# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_Al(RR-1)Me _database_code_depnum_ccdc_archive 'CCDC 917781' #TrackingRef 'Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_absolute_configuration syn _chemical_formula_sum 'C44 H73 Al N2 O2' _chemical_formula_weight 689.02 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' O O 0.0106 0.0060 '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' 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.159(2) _cell_length_b 10.235(4) _cell_length_c 14.801(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.574(7) _cell_angle_gamma 90.00 _cell_volume 2142.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24302 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38513 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.08 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9665 _reflns_number_gt 7629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0532P)^2^+0.3220P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(13) _refine_ls_number_reflns 9665 _refine_ls_number_parameters 458 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.10208(4) 0.61908(5) 0.38873(4) 0.02353(13) Uani 1 1 d . . . O1 O 0.14852(8) 0.75467(13) 0.33171(8) 0.0262(3) Uani 1 1 d . . . N1 N -0.03926(11) 0.67847(16) 0.33438(10) 0.0251(3) Uani 1 1 d . . . C1 C 0.09810(15) 0.4474(2) 0.32883(15) 0.0342(5) Uani 1 1 d . . . H1A H 0.1463 0.3903 0.3574 0.051 Uiso 1 1 calc R . . H1B H 0.1105 0.4582 0.2647 0.051 Uiso 1 1 calc R . . H1C H 0.0355 0.4083 0.3346 0.051 Uiso 1 1 calc R . . O2 O 0.21004(9) 0.59069(13) 0.45912(8) 0.0273(3) Uani 1 1 d . . . N2 N 0.03431(10) 0.65303(16) 0.50051(11) 0.0265(4) Uani 1 1 d . . . C2 C 0.11594(13) 0.83319(19) 0.26407(13) 0.0252(4) Uani 1 1 d . . . C3 C 0.17427(13) 0.87359(19) 0.19452(13) 0.0255(4) Uani 1 1 d . . . C4 C 0.13659(14) 0.9637(2) 0.13121(13) 0.0283(4) Uani 1 1 d . . . H4 H 0.1758 0.9922 0.0847 0.034 Uiso 1 1 calc R . . C5 C 0.04528(14) 1.0142(2) 0.13228(13) 0.0281(4) Uani 1 1 d . . . C6 C -0.01202(14) 0.9656(2) 0.19922(13) 0.0279(4) Uani 1 1 d . . . H6 H -0.0759 0.9938 0.2004 0.033 Uiso 1 1 calc R . . C7 C 0.02201(13) 0.87730(19) 0.26382(13) 0.0267(4) Uani 1 1 d . . . C8 C 0.27664(13) 0.8229(2) 0.18902(13) 0.0282(4) Uani 1 1 d . . . C9 C 0.33641(14) 0.8713(2) 0.27109(14) 0.0325(5) Uani 1 1 d . . . H9A H 0.4002 0.8344 0.2695 0.049 Uiso 1 1 calc R . . H9B H 0.3071 0.8436 0.3267 0.049 Uiso 1 1 calc R . . H9C H 0.3402 0.9669 0.2696 0.049 Uiso 1 1 calc R . . C10 C 0.27752(15) 0.6726(2) 0.18690(15) 0.0359(5) Uani 1 1 d . . . H10A H 0.2506 0.6387 0.2421 0.054 Uiso 1 1 calc R . . H10B H 0.3427 0.6416 0.1833 0.054 Uiso 1 1 calc R . . H10C H 0.2398 0.6418 0.1340 0.054 Uiso 1 1 calc R . . C11 C 0.32320(16) 0.8696(3) 0.10366(16) 0.0431(6) Uani 1 1 d . . . H11A H 0.2854 0.8409 0.0502 0.065 Uiso 1 1 calc R . . H11B H 0.3869 0.8326 0.1019 0.065 Uiso 1 1 calc R . . H11C H 0.3272 0.9652 0.1041 0.065 Uiso 1 1 calc R . . C12 C 0.00808(13) 1.1204(2) 0.06747(12) 0.0305(4) Uani 1 1 d . . . C13 C -0.0079(2) 1.2452(2) 0.12189(16) 0.0506(6) Uani 1 1 d . . . H13A H 0.0524 1.2749 0.1497 0.076 Uiso 1 1 calc R . . H13B H -0.0524 1.2271 0.1692 0.076 Uiso 1 1 calc R . . H13C H -0.0340 1.3133 0.0815 0.076 Uiso 1 1 calc R . . C14 C -0.08610(19) 1.0785(3) 0.0203(2) 0.0597(8) Uani 1 1 d . . . H14A H -0.1324 1.0602 0.0660 0.090 Uiso 1 1 calc R . . H14B H -0.0762 0.9997 -0.0156 0.090 Uiso 1 1 calc R . . H14C H -0.1098 1.1490 -0.0194 0.090 Uiso 1 1 calc R . . C15 C 0.07730(18) 1.1536(3) -0.00523(15) 0.0469(6) Uani 1 1 d . . . H15A H 0.0900 1.0751 -0.0406 0.070 Uiso 1 1 calc R . . H15B H 0.1365 1.1858 0.0235 0.070 Uiso 1 1 calc R . . H15C H 0.0498 1.2212 -0.0453 0.070 Uiso 1 1 calc R . . C16 C -0.04188(13) 0.82417(19) 0.33308(13) 0.0268(4) Uani 1 1 d . . . H16A H -0.0218 0.8581 0.3936 0.032 Uiso 1 1 calc R . . H16B H -0.1074 0.8540 0.3190 0.032 Uiso 1 1 calc R . . C17 C -0.06274(13) 0.6283(2) 0.24239(12) 0.0312(4) Uani 