# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Carl Redshaw' 'Abdessamad Arbaoui' 'D. Hughes' _publ_contact_author_name 'Dr Carl Redshaw ' _publ_contact_author_email CARL.REDSHAW@UEA.AC.UK _publ_section_title ; Multi-Nuclear Alkylaluminium Macrocyclic Schiff Base Complexes: Influence of Procatalyst Structure on the Ring Opening Polymerisation of ?-Caprolactone ; data_abdea8 _database_code_depnum_ccdc_archive 'CCDC 692213' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 3' _chemical_melting_point ? _chemical_formula_structural '[(Al Me2)2 (L)]' _chemical_formula_moiety 'C58 H70 Al2 N4 O2' _chemical_formula_sum 'C58 H70 Al2 N4 O2' _chemical_formula_weight 909.14 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.8444(9) _cell_length_b 12.1356(11) _cell_length_c 12.3556(11) _cell_angle_alpha 113.895(9) _cell_angle_beta 109.772(8) _cell_angle_gamma 99.385(7) _cell_volume 1311.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.991 _exptl_absorpt_correction_T_max 1.008 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 17941 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0442 _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 -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11514 _reflns_number_gt 9879 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0502P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(8) _chemical_absolute_configuration ad _refine_ls_number_reflns 11514 _refine_ls_number_parameters 630 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 0.36092(5) 0.61127(5) 0.45620(5) 0.01797(11) Uani 1 1 d . A . Al2 Al 0.96106(5) 0.74556(5) 0.70853(5) 0.01726(11) Uani 1 1 d . . . O1 O 0.45190(12) 0.72506(11) 0.42877(11) 0.0199(3) Uani 1 1 d . . . C11 C 0.47199(17) 0.85021(16) 0.48719(16) 0.0172(3) Uani 1 1 d . . . C12 C 0.47597(17) 0.91487(16) 0.61353(16) 0.0176(3) Uani 1 1 d . . . C13 C 0.48747(18) 1.04504(17) 0.66871(17) 0.0201(4) Uani 1 1 d . . . H13 H 0.4911 1.0866 0.7522 0.024 Uiso 1 1 calc R . . C14 C 0.49349(18) 1.11283(17) 0.60338(17) 0.0195(3) Uani 1 1 d . . . C141 C 0.4830(2) 1.24744(17) 0.65201(18) 0.0233(4) Uani 1 1 d . . . C142 C 0.4962(3) 1.3047(2) 0.7917(2) 0.0410(5) Uani 1 1 d . . . H14A H 0.4261 1.2476 0.7943 0.062 Uiso 1 1 calc R . . H14B H 0.4835 1.3864 0.8170 0.062 Uiso 1 1 calc R . . H14C H 0.5872 1.3162 0.8518 0.062 Uiso 1 1 calc R . . C143 C 0.3370(2) 1.2330(2) 0.5577(2) 0.0375(5) Uani 1 1 d . . . H14D H 0.2662 1.1748 0.5584 0.056 Uiso 1 1 calc R . . H14E H 0.3284 1.1999 0.4695 0.056 Uiso 1 1 calc R . . H14F H 0.3259 1.3154 0.5868 0.056 Uiso 1 1 calc R . . C144 C 0.5954(2) 1.3392(2) 0.6498(2) 0.0352(5) Uani 1 1 d . . . H14G H 0.5875 1.3043 0.5618 0.053 Uiso 1 1 calc R . . H14H H 0.6861 1.3498 0.7097 0.053 Uiso 1 1 calc R . . H14I H 0.5831 1.4211 0.6764 0.053 Uiso 1 1 calc R . . C15 C 0.49648(18) 1.04762(17) 0.48149(17) 0.0199(4) Uani 1 1 d . . . H15 H 0.5049 1.0926 0.4372 0.024 Uiso 1 1 calc R . . C16 C 0.48772(17) 0.92060(16) 0.42343(16) 0.0179(3) Uani 1 1 d . . . C17 C 0.47259(18) 0.85329(17) 0.28315(16) 0.0203(4) Uani 1 1 d . . . H17 H 0.5103 0.9196 0.2654 0.024 Uiso 1 1 calc R . . C171 C 0.3169(2) 0.7851(2) 0.18571(18) 0.0302(4) Uani 1 1 d . . . H17A H 0.3065 0.7432 0.0968 0.045 Uiso 1 1 calc R . . H17B H 0.2707 0.8471 0.1954 0.045 Uiso 1 1 calc R . . H17C H 0.2761 0.7223 0.2038 0.045 Uiso 1 1 calc R . . N18 N 0.54356(15) 0.75990(14) 0.25586(14) 0.0197(3) Uani 1 1 d . . . C21 C 0.68737(18) 0.79762(16) 0.29812(16) 0.0184(3) Uani 1 1 d . . . C22 C 0.77346(19) 0.92688(17) 0.36589(18) 0.0236(4) Uani 1 1 d . . . H22 H 0.7351 0.9909 0.3889 0.028 Uiso 1 1 calc R . . C23 C 0.9148(2) 0.96078(19) 0.3991(2) 0.0309(4) Uani 1 1 d . . . H23 H 0.9700 1.0471 0.4436 0.037 Uiso 1 1 calc R . . C24 C 0.9744(2) 0.8677(2) 0.3670(2) 0.0368(5) Uani 1 1 d . . . H24 H 1.0693 0.8903 0.3893 0.044 Uiso 1 1 calc R . . C25 C 0.8899(2) 0.7400(2) 0.3008(2) 0.0305(4) Uani 1 1 d . . . H25 H 0.9300 0.6771 0.2791 0.037 Uiso 1 1 calc R . . C26 C 0.74849(19) 0.70195(17) 0.26547(17) 0.0214(4) Uani 1 1 d . . . C27 C 0.66282(19) 0.56008(17) 0.18999(17) 0.0232(4) Uani 1 1 d . . . H27A H 0.6945 0.5150 0.1258 0.028 Uiso 1 1 calc R . . H27B H 0.5658 0.5482 0.1416 0.028 Uiso 1 1 calc R . . C28 C 0.67212(19) 0.50015(17) 0.27907(17) 0.0237(4) Uani 1 1 d . . . H28A H 0.7699 0.5238 0.3371 0.028 Uiso 1 1 calc R . . H28B H 0.6280 0.5370 0.3344 0.028 Uiso 1 1 calc R . . C31 C 0.60510(17) 0.35494(16) 0.20614(16) 0.0190(3) Uani 1 1 d . . . C32 C 0.50586(19) 0.28669(18) 0.07401(18) 0.0246(4) Uani 1 1 d . . . H32 H 0.4751 0.3321 0.0316 0.030 Uiso 1 1 calc R . . C33 C 0.45112(18) 0.15338(18) 0.00318(17) 0.0243(4) Uani 1 1 d . . . H33 H 0.3841 0.1103 -0.0848 0.029 Uiso 1 1 calc R . . C34 C 0.49737(18) 0.08585(18) 0.06499(18) 0.0240(4) Uani 1 1 d . . . H34 H 0.4639 -0.0036 0.0176 0.029 Uiso 1 1 calc R . . C35 C 0.59316(18) 0.14984(17) 0.19698(17) 0.0225(4) Uani 1 1 d . . . H35 H 0.6235 0.1028 0.2375 0.027 Uiso 1 1 calc R . . C36 C 0.64535(17) 0.28429(16) 0.27084(16) 0.0181(3) Uani 1 1 d . . . N37 N 0.73145(16) 0.34760(15) 0.40668(14) 0.0207(3) Uani 1 1 d . . . C38 C 0.84393(18) 0.30537(16) 0.46181(16) 0.0195(4) Uani 1 1 d . . . H38 H 0.8038 0.2124 0.4252 0.023 Uiso 1 1 calc R . . C381 C 0.9594(2) 0.3291(2) 0.42188(19) 0.0323(5) Uani 1 1 d . . . H38A H 0.9202 0.2881 0.3271 0.048 Uiso 1 1 calc R . . H38B H 1.0276 0.2944 0.4539 0.048 Uiso 1 1 calc R . . H38C H 1.0032 0.4199 0.4594 0.048 Uiso 1 1 calc R . . O4 O 0.91586(13) 0.57518(11) 0.63566(11) 0.0214(3) Uani 1 1 d . . . C41 C 0.93165(17) 0.50042(16) 0.68987(16) 0.0171(3) Uani 1 1 d . . . C42 C 0.90053(16) 0.36829(16) 0.61103(16) 0.0176(3) Uani 1 1 d . . . C43 C 0.92729(18) 0.29492(17) 0.67160(18) 0.0213(4) Uani 1 1 d . . . H43 H 0.9078 0.2079 0.6180 0.026 Uiso 1 1 calc R . . C44 C 0.98187(19) 0.34362(17) 0.80850(18) 0.0241(4) Uani 1 1 d . A . C441 C 1.0140(2) 0.25951(19) 0.8719(2) 0.0336(5) Uani 1 1 d . . . C442 C 1.0186(17) 0.1378(13) 0.7772(13) 0.153(8) Uani 0.50 1 d P A 1 H44A H 1.0942 0.1572 0.7565 0.230 Uiso 0.50 1 calc PR A 1 H44B H 0.9320 0.0936 0.6976 0.230 Uiso 0.50 1 calc PR A 1 H44C H 1.0327 0.0842 0.8166 0.230 Uiso 0.50 1 calc PR A 1 C443 C 1.1578(10) 0.3358(11) 0.9909(10) 0.073(3) Uani 0.50 1 d P A 1 H44D H 1.2253 0.3582 0.9623 0.109 Uiso 0.50 1 calc PR A 1 H44E H 1.1837 0.2845 1.0308 0.109 Uiso 0.50 1 calc PR A 1 H44F H 1.1549 0.4128 1.0544 0.109 Uiso 0.50 1 calc PR A 1 C444 C 0.9075(10) 0.2337(10) 0.9187(11) 0.085(3) Uani 0.50 1 d P A 1 H44G H 0.8970 0.3129 0.9687 0.128 Uiso 0.50 1 calc PR A 1 H44H H 0.9378 0.1964 0.9738 0.128 Uiso 0.50 1 calc PR A 1 H44I H 0.8194 0.1752 0.8437 0.128 Uiso 0.50 1 calc PR A 1 C445 C 1.0797(11) 0.1693(11) 0.8078(10) 0.061(3) Uani 0.50 1 d P A 2 H44J H 1.0980 0.1180 0.8494 0.091 Uiso 0.50 1 calc PR A 2 H44K H 1.1659 0.2181 0.8179 0.091 Uiso 0.50 1 calc PR A 2 H44L H 1.0171 0.1142 0.7154 0.091 Uiso 0.50 1 calc PR A 2 C446 C 1.1052(13) 0.3361(9) 1.0188(8) 0.094(5) Uani 0.50 1 d P A 2 H44M H 1.1212 0.2786 1.0529 0.141 Uiso 0.50 1 calc PR A 2 H44N H 1.0597 0.3883 1.0606 0.141 Uiso 0.50 1 calc PR A 2 H44O H 1.1930 0.3902 1.0369 0.141 Uiso 0.50 1 calc PR A 2 C447 C 0.8728(11) 0.1702(8) 0.8418(9) 0.069(3) Uani 0.50 1 d P A 2 H44P H 0.8900 0.1165 0.8806 0.103 Uiso 0.50 1 calc PR A 2 H44Q H 0.8175 0.1173 0.7477 0.103 Uiso 0.50 1 calc PR A 2 H44R H 0.8234 0.2214 0.8783 0.103 Uiso 0.50 1 calc PR A 2 C45 C 1.00308(18) 0.47164(17) 0.88385(17) 0.0215(4) Uani 1 1 d . . . H45 H 1.0347 0.5068 0.9748 0.026 Uiso 1 1 calc R A . C46 C 0.97841(17) 0.55059(16) 0.82752(16) 0.0187(3) Uani 1 1 d . A . C47 C 1.00338(16) 0.68185(16) 0.91638(16) 0.0180(3) Uani 1 1 d . . . H47 H 1.0254 0.7042 1.0038 0.022 Uiso 1 1 calc R A . N48 N 0.99822(14) 0.77200(13) 0.88659(13) 0.0167(3) Uani 1 1 d . A . C51 C 1.02786(17) 0.89769(16) 0.99415(16) 0.0166(3) Uani 1 1 d . . . C52 C 1.15325(17) 0.99285(17) 1.03961(17) 0.0205(4) Uani 1 1 d . A . H52 H 1.2118 0.9750 0.9996 0.025 Uiso 1 1 calc R . . C53 C 1.19031(18) 1.11396(17) 1.14451(17) 0.0224(4) Uani 1 1 d . . . H53 H 1.2748 1.1773 1.1767 0.027 Uiso 1 1 calc R A . C54 C 1.10120(19) 1.14015(17) 1.20109(17) 0.0243(4) Uani 1 1 d . A . H54 H 1.1249 1.2217 1.2708 0.029 Uiso 1 1 calc R . . C55 C 0.97620(19) 1.04488(18) 1.15406(18) 0.0239(4) Uani 1 1 d . . . H55 H 0.9172 1.0641 1.1933 0.029 Uiso 1 1 calc R A . C56 C 0.93640(17) 0.92162(17) 1.05007(17) 0.0194(4) Uani 1 1 d . A . C57 C 0.79852(18) 