# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1658 data_global _publ_contact_letter ; These are the CIF format data (2 compounds) for the paper "An unprecedented coordination mode for hemi-labile 1,4,7-triazacyclononanes and the synthesis of cationic organo-aluminium complexes" D. A. Robson, L. H. Rees, P. Mountford* and M. Schroeder ; _publ_contact_author ; Dr P. Mountford Inorganic Chemistry Laboratory South Parks Road Oxford OX1 3QR UK ; _publ_contact_author_phone '+44 1865 272679' _contact_author_fax '+44 1865 272690' _publ_contact_author_email Philip.Mountford@chem.ox.ac.uk data_compound1 # Local code STR35 _audit_creation_method SHELXL _chemical_name_systematic ; [Al(L-1)Me2] ; _chemical_name_common ? _chemical_formula_moiety 'C29 H54 Al N3 O' _chemical_formula_structural 'C29 H54 AL N3 O' _chemical_formula_analytical ? _chemical_formula_sum 'C29 H54 Al N3 O' _chemical_formula_weight 487.73 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.3380(6) _cell_length_b 13.9560(7) _cell_length_c 20.8520(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3008.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 130 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method none _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Enraf-Nonius DIP2000 Image Plate Diffractometer' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7450 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3926 _reflns_number_observed 3832 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius DIP2000 Software - XPRESS' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+3.4590P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.59(36) _refine_ls_number_reflns 3924 _refine_ls_number_parameters 319 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_obs 0.0715 _refine_ls_wR_factor_all 0.1466 _refine_ls_wR_factor_obs 0.1446 _refine_ls_goodness_of_fit_all 1.410 _refine_ls_goodness_of_fit_obs 1.421 _refine_ls_restrained_S_all 1.421 _refine_ls_restrained_S_obs 1.420 _refine_ls_shift/esd_max -0.017 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.31200(13) 0.11801(10) 0.17284(7) 0.0223(3) Uani 1 d . . O17 O 0.3899(3) 0.0138(2) 0.1453(2) 0.0311(9) Uani 1 d . . N7 N 0.6626(4) 0.3524(3) 0.1117(2) 0.0248(10) Uani 1 d . . N1 N 0.4716(3) 0.2003(3) 0.1701(2) 0.0194(8) Uani 1 d . . N4 N 0.3603(4) 0.4004(3) 0.1251(2) 0.0235(9) Uani 1 d . . C10 C 0.5720(4) 0.1409(3) 0.2037(2) 0.0216(11) Uani 1 d . . H10A H 0.6496(4) 0.1793(3) 0.2085(2) 0.026 Uiso 1 calc R . H10B H 0.5407(4) 0.1260(3) 0.2464(2) 0.026 Uiso 1 calc R . C3 C 0.3471(5) 0.3567(3) 0.1877(2) 0.0236(11) Uani 1 d . . H3A H 0.2674(5) 0.3201(3) 0.1885(2) 0.028 Uiso 1 calc R . H3B H 0.3392(5) 0.4073(3) 0.2194(2) 0.028 Uiso 1 calc R . C12 C 0.7368(4) 0.0226(3) 0.1709(2) 0.0233(11) Uani 1 d . . H12 H 0.7975(4) 0.0650(3) 0.1875(2) 0.028 Uiso 1 calc R . C13 C 0.7791(4) -0.0636(3) 0.1472(2) 0.0214(11) Uani 1 d . . C14 C 0.6840(5) -0.1226(3) 0.1215(2) 0.0271(11) Uani 1 d . . H14 H 0.7095(5) -0.1812(3) 0.1046(2) 0.033 Uiso 1 calc R . C15 C 0.5535(5) -0.0998(3) 0.1195(2) 0.0219(11) Uani 1 d . . C5 C 0.4714(5) 0.4641(3) 0.1193(3) 0.0315(13) Uani 1 d . . H5A H 0.5030(5) 0.4787(3) 0.1620(3) 0.038 Uiso 1 calc R . H5B H 0.4428(5) 0.5237(3) 0.1001(3) 0.038 Uiso 1 calc R . C8 C 0.6403(4) 0.2554(3) 0.0875(2) 0.0224(11) Uani 1 d . . H8A H 0.7042(4) 0.2129(3) 0.1062(2) 0.027 Uiso 1 calc R . H8B H 0.6534(4) 