# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_c1 _database_code_depnum_ccdc_archive 'CCDC 885173' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H58 Al N O' _chemical_formula_weight 739.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.403(2) _cell_length_b 12.914(3) _cell_length_c 17.170(3) _cell_angle_alpha 102.93(3) _cell_angle_beta 90.60(3) _cell_angle_gamma 94.86(3) _cell_volume 2239.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2600 _exptl_crystal_size_min 0.2200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.098 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8200 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 20071 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10186 _reflns_number_gt 8860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (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^)+(0.0847P)^2^+0.9406P] 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 10186 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0899 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _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 0.59456(6) 0.66117(5) 0.30311(4) 0.02794(17) Uani 1 1 d . . . O1 O 0.65692(14) 0.70175(13) 0.40261(9) 0.0319(4) Uani 1 1 d . . . N1 N 0.76123(16) 0.68872(13) 0.25539(10) 0.0235(3) Uani 1 1 d . . . C11 C 0.77998(19) 0.61647(16) 0.11059(12) 0.0243(4) Uani 1 1 d . . . C1 C 0.88054(19) 0.68975(16) 0.37929(12) 0.0250(4) Uani 1 1 d . . . C2 C 0.7755(2) 0.70154(17) 0.43117(12) 0.0261(4) Uani 1 1 d . . . C7 C 0.86819(19) 0.69121(16) 0.29614(12) 0.0246(4) Uani 1 1 d . . . H7A H 0.9444 0.6942 0.2686 0.029 Uiso 1 1 calc R . . C10 C 0.77233(18) 0.70423(16) 0.17438(11) 0.0235(4) Uani 1 1 d . . . C14 C 0.7844(2) 0.82261(18) 0.08470(13) 0.0297(5) Uani 1 1 d . . . H14A H 0.7844 0.8912 0.0761 0.036 Uiso 1 1 calc R . . C13 C 0.7927(2) 0.73757(18) 0.01953(12) 0.0274(4) Uani 1 1 d . . . C3 C 0.8011(2) 0.71773(17) 0.51470(12) 0.0281(4) Uani 1 1 d . . . C15 C 0.7761(2) 0.80813(17) 0.16239(12) 0.0263(4) Uani 1 1 d . . . C6 C 1.0066(2) 0.68653(17) 0.40913(12) 0.0276(4) Uani 1 1 d . . . H6A H 1.0739 0.6773 0.3737 0.033 Uiso 1 1 calc R . . C16 C 0.79190(19) 0.50660(16) 0.12723(12) 0.0248(4) Uani 1 1 d . . . H16A H 0.7327 0.5008 0.1704 0.030 Uiso 1 1 calc R . . C18 C 0.7484(2) 0.41369(17) 0.05727(12) 0.0265(4) Uani 1 1 d . . . C5 C 1.0324(2) 0.69668(17) 0.48893(13) 0.0282(4) Uani 1 1 d . . . C4 C 0.9267(2) 0.71408(19) 0.53987(13) 0.0314(5) Uani 1 1 d . . . H4A H 0.9431 0.7238 0.5945 0.038 Uiso 1 1 calc R . . C12 C 0.7907(2) 0.63528(17) 0.03380(12) 0.0264(4) Uani 1 1 d . . . H12A H 0.7968 0.5777 -0.0092 0.032 Uiso 1 1 calc R . . C24 C 0.9266(2) 0.50093(16) 0.16077(12) 0.0265(4) Uani 1 1 d . . . C25 C 1.0361(2) 0.54951(18) 0.13295(13) 0.0325(5) Uani 1 1 d . . . H25A H 1.0280 0.5830 0.0908 0.039 Uiso 1 1 calc R . . C42 C 0.8028(2) 0.75197(19) -0.06584(13) 0.0346(5) Uani 1 1 d . . . H42A H 0.8573 0.6981 -0.0939 0.042 Uiso 1 1 calc R . . C49 C 1.1674(2) 0.6905(2) 0.52332(13) 0.0340(5) Uani 1 1 d . . . C17 C 0.7885(2) 0.90324(17) 0.23466(12) 0.0282(4) Uani 1 1 d . . . H17A H 0.7293 0.8852 0.2746 0.034 Uiso 1 1 calc R . . C19 C 0.6223(2) 0.40439(19) 0.02716(14) 0.0346(5) Uani 1 1 d . . . H19A H 0.5683 0.4572 0.0476 0.041 Uiso 1 1 calc R . . C45 C 0.6899(2) 0.7356(2) 0.57340(13) 0.0374(6) Uani 1 1 d . . . C36 C 0.9247(2) 0.91599(17) 0.27182(13) 0.0317(5) Uani 1 1 d . . . C23 C 0.8271(2) 0.33433(18) 0.02546(13) 0.0323(5) Uani 1 1 d . . . H23A H 0.9123 0.3395 0.0439 0.039 Uiso 1 1 calc R . . C29 C 0.9420(2) 0.45123(19) 0.22373(14) 0.0337(5) Uani 1 1 d . . . H29A H 0.8704 0.4180 0.2430 0.040 Uiso 1 1 calc R . . C30 C 0.7469(2) 1.00524(18) 0.21487(13) 0.0338(5) Uani 1 1 d . . . C9 C 0.4705(2) 0.7566(2) 0.27978(16) 0.0433(6) Uani 1 1 d . . . H9A H 0.5068 0.8292 0.2965 0.065 Uiso 1 1 calc R . . H9B H 0.3928 0.7470 0.3080 0.065 Uiso 1 1 calc R . . H9C H 0.4510 0.7404 0.2234 0.065 Uiso 1 1 calc R . . C26 C 1.1569(2) 0.5484(2) 0.16740(15) 0.0396(6) Uani 1 1 d . . . H26A H 1.2290 0.5810 0.1480 0.048 Uiso 1 1 calc R . . C21 C 0.6548(3) 0.2388(2) -0.06275(15) 0.0427(6) Uani 1 1 d . . . H21A H 0.6236 0.1802 -0.1024 0.051 Uiso 1 1 calc R . . C28 C 1.0630(3) 0.4506(2) 0.25808(15) 0.0435(6) Uani 1 1 d . . . H28A H 1.0718 0.4172 0.3003 0.052 Uiso 1 1 calc R . . C27 C 1.1709(2) 0.4995(2) 0.23007(15) 0.0441(6) Uani 1 1 d . . . H27A H 1.2520 0.4993 0.2533 0.053 Uiso 1 1 calc R . . C37 C 0.9445(3) 0.9480(2) 0.35378(15) 0.0424(6) Uani 1 1 d . . . H37A H 0.8751 0.9665 0.3860 0.051 Uiso 1 1 calc R . . C22 C 0.7795(3) 0.2469(2) -0.03402(15) 0.0414(6) Uani 1 1 d . . . H22A H 0.8328 0.1937 -0.0544 0.050 Uiso 1 1 calc R . . C20 C 0.5754(2) 0.3182(2) -0.03251(15) 0.0411(6) Uani 1 1 d . . . H20A H 0.4910 0.3136 -0.0522 0.049 Uiso 1 1 calc R . . C8 C 0.5431(2) 0.5074(2) 0.27510(16) 0.0427(6) Uani 1 1 d . . . H8A H 0.4617 0.4933 0.2983 0.064 Uiso 1 1 calc R . . H8B H 0.6073 0.4702 0.2953 0.064 Uiso 1 1 calc R . . H8C H 0.5349 0.4834 0.2180 0.064 Uiso 1 1 calc R . . C41 C 1.0313(2) 0.8911(2) 0.22570(16) 0.0436(6) Uani 1 1 d . . . H41A H 1.0210 0.8714 0.1703 0.052 Uiso 1 1 calc R . . C46 C 0.6156(2) 0.8292(2) 0.56155(15) 0.0420(6) Uani 1 1 d . . . H46A H 0.5818 0.8147 0.5076 0.063 Uiso 1 1 calc R . . H46B H 0.6728 0.8934 0.5718 0.063 Uiso 1 1 calc R . . H46C H 0.5458 0.8379 0.5979 0.063 Uiso 1 1 calc R . . C31 C 0.8346(3) 1.0803(2) 0.19426(16) 0.0452(6) Uani 1 1 d . . . H31A H 0.9222 1.0706 0.1945 0.054 Uiso 1 1 calc R . . C35 C 0.6180(3) 1.0230(2) 0.21622(18) 0.0490(7) Uani 1 1 d . . . H35A H 0.5578 0.9737 0.2306 0.059 Uiso 1 1 calc R . . C40 C 1.1533(3) 0.8951(3) 0.2608(2) 0.0551(7) Uani 1 1 d . . . H40A H 1.2234 0.8769 0.2290 0.066 Uiso 1 1 calc R . . C47 C 0.7404(3) 0.7639(3) 0.66071(15) 0.0687(11) Uani 1 1 d . . . H47A H 0.7971 0.8284 0.6698 0.103 Uiso 1 1 calc R . . H47B H 0.7867 0.7070 0.6711 0.103 Uiso 1 1 calc R . . H47C H 0.6690 0.7742 0.6957 0.103 Uiso 1 1 calc R . . C44 C 0.6712(3) 0.7294(3) -0.10819(17) 0.0609(9) Uani 1 1 d . . . H44A H 0.6337 0.6604 -0.1039 0.091 Uiso 1 1 calc R . . H44B H 0.6805 0.7305 -0.1636 0.091 Uiso 1 1 calc R . . H44C H 0.6162 0.7829 -0.0839 0.091 Uiso 1 1 calc R . . C39 C 1.1703(3) 0.9257(2) 0.3423(2) 0.0552(7) Uani 1 1 d . . . H39A H 1.2518 0.9279 0.3658 0.066 Uiso 1 1 calc R . . C52 C 1.2667(3) 0.6712(3) 0.45746(18) 0.0582(8) Uani 1 1 d . . . H52A H 1.2702 0.7283 0.4299 0.087 Uiso 1 1 calc R . . H52B H 1.2421 0.6049 0.4203 0.087 Uiso 1 1 calc R . . H52C H 1.3501 0.6684 0.4810 0.087 Uiso 1 1 calc R . . C38 C 1.0672(3) 0.9530(2) 0.38876(18) 0.0560(8) Uani 1 1 d . . . H38A H 1.0788 0.9749 0.4440 0.067 Uiso 1 1 calc R . . C48 C 0.5980(3) 0.6334(3) 0.55959(19) 0.0556(8) Uani 1 1 d . . . H48A H 0.5666 0.6152 0.5050 0.083 Uiso 1 1 calc R . . H48B H 0.5266 0.6449 0.5945 0.083 Uiso 1 1 calc R . . H48C H 0.6433 0.5763 0.5706 0.083 Uiso 1 1 calc R . . C32 C 0.7930(4) 1.1701(2) 0.17312(19) 0.0582(8) Uani 1 1 d . . . H32A H 0.8529 1.2195 0.1584 0.070 Uiso 1 1 calc R . . C33 C 0.6654(4) 1.1865(2) 0.1738(2) 0.0651(9) Uani 1 1 d . . . H33A H 0.6380 1.2463 0.1591 0.078 Uiso 1 1 calc R . . C43 C 0.8667(4) 0.8601(3) -0.07179(18) 0.0676(10) Uani 1 1 d . . . H43A H 0.8703 0.8638 -0.1269 0.101 Uiso 1 1 calc R . . H43B H 0.9526 0.8694 -0.0488 0.101 Uiso 1 1 calc R . . H43C H 0.8174 0.9153 -0.0433 0.101 Uiso 1 1 calc R . . C34 C 0.5771(4) 1.1138(3) 0.1963(2) 0.0674(9) Uani 1 1 d . . . H34A H 0.4901 1.1255 0.1982 0.081 Uiso 1 1 calc R . . C51 C 1.1654(3) 0.5982(3) 0.5650(3) 0.0781(12) Uani 1 1 d . . . H51A H 1.1039 0.6079 0.6067 0.117 Uiso 1 1 calc R . . H51B H 1.2496 0.5958 0.5876 0.117 Uiso 1 1 calc R . . H51C H 1.1415 0.5324 0.5269 0.117 Uiso 1 1 calc R . . C50 C 1.2123(3) 0.7949(3) 0.5812(3) 0.0893(14) Uani 1 1 d . . . H50A H 1.1512 0.8100 0.6228 0.134 Uiso 1 1 calc R . . H50B H 1.2190 0.8514 0.5531 0.134 Uiso 1 1 calc R . . H50C H 1.2952 0.7891 0.6042 0.134 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 