0.82309(18) 1.00398(18) 0.0227(4) Uani 1 1 d . . . H57A H 0.7883 0.8279 1.0806 0.027 Uiso 1 1 calc R A . H57B H 0.7987 0.7378 0.9530 0.027 Uiso 1 1 calc R . . C58 C 0.67374(17) 0.84307(18) 0.91910(17) 0.0219(4) Uani 1 1 d . A . H58A H 0.6719 0.9271 0.9715 0.026 Uiso 1 1 calc R . . H58B H 0.6864 0.8421 0.8447 0.026 Uiso 1 1 calc R . . C61 C 0.53448(17) 0.74199(17) 0.86707(16) 0.0181(3) Uani 1 1 d . . . C62 C 0.51030(18) 0.69534(18) 0.94748(17) 0.0225(4) Uani 1 1 d . A . H62 H 0.5785 0.7309 1.0341 0.027 Uiso 1 1 calc R . . C63 C 0.38832(18) 0.59817(18) 0.90227(18) 0.0214(4) Uani 1 1 d . . . H63 H 0.3750 0.5705 0.9589 0.026 Uiso 1 1 calc R A . C64 C 0.28657(17) 0.54213(17) 0.77398(17) 0.0200(4) Uani 1 1 d . A . H64 H 0.2057 0.4748 0.7424 0.024 Uiso 1 1 calc R . . C65 C 0.30623(17) 0.58732(17) 0.69274(17) 0.0201(4) Uani 1 1 d . . . H65 H 0.2378 0.5499 0.6059 0.024 Uiso 1 1 calc R A . C66 C 0.42591(17) 0.68715(16) 0.73831(16) 0.0161(3) Uani 1 1 d . A . N67 N 0.43191(14) 0.73085(13) 0.64694(13) 0.0159(3) Uani 1 1 d . . . C68 C 0.46520(17) 0.85308(17) 0.68927(16) 0.0182(3) Uani 1 1 d . A . H68 H 0.4838 0.9057 0.7766 0.022 Uiso 1 1 calc R . . C71 C 0.4252(2) 0.46611(19) 0.4245(2) 0.0303(4) Uani 1 1 d . . . H71A H 0.5249 0.4968 0.4750 0.045 Uiso 1 1 calc R A . H71B H 0.4002 0.4170 0.3320 0.045 Uiso 1 1 calc R . . H71C H 0.3821 0.4126 0.4510 0.045 Uiso 1 1 calc R . . C72 C 0.1609(2) 0.5801(2) 0.3678(2) 0.0361(5) Uani 1 1 d . . . H72A H 0.1459 0.6609 0.3933 0.054 Uiso 0.50 1 calc PR A . H72B H 0.1108 0.5302 0.3932 0.054 Uiso 0.50 1 calc PR . . H72C H 0.1279 0.5340 0.2736 0.054 Uiso 0.50 1 calc PR . . H72D H 0.1105 0.4892 0.3134 0.054 Uiso 0.50 1 calc PR . . H72E H 0.1456 0.6198 0.3136 0.054 Uiso 0.50 1 calc PR . . H72F H 0.1285 0.6160 0.4331 0.054 Uiso 0.50 1 calc PR . . C73 C 0.7988(2) 0.7921(2) 0.64274(19) 0.0308(4) Uani 1 1 d . . . H73A H 0.7215 0.7445 0.6460 0.046 Uiso 1 1 calc R . . H73B H 0.7745 0.7720 0.5530 0.046 Uiso 1 1 calc R . . H73C H 0.8206 0.8825 0.6969 0.046 Uiso 1 1 calc R . . C74 C 1.1357(2) 0.82601(19) 0.71388(19) 0.0294(4) Uani 1 1 d . . . H74A H 1.2052 0.7936 0.7485 0.044 Uiso 1 1 calc R . . H74B H 1.1671 0.9175 0.7698 0.044 Uiso 1 1 calc R . . H74C H 1.1207 0.8066 0.6260 0.044 Uiso 1 1 calc R . . H18 H 0.516(2) 0.699(2) 0.2751(19) 0.024(5) Uiso 1 1 d . . . H37 H 0.761(2) 0.429(2) 0.446(2) 0.023(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0203(3) 0.0153(3) 0.0161(2) 0.0079(2) 0.0065(2) 0.0044(2) Al2 0.0208(3) 0.0113(3) 0.0172(3) 0.0064(2) 0.0072(2) 0.0046(2) O1 0.0277(6) 0.0152(6) 0.0189(6) 0.0093(5) 0.0114(5) 0.0083(5) C11 0.0180(8) 0.0155(8) 0.0173(8) 0.0082(7) 0.0065(7) 0.0070(7) C12 0.0201(8) 0.0173(9) 0.0174(8) 0.0103(7) 0.0079(7) 0.0073(7) C13 0.0236(9) 0.0195(9) 0.0197(9) 0.0094(7) 0.0115(7) 0.0098(7) C14 0.0230(9) 0.0155(9) 0.0226(9) 0.0107(7) 0.0106(7) 0.0080(7) C141 0.0346(10) 0.0172(9) 0.0265(9) 0.0128(8) 0.0182(8) 0.0137(8) C142 0.0720(16) 0.0283(12) 0.0349(12) 0.0174(10) 0.0298(11) 0.0279(12) C143 0.0407(12) 0.0320(12) 0.0489(13) 0.0237(11) 0.0217(10) 0.0204(10) C144 0.0440(12) 0.0219(10) 0.0436(12) 0.0165(10) 0.0228(10) 0.0131(9) C15 0.0262(9) 0.0195(9) 0.0216(8) 0.0145(8) 0.0126(7) 0.0104(8) C16 0.0184(8) 0.0189(9) 0.0177(8) 0.0102(7) 0.0075(7) 0.0077(7) C17 0.0262(9) 0.0197(9) 0.0195(8) 0.0122(7) 0.0106(7) 0.0115(8) C171 0.0319(10) 0.0351(12) 0.0191(9) 0.0113(9) 0.0076(8) 0.0148(9) N18 0.0273(8) 0.0157(8) 0.0201(8) 0.0104(6) 0.0129(6) 0.0081(7) C21 0.0261(9) 0.0178(9) 0.0140(8) 0.0100(7) 0.0095(7) 0.0073(7) C22 0.0312(10) 0.0176(9) 0.0221(9) 0.0105(8) 0.0113(8) 0.0083(8) C23 0.0297(10) 0.0214(10) 0.0334(11) 0.0131(9) 0.0089(8) 0.0020(8) C24 0.0251(10) 0.0371(13) 0.0446(13) 0.0207(11) 0.0124(9) 0.0085(9) C25 0.0309(10) 0.0275(11) 0.0364(11) 0.0175(9) 0.0143(9) 0.0150(9) C26 0.0290(9) 0.0196(9) 0.0187(9) 0.0124(7) 0.0097(7) 0.0099(8) C27 0.0329(10) 0.0181(9) 0.0191(8) 0.0091(8) 0.0104(8) 0.0130(8) C28 0.0294(10) 0.0163(9) 0.0183(9) 0.0074(7) 0.0061(7) 0.0048(8) C31 0.0200(8) 0.0153(9) 0.0177(8) 0.0058(7) 0.0083(7) 0.0041(7) C32 0.0261(9) 0.0231(10) 0.0210(9) 0.0110(8) 0.0076(7) 0.0065(8) C33 0.0200(9) 0.0245(10) 0.0148(8) 0.0035(7) 0.0041(7) 0.0014(8) C34 0.0222(9) 0.0149(9) 0.0239(9) 0.0033(8) 0.0090(7) 0.0011(7) C35 0.0238(9) 0.0173(9) 0.0239(9) 0.0102(8) 0.0087(7) 0.0054(7) C36 0.0189(8) 0.0154(9) 0.0145(8) 0.0048(7) 0.0064(7) 0.0025(7) N37 0.0272(8) 0.0106(7) 0.0165(7) 0.0041(6) 0.0051(6) 0.0057(6) C38 0.0226(9) 0.0099(8) 0.0186(8) 0.0049(7) 0.0047(7) 0.0043(7) C381 0.0277(10) 0.0372(12) 0.0232(10) 0.0076(9) 0.0120(8) 0.0095(9) O4 0.0309(7) 0.0112(6) 0.0170(6) 0.0067(5) 0.0067(5) 0.0048(5) C41 0.0161(8) 0.0133(8) 0.0186(8) 0.0078(7) 0.0047(6) 0.0040(7) C42 0.0148(8) 0.0149(9) 0.0190(8) 0.0075(7) 0.0050(7) 0.0038(7) C43 0.0224(9) 0.0116(8) 0.0224(9) 0.0064(7) 0.0049(7) 0.0051(7) C44 0.0277(9) 0.0163(9) 0.0233(9) 0.0103(8) 0.0053(7) 0.0079(8) C441 0.0488(12) 0.0188(10) 0.0273(10) 0.0140(9) 0.0072(9) 0.0126(9) C442 0.32(2) 0.063(6) 0.058(6) 0.036(5) 0.037(10) 0.122(11) C443 0.062(4) 0.070(5) 0.083(8) 0.067(6) -0.005(4) 0.019(4) C444 0.067(5) 0.119(9) 0.140(9) 0.120(8) 0.049(7) 0.039(7) C445 0.097(5) 0.094(8) 0.060(6) 0.062(6) 0.055(5) 0.084(6) C446 0.180(13) 0.025(3) 0.021(3) 0.013(3) -0.006(5) 0.015(6) C447 0.093(7) 0.057(5) 0.110(7) 0.068(5) 0.063(7) 0.041(5) C45 0.0246(9) 0.0192(9) 0.0170(8) 0.0092(7) 0.0051(7) 0.0072(8) C46 0.0176(8) 0.0138(8) 0.0185(8) 0.0060(7) 0.0046(7) 0.0045(7) C47 0.0140(8) 0.0195(9) 0.0165(8) 0.0088(7) 0.0035(6) 0.0041(7) N48 0.0162(7) 0.0112(7) 0.0156(7) 0.0042(6) 0.0036(5) 0.0025(6) C51 0.0186(8) 0.0125(8) 0.0142(8) 0.0059(7) 0.0034(6) 0.0054(7) C52 0.0201(9) 0.0189(9) 0.0200(8) 0.0082(7) 0.0087(7) 0.0057(7) C53 0.0205(9) 0.0144(9) 0.0199(9) 0.0051(7) 0.0029(7) -0.0005(7) C54 0.0299(10) 0.0151(9) 0.0190(9) 0.0041(7) 0.0077(7) 0.0061(8) C55 0.0263(9) 0.0236(10) 0.0231(9) 0.0100(8) 0.0136(7) 0.0100(8) C56 0.0190(8) 0.0183(9) 0.0186(8) 0.0106(7) 0.0045(7) 0.0058(7) C57 0.0200(9) 0.0216(10) 0.0290(9) 0.0148(8) 0.0110(7) 0.0073(8) C58 0.0196(9) 0.0223(10) 0.0197(9) 0.0118(8) 0.0056(7) 0.0012(7) C61 0.0192(8) 0.0174(9) 0.0173(8) 0.0085(7) 0.0082(7) 0.0055(7) C62 0.0215(9) 0.0284(10) 0.0163(8) 0.0123(8) 0.0067(7) 0.0062(8) C63 0.0274(9) 0.0236(10) 0.0238(9) 0.0163(8) 0.0158(8) 0.0116(8) C64 0.0177(8) 0.0172(9) 0.0288(9) 0.0132(8) 0.0121(7) 0.0064(7) C65 0.0185(8) 0.0205(9) 0.0198(8) 0.0104(7) 0.0064(7) 0.0076(7) C66 0.0208(8) 0.0160(8) 0.0152(8) 0.0088(7) 0.0098(7) 0.0086(7) N67 0.0173(7) 0.0162(7) 0.0163(7) 0.0106(6) 0.0068(6) 0.0053(6) C68 0.0195(8) 0.0213(9) 0.0169(8) 0.0106(7) 0.0088(7) 0.0095(7) C71 0.0409(11) 0.0188(10) 0.0328(11) 0.0123(9) 0.0188(9) 0.0104(9) C72 0.0260(10) 0.0516(15) 0.0254(10) 0.0194(10) 0.0076(8) 0.0088(10) C73 0.0346(11) 0.0306(11) 0.0266(10) 0.0135(9) 0.0111(8) 0.0175(9) C74 0.0328(10) 0.0198(10) 0.0296(10) 0.0062(8) 0.0171(8) 0.0046(8) _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 1.7766(13) . ? Al1 C71 1.941(2) . ? Al1 C72 1.959(2) . ? Al1 N67 1.9723(15) . ? Al2 O4 1.7858(13) . ? Al2 C73 1.9499(19) . ? Al2 C74 1.950(2) . ? Al2 N48 1.9727(14) . ? O1 C11 1.332(2) . ? C11 C16 1.403(2) . ? C11 C12 1.416(2) . ? C12 C13 1.408(2) . ? C12 C68 1.437(2) . ? C13 C14 1.374(2) . ? C13 H13 0.9300 . ? C14 C15 1.404(2) . ? C14 C141 1.534(2) . ? C141 C142 1.520(3) . ? C141 C144 1.527(3) . ? C141 C143 1.546(3) . ? C142 H14A 0.9600 . ? C142 H14B 0.9600 . ? C142 H14C 0.9600 . ? C143 H14D 0.9600 . ? C143 H14E 0.9600 . ? C143 H14F 0.9600 . ? C144 H14G 0.9600 . ? C144 H14H 0.9600 . ? C144 H14I 0.9600 . ? C15 C16 1.382(2) . ? C15 H15 0.9300 . ? C16 C17 1.522(2) . ? C17 N18 1.463(2) . ? C17 C171 1.532(3) . ? C17 H17 0.9800 . ? C171 H17A 0.9600 . ? C171 H17B 0.9600 . ? C171 H17C 0.9600 . ? N18 C21 1.392(2) . ? N18 H18 0.90(2) . ? C21 C22 1.401(2) . ? C21 C26 1.415(2) . ? C22 C23 1.385(3) . ? C22 H22 0.9300 . ? C23 C24 1.379(3) . ? C23 H23 0.9300 . ? C24 C25 1.383(3) . ? C24 H24 0.9300 . ? C25 C26 1.382(3) . ? C25 H25 0.9300 . ? C26 C27 1.513(3) . ? C27 C28 1.532(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C31 1.516(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C31 C32 1.391(2) . ? C31 C36 1.416(2) . ? C32 C33 1.387(3) . ? C32 H32 0.9300 . ? C33 C34 1.374(3) . ? C33 H33 0.9300 . ? C34 C35 1.381(2) . ? C34 H34 0.9300 . ? C35 C36 1.400(2) . ? C35 H35 0.9300 . ? C36 N37 1.393(2) . ? N37 C38 1.463(2) . ? N37 