0.2554(3) 0.0414(2) 0.027 Uiso 1 calc R . C71 C 0.8005(4) 0.3768(4) 0.1155(2) 0.0312(12) Uani 1 d . . H71 H 0.8048(4) 0.4451(4) 0.1261(2) 0.037 Uiso 1 calc R . C9 C 0.5073(4) 0.2162(3) 0.1016(2) 0.0210(11) Uani 1 d . . H9A H 0.4443(4) 0.2598(3) 0.0832(2) 0.025 Uiso 1 calc R . H9B H 0.4986(4) 0.1556(3) 0.0793(2) 0.025 Uiso 1 calc R . C11 C 0.6079(4) 0.0491(3) 0.1712(2) 0.0174(10) Uani 1 d . . C2 C 0.4565(5) 0.2916(3) 0.2075(2) 0.0217(11) Uani 1 d U . H2A H 0.5367(5) 0.3274(3) 0.2042(2) 0.026 Uiso 1 calc R . H2B H 0.4447(5) 0.2751(3) 0.2523(2) 0.026 Uiso 1 calc R . C6 C 0.5835(5) 0.4248(3) 0.0797(2) 0.0297(13) Uani 1 d . . H6A H 0.5489(5) 0.3973(3) 0.0406(2) 0.036 Uiso 1 calc R . H6B H 0.6390(5) 0.4779(3) 0.0676(2) 0.036 Uiso 1 calc R . C131 C 0.9217(5) -0.0938(4) 0.1469(2) 0.0290(12) Uani 1 d . . C16 C 0.5155(5) -0.0120(3) 0.1460(2) 0.0239(11) Uani 1 d . . C151 C 0.4541(5) -0.1681(3) 0.0886(2) 0.0296(12) Uani 1 d . . C43 C 0.2428(5) 0.4578(4) 0.0303(3) 0.045(2) Uani 1 d . . H43A H 0.2995(29) 0.5106(18) 0.0214(3) 0.068 Uiso 1 calc R . H43B H 0.1576(8) 0.4723(26) 0.0147(4) 0.068 Uiso 1 calc R . H43C H 0.2746(34) 0.4013(10) 0.0093(3) 0.068 Uiso 1 calc R . C153 C 0.3479(5) -0.1947(4) 0.1351(3) 0.0372(14) Uani 1 d . . H15A H 0.2826(16) -0.2309(21) 0.1130(4) 0.056 Uiso 1 calc R . H15B H 0.3102(22) -0.1374(4) 0.1525(12) 0.056 Uiso 1 calc R . H15C H 0.3834(8) -0.2326(20) 0.1692(9) 0.056 Uiso 1 calc R . C132 C 1.0032(5) -0.0308(4) 0.1916(3) 0.046(2) Uani 1 d . . H13A H 1.0914(9) -0.0523(17) 0.1909(14) 0.069 Uiso 1 calc R . H13B H 0.9700(22) -0.0352(21) 0.2345(4) 0.069 Uiso 1 calc R . H13C H 0.9991(29) 0.0346(6) 0.1773(10) 0.069 Uiso 1 calc R . C42 C 0.1922(6) 0.5291(4) 0.1372(3) 0.046(2) Uani 1 d . . H42A H 0.1058(15) 0.5447(16) 0.1240(13) 0.069 Uiso 1 calc R . H42B H 0.2488(22) 0.5817(8) 0.1276(14) 0.069 Uiso 1 calc R . H42C H 0.1934(34) 0.5169(10) 0.1825(3) 0.069 Uiso 1 calc R . C41 C 0.2373(4) 0.4409(4) 0.1018(2) 0.0277(12) Uani 1 d . . H41 H 0.1712(4) 0.3917(4) 0.1088(2) 0.033 Uiso 1 calc R . C19 C 0.1863(5) 0.1634(3) 0.1099(2) 0.0308(12) Uani 1 d . . H19A H 0.2255(10) 0.2115(16) 0.0833(10) 0.046 Uiso 1 calc R . H19B H 0.1130(14) 0.1903(20) 0.1317(2) 0.046 Uiso 1 calc R . H19C H 0.1586(23) 0.1107(5) 0.0837(10) 0.046 Uiso 1 calc R . C72 C 0.8735(5) 0.3646(4) 0.0528(2) 0.0366(14) Uani 1 d . . H72A H 0.8810(28) 0.2977(4) 0.0430(8) 0.055 Uiso 1 calc R . H72B H 0.9583(13) 0.3920(21) 0.0569(6) 0.055 Uiso 1 calc R . H72C H 0.8274(18) 0.3965(21) 0.0190(4) 0.055 Uiso 1 calc R . C73 C 0.8664(5) 0.3246(4) 0.1693(3) 0.0424(14) Uani 1 d . . H73A H 0.9537(12) 0.3471(18) 0.1733(11) 0.064 Uiso 1 calc R . H73B H 0.8668(29) 0.2571(5) 0.1604(8) 0.064 Uiso 1 calc R . H73C H 0.8207(20) 0.3363(20) 0.2086(4) 0.064 Uiso 1 calc R . C154 C 0.3937(6) -0.1183(4) 0.0304(3) 0.0459(15) Uani 1 d . . H15D H 0.3487(32) -0.0618(16) 0.0442(3) 0.069 Uiso 1 calc R . H15E H 0.3340(29) -0.1611(11) 0.0099(11) 0.069 Uiso 1 calc R . H15F H 0.4606(7) -0.1008(25) 0.0007(9) 0.069 Uiso 1 calc R . C133 C 0.9762(6) -0.0822(6) 0.0806(3) 0.062(2) Uani 1 d . . H13D H 1.0663(12) -0.0987(31) 0.0808(5) 0.093 Uiso 1 calc R . H13E H 0.9661(38) -0.0169(9) 0.0670(9) 0.093 Uiso 1 calc R . H13F H 0.9308(29) -0.1237(23) 0.0515(5) 0.093 Uiso 1 calc R . C18 C 0.2616(5) 0.1061(4) 0.2634(2) 0.0388(13) Uani 1 d . . H18A H 0.1698(7) 0.1148(24) 0.2673(3) 0.058 Uiso 1 calc R . H18B H 0.3055(26) 