# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Aluminum complexes of the redox-active [ONO] pincer ligand ; _publ_contact_author_name 'Alan Heyduk' _publ_contact_author_email aheyduk@uci.edu loop_ _publ_author_name A.Heyduk G.Szigethy data_afh265-1b _database_code_depnum_ccdc_archive 'CCDC 867891' #TrackingRef '- Al(ONO) combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (ONO)HAlBr.THF _chemical_melting_point 'not measured' _chemical_formula_moiety 'C32 H49 Al Br N O3' _chemical_formula_sum 'C32 H49 Al Br N O3' _chemical_formula_weight 602.61 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1640(6) _cell_length_b 11.6148(6) _cell_length_c 25.4263(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.3700(10) _cell_angle_gamma 90.00 _cell_volume 3276.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 9614 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.77 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.312 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5208 _exptl_absorpt_correction_T_max 0.8756 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38254 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.87 _reflns_number_total 7785 _reflns_number_gt 7071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. All non-hydrogen atoms are refined anisotropically. Hyrogen atoms, though visible in the Fourier map, were generated in calculated positions and refined using the riding model. Data were cut at 0.76 Angstroms because below that resolution completeness dropped below 76%. ; _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^)+(0.0332P)^2^+1.2206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7785 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0629 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.60554(3) 0.58973(3) 0.736997(13) 0.01268(7) Uani 1 1 d . . . Br1 Br 0.520193(11) 0.408323(10) 0.747511(5) 0.01859(4) Uani 1 1 d . . . O2 O 0.65633(7) 0.66709(7) 0.79493(3) 0.01480(16) Uani 1 1 d . . . O1 O 0.60422(7) 0.65399(7) 0.67415(3) 0.01495(16) Uani 1 1 d . . . O3 O 0.76453(7) 0.53132(7) 0.73250(3) 0.01544(17) Uani 1 1 d . . . N1 N 0.44168(9) 0.67934(8) 0.74108(4) 0.01259(18) Uani 1 1 d . . . H1 H 0.3793 0.6268 0.7427 0.015 Uiso 1 1 calc R . . C15 C 0.46011(10) 0.74448(9) 0.79084(4) 0.0125(2) Uani 1 1 d . . . C16 C 0.57542(10) 0.73112(10) 0.81790(4) 0.0134(2) Uani 1 1 d . . . C17 C 0.60218(10) 0.78139(10) 0.86820(4) 0.0134(2) Uani 1 1 d . . . C18 C 0.50957(11) 0.84280(10) 0.88830(5) 0.0150(2) Uani 1 1 d . . . H18A H 0.5266 0.8781 0.9220 0.018 Uiso 1 1 calc R . . C19 C 0.39384(11) 0.85558(10) 0.86205(4) 0.0144(2) Uani 1 1 d . . . C20 C 0.36994(10) 0.80451(10) 0.81222(4) 0.0136(2) Uani 1 1 d . . . H20A H 0.2921 0.8110 0.7931 0.016 Uiso 1 1 calc R . . C21 C 0.72557(11) 0.76508(10) 0.90026(5) 0.0160(2) Uani 1 1 d . . . C24 C 0.74716(12) 0.63548(11) 0.91040(5) 0.0203(2) Uani 1 1 d . . . H24A H 0.6833 0.6046 0.9298 0.030 Uiso 1 1 calc R . . H24B H 0.8255 0.6243 0.9313 0.030 Uiso 1 1 calc R . . H24C H 0.7465 0.5952 0.8765 0.030 Uiso 1 1 calc R . . C23 C 0.73281(12) 0.82584(12) 0.95414(5) 0.0218(3) Uani 1 1 d . . . H23A H 0.7193 0.9086 0.9487 0.033 Uiso 1 1 calc R . . H23B H 0.8127 0.8133 0.9734 0.033 Uiso 1 1 calc R . . H23C H 0.6710 0.7945 0.9746 0.033 Uiso 1 1 calc R . . C22 C 0.82499(11) 0.81515(12) 0.86978(5) 0.0215(3) Uani 1 1 d . . . H22A H 0.8103 0.8975 0.8636 0.032 Uiso 1 1 calc R . . H22B H 0.8245 0.7754 0.8358 0.032 Uiso 1 1 calc R . . H22C H 0.9035 0.8045 0.8906 0.032 Uiso 1 1 calc R . . C25 C 0.29446(11) 0.92097(10) 0.88657(5) 0.0172(2) Uani 1 1 d . . . C26 C 0.33681(13) 0.96665(14) 0.94220(5) 0.0286(3) Uani 1 1 d . . . H26A H 0.4059 1.0180 0.9405 0.043 Uiso 1 1 calc R . . H26B H 0.3605 0.9019 0.9658 0.043 Uiso 1 1 calc R . . H26C H 0.2710 1.0092 0.9558 0.043 Uiso 1 1 calc R . . C27 C 0.25412(13) 1.02421(12) 0.85149(6) 0.0260(3) Uani 1 1 d . . . H27A H 0.3230 1.0754 0.8488 0.039 Uiso 1 1 calc R . . H27B H 0.1907 1.0663 0.8671 0.039 Uiso 1 1 calc R . . H27C H 0.2228 0.9970 0.8161 0.039 Uiso 1 1 calc R . . C28 C 0.18633(12) 0.84100(12) 0.89076(6) 0.0255(3) Uani 1 1 d . . . H28A H 0.1577 0.8107 0.8556 0.038 Uiso 1 1 calc R . . H28B H 0.1214 0.8843 0.9047 0.038 Uiso 1 1 calc R . . H28C H 0.2109 0.7770 0.9146 0.038 Uiso 1 1 calc R . . C1 C 0.42251(10) 0.74377(10) 0.69114(4) 0.0127(2) Uani 1 1 d . . . C2 C 0.51179(10) 0.72465(10) 0.65738(4) 0.0129(2) Uani 1 1 d . . . C3 C 0.49973(10) 0.77689(10) 0.60695(4) 0.0136(2) Uani 1 1 d . . . C4 C 0.39613(10) 0.84298(10) 0.59322(4) 0.0147(2) Uani 1 1 d . . . H4A H 0.3871 0.8787 0.5594 0.018 Uiso 1 1 calc R . . C5 C 0.30522(10) 0.85975(10) 0.62600(4) 0.0142(2) Uani 1 1 d . . . C6 C 0.32064(10) 0.80875(10) 0.67610(4) 0.0137(2) Uani 1 1 d . . . H6A H 0.2613 0.8187 0.6998 0.016 Uiso 1 1 calc R . . C7 C 0.59448(11) 0.75764(10) 0.56841(5) 0.0153(2) Uani 1 1 d . . . C10 C 0.59690(13) 0.62899(11) 0.55388(5) 0.0222(3) Uani 1 1 d . . . H10A H 0.5167 0.6052 0.5380 0.033 Uiso 1 1 calc R . . H10B H 0.6199 0.5836 0.5859 0.033 Uiso 1 1 calc R . . H10C H 0.6556 0.6164 0.5285 0.033 Uiso 1 1 calc R . . C9 C 0.56600(12) 0.82622(11) 0.51692(5) 0.0204(2) Uani 1 1 d . . . H9A H 0.5639 0.9086 0.5251 0.031 Uiso 1 1 calc R . . H9B H 0.4875 0.8023 0.4993 0.031 Uiso 1 1 calc R . . H9C H 0.6284 0.8116 0.4935 0.031 Uiso 1 1 calc R . . C8 C 0.71958(11) 0.79693(12) 0.59343(5) 0.0219(3) Uani 1 1 d . . . H8A H 0.7167 0.8788 0.6025 0.033 Uiso 1 1 calc R . . H8B H 0.7787 0.7849 0.5682 0.033 Uiso 1 1 calc R . . H8C H 0.7430 0.7521 0.6256 0.033 Uiso 1 1 calc R . . C11 C 0.19037(11) 0.92912(11) 0.60888(5) 0.0173(2) Uani 1 1 d . . . C14 C 0.18029(12) 1.02864(11) 0.64781(5) 0.0228(3) Uani 1 1 d . . . H14A H 0.2509 1.0789 0.6479 0.034 Uiso 1 1 calc R . . H14B H 0.1766 0.9976 0.6834 0.034 Uiso 1 1 calc R . . H14C H 0.1070 1.0730 0.6370 0.034 Uiso 1 1 calc R . . C13 C 0.07978(12) 0.85023(12) 0.60869(6) 0.0255(3) Uani 1 1 d . . . H13A H 0.0065 0.8945 0.5978 0.038 Uiso 1 1 calc R . . H13B H 0.0759 0.8193 0.6443 0.038 Uiso 1 1 calc R . . H13C H 0.0864 0.7866 0.5839 0.038 Uiso 1 1 calc R . . C12 C 0.19070(13) 0.98063(13) 0.55343(5) 0.0289(3) Uani 1 1 d . . . H12A H 0.2607 1.0313 0.5528 0.043 Uiso 1 1 calc R . . H12B H 0.1167 1.0251 0.5444 0.043 Uiso 1 1 calc R . . H12C H 0.1949 0.9185 0.5276 0.043 Uiso 1 1 calc R . . C29 C 0.85440(11) 0.60280(11) 0.70924(5) 0.0205(3) Uani 1 1 d . . . H29A H 0.8389 0.6856 0.7147 0.025 Uiso 1 1 calc R . . H29B H 0.8521 0.5879 0.6708 0.025 Uiso 1 1 calc R . . C30 C 0.97524(12) 0.56772(12) 0.73804(6) 0.0242(3) Uani 1 1 d . . . H30A H 1.0319 0.6336 0.7417 0.029 Uiso 1 1 calc R . . H30B H 1.0119 0.5041 0.7194 0.029 Uiso 1 1 calc R . . C31 C 0.94170(12) 0.52851(12) 0.79204(5) 0.0238(3) Uani 1 1 d . . . H31A H 1.0045 0.4778 0.8102 0.029 Uiso 1 1 calc R . . H31B H 0.9287 0.5950 0.8151 0.029 Uiso 1 1 calc R . . C32 C 0.82614(11) 0.46369(11) 0.77669(5) 0.0197(2) Uani 1 1 d . . . H32A H 0.8428 0.3844 0.7652 0.024 Uiso 1 1 calc R . . H32B H 0.7767 0.4599 0.8067 0.024 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.01501(17) 0.01232(16) 0.01081(16) -0.00019(12) 0.00185(12) 0.00151(12) Br1 0.02186(7) 0.01250(6) 0.02222(7) 0.00085(4) 0.00606(5) -0.00019(4) O2 0.0146(4) 0.0163(4) 0.0134(4) -0.0026(3) 0.0016(3) 0.0030(3) O1 0.0151(4) 0.0165(4) 0.0133(4) 0.0018(3) 0.0025(3) 0.0033(3) O3 0.0164(4) 0.0157(4) 0.0143(4) 0.0021(3) 0.0022(3) 0.0032(3) N1 0.0147(4) 0.0122(4) 0.0108(4) -0.0002(3) 0.0011(3) -0.0013(4) C15 0.0167(5) 0.0110(5) 0.0100(5) 0.0003(4) 0.0022(4) -0.0015(4) C16 0.0161(5) 0.0114(5) 0.0133(5) 0.0008(4) 0.0041(4) 0.0003(4) C17 0.0151(5) 0.0121(5) 0.0130(5) 0.0010(4) 0.0014(4) -0.0003(4) C18 0.0193(6) 0.0139(5) 0.0118(5) -0.0007(4) 0.0024(4) 0.0000(4) C19 0.0176(5) 0.0123(5) 0.0138(5) 0.0016(4) 0.0047(4) 0.0020(4) C20 0.0141(5) 0.0135(5) 0.0131(5) 0.0027(4) 0.0015(4) 0.0004(4) C21 0.0162(5) 0.0174(6) 0.0138(5) -0.0025(4) -0.0007(4) 0.0016(4) C24 0.0240(6) 0.0195(6) 0.0163(6) -0.0003(5) -0.0023(5) 0.0049(5) C23 0.0207(6) 0.0259(6) 0.0177(6) -0.0064(5) -0.0028(5) 0.0031(5) C22 0.0170(6) 0.0239(6) 0.0235(6) -0.0031(5) 0.0019(5) -0.0024(5) C25 0.0182(6) 0.0184(6) 0.0156(6) -0.0013(4) 0.0044(4) 0.0046(4) C26 0.0273(7) 0.0378(8) 0.0207(6) -0.0104(6) 0.0031(5) 0.0107(6) C27 0.0284(7) 0.0216(6) 0.0288(7) 0.0032(5) 0.0064(5) 0.0101(5) C28 0.0234(6) 0.0277(7) 0.0274(7) -0.0006(5) 0.0121(5) 0.0019(5) C1 0.0159(5) 0.0122(5) 0.0099(5) -0.0001(4) 0.0011(4) -0.0019(4) C2 0.0136(5) 0.0118(5) 0.0130(5) -0.0011(4) -0.0001(4) -0.0003(4) C3 0.0151(5) 0.0132(5) 0.0127(5) -0.0009(4) 0.0031(4) -0.0011(4) C4 0.0181(5) 0.0138(5) 0.0121(5) 0.0004(4) 0.0010(4) 0.0003(4) C5 0.0152(5) 0.0127(5) 0.0141(5) -0.0019(4) -0.0005(4) 0.0009(4) C6 0.0153(5) 0.0130(5) 0.0129(5) -0.0024(4) 0.0023(4) -0.0006(4) C7 0.0165(5) 0.0171(6) 0.0129(5) 0.0011(4) 0.0038(4) 0.0019(4) C10 0.0301(7) 0.0192(6) 0.0186(6) -0.0017(5) 0.0087(5) 0.0040(5) C9 0.0228(6) 0.0240(6) 0.0152(6) 0.0039(5) 0.0062(5) 0.0032(5) C8 0.0178(6) 0.0287(7) 0.0196(6) 0.0031(5) 0.0043(5) -0.0012(5) C11 0.0181(6) 0.0186(6) 0.0152(5) 0.0007(4) 0.0021(4) 0.0050(5) C14 0.0264(7) 0.0193(6) 0.0231(6) -0.0011(5) 0.0051(5) 0.0063(5) C13 0.0173(6) 0.0282(7) 0.0296(7) -0.0014(6) -0.0028(5) 0.0024(5) C12 0.0301(7) 0.0375(8) 0.0196(6) 0.0089(6) 0.0047(5) 0.0172(6) C29 0.0176(6) 0.0208(6) 0.0237(6) 0.0031(5) 0.0046(5) 0.0004(5) C30 0.0173(6) 0.0205(6) 0.0348(7) 0.0000(5) 0.0038(5) 0.0042(5) C31 0.0223(6) 0.0225(6) 0.0253(7) -0.0021(5) -0.0038(5) 0.0074(5) C32 0.0224(6) 0.0185(6) 0.0178(6) 0.0035(5) 0.0008(5) 0.0078(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7624(9) . ? Al1 O2 1.7644(9) . ? Al1 O3 1.9154(9) . ? Al1 N1 2.1172(10) . ? Al1 Br1 2.3399(4) . ? O2 C16 1.3517(14) . ? O1 C2 1.3500(14) . ? O3 C29 1.4756(15) . ? O3 C32 1.4770(14) . ? N1 C1 1.4689(14) . ? N1 C15 1.4688(14) . ? N1 H1 0.9300 . ? C15 C20 1.3844(16) . ? C15 C16 1.3994(16) . ? C16 C17 1.4075(15) . ? C17 C18 1.3986(16) . ? C17 C21 1.5325(16) . ? C18 C19 1.3948(16) . ? C18 H18A 0.9500 . ? C19 C20 1.3976(16) . ? C19 C25 1.5330(16) . ? C20 H20A 0.9500 . ? C21 C23 1.5352(16) . ? C21 C22 1.5367(17) . ? C21 C24 1.5416(17) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C25 C27 1.5320(17) . ? C25 C26 1.5353(17) . ? C25 C28 1.5363(18) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C1 C6 1.3831(16) . ? C1 C2 1.4033(16) . ? C2 C3 1.4114(15) . ? C3 C4 1.3997(16) . ? C3 C7 1.5362(15) . ? C4 C5 1.3966(16) . ? C4 H4A 0.9500 . ? C5 C6 1.3980(16) . ? C5 C11 1.5358(16) . ? C6 H6A 0.9500 . ? C7 C9 1.5352(16) . ? C7 C8 1.5383(17) . ? C7 C10 1.5401(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.5318(17) . ? C11 C14 1.5342(17) . ? C11 C13 1.5371(18) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C29 C30 1.5176(18) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.532(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.5073(18) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? 