H37 0.85(2) . ? C38 C42 1.517(2) . ? C38 C381 1.519(3) . ? C38 H38 0.9800 . ? C381 H38A 0.9600 . ? C381 H38B 0.9600 . ? C381 H38C 0.9600 . ? O4 C41 1.329(2) . ? C41 C42 1.403(2) . ? C41 C46 1.413(2) . ? C42 C43 1.384(2) . ? C43 C44 1.400(3) . ? C43 H43 0.9300 . ? C44 C45 1.378(2) . ? C44 C441 1.535(2) . ? C441 C442 1.489(12) . ? C441 C444 1.499(11) . ? C441 C446 1.502(9) . ? C441 C445 1.506(8) . ? C441 C443 1.525(10) . ? C441 C447 1.550(11) . ? C442 H44A 0.9600 . ? C442 H44B 0.9600 . ? C442 H44C 0.9600 . ? C443 H44D 0.9600 . ? C443 H44E 0.9600 . ? C443 H44F 0.9600 . ? C444 H44G 0.9600 . ? C444 H44H 0.9600 . ? C444 H44I 0.9600 . ? C445 H44J 0.9600 . ? C445 H44K 0.9600 . ? C445 H44L 0.9600 . ? C446 H44M 0.9600 . ? C446 H44N 0.9600 . ? C446 H44O 0.9600 . ? C447 H44P 0.9600 . ? C447 H44Q 0.9600 . ? C447 H44R 0.9600 . ? C45 C46 1.404(2) . ? C45 H45 0.9300 . ? C46 C47 1.434(2) . ? C47 N48 1.291(2) . ? C47 H47 0.9300 . ? N48 C51 1.451(2) . ? C51 C56 1.393(2) . ? C51 C52 1.394(2) . ? C52 C53 1.383(2) . ? C52 H52 0.9300 . ? C53 C54 1.379(3) . ? C53 H53 0.9300 . ? C54 C55 1.387(3) . ? C54 H54 0.9300 . ? C55 C56 1.390(2) . ? C55 H55 0.9300 . ? C56 C57 1.510(2) . ? C57 C58 1.530(2) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C61 1.516(2) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C61 C62 1.400(2) . ? C61 C66 1.407(2) . ? C62 C63 1.382(3) . ? C62 H62 0.9300 . ? C63 C64 1.375(2) . ? C63 H63 0.9300 . ? C64 C65 1.381(2) . ? C64 H64 0.9300 . ? C65 C66 1.382(2) . ? C65 H65 0.9300 . ? C66 N67 1.443(2) . ? N67 C68 1.294(2) . ? C68 H68 0.9300 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C72 H72D 0.9600 . ? C72 H72E 0.9600 . ? C72 H72F 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 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 C71 112.12(8) . . ? O1 Al1 C72 107.87(8) . . ? C71 Al1 C72 119.42(10) . . ? O1 Al1 N67 94.24(6) . . ? C71 Al1 N67 111.90(7) . . ? C72 Al1 N67 108.33(8) . . ? O4 Al2 C73 111.32(8) . . ? O4 Al2 C74 111.76(7) . . ? C73 Al2 C74 119.32(9) . . ? O4 Al2 N48 93.79(6) . . ? C73 Al2 N48 108.78(7) . . ? C74 Al2 N48 108.78(8) . . ? C11 O1 Al1 125.18(11) . . ? O1 C11 C16 120.38(15) . . ? O1 C11 C12 121.10(15) . . ? C16 C11 C12 118.52(15) . . ? C13 C12 C11 119.79(15) . . ? C13 C12 C68 117.06(15) . . ? C11 C12 C68 123.13(15) . . ? C14 C13 C12 122.25(16) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 116.34(16) . . ? C13 C14 C141 122.69(15) . . ? C15 C14 C141 120.71(15) . . ? C142 C141 C144 108.72(17) . . ? C142 C141 C14 111.55(15) . . ? C144 C141 C14 111.48(15) . . ? C142 C141 C143 108.47(17) . . ? C144 C141 C143 109.31(16) . . ? C14 C141 C143 107.24(16) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C16 C15 C14 123.90(15) . . ? C16 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C15 C16 C11 118.98(15) . . ? C15 C16 C17 119.92(14) . . ? C11 C16 C17 120.42(15) . . ? N18 C17 C16 116.15(13) . . ? N18 C17 C171 108.42(15) . . ? C16 C17 C171 108.95(14) . . ? N18 C17 H17 107.7 . . ? C16 C17 H17 107.7 . . ? C171 C17 H17 107.7 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C21 N18 C17 122.05(15) . . ? C21 N18 H18 110.4(12) . . ? C17 N18 H18 110.9(13) . . ? N18 C21 C22 122.54(15) . . ? N18 C21 C26 118.96(16) . . ? C22 C21 C26 118.41(16) . . ? C23 C22 C21 121.05(17) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C24 C23 C22 120.61(19) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 118.50(19) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? C26 C25 C24 122.78(18) . . ? C26 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? C25 C26 C21 118.64(17) . . ? C25 C26 C27 119.41(16) . . ? C21 C26 C27 121.92(16) . . ? C26 C27 C28 113.40(14) . . ? C26 C27 H27A 108.9 . . ? C28 C27 H27A 108.9 . . ? C26 C27 H27B 108.9 . . ? C28 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C31 C28 C27 114.97(14) . . ? C31 C28 H28A 108.5 . . ? C27 C28 H28A 108.5 . . ? C31 C28 H28B 108.5 . . ? C27 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C32 C31 C36 117.93(16) . . ? C32 C31 C28 121.72(15) . . ? C36 C31 C28 120.33(14) . . ? C33 C32 C31 122.40(16) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C34 C33 C32 119.02(16) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 120.45(17) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 121.07(16) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? N37 C36 C35 120.57(15) . . ? N37 C36 C31 120.47(15) . . ? C35 C36 C31 118.93(15) . . ? C36 N37 C38 120.78(14) . . ? C36 N37 H37 116.1(13) . . ? C38 N37 H37 108.9(13) . . ? N37 C38 C42 110.66(13) . . ? N37 C38 C381 111.76(15) . . ? C42 C38 C381 111.56(14) . . ? N37 C38 H38 107.5 . . ? C42 C38 H38 107.5 . . ? C381 C38 H38 107.5 . . ? C38 C381 H38A 109.5 . . ? C38 C381 H38B 109.5 . . ? H38A C381 H38B 109.5 . . ? C38 C381 H38C 109.5 . . ? H38A C381 H38C 109.5 . . ? H38B C381 H38C 109.5 . . ? C41 O4 Al2 131.33(11) . . ? O4 C41 C42 120.59(15) . . ? O4 C41 C46 121.38(15) . . ? C42 C41 C46 118.03(14) . . ? C43 C42 C41 119.07(15) . . ? C43 C42 C38 119.34(15) . . ? C41 C42 C38 121.55(14) . . ? C42 C43 C44 124.05(16) . . ? C42 C43 H43 118.0 . . ? C44 C43 H43 118.0 . . ? C45 C44 C43 116.19(15) . . ? C45 C44 C441 121.47(16) . . ? C43 C44 C441 122.33(16) . . ? C442 C441 C444 111.5(8) . . ? C442 C441 C446 126.5(7) . . ? C444 C441 C446 80.5(6) . . ? C442 C441 C445 23.1(9) . . ? C444 C441 C445 128.3(6) . . ? C446 C441 C445 109.4(6) . . ? C442 C441 C443 108.8(7) . . ? C444 C441 C443 109.1(6) . . ? C446 C441 C443 29.1(6) . . ? C445 C441 C443 87.1(6) . . ? C442 C441 C44 110.7(5) . . ? C444 C441 C44 109.6(4) . . ? C446 C441 C44 113.2(4) . . ? C445 C441 C44 111.6(4) . . ? C443 C441 C44 107.0(4) . . ? C442 C441 C447 83.4(8) . . ? C444 C441 C447 32.0(5) . . ? C446 C441 C447 109.8(6) . . ? C445 C441 C447 104.6(6) . . ? C443 C441 C447 135.6(5) . . ? C44 C441 C447 107.8(4) . . ? C441 C442 H44A 109.5 . . ? C441 C442 H44B 109.5 . . ? H44A C442 H44B 109.5 . . ? C441 C442 H44C 109.5 . . ? H44A C442 H44C 109.5 . . ? H44B C442 H44C 109.5 . . ? C441 C443 H44D 109.5 . . ? C441 C443 H44E 109.5 . . ? H44D C443 H44E 109.5 . . ? C441 C443 H44F 109.5 . . ? H44D C443 H44F 109.5 . . ? H44E C443 H44F 109.5 . . ? C441 C444 H44G 109.5 . . ? C441 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C441 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C441 C445 H44J 109.5 . . ? C441 C445 H44K 109.5 . . ? H44J C445 H44K 109.5 . . ? C441 C445 H44L 109.5 . . ? H44J C445 H44L 109.5 . . ? H44K C445 H44L 109.5 . . ? C441 C446 H44M 109.5 . . ? C441 C446 H44N 109.5 . . ? H44M C446 H44N 109.5 . . ? C441 C446 H44O 109.5 . . ? H44M C446 H44O 109.5 . . ? H44N C446 H44O 109.5 . . ? C441 C447 H44P 109.5 . . ? C441 C447 H44Q 109.5 . . ? H44P C447 H44Q 109.5 . . ? C441 C447 H44R 109.5 . . ? H44P C447 H44R 109.5 . . ? H44Q C447 H44R 109.5 . . ? C44 C45 C46 122.01(16) . . ? C44 C45 H45 119.0 . . ? C46 C45 H45 119.0 . . ? C45 C46 C41 120.39(15) . . ? C45 C46 C47 116.63(15) . . ? C41 C46 C47 122.98(15) . . ? N48 C47 C46 126.25(16) . . ? N48 C47 H47 116.9 . . ? C46 C47 H47 116.9 . . ? C47 N48 C51 116.02(14) . . ? C47 N48 Al2 122.94(12) . . ? C51 N48 Al2 120.98(10) . . ? C56 C51 C52 121.73(16) . . ? C56 C51 N48 121.68(15) . . ? C52 C51 N48 116.58(15) . . ? C53 C52 C51 119.75(16) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C54 C53 C52 119.58(17) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 120.04(17) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 121.99(17) . . ? C54 C55 H55 119.0 . . ? C56 C55 H55 119.0 . . ? C55 C56 C51 116.90(16) . . ? C55 C56 C57 118.97(16) . . ? C51 C56 C57 124.13(16) . . ? C56 C57 C58 112.46(14) . . ? C56 C57 H57A 109.1 . . ? C58 C57 H57A 109.1 . . ? C56 C57 H57B 109.1 . . ? C58 C57 H57B 109.1 . . ? H57A C57 H57B 107.8 . . ? C61 C58 C57 113.40(14) . . ? C61 C58 H58A 108.9 . . ? C57 C58 H58A 108.9 . . ? C61 C58 H58B 108.9 . . ? C57 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? C62 C61 C66 116.37(15) . . ? C62 C61 C58 119.85(15) . . ? C66 C61 C58 123.75(15) . . ? C63 C62 C61 122.11(16) . . ? C63 C62 H62 118.9 . . ? C61 C62 H62 118.9 . . ? C64 C63 C62 120.31(16) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 119.00(16) . . ? C63 C64 H64 120.5 . . ? C65 C64 H64 120.5 . . ? C64 C65 C66 121.09(15) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C65 C66 C61 121.00(15) . . ? C65 C66 N67 116.26(14) . . ? C61 C66 N67 122.74(15) . . ? C68 N67 C66 117.60(14) . . ? C68 N67 Al1 