0521(2) 0.0233(6) Uani 1 1 d . . . C2 C 0.04086(13) -0.09375(15) -0.0215(2) 0.0288(6) Uani 1 1 d . . . H2A H 0.0289 -0.1408 0.0294 0.035 Uiso 1 1 calc R . . H2B H -0.0039 -0.0707 -0.0514 0.035 Uiso 1 1 calc R . . C3 C 0.08360(14) -0.12516(17) -0.1230(2) 0.0358(7) Uani 1 1 d . . . H3A H 0.0925 -0.0801 -0.1790 0.043 Uiso 1 1 calc R . . H3B H 0.0577 -0.1695 -0.1636 0.043 Uiso 1 1 calc R . . C4 C 0.15300(14) -0.15789(17) -0.0755(3) 0.0332(7) Uani 1 1 d . . . H4A H 0.1819 -0.1792 -0.1406 0.040 Uiso 1 1 calc R . . H4B H 0.1433 -0.2043 -0.0220 0.040 Uiso 1 1 calc R . . C5 C 0.19518(13) -0.09122(15) -0.0099(2) 0.0260(6) Uani 1 1 d . . . C6 C 0.03425(12) -0.01996(15) 0.1639(2) 0.0251(6) Uani 1 1 d . . . H6A H 0.0343 -0.0728 0.2050 0.038 Uiso 1 1 calc R . . H6B H -0.0143 -0.0049 0.1440 0.038 Uiso 1 1 calc R . . H6C H 0.0547 0.0226 0.2140 0.038 Uiso 1 1 calc R . . C7 C 0.07503(13) 0.05556(14) -0.0130(2) 0.0273(6) Uani 1 1 d . . . H7A H 0.1049 0.0958 0.0271 0.041 Uiso 1 1 calc R . . H7B H 0.0262 0.0755 -0.0145 0.041 Uiso 1 1 calc R . . H7C H 0.0920 0.0481 -0.0928 0.041 Uiso 1 1 calc R . . C8 C 0.25814(13) -0.13555(16) 0.0469(3) 0.0307(6) Uani 1 1 d . . . H8A H 0.2876 -0.0953 0.0876 0.046 Uiso 1 1 calc R . . H8B H 0.2861 -0.1631 -0.0133 0.046 Uiso 1 1 calc R . . H8C H 0.2407 -0.1765 0.1024 0.046 Uiso 1 1 calc R . . C9 C 0.22539(14) -0.03083(16) -0.1005(2) 0.0307(6) Uani 1 1 d . . . H9A H 0.1866 -0.0058 -0.1443 0.046 Uiso 1 1 calc R . . H9B H 0.2565 -0.0606 -0.1540 0.046 Uiso 1 1 calc R . . H9C H 0.2523 0.0123 -0.0607 0.046 Uiso 1 1 calc R . . C18 C 0.15407(14) 0.10437(15) 0.2927(2) 0.0219(6) Uani 1 1 d . . . C19 C 0.11390(13) 0.18004(14) 0.2454(2) 0.0237(6) Uani 1 1 d . . . H19 H 0.0712 0.1598 0.2031 0.028 Uiso 1 1 calc R . . C21 C 0.15784(14) 0.23003(15) 0.1608(2) 0.0307(6) Uani 1 1 d . . . H21A H 0.1282 0.2721 0.1243 0.046 Uiso 1 1 calc R . . H21B H 0.1771 0.1936 0.1008 0.046 Uiso 1 1 calc R . . H21C H 0.1966 0.2567 0.2027 0.046 Uiso 1 1 calc R . . C20 C 0.08910(14) 0.23681(15) 0.3435(2) 0.0301(6) Uani 1 1 d . . . H20A H 0.1302 0.2597 0.3838 0.045 Uiso 1 1 calc R . . H20B H 0.0604 0.2053 0.3987 0.045 Uiso 1 1 calc R . . H20C H 0.0609 0.2817 0.3108 0.045 Uiso 1 1 calc R . . C14 C 0.29307(13) 0.06943(16) 0.1385(2) 0.0245(6) Uani 1 1 d . . . C15 C 0.33266(12) 0.13127(14) 0.2170(2) 0.0276(6) Uani 1 1 d . . . H15 H 0.2976 0.1727 0.2452 0.033 Uiso 1 1 calc R . . C16 C 0.36530(15) 0.09051(18) 0.3228(3) 0.0387(7) Uani 1 1 d . . . H16A H 0.3967 0.0460 0.2977 0.058 Uiso 1 1 calc R . . H16B H 0.3279 0.0678 0.3721 0.058 Uiso 1 1 calc R . . H16C H 0.3923 0.1313 0.3669 0.058 Uiso 1 1 calc R . . C17 C 0.38984(15) 0.17767(17) 0.1487(3) 0.0397(7) Uani 1 1 d . . . H17A H 0.4132 0.2173 0.2001 0.060 Uiso 1 1 calc R . . H17B H 0.3681 0.2070 0.0835 0.060 Uiso 1 1 calc R . . H17C H 0.4247 0.1383 0.1191 0.060 Uiso 1 1 calc R . . C10 C 0.23183(15) -0.07211(15) 0.3236(2) 0.0258(6) Uani 1 1 d . . . C11 C 0.20650(15) -0.06169(16) 0.4489(2) 0.0329(7) Uani 1 1 d . . . H11 H 0.2086 -0.0017 0.4680 0.040 Uiso 1 1 calc R . . C13 C 0.13063(16) -0.08922(19) 0.4631(3) 0.0426(8) Uani 1 1 d . . . H13A H 0.1267 -0.1478 0.4437 0.064 Uiso 1 1 calc R . . H13B H 0.1003 -0.0571 0.4111 0.064 Uiso 1 1 calc R . . H13C H 0.1157 -0.0806 0.5438 0.064 Uiso 1 1 calc R . . C12 C 0.25315(17) -0.10720(19) 0.5366(3) 0.0487(8) Uani 1 1 d . . . H12A H 0.2490 -0.1667 0.5242 0.073 Uiso 1 1 calc R . . H12B H 0.2380 -0.0936 0.6157 0.073 Uiso 1 1 calc R . . H12C H 0.3024 -0.0904 0.5259 0.073 Uiso 1 1 calc R . . C22 C 0.11864(13) -0.31486(14) 0.2310(2) 0.0251(6) Uani 1 1 d . . . C23 C 0.19670(12) -0.33041(13) 0.2271(2) 0.0222(6) Uani 1 1 d . . . C24 C 0.23011(14) -0.35691(15) 0.1277(2) 0.0292(6) Uani 1 1 d . . . H24 H 0.2031 -0.3725 0.0617 0.035 Uiso 1 1 calc R . . C25 C 0.30341(14) -0.36091(16) 0.1238(3) 0.0317(6) Uani 1 1 d . . . H25 H 0.3265 -0.3784 0.0548 0.038 Uiso 1 1 calc R . . C26 C 0.34250(12) -0.33947(14) 0.2202(3) 0.0282(6) Uani 1 1 d . . . H26 H 0.3925 -0.3429 0.2179 0.034 Uiso 1 1 calc R . . C27 C 0.30909(13) -0.31301(16) 0.3200(2) 0.0290(6) Uani 1 1 d . . . H27 H 0.3362 -0.2979 0.3861 0.035 Uiso 1 1 calc R . . C28 C 0.23641(13) -0.30838(14) 0.3240(2) 0.0243(6) Uani 1 1 d . . . H28 H 0.2135 -0.2902 0.3928 0.029 Uiso 1 1 calc R . . C29 C 0.09731(14) -0.46488(14) 0.2490(2) 0.0292(6) Uani 1 1 d . . . H29 H 0.1500 -0.4650 0.2457 0.035 Uiso 1 1 calc R . . C30 C 0.07576(14) -0.50125(16) 0.3658(3) 0.0358(7) Uani 1 1 d . . . H30A H 0.0934 -0.4661 0.4287 0.054 Uiso 1 1 calc R . . H30B H 0.0959 -0.5565 0.3738 0.054 Uiso 1 1 calc R . . H30C H 0.0242 -0.5045 0.3702 0.054 Uiso 1 1 calc R . . C31 C 0.07087(16) -0.51551(16) 0.1469(3) 0.0385(7) Uani 1 1 d . . . H31A H 0.0192 -0.5179 0.1489 0.058 Uiso 1 1 calc R . . H31B H 0.0901 -0.5714 0.1519 0.058 Uiso 1 1 calc R . . H31C H 0.0862 -0.4899 0.0740 0.058 Uiso 1 1 calc R . . C32 C -0.00400(13) -0.36298(15) 0.2425(2) 0.0302(6) Uani 1 1 d . . . H32 H -0.0265 -0.4184 0.2493 0.036 Uiso 1 1 calc R . . C33 C -0.02628(14) -0.31504(19) 0.3503(3) 0.0413(8) Uani 1 1 d . . . H33A H -0.0052 -0.3403 0.4194 0.062 Uiso 1 1 calc R . . H33B H -0.0778 -0.3161 0.3571 0.062 Uiso 1 1 calc R . . H33C H -0.0101 -0.2579 0.3435 0.062 Uiso 1 1 calc R . . C34 C -0.03088(15) -0.32592(17) 0.1294(3) 0.0372(7) Uani 1 1 d . . . H34A H -0.0112 -0.2706 0.1196 0.056 Uiso 1 1 calc R . . H34B H -0.0825 -0.3226 0.1316 0.056 Uiso 1 1 calc R . . H34C H -0.0163 -0.3607 0.0640 0.056 Uiso 1 1 calc R . . H18B H 0.1952(13) 0.1271(15) 0.339(2) 0.024(7) Uiso 1 1 d . . . H18A H 0.1250(12) 0.0809(14) 0.350(2) 0.023(7) Uiso 1 1 d . . . H10A H 0.2853(14) -0.0636(16) 0.319(2) 0.035(7) Uiso 1 1 d . . . H10B H 0.2260(13) -0.1291(17) 0.304(2) 0.032(7) Uiso 1 1 d . . . H14B H 0.2768(15) 0.0989(17) 0.065(3) 0.046(8) Uiso 1 1 d . . . H14A H 0.3280(13) 0.0272(16) 0.113(2) 0.028(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0200(3) 0.0172(3) 0.0234(4) -0.0001(3) -0.0005(3) -0.0001(3) Li1 0.032(2) 0.024(2) 0.041(3) 0.004(2) -0.005(2) -0.0012(18) O1 0.0297(9) 0.0185(8) 0.0424(12) 0.0008(8) -0.0036(9) 0.0015(7) N1 0.0174(10) 0.0205(10) 0.0230(11) -0.0038(9) 0.0017(9) 0.0001(9) N2 0.0206(10) 0.0196(10) 0.0358(13) 0.0018(10) -0.0036(10) -0.0004(9) C1 0.0189(13) 0.0244(13) 0.0267(15) -0.0031(11) -0.0019(11) -0.0012(11) C2 0.0259(14) 0.0292(13) 0.0314(16) -0.0028(12) -0.0048(12) -0.0042(12) C3 0.0371(16) 0.0376(16) 0.0327(17) -0.0103(13) -0.0021(14) -0.0086(13) C4 0.0361(16) 0.0312(14) 0.0322(16) -0.0114(12) 0.0037(13) -0.0039(13) C5 0.0273(14) 0.0219(13) 0.0289(15) -0.0061(11) 0.0012(12) -0.0010(11) C6 0.0197(12) 0.0235(12) 0.0321(16) -0.0004(11) -0.0014(11) -0.0003(11) C7 