0.0220(3) 0.0386(4) 0.0245(3) 0.0104(3) -0.0002(2) 0.0017(3) O1 0.0223(7) 0.0483(10) 0.0260(7) 0.0098(7) 0.0009(6) 0.0043(6) N1 0.0259(8) 0.0254(8) 0.0201(8) 0.0069(7) 0.0011(6) 0.0031(6) C11 0.0212(9) 0.0281(10) 0.0241(9) 0.0076(8) -0.0002(7) 0.0017(7) C1 0.0252(10) 0.0272(10) 0.0226(9) 0.0060(8) 0.0000(8) 0.0011(8) C2 0.0254(10) 0.0289(11) 0.0247(10) 0.0080(8) -0.0007(8) 0.0018(8) C7 0.0234(9) 0.0275(10) 0.0230(9) 0.0060(8) 0.0023(7) 0.0022(8) C10 0.0211(9) 0.0309(11) 0.0202(9) 0.0087(8) 0.0009(7) 0.0038(8) C14 0.0320(11) 0.0293(11) 0.0297(11) 0.0108(9) 0.0021(8) 0.0033(8) C13 0.0266(10) 0.0345(11) 0.0236(10) 0.0110(9) 0.0009(8) 0.0037(8) C3 0.0301(11) 0.0315(11) 0.0244(10) 0.0084(9) 0.0034(8) 0.0064(8) C15 0.0264(10) 0.0285(11) 0.0251(10) 0.0077(8) 0.0016(8) 0.0046(8) C6 0.0262(10) 0.0302(11) 0.0276(10) 0.0085(9) 0.0024(8) 0.0041(8) C16 0.0241(10) 0.0266(10) 0.0249(10) 0.0079(8) 0.0031(8) 0.0030(8) C18 0.0295(10) 0.0270(10) 0.0240(10) 0.0088(8) 0.0014(8) 0.0003(8) C5 0.0273(10) 0.0306(11) 0.0273(10) 0.0073(9) -0.0014(8) 0.0046(8) C4 0.0333(11) 0.0391(12) 0.0229(10) 0.0075(9) -0.0012(8) 0.0083(9) C12 0.0285(10) 0.0295(11) 0.0211(9) 0.0049(8) 0.0009(8) 0.0050(8) C24 0.0285(10) 0.0247(10) 0.0255(10) 0.0031(8) 0.0004(8) 0.0051(8) C25 0.0319(11) 0.0348(12) 0.0311(11) 0.0078(10) 0.0024(9) 0.0044(9) C42 0.0428(13) 0.0391(13) 0.0246(10) 0.0115(10) 0.0039(9) 0.0066(10) C49 0.0271(11) 0.0445(13) 0.0297(11) 0.0057(10) -0.0054(9) 0.0071(9) C17 0.0327(11) 0.0280(11) 0.0247(10) 0.0063(9) 0.0038(8) 0.0056(8) C19 0.0297(11) 0.0375(13) 0.0354(12) 0.0061(10) -0.0002(9) 0.0031(9) C45 0.0352(12) 0.0580(16) 0.0237(10) 0.0132(11) 0.0073(9) 0.0193(11) C36 0.0356(12) 0.0259(11) 0.0328(11) 0.0050(9) -0.0004(9) 0.0023(9) C23 0.0332(11) 0.0342(12) 0.0300(11) 0.0082(9) 0.0026(9) 0.0035(9) C29 0.0362(12) 0.0357(12) 0.0320(11) 0.0128(10) -0.0005(9) 0.0054(9) C30 0.0476(14) 0.0275(11) 0.0265(11) 0.0045(9) 0.0023(9) 0.0083(10) C9 0.0318(12) 0.0614(17) 0.0417(13) 0.0197(13) 0.0026(10) 0.0114(11) C26 0.0284(11) 0.0452(14) 0.0415(13) 0.0025(11) 0.0026(10) 0.0014(10) C21 0.0489(15) 0.0393(14) 0.0337(12) -0.0015(11) -0.0042(11) -0.0044(11) C28 0.0468(15) 0.0515(15) 0.0366(13) 0.0144(12) -0.0044(11) 0.0170(12) C27 0.0321(12) 0.0576(16) 0.0396(13) 0.0005(12) -0.0059(10) 0.0152(11) C37 0.0490(15) 0.0385(14) 0.0356(13) -0.0013(11) -0.0035(11) 0.0079(11) C22 0.0492(15) 0.0339(13) 0.0378(13) -0.0005(10) 0.0040(11) 0.0075(11) C20 0.0359(13) 0.0453(14) 0.0380(13) 0.0042(11) -0.0043(10) -0.0061(10) C8 0.0348(13) 0.0488(15) 0.0435(14) 0.0130(12) 0.0064(10) -0.0086(11) C41 0.0370(13) 0.0500(15) 0.0401(13) 0.0041(12) 0.0002(10) -0.0003(11) C46 0.0376(13) 0.0512(15) 0.0352(12) 0.0012(11) 0.0015(10) 0.0159(11) C31 0.0555(16) 0.0323(13) 0.0503(15) 0.0138(12) 0.0064(12) 0.0046(11) C35 0.0493(16) 0.0430(15) 0.0611(17) 0.0215(13) 0.0063(13) 0.0134(12) C40 0.0338(14) 0.0580(18) 0.0669(19) 0.0019(15) 0.0015(13) 0.0001(12) C47 0.0593(19) 0.129(3) 0.0254(12) 0.0185(16) 0.0103(12) 0.049(2) C44 0.0530(17) 0.103(3) 0.0338(14) 0.0308(16) -0.0043(12) 0.0064(17) C39 0.0427(15) 0.0495(16) 0.0671(19) 0.0020(14) -0.0180(14) 0.0007(12) C52 0.0306(13) 0.097(3) 0.0497(16) 0.0196(16) -0.0020(11) 0.0147(14) C38 0.0614(19) 0.0538(17) 0.0449(15) -0.0042(13) -0.0192(14) 0.0044(14) C48 0.0485(16) 0.0685(19) 0.0653(19) 0.0421(16) 0.0268(14) 0.0181(14) C32 0.082(2) 0.0362(15) 0.0619(19) 0.0230(14) 0.0072(16) 0.0051(14) C33 0.097(3) 0.0393(16) 0.068(2) 0.0235(15) 0.0105(19) 0.0261(16) C43 0.106(3) 0.061(2) 0.0383(15) 0.0243(15) 0.0132(16) -0.0182(18) C34 0.067(2) 0.063(2) 0.085(2) 0.0324(19) 0.0114(18) 0.0353(17) C51 0.0414(17) 0.114(3) 0.105(3) 0.076(3) 0.0003(17) 0.0192(18) C50 0.0506(19) 0.094(3) 0.095(3) -0.041(2) -0.0354(19) 0.0199(19) _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 1.7698(17) . ? Al1 C9 1.956(3) . ? Al1 C8 1.962(3) . ? Al1 N1 1.9647(19) . ? O1 C2 1.324(2) . ? N1 C7 1.302(3) . ? N1 C10 1.453(2) . ? C11 C12 1.397(3) . ? C11 C10 1.397(3) . ? C11 C16 1.523(3) . ? C1 C6 1.411(3) . ? C1 C2 1.413(3) . ? C1 C7 1.436(3) . ? C2 C3 1.421(3) . ? C7 H7A 0.9300 . ? C10 C15 1.400(3) . ? C14 C15 1.390(3) . ? C14 C13 1.390(3) . ? C14 H14A 0.9300 . ? C13 C12 1.395(3) . ? C13 C42 1.522(3) . ? C3 C4 1.380(3) . ? C3 C45 1.540(3) . ? C15 C17 1.534(3) . ? C6 C5 1.368(3) . ? C6 H6A 0.9300 . ? C16 C24 1.523(3) . ? C16 C18 1.529(3) . ? C16 H16A 0.9800 . ? C18 C23 1.386(3) . ? C18 C19 1.391(3) . ? C5 C4 1.413(3) . ? C5 C49 1.533(3) . ? C4 H4A 0.9300 . ? C12 H12A 0.9300 . ? C24 C29 1.389(3) . ? C24 C25 1.394(3) . ? C25 C26 1.385(3) . ? C25 H25A 0.9300 . ? C42 C44 1.518(4) . ? C42 C43 1.519(4) . ? C42 H42A 0.9800 . ? C49 C50 1.518(4) . ? C49 C51 1.521(4) . ? C49 C52 1.533(4) . ? C17 C30 1.527(3) . ? C17 C36 1.529(3) . ? C17 H17A 0.9800 . ? C19 C20 1.383(3) . ? C19 H19A 0.9300 . ? C45 C48 1.533(4) . ? C45 C47 1.537(3) . ? C45 C46 1.538(3) . ? C36 C37 1.383(3) . ? C36 C41 1.387(3) . ? C23 C22 1.393(3) . ? C23 H23A 0.9300 . ? C29 C28 1.385(3) . ? C29 H29A 0.9300 . ? C30 C35 1.379(4) . ? C30 C31 1.381(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C26 C27 1.377(4) . ? C26 H26A 0.9300 . ? C21 C22 1.370(4) . ? C21 C20 1.385(4) . ? C21 H21A 0.9300 . ? C28 C27 1.384(4) . ? C28 H28A 0.9300 . ? C27 H27A 0.9300 . ? C37 C38 1.395(4) . ? C37 H37A 0.9300 . ? C22 H22A 0.9300 . ? C20 H20A 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C41 C40 1.392(4) . ? C41 H41A 0.9300 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C31 C32 1.392(4) . ? C31 H31A 0.9300 . ? C35 C34 1.391(4) . ? C35 H35A 0.9300 . ? C40 C39 1.371(4) . ? C40 H40A 0.9300 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C39 C38 1.367(5) . ? C39 H39A 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C38 H38A 0.9300 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C32 C33 1.362(5) . ? C32 H32A 0.9300 . ? C33 C34 1.378(5) . ? C33 H33A 0.9300 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C34 H34A 0.9300 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 C9 111.78(11) . . ? O1 Al1 C8 111.06(11) . . ? C9 Al1 C8 117.63(12) . . ? O1 Al1 N1 94.14(8) . . ? C9 Al1 N1 110.72(10) . . ? C8 Al1 N1 109.00(10) . . ? C2 O1 Al1 129.83(14) . . ? C7 N1 C10 117.14(17) . . ? C7 N1 Al1 119.91(14) . . ? C10 N1 Al1 122.93(13) . . ? C12 C11 C10 117.93(19) . . ? C12 C11 C16 122.05(18) . . ? C10 C11 C16 119.63(17) . . ? C6 C1 C2 120.74(18) . . ? C6 C1 C7 116.32(18) . . ? C2 C1 C7 122.66(18) . . ? O1 C2 C1 120.50(18) . . ? O1 C2 C3 120.93(18) . . ? C1 C2 C3 118.51(19) . . ? N1 C7 C1 126.69(18) . . ? N1 C7 H7A 116.7 . . ? C1 C7 H7A 116.7 . . ? C11 C10 C15 121.43(18) . . ? C11 C10 N1 119.96(18) . . ? C15 C10 N1 118.60(18) . . ? C15 C14 C13 121.9(2) . . ? C15 C14 H14A 119.0 . . ? C13 C14 H14A 119.0 . . ? C14 C13 C12 118.03(19) . . ? C14 C13 C42 122.7(2) . . ? C12 C13 C42 119.29(19) . . ? C4 C3 C2 117.62(19) . . ? C4 C3 C45 122.34(19) . . ? C2 C3 C45 120.02(19) . . ? C14 C15 C10 118.50(19) . . ? C14 C15 C17 121.37(19) . . ? C10 C15 C17 119.66(18) . . ? C5 C6 C1 121.59(19) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? C11 C16 C24 110.01(16) . . ? C11 C16 C18 114.32(17) . . ? C24 C16 C18 113.89(17) . . ? C11 C16 H16A 106.0 . . ? C24 C16 H16A 106.0 . . ? C18 C16 H16A 106.0 . . ? C23 C18 C19 118.2(2) . . ? C23 C18 C16 122.67(19) . . ? C19 C18 C16 119.00(19) . . ? C6 C5 C4 116.40(19) . . ? C6 C5 C49 123.11(19) . . ? C4 C5 C49 120.50(19) . . ? C3 C4 C5 125.0(2) . . ? C3 C4 H4A 117.5 . . ? C5 C4 H4A 117.5 . . ? C13 C12 C11 122.14(19) . . ? C13 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? C29 C24 C25 118.2(2) . . ? C29 C24 C16 119.89(19) . . ? C25 C24 C16 121.81(19) . . ? C26 C25 C24 120.8(2) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C44 C42 C43 111.4(2) . . ? C44 C42 C13 110.4(2) . . ? C43 C42 C13 113.7(2) . . ? C44 C42 H42A 107.0 . . ? C43 C42 H42A 107.0 . . ? C13 C42 H42A 107.0 . . ? C50 C49 C51 110.5(3) . . ? C50 C49 C5 110.1(2) . . ? C51 