119.18(11) . . ? C66 N67 Al1 122.35(11) . . ? N67 C68 C12 125.89(15) . . ? N67 C68 H68 117.1 . . ? C12 C68 H68 117.1 . . ? Al1 C71 H71A 109.5 . . ? Al1 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Al1 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? Al1 C72 H72A 109.5 . . ? Al1 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Al1 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? Al1 C72 H72D 109.5 . . ? H72A C72 H72D 141.1 . . ? H72B C72 H72D 56.3 . . ? H72C C72 H72D 56.3 . . ? Al1 C72 H72E 109.5 . . ? H72A C72 H72E 56.3 . . ? H72B C72 H72E 141.1 . . ? H72C C72 H72E 56.3 . . ? H72D C72 H72E 109.5 . . ? Al1 C72 H72F 109.5 . . ? H72A C72 H72F 56.3 . . ? H72B C72 H72F 56.3 . . ? H72C C72 H72F 141.1 . . ? H72D C72 H72F 109.5 . . ? H72E C72 H72F 109.5 . . ? Al2 C73 H73A 109.5 . . ? Al2 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? Al2 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? Al2 C74 H74A 109.5 . . ? Al2 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? Al2 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 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 C71 Al1 O1 C11 -152.83(13) . . . . ? C72 Al1 O1 C11 73.70(14) . . . . ? N67 Al1 O1 C11 -37.12(13) . . . . ? Al1 O1 C11 C16 -152.12(12) . . . . ? Al1 O1 C11 C12 27.0(2) . . . . ? O1 C11 C12 C13 -175.52(15) . . . . ? C16 C11 C12 C13 3.6(2) . . . . ? O1 C11 C12 C68 2.8(2) . . . . ? C16 C11 C12 C68 -178.06(15) . . . . ? C11 C12 C13 C14 0.8(3) . . . . ? C68 C12 C13 C14 -177.68(16) . . . . ? C12 C13 C14 C15 -3.9(3) . . . . ? C12 C13 C14 C141 170.20(16) . . . . ? C13 C14 C141 C142 11.9(3) . . . . ? C15 C14 C141 C142 -174.25(18) . . . . ? C13 C14 C141 C144 133.66(18) . . . . ? C15 C14 C141 C144 -52.5(2) . . . . ? C13 C14 C141 C143 -106.7(2) . . . . ? C15 C14 C141 C143 67.1(2) . . . . ? C13 C14 C15 C16 2.9(3) . . . . ? C141 C14 C15 C16 -171.35(16) . . . . ? C14 C15 C16 C11 1.4(3) . . . . ? C14 C15 C16 C17 171.95(16) . . . . ? O1 C11 C16 C15 174.55(15) . . . . ? C12 C11 C16 C15 -4.6(2) . . . . ? O1 C11 C16 C17 4.0(2) . . . . ? C12 C11 C16 C17 -175.09(15) . . . . ? C15 C16 C17 N18 144.64(16) . . . . ? C11 C16 C17 N18 -44.9(2) . . . . ? C15 C16 C17 C171 -92.61(19) . . . . ? C11 C16 C17 C171 77.83(19) . . . . ? C16 C17 N18 C21 -76.6(2) . . . . ? C171 C17 N18 C21 160.35(15) . . . . ? C17 N18 C21 C22 -2.0(2) . . . . ? C17 N18 C21 C26 -178.53(14) . . . . ? N18 C21 C22 C23 -175.84(17) . . . . ? C26 C21 C22 C23 0.7(2) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C23 C24 C25 C26 0.1(3) . . . . ? C24 C25 C26 C21 0.2(3) . . . . ? C24 C25 C26 C27 178.40(18) . . . . ? N18 C21 C26 C25 176.13(16) . . . . ? C22 C21 C26 C25 -0.5(2) . . . . ? N18 C21 C26 C27 -2.1(2) . . . . ? C22 C21 C26 C27 -178.73(15) . . . . ? C25 C26 C27 C28 82.4(2) . . . . ? C21 C26 C27 C28 -99.38(18) . . . . ? C26 C27 C28 C31 -171.57(15) . . . . ? C27 C28 C31 C32 -19.9(2) . . . . ? C27 C28 C31 C36 158.39(15) . . . . ? C36 C31 C32 C33 -3.2(3) . . . . ? C28 C31 C32 C33 175.19(17) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? C32 C33 C34 C35 2.3(3) . . . . ? C33 C34 C35 C36 0.0(3) . . . . ? C34 C35 C36 N37 173.82(16) . . . . ? C34 C35 C36 C31 -3.9(3) . . . . ? C32 C31 C36 N37 -172.38(16) . . . . ? C28 C31 C36 N37 9.3(2) . . . . ? C32 C31 C36 C35 5.3(2) . . . . ? C28 C31 C36 C35 -173.02(16) . . . . ? C35 C36 N37 C38 43.3(2) . . . . ? C31 C36 N37 C38 -139.01(17) . . . . ? C36 N37 C38 C42 -167.18(15) . . . . ? C36 N37 C38 C381 67.8(2) . . . . ? C73 Al2 O4 C41 -124.14(15) . . . . ? C74 Al2 O4 C41 99.66(16) . . . . ? N48 Al2 O4 C41 -12.29(15) . . . . ? Al2 O4 C41 C42 -173.24(12) . . . . ? Al2 O4 C41 C46 7.5(2) . . . . ? O4 C41 C42 C43 175.56(15) . . . . ? C46 C41 C42 C43 -5.1(2) . . . . ? O4 C41 C42 C38 -1.9(2) . . . . ? C46 C41 C42 C38 177.38(15) . . . . ? N37 C38 C42 C43 136.48(16) . . . . ? C381 C38 C42 C43 -98.42(19) . . . . ? N37 C38 C42 C41 -46.1(2) . . . . ? C381 C38 C42 C41 79.0(2) . . . . ? C41 C42 C43 C44 1.3(3) . . . . ? C38 C42 C43 C44 178.79(16) . . . . ? C42 C43 C44 C45 3.0(3) . . . . ? C42 C43 C44 C441 -178.19(18) . . . . ? C45 C44 C441 C442 -165.0(8) . . . . ? C43 C44 C441 C442 16.2(8) . . . . ? C45 C44 C441 C444 71.5(5) . . . . ? C43 C44 C441 C444 -107.2(5) . . . . ? C45 C44 C441 C446 -16.4(6) . . . . ? C43 C44 C441 C446 164.8(6) . . . . ? C45 C44 C441 C445 -140.3(5) . . . . ? C43 C44 C441 C445 40.9(5) . . . . ? C45 C44 C441 C443 -46.7(5) . . . . ? C43 C44 C441 C443 134.6(5) . . . . ? C45 C44 C441 C447 105.3(4) . . . . ? C43 C44 C441 C447 -73.4(4) . . . . ? C43 C44 C45 C46 -3.2(3) . . . . ? C441 C44 C45 C46 177.91(17) . . . . ? C44 C45 C46 C41 -0.6(3) . . . . ? C44 C45 C46 C47 179.51(17) . . . . ? O4 C41 C46 C45 -175.82(16) . . . . ? C42 C41 C46 C45 4.9(2) . . . . ? O4 C41 C46 C47 4.0(3) . . . . ? C42 C41 C46 C47 -175.24(15) . . . . ? C45 C46 C47 N48 173.91(16) . . . . ? C41 C46 C47 N48 -6.0(3) . . . . ? C46 C47 N48 C51 -179.90(15) . . . . ? C46 C47 N48 Al2 -2.6(2) . . . . ? O4 Al2 N48 C47 9.41(14) . . . . ? C73 Al2 N48 C47 123.45(14) . . . . ? C74 Al2 N48 C47 -105.10(14) . . . . ? O4 Al2 N48 C51 -173.43(12) . . . . ? C73 Al2 N48 C51 -59.38(14) . . . . ? C74 Al2 N48 C51 72.06(13) . . . . ? C47 N48 C51 C56 -69.17(19) . . . . ? Al2 N48 C51 C56 113.48(15) . . . . ? C47 N48 C51 C52 110.14(17) . . . . ? Al2 N48 C51 C52 -67.21(17) . . . . ? C56 C51 C52 C53 1.2(2) . . . . ? N48 C51 C52 C53 -178.11(14) . . . . ? C51 C52 C53 C54 -1.5(3) . . . . ? C52 C53 C54 C55 0.9(3) . . . . ? C53 C54 C55 C56 0.0(3) . . . . ? C54 C55 C56 C51 -0.3(2) . . . . ? C54 C55 C56 C57 -179.80(16) . . . . ? C52 C51 C56 C55 -0.3(2) . . . . ? N48 C51 C56 C55 178.95(14) . . . . ? C52 C51 C56 C57 179.18(15) . . . . ? N48 C51 C56 C57 -1.5(2) . . . . ? C55 C56 C57 C58 77.0(2) . . . . ? C51 C56 C57 C58 -102.54(19) . . . . ? C56 C57 C58 C61 177.68(15) . . . . ? C57 C58 C61 C62 38.3(2) . . . . ? C57 C58 C61 C66 -139.66(17) . . . . ? C66 C61 C62 C63 1.8(3) . . . . ? C58 C61 C62 C63 -176.30(17) . . . . ? C61 C62 C63 C64 1.1(3) . . . . ? C62 C63 C64 C65 -2.1(3) . . . . ? C63 C64 C65 C66 0.1(2) . . . . ? C64 C65 C66 C61 3.0(2) . . . . ? C64 C65 C66 N67 -176.86(14) . . . . ? C62 C61 C66 C65 -3.8(2) . . . . ? C58 C61 C66 C65 174.20(17) . . . . ? C62 C61 C66 N67 176.02(15) . . . . ? C58 C61 C66 N67 -6.0(2) . . . . ? C65 C66 N67 C68 130.10(16) . . . . ? C61 C66 N67 C68 -49.7(2) . . . . ? C65 C66 N67 Al1 -39.14(18) . . . . ? C61 C66 N67 Al1 141.02(13) . . . . ? O1 Al1 N67 C68 27.91(13) . . . . ? C71 Al1 N67 C68 143.81(13) . . . . ? C72 Al1 N67 C68 -82.50(14) . . . . ? O1 Al1 N67 C66 -163.01(12) . . . . ? C71 Al1 N67 C66 -47.11(14) . . . . ? C72 Al1 N67 C66 86.58(14) . . . . ? C66 N67 C68 C12 -179.66(15) . . . . ? Al1 N67 C68 C12 -10.1(2) . . . . ? C13 C12 C68 N67 168.31(16) . . . . ? C11 C12 C68 N67 -10.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.250 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.035 #===END data_abdea17 _database_code_depnum_ccdc_archive 'CCDC 692214' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4' _chemical_melting_point ? _chemical_formula_structural Al4-complex _chemical_formula_moiety 'C66 H86 Al4 N6 O2' _chemical_formula_sum 'C66 H86 Al4 N6 O2' _chemical_formula_weight 1103.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 2(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 20.7137(6) _cell_length_b 13.6334(3) _cell_length_c 23.6742(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.436(3) _cell_angle_gamma 90.00 _cell_volume 6378.