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 O1 Al1 O2 120.72(4) . . ? O1 Al1 O3 90.60(4) . . ? O2 Al1 O3 90.92(4) . . ? O1 Al1 N1 85.18(4) . . ? O2 Al1 N1 84.73(4) . . ? O3 Al1 N1 171.29(4) . . ? O1 Al1 Br1 121.49(3) . . ? O2 Al1 Br1 117.41(3) . . ? O3 Al1 Br1 94.57(3) . . ? N1 Al1 Br1 94.13(3) . . ? C16 O2 Al1 118.21(7) . . ? C2 O1 Al1 118.23(7) . . ? C29 O3 C32 108.91(9) . . ? C29 O3 Al1 120.03(7) . . ? C32 O3 Al1 119.96(7) . . ? C1 N1 C15 118.37(9) . . ? C1 N1 Al1 104.59(7) . . ? C15 N1 Al1 104.85(7) . . ? C1 N1 H1 109.5 . . ? C15 N1 H1 109.5 . . ? Al1 N1 H1 109.5 . . ? C20 C15 C16 122.15(10) . . ? C20 C15 N1 124.00(10) . . ? C16 C15 N1 113.56(10) . . ? O2 C16 C15 118.09(10) . . ? O2 C16 C17 122.43(10) . . ? C15 C16 C17 119.45(10) . . ? C18 C17 C16 116.91(10) . . ? C18 C17 C21 121.74(10) . . ? C16 C17 C21 121.31(10) . . ? C19 C18 C17 124.23(11) . . ? C19 C18 H18A 117.9 . . ? C17 C18 H18A 117.9 . . ? C18 C19 C20 117.53(10) . . ? C18 C19 C25 122.13(10) . . ? C20 C19 C25 120.33(10) . . ? C15 C20 C19 119.72(11) . . ? C15 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C17 C21 C23 111.90(10) . . ? C17 C21 C22 109.99(10) . . ? C23 C21 C22 107.86(10) . . ? C17 C21 C24 108.92(10) . . ? C23 C21 C24 107.92(10) . . ? C22 C21 C24 110.22(10) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C27 C25 C19 109.29(10) . . ? C27 C25 C26 107.85(11) . . ? C19 C25 C26 112.53(10) . . ? C27 C25 C28 109.34(11) . . ? C19 C25 C28 109.78(10) . . ? C26 C25 C28 108.00(11) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C6 C1 C2 122.36(10) . . ? C6 C1 N1 123.61(10) . . ? C2 C1 N1 113.76(10) . . ? O1 C2 C1 118.23(10) . . ? O1 C2 C3 122.73(10) . . ? C1 C2 C3 119.01(10) . . ? C4 C3 C2 117.09(10) . . ? C4 C3 C7 121.94(10) . . ? C2 C3 C7 120.93(10) . . ? C5 C4 C3 124.24(11) . . ? C5 C4 H4A 117.9 . . ? C3 C4 H4A 117.9 . . ? C4 C5 C6 117.42(10) . . ? C4 C5 C11 122.89(10) . . ? C6 C5 C11 119.68(10) . . ? C1 C6 C5 119.84(11) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C9 C7 C3 112.11(10) . . ? C9 C7 C8 106.94(10) . . ? C3 C7 C8 110.53(10) . . ? C9 C7 C10 107.84(10) . . ? C3 C7 C10 109.02(10) . . ? C8 C7 C10 110.35(10) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 . . ? C12 C11 C14 107.90(11) . . ? C12 C11 C5 112.25(10) . . ? C14 C11 C5 109.33(10) . . ? C12 C11 C13 108.30(11) . . ? C14 C11 C13 109.55(11) . . ? C5 C11 C13 109.46(10) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? 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 . . ? O3 C29 C30 105.26(10) . . ? O3 C29 H29A 110.7 . . ? C30 C29 H29A 110.7 . . ? O3 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C29 C30 C31 102.69(10) . . ? C29 C30 H30A 111.2 . . ? C31 C30 H30A 111.2 . . ? C29 C30 H30B 111.2 . . ? C31 C30 H30B 111.2 . . ? H30A C30 H30B 109.1 . . ? C32 C31 C30 101.76(10) . . ? C32 C31 H31A 111.4 . . ? C30 C31 H31A 111.4 . . ? C32 C31 H31B 111.4 . . ? C30 C31 H31B 111.4 . . ? H31A C31 H31B 109.3 . . ? O3 C32 C31 104.14(10) . . ? O3 C32 H32A 110.9 . . ? C31 C32 H32A 110.9 . . ? O3 C32 H32B 110.9 . . ? C31 C32 H32B 110.9 . . ? H32A C32 H32B 108.9 . . ? 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 O1 Al1 O2 C16 88.38(9) . . . . ? O3 Al1 O2 C16 179.63(8) . . . . ? N1 Al1 O2 C16 7.19(8) . . . . ? Br1 Al1 O2 C16 -84.74(8) . . . . ? O2 Al1 O1 C2 -80.57(9) . . . . ? O3 Al1 O1 C2 -172.00(8) . . . . ? N1 Al1 O1 C2 0.37(8) . . . . ? Br1 Al1 O1 C2 92.27(8) . . . . ? O1 Al1 O3 C29 39.37(9) . . . . ? O2 Al1 O3 C29 -81.37(8) . . . . ? Br1 Al1 O3 C29 161.04(8) . . . . ? O1 Al1 O3 C32 179.31(8) . . . . ? O2 Al1 O3 C32 58.57(8) . . . . ? Br1 Al1 O3 C32 -59.03(8) . . . . ? O1 Al1 N1 C1 -1.10(7) . . . . ? O2 Al1 N1 C1 120.42(7) . . . . ? Br1 Al1 N1 C1 -122.40(6) . . . . ? O1 Al1 N1 C15 -126.33(7) . . . . ? O2 Al1 N1 C15 -4.82(7) . . . . ? Br1 Al1 N1 C15 112.37(6) . . . . ? C1 N1 C15 C20 72.00(14) . . . . ? Al1 N1 C15 C20 -171.94(9) . . . . ? C1 N1 C15 C16 -114.11(11) . . . . ? Al1 N1 C15 C16 1.94(11) . . . . ? Al1 O2 C16 C15 -8.20(13) . . . . ? Al1 O2 C16 C17 170.00(9) . . . . ? C20 C15 C16 O2 177.29(10) . . . . ? N1 C15 C16 O2 3.28(14) . . . . ? C20 C15 C16 C17 -0.96(17) . . . . ? N1 C15 C16 C17 -174.97(10) . . . . ? O2 C16 C17 C18 -178.14(10) . . . . ? C15 C16 C17 C18 0.03(16) . . . . ? O2 C16 C17 C21 -0.61(17) . . . . ? C15 C16 C17 C21 177.55(10) . . . . ? C16 C17 C18 C19 0.81(17) . . . . ? C21 C17 C18 C19 -176.71(11) . . . . ? C17 C18 C19 C20 -0.71(17) . . . . ? C17 C18 C19 C25 178.22(11) . . . . ? C16 C15 C20 C19 1.07(17) . . . . ? N1 C15 C20 C19 174.45(10) . . . . ? C18 C19 C20 C15 -0.25(16) . . . . ? C25 C19 C20 C15 -179.19(10) . . . . ? C18 C17 C21 C23 -1.50(16) . . . . ? C16 C17 C21 C23 -178.91(11) . . . . ? C18 C17 C21 C22 -121.37(12) . . . . ? C16 C17 C21 C22 61.23(14) . . . . ? C18 C17 C21 C24 117.73(12) . . . . ? C16 C17 C21 C24 -59.68(14) . . . . ? C18 C19 C25 C27 118.64(13) . . . . ? C20 C19 C25 C27 -62.47(14) . . . . ? C18 C19 C25 C26 -1.14(17) . . . . ? C20 C19 C25 C26 177.75(11) . . . . ? C18 C19 C25 C28 -121.45(12) . . . . ? C20 C19 C25 C28 57.44(14) . . . . ? C15 N1 C1 C6 -68.07(14) . . . . ? Al1 N1 C1 C6 175.73(9) . . . . ? C15 N1 C1 C2 117.81(11) . . . . ? Al1 N1 C1 C2 1.61(11) . . . . ? Al1 O1 C2 C1 0.55(13) . . . . ? Al1 O1 C2 C3 -177.51(9) . . . . ? C6 C1 C2 O1 -175.76(10) . . . . ? N1 C1 C2 O1 -1.57(15) . . . . ? C6 C1 C2 C3 2.37(17) . . . . ? N1 C1 C2 C3 176.57(10) . . . . ? O1 C2 C3 C4 176.39(10) . . . . ? C1 C2 C3 C4 -1.66(16) . . . . ? O1 C2 C3 C7 -1.38(17) . . . . ? C1 C2 C3 C7 -179.42(10) . . . . ? C2 C3 C4 C5 -0.14(17) . . . . ? C7 C3 C4 C5 177.60(11) . . . . ? C3 C4 C5 C6 1.31(18) . . . . ? C3 C4 C5 C11 -177.64(11) . . . . ? C2 C1 C6 C5 -1.18(17) . . . . ? N1 C1 C6 C5 -174.80(10) . . . . ? C4 C5 C6 C1 -0.64(16) . . . . ? C11 C5 C6 C1 178.35(10) . . . . ? C4 C3 C7 C9 4.59(16) . . . . ? C2 C3 C7 C9 -177.75(10) . . . . ? C4 C3 C7 C8 123.80(12) . . . . ? C2 C3 C7 C8 -58.54(14) . . . . ? C4 C3 C7 C10 -114.74(12) . . . . ? C2 C3 C7 C10 62.92(14) . . . . ? C4 C5 C11 C12 -2.37(17) . . . . ? C6 C5 C11 C12 178.71(11) . . . . ? C4 C5 C11 C14 -122.07(12) . . . . ? C6 C5 C11 C14 59.01(14) . . . . ? C4 C5 C11 C13 117.93(13) . . . . ? C6 C5 C11 C13 -61.00(14) . . . . ? C32 O3 C29 C30 4.95(13) . . . . ? Al1 O3 C29 C30 148.83(8) . . . . ? O3 C29 C30 C31 -28.27(13) . . . . ? C29 C30 C31 C32 40.60(12) . . . . ? C29 O3 C32 C31 20.89(12) . . . . ? Al1 O3 C32 C31 -123.03(9) . . . . ? C30 C31 C32 O3 -37.78(12) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.387 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.049 #===END data_afh254-6 _database_code_depnum_ccdc_archive 'CCDC 867893' #TrackingRef '- Al(ONO) combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (ONO)Al(tetrachloroquinone)(py) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C39 H45 N2 O4 Al Cl4, C4 H10 O' _chemical_formula_sum 'C43 H55 Al Cl4 N2 O5' _chemical_formula_weight 848.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3772(8) _cell_length_b 19.3065(9) _cell_length_c 17.0976(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.7960(10) _cell_angle_gamma 90.00 _cell_volume 5064.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 9994 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.58 _exptl_crystal_description rhombohedron _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.290 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9454 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; Crystallized from a saturated solution in Et2O at -35 deg. C' ; _diffrn_ambient_temperature 143(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 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40592 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10357 _reflns_number_gt 7131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. All non-hydrogen atoms are refined anisotropically. Hydrogen atoms were generated in calculated positions and refined using the riding model. The data were cut at 0.80 Angstroms because beyond that the data:parameter ration dropped below 2.0 and the completeness was low. There was a pocket of disordered solvent that was positioned accross an inversion center. Although ether molecules could be seen in this disorder, modeling them using standard modeling procedures was not very stable. Additionally, the largest Q-peak was directly on the inversion center too far from another atom to be included in reasonable disorder modeling. Thus, SQUEEZE was run on the data set, and the solvent pocket was calculated to contain 69 electrons of unassigned electron density. This roughly corresponds to 1.5 diethyl-ether molecules, resulting in a total of 3 disordered ether molecules per unit cell, consitent with the disorder observed in the structure during initial refinement. ; _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^)+(0.0597P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef 0.28 _refine_ls_number_reflns 10357 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.21793(4) 0.32688(3) 0.88317(4) 0.02511(15) Uani 1 1 d . . . Cl1 Cl 0.25688(4) 0.54473(3) 1.01859(3) 0.03364(14) Uani 1 1 d . . . Cl2 Cl 0.27725(4) 0.66588(3) 0.89786(4) 0.03649(15) Uani 1 1 d . . . Cl3 Cl 0.27323(4) 0.63276(3) 0.71849(4) 0.03841(15) Uani 1 1 d . . . Cl4 Cl 0.24869(4) 0.47922(3) 0.66087(3) 0.03862(15) Uani 1 1 d . . . O1 O 0.09701(8) 0.31308(7) 0.85767(8) 0.0262(3) Uani 1 1 d . . . O2 O 0.34097(9) 0.30837(7) 0.89316(8) 0.0277(3) Uani 1 1 d . . . O3 O 0.22458(9) 0.40701(7) 0.93937(8) 0.0263(3) Uani 1 1 d . . . O4 O 0.22861(9) 0.37930(7) 0.79314(8) 0.0279(3) Uani 1 1 d . . . O5 O 0.01981(16) 0.09344(11) 0.94767(12) 0.0714(7) Uani 1 1 d . . . N1 N 0.22272(10) 0.23762(9) 0.82002(10) 0.0231(4) Uani 1 1 d . . . N2 N 0.20990(11) 0.27326(9) 0.98469(10) 0.0259(4) Uani 1 1 d . . . C1 C 0.14587(13) 0.22038(11) 0.78265(12) 0.0234(5) Uani 1 1 d . . . C2 C 0.07793(13) 0.26785(11) 0.80402(12) 0.0244(5) Uani 1 1 d . . . C3 C -0.00754(13) 0.26255(11) 0.76379(12) 0.0253(5) Uani 1 1 d . . . C4 C -0.01965(13) 0.20952(11) 0.71163(12) 0.0247(5) Uani 1 1 d . . . H4A H -0.0763 0.2042 0.6867 0.030 Uiso 1 1 calc R . . C5 C 0.04591(13) 0.16102(11) 0.69105(12) 0.0249(5) Uani 1 1 d . . . C6 C 0.12736(13) 0.16768(11) 0.72629(12) 0.0245(5) Uani 1 1 d . . . H6A H 0.1722 0.1368 0.7130 0.029 Uiso 1 1 calc R . . C7 C -0.07761(14) 0.31626(11) 0.77824(14) 0.0333(5) Uani 1 1 d . . . C8 C -0.10317(16) 0.31136(16) 0.86338(15) 0.0548(8) Uani 1 1 d . . . H8A H -0.0516 0.3190 0.8991 0.082 Uiso 1 1 calc R . . H8B H -0.1271 0.2653 0.8727 0.082 Uiso 1 1 calc R . . H8C H -0.1472 0.3466 0.8727 0.082 Uiso 1 1 calc R . . C9 C -0.04249(18) 0.38889(13) 0.7607(2) 0.0582(8) Uani 1 1 d . . . H9A H 0.0098 0.3981 0.7951 0.087 Uiso 1 1 calc R . . H9B H -0.0871 0.4236 0.7701 0.087 Uiso 1 1 calc R . . H9C H -0.0278 0.3912 0.7059 0.087 Uiso 1 1 calc R . . C10 C -0.16037(14) 0.30499(12) 0.72455(15) 0.0406(6) Uani 1 1 d . . . H10A H -0.1850 0.2594 0.7350 0.061 Uiso 1 1 calc R . . H10B H -0.1458 0.3074 0.6697 0.061 Uiso 1 1 calc R . . H10C H -0.2031 0.3410 0.7347 0.061 Uiso 1 1 calc R . . C11 C 0.02219(13) 0.10412(11) 0.63153(13) 0.0277(5) Uani 1 1 d . . . C12 C -0.01797(16) 0.13586(13) 0.55557(14) 0.0411(6) Uani 1 1 d . . . H12A H -0.0689 0.1637 0.5670 0.062 Uiso 1 1 calc R . . H12B H -0.0360 0.0988 0.5188 0.062 Uiso 1 1 calc R . . H12C H 0.0252 0.1654 0.5322 0.062 Uiso 1 1 calc R . . C13 C -0.04326(14) 0.05558(11) 0.66660(14) 0.0324(5) Uani 1 1 d . . . H13A H -0.0945 0.0821 0.6800 0.049 Uiso 1 1 calc R . . H13B H -0.0163 0.0338 0.7140 0.049 Uiso 1 1 calc R . . H13C H -0.0610 0.0197 0.6283 0.049 Uiso 1 1 calc R . . C14 C 0.10139(14) 0.06131(12) 0.61120(14) 0.0355(6) Uani 1 1 d . . . H14A H 0.1443 0.0916 0.5886 0.053 Uiso 1 1 calc R . . H14B H 0.0830 0.0254 0.5731 0.053 Uiso 1 1 calc R . . H14C H 0.1276 0.0395 0.6589 0.053 Uiso 1 1 calc R . . C15 C 0.30275(13) 0.21031(11) 0.81756(12) 0.0256(5) Uani 1 1 d . . . C16 C 0.36768(13) 0.25538(11) 0.85829(12) 0.0256(5) Uani 1 1 d . . . C17 C 0.45914(13) 0.23853(12) 0.85559(13) 0.0292(5) Uani 1 1 d . . . C18 C 0.47879(13) 0.18057(11) 0.81531(13) 0.0302(5) Uani 1 1 d . . . H18A H 0.5387 0.1702 0.8110 0.036 Uiso 1 1 calc R . . C19 C 0.41558(13) 0.13336(11) 0.77843(13) 0.0285(5) Uani 1 1 d . . . C20 C 0.32960(13) 0.14857(11) 0.78113(12) 0.0284(5) Uani 1 1 d . . . H20A H 0.2871 0.1176 0.7584 0.034 Uiso 1 1 calc R . . C21 C 0.52699(14) 0.28578(13) 0.89794(15) 0.0400(6) Uani 1 1 d . . . C22 C 0.51998(18) 0.35906(14) 0.8647(2) 0.0614(9) Uani 1 1 d . . . H22A H 0.4614 0.3772 0.8711 0.092 Uiso 1 1 calc R . . H22B H 0.5310 0.3582 