C49 C5 109.8(2) . . ? C50 C49 C52 107.3(3) . . ? C51 C49 C52 107.4(2) . . ? C5 C49 C52 111.56(19) . . ? C30 C17 C36 113.55(19) . . ? C30 C17 C15 112.73(17) . . ? C36 C17 C15 109.59(17) . . ? C30 C17 H17A 106.8 . . ? C36 C17 H17A 106.8 . . ? C15 C17 H17A 106.8 . . ? C20 C19 C18 121.3(2) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C48 C45 C47 109.2(2) . . ? C48 C45 C46 109.7(2) . . ? C47 C45 C46 106.6(2) . . ? C48 C45 C3 109.0(2) . . ? C47 C45 C3 111.5(2) . . ? C46 C45 C3 110.9(2) . . ? C37 C36 C41 117.7(2) . . ? C37 C36 C17 120.5(2) . . ? C41 C36 C17 121.7(2) . . ? C18 C23 C22 120.4(2) . . ? C18 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C28 C29 C24 120.7(2) . . ? C28 C29 H29A 119.6 . . ? C24 C29 H29A 119.6 . . ? C35 C30 C31 118.5(2) . . ? C35 C30 C17 119.5(2) . . ? C31 C30 C17 121.9(2) . . ? Al1 C9 H9A 109.5 . . ? Al1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Al1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C27 C26 C25 120.5(2) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C22 C21 C20 119.7(2) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C27 C28 C29 120.5(2) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C26 C27 C28 119.3(2) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C36 C37 C38 121.0(3) . . ? C36 C37 H37A 119.5 . . ? C38 C37 H37A 119.5 . . ? C21 C22 C23 120.6(2) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C19 C20 C21 119.7(2) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? Al1 C8 H8A 109.5 . . ? Al1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Al1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C36 C41 C40 121.2(3) . . ? C36 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? C30 C35 C34 120.7(3) . . ? C30 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C39 C40 C41 120.1(3) . . ? C39 C40 H40A 120.0 . . ? C41 C40 H40A 120.0 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C39 C40 119.7(3) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 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 C9 Al1 O1 C2 -140.78(19) . . . . ? C8 Al1 O1 C2 85.7(2) . . . . ? N1 Al1 O1 C2 -26.52(19) . . . . ? O1 Al1 N1 C7 22.08(17) . . . . ? C9 Al1 N1 C7 137.24(17) . . . . ? C8 Al1 N1 C7 -91.87(18) . . . . ? O1 Al1 N1 C10 -159.55(15) . . . . ? C9 Al1 N1 C10 -44.39(19) . . . . ? C8 Al1 N1 C10 86.50(18) . . . . ? Al1 O1 C2 C1 15.2(3) . . . . ? Al1 O1 C2 C3 -167.57(16) . . . . ? C6 C1 C2 O1 -178.24(19) . . . . ? C7 C1 C2 O1 8.2(3) . . . . ? C6 C1 C2 C3 4.4(3) . . . . ? C7 C1 C2 C3 -169.16(19) . . . . ? C10 N1 C7 C1 172.57(19) . . . . ? Al1 N1 C7 C1 -9.0(3) . . . . ? C6 C1 C7 N1 176.28(19) . . . . ? C2 C1 C7 N1 -9.9(3) . . . . ? C12 C11 C10 C15 -0.4(3) . . . . ? C16 C11 C10 C15 172.61(18) . . . . ? C12 C11 C10 N1 -179.91(18) . . . . ? C16 C11 C10 N1 -6.9(3) . . . . ? C7 N1 C10 C11 89.8(2) . . . . ? Al1 N1 C10 C11 -88.6(2) . . . . ? C7 N1 C10 C15 -89.7(2) . . . . ? Al1 N1 C10 C15 91.9(2) . . . . ? C15 C14 C13 C12 0.8(3) . . . . ? C15 C14 C13 C42 -179.5(2) . . . . ? O1 C2 C3 C4 178.6(2) . . . . ? C1 C2 C3 C4 -4.1(3) . . . . ? O1 C2 C3 C45 0.2(3) . . . . ? C1 C2 C3 C45 177.5(2) . . . . ? C13 C14 C15 C10 -1.9(3) . . . . ? C13 C14 C15 C17 170.3(2) . . . . ? C11 C10 C15 C14 1.7(3) . . . . ? N1 C10 C15 C14 -178.85(18) . . . . ? C11 C10 C15 C17 -170.61(18) . . . . ? N1 C10 C15 C17 8.9(3) . . . . ? C2 C1 C6 C5 -1.3(3) . . . . ? C7 C1 C6 C5 172.7(2) . . . . ? C12 C11 C16 C24 100.1(2) . . . . ? C10 C11 C16 C24 -72.7(2) . . . . ? C12 C11 C16 C18 -29.5(3) . . . . ? C10 C11 C16 C18 157.71(18) . . . . ? C11 C16 C18 C23 125.0(2) . . . . ? C24 C16 C18 C23 -2.6(3) . . . . ? C11 C16 C18 C19 -58.9(3) . . . . ? C24 C16 C18 C19 173.41(19) . . . . ? C1 C6 C5 C4 -2.0(3) . . . . ? C1 C6 C5 C49 178.3(2) . . . . ? C2 C3 C4 C5 0.8(3) . . . . ? C45 C3 C4 C5 179.2(2) . . . . ? C6 C5 C4 C3 2.3(3) . . . . ? C49 C5 C4 C3 -178.0(2) . . . . ? C14 C13 C12 C11 0.5(3) . . . . ? C42 C13 C12 C11 -179.2(2) . . . . ? C10 C11 C12 C13 -0.7(3) . . . . ? C16 C11 C12 C13 -173.51(19) . . . . ? C11 C16 C24 C29 138.3(2) . . . . ? C18 C16 C24 C29 -91.9(2) . . . . ? C11 C16 C24 C25 -38.2(3) . . . . ? C18 C16 C24 C25 91.6(2) . . . . ? C29 C24 C25 C26 -0.2(3) . . . . ? C16 C24 C25 C26 176.3(2) . . . . ? C14 C13 C42 C44 -97.8(3) . . . . ? C12 C13 C42 C44 81.8(3) . . . . ? C14 C13 C42 C43 28.1(3) . . . . ? C12 C13 C42 C43 -152.2(3) . . . . ? C6 C5 C49 C50 118.7(3) . . . . ? C4 C5 C49 C50 -61.0(3) . . . . ? C6 C5 C49 C51 -119.3(3) . . . . ? C4 C5 C49 C51 61.0(3) . . . . ? C6 C5 C49 C52 -0.3(3) . . . . ? C4 C5 C49 C52 180.0(2) . . . . ? C14 C15 C17 C30 27.1(3) . . . . ? C10 C15 C17 C30 -160.86(19) . . . . ? C14 C15 C17 C36 -100.4(2) . . . . ? C10 C15 C17 C36 71.6(2) . . . . ? C23 C18 C19 C20 0.5(3) . . . . ? C16 C18 C19 C20 -175.7(2) . . . . ? C4 C3 C45 C48 -112.5(3) . . . . ? C2 C3 C45 C48 65.9(3) . . . . ? C4 C3 C45 C47 8.1(4) . . . . ? C2 C3 C45 C47 -173.5(2) . . . . ? C4 C3 C45 C46 126.7(2) . . . . ? C2 C3 C45 C46 -55.0(3) . . . . ? C30 C17 C36 C37 89.3(3) . . . . ? C15 C17 C36 C37 -143.7(2) . . . . ? C30 C17 C36 C41 -94.0(3) . . . . ? C15 C17 C36 C41 33.1(3) . . . . ? C19 C18 C23 C22 -1.2(3) . . . . ? C16 C18 C23 C22 174.9(2) . . . . ? C25 C24 C29 C28 0.4(3) . . . . ? C16 C24 C29 C28 -176.3(2) . . . . ? C36 C17 C30 C35 -150.7(2) . . . . ? C15 C17 C30 C35 83.9(3) . . . . ? C36 C17 C30 C31 30.3(3) . . . . ? C15 C17 C30 C31 -95.1(3) . . . . ? C24 C25 C26 C27 -0.2(4) . . . . ? C24 C29 C28 C27 -0.1(4) . . . . ? C25 C26 C27 C28 0.4(4) . . . . ? C29 C28 C27 C26 -0.3(4) . . . . ? C41 C36 C37 C38 -1.2(4) . . . . ? C17 C36 C37 C38 175.6(2) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C18 C23 C22 C21 0.9(4) . . . . ? C18 C19 C20 C21 0.5(4) . . . . ? C22 C21 C20 C19 -0.8(4) . . . . ? C37 C36 C41 C40 1.9(4) . . . . ? C17 C36 C41 C40 -174.9(2) . . . . ? C35 C30 C31 C32 -1.8(4) . . . . ? C17 C30 C31 C32 177.2(2) . . . . ? C31 C30 C35 C34 0.8(4) . . . . ? C17 C30 C35 C34 -178.2(3) . . . . ? C36 C41 C40 C39 -1.1(4) . . . . ? C41 C40 C39 C38 -0.4(5) . . . . ? C40 C39 C38 C37 1.1(5) . . . . ? C36 C37 C38 C39 -0.2(4) . . . . ? C30 C31 C32 C33 1.2(5) . . . . ? C31 C32 C33 C34 0.6(5) . . . . ? C32 C33 C34 C35 -1.7(5) . . . . ? C30 C35 C34 C33 1.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.415 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.114 data_c5 _database_code_depnum_ccdc_archive 'CCDC 885174' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H52 Al N O' _chemical_formula_weight 697.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.114(2) _cell_length_b 15.129(3) _cell_length_c 23.294(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.69(3) _cell_angle_gamma 90.00 _cell_volume 4208.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9894 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.2200 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.6898 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 19583 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9525 _reflns_number_gt 8446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (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^)+(0.0774P)^2^+1.9312P] 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 9894 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1978 _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_restrained_S_all 1.236 _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 0.67234(6) 0.08331(5) 0.18166(3) 0.03293(19) Uani 1 1 d . . . N1 N 0.65746(15) -0.01693(12) 0.23371(8) 0.0278(4) Uani 1 1 d . . . O1 O 0.71362(17) 0.01593(12) 0.12680(8) 0.0436(5) Uani 1 1 d . . . C10 C 0.59485(18) -0.01713(14) 0.28207(10) 0.0270(4) Uani 1 1 d . . . C15 C 0.48069(19) -0.03743(14) 0.27000(10) 0.0293(5) Uani 1 1 d . . . C14 C 0.42239(19) -0.04418(16) 0.31677(10) 0.0324(5) Uani 1 1 d . . . H14A H 0.3450 -0.0587 0.3093 0.039 Uiso 1 1 calc R . . C16 C 0.77500(19) 0.02199(15) 0.35030(10) 0.0296(5) Uani 1 1 d . . . H16A H 0.7893 