# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- complex 5.cif' #============================================================================== _audit_creation_method SHELXL-97 # 1. Submission Details _publ_contact_author_name 'Haiyan Ma' _publ_contact_author_address ; Shanghai Key Laboratory of Functional Materials Chemistry and Laboratory of Organometallic Chemistry East China University of Science and Technology 130 Meilong Road, P.O.Box 310# 200237,Shanghai P. R. China ; _publ_contact_author_phone '0086 21 64253519' _publ_contact_author_fax '0086 21 64253519' _publ_contact_author_email haiyanma@ecust.edu.cn _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; This crystal structure is part of a manuscript that is submitted for publication in the Journal 'Chemical Communications' ; #============================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; Exploitation of dinuclear salan aluminum complexes for versatile copolymerization of epsilon-caprolactone and L-lactide ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address W.Yuan ; Shanghai Key Laboratory of Functional Materials Chemistry and Laboratory of Organometallic Chemistry East China University of Science and Technology 130 Meilong Road, P.O.Box 310# 200237 Shanghai P.R.China ; M.Haiyan ; Shanghai Key Laboratory of Functional Materials Chemistry and Laboratory of Organometallic Chemistry East China University of Science and Technology 130 Meilong Road, P.P.Box 310# 200237 Shanghai P.R.China ; #=========================================================================== data_cd211303 _database_code_depnum_ccdc_archive 'CCDC 870489' #TrackingRef '- complex 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H68 Al2 N2 O2' _chemical_formula_weight 650.91 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.154(4) _cell_length_b 7.8830(8) _cell_length_c 12.4485(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.660(2) _cell_angle_gamma 90.00 _cell_volume 4123.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1650 _cell_measurement_theta_min 5.258 _cell_measurement_theta_max 41.492 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.316 _exptl_crystal_size_mid 0.305 _exptl_crystal_size_min 0.127 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.66452 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 10713 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4047 _reflns_number_gt 2545 _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^)+(0.0793P)^2^+1.0325P] 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 4047 _refine_ls_number_parameters 243 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.051649(15) 0.81380(9) 0.41600(6) 0.0435(2) Uani 1 1 d . . . N1 N 0.05811(4) 0.6187(2) 0.31186(14) 0.0396(5) Uani 1 1 d . . . O1 O 0.08794(4) 0.7957(2) 0.49305(14) 0.0553(5) Uani 1 1 d . . . C1 C 0.11557(5) 0.7362(3) 0.4604(2) 0.0459(6) Uani 1 1 d . . . C2 C 0.14485(5) 0.8131(3) 0.4930(2) 0.0461(6) Uani 1 1 d . . . C3 C 0.17182(5) 0.7419(3) 0.4545(2) 0.0528(7) Uani 1 1 d . . . H3 H 0.1914 0.7909 0.4759 0.063 Uiso 1 1 calc R . . C4 C 0.17162(5) 0.6033(3) 0.3865(2) 0.0523(7) Uani 1 1 d . A . C5 C 0.14241(5) 0.5305(3) 0.3570(2) 0.0535(7) Uani 1 1 d . . . H5 H 