1 1 d . . . H17A H -0.0094 0.6436 0.2038 0.047 Uiso 1 1 calc R . . H17B H -0.1188 0.6737 0.2170 0.047 Uiso 1 1 calc R . . H17C H -0.0756 0.5344 0.2454 0.047 Uiso 1 1 calc R . . C18 C -0.10390(12) 0.6220(2) 0.40063(12) 0.0266(4) Uani 1 1 d . . . H18 H -0.0958 0.5250 0.3977 0.032 Uiso 1 1 calc R . . C19 C -0.20949(13) 0.6483(2) 0.38632(13) 0.0314(5) Uani 1 1 d . . . H19A H -0.2221 0.7428 0.3932 0.038 Uiso 1 1 calc R . . H19B H -0.2309 0.6219 0.3244 0.038 Uiso 1 1 calc R . . C20 C -0.26338(14) 0.5712(2) 0.45544(15) 0.0354(5) Uani 1 1 d . . . H20A H -0.2563 0.4765 0.4436 0.042 Uiso 1 1 calc R . . H20B H -0.3315 0.5929 0.4486 0.042 Uiso 1 1 calc R . . C21 C -0.22786(13) 0.6008(2) 0.55203(13) 0.0341(5) Uani 1 1 d . . . H21A H -0.2605 0.5431 0.5943 0.041 Uiso 1 1 calc R . . H21B H -0.2434 0.6924 0.5670 0.041 Uiso 1 1 calc R . . C22 C -0.12083(14) 0.5805(2) 0.56438(14) 0.0330(5) Uani 1 1 d . . . H22A H -0.0992 0.6060 0.6264 0.040 Uiso 1 1 calc R . . H22B H -0.1054 0.4871 0.5558 0.040 Uiso 1 1 calc R . . C23 C -0.07084(12) 0.6630(2) 0.49581(12) 0.0261(4) Uani 1 1 d . . . H23 H -0.0886 0.7566 0.5047 0.031 Uiso 1 1 calc R . . C24 C 0.07653(13) 0.6924(2) 0.57592(13) 0.0277(4) Uani 1 1 d . . . H24 H 0.0370 0.7235 0.6214 0.033 Uiso 1 1 calc R . . C25 C 0.17607(13) 0.6935(2) 0.59725(13) 0.0268(4) Uani 1 1 d . . . C26 C 0.20833(14) 0.7509(2) 0.67969(13) 0.0301(4) Uani 1 1 d . . . H26 H 0.1641 0.7904 0.7176 0.036 Uiso 1 1 calc R . . C27 C 0.30232(13) 0.7508(2) 0.70601(13) 0.0296(4) Uani 1 1 d . . . C28 C 0.36325(13) 0.6826(2) 0.64983(13) 0.0291(4) Uani 1 1 d . . . H28 H 0.4280 0.6772 0.6694 0.035 Uiso 1 1 calc R . . C29 C 0.33719(12) 0.6230(2) 0.56904(12) 0.0265(4) Uani 1 1 d . . . C30 C 0.24004(13) 0.63507(19) 0.53823(12) 0.0254(4) Uani 1 1 d . . . C31 C 0.34296(14) 0.8177(2) 0.79197(14) 0.0332(5) Uani 1 1 d . . . C32 C 0.38650(18) 0.7149(3) 0.85726(15) 0.0459(6) Uani 1 1 d . . . H32A H 0.4358 0.6664 0.8271 0.069 Uiso 1 1 calc R . . H32B H 0.3372 0.6542 0.8752 0.069 Uiso 1 1 calc R . . H32C H 0.4143 0.7585 0.9111 0.069 Uiso 1 1 calc R . . C33 C 0.26773(16) 0.8921(2) 0.84185(14) 0.0392(5) Uani 1 1 d . . . H33A H 0.2201 0.8307 0.8623 0.059 Uiso 1 1 calc R . . H33B H 0.2374 0.9565 0.8010 0.059 Uiso 1 1 calc R . . H33C H 0.2974 0.9370 0.8943 0.059 Uiso 1 1 calc R . . C34 C 0.41894(17) 0.9156(3) 0.76585(17) 0.0473(6) Uani 1 1 d . . . H34A H 0.3906 0.9815 0.7250 0.071 Uiso 1 1 calc R . . H34B H 0.4692 0.8695 0.7354 0.071 Uiso 1 1 calc R . . H34C H 0.4456 0.9584 0.8205 0.071 Uiso 1 1 calc R . . C35 C 0.40801(13) 0.54772(19) 0.51345(14) 0.0274(4) Uani 1 1 d . . . C36 C 0.37118(15) 0.4088(2) 0.49356(17) 0.0382(5) Uani 1 1 d . . . H36A H 0.3634 0.3624 0.5507 0.057 Uiso 1 1 calc R . . H36B H 0.4166 0.3618 0.4575 0.057 Uiso 1 1 calc R . . H36C H 0.3101 0.4138 0.4598 0.057 Uiso 1 1 calc R . . C37 C 0.42275(14) 0.6189(2) 0.42383(13) 0.0355(4) Uani 1 1 d . . . H37A H 0.4696 0.5716 0.3896 0.053 Uiso 1 1 calc R . . H37B H 0.4454 0.7078 0.4363 0.053 Uiso 1 1 calc R . . H37C H 0.3627 0.6226 0.3883 0.053 Uiso 1 1 calc R . . C38 C 0.50455(13) 0.5340(2) 0.56406(15) 0.0339(5) Uani 1 1 d . . . H38A H 0.5463 0.4803 0.5283 0.051 Uiso 1 1 calc R . . H38B H 0.4963 0.4922 0.6228 0.051 Uiso 1 1 calc R . . H38C H 0.5327 0.6207 0.5735 0.051 Uiso 1 1 calc R . . C39 C 0.3161(2) 0.2644(4) 0.2004(3) 0.0858(10) Uani 1 1 d . . . H39A H 0.3730 0.2111 0.2111 0.129 Uiso 1 1 calc R . . H39B H 0.2603 0.2076 0.1972 0.129 Uiso 1 1 calc R . . H39C H 0.3106 0.3268 0.2502 0.129 Uiso 1 1 calc R . . C40 C 0.3226(3) 0.3374(3) 0.1129(3) 0.0864(12) Uani 1 1 d . . . H40A H 0.2607 0.3793 0.0986 0.104 Uiso 1 1 calc R . . H40B H 0.3698 0.4080 0.1221 0.104 Uiso 1 1 calc R . . C41 C 0.3488(2) 0.2587(3) 0.0328(2) 0.0672(8) Uani 1 1 d . . . H41A H 0.3031 0.1861 0.0242 0.081 Uiso 1 1 calc R . . H41B H 0.4121 0.2199 0.0454 0.081 Uiso 1 1 calc R . . C42 C 0.3504(3) 0.3365(4) -0.0534(3) 0.0864(11) Uani 1 1 d . . . H42A H 0.2878 