0.8089 0.092 Uiso 1 1 calc R . . H22C H 0.5631 0.3889 0.8929 0.092 Uiso 1 1 calc R . . C23 C 0.51289(16) 0.28582(17) 0.98550(16) 0.0584(8) Uani 1 1 d . . . H23A H 0.4541 0.3028 0.9937 0.088 Uiso 1 1 calc R . . H23B H 0.5560 0.3161 1.0129 0.088 Uiso 1 1 calc R . . H23C H 0.5195 0.2386 1.0061 0.088 Uiso 1 1 calc R . . C24 C 0.62028(14) 0.25952(15) 0.88718(18) 0.0521(8) Uani 1 1 d . . . H24A H 0.6312 0.2599 0.8314 0.078 Uiso 1 1 calc R . . H24B H 0.6265 0.2122 0.9075 0.078 Uiso 1 1 calc R . . H24C H 0.6624 0.2898 0.9159 0.078 Uiso 1 1 calc R . . C25 C 0.44807(14) 0.06957(13) 0.73652(15) 0.0389(6) Uani 1 1 d . . . C26 C 0.49654(18) 0.09420(16) 0.66574(16) 0.0561(8) Uani 1 1 d . . . H26A H 0.5449 0.1245 0.6838 0.084 Uiso 1 1 calc R . . H26B H 0.4562 0.1197 0.6295 0.084 Uiso 1 1 calc R . . H26C H 0.5195 0.0540 0.6388 0.084 Uiso 1 1 calc R . . C27 C 0.50998(16) 0.02727(13) 0.79106(17) 0.0462(7) Uani 1 1 d . . . H27A H 0.5595 0.0562 0.8096 0.069 Uiso 1 1 calc R . . H27B H 0.5312 -0.0128 0.7626 0.069 Uiso 1 1 calc R . . H27C H 0.4791 0.0112 0.8360 0.069 Uiso 1 1 calc R . . C28 C 0.37194(17) 0.02286(14) 0.7070(2) 0.0618(9) Uani 1 1 d . . . H28A H 0.3404 0.0070 0.7516 0.093 Uiso 1 1 calc R . . H28B H 0.3946 -0.0173 0.6797 0.093 Uiso 1 1 calc R . . H28C H 0.3323 0.0491 0.6708 0.093 Uiso 1 1 calc R . . C29 C 0.24051(12) 0.46064(11) 0.89340(12) 0.0236(5) Uani 1 1 d . . . C30 C 0.24059(12) 0.44552(11) 0.81228(13) 0.0250(5) Uani 1 1 d . . . C31 C 0.25219(13) 0.49822(12) 0.75984(13) 0.0276(5) Uani 1 1 d . . . C32 C 0.26434(13) 0.56680(11) 0.78598(13) 0.0275(5) Uani 1 1 d . . . C33 C 0.26635(12) 0.58128(11) 0.86511(14) 0.0270(5) Uani 1 1 d . . . C34 C 0.25530(12) 0.52762(11) 0.91937(12) 0.0255(5) Uani 1 1 d . . . C35 C 0.26896(15) 0.28850(13) 1.04464(13) 0.0359(6) Uani 1 1 d . . . H35A H 0.3073 0.3264 1.0388 0.043 Uiso 1 1 calc R . . C36 C 0.27578(17) 0.25157(14) 1.11333(15) 0.0441(6) Uani 1 1 d . . . H36A H 0.3187 0.2635 1.1536 0.053 Uiso 1 1 calc R . . C37 C 0.21963(18) 0.19679(14) 1.12355(15) 0.0467(7) Uani 1 1 d . . . H37A H 0.2233 0.1704 1.1705 0.056 Uiso 1 1 calc R . . C38 C 0.15833(18) 0.18166(13) 1.06381(15) 0.0459(7) Uani 1 1 d . . . H38A H 0.1180 0.1450 1.0694 0.055 Uiso 1 1 calc R . . C39 C 0.15596(16) 0.22028(13) 0.99548(14) 0.0390(6) Uani 1 1 d . . . H39A H 0.1140 0.2086 0.9543 0.047 Uiso 1 1 calc R . . C40 C -0.0982(3) 0.1522(3) 1.0001(3) 0.1127(15) Uani 1 1 d . . . H40A H -0.1603 0.1630 0.9911 0.169 Uiso 1 1 calc R . . H40B H -0.0644 0.1953 1.0021 0.169 Uiso 1 1 calc R . . H40C H -0.0884 0.1274 1.0499 0.169 Uiso 1 1 calc R . . C41 C -0.0699(3) 0.1078(2) 0.9347(2) 0.0970(14) Uani 1 1 d . . . H41A H -0.1035 0.0640 0.9326 0.116 Uiso 1 1 calc R . . H41B H -0.0810 0.1321 0.8841 0.116 Uiso 1 1 calc R . . C42 C 0.0499(3) 0.0477(2) 0.8932(2) 0.0960(14) Uani 1 1 d . . . H42A H 0.0364 0.0659 0.8397 0.115 Uiso 1 1 calc R . . H42B H 0.0200 0.0025 0.8974 0.115 Uiso 1 1 calc R . . C43 C 0.1465(4) 0.0378(2) 0.9071(3) 0.1173(16) Uani 1 1 d . . . H43A H 0.1669 0.0050 0.8686 0.176 Uiso 1 1 calc R . . H43B H 0.1597 0.0197 0.9600 0.176 Uiso 1 1 calc R . . H43C H 0.1760 0.0824 0.9016 0.176 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0247(3) 0.0238(4) 0.0267(3) -0.0031(3) 0.0004(3) -0.0022(3) Cl1 0.0382(3) 0.0298(3) 0.0326(3) -0.0070(2) 0.0002(2) -0.0045(2) Cl2 0.0353(3) 0.0232(3) 0.0498(4) -0.0017(3) -0.0064(3) -0.0038(2) Cl3 0.0387(3) 0.0314(3) 0.0450(4) 0.0103(3) 0.0015(3) -0.0027(3) Cl4 0.0491(4) 0.0376(3) 0.0293(3) 0.0019(3) 0.0033(3) -0.0023(3) O1 0.0241(7) 0.0248(8) 0.0292(8) -0.0055(6) -0.0008(6) 0.0003(6) O2 0.0249(7) 0.0266(8) 0.0314(8) -0.0064(7) 0.0012(6) -0.0013(6) O3 0.0291(8) 0.0233(8) 0.0265(8) -0.0029(6) 0.0017(6) -0.0026(6) O4 0.0320(8) 0.0236(8) 0.0283(8) -0.0022(6) 0.0026(6) -0.0016(6) O5 0.1016(18) 0.0579(14) 0.0522(13) -0.0041(11) -0.0141(12) -0.0281(13) N1 0.0213(8) 0.0223(9) 0.0257(9) 0.0014(7) 0.0012(7) -0.0013(7) N2 0.0279(9) 0.0217(10) 0.0283(10) -0.0030(8) 0.0029(8) -0.0001(8) C1 0.0230(10) 0.0224(11) 0.0248(11) 0.0013(9) 0.0018(8) -0.0023(9) C2 0.0261(11) 0.0210(11) 0.0260(11) 0.0004(9) 0.0022(9) -0.0032(9) C3 0.0226(10) 0.0232(12) 0.0297(12) 0.0012(9) -0.0003(9) -0.0003(9) C4 0.0200(10) 0.0237(12) 0.0297(12) 0.0015(9) -0.0026(8) 0.0001(9) C5 0.0235(10) 0.0254(12) 0.0257(11) 0.0022(9) 0.0014(8) -0.0043(9) C6 0.0248(10) 0.0214(11) 0.0278(11) -0.0008(9) 0.0047(9) -0.0010(9) C7 0.0279(11) 0.0244(12) 0.0464(14) -0.0084(10) -0.0065(10) 0.0077(9) C8 0.0345(14) 0.080(2) 0.0493(17) -0.0231(15) -0.0003(12) 0.0208(14) C9 0.0483(16) 0.0230(14) 0.100(2) -0.0058(15) -0.0216(16) 0.0056(12) C10 0.0319(12) 0.0311(14) 0.0569(16) -0.0117(12) -0.0111(11) 0.0095(11) C11 0.0234(11) 0.0253(12) 0.0341(12) -0.0050(10) -0.0001(9) -0.0031(9) C12 0.0488(15) 0.0392(15) 0.0343(13) -0.0072(11) -0.0044(11) -0.0045(12) C13 0.0240(11) 0.0255(13) 0.0475(14) -0.0060(11) 0.0005(10) -0.0016(9) C14 0.0265(11) 0.0370(14) 0.0434(14) -0.0165(11) 0.0042(10) -0.0054(10) C15 0.0238(10) 0.0248(12) 0.0280(11) 0.0013(9) 0.0001(9) -0.0001(9) C16 0.0250(11) 0.0271(12) 0.0249(11) 0.0017(9) 0.0025(9) -0.0009(9) C17 0.0235(11) 0.0306(13) 0.0334(12) -0.0010(10) 0.0010(9) -0.0034(9) C18 0.0223(11) 0.0327(13) 0.0355(13) 0.0012(10) 0.0022(9) -0.0021(9) C19 0.0272(11) 0.0285(12) 0.0294(12) -0.0019(10) -0.0009(9) 0.0017(9) C20 0.0269(11) 0.0258(12) 0.0317(12) -0.0027(10) -0.0042(9) -0.0023(9) C21 0.0231(11) 0.0404(15) 0.0565(16) -0.0166(13) 0.0037(11) -0.0057(10) C22 0.0382(15) 0.0382(17) 0.108(3) -0.0107(17) 0.0101(16) -0.0126(13) C23 0.0291(13) 0.088(2) 0.0559(18) -0.0324(17) -0.0091(12) 0.0006(14) C24 0.0217(12) 0.0588(19) 0.075(2) -0.0246(15) 0.0015(12) -0.0082(12) C25 0.0292(12) 0.0351(14) 0.0511(16) -0.0128(12) -0.0072(11) 0.0072(10) C26 0.0519(17) 0.074(2) 0.0427(16) -0.0138(15) 0.0032(13) 0.0209(15) C27 0.0360(13) 0.0319(14) 0.0694(19) -0.0055(13) -0.0063(12) 0.0058(11) C28 0.0381(15) 0.0479(17) 0.097(2) -0.0401(17) -0.0154(15) 0.0130(13) C29 0.0149(9) 0.0252(12) 0.0307(12) 0.0009(9) 0.0019(8) -0.0001(8) C30 0.0172(10) 0.0248(12) 0.0328(12) -0.0012(9) 0.0007(8) 0.0007(8) C31 0.0206(10) 0.0316(13) 0.0308(12) -0.0007(10) 0.0025(9) 0.0003(9) C32 0.0184(10) 0.0292(12) 0.0349(13) 0.0049(10) 0.0011(9) -0.0007(9) C33 0.0169(10) 0.0199(11) 0.0440(14) -0.0008(10) -0.0009(9) -0.0016(8) C34 0.0173(10) 0.0290(12) 0.0301(12) -0.0067(10) 0.0005(8) -0.0005(9) C35 0.0390(13) 0.0343(14) 0.0342(13) -0.0029(11) 0.0013(10) 0.0032(11) C36 0.0559(16) 0.0433(16) 0.0322(14) -0.0042(12) -0.0031(12) 0.0067(13) C37 0.0727(19) 0.0354(15) 0.0320(14) 0.0012(11) 0.0037(13) 0.0115(14) C38 0.0646(17) 0.0353(15) 0.0385(15) 0.0047(12) 0.0092(13) -0.0058(13) C39 0.0451(14) 0.0349(14) 0.0368(14) 0.0002(11) 0.0011(11) -0.0016(12) C40 0.105(4) 0.124(4) 0.110(4) 0.017(3) 0.011(3) -0.019(3) C41 0.093(3) 0.109(3) 0.085(3) 0.017(3) -0.022(2) -0.045(3) C42 0.156(4) 0.070(3) 0.062(2) -0.010(2) 0.008(3) -0.039(3) C43 0.174(5) 0.069(3) 0.112(4) -0.009(3) 0.034(4) 0.005(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 O3 1.8206(15) . ? Al1 O4 1.8586(16) . ? Al1 O1 1.9003(14) . ? Al1 O2 1.9220(15) . ? Al1 N2 2.0317(19) . ? Al1 N1 2.0375(18) . ? Cl1 C34 1.727(2) . ? Cl2 C33 1.731(2) . ? Cl3 C32 1.730(2) . ? Cl4 C31 1.729(2) . ? O1 C2 1.286(2) . ? O2 C16 1.266(2) . ? O3 C29 1.332(2) . ? O4 C30 1.330(2) . ? O5 C42 1.385(4) . ? O5 C41 1.410(4) . ? N1 C15 1.342(3) . ? N1 C1 1.347(2) . ? N2 C39 1.337(3) . ? N2 C35 1.356(3) . ? C1 C6 1.417(3) . ? C1 C2 1.455(3) . ? C2 C3 1.446(3) . ? C3 C4 1.362(3) . ? C3 C7 1.527(3) . ? C4 C5 1.437(3) . ? C4 H4A 0.9500 . ? C5 C6 1.360(3) . ? C5 C11 1.525(3) . ? C6 H6A 0.9500 . ? C7 C10 1.535(3) . ? C7 C8 1.536(4) . ? C7 C9 1.539(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.527(3) . ? C11 C12 1.529(3) . ? C11 C14 1.531(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.419(3) . ? C15 C16 1.465(3) . ? C16 C17 1.447(3) . ? C17 C18 1.358(3) . ? C17 C21 1.531(3) . ? C18 C19 1.446(3) . ? C18 H18A 0.9500 . ? C19 C20 1.358(3) . ? C19 C25 1.526(3) . ? C20 H20A 0.9500 . ? C21 C22 1.526(4) . ? C21 C23 1.527(4) . ? C21 C24 1.544(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.525(3) . ? C25 C28 1.536(3) . ? C25 C26 1.538(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.381(3) . ? C29 C30 1.417(3) . ? C30 C31 1.375(3) . ? C31 C32 1.406(3) . ? C32 C33 1.380(3) . ? C33 C34 1.409(3) . ? C35 C36 1.372(3) . ? C35 H35A 0.9500 . ? C36 C37 1.384(4) . ? C36 H36A 0.9500 . ? C37 C38 1.375(4) . ? C37 H37A 0.9500 . ? C38 C39 1.384(3) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.496(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.502(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 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 O3 Al1 O4 88.25(7) . . ? O3 Al1 O1 105.08(7) . . ? O4 Al1 O1 91.43(7) . . ? O3 Al1 O2 95.19(7) . . ? O4 Al1 O2 91.97(7) . . ? O1 Al1 O2 159.53(7) . . ? O3 Al1 N2 89.23(7) . . ? O4 Al1 N2 177.09(7) . . ? O1 Al1 N2 90.62(7) . . ? O2 Al1 N2 86.82(7) . . ? O3 Al1 N1 174.69(7) . . ? O4 Al1 N1 90.77(7) . . ? O1 Al1 N1 80.16(6) . . ? O2 Al1 N1 79.62(7) . . ? N2 Al1 N1 91.61(7) . . ? C2 O1 Al1 115.62(13) . . ? C16 O2 Al1 117.16(13) . . ? C29 O3 Al1 110.80(13) . . ? C30 O4 Al1 109.77(13) . . ? C42 O5 C41 112.7(3) . . ? C15 N1 C1 131.71(18) . . ? C15 N1 Al1 114.48(13) . . ? C1 N1 Al1 113.51(13) . . ? C39 N2 C35 116.9(2) . . ? C39 N2 Al1 125.51(15) . . ? C35 N2 Al1 117.37(15) . . ? N1 C1 C6 129.06(19) . . ? N1 C1 C2 110.32(17) . . ? C6 C1 C2 120.53(17) . . ? O1 C2 C3 122.99(19) . . ? O1 C2 C1 118.25(17) . . ? C3 C2 C1 118.76(18) . . ? C4 C3 C2 116.43(18) . . ? C4 C3 C7 123.29(18) . . ? C2 C3 C7 120.24(18) . . ? C3 C4 C5 125.62(18) . . ? C3 C4 H4A 117.2 . . ? C5 C4 H4A 117.2 . . ? C6 C5 C4 118.07(19) . . ? C6 C5 C11 122.44(19) . . ? C4 C5 C11 119.48(17) . . ? C5 C6 C1 120.46(19) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? C3 C7 C10 111.89(18) . . ? C3 C7 C8 109.82(19) . . ? C10 C7 C8 107.7(2) . . ? C3 C7 C9 109.1(2) . . ? C10 C7 C9 107.50(19) . . ? C8 C7 C9 110.8(2) . . ? 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 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 C13 108.36(18) . . ? C5 C11 C12 110.09(18) . . ? C13 C11 C12 109.88(18) . . ? C5 C11 C14 112.43(16) . . ? C13 C11 C14 108.23(18) . . ? C12 C11 C14 107.83(19) . . ? 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 . . ? 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 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C20 129.64(19) . . ? N1 C15 C16 110.44(18) . . ? C20 C15 C16 119.90(18) . . ? O2 C16 C17 122.88(19) . . ? O2 C16 C15 118.13(18) . . ? C17 C16 C15 118.97(19) . . ? C18 C17 C16 116.79(19) . . ? C18 C17 C21 124.26(19) . . ? C16 C17 C21 119.0(2) . . ? C17 C18 C19 125.1(2) . . ? C17 C18 H18A 117.5 . . ? C19 C18 H18A 117.5 . . ? C20 C19 C18 118.5(2) . . ? C20 C19 C25 122.70(19) . . ? C18 C19 C25 118.82(19) . . ? C19 C20 C15 120.58(19) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? C22 C21 C23 110.7(2) . . ? C22 C21 C17 110.3(2) . . ? C23 C21 C17 109.1(2) . . ? C22 C21 C24 107.7(2) . . ? C23 C21 C24 108.1(2) . . ? C17 C21 C24 110.9(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C19 110.8(2) . . ? C27 C25 C28 108.5(2) . . ? C19 C25 C28 111.24(19) . . ? C27 C25 C26 109.3(2) . . ? C19 C25 C26 108.1(2) . . ? C28 C25 C26 108.7(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C34 124.79(19) . . ? O3 C29 C30 115.43(18) . . ? C34 C29 C30 119.8(2) . . ? O4 C30 C31 124.9(2) . . ? O4 C30 C29 115.45(19) . . ? C31 C30 C29 119.6(2) . . ? C30 C31 C32 120.6(2) . . ? C30 C31 Cl4 118.95(17) . . ? C32 C31 Cl4 120.39(17) . . ? C33 C32 C31 119.8(2) . . ? C33 C32 Cl3 120.48(17) . . ? C31 C32 Cl3 119.73(17) . . ? C32 C33 C34 120.06(19) . . ? C32 C33 Cl2 120.24(17) . . ? C34 C33 Cl2 119.62(17) . . ? C29 C34 C33 120.09(19) . . ? C29 C34 Cl1 119.09(17) . . ? C33 C34 Cl1 120.79(16) . . ? N2 C35 C36 122.9(2) . . ? N2 C35 H35A 118.5 . . ? C36 C35 H35A 118.5 . . ? C35 C36 C37 119.5(2) . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? C38 C37 C36 118.1(2) . . ? C38 C37 H37A 120.9 . . ? C36 C37 H37A 120.9 . . ? C37 C38 C39 119.4(2) . . ? C37 C38 H38A 120.3 . . ? C39 C38 H38A 120.3 . . ? N2 C39 C38 123.1(2) . . ? N2 C39 H39A 118.4 . . ? C38 C39 H39A 118.4 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O5 C41 C40 109.0(3) . . ? O5 C41 H41A 109.9 . . ? C40 C41 H41A 109.9 . . ? O5 C41 H41B 109.9 . . ? C40 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? O5 C42 C43 110.2(3) . . ? O5 C42 H42A 109.6 . . ? C43 C42 H42A 109.6 . . ? O5 C42 H42B 109.6 . . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 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 O3 Al1 O1 C2 165.54(14) . . . . ? O4 Al1 O1 C2 76.97(15) . . . . ? O2 Al1 O1 C2 -22.5(3) . . . . ? N2 Al1 O1 C2 -105.09(15) . . . . ? N1 Al1 O1 C2 -13.56(14) . . . . ? O3 Al1 O2 C16 -177.47(15) . . . . ? O4 Al1 O2 C16 -89.05(15) . . . . ? O1 Al1 O2 C16 10.4(3) . . . . ? N2 Al1 O2 C16 93.60(15) . . . . ? N1 Al1 O2 C16 1.37(15) . . . . ? O4 Al1 O3 C29 -5.12(12) . . . . ? O1 Al1 O3 C29 -96.13(13) . . . . ? O2 Al1 O3 C29 86.70(13) . . . . ? N2 Al1 O3 C29 173.44(12) . . . . ? O3 Al1 O4 C30 3.57(13) . . . . ? O1 Al1 O4 C30 108.62(13) . . . . ? O2 Al1 O4 C30 -91.57(13) . . . . ? N1 Al1 O4 C30 -171.21(13) . . . . ? O4 Al1 N1 C15 93.21(15) . . . . ? O1 Al1 N1 C15 -175.47(15) . . . . ? O2 Al1 N1 C15 1.35(14) . . . . ? N2 Al1 N1 C15 -85.12(15) . . . . ? O4 Al1 N1 C1 -81.16(14) . . . . ? O1 Al1 N1 C1 10.16(14) . . . . ? O2 Al1 N1 C1 -173.02(15) . . . . ? N2 Al1 N1 C1 100.51(14) . . . . ? O3 Al1 N2 C39 137.36(19) . . . . ? O1 Al1 N2 C39 32.29(19) . . . . ? O2 Al1 N2 C39 -127.40(19) . . . . ? N1 Al1 N2 C39 -47.89(19) . . . . ? O3 Al1 N2 C35 -48.49(16) . . . . ? O1 Al1 N2 C35 -153.56(16) . . . . ? O2 Al1 N2 C35 46.75(16) . . . . ? N1 Al1 N2 C35 126.26(16) . . . . ? C15 N1 C1 C6 -2.0(4) . . . . ? Al1 N1 C1 C6 171.12(18) . . . . ? C15 N1 C1 C2 -178.4(2) . . . . ? Al1 N1 C1 C2 -5.3(2) . . . . ? Al1 O1 C2 C3 -164.36(16) . . . . ? Al1 O1 C2 C1 15.1(2) . . . . ? N1 C1 C2 O1 -5.9(3) . . . . ? C6 C1 C2 O1 177.32(19) . . . . ? N1 C1 C2 C3 173.57(18) . . . . ? C6 C1 C2 C3 -3.2(3) . . . . ? O1 C2 C3 C4 -176.24(19) . . . . ? C1 C2 C3 C4 4.3(3) . . . . ? O1 C2 C3 C7 6.1(3) . . . . ? C1 C2 C3 C7 -173.40(19) . . . . ? C2 C3 C4 C5 -3.0(3) . . . . ? C7 C3 C4 C5 174.6(2) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C3 C4 C5 C11 179.9(2) . . . . ? C4 C5 C6 C1 1.1(3) . . . . ? C11 C5 C6 C1 -178.50(19) . . . . ? N1 C1 C6 C5 -175.7(2) . . . . ? C2 C1 C6 C5 0.4(3) . . . . ? C4 C3 C7 C10 -2.7(3) . . . . ? C2 C3 C7 C10 174.8(2) . . . . ? C4 C3 C7 C8 116.9(2) . . . . ? C2 C3 C7 C8 -65.6(3) . . . . ? C4 C3 C7 C9 -121.5(2) . . . . ? C2 C3 C7 C9 56.0(3) . . . . ? C6 C5 C11 C13 114.1(2) . . . . ? C4 C5 C11 C13 -65.5(2) . . . . ? C6 C5 C11 C12 -125.7(2) . . . . ? C4 C5 C11 C12 54.7(3) . . . . ? C6 C5 C11 C14 -5.5(3) . . . . ? C4 C5 C11 C14 174.92(19) . . . . ? C1 N1 C15 C20 -8.6(4) . . . . ? Al1 N1 C15 C20 178.36(19) . . . . ? C1 N1 C15 C16 169.7(2) . . . . ? Al1 N1 C15 C16 -3.3(2) . . . . ? Al1 O2 C16 C17 174.82(16) . . . . ? Al1 O2 C16 C15 -3.7(2) . . . . ? N1 C15 C16 O2 4.7(3) . . . . ? C20 C15 C16 O2 -176.84(19) . . . . ? N1 C15 C16 C17 -173.95(18) . . . . ? C20 C15 C16 C17 4.5(3) . . . . ? O2 C16 C17 C18 -179.2(2) . . . . ? C15 C16 C17 C18 -0.6(3) . . . . ? O2 C16 C17 C21 1.2(3) . . . . ? C15 C16 C17 C21 179.8(2) . . . . ? C16 C17 C18 C19 -2.9(3) . . . . ? C21 C17 C18 C19 176.6(2) . . . . ? C17 C18 C19 C20 2.6(3) . . . . ? C17 C18 C19 C25 -178.8(2) . . . . ? C18 C19 C20 C15 1.6(3) . . . . ? C25 C19 C20 C15 -176.9(2) . . . . ? N1 C15 C20 C19 173.1(2) . . . . ? C16 C15 C20 C19 -5.0(3) . . . . ? C18 C17 C21 C22 120.4(3) . . . . ? C16 C17 C21 C22 -60.1(3) . . . . ? C18 C17 C21 C23 -117.8(3) . . . . ? C16 C17 C21 C23 61.7(3) . . . . ? C18 C17 C21 C24 1.2(3) . . . . ? C16 C17 C21 C24 -179.3(2) . . . . ? C20 C19 C25 C27 -126.9(2) . . . . ? C18 C19 C25 C27 54.6(3) . . . . ? C20 C19 C25 C28 -6.1(3) . . . . ? C18 C19 C25 C28 175.4(2) . . . . ? C20 C19 C25 C26 113.2(2) . . . . ? C18 C19 C25 C26 -65.3(3) . . . . ? Al1 O3 C29 C34 -175.19(16) . . . . ? Al1 O3 C29 C30 5.6(2) . . . . ? Al1 O4 C30 C31 179.00(16) . . . . ? Al1 O4 C30 C29 -1.3(2) . . . . ? O3 C29 C30 O4 -2.9(2) . . . . ? C34 C29 C30 O4 177.89(17) . . . . ? O3 C29 C30 C31 176.84(17) . . . . ? C34 C29 C30 C31 -2.4(3) . . . . ? O4 C30 C31 C32 179.96(18) . . . . ? C29 C30 C31 C32 0.3(3) . . . . ? O4 C30 C31 Cl4 1.7(3) . . . . ? C29 C30 C31 Cl4 -178.00(15) . . . . ? C30 C31 C32 C33 1.3(3) . . . . ? Cl4 C31 C32 C33 179.52(15) . . . . ? C30 C31 C32 Cl3 -176.71(15) . . . . ? Cl4 C31 C32 Cl3 1.5(2) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? Cl3 C32 C33 C34 177.27(15) . . . . ? C31 C32 C33 Cl2 -177.62(15) . . . . ? Cl3 C32 C33 Cl2 0.3(2) . . . . ? O3 C29 C34 C33 -176.19(17) . . . . ? C30 C29 C34 C33 3.0(3) . . . . ? O3 C29 C34 Cl1 2.0(3) . . . . ? C30 C29 C34 Cl1 -178.86(15) . . . . ? C32 C33 C34 C29 -1.4(3) . . . . ? Cl2 C33 C34 C29 175.51(15) . . . . ? C32 C33 C34 Cl1 -179.57(15) . . . . ? Cl2 C33 C34 Cl1 -2.6(2) . . . . ? C39 N2 C35 C36 1.1(3) . . . . ? Al1 N2 C35 C36 -173.55(19) . . . . ? N2 C35 C36 C37 -1.0(4) . . . . ? C35 C36 C37 C38 -0.3(4) . . . . ? C36 C37 C38 C39 1.4(4) . . . . ? C35 N2 C39 C38 0.0(3) . . . . ? Al1 N2 C39 C38 174.22(19) . . . . ? C37 C38 C39 N2 -1.3(4) . . . . ? C42 O5 C41 C40 174.9(3) . . . . ? C41 O5 C42 C43 176.6(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.291 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.051 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.500 389 69 'ca. 1.5 Et2O' 2 0.500 1.000 1.000 389 69 'ca. 1.5 Et2O' 3 0.500 0.500 0.000 45 1 ' ' 4 0.500 0.000 0.500 45 1 ' ' _platon_squeeze_details ; ; #===END data_afh249-8 _database_code_depnum_ccdc_archive 'CCDC 867894' #TrackingRef '- Al(ONO) combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (ONO)Al(py)(pyrene-quinone) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C49 H53 Al N2 O4, 2(C4 H8 O)' _chemical_formula_sum 'C57 H69 Al N2 O6' _chemical_formula_weight 905.12 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9047(13) _cell_length_b 18.0625(17) _cell_length_c 19.4014(18) _cell_angle_alpha 90.00 _cell_angle_beta 93.1500(10) _cell_angle_gamma 90.00 _cell_volume 4865.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 3246 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 22.10 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9749 _exptl_absorpt_correction_T_max 0.9943 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39430 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9955 _reflns_number_gt 6253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX2' _computing_cell_refinement 'Bruker SMART APEX2/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0629P)^2^+0.8743P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9955 _refine_ls_number_parameters 623 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1023 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 1.14506(5) 1.33162(4) 0.30797(4) 0.01773(17) Uani 1 1 d . . . O1 O 1.23743(11) 1.40593(8) 0.30175(8) 0.0191(4) Uani 1 1 d . . . O2 O 1.08126(11) 1.24137(8) 0.31458(8) 0.0200(4) Uani 1 1 d . . . O3 O 1.03670(11) 1.39195(8) 0.28498(8) 0.0180(4) Uani 1 1 d . . . O4 O 1.11381(11) 1.35209(9) 0.40212(8) 0.0195(4) Uani 1 1 d . . . O5 O 1.41813(14) 1.18317(11) 0.11550(10) 0.0413(5) Uani 1 1 d . . . N1 N 1.25797(13) 1.27162(10) 0.33723(10) 0.0176(4) Uani 1 1 d . . . N2 N 1.15594(13) 1.31370(10) 0.20389(10) 0.0191(4) Uani 1 1 d . . . C1 C 1.34302(16) 1.30861(13) 0.33672(12) 0.0179(5) Uani 1 1 d . . . C2 C 1.32794(16) 1.38396(13) 0.31394(12) 0.0176(5) Uani 1 1 d . . . C3 C 1.40888(16) 1.43054(13) 0.30466(12) 0.0190(5) Uani 1 1 d . . . C4 C 1.49901(16) 1.40126(13) 0.32320(12) 0.0203(5) Uani 1 1 d . . . H4A H 1.5534 1.4325 0.3196 0.024 Uiso 1 1 calc R . . C5 C 1.51525(17) 1.32817(13) 0.34702(13) 0.0220(5) Uani 1 1 d . . . C6 C 1.43725(16) 1.28261(13) 0.35248(12) 0.0206(5) Uani 1 1 d . . . H6A H 1.4468 1.2328 0.3671 0.025 Uiso 1 1 calc R . . C7 C 1.39666(16) 1.50804(13) 0.27291(12) 0.0209(5) Uani 1 1 d . . . C8 C 1.49369(17) 1.54702(14) 0.26743(14) 0.0263(6) Uani 1 1 d . . . H8A H 1.5262 1.5508 0.3134 0.039 Uiso 1 1 calc R . . H8B H 1.4831 1.5967 0.2483 0.039 Uiso 1 1 calc R . . H8C H 1.5339 1.5185 0.2371 0.039 Uiso 1 1 calc R . . C9 C 1.34924(19) 1.50126(14) 0.19975(13) 0.0297(6) Uani 1 1 d . . . H9A H 1.3886 1.4692 0.1718 0.045 Uiso 1 1 calc R . . H9B H 1.3441 1.5504 0.1785 0.045 Uiso 1 1 calc R . . H9C H 1.2848 1.4798 0.2022 0.045 Uiso 1 1 calc R . . C10 C 1.33350(18) 1.55716(14) 0.31629(14) 0.0291(6) Uani 1 1 d . . . H10A H 1.3629 1.5614 0.3632 0.044 Uiso 1 1 calc R . . H10B H 1.2693 1.5350 0.3180 0.044 Uiso 1 1 calc R . . H10C H 1.3279 1.6065 0.2954 0.044 Uiso 1 1 calc R . . C11 C 1.61931(17) 1.30298(14) 0.36512(14) 0.0283(6) Uani 1 1 d . . . C12 C 1.68306(19) 1.31775(18) 0.30499(16) 0.0449(8) Uani 1 1 d . . . H12A H 1.7491 1.3019 0.3176 0.067 Uiso 1 1 calc R . . H12B H 1.6826 1.3708 0.2944 0.067 Uiso 1 1 calc R . . H12C H 1.6584 1.2901 0.2643 0.067 Uiso 1 1 calc R . . C13 C 1.62418(19) 1.21990(15) 0.38220(19) 0.0482(9) Uani 1 1 d . . . H13A H 1.6911 1.2058 0.3940 0.072 Uiso 1 1 calc R . . H13B H 1.5997 1.1913 0.3420 0.072 Uiso 1 1 calc R . . H13C H 1.5848 1.2096 0.4215 0.072 Uiso 1 1 calc R . . C14 C 1.65930(19) 1.34556(16) 0.42827(15) 0.0387(7) Uani 1 1 d . . . H14A H 1.7255 1.3295 0.4400 0.058 Uiso 1 1 calc R . . H14B H 1.6193 1.3358 0.4673 0.058 Uiso 1 1 calc R . . H14C H 1.6587 1.3987 0.4181 0.058 Uiso 1 1 calc R . . C15 C 1.23450(16) 1.20151(12) 0.35753(12) 0.0172(5) Uani 1 1 d . . . C16 C 1.13267(16) 1.18938(13) 0.34695(12) 0.0176(5) Uani 1 1 d . . . C17 C 1.09204(16) 1.12292(13) 0.37176(12) 0.0182(5) Uani 1 1 d . . . C18 C 1.15488(16) 1.07004(13) 0.39965(12) 0.0192(5) Uani 1 1 d . . . H18A H 1.1282 1.0253 0.4159 0.023 Uiso 1 1 calc R . . C19 C 1.25593(16) 1.07816(13) 0.40561(12) 0.0188(5) Uani 1 1 d . . . C20 C 1.29407(16) 1.14497(12) 0.38596(12) 0.0191(5) Uani 1 1 d . . . H20A H 1.3616 1.1529 0.3917 0.023 Uiso 1 1 calc R . . C21 C 0.98231(16) 1.11282(13) 0.36731(13) 0.0217(5) Uani 1 1 d . . . C22 C 0.93421(19) 1.17807(15) 0.40309(16) 0.0373(7) Uani 1 1 d . . . H22A H 0.8641 1.1715 0.3999 0.056 Uiso 1 1 calc R . . H22B H 0.9508 1.2245 0.3804 0.056 Uiso 1 1 calc R . . H22C H 0.9571 1.1798 0.4518 0.056 Uiso 1 1 calc R . . C23 C 0.94371(17) 1.10858(15) 0.29163(13) 0.0280(6) Uani 1 1 d . . . H23A H 0.8735 1.1028 0.2899 0.042 Uiso 1 1 calc R . . H23B H 0.9727 1.0661 0.2692 0.042 Uiso 1 1 calc R . . H23C H 0.9603 1.1542 0.2676 0.042 Uiso 1 1 calc R . . C24 C 0.95271(18) 1.04232(14) 0.40314(14) 0.0308(6) Uani 1 1 d . . . H24A H 0.8824 1.0378 0.3996 0.046 Uiso 1 1 calc R . . H24B H 0.9752 1.0442 0.4519 0.046 Uiso 1 1 calc R . . H24C H 0.9815 0.9995 0.3810 0.046 Uiso 1 1 calc R . . C25 C 1.32051(17) 1.01365(13) 0.43152(13) 0.0229(6) Uani 1 1 d . . . C26 C 1.3000(2) 0.94480(14) 0.38622(16) 0.0406(8) Uani 1 1 d . . . H26A H 1.3111 0.9567 0.3380 0.061 Uiso 1 1 calc R . . H26B H 1.2329 0.9294 0.3900 0.061 Uiso 1 1 calc R . . H26C H 1.3430 0.9044 0.4018 0.061 Uiso 1 1 calc R . . C27 C 1.3015(2) 0.99551(17) 0.50588(14) 0.0392(7) Uani 1 1 d . . . H27A H 1.3135 1.0395 0.5346 0.059 Uiso 1 1 calc R . . H27B H 1.3445 0.9555 0.5223 0.059 Uiso 1 1 calc R . . H27C H 1.2344 0.9798 0.5088 0.059 Uiso 1 1 calc R . . C28 C 1.42722(18) 1.03114(14) 0.42623(14) 0.0306(6) Uani 1 1 d . . . H28A H 