0.1540(16) 0.2882(3) 0.058 Uiso 1 calc R . H18C H 0.2848(30) 0.0436(10) 0.2788(5) 0.058 Uiso 1 calc R . C152 C 0.5155(6) -0.2603(4) 0.0653(3) 0.050(2) Uani 1 d . . H15G H 0.5782(28) -0.2460(4) 0.0327(14) 0.075 Uiso 1 calc R . H15H H 0.4499(8) -0.3015(12) 0.0479(17) 0.075 Uiso 1 calc R . H15I H 0.5574(33) -0.2919(15) 0.1006(5) 0.075 Uiso 1 calc R . C134 C 0.9363(6) -0.1959(4) 0.1704(4) 0.062(2) Uani 1 d . . H13G H 0.8964(37) -0.2021(9) 0.2118(10) 0.093 Uiso 1 calc R . H13H H 1.0265(6) -0.2115(11) 0.1737(20) 0.093 Uiso 1 calc R . H13I H 0.8953(37) -0.2388(5) 0.1407(11) 0.093 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0229(7) 0.0201(8) 0.0238(7) 0.0038(7) 0.0001(6) -0.0010(7) O17 0.018(2) 0.026(2) 0.049(2) -0.003(2) -0.005(2) -0.005(2) N7 0.023(2) 0.025(2) 0.026(2) -0.002(2) -0.001(2) -0.003(2) N1 0.026(2) 0.017(2) 0.015(2) 0.001(2) -0.005(2) -0.002(2) N4 0.026(2) 0.016(2) 0.029(2) 0.003(2) 0.005(2) -0.002(2) C10 0.023(3) 0.021(3) 0.020(3) 0.000(2) -0.003(2) 0.001(2) C3 0.035(3) 0.017(3) 0.019(3) -0.003(2) 0.003(2) 0.001(2) C12 0.028(3) 0.019(2) 0.023(3) -0.003(2) -0.003(2) -0.007(2) C13 0.026(3) 0.023(3) 0.015(2) 0.005(2) 0.000(2) -0.001(2) C14 0.035(3) 0.021(3) 0.025(3) -0.002(2) 0.011(2) 0.004(3) C15 0.035(3) 0.012(2) 0.019(2) 0.001(2) -0.002(2) 0.001(2) C5 0.032(3) 0.015(2) 0.048(3) 0.003(2) -0.005(3) -0.004(2) C8 0.023(3) 0.024(3) 0.020(3) -0.001(2) 0.001(2) 0.000(2) C71 0.025(3) 0.029(3) 0.040(3) -0.008(3) 0.007(2) -0.008(3) C9 0.026(3) 0.017(2) 0.020(3) -0.008(2) -0.002(2) 0.002(2) C11 0.018(2) 0.015(2) 0.019(2) 0.005(2) -0.001(2) 0.004(2) C2 0.033(3) 0.018(2) 0.013(2) 0.003(2) 0.001(2) 0.000(2) C6 0.029(3) 0.026(3) 0.034(3) 0.006(2) 0.003(2) -0.008(2) C131 0.025(3) 0.031(3) 0.031(3) -0.004(2) 0.005(2) 0.004(2) C16 0.027(3) 0.022(3) 0.023(3) 0.003(2) 0.002(2) -0.005(2) C151 0.038(3) 0.023(3) 0.027(3) -0.003(2) -0.008(3) -0.007(2) C43 0.040(3) 0.056(4) 0.040(3) 0.018(3) -0.007(3) -0.003(3) C153 0.043(3) 0.027(3) 0.042(3) 0.006(3) -0.013(3) -0.010(3) C132 0.033(3) 0.058(4) 0.048(4) -0.003(3) -0.004(3) 0.010(3) C42 0.039(3) 0.040(3) 0.058(4) 0.011(3) 0.013(3) 0.012(3) C41 0.018(3) 0.028(3) 0.037(3) 0.015(2) 0.000(2) 0.003(2) C19 0.030(3) 0.028(3) 0.035(3) 0.003(2) 0.000(3) -0.004(2) C72 0.023(3) 0.051(4) 0.035(3) -0.002(3) -0.001(2) -0.009(3) C73 0.032(3) 0.058(4) 0.037(3) -0.011(3) -0.008(3) -0.004(3) C154 0.057(4) 0.042(3) 0.039(3) -0.005(3) -0.015(3) -0.016(3) C133 0.033(3) 0.108(6) 0.043(4) 0.003(4) 0.002(3) 0.018(4) C18 0.039(3) 0.042(3) 0.036(3) 0.001(3) 0.002(2) -0.001(3) C152 0.055(4) 0.027(3) 0.069(4) -0.013(3) -0.013(3) -0.001(3) C134 0.036(3) 0.044(4) 0.104(6) 0.012(4) -0.012(4) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O17 1.759(4) . ? Al1 C19 1.953(5) . ? Al1 C18 1.965(5) . ? Al1 N1 2.011(4) . ? O17 C16 1.348(6) . ? N7 C6 1.461(6) . ? N7 C8 1.463(6) . ? N7 C71 1.468(6) . ? N1 C9 1.492(6) . ? N1 C2 1.501(6) . ? N1 C10 1.502(5) . ? N4 C3 1.447(6) . ? N4 C5 1.458(6) . ? N4 C41 1.473(6) . ? C10 C11 1.495(6) . ? C3 C2 1.508(6) . ? C12 C13 1.371(6) . ? C12 C11 1.383(6) . ? C13 C14 1.390(6) . ? C13 C131 1.533(7) . ? C14 C15 1.386(7) . ? C15 C16 1.401(6) . ? C15 C151 1.543(7) . ? C5 C6 1.524(7) . ? C8 C9 1.509(6) . ? C71 C73 1.501(7) . ? C71 C72 1.518(7) . ? C11 C16 1.384(6) . ? C131 C133 1.502(7) . ? C131 C134 1.515(8) . ? C131 C132 1.533(7) . ? C151 C153 1.510(7) . ? C151 C152 1.515(7) . ? C151 C154 1.532(7) . ? C43 C41 1.511(7) . ? C42 C41 1.509(7) . ? 