0.3782 -0.0641 0.104 Uiso 1 1 calc R . . H42B H 0.3977 0.4073 -0.0449 0.104 Uiso 1 1 calc R . . C43 C 0.3723(3) 0.2625(4) -0.1336(3) 0.0991(12) Uani 1 1 d . . . H43A H 0.3257 0.1909 -0.1416 0.119 Uiso 1 1 calc R . . H43B H 0.4354 0.2220 -0.1233 0.119 Uiso 1 1 calc R . . C44 C 0.3724(3) 0.3418(4) -0.2213(3) 0.0938(12) Uani 1 1 d . . . H44A H 0.4222 0.4083 -0.2164 0.141 Uiso 1 1 calc R . . H44B H 0.3109 0.3845 -0.2316 0.141 Uiso 1 1 calc R . . H44C H 0.3841 0.2835 -0.2721 0.141 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 0.0216(2) 0.0248(3) 0.0243(3) 0.0007(2) 0.0019(2) -0.0002(2) O1 0.0216(6) 0.0300(7) 0.0268(7) 0.0044(6) -0.0009(5) -0.0013(6) N1 0.0242(8) 0.0271(8) 0.0242(8) -0.0009(7) 0.0027(6) -0.0039(7) C1 0.0344(11) 0.0280(11) 0.0403(12) -0.0023(9) 0.0012(10) -0.0001(9) O2 0.0237(6) 0.0325(8) 0.0255(7) -0.0016(6) 0.0010(5) 0.0043(5) N2 0.0208(7) 0.0310(9) 0.0278(8) 0.0023(7) 0.0012(6) 0.0024(6) C2 0.0260(9) 0.0239(10) 0.0254(10) -0.0002(8) -0.0039(8) -0.0032(8) C3 0.0244(9) 0.0263(10) 0.0257(9) -0.0020(8) -0.0008(8) -0.0003(8) C4 0.0291(10) 0.0326(11) 0.0232(9) 0.0023(8) 0.0026(8) -0.0031(8) C5 0.0302(10) 0.0285(10) 0.0252(10) 0.0009(8) -0.0024(8) -0.0011(8) C6 0.0240(9) 0.0283(10) 0.0312(10) 0.0017(8) -0.0013(8) 0.0021(8) C7 0.0260(9) 0.0273(11) 0.0265(10) -0.0010(8) -0.0015(8) -0.0022(8) C8 0.0234(9) 0.0355(11) 0.0257(10) 0.0016(9) 0.0025(8) 0.0003(8) C9 0.0275(10) 0.0334(11) 0.0365(11) -0.0004(9) 0.0015(9) -0.0027(9) C10 0.0328(11) 0.0394(12) 0.0354(11) -0.0074(9) 0.0008(9) 0.0060(9) C11 0.0334(11) 0.0588(16) 0.0381(12) 0.0085(11) 0.0106(10) 0.0102(11) C12 0.0318(9) 0.0312(10) 0.0282(9) 0.0041(9) -0.0027(8) 0.0023(9) C13 0.0739(17) 0.0381(13) 0.0407(13) 0.0070(11) 0.0123(12) 0.0154(13) C14 0.0507(14) 0.0555(17) 0.0702(18) 0.0218(14) -0.0269(14) -0.0057(12) C15 0.0554(14) 0.0510(15) 0.0348(12) 0.0172(11) 0.0072(11) 0.0122(12) C16 0.0227(9) 0.0279(11) 0.0298(10) 0.0006(8) -0.0017(8) 0.0001(8) C17 0.0279(9) 0.0384(11) 0.0272(9) -0.0034(10) 0.0001(8) -0.0060(9) C18 0.0230(8) 0.0287(10) 0.0285(9) 0.0028(9) 0.0030(7) -0.0029(9) C19 0.0215(9) 0.0404(13) 0.0322(10) -0.0002(9) 0.0007(8) -0.0039(8) C20 0.0236(10) 0.0397(12) 0.0433(12) 0.0041(10) 0.0068(9) -0.0048(9) C21 0.0269(9) 0.0409(13) 0.0348(10) 0.0072(10) 0.0066(8) -0.0006(9) C22 0.0307(10) 0.0353(12) 0.0333(11) 0.0082(9) 0.0051(8) 0.0036(9) C23 0.0195(8) 0.0322(10) 0.0269(9) 0.0020(8) 0.0031(7) 0.0040(7) C24 0.0285(10) 0.0306(10) 0.0241(9) 0.0021(8) 0.0022(8) 0.0042(8) C25 0.0237(9) 0.0310(10) 0.0256(10) 0.0024(8) 0.0008(7) 0.0029(8) C26 0.0294(10) 0.0344(11) 0.0265(10) 0.0013(9) 0.0023(8) 0.0061(9) C27 0.0294(10) 0.0334(11) 0.0257(10) 0.0039(9) -0.0009(8) 0.0021(9) C28 0.0225(9) 0.0325(10) 0.0319(10) 0.0048(9) -0.0019(8) 0.0007(8) C29 0.0247(8) 0.0268(9) 0.0279(9) 0.0046(9) 0.0016(7) 0.0003(8) C30 0.0270(9) 0.0251(10) 0.0241(9) 0.0027(8) -0.0005(7) 0.0011(8) C31 0.0324(10) 0.0378(12) 0.0292(11) -0.0008(9) -0.0009(9) 0.0006(9) C32 0.0499(13) 0.0534(15) 0.0331(11) -0.0012(11) -0.0119(10) 0.0098(11) C33 0.0408(12) 0.0468(14) 0.0298(11) -0.0031(10) -0.0015(10) 0.0028(10) C34 0.0434(13) 0.0493(14) 0.0488(14) -0.0099(12) -0.0009(12) -0.0061(11) C35 0.0238(9) 0.0267(10) 0.0319(10) 0.0031(8) 0.0014(8) 0.0020(8) C36 0.0285(10) 0.0308(11) 0.0552(14) 0.0002(10) 0.0022(10) 0.0019(9) C37 0.0324(10) 0.0414(12) 0.0331(10) 0.0044(10) 0.0062(8) 0.0050(10) C38 0.0232(9) 0.0371(12) 0.0413(12) 0.0041(9) 0.0020(9) 0.0023(9) C39 0.072(2) 0.071(2) 0.115(3) -0.007(2) 0.020(2) -0.0055(18) C40 0.079(2) 0.0499(19) 0.127(3) -0.013(2) -0.028(2) 0.0066(17) C41 0.0478(15) 0.0617(18) 0.092(2) 0.0126(18) -0.0042(15) -0.0081(14) C42 0.097(3) 0.0550(19) 0.105(3) -0.0024(19) -0.023(2) -0.0095(18) C43 0.103(3) 0.068(2) 0.127(3) -0.005(3) 0.020(3) -0.023(2) C44 0.111(3) 0.082(2) 0.086(3) 0.001(2) -0.008(2) -0.033(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 1.7665(15) . ? Al1 O2 1.8339(13) . ? Al1 C1 1.968(2) . ? Al1 N2 