# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_110117e _database_code_depnum_ccdc_archive 'CCDC 906746' #TrackingRef '6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H40 Al2 N2 O2' _chemical_formula_weight 454.55 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 16.1331(15) _cell_length_b 9.5710(8) _cell_length_c 22.699(2) _cell_angle_alpha 90.00 _cell_angle_beta 128.290(2) _cell_angle_gamma 90.00 _cell_volume 2751.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1493 _cell_measurement_theta_min 2.416 _cell_measurement_theta_max 26.235 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9701 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13616 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.1030 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4850 _reflns_number_gt 1924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0594P)^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 ? _refine_ls_number_reflns 4850 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1572 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.16380(11) 0.29662(14) 0.40990(8) 0.0629(4) Uani 1 1 d . . . Al2 Al 0.30603(12) 0.76414(14) 0.77759(8) 0.0720(5) Uani 1 1 d . . . N1 N 0.1293(3) 0.1176(3) 0.4384(2) 0.0660(10) Uani 1 1 d . . . N2 N 0.4424(3) 0.8495(5) 0.8121(2) 0.0884(13) Uani 1 1 d . . . O1 O 0.1908(2) 0.3982(3) 0.48461(16) 0.0645(8) Uani 1 1 d . . . O2 O 0.2451(3) 0.7636(3) 0.68114(18) 0.0865(10) Uani 1 1 d . . . C1 C 0.2012(4) 0.1128(4) 0.5221(3) 0.0708(13) Uani 1 1 d . . . H1A H 0.2737 0.1193 0.5404 0.085 Uiso 1 1 calc R . . H1B H 0.1929 0.0234 0.5380 0.085 Uiso 1 1 calc R . . C2 C 0.1807(3) 0.2288(4) 0.5571(2) 0.0585(11) Uani 1 1 d . . . C3 C 0.1766(3) 0.3657(4) 0.5359(2) 0.0535(11) Uani 1 1 d . . . C4 C 0.1551(3) 0.4739(4) 0.5665(2) 0.0535(11) Uani 1 1 d . . . C5 C 0.1389(3) 0.4379(5) 0.6180(2) 0.0672(13) Uani 1 1 d . . . H5 H 0.1243 0.5088 0.6384 0.081 Uiso 1 1 calc R . . C6 C 0.1434(4) 0.3020(5) 0.6403(3) 0.0725(13) Uani 1 1 d . . . C7 C 0.1644(4) 0.1991(5) 0.6088(3) 0.0726(13) Uani 1 1 d . . . H7 H 0.1676 0.1066 0.6228 0.087 Uiso 1 1 calc R . . C8 C 0.1219(5) 0.2706(5) 0.6956(3) 0.121(2) Uani 1 1 d . . . H8A H 0.0934 0.1781 0.6868 0.181 Uiso 1 1 calc R . . H8B H 0.0722 0.3371 0.6889 0.181 Uiso 1 1 calc R . . H8C H 0.1867 0.2768 0.7460 0.181 Uiso 1 1 calc R . . C9 C 0.4259(5) 0.9327(7) 0.7547(4) 0.139(3) Uani 1 1 d . . . H9A H 0.4908 0.9806 0.7731 0.167 Uiso 1 1 calc R . . H9B H 0.3725 1.0026 0.7396 0.167 Uiso 1 1 calc R . . C10 C 0.3880(5) 0.8370(6) 0.6833(3) 0.0958(18) Uani 1 1 d . . . C11 C 0.2937(4) 0.7653(5) 0.6490(3) 0.0765(14) Uani 1 1 d . . . C12 C 0.2464(3) 0.7004(4) 0.5796(3) 0.0582(11) Uani 1 1 d . . . C13 C 0.2957(4) 0.7114(4) 0.5469(3) 0.0673(12) Uani 1 1 d . . . H13 H 0.2633 0.6706 0.5001 0.081 Uiso 1 1 calc R . . C14 C 0.3910(4) 0.7802(5) 0.5806(3) 0.0742(14) Uani 1 1 d . . . C15 C 0.4360(4) 0.8397(5) 0.6490(3) 0.0964(18) Uani 1 1 d . . . H15 H 0.5011 0.8837 0.6738 0.116 Uiso 1 1 calc R . . C16 C 0.4400(4) 0.7921(5) 0.5408(3) 0.1071(19) Uani 1 1 d . . . H16A H 0.4289 0.8848 0.5209 0.161 Uiso 1 1 calc R . . H16B H 0.4074 0.7255 0.5005 0.161 Uiso 1 1 calc R . . H16C H 0.5144 0.7736 0.5759 0.161 Uiso 1 1 calc R . . C17 C 0.1431(3) 0.6231(4) 0.5402(2) 0.0606(12) Uani 1 1 d . . . H17A H 0.1076 0.6227 0.4867 0.073 Uiso 1 1 calc R . . H17B H 0.0984 0.6731 0.5481 0.073 Uiso 1 1 calc R . . C18 C 0.0175(4) 0.1120(5) 0.4095(3) 0.0807(15) Uani 1 1 d . . . H18A H 0.0078 0.0319 0.4301 0.121 Uiso 1 1 calc R . . H18B H -0.0285 0.1051 0.3557 0.121 Uiso 1 1 calc R . . H18C H 0.0012 0.1953 0.4240 0.121 Uiso 1 1 calc R . . C19 C 0.5174(5) 0.7311(8) 0.8268(4) 0.160(3) Uani 1 1 d . . . H19A H 0.4778 0.6582 0.7905 0.240 Uiso 1 1 calc R . . H19B H 0.5521 0.6944 0.8763 0.240 Uiso 1 1 calc R . . H19C H 0.5693 0.7668 0.8227 0.240 Uiso 1 1 calc R . . C20 C 0.4997(5) 0.9236(6) 0.8843(3) 0.138(2) Uani 1 1 d . . . H20A H 0.5695 0.9464 0.9017 0.207 Uiso 1 1 calc R . . H20B H 0.5042 0.8647 0.9205 0.207 Uiso 1 1 calc R . . H20C H 0.4626 1.0078 0.8779 0.207 Uiso 1 1 calc R . . C21 C 0.0386(4) 0.3569(5) 0.3119(3) 0.0879(16) Uani 1 1 d . . . H21A H -0.0182 0.3723 0.3141 0.132 Uiso 1 1 calc R . . H21B H 0.0186 0.2860 0.2753 0.132 Uiso 1 1 calc R . . H21C H 0.0537 0.4422 0.2979 0.132 Uiso 1 1 calc R . . C22 C 0.2925(4) 0.2615(5) 0.4216(3) 0.0901(16) Uani 1 1 d . . . H22A H 0.3247 0.3488 0.4253 0.135 Uiso 1 1 calc R . . H22B H 0.2753 0.2105 0.3788 0.135 Uiso 1 1 calc R . . H22C H 0.3407 0.2077 0.4663 0.135 Uiso 1 1 calc R . . C23 C 0.3320(5) 0.5783(6) 0.8210(4) 0.138(2) Uani 1 1 d . . . H23A H 0.2779 0.5557 0.8253 0.206 Uiso 1 1 calc R . . H23B H 0.3996 0.5767 0.8698 0.206 Uiso 1 1 calc R . . H23C H 0.3311 0.5111 0.7892 0.206 Uiso 1 1 calc R . . C24 C 0.2365(4) 0.8870(6) 0.8024(3) 0.127(2) Uani 1 1 d . . . H24A H 0.2287 0.9780 0.7817 0.191 Uiso 1 1 calc R . . H24B H 0.2783 0.8939 0.8560 0.191 Uiso 1 1 calc R . . H24C H 0.1682 0.8500 0.7819 0.191 Uiso 1 1 calc R . . C51 C 0.1494(4) -0.0079(5) 0.4093(3) 0.0958(17) Uani 1 1 d . . . H51A H 0.2232 -0.0127 