0.1414 0.4372 0.3111 0.064 Uiso 1 1 calc R . . C6 C 0.11446(5) 0.5935(3) 0.3941(2) 0.0475(6) Uani 1 1 d . . . C7 C 0.08306(5) 0.5064(3) 0.3678(2) 0.0500(6) Uani 1 1 d . . . H7A H 0.0864 0.4092 0.3223 0.060 Uiso 1 1 calc R . . H7B H 0.0753 0.4647 0.4341 0.060 Uiso 1 1 calc R . . C8 C 0.02873(5) 0.5171(3) 0.2866(2) 0.0460(6) Uani 1 1 d . . . H8A H 0.0241 0.4537 0.3504 0.055 Uiso 1 1 calc R . . H8B H 0.0326 0.4359 0.2306 0.055 Uiso 1 1 calc R . . C9 C 0.0000 0.6224(5) 0.2500 0.0526(9) Uani 1 2 d S . . H9A H -0.0053 0.6950 0.3089 0.063 Uiso 0.50 1 calc PR . . H9B H 0.0053 0.6950 0.1911 0.063 Uiso 0.50 1 calc PR . . C10 C 0.07031(6) 0.6786(4) 0.2090(2) 0.0619(8) Uani 1 1 d . . . H10A H 0.0739 0.5828 0.1640 0.093 Uiso 1 1 calc R . . H10B H 0.0899 0.7388 0.2246 0.093 Uiso 1 1 calc R . . H10C H 0.0549 0.7527 0.1723 0.093 Uiso 1 1 calc R . . C11 C 0.14652(6) 0.9680(3) 0.5678(2) 0.0559(7) Uani 1 1 d . . . C12 C 0.13137(8) 0.9284(4) 0.6729(2) 0.0753(9) Uani 1 1 d . . . H12A H 0.1093 0.9019 0.6571 0.113 Uiso 1 1 calc R . . H12B H 0.1334 1.0253 0.7197 0.113 Uiso 1 1 calc R . . H12C H 0.1420 0.8332 0.7078 0.113 Uiso 1 1 calc R . . C13 C 0.12908(8) 1.1186(4) 0.5112(3) 0.0760(9) Uani 1 1 d . . . H13A H 0.1380 1.1409 0.4441 0.114 Uiso 1 1 calc R . . H13B H 0.1314 1.2171 0.5564 0.114 Uiso 1 1 calc R . . H13C H 0.1069 1.0918 0.4976 0.114 Uiso 1 1 calc R . . C14 C 0.18096(7) 1.0213(4) 0.5987(3) 0.0912(11) Uani 1 1 d . . . H14A H 0.1924 0.9284 0.6335 0.137 Uiso 1 1 calc R . . H14B H 0.1812 1.1163 0.6471 0.137 Uiso 1 1 calc R . . H14C H 0.1909 1.0528 0.5350 0.137 Uiso 1 1 calc R . . C15 C 0.20255(6) 0.5291(4) 0.3491(3) 0.0684(8) Uani 1 1 d D . . C16 C 0.22508(17) 0.6713(11) 0.3208(6) 0.097(3) Uani 0.70 1 d PDU A 1 H16A H 0.2445 0.6230 0.2995 0.145 Uiso 0.70 1 calc PR A 1 H16B H 0.2297 0.7426 0.3826 0.145 Uiso 0.70 1 calc PR A 1 H16C H 0.2152 0.7375 0.2626 0.145 Uiso 0.70 1 calc PR A 1 C17 C 0.22256(15) 0.4628(10) 0.4609(7) 0.088(2) Uani 0.50 1 d PDU A 1 H17A H 0.2097 0.3844 0.4974 0.132 Uiso 0.50 1 calc PR A 1 H17B H 0.2279 0.5581 0.5069 0.132 Uiso 0.50 1 calc PR A 1 H17C H 0.2417 0.4074 0.4433 0.132 Uiso 0.50 1 calc PR A 1 C18 C 0.19867(18) 0.3877(15) 0.2773(10) 0.130(4) Uani 0.50 1 d PDU A 1 H18A H 0.2192 0.3492 0.2593 0.194 Uiso 0.50 1 calc PR A 1 H18B H 0.1862 0.4214 0.2129 0.194 Uiso 0.50 1 calc PR A 1 H18C H 0.1880 0.2975 0.3117 0.194 Uiso 0.50 1 calc PR A 1 C16' C 0.2314(3) 0.630(2) 0.3746(15) 0.090(5) Uani 0.30 1 d PDU A 2 H16D H 0.2483 0.5862 0.3357 0.135 Uiso 0.30 1 calc PR A 2 H16E H 0.2373 0.6240 0.4506 0.135 Uiso 0.30 1 calc PR A 2 H16F H 0.2273 0.7460 0.3542 0.135 Uiso 0.30 1 calc PR A 2 C17' C 0.20782(19) 0.3564(11) 0.3923(7) 0.096(3) Uani 0.50 1 d PDU A 2 H17D H 0.1909 0.2835 0.3640 0.144 Uiso 0.50 1 calc PR A 2 H17E H 0.2082 0.3593 0.4695 0.144 Uiso 0.50 1 calc PR A 2 H17F H 0.2278 0.3139 0.3717 0.144 Uiso 0.50 1 calc PR A 2 C18' C 0.19685(17) 0.4999(9) 0.2178(5) 0.072(2) Uani 0.50 1 d PDU A 2 H18D H 0.2148 0.4410 0.1928 0.108 Uiso 0.50 1 calc PR A 2 H18E H 0.1945 0.6079 0.1823 0.108 Uiso 0.50 1 calc PR A 2 H18F H 0.1779 0.4338 0.2018 0.108 Uiso 0.50 1 calc PR A 2 C19 C 0.04687(7) 1.0215(4) 0.3318(3) 0.0742(9) Uani 1 1 d . . . H19A H 0.0434 1.1151 0.3787 0.111 Uiso 