0.0280(14) 0.0258(13) 0.0281(15) -0.0003(12) -0.0038(12) 0.0014(12) C8 0.0280(14) 0.0266(14) 0.0375(16) -0.0060(12) 0.0036(13) 0.0027(12) C9 0.0321(15) 0.0315(14) 0.0286(15) -0.0066(12) 0.0033(12) -0.0007(12) C18 0.0232(14) 0.0203(13) 0.0223(14) 0.0019(11) 0.0023(12) -0.0025(11) C19 0.0257(13) 0.0195(11) 0.0260(15) 0.0005(11) -0.0008(12) 0.0001(11) C21 0.0351(15) 0.0231(13) 0.0337(16) 0.0051(11) 0.0023(13) 0.0019(12) C20 0.0323(15) 0.0208(13) 0.0371(17) -0.0042(12) 0.0035(13) -0.0013(12) C14 0.0220(13) 0.0231(13) 0.0284(15) -0.0018(12) 0.0018(12) 0.0015(12) C15 0.0223(12) 0.0262(13) 0.0344(16) -0.0057(13) 0.0019(13) 0.0025(10) C16 0.0321(15) 0.0458(17) 0.0382(18) -0.0069(14) -0.0043(14) -0.0039(14) C17 0.0346(16) 0.0389(16) 0.0457(19) -0.0021(15) 0.0002(15) -0.0158(14) C10 0.0282(15) 0.0186(12) 0.0305(16) 0.0021(12) -0.0033(12) -0.0002(12) C11 0.0460(17) 0.0207(13) 0.0321(16) -0.0001(12) -0.0090(14) 0.0068(13) C13 0.0462(18) 0.0451(17) 0.0365(19) 0.0088(15) 0.0079(15) 0.0092(15) C12 0.066(2) 0.0450(18) 0.0349(18) 0.0025(15) -0.0212(16) 0.0073(17) C22 0.0275(13) 0.0208(12) 0.0270(15) -0.0006(11) -0.0035(12) -0.0028(11) C23 0.0255(12) 0.0151(11) 0.0261(15) 0.0032(10) 0.0000(12) -0.0039(10) C24 0.0339(15) 0.0266(13) 0.0271(15) -0.0054(12) -0.0037(13) -0.0063(13) C25 0.0337(16) 0.0295(14) 0.0319(16) -0.0025(12) 0.0060(13) -0.0028(13) C26 0.0201(12) 0.0251(12) 0.0393(17) 0.0039(12) 0.0023(13) -0.0027(11) C27 0.0274(15) 0.0303(14) 0.0292(16) 0.0028(12) -0.0074(13) -0.0038(12) C28 0.0294(14) 0.0199(12) 0.0234(14) 0.0026(11) 0.0038(12) -0.0021(12) C29 0.0242(13) 0.0174(11) 0.0459(18) 0.0044(12) 0.0005(13) -0.0003(11) C30 0.0313(16) 0.0270(14) 0.0492(19) 0.0096(14) -0.0049(14) -0.0017(12) C31 0.0381(16) 0.0259(14) 0.051(2) -0.0049(14) 0.0027(15) -0.0025(13) C32 0.0215(13) 0.0248(13) 0.0442(18) 0.0030(12) -0.0028(13) -0.0023(11) C33 0.0291(16) 0.0446(17) 0.050(2) 0.0046(15) 0.0032(15) 0.0107(14) C34 0.0307(16) 0.0334(15) 0.0476(19) 0.0019(14) -0.0098(15) 0.0023(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.974(2) . ? Al1 C14 2.032(3) . ? Al1 C18 2.037(3) . ? Al1 C10 2.073(3) . ? Al1 Li1 2.767(4) . ? Li1 O1 1.872(4) . ? Li1 N1 2.018(5) . ? Li1 C10 2.403(5) . ? Li1 H10B 1.92(3) . ? O1 C22 1.254(3) . ? N1 C1 1.507(3) . ? N1 C5 1.508(3) . ? N2 C22 1.334(3) . ? N2 C29 1.490(3) . ? N2 C32 1.492(3) . ? C1 C6 1.537(3) . ? C1 C2 1.542(3) . ? C1 C7 1.544(3) . ? C2 C3 1.510(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.543(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.540(4) . ? C5 C9 1.541(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C18 C19 1.545(3) . ? C18 H18B 1.01(3) . ? C18 H18A 0.94(3) . ? C19 C21 1.517(3) . ? C19 C20 1.531(3) . ? C19 H19 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C14 C15 1.545(4) . ? C14 H14B 1.02(3) . ? C14 H14A 1.00(3) . ? C15 C16 1.518(4) . ? C15 C17 1.536(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C10 C11 1.528(4) . ? C10 H10A 1.03(3) . ? C10 H10B 0.96(3) . ? C11 C13 1.515(4) . ? C11 C12 1.532(4) . ? C11 H11 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C22 C23 1.502(3) . ? C23 C24 1.376(4) . ? C23 C28 1.392(4) . ? C24 C25 1.392(4) . ? C24 H24 0.9500 . ? C25 C26 1.378(4) . ? C25 H25 0.9500 . ? C26 C27 1.380(4) . ? C26 H26 0.9500 . ? C27 C28 1.381(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C31 1.519(4) . ? C29 C30 1.524(4) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.522(4) . ? C32 C33 1.523(4) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 C14 114.95(10) . . ? N1 Al1 C18 120.65(10) . . ? C14 Al1 C18 104.95(11) . . ? N1 Al1 C10 102.11(10) . . ? C14 Al1 C10 109.02(11) . . ? C18 Al1 C10 104.23(11) . . ? N1 Al1 Li1 46.79(12) . . ? C14 Al1 Li1 138.90(12) . . ? C18 Al1 Li1 115.85(13) . . ? C10 Al1 Li1 57.42(12) . . ? O1 Li1 N1 137.9(3) . . ? O1 Li1 C10 131.2(2) . . ? N1 Li1 C10 90.36(16) . . ? O1 Li1 Al1 174.6(3) . . ? N1 Li1 Al1 45.47(10) . . ? C10 Li1 Al1 46.62(9) . . ? O1 Li1 H10B 112.7(8) . . ? N1 Li1 H10B 105.8(8) . . ? C10 Li1 H10B 22.2(8) . . ? Al1 Li1 H10B 66.4(8) . . ? C22 O1 Li1 134.6(2) . . ? C1 N1 C5 115.57(19) . . ? C1 N1 Al1 119.28(14) . . ? C5 N1 Al1 116.61(14) . . ? C1 N1 Li1 106.81(18) . . ? C5 N1 Li1 104.78(19) . . ? Al1 N1 Li1 87.74(15) . . ? C22 N2 C29 122.7(2) . . ? C22 N2 C32 120.67(19) . . ? C29 N2 C32 116.59(19) . . ? N1 C1 C6 108.22(19) . . ? N1 C1 C2 112.42(19) . . ? C6 C1 C2 105.45(19) . . ? N1 C1 C7 112.94(19) . . ? C6 C1 C7 108.4(2) . . ? C2 C1 C7 109.1(2) . . ? C3 C2 C1 114.5(2) . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2B 108.6 . . ? C1 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C2 C3 C4 107.7(2) . . ? C2 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? C2 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C3 C4 C5 112.3(2) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N1 C5 C8 108.0(2) . . ? N1 C5 C9 115.0(2) . . ? C8 C5 C9 107.2(2) . . ? N1 C5 C4 111.8(2) . . ? C8 C5 C4 106.3(2) . . ? C9 C5 C4 108.0(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C19 C18 Al1 127.82(19) . . ? C19 C18 H18B 105.9(13) . . ? Al1 C18 H18B 100.2(13) . . ? C19 C18 H18A 106.4(14) . . ? Al1 C18 H18A 110.6(14) . . ? H18B C18 H18A 103(2) . . ? C21 C19 C20 108.59(19) . . ? C21 C19 C18 112.4(2) . . ? C20 C19 C18 111.8(2) . . ? C21 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? C18 C19 H19 108.0 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C14 Al1 118.90(18) . . ? C15 C14 H14B 109.0(16) . . ? Al1 C14 H14B 104.1(16) . . ? C15 C14 H14A 107.2(14) . . ? Al1 C14 H14A 110.7(14) . . ? H14B C14 H14A 106(2) . . ? C16 C15 C17 109.7(2) . . ? C16 C15 C14 112.5(2) . . ? C17 C15 C14 111.3(2) . . ? C16 C15 H15 107.7 . . ? C17 C15 H15 107.7 . . ? C14 C15 H15 107.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C10 Al1 119.44(18) . . ? C11 C10 Li1 110.6(2) . . ? Al1 C10 Li1 75.96(13) . . ? C11 C10 H10A 110.5(16) . . ? Al1 C10 H10A 96.9(15) . . ? Li1 C10 H10A 136.1(16) . . ? C11 C10 H10B 106.7(17) . . ? Al1 C10 H10B 118.2(17) . . ? Li1 C10 H10B 49.5(16) . . ? H10A C10 H10B 103(2) . . ? C13 C11 C10 111.6(2) . . ? C13 C11 C12 109.6(2) . . ? C10 C11 C12 112.7(2) . . ? C13 C11 H11 107.6 . . ? C10 C11 H11 107.6 . . ? C12 C11 H11 107.6 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C22 N2 122.3(2) . . ? O1 C22 C23 117.5(2) . . ? N2 C22 C23 120.2(2) . . ? C24 C23 C28 119.8(2) . . ? C24 C23 C22 122.0(2) . . ? C28 C23 C22 117.8(2) . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.1(2) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.2(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C23 119.9(2) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? N2 C29 C31 110.7(2) . . ? N2 C29 C30 110.9(2) . . ? C31 C29 C30 112.6(2) . . ? N2 C29 H29 107.5 . . ? C31 C29 H29 107.5 . . ? C30 C29 H29 107.