1.4438 1.0753 0.4536 0.046 Uiso 1 1 calc R . . H28B H 1.4405 1.0402 0.3779 0.046 Uiso 1 1 calc R . . H28C H 1.4659 0.9892 0.4438 0.046 Uiso 1 1 calc R . . C29 C 0.99055(15) 1.41119(12) 0.33867(12) 0.0160(5) Uani 1 1 d . . . C30 C 1.03321(16) 1.38668(12) 0.40398(12) 0.0184(5) Uani 1 1 d . . . C31 C 0.98541(16) 1.40205(12) 0.46645(12) 0.0184(5) Uani 1 1 d . . . C32 C 1.02346(17) 1.37689(13) 0.53046(13) 0.0216(5) Uani 1 1 d . . . H32A H 1.0794 1.3466 0.5328 0.026 Uiso 1 1 calc R . . C33 C 0.97987(17) 1.39597(13) 0.59056(13) 0.0237(6) Uani 1 1 d . . . H33A H 1.0055 1.3778 0.6337 0.028 Uiso 1 1 calc R . . C34 C 0.89977(17) 1.44097(13) 0.58827(13) 0.0245(6) Uani 1 1 d . . . H34A H 0.8723 1.4551 0.6301 0.029 Uiso 1 1 calc R . . C35 C 0.85788(16) 1.46640(13) 0.52474(13) 0.0202(5) Uani 1 1 d . . . C36 C 0.77586(17) 1.51444(13) 0.52121(13) 0.0223(6) Uani 1 1 d . . . H36A H 0.7469 1.5282 0.5625 0.027 Uiso 1 1 calc R . . C37 C 0.73892(17) 1.54053(13) 0.46001(13) 0.0231(6) Uani 1 1 d . . . H37A H 0.6842 1.5721 0.4590 0.028 Uiso 1 1 calc R . . C38 C 0.78113(16) 1.52128(13) 0.39663(12) 0.0193(5) Uani 1 1 d . . . C39 C 0.74555(16) 1.55024(13) 0.33296(13) 0.0219(6) Uani 1 1 d . . . H39A H 0.6915 1.5825 0.3316 0.026 Uiso 1 1 calc R . . C40 C 0.78793(16) 1.53248(13) 0.27221(13) 0.0211(5) Uani 1 1 d . . . H40A H 0.7635 1.5531 0.2297 0.025 Uiso 1 1 calc R . . C41 C 0.86634(16) 1.48444(12) 0.27330(12) 0.0185(5) Uani 1 1 d . . . H41A H 0.8936 1.4711 0.2312 0.022 Uiso 1 1 calc R . . C42 C 0.90519(16) 1.45573(12) 0.33520(12) 0.0174(5) Uani 1 1 d . . . C43 C 0.86196(16) 1.47367(12) 0.39838(12) 0.0182(5) Uani 1 1 d . . . C44 C 0.90089(16) 1.44660(13) 0.46289(12) 0.0183(5) Uani 1 1 d . . . C45 C 1.14032(17) 1.36935(13) 0.15791(13) 0.0234(6) Uani 1 1 d . . . H45A H 1.1204 1.4162 0.1743 0.028 Uiso 1 1 calc R . . C46 C 1.15212(18) 1.36083(15) 0.08827(14) 0.0295(6) Uani 1 1 d . . . H46A H 1.1396 1.4013 0.0577 0.035 Uiso 1 1 calc R . . C47 C 1.18163(19) 1.29460(15) 0.06298(14) 0.0316(6) Uani 1 1 d . . . H47A H 1.1897 1.2881 0.0150 0.038 Uiso 1 1 calc R . . C48 C 1.19933(19) 1.23773(15) 0.10875(14) 0.0307(6) Uani 1 1 d . . . H48A H 1.2216 1.1913 0.0930 0.037 Uiso 1 1 calc R . . C49 C 1.18464(17) 1.24821(14) 0.17804(14) 0.0258(6) Uani 1 1 d . . . H49A H 1.1951 1.2077 0.2088 0.031 Uiso 1 1 calc R . . C50 C 1.4496(3) 1.2142(2) 0.0544(2) 0.0785(13) Uani 1 1 d . . . H50A H 1.4001 1.2066 0.0164 0.094 Uiso 1 1 calc R . . H50B H 1.5097 1.1896 0.0416 0.094 Uiso 1 1 calc R . . C51 C 1.4668(3) 1.2934(2) 0.0645(2) 0.0754(13) Uani 1 1 d . . . H51A H 1.4210 1.3230 0.0349 0.091 Uiso 1 1 calc R . . H51B H 1.5333 1.3066 0.0533 0.091 Uiso 1 1 calc R . . C52 C 1.4517(3) 1.30725(18) 0.13999(19) 0.0566(10) Uani 1 1 d . . . H52A H 1.5042 1.3379 0.1614 0.068 Uiso 1 1 calc R . . H52B H 1.3893 1.3321 0.1461 0.068 Uiso 1 1 calc R . . C53 C 1.4527(2) 1.23120(16) 0.16989(16) 0.0455(8) Uani 1 1 d . . . H53C H 1.5188 1.2171 0.1863 0.055 Uiso 1 1 calc R . . H53D H 1.4103 1.2286 0.2092 0.055 Uiso 1 1 calc R . . C56 C 0.9050(3) 1.2989(3) 0.1103(3) 0.0353(13) Uani 0.647(5) 1 d PD A 1 H56A H 0.9658 1.2727 0.1017 0.042 Uiso 0.647(5) 1 calc PR A 1 H56B H 0.9136 1.3522 0.1005 0.042 Uiso 0.647(5) 1 calc PR A 1 C54 C 0.82302(19) 1.26762(16) 0.06555(15) 0.0376(7) Uani 0.647(5) 1 d PD A 1 H54A H 0.7892 1.3078 0.0393 0.045 Uiso 0.647(5) 1 calc PR A 1 H54B H 0.8477 1.2317 0.0322 0.045 Uiso 0.647(5) 1 calc PR A 1 O6 O 0.8135(2) 1.22100(19) 0.17556(17) 0.0407(10) Uani 0.647(5) 1 d PD A 1 C55 C 0.7554(3) 1.2300(3) 0.1117(2) 0.0367(13) Uani 0.647(5) 1 d PD A 1 H55A H 0.6980 1.2610 0.1187 0.044 Uiso 0.647(5) 1 calc PR A 1 H55B H 0.7342 1.1814 0.0926 0.044 Uiso 0.647(5) 1 calc PR A 1 C57 C 0.8791(3) 1.28795(17) 0.18237(17) 0.0504(9) Uani 0.647(5) 1 d PD A 1 H57A H 0.8449 1.3315 0.1999 0.060 Uiso 0.647(5) 1 calc PR A 1 H57B H 0.9367 1.2777 0.2132 0.060 Uiso 0.647(5) 1 calc PR A 1 C56A C 0.8011(7) 1.2548(6) 0.1403(4) 0.058(4) Uani 0.353(5) 1 d PD A 2 H56C H 0.7389 1.2781 0.1504 0.070 Uiso 0.353(5) 1 calc PR A 2 H56D H 0.7969 1.2011 0.1499 0.070 Uiso 0.353(5) 1 calc PR A 2 C54A C 0.82302(19) 1.26762(16) 0.06555(15) 0.0376(7) Uani 0.353(5) 1 d PD A 2 H54C H 0.8487 1.2224 0.0444 0.045 Uiso 0.353(5) 1 calc PR A 2 H54D H 0.7653 1.2846 0.0378 0.045 Uiso 0.353(5) 1 calc PR A 2 C55A C 0.8987(6) 1.3279(5) 0.0727(4) 0.040(2) Uani 0.353(5) 1 d PD A 2 H55C H 0.9613 1.3078 0.0596 0.048 Uiso 0.353(5) 1 calc PR A 2 H55D H 0.8807 1.3688 0.0406 0.048 Uiso 0.353(5) 1 calc PR A 2 O6A O 0.9087(4) 1.3559(3) 0.1404(3) 0.0395(19) Uani 0.353(5) 1 d PD A 2 C57A C 0.8791(3) 1.28795(17) 0.18237(17) 0.0504(9) Uani 0.353(5) 1 d PD A 2 H57C H 0.9336 1.2530 0.1894 0.060 Uiso 0.353(5) 1 calc PR A 2 H57D H 0.8571 1.3031 0.2279 0.060 Uiso 0.353(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0131(3) 0.0179(4) 0.0220(4) 0.0009(3) -0.0004(3) 0.0009(3) O1 0.0143(8) 0.0182(9) 0.0245(10) 0.0001(7) -0.0004(7) -0.0005(7) O2 0.0142(8) 0.0185(9) 0.0271(10) 0.0032(7) -0.0018(7) 0.0005(7) O3 0.0171(8) 0.0183(8) 0.0187(9) -0.0005(7) 0.0008(7) 0.0015(7) O4 0.0151(8) 0.0231(9) 0.0203(9) 0.0016(7) -0.0006(7) 0.0020(7) O5 0.0444(12) 0.0401(12) 0.0395(13) 0.0028(10) 0.0020(10) -0.0113(10) N1 0.0149(10) 0.0177(10) 0.0201(11) -0.0002(8) 0.0010(8) -0.0001(8) N2 0.0160(10) 0.0174(10) 0.0239(12) 0.0003(9) -0.0007(8) -0.0001(8) C1 0.0157(12) 0.0212(12) 0.0165(13) -0.0004(10) -0.0009(10) -0.0005(10) C2 0.0171(12) 0.0207(12) 0.0149(12) -0.0023(10) -0.0001(10) 0.0020(10) C3 0.0181(12) 0.0199(12) 0.0189(13) -0.0014(10) 0.0005(10) -0.0019(10) C4 0.0159(12) 0.0237(13) 0.0211(14) 0.0004(10) -0.0006(10) -0.0054(10) C5 0.0178(12) 0.0224(13) 0.0254(14) -0.0017(11) -0.0006(10) -0.0013(10) C6 0.0186(12) 0.0202(13) 0.0227(14) 0.0027(10) -0.0022(10) 0.0014(10) C7 0.0178(12) 0.0206(13) 0.0241(14) 0.0022(11) -0.0002(10) -0.0025(10) C8 0.0214(13) 0.0235(14) 0.0340(16) 0.0056(12) 0.0012(11) -0.0035(11) C9 0.0324(15) 0.0292(15) 0.0270(15) 0.0055(12) -0.0049(12) -0.0053(12) C10 0.0297(14) 0.0215(14) 0.0370(17) 0.0001(12) 0.0095(12) 0.0017(11) C11 0.0144(12) 0.0300(15) 0.0400(17) 0.0039(12) -0.0020(11) -0.0008(11) C12 0.0179(14) 0.060(2) 0.058(2) 0.0047(17) 0.0048(14) 0.0084(14) C13 0.0177(14) 0.0318(17) 0.094(3) 0.0103(17) -0.0083(15) 0.0031(12) C14 0.0253(15) 0.0465(18) 0.0427(19) 0.0117(15) -0.0135(13) -0.0073(13) C15 0.0163(12) 0.0187(12) 0.0166(13) -0.0013(10) 0.0014(10) 0.0010(9) C16 0.0178(12) 0.0178(12) 0.0172(13) -0.0010(10) 0.0006(10) 0.0011(9) C17 0.0178(12) 0.0205(13) 0.0165(13) -0.0020(10) 0.0015(10) -0.0001(10) C18 0.0211(12) 0.0173(12) 0.0192(13) 0.0016(10) 0.0019(10) -0.0030(10) C19 0.0191(12) 0.0212(13) 0.0159(13) -0.0014(10) -0.0016(10) 0.0034(10) C20 0.0152(12) 0.0220(13) 0.0199(13) -0.0018(10) -0.0011(10) -0.0003(10) C21 0.0152(12) 0.0235(13) 0.0263(14) 0.0021(11) 0.0010(10) -0.0027(10) C22 0.0230(14) 0.0370(17) 0.053(2) -0.0086(14) 0.0119(13) -0.0004(12) C23 0.0184(13) 0.0308(15) 0.0343(16) 0.0068(12) -0.0042(11) -0.0014(11) C24 0.0231(14) 0.0316(15) 0.0378(17) 0.0089(13) 0.0032(12) -0.0080(11) C25 0.0229(13) 0.0212(13) 0.0238(14) 0.0042(11) -0.0050(11) 0.0011(10) C26 0.0413(17) 0.0220(15) 0.056(2) -0.0008(14) -0.0151(15) 0.0083(13) C27 0.0332(16) 0.0481(19) 0.0365(18) 0.0171(14) 0.0045(13) 0.0123(14) C28 0.0278(14) 0.0270(14) 0.0369(17) 0.0060(12) 0.0008(12) 0.0071(11) C29 0.0137(11) 0.0146(12) 0.0197(13) -0.0016(10) 0.0007(10) -0.0027(9) C30 0.0146(12) 0.0167(12) 0.0241(14) -0.0004(10) 0.0019(10) -0.0021(9) C31 0.0169(12) 0.0182(12) 0.0199(13) 0.0005(10) -0.0017(10) -0.0030(9) C32 0.0174(12) 0.0215(13) 0.0258(14) 0.0019(11) 0.0005(10) -0.0018(10) C33 0.0233(13) 0.0276(14) 0.0199(14) 0.0044(11) -0.0012(11) -0.0044(11) C34 0.0253(13) 0.0264(14) 0.0223(15) -0.0026(11) 0.0060(11) -0.0075(11) C35 0.0176(12) 0.0201(13) 0.0230(14) -0.0002(10) 0.0022(10) -0.0073(10) C36 0.0193(13) 0.0249(13) 0.0235(14) -0.0049(11) 0.0071(11) -0.0042(10) C37 0.0171(12) 0.0207(13) 0.0318(16) -0.0026(11) 0.0053(11) -0.0007(10) C38 0.0150(12) 0.0187(12) 0.0245(14) -0.0013(10) 0.0020(10) -0.0022(9) C39 0.0137(12) 0.0195(13) 0.0323(16) -0.0010(11) 0.0005(11) 0.0018(10) C40 0.0177(12) 0.0226(13) 0.0227(14) 0.0051(11) -0.0020(10) -0.0003(10) C41 0.0180(12) 0.0172(12) 0.0205(13) -0.0024(10) 0.0021(10) -0.0013(10) C42 0.0158(11) 0.0143(12) 0.0222(13) -0.0007(10) 0.0015(10) -0.0022(9) C43 0.0143(11) 0.0161(12) 0.0240(14) -0.0012(10) 0.0008(10) -0.0056(9) C44 0.0155(12) 0.0188(12) 0.0204(14) 0.0003(10) -0.0005(10) -0.0047(9) C45 0.0217(13) 0.0204(13) 0.0282(15) 0.0002(11) 0.0014(11) 0.0009(10) C46 0.0299(15) 0.0287(15) 0.0300(16) 0.0011(12) 0.0044(12) 0.0004(12) C47 0.0296(15) 0.0361(16) 0.0288(16) -0.0018(13) 0.0003(12) 0.0001(12) C48 0.0305(15) 0.0308(15) 0.0307(17) -0.0053(12) -0.0001(12) -0.0019(12) C49 0.0242(14) 0.0218(13) 0.0315(16) 0.0008(11) 0.0011(12) 0.0021(11) C50 0.115(4) 0.068(3) 0.057(3) -0.005(2) 0.046(2) -0.035(3) C51 0.098(3) 0.069(3) 0.057(3) 0.027(2) -0.016(2) -0.039(2) C52 0.057(2) 0.0367(19) 0.074(3) 0.0001(18) -0.0143(19) -0.0050(16) C53 0.052(2) 0.0426(19) 0.041(2) -0.0023(15) -0.0070(16) -0.0037(15) C56 0.026(2) 0.027(3) 0.054(4) -0.013(2) 0.007(2) -0.004(2) C54 0.0308(16) 0.0402(17) 0.0414(19) -0.0022(14) 0.0001(14) -0.0011(13) O6 0.0386(19) 0.044(2) 0.038(2) -0.0067(17) -0.0065(16) -0.0055(16) C55 0.028(3) 0.044(3) 0.037(3) -0.006(2) -0.006(2) -0.018(2) C57 0.060(2) 0.0417(19) 0.048(2) 0.0021(16) -0.0038(18) 0.0085(17) C56A 0.068(9) 0.034(6) 0.075(10) 0.037(6) 0.027(7) 0.021(6) C54A 0.0308(16) 0.0402(17) 0.0414(19) -0.0022(14) 0.0001(14) -0.0011(13) C55A 0.045(5) 0.037(6) 0.037(6) -0.003(4) -0.017(5) 0.008(4) O6A 0.037(3) 0.048(4) 0.034(4) 0.009(3) 0.006(3) 0.000(3) C57A 0.060(2) 0.0417(19) 0.048(2) 0.0021(16) -0.0038(18) 0.0085(17) _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 1.8637(17) . ? Al1 O1 1.8663(16) . ? Al1 O3 1.8928(16) . ? Al1 O4 1.9363(17) . ? Al1 N1 1.966(2) . ? Al1 N2 2.059(2) . ? O1 C2 1.328(3) . ? O2 C16 1.318(3) . ? O3 C29 1.300(3) . ? O4 C30 1.285(3) . ? O5 C50 1.403(4) . ? O5 C53 1.429(3) . ? N1 C1 1.359(3) . ? N1 C15 1.371(3) . ? N2 C45 1.354(3) . ? N2 C49 1.353(3) . ? C1 C6 1.410(3) . ? C1 C2 1.443(3) . ? C2 C3 1.425(3) . ? C3 C4 1.389(3) . ? C3 C7 1.535(3) . ? C4 C5 1.413(3) . ? C4 H4A 0.9500 . ? C5 C6 1.370(3) . ? C5 C11 1.539(3) . ? C6 H6A 0.9500 . ? C7 C8 1.531(3) . ? C7 C10 1.532(3) . ? C7 C9 1.537(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.525(4) . ? C11 C12 1.527(4) . ? C11 C13 1.537(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.408(3) . ? C15 C16 1.436(3) . ? C16 C17 1.422(3) . ? C17 C18 1.384(3) . ? C17 C21 1.534(3) . ? C18 C19 1.411(3) . ? C18 H18A 0.9500 . ? C19 C20 1.380(3) . ? C19 C25 1.539(3) . ? C20 H20A 0.9500 . ? C21 C24 1.518(3) . ? C21 C23 1.537(3) . ? C21 C22 1.539(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.517(3) . ? C25 C28 1.526(3) . ? C25 C26 1.540(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C42 1.432(3) . ? C29 C30 1.439(3) . ? C30 C31 1.441(3) . ? C31 C32 1.399(3) . ? C31 C44 1.423(3) . ? C32 C33 1.387(3) . ? C32 H32A 0.9500 . ? C33 C34 1.378(3) . ? C33 H33A 0.9500 . ? C34 C35 1.411(3) . ? C34 H34A 0.9500 . ? C35 C44 1.416(3) . ? C35 C36 1.432(3) . ? C36 C37 1.352(3) . ? C36 H36A 0.9500 . ? C37 C38 1.434(3) . ? C37 H37A 0.9500 . ? C38 C39 1.406(3) . ? C38 C43 1.414(3) . ? C39 C40 1.384(3) . ? C39 H39A 0.9500 . ? C40 C41 1.393(3) . ? C40 H40A 0.9500 . ? C41 C42 1.390(3) . ? C41 H41A 0.9500 . ? C42 C43 1.432(3) . ? C43 C44 1.423(3) . ? C45 C46 1.379(3) . ? C45 H45A 0.9500 . ? C46 C47 1.365(4) . ? C46 H46A 0.9500 . ? C47 C48 1.371(4) . ? C47 H47A 0.9500 . ? C48 C49 1.384(4) . ? C48 H48A 0.9500 . ? C49 H49A 0.9500 . ? C50 C51 1.462(5) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.512(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.491(4) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53C 0.9900 . ? C53 H53D 0.9900 . ? C56 C57 1.477(5) . ? C56 C54 1.505(5) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C54 C55 1.497(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? O6 C55 1.451(5) . ? O6 C57 1.516(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C56A H56C 0.9900 . ? C56A H56D 0.9900 . ? C55A O6A 1.407(8) . ? C55A H55C 0.9900 . ? C55A H55D 0.9900 . ? 