1 1 calc R . . H19B H 0.0290 1.0106 0.2791 0.111 Uiso 1 1 calc R . . H19C H 0.0659 1.0413 0.2959 0.111 Uiso 1 1 calc R . . C20 C 0.01893(6) 0.7521(4) 0.5112(2) 0.0679(8) Uani 1 1 d . . . H20A H 0.0181 0.6309 0.5178 0.102 Uiso 1 1 calc R . . H20B H -0.0014 0.7934 0.4815 0.102 Uiso 1 1 calc R . . H20C H 0.0239 0.8016 0.5809 0.102 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 0.0329(4) 0.0416(4) 0.0571(5) -0.0028(4) 0.0102(3) 0.0019(3) N1 0.0289(9) 0.0440(11) 0.0460(11) 0.0006(9) 0.0044(8) -0.0009(8) O1 0.0370(9) 0.0630(12) 0.0659(12) -0.0189(9) 0.0037(8) 0.0072(8) C1 0.0341(13) 0.0466(15) 0.0566(15) -0.0062(12) 0.0020(11) 0.0054(11) C2 0.0367(12) 0.0425(14) 0.0582(15) -0.0032(12) -0.0016(11) -0.0017(11) C3 0.0318(13) 0.0537(16) 0.0719(18) -0.0009(14) -0.0017(11) -0.0060(11) C4 0.0319(12) 0.0534(16) 0.0719(18) -0.0054(14) 0.0054(12) 0.0031(11) C5 0.0355(13) 0.0518(16) 0.0732(18) -0.0144(14) 0.0036(12) 0.0054(11) C6 0.0310(12) 0.0458(15) 0.0648(16) -0.0074(13) -0.0008(11) 0.0020(10) C7 0.0369(13) 0.0445(15) 0.0678(17) -0.0062(13) -0.0006(11) 0.0047(11) C8 0.0319(12) 0.0487(15) 0.0570(15) -0.0049(12) 0.0018(10) -0.0026(10) C9 0.0350(18) 0.054(2) 0.067(2) 0.000 -0.0045(16) 0.000 C10 0.0501(15) 0.082(2) 0.0556(16) -0.0020(15) 0.0157(12) -0.0062(14) C11 0.0508(15) 0.0479(16) 0.0674(18) -0.0106(14) -0.0043(13) -0.0011(12) C12 0.085(2) 0.075(2) 0.064(2) -0.0154(17) -0.0035(16) 0.0095(18) C13 0.089(2) 0.0467(18) 0.090(2) -0.0058(17) -0.0033(18) 0.0005(16) C14 0.065(2) 0.078(2) 0.127(3) -0.042(2) -0.0141(19) -0.0125(17) C15 0.0362(14) 0.070(2) 0.101(2) -0.0059(19) 0.0182(15) 0.0075(14) C16 0.052(4) 0.129(6) 0.113(6) 0.027(5) 0.028(3) 0.011(4) C17 0.053(4) 0.086(5) 0.126(7) 0.026(5) 0.010(4) 0.027(4) C18 0.048(4) 0.160(9) 0.184(10) -0.087(8) 0.035(6) 0.009(5) C16' 0.033(6) 0.105(11) 0.132(13) -0.036(10) 0.010(8) 0.002(7) C17' 0.076(5) 0.118(7) 0.097(6) 0.024(5) 0.027(4) 0.055(5) C18' 0.066(4) 0.072(5) 0.082(5) 0.002(4) 0.032(3) 0.017(4) C19 0.072(2) 0.0531(18) 0.099(2) 0.0121(17) 0.0157(17) 0.0018(15) C20 0.0570(17) 0.085(2) 0.0642(18) -0.0098(16) 0.0212(14) -0.0013(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7441(17) . ? Al1 C19 1.946(3) . ? Al1 C20 1.951(3) . ? Al1 N1 2.044(2) . ? N1 C8 1.487(3) . ? N1 C10 1.495(3) . ? N1 C7 1.502(3) . ? O1 C1 1.349(3) . ? C1 C6 1.393(3) . ? C1 C2 1.405(3) . ? C2 C3 1.388(3) . ? C2 C11 1.534(3) . ? C3 C4 1.382(4) . ? C3 H3 0.9300 . ? C4 C5 1.381(3) . ? C4 C15 1.535(3) . ? C5 C6 1.392(3) . ? C5 H5 0.9300 . ? C6 C7 1.503(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.508(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C8 1.508(3) 2 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C14 1.531(4) . ? C11 C12 1.534(4) . ? C11 C13 1.537(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C18 1.430(8) . ? C15 C16' 1.464(13) . ? C15 C17' 1.475(7) . ? C15 C16 1.528(8) . ? C15 C18' 1.649(7) . ? C15 C17 1.653(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 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 . ? 