1.9801(17) . ? Al1 N1 2.2083(16) . ? O1 C2 1.349(2) . ? N1 C17 1.479(2) . ? N1 C18 1.488(2) . ? N1 C16 1.492(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C30 1.309(2) . ? N2 C24 1.306(2) . ? N2 C23 1.491(2) . ? C2 C7 1.404(3) . ? C2 C3 1.410(3) . ? C3 C4 1.403(3) . ? C3 C8 1.545(3) . ? C4 C5 1.393(3) . ? C4 H4 0.9500 . ? C5 C6 1.400(3) . ? C5 C12 1.527(3) . ? C6 C7 1.386(3) . ? C6 H6 0.9500 . ? C7 C16 1.499(3) . ? C8 C11 1.528(3) . ? C8 C9 1.531(3) . ? C8 C10 1.539(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.526(3) . ? C12 C13 1.532(3) . ? C12 C14 1.538(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.524(3) . ? C18 C19 1.524(2) . ? C18 H18 1.0000 . ? C19 C20 1.524(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.525(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.532(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.520(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23 1.0000 . ? C24 C25 1.430(3) . ? C24 H24 0.9500 . ? C25 C26 1.412(3) . ? C25 C30 1.418(3) . ? C26 C27 1.370(3) . ? C26 H26 0.9500 . ? C27 C28 1.410(3) . ? C27 C31 1.534(3) . ? C28 C29 1.378(3) . ? C28 H28 0.9500 . ? C29 C30 1.435(2) . ? C29 C35 1.533(3) . ? C31 C33 1.527(3) . ? C31 C34 1.533(3) . ? C31 C32 1.538(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C38 1.535(3) . ? C35 C37 1.536(3) . ? C35 C36 1.538(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 C40 1.501(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.494(5) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.505(5) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.454(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.531(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? 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 O2 94.43(6) . . ? O1 Al1 C1 119.33(9) . . ? O2 Al1 C1 96.93(8) . . ? O1 Al1 N2 117.78(7) . . ? O2 Al1 N2 88.62(6) . . ? C1 Al1 N2 121.87(9) . . ? O1 Al1 N1 87.73(6) . . ? O2 Al1 N1 165.72(6) . . ? C1 Al1 N1 94.27(8) . . ? N2 Al1 N1 77.93(6) . . ? C2 O1 Al1 134.46(11) . . ? C17 N1 C18 110.62(14) . . ? C17 N1 C16 109.31(16) . . ? C18 N1 C16 112.41(16) . . ? C17 N1 Al1 113.73(12) . . ? C18 N1 Al1 103.13(11) . . ? C16 N1 Al1 107.55(11) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C30 O2 Al1 133.00(12) . . ? C24 N2 C23 115.88(16) . . ? C24 N2 Al1 123.22(13) . . ? C23 N2 Al1 119.57(11) . . ? O1 C2 C7 119.06(17) . . ? O1 C2 C3 121.63(16) . . ? C7 C2 C3 119.30(17) . . ? C4 C3 C2 117.56(17) . . ? C4 C3 C8 121.00(17) . . ? C2 C3 C8 121.44(16) . . ? C5 C4 C3 124.16(18) . . ? C5 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? C4 C5 C6 116.34(18) . . ? C4 C5 C12 123.43(18) . . ? C6 C5 C12 120.20(17) . . ? C7 C6 C5 121.70(18) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C2 120.74(18) . . ? C6 C7 C16 120.42(17) . . ? C2 C7 C16 118.82(17) . . ? C11 C8 C9 108.14(17) . . ? C11 C8 C10 106.94(18) . . ? C9 C8 C10 109.56(17) . . ? C11 C8 C3 112.29(17) . . ? C9 C8 C3 109.63(16) . . ? C10 C8 C3 110.19(16) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C5 112.76(17) . . ? C15 C12 C13 107.5(2) . . ? C5 C12 C13 108.53(16) . . ? C15 C12 C14 108.27(19) . . ? C5 C12 C14 110.73(18) . . ? C13 C12 C14 109.0(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C7 110.85(16) . . ? N1 C16 H16A 109.5 . . ? C7 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? C7 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C23 109.25(14) . . ? N1 C18 C19 117.93(15) . . ? C23 C18 C19 109.78(15) . . ? N1 C18 H18 106.4 . . ? C23 C18 H18 106.4 . . ? C19 C18 H18 106.4 . . ? C20 C19 C18 109.45(16) . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19B 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C19 C20 C21 111.86(16) . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 111.57(17) . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C21 109.42(16) . . ? C23 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C23 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? N2 C23 C22 115.13(15) . . ? N2 C23 C18 106.79(14) . . ? C22 C23 C18 109.34(16) . . ? N2 C23 H23 108.5 . . ? C22 C23 H23 108.5 . . ? C18 C23 H23 108.5 . . ? N2 C24 C25 126.84(18) . . ? N2 C24 H24 116.6 . . ? C25 C24 H24 116.6 . . ? C26 C25 C30 121.13(17) . . ? C26 C25 C24 118.12(17) . . ? C30 C25 C24 120.72(17) . . ? C27 C26 C25 121.19(19) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 116.44(18) . . ? C26 C27 C31 123.99(18) . . ? C28 C27 C31 119.57(17) . . ? C29 C28 C27 125.72(17) . . ? C29 C28 H28 117.1 . . ? C27 C28 H28 117.1 . . ? C28 C29 C30 116.97(17) . . ? C28 C29 C35 122.15(16) . . ? C30 C29 C35 120.89(16) . . ? O2 C30 C25 120.44(16) . . ? O2 C30 C29 121.50(17) . . ? C25 C30 C29 118.03(16) . . ? C33 C31 C34 107.96(19) . . ? C33 C31 C27 112.33(16) . . ? C34 C31 C27 108.90(17) . . ? C33 C31 C32 107.84(18) . . ? C34 C31 C32 109.86(19) . . ? C27 C31 C32 109.93(18) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C35 C38 111.94(16) . . ? C29 C35 C37 110.04(16) . . ? C38 C35 C37 108.20(16) . . ? C29 C35 C36 110.06(17) . . ? C38 C35 C36 107.19(16) . . ? C37 C35 C36 109.33(18) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 H39A 109.5 . . ? C40 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C40 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C39 116.3(3) . . ? C41 C40 H40A 108.2 . . ? C39 C40 H40A 108.2 . . ? C41 C40 H40B 108.2 . . ? C39 C40 H40B 108.2 . . ? H40A C40 H40B 107.4 . . ? C40 C41 C42 113.7(3) . . ? C40 C41 H41A 108.8 . . ? C42 C41 H41A 108.8 . . ? C40 C41 H41B 108.8 . . ? C42 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? C43 C42 C41 115.4(3) . . ? C43 C42 H42A 108.4 . . ? C41 C42 H42A 108.4 . . ? C43 C42 H42B 108.4 . . ? C41 C42 H42B 108.4 . . ? H42A C42 H42B 107.5 . . ? C42 C43 C44 115.1(4) . . ? C42 C43 H43A 108.5 . . ? C44 C43 H43A 108.5 . . ? C42 C43 H43B 108.5 . . ? C44 C43 H43B 108.5 . . ? H43A C43 H43B 107.5 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.308 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.050 data_Al(1)Me _database_code_depnum_ccdc_archive 'CCDC 917782' #TrackingRef 'Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H59 Al N2 O2' _chemical_formula_weight 602.85 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' O O 0.0106 0.0060 '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' 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 P21/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 11.8730(6) _cell_length_b 10.6560(7) _cell_length_c 28.8840(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.668(5) _cell_angle_gamma 90.00 _cell_volume 3642.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35091 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20442 _diffrn_reflns_av_R_equivalents 0.1590 _diffrn_reflns_av_sigmaI/netI 0.1794 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6315 _reflns_number_gt 3169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0000P)^2^+13.8944P] 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 6315 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2204 _refine_ls_R_factor_gt 0.1147 _refine_ls_wR_factor_ref 0.2450 _refine_ls_wR_factor_gt 0.2056 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.38011(16) 0.94581(18) 0.26081(6) 0.0337(5) Uani 1 1 d . . . O1 O 0.4318(3) 1.0864(4) 0.23779(13) 0.0325(10) Uani 1 1 d . . . N1 N 0.2905(4) 0.9080(4) 0.19346(17) 0.0333(13) Uani 1 1 d . . . C1 C 0.2437(5) 0.9489(7) 0.2952(2) 0.0462(17) Uani 1 1 d . . . H1A H 0.1812 0.9864 0.2757 0.069 Uiso 1 1 calc R . . H1B H 0.2584 0.9989 0.3235 0.069 Uiso 1 1 calc R . . H1C H 0.2238 0.8630 0.3035 0.069 Uiso 1 1 calc R . . O2 O 0.4839(3) 0.9490(4) 0.31140(13) 0.0397(11) Uani 1 1 d . . . N2 N 0.4493(4) 0.7859(5) 0.24276(17) 0.0376(13) Uani 1 1 d . . . C2 C 0.4316(5) 1.1394(5) 0.1954(2) 0.0317(15) Uani 1 1 d . . . C3 C 0.5221(5) 1.2159(5) 0.1839(2) 0.0303(15) Uani 1 1 d . . . C4 C 0.5168(6) 1.2629(6) 0.1391(2) 