0.0555 0.3153 0.036 Uiso 1 1 calc R . . C1 C 0.76296(19) -0.11674(15) 0.17970(10) 0.0311(5) Uani 1 1 d . . . C7 C 0.70692(18) -0.09207(15) 0.22675(10) 0.0295(5) Uani 1 1 d . . . H7A H 0.7055 -0.1352 0.2563 0.035 Uiso 1 1 calc R . . C36 C 0.45891(19) -0.13670(15) 0.18063(11) 0.0324(5) Uani 1 1 d . . . C30 C 0.2956(2) -0.03969(16) 0.19929(10) 0.0329(5) Uani 1 1 d . . . C18 C 0.80735(19) 0.08450(15) 0.40217(10) 0.0309(5) Uani 1 1 d . . . C12 C 0.5880(2) -0.00664(16) 0.38418(10) 0.0329(5) Uani 1 1 d . . . H12A H 0.6238 0.0053 0.4229 0.039 Uiso 1 1 calc R . . C2 C 0.7580(2) -0.06433(16) 0.12905(11) 0.0348(5) Uani 1 1 d . . . C24 C 0.84748(19) -0.06091(16) 0.35315(10) 0.0322(5) Uani 1 1 d . . . C17 C 0.42278(19) -0.05109(15) 0.20683(10) 0.0292(5) Uani 1 1 d . . . H17A H 0.4501 -0.0022 0.1840 0.035 Uiso 1 1 calc R . . C13 C 0.4752(2) -0.03011(16) 0.37417(10) 0.0342(5) Uani 1 1 d . . . C6 C 0.8138(2) -0.20076(16) 0.18307(11) 0.0354(5) Uani 1 1 d . . . H6A H 0.8169 -0.2349 0.2175 0.042 Uiso 1 1 calc R . . C29 C 0.8174(2) -0.14010(17) 0.37656(12) 0.0401(6) Uani 1 1 d . . . H29A H 0.7506 -0.1433 0.3928 0.048 Uiso 1 1 calc R . . C11 C 0.64994(19) -0.00024(14) 0.33908(10) 0.0294(5) Uani 1 1 d . . . C23 C 0.8735(2) 0.06002(18) 0.45431(11) 0.0399(6) Uani 1 1 d . . . H23A H 0.8989 0.0007 0.4596 0.048 Uiso 1 1 calc R . . C5 C 0.8589(2) -0.23385(17) 0.13732(12) 0.0400(6) Uani 1 1 d . . . C3 C 0.7985(2) -0.09986(18) 0.07991(11) 0.0401(6) Uani 1 1 d . . . C37 C 0.4779(2) -0.13618(19) 0.12335(12) 0.0444(6) Uani 1 1 d . . . H37A H 0.4654 -0.0834 0.1011 0.053 Uiso 1 1 calc R . . C41 C 0.4776(2) -0.21433(16) 0.21241(13) 0.0416(6) Uani 1 1 d . . . H41A H 0.4651 -0.2163 0.2516 0.050 Uiso 1 1 calc R . . C22 C 0.9030(2) 0.12102(19) 0.49886(12) 0.0472(7) Uani 1 1 d . . . H22A H 0.9481 0.1029 0.5343 0.057 Uiso 1 1 calc R . . C42 C 0.4126(2) -0.0396(2) 0.42522(11) 0.0451(6) Uani 1 1 d . . . H42A H 0.4515 0.0002 0.4565 0.054 Uiso 1 1 calc R . . C27 C 0.9809(2) -0.2114(2) 0.35266(13) 0.0485(7) Uani 1 1 d . . . H27A H 1.0261 -0.2627 0.3524 0.058 Uiso 1 1 calc R . . C4 C 0.8482(2) -0.18248(19) 0.08650(12) 0.0436(6) Uani 1 1 d . . . H4A H 0.8772 -0.2061 0.0543 0.052 Uiso 1 1 calc R . . C25 C 0.9456(2) -0.05896(18) 0.32957(12) 0.0417(6) Uani 1 1 d . . . H25A H 0.9677 -0.0056 0.3133 0.050 Uiso 1 1 calc R . . C9 C 0.5318(2) 0.14488(18) 0.15128(14) 0.0477(7) Uani 1 1 d . . . H9A H 0.5470 0.1935 0.1259 0.072 Uiso 1 1 calc R . . H9B H 0.4990 0.1685 0.1838 0.072 Uiso 1 1 calc R . . H9C H 0.4792 0.1033 0.1289 0.072 Uiso 1 1 calc R . . C21 C 0.8676(2) 0.20727(18) 0.49218(13) 0.0462(7) Uani 1 1 d . . . H21A H 0.8891 0.2491 0.5224 0.055 Uiso 1 1 calc R . . C26 C 1.0116(2) -0.1339(2) 0.32946(13) 0.0485(7) Uani 1 1 d . . . H26A H 1.0784 -0.1314 0.3132 0.058 Uiso 1 1 calc R . . C28 C 0.8844(3) -0.21471(18) 0.37644(13) 0.0489(7) Uani 1 1 d . . . H28A H 0.8634 -0.2683 0.3929 0.059 Uiso 1 1 calc R . . C49 C 0.9189(3) -0.3221(2) 0.14103(16) 0.0572(8) Uani 1 1 d . . . H49A H 0.9179 -0.3486 0.1793 0.086 Uiso 1 1 calc R . . H49B H 0.9966 -0.3132 0.1356 0.086 Uiso 1 1 calc R . . H49C H 0.8810 -0.3616 0.1106 0.086 Uiso 1 1 calc R . . C19 C 0.7707(2) 0.17125(18) 0.39653(13) 0.0462(7) Uani 1 1 d . . . H19A H 0.7242 0.1894 0.3615 0.055 Uiso 1 1 calc R . . C8 C 0.7944(3) 0.1605(2) 0.21887(14) 0.0539(8) Uani 1 1 d . . . H8A H 0.8022 0.2106 0.1932 0.081 Uiso 1 1 calc R . . H8B H 0.8646 0.1270 0.2260 0.081 Uiso 1 1 calc R . . H8C H 0.7772 0.1824 0.2560 0.081 Uiso 1 1 calc R . . C32 C 0.1366(2) 0.0577(2) 0.19821(14) 0.0539(8) Uani 1 1 d . . . H32A H 0.1082 0.1155 0.2019 0.065 Uiso 1 1 calc R . . C45 C 0.7882(3) -0.0469(2) 0.02325(13) 0.0594(9) Uani 1 1 d . . . C31 C 0.2510(2) 0.04434(19) 0.20328(14) 0.0468(7) Uani 1 1 d . . . H31A H 0.3000 0.0937 0.2096 0.056 Uiso 1 1 calc R . . C20 C 0.8004(3) 0.23234(19) 0.44094(14) 0.0538(8) Uani 1 1 d . . . H20A H 0.7744 0.2915 0.4360 0.065 Uiso 1 1 calc R . . C39 C 0.5331(3) -0.2877(2) 0.12999(18) 0.0623(9) Uani 1 1 d . . . H39A H 0.5583 -0.3393 0.1129 0.075 Uiso 1 1 calc R . . C38 C 0.5148(3) -0.2114(2) 0.09797(15) 0.0579(8) Uani 1 1 d . . . H38A H 0.5273 -0.2099 0.0588 0.069 Uiso 1 1 calc R . . C35 C 0.2212(2) -0.1091(2) 0.18944(16) 0.0574(8) Uani 1 1 d . . . H35A H 0.2488 -0.1675 0.1865 0.069 Uiso 1 1 calc R . . C40 C 0.5150(3) -0.28985(18) 0.18674(17) 0.0555(8) Uani 1 1 d . . . H40A H 0.5279 -0.3429 0.2086 0.067 Uiso 1 1 calc R . . C33 C 0.0645(2) -0.0124(3) 0.18789(15) 0.0610(9) Uani 1 1 d . . . H33A H -0.0140 -0.0034 0.1837 0.073 Uiso 1 1 calc R . . C34 C 0.1066(3) -0.0952(3) 0.1837(2) 0.0766(12) Uani 1 1 d . . . H34A H 0.0569 -0.1441 0.1768 0.092 Uiso 1 1 calc R . . C47 C 0.6648(4) -0.0248(3) 0.00043(16) 0.0897(14) Uani 1 1 d . . . H47A H 0.6347 0.0106 0.0295 0.135 Uiso 1 1 calc R . . H47B H 0.6218 -0.0797 -0.0069 0.135 Uiso 1 1 calc R . . H47C H 0.6593 0.0088 -0.0359 0.135 Uiso 1 1 calc R . . C48 C 0.8596(4) 0.0374(2) 0.03369(18) 0.0806(13) Uani 1 1 d . . . H48A H 0.8335 0.0734 0.0637 0.121 Uiso 1 1 calc R . . H48B H 0.8525 0.0714 -0.0026 0.121 Uiso 1 1 calc R . . H48C H 0.9382 0.0213 0.0466 0.121 Uiso 1 1 calc R . . C46 C 0.8304(4) -0.1008(3) -0.02480(16) 0.0838(13) Uani 1 1 d . . . H46A H 0.9091 -0.1166 -0.0120 0.126 Uiso 1 1 calc R . . H46B H 0.8234 -0.0652 -0.0604 0.126 Uiso 1 1 calc R . . H46C H 0.7856 -0.1547 -0.0326 0.126 Uiso 1 1 calc R . . C43 C 0.4236(6) -0.1304(3) 0.4496(2) 0.117(2) Uani 1 1 d . . . H43A H 0.5028 -0.1473 0.4574 0.176 Uiso 1 1 calc R . . H43B H 0.3821 -0.1717 0.4216 0.176 Uiso 1 1 calc R . . H43C H 0.3930 -0.1321 0.4860 0.176 Uiso 1 1 calc R . . C44 C 0.2918(3) -0.0077(4) 0.41180(18) 0.0966(16) Uani 1 1 d . . . H44A H 0.2563 -0.0153 0.4463 0.145 Uiso 1 1 calc R . . H44B H 0.2508 -0.0422 0.3795 0.145 Uiso 1 1 calc R . . H44C H 0.2904 0.0550 0.4010 0.145 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 0.0379(4) 0.0283(4) 0.0338(4) 0.0025(3) 0.0092(3) -0.0005(3) N1 0.0270(9) 0.0289(9) 0.0267(9) -0.0006(8) 0.0024(7) -0.0028(7) O1 0.0612(12) 0.0375(9) 0.0356(10) 0.0059(8) 0.0184(9) 0.0108(9) C10 0.0277(11) 0.0244(10) 0.0288(11) 0.0012(9) 0.0041(8) -0.0010(8) C15 0.0299(11) 0.0266(11) 0.0304(11) 0.0011(9) 0.0019(9) -0.0008(9) C14 0.0270(11) 0.0366(12) 0.0327(12) 0.0001(10) 0.0029(9) -0.0047(9) C16 0.0283(11) 0.0323(11) 0.0268(11) 0.0020(9) 0.0004(8) -0.0025(9) C1 0.0275(11) 0.0329(12) 0.0317(12) -0.0015(10) 0.0014(9) -0.0019(9) C7 0.0271(11) 0.0298(11) 0.0300(11) 0.0002(9) 0.0005(9) -0.0025(9) C36 0.0288(11) 0.0308(11) 0.0353(12) -0.0042(10) -0.0013(9) -0.0036(9) C30 0.0312(12) 0.0343(12) 0.0310(12) 0.0015(10) -0.0016(9) -0.0051(9) C18 0.0278(11) 0.0324(12) 0.0311(12) -0.0015(10) 0.0011(9) -0.0022(9) C12 0.0339(12) 0.0380(12) 0.0261(11) -0.0007(10) 0.0033(9) -0.0021(10) C2 0.0344(12) 0.0383(13) 0.0316(12) -0.0022(10) 0.0050(10) 0.0014(10) C24 0.0297(11) 0.0361(12) 0.0284(11) -0.0034(10) -0.0015(9) -0.0002(9) C17 0.0285(11) 0.0291(11) 0.0280(11) 0.0006(9) -0.0006(9) -0.0053(9) C13 0.0333(12) 0.0392(13) 0.0303(12) -0.0003(10) 0.0055(9) -0.0032(10) C6 0.0300(12) 0.0343(12) 0.0408(13) 0.0004(10) 0.0027(10) 0.0007(9) C29 0.0413(14) 0.0381(13) 0.0413(14) 0.0025(11) 0.0078(11) 0.0027(11) C11 0.0302(11) 0.0275(11) 0.0289(11) -0.0006(9) 0.0009(9) -0.0008(9) C23 0.0436(14) 0.0386(13) 0.0348(13) -0.0049(11) -0.0016(11) 0.0063(11) C5 0.0292(12) 0.0372(13) 0.0539(16) -0.0073(12) 0.0079(11) 0.0013(10) C3 0.0389(13) 0.0464(14) 0.0366(13) -0.0035(11) 0.0112(11) 0.0009(11) C37 0.0458(15) 0.0453(15) 0.0404(14) -0.0067(12) 0.0025(12) -0.0057(12) C41 0.0406(14) 0.0329(13) 0.0487(15) 0.0001(11) -0.0002(12) -0.0036(10) C22 0.0467(15) 0.0519(16) 0.0376(14) -0.0099(13) -0.0083(12) 0.0079(13) C42 0.0424(14) 0.0628(18) 0.0314(13) -0.0037(12) 0.0093(11) -0.0091(13) C27 0.0472(16) 0.0461(16) 0.0487(16) -0.0092(13) -0.0022(13) 0.0122(13) C4 0.0361(13) 0.0514(16) 0.0457(15) -0.0100(13) 0.0138(11) 0.0009(12) C25 0.0329(13) 0.0415(14) 0.0500(15) -0.0041(12) 