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.983 _exptl_absorpt_correction_T_max 1.014 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_reflns_number 65005 _diffrn_reflns_av_R_equivalents 0.1144 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11208 _reflns_number_gt 6299 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0437P)^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 11208 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.69937(4) 0.02227(6) 0.26878(4) 0.0208(2) Uani 1 1 d . . . Al2 Al 0.43206(4) 0.42816(7) 0.13155(4) 0.0227(2) Uani 1 1 d . . . Al3 Al 0.68796(4) 0.18381(6) 0.36414(4) 0.0203(2) Uani 1 1 d . . . Al4 Al 0.37818(4) 0.29565(6) 0.22103(4) 0.0254(2) Uani 1 1 d . . . C1 C 0.74008(15) -0.1022(2) 0.29954(13) 0.0316(8) Uani 1 1 d . . . H1A H 0.7645 -0.1277 0.2741 0.047 Uiso 1 1 calc R . . H1B H 0.7053 -0.1477 0.3012 0.047 Uiso 1 1 calc R . . H1C H 0.7706 -0.0929 0.3386 0.047 Uiso 1 1 calc R . . C2 C 0.74609(14) 0.1233(2) 0.23839(13) 0.0302(8) Uani 1 1 d . . . H2A H 0.7165 0.1784 0.2253 0.045 Uiso 1 1 calc R . . H2B H 0.7592 0.0977 0.2057 0.045 Uiso 1 1 calc R . . H2C H 0.7856 0.1439 0.2691 0.045 Uiso 1 1 calc R . . C3 C 0.39921(15) 0.3272(2) 0.07151(13) 0.0329(8) Uani 1 1 d . . . H3A H 0.4200 0.2656 0.0862 0.049 Uiso 0.50 1 calc PR . . H3B H 0.4104 0.3448 0.0363 0.049 Uiso 0.50 1 calc PR . . H3C H 0.3510 0.3214 0.0625 0.049 Uiso 0.50 1 calc PR . . H3D H 0.3676 0.3556 0.0371 0.049 Uiso 0.50 1 calc PR . . H3E H 0.3772 0.2764 0.0870 0.049 Uiso 0.50 1 calc PR . . H3F H 0.4366 0.2998 0.0608 0.049 Uiso 0.50 1 calc PR . . C4 C 0.40236(15) 0.5640(2) 0.11946(14) 0.0345(8) Uani 1 1 d . . . H4A H 0.4000 0.5838 0.0800 0.052 Uiso 1 1 calc R . . H4B H 0.4340 0.6050 0.1475 0.052 Uiso 1 1 calc R . . H4C H 0.3585 0.5701 0.1250 0.052 Uiso 1 1 calc R . . C5 C 0.42347(19) 0.1705(2) 0.22155(16) 0.0544(11) Uani 1 1 d . . . H5A H 0.4211 0.1527 0.1818 0.082 Uiso 1 1 calc R . . H5B H 0.4017 0.1211 0.2382 0.082 Uiso 1 1 calc R . . H5C H 0.4700 0.1761 0.2449 0.082 Uiso 1 1 calc R . . C6 C 0.29407(15) 0.3184(3) 0.15654(14) 0.0476(10) Uani 1 1 d . . . H6A H 0.2992 0.2942 0.1200 0.071 Uiso 1 1 calc R . . H6B H 0.2846 0.3875 0.1530 0.071 Uiso 1 1 calc R . . H6C H 0.2574 0.2847 0.1651 0.071 Uiso 1 1 calc R . . C7 C 0.65093(15) 0.2994(2) 0.31714(13) 0.0304(8) Uani 1 1 d . . . H7A H 0.6731 0.3087 0.2873 0.046 Uiso 1 1 calc R . . H7B H 0.6581 0.3560 0.3424 0.046 Uiso 1 1 calc R . . H7C H 0.6033 0.2904 0.2986 0.046 Uiso 1 1 calc R . . C8 C 0.78655(13) 0.1608(2) 0.38544(13) 0.0274(7) Uani 1 1 d . . . H8A H 0.8020 0.1745 0.3519 0.041 Uiso 0.50 1 calc PR . . H8B H 0.7961 0.0937 0.3971 0.041 Uiso 0.50 1 calc PR . . H8C H 0.8094 0.2031 0.4177 0.041 Uiso 0.50 1 calc PR . . H8D H 0.8030 0.1397 0.4259 0.041 Uiso 0.50 1 calc PR . . H8E H 0.8089 0.2205 0.3806 0.041 Uiso 0.50 1 calc PR . . H8F H 0.7956 0.1111 0.3601 0.041 Uiso 0.50 1 calc PR . . O1 O 0.65277(9) 0.06916(13) 0.31858(8) 0.0190(4) Uani 1 1 d . . . C11 C 0.59615(13) 0.01949(19) 0.32387(12) 0.0188(7) Uani 1 1 d . . . C12 C 0.55169(13) -0.0260(2) 0.27375(12) 0.0189(7) Uani 1 1 d . . . C14 C 0.47647(14) -0.07229(19) 0.33092(13) 0.0207(7) Uani 1 1 d . . . C15 C 0.52291(14) -0.0297(2) 0.37948(13) 0.0229(7) Uani 1 1 d . . . H15 H 0.5139 -0.0323 0.4156 0.027 Uiso 1 1 calc R . . C16 C 0.58224(13) 0.01666(19) 0.37777(12) 0.0175(6) Uani 1 1 d . . . C17 C 0.62923(14) 0.0623(2) 0.43354(12) 0.0218(7) Uani 1 1 d . . . H17 H 0.6045 0.0662 0.4629 0.026 Uiso 1 1 calc R . . C171 C 0.69126(14) -0.0030(2) 0.45939(13) 0.0294(8) Uani 1 1 d . . . H17A H 0.7201 0.0264 0.4949 0.044 Uiso 1 1 calc R . . H17B H 0.7157 -0.0100 0.4310 0.044 Uiso 1 1 calc R . . H17C H 0.6768 -0.0664 0.4685 0.044 Uiso 1 1 calc R . . N18 N 0.64765(11) 0.16188(16) 0.42210(10) 0.0203(6) Uani 1 1 d . . . C13 C 0.49304(14) -0.0701(2) 0.27864(13) 0.0227(7) Uani 1 1 d . . . H13 H 0.4638 -0.0995 0.2453 0.027 Uiso 1 1 calc R . . C141 C 0.40958(14) -0.1166(2) 0.33318(13) 0.0251(7) Uani 1 1 d . . . C142 C 0.35146(15) -0.0611(2) 0.29031(15) 0.0427(9) Uani 1 1 d . . . H14A H 0.3092 -0.0884 0.2916 0.064 Uiso 1 1 calc R . . H14B H 0.3549 -0.0668 0.2509 0.064 Uiso 1 1 calc R . . H14C H 0.3537 0.0068 0.3014 0.064 Uiso 1 1 calc R . . C143 C 0.40613(17) -0.2245(2) 0.31499(17) 0.0491(10) Uani 1 1 d . . . H14D H 0.4425 -0.2598 0.3421 0.074 Uiso 1 1 calc R . . H14E H 0.4101 -0.2297 0.2757 0.074 Uiso 1 1 calc R . . H14F H 0.3636 -0.2518 0.3157 0.074 Uiso 1 1 calc R . . C144 C 0.40098(16) -0.1097(3) 0.39477(14) 0.0436(9) Uani 1 1 d . . . H14G H 0.4369 -0.1449 0.4225 0.065 Uiso 1 1 calc R . . H14H H 0.3583 -0.1378 0.3942 0.065 Uiso 1 1 calc R . . H14I H 0.4023 -0.0421 0.4064 0.065 Uiso 1 1 calc R . . C21 C 0.64702(14) 0.2346(2) 0.46451(12) 0.0199(7) Uani 1 1 d . . . C22 C 0.58755(14) 0.2646(2) 0.47646(12) 0.0218(7) Uani 1 1 d . . . C23 C 0.59214(15) 0.3383(2) 0.51817(13) 0.0280(8) Uani 1 1 d . . . H23 H 0.5531 0.3575 0.5268 0.034 Uiso 1 1 calc R . . C24 C 0.65248(15) 0.3840(2) 0.54726(14) 0.0317(8) Uani 1 1 d . . . H24 H 0.6539 0.4331 0.5749 0.038 Uiso 1 1 calc R . . C25 C 0.71051(15) 0.3557(2) 0.53471(13) 0.0275(8) Uani 1 1 d . . . H25 H 0.7515 0.3865 0.5532 0.033 Uiso 1 1 calc R . . C26 C 0.70726(15) 0.2811(2) 0.49445(12) 0.0250(7) Uani 1 1 d . . . H26 H 0.7469 0.2613 0.4871 0.030 Uiso 1 1 calc R . . C27 C 0.51941(13) 0.2204(2) 0.44527(13) 0.0287(8) Uani 1 1 d . . . H27A H 0.5050 0.1809 0.4734 0.034 Uiso 1 1 calc R . . H27B H 0.5242 0.1771 0.4143 0.034 Uiso 1 1 calc R . . C28 C 0.46468(13) 0.2951(2) 0.41806(13) 0.0269(7) Uani 1 1 d . . . H28A H 0.4628 0.3419 0.4484 0.032 Uiso 1 1 calc R . . H28B H 0.4775 0.3309 0.3876 0.032 Uiso 1 1 calc R . . C31 C 0.39458(14) 0.2531(2) 0.39096(13) 0.0213(7) Uani 1 1 d . . . C32 C 0.36741(14) 0.1888(2) 0.42362(13) 0.0265(7) Uani 1 1 d . . . H32 H 0.3922 0.1750 0.4626 0.032 Uiso 1 1 calc R . . C33 C 0.30489(15) 0.1448(2) 0.40019(14) 0.0313(8) Uani 1 1 d . . . H33 H 0.2878 0.1027 0.4232 0.038 Uiso 1 1 calc R . . C34 C 0.26838(15) 0.1641(2) 0.34247(14) 0.0315(8) Uani 1 1 d . . . H34 H 0.2267 0.1339 0.3258 0.038 Uiso 1 1 calc R . . C35 C 0.29366(14) 0.2281(2) 0.30938(13) 0.0263(7) Uani 1 1 d . . . H35 H 0.2683 0.2411 0.2705 0.032 Uiso 1 1 calc R . . C36 C 0.35668(14) 0.2745(2) 0.33264(13) 0.0206(7) Uani 1 1 d . . . N37 N 0.37997(11) 0.33594(16) 0.29526(10) 0.0217(6) Uani 1 1 d . . . C38 C 0.39381(13) 0.4389(2) 0.31339(12) 0.0206(7) Uani 1 1 d . . . H38 H 0.3988 0.4427 0.3558 0.025 Uiso 1 1 calc R . . C381 C 0.33499(14) 0.5061(2) 0.28133(14) 0.0294(8) Uani 1 1 d . . . H38A H 0.2940 0.4828 0.2878 0.044 Uiso 1 1 calc R . . H38B H 0.3299 0.5059 0.2397 0.044 Uiso 1 1 calc R . . H38C H 0.3441 0.5716 0.2964 0.044 Uiso 1 1 calc R . . O4 O 0.43522(9) 0.39745(13) 0.20809(8) 0.0193(5) Uani 1 1 d . . . C41 C 0.47740(13) 0.45319(19) 0.25385(12) 0.0185(7) Uani 1 1 d . . . C42 C 0.53931(14) 0.48662(19) 0.24870(12) 0.0169(6) Uani 1 1 d . . . C43 C 0.58204(14) 0.54188(19) 0.29446(12) 0.0211(7) Uani 1 1 d . . . H43 H 0.6229 0.5639 0.2905 0.025 Uiso 1 1 calc R . . C44 C 0.56589(14) 0.5650(2) 0.34533(12) 0.0187(6) Uani 1 1 d . . . C45 C 0.50404(14) 0.5297(2) 0.34855(12) 0.0217(7) Uani 1 1 d . . . H45 H 0.4917 0.5443 0.3823 0.026 Uiso 1 1 calc R . . C46 C 0.45941(13) 0.47386(19) 0.30462(12) 0.0170(6) Uani 1 1 d . . . C47 C 0.56576(14) 0.45908(19) 0.20085(13) 0.0203(7) Uani 1 1 d . . . H47 H 0.6117 0.4687 0.2065 0.024 Uiso 1 1 calc R . . N48 N 0.53065(11) 0.42229(16) 0.15103(10) 0.0190(5) Uani 1 1 d . . . C441 C 0.61582(14) 0.6241(2) 0.39427(13) 0.0250(7) Uani 1 1 d . . . C442 C 0.68270(15) 0.5679(2) 0.41541(14) 0.0395(9) Uani 1 1 d . . . H44A H 0.7143 0.6043 0.4463 0.059 Uiso 1 1 calc R . . H44B H 0.7009 0.5593 0.3829 0.059 Uiso 1 1 calc R . . H44C H 0.6750 0.5049 0.4303 0.059 Uiso 1 1 calc R . . C443 C 0.62832(16) 0.7234(2) 0.36958(14) 0.0402(9) Uani 1 1 d . . . H44D H 0.6598 0.7605 0.4001 0.060 Uiso 1 1 calc R . . H44E H 0.5864 0.7586 0.3558 0.060 Uiso 1 1 calc R . . H44F H 0.6466 0.7135 0.3373 0.060 Uiso 1 1 calc R . . C444 C 0.59005(16) 0.6394(2) 0.44742(14) 0.0415(9) Uani 1 1 d . . . H44G H 0.6228 0.6760 0.4772 0.062 Uiso 1 1 calc R . . H44H H 0.5829 0.5769 0.4632 0.062 Uiso 1 1 calc R . . H44I H 0.5481 0.6750 0.4354 0.062 Uiso 1 1 calc R . . C51 C 0.56777(13) 0.3925(2) 0.11080(12) 0.0189(7) Uani 1 1 d . . . C52 C 0.58438(14) 0.4629(2) 0.07589(13) 0.0267(7) Uani 1 1 d . . . H52 H 0.5698 0.5272 0.0770 0.032 Uiso 1 1 calc R . . C53 C 0.62258(15) 0.4382(2) 0.03937(14) 0.0316(8) Uani 1 1 d . . . H53 H 0.6342 0.4857 0.0159 0.038 Uiso 1 1 calc R . . C54 C 0.64338(15) 0.3426(2) 0.03801(13) 0.0291(8) Uani 1 1 d . . . H54 H 0.6694 0.3254 0.0136 0.035 Uiso 1 1 calc R . . C55 C 0.62595(14) 0.2725(2) 0.07246(13) 0.0274(7) Uani 1 1 d . . . H55 H 0.6413 0.2086 0.0716 0.033 Uiso 1 1 calc R . . C56 C 0.58577(13) 0.2949(2) 0.10875(12) 0.0200(7) Uani 1 1 d . . . C57 C 0.56578(15) 0.2158(2) 0.14540(13) 0.0262(7) Uani 1 1 d . . . H57A H 0.5359 0.2445 0.1655 0.031 Uiso 1 1 calc R . . H57B H 0.6061 0.1937 0.1755 0.031 Uiso 1 1 calc R . . C58 C 0.53026(14) 0.1257(2) 0.10980(13) 0.0242(7) Uani 1 1 d . . . H58A H 0.5015 0.0963 0.1308 0.029 Uiso 1 1 calc R . . H58B H 0.5012 0.1483 0.0718 0.029 Uiso 1 1 calc R . . C61 C 0.57672(14) 0.04740(19) 0.09886(13) 0.0204(7) Uani 1 1 d . . . C62 C 0.58272(15) 0.0331(2) 