0.4322 0.144 Uiso 1 1 calc R . . H51B H 0.1088 -0.0005 0.3558 0.144 Uiso 1 1 calc R . . H51C H 0.1291 -0.0909 0.4212 0.144 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 0.0595(9) 0.0713(9) 0.0588(10) -0.0027(7) 0.0371(8) 0.0040(7) Al2 0.0832(11) 0.0635(9) 0.0629(10) -0.0078(7) 0.0421(9) 0.0025(8) N1 0.062(3) 0.064(2) 0.057(3) -0.0077(19) 0.030(2) 0.003(2) N2 0.071(3) 0.095(3) 0.064(3) -0.005(3) 0.024(3) -0.008(3) O1 0.081(2) 0.0600(19) 0.067(2) -0.0047(15) 0.0529(19) -0.0061(15) O2 0.089(2) 0.107(3) 0.069(2) -0.0270(18) 0.051(2) -0.039(2) C1 0.069(3) 0.062(3) 0.064(4) 0.000(2) 0.033(3) 0.000(2) C2 0.059(3) 0.059(3) 0.048(3) -0.001(2) 0.028(3) -0.008(2) C3 0.051(3) 0.059(3) 0.049(3) -0.003(2) 0.030(2) -0.006(2) C4 0.053(3) 0.058(3) 0.045(3) -0.005(2) 0.027(2) -0.010(2) C5 0.077(3) 0.068(3) 0.062(3) -0.015(2) 0.046(3) -0.020(3) C6 0.090(4) 0.074(3) 0.053(3) -0.007(3) 0.044(3) -0.022(3) C7 0.080(4) 0.066(3) 0.053(3) 0.001(3) 0.032(3) -0.021(3) C8 0.190(6) 0.113(5) 0.096(5) -0.021(3) 0.107(5) -0.055(4) C9 0.111(5) 0.164(6) 0.097(6) -0.003(5) 0.041(5) -0.073(5) C10 0.096(4) 0.107(4) 0.077(4) -0.022(3) 0.049(4) -0.053(3) C11 0.079(4) 0.084(4) 0.066(4) -0.008(3) 0.044(3) -0.026(3) C12 0.064(3) 0.052(3) 0.057(3) 0.002(2) 0.037(3) -0.006(2) C13 0.074(4) 0.058(3) 0.067(3) 0.000(2) 0.042(3) -0.002(3) C14 0.081(4) 0.067(3) 0.082(4) -0.002(3) 0.054(4) -0.011(3) C15 0.091(4) 0.099(4) 0.087(5) -0.006(3) 0.050(4) -0.043(3) C16 0.114(5) 0.106(4) 0.141(6) 0.006(4) 0.098(5) -0.011(4) C17 0.061(3) 0.063(3) 0.052(3) -0.006(2) 0.032(3) -0.002(2) C18 0.063(3) 0.093(4) 0.067(4) -0.009(3) 0.030(3) -0.016(3) C19 0.072(4) 0.189(8) 0.173(8) -0.026(6) 0.053(5) -0.001(5) C20 0.144(6) 0.130(5) 0.082(5) -0.037(4) 0.041(5) -0.056(5) C21 0.076(4) 0.110(4) 0.073(4) 0.008(3) 0.044(3) 0.010(3) C22 0.074(4) 0.129(5) 0.075(4) -0.009(3) 0.050(3) 0.002(3) C23 0.181(7) 0.116(5) 0.139(6) 0.036(4) 0.110(6) 0.016(5) C24 0.103(5) 0.149(6) 0.100(5) -0.029(4) 0.048(4) 0.021(4) C51 0.116(5) 0.070(3) 0.093(4) -0.019(3) 0.061(4) 0.009(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 O1 1.760(3) . ? Al1 C21 1.948(5) . ? Al1 C22 1.952(4) . ? Al1 N1 2.027(4) . ? Al2 O2 1.758(3) . ? Al2 C24 1.935(5) . ? Al2 C23 1.949(5) . ? Al2 N2 1.996(4) . ? N1 C18 1.490(5) . ? N1 C1 1.492(5) . ? N1 C51 1.500(5) . ? N2 C9 1.404(6) . ? N2 C20 1.472(6) . ? N2 C19 1.536(7) . ? O1 C3 1.353(4) . ? O2 C11 1.362(5) . ? C1 C2 1.517(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C7 1.382(5) . ? C2 C3 1.383(5) . ? C3 C4 1.405(5) . ? C4 C5 1.390(5) . ? C4 C17 1.513(5) . ? C5 C6 1.381(6) . ? C5 H5 0.9300 . ? C6 C7 1.376(6) . ? C6 C8 1.526(6) . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.617(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.387(6) . ? C10 C15 1.396(6) . ? C11 C12 1.400(6) . ? C12 C13 1.390(5) . ? C12 C17 1.509(5) . ? C13 C14 1.387(6) . ? C13 H13 0.9300 . ? C14 C15 1.367(6) . ? C14 C16 1.529(6) . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? 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 C21 113.55(18) . . ? O1 Al1 C22 110.95(18) . . ? C21 Al1 C22 117.9(2) . . ? O1 Al1 N1 96.45(14) . . ? C21 Al1 N1 108.64(19) . . ? C22 Al1 N1 106.85(19) . . ? O2 Al2 C24 112.8(2) . . ? O2 Al2 C23 114.0(2) . . ? C24 Al2 C23 112.9(3) . . ? O2 Al2 N2 96.88(17) . . ? C24 Al2 N2 109.5(2) . . ? C23 Al2 N2 109.6(2) . . ? C18 N1 C1 109.5(3) . . ? C18 N1 C51 108.1(3) . . ? C1 N1 C51 109.1(3) . . ? C18 N1 Al1 112.7(3) . . ? C1 N1 Al1 106.4(3) . . ? C51 N1 Al1 111.1(3) . . ? C9 N2 C20 112.8(5) . . ? C9 N2 C19 106.9(5) . . ? C20 N2 C19 104.3(5) . . ? C9 N2 Al2 109.8(4) . . ? C20 N2 Al2 114.3(4) . . ? C19 N2 Al2 108.2(3) . . ? C3 O1 Al1 129.0(3) . . ? C11 O2 Al2 127.1(3) . . ? N1 C1 C2 113.3(3) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C7 C2 C3 119.9(4) . . ? C7 C2 C1 120.8(4) . . ? C3 C2 C1 119.3(4) . . ? O1 C3 C2 121.4(4) . . ? O1 C3 C4 118.7(4) . . ? C2 C3 C4 119.9(4) . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C17 121.3(4) . . ? C3 C4 C17 120.8(4) . . ? C6 C5 C4 123.1(4) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C7 C6 C5 117.3(4) . . ? C7 C6 C8 122.7(4) . . ? C5 C6 C8 120.0(4) . . ? C6 C7 C2 122.0(4) . . ? C6 C7 H7 119.0 . . ? C2 C7 H7 119.0 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 110.2(5) . . ? N2 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? N2 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C15 119.4(5) . . ? C11 C10 C9 116.3(5) . . ? C15 C10 C9 123.6(5) . . ? O2 C11 C10 120.1(5) . . ? O2 C11 C12 120.2(4) . . ? C10 C11 C12 119.6(5) . . ? C13 C12 C11 118.3(4) . . ? C13 C12 C17 120.5(4) . . ? C11 C12 C17 121.1(4) . . ? C14 C13 C12 123.2(4) . . ? C14 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? C15 C14 C13 116.8(4) . . ? C15 C14 C16 122.4(5) . . ? C13 C14 C16 120.8(5) . . ? C14 C15 C10 122.6(5) . . ? C14 C15 H15 118.7 . . ? C10 C15 H15 118.7 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 C4 113.9(4) . . ? C12 C17 H17A 108.8 . . ? C4 C17 H17A 108.8 . . ? C12 C17 H17B 108.8 . . ? C4 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? N1 