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 C34 111.6(2) . . ? N2 C32 C33 112.3(2) . . ? C34 C32 C33 113.6(2) . . ? N2 C32 H32 106.2 . . ? C34 C32 H32 106.2 . . ? C33 C32 H32 106.2 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Al1 Li1 O1 -131(2) . . . . ? C14 Al1 Li1 O1 150(2) . . . . ? C18 Al1 Li1 O1 -23(2) . . . . ? C10 Al1 Li1 O1 68(2) . . . . ? C14 Al1 Li1 N1 -78.7(2) . . . . ? C18 Al1 Li1 N1 108.79(15) . . . . ? C10 Al1 Li1 N1 -160.38(19) . . . . ? N1 Al1 Li1 C10 160.38(19) . . . . ? C14 Al1 Li1 C10 81.7(2) . . . . ? C18 Al1 Li1 C10 -90.83(14) . . . . ? N1 Li1 O1 C22 108.3(4) . . . . ? C10 Li1 O1 C22 -60.9(5) . . . . ? Al1 Li1 O1 C22 -125(2) . . . . ? C14 Al1 N1 C1 -117.27(18) . . . . ? C18 Al1 N1 C1 10.1(2) . . . . ? C10 Al1 N1 C1 124.86(18) . . . . ? Li1 Al1 N1 C1 108.0(2) . . . . ? C14 Al1 N1 C5 29.3(2) . . . . ? C18 Al1 N1 C5 156.61(16) . . . . ? C10 Al1 N1 C5 -88.59(18) . . . . ? Li1 Al1 N1 C5 -105.4(2) . . . . ? C14 Al1 N1 Li1 134.70(16) . . . . ? C18 Al1 N1 Li1 -97.98(16) . . . . ? C10 Al1 N1 Li1 16.82(16) . . . . ? O1 Li1 N1 C1 54.0(4) . . . . ? C10 Li1 N1 C1 -134.09(17) . . . . ? Al1 Li1 N1 C1 -119.96(16) . . . . ? O1 Li1 N1 C5 -69.1(4) . . . . ? C10 Li1 N1 C5 102.82(18) . . . . ? Al1 Li1 N1 C5 116.94(16) . . . . ? O1 Li1 N1 Al1 174.0(4) . . . . ? C10 Li1 N1 Al1 -14.13(13) . . . . ? C5 N1 C1 C6 159.00(19) . . . . ? Al1 N1 C1 C6 -54.1(2) . . . . ? Li1 N1 C1 C6 42.9(2) . . . . ? C5 N1 C1 C2 42.9(3) . . . . ? Al1 N1 C1 C2 -170.17(16) . . . . ? Li1 N1 C1 C2 -73.2(2) . . . . ? C5 N1 C1 C7 -81.0(2) . . . . ? Al1 N1 C1 C7 65.9(2) . . . . ? Li1 N1 C1 C7 162.9(2) . . . . ? N1 C1 C2 C3 -49.1(3) . . . . ? C6 C1 C2 C3 -166.8(2) . . . . ? C7 C1 C2 C3 77.0(3) . . . . ? C1 C2 C3 C4 56.7(3) . . . . ? C2 C3 C4 C5 -59.2(3) . . . . ? C1 N1 C5 C8 -162.73(19) . . . . ? Al1 N1 C5 C8 49.5(2) . . . . ? Li1 N1 C5 C8 -45.5(2) . . . . ? C1 N1 C5 C9 77.5(3) . . . . ? Al1 N1 C5 C9 -70.3(2) . . . . ? Li1 N1 C5 C9 -165.2(2) . . . . ? C1 N1 C5 C4 -46.1(3) . . . . ? Al1 N1 C5 C4 166.09(17) . . . . ? Li1 N1 C5 C4 71.1(2) . . . . ? C3 C4 C5 N1 54.8(3) . . . . ? C3 C4 C5 C8 172.4(2) . . . . ? C3 C4 C5 C9 -72.7(3) . . . . ? N1 Al1 C18 C19 -58.4(2) . . . . ? C14 Al1 C18 C19 73.4(2) . . . . ? C10 Al1 C18 C19 -172.1(2) . . . . ? Li1 Al1 C18 C19 -111.7(2) . . . . ? Al1 C18 C19 C21 -52.6(3) . . . . ? Al1 C18 C19 C20 -175.05(18) . . . . ? N1 Al1 C14 C15 172.78(17) . . . . ? C18 Al1 C14 C15 37.9(2) . . . . ? C10 Al1 C14 C15 -73.3(2) . . . . ? Li1 Al1 C14 C15 -135.2(2) . . . . ? Al1 C14 C15 C16 67.0(3) . . . . ? Al1 C14 C15 C17 -169.48(18) . . . . ? N1 Al1 C10 C11 -120.4(2) . . . . ? C14 Al1 C10 C11 117.5(2) . . . . ? C18 Al1 C10 C11 5.9(2) . . . . ? Li1 Al1 C10 C11 -105.9(3) . . . . ? N1 Al1 C10 Li1 -14.50(14) . . . . ? C14 Al1 C10 Li1 -136.53(15) . . . . ? C18 Al1 C10 Li1 111.83(15) . . . . ? O1 Li1 C10 C11 -56.8(4) . . . . ? N1 Li1 C10 C11 130.4(2) . . . . ? Al1 Li1 C10 C11 116.6(2) . . . . ? O1 Li1 C10 Al1 -173.3(3) . . . . ? N1 Li1 C10 Al1 13.85(13) . . . . ? Al1 C10 C11 C13 79.6(3) . . . . ? Li1 C10 C11 C13 -5.4(3) . . . . ? Al1 C10 C11 C12 -156.6(2) . . . . ? Li1 C10 C11 C12 118.3(2) . . . . ? Li1 O1 C22 N2 -175.9(3) . . . . ? Li1 O1 C22 C23 4.5(4) . . . . ? C29 N2 C22 O1 -176.9(2) . . . . ? C32 N2 C22 O1 0.5(4) . . . . ? C29 N2 C22 C23 2.6(4) . . . . ? C32 N2 C22 C23 -180.0(2) . . . . ? O1 C22 C23 C24 -102.7(3) . . . . ? N2 C22 C23 C24 77.6(3) . . . . ? O1 C22 C23 C28 70.1(3) . . . . ? N2 C22 C23 C28 -109.5(3) . . . . ? C28 C23 C24 C25 -0.6(4) . . . . ? C22 C23 C24 C25 172.2(2) . . . . ? C23 C24 C25 C26 1.0(4) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C25 C26 C27 C28 0.4(4) . . . . ? C26 C27 C28 C23 0.0(4) . . . . ? C24 C23 C28 C27 0.1(4) . . . . ? C22 C23 C28 C27 -172.9(2) . . . . ? C22 N2 C29 C31 -119.1(3) . . . . ? C32 N2 C29 C31 63.4(3) . . . . ? C22 N2 C29 C30 115.2(3) . . . . ? C32 N2 C29 C30 -62.3(3) . . . . ? C22 N2 C32 C34 65.3(3) . . . . ? C29 N2 C32 C34 -117.1(2) . . . . ? C22 N2 C32 C33 -63.6(3) . . . . ? C29 N2 C32 C33 113.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.172 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.040 ############################################################ ########### COMPOUND 4 ################################### ######################################################### data_grem266 _database_code_depnum_ccdc_archive 'CCDC 634096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H114 Al2 Li2 N2 O8' _chemical_formula_weight 1083.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8338(4) _cell_length_b 11.8351(3) _cell_length_c 13.8446(4) _cell_angle_alpha 111.793(2) _cell_angle_beta 95.568(2) _cell_angle_gamma 101.398(2) _cell_volume 1733.71(9) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7603 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39049 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.14 _reflns_number_total 7639 _reflns_number_gt 4855 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Denzo & Collect' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution SHELXS _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^)+(0.0598P)^2^+0.7765P] 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 7639 _refine_ls_number_parameters 379 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.030 _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 0.14500(6) 0.62993(6) 0.25163(5) 0.03398(17) Uani 1 1 d . . . Li1 Li 0.0708(3) 0.8893(3) 0.2620(3) 0.0331(8) Uani 1 1 d . . . O1 O 0.17600(13) 1.01768(13) 0.24496(11) 0.0375(4) Uani 1 1 d . . . O2 O 0.05305(13) 0.71280(13) 0.20604(11) 0.0363(3) Uani 1 1 d . . . O3 O -0.08831(12) 0.84564(13) 0.16279(11) 0.0370(4) Uani 1 1 d . . . O4 O 0.01967(13) 0.96039(12) 0.39542(10) 0.0350(3) Uani 1 1 d . . . N1 N 0.31226(15) 1.13923(15) 0.19717(13) 0.0312(4) Uani 1 1 d . . . C1 C 0.26561(18) 1.10507(18) 0.26950(16) 0.0308(4) Uani 1 1 d . . . C2 C 0.31693(17) 1.17738(18) 0.38526(16) 0.0303(4) Uani 1 1 d . . . C3 C 0.34819(18) 1.1146(2) 0.44667(17) 0.0363(5) Uani 1 1 d . . . H3 H 0.3459 1.0278 0.4140 0.044 Uiso 1 1 calc R . . C4 C 0.3826(2) 1.1783(2) 0.55526(18) 0.0453(6) Uani 1 1 d . . . H4 H 0.4047 1.1351 0.5968 0.054 Uiso 1 1 calc R . . C5 C 0.3851(2) 1.3033(2) 0.60337(19) 0.0514(6) Uani 1 1 d . . . H5 H 0.4092 1.3465 0.6780 0.062 Uiso 1 1 calc R . . C6 C 0.3527(2) 1.3664(2) 0.54350(19) 0.0503(6) Uani 1 1 d . . . H6 H 0.3533 1.4527 0.5770 0.060 Uiso 1 1 calc R . . C7 C 0.3194(2) 1.3040(2) 0.43466(17) 0.0411(5) Uani 1 1 d . . . H7 H 0.2981 1.3480 0.3935 0.049 Uiso 1 1 calc R . . C8 C 0.4255(2) 1.3443(2) 0.2047(2) 0.0519(6) Uani 1 1 d . . . H8A H 0.3953 1.3229 0.1300 0.078 Uiso 1 1 calc R . . H8B H 0.5044 1.4008 0.2256 0.078 Uiso 1 1 calc R . . H8C H 0.3734 1.3861 0.2483 0.078 Uiso 1 1 calc R . . C9 C 0.43065(19) 1.2247(2) 0.22063(18) 0.0373(5) Uani 1 1 d . . . H9 H 0.4637 1.2500 0.2970 0.045 Uiso 1 1 calc R . . C10 C 0.5122(2) 1.1564(2) 0.1559(2) 0.0484(6) Uani 1 1 d . . . H10A H 0.5149 1.0814 0.1696 0.073 Uiso 1 1 calc R . . H10B H 0.5912 1.2125 0.1760 0.073 Uiso 1 1 calc R . . H10C H 0.4829 1.1313 0.0803 0.073 Uiso 1 1 calc R . . C11 C 0.2292(2) 0.9466(2) 0.02775(18) 0.0496(6) Uani 1 1 d . . . H11A H 0.3054 0.9264 0.0330 0.074 Uiso 1 1 calc R . . H11B H 0.1952 0.9208 -0.0469 0.074 Uiso 1 1 calc R . . H11C H 0.1764 0.9017 0.0595 0.074 Uiso 1 1 calc R . . C12 C 0.2457(2) 1.0879(2) 0.08645(16) 0.0372(5) Uani 1 1 d . . . H12 H 0.2942 1.1290 0.0476 0.045 Uiso 1 1 calc R . . C13 C 0.1314(2) 1.1276(3) 0.08468(19) 0.0522(6) Uani 1 1 d . . . H13A H 0.0792 1.0865 0.1193 0.078 Uiso 1 1 calc R . . H13B H 0.0937 1.1030 0.0112 0.078 Uiso 1 1 calc R . . H13C H 0.1476 1.2191 0.1225 0.078 Uiso 1 1 calc R . . C14 C -0.0247(2) 0.6590(2) 0.10718(18) 0.0456(6) Uani 1 1 d . . . H14A H -0.0488 0.5664 0.0834 0.055 Uiso 1 1 calc R . . H14B H 0.0153 0.6784 0.0535 0.055 Uiso 1 1 calc R . . C15 C -0.1309(2) 0.7112(2) 0.11798(19) 0.0442(6) Uani 1 1 d . . . H15A H -0.1819 0.6820 0.0479 0.053 Uiso 1 1 calc R . . H15B H -0.1769 0.6836 0.1649 0.053 Uiso 1 1 calc R . . C16 C -0.1702(2) 0.9134(2) 0.18631(18) 0.0444(6) Uani 1 1 d . . . H16 H -0.1407 1.0022 0.2196 0.053 Uiso 1 1 calc R . . C17 C -0.2845(2) 0.8711(3) 0.1687(2) 0.0608(7) Uani 1 1 d . . . H17A H -0.3193 0.7832 0.1356 0.073 Uiso 1 1 calc R . . H17B H -0.3325 0.9284 0.1889 0.073 Uiso 1 1 calc R . . C18 C 0.0265(2) 1.08947(19) 0.45728(17) 0.0390(5) Uani 1 1 d . . . H18A H -0.0508 1.1069 0.4445 0.047 Uiso 1 1 calc R . . H18B H 0.0846 1.1437 0.4358 0.047 Uiso 1 1 calc R . . C19 C -0.0618(2) 0.8808(2) 0.42787(17) 0.0419(5) Uani 1 1 d . . . H19A H -0.0646 0.7917 0.3858 0.050 Uiso 1 1 calc R . . H19B H -0.1413 0.8930 0.4144 0.050 Uiso 1 1 calc R . . C20 C 0.2643(2) 0.5939(2) 0.1583(2) 0.0413(5) Uani 1 1 d . . . C21 C 0.3905(3) 0.6328(3) 0.0299(3) 0.0827(10) Uani 1 1 d . . . H21A H 0.4538 0.6090 0.0627 0.124 Uiso 1 1 calc R . . H21B H 0.4241 0.6968 0.0046 0.124 Uiso 1 1 calc R . . H21C H 0.3413 0.5586 -0.0299 0.124 Uiso 1 1 calc R . . C22 C 0.3157(2) 0.6859(2) 0.11154(19) 0.0467(6) Uani 1 1 d . . . H22 H 0.2487 0.7035 0.0746 0.056 Uiso 1 1 calc R . . C23 C 0.3867(2) 0.8087(2) 0.1966(2) 0.0584(7) Uani 1 1 d . . . H23A H 0.3372 0.8451 0.2463 0.088 Uiso 1 1 calc R . . H23B H 0.4164 0.8669 0.1643 0.088 Uiso 1 1 calc R . . H23C H 0.4529 0.7943 0.2346 0.088 Uiso 1 1 calc R . . C24 C 0.0574(3) 0.4597(2) 0.2372(2) 0.0501(6) Uani 1 1 d . . . C25 C -0.1475(5) 0.4547(6) 0.2604(6) 0.0641(17) Uiso 0.50 1 d PD A 1 H25A H -0.1360 0.5370 0.2563 0.096 Uiso 0.50 1 calc PR A 1 H25B H -0.2050 0.4473 0.3055 0.096 Uiso 0.50 1 calc PR A 1 H25C H -0.1763 0.3881 0.1892 0.096 Uiso 0.50 1 calc PR A 1 C26 C -0.0256(3) 0.4412(3) 0.3095(3) 0.0699(9) Uani 1 1 d D A 1 H26 H 0.0037 0.4992 0.3856 0.084 Uiso 1 1 calc R A 1 C27 C -0.0699(7) 0.3029(6) 0.2917(6) 0.067(2) Uiso 0.50 1 d P A 1 H27A H -0.1163 0.2553 0.2200 0.100 Uiso 0.50 1 calc PR A 1 H27B H -0.1190 0.2968 0.3435 0.100 Uiso 0.50 1 calc PR A 1 H27C H -0.0028 0.2681 0.3001 0.100 Uiso 0.50 1 calc PR A 1 C28 C 0.1995(3) 0.7505(2) 0.40300(19) 0.0504(7) Uani 1 1 d . . . C29 C 0.3201(3) 0.6310(2) 0.4661(2) 0.0643(8) Uani 1 1 d . A 1 H29A H 0.2599 0.6041 0.5023 0.096 Uiso 1 1 calc R A 1 H29B H 0.3978 0.6386 0.5033 0.096 Uiso 1 1 calc R A 1 H29C H 0.3070 0.5687 0.3931 0.096 Uiso 1 1 calc R A 1 C30 C 0.3134(2) 0.7581(3) 0.4653(2) 0.0377(6) Uani 0.80 1 d P A 1 H30 H 0.3786 0.7867 0.4322 0.045 Uiso 0.80 1 calc PR A 1 C31 C 0.3330(3) 0.8542(2) 0.5834(2) 0.0600(7) Uani 1 1 d . A 1 H31A H 0.3194 0.9340 0.5852 0.090 Uiso 1 1 calc R A 1 H31B H 0.4137 0.8684 0.6183 0.090 Uiso 1 1 calc R A 1 H31C H 0.2781 0.8202 0.6203 0.090 Uiso 1 1 calc R A 1 C30A C 0.2461(12) 0.7434(11) 0.4948(9) 0.041(3) Uiso 0.20 1 d P A 2 H30A H 0.1788 0.7161 0.5262 0.050 Uiso 0.20 1 d PR A 2 C25A C -0.1259(6) 0.4915(8) 0.3100(7) 0.096(3) Uiso 0.50 1 d PD B 2 H25D H -0.1106 0.5733 0.3696 0.144 Uiso 0.50 1 d PR B 2 H25E H -0.1930 0.4331 0.3166 0.144 Uiso 0.50 1 d PR B 2 H25F H -0.1435 0.5014 0.2435 0.144 Uiso 0.50 1 d PR B 2 C27A C -0.0340(7) 0.3142(6) 0.3236(6) 0.0635(19) Uiso 0.50 1 d P C 2 H27D H -0.0902 0.3064 0.3698 0.095 Uiso 0.50 1 d PR C 2 H27E H 0.0432 0.3131 0.3554 0.095 Uiso 0.50 1 d PR C 2 H27F H -0.0607 0.2437 0.2542 0.095 Uiso 0.50 1 d PR C 2 H20A H 0.333(2) 0.580(2) 0.200(2) 0.065(8) Uiso 1 1 d . . . H20B H 0.233(2) 0.512(3) 0.103(2) 0.063(8) Uiso 1 1 d . . . H24B H 0.018(2) 0.410(3) 0.165(2) 0.067(8) Uiso 1 1 d . . . H24A H 0.130(3) 0.423(3) 0.252(2) 0.092(10) Uiso 1 1 d . . . H28B H 0.130(3) 0.722(3) 0.456(3) 0.100(11) Uiso 1 1 d . . . H28A H 0.198(2) 0.839(2) 0.4124(19) 0.056(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0432(4) 0.0278(3) 0.0339(4) 0.0122(3) 0.0130(3) 0.0129(3) Li1 0.0358(19) 0.0328(18) 0.0283(18) 0.0092(14) 0.0090(15) 0.0077(15) O1 0.0372(8) 0.0354(8) 0.0349(8) 0.0129(7) 0.0066(7) 0.0003(7) O2 0.0411(9) 0.0327(8) 0.0319(8) 0.0078(6) 0.0044(6) 0.0132(7) O3 0.0382(8) 0.0338(8) 0.0350(8) 0.0094(6) 0.0028(7) 0.0108(7) O4 0.0451(9) 0.0326(8) 0.0281(7) 0.0103(6) 0.0170(6) 0.0105(7) N1 0.0364(10) 0.0296(9) 0.0290(9) 0.0134(7) 0.0076(7) 0.0074(7) C1 0.0336(11) 0.0271(10) 0.0337(11) 0.0126(9) 0.0082(9) 0.0105(9) C2 0.0296(11) 0.0305(10) 0.0307(11) 0.0125(9) 0.0093(9) 0.0050(9) C3 0.0382(12) 0.0316(11) 0.0384(12) 0.0155(10) 0.0063(10) 0.0046(9) C4 0.0489(14) 0.0476(14) 0.0383(13) 0.0233(11) 0.0024(11) 0.0004(11) C5 0.0608(16) 0.0509(15) 0.0313(13) 0.0131(11) 0.0056(11) -0.0020(13) C6 0.0657(17) 0.0386(13) 0.0396(14) 0.0082(11) 0.0128(12) 0.0106(12) C7 0.0516(14) 0.0371(12) 0.0375(13) 0.0157(10) 0.0103(11) 0.0150(11) C8 0.0693(18) 0.0337(12) 0.0539(15) 0.0201(11) 0.0191(13) 0.0066(12) C9 0.0395(12) 0.0361(12) 0.0354(12) 0.0164(10) 0.0085(10) 0.0029(10) C10 0.0433(14) 0.0555(15) 0.0536(15) 0.0272(13) 0.0194(12) 0.0128(12) C11 0.0689(17) 0.0412(13) 0.0326(12) 0.0086(10) 0.0063(11) 0.0143(12) C12 0.0472(13) 0.0369(12) 0.0259(11) 0.0121(9) 0.0037(9) 0.0099(10) C13 0.0558(16) 0.0629(16) 0.0379(13) 0.0186(12) 0.0005(11) 0.0227(13) C14 0.0560(15) 0.0373(12) 0.0328(12) 0.0017(10) 0.0015(11) 0.0160(11) C15 0.0443(14) 0.0326(12) 0.0410(13) 0.0029(10) -0.0034(10) 0.0065(10) C16 