0.04244(13) 0.0275(7) Uani 1 1 d . . . H62 H 0.5551 0.0692 0.0111 0.033 Uiso 1 1 calc R . . C63 C 0.62801(16) -0.0325(2) 0.03129(14) 0.0304(8) Uani 1 1 d . . . H63 H 0.6303 -0.0405 -0.0071 0.036 Uiso 1 1 calc R . . C64 C 0.66975(15) -0.0860(2) 0.07687(14) 0.0310(8) Uani 1 1 d . . . H64 H 0.7014 -0.1289 0.0699 0.037 Uiso 1 1 calc R . . C65 C 0.66422(14) -0.0753(2) 0.13294(13) 0.0264(7) Uani 1 1 d . . . H65 H 0.6919 -0.1121 0.1639 0.032 Uiso 1 1 calc R . . C66 C 0.61811(14) -0.0107(2) 0.14386(12) 0.0192(7) Uani 1 1 d . . . N67 N 0.61632(11) -0.00407(15) 0.20446(10) 0.0190(5) Uani 1 1 d . . . C68 C 0.56124(14) -0.02736(19) 0.21594(12) 0.0207(7) Uani 1 1 d . . . H68 H 0.5246 -0.0467 0.1843 0.025 Uiso 1 1 calc R . . N91 N 0.56725(17) 0.7228(3) 0.18789(17) 0.0751(12) Uani 1 1 d . . . C92 C 0.54723(17) 0.7381(3) 0.13891(19) 0.0451(10) Uani 1 1 d . . . C93 C 0.52333(18) 0.7590(3) 0.07618(16) 0.0510(10) Uani 1 1 d . . . H93A H 0.5544 0.7323 0.0573 0.076 Uiso 1 1 calc R . . H93B H 0.5201 0.8287 0.0702 0.076 Uiso 1 1 calc R . . H93C H 0.4795 0.7299 0.0594 0.076 Uiso 1 1 calc R . . N101 N 0.40360(18) 0.9111(3) 0.11233(15) 0.0701(11) Uani 1 1 d . . . C102 C 0.3485(2) 0.9011(3) 0.10699(17) 0.0520(11) Uani 1 1 d . . . C103 C 0.2764(2) 0.8913(3) 0.0995(2) 0.0881(16) Uani 1 1 d . . . H10A H 0.2512 0.9260 0.0646 0.132 Uiso 1 1 calc R . . H10B H 0.2664 0.9181 0.1334 0.132 Uiso 1 1 calc R . . H10C H 0.2641 0.8231 0.0955 0.132 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 0.0209(5) 0.0220(5) 0.0211(5) -0.0006(4) 0.0087(4) 0.0000(4) Al2 0.0233(5) 0.0279(5) 0.0172(5) 0.0005(4) 0.0066(4) 0.0009(4) Al3 0.0234(5) 0.0186(5) 0.0200(5) -0.0002(4) 0.0081(4) -0.0010(4) Al4 0.0283(5) 0.0258(6) 0.0267(6) -0.0065(4) 0.0153(4) -0.0073(4) C1 0.0356(19) 0.0298(19) 0.029(2) -0.0023(15) 0.0090(16) 0.0029(15) C2 0.0289(18) 0.035(2) 0.029(2) -0.0023(15) 0.0129(15) -0.0037(14) C3 0.0292(18) 0.044(2) 0.0256(19) -0.0034(16) 0.0089(15) -0.0002(15) C4 0.036(2) 0.039(2) 0.027(2) 0.0075(16) 0.0086(16) 0.0046(16) C5 0.084(3) 0.031(2) 0.070(3) -0.0003(19) 0.057(2) -0.0003(19) C6 0.031(2) 0.083(3) 0.032(2) -0.019(2) 0.0139(17) -0.0145(19) C7 0.0344(19) 0.0285(19) 0.031(2) 0.0027(15) 0.0141(16) 0.0022(15) C8 0.0275(17) 0.0256(18) 0.031(2) -0.0017(14) 0.0119(15) -0.0002(14) O1 0.0191(10) 0.0205(11) 0.0205(12) 0.0001(9) 0.0106(9) -0.0031(8) C11 0.0171(16) 0.0172(16) 0.0229(18) 0.0025(13) 0.0072(13) 0.0013(13) C12 0.0218(16) 0.0179(16) 0.0172(17) 0.0043(13) 0.0064(13) 0.0026(13) C14 0.0210(16) 0.0141(16) 0.0282(19) 0.0050(14) 0.0093(14) 0.0024(13) C15 0.0288(17) 0.0244(17) 0.0184(18) 0.0035(14) 0.0116(14) -0.0011(14) C16 0.0217(16) 0.0137(15) 0.0172(17) 0.0024(13) 0.0060(13) 0.0012(12) C17 0.0269(17) 0.0233(17) 0.0180(17) -0.0003(13) 0.0110(14) -0.0034(13) C171 0.0329(19) 0.0272(19) 0.0245(19) 0.0039(14) 0.0032(15) -0.0022(14) N18 0.0265(14) 0.0158(14) 0.0197(14) -0.0022(11) 0.0088(11) -0.0015(11) C13 0.0229(17) 0.0204(17) 0.0229(18) -0.0018(14) 0.0040(14) -0.0016(13) C141 0.0237(17) 0.0252(18) 0.0278(19) 0.0038(14) 0.0100(15) -0.0022(13) C142 0.0292(19) 0.050(2) 0.051(2) 0.0158(19) 0.0159(17) 0.0005(16) C143 0.043(2) 0.032(2) 0.081(3) -0.005(2) 0.032(2) -0.0113(16) C144 0.036(2) 0.060(3) 0.039(2) 0.0034(19) 0.0179(18) -0.0198(17) C21 0.0241(17) 0.0199(17) 0.0141(17) 0.0048(13) 0.0034(13) -0.0014(13) C22 0.0271(17) 0.0215(17) 0.0181(18) -0.0004(14) 0.0088(14) -0.0010(13) C23 0.0248(17) 0.034(2) 0.028(2) -0.0030(15) 0.0126(15) 0.0007(14) C24 0.037(2) 0.033(2) 0.026(2) -0.0110(15) 0.0095(16) -0.0028(16) C25 0.0257(18) 0.0286(19) 0.025(2) -0.0031(15) 0.0027(15) -0.0065(14) C26 0.0297(18) 0.0262(18) 0.0211(18) 0.0010(14) 0.0107(14) 0.0004(14) C27 0.0259(18) 0.0297(19) 0.032(2) -0.0075(15) 0.0112(15) -0.0023(14) C28 0.0255(17) 0.0288(19) 0.0259(19) 0.0014(15) 0.0071(14) -0.0046(14) C31 0.0238(17) 0.0191(17) 0.0239(19) -0.0022(14) 0.0115(14) 0.0010(13) C32 0.0319(18) 0.0282(19) 0.0204(18) -0.0002(14) 0.0094(15) -0.0028(15) C33 0.038(2) 0.0303(19) 0.031(2) 0.0029(15) 0.0191(17) -0.0106(15) C34 0.0291(18) 0.037(2) 0.030(2) -0.0084(16) 0.0113(16) -0.0157(15) C35 0.0234(17) 0.0321(19) 0.0225(19) -0.0017(15) 0.0056(14) -0.0021(14) C36 0.0233(16) 0.0184(17) 0.0235(19) -0.0030(13) 0.0121(14) -0.0010(13) N37 0.0251(14) 0.0185(14) 0.0233(15) 0.0002(11) 0.0100(11) -0.0025(11) C38 0.0260(17) 0.0230(18) 0.0147(17) -0.0046(13) 0.0092(14) -0.0005(13) C381 0.0275(18) 0.0236(18) 0.038(2) -0.0004(15) 0.0120(15) 0.0022(14) O4 0.0232(11) 0.0214(11) 0.0124(11) -0.0033(8) 0.0040(9) -0.0033(8) C41 0.0227(16) 0.0130(16) 0.0181(17) 0.0011(12) 0.0036(13) 0.0001(12) C42 0.0232(16) 0.0163(16) 0.0127(16) 0.0027(13) 0.0075(13) 0.0031(12) C43 0.0212(16) 0.0213(17) 0.0234(18) 0.0027(13) 0.0106(14) -0.0019(13) C44 0.0229(16) 0.0173(16) 0.0165(17) -0.0005(13) 0.0071(13) 0.0009(13) C45 0.0288(17) 0.0209(17) 0.0181(17) 0.0001(13) 0.0113(14) 0.0028(13) C46 0.0233(16) 0.0105(15) 0.0189(17) 0.0012(13) 0.0086(13) 0.0018(12) C47 0.0197(16) 0.0201(17) 0.0227(19) 0.0050(14) 0.0088(14) -0.0004(13) N48 0.0254(14) 0.0171(13) 0.0166(14) -0.0012(11) 0.0094(11) 0.0007(11) C441 0.0282(18) 0.0265(18) 0.0225(19) -0.0078(14) 0.0112(15) -0.0047(14) C442 0.033(2) 0.055(2) 0.026(2) -0.0097(17) 0.0025(16) 0.0013(17) C443 0.047(2) 0.032(2) 0.042(2) -0.0103(17) 0.0145(18) -0.0126(16) C444 0.038(2) 0.056(2) 0.032(2) -0.0222(18) 0.0131(17) -0.0166(17) C51 0.0219(16) 0.0238(18) 0.0114(16) -0.0014(13) 0.0053(13) -0.0030(13) C52 0.0324(18) 0.0236(18) 0.0251(19) 0.0008(14) 0.0102(15) 0.0007(14) C53 0.042(2) 0.032(2) 0.026(2) -0.0010(15) 0.0183(16) -0.0112(16) C54 0.0335(19) 0.037(2) 0.0235(19) -0.0084(15) 0.0185(15) -0.0072(15) C55 0.0301(18) 0.0247(18) 0.0286(19) -0.0062(15) 0.0107(15) 0.0012(14) C56 0.0192(16) 0.0241(18) 0.0166(17) -0.0013(13) 0.0050(13) 0.0008(13) C57 0.0330(18) 0.0240(18) 0.0247(19) 0.0027(14) 0.0135(15) 0.0070(14) C58 0.0270(17) 0.0237(18) 0.0227(19) 0.0050(14) 0.0085(14) 0.0050(14) C61 0.0255(17) 0.0176(17) 0.0187(17) -0.0013(13) 0.0075(14) -0.0044(13) C62 0.0321(18) 0.0247(19) 0.0254(19) 0.0033(15) 0.0084(15) -0.0029(14) C63 0.042(2) 0.031(2) 0.023(2) -0.0066(15) 0.0181(16) -0.0080(16) C64 0.0353(19) 0.0290(19) 0.035(2) -0.0074(16) 0.0208(17) 0.0036(15) C65 0.0282(18) 0.0252(18) 0.026(2) -0.0012(14) 0.0088(15) 0.0030(14) C66 0.0232(16) 0.0182(16) 0.0175(17) -0.0031(13) 0.0080(13) -0.0038(13) N67 0.0241(14) 0.0179(14) 0.0165(14) 0.0010(10) 0.0086(11) 0.0018(10) C68 0.0249(17) 0.0145(16) 0.0202(18) 0.0022(13) 0.0028(14) 0.0015(13) N91 0.067(3) 0.092(3) 0.060(3) 0.029(2) 0.010(2) -0.008(2) C92 0.036(2) 0.043(2) 0.057(3) 0.015(2) 0.015(2) -0.0007(17) C93 0.056(3) 0.046(2) 0.047(3) 0.0048(19) 0.011(2) -0.0015(18) N101 0.058(2) 0.086(3) 0.059(3) 0.005(2) 0.006(2) -0.004(2) C102 0.057(3) 0.059(3) 0.036(2) 0.0126(19) 0.008(2) -0.004(2) C103 0.068(3) 0.103(4) 0.095(4) 0.039(3) 0.027(3) -0.013(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 1.8473(19) . ? Al1 C1 1.937(3) . ? Al1 C2 1.942(3) . ? Al1 N67 1.959(2) . ? Al2 O4 1.842(2) . ? Al2 C4 1.945(3) . ? Al2 C3 1.949(3) . ? Al2 N48 1.956(2) . ? Al3 N18 1.832(2) . ? Al3 O1 1.9149(19) . ? Al3 C7 1.949(3) . ? Al3 C8 1.976(3) . ? Al4 N37 1.831(2) . ? Al4 O4 1.9059(19) . ? Al4 C5 1.945(3) . ? Al4 C6 1.967(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 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? C3 H3E 0.9600 . ? C3 H3F 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8D 0.9600 . ? C8 H8E 0.9600 . ? C8 H8F 0.9600 . ? O1 C11 1.392(3) . ? C11 C16 1.390(4) . ? C11 C12 1.409(4) . ? C12 C13 1.392(4) . ? C12 C68 1.440(4) . ? C14 C13 1.380(4) . ? C14 C15 1.386(4) . ? C14 C141 1.527(4) . ? C15 C16 1.393(4) . ? C15 H15 0.9300 . ? C16 C17 1.519(4) . ? C17 N18 1.457(3) . ? C17 C171 1.532(4) . ? C17 H17 0.9800 . ? C171 H17A 0.9600 . ? C171 H17B 0.9600 . ? C171 H17C 0.9600 . ? N18 C21 1.414(3) . ? C13 H13 0.9300 . ? C141 C142 1.523(4) . ? C141 C144 1.524(4) . ? C141 C143 1.528(4) . ? C142 H14A 0.9600 . ? C142 H14B 0.9600 . ? C142 H14C 0.9600 . ? C143 H14D 0.9600 . ? C143 H14E 0.9600 . ? C143 H14F 0.9600 . ? C144 H14G 0.9600 . ? C144 H14H 0.9600 . ? C144 H14I 0.9600 . ? C21 C26 1.390(4) . ? C21 C22 1.405(4) . ? C22 C23 1.392(4) . ? C22 C27 1.509(4) . ? C23 C24 1.382(4) . ? C23 H23 0.9300 . ? C24 C25 1.377(4) . ? C24 H24 0.9300 . ? C25 C26 1.381(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.517(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C31 