0.0415(17) Uani 1 1 d . . . H4 H 0.5779 1.3136 0.1309 0.050 Uiso 1 1 calc R . . C5 C 0.4297(6) 1.2417(6) 0.1053(2) 0.0457(18) Uani 1 1 d . . . C6 C 0.3415(6) 1.1660(6) 0.1185(2) 0.0455(18) Uani 1 1 d . . . H6 H 0.2799 1.1483 0.0964 0.055 Uiso 1 1 calc R . . C7 C 0.3412(5) 1.1164(6) 0.1622(2) 0.0364(16) Uani 1 1 d . . . C8 C 0.6235(5) 1.2418(6) 0.2187(2) 0.0336(15) Uani 1 1 d . . . C9 C 0.5875(6) 1.3017(6) 0.2634(2) 0.0460(18) Uani 1 1 d . . . H9A H 0.5372 1.2443 0.2783 0.069 Uiso 1 1 calc R . . H9B H 0.5477 1.3806 0.2558 0.069 Uiso 1 1 calc R . . H9C H 0.6545 1.3186 0.2845 0.069 Uiso 1 1 calc R . . C10 C 0.7103(5) 1.3300(6) 0.1993(2) 0.0392(16) Uani 1 1 d . . . H10A H 0.6745 1.4110 0.1914 0.059 Uiso 1 1 calc R . . H10B H 0.7380 1.2927 0.1713 0.059 Uiso 1 1 calc R . . H10C H 0.7738 1.3427 0.2227 0.059 Uiso 1 1 calc R . . C11 C 0.6854(5) 1.1151(6) 0.2313(2) 0.0426(17) Uani 1 1 d . . . H11A H 0.7093 1.0763 0.2029 0.064 Uiso 1 1 calc R . . H11B H 0.6338 1.0584 0.2459 0.064 Uiso 1 1 calc R . . H11C H 0.7518 1.1314 0.2529 0.064 Uiso 1 1 calc R . . C12 C 0.4272(7) 1.2937(9) 0.0555(3) 0.072(3) Uani 1 1 d . . . C13 C 0.4099(14) 1.1828(13) 0.0210(3) 0.186(8) Uani 1 1 d . . . H13A H 0.4494 1.1086 0.0341 0.278 Uiso 1 1 calc R . . H13B H 0.4402 1.2053 -0.0085 0.278 Uiso 1 1 calc R . . H13C H 0.3290 1.1645 0.0155 0.278 Uiso 1 1 calc R . . C14 C 0.3316(8) 1.3906(13) 0.0488(4) 0.150(6) Uani 1 1 d . . . H14A H 0.3311 1.4274 0.0177 0.225 Uiso 1 1 calc R . . H14B H 0.3436 1.4568 0.0723 0.225 Uiso 1 1 calc R . . H14C H 0.2590 1.3493 0.0523 0.225 Uiso 1 1 calc R . . C15 C 0.5363(7) 1.3571(7) 0.0461(2) 0.061(2) Uani 1 1 d . . . H15A H 0.5991 1.2983 0.0523 0.091 Uiso 1 1 calc R . . H15B H 0.5479 1.4306 0.0664 0.091 Uiso 1 1 calc R . . H15C H 0.5328 1.3838 0.0136 0.091 Uiso 1 1 calc R . . C16 C 0.2490(5) 1.0293(6) 0.1741(2) 0.0405(17) Uani 1 1 d . . . H16A H 0.2036 1.0710 0.1969 0.049 Uiso 1 1 calc R . . H16B H 0.1985 1.0132 0.1457 0.049 Uiso 1 1 calc R . . C17 C 0.1903(5) 0.8234(6) 0.1966(2) 0.0471(18) Uani 1 1 d . . . H17A H 0.1583 0.8020 0.1652 0.071 Uiso 1 1 calc R . . H17B H 0.1330 0.8664 0.2133 0.071 Uiso 1 1 calc R . . H17C H 0.2141 0.7465 0.2132 0.071 Uiso 1 1 calc R . . C18 C 0.3780(5) 0.8531(6) 0.1657(2) 0.0373(16) Uani 1 1 d . . . H18 H 0.4376 0.9186 0.1632 0.045 Uiso 1 1 calc R . . C19 C 0.3413(6) 0.8098(8) 0.1166(2) 0.054(2) Uani 1 1 d . . . H19A H 0.3026 0.8789 0.0988 0.064 Uiso 1 1 calc R . . H19B H 0.2884 0.7382 0.1175 0.064 Uiso 1 1 calc R . . C20 C 0.4479(7) 0.7698(9) 0.0936(3) 0.075(3) Uani 1 1 d . . . H20A H 0.4259 0.7373 0.0621 0.090 Uiso 1 1 calc R . . H20B H 0.4969 0.8440 0.0904 0.090 Uiso 1 1 calc R . . C21 C 0.5138(7) 0.6696(10) 0.1216(3) 0.086(3) Uani 1 1 d . . . H21A H 0.5853 0.6526 0.1073 0.103 Uiso 1 1 calc R . . H21B H 0.4692 0.5910 0.1206 0.103 Uiso 1 1 calc R . . C22 C 0.5405(6) 0.7091(8) 0.1721(2) 0.064(2) Uani 1 1 d . . . H22A H 0.5787 0.6393 0.1898 0.077 Uiso 1 1 calc R . . H22B H 0.5924 0.7820 0.1735 0.077 Uiso 1 1 calc R . . C23 C 0.4332(6) 0.7435(6) 0.1938(2) 0.0432(17) Uani 1 1 d . . . H23 H 0.3807 0.6700 0.1918 0.052 Uiso 1 1 calc R . . C24 C 0.4912(5) 0.7066(6) 0.2736(2) 0.0393(16) Uani 1 1 d . . . H24 H 0.5030 0.6236 0.2631 0.047 Uiso 1 1 calc R . . C25 C 0.5212(5) 0.7301(6) 0.3212(2) 0.0367(16) Uani 1 1 d . . . C26 C 0.5616(5) 0.6317(7) 0.3499(2) 0.0462(18) Uani 1 1 d . . . H26 H 0.5618 0.5491 0.3375 0.055 Uiso 1 1 calc R . . C27 C 0.6009(6) 0.6503(8) 0.3950(3) 0.052(2) Uani 1 1 d . . . C28 C 0.6025(6) 0.7748(8) 0.4119(2) 0.053(2) Uani 1 1 d . . . H28 H 0.6307 0.7894 0.4431 0.063 Uiso 1 1 calc R . . C29 C 0.5645(5) 0.8777(7) 0.3848(2) 0.0425(17) Uani 1 1 d . . . C30 C 0.5203(5) 0.8550(6) 0.3386(2) 0.0339(15) Uani 1 1 d . . . C31 C 0.6442(6) 0.5410(9) 0.4255(3) 0.066(2) Uani 1 1 d . . . C32 C 0.5521(8) 0.4415(10) 0.4274(4) 0.108(4) Uani 1 1 d . . . H32A H 0.5799 0.3728 0.4478 0.163 Uiso 1 1 calc R . . H32B H 0.5322 0.4088 0.3961 0.163 Uiso 