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 O17 Al1 C19 110.7(2) . . ? O17 Al1 C18 111.4(2) . . ? C19 Al1 C18 119.8(2) . . ? O17 Al1 N1 95.0(2) . . ? C19 Al1 N1 110.0(2) . . ? C18 Al1 N1 107.0(2) . . ? C16 O17 Al1 131.2(3) . . ? C6 N7 C8 113.2(4) . . ? C6 N7 C71 114.0(4) . . ? C8 N7 C71 112.7(4) . . ? C9 N1 C2 113.3(3) . . ? C9 N1 C10 110.9(3) . . ? C2 N1 C10 107.4(3) . . ? C9 N1 Al1 108.4(3) . . ? C2 N1 Al1 112.7(3) . . ? C10 N1 Al1 103.8(3) . . ? C3 N4 C5 114.0(4) . . ? C3 N4 C41 112.2(4) . . ? C5 N4 C41 114.7(4) . . ? C11 C10 N1 115.7(4) . . ? N4 C3 C2 115.4(4) . . ? C13 C12 C11 123.0(4) . . ? C12 C13 C14 115.6(4) . . ? C12 C13 C131 123.3(4) . . ? C14 C13 C131 121.1(4) . . ? C15 C14 C13 124.4(4) . . ? C14 C15 C16 117.5(4) . . ? C14 C15 C151 121.3(4) . . ? C16 C15 C151 121.2(4) . . ? N4 C5 C6 115.2(4) . . ? N7 C8 C9 114.3(4) . . ? N7 C71 C73 111.6(4) . . ? N7 C71 C72 114.3(4) . . ? C73 C71 C72 111.3(4) . . ? N1 C9 C8 117.8(4) . . ? C12 C11 C16 119.8(4) . . ? C12 C11 C10 118.1(4) . . ? C16 C11 C10 121.9(4) . . ? N1 C2 C3 116.6(4) . . ? N7 C6 C5 115.3(4) . . ? C133 C131 C134 111.2(5) . . ? C133 C131 C132 107.0(5) . . ? C134 C131 C132 106.7(5) . . ? C133 C131 C13 109.6(4) . . ? C134 C131 C13 110.7(4) . . ? C132 C131 C13 111.6(4) . . ? O17 C16 C11 120.3(4) . . ? O17 C16 C15 119.9(4) . . ? C11 C16 C15 119.7(4) . . ? C153 C151 C152 107.6(4) . . ? C153 C151 C154 108.9(4) . . ? C152 C151 C154 107.6(5) . . ? C153 C151 C15 111.6(4) . . ? C152 C151 C15 112.3(4) . . ? C154 C151 C15 108.8(4) . . ? N4 C41 C42 114.7(4) . . ? N4 C41 C43 110.7(4) . . ? C42 C41 C43 111.5(4) . . ? _refine_diff_density_max 0.302 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.056 #===end data_compound2 # Local code str28 _chemical_name_systematic ; [Al2(L-2)Me4] ; _audit_creation_method SHELXL _chemical_name_common ? _chemical_formula_moiety 'C34 H76 Al2 N6 O2' _chemical_formula_structural 'C34 H76 AL2 N6 O2' _chemical_formula_analytical ? _chemical_formula_sum 'C34 H76 Al2 N6 O2' _chemical_formula_weight 654.97 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.2690(5) _cell_length_b 13.4100(6) _cell_length_c 12.4290(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.998(2) _cell_angle_gamma 90.00 _cell_volume 2033.71(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.070 _exptl_crystal_density_method none _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.106 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Enraf-Nonius DIP2000 Image Plate Diffractometer' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4232 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.49 _reflns_number_total 4232 _reflns_number_observed 4128 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius DIP2000 Software - XPRESS' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses of fit S are based on F^2^, conventional R- factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+1.6410P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(28) _refine_ls_number_reflns 4231 _refine_ls_number_parameters 411 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_obs 0.0691 _refine_ls_wR_factor_all 0.1740 _refine_ls_wR_factor_obs 0.1677 _refine_ls_goodness_of_fit_all 1.298 _refine_ls_goodness_of_fit_obs 1.311 _refine_ls_restrained_S_all 1.342 _refine_ls_restrained_S_obs 1.310 _refine_ls_shift/esd_max 