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Al1 C21 H21A 109.5 . . ? Al1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Al1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Al1 C22 H22A 109.5 . . ? Al1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Al1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Al2 C23 H23A 109.5 . . ? Al2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al2 C24 H24A 109.5 . . ? Al2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C51 H51A 109.5 . . ? N1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 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 O1 Al1 N1 C18 84.3(3) . . . . ? C21 Al1 N1 C18 -33.2(3) . . . . ? C22 Al1 N1 C18 -161.4(3) . . . . ? O1 Al1 N1 C1 -35.6(3) . . . . ? C21 Al1 N1 C1 -153.2(3) . . . . ? C22 Al1 N1 C1 78.6(3) . . . . ? O1 Al1 N1 C51 -154.2(3) . . . . ? C21 Al1 N1 C51 88.3(3) . . . . ? C22 Al1 N1 C51 -40.0(3) . . . . ? O2 Al2 N2 C9 27.0(4) . . . . ? C24 Al2 N2 C9 -90.1(5) . . . . ? C23 Al2 N2 C9 145.5(5) . . . . ? O2 Al2 N2 C20 155.0(4) . . . . ? C24 Al2 N2 C20 37.9(5) . . . . ? C23 Al2 N2 C20 -86.5(4) . . . . ? O2 Al2 N2 C19 -89.3(4) . . . . ? C24 Al2 N2 C19 153.6(4) . . . . ? C23 Al2 N2 C19 29.2(4) . . . . ? C21 Al1 O1 C3 105.6(4) . . . . ? C22 Al1 O1 C3 -118.9(3) . . . . ? N1 Al1 O1 C3 -8.0(3) . . . . ? C24 Al2 O2 C11 137.9(4) . . . . ? C23 Al2 O2 C11 -91.7(4) . . . . ? N2 Al2 O2 C11 23.4(4) . . . . ? C18 N1 C1 C2 -57.0(4) . . . . ? C51 N1 C1 C2 -175.0(4) . . . . ? Al1 N1 C1 C2 65.1(4) . . . . ? N1 C1 C2 C7 127.3(4) . . . . ? N1 C1 C2 C3 -51.6(5) . . . . ? Al1 O1 C3 C2 28.3(6) . . . . ? Al1 O1 C3 C4 -150.3(3) . . . . ? C7 C2 C3 O1 -179.1(4) . . . . ? C1 C2 C3 O1 -0.1(6) . . . . ? C7 C2 C3 C4 -0.5(6) . . . . ? C1 C2 C3 C4 178.4(4) . . . . ? O1 C3 C4 C5 178.8(4) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? O1 C3 C4 C17 2.7(6) . . . . ? C2 C3 C4 C17 -175.9(4) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? C17 C4 C5 C6 176.4(4) . . . . ? C4 C5 C6 C7 -0.5(7) . . . . ? C4 C5 C6 C8 -178.4(4) . . . . ? C5 C6 C7 C2 0.2(7) . . . . ? C8 C6 C7 C2 178.1(5) . . . . ? C3 C2 C7 C6 0.3(7) . . . . ? C1 C2 C7 C6 -178.6(4) . . . . ? C20 N2 C9 C10 166.8(5) . . . . ? C19 N2 C9 C10 52.7(6) . . . . ? Al2 N2 C9 C10 -64.4(6) . . . . ? N2 C9 C10 C11 61.4(7) . . . . ? N2 C9 C10 C15 -128.2(6) . . . . ? Al2 O2 C11 C10 -33.7(6) . . . . ? Al2 O2 C11 C12 149.3(3) . . . . ? C15 C10 C11 O2 -178.9(5) . . . . ? C9 C10 C11 O2 -8.2(8) . . . . ? C15 C10 C11 C12 -1.9(8) . . . . ? C9 C10 C11 C12 168.9(5) . . . . ? O2 C11 C12 C13 176.4(4) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? O2 C11 C12 C17 -2.2(7) . . . . ? C10 C11 C12 C17 -179.2(4) . . . . ? C11 C12 C13 C14 1.8(6) . . . . ? C17 C12 C13 C14 -179.5(4) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C12 C13 C14 C16 -178.4(4) . . . . ? C13 C14 C15 C10 -2.2(8) . . . . ? C16 C14 C15 C10 175.6(5) . . . . ? C11 C10 C15 C14 3.4(9) . . . . ? C9 C10 C15 C14 -166.6(6) . . . . ? C13 C12 C17 C4 97.3(5) . . . . ? C11 C12 C17 C4 -84.1(5) . . . . ? C5 C4 C17 C12 99.3(5) . . . . ? C3 C4 C17 C12 -84.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.607 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.049 data_110309a _database_code_depnum_ccdc_archive 'CCDC 906747' #TrackingRef '16.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38.50 H44 Al2 N2 O2' _chemical_formula_weight 620.72 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1161(8) _cell_length_b 13.6920(11) _cell_length_c 15.7135(13) _cell_angle_alpha 104.683(2) _cell_angle_beta 91.7960(10) _cell_angle_gamma 103.913(2) _cell_volume 1832.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1255 _cell_measurement_theta_min 2.345 _cell_measurement_theta_max 26.133 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9767 _exptl_absorpt_correction_T_max 0.9922 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9701 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.1492 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6382 _reflns_number_gt 2380 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0156P)^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 ? _refine_ls_number_reflns 6382 _refine_ls_number_parameters 441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1700 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0911 _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 0.56133(14) 0.65619(11) 0.21429(9) 0.0601(4) Uani 1 1 d . . . Al2 Al 1.02890(14) 0.90452(11) 0.73585(9) 0.0607(4) Uani 1 1 d . . . N1 N 0.3815(4) 0.5633(3) 0.2445(2) 0.0570(9) Uani 1 1 d . . . N2 N 1.2250(4) 0.8791(2) 0.7028(2) 0.0556(9) Uani 1 1 d . . . O1 O 0.6052(3) 0.7420(2) 0.32225(17) 0.0624(8) Uani 1 1 d . . . O2 O 0.9609(3) 0.8972(2) 0.62762(17) 0.0601(8) Uani 1 1 d . . . C1 C 0.7744(4) 0.8857(3) 0.4763(2) 0.0498(11) Uani 1 1 d . . . H1A H 0.7749 0.9413 0.5289 0.060 Uiso 1 1 calc R . . H1B H 0.7497 0.9088 0.4254 0.060 Uiso 1 1 calc R . . C2 C 0.3616(5) 0.5653(3) 0.3259(3) 0.0585(12) Uani 1 1 d . . . H2 H 0.2773 0.5171 0.3357 0.070 Uiso 1 1 calc R . . C3 C 