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 C19 114.38(12) . . ? O1 Al1 C20 106.10(11) . . ? C19 Al1 C20 119.31(13) . . ? O1 Al1 N1 97.54(8) . . ? C19 Al1 N1 107.74(11) . . ? C20 Al1 N1 109.55(11) . . ? C8 N1 C10 109.15(19) . . ? C8 N1 C7 108.71(18) . . ? C10 N1 C7 107.87(18) . . ? C8 N1 Al1 112.79(14) . . ? C10 N1 Al1 112.23(16) . . ? C7 N1 Al1 105.87(14) . . ? C1 O1 Al1 127.08(16) . . ? O1 C1 C6 118.1(2) . . ? O1 C1 C2 121.5(2) . . ? C6 C1 C2 120.4(2) . . ? C3 C2 C1 116.8(2) . . ? C3 C2 C11 122.2(2) . . ? C1 C2 C11 121.0(2) . . ? C4 C3 C2 124.5(2) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C5 C4 C3 116.9(2) . . ? C5 C4 C15 121.5(2) . . ? C3 C4 C15 121.6(2) . . ? C4 C5 C6 121.6(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.8(2) . . ? C5 C6 C7 121.3(2) . . ? C1 C6 C7 118.9(2) . . ? N1 C7 C6 113.8(2) . . ? N1 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C9 113.7(2) . . ? N1 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? N1 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C8 113.2(3) 2 . ? C8 C9 H9A 108.9 2 . ? C8 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 2 . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C2 111.5(2) . . ? C14 C11 C12 107.1(2) . . ? C2 C11 C12 110.8(2) . . ? C14 C11 C13 108.2(2) . . ? C2 C11 C13 109.8(2) . . ? C12 C11 C13 109.4(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 . . ? C18 C15 C16' 127.6(8) . . ? C18 C15 C17' 60.9(6) . . ? C16' C15 C17' 108.9(8) . . ? C18 C15 C16 118.0(6) . . ? C16' C15 C16 29.8(7) . . ? C17' C15 C16 133.1(5) . . ? C18 C15 C4 115.4(4) . . ? C16' C15 C4 115.9(7) . . ? C17' C15 C4 110.3(3) . . ? C16 C15 C4 110.5(4) . . ? C18 C15 C18' 43.3(6) . . ? C16' C15 C18' 110.0(8) . . ? C17' C15 C18' 103.8(5) . . ? C16 C15 C18' 85.3(4) . . ? C4 C15 C18' 107.1(3) . . ? C18 C15 C17 107.7(6) . . ? C16' C15 C17 68.4(7) . . ? C17' C15 C17 49.4(4) . . ? C16 C15 C17 98.1(4) . . ? C4 C15 C17 104.7(3) . . ? C18' C15 C17 144.5(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? C15 C16' H16D 109.5 . . ? C15 C16' H16E 109.5 . . ? H16D C16' H16E 109.5 . . ? C15 C16' H16F 109.5 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C15 C17' H17D 109.5 . . ? C15 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C15 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C15 C18' H18D 109.5 . . ? C15 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C15 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? Al1 C19 H19A 109.5 . . ? Al1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al1 C20 H20A 109.5 . . ? Al1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 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 C8 139.96(16) . . . . ? C19 Al1 N1 C8 -101.39(17) . . . . ? C20 Al1 N1 C8 29.84(19) . . . . ? O1 Al1 N1 C10 -96.25(16) . . . . ? C19 Al1 N1 C10 22.40(19) . . . . ? C20 Al1 N1 C10 153.63(17) . . . . ? O1 Al1 N1 C7 21.20(15) . . . . ? C19 Al1 N1 C7 139.85(16) . . . . ? C20 Al1 N1 C7 -88.92(16) . . . . ? C19 Al1 O1 C1 -84.9(2) . . . . ? C20 Al1 O1 C1 141.4(2) . . . . ? N1 Al1 O1 C1 28.5(2) . . . . ? Al1 O1 C1 C6 -41.2(3) . . . . ? Al1 O1 C1 C2 139.7(2) . . . . ? O1 C1 C2 C3 -179.9(2) . . . . ? C6 C1 C2 C3 1.1(4) . . . . ? O1 C1 C2 C11 0.3(4) . . . . ? C6 C1 C2 C11 -178.7(2) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C11 C2 C3 C4 -179.6(2) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? C2 C3 C4 C15 -178.7(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C15 