0.011 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al1 Al 0.71753(11) 0.95307(10) 0.74961(10) 0.0161(3) Uani 1 d . . Al2 Al 0.71583(10) 1.12201(10) 0.59199(10) 0.0158(3) Uani 1 d . . N1 N 0.8669(3) 0.8556(3) 0.7579(3) 0.0198(8) Uani 1 d . . C2 C 0.8583(4) 0.7551(4) 0.8075(4) 0.0227(10) Uani 1 d . . H2A H 0.9273(4) 0.7206(4) 0.8037(4) 0.027 Uiso 1 calc R . H2B H 0.8023(4) 0.7178(4) 0.7637(4) 0.027 Uiso 1 calc R . C3 C 0.8317(4) 0.7519(4) 0.9234(4) 0.0263(11) Uani 1 d . . H3A H 0.7659(4) 0.7908(4) 0.9290(4) 0.032 Uiso 1 calc R . H3B H 0.8155(4) 0.6834(4) 0.9414(4) 0.032 Uiso 1 calc R . N4 N 0.9176(3) 0.7888(3) 1.0025(3) 0.0242(9) Uani 1 d . . C41 C 0.8778(5) 0.8070(5) 1.1080(4) 0.0337(13) Uani 1 d . . H41 H 0.8098(5) 0.8454(5) 1.0938(4) 0.040 Uiso 1 calc R . C42 C 0.9573(6) 0.8726(6) 1.1770(5) 0.045(2) Uani 1 d . . H42A H 0.9249(17) 0.8929(31) 1.2406(21) 0.067 Uiso 1 calc R . H42B H 0.9741(33) 0.9305(19) 1.1364(15) 0.067 Uiso 1 calc R . H42C H 1.0234(17) 0.8361(13) 1.1979(34) 0.067 Uiso 1 calc R . C43 C 0.8487(6) 0.7132(6) 1.1688(5) 0.047(2) Uani 1 d . . H43A H 0.8188(39) 0.7319(6) 1.2343(21) 0.071 Uiso 1 calc R . H43B H 0.9134(9) 0.6738(19) 1.1862(36) 0.071 Uiso 1 calc R . H43C H 0.7955(31) 0.6749(20) 1.1241(17) 0.071 Uiso 1 calc R . C5 C 1.0193(4) 0.7309(4) 1.0065(4) 0.0281(11) Uani 1 d . . H5A H 1.0041(4) 0.6687(4) 0.9678(4) 0.034 Uiso 1 calc R . H5B H 1.0430(4) 0.7145(4) 1.0813(4) 0.034 Uiso 1 calc R . C6 C 1.1132(4) 0.7845(5) 0.9579(4) 0.0292(11) Uani 1 d . . H6A H 1.1169(4) 0.8525(5) 0.9845(4) 0.035 Uiso 1 calc R . H6B H 1.1815(4) 0.7519(5) 0.9839(4) 0.035 Uiso 1 calc R . N7 N 1.1039(3) 0.7868(3) 0.8390(3) 0.0254(9) Uani 1 d . . C71 C 1.1963(5) 0.7400(5) 0.7908(5) 0.0332(12) Uani 1 d . . H71 H 1.1812(5) 0.7485(5) 0.7124(5) 0.040 Uiso 1 calc R . C72 C 1.3065(5) 0.7889(7) 0.8229(6) 0.055(2) Uani 1 d . . H72A H 1.3609(11) 0.7594(31) 0.7826(35) 0.083 Uiso 1 calc R . H72B H 1.3270(23) 0.7792(38) 0.8988(12) 0.083 Uiso 1 calc R . H72C H 1.3015(14) 0.8590(10) 0.8075(44) 0.083 Uiso 1 calc R . C73 C 1.1972(6) 0.6289(6) 0.8115(5) 0.051(2) Uani 1 d . . H73A H 1.2173(40) 0.6165(6) 0.8871(9) 0.076 Uiso 1 calc R . H73B H 1.2493(30) 0.5975(8) 0.7700(32) 0.076 Uiso 1 calc R . H73C H 1.1256(12) 0.6020(9) 0.7907(38) 0.076 Uiso 1 calc R . C8 C 1.0750(4) 0.8842(4) 0.7939(4) 0.0266(11) Uani 1 d . . H8A H 1.0836(4) 0.8833(4) 0.7172(4) 0.032 Uiso 1 calc R . H8B H 1.1258(4) 0.9331(4) 0.8277(4) 0.032 Uiso 1 calc R . C9 C 0.9590(4) 0.9169(4) 0.8085(4) 0.0208(10) Uani 1 d . . H9A H 0.9525(4) 0.9200(4) 0.8856(4) 0.025 Uiso 1 calc R . H9B H 0.9494(4) 0.9842(4) 0.7806(4) 0.025 Uiso 1 calc R . C10 C 0.8754(4) 0.8398(4) 0.6417(4) 0.0213(10) Uani 1 d . . H10A H 0.8196(4) 0.7930(4) 0.6129(4) 0.026 Uiso 1 calc R . H10B H 0.9465(4) 0.8116(4) 0.6320(4) 0.026 Uiso 1 calc R . C11 C 0.8610(4) 0.9377(4) 0.5807(4) 0.0213(10) Uani 1 d . . H11 H 0.9286(4) 0.9768(4) 0.5932(4) 0.026 Uiso 1 calc R . C12 C 0.8362(5) 0.9175(5) 0.4610(4) 0.0326(12) Uani 1 d . . H12A H 0.8935(19) 0.8772(27) 0.4366(8) 0.049 Uiso 1 calc R . H12B H 0.8319(34) 0.9796(5) 0.4223(5) 0.049 Uiso 1 calc R . H12C H 0.7676(18) 0.8829(28) 0.4481(6) 0.049 Uiso 1 calc R . O13 O 0.7751(3) 0.9893(2) 0.6236(2) 0.0183(7) Uani 1 d . . C14 C 0.7527(4) 1.0093(4) 0.8961(4) 0.0231(10) Uani 1 d . . H14A H 0.7981(26) 0.9633(13) 0.9398(10) 0.035 Uiso 1 calc R . H14B H 0.6861(4) 1.0206(26) 0.9286(12) 0.035 Uiso 