0.4560(5) 0.6338(3) 0.4025(3) 0.0514(11) Uani 1 1 d . . . C4 C 0.5726(5) 0.7208(3) 0.3987(3) 0.0494(11) Uani 1 1 d . . . C5 C 0.6524(4) 0.7894(3) 0.4784(3) 0.0472(11) Uani 1 1 d . . . C6 C 0.6171(4) 0.7655(3) 0.5574(3) 0.0523(11) Uani 1 1 d . . . H6 H 0.6704 0.8104 0.6097 0.063 Uiso 1 1 calc R . . C7 C 0.5058(5) 0.6776(4) 0.5624(3) 0.0542(12) Uani 1 1 d . . . C8 C 0.4262(4) 0.6143(3) 0.4854(3) 0.0564(12) Uani 1 1 d . . . H8 H 0.3498 0.5562 0.4873 0.068 Uiso 1 1 calc R . . C9 C 0.4751(5) 0.6553(3) 0.6509(2) 0.0778(14) Uani 1 1 d . . . H9A H 0.3680 0.6279 0.6518 0.117 Uiso 1 1 calc R . . H9B H 0.5102 0.7188 0.6974 0.117 Uiso 1 1 calc R . . H9C H 0.5278 0.6052 0.6596 0.117 Uiso 1 1 calc R . . C10 C 1.2593(4) 0.8625(3) 0.6218(3) 0.0536(12) Uani 1 1 d . . . H10 H 1.3563 0.8542 0.6123 0.064 Uiso 1 1 calc R . . C11 C 1.1639(4) 0.8555(3) 0.5456(3) 0.0483(11) Uani 1 1 d . . . C12 C 1.0175(4) 0.8739(3) 0.5502(3) 0.0452(11) Uani 1 1 d . . . C13 C 0.9318(4) 0.8671(3) 0.4717(3) 0.0448(10) Uani 1 1 d . . . C14 C 0.9939(4) 0.8447(3) 0.3928(3) 0.0509(11) Uani 1 1 d . . . H14 H 0.9370 0.8411 0.3414 0.061 Uiso 1 1 calc R . . C15 C 1.1391(5) 0.8268(3) 0.3857(3) 0.0537(11) Uani 1 1 d . . . C16 C 1.2204(4) 0.8324(3) 0.4618(3) 0.0527(11) Uani 1 1 d . . . H16 H 1.3166 0.8205 0.4587 0.063 Uiso 1 1 calc R . . C17 C 1.2021(4) 0.8047(3) 0.2967(2) 0.0779(14) Uani 1 1 d . . . H17A H 1.2113 0.8639 0.2731 0.117 Uiso 1 1 calc R . . H17B H 1.1347 0.7444 0.2569 0.117 Uiso 1 1 calc R . . H17C H 1.3002 0.7919 0.3038 0.117 Uiso 1 1 calc R . . C18 C 0.2663(5) 0.4941(3) 0.1762(3) 0.0588(12) Uani 1 1 d . . . C19 C 0.1156(5) 0.4930(3) 0.1799(3) 0.0708(13) Uani 1 1 d . . . H19 H 0.0853 0.5366 0.2279 0.085 Uiso 1 1 calc R . . C20 C 0.0084(5) 0.4269(4) 0.1123(3) 0.0760(14) Uani 1 1 d . . . H20 H -0.0933 0.4266 0.1159 0.091 Uiso 1 1 calc R . . C21 C 0.0490(6) 0.3620(4) 0.0404(3) 0.0719(14) Uani 1 1 d . . . C22 C 0.1996(6) 0.3641(4) 0.0379(3) 0.0833(15) Uani 1 1 d . . . H22 H 0.2298 0.3202 -0.0099 0.100 Uiso 1 1 calc R . . C23 C 0.3077(5) 0.4295(4) 0.1041(3) 0.0775(14) Uani 1 1 d . . . H23 H 0.4094 0.4299 0.1000 0.093 Uiso 1 1 calc R . . C24 C -0.0687(5) 0.2906(4) -0.0327(3) 0.1141(18) Uani 1 1 d . . . H24A H -0.0355 0.2972 -0.0888 0.171 Uiso 1 1 calc R . . H24B H -0.1633 0.3095 -0.0255 0.171 Uiso 1 1 calc R . . H24C H -0.0823 0.2196 -0.0302 0.171 Uiso 1 1 calc R . . C25 C 1.3442(5) 0.8904(4) 0.7704(3) 0.0603(13) Uani 1 1 d . . . C26 C 1.3179(5) 0.8325(4) 0.8305(3) 0.0795(15) Uani 1 1 d . . . H26 H 1.2234 0.7868 0.8284 0.095 Uiso 1 1 calc R . . C27 C 1.4331(7) 0.8425(4) 0.8943(3) 0.0911(17) Uani 1 1 d . . . H27 H 1.4157 0.8008 0.9332 0.109 Uiso 1 1 calc R . . C28 C 1.5704(6) 0.9115(5) 0.9014(3) 0.0797(16) Uani 1 1 d . . . C29 C 1.5938(5) 0.9703(4) 0.8422(3) 0.0894(16) Uani 1 1 d . . . H29 H 1.6870 1.0182 0.8461 0.107 Uiso 1 1 calc R . . C30 C 1.4819(6) 0.9602(4) 0.7766(3) 0.0764(14) Uani 1 1 d . . . H30 H 1.5004 1.0008 0.7369 0.092 Uiso 1 1 calc R . . C31 C 1.6956(5) 0.9228(4) 0.9729(3) 0.1143(19) Uani 1 1 d . . . H31A H 1.6551 0.9305 1.0292 0.171 Uiso 1 1 calc R . . H31B H 1.7765 0.9833 0.9750 0.171 Uiso 1 1 calc R . . H31C H 1.7339 0.8618 0.9594 0.171 Uiso 1 1 calc R . . C32 C 0.4954(4) 0.7214(3) 0.1289(3) 0.0788(14) Uani 1 1 d . . . H32A H 0.4172 0.7540 0.1513 0.118 Uiso 1 1 calc R . . H32B H 0.4565 0.6692 0.0743 0.118 Uiso 1 1 calc R . . H32C H 0.5800 0.7731 0.1190 0.118 Uiso 1 1 calc R . . C33 C 0.7135(5) 0.5759(3) 0.1849(3) 0.0960(16) Uani 1 1 d . . . H33A H 0.8131 0.6229 0.1953 0.144 Uiso 1 1 calc R . . H33B H 0.6945 0.5370 0.1238 0.144 Uiso 1 1 calc R . . H33C H 0.7073 0.5286 0.2213 0.144 Uiso 1 1 calc R . . C34 C 0.9065(5) 0.7908(3) 0.7768(3) 0.1015(18) Uani 1 1 d . . . H34A H 0.8065 0.8008 0.7843 0.152 Uiso 1 1 calc R . . H34B H 0.9530 0.7903 0.8323 0.152 Uiso 1 1 calc R . . H34C H 0.8996 0.7255 0.7340 0.152 Uiso 1 1 calc R . . C35 C 1.0731(5) 1.0460(3) 0.8142(3) 0.0945(16) Uani 1 1 d . . . H35A H 1.1509 1.0914 0.7922 0.142 Uiso 1 1 calc R . . H35B H 1.1073 1.0456 0.8725 0.142 Uiso 1 1 calc R . . H35C H 0.9828 1.0706 0.8165 0.142 Uiso 1 1 calc R . . C36 C 0.036(2) 0.470(2) 0.532(3) 0.090(5) Uani 0.50 1 d P . . C37 C -0.001(11) 0.563(7) 0.572(5) 0.093(19) Uani 0.50 1 d P . . H37 H 0.0218 0.5928 0.6325 0.111 Uiso 0.50 1 d PR . . C38 C -0.072(2) 0.6108(16) 0.521(3) 0.105(7) Uani 0.50 1 d P . . H38 H -0.0961 0.6730 0.5472 0.126 Uiso 0.50 1 d PR . . C39 C -0.106(5) 0.566(4) 0.430(4) 0.107(10) Uani 0.50 1 d P . . H39 H -0.1530 0.5982 0.3963 0.128 Uiso 0.50 1 d PR . . C40 C -0.069(3) 0.473(3) 0.391(2) 0.117(7) Uani 0.50 1 d P . . H40 H -0.0918 0.4431 0.3305 0.140 Uiso 0.50 1 d PR . . C41 C 0.002(11) 0.425(7) 0.442(6) 0.10(2) Uani 0.50 1 d P . . H41 H 0.0261 0.3629 0.4158 0.117 Uiso 0.50 1 d PR . . C42 C 0.111(6) 0.420(5) 0.588(5) 0.15(3) Uani 0.50 1 d P . . H42A H 0.1903 0.3949 0.5581 0.219 Uiso 0.50 1 d PR . . H42B H 0.0382 0.3628 0.5999 0.219 Uiso 0.50 1 d PR . . H42C H 0.1546 0.4706 0.6432 0.219 Uiso 0.50 1 d PR . . 