0.0531(15) 0.0463(13) 0.0356(13) 0.0139(11) 0.0044(11) 0.0232(12) C17 0.0530(17) 0.078(2) 0.0599(17) 0.0284(15) 0.0131(13) 0.0326(15) C18 0.0535(14) 0.0330(11) 0.0420(13) 0.0189(10) 0.0260(11) 0.0197(10) C19 0.0445(13) 0.0347(12) 0.0375(13) 0.0067(10) 0.0175(10) 0.0011(10) C20 0.0477(14) 0.0310(12) 0.0455(14) 0.0126(11) 0.0155(12) 0.0126(11) C21 0.084(2) 0.085(2) 0.071(2) 0.0254(18) 0.0439(18) 0.0038(18) C22 0.0426(14) 0.0551(15) 0.0485(14) 0.0258(12) 0.0138(11) 0.0129(12) C23 0.0566(17) 0.0444(14) 0.0760(19) 0.0287(14) 0.0137(14) 0.0070(13) C24 0.0643(18) 0.0367(13) 0.0488(16) 0.0154(12) 0.0229(14) 0.0090(13) C26 0.087(2) 0.0450(15) 0.078(2) 0.0229(14) 0.0431(18) 0.0069(15) C28 0.0766(19) 0.0368(13) 0.0389(13) 0.0119(11) 0.0013(13) 0.0278(13) C29 0.077(2) 0.0561(16) 0.0710(19) 0.0316(15) 0.0021(15) 0.0344(15) C30 0.0352(15) 0.0435(16) 0.0410(16) 0.0220(13) 0.0121(13) 0.0122(13) C31 0.0710(19) 0.0522(15) 0.0484(16) 0.0204(13) -0.0105(13) 0.0074(14) _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 1.8145(15) . ? Al1 C28 1.999(2) . ? Al1 C24 2.002(2) . ? Al1 C20 2.007(2) . ? Li1 O1 1.867(4) . ? Li1 O2 1.898(4) . ? Li1 O4 1.937(4) . ? Li1 O3 2.070(4) . ? Li1 C14 2.697(4) . ? O1 C1 1.243(2) . ? O2 C14 1.415(3) . ? O3 C16 1.365(3) . ? O3 C15 1.435(2) . ? O4 C18 1.428(2) . ? O4 C19 1.435(2) . ? N1 C1 1.338(3) . ? N1 C9 1.483(3) . ? N1 C12 1.491(3) . ? C1 C2 1.502(3) . ? C2 C3 1.388(3) . ? C2 C7 1.390(3) . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.372(3) . ? C4 H4 0.9500 . ? C5 C6 1.379(3) . ? C5 H5 0.9500 . ? C6 C7 1.384(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.523(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.525(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.525(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.518(3) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.504(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.310(3) . ? C16 H16 0.9500 . ? C17 H17A 0.9500 . ? C17 H17B 0.9500 . ? C18 C19 1.491(3) 2_576 ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C18 1.491(3) 2_576 ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C22 1.521(3) . ? C20 H20A 1.02(3) . ? C20 H20B 0.95(3) . ? C21 C22 1.531(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.504(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.511(4) . ? C24 H24B 0.96(3) . ? C24 H24A 1.07(3) . ? C25 C26 1.597(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 1.5820 . ? C25 H25E 1.0669 . ? C25 H25F 0.6715 . ? C26 C27 1.533(7) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 1.1184 . ? C27 H27E 1.4877 . ? C27 H27F 0.7360 . ? C28 C30A 1.374(12) . ? C28 C30 1.495(4) . ? C28 H28B 1.23(3) . ? C28 H28A 1.01(3) . ? C29 C30 1.525(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.569(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C30A H30A 1.0000 . ? C30A H28B 1.37(3) . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C27A H27D 0.9800 . ? C27A H27E 0.9800 . ? C27A H27F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al1 C28 99.70(8) . . ? O2 Al1 C24 113.32(11) . . ? C28 Al1 C24 112.24(12) . . ? O2 Al1 C20 108.99(9) . . ? C28 Al1 C20 118.90(12) . . ? C24 Al1 C20 104.01(10) . . ? O1 Li1 O2 131.17(19) . . ? O1 Li1 O4 108.40(17) . . ? O2 Li1 O4 115.95(18) . . ? O1 Li1 O3 109.03(17) . . ? O2 Li1 O3 84.78(14) . . ? O4 Li1 O3 97.74(16) . . ? O1 Li1 C14 124.18(16) . . ? O2 Li1 C14 29.89(8) . . ? O4 Li1 C14 126.27(17) . . ? O3 Li1 C14 57.41(10) . . ? C1 O1 Li1 155.96(18) . . ? C14 O2 Al1 123.84(13) . . ? C14 O2 Li1 108.15(16) . . ? Al1 O2 Li1 126.36(13) . . ? C16 O3 C15 116.66(18) . . ? C16 O3 Li1 123.62(16) . . ? C15 O3 Li1 107.03(15) . . ? C18 O4 C19 110.09(15) . . ? C18 O4 Li1 128.13(15) . . ? C19 O4 Li1 119.65(15) . . ? C1 N1 C9 123.00(17) . . ? C1 N1 C12 119.86(17) . . ? C9 N1 C12 117.11(16) . . ? O1 C1 N1 122.10(19) . . ? O1 C1 C2 117.49(18) . . ? N1 C1 C2 120.31(18) . . ? C3 C2 C7 119.07(19) . . ? C3 C2 C1 119.98(18) . . ? C7 C2 C1 120.42(18) . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.5(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.0(2) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.3(2) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C8 111.80(19) . . ? N1 C9 C10 110.71(18) . . ? C8 C9 C10 111.86(19) . . ? N1 C9 H9 107.4 . . ? C8 C9 H9 107.4 . . ? C10 C9 H9 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C13 110.34(17) . . ? N1 C12 C11 113.46(17) . . ? C13 C12 C11 113.2(2) . . ? N1 C12 H12 106.4 . . ? C13 C12 H12 106.4 . . ? C11 C12 H12 106.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 C15 109.45(17) . . ? O2 C14 Li1 41.96(11) . . ? C15 C14 Li1 79.69(14) . . ? O2 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? Li1 C14 H14A 150.1 . . ? O2 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? Li1 C14 H14B 94.0 . . ? H14A C14 H14B 108.2 . . ? O3 C15 C14 106.51(18) . . ? O3 C15 H15A 110.4 . . ? C14 C15 H15A 110.4 . . ? O3 C15 H15B 110.4 . . ? C14 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? C17 C16 O3 128.0(2) . . ? C17 C16 H16 116.0 . . ? O3 C16 H16 116.0 . . ? C16 C17 H17A 120.0 . . ? C16 C17 H17B 120.0 . . ? H17A C17 H17B 120.0 . . ? O4 C18 C19 110.32(17) . 2_576 ? O4 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 2_576 . ? O4 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 2_576 . ? H18A C18 H18B 108.1 . . ? O4 C19 C18 110.60(18) . 2_576 ? O4 C19 H19A 109.5 . . ? C18 C19 H19A 109.5 2_576 . ? O4 C19 H19B 109.5 . . ? C18 C19 H19B 109.5 2_576 . ? H19A C19 H19B 108.1 . . ? C22 C20 Al1 120.77(16) . . ? C22 C20 H20A 107.2(15) . . ? Al1 C20 H20A 107.9(15) . . ? C22 C20 H20B 109.8(16) . . ? Al1 C20 H20B 107.9(16) . . ? H20A C20 H20B 102(2) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C20 111.4(2) . . ? C23 C22 C21 109.7(2) . . ? C20 C22 C21 112.7(2) . . ? C23 C22 H22 107.6 . . ? C20 C22 H22 107.6 . . ? C21 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 Al1 122.80(18) . . ? C26 C24 H24B 108.7(17) . . ? Al1 C24 H24B 109.9(16) . . ? C26 C24 H24A 106.8(17) . . ? Al1 C24 H24A 99.8(17) . . ? H24B C24 H24A 108(2) . . ? C26 C25 H25D 77.6 . . ? H25A C25 H25D 63.8 . . ? H25B C25 H25D 70.5 . . ? H25C C25 H25D 172.0 . . ? C26 C25 H25E 93.8 . . ? H25A C25 H25E 122.2 . . ? H25B C25 H25E 16.8 . . ? H25C C25 H25E 111.0 . . ? H25D C25 H25E 71.3 . . ? C26 C25 H25F 115.4 . . ? H25A C25 H25F 15.5 . . ? H25B C25 H25F 117.7 . . ? H25C C25 H25F 94.0 . . ? H25D C25 H25F 79.3 . . ? H25E C25 H25F 132.7 . . ? C24 C26 C27 112.9(3) . . ? C24 C26 C25 105.1(3) . . ? C27 C26 C25 96.0(4) . . ? C24 C26 H26 113.7 . . ? C27 C26 H26 113.7 . . ? C25 C26 H26 113.7 . . ? C26 C27 H27D 104.4 . . ? H27A C27 H27D 