# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew Johnson' _publ_contact_author_email CHSALJ@BATH.AC.UK _publ_section_title ; Synthesis and Structure of Aluminium Amine-phenolate Complexes ; loop_ _publ_author_name 'Andrew Johnson' 'M Davidson' 'Matthew D Jones' 'Nicolas Merle' 'Yolanda Perez' 'Paul Raithby' ; S.P.Richards ; # Attachment '[Al_L2_]2.cif' data_[Al(L2)]2 _database_code_depnum_ccdc_archive 'CCDC 729812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Al(L2))2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H72 Al2 N2 O6' _chemical_formula_weight 983.16 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7360(1) _cell_length_b 15.6960(2) _cell_length_c 17.5490(3) _cell_angle_alpha 83.346(1) _cell_angle_beta 74.345(1) _cell_angle_gamma 74.317(1) _cell_volume 2738.57(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 54058 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 28.283 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD' _diffrn_measurement_method 'Omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 46610 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.56 _reflns_number_total 12512 _reflns_number_gt 10478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0496P)^2^+1.0771P] 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 12512 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.60110(4) 0.28747(3) 0.43042(2) 0.02080(9) Uani 1 1 d . . . N1 N 0.71175(11) 0.19808(7) 0.34221(7) 0.0220(2) Uani 1 1 d . . . O1 O 0.50880(9) 0.20204(6) 0.46297(6) 0.0246(2) Uani 1 1 d . . . C1 C 0.55329(15) 0.11897(9) 0.42689(9) 0.0274(3) Uani 1 1 d . . . H1A H 0.4763 0.0953 0.4276 0.033 Uiso 1 1 calc R . . H1B H 0.6129 0.0756 0.4554 0.033 Uiso 1 1 calc R . . C2 C 0.62816(14) 0.13597(10) 0.34240(8) 0.0272(3) Uani 1 1 d . . . H2A H 0.6857 0.0795 0.3196 0.033 Uiso 1 1 calc R . . H2B H 0.5640 0.1621 0.3096 0.033 Uiso 1 1 calc R . . O2 O 0.73865(9) 0.29136(7) 0.46398(6) 0.0256(2) Uani 1 1 d . . . C21 C 0.86860(13) 0.27500(9) 0.42395(8) 0.0236(3) Uani 1 1 d . . . C22 C 0.94973(14) 0.32605(10) 0.43652(9) 0.0278(3) Uani 1 1 d . . . C23 C 1.08305(15) 0.30772(10) 0.39433(10) 0.0330(3) Uani 1 1 d . . . H23 H 1.1384 0.3417 0.4032 0.040 Uiso 1 1 calc R . . C24 C 1.13870(14) 0.24174(11) 0.33977(10) 0.0334(3) Uani 1 1 d . . . C25 C 1.05678(14) 0.19188(10) 0.32836(9) 0.0284(3) Uani 1 1 d . . . H25 H 1.0923 0.1470 0.2908 0.034 Uiso 1 1 calc R . . C26 C 0.92334(13) 0.20637(9) 0.37097(8) 0.0246(3) Uani 1 1 d . . . C27 C 0.89141(16) 0.39789(11) 0.49526(10) 0.0359(3) Uani 1 1 d . . . H27A H 0.9589 0.4296 0.4945 0.054 Uiso 1 1 calc R . . H27B H 0.8634 0.3714 0.5485 0.054 Uiso 1 1 calc R . . H27C H 0.8140 0.4395 0.4811 0.054 Uiso 1 1 calc R . . C28 C 1.28425(16) 0.22376(13) 0.29493(13) 0.0499(5) Uani 1 1 d . . . H28A H 1.3195 0.1602 0.2862 0.075 Uiso 1 1 calc R . . H28B H 1.3351 0.2424 0.3258 0.075 Uiso 1 1 calc R . . H28C H 1.2924 0.2570 0.2437 0.075 Uiso 1 1 calc R . . C29 C 0.83852(13) 0.14740(9) 0.36343(8) 0.0252(3) Uani 1 1 d . . . H29A H 0.8903 0.1045 0.3222 0.030 Uiso 1 1 calc R . . H29B H 0.8163 0.1135 0.4143 0.030 Uiso 1 1 calc R . . O3 O 0.55169(10) 0.37242(7) 0.36298(6) 0.0274(2) Uani 1 1 d . . . C31 C 0.53616(14) 0.36585(9) 0.29024(8) 0.0255(3) Uani 1 1 d . . . C32 C 0.42746(15) 0.42479(10) 0.26681(9) 0.0305(3) Uani 1 1 d . . . C33 C 0.41568(17) 0.42082(11) 0.19038(10) 0.0377(4) Uani 1 1 d . . . H33 H 0.3438 0.4617 0.1738 0.045 Uiso 1 1 calc R . . C34 C 0.50421(18) 0.35976(12) 0.13720(10) 0.0395(4) Uani 1 1 d . . . C35 C 0.60877(16) 0.30049(11) 0.16261(9) 0.0331(3) Uani 1 1 d . . . H35 H 0.6696 0.2573 0.1277 0.040 Uiso 1 1 calc R . . C36 C 0.62639(14) 0.30300(10) 0.23824(8) 0.0266(3) Uani 1 1 d . . . C37 C 0.32722(16) 0.48799(11) 0.32541(11) 0.0397(4) Uani 1 1 d . . . H37A H 0.3669 0.5347 0.3332 0.059 Uiso 1 1 calc R . . H37B H 0.3014 0.4558 0.3761 0.059 Uiso 1 1 calc R . . H37C H 0.2480 0.5147 0.3052 0.059 Uiso 1 1 calc R . . C38 C 0.4858(2) 0.35629(17) 0.05516(12) 0.0624(6) Uani 1 1 d . . . H38A H 0.3989 0.3446 0.0596 0.094 Uiso 1 1 calc R . . H38B H 0.5570 0.3089 0.0267 0.094 Uiso 1 1 calc R . . H38C H 0.4895 0.4131 0.0261 0.094 Uiso 1 1 calc R . . C39 C 0.74604(14) 0.24212(10) 0.26177(8) 0.0258(3) Uani 1 1 d . . . H39A H 0.7893 0.1960 0.2223 0.031 Uiso 1 1 calc R . . H39B H 0.8113 0.2765 0.2608 0.031 Uiso 1 1 calc R . . Al2 Al 0.40620(4) 0.23592(3) 0.56349(2) 0.02086(9) Uani 1 1 d . . . N2 N 0.32635(11) 0.31098(7) 0.66256(7) 0.0218(2) Uani 1 1 d . . . O4 O 0.47631(9) 0.33072(6) 0.52301(6) 0.0240(2) Uani 1 1 d . . . C3 C 0.46066(14) 0.40178(9) 0.57115(8) 0.0252(3) Uani 1 1 d . . . H3A H 0.3914 0.4538 0.5592 0.030 Uiso 1 1 calc R . . H3B H 0.5458 0.4193 0.5613 0.030 Uiso 1 1 calc R . . C4 C 0.41900(14) 0.36858(9) 0.65680(8) 0.0249(3) Uani 1 1 d . . . H4A H 0.4988 0.3345 0.6748 0.030 Uiso 1 1 calc R . . H4B H 0.3738 0.4194 0.6912 0.030 Uiso 1 1 calc R . . O5 O 0.25382(9) 0.22834(7) 0.55119(6) 0.0256(2) Uani 1 1 d . . . C51 C 0.13271(13) 0.24466(9) 0.60332(8) 0.0230(3) Uani 1 1 d . . . C52 C 0.04308(14) 0.19411(9) 0.60236(8) 0.0258(3) Uani 1 1 d . . . C53 C -0.08128(14) 0.21189(10) 0.65645(9) 0.0293(3) Uani 1 1 d . . . H53 H -0.1428 0.1788 0.6552 0.035 Uiso 1 1 calc R . . C54 C -0.11930(14) 0.27645(10) 0.71251(9) 0.0292(3) Uani 1 1 d . . . C55 C -0.02857(14) 0.32517(10) 0.71229(9) 0.0265(3) Uani 1 1 d . . . H55 H -0.0518 0.3692 0.7500 0.032 Uiso 1 1 calc R . . C56 C 0.09580(13) 0.31084(9) 0.65791(8) 0.0239(3) Uani 1 1 d . . . C57 C 0.08472(16) 0.12135(10) 0.54525(10) 0.0329(3) Uani 1 1 d . . . H57A H 0.0110 0.0933 0.5517 0.049 Uiso 1 1 calc R . . H57B H 0.1628 0.0770 0.5559 0.049 Uiso 1 1 calc R . . H57C H 0.1075 0.1462 0.4909 0.049 Uiso 1 1 calc R . . C58 C -0.25256(15) 0.29119(12) 0.77256(10) 0.0393(4) Uani 1 1 d . . . H58A H -0.2448 0.2503 0.8187 0.059 Uiso 1 1 calc R . . H58B H -0.3194 0.2805 0.7488 0.059 Uiso 1 1 calc R . . H58C H -0.2801 0.3524 0.7893 0.059 Uiso 1 1 calc R . . C59 C 0.19084(13) 0.36629(9) 0.65732(9) 0.0246(3) Uani 1 1 d . . . H59A H 0.2000 0.4042 0.6080 0.030 Uiso 1 1 calc R . . H59B H 0.1531 0.4056 0.7026 0.030 Uiso 1 1 calc R . . O6 O 0.49346(10) 0.14719(7) 0.61382(6) 0.0285(2) Uani 1 1 d . . . C61 C 0.52346(14) 0.14024(9) 0.68418(8) 0.0244(3) Uani 1 1 d . . . C62 C 0.63979(14) 0.07705(9) 0.69407(9) 0.0280(3) Uani 1 1 d . . . C63 C 0.66777(15) 0.06521(10) 0.76805(10) 0.0327(3) Uani 1 1 d . . . H63 H 0.7450 0.0215 0.7752 0.039 Uiso 1 1 calc R . . C64 C 0.58686(16) 0.11502(11) 0.83202(9) 0.0328(3) Uani 1 1 d . . . C65 C 0.47502(15) 0.17939(10) 0.81998(9) 0.0292(3) Uani 1 1 d . . . H65 H 0.4200 0.2154 0.8624 0.035 Uiso 1 1 calc R . . C66 C 0.44175(14) 0.19234(9) 0.74734(8) 0.0248(3) Uani 1 1 d . . . C67 C 0.72927(16) 0.02540(11) 0.62408(10) 0.0373(4) Uani 1 1 d . . . H67A H 0.8108 -0.0106 0.6380 0.056 Uiso 1 1 calc R . . H67B H 0.7528 0.0665 0.5793 0.056 Uiso 1 1 calc R . . H67C H 0.6825 -0.0134 0.6093 0.056 Uiso 1 1 calc R . . C68 C 0.61966(19) 0.10115(14) 0.91174(10) 0.0459(4) Uani 1 1 d . . . H68A H 0.5547 0.1446 0.9480 0.069 Uiso 1 1 calc R . . H68B H 0.7096 0.1086 0.9056 0.069 Uiso 1 1 calc R . . H68C H 0.6159 0.0412 0.9334 0.069 Uiso 1 1 calc R . . C69 C 0.31349(14) 0.25733(9) 0.73895(8) 0.0252(3) Uani 1 1 d . . . H69A H 0.2449 0.2243 0.7436 0.030 Uiso 1 1 calc R . . H69B H 0.2817 0.2980 0.7832 0.030 Uiso 1 1 calc R . . C1S C 0.72951(16) 0.03110(10) 0.14652(9) 0.0320(3) Uani 1 1 d . . . C2S C 0.74375(17) -0.03143(10) 0.20862(9) 0.0333(3) Uani 1 1 d . . . H2S H 0.6676 -0.0495 0.2404 0.040 Uiso 1 1 calc R . . C3S C 0.86694(19) -0.06786(11) 0.22501(10) 0.0413(4) Uani 1 1 d . . . H3S H 0.8748 -0.1104 0.2677 0.050 Uiso 1 1 calc R . . C4S C 0.9778(2) -0.04235(13) 0.17940(14) 0.0522(5) Uani 1 1 d . . . H4S H 1.0624 -0.0671 0.1906 0.063 Uiso 1 1 calc R . . C5S C 0.9660(2) 0.01928(14) 0.11723(14) 0.0567(5) Uani 1 1 d . . . H5S H 1.0426 0.0369 0.0856 0.068 Uiso 1 1 calc R . . C6S C 0.8427(2) 0.05540(12) 0.10095(11) 0.0445(4) Uani 1 1 d . . . H6S H 0.8357 0.0975 0.0579 0.053 Uiso 1 1 calc R . . C7S C 0.5944(2) 0.07138(13) 0.13057(12) 0.0497(5) Uani 1 1 d . . . H7S1 H 0.5414 0.1144 0.1706 0.075 Uiso 1 1 calc R . . H7S2 H 0.5485 0.0247 0.1328 0.075 Uiso 1 1 calc R . . H7S3 H 0.6054 0.1013 0.0779 0.075 Uiso 1 1 calc R . . C11S C 0.17102(19) 0.48282(11) 0.86570(11) 0.0422(4) Uani 1 1 d . . . C12S C 0.0477(2) 0.46383(13) 0.89970(11) 0.0480(4) Uani 1 1 d . . . H12S H 0.0373 0.4259 0.9461 0.058 Uiso 1 1 calc R . . C13S C -0.05948(19) 0.49934(13) 0.86689(12) 0.0475(4) Uani 1 1 d . . . H13S H -0.1429 0.4860 0.8911 0.057 Uiso 1 1 calc R . . C14S C -0.04684(19) 0.55379(11) 0.79972(11) 0.0427(4) Uani 1 1 d . . . H14S H -0.1210 0.5780 0.7773 0.051 Uiso 1 1 calc R . . C15S C 0.07409(19) 0.57305(11) 0.76507(10) 0.0389(4) Uani 1 1 d . . . H15S H 0.0836 0.6105 0.7184 0.047 Uiso 1 1 calc R . . C16S C 0.18173(18) 0.53826(11) 0.79767(10) 0.0384(4) Uani 1 1 d . . . H16S H 0.2645 0.5524 0.7732 0.046 Uiso 1 1 calc R . . C17S C 0.2880(3) 0.44590(17) 0.90193(17) 0.0742(7) Uani 1 1 d . . . H17A H 0.3669 0.4194 0.8609 0.111 Uiso 1 1 calc R . . H17B H 0.2671 0.4006 0.9432 0.111 Uiso 1 1 calc R . . H17C H 0.3060 0.4937 0.9253 0.111 Uiso 1 1 calc R . . C21S C 0.9851(2) -0.23748(12) 0.00312(11) 0.0456(4) Uani 1 1 d . . . C22S C 0.8727(2) -0.17466(13) 0.03699(11) 0.0495(5) Uani 1 1 d . . . H22S H 0.8654 -0.1528 0.0867 0.059 Uiso 1 1 calc R . . C23S C 0.7700(2) -0.14281(14) -0.00045(13) 0.0577(5) Uani 1 1 d . . . H23S H 0.6936 -0.0986 0.0234 0.069 Uiso 1 1 calc R . . C24S C 0.7774(2) -0.17438(14) -0.07168(14) 0.0562(5) Uani 1 1 d . . . H24S H 0.7062 -0.1530 -0.0969 0.067 Uiso 1 1 calc R . . C25S C 0.8900(3) -0.23771(14) -0.10621(13) 0.0595(6) Uani 1 1 d . . . H25S H 0.8969 -0.2594 -0.1559 0.071 Uiso 1 1 calc R . . C26S C 0.9923(2) -0.26958(12) -0.06886(11) 0.0483(5) Uani 1 1 d . . . H26S H 1.0685 -0.3139 -0.0926 0.058 Uiso 1 1 calc R . . C27S C 1.0977(3) -0.27091(16) 0.04362(15) 0.0677(6) Uani 1 1 d . . . H27D H 1.1438 -0.2242 0.0410 0.102 Uiso 1 1 calc R . . H27E H 1.1609 -0.3228 0.0170 0.102 Uiso 1 1 calc R . . H27F H 1.0615 -0.2874 0.0992 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 0.01806(19) 0.0225(2) 0.02170(19) -0.00255(15) -0.00501(15) -0.00412(15) N1 0.0198(5) 0.0247(6) 0.0221(5) -0.0032(4) -0.0063(4) -0.0043(4) O1 0.0242(5) 0.0238(5) 0.0256(5) -0.0066(4) -0.0021(4) -0.0073(4) C1 0.0282(7) 0.0244(7) 0.0303(7) -0.0076(6) -0.0046(6) -0.0078(6) C2 0.0264(7) 0.0285(7) 0.0283(7) -0.0088(6) -0.0063(6) -0.0070(6) O2 0.0196(5) 0.0319(5) 0.0262(5) -0.0061(4) -0.0061(4) -0.0057(4) C21 0.0191(6) 0.0267(7) 0.0250(7) 0.0023(5) -0.0089(5) -0.0038(5) C22 0.0265(7) 0.0271(7) 0.0328(7) 0.0041(6) -0.0148(6) -0.0065(6) C23 0.0257(7) 0.0336(8) 0.0444(9) 0.0089(7) -0.0170(6) -0.0113(6) C24 0.0200(7) 0.0357(8) 0.0406(8) 0.0097(7) -0.0093(6) -0.0040(6) C25 0.0219(7) 0.0291(7) 0.0292(7) 0.0032(6) -0.0071(5) 0.0006(5) C26 0.0209(6) 0.0266(7) 0.0254(7) 0.0029(5) -0.0095(5) -0.0025(5) C27 0.0359(8) 0.0319(8) 0.0462(9) -0.0034(7) -0.0193(7) -0.0094(6) C28 0.0212(8) 0.0518(11) 0.0693(13) 0.0055(9) -0.0038(8) -0.0077(7) C29 0.0217(6) 0.0234(7) 0.0281(7) -0.0022(5) -0.0072(5) -0.0004(5) O3 0.0294(5) 0.0262(5) 0.0253(5) -0.0020(4) -0.0093(4) -0.0020(4) C31 0.0242(7) 0.0286(7) 0.0257(7) 0.0025(5) -0.0089(5) -0.0087(5) C32 0.0258(7) 0.0288(7) 0.0394(8) 0.0038(6) -0.0136(6) -0.0078(6) C33 0.0334(8) 0.0396(9) 0.0457(9) 0.0084(7) -0.0239(7) -0.0085(7) C34 0.0440(9) 0.0472(10) 0.0348(8) 0.0049(7) -0.0228(7) -0.0136(8) C35 0.0348(8) 0.0403(9) 0.0272(7) -0.0009(6) -0.0118(6) -0.0105(7) C36 0.0245(7) 0.0320(7) 0.0252(7) 0.0012(6) -0.0092(5) -0.0084(6) C37 0.0307(8) 0.0317(8) 0.0547(10) -0.0018(7) -0.0169(7) 0.0014(6) C38 0.0723(15) 0.0780(15) 0.0446(11) 0.0010(10) -0.0388(11) -0.0090(12) C39 0.0225(7) 0.0326(7) 0.0206(6) -0.0025(5) -0.0050(5) -0.0038(5) Al2 0.01833(19) 0.0219(2) 0.0224(2) -0.00276(15) -0.00497(15) -0.00451(15) N2 0.0177(5) 0.0236(6) 0.0245(6) -0.0022(4) -0.0055(4) -0.0051(4) O4 0.0240(5) 0.0231(5) 0.0245(5) -0.0059(4) -0.0020(4) -0.0072(4) C3 0.0247(7) 0.0231(7) 0.0279(7) -0.0063(5) -0.0037(5) -0.0069(5) C4 0.0226(6) 0.0267(7) 0.0280(7) -0.0056(5) -0.0064(5) -0.0086(5) O5 0.0204(5) 0.0308(5) 0.0265(5) -0.0054(4) -0.0050(4) -0.0069(4) C51 0.0192(6) 0.0256(7) 0.0244(6) 0.0022(5) -0.0084(5) -0.0043(5) C52 0.0252(7) 0.0261(7) 0.0286(7) 0.0038(5) -0.0122(6) -0.0071(5) C53 0.0242(7) 0.0311(7) 0.0357(8) 0.0074(6) -0.0119(6) -0.0114(6) C54 0.0211(7) 0.0324(8) 0.0320(7) 0.0072(6) -0.0072(6) -0.0058(6) C55 0.0207(6) 0.0270(7) 0.0293(7) 0.0007(5) -0.0070(5) -0.0021(5) C56 0.0198(6) 0.0242(7) 0.0279(7) 0.0012(5) -0.0086(5) -0.0044(5) C57 0.0352(8) 0.0317(8) 0.0375(8) -0.0016(6) -0.0135(7) -0.0134(6) C58 0.0233(7) 0.0461(10) 0.0439(9) 0.0042(7) -0.0010(7) -0.0112(7) C59 0.0193(6) 0.0226(7) 0.0308(7) -0.0042(5) -0.0058(5) -0.0025(5) O6 0.0299(5) 0.0263(5) 0.0286(5) -0.0048(4) -0.0120(4) 0.0001(4) C61 0.0245(7) 0.0237(7) 0.0268(7) 0.0025(5) -0.0087(5) -0.0082(5) C62 0.0260(7) 0.0239(7) 0.0347(8) 0.0030(6) -0.0098(6) -0.0066(5) C63 0.0298(8) 0.0300(8) 0.0398(8) 0.0083(6) -0.0159(6) -0.0068(6) C64 0.0353(8) 0.0364(8) 0.0316(8) 0.0099(6) -0.0157(6) -0.0145(6) C65 0.0300(7) 0.0341(8) 0.0257(7) 0.0031(6) -0.0076(6) -0.0129(6) C66 0.0226(7) 0.0266(7) 0.0268(7) 0.0017(5) -0.0071(5) -0.0092(5) C67 0.0319(8) 0.0309(8) 0.0443(9) -0.0036(7) -0.0125(7) 0.0037(6) C68 0.0493(10) 0.0565(11) 0.0347(9) 0.0117(8) -0.0221(8) -0.0121(9) C69 0.0225(7) 0.0302(7) 0.0224(6) -0.0013(5) -0.0045(5) -0.0066(5) C1S 0.0428(9) 0.0269(7) 0.0272(7) -0.0057(6) -0.0075(6) -0.0098(6) C2S 0.0472(9) 0.0288(8) 0.0258(7) -0.0044(6) -0.0043(6) -0.0162(7) C3S 0.0613(11) 0.0301(8) 0.0371(9) 