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 0.0472(9) 0.0741(10) 0.0584(10) 0.0201(8) 0.0066(7) 0.0121(8) Al2 0.0562(9) 0.0788(11) 0.0533(9) 0.0208(8) 0.0060(7) 0.0258(8) N1 0.054(2) 0.057(3) 0.056(3) 0.009(2) 0.006(2) 0.012(2) N2 0.055(2) 0.066(3) 0.052(2) 0.021(2) 0.002(2) 0.019(2) O1 0.0551(19) 0.070(2) 0.056(2) 0.0238(18) 0.0039(16) -0.0004(16) O2 0.0507(18) 0.082(2) 0.052(2) 0.0190(17) 0.0064(15) 0.0228(16) C1 0.048(3) 0.043(3) 0.057(3) 0.014(2) -0.003(2) 0.010(2) C2 0.055(3) 0.051(3) 0.066(4) 0.014(3) 0.012(3) 0.009(2) C3 0.045(3) 0.054(3) 0.053(3) 0.012(3) 0.003(2) 0.009(3) C4 0.038(3) 0.052(3) 0.061(3) 0.019(3) 0.006(2) 0.012(2) C5 0.036(3) 0.047(3) 0.061(3) 0.018(3) 0.000(2) 0.013(2) C6 0.052(3) 0.049(3) 0.055(3) 0.011(2) 0.000(2) 0.013(2) C7 0.050(3) 0.060(3) 0.055(3) 0.020(3) 0.010(3) 0.013(3) C8 0.048(3) 0.057(3) 0.061(3) 0.019(3) 0.004(3) 0.004(2) C9 0.081(3) 0.088(4) 0.059(3) 0.023(3) 0.010(3) 0.006(3) C10 0.041(3) 0.060(3) 0.065(3) 0.023(3) 0.001(2) 0.017(2) C11 0.047(3) 0.048(3) 0.055(3) 0.018(2) 0.004(2) 0.016(2) C12 0.046(3) 0.039(3) 0.048(3) 0.011(2) 0.004(2) 0.008(2) C13 0.046(3) 0.037(3) 0.049(3) 0.015(2) -0.001(2) 0.005(2) C14 0.049(3) 0.050(3) 0.050(3) 0.018(2) -0.008(2) 0.004(2) C15 0.051(3) 0.053(3) 0.057(3) 0.016(3) 0.006(3) 0.011(2) C16 0.047(3) 0.052(3) 0.063(3) 0.020(3) 0.009(3) 0.016(2) C17 0.071(3) 0.108(4) 0.059(3) 0.021(3) 0.014(3) 0.029(3) C18 0.054(3) 0.058(3) 0.055(3) 0.008(3) 0.006(3) 0.004(3) C19 0.054(3) 0.069(3) 0.079(4) 0.001(3) 0.008(3) 0.017(3) C20 0.050(3) 0.079(4) 0.087(4) 0.008(3) -0.007(3) 0.011(3) C21 0.067(4) 0.072(4) 0.063(4) 0.006(3) -0.002(3) 0.005(3) C22 0.074(4) 0.097(4) 0.059(4) -0.004(3) 0.006(3) 0.010(3) C23 0.059(4) 0.091(4) 0.076(4) 0.012(3) 0.014(3) 0.017(3) C24 0.105(4) 0.120(5) 0.085(4) -0.012(4) -0.021(3) 0.013(4) C25 0.052(3) 0.080(4) 0.057(3) 0.024(3) 0.003(3) 0.027(3) C26 0.068(4) 0.109(4) 0.074(4) 0.043(3) 0.006(3) 0.025(3) C27 0.084(4) 0.137(5) 0.071(4) 0.048(4) 0.005(3) 0.044(4) C28 0.069(4) 0.121(5) 0.057(4) 0.022(3) -0.007(3) 0.043(4) C29 0.065(4) 0.114(5) 0.089(4) 0.037(4) -0.012(3) 0.017(3) C30 0.063(3) 0.099(4) 0.072(4) 0.043(3) -0.006(3) 0.010(3) C31 0.099(4) 0.181(6) 0.075(4) 0.035(4) -0.012(3) 0.062(4) C32 0.069(3) 0.099(4) 0.071(3) 0.030(3) 0.007(3) 0.017(3) C33 0.075(4) 0.125(4) 0.101(4) 0.034(4) 0.019(3) 0.043(3) C34 0.089(4) 0.130(5) 0.110(4) 0.065(4) 0.033(3) 0.036(3) C35 0.105(4) 0.110(4) 0.068(4) 0.003(3) -0.012(3) 0.053(3) C36 0.057(10) 0.069(15) 0.15(2) 0.040(15) 0.019(14) 0.011(11) C37 0.07(3) 0.07(3) 0.15(4) 0.04(3) 0.03(3) 0.010(19) C38 0.073(12) 0.073(14) 0.17(3) 0.038(17) 0.015(13) 0.010(10) C39 0.08(2) 0.09(2) 0.16(3) 0.06(3) 0.01(2) 0.002(17) C40 0.081(14) 0.10(2) 0.15(2) 0.036(19) 0.017(14) -0.008(13) C41 0.07(3) 0.07(3) 0.15(4) 0.04(4) 0.02(3) 0.00(2) C42 0.11(2) 0.12(3) 0.21(5) 0.09(2) -0.008(19) -0.004(16) _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 1.772(3) . ? Al1 C32 1.942(4) . ? Al1 C33 1.965(4) . ? Al1 N1 1.970(3) . ? Al2 O2 1.762(3) . ? Al2 C34 1.949(4) . ? Al2 C35 1.954(4) . ? Al2 N2 1.963(3) . ? N1 C2 1.292(4) . ? N1 C18 1.445(5) . ? N2 C10 1.297(4) . ? N2 C25 1.447(5) . ? O1 C4 1.331(4) . ? O2 C12 1.331(4) . ? C1 C5 1.515(5) . ? C1 C13 1.517(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.430(5) . ? C2 H2 0.9300 . ? C3 C4 1.409(5) . ? C3 C8 1.416(5) . ? C4 C5 1.414(5) . ? C5 C6 1.390(4) . ? C6 C7 1.396(5) . ? C6 H6 0.9300 . ? C7 C8 1.361(5) . ? C7 C9 1.518(5) . ? C8 H8 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.427(5) . ? C10 H10 0.9300 . ? C11 C16 1.417(4) . ? C11 C12 1.417(4) . ? C12 C13 1.409(5) . ? C13 C14 1.374(4) . ? C14 C15 1.405(4) . ? C14 H14 0.9300 . ? C15 C16 1.363(5) . ? C15 C17 1.515(4) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.373(5) . ? C18 C23 1.375(5) . ? C19 C20 1.387(5) . ? C19 H19 0.9300 . ? C20 C21 1.371(5) . ? C20 H20 0.9300 . ? C21 C22 1.369(5) . ? C21 C24 1.509(6) . ? C22 C23 1.375(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C30 1.366(5) . ? C25 C26 1.370(5) . ? C26 C27 1.386(6) . ? C26 H26 0.9300 . ? C27 C28 1.357(6) . ? C27 H27 0.9300 . ? C28 C29 1.367(5) . ? C28 C31 1.528(6) . ? C29 C30 1.384(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C39 1.12(7) 2_566 ? C36 C40 1.24(4) 2_566 ? C36 C38 1.32(4) 2_566 ? C36 C41 1.39(8) . ? C36 C37 1.39(9) . ? C36 C42 1.48(7) . ? C36 C41 1.52(11) 2_566 ? C36 C37 1.59(9) 2_566 ? C36 C36 1.67(6) 2_566 ? C37 C41 0.31(19) 2_566 ? C37 C40 1.12(12) 2_566 ? C37 C38 1.39(10) . ? C37 C36 1.59(9) 2_566 ? C37 H37 0.9300 . ? C38 C41 1.12(12) 2_566 ? C38 C36 1.32(4) 2_566 ? C38 C39 1.39(7) . ? C38 C42 1.67(7) 2_566 ? C38 H38 0.9300 . ? C39 C42 0.40(14) 2_566 ? C39 C36 1.12(7) 2_566 ? C39 C40 1.39(7) . ? C39 H39 0.9300 . ? C40 C37 1.12(12) 2_566 ? C40 C36 1.24(4) 2_566 ? C40 C41 1.39(11) . ? C40 C42 1.56(7) 2_566 ? C40 H40 0.9300 . ? C41 C37 0.31(19) 2_566 ? C41 C38 1.12(12) 2_566 ? C41 C36 1.52(11) 2_566 ? C41 H41 0.9300 . ? C42 C39 0.40(14) 2_566 ? C42 C40 1.56(7) 2_566 ? C42 C38 1.67(7) 2_566 ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 C32 112.55(16) . . ? O1 Al1 C33 111.28(18) . . ? C32 Al1 C33 119.36(17) . . ? O1 