130.5 . . ? H27B C27 H27D 22.9 . . ? H27C C27 H27D 91.3 . . ? C26 C27 H27E 88.8 . . ? H27A C27 H27E 139.6 . . ? H27B C27 H27E 96.8 . . ? H27C C27 H27E 30.8 . . ? H27D C27 H27E 74.3 . . ? C26 C27 H27F 133.5 . . ? H27A C27 H27F 56.1 . . ? H27B C27 H27F 117.0 . . ? H27C C27 H27F 54.2 . . ? H27D C27 H27F 117.8 . . ? H27E C27 H27F 84.9 . . ? C30A C28 C30 38.1(6) . . ? C30A C28 Al1 135.4(5) . . ? C30 C28 Al1 121.41(19) . . ? C30A C28 H28B 63.1(15) . . ? C30 C28 H28B 101.1(15) . . ? Al1 C28 H28B 108.7(15) . . ? C30A C28 H28A 113.0(15) . . ? C30 C28 H28A 107.5(14) . . ? Al1 C28 H28A 111.4(14) . . ? H28B C28 H28A 105(2) . . ? C28 C30 C29 112.0(2) . . ? C28 C30 C31 111.7(2) . . ? C29 C30 C31 107.7(2) . . ? C28 C30 H30 108.5 . . ? C29 C30 H30 108.5 . . ? C31 C30 H30 108.5 . . ? C28 C30A H30A 107.1 . . ? C28 C30A H28B 53.4(15) . . ? H30A C30A H28B 53.7 . . ? H25D C25A H25E 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? H27D C27A H27E 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Li1 O1 C1 -98.0(5) . . . . ? O4 Li1 O1 C1 56.7(5) . . . . ? O3 Li1 O1 C1 162.0(4) . . . . ? C14 Li1 O1 C1 -135.0(4) . . . . ? C28 Al1 O2 C14 -168.69(18) . . . . ? C24 Al1 O2 C14 -49.23(19) . . . . ? C20 Al1 O2 C14 66.05(19) . . . . ? C28 Al1 O2 Li1 27.72(18) . . . . ? C24 Al1 O2 Li1 147.18(17) . . . . ? C20 Al1 O2 Li1 -97.54(17) . . . . ? O1 Li1 O2 C14 -88.6(3) . . . . ? O4 Li1 O2 C14 118.3(2) . . . . ? O3 Li1 O2 C14 22.17(18) . . . . ? O1 Li1 O2 Al1 77.1(3) . . . . ? O4 Li1 O2 Al1 -76.0(2) . . . . ? O3 Li1 O2 Al1 -172.12(10) . . . . ? C14 Li1 O2 Al1 165.7(2) . . . . ? O1 Li1 O3 C16 -81.0(2) . . . . ? O2 Li1 O3 C16 147.12(18) . . . . ? O4 Li1 O3 C16 31.6(2) . . . . ? C14 Li1 O3 C16 160.02(19) . . . . ? O1 Li1 O3 C15 138.91(18) . . . . ? O2 Li1 O3 C15 7.01(18) . . . . ? O4 Li1 O3 C15 -108.52(17) . . . . ? C14 Li1 O3 C15 19.91(14) . . . . ? O1 Li1 O4 C18 18.5(3) . . . . ? O2 Li1 O4 C18 177.46(18) . . . . ? O3 Li1 O4 C18 -94.6(2) . . . . ? C14 Li1 O4 C18 -149.55(19) . . . . ? O1 Li1 O4 C19 -179.82(17) . . . . ? O2 Li1 O4 C19 -20.8(3) . . . . ? O3 Li1 O4 C19 67.1(2) . . . . ? C14 Li1 O4 C19 12.2(3) . . . . ? Li1 O1 C1 N1 156.8(4) . . . . ? Li1 O1 C1 C2 -26.7(5) . . . . ? C9 N1 C1 O1 -167.44(18) . . . . ? C12 N1 C1 O1 10.8(3) . . . . ? C9 N1 C1 C2 16.2(3) . . . . ? C12 N1 C1 C2 -165.56(17) . . . . ? O1 C1 C2 C3 56.2(3) . . . . ? N1 C1 C2 C3 -127.2(2) . . . . ? O1 C1 C2 C7 -115.4(2) . . . . ? N1 C1 C2 C7 61.2(3) . . . . ? C7 C2 C3 C4 -0.8(3) . . . . ? C1 C2 C3 C4 -172.5(2) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C4 C5 C6 C7 -1.0(4) . . . . ? C5 C6 C7 C2 0.8(4) . . . . ? C3 C2 C7 C6 0.1(3) . . . . ? C1 C2 C7 C6 171.7(2) . . . . ? C1 N1 C9 C8 -118.7(2) . . . . ? C12 N1 C9 C8 63.0(2) . . . . ? C1 N1 C9 C10 115.8(2) . . . . ? C12 N1 C9 C10 -62.5(2) . . . . ? C1 N1 C12 C13 61.9(2) . . . . ? C9 N1 C12 C13 -119.7(2) . . . . ? C1 N1 C12 C11 -66.3(2) . . . . ? C9 N1 C12 C11 112.0(2) . . . . ? Al1 O2 C14 C15 146.42(16) . . . . ? Li1 O2 C14 C15 -47.4(2) . . . . ? Al1 O2 C14 Li1 -166.1(2) . . . . ? O1 Li1 C14 O2 114.6(3) . . . . ? O4 Li1 C14 O2 -79.2(2) . . . . ? O3 Li1 C14 O2 -153.5(2) . . . . ? O1 Li1 C14 C15 -110.4(2) . . . . ? O2 Li1 C14 C15 135.1(2) . . . . ? O4 Li1 C14 C15 55.9(2) . . . . ? O3 Li1 C14 C15 -18.41(13) . . . . ? C16 O3 C15 C14 -175.77(18) . . . . ? Li1 O3 C15 C14 -32.5(2) . . . . ? O2 C14 C15 O3 53.6(2) . . . . ? Li1 C14 C15 O3 23.60(16) . . . . ? C15 O3 C16 C17 -3.4(3) . . . . ? Li1 O3 C16 C17 -140.1(2) . . . . ? C19 O4 C18 C19 57.7(3) . . . 2_576 ? Li1 O4 C18 C19 -139.2(2) . . . 2_576 ? C18 O4 C19 C18 -57.8(3) . . . 2_576 ? Li1 O4 C19 C18 137.42(19) . . . 2_576 ? O2 Al1 C20 C22 34.3(2) . . . . ? C28 Al1 C20 C22 -78.8(2) . . . . ? C24 Al1 C20 C22 155.5(2) . . . . ? Al1 C20 C22 C23 64.9(3) . . . . ? Al1 C20 C22 C21 -171.3(2) . . . . ? O2 Al1 C24 C26 -74.0(3) . . . . ? C28 Al1 C24 C26 38.0(3) . . . . ? C20 Al1 C24 C26 167.8(3) . . . . ? Al1 C24 C26 C27 -172.8(4) . . . . ? Al1 C24 C26 C25 83.8(4) . . . . ? O2 Al1 C28 C30A 160.3(9) . . . . ? C24 Al1 C28 C30A 40.1(9) . . . . ? C20 Al1 C28 C30A -81.6(9) . . . . ? O2 Al1 C28 C30 -153.6(2) . . . . ? C24 Al1 C28 C30 86.1(3) . . . . ? C20 Al1 C28 C30 -35.5(3) . . . . ? C30A C28 C30 C29 68.9(8) . . . . ? Al1 C28 C30 C29 -56.0(3) . . . . ? C30A C28 C30 C31 -51.9(8) . . . . ? Al1 C28 C30 C31 -176.87(18) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.483 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.044 ############################################################ ########### COMPOUND 5 ################################### ######################################################### data_dvgrem17 _database_code_depnum_ccdc_archive 'CCDC 634097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H68 Al Li O8' _chemical_formula_weight 614.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.1742(10) _cell_length_b 19.4623(9) _cell_length_c 19.9819(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7456.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4879 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 21.97 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; V weakly diffracting. Even with long count times, essentially zero intensity at higher angles. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8504 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 21.98 _reflns_number_total 4540 _reflns_number_gt 3283 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+20.5487P] 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 4540 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _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 C18 C 0.8436(3) -0.0186(3) 0.4864(3) 0.0362(13) Uani 1 1 d . . . C19 C 0.9097(3) -0.0616(3) 0.4812(3) 0.0480(14) Uani 1 1 d . . . H19A H 0.9116 -0.0836 0.4371 0.072 Uiso 1 1 calc R . . H19B H 0.9094 -0.0969 0.5161 0.072 Uiso 1 1 calc R . . H19C H 0.9505 -0.0319 0.4870 0.072 Uiso 1 1 calc R . . C20 C 0.8397(3) 0.0139(3) 0.5546(3) 0.0653(18) Uani 1 1 d . . . H20A H 0.7967 0.0410 0.5582 0.098 Uiso 1 1 calc R . . H20B H 0.8801 0.0441 0.5611 0.098 Uiso 1 1 calc R . . H20C H 0.8397 -0.0220 0.5890 0.098 Uiso 1 1 calc R . . C22 C 0.7569(3) 0.0907(2) 0.2635(2) 0.0340(12) Uani 1 1 d . . . C23 C 0.6861(3) 0.0589(2) 0.2465(3) 0.0414(13) Uani 1 1 d . . . H23A H 0.6903 0.0315 0.2056 0.062 Uiso 1 1 calc R . . H23B H 0.6517 0.0955 0.2397 0.062 Uiso 1 1 calc R . . H23C H 0.6710 0.0293 0.2835 0.062 Uiso 1 1 calc R . . C24 C 0.7839(3) 0.1309(3) 0.2033(2) 0.0445(14) Uani 1 1 d . . . H24A H 0.7852 0.1008 0.1640 0.067 Uiso 1 1 calc R . . H24B H 0.8309 0.1480 0.2128 0.067 Uiso 1 1 calc R . . H24C H 0.7528 0.1698 0.1944 