0.0053(11) -0.0030(11) C9 0.0469(15) 0.0367(14) 0.0595(18) 0.0132(13) 0.0090(13) 0.0042(12) C21 0.0471(15) 0.0431(15) 0.0444(15) -0.0154(12) -0.0042(12) -0.0006(12) C26 0.0343(13) 0.0537(17) 0.0573(18) -0.0150(14) 0.0076(12) 0.0048(12) C28 0.0629(19) 0.0362(14) 0.0465(16) 0.0036(12) 0.0058(14) 0.0058(13) C49 0.0490(17) 0.0451(16) 0.080(2) -0.0059(16) 0.0179(16) 0.0128(13) C19 0.0506(16) 0.0369(14) 0.0443(15) -0.0021(12) -0.0121(12) 0.0021(12) C8 0.0550(17) 0.0450(16) 0.0603(19) 0.0100(14) 0.0062(14) -0.0181(14) C32 0.0395(15) 0.0593(18) 0.0618(19) 0.0120(15) 0.0058(13) 0.0120(13) C45 0.075(2) 0.071(2) 0.0372(15) 0.0074(15) 0.0227(15) 0.0167(18) C31 0.0354(14) 0.0403(14) 0.0625(18) 0.0070(13) 0.0025(12) 0.0002(11) C20 0.0605(19) 0.0368(14) 0.0569(18) -0.0094(13) -0.0104(14) 0.0053(13) C39 0.0517(18) 0.0491(18) 0.087(3) -0.0298(18) 0.0156(17) -0.0069(14) C38 0.061(2) 0.0567(19) 0.0571(19) -0.0233(16) 0.0125(15) -0.0101(15) C35 0.0367(15) 0.0457(16) 0.088(2) -0.0154(16) 0.0047(15) -0.0107(12) C40 0.0478(17) 0.0308(14) 0.084(2) -0.0029(14) -0.0009(16) -0.0040(12) C33 0.0282(14) 0.085(2) 0.067(2) -0.0043(18) 0.0002(13) 0.0001(15) C34 0.0348(16) 0.076(2) 0.117(3) -0.028(2) 0.0073(18) -0.0209(16) C47 0.098(3) 0.130(4) 0.0385(18) 0.012(2) 0.0033(18) 0.046(3) C48 0.122(4) 0.061(2) 0.073(2) 0.0198(19) 0.057(3) 0.011(2) C46 0.114(4) 0.098(3) 0.048(2) 0.004(2) 0.040(2) 0.025(3) C43 0.211(6) 0.072(3) 0.098(3) 0.029(2) 0.107(4) 0.015(3) C44 0.051(2) 0.177(5) 0.069(2) 0.020(3) 0.0320(19) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.7713(19) . ? Al1 C9 1.965(3) . ? Al1 C8 1.967(3) . ? Al1 N1 1.969(2) . ? N1 C7 1.308(3) . ? N1 C10 1.460(3) . ? O1 C2 1.325(3) . ? C10 C15 1.398(3) . ? C10 C11 1.406(3) . ? C15 C14 1.398(3) . ? C15 C17 1.534(3) . ? C14 C13 1.398(3) . ? C14 H14A 0.9500 . ? C16 C24 1.526(3) . ? C16 C11 1.531(3) . ? C16 C18 1.533(3) . ? C16 H16A 1.0000 . ? C1 C6 1.409(3) . ? C1 C2 1.414(3) . ? C1 C7 1.432(3) . ? C7 H7A 0.9500 . ? C36 C41 1.386(4) . ? C36 C37 1.392(4) . ? C36 C17 1.527(3) . ? C30 C35 1.378(4) . ? C30 C31 1.391(4) . ? C30 C17 1.531(3) . ? C18 C19 1.385(4) . ? C18 C23 1.388(3) . ? C12 C11 1.393(3) . ? C12 C13 1.394(3) . ? C12 H12A 0.9500 . ? C2 C3 1.425(3) . ? C24 C29 1.390(4) . ? C24 C25 1.391(4) . ? C17 H17A 1.0000 . ? C13 C42 1.521(3) . ? C6 C5 1.371(4) . ? C6 H6A 0.9500 . ? C29 C28 1.390(4) . ? C29 H29A 0.9500 . ? C23 C22 1.390(4) . ? C23 H23A 0.9500 . ? C5 C4 1.404(4) . ? C5 C49 1.516(4) . ? C3 C4 1.385(4) . ? C3 C45 1.530(4) . ? C37 C38 1.390(4) . ? C37 H37A 0.9500 . ? C41 C40 1.400(4) . ? C41 H41A 0.9500 . ? C22 C21 1.374(4) . ? C22 H22A 0.9500 . ? C42 C43 1.484(5) . ? C42 C44 1.524(5) . ? C42 H42A 1.0000 . ? C27 C26 1.369(4) . ? C27 C28 1.377(4) . ? C27 H27A 0.9500 . ? C4 H4A 0.9500 . ? C25 C26 1.387(4) . ? C25 H25A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C21 C20 1.380(4) . ? C21 H21A 0.9500 . ? C26 H26A 0.9500 . ? C28 H28A 0.9500 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C19 C20 1.389(4) . ? C19 H19A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C32 C33 1.369(5) . ? C32 C31 1.385(4) . ? C32 H32A 0.9500 . ? C45 C47 1.536(5) . ? C45 C48 1.539(6) . ? C45 C46 1.540(4) . ? C31 H31A 0.9500 . ? C20 H20A 0.9500 . ? C39 C38 1.372(5) . ? C39 C40 1.376(5) . ? C39 H39A 0.9500 . ? C38 H38A 0.9500 . ? C35 C34 1.388(4) . ? C35 H35A 0.9500 . ? C40 H40A 0.9500 . ? C33 C34 1.362(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 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 . ? 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 C9 110.23(12) . . ? O1 Al1 C8 112.15(13) . . ? C9 Al1 C8 114.74(14) . . ? O1 Al1 N1 93.86(8) . . ? C9 Al1 N1 115.04(11) . . ? C8 Al1 N1 109.03(11) . . ? C7 N1 C10 113.72(18) . . ? C7 N1 Al1 120.12(16) . . ? C10 N1 Al1 126.16(14) . . ? C2 O1 Al1 131.35(16) . . ? C15 C10 C11 121.7(2) . . ? C15 C10 N1 118.03(19) . . ? C11 C10 N1 120.19(19) . . ? C14 C15 C10 118.1(2) . . ? C14 C15 C17 121.9(2) . . ? C10 C15 C17 120.0(2) . . ? C13 C14 C15 121.6(2) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C24 C16 C11 111.87(18) . . ? C24 C16 C18 113.83(18) . . ? C11 C16 C18 112.61(19) . . ? C24 C16 H16A 105.9 . . ? C11 C16 H16A 105.9 . . ? C18 C16 H16A 105.9 . . ? C6 C1 C2 120.6(2) . . ? C6 C1 C7 116.8(2) . . ? C2 C1 C7 122.2(2) . . ? N1 C7 C1 127.4(2) . . ? N1 C7 H7A 116.3 . . ? C1 C7 H7A 116.3 . . ? C41 C36 C37 118.6(2) . . ? C41 C36 C17 122.5(2) . . ? C37 C36 C17 118.9(2) . . ? C35 C30 C31 117.3(2) . . ? C35 C30 C17 123.4(2) . . ? C31 C30 C17 119.3(2) . . ? C19 C18 C23 117.7(2) . . ? C19 C18 C16 118.3(2) . . ? C23 C18 C16 124.0(2) . . ? C11 C12 C13 121.9(2) . . ? C11 C12 H12A 119.0 . . ? C13 C12 H12A 119.0 . . ? O1 C2 C1 120.4(2) . . ? O1 C2 C3 120.4(2) . . ? C1 C2 C3 119.1(2) . . ? C29 C24 C25 118.1(2) . . ? C29 C24 C16 122.6(2) . . ? C25 C24 C16 119.3(2) . . ? C36 C17 C30 113.60(18) . . ? C36 C17 C15 112.47(19) . . ? C30 C17 C15 112.57(19) . . ? C36 C17 H17A 105.8 . . ? C30 C17 H17A 105.8 . . ? C15 C17 H17A 105.8 . . ? C12 C13 C14 118.5(2) . . ? C12 C13 C42 119.8(2) . . ? C14 C13 C42 121.7(2) . . ? C5 C6 C1 120.9(2) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? C24 C29 C28 120.5(3) . . ? C24 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C12 C11 C10 118.0(2) . . ? C12 C11 C16 122.0(2) . . ? C10 C11 C16 120.0(2) . . ? C18 C23 C22 121.0(2) . . ? C18 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C6 C5 C4 117.5(2) . . ? C6 C5 C49 121.8(3) . . ? C4 C5 C49 120.7(3) . . ? C4 C3 C2 117.0(2) . . ? C4 C3 C45 122.6(2) . . ? C2 C3 C45 120.4(2) . . ? C38 C37 C36 121.3(3) . . ? C38 C37 H37A 119.3 . . ? C36 C37 H37A 119.3 . . ? C36 C41 C40 119.9(3) . . ? C36 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C21 C22 C23 120.6(3) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C43 C42 C13 111.3(3) . . ? C43 C42 C44 113.1(4) . . ? C13 C42 C44 113.4(2) . . ? C43 C42 H42A 106.1 . . ? C13 C42 H42A 106.1 . . ? C44 C42 H42A 106.1 . . ? C26 C27 C28 119.7(3) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C3 C4 C5 124.7(2) . . ? C3 C4 H4A 117.6 . . ? C5 C4 H4A 117.6 . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? Al1 C9 H9A 109.5 . . ? Al1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Al1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C22 C21 C20 119.1(3) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C5 C49 H49A 109.5 . . ? C5 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C5 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C18 C19 C20 121.4(3) . . ? C18 C19 H19A 119.3 . . ? C20 C19 H19A 119.3 . . ? Al1 C8 H8A 109.5 . . ? Al1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Al1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C33 C32 C31 120.1(3) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C3 C45 C47 110.2(3) . . ? C3 C45 C48 109.6(3) . . ? C47 C45 C48 111.2(3) . . ? C3 C45 C46 111.2(3) . . ? C47 C45 C46 106.6(3) . . ? C48 C45 C46 107.9(3) . . ? C32 C31 C30 121.4(3) . . ? C32 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C38 C39 C40 120.3(3) . . ? C38 C39 H39A 119.8 . . ? C40 C39 H39A 119.8 . . ? C39 C38 C37 119.4(3) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C30 C35 C34 121.0(3) . . ? C30 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C34 C33 C32 119.3(3) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Al1 N1 C7 19.33(19) . . . . ? C9 Al1 N1 C7 133.78(19) . . . . ? C8 Al1 N1 C7 -95.7(2) . . . . ? O1 Al1 N1 C10 -161.11(18) . . . . ? C9 Al1 N1 C10 -46.7(2) . . . . ? C8 Al1 N1 C10 83.9(2) . . . . ? C9 Al1 O1 C2 -140.2(2) . . . . ? C8 Al1 O1 C2 90.6(3) . . . . ? N1 Al1 O1 C2 -21.7(2) . . . . ? C7 N1 C10 C15 -93.8(2) . . . . ? Al1 N1 C10 C15 86.6(2) . . . . ? C7 N1 C10 C11 84.1(2) . . . . ? Al1 N1 C10 C11 -95.5(2) . . . . ? C11 C10 C15 C14 -2.5(3) . . . . ? N1 C10 C15 C14 175.3(2) . . . . ? C11 C10 C15 C17 177.1(2) . . . . ? N1 C10 C15 C17 -5.1(3) . . . . ? C10 C15 C14 C13 0.8(3) . . . . ? C17 C15 C14 C13 -178.8(2) . . . . ? C10 N1 C7 C1 171.9(2) . . . . ? Al1 N1 C7 C1 -8.5(3) . . . . ? C6 C1 C7 N1 177.6(2) . . . . ? C2 C1 C7 N1 -9.1(4) . . . . ? C24 C16 C18 C19 161.7(2) . . . . ? C11 C16 C18 C19 -69.6(3) . . . . ? C24 C16 C18 C23 -16.9(3) . . . . ? C11 C16 C18 C23 111.8(3) . . . . ? Al1 O1 C2 C1 10.6(4) . . . . ? Al1 O1 C2 C3 -171.2(2) . . . . ? C6 C1 C2 O1 -177.6(2) . . . . ? C7 C1 C2 O1 9.3(4) . . . . ? C6 C1 C2 C3 4.1(4) . . . . ? C7 C1 C2 C3 -169.0(2) . . . . ? C11 C16 C24 C29 -35.0(3) . . . . ? C18 C16 C24 C29 94.0(3) . . . . ? C11 C16 C24 C25 142.5(2) . . . . ? C18 C16 C24 C25 -88.5(3) . . . . ? C41 C36 C17 C30 -90.9(3) . . . . ? C37 C36 C17 C30 91.5(3) . . . . ? C41 C36 C17 C15 38.4(3) . . . . ? C37 C36 C17 C15 -139.1(2) . . . . ? C35 C30 C17 C36 21.8(4) . . . . ? C31 C30 C17 C36 -159.2(2) . . . . ? C35 C30 C17 C15 -107.5(3) . . . . ? C31 C30 C17 C15 71.5(3) . . . . ? C14 C15 C17 C36 -109.7(2) . . . . ? C10 C15 C17 C36 70.7(3) . . . . ? C14 C15 C17 C30 20.2(3) . . . . ? C10 C15 C17 C30 -159.4(2) . . . . ? C11 C12 C13 C14 -2.5(4) . . . . ? C11 C12 C13 C42 177.6(2) . . . . ? C15 C14 C13 C12 1.6(4) . . . . ? C15 C14 C13 C42 -178.5(2) . . . . ? C2 C1 C6 C5 -0.5(4) . . . . ? C7 C1 C6 C5 173.0(2) . . . . ? C25 C24 C29 C28 0.3(4) . . . . ? C16 C24 C29 C28 177.8(2) . . . . ? C13 C12 C11 C10 0.8(4) . . . . ? C13 C12 C11 C16 -177.6(2) . . . . ? C15 C10 C11 C12 1.7(3) . . . . ? N1 C10 C11 C12 -176.0(2) . . . . ? C15 C10 C11 C16 -179.8(2) . . . . ? N1 C10 C11 C16 2.4(3) . . . . ? C24 C16 C11 C12 96.7(3) . . . . ? C18 C16 C11 C12 -33.0(3) . . . . ? C24 C16 C11 C10 -81.7(3) . . . . ? C18 C16 C11 C10 148.6(2) . . . . ? C19 C18 C23 C22 -0.9(4) . . . . ? C16 C18 C23 C22 177.6(3) . . . . ? C1 C6 C5 C4 -2.5(4) . . . . ? C1 C6 C5 C49 177.0(2) . . . . ? O1 C2 C3 C4 177.2(2) . . . . ? C1 C2 C3 C4 -4.5(4) . . . . ? O1 C2 C3 C45 -1.8(4) . . . . ? C1 C2 C3 C45 176.5(3) . . . . ? C41 C36 C37 C38 0.0(4) . . . . ? C17 C36 C37 C38 177.6(2) . . . . ? C37 C36 C41 C40 0.1(4) . . . . ? C17 C36 C41 C40 -177.4(2) . . . . ? C18 C23 C22 C21 -0.2(5) . . . . ? C12 C13 C42 C43 -87.9(4) . . . . ? C14 C13 C42 C43 92.3(4) . . . . ? C12 C13 C42 C44 143.2(3) . . . . ? C14 C13 C42 C44 -36.6(4) . . . . ? C2 C3 C4 C5 1.6(4) . . . . ? C45 C3 C4 C5 -179.4(3) . . . . ? C6 C5 C4 C3 2.0(4) . . . . ? C49 C5 C4 C3 -177.5(3) . . . . ? C29 C24 C25 C26 -0.1(4) . . . . ? C16 C24 C25 C26 -177.7(2) . . . . ? C23 C22 C21 C20 1.2(5) . . . . ? C28 C27 C26 C25 -0.3(4) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? C26 C27 C28 C29 0.6(4) . . . . ? C24 C29 C28 C27 -0.6(4) . . . . ? C23 C18 C19 C20 1.1(4) . . . . ? C16 C18 C19 C20 -177.5(3) . . . . ? C4 C3 C45 C47 122.8(3) . . . . ? C2 C3 C45 C47 -58.2(4) . . . . ? C4 C3 C45 C48 -114.4(3) . . . . ? C2 C3 C45 C48 64.5(4) . . . . ? C4 C3 C45 C46 4.7(5) . . . . ? C2 C3 C45 C46 -176.3(3) . . . . ? C33 C32 C31 C30 -1.3(5) . . . . ? C35 C30 C31 C32 0.7(4) . . . . ? C17 C30 C31 C32 -178.4(3) . . . . ? C22 C21 C20 C19 -1.0(5) . . . . ? C18 C19 C20 C21 -0.2(5) . . . . ? C40 C39 C38 C37 0.0(5) . . . . ? C36 C37 C38 C39 -0.1(5) . . . . ? C31 C30 C35 C34 0.1(5) . . . . ? C17 C30 C35 C34 179.1(3) . . . . ? C38 C39 C40 C41 0.1(5) . . . . ? C36 C41 C40 C39 -0.2(4) . . . . ? C31 C32 C33 C34 1.2(5) . . . . ? C32 C33 C34 C35 -0.4(6) . . . . ? C30 C35 C34 C33 -0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.567 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.131 data_c7 _database_code_depnum_ccdc_archive 'CCDC 885175' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H48 Al N O' _chemical_formula_weight 669.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.054(2) _cell_length_b 14.116(3) _cell_length_c 15.935(3) _cell_angle_alpha 91.37(3) _cell_angle_beta 98.60(3) _cell_angle_gamma 90.67(3) _cell_volume 2235.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2800 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.2200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5656 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 29159 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.46 _reflns_number_total 10182 _reflns_number_gt 8251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (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^)+(0.1023P)^2^+1.0221P] 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 10182 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0948 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.2214 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 0.88528(7) 0.81050(5) 0.09130(4) 0.03097(19) Uani 1 1 d . . . O1 O 0.88618(19) 0.73270(12) 0.17776(10) 0.0394(4) Uani 1 1 d . . . N1 N 0.7327(2) 0.74433(13) 0.02059(11) 0.0289(4) Uani 1 1 d . . . C12 C 0.6188(2) 0.81963(16) -0.20110(13) 0.0293(5) Uani 1 1 d . . . H12A H 0.6441 0.8125 -0.2560 0.035 Uiso 1 1 calc R . . C7 C 0.6972(2) 0.65922(16) 0.03849(13) 0.0292(5) Uani 1 1 d . . . H7A H 0.6249 0.6305 0.0010 0.035 Uiso 1 1 calc R . . C11 C 0.6939(2) 0.77530(15) -0.13307(13) 0.0275(4) Uani 1 1 d . . . C15 C 0.5385(2) 0.83790(15) -0.04099(14) 0.0294(5) Uani 1 1 d . . . C13 C 0.5077(2) 0.87412(15) -0.19088(13) 0.0282(5) Uani 1 1 d . . . C14 C 0.4682(2) 0.88156(16) -0.11103(14) 0.0303(5) Uani 1 1 d . . . H14A H 0.3911 0.9175 -0.1041 0.036 Uiso 1 1 calc R . . C10 C 0.6529(2) 0.78668(15) -0.05248(13) 0.0272(4) Uani 1 1 d . . . C6 C 0.7162(2) 0.50717(16) 0.10705(15) 0.0327(5) Uani 1 1 d . . . H6A H 0.6560 0.4822 0.0598 0.039 Uiso 1 1 calc R . . C1 C 0.7554(2) 0.60370(16) 0.10884(14) 0.0303(5) Uani 1 1 d . . . C2 C 0.8456(2) 0.64272(16) 0.17821(14) 0.0308(5) Uani 1 1 d . . . C36 C 0.4880(2) 1.03147(16) -0.26285(14) 0.0307(5) Uani 1 1 d . . . C24 C 0.7832(2) 0.60768(16) -0.13762(14) 0.0305(5) Uani 1 1 d . . . C3 C 0.8881(2) 0.58514(17) 0.24879(14) 0.0319(5) Uani 1 1 d . . . C18 C 0.8711(2) 0.73728(16) -0.22471(15) 0.0324(5) Uani 1 1 d . . . C16 C 0.8140(2) 0.71343(16) -0.14445(14) 0.0298(5) Uani 1 1 d . . . H16A H 0.8861 0.7302 -0.0959 0.036 Uiso 1 1 calc R . . C30 C 0.4315(2) 0.87730(16) -0.34947(14) 0.0310(5) Uani 1 1 d . . . C4 C 0.8477(3) 0.49075(17) 0.24213(16) 0.0368(5) Uani 1 1 d . . . H4A H 0.8792 0.4512 0.2881 0.044 Uiso 1 1 calc R . . C17 C 0.4333(2) 0.92987(16) -0.26412(13) 0.0291(5) Uani 1 1 d . . . H17A H 0.3376 0.9341 -0.2542 0.035 Uiso 1 1 calc R . . C25 C 0.6548(2) 0.56808(18) -0.16074(16) 0.0360(5) Uani 1 1 d . . . H25A H 0.5826 0.6069 -0.1839 0.043 Uiso 1 1 calc R . . C28 C 0.8635(3) 0.45256(18) -0.09544(17) 0.0400(6) Uani 1 1 d . . . H28A H 0.9357 0.4130 -0.0735 0.048 Uiso 1 1 calc R . . C26 C 0.6317(3) 0.47222(18) -0.15004(17) 0.0424(6) Uani 1 1 d . . . H26A H 0.5438 0.4459 -0.1658 0.051 Uiso 1 1 calc R . . C41 C 0.6248(3) 1.05235(18) -0.24420(16) 0.0392(6) Uani 1 1 d . . . H41A H 0.6867 1.0027 -0.2307 0.047 Uiso 1 1 calc R . . C43 C 0.9787(3) 0.62582(19) 0.32832(15) 0.0394(6) Uani 1 1 d . . . C37 C 0.3994(3) 1.10577(17) -0.28085(15) 0.0361(5) Uani 1 1 d . . . H37A H 0.3054 1.0930 -0.2935 0.043 Uiso 1 1 calc R . . C9 C 0.8404(3) 0.94040(19) 0.12080(19) 0.0489(7) Uani 1 1 d . . . H9A H 0.9184 0.9710 0.1557 0.073 Uiso 1 1 calc R . . H9B H 0.7643 0.9394 0.1527 0.073 Uiso 1 1 calc R . . H9C H 0.8162 0.9759 0.0688 0.073 Uiso 1 1 calc R . . C19 C 0.9560(3) 0.8152(2) -0.22368(17) 0.0431(6) Uani 1 1 d . . . H19A H 0.9816 0.8503 -0.1721 0.052 Uiso 1 1 calc R . . C35 C 0.5167(3) 0.9007(2) -0.40734(16) 0.0453(6) Uani 1 1 d . . . H35A H 0.5781 0.9527 -0.3954 0.054 Uiso 1 1 calc R . . C29 C 0.8874(2) 0.54860(17) -0.10596(15) 0.0341(5) Uani 1 1 d . . . H29A H 0.9760 0.5740 -0.0913 0.041 Uiso 1 1 calc R . . C38 C 0.4474(3) 1.19908(18) -0.28045(17) 0.0440(6) Uani 1 1 d . . . H38A H 0.3858 1.2492 -0.2922 0.053 Uiso 1 1 calc R . . C27 C 0.7363(3) 0.41474(18) -0.11651(17) 0.0435(6) Uani 1 1 d . . . H27A H 0.7199 0.3495 -0.1082 0.052 Uiso 1 1 calc R . . C8 C 1.0493(3) 0.8033(2) 0.03823(17) 0.0435(6) Uani 1 1 d . . . H8A H 1.1233 0.8366 0.0746 0.065 Uiso 1 1 calc R . . H8B H 1.0336 0.8329 -0.0173 0.065 Uiso 1 1 calc R . . H8C H 1.0728 0.7367 0.0309 0.065 Uiso 1 1 calc R . . C40 C 0.6717(3) 1.1449(2) -0.24505(17) 0.0435(6) Uani 1 1 d . . . H40A H 0.7656 1.1580 -0.2331 0.052 Uiso 1 1 calc R . . C5 C 0.7629(3) 0.44900(17) 0.17178(17) 0.0376(5) Uani 1 1 d . . . C39 C 0.5828(3) 1.21891(19) -0.26315(17) 0.0449(6) Uani 1 1 d . . . H39A H 0.6153 1.2823 -0.2636 0.054 Uiso 1 1 calc R . . C42 C 0.4886(3) 0.8452(2) 0.04358(15) 0.0429(6) Uani 1 1 d . . . H42A H 0.4082 0.8846 0.0383 0.064 Uiso 1 1 calc R . . H42B H 0.5589 0.8741 0.0860 0.064 Uiso 1 1 calc R . . H42C H 0.4661 0.7817 0.0613 0.064 Uiso 1 1 calc R . . C31 C 0.3410(3) 0.8018(2) -0.36962(17) 0.0469(7) Uani 1 1 d . . . H31A H 0.2814 0.7852 -0.3311 0.056 Uiso 1 1 calc R . . C46 C 1.1133(3) 0.6583(2) 0.30545(18) 0.0536(8) Uani 1 1 d . . . H46A H 1.0982 0.7055 0.2610 0.080 Uiso 1 1 calc R . . H46B H 1.1596 0.6038 0.2847 0.080 Uiso 1 1 calc R . . H46C H 1.1687 0.6865 0.3559 0.080 Uiso 1 1 calc R . . C45 C 1.0077(3) 0.5512(2) 0.39740(18) 0.0523(7) Uani 1 1 d . . . H45A H 1.0522 0.4969 0.3748 0.078 Uiso 1 1 calc R . . H45B H 0.9229 0.5301 0.4147 0.078 Uiso 1 1 calc R . . H45C H 1.0665 0.5792 0.4466 0.078 Uiso 1 1 calc R . . C23 C 0.8372(3) 0.6866(2) -0.30077(17) 0.0481(7) Uani 1 1 d . . . H23A H 0.7810 0.6317 -0.3028 0.058 Uiso 1 1 calc R . . C21 C 0.9692(3) 0.7931(2) -0.37151(18) 0.0518(7) Uani 1 1 d . . . H21A H 1.0027 0.8120 -0.4213 0.062 Uiso 1 1 calc R . . C22 C 0.8843(4) 0.7150(2) -0.37403(18) 0.0565(8) Uani 1 1 d . . . H22A H 0.8581 0.6806 -0.4260 0.068 Uiso 1 1 calc R . . C47 C 0.7268(3) 0.34440(19) 0.1686(2) 0.0558(8) Uani 1 1 d . . . H47A H 0.6669 0.3288 0.1156 0.084 Uiso 1 1 calc R . . H47B H 0.6812 0.3295 0.2170 0.084 Uiso 1 1 calc R . . H47C H 0.8090 0.3072 0.1711 0.084 Uiso 1 1 calc R . . C44 C 0.9087(4) 0.7089(2) 0.36664(18) 0.0556(8) Uani 1 1 d . . . H44A H 0.8884 0.7577 0.3240 0.083 Uiso 1 1 calc R . . H44B H 0.9682 0.7359 0.4160 0.083 Uiso 1 1 calc R . . H44C H 0.8250 0.6862 0.3844 0.083 Uiso 1 1 calc R . . C20 C 1.0045(3) 0.8431(2) -0.2963(2) 0.0525(7) Uani 1 1 d . . . H20A H 1.0625 0.8971 -0.2941 0.063 Uiso 1 1 calc R . . C34 C 0.5120(4) 0.8479(3) -0.48266(18) 0.0596(8) Uani 1 1 d . . . H34A H 0.5707 0.8643 -0.5218 0.072 Uiso 1 1 calc R . . C32 C 0.3371(4) 0.7507(2) -0.4451(2) 0.0673(10) Uani 1 1 d . . . H32A H 0.2739 0.7000 -0.4585 0.081 Uiso 1 1 calc R . . C33 C 0.4245(4) 0.7729(3) -0.50132(19) 0.0668(10) Uani 1 1 d . . . H33A H 0.4237 0.7364 -0.5523 0.080 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 0.0421(4) 0.0260(3) 0.0232(3) 0.0039(3) -0.0011(3) -0.0008(3) O1 0.0588(11) 0.0323(8) 0.0237(8) 0.0068(7) -0.0059(7) -0.0065(8) N1 0.0399(10) 0.0277(9) 0.0188(8) 0.0043(7) 0.0030(7) 0.0041(8) C12 0.0360(12) 0.0322(11) 0.0198(10) 0.0008(8) 0.0037(9) 0.0048(9) C7 0.0365(12) 0.0295(11) 0.0215(10) 0.0020(8) 0.0041(9) 0.0002(9) C11 0.0352(11) 0.0261(10) 0.0210(10) 0.0004(8) 0.0032(8) 0.0040(9) C15 0.0367(12) 0.0279(10) 0.0239(10) 0.0010(8) 0.0056(9) 0.0006(9) C13 0.0353(11) 0.0254(10) 0.0229(10) 0.0011(8) 0.0015(9) 0.0000(9) C14 0.0370(12) 0.0283(11) 0.0262(11) 0.0004(9) 0.0061(9) 0.0049(9) C10 0.0364(11) 0.0236(10) 0.0199(10) 0.0024(8) -0.0014(8) 0.0018(9) C6 0.0337(12) 0.0314(11) 0.0327(12) 0.0042(9) 0.0035(9) 0.0000(9) C1 0.0319(11) 0.0322(11) 0.0272(11) 0.0051(9) 0.0044(9) 0.0030(9) C2 0.0373(12) 0.0305(11) 0.0250(10) 0.0066(9) 0.0054(9) -0.0009(9) C36 0.0401(12) 0.0301(11) 0.0213(10) 0.0019(8) 0.0030(9) 0.0014(9) C24 0.0362(12) 0.0330(11) 0.0226(10) -0.0029(9) 0.0053(9) 0.0053(9) C3 0.0344(12) 0.0353(12) 0.0269(11) 0.0088(9) 0.0060(9) 0.0038(9) C18 0.0365(12) 0.0327(11) 0.0286(11) 0.0031(9) 0.0057(9) 0.0103(10) C16 0.0341(11) 0.0325(11) 0.0218(10) 0.0009(8) 0.0008(9) 0.0042(9) C30 0.0365(12) 0.0323(11) 0.0222(10) 0.0040(9) -0.0030(9) 0.0043(9) C4 0.0402(13) 0.0359(12) 0.0355(12) 0.0167(10) 0.0067(10) 0.0056(10) C17 0.0325(11) 0.0316(11) 0.0230(10) 0.0032(8) 0.0028(9) -0.0001(9) C25 0.0350(12) 0.0368(12) 0.0352(12) -0.0018(10) 0.0023(10) 0.0063(10) C28 0.0454(14) 0.0362(13) 0.0385(13) 0.0061(10) 0.0049(11) 0.0106(11) C26 0.0472(15) 0.0373(13) 0.0421(14) -0.0059(11) 0.0062(12) -0.0060(11) C41 0.0403(13) 0.0379(13) 0.0374(13) 0.0078(10) -0.0016(11) 0.0000(11) C43 0.0484(14) 0.0429(13) 0.0257(11) 0.0108(10) 0.0001(10) 0.0050(11) C37 0.0418(13) 0.0358(12) 0.0289(11) 0.0059(10) -0.0015(10) 0.0033(10) C9 0.0664(19) 0.0352(13) 0.0460(16) -0.0011(12) 0.0118(14) -0.0009(13) C19 0.0427(14) 0.0507(15) 0.0360(13) 0.0020(11) 0.0060(11) -0.0023(12) C35 0.0540(16) 0.0516(16) 0.0299(12) -0.0018(11) 0.0068(11) -0.0130(13) C29 0.0349(12) 0.0368(12) 0.0316(12) 0.0030(10) 0.0072(10) 0.0049(10) C38 0.0600(17) 0.0320(12) 0.0394(14) 0.0044(11) 0.0050(12) 0.0033(12) C27 0.0632(17) 0.0299(12) 0.0391(14) -0.0010(10) 0.0132(13) 0.0027(12) C8 0.0466(15) 0.0453(14) 0.0356(13) -0.0002(11) -0.0035(11) -0.0008(12) C40 0.0473(15) 0.0464(15) 0.0356(13) 0.0024(11) 0.0023(11) -0.0090(12) C5 0.0373(13) 0.0304(11) 0.0456(14) 0.0109(10) 0.0062(11) 0.0013(10) C39 0.0659(18) 0.0340(13) 0.0338(13) 0.0001(10) 0.0049(12) -0.0079(12) C42 0.0514(15) 0.0542(16) 0.0250(12) 0.0039(11) 0.0109(11) 0.0114(13) C31 0.0588(17) 0.0471(15) 0.0323(13) -0.0006(11) -0.0006(12) -0.0105(13) C46 0.0491(16) 0.073(2) 0.0346(14) 0.0061(13) -0.0052(12) -0.0150(15) C45 0.0615(18) 0.0569(17) 0.0353(14) 0.0194(13) -0.0071(13) 0.0064(14) C23 0.075(2) 0.0407(14) 0.0314(13) 0.0009(11) 0.0156(13) -0.0017(13) C21 0.0617(18) 0.0593(18) 0.0387(15) 0.0128(13) 0.0191(13) 0.0089(15) C22 0.086(2) 0.0524(17) 0.0334(14) -0.0022(12) 0.0173(15) 0.0024(16) C47 0.0606(18) 0.0333(14) 0.071(2) 0.0163(14) -0.0025(16) -0.0014(13) C44 0.076(2) 0.0580(18) 0.0295(13) 0.0012(12) -0.0037(13) 0.0145(16) C20 0.0513(17) 0.0578(18) 0.0498(17) 0.0107(14) 0.0117(14) -0.0075(14) C34 0.073(2) 0.075(2) 0.0323(14) -0.0077(14) 0.0155(14) -0.0094(17) C32 0.094(3) 0.0586(19) 0.0445(17) -0.0129(15) 0.0008(17) -0.0268(18) C33 0.103(3) 0.066(2) 0.0299(14) -0.0133(14) 0.0077(16) -0.009(2) _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 1.7814(18) . ? Al1 C9 1.957(3) . ? Al1 C8 1.965(3) . ? Al1 N1 1.974(2) . ? O1 C2 1.330(3) . ? N1 C7 1.299(3) . ? N1 C10 1.457(3) . ? C12 C13 1.391(3) . ? C12 C11 1.391(3) . ? C12 H12A 0.9500 . ? C7 C1 1.439(3) . ? C7 H7A 0.9500 . ? C11 C10 1.413(3) . ? C11 C16 1.528(3) . ? C15 C14 1.390(3) . ? C15 C10 1.398(3) . ? C15 C42 1.509(3) . ? C13 C14 1.390(3) . ? C13 C17 1.529(3) . ? C14 H14A 0.9500 . ? C6 C5 1.365(3) . ? C6 C1 1.413(3) . ? C6 H6A 0.9500 . ? C1 C2 1.417(3) . ? C2 C3 1.420(3) . ? C36 C41 1.390(3) . ? C36 C37 1.391(3) . ? C36 C17 1.529(3) . ? C24 C29 1.389(3) . ? C24 C25 1.395(3) . ? C24 C16 1.531(3) . ? C3 C4 1.385(3) . ? C3 C43 1.540(3) . ? C18 C19 1.383(4) . ? C18 C23 1.388(3) . ? C18 C16 1.521(3) . ? C16 H16A 1.0000 . ? C30 C35 1.392(3) . ? C30 C31 1.393(4) . ? C30 C17 1.531(3) . ? C4 C5 1.415(4) . ? C4 H4A 0.9500 . ? C17 H17A 1.0000 . ? C25 C26 1.389(4) . ? C25 H25A 0.9500 . ? C28 C27 1.372(4) . ? C28 C29 1.393(3) . ? C28 H28A 0.9500 . ? C26 C27 1.387(4) . ? C26 H26A 0.9500 . ? C41 C40 1.385(4) . ? C41 H41A 0.9500 . ? C43 C46 1.521(4) . ? C43 C44 1.535(4) . ? C43 C45 1.541(3) . ? C37 C38 1.397(3) . ? C37 H37A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C19 C20 1.385(4) . ? C19 H19A 0.9500 . ? C35 C34 1.392(4) . ? C35 H35A 0.9500 . ? C29 H29A 0.9500 . ? C38 C39 1.372(4) . ? C38 H38A 0.9500 . ? C27 H27A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C40 C39 1.389(4) . ? C40 H40A 0.9500 . ? C5 C47 1.514(4) . ? C39 H39A 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C31 C32 1.383(4) . ? C31 H31A 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C23 C22 1.390(4) . ? C23 H23A 0.9500 . ? C21 C20 1.374(4) . ? C21 C22 1.383(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C20 H20A 0.9500 . ? C34 C33 1.367(5) . ? C34 H34A 0.9500 . ? C32 C33 1.384(5) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 