1 calc R . H14C H 0.7910(27) 1.0713(14) 0.8913(4) 0.035 Uiso 1 calc R . C15 C 0.6090(4) 0.8448(4) 0.7256(5) 0.0273(11) Uani 1 d . . H15A H 0.5396(9) 0.8721(5) 0.6971(30) 0.041 Uiso 1 calc R . H15B H 0.6013(24) 0.8118(19) 0.7930(7) 0.041 Uiso 1 calc R . H15C H 0.6332(16) 0.7977(16) 0.6751(25) 0.041 Uiso 1 calc R . N16 N 0.6268(3) 1.2606(3) 0.6395(3) 0.0190(8) Uani 1 d . . C17 C 0.5905(4) 1.3326(4) 0.5514(4) 0.0226(10) Uani 1 d . . H17A H 0.5460(4) 1.3834(4) 0.5812(4) 0.027 Uiso 1 calc R . H17B H 0.5438(4) 1.2972(4) 0.4963(4) 0.027 Uiso 1 calc R . C18 C 0.6797(4) 1.3839(4) 0.4975(4) 0.0241(10) Uani 1 d . . H18A H 0.7310(4) 1.3339(4) 0.4774(4) 0.029 Uiso 1 calc R . H18B H 0.6471(4) 1.4152(4) 0.4315(4) 0.029 Uiso 1 calc R . N19 N 0.7403(3) 1.4594(3) 0.5640(3) 0.0239(9) Uani 1 d . . C191 C 0.8379(4) 1.4948(4) 0.5177(4) 0.0254(10) Uani 1 d . . H191 H 0.8772(4) 1.4353(4) 0.4972(4) 0.030 Uiso 1 calc R . C192 C 0.9137(4) 1.5484(5) 0.6019(5) 0.0315(12) Uani 1 d . . H19A H 0.9810(14) 1.5638(29) 0.5726(12) 0.047 Uiso 1 calc R . H19B H 0.9286(28) 1.5064(13) 0.6643(14) 0.047 Uiso 1 calc R . H19C H 0.8796(15) 1.6090(16) 0.6223(26) 0.047 Uiso 1 calc R . C193 C 0.8155(5) 1.5577(5) 0.4153(5) 0.0336(13) Uani 1 d . . H19D H 0.8836(5) 1.5741(28) 0.3880(20) 0.050 Uiso 1 calc R . H19E H 0.7785(32) 1.6180(15) 0.4320(8) 0.050 Uiso 1 calc R . H19F H 0.7702(30) 1.5207(13) 0.3617(13) 0.050 Uiso 1 calc R . C20 C 0.6706(4) 1.5382(4) 0.6011(5) 0.0285(11) Uani 1 d . . H20A H 0.5988(4) 1.5334(4) 0.5606(5) 0.034 Uiso 1 calc R . H20B H 0.7014(4) 1.6023(4) 0.5842(5) 0.034 Uiso 1 calc R . C21 C 0.6563(4) 1.5360(4) 0.7215(4) 0.0289(11) Uani 1 d . . H21A H 0.7279(4) 1.5266(4) 0.7613(4) 0.035 Uiso 1 calc R . H21B H 0.6296(4) 1.6008(4) 0.7416(4) 0.035 Uiso 1 calc R . N22 N 0.5826(3) 1.4598(3) 0.7569(3) 0.0233(8) Uani 1 d . . C221 C 0.5006(5) 1.5032(4) 0.8230(4) 0.0293(11) Uani 1 d . . H221 H 0.4699(5) 1.5619(4) 0.7839(4) 0.035 Uiso 1 calc R . C222 C 0.4064(5) 1.4315(5) 0.8318(5) 0.0379(14) Uani 1 d . . H22A H 0.3508(18) 1.4636(12) 0.8683(34) 0.057 Uiso 1 calc R . H22B H 0.4326(9) 1.3736(16) 0.8719(33) 0.057 Uiso 1 calc R . H22C H 0.3760(25) 1.4118(27) 0.7606(5) 0.057 Uiso 1 calc R . C223 C 0.5484(6) 1.5390(5) 0.9337(5) 0.046(2) Uani 1 d . . H22D H 0.4924(12) 1.5717(34) 0.9692(18) 0.068 Uiso 1 calc R . H22E H 0.6070(29) 1.5850(30) 0.9258(6) 0.068 Uiso 1 calc R . H22F H 0.5761(38) 1.4830(7) 0.9763(15) 0.068 Uiso 1 calc R . C23 C 0.6403(4) 1.3749(4) 0.8078(4) 0.0255(10) Uani 1 d . . H23A H 0.5888(4) 1.3353(4) 0.8439(4) 0.031 Uiso 1 calc R . H23B H 0.6959(4) 1.3991(4) 0.8627(4) 0.031 Uiso 1 calc R . C24 C 0.6950(4) 1.3077(3) 0.7306(4) 0.0189(9) Uani 1 d . . H24A H 0.7510(4) 1.3466(3) 0.7004(4) 0.023 Uiso 1 calc R . H24B H 0.7321(4) 1.2547(3) 0.7731(4) 0.023 Uiso 1 calc R . C25 C 0.5279(4) 1.2144(4) 0.6739(4) 0.0201(10) Uani 1 d . . H25A H 0.4815(4) 1.1907(4) 0.6111(4) 0.024 Uiso 1 calc R . H25B H 0.4869(4) 1.2633(4) 0.7108(4) 0.024 Uiso 1 calc R . C26 C 0.5594(4) 1.1280(4) 0.7492(3) 0.0198(9) Uani 1 d . . H26 H 0.5930(4) 1.1540(4) 0.8186(3) 0.024 Uiso 1 calc R . C27 C 0.4611(4) 1.0653(4) 0.7683(5) 0.0297(11) Uani 1 d . . H27A H 0.4094(16) 1.1053(9) 0.8020(30) 0.044 Uiso 1 calc R . H27B H 0.4841(6) 1.0103(18) 0.8147(27) 0.044 Uiso 1 calc R . H27C H 0.4274(20) 1.0404(26) 0.7004(6) 0.044 Uiso 1 calc R . O28 O 0.6384(3) 1.0719(2) 0.6995(3) 0.0179(7) Uani 1 d . . C29 C 0.6394(4) 