0.067 Uiso 1 1 calc R . . C26 C 0.7708(3) 0.2351(2) 0.4650(3) 0.0376(13) Uani 1 1 d . . . C27 C 0.8498(3) 0.2255(3) 0.4642(3) 0.0580(17) Uani 1 1 d . . . H27A H 0.8722 0.2688 0.4514 0.087 Uiso 1 1 calc R . . H27B H 0.8621 0.1897 0.4317 0.087 Uiso 1 1 calc R . . H27C H 0.8658 0.2118 0.5088 0.087 Uiso 1 1 calc R . . C28 C 0.7516(3) 0.2959(2) 0.5092(3) 0.0488(14) Uani 1 1 d . . . H28A H 0.7769 0.3368 0.4940 0.073 Uiso 1 1 calc R . . H28B H 0.7643 0.2858 0.5556 0.073 Uiso 1 1 calc R . . H28C H 0.7013 0.3043 0.5063 0.073 Uiso 1 1 calc R . . C30 C 0.6464(3) -0.0159(3) 0.4885(2) 0.0375(13) Uani 1 1 d . . . C31 C 0.6277(3) 0.0324(3) 0.5448(3) 0.0614(17) Uani 1 1 d . . . H31A H 0.6173 0.0058 0.5852 0.092 Uiso 1 1 calc R . . H31B H 0.5868 0.0595 0.5321 0.092 Uiso 1 1 calc R . . H31C H 0.6671 0.0633 0.5536 0.092 Uiso 1 1 calc R . . C32 C 0.5873(3) -0.0679(3) 0.4789(3) 0.0453(14) Uani 1 1 d . . . H32A H 0.5783 -0.0915 0.5214 0.068 Uiso 1 1 calc R . . H32B H 0.6008 -0.1016 0.4449 0.068 Uiso 1 1 calc R . . H32C H 0.5450 -0.0438 0.4645 0.068 Uiso 1 1 calc R . . H18 H 0.808(2) -0.049(2) 0.480(2) 0.030(13) Uiso 1 1 d . . . H22 H 0.792(2) 0.051(2) 0.268(2) 0.044(14) Uiso 1 1 d . . . H26 H 0.753(2) 0.248(2) 0.417(2) 0.046(13) Uiso 1 1 d . . . H30 H 0.697(2) -0.040(2) 0.507(2) 0.040(13) Uiso 1 1 d . . . Li1 Li 0.9234(4) -0.1387(4) 0.2705(4) 0.0348(19) Uani 1 1 d . . . Al1 Al 0.74580(7) 0.08809(7) 0.41894(6) 0.0292(3) Uani 1 1 d . . . O1 O 0.94568(16) -0.20037(15) 0.19665(15) 0.0353(8) Uani 1 1 d . . . O2 O 0.93879(18) -0.28357(17) 0.08096(17) 0.0478(10) Uani 1 1 d . . . O3 O 0.95416(15) -0.18661(15) 0.34894(15) 0.0333(8) Uani 1 1 d . . . O4 O 1.01972(18) -0.30405(16) 0.40416(16) 0.0430(9) Uani 1 1 d . . . O5 O 0.97350(16) -0.05260(15) 0.26095(16) 0.0359(8) Uani 1 1 d . . . O6 O 0.99714(19) 0.09019(15) 0.24613(18) 0.0448(9) Uani 1 1 d . . . O7 O 0.82153(15) -0.13167(15) 0.26487(15) 0.0328(8) Uani 1 1 d . . . O8 O 0.67494(16) -0.13599(16) 0.24447(18) 0.0434(9) Uani 1 1 d . . . C1 C 1.0021(3) -0.2019(3) 0.1477(3) 0.0455(14) Uani 1 1 d . . . H1A H 1.0365 -0.2377 0.1602 0.055 Uiso 1 1 calc R . . H1B H 1.0263 -0.1570 0.1468 0.055 Uiso 1 1 calc R . . C2 C 0.9721(3) -0.2174(3) 0.0801(3) 0.0472(14) Uani 1 1 d . . . H2A H 0.9377 -0.1817 0.0679 0.057 Uiso 1 1 calc R . . H2B H 1.0097 -0.2171 0.0461 0.057 Uiso 1 1 calc R . . C3 C 0.8845(3) -0.2822(3) 0.1284(2) 0.0425(14) Uani 1 1 d . . . H3A H 0.8610 -0.3275 0.1293 0.051 Uiso 1 1 calc R . . H3B H 0.8496 -0.2473 0.1151 0.051 Uiso 1 1 calc R . . C4 C 0.9113(3) -0.2658(2) 0.1968(2) 0.0393(13) Uani 1 1 d . . . H4A H 0.8721 -0.2649 0.2290 0.047 Uiso 1 1 calc R . . H4B H 0.9445 -0.3019 0.2112 0.047 Uiso 1 1 calc R . . C5 C 1.0280(2) -0.1877(2) 0.3635(3) 0.0399(13) Uani 1 1 d . . . H5A H 1.0363 -0.1693 0.4090 0.048 Uiso 1 1 calc R . . H5B H 1.0532 -0.1582 0.3312 0.048 Uiso 1 1 calc R . . C6 C 1.0551(3) -0.2602(3) 0.3592(3) 0.0478(14) Uani 1 1 d . . . H6A H 1.0490 -0.2775 0.3129 0.057 Uiso 1 1 calc R . . H6B H 1.1056 -0.2606 0.3695 0.057 Uiso 1 1 calc R . . C7 C 0.9473(3) -0.3043(2) 0.3890(3) 0.0416(13) Uani 1 1 d . . . H7A H 0.9225 -0.3349 0.4207 0.050 Uiso 1 1 calc R . . H7B H 0.9401 -0.3223 0.3432 0.050 Uiso 1 1 calc R . . C8 C 0.9180(3) -0.2323(2) 0.3940(3) 0.0396(13) Uani 1 1 d . . . H8A H 0.8677 -0.2330 0.3827 0.048 Uiso 1 1 calc R . . H8B H 0.9229 -0.2154 0.4405 0.048 Uiso 1 1 calc R . . C9 C 1.0030(3) -0.0119(3) 0.3138(3) 0.0527(16) Uani 1 1 d . . . H9A H 1.0545 -0.0130 0.3107 0.063 Uiso 1 1 calc R . . H9B H 0.9892 -0.0313 0.3576 0.063 Uiso 1 1 calc R . . C10 C 0.9784(3) 0.0605(3) 0.3090(3) 0.0563(16) Uani 1 1 d . . . H10A H 0.9270 0.0617 0.3142 0.068 Uiso 1 1 calc R . . H10B H 0.9992 0.0877 0.3458 0.068 Uiso 1 1 calc R . . C11 C 0.9670(3) 0.0502(2) 0.1943(3) 0.0447(14) Uani 1 1 d . . . H11A H 0.9795 0.0702 0.1504 0.054 Uiso 1 1 calc R . . H11B H 0.9155 0.0512 0.1986 0.054 Uiso 1 1 calc R . . C12 C 0.9921(3) -0.0228(2) 0.1977(2) 0.0406(13) Uani 1 1 d . . . H12A H 0.9708 -0.0497 0.1610 0.049 Uiso 1 1 calc R . . H12B H 1.0434 -0.0240 0.1921 0.049 Uiso 1 1 calc R . . C13 C 0.7905(2) -0.1123(3) 0.2026(2) 0.0408(13) Uani 1 1 d . . . H13A H 0.8228 -0.1235 0.1655 0.049 Uiso 1 1 calc R . . H13B H 0.7824 -0.0621 0.2022 0.049 Uiso 1 1 calc R . . C14 C 0.7227(3) -0.1489(3) 0.1920(2) 0.0431(14) Uani 1 1 d . . . H14A H 0.7020 -0.1338 0.1491 0.052 Uiso 1 1 calc R . . H14B H 0.7314 -0.1990 0.1890 0.052 Uiso 1 1 calc R . . C15 C 0.7060(2) -0.1550(3) 0.3062(3) 0.0404(13) Uani 1 1 d . . . H15A H 0.7151 -0.2051 0.3061 0.048 Uiso 1 1 calc R . . H15B H 0.6732 -0.1450 0.3432 0.048 Uiso 1 1 calc R . . C16 C 0.7727(2) -0.1177(2) 0.3182(2) 0.0381(13) Uani 1 1 d . . . H16A H 0.7635 -0.0677 0.3206 0.046 Uiso 1 1 calc R . . H16B H 0.7929 -0.1323 0.3615 0.046 Uiso 1 1 calc R . . C17 C 0.8350(2) 0.0337(2) 0.4305(2) 0.0304(11) Uani 1 1 d . . . H17A H 0.8433 0.0091 0.3879 0.036 Uiso 1 1 calc R . . H17B H 0.8733 0.0674 0.4354 0.036 Uiso 1 1 calc R . . C21 C 0.7531(3) 0.1326(2) 0.3272(2) 0.0345(11) Uani 1 1 d . . . H21A H 0.7124 0.1636 0.3226 0.041 Uiso 1 1 calc R . . H21B H 0.7950 0.1622 0.3280 0.041 Uiso 1 1 calc R . . C25 C 0.7345(2) 0.1687(2) 0.4831(2) 0.0345(12) Uani 1 1 d . . . H25A H 0.6840 0.1784 0.4876 0.041 Uiso 1 1 calc R . . H25B H 0.7515 0.1540 0.5276 0.041 Uiso 1 1 calc R . . C29 C 0.6636(2) 0.0229(2) 0.4240(2) 0.0309(12) Uani 1 1 d . . . H29A H 0.6216 0.0496 0.4117 0.037 Uiso 1 1 calc R . . H29B H 0.6703 -0.0120 0.3885 0.037 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 C18 0.033(3) 0.033(3) 0.043(3) 0.002(3) -0.001(3) 0.000(3) C19 0.047(3) 0.042(3) 0.055(4) 0.007(3) -0.009(3) 0.001(3) C20 0.091(5) 0.067(4) 0.037(3) 0.006(3) -0.001(3) 0.035(4) C22 0.039(3) 0.027(3) 0.036(3) 0.005(2) 0.002(3) 0.004(3) C23 0.046(3) 0.039(3) 0.039(3) 0.002(3) -0.004(3) -0.002(3) C24 0.050(3) 0.048(3) 0.036(3) 0.006(3) 0.006(3) 0.002(3) C26 0.049(3) 0.025(3) 0.039(3) 0.000(2) 0.002(3) -0.002(2) C27 0.044(3) 0.042(3) 0.088(5) -0.019(3) 0.002(3) -0.008(3) C28 0.056(3) 0.032(3) 0.059(3) -0.008(3) 0.009(3) -0.006(3) C30 0.040(3) 0.036(3) 0.036(3) 0.001(3) 0.005(3) -0.005(3) C31 0.076(4) 0.064(4) 0.045(4) -0.012(3) 0.022(3) -0.029(3) C32 0.050(3) 0.037(3) 0.049(3) 0.003(3) 0.006(3) -0.011(3) Li1 0.041(5) 0.030(4) 0.034(5) 0.000(4) -0.006(4) -0.003(4) Al1 0.0360(8) 0.0227(7) 0.0288(7) -0.0003(6) -0.0011(7) -0.0020(7) O1 0.0395(19) 0.0303(19) 0.0361(19) -0.0042(16) 0.0068(17) -0.0056(16) O2 0.058(2) 0.044(2) 0.042(2) -0.0113(18) 0.008(2) -0.0068(19) O3 0.0325(19) 0.0321(18) 0.0354(19) 0.0073(16) 0.0003(16) 0.0006(15) O4 0.052(2) 0.033(2) 0.043(2) 0.0052(17) -0.0034(18) 0.0114(18) O5 0.0419(19) 0.0288(17) 