C4 C5 C6 177.5(3) . . . . ? C4 C5 C6 C1 1.8(4) . . . . ? C4 C5 C6 C7 -175.7(2) . . . . ? O1 C1 C6 C5 178.7(2) . . . . ? C2 C1 C6 C5 -2.3(4) . . . . ? O1 C1 C6 C7 -3.8(4) . . . . ? C2 C1 C6 C7 175.3(2) . . . . ? C8 N1 C7 C6 177.9(2) . . . . ? C10 N1 C7 C6 59.7(3) . . . . ? Al1 N1 C7 C6 -60.7(2) . . . . ? C5 C6 C7 N1 -123.1(3) . . . . ? C1 C6 C7 N1 59.4(3) . . . . ? C10 N1 C8 C9 -73.8(2) . . . . ? C7 N1 C8 C9 168.78(17) . . . . ? Al1 N1 C8 C9 51.7(2) . . . . ? N1 C8 C9 C8 173.8(2) . . . 2 ? C3 C2 C11 C14 -4.0(4) . . . . ? C1 C2 C11 C14 175.8(3) . . . . ? C3 C2 C11 C12 -123.2(3) . . . . ? C1 C2 C11 C12 56.7(3) . . . . ? C3 C2 C11 C13 115.9(3) . . . . ? C1 C2 C11 C13 -64.3(3) . . . . ? C5 C4 C15 C18 3.6(8) . . . . ? C3 C4 C15 C18 -178.9(7) . . . . ? C5 C4 C15 C16' 172.6(8) . . . . ? C3 C4 C15 C16' -9.9(9) . . . . ? C5 C4 C15 C17' -63.0(6) . . . . ? C3 C4 C15 C17' 114.5(5) . . . . ? C5 C4 C15 C16 140.7(4) . . . . ? C3 C4 C15 C16 -41.8(5) . . . . ? C5 C4 C15 C18' 49.4(4) . . . . ? C3 C4 C15 C18' -133.1(4) . . . . ? C5 C4 C15 C17 -114.6(4) . . . . ? C3 C4 C15 C17 62.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.270 _refine_diff_density_min -0.134 _refine_diff_density_rms 0.044 data_a00514a _database_code_depnum_ccdc_archive 'CCDC 870490' #TrackingRef '- complex 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H76 Al2 N2 O2' _chemical_formula_weight 899.18 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 Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.068(6) _cell_length_b 20.068(6) _cell_length_c 28.016(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11282(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 911 _cell_measurement_theta_min 2.382 _cell_measurement_theta_max 24.304 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9864 _exptl_absorpt_correction_T_max 0.9927 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_% 4.32 _diffrn_reflns_number 27283 _diffrn_reflns_av_R_equivalents 0.1012 _diffrn_reflns_av_sigmaI/netI 0.0983 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.01 _reflns_number_total 6131 _reflns_number_gt 2739 _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^)+(0.0875P)^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 6131 _refine_ls_number_parameters 301 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.83680(4) 0.22266(4) 0.02497(3) 0.0524(2) Uani 1 1 d . . . O1 O 0.75803(8) 0.26004(8) 0.02509(6) 0.0517(5) Uani 1 1 d . . . N1 N 0.88445(9) 0.30035(10) -0.00604(7) 0.0477(5) Uani 1 1 d . . . C1 C 0.87000(15) 0.20828(18) 0.08957(9) 0.0817(10) Uani 1 1 d . . . H1A H 0.8714 0.2500 0.1063 0.123 Uiso 1 1 calc R . . H1B H 0.9140 0.1896 0.0881 0.123 Uiso 1 1 calc R . . H1C H 0.8409 0.1781 0.1061 0.123 Uiso 1 1 calc R . . C2 C 0.84333(16) 0.14873(16) -0.01950(13) 0.0880(10) Uani 1 1 d . . . H2A H 0.8152 0.1130 -0.0089 0.132 Uiso 1 1 calc R . . H2B H 0.8887 0.1336 -0.0209 0.132 Uiso 1 1 calc R . . H2C H 0.8294 0.1631 -0.0506 0.132 Uiso 1 1 calc R . . C3 C 0.73542(11) 0.31741(12) 0.00699(8) 0.0436(6) Uani 1 1 d . . . C4 C 0.67312(12) 0.34272(12) 0.02176(8) 0.0457(6) Uani 1 1 d . . . C5 C 0.65038(13) 0.40084(13) 0.00062(10) 0.0562(7) Uani 1 1 d . . . H5 H 0.6085 0.4166 0.0092 0.067 