C9 112.47(11) . . ? O1 Al1 C8 113.12(11) . . ? C9 Al1 C8 112.94(13) . . ? O1 Al1 N1 93.94(8) . . ? C9 Al1 N1 111.75(12) . . ? C8 Al1 N1 111.22(10) . . ? C2 O1 Al1 129.97(15) . . ? C7 N1 C10 116.29(19) . . ? C7 N1 Al1 120.50(16) . . ? C10 N1 Al1 123.20(14) . . ? C13 C12 C11 121.7(2) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? N1 C7 C1 127.2(2) . . ? N1 C7 H7A 116.4 . . ? C1 C7 H7A 116.4 . . ? C12 C11 C10 117.7(2) . . ? C12 C11 C16 121.88(19) . . ? C10 C11 C16 120.43(19) . . ? C14 C15 C10 118.0(2) . . ? C14 C15 C42 119.7(2) . . ? C10 C15 C42 122.3(2) . . ? C14 C13 C12 118.9(2) . . ? C14 C13 C17 119.6(2) . . ? C12 C13 C17 121.45(19) . . ? C15 C14 C13 121.8(2) . . ? C15 C14 H14A 119.1 . . ? C13 C14 H14A 119.1 . . ? C15 C10 C11 121.8(2) . . ? C15 C10 N1 119.28(19) . . ? C11 C10 N1 118.92(19) . . ? C5 C6 C1 121.4(2) . . ? C5 C6 H6A 119.3 . . ? C1 C6 H6A 119.3 . . ? C6 C1 C2 120.5(2) . . ? C6 C1 C7 116.8(2) . . ? C2 C1 C7 122.7(2) . . ? O1 C2 C1 120.1(2) . . ? O1 C2 C3 120.9(2) . . ? C1 C2 C3 118.9(2) . . ? C41 C36 C37 118.5(2) . . ? C41 C36 C17 121.9(2) . . ? C37 C36 C17 119.7(2) . . ? C29 C24 C25 118.5(2) . . ? C29 C24 C16 118.6(2) . . ? C25 C24 C16 122.9(2) . . ? C4 C3 C2 117.3(2) . . ? C4 C3 C43 121.6(2) . . ? C2 C3 C43 121.1(2) . . ? C19 C18 C23 117.9(2) . . ? C19 C18 C16 119.1(2) . . ? C23 C18 C16 122.9(2) . . ? C18 C16 C11 111.52(18) . . ? C18 C16 C24 113.36(18) . . ? C11 C16 C24 112.52(19) . . ? C18 C16 H16A 106.3 . . ? C11 C16 H16A 106.3 . . ? C24 C16 H16A 106.3 . . ? C35 C30 C31 118.6(2) . . ? C35 C30 C17 123.2(2) . . ? C31 C30 C17 118.2(2) . . ? C3 C4 C5 124.7(2) . . ? C3 C4 H4A 117.7 . . ? C5 C4 H4A 117.7 . . ? C36 C17 C13 111.05(18) . . ? C36 C17 C30 113.61(18) . . ? C13 C17 C30 111.55(18) . . ? C36 C17 H17A 106.7 . . ? C13 C17 H17A 106.7 . . ? C30 C17 H17A 106.7 . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C27 C26 C25 120.3(3) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C40 C41 C36 120.6(2) . . ? C40 C41 H41A 119.7 . . ? C36 C41 H41A 119.7 . . ? C46 C43 C44 110.3(3) . . ? C46 C43 C3 110.1(2) . . ? C44 C43 C3 109.9(2) . . ? C46 C43 C45 107.4(2) . . ? C44 C43 C45 107.4(2) . . ? C3 C43 C45 111.7(2) . . ? C36 C37 C38 120.5(2) . . ? C36 C37 H37A 119.7 . . ? C38 C37 H37A 119.7 . . ? Al1 C9 H9A 109.5 . . ? Al1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Al1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C18 C19 C20 121.4(3) . . ? C18 C19 H19A 119.3 . . ? C20 C19 H19A 119.3 . . ? C34 C35 C30 120.0(3) . . ? C34 C35 H35A 120.0 . . ? C30 C35 H35A 120.0 . . ? C24 C29 C28 120.7(2) . . ? C24 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C39 C38 C37 120.6(3) . . ? C39 C38 H38A 119.7 . . ? C37 C38 H38A 119.7 . . ? C28 C27 C26 119.7(2) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? Al1 C8 H8A 109.5 . . ? Al1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Al1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C41 C40 C39 120.7(3) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C6 C5 C4 116.9(2) . . ? C6 C5 C47 121.8(2) . . ? C4 C5 C47 121.3(2) . . ? C38 C39 C40 119.1(2) . . ? C38 C39 H39A 120.5 . . ? C40 C39 H39A 120.5 . . ? C15 C42 H42A 109.5 . . ? C15 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C15 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C18 C23 C22 120.9(3) . . ? C18 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C20 C21 C22 119.3(3) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C5 C47 H47A 109.5 . . ? C5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C33 C34 C35 121.1(3) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C31 C32 C33 120.5(3) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C34 C33 C32 119.3(3) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? 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 C9 Al1 O1 C2 142.3(2) . . . . ? C8 Al1 O1 C2 -88.3(2) . . . . ? N1 Al1 O1 C2 26.8(2) . . . . ? O1 Al1 N1 C7 -16.73(19) . . . . ? C9 Al1 N1 C7 -132.83(19) . . . . ? C8 Al1 N1 C7 99.94(19) . . . . ? O1 Al1 N1 C10 162.35(17) . . . . ? C9 Al1 N1 C10 46.2(2) . . . . ? C8 Al1 N1 C10 -80.98(19) . . . . ? C10 N1 C7 C1 -177.2(2) . . . . ? Al1 N1 C7 C1 1.9(3) . . . . ? C13 C12 C11 C10 0.6(3) . . . . ? C13 C12 C11 C16 178.5(2) . . . . ? C11 C12 C13 C14 -2.3(3) . . . . ? C11 C12 C13 C17 174.4(2) . . . . ? C10 C15 C14 C13 1.0(3) . . . . ? C42 C15 C14 C13 -177.8(2) . . . . ? C12 C13 C14 C15 1.5(3) . . . . ? C17 C13 C14 C15 -175.2(2) . . . . ? C14 C15 C10 C11 -2.8(3) . . . . ? C42 C15 C10 C11 175.9(2) . . . . ? C14 C15 C10 N1 176.8(2) . . . . ? C42 C15 C10 N1 -4.5(3) . . . . ? C12 C11 C10 C15 2.0(3) . . . . ? C16 C11 C10 C15 -175.9(2) . . . . ? C12 C11 C10 N1 -177.54(19) . . . . ? C16 C11 C10 N1 4.5(3) . . . . ? C7 N1 C10 C15 88.7(3) . . . . ? Al1 N1 C10 C15 -90.5(2) . . . . ? C7 N1 C10 C11 -91.8(3) . . . . ? Al1 N1 C10 C11 89.1(2) . . . . ? C5 C6 C1 C2 0.4(4) . . . . ? C5 C6 C1 C7 -178.3(2) . . . . ? N1 C7 C1 C6 -169.2(2) . . . . ? N1 C7 C1 C2 12.2(4) . . . . ? Al1 O1 C2 C1 -19.8(3) . . . . ? Al1 O1 C2 C3 162.17(18) . . . . ? C6 C1 C2 O1 177.3(2) . . . . ? C7 C1 C2 O1 -4.1(3) . . . . ? C6 C1 C2 C3 -4.6(3) . . . . ? C7 C1 C2 C3 174.0(2) . . . . ? O1 C2 C3 C4 -176.3(2) . . . . ? C1 C2 C3 C4 5.6(3) . . . . ? O1 C2 C3 C43 2.1(3) . . . . ? C1 C2 C3 C43 -176.0(2) . . . . ? C19 C18 C16 C11 80.2(3) . . . . ? C23 C18 C16 C11 -96.9(3) . . . . ? C19 C18 C16 C24 -151.5(2) . . . . ? C23 C18 C16 C24 31.3(3) . . . . ? C12 C11 C16 C18 22.1(3) . . . . ? C10 C11 C16 C18 -160.0(2) . . . . ? C12 C11 C16 C24 -106.6(2) . . . . ? C10 C11 C16 C24 71.3(3) . . . . ? C29 C24 C16 C18 83.1(3) . . . . ? C25 C24 C16 C18 -97.8(3) . . . . ? C29 C24 C16 C11 -149.2(2) . . . . ? C25 C24 C16 C11 29.9(3) . . . . ? C2 C3 C4 C5 -2.8(4) . . . . ? C43 C3 C4 C5 178.9(2) . . . . ? C41 C36 C17 C13 40.5(3) . . . . ? C37 C36 C17 C13 -139.6(2) . . . . ? C41 C36 C17 C30 -86.2(3) . . . . ? C37 C36 C17 C30 93.7(3) . . . . ? C14 C13 C17 C36 83.6(3) . . . . ? C12 C13 C17 C36 -93.1(2) . . . . ? C14 C13 C17 C30 -148.6(2) . . . . ? C12 C13 C17 C30 34.7(3) . . . . ? C35 C30 C17 C36 24.8(3) . . . . ? C31 C30 C17 C36 -155.9(2) . . . . ? C35 C30 C17 C13 -101.7(3) . . . . ? C31 C30 C17 C13 77.7(3) . . . . ? C29 C24 C25 C26 1.7(3) . . . . ? C16 C24 C25 C26 -177.5(2) . . . . ? C24 C25 C26 C27 -0.2(4) . . . . ? C37 C36 C41 C40 -1.1(4) . . . . ? C17 C36 C41 C40 178.8(2) . . . . ? C4 C3 C43 C46 115.7(3) . . . . ? C2 C3 C43 C46 -62.6(3) . . . . ? C4 C3 C43 C44 -122.7(3) . . . . ? C2 C3 C43 C44 59.0(3) . . . . ? C4 C3 C43 C45 -3.6(3) . . . . ? C2 C3 C43 C45 178.1(2) . . . . ? C41 C36 C37 C38 0.3(4) . . . . ? C17 C36 C37 C38 -179.7(2) . . . . ? C23 C18 C19 C20 1.0(4) . . . . ? C16 C18 C19 C20 -176.3(3) . . . . ? C31 C30 C35 C34 -1.2(4) . . . . ? C17 C30 C35 C34 178.1(3) . . . . ? C25 C24 C29 C28 -1.7(3) . . . . ? C16 C24 C29 C28 177.5(2) . . . . ? C27 C28 C29 C24 0.2(4) . . . . ? C36 C37 C38 C39 0.7(4) . . . . ? C29 C28 C27 C26 1.3(4) . . . . ? C25 C26 C27 C28 -1.3(4) . . . . ? C36 C41 C40 C39 1.1(4) . . . . ? C1 C6 C5 C4 2.6(4) . . . . ? C1 C6 C5 C47 -177.0(2) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? C3 C4 C5 C47 178.2(3) . . . . ? C37 C38 C39 C40 -0.7(4) . . . . ? C41 C40 C39 C38 -0.1(4) . . . . ? C35 C30 C31 C32 0.6(4) . . . . ? C17 C30 C31 C32 -178.7(3) . . . . ? C19 C18 C23 C22 -1.8(4) . . . . ? C16 C18 C23 C22 175.4(3) . . . . ? C20 C21 C22 C23 -1.1(5) . . . . ? C18 C23 C22 C21 1.8(5) . . . . ? C22 C21 C20 C19 0.3(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C30 C35 C34 C33 0.1(5) . . . . ? C30 C31 C32 C33 1.0(5) . . . . ? C35 C34 C33 C32 1.5(6) . . . . ? C31 C32 C33 C34 -2.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.292 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.074 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 182.1 38.5 2 0.154 0.022 0.084 18.0 1.3 3 0.500 0.500 0.500 199.2 46.1 4 0.846 0.978 0.916 17.9 1.2 _platon_squeeze_details ; ? ; #==END