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 O1 164.89(8) . . ? O2 Al1 O3 98.28(7) . . ? O1 Al1 O3 96.46(7) . . ? O2 Al1 O4 88.28(7) . . ? O1 Al1 O4 96.58(7) . . ? O3 Al1 O4 84.00(7) . . ? O2 Al1 N1 82.73(8) . . ? O1 Al1 N1 82.74(8) . . ? O3 Al1 N1 176.66(8) . . ? O4 Al1 N1 92.86(8) . . ? O2 Al1 N2 89.47(8) . . ? O1 Al1 N2 87.80(8) . . ? O3 Al1 N2 87.70(7) . . ? O4 Al1 N2 170.99(8) . . ? N1 Al1 N2 95.51(8) . . ? C2 O1 Al1 114.98(14) . . ? C16 O2 Al1 114.09(14) . . ? C29 O3 Al1 112.74(14) . . ? C30 O4 Al1 111.13(14) . . ? C50 O5 C53 105.9(2) . . ? C1 N1 C15 132.6(2) . . ? C1 N1 Al1 114.10(15) . . ? C15 N1 Al1 113.16(15) . . ? C45 N2 C49 116.4(2) . . ? C45 N2 Al1 120.79(16) . . ? C49 N2 Al1 122.68(17) . . ? N1 C1 C6 129.3(2) . . ? N1 C1 C2 110.75(19) . . ? C6 C1 C2 119.9(2) . . ? O1 C2 C3 123.3(2) . . ? O1 C2 C1 117.2(2) . . ? C3 C2 C1 119.6(2) . . ? C4 C3 C2 116.7(2) . . ? C4 C3 C7 122.0(2) . . ? C2 C3 C7 121.2(2) . . ? C3 C4 C5 124.5(2) . . ? C3 C4 H4A 117.8 . . ? C5 C4 H4A 117.8 . . ? C6 C5 C4 118.3(2) . . ? C6 C5 C11 122.9(2) . . ? C4 C5 C11 118.8(2) . . ? C5 C6 C1 120.9(2) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? C8 C7 C10 107.8(2) . . ? C8 C7 C3 111.64(19) . . ? C10 C7 C3 111.2(2) . . ? C8 C7 C9 107.9(2) . . ? C10 C7 C9 108.9(2) . . ? C3 C7 C9 109.29(19) . . ? 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 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 108.9(2) . . ? C14 C11 C13 108.0(2) . . ? C12 C11 C13 108.3(2) . . ? C14 C11 C5 109.3(2) . . ? C12 C11 C5 110.6(2) . . ? C13 C11 C5 111.6(2) . . ? 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 . . ? 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 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C20 129.7(2) . . ? N1 C15 C16 110.38(19) . . ? C20 C15 C16 120.0(2) . . ? O2 C16 C17 123.2(2) . . ? O2 C16 C15 117.6(2) . . ? C17 C16 C15 119.2(2) . . ? C18 C17 C16 117.4(2) . . ? C18 C17 C21 123.0(2) . . ? C16 C17 C21 119.6(2) . . ? C17 C18 C19 124.4(2) . . ? C17 C18 H18A 117.8 . . ? C19 C18 H18A 117.8 . . ? C20 C19 C18 117.7(2) . . ? C20 C19 C25 121.7(2) . . ? C18 C19 C25 120.6(2) . . ? C19 C20 C15 121.0(2) . . ? C19 C20 H20A 119.5 . . ? C15 C20 H20A 119.5 . . ? C24 C21 C17 111.6(2) . . ? C24 C21 C23 107.8(2) . . ? C17 C21 C23 110.70(19) . . ? C24 C21 C22 107.5(2) . . ? C17 C21 C22 109.8(2) . . ? C23 C21 C22 109.3(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C28 109.2(2) . . ? C27 C25 C19 110.2(2) . . ? C28 C25 C19 111.9(2) . . ? C27 C25 C26 109.4(2) . . ? C28 C25 C26 106.2(2) . . ? C19 C25 C26 109.8(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C42 123.8(2) . . ? O3 C29 C30 115.2(2) . . ? C42 C29 C30 121.0(2) . . ? O4 C30 C29 116.3(2) . . ? O4 C30 C31 124.1(2) . . ? C29 C30 C31 119.6(2) . . ? C32 C31 C44 119.9(2) . . ? C32 C31 C30 121.0(2) . . ? C44 C31 C30 119.1(2) . . ? C33 C32 C31 120.3(2) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C34 C33 C32 120.6(2) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 121.0(2) . . ? C33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C34 C35 C44 119.0(2) . . ? C34 C35 C36 121.9(2) . . ? C44 C35 C36 119.0(2) . . ? C37 C36 C35 121.1(2) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 121.0(2) . . ? C36 C37 H37A 119.5 . . ? C38 C37 H37A 119.5 . . ? C39 C38 C43 119.2(2) . . ? C39 C38 C37 121.5(2) . . ? C43 C38 C37 119.3(2) . . ? C40 C39 C38 121.1(2) . . ? C40 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C39 C40 C41 120.1(2) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C42 C41 C40 120.8(2) . . ? C42 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C41 C42 C43 119.6(2) . . ? C41 C42 C29 122.1(2) . . ? C43 C42 C29 118.2(2) . . ? C38 C43 C44 119.6(2) . . ? C38 C43 C42 119.2(2) . . ? C44 C43 C42 121.2(2) . . ? C35 C44 C43 120.1(2) . . ? C35 C44 C31 119.2(2) . . ? C43 C44 C31 120.7(2) . . ? N2 C45 C46 122.7(2) . . ? N2 C45 H45A 118.7 . . ? C46 C45 H45A 118.7 . . ? C47 C46 C45 120.3(3) . . ? C47 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C46 C47 C48 118.1(3) . . ? C46 C47 H47A 121.0 . . ? C48 C47 H47A 121.0 . . ? C47 C48 C49 119.7(3) . . ? C47 C48 H48A 120.1 . . ? C49 C48 H48A 120.1 . . ? N2 C49 C48 122.8(2) . . ? N2 C49 H49A 118.6 . . ? C48 C49 H49A 118.6 . . ? O5 C50 C51 109.5(3) . . ? O5 C50 H50A 109.8 . . ? C51 C50 H50A 109.8 . . ? O5 C50 H50B 109.8 . . ? C51 C50 H50B 109.8 . . ? H50A C50 H50B 108.2 . . ? C50 C51 C52 105.1(3) . . ? C50 C51 H51A 110.7 . . ? C52 C51 H51A 110.7 . . ? C50 C51 H51B 110.7 . . ? C52 C51 H51B 110.7 . . ? H51A C51 H51B 108.8 . . ? C53 C52 C51 103.1(3) . . ? C53 C52 H52A 111.1 . . ? C51 C52 H52A 111.1 . . ? C53 C52 H52B 111.1 . . ? C51 C52 H52B 111.1 . . ? H52A C52 H52B 109.1 . . ? O5 C53 C52 106.1(2) . . ? O5 C53 H53C 110.5 . . ? C52 C53 H53C 110.5 . . ? O5 C53 H53D 110.5 . . ? C52 C53 H53D 110.5 . . ? H53C C53 H53D 108.7 . . ? C57 C56 C54 106.2(3) . . ? C57 C56 H56A 110.5 . . ? C54 C56 H56A 110.5 . . ? C57 C56 H56B 110.5 . . ? C54 C56 H56B 110.5 . . ? H56A C56 H56B 108.7 . . ? C55 C54 C56 107.9(3) . . ? C55 C54 H54A 110.1 . . ? C56 C54 H54A 110.1 . . ? C55 C54 H54B 110.1 . . ? C56 C54 H54B 110.1 . . ? H54A C54 H54B 108.4 . . ? C55 O6 C57 106.8(3) . . ? O6 C55 C54 102.9(3) . . ? O6 C55 H55A 111.2 . . ? C54 C55 H55A 111.2 . . ? O6 C55 H55B 111.2 . . ? C54 C55 H55B 111.2 . . ? H55A C55 H55B 109.1 . . ? C56 C57 O6 101.6(3) . . ? C56 C57 H57A 111.4 . . ? O6 C57 H57A 111.4 . . ? C56 C57 H57B 111.4 . . ? O6 C57 H57B 111.4 . . ? H57A C57 H57B 109.3 . . ? H56C C56A H56D 108.6 . . ? O6A C55A H55C 109.2 . . ? O6A C55A H55D 109.2 . . ? H55C C55A H55D 107.9 . . ? 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 Al1 O1 C2 -11.7(4) . . . . ? O3 Al1 O1 C2 -178.95(15) . . . . ? O4 Al1 O1 C2 96.39(15) . . . . ? N1 Al1 O1 C2 4.32(15) . . . . ? N2 Al1 O1 C2 -91.51(15) . . . . ? O1 Al1 O2 C16 29.1(4) . . . . ? O3 Al1 O2 C16 -163.75(15) . . . . ? O4 Al1 O2 C16 -80.08(16) . . . . ? N1 Al1 O2 C16 13.03(16) . . . . ? N2 Al1 O2 C16 108.65(16) . . . . ? O2 Al1 O3 C29 81.52(15) . . . . ? O1 Al1 O3 C29 -101.82(15) . . . . ? O4 Al1 O3 C29 -5.85(14) . . . . ? N1 Al1 O3 C29 -25.9(15) . . . . ? N2 Al1 O3 C29 170.65(15) . . . . ? O2 Al1 O4 C30 -90.92(15) . . . . ? O1 Al1 O4 C30 103.43(15) . . . . ? O3 Al1 O4 C30 7.59(15) . . . . ? N1 Al1 O4 C30 -173.55(15) . . . . ? N2 Al1 O4 C30 -15.3(6) . . . . ? O2 Al1 N1 C1 173.71(17) . . . . ? O1 Al1 N1 C1 -2.12(16) . . . . ? O3 Al1 N1 C1 -78.5(14) . . . . ? O4 Al1 N1 C1 -98.39(16) . . . . ? N2 Al1 N1 C1 84.95(16) . . . . ? O2 Al1 N1 C15 -9.43(16) . . . . ? O1 Al1 N1 C15 174.74(16) . . . . ? O3 Al1 N1 C15 98.4(14) . . . . ? O4 Al1 N1 C15 78.47(16) . . . . ? N2 Al1 N1 C15 -98.19(16) . . . . ? O2 Al1 N2 C45 138.15(17) . . . . ? O1 Al1 N2 C45 -56.72(17) . . . . ? O3 Al1 N2 C45 39.84(18) . . . . ? O4 Al1 N2 C45 62.6(6) . . . . ? N1 Al1 N2 C45 -139.21(17) . . . . ? O2 Al1 N2 C49 -46.17(19) . . . . ? O1 Al1 N2 C49 118.96(18) . . . . ? O3 Al1 N2 C49 -144.48(18) . . . . ? O4 Al1 N2 C49 -121.7(5) . . . . ? N1 Al1 N2 C49 36.48(19) . . . . ? C15 N1 C1 C6 5.9(4) . . . . ? Al1 N1 C1 C6 -178.0(2) . . . . ? C15 N1 C1 C2 -176.4(2) . . . . ? Al1 N1 C1 C2 -0.3(2) . . . . ? Al1 O1 C2 C3 173.23(18) . . . . ? Al1 O1 C2 C1 -5.9(3) . . . . ? N1 C1 C2 O1 3.9(3) . . . . ? C6 C1 C2 O1 -178.1(2) . . . . ? N1 C1 C2 C3 -175.2(2) . . . . ? C6 C1 C2 C3 2.8(3) . . . . ? O1 C2 C3 C4 176.5(2) . . . . ? C1 C2 C3 C4 -4.5(3) . . . . ? O1 C2 C3 C7 -5.9(3) . . . . ? C1 C2 C3 C7 173.1(2) . . . . ? C2 C3 C4 C5 3.3(4) . . . . ? C7 C3 C4 C5 -174.3(2) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C3 C4 C5 C11 179.5(2) . . . . ? C4 C5 C6 C1 -1.9(4) . . . . ? C11 C5 C6 C1 178.6(2) . . . . ? N1 C1 C6 C5 178.0(2) . . . . ? C2 C1 C6 C5 0.5(4) . . . . ? C4 C3 C7 C8 -1.9(3) . . . . ? C2 C3 C7 C8 -179.3(2) . . . . ? C4 C3 C7 C10 -122.3(2) . . . . ? C2 C3 C7 C10 60.2(3) . . . . ? C4 C3 C7 C9 117.4(2) . . . . ? C2 C3 C7 C9 -60.0(3) . . . . ? C6 C5 C11 C14 -113.5(3) . . . . ? C4 C5 C11 C14 67.0(3) . . . . ? C6 C5 C11 C12 126.5(3) . . . . ? C4 C5 C11 C12 -53.0(3) . . . . ? C6 C5 C11 C13 5.9(4) . . . . ? C4 C5 C11 C13 -173.6(2) . . . . ? C1 N1 C15 C20 1.0(4) . . . . ? Al1 N1 C15 C20 -175.1(2) . . . . ? C1 N1 C15 C16 -179.7(2) . . . . ? Al1 N1 C15 C16 4.2(2) . . . . ? Al1 O2 C16 C17 164.96(18) . . . . ? Al1 O2 C16 C15 -14.7(3) . . . . ? N1 C15 C16 O2 6.6(3) . . . . ? C20 C15 C16 O2 -174.1(2) . . . . ? N1 C15 C16 C17 -173.1(2) . . . . ? C20 C15 C16 C17 6.2(3) . . . . ? O2 C16 C17 C18 174.6(2) . . . . ? C15 C16 C17 C18 -5.7(3) . . . . ? O2 C16 C17 C21 -5.9(3) . . . . ? C15 C16 C17 C21 173.8(2) . . . . ? C16 C17 C18 C19 0.7(4) . . . . ? C21 C17 C18 C19 -178.8(2) . . . . ? C17 C18 C19 C20 3.9(4) . . . . ? C17 C18 C19 C25 -174.6(2) . . . . ? C18 C19 C20 C15 -3.3(3) . . . . ? C25 C19 C20 C15 175.2(2) . . . . ? N1 C15 C20 C19 177.6(2) . . . . ? C16 C15 C20 C19 -1.6(3) . . . . ? C18 C17 C21 C24 5.5(3) . . . . ? C16 C17 C21 C24 -173.9(2) . . . . ? C18 C17 C21 C23 -114.6(2) . . . . ? C16 C17 C21 C23 66.0(3) . . . . ? C18 C17 C21 C22 124.6(3) . . . . ? C16 C17 C21 C22 -54.9(3) . . . . ? C20 C19 C25 C27 116.8(3) . . . . ? C18 C19 C25 C27 -64.8(3) . . . . ? C20 C19 C25 C28 -5.0(3) . . . . ? C18 C19 C25 C28 173.5(2) . . . . ? C20 C19 C25 C26 -122.7(3) . . . . ? C18 C19 C25 C26 55.8(3) . . . . ? Al1 O3 C29 C42 -178.94(17) . . . . ? Al1 O3 C29 C30 3.2(2) . . . . ? Al1 O4 C30 C29 -7.9(2) . . . . ? Al1 O4 C30 C31 172.57(18) . . . . ? O3 C29 C30 O4 3.3(3) . . . . ? C42 C29 C30 O4 -174.6(2) . . . . ? O3 C29 C30 C31 -177.10(19) . . . . ? C42 C29 C30 C31 5.0(3) . . . . ? O4 C30 C31 C32 -2.5(3) . . . . ? C29 C30 C31 C32 177.9(2) . . . . ? O4 C30 C31 C44 174.3(2) . . . . ? C29 C30 C31 C44 -5.2(3) . . . . ? C44 C31 C32 C33 -0.8(3) . . . . ? C30 C31 C32 C33 176.0(2) . . . . ? C31 C32 C33 C34 -1.2(4) . . . . ? C32 C33 C34 C35 2.5(4) . . . . ? C33 C34 C35 C44 -1.6(3) . . . . ? C33 C34 C35 C36 -178.7(2) . . . . ? C34 C35 C36 C37 177.4(2) . . . . ? C44 C35 C36 C37 0.4(3) . . . . ? C35 C36 C37 C38 -0.4(4) . . . . ? C36 C37 C38 C39 -177.6(2) . . . . ? C36 C37 C38 C43 0.7(3) . . . . ? C43 C38 C39 C40 0.4(3) . . . . ? C37 C38 C39 C40 178.7(2) . . . . ? C38 C39 C40 C41 0.9(3) . . . . ? C39 C40 C41 C42 -2.2(3) . . . . ? C40 C41 C42 C43 2.2(3) . . . . ? C40 C41 C42 C29 -174.7(2) . . . . ? O3 C29 C42 C41 -2.3(3) . . . . ? C30 C29 C42 C41 175.4(2) . . . . ? O3 C29 C42 C43 -179.3(2) . . . . ? C30 C29 C42 C43 -1.6(3) . . . . ? C39 C38 C43 C44 177.4(2) . . . . ? C37 C38 C43 C44 -0.9(3) . . . . ? C39 C38 C43 C42 -0.4(3) . . . . ? C37 C38 C43 C42 -178.7(2) . . . . ? C41 C42 C43 C38 -0.9(3) . . . . ? C29 C42 C43 C38 176.2(2) . . . . ? C41 C42 C43 C44 -178.7(2) . . . . ? C29 C42 C43 C44 -1.6(3) . . . . ? C34 C35 C44 C43 -177.8(2) . . . . ? C36 C35 C44 C43 -0.7(3) . . . . ? C34 C35 C44 C31 -0.4(3) . . . . ? C36 C35 C44 C31 176.7(2) . . . . ? C38 C43 C44 C35 1.0(3) . . . . ? C42 C43 C44 C35 178.7(2) . . . . ? C38 C43 C44 C31 -176.4(2) . . . . ? C42 C43 C44 C31 1.4(3) . . . . ? C32 C31 C44 C35 1.6(3) . . . . ? C30 C31 C44 C35 -175.3(2) . . . . ? C32 C31 C44 C43 179.0(2) . . . . ? C30 C31 C44 C43 2.1(3) . . . . ? C49 N2 C45 C46 0.3(3) . . . . ? Al1 N2 C45 C46 176.26(18) . . . . ? N2 C45 C46 C47 -0.7(4) . . . . ? C45 C46 C47 C48 -0.3(4) . . . . ? C46 C47 C48 C49 1.7(4) . . . . ? C45 N2 C49 C48 1.1(3) . . . . ? Al1 N2 C49 C48 -174.75(19) . . . . ? C47 C48 C49 N2 -2.1(4) . . . . ? C53 O5 C50 C51 -23.6(4) . . . . ? O5 C50 C51 C52 5.0(5) . . . . ? C50 C51 C52 C53 14.5(4) . . . . ? C50 O5 C53 C52 32.9(4) . . . . ? C51 C52 C53 O5 -28.9(3) . . . . ? C57 C56 C54 C55 -7.0(5) . . . . ? C57 O6 C55 C54 34.4(4) . . . . ? C56 C54 C55 O6 -16.9(4) . . . . ? C54 C56 C57 O6 26.8(4) . . . . ? C55 O6 C57 C56 -39.