Al1 N1 94.45(14) . . ? C32 Al1 N1 108.57(17) . . ? C33 Al1 N1 107.53(17) . . ? O2 Al2 C34 110.61(18) . . ? O2 Al2 C35 112.69(16) . . ? C34 Al2 C35 118.14(19) . . ? O2 Al2 N2 94.59(13) . . ? C34 Al2 N2 111.68(16) . . ? C35 Al2 N2 106.55(17) . . ? C2 N1 C18 118.5(4) . . ? C2 N1 Al1 120.8(3) . . ? C18 N1 Al1 120.6(3) . . ? C10 N2 C25 117.1(3) . . ? C10 N2 Al2 122.2(3) . . ? C25 N2 Al2 120.3(3) . . ? C4 O1 Al1 128.2(3) . . ? C12 O2 Al2 132.5(2) . . ? C5 C1 C13 113.0(3) . . ? C5 C1 H1A 109.0 . . ? C13 C1 H1A 109.0 . . ? C5 C1 H1B 109.0 . . ? C13 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C3 126.7(4) . . ? N1 C2 H2 116.6 . . ? C3 C2 H2 116.6 . . ? C4 C3 C8 119.5(4) . . ? C4 C3 C2 122.6(4) . . ? C8 C3 C2 117.9(4) . . ? O1 C4 C3 121.6(4) . . ? O1 C4 C5 119.4(4) . . ? C3 C4 C5 118.9(4) . . ? C6 C5 C4 118.5(4) . . ? C6 C5 C1 121.6(4) . . ? C4 C5 C1 120.0(4) . . ? C5 C6 C7 123.5(4) . . ? C5 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C8 C7 C6 117.4(4) . . ? C8 C7 C9 122.0(4) . . ? C6 C7 C9 120.6(4) . . ? C7 C8 C3 122.2(4) . . ? C7 C8 H8 118.9 . . ? C3 C8 H8 118.9 . . ? 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 . . ? N2 C10 C11 126.9(4) . . ? N2 C10 H10 116.5 . . ? C11 C10 H10 116.5 . . ? C16 C11 C12 118.6(4) . . ? C16 C11 C10 118.3(4) . . ? C12 C11 C10 123.0(4) . . ? O2 C12 C13 120.1(4) . . ? O2 C12 C11 120.5(4) . . ? C13 C12 C11 119.4(3) . . ? C14 C13 C12 118.9(4) . . ? C14 C13 C1 121.6(4) . . ? C12 C13 C1 119.5(3) . . ? C13 C14 C15 123.3(4) . . ? C13 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C16 C15 C14 117.3(4) . . ? C16 C15 C17 122.1(4) . . ? C14 C15 C17 120.6(4) . . ? C15 C16 C11 122.5(4) . . ? C15 C16 H16 118.8 . . ? C11 C16 H16 118.8 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 118.6(4) . . ? C19 C18 N1 121.7(4) . . ? C23 C18 N1 119.7(4) . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 121.5(4) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C20 117.5(5) . . ? C22 C21 C24 121.5(5) . . ? C20 C21 C24 121.0(5) . . ? C21 C22 C23 121.8(5) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C18 C23 C22 120.4(5) . . ? C18 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? 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 . . ? C30 C25 C26 119.3(5) . . ? C30 C25 N2 120.8(4) . . ? C26 C25 N2 119.9(5) . . ? C25 C26 C27 119.7(5) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 121.7(5) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 117.9(5) . . ? C27 C28 C31 121.2(5) . . ? C29 C28 C31 120.9(5) . . ? C28 C29 C30 121.5(5) . . ? C28 C29 H29 119.2 . . ? C30 C29 H29 119.2 . . ? C25 C30 C29 119.8(4) . . ? C25 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Al1 C32 H32A 109.5 . . ? Al1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Al1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Al1 C33 H33A 109.5 . . ? Al1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Al1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al2 C34 H34A 109.5 . . ? Al2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Al2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Al2 C35 H35A 109.5 . . ? Al2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Al2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C40 72(4) 2_566 2_566 ? C39 C36 C38 69(3) 2_566 2_566 ? C40 C36 C38 140(4) 2_566 2_566 ? C39 C36 C41 118(6) 2_566 . ? C40 C36 C41 168(5) 2_566 . ? C38 C36 C41 49(5) 2_566 . ? C39 C36 C37 122(6) 2_566 . ? C40 C36 C37 50(5) 2_566 . ? C38 C36 C37 167(5) 2_566 . ? C41 C36 C37 120(8) . . ? C39 C36 C42 7(4) 2_566 . ? C40 C36 C42 69(4) 2_566 . ? C38 C36 C42 73(3) 2_566 . ? C41 C36 C42 121(6) . . ? C37 C36 C42 119(6) . . ? C39 C36 C41 131(6) 2_566 2_566 ? C40 C36 C41 60(4) 2_566 2_566 ? C38 C36 C41 156(5) 2_566 2_566 ? C41 C36 C41 110(5) . 2_566 ? C37 C36 C41 11(6) . 2_566 ? C42 C36 C41 129(6) . 2_566 ? C39 C36 C37 124(5) 2_566 2_566 ? C40 C36 C37 159(4) 2_566 2_566 ? C38 C36 C37 56(4) 2_566 2_566 ? C41 C36 C37 9(7) . 2_566 ? C37 C36 C37 112(4) . 2_566 ? C42 C36 C37 129(5) . 2_566 ? C41 C36 C37 102(6) 2_566 2_566 ? C39 C36 C36 168(3) 2_566 2_566 ? C40 C36 C36 111(3) 2_566 2_566 ? C38 C36 C36 106(4) 2_566 2_566 ? C41 C36 C36 59(5) . 2_566 ? C37 C36 C36 62(4) . 2_566 ? C42 C36 C36 175(3) . 2_566 ? C41 C36 C36 51(3) 2_566 2_566 ? C37 C36 C36 50(4) 2_566 2_566 ? C41 C37 C40 146(10) 2_566 2_566 ? C41 C37 C38 27(10) 2_566 . ? C40 C37 C38 173(7) 2_566 . ? C41 C37 C36 108(10) 2_566 . ? C40 C37 C36 58(4) 2_566 . ? C38 C37 C36 120(7) . . ? C41 C37 C36 45(10) 2_566 2_566 ? C40 C37 C36 124(6) 2_566 2_566 ? C38 C37 C36 52(4) . 2_566 ? C36 C37 C36 68(4) . 2_566 ? C41 C37 H37 125.4 2_566 . ? C40 C37 H37 62.6 2_566 . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.0 . . ? C36 C37 H37 170.8 2_566 . ? C41 C38 C36 69(5) 2_566 2_566 ? C41 C38 C39 117(6) 2_566 . ? C36 C38 C39 49(3) 2_566 . ? C41 C38 C37 7(7) 2_566 . ? C36 C38 C37 72(4) 2_566 . ? C39 C38 C37 120(4) . . ? C41 C38 C42 126(6) 2_566 2_566 ? C36 C38 C42 58(3) 2_566 2_566 ? C39 C38 C42 11(5) . 2_566 ? C37 C38 C42 130(4) . 