1.1074(4) 0.4457(4) 0.0253(11) Uani 1 d . . H29A H 0.6275(28) 1.0380(4) 0.4299(12) 0.038 Uiso 1 calc R . H29B H 0.6833(15) 1.1360(26) 0.3940(5) 0.038 Uiso 1 calc R . H29C H 0.5702(15) 1.1412(25) 0.4419(10) 0.038 Uiso 1 calc R . C30 C 0.8624(4) 1.1859(4) 0.6065(5) 0.0252(11) Uani 1 d . . H30A H 0.8542(4) 1.2567(5) 0.5972(31) 0.038 Uiso 1 calc R . H30B H 0.9050(12) 1.1598(21) 0.5524(20) 0.038 Uiso 1 calc R . H30C H 0.8990(13) 1.1722(24) 0.6771(12) 0.038 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0199(6) 0.0144(6) 0.0138(6) 0.0006(5) 0.0011(5) -0.0012(6) Al2 0.0160(6) 0.0166(6) 0.0147(6) 0.0018(5) 0.0005(5) -0.0022(5) N1 0.026(2) 0.015(2) 0.019(2) 0.000(2) 0.003(2) 0.002(2) C2 0.028(2) 0.018(2) 0.021(2) -0.002(2) 0.000(2) -0.003(2) C3 0.028(2) 0.021(3) 0.031(3) 0.009(2) 0.007(2) -0.001(2) N4 0.024(2) 0.027(2) 0.022(2) 0.002(2) 0.005(2) 0.003(2) C41 0.035(3) 0.045(3) 0.023(2) 0.008(2) 0.012(2) 0.014(3) C42 0.055(4) 0.055(4) 0.025(3) -0.007(3) 0.007(3) 0.013(3) C43 0.047(4) 0.063(5) 0.035(3) 0.018(3) 0.018(3) 0.008(3) C5 0.034(3) 0.033(3) 0.017(2) 0.006(2) 0.004(2) 0.005(2) C6 0.026(2) 0.037(3) 0.025(2) 0.001(2) 0.000(2) 0.012(2) N7 0.023(2) 0.029(2) 0.025(2) 0.004(2) 0.003(2) 0.005(2) C71 0.031(3) 0.039(3) 0.031(3) 0.006(2) 0.008(2) 0.009(2) C72 0.028(3) 0.075(5) 0.065(4) 0.006(4) 0.014(3) 0.009(3) C73 0.064(4) 0.051(4) 0.041(3) 0.011(3) 0.022(3) 0.028(4) C8 0.019(2) 0.032(3) 0.029(3) -0.001(2) 0.002(2) -0.002(2) C9 0.021(2) 0.020(2) 0.021(2) 0.003(2) -0.001(2) 0.003(2) C10 0.024(2) 0.018(2) 0.022(2) -0.005(2) 0.002(2) 0.004(2) C11 0.024(2) 0.022(3) 0.019(2) 0.000(2) 0.008(2) 0.003(2) C12 0.042(3) 0.033(3) 0.024(3) 0.000(2) 0.008(2) 0.013(2) O13 0.026(2) 0.014(2) 0.0155(15) 0.0024(12) 0.0049(13) 0.0028(13) C14 0.029(2) 0.022(3) 0.017(2) -0.004(2) -0.003(2) 0.007(2) C15 0.022(2) 0.021(3) 0.039(3) 0.003(2) -0.001(2) -0.004(2) N16 0.016(2) 0.019(2) 0.022(2) 0.003(2) -0.0001(15) -0.002(2) C17 0.025(2) 0.019(2) 0.022(2) 0.000(2) -0.005(2) 0.002(2) C18 0.029(2) 0.022(2) 0.020(2) 0.002(2) 0.000(2) 0.006(2) N19 0.025(2) 0.020(2) 0.027(2) 0.002(2) 0.006(2) 0.007(2) C191 0.027(2) 0.020(2) 0.030(3) 0.003(2) 0.008(2) 0.003(2) C192 0.025(2) 0.035(3) 0.036(3) -0.001(2) 0.007(2) -0.002(2) C193 0.029(3) 0.041(3) 0.033(3) 0.009(2) 0.012(2) 0.003(2) C20 0.031(3) 0.018(3) 0.039(3) 0.002(2) 0.013(2) 0.003(2) C21 0.033(3) 0.019(3) 0.036(3) -0.003(2) 0.012(2) 0.002(2) N22 0.026(2) 0.018(2) 0.027(2) 0.000(2) 0.007(2) 0.001(2) C221 0.036(3) 0.024(3) 0.030(3) -0.001(2) 0.010(2) 0.010(2) C222 0.032(3) 0.035(3) 0.049(3) 0.007(3) 0.018(3) 0.009(2) C223 0.056(4) 0.044(4) 0.040(3) -0.007(3) 0.021(3) 0.009(3) C23 0.027(2) 0.024(3) 0.025(2) -0.003(2) 0.000(2) 0.000(2) C24 0.018(2) 0.015(2) 0.023(2) 0.008(2) -0.001(2) 0.008(2) C25 0.018(2) 0.020(2) 0.021(2) -0.004(2) 0.000(2) 0.002(2) C26 0.020(2) 0.022(2) 0.016(2) -0.002(2) 0.000(2) -0.003(2) C27 0.027(2) 0.030(3) 0.033(3) -0.002(2) 0.011(2) 0.000(2) O28 0.019(2) 0.017(2) 0.018(2) 0.0068(13) 0.0054(13) 0.0036(13) C29 0.031(2) 0.029(3) 0.015(2) -0.001(2) -0.001(2) -0.001(2) C30 0.014(2) 0.025(3) 0.037(3) -0.004(2) 0.003(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O13 1.849(3) . ? Al1 O28 1.935(3) . ? Al1 C15 1.972(5) . ? Al1 C14 1.977(5) . ? Al1 N1 2.245(4) . ? Al1 Al2 2.994(2) . ? Al2 O28 1.845(3) . ? Al2 O13 1.946(3) . ? Al2 C29 1.966(5) . ? Al2 C30 1.983(5) . ? Al2 N16 2.265(4) . ? N1 C10 