Uiso 1 1 calc R . . C6 C 0.68680(13) 0.43694(13) -0.03277(10) 0.0601(7) Uani 1 1 d . . . C7 C 0.74876(13) 0.41250(13) -0.04475(10) 0.0573(7) Uani 1 1 d . . . H7 H 0.7750 0.4363 -0.0661 0.069 Uiso 1 1 calc R . . C8 C 0.77307(12) 0.35333(12) -0.02586(9) 0.0466(6) Uani 1 1 d . . . C9 C 0.83794(12) 0.32526(13) -0.04405(8) 0.0516(6) Uani 1 1 d . . . H9A H 0.8281 0.2888 -0.0657 0.062 Uiso 1 1 calc R . . H9B H 0.8606 0.3595 -0.0623 0.062 Uiso 1 1 calc R . . C10 C 0.94732(12) 0.28068(14) -0.03109(9) 0.0586(7) Uani 1 1 d . . . H10A H 0.9660 0.3199 -0.0463 0.070 Uiso 1 1 calc R . . H10B H 0.9362 0.2491 -0.0561 0.070 Uiso 1 1 calc R . . C11 C 1.0000 0.2500 0.00041(14) 0.0628(11) Uani 1 2 d S . . H11A H 1.0197 0.2839 0.0207 0.075 Uiso 0.50 1 calc PR . . H11B H 0.9803 0.2161 0.0207 0.075 Uiso 0.50 1 calc PR . . C12 C 0.63365(12) 0.30436(13) 0.05967(9) 0.0528(7) Uani 1 1 d . . . C13 C 0.67685(13) 0.29581(13) 0.10435(9) 0.0507(6) Uani 1 1 d . . . C14 C 0.71600(13) 0.34808(14) 0.12028(10) 0.0591(7) Uani 1 1 d . . . H14 H 0.7158 0.3879 0.1033 0.071 Uiso 1 1 calc R . . C15 C 0.75508(15) 0.34290(17) 0.16033(11) 0.0717(9) Uani 1 1 d . . . H15 H 0.7818 0.3785 0.1696 0.086 Uiso 1 1 calc R . . C16 C 0.75478(18) 0.2854(2) 0.18655(11) 0.0805(10) Uani 1 1 d . . . H16 H 0.7808 0.2820 0.2139 0.097 Uiso 1 1 calc R . . C17 C 0.71624(18) 0.23348(19) 0.17245(12) 0.0835(10) Uani 1 1 d . . . H17 H 0.7161 0.1943 0.1901 0.100 Uiso 1 1 calc R . . C18 C 0.67712(15) 0.23860(15) 0.13181(11) 0.0694(8) Uani 1 1 d . . . H18 H 0.6505 0.2028 0.1228 0.083 Uiso 1 1 calc R . . C19 C 0.57056(14) 0.34281(15) 0.07548(11) 0.0720(9) Uani 1 1 d . . . H19A H 0.5486 0.3187 0.1006 0.108 Uiso 1 1 calc R . . H19B H 0.5408 0.3474 0.0488 0.108 Uiso 1 1 calc R . . H19C H 0.5831 0.3862 0.0868 0.108 Uiso 1 1 calc R . . C20 C 0.61056(14) 0.23771(15) 0.03835(11) 0.0738(9) Uani 1 1 d . . . H20A H 0.6487 0.2105 0.0314 0.111 Uiso 1 1 calc R . . H20B H 0.5861 0.2459 0.0095 0.111 Uiso 1 1 calc R . . H20C H 0.5824 0.2151 0.0609 0.111 Uiso 1 1 calc R . . C21 C 0.65604(16) 0.49991(16) -0.05501(14) 0.0822(10) Uani 1 1 d U . . C22 C 0.59666(17) 0.47588(17) -0.08698(13) 0.0802(10) Uani 1 1 d . . . C23 C 0.5318(2) 0.4935(2) -0.07908(15) 0.1059(13) Uani 1 1 d . . . H23 H 0.5218 0.5220 -0.0539 0.127 Uiso 1 1 calc R . . C24 C 0.4806(2) 0.4700(2) -0.10750(18) 0.1176(15) Uani 1 1 d . . . H24 H 0.4370 0.4832 -0.1012 0.141 Uiso 1 1 calc R . . C25 C 0.4927(3) 0.4285(2) -0.14395(17) 0.1174(15) Uani 1 1 d . . . H25 H 0.4581 0.4124 -0.1628 0.141 Uiso 1 1 calc R . . C26 C 0.5576(3) 0.4103(3) -0.15279(15) 0.1431(19) Uani 1 1 d . . . H26 H 0.5670 0.3817 -0.1780 0.172 Uiso 1 1 calc R . . C27 C 0.6084(2) 0.4337(2) -0.12492(15) 0.1194(15) Uani 1 1 d . . . H27 H 0.6519 0.4209 -0.1317 0.143 Uiso 1 1 calc R . . C28 C 0.6342(2) 0.54741(17) -0.01599(15) 0.1175(15) Uani 1 1 d . . . H28A H 0.6023 0.5257 0.0042 0.176 Uiso 1 1 calc R . . H28B H 0.6144 0.5862 -0.0301 0.176 Uiso 1 1 calc R . . H28C H 0.6722 0.5604 0.0026 0.176 Uiso 1 1 calc R . . C29 C 0.70533(19) 0.53677(19) -0.08802(15) 0.1200(15) Uani 1 1 d U . . H29A H 0.6857 0.5778 -0.0986 0.180 Uiso 1 1 calc R . . H29B H 0.7153 0.5093 -0.1152 0.180 Uiso 1 1 calc R . . H29C H 0.7456 0.5461 -0.0708 0.180 Uiso 