2_566 ? C41 C38 H38 122.1 2_566 . ? C36 C38 H38 167.2 2_566 . ? C39 C38 H38 120.0 . . ? C37 C38 H38 119.9 . . ? C42 C38 H38 110.1 2_566 . ? C42 C39 C36 151(10) 2_566 2_566 ? C42 C39 C38 128(10) 2_566 . ? C36 C39 C38 63(4) 2_566 . ? C42 C39 C40 108(10) 2_566 . ? C36 C39 C40 58(3) 2_566 . ? C38 C39 C40 120(5) . . ? C42 C39 H39 21.7 2_566 . ? C36 C39 H39 172.9 2_566 . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C37 C40 C36 72(5) 2_566 2_566 ? C37 C40 C41 7(7) 2_566 . ? C36 C40 C41 70(4) 2_566 . ? C37 C40 C39 122(6) 2_566 . ? C36 C40 C39 50(3) 2_566 . ? C41 C40 C39 120(6) . . ? C37 C40 C42 134(6) 2_566 2_566 ? C36 C40 C42 63(3) 2_566 2_566 ? C41 C40 C42 133(6) . 2_566 ? C39 C40 C42 14(5) . 2_566 ? C37 C40 H40 117.4 2_566 . ? C36 C40 H40 168.2 2_566 . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.0 . . ? C42 C40 H40 106.7 2_566 . ? C37 C41 C38 146(10) 2_566 2_566 ? C37 C41 C36 125(10) 2_566 . ? C38 C41 C36 63(4) 2_566 . ? C37 C41 C40 27(10) 2_566 . ? C38 C41 C40 173(8) 2_566 . ? C36 C41 C40 120(8) . . ? C37 C41 C36 61(10) 2_566 2_566 ? C38 C41 C36 131(7) 2_566 2_566 ? C36 C41 C36 70(5) . 2_566 ? C40 C41 C36 50(4) . 2_566 ? C37 C41 H41 108.2 2_566 . ? C38 C41 H41 57.9 2_566 . ? C36 C41 H41 120.0 . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 168.9 2_566 . ? C39 C42 C36 21(10) 2_566 . ? C39 C42 C40 58(10) 2_566 2_566 ? C36 C42 C40 48(2) . 2_566 ? C39 C42 C38 41(10) 2_566 2_566 ? C36 C42 C38 49(3) . 2_566 ? C40 C42 C38 97(4) 2_566 2_566 ? C39 C42 H42A 89.5 2_566 . ? C36 C42 H42A 109.4 . . ? C40 C42 H42A 133.6 2_566 . ? C38 C42 H42A 68.8 2_566 . ? C39 C42 H42B 125.3 2_566 . ? C36 C42 H42B 109.5 . . ? C40 C42 H42B 116.3 2_566 . ? C38 C42 H42B 98.2 2_566 . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 111.3 2_566 . ? C36 C42 H42C 109.5 . . ? C40 C42 H42C 62.4 2_566 . ? C38 C42 H42C 150.5 2_566 . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 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 O1 Al1 N1 C2 -17.5(3) . . . . ? C32 Al1 N1 C2 -133.1(3) . . . . ? C33 Al1 N1 C2 96.5(3) . . . . ? O1 Al1 N1 C18 160.3(3) . . . . ? C32 Al1 N1 C18 44.7(3) . . . . ? C33 Al1 N1 C18 -85.7(3) . . . . ? O2 Al2 N2 C10 -1.3(3) . . . . ? C34 Al2 N2 C10 113.0(4) . . . . ? C35 Al2 N2 C10 -116.6(3) . . . . ? O2 Al2 N2 C25 171.4(3) . . . . ? C34 Al2 N2 C25 -74.3(4) . . . . ? C35 Al2 N2 C25 56.1(3) . . . . ? C32 Al1 O1 C4 139.0(3) . . . . ? C33 Al1 O1 C4 -84.0(3) . . . . ? N1 Al1 O1 C4 26.8(3) . . . . ? C34 Al2 O2 C12 -110.2(3) . . . . ? C35 Al2 O2 C12 115.1(3) . . . . ? N2 Al2 O2 C12 5.0(4) . . . . ? C18 N1 C2 C3 -174.7(4) . . . . ? Al1 N1 C2 C3 3.2(6) . . . . ? N1 C2 C3 C4 10.4(6) . . . . ? N1 C2 C3 C8 -171.7(4) . . . . ? Al1 O1 C4 C3 -20.6(5) . . . . ? Al1 O1 C4 C5 162.0(3) . . . . ? C8 C3 C4 O1 179.6(3) . . . . ? C2 C3 C4 O1 -2.5(6) . . . . ? C8 C3 C4 C5 -3.0(5) . . . . ? C2 C3 C4 C5 175.0(4) . . . . ? O1 C4 C5 C6 -179.7(3) . . . . ? C3 C4 C5 C6 2.9(5) . . . . ? O1 C4 C5 C1 -0.2(5) . . . . ? C3 C4 C5 C1 -177.7(3) . . . . ? C13 C1 C5 C6 87.4(4) . . . . ? C13 C1 C5 C4 -92.0(4) . . . . ? C4 C5 C6 C7 -0.5(5) . . . . ? C1 C5 C6 C7 -179.9(3) . . . . ? C5 C6 C7 C8 -1.7(6) . . . . ? C5 C6 C7 C9 178.9(3) . . . . ? C6 C7 C8 C3 1.6(6) . . . . ? C9 C7 C8 C3 -179.0(3) . . . . ? C4 C3 C8 C7 0.7(6) . . . . ? C2 C3 C8 C7 -177.3(4) . . . . ? C25 N2 C10 C11 -175.8(4) . . . . ? Al2 N2 C10 C11 -2.8(6) . . . . ? N2 C10 C11 C16 -177.3(4) . . . . ? N2 C10 C11 C12 4.7(7) . . . . ? Al2 O2 C12 C13 175.6(3) . . . . ? Al2 O2 C12 C11 -4.4(5) . . . . ? C16 C11 C12 O2 -179.1(3) . . . . ? C10 C11 C12 O2 -1.1(6) . . . . ? C16 C11 C12 C13 1.0(5) . . . . ? C10 C11 C12 C13 178.9(3) . . . . ? O2 C12 C13 C14 178.9(3) . . . . ? C11 C12 C13 C14 -1.2(5) . . . . ? O2 C12 C13 C1 -0.5(5) . . . . ? C11 C12 C13 C1 179.4(3) . . . . ? C5 C1 C13 C14 96.9(4) . . . . ? C5 C1 C13 C12 -83.7(4) . . . . ? C12 C13 C14 C15 0.7(6) . . . . ? C1 C13 C14 C15 -179.9(3) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C13 C14 C15 C17 -178.7(4) . . . . ? C14 C15 C16 C11 -0.3(6) . . . . ? C17 C15 C16 C11 178.4(4) . . . . ? C12 C11 C16 C15 -0.2(6) . . . . ? C10 C11 C16 C15 -178.3(4) . . . . ? C2 N1 C18 C19 50.8(6) . . . . ? Al1 N1 C18 C19 -127.0(4) . . . . ? C2 N1 C18 C23 -131.0(4) . . . . ? Al1 N1 C18 C23 51.1(5) . . . . ? C23 C18 C19 C20 0.6(6) . . . . ? N1 C18 C19 C20 178.8(4) . . . . ? C18 C19 C20 C21 -0.4(7) . . . . ? C19 C20 C21 C22 0.5(7) . . . . ? C19 C20 C21 C24 -180.0(4) . . . . ? C20 C21 C22 C23 -0.8(7) . . . . ? C24 C21 C22 C23 179.6(5) . . . . ? C19 C18 C23 C22 -0.9(7) . . . . ? N1 C18 C23 C22 -179.2(4) . . . . ? C21 C22 C23 C18 1.1(7) . . . . ? C10 N2 C25 C30 52.6(5) . . . . ? Al2 N2 C25 C30 -120.5(4) . . . . ? C10 N2 C25 C26 -129.2(4) . . . . ? Al2 N2 C25 C26 57.7(5) . . . . ? C30 C25 C26 C27 -2.6(7) . . . . ? N2 C25 C26 C27 179.1(4) . . . . ? C25 C26 C27 C28 2.7(7) . . . . ? C26 C27 C28 C29 -1.3(8) . . . . ? C26 C27 C28 C31 179.1(4) . . . . ? C27 C28 C29 C30 -0.2(7) . . . . ? C31 C28 C29 C30 179.4(4) . . . . ? C26 C25 C30 C29 1.2(7) . . . . ? N2 C25 C30 C29 179.5(4) . . . . ? C28 C29 C30 C25 0.2(7) . . . . ? C39 C36 C37 C41 145(35) 2_566 . . 