1.514(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C31 C32 1.394(4) . ? C31 C36 1.399(4) . ? C32 C33 1.384(4) . ? C32 H32 0.9300 . ? C33 C34 1.375(4) . ? C33 H33 0.9300 . ? C34 C35 1.378(4) . ? C34 H34 0.9300 . ? C35 C36 1.405(4) . ? C35 H35 0.9300 . ? C36 N37 1.405(3) . ? N37 C38 1.471(3) . ? C38 C46 1.512(4) . ? C38 C381 1.531(4) . ? C38 H38 0.9800 . ? C381 H38A 0.9600 . ? C381 H38B 0.9600 . ? C381 H38C 0.9600 . ? O4 C41 1.396(3) . ? C41 C46 1.390(4) . ? C41 C42 1.400(4) . ? C42 C43 1.396(4) . ? C42 C47 1.448(4) . ? C43 C44 1.379(4) . ? C43 H43 0.9300 . ? C44 C45 1.392(4) . ? C44 C441 1.531(4) . ? C45 C46 1.392(4) . ? C45 H45 0.9300 . ? C47 N48 1.287(3) . ? C47 H47 0.9300 . ? N48 C51 1.450(3) . ? C441 C444 1.522(4) . ? C441 C443 1.527(4) . ? C441 C442 1.530(4) . ? C442 H44A 0.9600 . ? C442 H44B 0.9600 . ? C442 H44C 0.9600 . ? C443 H44D 0.9600 . ? C443 H44E 0.9600 . ? C443 H44F 0.9600 . ? C444 H44G 0.9600 . ? C444 H44H 0.9600 . ? C444 H44I 0.9600 . ? C51 C52 1.375(4) . ? C51 C56 1.387(4) . ? C52 C53 1.377(4) . ? C52 H52 0.9300 . ? C53 C54 1.377(4) . ? C53 H53 0.9300 . ? C54 C55 1.373(4) . ? C54 H54 0.9300 . ? C55 C56 1.397(4) . ? C55 H55 0.9300 . ? C56 C57 1.517(4) . ? C57 C58 1.545(4) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C61 1.511(4) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C61 C62 1.392(4) . ? C61 C66 1.396(4) . ? C62 C63 1.378(4) . ? C62 H62 0.9300 . ? C63 C64 1.373(4) . ? C63 H63 0.9300 . ? C64 C65 1.374(4) . ? C64 H64 0.9300 . ? C65 C66 1.380(4) . ? C65 H65 0.9300 . ? C66 N67 1.449(3) . ? N67 C68 1.289(3) . ? C68 H68 0.9300 . ? N91 C92 1.128(4) . ? C92 C93 1.446(5) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? N101 C102 1.118(4) . ? C102 C103 1.456(5) . ? C103 H10A 0.9600 . ? C103 H10B 0.9600 . ? C103 H10C 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 C1 108.36(12) . . ? O1 Al1 C2 113.87(12) . . ? C1 Al1 C2 123.49(13) . . ? O1 Al1 N67 93.12(9) . . ? C1 Al1 N67 108.27(11) . . ? C2 Al1 N67 105.15(12) . . ? O4 Al2 C4 106.12(11) . . ? O4 Al2 C3 117.29(12) . . ? C4 Al2 C3 122.63(14) . . ? O4 Al2 N48 91.84(9) . . ? C4 Al2 N48 109.61(12) . . ? C3 Al2 N48 104.76(12) . . ? N18 Al3 O1 96.12(9) . . ? N18 Al3 C7 111.71(12) . . ? O1 Al3 C7 108.67(11) . . ? N18 Al3 C8 116.81(12) . . ? O1 Al3 C8 101.78(11) . . ? C7 Al3 C8 118.28(13) . . ? N37 Al4 O4 95.77(10) . . ? N37 Al4 C5 112.70(14) . . ? O4 Al4 C5 108.58(12) . . ? N37 Al4 C6 117.14(13) . . ? O4 Al4 C6 102.00(13) . . ? C5 Al4 C6 117.18(16) . . ? 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 . . ? Al2 C3 H3A 109.5 . . ? Al2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Al2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Al2 C3 H3D 109.5 . . ? H3A C3 H3D 141.1 . . ? H3B C3 H3D 56.3 . . ? H3C C3 H3D 56.3 . . ? Al2 C3 H3E 109.5 . . ? H3A C3 H3E 56.3 . . ? H3B C3 H3E 141.1 . . ? H3C C3 H3E 56.3 . . ? H3D C3 H3E 109.5 . . ? Al2 C3 H3F 109.5 . . ? H3A C3 H3F 56.3 . . ? H3B C3 H3F 56.3 . . ? H3C C3 H3F 141.1 . . ? H3D C3 H3F 109.5 . . ? H3E C3 H3F 109.5 . . ? Al2 C4 H4A 109.5 . . ? Al2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Al2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Al4 C5 H5A 109.5 . . ? Al4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Al4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Al4 C6 H6A 109.5 . . ? Al4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Al4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Al3 C7 H7A 109.5 . . ? Al3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Al3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Al3 C8 H8A 109.5 . . ? Al3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Al3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Al3 C8 H8D 109.5 . . ? H8A C8 H8D 141.1 . . ? H8B C8 H8D 56.3 . . ? H8C C8 H8D 56.3 . . ? Al3 C8 H8E 109.5 . . ? H8A C8 H8E 56.3 . . ? H8B C8 H8E 141.1 . . ? H8C C8 H8E 56.3 . . ? H8D C8 H8E 109.5 . . ? Al3 C8 H8F 109.5 . . ? H8A C8 H8F 56.3 . . ? H8B C8 H8F 56.3 . . ? H8C C8 H8F 141.1 . . ? H8D C8 H8F 109.5 . . ? H8E C8 H8F 109.5 . . ? C11 O1 Al1 120.30(16) . . ? C11 O1 Al3 122.36(16) . . ? Al1 O1 Al3 117.28(9) . . ? C16 C11 O1 120.5(2) . . ? C16 C11 C12 119.9(3) . . ? O1 C11 C12 119.6(2) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 C68 116.4(3) . . ? C11 C12 C68 124.4(3) . . ? C13 C14 C15 115.9(3) . . ? C13 C14 C141 120.8(3) . . ? C15 C14 C141 123.2(3) . . ? C14 C15 C16 124.4(3) . . ? C14 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C11 C16 C15 117.8(3) . . ? C11 C16 C17 122.1(2) . . ? C15 C16 C17 120.1(2) . . ? N18 C17 C16 110.8(2) . . ? N18 C17 C171 112.4(2) . . ? C16 C17 C171 110.5(2) . . ? N18 C17 H17 107.6 . . ? C16 C17 H17 107.6 . . ? C171 C17 H17 107.6 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C21 N18 C17 117.5(2) . . ? C21 N18 Al3 121.39(18) . . ? C17 N18 Al3 119.66(18) . . ? C14 C13 C12 122.8(3) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C142 C141 C144 108.1(3) . . ? C142 C141 C14 108.9(2) . . ? C144 C141 C14 112.1(2) . . ? C142 C141 C143 109.2(3) . . ? C144 C141 C143 108.7(3) . . ? C14 C141 C143 109.7(2) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? C26 C21 C22 118.1(3) . . ? C26 C21 N18 119.0(3) . . ? C22 C21 N18 122.9(2) . . ? C23 C22 C21 118.4(3) . . ? C23 C22 C27 119.4(3) . . ? C21 C22 C27 122.2(3) . . ? C24 C23 C22 122.6(3) . . ? C24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C25 C24 C23 118.9(3) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C24 C25 C26 119.4(3) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C21 122.6(3) . . ? C25 C26 H26 118.7 . . ? C21 C26 H26 118.7 . . ? C22 C27 C28 114.2(2) . . ? C22 C27 H27A 108.7 . . ? C28 C27 H27A 108.7 . . ? C22 C27 H27B 108.7 . . ? C28 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C31 C28 C27 115.2(2) . . ? C31 C28 H28A 108.5 . . ? C27 C28 H28A 108.5 . . ? C31 C28 H28B 108.5 . . ? C27 C28 H28B 108.5 . . ? H28A C28 H28B 107.5 . . ? C32 C31 C36 118.5(3) . . ? C32 C31 C28 119.9(3) . . ? C36 C31 C28 121.5(3) . . ? C33 C32 C31 122.4(3) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C34 C33 C32 119.1(3) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 119.8(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 121.9(3) . . ? C34 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C31 C36 N37 123.3(2) . . ? C31 C36 C35 118.3(3) . . ? N37 C36 C35 118.4(3) . . ? C36 N37 C38 117.3(2) . . ? C36 N37 Al4 120.90(18) . . ? C38 N37 Al4 120.83(18) . . ? N37 C38 C46 111.4(2) . . ? N37 C38 C381 111.7(2) . . ? C46 C38 C381 111.0(2) . . ? N37 C38 H38 107.5 . . ? C46 C38 H38 107.5 . . ? C381 C38 H38 107.5 . . ? C38 C381 H38A 109.5 . . ? C38 C381 H38B 109.5 . . ? H38A C381 H38B 109.5 . . ? C38 C381 H38C 109.5 . . ? H38A C381 H38C 109.5 . . ? H38B C381 H38C 109.5 . . ? C41 O4 Al2 117.99(16) . . ? C41 O4 Al4 123.08(16) . . ? Al2 O4 Al4 118.86(10) . . ? C46 C41 O4 120.9(2) . . ? C46 C41 C42 119.9(2) . . ? O4 C41 C42 119.1(2) . . ? C43 C42 C41 119.5(3) . . ? C43 C42 C47 116.5(3) . . ? C41 C42 C47 123.7(3) . . ? C44 C43 C42 122.5(3) . . ? C44 C43 H43 118.7 . . ? C42 C43 H43 118.7 . . ? C43 C44 C45 115.9(3) . . ? C43 C44 C441 119.7(2) . . ? C45 C44 C441 124.4(3) . . ? C46 C45 C44 124.3(3) . . ? C46 C45 H45 117.8 . . ? C44 C45 H45 117.8 . . ? C41 C46 C45 117.8(3) . . ? C41 C46 C38 122.7(2) . . ? C45 C46 C38 119.5(2) . . ? N48 C47 C42 125.1(3) . . ? N48 C47 H47 117.4 . . ? C42 C47 H47 117.4 . . ? C47 N48 C51 116.5(2) . . ? C47 N48 Al2 117.60(19) . . ? C51 N48 Al2 125.34(18) . . ? C444 C441 C443 109.7(3) . . ? C444 C441 C442 107.8(3) . . ? C443 C441 C442 109.2(3) . . ? C444 C441 C44 111.9(2) . . ? C443 C441 C44 109.3(2) . . ? C442 C441 C44 108.9(2) . . ? C441 C442 H44A 109.5 . . ? C441 C442 H44B 109.5 . . ? H44A C442 H44B 109.5 . . ? C441 C442 H44C 109.5 . . ? H44A C442 H44C 109.5 . . ? H44B C442 H44C 109.5 . . ? C441 C443 H44D 109.5 . . ? C441 C443 H44E 109.5 . . ? H44D C443 H44E 109.5 . . ? C441 C443 H44F 109.5 . . ? H44D C443 H44F 109.5 . . ? H44E C443 H44F 109.5 . . ? C441 C444 H44G 109.5 . . ? C441 C444 H44H 109.5 . . ? H44G C444 H44H 109.5 . . ? C441 C444 H44I 109.5 . . ? H44G C444 H44I 109.5 . . ? H44H C444 H44I 109.5 . . ? C52 C51 C56 122.0(3) . . ? C52 C51 N48 118.5(2) . . ? C56 C51 N48 119.5(2) . . ? C51 C52 C53 120.1(3) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 119.2(3) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C55 