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.349 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.056 #===END #===END data_afh279-2 _database_code_depnum_ccdc_archive 'CCDC 867896' #TrackingRef '- Al(ONO) combined.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (ONOq)AlCl(Ph2acac) _chemical_melting_point 'not measured' _chemical_formula_moiety 'C43 H51 Al Cl N O4, C6 H6' _chemical_formula_sum 'C49 H57 Al Cl N O4' _chemical_formula_weight 786.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7048(3) _cell_length_b 19.0132(6) _cell_length_c 24.0765(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.92 _cell_angle_gamma 90.00 _cell_volume 4418.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.03 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9459 _exptl_absorpt_correction_T_max 0.9719 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 39390 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.04 _reflns_number_total 10496 _reflns_number_gt 8813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0444P)^2^+1.7242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10496 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.74163(4) 0.272632(18) -0.042382(15) 0.01364(8) Uani 1 1 d . . . Cl1 Cl 0.86904(3) 0.197846(15) 0.016601(12) 0.01757(7) Uani 1 1 d . . . N1 N 0.64318(10) 0.18720(5) -0.07711(4) 0.01334(19) Uani 1 1 d . . . O1 O 0.59000(9) 0.26836(4) 0.00202(3) 0.01549(17) Uani 1 1 d . . . O2 O 0.85411(9) 0.25688(4) -0.10048(4) 0.01571(17) Uani 1 1 d . . . O3 O 0.82636(9) 0.34874(4) -0.00741(4) 0.01581(17) Uani 1 1 d . . . O4 O 0.63010(9) 0.33354(4) -0.09135(4) 0.01637(17) Uani 1 1 d . . . C1 C 0.52916(12) 0.16924(6) -0.05385(5) 0.0135(2) Uani 1 1 d . . . C2 C 0.50446(12) 0.21803(6) -0.00876(5) 0.0136(2) Uani 1 1 d . . . C3 C 0.38634(12) 0.20708(6) 0.02224(5) 0.0144(2) Uani 1 1 d . . . C4 C 0.30714(12) 0.14898(6) 0.00849(5) 0.0152(2) Uani 1 1 d . . . H4A H 0.2302 0.1406 0.0290 0.018 Uiso 1 1 calc R . . C5 C 0.33161(12) 0.09932(6) -0.03493(5) 0.0143(2) Uani 1 1 d . . . C6 C 0.43816(12) 0.11115(6) -0.06601(5) 0.0147(2) Uani 1 1 d . . . H6A H 0.4523 0.0805 -0.0961 0.018 Uiso 1 1 calc R . . C7 C 0.35470(13) 0.25964(7) 0.06723(5) 0.0188(3) Uani 1 1 d . . . C8 C 0.32844(15) 0.33237(7) 0.03998(7) 0.0272(3) Uani 1 1 d . . . H8A H 0.3098 0.3667 0.0686 0.041 Uiso 1 1 calc R . . H8B H 0.2484 0.3297 0.0117 0.041 Uiso 1 1 calc R . . H8C H 0.4104 0.3470 0.0223 0.041 Uiso 1 1 calc R . . C9 C 0.47670(15) 0.26374(9) 0.11332(6) 0.0288(3) Uani 1 1 d . . . H9A H 0.4553 0.2979 0.1417 0.043 Uiso 1 1 calc R . . H9B H 0.5605 0.2785 0.0970 0.043 Uiso 1 1 calc R . . H9C H 0.4920 0.2174 0.1307 0.043 Uiso 1 1 calc R . . C10 C 0.22461(14) 0.23906(8) 0.09463(6) 0.0255(3) Uani 1 1 d . . . H10A H 0.2083 0.2736 0.1234 0.038 Uiso 1 1 calc R . . H10B H 0.2378 0.1924 0.1117 0.038 Uiso 1 1 calc R . . H10C H 0.1446 0.2379 0.0662 0.038 Uiso 1 1 calc R . . C11 C 0.24032(12) 0.03377(6) -0.04195(5) 0.0161(2) Uani 1 1 d . . . C12 C 0.26185(13) -0.00790(7) 0.01309(6) 0.0211(3) Uani 1 1 d . . . H12A H 0.2378 0.0218 0.0439 0.032 Uiso 1 1 calc R . . H12B H 0.3590 -0.0223 0.0200 0.032 Uiso 1 1 calc R . . H12C H 0.2024 -0.0497 0.0104 0.032 Uiso 1 1 calc R . . C13 C 0.08677(13) 0.05454(7) -0.05373(6) 0.0204(3) Uani 1 1 d . . . H13A H 0.0730 0.0810 -0.0888 0.031 Uiso 1 1 calc R . . H13B H 0.0601 0.0838 -0.0231 0.031 Uiso 1 1 calc R . . H13C H 0.0294 0.0120 -0.0568 0.031 Uiso 1 1 calc R . . C14 C 0.27873(15) -0.01383(7) -0.08917(6) 0.0275(3) Uani 1 1 d . . . H14A H 0.2655 0.0118 -0.1246 0.041 Uiso 1 1 calc R . . H14B H 0.2194 -0.0557 -0.0914 0.041 Uiso 1 1 calc R . . H14C H 0.3759 -0.0282 -0.0818 0.041 Uiso 1 1 calc R . . C15 C 0.71535(12) 0.15556(6) -0.11500(5) 0.0135(2) Uani 1 1 d . . . C16 C 0.83249(12) 0.19871(6) -0.12714(5) 0.0139(2) Uani 1 1 d . . . C17 C 0.91928(12) 0.17453(6) -0.16837(5) 0.0146(2) Uani 1 1 d . . . C18 C 0.89105(13) 0.10914(6) -0.19077(5) 0.0157(2) Uani 1 1 d . . . H18A H 0.9483 0.0925 -0.2177 0.019 Uiso 1 1 calc R . . C19 C 0.78128(12) 0.06393(6) -0.17656(5) 0.0150(2) Uani 1 1 d . . . C20 C 0.69454(12) 0.08796(6) -0.13987(5) 0.0145(2) Uani 1 1 d . . . H20A H 0.6196 0.0595 -0.1308 0.017 Uiso 1 1 calc R . . C21 C 1.03744(13) 0.22095(6) -0.18488(5) 0.0172(2) Uani 1 1 d . . . C22 C 0.97485(15) 0.28982(7) -0.21008(6) 0.0233(3) Uani 1 1 d . . . H22A H 0.9081 0.2789 -0.2423 0.035 Uiso 1 1 calc R . . H22B H 1.0489 0.3195 -0.2221 0.035 Uiso 1 1 calc R . . H22C H 0.9277 0.3149 -0.1819 0.035 Uiso 1 1 calc R . . C23 C 1.11690(15) 0.18542(7) -0.22915(6) 0.0247(3) Uani 1 1 d . . . H23A H 1.0527 0.1745 -0.2621 0.037 Uiso 1 1 calc R . . H23B H 1.1595 0.1419 -0.2138 0.037 Uiso 1 1 calc R . . H23C H 1.1892 0.2172 -0.2397 0.037 Uiso 1 1 calc R . . C24 C 1.14151(13) 0.23641(7) -0.13360(6) 0.0213(3) Uani 1 1 d . . . H24A H 1.2159 0.2666 -0.1447 0.032 Uiso 1 1 calc R . . H24B H 1.1810 0.1921 -0.1185 0.032 Uiso 1 1 calc R . . H24C H 1.0939 0.2604 -0.1050 0.032 Uiso 1 1 calc R . . C25 C 0.77003(13) -0.01062(6) -0.20100(5) 0.0183(2) Uani 1 1 d . . . C26 C 0.76765(16) -0.00800(8) -0.26487(6) 0.0276(3) Uani 1 1 d . . . H26A H 0.8532 0.0139 -0.2748 0.041 Uiso 1 1 calc R . . H26B H 0.6878 0.0197 -0.2806 0.041 Uiso 1 1 calc R . . H26C H 0.7604 -0.0559 -0.2799 0.041 Uiso 1 1 calc R . . C27 C 0.89654(15) -0.05309(7) -0.17622(6) 0.0270(3) Uani 1 1 d . . . H27A H 0.8974 -0.0552 -0.1355 0.040 Uiso 1 1 calc R . . H27B H 0.9815 -0.0303 -0.1858 0.040 Uiso 1 1 calc R . . H27C H 0.8914 -0.1009 -0.1915 0.040 Uiso 1 1 calc R . . C28 C 0.63880(14) -0.04847(7) -0.18680(6) 0.0245(3) Uani 1 1 d . . . H28A H 0.6399 -0.0522 -0.1462 0.037 Uiso 1 1 calc R . . H28B H 0.6355 -0.0957 -0.2032 0.037 Uiso 1 1 calc R . . H28C H 0.5571 -0.0218 -0.2019 0.037 Uiso 1 1 calc R . . C29 C 0.77709(12) 0.41114(6) -0.00274(5) 0.0149(2) Uani 1 1 d . . . C30 C 0.65917(13) 0.43525(6) -0.03506(5) 0.0174(2) Uani 1 1 d . . . H30A H 0.6187 0.4785 -0.0256 0.021 Uiso 1 1 calc R . . C31 C 0.59877(12) 0.39736(6) -0.08110(5) 0.0156(2) Uani 1 1 d . . . C32 C 0.49654(12) 0.43186(6) -0.12316(5) 0.0170(2) Uani 1 1 d . . . C33 C 0.42154(14) 0.39020(7) -0.16338(6) 0.0218(3) Uani 1 1 d . . . H33A H 0.4343 0.3407 -0.1629 0.026 Uiso 1 1 calc R . . C34 C 0.32861(15) 0.42043(8) -0.20407(6) 0.0268(3) Uani 1 1 d . . . H34A H 0.2781 0.3916 -0.2312 0.032 Uiso 1 1 calc R . . C35 C 0.30923(15) 0.49276(8) -0.20518(6) 0.0278(3) Uani 1 1 d . . . H35A H 0.2458 0.5134 -0.2332 0.033 Uiso 1 1 calc R . . C36 C 0.38240(14) 0.53486(7) -0.16539(6) 0.0251(3) Uani 1 1 d . . . H36A H 0.3687 0.5843 -0.1660 0.030 Uiso 1 1 calc R . . C37 C 0.47570(13) 0.50472(7) -0.12467(6) 0.0206(3) Uani 1 1 d . . . H37A H 0.5259 0.5338 -0.0976 0.025 Uiso 1 1 calc R . . C38 C 0.86031(13) 0.45791(6) 0.03730(5) 0.0153(2) Uani 1 1 d . . . C39 C 0.99219(13) 0.43598(6) 0.05871(5) 0.0172(2) Uani 1 1 d . . . H39A H 1.0247 0.3908 0.0493 0.021 Uiso 1 1 calc R . . C40 C 1.07635(14) 0.47971(7) 0.09376(5) 0.0201(3) Uani 1 1 d . . . H40A H 1.1663 0.4645 0.1081 0.024 Uiso 1 1 calc R . . C41 C 1.02919(14) 0.54566(7) 0.10781(5) 0.0217(3) Uani 1 1 d . . . H41A H 1.0874 0.5759 0.1312 0.026 Uiso 1 1 calc R . . C42 C 0.89703(15) 0.56733(7) 0.08761(5) 0.0230(3) Uani 1 1 d . . . H42A H 0.8641 0.6120 0.0979 0.028 Uiso 1 1 calc R . . C43 C 0.81271(14) 0.52403(6) 0.05239(5) 0.0197(3) Uani 1 1 d . . . H43A H 0.7225 0.5393 0.0385 0.024 Uiso 1 1 calc R . . C48 C 0.88840(14) 0.30200(8) 0.14938(6) 0.0251(3) Uani 1 1 d . . . H48A H 0.8476 0.3079 0.1121 0.030 Uiso 1 1 calc R . . C49 C 0.92127(15) 0.36005(8) 0.18266(6) 0.0264(3) Uani 1 1 d . . . H49A H 0.9034 0.4060 0.1681 0.032 Uiso 1 1 calc R . . C47 C 0.91542(17) 0.23510(8) 0.17077(6) 0.0307(3) Uani 1 1 d . . . H47A H 0.8931 0.1949 0.1482 0.037 Uiso 1 1 calc R . . C45 C 1.00706(17) 0.28512(9) 0.25827(6) 0.0356(4) Uani 1 1 d . . . H45A H 1.0476 0.2793 0.2956 0.043 Uiso 1 1 calc R . . C46 C 0.97506(18) 0.22715(8) 0.22513(6) 0.0351(4) Uani 1 1 d . . . H46A H 0.9941 0.1813 0.2397 0.042 Uiso 1 1 calc R . . C44 C 0.97999(16) 0.35169(8) 0.23701(6) 0.0322(3) Uani 1 1 d . . . H44A H 1.0018 0.3918 0.2598 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.01459(17) 0.00980(16) 0.01689(17) -0.00241(13) 0.00331(13) -0.00152(13) Cl1 0.01916(15) 0.01314(14) 0.01988(14) -0.00164(10) -0.00060(11) 0.00048(10) N1 0.0144(5) 0.0107(5) 0.0149(5) -0.0003(4) 0.0015(4) 0.0005(4) O1 0.0162(4) 0.0118(4) 0.0188(4) -0.0028(3) 0.0031(3) -0.0018(3) O2 0.0173(4) 0.0116(4) 0.0188(4) -0.0025(3) 0.0046(3) -0.0024(3) O3 0.0169(4) 0.0100(4) 0.0208(4) -0.0025(3) 0.0029(3) -0.0008(3) O4 0.0179(4) 0.0117(4) 0.0197(4) -0.0014(3) 0.0023(3) -0.0007(3) C1 0.0131(5) 0.0114(5) 0.0159(5) 0.0003(4) 0.0009(4) 0.0010(4) C2 0.0138(5) 0.0102(5) 0.0165(5) 0.0009(4) 0.0004(4) 0.0006(4) C3 0.0148(6) 0.0131(5) 0.0152(5) -0.0005(4) 0.0008(4) 0.0011(4) C4 0.0139(6) 0.0147(6) 0.0173(6) 0.0009(4) 0.0031(4) 0.0003(4) C5 0.0136(5) 0.0117(5) 0.0172(5) 0.0001(4) -0.0001(4) -0.0004(4) C6 0.0156(6) 0.0110(5) 0.0175(6) -0.0010(4) 0.0012(4) 0.0001(4) C7 0.0173(6) 0.0189(6) 0.0211(6) -0.0069(5) 0.0062(5) -0.0029(5) C8 0.0261(7) 0.0165(6) 0.0410(8) -0.0063(6) 0.0130(6) 0.0015(5) C9 0.0248(7) 0.0415(9) 0.0206(7) -0.0108(6) 0.0044(5) -0.0072(6) C10 0.0235(7) 0.0269(7) 0.0279(7) -0.0106(6) 0.0121(6) -0.0056(5) C11 0.0147(6) 0.0126(5) 0.0210(6) -0.0019(4) 0.0026(5) -0.0028(4) C12 0.0187(6) 0.0141(6) 0.0300(7) 0.0053(5) 0.0000(5) -0.0013(5) C13 0.0153(6) 0.0201(6) 0.0253(6) 0.0019(5) -0.0006(5) -0.0034(5) C14 0.0268(7) 0.0213(7) 0.0362(8) -0.0124(6) 0.0116(6) -0.0106(5) C15 0.0149(6) 0.0117(5) 0.0140(5) -0.0001(4) 0.0010(4) 0.0004(4) C16 0.0155(6) 0.0110(5) 0.0150(5) 0.0014(4) 0.0000(4) 0.0005(4) C17 0.0151(6) 0.0137(6) 0.0151(5) 0.0018(4) 0.0017(4) 0.0006(4) C18 0.0172(6) 0.0157(6) 0.0144(5) 0.0000(4) 0.0033(4) 0.0017(4) C19 0.0172(6) 0.0130(5) 0.0145(5) -0.0015(4) -0.0001(4) 0.0002(4) C20 0.0149(6) 0.0122(5) 0.0163(5) -0.0008(4) 0.0012(4) -0.0018(4) C21 0.0190(6) 0.0134(6) 0.0201(6) 0.0007(4) 0.0067(5) -0.0010(4) C22 0.0283(7) 0.0165(6) 0.0260(7) 0.0057(5) 0.0079(5) 0.0003(5) C23 0.0268(7) 0.0212(7) 0.0286(7) -0.0021(5) 0.0144(6) -0.0029(5) C24 0.0179(6) 0.0177(6) 0.0283(7) -0.0003(5) 0.0031(5) -0.0032(5) C25 0.0211(6) 0.0141(6) 0.0202(6) -0.0060(5) 0.0039(5) -0.0015(5) C26 0.0345(8) 0.0272(7) 0.0217(7) -0.0100(5) 0.0061(6) -0.0060(6) C27 0.0264(7) 0.0165(6) 0.0378(8) -0.0069(6) 0.0021(6) 0.0038(5) C28 0.0260(7) 0.0167(6) 0.0318(7) -0.0086(5) 0.0075(6) -0.0049(5) C29 0.0179(6) 0.0113(5) 0.0166(5) -0.0011(4) 0.0071(5) -0.0029(4) C30 0.0191(6) 0.0118(5) 0.0218(6) -0.0020(4) 0.0051(5) 0.0009(4) C31 0.0143(6) 0.0140(6) 0.0195(6) 0.0015(4) 0.0064(5) -0.0015(4) C32 0.0150(6) 0.0168(6) 0.0198(6) 0.0023(5) 0.0052(5) -0.0007(4) C33 0.0224(7) 0.0178(6) 0.0252(7) 0.0016(5) 0.0025(5) -0.0013(5) C34 0.0253(7) 0.0271(7) 0.0271(7) 0.0006(6) -0.0029(6) -0.0033(6) C35 0.0238(7) 0.0299(7) 0.0289(7) 0.0089(6) -0.0011(6) 0.0024(6) C36 0.0239(7) 0.0192(6) 0.0322(7) 0.0072(5) 0.0034(6) 0.0021(5) C37 0.0203(6) 0.0174(6) 0.0245(6) 0.0013(5) 0.0036(5) -0.0017(5) C38 0.0199(6) 0.0120(5) 0.0149(5) -0.0010(4) 0.0066(5) -0.0035(4) C39 0.0218(6) 0.0132(6) 0.0174(6) -0.0006(4) 0.0051(5) -0.0021(5) C40 0.0213(6) 0.0200(6) 0.0190(6) -0.0010(5) 0.0021(5) -0.0035(5) C41 0.0297(7) 0.0181(6) 0.0174(6) -0.0039(5) 0.0028(5) -0.0077(5) C42 0.0331(7) 