0.0006(7) -0.0203(8) -0.0118(8) C4S 0.0447(11) 0.0447(11) 0.0724(14) -0.0067(10) -0.0227(10) -0.0101(8) C5S 0.0440(11) 0.0505(12) 0.0704(14) -0.0023(10) 0.0038(10) -0.0213(9) C6S 0.0569(11) 0.0345(9) 0.0362(9) 0.0041(7) -0.0018(8) -0.0136(8) C7S 0.0541(11) 0.0452(10) 0.0532(11) -0.0081(9) -0.0237(9) -0.0051(9) C11S 0.0504(10) 0.0336(9) 0.0487(10) -0.0070(7) -0.0240(8) -0.0070(7) C12S 0.0683(13) 0.0431(10) 0.0373(9) 0.0087(8) -0.0171(9) -0.0223(9) C13S 0.0436(10) 0.0490(11) 0.0508(11) 0.0009(8) -0.0090(8) -0.0169(8) C14S 0.0463(10) 0.0324(9) 0.0513(10) -0.0024(7) -0.0194(8) -0.0057(7) C15S 0.0555(11) 0.0259(8) 0.0354(8) -0.0021(6) -0.0115(7) -0.0098(7) C16S 0.0408(9) 0.0303(8) 0.0443(9) -0.0111(7) -0.0036(7) -0.0122(7) C17S 0.0814(17) 0.0599(14) 0.100(2) -0.0048(13) -0.0642(16) -0.0073(12) C21S 0.0582(11) 0.0384(9) 0.0386(9) 0.0054(7) -0.0051(8) -0.0192(8) C22S 0.0662(13) 0.0433(10) 0.0342(9) -0.0106(8) 0.0047(8) -0.0196(9) C23S 0.0518(12) 0.0504(12) 0.0578(13) -0.0068(10) 0.0066(10) -0.0097(9) C24S 0.0554(12) 0.0525(12) 0.0635(13) -0.0004(10) -0.0183(10) -0.0159(10) C25S 0.0863(16) 0.0509(12) 0.0436(11) -0.0078(9) -0.0177(11) -0.0172(11) C26S 0.0609(12) 0.0374(9) 0.0360(9) -0.0074(7) 0.0023(8) -0.0069(8) C27S 0.0812(17) 0.0656(14) 0.0673(15) 0.0264(12) -0.0323(13) -0.0349(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.7466(11) . ? Al1 O2 1.7488(10) . ? Al1 O1 1.8279(10) . ? Al1 O4 1.8669(10) . ? Al1 N1 2.0941(12) . ? Al1 Al2 2.8856(6) . ? N1 C2 1.4921(17) . ? N1 C39 1.4957(17) . ? N1 C29 1.4977(17) . ? O1 C1 1.4215(16) . ? O1 Al2 1.8602(10) . ? C1 C2 1.516(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O2 C21 1.3509(16) . ? C21 C26 1.4018(19) . ? C21 C22 1.404(2) . ? C22 C23 1.391(2) . ? C22 C27 1.505(2) . ? C23 C24 1.390(2) . ? C23 H23 0.9500 . ? C24 C25 1.389(2) . ? C24 C28 1.513(2) . ? C25 C26 1.3958(19) . ? C25 H25 0.9500 . ? C26 C29 1.5009(19) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? O3 C31 1.3500(17) . ? C31 C36 1.400(2) . ? C31 C32 1.4050(19) . ? C32 C33 1.391(2) . ? C32 C37 1.504(2) . ? C33 C34 1.389(3) . ? C33 H33 0.9500 . ? C34 C35 1.391(2) . ? C34 C38 1.514(2) . ? C35 C36 1.397(2) . ? C35 H35 0.9500 . ? C36 C39 1.5049(19) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? Al2 O5 1.7433(10) . ? Al2 O6 1.7475(11) . ? Al2 O4 1.8322(10) . ? Al2 N2 2.0663(12) . ? N2 C69 1.4923(17) . ? N2 C4 1.4925(17) . ? N2 C59 1.4999(16) . ? O4 C3 1.4235(16) . ? C3 C4 1.521(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O5 C51 1.3510(16) . ? C51 C56 1.3990(19) . ? C51 C52 1.4072(19) . ? C52 C53 1.392(2) . ? C52 C57 1.502(2) . ? C53 C54 1.397(2) . ? C53 H53 0.9500 . ? C54 C55 1.391(2) . ? C54 C58 1.508(2) . ? C55 C56 1.3942(19) . ? C55 H55 0.9500 . ? C56 C59 1.5070(19) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? O6 C61 1.3433(17) . ? C61 C66 1.402(2) . ? C61 C62 1.4075(19) . ? C62 C63 1.391(2) . ? C62 C67 1.504(2) . ? C63 C64 1.391(2) . ? C63 H63 0.9500 . ? C64 C65 1.392(2) . ? C64 C68 1.511(2) . ? C65 C66 1.393(2) . ? C65 H65 0.9500 . ? C66 C69 1.5078(19) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C1S C6S 1.385(2) . ? C1S C2S 1.391(2) . ? C1S C7S 1.505(2) . ? C2S C3S 1.385(2) . ? C2S H2S 0.9500 . ? C3S C4S 1.374(3) . ? C3S H3S 0.9500 . ? C4S C5S 1.381(3) . ? C4S H4S 0.9500 . ? C5S C6S 1.384(3) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C11S C16S 1.391(3) . ? C11S C12S 1.394(3) . ? C11S C17S 1.506(3) . ? C12S C13S 1.379(3) . ? C12S H12S 0.9500 . ? C13S C14S 1.372(3) . ? C13S H13S 0.9500 . ? C14S C15S 1.375(3) . ? C14S H14S 0.9500 . ? C15S C16S 1.380(3) . ? C15S H15S 0.9500 . ? C16S H16S 0.9500 . ? C17S H17A 0.9800 . ? C17S H17B 0.9800 . ? C17S H17C 0.9800 . ? C21S C22S 1.374(3) . ? C21S C26S 1.389(3) . ? C21S C27S 1.508(3) . ? C22S C23S 1.383(3) . ? C22S H22S 0.9500 . ? C23S C24S 1.372(3) . ? C23S H23S 0.9500 . ? C24S C25S 1.383(3) . ? C24S H24S 0.9500 . ? C25S C26S 1.379(3) . ? C25S H25S 0.9500 . ? C26S H26S 0.9500 . ? C27S H27D 0.9800 . ? C27S H27E 0.9800 . ? C27S H27F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O2 116.21(5) . . ? O3 Al1 O1 120.00(5) . . ? O2 Al1 O1 123.79(5) . . ? O3 Al1 O4 99.43(5) . . ? O2 Al1 O4 94.19(5) . . ? O1 Al1 O4 76.43(4) . . ? O3 Al1 N1 93.83(5) . . ? O2 Al1 N1 94.99(5) . . ? O1 Al1 N1 82.35(4) . . ? O4 Al1 N1 158.55(5) . . ? O3 Al1 Al2 120.59(4) . . ? O2 Al1 Al2 108.03(4) . . ? O1 Al1 Al2 38.92(3) . . ? O4 Al1 Al2 38.30(3) . . ? N1 Al1 Al2 120.25(4) . . ? C2 N1 C39 110.22(10) . . ? C2 N1 C29 109.38(11) . . ? C39 N1 C29 108.77(10) . . ? C2 N1 Al1 106.24(8) . . ? C39 N1 Al1 113.21(8) . . ? C29 N1 Al1 108.94(8) . . ? C1 O1 Al1 121.16(8) . . ? C1 O1 Al2 132.01(9) . . ? Al1 O1 Al2 102.96(5) . . ? O1 C1 C2 106.22(11) . . ? O1 C1 H1A 110.5 . . ? C2 C1 H1A 110.5 . . ? O1 C1 H1B 110.5 . . ? C2 C1 H1B 110.5 . . ? H1A C1 H1B 108.7 . . ? N1 C2 C1 108.98(11) . . ? N1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C21 O2 Al1 128.50(9) . . ? O2 C21 C26 120.34(12) . . ? O2 C21 C22 119.79(13) . . ? C26 C21 C22 119.86(13) . . ? C23 C22 C21 118.45(14) . . ? C23 C22 C27 121.91(14) . . ? C21 C22 C27 119.64(13) . . ? C24 C23 C22 122.77(14) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C25 C24 C23 117.86(14) . . ? C25 C24 C28 120.88(16) . . ? C23 C24 C28 121.26(15) . . ? C24 C25 C26 121.32(14) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C25 C26 C21 119.68(13) . . ? C25 C26 C29 121.07(13) . . ? C21 C26 C29 119.21(12) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 C26 112.62(11) . . ? N1 C29 H29A 109.1 . . ? C26 C29 H29A 109.1 . . ? N1 C29 H29B 109.1 . . ? C26 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 O3 Al1 128.55(9) . . ? O3 C31 C36 121.48(12) . . ? O3 C31 C32 118.45(13) . . ? C36 C31 C32 120.07(13) . . ? C33 C32 C31 118.26(14) . . ? C33 C32 C37 122.64(14) . . ? C31 C32 C37 119.08(14) . . ? C34 C33 C32 122.99(14) . . ? C34 C33 H33 118.5 . . ? C32 C33 H33 118.5 . . ? C33 C34 C35 117.62(14) . . ? C33 C34 C38 121.26(16) . . ? C35 C34 C38 121.11(17) . . ? C34 C35 C36 121.53(15) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C35 C36 C31 119.49(13) . . ? C35 C36 C39 120.10(13) . . ? C31 C36 C39 120.30(12) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 C36 113.14(11) . . ? N1 C39 H39A 109.0 . . ? C36 C39 H39A 109.0 . . ? N1 C39 H39B 109.0 . . ? C36 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? O5 Al2 O6 117.23(5) . . ? O5 Al2 O4 122.05(5) . . ? O6 Al2 O4 120.70(5) . . ? O5 Al2 O1 97.19(5) . . ? O6 Al2 O1 95.08(5) . . ? O4 Al2 O1 76.49(4) . . ? O5 Al2 N2 96.02(5) . . ? O6 Al2 N2 93.37(5) . . ? O4 Al2 N2 82.60(4) . . ? O1 Al2 N2 158.93(5) . . ? O5 Al2 Al1 120.05(4) . . ? O6 Al2 Al1 106.64(4) . . ? O4 Al2 Al1 39.16(3) . . ? O1 Al2 Al1 38.12(3) . . ? N2 Al2 Al1 120.83(4) . . ? C69 N2 C4 110.51(10) . . ? C69 N2 C59 109.14(10) . . ? C4 N2 C59 110.39(10) . . ? C69 N2 Al2 113.85(8) . . ? C4 N2 Al2 105.08(8) . . ? C59 N2 Al2 107.78(8) . . ? C3 O4 Al2 121.17(8) . . ? C3 O4 Al1 133.15(8) . . ? Al2 O4 Al1 102.53(5) . . ? O4 C3 C4 106.80(11) . . ? O4 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? O4 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? N2 C4 C3 108.98(11) . . ? N2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C51 O5 Al2 128.95(9) . . ? O5 C51 C56 120.87(12) . . ? O5 C51 C52 119.24(12) . . ? C56 C51 C52 119.90(12) . . ? C53 C52 C51 118.44(13) . . ? C53 C52 C57 121.85(13) . . ? C51 C52 C57 119.68(13) . . ? C52 C53 C54 122.66(13) . . ? C52 C53 H53 118.7 . . ? C54 C53 H53 118.7 . . ? C55 C54 C53 117.65(13) . . ? C55 C54 C58 121.12(14) . . ? C53 C54 C58 121.21(14) . . ? C54 C55 C56 121.48(14) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C55 C56 C51 119.85(13) . . ? C55 C56 C59 120.49(13) . . ? C51 C56 C59 119.66(12) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N2 C59 C56 112.43(11) . . ? N2 C59 H59A 109.1 . . ? C56 C59 H59A 109.1 . . ? N2 C59 H59B 109.1 . . ? C56 C59 H59B 109.1 . . ? H59A C59 H59B 107.8 . . ? C61 O6 Al2 132.10(9) . . ? O6 C61 C66 122.12(12) . . ? O6 C61 C62 118.03(13) . . ? C66 C61 C62 119.84(13) . . ? C63 C62 C61 118.70(14) . . ? C63 C62 C67 122.63(13) . . ? C61 C62 C67 118.67(13) . . ? C62 C63 C64 122.45(14) . . ? C62 C63 H63 118.8 . . ? C64 C63 H63 118.8 . . ? C63 C64 C65 117.77(14) . . ? C63 C64 C68 121.46(15) . . ? C65 C64 C68 120.76(15) . . ? C64 C65 C66 121.71(14) . . ? C64 C65 H65 119.1 . . ? C66 C65 H65 119.1 . . ? C65 C66 C61 119.46(13) . . ? C65 C66 C69 119.88(13) . . ? C61 C66 C69 120.51(12) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 H68A 109.5 . . ? C64 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C64 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? N2 C69 C66 113.87(11) . . ? N2 C69 H69A 108.8 . . ? C66 C69 H69A 108.8 . . ? N2 C69 H69B 108.8 . . ? C66 C69 H69B 108.8 . . ? H69A C69 H69B 107.7 . . ? C6S C1S C2S 117.96(16) . . ? C6S C1S C7S 121.53(16) . . ? C2S C1S C7S 120.51(16) . . ? C3S C2S C1S 121.21(15) . . ? C3S C2S H2S 119.4 . . ? C1S C2S H2S 119.4 . . ? C4S C3S C2S 119.87(17) . . ? C4S C3S H3S 120.1 . . ? C2S C3S H3S 120.1 . . ? C3S C4S C5S 119.84(18) . . ? C3S C4S H4S 120.1 . . ? C5S C4S H4S 120.1 . . ? C4S C5S C6S 120.10(18) . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 121.01(17) . . ? C5S C6S H6S 119.5 . . ? C1S C6S H6S 119.5 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C16S C11S C12S 117.58(16) . . ? C16S C11S C17S 121.1(2) . . ? C12S C11S C17S 121.3(2) . . ? C13S C12S C11S 120.84(17) . . ? C13S C12S H12S 119.6 . . ? C11S C12S H12S 119.6 . . ? C14S C13S C12S 120.68(18) . . ? C14S C13S H13S 119.7 . . ? C12S C13S H13S 119.7 . . ? C13S C14S C15S 119.40(17) . . ? C13S C14S H14S 120.3 . . ? C15S C14S H14S 120.3 . . ? C14S C15S C16S 120.38(16) . . ? C14S C15S H15S 119.8 . . ? C16S C15S H15S 119.8 . . ? C15S C16S C11S 121.11(16) . . ? C15S C16S H16S 119.4 . . ? C11S C16S H16S 119.4 . . ? C11S C17S H17A 109.5 . . ? C11S C17S H17B 109.5 . . ? H17A C17S H17B 109.5 . . ? C11S C17S H17C 109.5 . . ? H17A C17S H17C 109.5 . . ? H17B C17S H17C 109.5 . . ? C22S C21S C26S 118.50(19) . . ? C22S C21S C27S 120.54(19) . . ? C26S C21S C27S 121.0(2) . . ? C21S C22S C23S 120.79(18) . . ? C21S C22S H22S 119.6 . . ? C23S C22S H22S 119.6 . . ? C24S C23S C22S 120.64(19) . . ? C24S C23S H23S 119.7 . . ? C22S C23S H23S 119.7 . . ? C23S C24S C25S 119.0(2) . . ? C23S C24S H24S 120.5 . . ? C25S C24S H24S 120.5 . . ? C26S C25S C24S 120.33(19) . . ? C26S C25S H25S 119.8 . . ? C24S C25S H25S 119.8 . . ? C25S C26S C21S 120.67(18) . . ? C25S C26S H26S 119.7 . . ? C21S C26S H26S 119.7 . . ? C21S C27S H27D 109.5 . . ? C21S C27S H27E 109.5 . . ? H27D C27S H27E 109.5 . . ? C21S C27S H27F 109.5 . . ? H27D C27S H27F 109.5 . . ? H27E C27S H27F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Al1 N1 C2 -102.55(9) . . . . ? O2 Al1 N1 C2 140.70(9) . . . . ? O1 Al1 N1 C2 17.23(8) . . . . ? O4 Al1 N1 C2 25.71(17) . . . . ? Al2 Al1 N1 C2 26.46(9) . . . . ? O3 Al1 N1 C39 18.56(9) . . . . ? O2 Al1 N1 C39 -98.19(9) . . . . ? O1 Al1 N1 C39 138.34(9) . . . . ? O4 Al1 N1 C39 146.82(12) . . . . ? Al2 Al1 N1 C39 147.57(8) . . . . ? O3 Al1 N1 C29 139.72(9) . . . . ? O2 Al1 N1 C29 22.97(9) . . . . ? O1 Al1 N1 C29 -100.51(9) . . . . ? O4 Al1 N1 C29 -92.03(15) . . . . ? Al2 Al1 N1 C29 -91.27(8) . . . . ? O3 Al1 O1 C1 96.93(11) . . . . ? O2 Al1 O1 C1 -83.98(11) . . . . ? O4 Al1 O1 C1 -169.90(11) . . . . ? N1 Al1 O1 C1 6.92(10) . . . . ? Al2 Al1 O1 C1 -160.33(13) . . . . ? O3 Al1 O1 Al2 -102.74(6) . . . . ? O2 Al1 O1 Al2 76.35(6) . . . . ? O4 Al1 O1 Al2 -9.57(5) . . . . ? N1 Al1 O1 Al2 167.25(5) . . . . ? Al1 O1 C1 C2 -28.72(14) . . . . ? Al2 O1 C1 C2 177.48(9) . . . . ? C39 N1 C2 C1 -159.13(11) . . . . ? C29 N1 C2 C1 81.32(13) . . . . ? Al1 N1 C2 C1 -36.12(13) . . . . ? O1 C1 C2 N1 41.22(15) . . . . ? O3 Al1 O2 C21 -71.75(12) . . . . ? O1 Al1 O2 C21 109.13(11) . . . . ? O4 Al1 O2 C21 -174.41(11) . . . . ? N1 Al1 O2 C21 25.01(12) . . . . ? Al2 Al1 O2 C21 149.07(10) . . . . ? Al1 O2 C21 C26 -38.61(18) . . . . ? Al1 O2 C21 C22 142.48(11) . . . . ? O2 C21 C22 C23 -179.89(12) . . . . ? C26 C21 C22 C23 1.2(2) . . . . ? O2 C21 C22 C27 0.7(2) . . . . ? C26 C21 C22 C27 -178.21(13) . . . . ? C21 C22 C23 C24 0.7(2) . . . . ? C27 C22 C23 C24 -179.91(14) . . . . ? C22 C23 C24 C25 -0.8(2) . . . . ? C22 C23 C24 C28 179.97(15) . . . . ? C23 C24 C25 C26 -0.9(2) . . . . ? C28 C24 C25 C26 178.26(14) . . . . ? C24 C25 C26 C21 2.8(2) . . . . ? C24 C25 C26 C29 -174.81(13) . . . . ? O2 C21 C26 C25 178.18(12) . . . . ? C22 C21 C26 C25 -2.9(2) . . . . ? O2 C21 C26 C29 -4.16(19) . . . . ? C22 C21 C26 C29 174.75(12) . . . . ? C2 N1 C29 C26 -175.35(11) . . . . ? C39 N1 C29 C26 64.21(14) . . . . ? Al1 N1 C29 C26 -59.62(12) . . . . ? C25 C26 C29 N1 -126.10(13) . . . . ? C21 C26 C29 N1 56.28(16) . . . . ? O2 Al1 O3 C31 124.99(11) . . . . ? O1 Al1 O3 C31 -55.85(13) . . . . ? O4 Al1 O3 C31 -135.55(11) . . . . ? N1 Al1 O3 C31 27.52(12) . . . . ? Al2 Al1 O3 C31 -101.24(11) . . . . ? Al1 O3 C31 C36 -40.58(19) . . . . ? Al1 O3 C31 C32 140.31(12) . . . . ? O3 C31 C32 C33 176.75(13) . . . . ? C36 C31 C32 C33 -2.4(2) . . . . ? O3 C31 C32 C37 -4.6(2) . . . . ? C36 C31 C32 C37 176.30(14) . . . . ? C31 C32 C33 C34 1.8(2) . . . . ? C37 C32 C33 C34 -176.77(16) . . . . ? C32 C33 C34 C35 0.0(3) . . . . ? C32 C33 C34 C38 178.50(18) . . . . ? C33 C34 C35 C36 -1.3(3) . . . . ? C38 C34 C35 C36 -179.81(17) . . . . ? C34 C35 C36 C31 0.7(2) . . . . ? C34 C35 C36 C39 -175.70(15) . . . . ? O3 C31 C36 C35 -177.95(13) . . . . ? C32 C31 C36 C35 1.1(2) . . . . ? O3 C31 C36 C39 -1.5(2) . . . . ? C32 C31 C36 C39 177.56(13) . . . . ? C2 N1 C39 C36 66.34(14) . . . . ? C29 N1 C39 C36 -173.74(11) . . . . ? Al1 N1 C39 C36 -52.49(13) . . . . ? C35 C36 C39 N1 -134.57(14) . . . . ? C31 C36 C39 N1 49.04(18) . . . . ? C1 O1 Al2 O5 -71.74(12) . . . . ? Al1 O1 Al2 O5 131.06(5) . . . . ? C1 O1 Al2 O6 46.57(12) . . . . ? Al1 O1 Al2 O6 -110.63(5) . . . . ? C1 O1 Al2 O4 166.94(12) . . . . ? Al1 O1 Al2 O4 9.75(5) . . . . ? C1 O1 Al2 N2 159.83(13) . . . . ? Al1 O1 Al2 N2 2.64(16) . . . . ? C1 O1 Al2 Al1 157.20(14) . . . . ? O3 Al1 Al2 O5 41.29(6) . . . . ? O2 Al1 Al2 O5 178.34(5) . . . . ? O1 Al1 Al2 O5 -59.80(6) . . . . ? O4 Al1 Al2 O5 105.09(7) . . . . ? N1 Al1 Al2 O5 -74.46(6) . . . . ? O3 Al1 Al2 O6 177.73(5) . . . . ? O2 Al1 Al2 O6 -45.22(5) . . . . ? O1 Al1 Al2 O6 76.64(6) . . . . ? O4 Al1 Al2 O6 -118.47(6) . . . . ? N1 Al1 Al2 O6 61.97(5) . . . . ? O3 Al1 Al2 O4 -63.80(7) . . . . ? O2 Al1 Al2 O4 73.25(6) . . . . ? O1 Al1 Al2 O4 -164.89(7) . . . . ? N1 Al1 Al2 O4 -179.55(6) . . . . ? O3 Al1 Al2 O1 101.09(7) . . . . ? O2 Al1 Al2 O1 -121.86(6) . . . . ? O4 Al1 Al2 O1 164.89(7) . . . . ? N1 Al1 Al2 O1 -14.67(6) . . . . ? O3 Al1 Al2 N2 -77.81(6) . . . . ? O2 Al1 Al2 N2 59.25(6) . . . . ? O1 Al1 Al2 N2 -178.90(7) . . . . ? O4 Al1 Al2 N2 -14.01(6) . . . . ? N1 Al1 Al2 N2 166.44(5) . . . . ? O5 Al2 N2 C69 91.39(9) . . . . ? O6 Al2 N2 C69 -26.45(9) . . . . ? O4 Al2 N2 C69 -146.98(9) . . . . ? O1 Al2 N2 C69 -140.02(13) . . . . ? Al1 Al2 N2 C69 -138.12(8) . . . . ? O5 Al2 N2 C4 -147.55(8) . . . . ? O6 Al2 N2 C4 94.61(9) . . . . ? O4 Al2 N2 C4 -25.93(8) . . . . ? O1 Al2 N2 C4 -18.96(18) . . . . ? Al1 Al2 N2 C4 -17.06(9) . . . . ? O5 Al2 N2 C59 -29.82(9) . . . . ? O6 Al2 N2 C59 -147.66(9) . . . . ? O4 Al2 N2 C59 91.81(9) . . . . ? O1 Al2 N2 C59 98.78(15) . . . . ? Al1 Al2 N2 C59 100.67(8) . . . . ? O5 Al2 O4 C3 97.96(10) . . . . ? O6 Al2 O4 C3 -84.06(11) . . . . ? O1 Al2 O4 C3 -171.95(10) . . . . ? N2 Al2 O4 C3 5.47(10) . . . . ? Al1 Al2 O4 C3 -162.43(12) . . . . ? O5 Al2 O4 Al1 -99.61(6) . . . . ? O6 Al2 O4 Al1 78.37(6) . . . . ? O1 Al2 O4 Al1 -9.53(5) . . . . ? N2 Al2 O4 Al1 167.90(5) . . . . ? O3 Al1 O4 C3 -72.27(12) . . . . ? O2 Al1 O4 C3 45.19(12) . . . . ? O1 Al1 O4 C3 168.96(12) . . . . ? N1 Al1 O4 C3 160.32(13) . . . . ? Al2 Al1 O4 C3 159.26(14) . . . . ? O3 Al1 O4 Al2 128.47(5) . . . . ? O2 Al1 O4 Al2 -114.08(5) . . . . ? O1 Al1 O4 Al2 9.70(5) . . . . ? N1 Al1 O4 Al2 1.05(15) . . . . ? Al2 O4 C3 C4 16.39(14) . . . . ? Al1 O4 C3 C4 -139.78(10) . . . . ? C69 N2 C4 C3 164.09(11) . . . . ? C59 N2 C4 C3 -75.08(13) . . . . ? Al2 N2 C4 C3 40.87(12) . . . . ? O4 C3 C4 N2 -37.73(14) . . . . ? O6 Al2 O5 C51 80.60(12) . . . . ? O4 Al2 O5 C51 -101.34(12) . . . . ? O1 Al2 O5 C51 -179.88(11) . . . . ? N2 Al2 O5 C51 -16.33(12) . . . . ? Al1 Al2 O5 C51 -147.35(10) . . . . ? Al2 O5 C51 C56 33.70(18) . . . . ? Al2 O5 C51 C52 -146.27(11) . . . . ? O5 C51 C52 C53 -179.95(12) . . . . ? C56 C51 C52 C53 0.1(2) . . . . ? O5 C51 C52 C57 1.77(19) . . . . ? C56 C51 C52 C57 -178.20(13) . . . . ? C51 C52 C53 C54 -1.4(2) . . . . ? C57 C52 C53 C54 176.87(14) . . . . ? C52 C53 C54 C55 1.1(2) . . . . ? C52 C53 C54 C58 -177.28(14) . . . . ? C53 C54 C55 C56 0.4(2) . . . . ? C58 C54 C55 C56 178.81(14) . . . . ? C54 C55 C56 C51 -1.6(2) . . . . ? C54 C55 C56 C59 178.21(13) . . . . ? O5 C51 C56 C55 -178.59(12) . . . . ? C52 C51 C56 C55 1.4(2) . . . . ? O5 C51 C56 C59 1.56(19) . . . . ? C52 C51 C56 C59 -178.47(12) . . . . ? C69 N2 C59 C56 -61.79(14) . . . . ? C4 N2 C59 C56 176.56(11) . . . . ? Al2 N2 C59 C56 62.31(12) . . . . ? C55 C56 C59 N2 126.70(13) . . . . ? C51 C56 C59 N2 -53.45(17) . . . . ? O5 Al2 O6 C61 -112.95(12) . . . . ? O4 Al2 O6 C61 68.97(14) . . . . ? O1 Al2 O6 C61 146.26(12) . . . . ? N2 Al2 O6 C61 -14.42(13) . . . . ? Al1 Al2 O6 C61 109.18(12) . . . . ? Al2 O6 C61 C66 29.4(2) . . . . ? Al2 O6 C61 C62 -151.86(11) . . . . ? O6 C61 C62 C63 -176.04(13) . . . . ? C66 C61 C62 C63 2.8(2) . . . . ? O6 C61 C62 C67 4.3(2) . . . . ? C66 C61 C62 C67 -176.89(13) . . . . ? C61 C62 C63 C64 -1.6(2) . . . . ? C67 C62 C63 C64 177.99(15) . . . . ? C62 C63 C64 C65 -0.7(2) . . . . ? C62 C63 C64 C68 -179.76(15) . . . . ? C63 C64 C65 C66 2.0(2) . . . . ? C68 C64 C65 C66 -178.96(15) . . . . ? C64 C65 C66 C61 -0.8(2) . . . . ? C64 C65 C66 C69 174.76(13) . . . . ? O6 C61 C66 C65 177.18(13) . . . . ? C62 C61 C66 C65 -1.6(2) . . . . ? O6 C61 C66 C69 1.6(2) . . . . ? C62 C61 C66 C69 -177.14(12) . . . . ? C4 N2 C69 C66 -64.05(14) . . . . ? C59 N2 C69 C66 174.37(11) . . . . ? Al2 N2 C69 C66 53.92(13) . . . . ? C65 C66 C69 N2 140.06(13) . . . . ? C61 C66 C69 N2 -44.39(18) . . . . ? C6S C1S C2S C3S 0.6(2) . . . . ? C7S C1S C2S C3S -178.75(15) . . . . ? C1S C2S C3S C4S -0.1(2) . . . . ? C2S C3S C4S C5S -0.2(3) . . . . ? C3S C4S C5S C6S 0.1(3) . . . . ? C4S C5S C6S C1S 0.4(3) . . . . ? C2S C1S C6S C5S -0.7(3) . . . . ? C7S C1S C6S C5S 178.62(17) . . . . ? C16S C11S C12S C13S -0.3(3) . . . . ? C17S C11S C12S C13S 178.76(19) . . . . ? C11S C12S C13S C14S 0.4(3) . . . . ? C12S C13S C14S C15S -0.1(3) . . . . ? C13S C14S C15S C16S -0.2(3) . . . . ? C14S C15S C16S C11S 0.3(2) . . . . ? C12S C11S C16S C15S 0.0(2) . . . . ? C17S C11S C16S C15S -179.12(17) . . . . ? C26S C21S C22S C23S -1.2(3) . . . . ? C27S C21S C22S C23S 179.03(19) . . . . ? C21S C22S C23S C24S 1.1(3) . . . . ? C22S C23S C24S C25S -0.9(3) . . . . ? C23S C24S C25S C26S 1.0(3) . . . . ? C24S C25S C26S C21S -1.2(3) . . . . ? C22S C21S C26S C25S 1.3(3) . . . . ? C27S C21S C26S C25S -178.95(19) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.377 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.080 # Attachment '[Al_L3_H].cif' data_[Al(L3)H] _database_code_depnum_ccdc_archive 'CCDC 729813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Al(L3)H) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48.50 H57 Al N2 O4' _chemical_formula_weight 758.94 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.8680(8) _cell_length_b 12.9740(8) _cell_length_c 19.3130(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.324(4) _cell_angle_gamma 90.00 _cell_volume 4192.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13451 _cell_measurement_theta_min 2.716 _cell_measurement_theta_max 30.508 _exptl_crystal_description Block _exptl_crystal_colour Colourless _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 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; This crystal was weakly diffracting and there was no observable data above the 2theta limit recorded. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa CCD diffractometer' _diffrn_measurement_method 'Omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23956 _diffrn_reflns_av_R_equivalents 0.1227 _diffrn_reflns_av_sigmaI/netI 0.0915 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 8.18 _diffrn_reflns_theta_max 22.49 _reflns_number_total 5176 _reflns_number_gt 3288 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0506P)^2^+4.2334P] 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_number_reflns 5176 _refine_ls_number_parameters 471 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1553 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.74850(7) 0.06338(8) 0.19270(6) 0.0322(3) Uani 1 1 d . . . N1 N 0.83428(19) 0.1395(2) 0.26428(16) 0.0341(8) Uani 1 1 d . . . N2 N 0.71968(19) 0.2103(2) 0.16061(16) 0.0313(8) Uani 1 1 d . . . O1 O 0.69633(15) 0.02577(18) 0.26099(13) 0.0354(7) Uani 1 1 d . . . O2 O 0.82169(16) -0.01129(18) 0.16159(14) 0.0387(7) Uani 1 1 d . . . O3 O 0.67103(16) 0.01961(18) 0.12605(13) 0.0344(7) Uani 1 1 d . . . O4 O 0.73110(18) 0.0366(2) 0.00749(16) 0.0419(7) Uani 1 1 d . . . C1 C 0.8018(2) 0.2451(3) 0.2726(2) 0.0354(10) Uani 1 1 d . . . H1A H 0.8444 0.2904 0.2959 0.042 Uiso 1 1 calc R . . H1B H 0.7579 0.2423 0.3020 0.042 Uiso 1 1 calc R . . C2 C 0.7712(2) 0.2881(3) 0.2018(2) 0.0353(10) Uani 1 1 d . . . H2A H 0.7399 0.3515 0.2072 0.042 Uiso 1 1 calc R . . H2B H 0.8168 0.3063 0.1766 0.042 Uiso 1 1 calc R . . C11 C 0.7026(3) 0.0430(3) 0.3309(2) 0.0346(10) Uani 1 1 d . . . C12 C 0.6347(3) 0.0281(3) 0.3645(2) 0.0378(10) Uani 1 1 d . . . C13 C 0.6420(3) 0.0437(3) 0.4360(2) 0.0458(11) Uani 1 1 d . . . H13 H 0.5964 0.0333 0.4593 0.055 Uiso 1 1 calc R . . C14 C 0.7127(3) 0.0738(3) 0.4749(2) 0.0490(12) Uani 1 1 d . . . C15 C 0.7786(3) 0.0893(3) 0.4400(2) 0.0450(11) Uani 1 1 d . . . H15 H 0.8275 0.1114 0.4656 0.054 Uiso 1 1 calc R . . C16 C 0.7749(3) 0.0734(3) 0.3685(2) 0.0369(10) Uani 1 1 d . . . C17 C 0.5570(3) -0.0012(3) 0.3221(2) 0.0486(11) Uani 1 1 d . . . H17A H 0.5140 0.0010 0.3518 0.073 Uiso 1 1 calc R . . H17B H 0.5612 -0.0711 0.3037 0.073 Uiso 1 1 calc R . . H17C H 0.5451 0.0473 0.2833 0.073 Uiso 1 1 calc R . . C18 C 0.7182(4) 0.0915(5) 0.5531(3) 0.0770(16) Uani 1 1 d . . . H18A H 0.7133 0.1654 0.5623 0.116 Uiso 1 1 calc R . . H18B H 0.7699 0.0665 0.5758 0.116 Uiso 1 1 calc R . . H18C H 0.6750 0.0542 0.5715 0.116 Uiso 1 1 calc R . . C19 C 0.8482(2) 0.0854(3) 0.3327(2) 0.0389(10) Uani 1 1 d . . . H19A H 0.8889 0.1240 0.3638 0.047 Uiso 1 1 calc R . . H19B H 0.8703 0.0161 0.3253 0.047 Uiso 1 1 calc R . . C21 C 0.9001(2) -0.0290(3) 0.1834(2) 0.0345(10) Uani 1 1 d . . . C22 C 0.9341(3) -0.1229(3) 0.1661(2) 0.0377(10) Uani 1 1 d . . . C23 C 1.0135(3) -0.1408(3) 0.1912(2) 0.0443(11) Uani 1 1 d . . . H23 H 1.0364 -0.2046 0.1800 0.053 Uiso 1 1 calc R . . C24 C 1.0618(3) -0.0705(3) 0.2319(2) 0.0434(11) Uani 1 1 d . . . C25 C 1.0265(3) 0.0225(3) 0.2460(2) 0.0417(10) Uani 1 1 d . . . H25 H 1.0577 0.0727 0.2729 0.050 Uiso 1 1 calc R . . C26 C 0.9474(2) 0.0446(3) 0.2221(2) 0.0364(10) Uani 1 1 d . . . C27 C 0.8848(3) -0.1981(3) 0.1202(2) 0.0466(11) Uani 1 1 d . . . H27A H 0.8732 -0.1695 0.0730 0.070 Uiso 1 1 calc R . . H27B H 0.8346 -0.2112 0.1392 0.070 Uiso 1 1 calc R . . H27C H 0.9144 -0.2628 0.1183 0.070 Uiso 1 1 calc R . . C28 C 1.1474(3) -0.0929(4) 0.2582(3) 0.0632(14) Uani 1 1 d . . . H28A H 1.1779 -0.0996 0.2186 0.095 Uiso 1 1 calc R . . H28B H 1.1508 -0.1573 0.2849 0.095 Uiso 1 1 calc R . . H28C H 1.1694 -0.0363 0.2884 0.095 Uiso 1 1 calc R . . C29 C 0.9120(2) 0.1471(3) 0.2351(2) 0.0388(10) Uani 1 1 d . . . H29A H 0.9036 0.1859 0.1906 0.047 Uiso 1 1 calc R . . H29B H 0.9504 0.1864 0.2680 0.047 Uiso 1 1 calc R . . C31 C 0.5938(2) 0.0506(3) 0.12294(19) 0.0322(9) Uani 1 1 d . . . C32 C 0.5327(2) -0.0165(3) 0.09581(19) 0.0354(10) Uani 1 1 d . . . C33 C 0.4538(3) 0.0188(3) 0.0908(2) 0.0426(11) Uani 1 1 d . . . H33 H 0.4123 -0.0263 0.0717 0.051 Uiso 1 1 calc R . . C34 C 0.4333(2) 0.1158(3) 0.1120(2) 0.0430(11) Uani 1 1 d . . . C35 C 0.4947(3) 0.1797(3) 0.1397(2) 0.0390(10) Uani 1 1 d . . . H35 H 0.4821 0.2463 0.1555 0.047 Uiso 1 1 calc R . . C36 C 0.5747(2) 0.1498(3) 0.1455(2) 0.0329(9) Uani 1 1 d . . . C37 C 0.5508(3) -0.1235(3) 0.0735(2) 0.0456(11) Uani 1 1 d . . . H37A H 0.6059 -0.1265 0.0624 0.068 Uiso 1 1 calc R . . H37B H 0.5139 -0.1422 0.0320 0.068 Uiso 1 1 calc R . . H37C H 0.5445 -0.1719 0.1113 0.068 Uiso 1 1 calc R . . C38 C 0.3482(3) 0.1529(4) 0.1020(3) 0.0682(15) Uani 1 1 d . . . H38A H 0.3427 0.2115 0.1330 0.102 Uiso 1 1 calc R . . H38B H 0.3128 0.0970 0.1130 0.102 Uiso 1 1 calc R . . H38C H 0.3337 0.1744 0.0534 0.102 Uiso 1 1 calc R . . C39 C 0.6360(2) 0.2247(3) 0.1786(2) 0.0345(9) Uani 1 1 d . . . H39A H 0.6377 0.2197 0.2299 0.041 Uiso 1 1 calc R . . H39B H 0.6181 0.2953 0.1648 0.041 Uiso 1 1 calc R . . C41 C 0.7941(3) 0.1023(3) 0.0163(2) 0.0373(10) Uani 1 1 d . . . C42 C 0.8608(3) 0.0759(3) -0.0168(2) 0.0403(10) Uani 1 1 d . . . C43 C 0.9250(3) 0.1426(3) -0.0117(2) 0.0478(11) Uani 1 1 d . . . H43 H 0.9706 0.1240 -0.0332 0.057 Uiso 1 1 calc R . . C44 C 0.9256(3) 0.2363(3) 0.0236(2) 0.0504(12) Uani 1 1 d . . . C45 C 0.8578(3) 0.2623(3) 0.0536(2) 0.0450(11) Uani 1 1 d . . . H45 H 0.8559 0.3275 0.0757 0.054 Uiso 1 1 calc R . . C46 C 0.7925(2) 0.1969(3) 0.0525(2) 0.0370(10) Uani 1 1 d . . . C47 C 0.8599(3) -0.0216(3) -0.0584(2) 0.0525(12) Uani 1 1 d . . . H47A H 0.9120 -0.0312 -0.0748 0.079 Uiso 1 1 calc R . . H47B H 0.8182 -0.0173 -0.0986 0.079 Uiso 1 1 calc R . . H47C H 0.8489 -0.0801 -0.0290 0.079 Uiso 1 1 calc R . . C48 C 0.9966(4) 0.3077(4) 0.0269(3) 0.0798(18) Uani 1 1 d . . . H48A H 0.9959 0.3554 0.0662 0.120 Uiso 1 1 calc R . . H48B H 0.9940 0.3468 -0.0167 0.120 Uiso 1 1 calc R . . H48C H 1.0460 0.2671 0.0335 0.120 Uiso 1 1 calc R . . C49 C 0.7186(2) 0.2309(3) 0.08311(19) 0.0348(10) Uani 1 1 d . . . H49A H 0.6717 0.1955 0.0576 0.042 Uiso 1 1 calc R . . H49B H 0.7112 0.3058 0.0749 0.042 Uiso 1 1 calc R . . C1S C 0.2550(2) 0.1780(3) 0.2968(2) 0.0812(18) Uani 1 1 d G A 1 C2S C 0.2484(2) 0.2354(3) 0.3566(2) 0.094(2) Uani 1 1 d G A 1 H2S H 0.2850 0.2244 0.3975 0.112 Uiso 1 1 calc R A 1 C3S C 0.1883(3) 0.3087(3) 0.35640(18) 0.0830(17) Uani 1 1 d G A 1 H3S H 0.1839 0.3480 0.3973 0.100 Uiso 1 1 calc R A 1 C4S C 0.1348(2) 0.3247(3) 0.2965(2) 0.0786(17) Uani 1 1 d G A 1 H4S H 0.0938 0.3749 0.2963 0.094 Uiso 1 1 calc R A 1 C5S C 0.1414(2) 0.2674(3) 0.23666(18) 0.0882(19) Uani 1 1 d G A 1 H5S H 0.1048 0.2783 0.1957 0.106 Uiso 1 1 calc R A 1 C6S C 0.2015(3) 0.1940(3) 0.2368(2) 0.0721(16) Uani 1 1 d G A 1 H6S H 0.2059 0.1548 0.1960 0.086 Uiso 1 1 calc R A 1 C7S C 0.3253(4) 0.1044(5) 0.2974(4) 0.104(2) Uani 1 1 d . A 1 H7S1 H 0.3675 0.1371 0.2746 0.156 Uiso 1 1 calc R A 1 H7S2 H 0.3076 0.0411 0.2723 0.156 Uiso 1 1 calc R A 1 H7S3 H 0.3462 0.0874 0.3458 0.156 Uiso 1 1 calc R A 1 C11S C 1.0386(4) 0.0510(4) 0.4730(3) 0.0555(10) Uiso 0.50 1 d PGD B -1 C12S C 1.0090(4) 0.0896(4) 0.5317(3) 0.0555(10) Uiso 0.50 1 d PGD B -1 H12S H 1.0213 0.1581 0.5468 0.067 Uiso 0.50 1 calc PR B -1 C13S C 0.9613(4) 0.0281(5) 0.5684(3) 0.0555(10) Uiso 0.50 1 d PG B -1 H13S H 0.9411 0.0545 0.6086 0.067 Uiso 0.50 1 calc PR B -1 C14S C 0.9432(4) -0.0722(4) 0.5463(3) 0.0555(10) Uiso 0.50 1 d PG B -1 H14S H 0.9106 -0.1143 0.5714 0.067 Uiso 0.50 1 calc PR B -1 C15S C 0.9728(4) -0.1108(4) 0.4876(3) 0.0555(10) Uiso 0.50 1 d PG B -1 H15S H 0.9605 -0.1793 0.4725 0.067 Uiso 0.50 1 calc PR B -1 C16S C 1.0205(4) -0.0492(4) 0.4509(3) 0.0555(10) Uiso 0.50 1 d PGD B -1 H16S H 1.0408 -0.0756 0.4108 0.067 Uiso 0.50 1 calc PR B -1 C17S C 1.0931(6) 0.1162(7) 0.4341(5) 0.0555(10) Uiso 0.50 1 d PD B -1 H17D H 1.0660 0.1807 0.4190 0.083 Uiso 0.50 1 calc PR B -1 H17E H 1.1062 0.0783 0.3931 0.083 Uiso 0.50 1 calc PR B -1 H17F H 1.1424 0.1316 0.4650 0.083 Uiso 0.50 1 calc PR B -1 H4O H 0.707(3) 0.029(3) 0.051(3) 0.053(13) 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 0.0355(7) 0.0263(6) 0.0341(7) -0.0015(5) 0.0014(5) 0.0003(5) N1 0.036(2) 0.0311(17) 0.035(2) -0.0016(14) 0.0033(16) 0.0028(14) N2 0.034(2) 0.0301(17) 0.0292(18) -0.0013(13) 0.0024(15) -0.0019(14) O1 0.0401(17) 0.0317(14) 0.0334(17) 0.0005(11) 0.0010(13) -0.0014(11) O2 0.0380(18) 0.0346(14) 0.0423(17) -0.0084(12) 0.0007(13) 0.0009(12) O3 0.0360(17) 0.0306(14) 0.0360(16) -0.0027(11) 0.0022(13) -0.0003(12) O4 0.0472(19) 0.0437(17) 0.0351(17) -0.0081(13) 0.0065(15) -0.0124(14) C1 0.036(2) 0.027(2) 0.043(3) -0.0098(17) 0.004(2) 0.0010(17) C2 0.042(3) 0.024(2) 0.039(2) -0.0054(17) 0.001(2) -0.0034(17) C11 0.047(3) 0.027(2) 0.029(2) -0.0003(16) 0.004(2) 0.0066(18) C12 0.045(3) 0.030(2) 0.040(3) 0.0065(18) 0.009(2) 0.0064(18) C13 0.059(3) 0.038(2) 0.043(3) 0.0061(19) 0.018(3) 0.006(2) C14 0.064(3) 0.048(3) 0.035(3) 0.001(2) 0.007(3) 0.007(2) C15 0.048(3) 0.046(3) 0.040(3) -0.0022(19) -0.001(2) 0.004(2) C16 0.045(3) 0.031(2) 0.034(3) 0.0008(17) 0.005(2) 0.0075(18) C17 0.044(3) 0.051(3) 0.052(3) 0.010(2) 0.012(2) 0.001(2) C18 0.090(4) 0.102(4) 0.040(3) -0.005(3) 0.012(3) -0.004(3) C19 0.038(2) 0.041(2) 0.035(2) -0.0038(18) -0.006(2) 0.0018(18) C21 0.035(3) 0.035(2) 0.034(2) 0.0039(18) 0.006(2) 0.0054(18) C22 0.048(3) 0.032(2) 0.036(2) 0.0024(17) 0.015(2) 0.0019(19) C23 0.050(3) 0.038(2) 0.049(3) 0.009(2) 0.020(2) 0.015(2) C24 0.037(3) 0.049(3) 0.045(3) 0.005(2) 0.009(2) 0.004(2) C25 0.039(3) 0.046(2) 0.040(3) -0.0005(19) 0.006(2) 0.001(2) C26 0.034(3) 0.040(2) 0.035(2) -0.0010(18) 0.004(2) 0.0025(19) C27 0.056(3) 0.035(2) 0.052(3) -0.007(2) 0.018(2) 0.002(2) C28 0.047(3) 0.069(3) 0.073(4) 0.006(3) 0.008(3) 0.018(2) C29 0.036(2) 0.035(2) 0.044(3) -0.0063(18) 0.001(2) -0.0002(18) C31 0.031(2) 0.041(2) 0.024(2) 0.0042(17) 0.0005(18) 0.0016(18) C32 0.037(3) 0.041(2) 0.028(2) 0.0014(17) 0.0001(19) -0.0070(19) C33 0.042(3) 0.048(3) 0.038(3) -0.001(2) 0.004(2) -0.012(2) C34 0.031(2) 0.057(3) 0.042(3) -0.007(2) 0.007(2) -0.004(2) C35 0.040(3) 0.045(2) 0.033(2) -0.0009(18) 0.008(2) 0.001(2) C36 0.034(2) 0.035(2) 0.029(2) 0.0012(17) 0.0028(18) -0.0018(18) C37 0.054(3) 0.036(2) 0.043(3) -0.0018(19) -0.004(2) -0.009(2) C38 0.044(3) 0.084(4) 0.077(4) -0.025(3) 0.009(3) -0.001(3) C39 0.034(2) 0.031(2) 0.038(2) 0.0002(17) 0.0050(19) 0.0036(17) C41 0.042(3) 0.038(2) 0.031(2) -0.0003(18) 0.001(2) -0.002(2) C42 0.046(3) 0.041(2) 0.035(2) -0.0026(18) 0.005(2) -0.001(2) C43 0.046(3) 0.056(3) 0.045(3) -0.008(2) 0.017(2) -0.006(2) C44 0.051(3) 0.050(3) 0.052(3) -0.011(2) 0.016(2) -0.015(2) C45 0.054(3) 0.037(2) 0.045(3) -0.0074(19) 0.010(2) -0.008(2) C46 0.036(3) 0.037(2) 0.037(2) -0.0020(18) 0.003(2) -0.0038(18) C47 0.059(3) 0.048(3) 0.052(3) -0.009(2) 0.014(2) -0.001(2) C48 0.071(4) 0.079(4) 0.098(4) -0.038(3) 0.043(3) -0.032(3) C49 0.042(3) 0.031(2) 0.031(2) 0.0007(17) 0.0011(19) 0.0003(18) C1S 0.084(5) 0.061(3) 0.105(5) -0.001(3) 0.036(4) -0.020(3) C2S 0.102(5) 0.099(5) 0.085(5) -0.013(4) 0.032(4) -0.012(4) C3S 0.084(4) 0.094(4) 0.070(4) -0.016(3) 0.008(4) 0.018(3) C4S 0.088(5) 0.069(3) 0.084(4) -0.024(3) 0.031(4) -0.013(3) C5S 0.080(5) 0.109(5) 0.079(4) -0.010(4) 0.019(4) -0.034(4) C6S 0.069(4) 0.080(4) 0.072(4) -0.033(3) 0.028(3) -0.025(3) C7S 0.098(5) 0.081(4) 0.139(6) 0.006(4) 0.037(5) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O2 1.736(3) . ? Al1 O1 1.746(3) . ? Al1 O3 1.805(3) . ? Al1 N2 2.044(3) . ? Al1 N1 2.114(3) . ? N1 C19 1.487(5) . ? N1 C1 1.492(5) . ? N1 C29 1.496(5) . ? N2 C2 1.493(5) . ? N2 C39 1.508(5) . ? N2 C49 1.518(5) . ? O1 C11 1.360(4) . ? O2 C21 1.355(5) . ? O3 C31 1.357(4) . ? O4 C41 1.355(5) . ? O4 H4O 0.98(5) . ? C1 C2 1.506(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C11 C16 1.395(6) . ? C11 C12 1.398(6) . ? C12 C13 1.386(6) . ? C12 C17 1.503(6) . ? C13 C14 1.382(7) . ? C13 H13 0.9500 . ? C14 C15 1.387(6) . ? C14 C18 1.517(7) . ? C15 C16 1.390(6) . ? C15 H15 0.9500 . ? C16 C19 1.500(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 C26 1.400(6) . ? C21 C22 1.405(5) . ? C22 C23 1.384(6) . ? C22 C27 1.497(6) . ? C23 C24 1.397(6) . ? C23 H23 0.9500 . ? C24 C25 1.387(6) . ? C24 C28 1.496(7) . ? C25 C26 1.384(6) . ? C25 H25 0.9500 . ? C26 C29 1.491(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C32 1.399(5) . ? C31 C36 1.409(5) . ? C32 C33 1.398(6) . ? C32 C37 1.498(6) . ? C33 C34 1.382(6) . ? C33 H33 0.9500 . ? C34 C35 1.381(6) . ? C34 C38 1.502(7) . ? C35 C36 1.394(6) . ? C35 H35 0.9500 . ? C36 C39 1.502(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C41 C42 1.405(6) . ? C41 C46 1.415(5) . ? C42 C43 1.380(6) . ? C42 C47 1.498(6) . ? C43 C44 1.393(6) . ? C43 H43 0.9500 . ? C44 C45 1.388(6) . ? C44 C48 1.509(7) . ? C45 C46 1.387(6) . ? C45 H45 0.9500 . ? C46 C49 1.513(6) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C1S C7S 1.523(7) . ? C2S C3S 1.3900 . ? C2S H2S 0.9500 . ? C3S C4S 1.3900 . ? C3S H3S 0.9500 . ? C4S C5S 1.3900 . ? C4S H4S 0.9500 . ? C5S C6S 1.3900 . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C11S C12S 1.3900 . ? C11S C16S 1.3900 . ? C11S C17S 1.517(8) . ? C12S C13S 1.3900 . ? C12S H12S 0.9500 . ? C13S C14S 1.3900 . ? C13S H13S 0.9500 . ? C14S C15S 1.3900 . ? C14S H14S 0.9500 . ? C15S C16S 1.3900 . ? C15S H15S 0.9500 . ? C16S H16S 0.9500 . ? C17S H17D 0.9800 . ? C17S H17E 0.9800 . ? C17S H17F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al1 O1 123.69(13) . . ? O2 Al1 O3 93.43(13) . . ? O1 Al1 O3 93.56(13) . . ? O2 Al1 N2 124.59(13) . . ? O1 Al1 N2 111.50(12) . . ? O3 Al1 N2 87.40(12) . . ? O2 Al1 N1 91.67(13) . . ? O1 Al1 N1 90.31(13) . . ? O3 Al1 N1 170.46(13) . . ? N2 Al1 N1 83.07(13) . . ? C19 N1 C1 110.9(3) . . ? C19 N1 C29 108.6(3) . . ? C1 N1 C29 109.3(3) . . ? C19 N1 Al1 112.2(2) . . ? C1 N1 Al1 105.6(2) . . ? C29 N1 Al1 110.1(2) . . ? C2 N2 C39 107.0(3) . . ? C2 N2 C49 109.8(3) . . ? C39 N2 C49 108.1(3) . . ? C2 N2 Al1 111.7(2) . . ? C39 N2 Al1 103.8(2) . . ? C49 N2 Al1 115.9(2) . . ? C11 O1 Al1 136.2(2) . . ? C21 O2 Al1 134.1(2) . . ? C31 O3 Al1 122.8(2) . . ? C41 O4 H4O 111(3) . . ? N1 C1 C2 109.3(3) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N2 C2 C1 110.0(3) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? O1 C11 C16 121.0(3) . . ? O1 C11 C12 118.3(4) . . ? C16 C11 C12 120.7(4) . . ? C13 C12 C11 117.9(4) . . ? C13 C12 C17 122.7(4) . . ? C11 C12 C17 119.4(4) . . ? C14 C13 C12 123.0(4) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? C13 C14 C15 117.8(4) . . ? C13 C14 C18 121.5(4) . . ? C15 C14 C18 120.7(5) . . ? C14 C15 C16 121.6(4) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C15 C16 C11 119.0(4) . . ? C15 C16 C19 120.5(4) . . ? C11 C16 C19 120.4(4) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C16 114.4(3) . . ? N1 C19 H19A 108.7 . . ? C16 C19 H19A 108.7 . . ? N1 C19 H19B 108.7 . . ? C16 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? O2 C21 C26 121.2(3) . . ? O2 C21 C22 119.1(4) . . ? C26 C21 C22 119.8(4) . . ? C23 C22 C21 118.0(4) . . ? C23 C22 C27 122.5(4) . . ? C21 C22 C27 119.5(4) . . ? C22 C23 C24 123.8(4) . . ? C22 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C25 C24 C23 116.4(4) . . ? C25 C24 C28 121.4(4) . . ? C23 C24 C28 122.2(4) . . ? C26 C25 C24 122.3(4) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C21 119.7(4) . . ? C25 C26 C29 121.2(4) . . ? C21 C26 C29 119.0(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 N1 113.2(3) . . ? C26 C29 H29A 108.9 . . ? N1 C29 H29A 108.9 . . ? C26 C29 H29B 108.9 . . ? N1 C29 H29B 108.9 . . ? H29A C29 H29B 107.8 . . ? O3 C31 C32 119.3(3) . . ? O3 C31 C36 120.9(3) . . ? C32 C31 C36 119.8(4) . . ? C33 C32 C31 118.1(4) . . ? C33 C32 C37 120.7(4) . . ? C31 C32 C37 121.2(4) . . ? C34 C33 C32 123.4(4) . . ? C34 C33 H33 118.3 . . ? C32 C33 H33 118.3 . . ? C35 C34 C33 117.2(4) . . ? C35 C34 C38 121.0(4) . . ? C33 C34 C38 121.7(4) . . ? C34 C35 C36 122.4(4) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 119.1(4) . . ? C35 C36 C39 117.4(3) . . ? C31 C36 C39 123.4(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 N2 115.8(3) . . ? C36 C39 H39A 108.3 . . ? N2 C39 H39A 108.3 . . ? C36 C39 H39B 108.3 . . ? N2 C39 H39B 108.3 . . ? H39A C39 H39B 107.4 . . ? O4 C41 C42 116.8(3) . . ? O4 C41 C46 123.0(4) . . ? C42 C41 C46 120.1(4) . . ? C43 C42 C41 118.8(4) . . ? C43 C42 C47 121.4(4) . . ? C41 C42 C47 119.7(4) . . ? C42 C43 C44 122.5(4) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 117.5(4) . . ? C45 C44 C48 121.7(4) . . ? C43 C44 C48 120.8(4) . . ? C46 C45 C44 122.6(4) . . ? C46 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 C46 C41 118.3(4) . . ? C45 C46 C49 120.5(3) . . ? C41 C46 C49 121.0(3) . . ? C42 C47 H47A 109.5 . . ? C42 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C42 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 N2 115.3(3) . . ? C46 C49 H49A 108.5 . . ? N2 C49 H49A 108.5 . . ? C46 C49 H49B 108.5 . . ? N2 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C2S C1S C6S 120.0 . . ? C2S C1S C7S 118.3(4) . . ? C6S C1S C7S 121.5(4) . . ? C1S C2S C3S 120.0 . . ? C1S C2S H2S 120.0 . . ? C3S C2S H2S 120.0 . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3S 120.0 . . ? C2S C3S H3S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C12S C11S C16S 120.0 . . ? C12S C11S C17S 120.5(5) . . ? C16S C11S C17S 119.5(5) . . ? C13S C12S C11S 120.0 . . ? C13S C12S H12S 120.0 . . ? C11S C12S H12S 120.0 . . ? C12S C13S C14S 120.0 . . ? C12S C13S H13S 120.0 . . ? C14S C13S H13S 120.0 . . ? C15S C14S C13S 120.0 . . ? C15S C14S H14S 120.0 . . ? C13S C14S H14S 120.0 . . ? C16S C15S C14S 120.0 . . ? C16S C15S H15S 120.0 . . ? C14S C15S H15S 120.0 . . ? C15S C16S C11S 120.0 . . ? C15S C16S H16S 120.0 . . ? C11S C16S H16S 120.0 . . ? C11S C17S H17D 109.5 . . ? C11S C17S H17E 109.5 . . ? H17D C17S H17E 109.5 . . ? C11S C17S H17F 109.5 . . ? H17D C17S H17F 109.5 . . ? H17E C17S H17F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4O O3 0.98(5) 1.65(5) 2.629(4) 176(4) . _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.318 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.043 # Attachment '[HMPAAl_L2_].cif' data_[HMPAAl(L2)] _database_code_depnum_ccdc_archive 'CCDC 729814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (HMPAAl(L2)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 Al N4 O4 P' _chemical_formula_weight 532.59 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' Al Al 0.0645 0.0514 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1050(2) _cell_length_b 15.5160(2) _cell_length_c 14.3840(2) _cell_angle_alpha 90.000 _cell_angle_beta 99.828(1) _cell_angle_gamma 90.000 _cell_volume 2881.88(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30684 _cell_measurement_theta_min 2.716 _cell_measurement_theta_max 30.508 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa CCD diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 47730 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 8.54 _diffrn_reflns_theta_max 30.57 _reflns_number_total 8019 _reflns_number_gt 5969 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0571P)^2^+1.1634P] 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 8019 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.24197(3) 0.11270(3) 0.06958(3) 0.02276(11) Uani 1 1 d . . . N1 N 0.12521(9) 0.17094(7) -0.03893(8) 0.0227(2) Uani 1 1 d . . . O1 O 0.21257(10) 0.01941(7) 0.00155(8) 0.0351(3) Uani 1 1 d . . . O2 O 0.16972(8) 0.14527(7) 0.15689(7) 0.0284(2) Uani 1 1 d . . . O3 O 0.33501(8) 0.18759(7) 0.04329(8) 0.0291(2) Uani 1 1 d . . . O4 O 0.34140(9) 0.05871(7) 0.15598(8) 0.0320(2) Uani 1 1 d . . . P1 P 0.39361(3) -0.02068(2) 0.19905(3) 0.02507(10) Uani 1 1 d . . . N1P N 0.49503(11) -0.03972(9) 0.15080(11) 0.0365(3) Uani 1 1 d . . . N2P N 0.42246(14) 0.00017(10) 0.31188(10) 0.0435(4) Uani 1 1 d . . . N3P N 0.33085(12) -0.11123(9) 0.18893(13) 0.0459(4) Uani 1 1 d . . . C1 C 0.13963(13) 0.02039(10) -0.08188(11) 0.0328(3) Uani 1 1 d . . . H1A H 0.1011 -0.0348 -0.0888 0.039 Uiso 1 1 calc R . . H1B H 0.1753 0.0272 -0.1368 0.039 Uiso 1 1 calc R . . C2 C 0.06469(12) 0.09485(10) -0.07862(11) 0.0289(3) Uani 1 1 d . . . H2A H 0.0275 0.1079 -0.1429 0.035 Uiso 1 1 calc R . . H2B H 0.0130 0.0794 -0.0386 0.035 Uiso 1 1 calc R . . C21 C 0.07004(11) 0.16614(9) 0.15513(10) 0.0248(3) Uani 1 1 d . . . C22 C 0.02371(12) 0.14677(9) 0.23422(11) 0.0289(3) Uani 1 1 d . . . C23 C -0.07913(12) 0.16944(10) 0.23376(11) 0.0305(3) Uani 1 1 d . . . H23 H -0.1094 0.1568 0.2877 0.037 Uiso 1 1 calc R . . C24 C -0.13931(11) 0.20998(9) 0.15695(11) 0.0279(3) Uani 1 1 d . . . C25 C -0.09269(11) 0.22853(9) 0.07986(11) 0.0262(3) Uani 1 1 d . . . H25 H -0.1321 0.2563 0.0267 0.031 Uiso 1 1 calc R . . C26 C 0.01045(11) 0.20765(8) 0.07781(10) 0.0241(3) Uani 1 1 d . . . C27 C 0.08592(16) 0.10146(13) 0.31750(12) 0.0425(4) Uani 1 1 d . . . H27A H 0.0452 0.0979 0.3686 0.064 Uiso 1 1 calc R . . H27B H 0.1498 0.1338 0.3393 0.064 Uiso 1 1 calc R . . H27C H 0.1033 0.0432 0.2989 0.064 Uiso 1 1 calc R . . C28 C -0.25123(13) 0.23286(12) 0.15660(13) 0.0375(4) Uani 1 1 d . . . H28A H -0.2819 0.2551 0.0943 