1 1 calc R . . H32C H 0.4852 0.4790 0.4396 0.163 Uiso 1 1 calc R . . C33 C 0.7480(7) 0.4823(8) 0.4056(3) 0.084(3) Uani 1 1 d . . . H33A H 0.7258 0.4461 0.3750 0.126 Uiso 1 1 calc R . . H33B H 0.7790 0.4162 0.4265 0.126 Uiso 1 1 calc R . . H33C H 0.8055 0.5471 0.4025 0.126 Uiso 1 1 calc R . . C34 C 0.6794(8) 0.5822(9) 0.4756(3) 0.100(4) Uani 1 1 d . . . H34A H 0.7465 0.6358 0.4759 0.151 Uiso 1 1 calc R . . H34B H 0.6967 0.5080 0.4949 0.151 Uiso 1 1 calc R . . H34C H 0.6174 0.6291 0.4879 0.151 Uiso 1 1 calc R . . C35 C 0.5740(6) 1.0119(7) 0.4045(2) 0.0507(19) Uani 1 1 d . . . C36 C 0.4548(6) 1.0725(7) 0.4039(2) 0.059(2) Uani 1 1 d . . . H36A H 0.4091 1.0264 0.4249 0.089 Uiso 1 1 calc R . . H36B H 0.4180 1.0693 0.3723 0.089 Uiso 1 1 calc R . . H36C H 0.4622 1.1601 0.4140 0.089 Uiso 1 1 calc R . . C37 C 0.6501(6) 1.0899(7) 0.3750(2) 0.057(2) Uani 1 1 d . . . H37A H 0.6148 1.0967 0.3433 0.085 Uiso 1 1 calc R . . H37B H 0.7238 1.0487 0.3745 0.085 Uiso 1 1 calc R . . H37C H 0.6603 1.1739 0.3885 0.085 Uiso 1 1 calc R . . C38 C 0.6263(7) 1.0152(9) 0.4550(2) 0.080(3) Uani 1 1 d . . . H38A H 0.7024 0.9788 0.4565 0.121 Uiso 1 1 calc R . . H38B H 0.5791 0.9666 0.4747 0.121 Uiso 1 1 calc R . . H38C H 0.6309 1.1023 0.4659 0.121 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 0.0324(11) 0.0285(11) 0.0402(11) 0.0022(9) 0.0026(8) -0.0016(9) O1 0.032(2) 0.030(2) 0.036(2) 0.0036(19) 0.0035(18) -0.0011(19) N1 0.028(3) 0.024(3) 0.047(3) 0.003(2) 0.001(2) -0.004(2) C1 0.040(4) 0.047(4) 0.054(4) 0.004(4) 0.012(3) -0.006(4) O2 0.044(3) 0.038(3) 0.036(2) 0.004(2) -0.0044(19) -0.001(2) N2 0.034(3) 0.032(3) 0.046(3) -0.002(3) -0.001(3) -0.006(3) C2 0.038(4) 0.020(3) 0.038(4) -0.004(3) 0.008(3) 0.004(3) C3 0.029(4) 0.023(3) 0.039(4) 0.001(3) 0.001(3) -0.006(3) C4 0.037(4) 0.041(4) 0.047(4) 0.000(3) 0.002(3) -0.008(3) C5 0.047(5) 0.048(5) 0.041(4) 0.014(3) -0.005(3) -0.007(4) C6 0.041(4) 0.040(4) 0.053(5) 0.005(3) -0.009(3) -0.005(4) C7 0.033(4) 0.029(4) 0.047(4) 0.003(3) -0.001(3) -0.002(3) C8 0.032(4) 0.032(4) 0.036(4) 0.001(3) 0.000(3) 0.003(3) C9 0.044(4) 0.047(5) 0.048(4) -0.010(3) 0.007(3) -0.001(4) C10 0.034(4) 0.034(4) 0.050(4) 0.000(3) 0.003(3) -0.006(3) C11 0.029(4) 0.041(4) 0.058(4) -0.004(3) 0.000(3) 0.005(3) C12 0.076(6) 0.092(7) 0.045(5) 0.023(5) -0.008(4) -0.044(6) C13 0.317(19) 0.208(14) 0.031(5) -0.010(7) 0.011(8) -0.198(15) C14 0.059(7) 0.219(15) 0.167(11) 0.134(11) -0.023(7) -0.006(8) C15 0.084(6) 0.059(5) 0.040(4) 0.005(4) 0.007(4) -0.012(5) C16 0.035(4) 0.039(4) 0.047(4) -0.003(3) -0.002(3) 0.004(3) C17 0.032(4) 0.042(4) 0.067(5) 0.002(4) 0.000(3) -0.012(3) C18 0.028(4) 0.043(4) 0.041(4) -0.010(3) 0.004(3) -0.001(3) C19 0.043(5) 0.069(6) 0.047(4) -0.018(4) -0.005(3) 0.003(4) C20 0.067(6) 0.102(7) 0.054(5) -0.034(5) -0.001(4) 0.012(5) C21 0.069(6) 0.117(8) 0.069(6) -0.052(6) -0.012(5) 0.034(6) C22 0.059(5) 0.066(6) 0.065(5) -0.023(4) -0.009(4) 0.026(4) C23 0.044(4) 0.033(4) 0.051(4) -0.016(3) -0.004(3) 0.004(3) C24 0.034(4) 0.027(4) 0.057(5) 0.007(3) -0.003(3) -0.007(3) C25 0.029(4) 0.033(4) 0.048(4) 0.002(3) 0.000(3) -0.002(3) C26 0.039(4) 0.041(4) 0.058(5) 0.015(4) 0.004(3) -0.001(3) C27 0.039(4) 0.060(6) 0.058(5) 0.027(4) 0.008(4) 0.006(4) C28 0.039(4) 0.073(6) 0.046(4) 0.011(4) 0.000(3) 0.012(4) C29 0.034(4) 0.053(5) 0.040(4) 0.002(3) 0.004(3) 0.006(4) C30 0.024(4) 0.039(4) 0.040(4) 0.006(3) 0.006(3) 0.000(3) C31 0.045(5) 0.089(7) 0.065(5) 0.029(5) 0.005(4) 0.012(5) C32 0.082(7) 0.096(8) 0.149(9) 0.079(7) 0.014(6) 0.017(6) C33 0.080(7) 0.088(7) 0.083(6) 0.032(5) 0.003(5) 0.036(6) C34 0.110(8) 0.118(9) 0.074(6) 0.054(6) 0.013(6) 0.054(7) C35 0.044(5) 0.064(5) 0.044(4) -0.007(4) -0.001(3) 0.000(4) C36 0.052(5) 0.065(6) 0.059(5) -0.010(4) -0.001(4) 0.011(4) C37 0.054(5) 0.050(5) 0.065(5) -0.021(4) 0.003(4) -0.012(4) C38 0.072(6) 0.111(8) 0.055(5) -0.026(5) -0.016(4) 0.029(5) _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 1.769(4) . ? Al1 O2 