1 1 calc R . . C30 C 0.89865(14) 0.35538(14) 0.02831(10) 0.0662(8) Uani 1 1 d . . . H30A H 0.9166 0.3929 0.0114 0.099 Uiso 1 1 calc R . . H30B H 0.9304 0.3404 0.0516 0.099 Uiso 1 1 calc R . . H30C H 0.8581 0.3682 0.0440 0.099 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 0.0481(5) 0.0563(5) 0.0527(5) 0.0061(4) 0.0044(4) 0.0121(4) O1 0.0451(10) 0.0526(11) 0.0573(10) 0.0109(9) 0.0062(8) 0.0086(8) N1 0.0394(11) 0.0616(14) 0.0421(11) 0.0027(10) -0.0003(9) 0.0061(9) C1 0.078(2) 0.106(3) 0.0617(19) 0.0237(18) 0.0015(16) 0.0249(19) C2 0.081(2) 0.075(2) 0.108(3) -0.0178(19) 0.013(2) 0.0117(18) C3 0.0412(14) 0.0461(15) 0.0436(14) -0.0021(11) -0.0055(11) 0.0052(11) C4 0.0399(14) 0.0488(15) 0.0484(14) -0.0024(12) -0.0041(12) 0.0037(11) C5 0.0404(15) 0.0571(17) 0.0712(18) -0.0029(15) -0.0018(13) 0.0077(12) C6 0.0528(17) 0.0514(16) 0.076(2) 0.0103(15) -0.0070(15) 0.0067(13) C7 0.0493(16) 0.0578(17) 0.0648(18) 0.0141(14) -0.0040(13) -0.0002(13) C8 0.0396(14) 0.0548(16) 0.0453(14) 0.0064(12) -0.0033(11) 0.0031(11) C9 0.0455(15) 0.0638(17) 0.0454(14) 0.0093(13) 0.0004(12) 0.0057(12) C10 0.0448(15) 0.081(2) 0.0497(15) 0.0060(14) 0.0065(12) 0.0062(14) C11 0.045(2) 0.090(3) 0.054(2) 0.000 0.000 0.016(2) C12 0.0431(15) 0.0552(16) 0.0601(17) -0.0069(13) 0.0089(12) 0.0010(12) C13 0.0483(16) 0.0540(16) 0.0497(15) -0.0018(13) 0.0141(12) 0.0037(13) C14 0.0629(18) 0.0582(18) 0.0561(17) -0.0009(14) 0.0008(14) 0.0063(14) C15 0.073(2) 0.080(2) 0.0622(19) -0.0101(17) -0.0009(16) 0.0064(16) C16 0.082(2) 0.104(3) 0.0561(19) 0.004(2) 0.0015(17) 0.015(2) C17 0.093(3) 0.090(3) 0.067(2) 0.0275(19) 0.016(2) 0.014(2) C18 0.070(2) 0.069(2) 0.069(2) 0.0065(16) 0.0138(17) -0.0034(16) C19 0.0499(17) 0.089(2) 0.077(2) -0.0021(17) 0.0117(15) 0.0095(15) C20 0.0617(19) 0.074(2) 0.086(2) -0.0141(17) 0.0098(16) -0.0171(15) C21 0.064(2) 0.061(2) 0.121(3) 0.025(2) -0.006(2) 0.0096(16) C22 0.076(2) 0.076(2) 0.089(2) 0.0267(19) -0.0023(19) 0.0237(18) C23 0.080(3) 0.112(3) 0.127(3) -0.008(3) -0.005(3) 0.025(2) C24 0.080(3) 0.139(4) 0.134(4) -0.008(3) -0.026(3) 0.020(3) C25 0.115(4) 0.131(4) 0.106(3) 0.011(3) -0.043(3) 0.018(3) C26 0.143(5) 0.199(6) 0.088(3) -0.023(3) -0.038(3) 0.040(4) C27 0.102(3) 0.173(4) 0.084(3) -0.004(3) -0.007(2) 0.048(3) C28 0.147(4) 0.061(2) 0.145(4) -0.009(2) -0.016(3) 0.029(2) C29 0.095(3) 0.097(3) 0.168(4) 0.064(3) -0.004(3) 0.028(2) C30 0.0602(18) 0.074(2) 0.0647(18) -0.0110(16) -0.0035(15) 0.0017(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7496(18) . ? Al1 C2 1.942(3) . ? Al1 C1 1.950(3) . ? Al1 N1 2.025(2) . ? O1 C3 1.337(3) . ? N1 C30 1.492(3) . ? N1 C10 1.497(3) . ? N1 C9 1.502(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C8 1.392(3) . ? C3 C4 1.412(3) . ? C4 C5 1.385(3) . ? C4 C12 1.532(3) . ? C5 C6 1.391(4) . ? C5 H5 0.9300 . ? C6 C7 1.378(4) . ? C6 C21 1.538(4) . ? C7 C8 1.389(3) . ? C7 H7 0.9300 . ? C8 C9 1.507(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.508(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C10 1.508(3) 6_654 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.532(3) . ? C12 C20 1.536(4) . ? C12 C19 1.547(3) . ? C13 C18 1.382(4) . ? C13 C14 1.384(3) . ? C14 C15 1.373(4) . ? C14 H14 0.9300 . ? C15 C16 1.368(4) . ? C15 