0.056 Uiso 1 1 calc R . . H28B H -0.2554 0.2770 0.2045 0.056 Uiso 1 1 calc R . . H28C H -0.2891 0.1813 0.1707 0.056 Uiso 1 1 calc R . . C29 C 0.05872(11) 0.23646(9) -0.00427(11) 0.0265(3) Uani 1 1 d . . . H29A H 0.0029 0.2528 -0.0567 0.032 Uiso 1 1 calc R . . H29B H 0.1008 0.2886 0.0144 0.032 Uiso 1 1 calc R . . C31 C 0.32327(11) 0.26696(9) 0.00644(10) 0.0252(3) Uani 1 1 d . . . C32 C 0.38987(12) 0.33312(10) 0.04678(11) 0.0310(3) Uani 1 1 d . . . C33 C 0.37702(13) 0.41525(10) 0.00821(13) 0.0356(4) Uani 1 1 d . . . H33 H 0.4226 0.4597 0.0348 0.043 Uiso 1 1 calc R . . C34 C 0.29983(14) 0.43491(10) -0.06798(13) 0.0364(4) Uani 1 1 d . . . C35 C 0.23406(12) 0.36886(10) -0.10625(11) 0.0304(3) Uani 1 1 d . . . H35 H 0.1799 0.3811 -0.1574 0.037 Uiso 1 1 calc R . . C36 C 0.24602(11) 0.28499(9) -0.07114(10) 0.0248(3) Uani 1 1 d . . . C37 C 0.47188(14) 0.31261(14) 0.13085(14) 0.0444(4) Uani 1 1 d . . . H37A H 0.5062 0.3660 0.1556 0.067 Uiso 1 1 calc R . . H37B H 0.5231 0.2734 0.1116 0.067 Uiso 1 1 calc R . . H37C H 0.4396 0.2851 0.1799 0.067 Uiso 1 1 calc R . . C38 C 0.28971(18) 0.52493(12) -0.10831(19) 0.0567(6) Uani 1 1 d . . . H38A H 0.3220 0.5661 -0.0604 0.085 Uiso 1 1 calc R . . H38B H 0.2162 0.5392 -0.1272 0.085 Uiso 1 1 calc R . . H38C H 0.3243 0.5280 -0.1635 0.085 Uiso 1 1 calc R . . C39 C 0.17712(11) 0.21217(9) -0.11213(10) 0.0257(3) Uani 1 1 d . . . H39A H 0.1240 0.2343 -0.1638 0.031 Uiso 1 1 calc R . . H39B H 0.2189 0.1685 -0.1390 0.031 Uiso 1 1 calc R . . C41 C 0.3864(2) 0.07291(15) 0.35741(15) 0.0626(6) Uani 1 1 d . . . H41A H 0.3425 0.0534 0.4020 0.094 Uiso 1 1 calc R . . H41B H 0.3461 0.1105 0.3100 0.094 Uiso 1 1 calc R . . H41C H 0.4457 0.1049 0.3915 0.094 Uiso 1 1 calc R . . C42 C 0.4857(3) -0.05933(18) 0.37716(16) 0.0731(8) Uani 1 1 d . . . H42A H 0.5458 -0.0285 0.4115 0.110 Uiso 1 1 calc R . . H42B H 0.5093 -0.1070 0.3414 0.110 Uiso 1 1 calc R . . H42C H 0.4441 -0.0822 0.4221 0.110 Uiso 1 1 calc R . . C43 C 0.55355(15) 0.03260(14) 0.12112(14) 0.0463(4) Uani 1 1 d . . . H43A H 0.6099 0.0481 0.1724 0.069 Uiso 1 1 calc R . . H43B H 0.5074 0.0822 0.1058 0.069 Uiso 1 1 calc R . . H43C H 0.5826 0.0160 0.0653 0.069 Uiso 1 1 calc R . . C44 C 0.55524(19) -0.11966(15) 0.16446(18) 0.0580(6) Uani 1 1 d . . . H44A H 0.5757 -0.1367 0.1047 0.087 Uiso 1 1 calc R . . H44B H 0.5130 -0.1653 0.1858 0.087 Uiso 1 1 calc R . . H44C H 0.6173 -0.1104 0.2121 0.087 Uiso 1 1 calc R . . C45 C 0.3094(3) -0.15505(13) 0.0971(2) 0.0810(10) Uani 1 1 d . . . H45A H 0.3119 -0.2176 0.1069 0.121 Uiso 1 1 calc R . . H45B H 0.3615 -0.1383 0.0592 0.121 Uiso 1 1 calc R . . H45C H 0.2405 -0.1386 0.0642 0.121 Uiso 1 1 calc R . . C46 C 0.2573(2) -0.13036(18) 0.2544(3) 0.0856(10) Uani 1 1 d . . . H46A H 0.1865 -0.1180 0.2229 0.128 Uiso 1 1 calc R . . H46B H 0.2741 -0.0944 0.3109 0.128 Uiso 1 1 calc R . . H46C H 0.2629 -0.1913 0.2725 0.128 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 0.0253(2) 0.01990(19) 0.0230(2) 0.00150(15) 0.00405(15) 0.00277(15) N1 0.0241(5) 0.0222(5) 0.0226(6) 0.0014(4) 0.0063(4) -0.0012(4) O1 0.0464(7) 0.0231(5) 0.0327(6) -0.0029(4) -0.0023(5) 0.0055(4) O2 0.0268(5) 0.0352(5) 0.0238(5) 0.0019(4) 0.0057(4) 0.0043(4) O3 0.0238(5) 0.0293(5) 0.0341(6) 0.0075(4) 0.0045(4) 0.0023(4) O4 0.0353(6) 0.0275(5) 0.0312(6) 0.0043(4) 0.0001(4) 0.0075(4) P1 0.02617(19) 0.02083(17) 0.02728(19) 0.00291(13) 0.00194(14) 0.00220(13) N1P 0.0348(7) 0.0341(7) 0.0419(8) 0.0040(6) 0.0106(6) 0.0085(6) N2P 0.0649(10) 0.0381(7) 0.0271(7) 0.0074(6) 0.0066(6) 0.0167(7) N3P 0.0389(8) 0.0262(7) 0.0695(11) 0.0020(7) -0.0001(7) -0.0053(6) C1 0.0409(8) 0.0277(7) 0.0290(7) -0.0047(6) 0.0036(6) -0.0036(6) C2 0.0301(7) 0.0300(7) 0.0258(7) -0.0007(5) 0.0027(5) -0.0058(6) C21 0.0265(7) 0.0219(6) 0.0267(7) -0.0023(5) 0.0068(5) -0.0005(5) C22 0.0367(8) 0.0255(7) 0.0261(7) -0.0009(5) 0.0102(6) -0.0011(6) C23 0.0368(8) 0.0279(7) 0.0309(8) -0.0035(6) 0.0172(6) -0.0039(6) C24 0.0286(7) 0.0229(6) 0.0346(8) -0.0068(5) 0.0122(6) -0.0035(5) C25 0.0256(7) 0.0225(6) 0.0313(7) -0.0009(5) 0.0067(5) -0.0015(5) C26 0.0261(7) 0.0199(6) 0.0278(7) -0.0004(5) 0.0089(5) -0.0017(5) C27 0.0526(10) 0.0492(10) 0.0283(8) 0.0087(7) 0.0140(7) 0.0090(8) C28 0.0315(8) 0.0402(9) 0.0446(9) -0.0029(7) 0.0172(7) -0.0003(7) C29 0.0261(7) 0.0249(6) 0.0300(7) 0.0058(5) 0.0089(5) 0.0039(5) C31 0.0239(6) 0.0258(6) 0.0282(7) 0.0014(5) 0.0108(5) -0.0005(5) C32 0.0263(7) 0.0354(8) 0.0329(8) -0.0033(6) 0.0100(6) -0.0031(6) C33 0.0352(8) 0.0306(7) 0.0447(9) -0.0070(6) 0.0171(7) -0.0091(6) C34 0.0409(9) 0.0257(7) 0.0472(10) 0.0043(6) 0.0208(7) -0.0005(6) C35 0.0314(7) 0.0293(7) 0.0331(8) 0.0082(6) 0.0124(6) 0.0022(6) C36 0.0254(7) 0.0256(6) 0.0255(7) 0.0020(5) 0.0107(5) 0.0001(5) C37 0.0332(8) 0.0542(11) 0.0434(10) -0.0040(8) 0.0000(7) -0.0100(8) C38 0.0591(13) 0.0297(9) 0.0838(16) 0.0146(9) 0.0196(11) -0.0038(8) C39 0.0271(7) 0.0292(7) 0.0218(6) 0.0029(5) 0.0065(5) -0.0006(5) C41 0.0961(18) 0.0490(11) 0.0362(10) -0.0093(8) -0.0073(11) 0.0214(12) C42 0.109(2) 0.0736(16) 0.0339(10) 0.0158(10) 0.0039(11) 0.0426(15) C43 0.0385(9) 0.0577(11) 0.0447(10) 0.0066(8) 0.0130(8) -0.0044(8) C44 0.0564(12) 0.0532(12) 0.0673(14) 0.0049(10) 0.0190(10) 0.0287(10) C45 0.105(2) 0.0283(9) 0.0876(18) -0.0062(10) -0.0475(16) -0.0074(11) C46 0.0533(14) 0.0528(13) 0.158(3) 0.0218(16) 0.0399(17) -0.0121(11) _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 1.7529(11) . ? Al1 O2 1.7706(11) . ? Al1 O3 1.7714(11) . ? Al1 O4 1.8415(11) . ? Al1 N1 2.1860(12) . ? N1 C29 1.4798(18) . ? N1 C2 1.4813(18) . ? N1 C39 1.4916(17) . ? O1 C1 1.4009(19) . ? O2 C21 1.3418(17) . ? O3 C31 1.3391(17) . ? O4 P1 1.4915(11) . ? P1 N3P 1.6220(15) . ? P1 N1P 1.6279(15) . ? P1 N2P 1.6347(15) . ? N1P C43 1.463(2) . ? N1P C44 1.465(2) . ? N2P C41 1.425(3) . ? N2P C42 1.468(2) . ? N3P C45 1.469(3) . ? N3P C46 1.488(3) . ? C1 C2 1.522(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C21 C26 1.402(2) . ? C21 C22 1.410(2) . ? C22 C23 1.392(2) . ? C22 C27 1.504(2) . ? C23 C24 1.393(2) . ? C23 H23 0.9500 . ? C24 C25 1.385(2) . ? C24 C28 1.508(2) . ? C25 C26 1.395(2) . ? C25 H25 0.9500 . ? C26 C29 1.4996(19) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C36 1.401(2) . ? C31 C32 1.407(2) . ? C32 C33 1.389(2) . ? C32 C37 1.508(2) . ? C33 C34 1.392(3) . ? C33 H33 0.9500 . ? C34 C35 1.391(2) . ? C34 C38 1.510(2) . ? C35 C36 1.395(2) . ? C35 H35 0.9500 . ? C36 C39 1.503(2) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 122.58(6) . . ? O1 Al1 O3 121.08(6) . . ? O2 Al1 O3 115.79(5) . . ? O1 Al1 O4 93.66(5) . . ? O2 Al1 O4 93.08(5) . . ? O3 Al1 O4 90.51(5) . . ? O1 Al1 N1 83.25(5) . . ? O2 Al1 N1 89.69(5) . . ? O3 Al1 N1 89.99(5) . . ? O4 Al1 N1 176.65(5) . . ? C29 N1 C2 111.72(11) . . ? C29 N1 C39 107.99(11) . . ? C2 N1 C39 110.39(11) . . ? C29 N1 Al1 115.09(9) . . ? C2 N1 Al1 102.07(8) . . ? C39 N1 Al1 109.47(8) . . ? C1 O1 Al1 121.47(9) . . ? C21 O2 Al1 133.81(9) . . ? C31 O3 Al1 130.62(9) . . ? P1 O4 Al1 151.36(8) . . ? O4 P1 N3P 119.23(7) . . ? O4 P1 N1P 108.84(7) . . ? N3P P1 N1P 104.06(8) . . ? O4 P1 N2P 105.13(7) . . ? N3P P1 N2P 106.76(9) . . ? N1P P1 N2P 113.07(8) . . ? C43 N1P C44 113.03(16) . . ? C43 N1P P1 119.46(12) . . ? C44 N1P P1 123.83(13) . . ? C41 N2P C42 113.53(16) . . ? C41 N2P P1 125.04(13) . . ? C42 N2P P1 121.36(14) . . ? C45 N3P C46 115.6(2) . . ? C45 N3P P1 119.86(17) . . ? C46 N3P P1 119.30(17) . . ? O1 C1 C2 109.35(12) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N1 C2 C1 108.12(12) . . ? N1 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N1 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O2 C21 C26 122.31(13) . . ? O2 C21 C22 119.03(13) . . ? C26 C21 C22 118.66(13) . . ? C23 C22 C21 119.49(14) . . ? C23 C22 C27 120.99(14) . . ? C21 C22 C27 119.52(14) . . ? C22 C23 C24 122.30(14) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 117.49(13) . . ? C25 C24 C28 120.67(15) . . ? C23 C24 C28 121.83(14) . . ? C24 C25 C26 122.02(14) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C21 120.03(13) . . ? C25 C26 C29 119.20(13) . . ? C21 C26 C29 120.58(12) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N1 C29 C26 114.35(11) . . ? N1 C29 H29A 108.7 . . ? C26 C29 H29A 108.7 . . ? N1 C29 H29B 108.7 . . ? C26 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? O3 C31 C36 121.16(13) . . ? O3 C31 C32 119.11(13) . . ? C36 C31 C32 119.73(13) . . ? C33 C32 C31 118.71(15) . . ? C33 C32 C37 122.36(15) . . ? C31 C32 C37 118.93(15) . . ? C32 C33 C34 122.53(15) . . ? C32 C33 H33 118.7 . . ? C34 C33 H33 118.7 . . ? C35 C34 C33 117.90(14) . . ? C35 C34 C38 121.46(17) . . ? C33 C34 C38 120.63(17) . . ? C34 C35 C36 121.35(15) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C35 C36 C31 119.73(14) . . ? C35 C36 C39 122.45(13) . . ? C31 C36 C39 117.81(12) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 C36 111.19(11) . . ? N1 C39 H39A 109.4 . . ? C36 C39 H39A 109.4 . . ? N1 C39 H39B 109.4 . . ? C36 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? N2P C41 H41A 109.5 . . ? N2P C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N2P C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N2P C42 H42A 109.5 . . ? N2P C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N2P C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N1P C43 H43A 109.5 . . ? N1P C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N1P C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N1P C44 H44A 109.5 . . ? N1P C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N1P C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3P C45 H45A 109.5 . . ? N3P C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N3P C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3P C46 H46A 109.5 . . ? N3P C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N3P C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.477 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.048 # Attachment '[HOiPrAl_L1_].cif' data_[HOiPrAl(L1)] _database_code_depnum_ccdc_archive 'CCDC 729815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common Alox _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.50 H50 Al N O4' _chemical_formula_weight 641.79 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5550(3) _cell_length_b 16.0370(5) _cell_length_c 17.7180(5) _cell_angle_alpha 76.594(1) _cell_angle_beta 73.352(1) _cell_angle_gamma 81.093(2) _cell_volume 3573.38(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19693 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 22.70 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9693 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; This crystal was weakly diffracting and there was no observable data above the 2theta limit recorded. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18899 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 7.86 _diffrn_reflns_theta_max 22.70 _reflns_number_total 8983 _reflns_number_gt 6924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0676P)^2^+5.5324P] 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_number_reflns 8983 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1749 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.21854(7) 0.22928(7) 0.88539(6) 0.0266(3) Uani 1 1 d . A . Al2 Al 0.18952(7) 0.22255(6) 1.17874(6) 0.0258(3) Uani 1 1 d . . . N1 N 0.1345(2) 0.26315(18) 0.80013(16) 0.0260(6) Uani 1 1 d . . . N2 N 0.2413(2) 0.13488(18) 1.26921(17) 0.0275(7) Uani 1 1 d . . . O1 O 0.10751(17) 0.25773(15) 0.96302(13) 0.0288(6) Uani 1 1 d . . . O2 O 0.30574(18) 0.30640(16) 0.83108(14) 0.0340(6) Uani 1 1 d . . . O3 O 0.24760(18) 0.12368(15) 0.86790(14) 0.0323(6) Uani 1 1 d . . . O4 O 0.29559(19) 0.19996(17) 0.96496(17) 0.0317(6) Uani 1 1 d . . . O5 O 0.20603(17) 0.14094(14) 1.12034(14) 0.0290(6) Uani 1 1 d . . . O6 O 0.06895(17) 0.24552(15) 1.24498(13) 0.0307(6) Uani 1 1 d . . . O7 O 0.28774(17) 0.28911(15) 1.16473(14) 0.0312(6) Uani 1 1 d . . . O8 O 0.14870(18) 0.30145(15) 1.09019(16) 0.0297(6) Uani 1 1 d . . . C1 C 0.0050(2) 0.2821(2) 0.9617(2) 0.0278(8) Uani 1 1 d . . . C2 C -0.0741(3) 0.2609(2) 1.0315(2) 0.0305(8) Uani 1 1 d . . . C3 C -0.1761(3) 0.2875(3) 1.0269(2) 0.0363(9) Uani 1 1 d . . . H3 H -0.2306 0.2735 1.0740 0.044 Uiso 1 1 calc R . . C4 C -0.2018(3) 0.3330(2) 0.9577(2) 0.0337(9) Uani 1 1 d . . . C5 C -0.1214(3) 0.3515(2) 0.8895(2) 0.0316(8) Uani 1 1 d . . . H5 H -0.1366 0.3821 0.8408 0.038 Uiso 1 1 calc R . . C6 C -0.0186(3) 0.3263(2) 0.8906(2) 0.0267(8) Uani 1 1 d . . . C7 C -0.0561(3) 0.2118(3) 1.1104(2) 0.0397(9) Uani 1 1 d . . . H7A H 0.0161 0.1872 1.1022 0.059 Uiso 1 1 calc R . . H7B H -0.1019 0.1655 1.1323 0.059 Uiso 1 1 calc R . . H7C H -0.0708 0.2509 1.1483 0.059 Uiso 1 1 calc R . . C8 C -0.3127(3) 0.3616(3) 0.9564(3) 0.0492(11) Uani 1 1 d . . . H8A H -0.3373 0.4110 0.9828 0.074 Uiso 1 1 calc R . . H8B H -0.3555 0.3142 0.9849 0.074 Uiso 1 1 calc R . . H8C H -0.3173 0.3780 0.9006 0.074 Uiso 1 1 calc R . . C9 C 0.0657(3) 0.3432(2) 0.8145(2) 0.0295(8) Uani 1 1 d . . . H9A H 0.0346 0.3662 0.7687 0.035 Uiso 1 1 calc R . . H9B H 0.1073 0.3872 0.8176 0.035 Uiso 1 1 calc R . . C21 C 0.3159(3) 0.3630(2) 0.7604(2) 0.0323(9) Uani 1 1 d . . . C22 C 0.3781(3) 0.4314(2) 0.7444(2) 0.0374(9) Uani 1 1 d . . . C23 C 0.3872(3) 0.4892(3) 0.6722(2) 0.0419(10) Uani 1 1 d . . . H23 H 0.4293 0.5349 0.6612 0.050 Uiso 1 1 calc R . . C24 C 0.3383(3) 0.4841(2) 0.6148(2) 0.0392(9) Uani 1 1 d . . . C25 C 0.2780(3) 0.4159(2) 0.6318(2) 0.0364(9) Uani 1 1 d . . . H25 H 0.2432 0.4108 0.5938 0.044 Uiso 1 1 calc R . . C26 C 0.2673(3) 0.3548(2) 0.7033(2) 0.0308(8) Uani 1 1 d . . . C27 C 0.4324(3) 0.4382(3) 0.8052(3) 0.0528(12) Uani 1 1 d . . . H27A H 0.4696 0.4900 0.7864 0.079 Uiso 1 1 calc