2_566 ? C40 C36 C37 C41 145(39) 2_566 . . 2_566 ? C38 C36 C37 C41 0(54) 2_566 . . 2_566 ? C41 C36 C37 C41 -27(42) . . . 2_566 ? C42 C36 C37 C41 153(35) . . . 2_566 ? C37 C36 C37 C41 -22(35) 2_566 . . 2_566 ? C36 C36 C37 C41 -22(35) 2_566 . . 2_566 ? C39 C36 C37 C40 0(6) 2_566 . . 2_566 ? C38 C36 C37 C40 -146(17) 2_566 . . 2_566 ? C41 C36 C37 C40 -172(4) . . . 2_566 ? C42 C36 C37 C40 8(5) . . . 2_566 ? C41 C36 C37 C40 -145(39) 2_566 . . 2_566 ? C37 C36 C37 C40 -167(5) 2_566 . . 2_566 ? C36 C36 C37 C40 -167(5) 2_566 . . 2_566 ? C39 C36 C37 C38 172(5) 2_566 . . . ? C40 C36 C37 C38 172(8) 2_566 . . . ? C38 C36 C37 C38 26(24) 2_566 . . . ? C41 C36 C37 C38 0(11) . . . . ? C42 C36 C37 C38 180(5) . . . . ? C41 C36 C37 C38 27(32) 2_566 . . . ? C37 C36 C37 C38 5(4) 2_566 . . . ? C36 C36 C37 C38 5(4) 2_566 . . . ? C39 C36 C37 C36 167(3) 2_566 . . 2_566 ? C40 C36 C37 C36 167(5) 2_566 . . 2_566 ? C38 C36 C37 C36 21(20) 2_566 . . 2_566 ? C41 C36 C37 C36 -5(8) . . . 2_566 ? C42 C36 C37 C36 175(3) . . . 2_566 ? C41 C36 C37 C36 22(35) 2_566 . . 2_566 ? C37 C36 C37 C36 0.000(6) 2_566 . . 2_566 ? C40 C37 C38 C41 0(32) 2_566 . . 2_566 ? C36 C37 C38 C41 -70(58) . . . 2_566 ? C36 C37 C38 C41 -64(59) 2_566 . . 2_566 ? C41 C37 C38 C36 64(59) 2_566 . . 2_566 ? C40 C37 C38 C36 64(63) 2_566 . . 2_566 ? C36 C37 C38 C36 -6(5) . . . 2_566 ? C41 C37 C38 C39 70(60) 2_566 . . . ? C40 C37 C38 C39 70(65) 2_566 . . . ? C36 C37 C38 C39 0(8) . . . . ? C36 C37 C38 C39 6(4) 2_566 . . . ? C41 C37 C38 C42 65(61) 2_566 . . 2_566 ? C40 C37 C38 C42 65(66) 2_566 . . 2_566 ? C36 C37 C38 C42 -6(9) . . . 2_566 ? C36 C37 C38 C42 0(5) 2_566 . . 2_566 ? C41 C38 C39 C42 -148(18) 2_566 . . 2_566 ? C36 C38 C39 C42 -148(20) 2_566 . . 2_566 ? C37 C38 C39 C42 -156(18) . . . 2_566 ? C41 C38 C39 C36 0(6) 2_566 . . 2_566 ? C37 C38 C39 C36 -8(5) . . . 2_566 ? C42 C38 C39 C36 148(20) 2_566 . . 2_566 ? C41 C38 C39 C40 8(7) 2_566 . . . ? C36 C38 C39 C40 8(2) 2_566 . . . ? C37 C38 C39 C40 0(6) . . . . ? C42 C38 C39 C40 156(21) 2_566 . . . ? C42 C39 C40 C37 152(16) 2_566 . . 2_566 ? C36 C39 C40 C37 0(6) 2_566 . . 2_566 ? C38 C39 C40 C37 -8(7) . . . 2_566 ? C42 C39 C40 C36 152(17) 2_566 . . 2_566 ? C38 C39 C40 C36 -8(2) . . . 2_566 ? C42 C39 C40 C41 160(16) 2_566 . . . ? C36 C39 C40 C41 8(5) 2_566 . . . ? C38 C39 C40 C41 0(6) . . . . ? C36 C39 C40 C42 -152(17) 2_566 . . 2_566 ? C38 C39 C40 C42 -160(19) . . . 2_566 ? C39 C36 C41 C37 -141(45) 2_566 . . 2_566 ? C40 C36 C41 C37 1(65) 2_566 . . 2_566 ? C38 C36 C41 C37 -141(48) 2_566 . . 2_566 ? C37 C36 C41 C37 32(51) . . . 2_566 ? C42 C36 C41 C37 -148(45) . . . 2_566 ? C41 C36 C41 C37 26(44) 2_566 . . 2_566 ? C36 C36 C41 C37 26(44) 2_566 . . 2_566 ? C39 C36 C41 C38 0(6) 2_566 . . 2_566 ? C40 C36 C41 C38 142(19) 2_566 . . 2_566 ? C37 C36 C41 C38 172(3) . . . 2_566 ? C42 C36 C41 C38 -7(6) . . . 2_566 ? C41 C36 C41 C38 167(5) 2_566 . . 2_566 ? C37 C36 C41 C38 141(48) 2_566 . . 2_566 ? C36 C36 C41 C38 167(5) 2_566 . . 2_566 ? C39 C36 C41 C40 -172(5) 2_566 . . . ? C40 C36 C41 C40 -31(26) 2_566 . . . ? C38 C36 C41 C40 -172(9) 2_566 . . . ? C37 C36 C41 C40 0(12) . . . . ? C42 C36 C41 C40 -180(5) . . . . ? C41 C36 C41 C40 -5(4) 2_566 . . . ? C37 C36 C41 C40 -31(41) 2_566 . . . ? C36 C36 C41 C40 -5(4) 2_566 . . . ? C39 C36 C41 C36 -167(3) 2_566 . . 2_566 ? C40 C36 C41 C36 -25(23) 2_566 . . 2_566 ? C38 C36 C41 C36 -167(5) 2_566 . . 2_566 ? C37 C36 C41 C36 5(8) . . . 2_566 ? C42 C36 C41 C36 -175(3) . . . 2_566 ? C41 C36 C41 C36 0.000(4) 2_566 . . 2_566 ? C37 C36 C41 C36 -26(44) 2_566 . . 2_566 ? C36 C40 C41 C37 -103(59) 2_566 . . 2_566 ? C39 C40 C41 C37 -110(58) . . . 2_566 ? C42 C40 C41 C37 -103(58) 2_566 . . 2_566 ? C37 C40 C41 C38 0(32) 2_566 . . 2_566 ? C36 C40 C41 C38 -103(69) 2_566 . . 2_566 ? C39 C40 C41 C38 -110(68) . . . 2_566 ? C42 C40 C41 C38 -103(68) 2_566 . . 2_566 ? C37 C40 C41 C36 110(61) 2_566 . . . ? C36 C40 C41 C36 6(5) 2_566 . . . ? C39 C40 C41 C36 0(8) . . . . ? C42 C40 C41 C36 6(10) 2_566 . . . ? C37 C40 C41 C36 103(59) 2_566 . . 2_566 ? C39 C40 C41 C36 -6(4) . . . 2_566 ? C42 C40 C41 C36 0(6) 2_566 . . 2_566 ? C40 C36 C42 C39 -110(40) 2_566 . . 2_566 ? C38 C36 C42 C39 57(39) 2_566 . . 2_566 ? C41 C36 C42 C39 63(40) . . . 2_566 ? C37 C36 C42 C39 -117(39) . . . 2_566 ? C41 C36 C42 C39 -110(39) 2_566 . . 2_566 ? C37 C36 C42 C39 57(41) 2_566 . . 2_566 ? C36 C36 C42 C39 -21(87) 2_566 . . 2_566 ? C39 C36 C42 C40 110(40) 2_566 . . 2_566 ? C38 C36 C42 C40 167.7(19) 2_566 . . 2_566 ? C41 C36 C42 C40 174(4) . . . 2_566 ? C37 C36 C42 C40 -6(4) . . . 2_566 ? C41 C36 C42 C40 0(5) 2_566 . . 2_566 ? C37 C36 C42 C40 167(4) 2_566 . . 2_566 ? C36 C36 C42 C40 90(62) 2_566 . . 2_566 ? C39 C36 C42 C38 -57(39) 2_566 . . 2_566 ? C40 C36 C42 C38 -167.7(19) 2_566 . . 2_566 ? C41 C36 C42 C38 6(5) . . . 2_566 ? C37 C36 C42 C38 -174(4) . . . 2_566 ? C41 C36 C42 C38 -168(5) 2_566 . . 2_566 ? C37 C36 C42 C38 0(5) 2_566 . . 2_566 ? C36 C36 C42 C38 -78(62) 2_566 . . 2_566 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.179 _refine_diff_density_min -0.140 _refine_diff_density_rms 0.037