H15 0.9300 . ? C16 C17 1.357(4) . ? C16 H16 0.9300 . ? C17 C18 1.387(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 C28 1.515(5) . ? C21 C29 1.543(5) . ? C21 C22 1.567(5) . ? C22 C23 1.367(5) . ? C22 C27 1.379(5) . ? C23 C24 1.383(5) . ? C23 H23 0.9300 . ? C24 C25 1.340(6) . ? C24 H24 0.9300 . ? C25 C26 1.375(6) . ? C25 H25 0.9300 . ? C26 C27 1.369(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 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 C2 112.94(12) . . ? O1 Al1 C1 111.74(11) . . ? C2 Al1 C1 117.34(15) . . ? O1 Al1 N1 95.60(8) . . ? C2 Al1 N1 106.33(13) . . ? C1 Al1 N1 110.54(13) . . ? C3 O1 Al1 132.43(15) . . ? C30 N1 C10 109.7(2) . . ? C30 N1 C9 109.2(2) . . ? C10 N1 C9 106.21(18) . . ? C30 N1 Al1 112.53(16) . . ? C10 N1 Al1 113.35(16) . . ? C9 N1 Al1 105.49(15) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O1 C3 C8 120.8(2) . . ? O1 C3 C4 119.9(2) . . ? C8 C3 C4 119.2(2) . . ? C5 C4 C3 118.0(2) . . ? C5 C4 C12 123.3(2) . . ? C3 C4 C12 118.7(2) . . ? C4 C5 C6 123.6(2) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C7 C6 C5 116.9(2) . . ? C7 C6 C21 123.8(3) . . ? C5 C6 C21 119.3(3) . . ? C6 C7 C8 121.9(2) . . ? C6 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C7 C8 C3 120.3(2) . . ? C7 C8 C9 119.6(2) . . ? C3 C8 C9 119.9(2) . . ? N1 C9 C8 114.93(19) . . ? N1 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? N1 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N1 C10 C11 115.1(2) . . ? N1 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? N1 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C10 C11 C10 108.4(3) 6_654 . ? C10 C11 H11A 110.0 6_654 . ? C10 C11 H11A 110.0 . . ? C10 C11 H11B 110.0 6_654 . ? C10 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C4 C12 C13 109.3(2) . . ? C4 C12 C20 108.9(2) . . ? C13 C12 C20 113.0(2) . . ? C4 C12 C19 111.8(2) . . ? C13 C12 C19 106.6(2) . . ? C20 C12 C19 107.4(2) . . ? C18 C13 C14 116.6(3) . . ? C18 C13 C12 123.4(3) . . ? C14 C13 C12 120.0(2) . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 119.6(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.3(3) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 121.4(3) . . ? C13 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C12 C20 H20A 109.5 . . ? C12 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C12 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C28 C21 C6 109.9(3) . . ? C28 C21 C29 108.4(3) . . ? C6 C21 C29 112.3(3) . . ? C28 C21 C22 112.7(3) . . ? C6 C21 C22 106.5(3) . . ? C29 C21 C22 107.0(3) . . ? C23 C22 C27 116.5(4) . . ? C23 C22 C21 123.5(4) . . ? C27 C22 C21 119.9(3) . . ? C22 C23 C24 121.8(4) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 118.3(4) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C27 C26 C25 120.8(5) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C22 121.5(4) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? C21 C28 H28A 109.5 . . ? C21 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C21 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C21 C29 H29A 109.5 . . ? C21 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C21 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.285 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.046