R . . H27B H 0.4817 0.3872 0.8123 0.079 Uiso 1 1 calc R . . H27C H 0.3815 0.4417 0.8566 0.079 Uiso 1 1 calc R . . C28 C 0.3493(3) 0.5499(3) 0.5372(3) 0.0513(11) Uani 1 1 d . . . H28A H 0.3474 0.6074 0.5480 0.077 Uiso 1 1 calc R . . H28B H 0.2924 0.5484 0.5139 0.077 Uiso 1 1 calc R . . H28C H 0.4154 0.5365 0.4994 0.077 Uiso 1 1 calc R . . C29 C 0.2070(3) 0.2794(2) 0.7179(2) 0.0293(8) Uani 1 1 d . . . H29A H 0.2558 0.2274 0.7107 0.035 Uiso 1 1 calc R . . H29B H 0.1668 0.2896 0.6774 0.035 Uiso 1 1 calc R . . C31 C 0.2175(3) 0.0780(2) 0.8242(2) 0.0292(8) Uani 1 1 d . . . C32 C 0.2708(3) -0.0023(2) 0.8131(2) 0.0335(9) Uani 1 1 d . . . C33 C 0.2400(3) -0.0480(2) 0.7679(2) 0.0369(9) Uani 1 1 d . . . H33 H 0.2771 -0.1020 0.7598 0.044 Uiso 1 1 calc R . . C34 C 0.1574(3) -0.0188(2) 0.7337(2) 0.0343(9) Uani 1 1 d . . . C35 C 0.1051(3) 0.0605(2) 0.7464(2) 0.0313(8) Uani 1 1 d . . . H35 H 0.0481 0.0821 0.7241 0.038 Uiso 1 1 calc R . . C36 C 0.1340(3) 0.1092(2) 0.7909(2) 0.0271(8) Uani 1 1 d . . . C37 C 0.3585(3) -0.0387(3) 0.8518(3) 0.0452(10) Uani 1 1 d . . . H37A H 0.3888 -0.0937 0.8361 0.068 Uiso 1 1 calc R . . H37B H 0.3320 -0.0478 0.9104 0.068 Uiso 1 1 calc R . . H37C H 0.4116 0.0019 0.8341 0.068 Uiso 1 1 calc R . . C38 C 0.1240(3) -0.0715(3) 0.6867(3) 0.0471(10) Uani 1 1 d . . . H38A H 0.0633 -0.1004 0.7207 0.071 Uiso 1 1 calc R . . H38B H 0.1805 -0.1147 0.6695 0.071 Uiso 1 1 calc R . . H38C H 0.1066 -0.0336 0.6394 0.071 Uiso 1 1 calc R . . C39 C 0.0714(3) 0.1924(2) 0.8058(2) 0.0288(8) Uani 1 1 d . . . H39A H 0.0296 0.2114 0.7663 0.035 Uiso 1 1 calc R . . H39B H 0.0230 0.1819 0.8600 0.035 Uiso 1 1 calc R . . C41 C 0.4096(11) 0.1767(10) 0.9426(10) 0.044(5) Uani 0.70 1 d P A 1 H41 H 0.4356 0.1850 0.8828 0.053 Uiso 0.70 1 calc PR A 1 C42 C 0.4333(5) 0.0859(5) 0.9791(4) 0.0527(17) Uani 0.70 1 d P A 1 H42A H 0.5062 0.0678 0.9565 0.079 Uiso 0.70 1 calc PR A 1 H42B H 0.3896 0.0497 0.9677 0.079 Uiso 0.70 1 calc PR A 1 H42C H 0.4199 0.0800 1.0374 0.079 Uiso 0.70 1 calc PR A 1 C43 C 0.4558(5) 0.2397(6) 0.9726(5) 0.0565(19) Uani 0.70 1 d P A 1 H43A H 0.4389 0.2987 0.9457 0.085 Uiso 0.70 1 calc PR A 1 H43B H 0.5311 0.2268 0.9607 0.085 Uiso 0.70 1 calc PR A 1 H43C H 0.4270 0.2341 1.0308 0.085 Uiso 0.70 1 calc PR A 1 C41' C 0.405(3) 0.200(2) 0.9555(18) 0.036(11) Uani 0.30 1 d P A 2 H41' H 0.4211 0.2603 0.9313 0.044 Uiso 0.30 1 calc PR A 2 C42' C 0.4647(13) 0.1458(12) 0.8913(11) 0.058(4) Uani 0.30 1 d P A 2 H42D H 0.4547 0.0848 0.9129 0.087 Uiso 0.30 1 calc PR A 2 H42E H 0.5385 0.1536 0.8772 0.087 Uiso 0.30 1 calc PR A 2 H42F H 0.4388 0.1651 0.8432 0.087 Uiso 0.30 1 calc PR A 2 C43' C 0.4436(10) 0.1756(11) 1.0279(9) 0.045(3) Uani 0.30 1 d P A 2 H43D H 0.4251 0.1179 1.0567 0.067 Uiso 0.30 1 calc PR A 2 H43E H 0.4127 0.2171 1.0630 0.067 Uiso 0.30 1 calc PR A 2 H43F H 0.5191 0.1759 1.0122 0.067 Uiso 0.30 1 calc PR A 2 C51 C 0.2212(3) 0.0519(2) 1.1413(2) 0.0295(8) Uani 1 1 d . . . C52 C 0.1792(3) -0.0007(2) 1.1075(2) 0.0325(8) Uani 1 1 d . . . C53 C 0.1996(3) -0.0895(3) 1.1302(2) 0.0403(10) Uani 1 1 d . . . H53 H 0.1726 -0.1255 1.1069 0.048 Uiso 1 1 calc R . . C54 C 0.2563(3) -0.1282(2) 1.1843(3) 0.0428(10) Uani 1 1 d . . . C55 C 0.2964(3) -0.0743(2) 1.2171(2) 0.0394(9) Uani 1 1 d . . . H55 H 0.3354 -0.0989 1.2549 0.047 Uiso 1 1 calc R . . C56 C 0.2804(3) 0.0149(2) 1.1955(2) 0.0308(8) Uani 1 1 d . . . C57 C 0.1122(3) 0.0339(3) 1.0504(2) 0.0406(9) Uani 1 1 d . . . H57A H 0.1309 0.0006 1.0075 0.061 Uiso 1 1 calc R . . H57B H 0.1228 0.0945 1.0268 0.061 Uiso 1 1 calc R . . H57C H 0.0394 0.0290 1.0796 0.061 Uiso 1 1 calc R . . C58 C 0.2729(4) -0.2251(3) 1.2084(3) 0.0615(13) Uani 1 1 d . . . H58A H 0.2430 -0.2519 1.1767 0.092 Uiso 1 1 calc R . . H58B H 0.2393 -0.2432 1.2656 0.092 Uiso 1 1 calc R . . H58C H 0.3472 -0.2431 1.1983 0.092 Uiso 1 1 calc R . . C59 C 0.3230(3) 0.0710(2) 1.2329(2) 0.0321(8) Uani 1 1 d . . . H59A H 0.3783 0.1020 1.1915 0.039 Uiso 1 1 calc R . . H59B H 0.3540 0.0345 1.2751 0.039 Uiso 1 1 calc R . . C61 C 0.0279(3) 0.2201(2) 1.3254(2) 0.0303(8) Uani 1 1 d . . . C62 C -0.0579(3) 0.2694(3) 1.3639(2) 0.0365(9) Uani 1 1 d . . . C63 C -0.0987(3) 0.2441(3) 1.4461(2) 0.0399(9) Uani 1 1 d . . . H63 H -0.1559 0.2786 1.4723 0.048 Uiso 1 1 calc R . . C64 C -0.0596(3) 0.1705(3) 1.4918(2) 0.0391(9) Uani 1 1 d . . . C65 C 0.0234(3) 0.1217(3) 1.4515(2) 0.0353(9) Uani 1 1 d . . . H65 H 0.0508 0.0704 1.4810 0.042 Uiso 1 1 calc R . . C66 C 0.0685(3) 0.1453(2) 1.3691(2) 0.0287(8) Uani 1 1 d . . . C67 C -0.1056(3) 0.3469(3) 1.3153(3) 0.0520(11) Uani 1 1 d . . . H67A H -0.1354 0.3281 1.2785 0.078 Uiso 1 1 calc R . . H67B H -0.0523 0.3855 1.2843 0.078 Uiso 1 1 calc R . . H67C H -0.1601 0.3775 1.3515 0.078 Uiso 1 1 calc R . . C68 C -0.1033(3) 0.1461(3) 1.5816(2) 0.0515(11) Uani 1 1 d . . . H68A H -0.0684 0.0908 1.6022 0.077 Uiso 1 1 calc R . . H68B H -0.1776 0.1409 1.5938 0.077 Uiso 1 1 calc R . . H68C H -0.0923 0.1906 1.6072 0.077 Uiso 1 1 calc R . . C69 C 0.1542(3) 0.0881(2) 1.3274(2) 0.0318(8) Uani 1 1 d . . . H69A H 0.1258 0.0560 1.2982 0.038 Uiso 1 1 calc R . . H69B H 0.1818 0.0454 1.3683 0.038 Uiso 1 1 calc R . . C71 C 0.3716(3) 0.2831(2) 1.1942(2) 0.0292(8) Uani 1 1 d . . . C72 C 0.4493(3) 0.3380(2) 1.1535(2) 0.0309(8) Uani 1 1 d . . . C73 C 0.5351(3) 0.3303(2) 1.1838(2) 0.0338(9) Uani 1 1 d . . . H73 H 0.5884 0.3670 1.1560 0.041 Uiso 1 1 calc R . . C74 C 0.5464(3) 0.2716(2) 1.2526(2) 0.0318(8) Uani 1 1 d . . . C75 C 0.4659(3) 0.2205(2) 1.2934(2) 0.0322(8) Uani 1 1 d . . . H75 H 0.4710 0.1803 1.3412 0.039 Uiso 1 1 calc R . . C76 C 0.3778(3) 0.2267(2) 1.2658(2) 0.0294(8) Uani 1 1 d . . . C77 C 0.4358(3) 0.4069(3) 1.0829(2) 0.0425(10) Uani 1 1 d . . . H77A H 0.4469 0.3809 1.0358 0.064 Uiso 1 1 calc R . . H77B H 0.4861 0.4490 1.0714 0.064 Uiso 1 1 calc R . . H77C H 0.3656 0.4359 1.0951 0.064 Uiso 1 1 calc R . . C78 C 0.6405(3) 0.2673(3) 1.2838(3) 0.0410(10) Uani 1 1 d . . . H78A H 0.7031 0.2543 1.2425 0.061 Uiso 1 1 calc R . . H78B H 0.6357 0.2219 1.3321 0.061 Uiso 1 1 calc R . . H78C H 0.6434 0.3228 1.2969 0.061 Uiso 1 1 calc R . . C79 C 0.2856(3) 0.1799(2) 1.3158(2) 0.0308(8) Uani 1 1 d . . . H79A H 0.3059 0.1369 1.3600 0.037 Uiso 1 1 calc R . . H79B H 0.2311 0.2217 1.3403 0.037 Uiso 1 1 calc R . . C81 C 0.1354(3) 0.3954(2) 1.0792(2) 0.0326(8) Uani 1 1 d . . . H81 H 0.1620 0.4119 1.1203 0.039 Uiso 1 1 calc R . . C82 C 0.1991(3) 0.4340(3) 0.9974(2) 0.0431(10) Uani 1 1 d . . . H82A H 0.2710 0.4087 0.9906 0.065 Uiso 1 1 calc R . . H82B H 0.1964 0.4964 0.9924 0.065 Uiso 1 1 calc R . . H82C H 0.1715 0.4220 0.9560 0.065 Uiso 1 1 calc R . . C83 C 0.0222(3) 0.4273(3) 1.0932(2) 0.0429(10) Uani 1 1 d . . . H83A H -0.0046 0.4151 1.0514 0.064 Uiso 1 1 calc R . . H83B H 0.0137 0.4895 1.0911 0.064 Uiso 1 1 calc R . . H83C H -0.0160 0.3979 1.1460 0.064 Uiso 1 1 calc R . . C101 C -0.2836(3) 0.5191(3) 0.7240(3) 0.117(2) Uiso 1 1 d G B 1 H101 H -0.3453 0.5433 0.7562 0.140 Uiso 1 1 calc R B 1 C102 C -0.1892(4) 0.5486(3) 0.7159(3) 0.104(2) Uiso 1 1 d G B 1 H102 H -0.1863 0.5929 0.7425 0.125 Uiso 1 1 calc R B 1 C103 C -0.0990(3) 0.5132(3) 0.6689(3) 0.108(2) Uiso 1 1 d G B 1 H103 H -0.0344 0.5333 0.6633 0.130 Uiso 1 1 calc R B 1 C104 C -0.1032(3) 0.4484(3) 0.6300(3) 0.0893(18) Uiso 1 1 d G B 1 C105 C -0.1976(3) 0.4189(3) 0.6381(3) 0.0909(18) Uiso 1 1 d G B 1 H105 H -0.2005 0.3746 0.6115 0.109 Uiso 1 1 calc R B 1 C106 C -0.2878(3) 0.4543(3) 0.6851(3) 0.114(2) Uiso 1 1 d G B 1 H106 H -0.3523 0.4341 0.6907 0.137 Uiso 1 1 calc R B 1 C107 C -0.0094(8) 0.4062(7) 0.5823(7) 0.149(3) Uiso 1 1 d . B 1 H10A H 0.0473 0.4430 0.5673 0.224 Uiso 1 1 calc R B 1 H10B H -0.0230 0.3967 0.5337 0.224 Uiso 1 1 calc R B 1 H10C H 0.0099 0.3507 0.6144 0.224 Uiso 1 1 calc R B 1 C301 C 0.33472(16) 0.28747(15) 0.47769(15) 0.0424(10) Uani 1 1 d G C 1 C302 C 0.23593(19) 0.31252(13) 0.46711(16) 0.0454(10) Uani 1 1 d G C 1 H302 H 0.2211 0.3677 0.4366 0.055 Uiso 1 1 calc R C 1 C303 C 0.15887(15) 0.25678(17) 0.50124(17) 0.0489(11) Uani 1 1 d G C 1 H303 H 0.0914 0.2739 0.4940 0.059 Uiso 1 1 calc R C 1 C304 C 0.18061(17) 0.17601(16) 0.54595(16) 0.0473(11) Uani 1 1 d G C 1 H304 H 0.1279 0.1379 0.5693 0.057 Uiso 1 1 calc R C 1 C305 C 0.27940(19) 0.15096(14) 0.55653(16) 0.0484(11) Uani 1 1 d G C 1 H305 H 0.2943 0.0958 0.5871 0.058 Uiso 1 1 calc R C 1 C306 C 0.35646(15) 0.20670(17) 0.52240(16) 0.0466(10) Uani 1 1 d G C 1 H306 H 0.4240 0.1896 0.5296 0.056 Uiso 1 1 calc R C 1 C307 C 0.4185(4) 0.3477(3) 0.4417(3) 0.0591(12) Uani 1 1 d . C 1 H30A H 0.4212 0.3704 0.3849 0.089 Uiso 1 1 calc R C 1 H30B H 0.4852 0.3164 0.4463 0.089 Uiso 1 1 calc R C 1 H30C H 0.4035 0.3954 0.4704 0.089 Uiso 1 1 calc R C 1 C401 C 0.5578(2) 1.17640(19) 0.61967(19) 0.0637(14) Uani 1 1 d G D 1 C402 C 0.6314(2) 1.1615(2) 0.55003(18) 0.0622(13) Uani 1 1 d G D 1 H402 H 0.6773 1.2037 0.5201 0.075 Uiso 1 1 calc R D 1 C403 C 0.6377(2) 1.0849(3) 0.52423(17) 0.0835(18) Uani 1 1 d G D 1 H403 H 0.6880 1.0747 0.4766 0.100 Uiso 1 1 calc R D 1 C404 C 0.5705(3) 1.0231(2) 0.5681(2) 0.0764(16) Uani 1 1 d G D 1 H404 H 0.5748 0.9707 0.5505 0.092 Uiso 1 1 calc R D 1 C405 C 0.4969(2) 1.0380(2) 0.6377(2) 0.0675(14) Uani 1 1 d G D 1 H405 H 0.4509 0.9958 0.6677 0.081 Uiso 1 1 calc R D 1 C406 C 0.4906(2) 1.1146(2) 0.66353(16) 0.0631(14) Uani 1 1 d G D 1 H406 H 0.4403 1.1248 0.7111 0.076 Uiso 1 1 calc R D 1 C407 C 0.5467(5) 1.2584(4) 0.6461(4) 0.094(2) Uani 1 1 d . D 1 H40A H 0.6143 1.2810 0.6306 0.141 Uiso 1 1 calc R D 1 H40B H 0.5195 1.2491 0.7046 0.141 Uiso 1 1 calc R D 1 H40C H 0.4988 1.2998 0.6206 0.141 Uiso 1 1 calc R D 1 H4 H 0.269(3) 0.176(3) 1.015(3) 0.047(13) Uiso 1 1 d . E 1 H8 H 0.133(3) 0.289(3) 1.053(3) 0.033(11) Uiso 1 1 d . F 1 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 0.0260(6) 0.0308(6) 0.0241(6) -0.0071(4) -0.0050(4) -0.0062(4) Al2 0.0277(6) 0.0260(6) 0.0238(6) -0.0042(4) -0.0085(4) -0.0006(4) N1 0.0277(15) 0.0268(16) 0.0222(15) -0.0043(12) -0.0027(12) -0.0065(12) N2 0.0283(15) 0.0251(16) 0.0303(16) -0.0059(13) -0.0089(12) -0.0029(12) O1 0.0262(13) 0.0358(14) 0.0250(13) -0.0067(11) -0.0069(10) -0.0033(10) O2 0.0337(14) 0.0410(15) 0.0284(14) -0.0057(12) -0.0062(11) -0.0125(11) O3 0.0335(13) 0.0336(14) 0.0342(14) -0.0108(11) -0.0131(11) -0.0020(11) O4 0.0234(15) 0.0450(16) 0.0264(16) -0.0100(13) -0.0041(11) -0.0027(11) O5 0.0339(13) 0.0261(14) 0.0287(13) -0.0048(10) -0.0125(10) -0.0001(10) O6 0.0312(13) 0.0360(14) 0.0225(13) -0.0049(11) -0.0057(10) 0.0003(10) O7 0.0317(13) 0.0301(14) 0.0313(14) -0.0002(11) -0.0122(11) -0.0032(10) O8 0.0384(14) 0.0265(14) 0.0264(14) -0.0054(11) -0.0144(12) 0.0018(10) C1 0.0229(18) 0.031(2) 0.032(2) -0.0109(16) -0.0073(15) -0.0012(15) C2 0.029(2) 0.033(2) 0.028(2) -0.0048(16) -0.0067(16) -0.0030(15) C3 0.029(2) 0.045(2) 0.034(2) -0.0109(18) -0.0028(16) -0.0053(17) C4 0.028(2) 0.038(2) 0.036(2) -0.0109(18) -0.0081(17) -0.0007(16) C5 0.037(2) 0.027(2) 0.032(2) -0.0073(16) -0.0135(17) 0.0022(16) C6 0.0290(19) 0.0244(19) 0.0268(19) -0.0062(15) -0.0071(15) -0.0020(14) C7 0.033(2) 0.053(3) 0.029(2) -0.0039(18) -0.0021(16) -0.0097(18) C8 0.032(2) 0.062(3) 0.051(3) -0.009(2) -0.0122(19) 0.0045(19) C9 0.0331(19) 0.028(2) 0.0262(19) -0.0031(15) -0.0074(15) -0.0029(15) C21 0.031(2) 0.033(2) 0.030(2) -0.0100(17) 0.0009(16) -0.0062(16) C22 0.033(2) 0.038(2) 0.038(2) -0.0143(19) 0.0053(17) -0.0100(17) C23 0.041(2) 0.033(2) 0.044(3) -0.0101(19) 0.0082(19) -0.0127(17) C24 0.038(2) 0.031(2) 0.037(2) -0.0044(17) 0.0063(18) -0.0030(17) C25 0.035(2) 0.035(2) 0.032(2) -0.0074(18) 0.0018(16) -0.0020(17) C26 0.0306(19) 0.030(2) 0.027(2) -0.0065(16) 0.0013(15) -0.0055(15) C27 0.054(3) 0.058(3) 0.050(3) -0.018(2) -0.001(2) -0.031(2) C28 0.050(3) 0.039(2) 0.050(3) 0.003(2) 0.003(2) -0.0075(19) C29 0.0324(19) 0.033(2) 0.0219(19) -0.0071(16) -0.0037(15) -0.0057(15) C31 0.033(2) 0.031(2) 0.0254(19) -0.0065(16) -0.0063(15) -0.0094(16) C32 0.035(2) 0.030(2) 0.036(2) -0.0062(17) -0.0088(16) -0.0069(16) C33 0.041(2) 0.028(2) 0.041(2) -0.0075(17) -0.0076(18) -0.0069(17) C34 0.042(2) 0.031(2) 0.031(2) -0.0064(17) -0.0069(17) -0.0126(17) C35 0.034(2) 0.033(2) 0.027(2) -0.0019(16) -0.0084(16) -0.0102(16) C36 0.0273(18) 0.029(2) 0.0239(19) -0.0034(15) -0.0030(15) -0.0091(15) C37 0.048(2) 0.035(2) 0.059(3) -0.016(2) -0.024(2) 0.0057(18) C38 0.058(3) 0.042(2) 0.051(3) -0.018(2) -0.020(2) -0.010(2) C39 0.0280(19) 0.034(2) 0.0279(19) -0.0064(16) -0.0091(15) -0.0084(15) C41 0.014(5) 0.087(11) 0.040(7) -0.043(6) -0.006(4) 0.011(5) C42 0.041(3) 0.072(5) 0.052(4) -0.030(4) -0.022(3) 0.020(3) C43 0.036(4) 0.090(6) 0.055(5) -0.025(5) -0.014(3) -0.017(4) C41' 0.054(18) 0.034(13) 0.008(11) -0.005(12) 0.002(9) 0.016(11) C42' 0.047(9) 0.086(12) 0.051(10) -0.030(10) -0.015(8) -0.004(8) C43' 0.033(7) 0.059(10) 0.046(9) -0.021(8) -0.012(6) 0.005(7) C51 0.0325(19) 0.025(2) 0.028(2) -0.0056(16) -0.0060(16) 0.0021(15) C52 0.036(2) 0.032(2) 0.030(2) -0.0077(16) -0.0075(16) -0.0046(16) C53 0.053(2) 0.035(2) 0.039(2) -0.0134(18) -0.0142(19) -0.0091(18) C54 0.054(2) 0.029(2) 0.048(2) -0.0121(19) -0.016(2) 0.0010(18) C55 0.048(2) 0.032(2) 0.040(2) -0.0082(18) -0.0200(19) 0.0066(17) C56 0.033(2) 0.026(2) 0.033(2) -0.0066(16) -0.0100(16) 0.0010(15) C57 0.050(2) 0.040(2) 0.038(2) -0.0077(18) -0.0180(19) -0.0109(18) C58 0.090(4) 0.031(2) 0.073(3) -0.013(2) -0.037(3) 0.000(2) C59 0.032(2) 0.029(2) 0.038(2) -0.0071(16) -0.0154(16) 0.0030(15) C61 0.0307(19) 0.037(2) 0.025(2) -0.0065(17) -0.0075(15) -0.0089(16) C62 0.029(2) 0.046(2) 0.033(2) -0.0096(18) -0.0063(17) -0.0028(17) C63 0.032(2) 0.051(3) 0.033(2) -0.0114(19) -0.0010(17) -0.0050(18) C64 0.037(2) 0.052(3) 0.029(2) -0.0064(19) -0.0044(17) -0.0164(19) C65 0.039(2) 0.038(2) 0.032(2) -0.0015(17) -0.0130(17) -0.0153(17) C66 0.0307(19) 