0.0139(6) 0.0226(6) -0.0051(5) 0.0059(5) -0.0008(5) C43 0.0243(7) 0.0153(6) 0.0200(6) -0.0017(5) 0.0044(5) 0.0002(5) C48 0.0247(7) 0.0310(7) 0.0200(6) -0.0001(5) 0.0042(5) -0.0001(6) C49 0.0260(7) 0.0240(7) 0.0305(7) 0.0023(6) 0.0095(6) -0.0017(5) C47 0.0429(9) 0.0241(7) 0.0272(7) -0.0057(6) 0.0133(6) -0.0017(6) C45 0.0335(8) 0.0476(10) 0.0247(7) -0.0004(7) -0.0015(6) 0.0058(7) C46 0.0499(10) 0.0283(8) 0.0292(8) 0.0066(6) 0.0144(7) 0.0148(7) C44 0.0307(8) 0.0335(8) 0.0325(8) -0.0078(6) 0.0038(6) -0.0099(6) _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 O3 1.8264(9) . ? Al1 O2 1.8848(9) . ? Al1 O4 1.9077(9) . ? Al1 O1 1.9078(9) . ? Al1 N1 2.0214(10) . ? Al1 Cl1 2.2815(5) . ? N1 C1 1.3352(15) . ? N1 C15 1.3477(15) . ? O1 C2 1.2758(14) . ? O2 C16 1.2852(14) . ? O3 C29 1.2885(14) . ? O4 C31 1.2811(15) . ? C1 C6 1.4255(16) . ? C1 C2 1.4663(16) . ? C2 C3 1.4461(17) . ? C3 C4 1.3668(16) . ? C3 C7 1.5280(16) . ? C4 C5 1.4464(16) . ? C4 H4A 0.9500 . ? C5 C6 1.3562(17) . ? C5 C11 1.5284(16) . ? C6 H6A 0.9500 . ? C7 C10 1.5343(18) . ? C7 C9 1.5389(18) . ? C7 C8 1.5404(19) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.5291(18) . ? C11 C13 1.5395(17) . ? C11 C12 1.5395(17) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C20 1.4235(16) . ? C15 C16 1.4557(16) . ? C16 C17 1.4420(17) . ? C17 C18 1.3715(17) . ? C17 C21 1.5317(16) . ? C18 C19 1.4373(17) . ? C18 H18A 0.9500 . ? C19 C20 1.3605(17) . ? C19 C25 1.5343(16) . ? C20 H20A 0.9500 . ? C21 C23 1.5352(18) . ? C21 C24 1.5406(17) . ? C21 C22 1.5413(17) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C28 1.5318(18) . ? C25 C26 1.5363(18) . ? C25 C27 1.5376(18) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.3933(17) . ? C29 C38 1.4872(16) . ? C30 C31 1.3991(17) . ? C30 H30A 0.9500 . ? C31 C32 1.4942(17) . ? C32 C33 1.3963(18) . ? C32 C37 1.3998(18) . ? C33 C34 1.3860(19) . ? C33 H33A 0.9500 . ? C34 C35 1.388(2) . ? C34 H34A 0.9500 . ? C35 C36 1.386(2) . ? C35 H35A 0.9500 . ? C36 C37 1.3879(18) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 C39 1.3934(18) . ? C38 C43 1.4000(17) . ? C39 C40 1.3886(17) . ? C39 H39A 0.9500 . ? C40 C41 1.3886(18) . ? C40 H40A 0.9500 . ? C41 C42 1.387(2) . ? C41 H41A 0.9500 . ? C42 C43 1.3869(18) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C48 C49 1.382(2) . ? C48 C47 1.387(2) . ? C48 H48A 0.9500 . ? C49 C44 1.382(2) . ? C49 H49A 0.9500 . ? C47 C46 1.384(2) . ? C47 H47A 0.9500 . ? C45 C46 1.377(2) . ? C45 C44 1.380(2) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C44 H44A 0.9500 . ? 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 O3 Al1 O2 101.55(4) . . ? O3 Al1 O4 90.21(4) . . ? O2 Al1 O4 88.45(4) . . ? O3 Al1 O1 96.43(4) . . ? O2 Al1 O1 161.50(4) . . ? O4 Al1 O1 87.18(4) . . ? O3 Al1 N1 176.82(4) . . ? O2 Al1 N1 81.40(4) . . ? O4 Al1 N1 91.05(4) . . ? O1 Al1 N1 80.71(4) . . ? O3 Al1 Cl1 91.00(3) . . ? O2 Al1 Cl1 92.56(3) . . ? O4 Al1 Cl1 178.23(3) . . ? O1 Al1 Cl1 91.41(3) . . ? N1 Al1 Cl1 87.67(3) . . ? C1 N1 C15 132.92(10) . . ? C1 N1 Al1 114.13(8) . . ? C15 N1 Al1 112.47(8) . . ? C2 O1 Al1 116.18(8) . . ? C16 O2 Al1 115.48(8) . . ? C29 O3 Al1 128.04(8) . . ? C31 O4 Al1 125.93(8) . . ? N1 C1 C6 129.39(11) . . ? N1 C1 C2 110.77(10) . . ? C6 C1 C2 119.81(11) . . ? O1 C2 C3 122.46(11) . . ? O1 C2 C1 118.20(11) . . ? C3 C2 C1 119.33(10) . . ? C4 C3 C2 116.57(11) . . ? C4 C3 C7 123.45(11) . . ? C2 C3 C7 119.98(10) . . ? C3 C4 C5 124.93(11) . . ? C3 C4 H4A 117.5 . . ? C5 C4 H4A 117.5 . . ? C6 C5 C4 118.81(11) . . ? C6 C5 C11 122.72(11) . . ? C4 C5 C11 118.41(10) . . ? C5 C6 C1 120.44(11) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? C3 C7 C10 111.86(10) . . ? C3 C7 C9 110.38(11) . . ? C10 C7 C9 107.99(11) . . ? C3 C7 C8 108.77(10) . . ? C10 C7 C8 107.75(11) . . ? C9 C7 C8 110.05(11) . . ? 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 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 C14 112.45(10) . . ? C5 C11 C13 110.50(10) . . ? C14 C11 C13 108.69(10) . . ? C5 C11 C12 107.39(10) . . ? C14 C11 C12 108.28(11) . . ? C13 C11 C12 109.47(10) . . ? 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 . . ? 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 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C20 128.80(11) . . ? N1 C15 C16 110.82(10) . . ? C20 C15 C16 120.28(11) . . ? O2 C16 C17 122.78(11) . . ? O2 C16 C15 118.38(10) . . ? C17 C16 C15 118.83(10) . . ? C18 C17 C16 116.90(11) . . ? C18 C17 C21 123.02(11) . . ? C16 C17 C21 120.07(10) . . ? C17 C18 C19 124.85(11) . . ? C17 C18 H18A 117.6 . . ? C19 C18 H18A 117.6 . . ? C20 C19 C18 118.50(11) . . ? C20 C19 C25 122.34(11) . . ? C18 C19 C25 119.10(11) . . ? C19 C20 C15 120.39(11) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? C17 C21 C23 111.70(10) . . ? C17 C21 C24 110.40(10) . . ? C23 C21 C24 107.79(11) . . ? C17 C21 C22 108.45(10) . . ? C23 C21 C22 107.84(11) . . ? C24 C21 C22 110.64(10) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C19 112.10(10) . . ? C28 C25 C26 108.16(11) . . ? C19 C25 C26 110.30(11) . . ? C28 C25 C27 108.40(11) . . ? C19 C25 C27 108.30(10) . . ? C26 C25 C27 109.53(11) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C29 C30 123.03(11) . . ? O3 C29 C38 115.19(11) . . ? C30 C29 C38 121.67(11) . . ? C29 C30 C31 121.73(11) . . ? C29 C30 H30A 119.1 . . ? C31 C30 H30A 119.1 . . ? O4 C31 C30 123.49(11) . . ? O4 C31 C32 116.07(11) . . ? C30 C31 C32 120.37(11) . . ? C33 C32 C37 118.68(12) . . ? C33 C32 C31 118.89(11) . . ? C37 C32 C31 122.41(11) . . ? C34 C33 C32 120.63(12) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 120.10(13) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.01(13) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C37 120.00(13) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C32 120.59(12) . . ? C36 C37 H37A 119.7 . . ? C32 C37 H37A 119.7 . . ? C39 C38 C43 119.19(11) . . ? C39 C38 C29 118.52(11) . . ? C43 C38 C29 122.24(11) . . ? C40 C39 C38 120.39(11) . . ? C40 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 . . ? C41 C40 C39 120.05(12) . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C42 C41 C40 119.94(12) . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C41 C42 C43 120.27(12) . . ? C41 C42 H42A 119.9 . . ? C43 C42 H42A 119.9 . . ? C42 C43 C38 120.14(12) . . ? C42 C43 H43A 119.9 . . ? C38 C43 H43A 119.9 . . ? C49 C48 C47 119.58(13) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C44 C49 C48 120.36(14) . . ? C44 C49 H49A 119.8 . . ? C48 C49 H49A 119.8 . . ? C46 C47 C48 119.73(14) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C46 C45 C44 119.76(14) . . ? C46 C45 H45A 120.1 . . ? C44 C45 H45A 120.1 . . ? C45 C46 C47 120.52(14) . . ? C45 C46 H46A 119.7 . . ? C47 C46 H46A 119.7 . . ? C45 C44 C49 120.05(14) . . ? C45 C44 H44A 120.0 . . ? C49 C44 H44A 120.0 . . ? 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 Al1 N1 C1 25.5(8) . . . . ? O2 Al1 N1 C1 -176.08(8) . . . . ? O4 Al1 N1 C1 -87.80(8) . . . . ? O1 Al1 N1 C1 -0.83(8) . . . . ? Cl1 Al1 N1 C1 90.97(8) . . . . ? O3 Al1 N1 C15 -147.5(8) . . . . ? O2 Al1 N1 C15 10.88(8) . . . . ? O4 Al1 N1 C15 99.15(8) . . . . ? O1 Al1 N1 C15 -173.88(8) . . . . ? Cl1 Al1 N1 C15 -82.07(8) . . . . ? O3 Al1 O1 C2 -177.83(8) . . . . ? O2 Al1 O1 C2 15.72(18) . . . . ? O4 Al1 O1 C2 92.28(8) . . . . ? N1 Al1 O1 C2 0.75(8) . . . . ? Cl1 Al1 O1 C2 -86.66(8) . . . . ? O3 Al1 O2 C16 169.08(8) . . . . ? O4 Al1 O2 C16 -101.02(8) . . . . ? O1 Al1 O2 C16 -24.66(18) . . . . ? N1 Al1 O2 C16 -9.72(8) . . . . ? Cl1 Al1 O2 C16 77.53(8) . . . . ? O2 Al1 O3 C29 115.84(10) . . . . ? O4 Al1 O3 C29 27.38(10) . . . . ? O1 Al1 O3 C29 -59.81(10) . . . . ? N1 Al1 O3 C29 -86.0(8) . . . . ? Cl1 Al1 O3 C29 -151.34(10) . . . . ? O3 Al1 O4 C31 -24.50(10) . . . . ? O2 Al1 O4 C31 -126.05(10) . . . . ? O1 Al1 O4 C31 71.93(10) . . . . ? N1 Al1 O4 C31 152.58(10) . . . . ? Cl1 Al1 O4 C31 108.9(11) . . . . ? C15 N1 C1 C6 -6.1(2) . . . . ? Al1 N1 C1 C6 -177.34(10) . . . . ? C15 N1 C1 C2 171.96(12) . . . . ? Al1 N1 C1 C2 0.75(12) . . . . ? Al1 O1 C2 C3 178.54(8) . . . . ? Al1 O1 C2 C1 -0.56(13) . . . . ? N1 C1 C2 O1 -0.16(15) . . . . ? C6 C1 C2 O1 178.14(10) . . . . ? N1 C1 C2 C3 -179.29(10) . . . . ? C6 C1 C2 C3 -0.99(16) . . . . ? O1 C2 C3 C4 -176.50(11) . . . . ? C1 C2 C3 C4 2.59(16) . . . . ? O1 C2 C3 C7 4.19(17) . . . . ? C1 C2 C3 C7 -176.72(10) . . . . ? C2 C3 C4 C5 -1.21(17) . . . . ? C7 C3 C4 C5 178.06(11) . . . . ? C3 C4 C5 C6 -1.96(18) . . . . ? C3 C4 C5 C11 175.12(11) . . . . ? C4 C5 C6 C1 3.64(17) . . . . ? C11 C5 C6 C1 -173.31(11) . . . . ? N1 C1 C6 C5 175.70(12) . . . . ? C2 C1 C6 C5 -2.24(17) . . . . ? C4 C3 C7 C10 0.07(17) . . . . ? C2 C3 C7 C10 179.32(11) . . . . ? C4 C3 C7 C9 120.35(13) . . . . ? C2 C3 C7 C9 -60.40(15) . . . . ? C4 C3 C7 C8 -118.82(13) . . . . ? C2 C3 C7 C8 60.43(14) . . . . ? C6 C5 C11 C14 -2.75(17) . . . . ? C4 C5 C11 C14 -179.72(11) . . . . ? C6 C5 C11 C13 -124.40(12) . . . . ? C4 C5 C11 C13 58.63(14) . . . . ? C6 C5 C11 C12 116.26(13) . . . . ? C4 C5 C11 C12 -60.71(14) . . . . ? C1 N1 C15 C20 -4.7(2) . . . . ? Al1 N1 C15 C20 166.61(10) . . . . ? C1 N1 C15 C16 178.94(11) . . . . ? Al1 N1 C15 C16 -9.74(12) . . . . ? Al1 O2 C16 C17 -172.73(9) . . . . ? Al1 O2 C16 C15 7.22(13) . . . . ? N1 C15 C16 O2 2.22(15) . . . . ? C20 C15 C16 O2 -174.49(10) . . . . ? N1 C15 C16 C17 -177.83(10) . . . . ? C20 C15 C16 C17 5.46(16) . . . . ? O2 C16 C17 C18 175.30(11) . . . . ? C15 C16 C17 C18 -4.65(16) . . . . ? O2 C16 C17 C21 -4.11(17) . . . . ? C15 C16 C17 C21 175.94(10) . . . . ? C16 C17 C18 C19 0.70(18) . . . . ? C21 C17 C18 C19 -179.91(11) . . . . ? C17 C18 C19 C20 2.70(18) . . . . ? C17 C18 C19 C25 -174.50(11) . . . . ? C18 C19 C20 C15 -1.90(17) . . . . ? C25 C19 C20 C15 175.20(11) . . . . ? N1 C15 C20 C19 -178.14(11) . . . . ? C16 C15 C20 C19 -2.08(17) . . . . ? C18 C17 C21 C23 0.51(16) . . . . ? C16 C17 C21 C23 179.89(11) . . . . ? C18 C17 C21 C24 -119.41(13) . . . . ? C16 C17 C21 C24 59.97(14) . . . . ? C18 C17 C21 C22 119.22(13) . . . . ? C16 C17 C21 C22 -61.40(14) . . . . ? C20 C19 C25 C28 9.17(17) . . . . ? C18 C19 C25 C28 -173.75(11) . . . . ? C20 C19 C25 C26 129.77(13) . . . . ? C18 C19 C25 C26 -53.15(15) . . . . ? C20 C19 C25 C27 -110.38(13) . . . . ? C18 C19 C25 C27 66.70(14) . . . . ? Al1 O3 C29 C30 -15.12(17) . . . . ? Al1 O3 C29 C38 168.69(8) . . . . ? O3 C29 C30 C31 -10.57(19) . . . . ? C38 C29 C30 C31 165.39(11) . . . . ? Al1 O4 C31 C30 9.69(17) . . . . ? Al1 O4 C31 C32 -173.14(8) . . . . ? C29 C30 C31 O4 12.71(19) . . . . ? C29 C30 C31 C32 -164.35(11) . . . . ? O4 C31 C32 C33 13.05(17) . . . . ? C30 C31 C32 C33 -169.68(12) . . . . ? O4 C31 C32 C37 -165.24(12) . . . . ? C30 C31 C32 C37 12.03(18) . . . . ? C37 C32 C33 C34 0.2(2) . . . . ? C31 C32 C33 C34 -178.17(12) . . . . ? C32 C33 C34 C35 0.0(2) . . . . ? C33 C34 C35 C36 -0.3(2) . . . . ? C34 C35 C36 C37 0.4(2) . . . . ? C35 C36 C37 C32 -0.2(2) . . . . ? C33 C32 C37 C36 -0.07(19) . . . . ? C31 C32 C37 C36 178.23(12) . . . . ? O3 C29 C38 C39 10.60(16) . . . . ? C30 C29 C38 C39 -165.66(12) . . . . ? O3 C29 C38 C43 -171.89(11) . . . . ? C30 C29 C38 C43 11.85(18) . . . . ? C43 C38 C39 C40 -1.19(18) . . . . ? C29 C38 C39 C40 176.40(11) . . . . ? C38 C39 C40 C41 0.17(19) . . . . ? C39 C40 C41 C42 1.2(2) . . . . ? C40 C41 C42 C43 -1.4(2) . . . . ? C41 C42 C43 C38 0.4(2) . . . . ? C39 C38 C43 C42 0.90(19) . . . . ? C29 C38 C43 C42 -176.60(12) . . . . ? C47 C48 C49 C44 -0.3(2) . . . . ? C49 C48 C47 C46 -0.1(2) . . . . ? C44 C45 C46 C47 -0.3(3) . . . . ? C48 C47 C46 C45 0.4(2) . . . . ? C46 C45 C44 C49 -0.1(2) . . . . ? C48 C49 C44 C45 0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.04 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.348 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.045