1.474(6) . ? N1 C9 1.484(6) . ? N1 C2 1.490(6) . ? C2 C3 1.510(7) . ? C3 N4 1.452(7) . ? N4 C5 1.466(7) . ? N4 C41 1.467(7) . ? C41 C42 1.512(9) . ? C41 C43 1.530(9) . ? C5 C6 1.534(8) . ? C6 N7 1.471(6) . ? N7 C8 1.451(7) . ? N7 C71 1.477(7) . ? C71 C73 1.512(10) . ? C71 C72 1.519(9) . ? C8 C9 1.518(7) . ? C10 C11 1.517(7) . ? C11 O13 1.412(5) . ? C11 C12 1.512(7) . ? N16 C25 1.466(6) . ? N16 C24 1.477(6) . ? N16 C17 1.492(6) . ? C17 C18 1.508(7) . ? C18 N19 1.461(7) . ? N19 C191 1.460(6) . ? N19 C20 1.464(6) . ? C191 C192 1.507(8) . ? C191 C193 1.528(7) . ? C20 C21 1.525(7) . ? C21 N22 1.463(7) . ? N22 C23 1.451(7) . ? N22 C221 1.482(6) . ? C221 C223 1.516(9) . ? C221 C222 1.517(8) . ? C23 C24 1.522(7) . ? C25 C26 1.513(7) . ? C26 O28 1.419(6) . ? C26 C27 1.509(7) . ? 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 O13 Al1 O28 74.56(14) . . ? O13 Al1 C15 112.2(2) . . ? O28 Al1 C15 104.5(2) . . ? O13 Al1 C14 127.9(2) . . ? O28 Al1 C14 92.1(2) . . ? C15 Al1 C14 120.0(2) . . ? O13 Al1 N1 79.05(15) . . ? O28 Al1 N1 151.0(2) . . ? C15 Al1 N1 96.5(2) . . ? C14 Al1 N1 94.7(2) . . ? O13 Al1 Al2 39.09(11) . . ? O28 Al1 Al2 36.59(10) . . ? C15 Al1 Al2 120.0(2) . . ? C14 Al1 Al2 107.5(2) . . ? N1 Al1 Al2 114.88(11) . . ? O28 Al2 O13 74.36(14) . . ? O28 Al2 C29 113.7(2) . . ? O13 Al2 C29 103.2(2) . . ? O28 Al2 C30 128.4(2) . . ? O13 Al2 C30 93.5(2) . . ? C29 Al2 C30 117.9(2) . . ? O28 Al2 N16 79.12(15) . . ? O13 Al2 N16 151.33(15) . . ? C29 Al2 N16 97.2(2) . . ? C30 Al2 N16 94.5(2) . . ? O28 Al2 Al1 38.68(10) . . ? O13 Al2 Al1 36.79(10) . . ? C29 Al2 Al1 120.0(2) . . ? C30 Al2 Al1 108.8(2) . . ? N16 Al2 Al1 114.89(11) . . ? C10 N1 C9 111.5(4) . . ? C10 N1 C2 106.9(4) . . ? C9 N1 C2 114.2(4) . . ? C10 N1 Al1 100.3(3) . . ? C9 N1 Al1 106.2(3) . . ? C2 N1 Al1 116.9(3) . . ? N1 C2 C3 116.9(4) . . ? N4 C3 C2 115.0(4) . . ? C3 N4 C5 113.4(4) . . ? C3 N4 C41 112.1(4) . . ? C5 N4 C41 114.8(4) . . ? N4 C41 C42 110.4(5) . . ? N4 C41 C43 114.9(5) . . ? C42 C41 C43 111.6(5) . . ? N4 C5 C6 114.2(4) . . ? N7 C6 C5 115.0(4) . . ? C8 N7 C6 113.5(4) . . ? C8 N7 C71 113.2(4) . . ? C6 N7 C71 114.6(4) . . ? N7 C71 C73 110.0(5) . . ? N7 C71 C72 114.2(5) . . ? C73 C71 C72 113.0(6) . . ? N7 C8 C9 114.0(4) . . ? N1 C9 C8 118.1(4) . . ? N1 C10 C11 110.4(4) . . ? O13 C11 C12 112.2(4) . . ? O13 C11 C10 106.8(4) . . ? C12 C11 C10 109.8(4) . . ? C11 O13 Al1 123.9(3) . . ? C11 O13 Al2 130.6(3) . . ? Al1 O13 Al2 104.1(2) . . ? C25 N16 C24 112.1(4) . . ? C25 N16 C17 107.2(4) . . ? C24 N16 C17 112.8(4) . . ? C25 N16 Al2 99.5(3) . . ? C24 N16 Al2 107.5(3) . . ? C17 N16 Al2 117.0(3) . . ? N16 C17 C18 116.5(4) . . ? N19 C18 C17 114.6(4) . . ? C191 N19 C18 113.1(4) . . ? C191 N19 C20 114.8(4) . . ? C18 N19 C20 113.5(4) . . ? N19 C191 C192 110.7(4) . . ? N19 C191 C193 115.1(4) . . ? C192 C191 C193 111.1(5) . . ? N19 C20 C21 115.2(4) . . ? N22 C21 C20 116.5(4) . . ? C23 N22 C21 113.0(4) . . ? C23 N22 C221 113.2(4) . . ? C21 N22 C221 111.7(4) . . ? N22 C221 C223 114.0(5) . . ? N22 C221 C222 110.9(5) . . ? C223 C221 C222 111.2(5) . . ? N22 C23 C24 114.6(4) . . ? N16 C24 C23 119.0(4) . . ? N16 C25 C26 109.8(4) . . ? O28 C26 C27 111.5(4) . . ? O28 C26 C25 106.2(3) . . ? C27 C26 C25 111.5(4) . . ? C26 O28 Al2 123.3(3) . . ? C26 O28 Al1 129.7(3) . . ? Al2 O28 Al1 104.7(2) . . ? _refine_diff_density_max 0.462 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.068 #=== end