0.031(2) 0.028(2) -0.0047(16) -0.0103(16) -0.0088(15) C67 0.041(2) 0.065(3) 0.037(2) -0.010(2) -0.0024(19) 0.017(2) C68 0.051(3) 0.066(3) 0.031(2) -0.002(2) -0.0014(19) -0.017(2) C69 0.037(2) 0.030(2) 0.030(2) -0.0004(16) -0.0126(16) -0.0071(16) C71 0.0283(19) 0.029(2) 0.033(2) -0.0086(17) -0.0111(16) 0.0002(15) C72 0.030(2) 0.029(2) 0.030(2) -0.0040(16) -0.0053(16) -0.0013(15) C73 0.028(2) 0.031(2) 0.041(2) -0.0117(18) -0.0028(16) -0.0047(15) C74 0.0264(19) 0.033(2) 0.041(2) -0.0177(18) -0.0087(16) -0.0014(16) C75 0.037(2) 0.032(2) 0.030(2) -0.0080(16) -0.0129(16) 0.0007(16) C76 0.031(2) 0.0270(19) 0.032(2) -0.0100(16) -0.0088(16) -0.0004(15) C77 0.035(2) 0.042(2) 0.043(2) 0.0038(19) -0.0067(18) -0.0081(18) C78 0.035(2) 0.039(2) 0.055(3) -0.0158(19) -0.0173(19) -0.0010(17) C79 0.036(2) 0.033(2) 0.0265(19) -0.0037(16) -0.0141(16) -0.0037(16) C81 0.043(2) 0.025(2) 0.031(2) -0.0058(16) -0.0157(17) 0.0031(16) C82 0.051(2) 0.036(2) 0.040(2) -0.0030(18) -0.0130(19) -0.0024(18) C83 0.046(2) 0.038(2) 0.039(2) -0.0057(19) -0.0115(18) 0.0099(18) C301 0.046(2) 0.054(3) 0.031(2) -0.013(2) -0.0068(18) -0.013(2) C302 0.054(3) 0.046(3) 0.040(2) -0.008(2) -0.017(2) -0.009(2) C303 0.046(2) 0.061(3) 0.048(3) -0.011(2) -0.022(2) -0.013(2) C304 0.053(3) 0.058(3) 0.036(2) -0.006(2) -0.0106(19) -0.023(2) C305 0.057(3) 0.054(3) 0.034(2) -0.006(2) -0.014(2) -0.007(2) C306 0.040(2) 0.062(3) 0.039(2) -0.008(2) -0.0119(19) -0.010(2) C307 0.060(3) 0.064(3) 0.055(3) -0.020(2) -0.004(2) -0.024(2) C401 0.055(3) 0.077(4) 0.062(3) -0.010(3) -0.030(3) 0.007(3) C402 0.039(3) 0.080(4) 0.058(3) 0.004(3) -0.012(2) -0.005(2) C403 0.062(3) 0.112(5) 0.064(4) -0.004(4) -0.017(3) 0.007(3) C404 0.086(4) 0.070(4) 0.079(4) -0.008(3) -0.046(3) 0.009(3) C405 0.058(3) 0.077(4) 0.060(3) 0.002(3) -0.021(3) 0.002(3) C406 0.042(3) 0.081(4) 0.057(3) 0.024(3) -0.022(2) -0.017(2) C407 0.103(5) 0.090(5) 0.109(5) -0.020(4) -0.068(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.757(3) . ? Al1 O2 1.761(2) . ? Al1 O1 1.805(2) . ? Al1 O4 1.919(3) . ? Al1 N1 2.071(3) . ? Al2 O6 1.760(2) . ? Al2 O7 1.761(2) . ? Al2 O5 1.799(2) . ? Al2 O8 1.931(3) . ? Al2 N2 2.082(3) . ? N1 C39 1.493(4) . ? N1 C9 1.492(4) . ? N1 C29 1.496(4) . ? N2 C59 1.495(5) . ? N2 C69 1.496(5) . ? N2 C79 1.502(4) . ? O1 C1 1.389(4) . ? O2 C21 1.351(4) . ? O3 C31 1.356(4) . ? O4 C41' 1.44(4) . ? O4 C41 1.491(14) . ? O4 H4 0.87(5) . ? O5 C51 1.387(4) . ? O6 C61 1.361(4) . ? O7 C71 1.363(4) . ? O8 C81 1.463(4) . ? O8 H8 0.82(4) . ? C1 C6 1.392(5) . ? C1 C2 1.398(5) . ? C2 C3 1.403(5) . ? C2 C7 1.503(5) . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C4 C5 1.384(5) . ? C4 C8 1.507(5) . ? C5 C6 1.394(5) . ? C5 H5 0.9500 . ? C6 C9 1.497(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C21 C26 1.396(5) . ? C21 C22 1.413(5) . ? C22 C23 1.381(6) . ? C22 C27 1.499(6) . ? C23 C24 1.385(6) . ? C23 H23 0.9500 . ? C24 C25 1.393(6) . ? C24 C28 1.512(6) . ? C25 C26 1.395(5) . ? C25 H25 0.9500 . ? C26 C29 1.495(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 C36 1.396(5) . ? C31 C32 1.403(5) . ? C32 C33 1.383(5) . ? C32 C37 1.513(5) . ? C33 C34 1.392(5) . ? C33 H33 0.9500 . ? C34 C35 1.389(5) . ? C34 C38 1.507(5) . ? C35 C36 1.394(5) . ? C35 H35 0.9500 . ? C36 C39 1.501(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C41 C42 1.476(17) . ? C41 C43 1.527(16) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C41' C43' 1.47(4) . ? C41' C42' 1.55(3) . ? C41' H41' 1.0000 . ? C42' H42D 0.9800 . ? C42' H42E 0.9800 . ? C42' H42F 0.9800 . ? C43' H43D 0.9800 . ? C43' H43E 0.9800 . ? C43' H43F 0.9800 . ? C51 C56 1.397(5) . ? C51 C52 1.404(5) . ? C52 C53 1.393(5) . ? C52 C57 1.506(5) . ? C53 C54 1.377(6) . ? C53 H53 0.9500 . ? C54 C55 1.391(6) . ? C54 C58 1.513(6) . ? C55 C56 1.392(5) . ? C55 H55 0.9500 . ? C56 C59 1.495(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C61 C66 1.397(5) . ? C61 C62 1.398(5) . ? C62 C63 1.387(5) . ? C62 C67 1.510(6) . ? C63 C64 1.393(6) . ? C63 H63 0.9500 . ? C64 C65 1.383(6) . ? C64 C68 1.510(6) . ? C65 C66 1.398(5) . ? C65 H65 0.9500 . ? C66 C69 1.493(5) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C71 C76 1.392(5) . ? C71 C72 1.401(5) . ? C72 C73 1.391(5) . ? C72 C77 1.500(5) . ? C73 C74 1.389(5) . ? C73 H73 0.9500 . ? C74 C75 1.392(5) . ? C74 C78 1.515(5) . ? C75 C76 1.396(5) . ? C75 H75 0.9500 . ? C76 C79 1.504(5) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C81 C82 1.503(6) . ? C81 C83 1.507(5) . ? C81 H81 1.0000 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C101 H101 0.9500 . ? C102 C103 1.3900 . ? C102 H102 0.9500 . ? C103 C104 1.3900 . ? C103 H103 0.9500 . ? C104 C105 1.3900 . ? C104 C107 1.473(11) . ? C105 C106 1.3900 . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? C301 C302 1.3900 . ? C301 C306 1.3900 . ? C301 C307 1.505(5) . ? C302 C303 1.3900 . ? C302 H302 0.9500 . ? C303 C304 1.3900 . ? C303 H303 0.9500 . ? C304 C305 1.3900 . ? C304 H304 0.9500 . ? C305 C306 1.3900 . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C307 H30A 0.9800 . ? C307 H30B 0.9800 . ? C307 H30C 0.9800 . ? C401 C402 1.3900 . ? C401 C406 1.3900 . ? C401 C407 1.468(7) . ? C402 C403 1.3900 . ? C402 H402 0.9500 . ? C403 C404 1.3900 . ? C403 H403 0.9500 . ? C404 C405 1.3900 . ? C404 H404 0.9500 . ? C405 C406 1.3900 . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? C407 H40A 0.9800 . ? C407 H40B 0.9800 . ? C407 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O2 118.79(12) . . ? O3 Al1 O1 121.43(12) . . ? O2 Al1 O1 119.59(12) . . ? O3 Al1 O4 89.75(11) . . ? O2 Al1 O4 88.15(12) . . ? O1 Al1 O4 87.70(11) . . ? O3 Al1 N1 91.32(11) . . ? O2 Al1 N1 91.44(11) . . ? O1 Al1 N1 91.63(11) . . ? O4 Al1 N1 178.92(12) . . ? O6 Al2 O7 117.57(12) . . ? O6 Al2 O5 120.41(12) . . ? O7 Al2 O5 121.72(12) . . ? O6 Al2 O8 91.08(11) . . ? O7 Al2 O8 87.43(11) . . ? O5 Al2 O8 86.12(11) . . ? O6 Al2 N2 92.33(11) . . ? O7 Al2 N2 91.53(11) . . ? O5 Al2 N2 91.64(11) . . ? O8 Al2 N2 176.54(12) . . ? C39 N1 C9 110.1(3) . . ? C39 N1 C29 108.7(3) . . ? C9 N1 C29 109.7(3) . . ? C39 N1 Al1 110.5(2) . . ? C9 N1 Al1 108.4(2) . . ? C29 N1 Al1 109.5(2) . . ? C59 N2 C69 109.0(3) . . ? C59 N2 C79 109.0(3) . . ? C69 N2 C79 107.5(3) . . ? C59 N2 Al2 109.6(2) . . ? C69 N2 Al2 110.7(2) . . ? C79 N2 Al2 111.0(2) . . ? C1 O1 Al1 130.6(2) . . ? C21 O2 Al1 134.3(2) . . ? C31 O3 Al1 135.1(2) . . ? C41' O4 C41 18.0(17) . . ? C41' O4 Al1 129.8(12) . . ? C41 O4 Al1 121.3(6) . . ? C41' O4 H4 107(3) . . ? C41 O4 H4 110(3) . . ? Al1 O4 H4 123(3) . . ? C51 O5 Al2 130.8(2) . . ? C61 O6 Al2 133.8(2) . . ? C71 O7 Al2 135.2(2) . . ? C81 O8 Al2 125.9(2) . . ? C81 O8 H8 108(3) . . ? Al2 O8 H8 126(3) . . ? O1 C1 C6 119.9(3) . . ? O1 C1 C2 119.8(3) . . ? C6 C1 C2 120.3(3) . . ? C1 C2 C3 117.4(3) . . ? C1 C2 C7 124.0(3) . . ? C3 C2 C7 118.6(3) . . ? C4 C3 C2 123.6(3) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 117.3(3) . . ? C3 C4 C8 121.5(3) . . ? C5 C4 C8 121.3(3) . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 119.9(3) . . ? C1 C6 C9 120.2(3) . . ? C5 C6 C9 119.8(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C6 111.4(3) . . ? N1 C9 H9A 109.4 . . ? C6 C9 H9A 109.4 . . ? N1 C9 H9B 109.4 . . ? C6 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? O2 C21 C26 121.4(3) . . ? O2 C21 C22 118.7(3) . . ? C26 C21 C22 119.9(3) . . ? C23 C22 C21 118.1(4) . . ? C23 C22 C27 122.5(3) . . ? C21 C22 C27 119.4(4) . . ? C22 C23 C24 123.7(4) . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C25 117.1(4) . . ? C23 C24 C28 121.7(4) . . ? C25 C24 C28 121.2(4) . . ? C24 C25 C26 121.7(4) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C21 119.5(3) . . ? C25 C26 C29 120.6(3) . . ? C21 C26 C29 119.8(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 N1 113.1(3) . . ? C26 C29 H29A 109.0 . . ? N1 C29 H29A 109.0 . . ? C26 C29 H29B 109.0 . . ? N1 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? O3 C31 C36 121.2(3) . . ? O3 C31 C32 119.1(3) . . ? C36 C31 C32 119.7(3) . . ? C33 C32 C31 118.7(3) . . ? C33 C32 C37 121.0(3) . . ? C31 C32 C37 120.3(3) . . ? C32 C33 C34 123.1(4) . . ? C32 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C35 C34 C33 117.0(3) . . ? C35 C34 C38 121.2(3) . . ? C33 C34 C38 121.7(3) . . ? C34 C35 C36 121.9(3) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C35 C36 C31 119.6(3) . . ? C35 C36 C39 119.4(3) . . ? C31 C36 C39 120.9(3) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 C36 114.2(3) . . ? N1 C39 H39A 108.7 . . ? C36 C39 H39A 108.7 . . ? N1 C39 H39B 108.7 . . ? C36 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C42 C41 O4 109.8(10) . . ? C42 C41 C43 113.0(11) . . ? O4 C41 C43 105.6(10) . . ? C42 C41 H41 109.5 . . ? O4 C41 H41 109.5 . . ? C43 C41 H41 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O4 C41' C43' 119(2) . . ? O4 C41' C42' 109(3) . . ? C43' C41' C42' 112(2) . . ? O4 C41' H41' 105.7 . . ? C43' C41' H41' 105.7 . . ? C42' C41' H41' 105.7 . . ? C41' C42' H42D 109.5 . . ? C41' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C41' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? C41' C43' H43D 109.5 . . ? C41' C43' H43E 109.5 . . ? H43D C43' H43E 109.5 . . ? C41' C43' H43F 109.5 . . ? H43D C43' H43F 109.5 . . ? H43E C43' H43F 109.5 . . ? O5 C51 C56 119.2(3) . . ? O5 C51 C52 120.7(3) . . ? C56 C51 C52 120.1(3) . . ? C53 C52 C51 117.4(3) . . ? C53 C52 C57 119.2(3) . . ? C51 C52 C57 123.5(3) . . ? C54 C53 C52 124.1(3) . . ? C54 C53 H53 117.9 . . ? C52 C53 H53 117.9 . . ? C53 C54 C55 117.1(4) . . ? C53 C54 C58 121.5(4) . . ? C55 C54 C58 121.4(4) . . ? C56 C55 C54 121.4(4) . . ? C56 C55 H55 119.3 . . ? C54 C55 H55 119.3 . . ? C55 C56 C51 119.8(3) . . ? C55 C56 C59 120.1(3) . . ? C51 C56 C59 120.1(3) . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C54 C58 H58A 109.5 . . ? C54 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C54 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 N2 111.9(3) . . ? C56 C59 H59A 109.2 . . ? N2 C59 H59A 109.2 . . ? C56 C59 H59B 109.2 . . ? N2 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? O6 C61 C66 121.2(3) . . ? O6 C61 C62 118.8(3) . . ? C66 C61 C62 120.0(3) . . ? C63 C62 C61 118.7(4) . . ? C63 C62 C67 121.7(3) . . ? C61 C62 C67 119.6(3) . . ? C62 C63 C64 122.9(4) . . ? C62 C63 H63 118.5 . . ? C64 C63 H63 118.5 . . ? C65 C64 C63 117.0(3) . . ? C65 C64 C68 121.1(4) . . ? C63 C64 C68 121.8(4) . . ? C64 C65 C66 122.2(4) . . ? C64 C65 H65 118.9 . . ? C66 C65 H65 118.9 . . ? C61 C66 C65 119.1(3) . . ? C61 C66 C69 120.5(3) . . ? C65 C66 C69 120.3(3) . . ? C62 C67 H67A 109.5 . . ? C62 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C62 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C64 C68 H68A 109.5 . . ? C64 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C64 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 N2 114.0(3) . . ? C66 C69 H69A 108.7 . . ? N2 C69 H69A 108.7 . . ? C66 C69 H69B 108.7 . . ? N2 C69 H69B 108.7 . . ? H69A C69 H69B 107.6 . . ? O7 C71 C76 120.9(3) . . ? O7 C71 C72 118.8(3) . . ? C76 C71 C72 120.2(3) . . ? C73 C72 C71 118.2(3) . . ? C73 C72 C77 121.4(3) . . ? C71 C72 C77 120.2(3) . . ? C74 C73 C72 123.0(3) . . ? C74 C73 H73 118.5 . . ? C72 C73 H73 118.5 . . ? C73 C74 C75 117.3(3) . . ? C73 C74 C78 120.8(3) . . ? C75 C74 C78 121.8(3) . . ? C74 C75 C76 121.5(3) . . ? C74 C75 H75 119.2 . . ? C76 C75 H75 119.2 . . ? C71 C76 C75 119.5(3) . . ? C71 C76 C79 119.2(3) . . ? C75 C76 C79 121.0(3) . . ? C72 C77 H77A 109.5 . . ? C72 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C72 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C74 C78 H78A 109.5 . . ? C74 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C74 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N2 C79 C76 113.7(3) . . ? N2 C79 H79A 108.8 . . ? C76 C79 H79A 108.8 . . ? N2 C79 H79B 108.8 . . ? C76 C79 H79B 108.8 . . ? H79A C79 H79B 107.7 . . ? O8 C81 C82 109.5(3) . . ? O8 C81 C83 110.2(3) . . ? C82 C81 C83 113.0(3) . . ? O8 C81 H81 108.0 . . ? C82 C81 H81 108.0 . . ? C83 C81 H81 108.0 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C102 C101 C106 120.0 . . ? C102 C101 H101 120.0 . . ? C106 C101 H101 120.0 . . ? C103 C102 C101 120.0 . . ? C103 C102 H102 120.0 . . ? C101 C102 H102 120.0 . . ? C104 C103 C102 120.0 . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C103 C104 C105 120.0 . . ? C103 C104 C107 122.1(5) . . ? C105 C104 C107 117.8(5) . . ? C106 C105 C104 120.0 . . ? C106 C105 H105 120.0 . . ? C104 C105 H105 120.0 . . ? C105 C106 C101 120.0 . . ? C105 C106 H106 120.0 . . ? C101 C106 H106 120.0 . . ? C104 C107 H10A 109.5 . . ? C104 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C104 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C302 C301 C306 120.0 . . ? C302 C301 C307 120.4(3) . . ? C306 C301 C307 119.6(3) . . ? C301 C302 C303 120.0 . . ? C301 C302 H302 120.0 . . ? C303 C302 H302 120.0 . . ? C302 C303 C304 120.0 . . ? C302 C303 H303 120.0 . . ? C304 C303 H303 120.0 . . ? C305 C304 C303 120.0 . . ? C305 C304 H304 120.0 . . ? C303 C304 H304 120.0 . . ? C304 C305 C306 120.0 . . ? C304 C305 H305 120.0 . . ? C306 C305 H305 120.0 . . ? C305 C306 C301 120.0 . . ? C305 C306 H306 120.0 . . ? C301 C306 H306 120.0 . . ? C301 C307 H30A 109.5 . . ? C301 C307 H30B 109.5 . . ? H30A C307 H30B 109.5 . . ? C301 C307 H30C 109.5 . . ? H30A C307 H30C 109.5 . . ? H30B C307 H30C 109.5 . . ? C402 C401 C406 120.0 . . ? C402 C401 C407 120.9(4) . . ? C406 C401 C407 119.0(4) . . ? C403 C402 C401 120.0 . . ? C403 C402 H402 120.0 . . ? C401 C402 H402 120.0 . . ? C402 C403 C404 120.0 . . ? C402 C403 H403 120.0 . . ? C404 C403 H403 120.0 . . ? C405 C404 C403 120.0 . . ? C405 C404 H404 120.0 . . ? C403 C404 H404 120.0 . . ? C406 C405 C404 120.0 . . ? C406 C405 H405 120.0 . . ? C404 C405 H405 120.0 . . ? C405 C406 C401 120.0 . . ? C405 C406 H406 120.0 . . ? C401 C406 H406 120.0 . . ? C401 C407 H40A 109.5 . . ? C401 C407 H40B 109.5 . . ? H40A C407 H40B 109.5 . . ? C401 C407 H40C 109.5 . . ? H40A C407 H40C 109.5 . . ? H40B C407 H40C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O5 0.87(5) 1.82(5) 2.680(4) 173(4) . O8 H8 O1 0.82(4) 1.91(5) 2.730(4) 176(4) . _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 22.70 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.091 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.052 # Attachment '[THFAl_L1_].cif' data_[THFAl(L1)] _database_code_depnum_ccdc_archive 'CCDC 729816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (THFAl(L1)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H38 Al N O4' _chemical_formula_weight 515.60 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' Al Al 0.0645 0.0514 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3390(2) _cell_length_b 17.5120(3) _cell_length_c 16.6540(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.712(1) _cell_angle_gamma 90.00 _cell_volume 2699.04(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34626 _cell_measurement_theta_min 8.20 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.112 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'SADABS (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius Kappa CCD' _diffrn_measurement_method 'Omega & phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34626 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 8.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6000 _reflns_number_gt 4266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius control software' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELX-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III (johnson, 1999)' _computing_publication_material 'WinGX (Farrugia, 2001)' _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^)+(0.0560P)^2^+1.1792P] 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 6000 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.83770(6) 0.11566(3) 0.82042(3) 0.02415(15) Uani 1 1 d . . . O1 O 0.69386(14) 0.10834(7) 0.73993(8) 0.0290(3) Uani 1 1 d . . . O2 O 0.91209(14) 0.20507(7) 0.85046(8) 0.0305(3) Uani 1 1 d . . . O3 O 0.89216(14) 0.03411(7) 0.87749(8) 0.0280(3) Uani 1 1 d . . . O4 O 0.69319(15) 0.13360(7) 0.89308(8) 0.0309(3) Uani 1 1 d . . . N1 N 0.98960(16) 0.09797(8) 0.74300(9) 0.0221(3) Uani 1 1 d . . . C1 C 0.6882(2) 0.09476(10) 0.65952(11) 0.0264(4) Uani 1 1 d . . . C2 C 0.5628(2) 0.11479(10) 0.60745(12) 0.0310(4) Uani 1 1 d . . . C3 C 0.5590(2) 0.10245(12) 0.52445(13) 0.0351(5) Uani 1 1 d . . . H3 H 0.4743 0.1162 0.4893 0.042 Uiso 1 1 calc R . . C4 C 0.6743(2) 0.07077(11) 0.49108(12) 0.0343(4) Uani 1 1 d . . . C5 C 0.7958(2) 0.05056(10) 0.54395(11) 0.0291(4) Uani 1 1 d . . . H5 H 0.8756 0.0284 0.5227 0.035 Uiso 1 1 calc R . . C6 C 0.8044(2) 0.06181(10) 0.62733(11) 0.0259(4) Uani 1 1 d . . . C9 C 0.9376(2) 0.03791(10) 0.68218(11) 0.0256(4) Uani 1 1 d . . . H9A H 0.9166 -0.0094 0.7110 0.031 Uiso 1 1 calc R . . H9B H 1.0152 0.0263 0.6490 0.031 Uiso 1 1 calc R . . C7 C 0.4368(2) 0.14916(13) 0.64188(15) 0.0416(5) Uani 1 1 d . . . H7A H 0.3584 0.1595 0.5979 0.062 Uiso 1 1 calc R . . H7B H 0.4669 0.1970 0.6697 0.062 Uiso 1 1 calc R . . H7C H 0.4029 0.1134 0.6805 0.062 Uiso 1 1 calc R . . C8 C 0.6697(3) 0.05980(15) 0.40106(13) 0.0482(6) Uani 1 1 d . . . H8A H 0.6649 0.1097 0.3742 0.072 Uiso 1 1 calc R . . H8B H 0.5842 0.0297 0.3803 0.072 Uiso 1 1 calc R . . H8C H 0.7569 0.0328 0.3901 0.072 Uiso 1 1 calc R . . C21 C 1.0211(2) 0.24731(10) 0.82777(11) 0.0262(4) Uani 1 1 d . . . C22 C 1.0804(2) 0.30671(10) 0.87914(11) 0.0286(4) Uani 1 1 d . . . C23 C 1.1876(2) 0.35224(10) 0.85383(12) 0.0292(4) Uani 1 1 d . . . H23 H 1.2269 0.3924 0.8882 0.035 Uiso 1 1 calc R . . C24 C 1.2397(2) 0.34152(10) 0.78023(12) 0.0288(4) Uani 1 1 d . . . C25 C 1.1842(2) 0.28039(10) 0.73235(11) 0.0266(4) Uani 1 1 d . . . H25 H 1.2209 0.2705 0.6828 0.032 Uiso 1 1 calc R . . C26 C 1.07671(19) 0.23342(10) 0.75507(11) 0.0247(4) Uani 1 1 d . . . C29 C 1.0155(2) 0.17047(10) 0.69940(11) 0.0257(4) Uiso 1 1 d . . . H29A H 0.9230 0.1879 0.6689 0.031 Uiso 1 1 calc R . . H29B H 1.0830 0.1600 0.6597 0.031 Uiso 1 1 calc R . . C27 C 1.0272(3) 0.32008(12) 0.95911(13) 0.0395(5) Uani 1 1 d . . . H27A H 1.0586 0.2780 0.9961 0.059 Uiso 1 1 calc R . . H27B H 0.9215 0.3228 0.9510 0.059 Uiso 1 1 calc R . . H27C H 1.0669 0.3682 0.9824 0.059 Uiso 1 1 calc R . . C28 C 1.3497(2) 0.39472(13) 0.75216(14) 0.0416(5) Uani 1 1 d . . . H28A H 1.4398 0.3668 0.7491 0.062 Uiso 1 1 calc R . . H28B H 1.3683 0.4370 0.7906 0.062 Uiso 1 1 calc R . . H28C H 1.3126 0.4149 0.6985 0.062 Uiso 1 1 calc R . . C31 C 0.9972(2) -0.01842(10) 0.87422(10) 0.0244(4) Uani 1 1 d . . . C32 C 0.9906(2) -0.08755(10) 0.91637(10) 0.0261(4) Uani 1 1 d . . . C33 C 1.0977(2) -0.14184(10) 0.91112(11) 0.0291(4) Uani 1 1 d . . . H33 H 1.0945 -0.1882 0.9405 0.035 Uiso 1 1 calc R . . C34 C 1.2094(2) -0.13118(10) 0.86466(12) 0.0292(4) Uani 1 1 d . . . C35 C 1.2160(2) -0.06123(10) 0.82529(11) 0.0265(4) Uani 1 1 d . . . H35 H 1.2924 -0.0520 0.7942 0.032 Uiso 1 1 calc R . . C36 C 1.1132(2) -0.00470(10) 0.83056(11) 0.0245(4) Uani 1 1 d . . . C39 C 1.12719(19) 0.07179(10) 0.79100(11) 0.0249(4) Uani 1 1 d . . . H39A H 1.1586 0.1101 0.8334 0.030 Uiso 1 1 calc R . . H39B H 1.2029 0.0685 0.7548 0.030 Uiso 1 1 calc R . . C37 C 0.8701(2) -0.10162(11) 0.96612(12) 0.0313(4) Uani 1 1 d . . . H37A H 0.7817 -0.1148 0.9302 0.047 Uiso 1 1 calc R . . H37B H 0.8535 -0.0554 0.9967 0.047 Uiso 1 1 calc R . . H37C H 0.8966 -0.1438 1.0038 0.047 Uiso 1 1 calc R . . C38 C 1.3167(2) -0.19364(12) 0.85484(14) 0.0388(5) Uani 1 1 d . . . H38A H 1.2901 -0.2191 0.8025 0.058 Uiso 1 1 calc R . . H38B H 1.3162 -0.2309 0.8987 0.058 Uiso 1 1 calc R . . H38C H 1.4135 -0.1715 0.8569 0.058 Uiso 1 1 calc R . . C41 C 0.6130(2) 0.20539(12) 0.89101(15) 0.0414(5) Uani 1 1 d . . . H41A H 0.6103 0.2303 0.8375 0.050 Uiso 1 1 calc R . . H41B H 0.6586 0.2408 0.9333 0.050 Uiso 1 1 calc R . . C42 C 0.4639(3) 0.18442(16) 0.9066(2) 0.0668(8) Uani 1 1 d . . . H42A H 0.4269 0.2222 0.9430 0.080 Uiso 1 1 calc R . . H42B H 0.3971 0.1825 0.8552 0.080 Uiso 1 1 calc R . . C43 C 0.4767(3) 0.10739(15) 0.94568(19) 0.0544(6) Uani 1 1 d . . . H43A H 0.4922 0.1121 1.0055 0.065 Uiso 1 1 calc R . . H43B H 0.3885 0.0767 0.9295 0.065 Uiso 1 1 calc R . . C44 C 0.6035(3) 0.07195(14) 0.91595(18) 0.0533(6) Uani 1 1 d . . . H44A H 0.6579 0.0405 0.9591 0.064 Uiso 1 1 calc R . . H44B H 0.5722 0.0388 0.8687 0.064 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 0.0253(3) 0.0216(3) 0.0270(3) 0.0012(2) 0.0089(2) 0.0017(2) O1 0.0255(6) 0.0314(7) 0.0313(7) 0.0005(5) 0.0083(5) 0.0011(5) O2 0.0338(7) 0.0248(6) 0.0357(7) -0.0042(5) 0.0147(6) -0.0025(5) O3 0.0297(7) 0.0266(6) 0.0300(7) 0.0040(5) 0.0121(5) 0.0044(5) O4 0.0313(7) 0.0264(6) 0.0383(7) 0.0024(5) 0.0162(6) 0.0035(5) N1 0.0233(7) 0.0194(7) 0.0241(7) 0.0000(5) 0.0047(6) 0.0001(6) C1 0.0263(9) 0.0230(8) 0.0301(9) 0.0015(7) 0.0045(7) -0.0045(7) C2 0.0248(9) 0.0262(9) 0.0412(11) 0.0018(8) 0.0024(8) -0.0038(8) C3 0.0293(10) 0.0348(10) 0.0386(11) 0.0015(8) -0.0046(8) -0.0043(8) C4 0.0363(11) 0.0334(10) 0.0317(10) -0.0001(8) -0.0012(8) -0.0077(9) C5 0.0309(10) 0.0258(9) 0.0314(10) -0.0015(7) 0.0069(8) -0.0061(8) C6 0.0276(9) 0.0199(8) 0.0301(9) 0.0003(7) 0.0039(7) -0.0046(7) C9 0.0290(9) 0.0225(8) 0.0262(9) -0.0021(7) 0.0071(7) 0.0002(7) C7 0.0274(10) 0.0425(12) 0.0545(14) -0.0021(10) 0.0047(9) 0.0006(9) C8 0.0502(14) 0.0582(14) 0.0334(12) -0.0061(10) -0.0043(10) -0.0025(11) C21 0.0272(9) 0.0200(8) 0.0318(10) 0.0022(7) 0.0050(7) 0.0024(7) C22 0.0330(10) 0.0213(8) 0.0313(10) -0.0003(7) 0.0040(8) 0.0071(8) C23 0.0305(10) 0.0202(8) 0.0355(10) -0.0011(7) -0.0005(8) 0.0022(7) C24 0.0247(9) 0.0227(9) 0.0379(11) 0.0041(7) 0.0001(8) 0.0008(7) C25 0.0262(9) 0.0238(9) 0.0299(9) 0.0033(7) 0.0047(7) 0.0027(7) C26 0.0257(9) 0.0201(8) 0.0282(9) 0.0026(7) 0.0028(7) 0.0021(7) C27 0.0513(13) 0.0300(10) 0.0395(12) -0.0094(8) 0.0148(10) -0.0017(9) C28 0.0378(11) 0.0391(11) 0.0480(13) -0.0009(9) 0.0058(10) -0.0122(9) C31 0.0273(9) 0.0235(8) 0.0225(8) -0.0021(7) 0.0035(7) 0.0028(7) C32 0.0304(9) 0.0263(9) 0.0219(9) -0.0001(7) 0.0044(7) 0.0000(7) C33 0.0328(10) 0.0236(9) 0.0308(10) 0.0024(7) 0.0044(8) 0.0000(8) C34 0.0308(10) 0.0253(9) 0.0311(10) -0.0010(7) 0.0029(8) 0.0032(8) C35 0.0265(9) 0.0259(9) 0.0279(9) -0.0007(7) 0.0062(7) 0.0015(7) C36 0.0266(9) 0.0241(8) 0.0228(9) 0.0001(7) 0.0033(7) -0.0002(7) C39 0.0227(9) 0.0253(9) 0.0276(9) 0.0017(7) 0.0063(7) 0.0012(7) C37 0.0355(10) 0.0300(9) 0.0295(10) 0.0043(7) 0.0087(8) 0.0002(8) C38 0.0403(11) 0.0276(10) 0.0503(13) 0.0034(9) 0.0127(10) 0.0076(9) C41 0.0414(12) 0.0326(10) 0.0540(13) -0.0006(9) 0.0204(10) 0.0097(9) C42 0.0379(13) 0.0544(16) 0.112(2) 0.0195(15) 0.0264(15) 0.0124(12) C43 0.0366(12) 0.0527(14) 0.0790(18) 0.0015(13) 0.0260(12) -0.0007(11) C44 0.0513(14) 0.0372(12) 0.0804(18) 0.0055(12) 0.0420(13) -0.0029(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O3 1.7528(13) . ? Al1 O2 1.7582(14) . ? Al1 O1 1.7704(14) . ? Al1 O4 1.9552(14) . ? Al1 N1 2.0645(16) . ? O1 C1 1.354(2) . ? O2 C21 1.353(2) . ? O3 C31 1.351(2) . ? O4 C44 1.448(3) . ? O4 C41 1.461(2) . ? N1 C39 1.492(2) . ? N1 C9 1.495(2) . ? N1 C29 1.498(2) . ? C1 C6 1.398(3) . ? C1 C2 1.405(3) . ? C2 C3 1.395(3) . ? C2 C7 1.502(3) . ? C3 C4 1.392(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 C8 1.506(3) . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 C9 1.500(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C21 C26 1.401(3) . ? C21 C22 1.412(3) . ? C22 C23 1.389(3) . ? C22 C27 1.501(3) . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 C25 1.393(3) . ? C24 C28 1.507(3) . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C29 1.503(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C31 C32 1.405(2) . ? C31 C36 1.404(3) . ? C32 C33 1.391(3) . ? C32 C37 1.505(3) . ? C33 C34 1.392(3) . ? C33 H33 0.9500 . ? C34 C35 1.395(3) . ? C34 C38 1.507(3) . ? C35 C36 1.389(3) . ? C35 H35 0.9500 . ? C36 C39 1.506(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C41 C42 1.497(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.495(4) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.480(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Al1 O2 119.77(7) . . ? O3 Al1 O1 119.14(7) . . ? O2 Al1 O1 120.71(7) . . ? O3 Al1 O4 88.25(6) . . ? O2 Al1 O4 87.71(6) . . ? O1 Al1 O4 87.92(6) . . ? O3 Al1 N1 92.44(6) . . ? O2 Al1 N1 91.89(6) . . ? O1 Al1 N1 91.80(6) . . ? O4 Al1 N1 179.31(6) . . ? C1 O1 Al1 133.36(12) . . ? C21 O2 Al1 133.71(12) . . ? C31 O3 Al1 133.81(11) . . ? C44 O4 C41 109.57(16) . . ? C44 O4 Al1 120.97(12) . . ? C41 O4 Al1 121.17(12) . . ? C39 N1 C9 108.98(13) . . ? C39 N1 C29 109.69(13) . . ? C9 N1 C29 109.07(13) . . ? C39 N1 Al1 109.03(10) . . ? C9 N1 Al1 109.91(11) . . ? C29 N1 Al1 110.15(11) . . ? O1 C1 C6 121.48(16) . . ? O1 C1 C2 119.04(17) . . ? C6 C1 C2 119.48(17) . . ? C3 C2 C1 118.76(18) . . ? C3 C2 C7 121.56(18) . . ? C1 C2 C7 119.68(18) . . ? C4 C3 C2 122.64(18) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C5 C4 C3 117.37(18) . . ? C5 C4 C8 120.8(2) . . ? C3 C4 C8 121.85(19) . . ? C4 C5 C6 121.98(18) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.76(17) . . ? C5 C6 C9 119.95(17) . . ? C1 C6 C9 120.29(16) . . ? N1 C9 C6 112.56(14) . . ? N1 C9 H9A 109.1 . . ? C6 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? C6 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C21 C26 121.77(16) . . ? O2 C21 C22 118.83(16) . . ? C26 C21 C22 119.39(17) . . ? C23 C22 C21 118.62(17) . . ? C23 C22 C27 121.18(17) . . ? C21 C22 C27 120.20(17) . . ? C22 C23 C24 122.81(17) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C23 C24 C25 117.46(17) . . ? C23 C24 C28 121.58(17) . . ? C25 C24 C28 120.95(18) . . ? C26 C25 C24 121.74(17) . . ? C26 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C25 C26 C21 119.85(16) . . ? C25 C26 C29 119.69(16) . . ? C21 C26 C29 120.38(16) . . ? N1 C29 C26 113.29(14) . . ? N1 C29 H29A 108.9 . . ? C26 C29 H29A 108.9 . . ? N1 C29 H29B 108.9 . . ? C26 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O3 C31 C32 119.06(16) . . ? O3 C31 C36 121.28(16) . . ? C32 C31 C36 119.66(16) . . ? C33 C32 C31 118.51(17) . . ? C33 C32 C37 121.33(17) . . ? C31 C32 C37 120.16(17) . . ? C34 C33 C32 122.82(17) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C33 C34 C35 117.55(17) . . ? C33 C34 C38 121.44(17) . . ? C35 C34 C38 120.98(18) . . ? C36 C35 C34 121.45(18) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C31 119.87(16) . . ? C35 C36 C39 120.33(16) . . ? C31 C36 C39 119.79(16) . . ? N1 C39 C36 112.89(14) . . ? N1 C39 H39A 109.0 . . ? C36 C39 H39A 109.0 . . ? N1 C39 H39B 109.0 . . ? C36 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C41 C42 105.70(18) . . ? O4 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? O4 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.7 . . ? C43 C42 C41 106.0(2) . . ? C43 C42 H42A 110.5 . . ? C41 C42 H42A 110.5 . . ? C43 C42 H42B 110.5 . . ? C41 C42 H42B 110.5 . . ? H42A C42 H42B 108.7 . . ? C44 C43 C42 104.7(2) . . ? C44 C43 H43A 110.8 . . ? C42 C43 H43A 110.8 . . ? C44 C43 H43B 110.8 . . ? C42 C43 H43B 110.8 . . ? H43A C43 H43B 108.9 . . ? O4 C44 C43 107.01(19) . . ? O4 C44 H44A 110.3 . . ? C43 C44 H44A 110.3 . . ? O4 C44 H44B 110.3 . . ? C43 C44 H44B 110.3 . . ? H44A C44 H44B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.417 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.045