C54 C53 120.3(3) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 121.7(3) . . ? C54 C55 H55 119.2 . . ? C56 C55 H55 119.2 . . ? C51 C56 C55 116.5(3) . . ? C51 C56 C57 122.7(3) . . ? C55 C56 C57 120.8(3) . . ? C56 C57 C58 114.8(2) . . ? C56 C57 H57A 108.6 . . ? C58 C57 H57A 108.6 . . ? C56 C57 H57B 108.6 . . ? C58 C57 H57B 108.6 . . ? H57A C57 H57B 107.5 . . ? C61 C58 C57 115.6(2) . . ? C61 C58 H58A 108.4 . . ? C57 C58 H58A 108.4 . . ? C61 C58 H58B 108.4 . . ? C57 C58 H58B 108.4 . . ? H58A C58 H58B 107.5 . . ? C62 C61 C66 116.2(3) . . ? C62 C61 C58 120.5(3) . . ? C66 C61 C58 123.2(3) . . ? C63 C62 C61 122.4(3) . . ? C63 C62 H62 118.8 . . ? C61 C62 H62 118.8 . . ? C64 C63 C62 119.9(3) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 119.2(3) . . ? C63 C64 H64 120.4 . . ? C65 C64 H64 120.4 . . ? C64 C65 C66 120.8(3) . . ? C64 C65 H65 119.6 . . ? C66 C65 H65 119.6 . . ? C65 C66 C61 121.4(3) . . ? C65 C66 N67 116.7(2) . . ? C61 C66 N67 121.9(2) . . ? C68 N67 C66 118.7(2) . . ? C68 N67 Al1 120.5(2) . . ? C66 N67 Al1 120.27(18) . . ? N67 C68 C12 125.4(3) . . ? N67 C68 H68 117.3 . . ? C12 C68 H68 117.3 . . ? N91 C92 C93 178.4(4) . . ? C92 C93 H93A 109.5 . . ? C92 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C92 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? N101 C102 C103 178.3(5) . . ? C102 C103 H10A 109.5 . . ? C102 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? C102 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 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 C1 Al1 O1 C11 -65.8(2) . . . . ? C2 Al1 O1 C11 152.66(19) . . . . ? N67 Al1 O1 C11 44.59(19) . . . . ? C1 Al1 O1 Al3 111.53(13) . . . . ? C2 Al1 O1 Al3 -29.97(16) . . . . ? N67 Al1 O1 Al3 -138.05(11) . . . . ? N18 Al3 O1 C11 20.0(2) . . . . ? C7 Al3 O1 C11 -95.4(2) . . . . ? C8 Al3 O1 C11 139.05(19) . . . . ? N18 Al3 O1 Al1 -157.32(11) . . . . ? C7 Al3 O1 Al1 87.29(14) . . . . ? C8 Al3 O1 Al1 -38.26(14) . . . . ? Al1 O1 C11 C16 145.3(2) . . . . ? Al3 O1 C11 C16 -31.9(3) . . . . ? Al1 O1 C11 C12 -36.4(3) . . . . ? Al3 O1 C11 C12 146.3(2) . . . . ? C16 C11 C12 C13 2.3(4) . . . . ? O1 C11 C12 C13 -176.0(2) . . . . ? C16 C11 C12 C68 180.0(3) . . . . ? O1 C11 C12 C68 1.7(4) . . . . ? C13 C14 C15 C16 2.3(4) . . . . ? C141 C14 C15 C16 -175.8(3) . . . . ? O1 C11 C16 C15 176.6(2) . . . . ? C12 C11 C16 C15 -1.6(4) . . . . ? O1 C11 C16 C17 -3.2(4) . . . . ? C12 C11 C16 C17 178.6(2) . . . . ? C14 C15 C16 C11 -0.7(4) . . . . ? C14 C15 C16 C17 179.1(3) . . . . ? C11 C16 C17 N18 48.7(3) . . . . ? C15 C16 C17 N18 -131.2(3) . . . . ? C11 C16 C17 C171 -76.6(3) . . . . ? C15 C16 C17 C171 103.6(3) . . . . ? C16 C17 N18 C21 136.4(2) . . . . ? C171 C17 N18 C21 -99.3(3) . . . . ? C16 C17 N18 Al3 -57.0(3) . . . . ? C171 C17 N18 Al3 67.3(3) . . . . ? O1 Al3 N18 C21 -169.2(2) . . . . ? C7 Al3 N18 C21 -56.3(2) . . . . ? C8 Al3 N18 C21 84.3(2) . . . . ? O1 Al3 N18 C17 24.7(2) . . . . ? C7 Al3 N18 C17 137.6(2) . . . . ? C8 Al3 N18 C17 -81.8(2) . . . . ? C15 C14 C13 C12 -1.7(4) . . . . ? C141 C14 C13 C12 176.5(2) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C68 C12 C13 C14 -178.4(3) . . . . ? C13 C14 C141 C142 -59.3(4) . . . . ? C15 C14 C141 C142 118.7(3) . . . . ? C13 C14 C141 C144 -178.9(3) . . . . ? C15 C14 C141 C144 -0.9(4) . . . . ? C13 C14 C141 C143 60.2(4) . . . . ? C15 C14 C141 C143 -121.7(3) . . . . ? C17 N18 C21 C26 117.0(3) . . . . ? Al3 N18 C21 C26 -49.4(3) . . . . ? C17 N18 C21 C22 -65.3(3) . . . . ? Al3 N18 C21 C22 128.3(2) . . . . ? C26 C21 C22 C23 -0.9(4) . . . . ? N18 C21 C22 C23 -178.6(3) . . . . ? C26 C21 C22 C27 178.5(3) . . . . ? N18 C21 C22 C27 0.8(4) . . . . ? C21 C22 C23 C24 1.3(4) . . . . ? C27 C22 C23 C24 -178.2(3) . . . . ? C22 C23 C24 C25 -0.1(5) . . . . ? C23 C24 C25 C26 -1.4(4) . . . . ? C24 C25 C26 C21 1.7(5) . . . . ? C22 C21 C26 C25 -0.6(4) . . . . ? N18 C21 C26 C25 177.2(3) . . . . ? C23 C22 C27 C28 50.9(4) . . . . ? C21 C22 C27 C28 -128.5(3) . . . . ? C22 C27 C28 C31 -175.1(2) . . . . ? C27 C28 C31 C32 50.8(4) . . . . ? C27 C28 C31 C36 -126.9(3) . . . . ? C36 C31 C32 C33 0.8(4) . . . . ? C28 C31 C32 C33 -177.1(3) . . . . ? C31 C32 C33 C34 0.7(5) . . . . ? C32 C33 C34 C35 -1.4(5) . . . . ? C33 C34 C35 C36 0.7(5) . . . . ? C32 C31 C36 N37 -178.1(3) . . . . ? C28 C31 C36 N37 -0.3(4) . . . . ? C32 C31 C36 C35 -1.5(4) . . . . ? C28 C31 C36 C35 176.3(3) . . . . ? C34 C35 C36 C31 0.8(4) . . . . ? C34 C35 C36 N37 177.6(3) . . . . ? C31 C36 N37 C38 -62.4(3) . . . . ? C35 C36 N37 C38 120.9(3) . . . . ? C31 C36 N37 Al4 128.5(2) . . . . ? C35 C36 N37 Al4 -48.1(3) . . . . ? O4 Al4 N37 C36 -166.5(2) . . . . ? C5 Al4 N37 C36 -53.6(2) . . . . ? C6 Al4 N37 C36 86.8(2) . . . . ? O4 Al4 N37 C38 24.8(2) . . . . ? C5 Al4 N37 C38 137.7(2) . . . . ? C6 Al4 N37 C38 -81.9(2) . . . . ? C36 N37 C38 C46 136.4(2) . . . . ? Al4 N37 C38 C46 -54.5(3) . . . . ? C36 N37 C38 C381 -98.8(3) . . . . ? Al4 N37 C38 C381 70.2(3) . . . . ? C4 Al2 O4 C41 -58.9(2) . . . . ? C3 Al2 O4 C41 159.73(18) . . . . ? N48 Al2 O4 C41 52.08(18) . . . . ? C4 Al2 O4 Al4 118.30(13) . . . . ? C3 Al2 O4 Al4 -23.02(17) . . . . ? N48 Al2 O4 Al4 -130.68(12) . . . . ? N37 Al4 O4 C41 18.3(2) . . . . ? C5 Al4 O4 C41 -98.0(2) . . . . ? C6 Al4 O4 C41 137.7(2) . . . . ? N37 Al4 O4 Al2 -158.75(12) . . . . ? C5 Al4 O4 Al2 84.94(16) . . . . ? C6 Al4 O4 Al2 -39.40(15) . . . . ? Al2 O4 C41 C46 145.5(2) . . . . ? Al4 O4 C41 C46 -31.7(3) . . . . ? Al2 O4 C41 C42 -36.0(3) . . . . ? Al4 O4 C41 C42 146.9(2) . . . . ? C46 C41 C42 C43 -1.0(4) . . . . ? O4 C41 C42 C43 -179.6(2) . . . . ? C46 C41 C42 C47 172.5(3) . . . . ? O4 C41 C42 C47 -6.1(4) . . . . ? C41 C42 C43 C44 0.3(4) . . . . ? C47 C42 C43 C44 -173.6(3) . . . . ? C42 C43 C44 C45 0.1(4) . . . . ? C42 C43 C44 C441 178.7(3) . . . . ? C43 C44 C45 C46 0.2(4) . . . . ? C441 C44 C45 C46 -178.3(3) . . . . ? O4 C41 C46 C45 179.8(2) . . . . ? C42 C41 C46 C45 1.2(4) . . . . ? O4 C41 C46 C38 -0.6(4) . . . . ? C42 C41 C46 C38 -179.2(2) . . . . ? C44 C45 C46 C41 -0.9(4) . . . . ? C44 C45 C46 C38 179.5(2) . . . . ? N37 C38 C46 C41 44.0(3) . . . . ? C381 C38 C46 C41 -81.2(3) . . . . ? N37 C38 C46 C45 -136.5(3) . . . . ? C381 C38 C46 C45 98.4(3) . . . . ? C43 C42 C47 N48 -168.4(3) . . . . ? C41 C42 C47 N48 18.0(4) . . . . ? C42 C47 N48 C51 -175.3(2) . . . . ? C42 C47 N48 Al2 13.1(4) . . . . ? O4 Al2 N48 C47 -40.7(2) . . . . ? C4 Al2 N48 C47 67.1(2) . . . . ? C3 Al2 N48 C47 -159.6(2) . . . . ? O4 Al2 N48 C51 148.4(2) . . . . ? C4 Al2 N48 C51 -103.7(2) . . . . ? C3 Al2 N48 C51 29.6(2) . . . . ? C43 C44 C441 C444 -178.2(3) . . . . ? C45 C44 C441 C444 0.3(4) . . . . ? C43 C44 C441 C443 60.1(3) . . . . ? C45 C44 C441 C443 -121.4(3) . . . . ? C43 C44 C441 C442 -59.1(3) . . . . ? C45 C44 C441 C442 119.4(3) . . . . ? C47 N48 C51 C52 -82.1(3) . . . . ? Al2 N48 C51 C52 88.8(3) . . . . ? C47 N48 C51 C56 97.6(3) . . . . ? Al2 N48 C51 C56 -91.5(3) . . . . ? C56 C51 C52 C53 -2.9(4) . . . . ? N48 C51 C52 C53 176.7(3) . . . . ? C51 C52 C53 C54 0.4(5) . . . . ? C52 C53 C54 C55 0.3(5) . . . . ? C53 C54 C55 C56 1.4(5) . . . . ? C52 C51 C56 C55 4.5(4) . . . . ? N48 C51 C56 C55 -175.2(2) . . . . ? C52 C51 C56 C57 -177.9(3) . . . . ? N48 C51 C56 C57 2.5(4) . . . . ? C54 C55 C56 C51 -3.7(4) . . . . ? C54 C55 C56 C57 178.6(3) . . . . ? C51 C56 C57 C58 127.6(3) . . . . ? C55 C56 C57 C58 -54.8(4) . . . . ? C56 C57 C58 C61 84.8(3) . . . . ? C57 C58 C61 C62 -108.8(3) . . . . ? C57 C58 C61 C66 67.9(4) . . . . ? C66 C61 C62 C63 -1.7(4) . . . . ? C58 C61 C62 C63 175.2(3) . . . . ? C61 C62 C63 C64 -0.6(5) . . . . ? C62 C63 C64 C65 2.0(5) . . . . ? C63 C64 C65 C66 -1.0(5) . . . . ? C64 C65 C66 C61 -1.5(4) . . . . ? C64 C65 C66 N67 -179.6(3) . . . . ? C62 C61 C66 C65 2.7(4) . . . . ? C58 C61 C66 C65 -174.1(3) . . . . ? C62 C61 C66 N67 -179.3(2) . . . . ? C58 C61 C66 N67 3.9(4) . . . . ? C65 C66 N67 C68 -118.4(3) . . . . ? C61 C66 N67 C68 63.5(3) . . . . ? C65 C66 N67 Al1 53.4(3) . . . . ? C61 C66 N67 Al1 -124.8(2) . . . . ? O1 Al1 N67 C68 -30.4(2) . . . . ? C1 Al1 N67 C68 80.1(2) . . . . ? C2 Al1 N67 C68 -146.2(2) . . . . ? O1 Al1 N67 C66 157.96(19) . . . . ? C1 Al1 N67 C66 -91.5(2) . . . . ? C2 Al1 N67 C66 42.2(2) . . . . ? C66 N67 C68 C12 179.1(2) . . . . ? Al1 N67 C68 C12 7.4(4) . . . . ? C13 C12 C68 N67 -168.8(3) . . . . ? C11 C12 C68 N67 13.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.301 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.046