0.037(2) 0.0064(16) -0.0028(17) -0.0093(15) O6 0.061(2) 0.0309(18) 0.043(2) 0.0003(19) 0.0048(18) -0.0156(18) O7 0.0302(18) 0.0340(18) 0.0342(19) 0.0021(15) 0.0009(17) 0.0040(15) O8 0.0334(19) 0.048(2) 0.049(2) 0.0064(18) -0.0033(19) 0.0015(17) C1 0.038(3) 0.041(3) 0.057(4) -0.011(3) 0.012(3) -0.004(3) C2 0.054(3) 0.049(3) 0.039(3) -0.001(3) 0.011(3) -0.007(3) C3 0.053(3) 0.036(3) 0.038(3) -0.003(2) 0.004(3) -0.011(3) C4 0.048(3) 0.029(3) 0.040(3) 0.001(2) 0.003(3) -0.006(2) C5 0.033(3) 0.042(3) 0.045(3) 0.003(3) -0.004(3) -0.002(3) C6 0.043(3) 0.051(3) 0.050(3) -0.003(3) -0.004(3) 0.011(3) C7 0.052(3) 0.027(3) 0.046(3) 0.003(3) 0.001(3) 0.002(3) C8 0.043(3) 0.030(3) 0.045(3) 0.006(3) 0.007(3) 0.002(2) C9 0.080(4) 0.045(4) 0.033(3) 0.006(3) -0.012(3) -0.026(3) C10 0.083(4) 0.044(4) 0.042(3) -0.004(3) 0.020(3) -0.024(3) C11 0.055(3) 0.035(3) 0.044(3) 0.007(3) -0.006(3) -0.009(3) C12 0.056(3) 0.031(3) 0.035(3) 0.006(2) -0.002(3) -0.008(3) C13 0.042(3) 0.040(3) 0.041(3) 0.007(3) 0.003(3) 0.004(3) C14 0.046(3) 0.048(3) 0.035(3) 0.005(3) -0.009(3) -0.001(3) C15 0.042(3) 0.035(3) 0.044(3) 0.001(3) 0.012(3) 0.000(3) C16 0.043(3) 0.036(3) 0.036(3) -0.006(2) 0.002(3) 0.004(2) C17 0.037(3) 0.025(3) 0.030(3) -0.003(2) -0.002(2) -0.004(2) C21 0.037(3) 0.029(3) 0.037(3) 0.002(2) -0.005(3) 0.003(2) C25 0.036(3) 0.036(3) 0.032(3) 0.000(2) -0.002(2) -0.002(2) C29 0.038(3) 0.024(3) 0.031(3) -0.003(2) 0.005(2) 0.003(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 C18 C20 1.504(7) . ? C18 C19 1.521(7) . ? C18 C17 1.522(6) . ? C22 C21 1.512(6) . ? C22 C24 1.526(6) . ? C22 C23 1.530(7) . ? C26 C25 1.512(6) . ? C26 C28 1.521(6) . ? C26 C27 1.526(7) . ? C30 C31 1.510(7) . ? C30 C29 1.529(6) . ? C30 C32 1.531(7) . ? Li1 O3 1.917(8) . ? Li1 O5 1.942(8) . ? Li1 O1 1.949(8) . ? Li1 O7 1.960(8) . ? Al1 C17 2.026(5) . ? Al1 C29 2.026(5) . ? Al1 C21 2.033(4) . ? Al1 C25 2.037(4) . ? O1 C4 1.434(5) . ? O1 C1 1.459(6) . ? O2 C3 1.409(6) . ? O2 C2 1.437(6) . ? O3 C8 1.443(5) . ? O3 C5 1.446(5) . ? O4 C6 1.413(6) . ? O4 C7 1.421(6) . ? O5 C12 1.436(5) . ? O5 C9 1.436(6) . ? O6 C11 1.418(6) . ? O6 C10 1.430(6) . ? O7 C13 1.430(5) . ? O7 C16 1.445(5) . ? O8 C14 1.415(6) . ? O8 C15 1.419(6) . ? C1 C2 1.499(7) . ? C3 C4 1.494(6) . ? C5 C6 1.507(7) . ? C7 C8 1.513(6) . ? C9 C10 1.487(7) . ? C11 C12 1.502(7) . ? C13 C14 1.497(6) . ? C15 C16 1.490(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 C18 C19 109.5(4) . . ? C20 C18 C17 112.2(4) . . ? C19 C18 C17 114.0(4) . . ? C21 C22 C24 113.7(4) . . ? C21 C22 C23 111.2(4) . . ? C24 C22 C23 109.5(4) . . ? C25 C26 C28 114.5(4) . . ? C25 C26 C27 110.9(4) . . ? C28 C26 C27 110.0(4) . . ? C31 C30 C29 111.8(4) . . ? C31 C30 C32 109.2(4) . . ? C29 C30 C32 112.4(4) . . ? O3 Li1 O5 110.3(4) . . ? O3 Li1 O1 104.6(4) . . ? O5 Li1 O1 110.4(4) . . ? O3 Li1 O7 112.8(4) . . ? O5 Li1 O7 115.3(4) . . ? O1 Li1 O7 102.6(4) . . ? C17 Al1 C29 108.91(18) . . ? C17 Al1 C21 105.5(2) . . ? C29 Al1 C21 111.4(2) . . ? C17 Al1 C25 114.88(19) . . ? C29 Al1 C25 111.58(19) . . ? C21 Al1 C25 104.33(19) . . ? C4 O1 C1 108.9(3) . . ? C4 O1 Li1 116.4(3) . . ? C1 O1 Li1 133.1(4) . . ? C3 O2 C2 108.6(4) . . ? C8 O3 C5 109.6(3) . . ? C8 O3 Li1 131.4(4) . . ? C5 O3 Li1 118.3(4) . . ? C6 O4 C7 109.6(4) . . ? C12 O5 C9 109.0(3) . . ? C12 O5 Li1 123.9(4) . . ? C9 O5 Li1 126.8(4) . . ? C11 O6 C10 108.5(3) . . ? C13 O7 C16 108.8(3) . . ? C13 O7 Li1 118.9(4) . . ? C16 O7 Li1 128.1(4) . . ? C14 O8 C15 109.0(3) . . ? O1 C1 C2 108.8(4) . . ? O2 C2 C1 109.9(4) . . ? O2 C3 C4 111.4(4) . . ? O1 C4 C3 110.3(4) . . ? O3 C5 C6 109.9(4) . . ? O4 C6 C5 111.3(4) . . ? O4 C7 C8 110.3(4) . . ? O3 C8 C7 110.5(4) . . ? O5 C9 C10 110.5(4) . . ? O6 C10 C9 111.0(4) . . ? O6 C11 C12 110.8(4) . . ? O5 C12 C11 110.0(4) . . ? O7 C13 C14 111.1(4) . . ? O8 C14 C13 111.8(4) . . ? O8 C15 C16 111.9(4) . . ? O7 C16 C15 110.2(4) . . ? C18 C17 Al1 121.6(3) . . ? C22 C21 Al1 122.2(3) . . ? C26 C25 Al1 117.3(3) . . ? C30 C29 Al1 121.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Li1 O1 C4 62.3(5) . . . . ? O5 Li1 O1 C4 -179.1(4) . . . . ? O7 Li1 O1 C4 -55.7(5) . . . . ? O3 Li1 O1 C1 -101.2(5) . . . . ? O5 Li1 O1 C1 17.5(7) . . . . ? O7 Li1 O1 C1 140.9(4) . . . . ? O5 Li1 O3 C8 148.8(4) . . . . ? O1 Li1 O3 C8 -92.5(5) . . . . ? O7 Li1 O3 C8 18.2(7) . . . . ? O5 Li1 O3 C5 -41.6(5) . . . . ? O1 Li1 O3 C5 77.1(5) . . . . ? O7 Li1 O3 C5 -172.2(4) . . . . ? O3 Li1 O5 C12 146.1(4) . . . . ? O1 Li1 O5 C12 31.0(6) . . . . ? O7 Li1 O5 C12 -84.6(5) . . . . ? O3 Li1 O5 C9 -28.1(6) . . . . ? O1 Li1 O5 C9 -143.2(4) . . . . ? O7 Li1 O5 C9 101.1(5) . . . . ? O3 Li1 O7 C13 -165.3(4) . . . . ? O5 Li1 O7 C13 66.7(5) . . . . ? O1 Li1 O7 C13 -53.3(5) . . . . ? O3 Li1 O7 C16 40.6(6) . . . . ? O5 Li1 O7 C16 -87.4(5) . . . . ? O1 Li1 O7 C16 152.6(4) . . . . ? C4 O1 C1 C2 59.2(5) . . . . ? Li1 O1 C1 C2 -136.4(5) . . . . ? C3 O2 C2 C1 60.8(5) . . . . ? O1 C1 C2 O2 -61.2(5) . . . . ? C2 O2 C3 C4 -59.3(5) . . . . ? C1 O1 C4 C3 -57.7(5) . . . . ? Li1 O1 C4 C3 135.0(4) . . . . ? O2 C3 C4 O1 58.9(5) . . . . ? C8 O3 C5 C6 56.5(5) . . . . ? Li1 O3 C5 C6 -115.3(5) . . . . ? C7 O4 C6 C5 59.7(5) . . . . ? O3 C5 C6 O4 -58.6(5) . . . . ? C6 O4 C7 C8 -59.0(5) . . . . ? C5 O3 C8 C7 -56.9(5) . . . . ? Li1 O3 C8 C7 113.4(5) . . . . ? O4 C7 C8 O3 58.4(5) . . . . ? C12 O5 C9 C10 57.6(6) . . . . ? Li1 O5 C9 C10 -127.4(5) . . . . ? C11 O6 C10 C9 58.9(6) . . . . ? O5 C9 C10 O6 -59.0(6) . . . . ? C10 O6 C11 C12 -59.2(5) . . . . ? C9 O5 C12 C11 -57.7(5) . . . . ? Li1 O5 C12 C11 127.2(4) . . . . ? O6 C11 C12 O5 59.8(5) . . . . ? C16 O7 C13 C14 -56.7(5) . . . . ? Li1 O7 C13 C14 144.6(4) . . . . ? C15 O8 C14 C13 -56.5(5) . . . . ? O7 C13 C14 O8 57.7(5) . . . . ? C14 O8 C15 C16 57.6(5) . . . . ? C13 O7 C16 C15 57.3(5) . . . . ? Li1 O7 C16 C15 -146.5(4) . . . . ? O8 C15 C16 O7 -59.0(5) . . . . ? C20 C18 C17 Al1 -63.0(6) . . . . ? C19 C18 C17 Al1 171.7(4) . . . . ? C29 Al1 C17 C18 -47.7(4) . . . . ? C21 Al1 C17 C18 -167.4(4) . . . . ? C25 Al1 C17 C18 78.3(4) . . . . ? C24 C22 C21 Al1 -162.5(3) . . . . ? C23 C22 C21 Al1 73.4(5) . . . . ? C17 Al1 C21 C22 63.1(4) . . . . ? C29 Al1 C21 C22 -55.0(5) . . . . ? C25 Al1 C21 C22 -175.5(4) . . . . ? C28 C26 C25 Al1 171.3(4) . . . . ? C27 C26 C25 Al1 -63.5(5) . . . . ? C17 Al1 C25 C26 82.3(4) . . . . ? C29 Al1 C25 C26 -153.1(3) . . . . ? C21 Al1 C25 C26 -32.7(4) . . . . ? C31 C30 C29 Al1 62.9(5) . . . . ? C32 C30 C29 Al1 -173.9(3) . . . . ? C17 Al1 C29 C30 65.1(4) . . . . ? C21 Al1 C29 C30 -178.9(3) . . . . ? C25 Al1 C29 C30 -62.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.265 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.054 ###=END