1.834(4) . ? Al1 C1 1.968(6) . ? Al1 N2 1.980(5) . ? Al1 N1 2.178(5) . ? O1 C2 1.349(7) . ? N1 C16 1.478(7) . ? N1 C18 1.484(7) . ? N1 C17 1.501(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C30 1.324(7) . ? N2 C24 1.298(7) . ? N2 C23 1.481(8) . ? C2 C7 1.402(8) . ? C2 C3 1.409(8) . ? C3 C4 1.386(8) . ? C3 C8 1.530(8) . ? C4 C5 1.381(8) . ? C4 H4 0.9500 . ? C5 C6 1.399(9) . ? C5 C12 1.539(9) . ? C6 C7 1.367(8) . ? C6 H6 0.9500 . ? C7 C16 1.497(8) . ? C8 C9 1.530(8) . ? C8 C10 1.535(8) . ? C8 C11 1.564(8) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.504(10) . ? C12 C14 1.535(13) . ? C12 C13 1.548(13) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.520(8) . ? C18 C23 1.539(9) . ? C18 H18 1.0000 . ? C19 C20 1.537(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.518(11) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.527(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.511(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23 1.0000 . ? C24 C25 1.413(8) . ? C24 H24 0.9500 . ? C25 C26 1.397(8) . ? C25 C30 1.424(9) . ? C26 C27 1.362(9) . ? C26 H26 0.9500 . ? C27 C28 1.413(10) . ? C27 C31 1.526(10) . ? C28 C29 1.400(9) . ? C28 H28 0.9500 . ? C29 C30 1.413(8) . ? C29 C35 1.540(9) . ? C31 C32 1.527(12) . ? C31 C34 1.536(11) . ? C31 C33 1.536(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.536(9) . ? C35 C38 1.538(9) . ? C35 C36 1.554(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 93.0(2) . . ? O1 Al1 C1 120.0(3) . . ? O2 Al1 C1 97.2(2) . . ? O1 Al1 N2 117.8(2) . . ? O2 Al1 N2 87.7(2) . . ? C1 Al1 N2 121.6(3) . . ? O1 Al1 N1 88.87(19) . . ? O2 Al1 N1 164.4(2) . . ? C1 Al1 N1 95.3(2) . . ? N2 Al1 N1 77.8(2) . . ? C2 O1 Al1 136.1(4) . . ? C16 N1 C18 111.5(5) . . ? C16 N1 C17 107.8(5) . . ? C18 N1 C17 112.9(5) . . ? C16 N1 Al1 107.5(4) . . ? C18 N1 Al1 104.1(3) . . ? C17 N1 Al1 112.9(4) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C30 O2 Al1 128.7(4) . . ? C24 N2 C23 118.0(5) . . ? C24 N2 Al1 121.5(4) . . ? C23 N2 Al1 119.3(4) . . ? O1 C2 C7 119.6(5) . . ? O1 C2 C3 120.7(5) . . ? C7 C2 C3 119.8(5) . . ? C4 C3 C2 116.8(5) . . ? C4 C3 C8 121.5(5) . . ? C2 C3 C8 121.6(5) . . ? C5 C4 C3 125.2(6) . . ? C5 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? C4 C5 C6 115.8(6) . . ? C4 C5 C12 123.9(6) . . ? C6 C5 C12 120.3(6) . . ? C7 C6 C5 122.2(6) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C2 120.3(6) . . ? C6 C7 C16 120.6(6) . . ? C2 C7 C16 119.0(5) . . ? C3 C8 C9 111.7(5) . . ? C3 C8 C10 112.7(5) . . ? C9 C8 C10 107.1(5) . . ? C3 C8 C11 109.0(5) . . ? C9 C8 C11 108.9(5) . . ? C10 C8 C11 107.3(5) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 108.3(7) . . ? C15 C12 C5 112.2(6) . . ? C14 C12 C5 108.4(8) . . ? C15 C12 C13 107.4(8) . . ? C14 C12 C13 112.0(10) . . ? C5 C12 C13 108.6(7) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C7 113.7(5) . . ? N1 C16 H16A 108.8 . . ? C7 C16 H16A 108.8 . . ? N1 C16 H16B 108.8 . . ? C7 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N1 C17 H17A 109.5 . . ? N1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N1 C18 C19 117.6(5) . . ? N1 C18 C23 107.5(5) . . ? C19 C18 C23 109.8(5) . . ? N1 C18 H18 107.2 . . ? C19 C18 H18 107.2 . . ? C23 C18 H18 107.2 . . ? C18 C19 C20 107.7(6) . . ? C18 C19 H19A 110.2 . . ? C20 C19 H19A 110.2 . . ? C18 C19 H19B 110.2 . . ? C20 C19 H19B 110.2 . . ? H19A C19 H19B 108.5 . . ? C21 C20 C19 111.8(7) . . ? C21 C20 H20A 109.3 . . ? C19 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 111.9(7) . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 110.3(6) . . ? C23 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? C23 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? N2 C23 C22 115.0(6) . . ? N2 C23 C18 106.8(5) . . ? C22 C23 C18 107.6(6) . . ? N2 C23 H23 109.1 . . ? C22 C23 H23 109.1 . . ? C18 C23 H23 109.1 . . ? N2 C24 C25 127.2(6) . . ? N2 C24 H24 116.4 . . ? C25 C24 H24 116.4 . . ? C26 C25 C24 119.4(6) . . ? C26 C25 C30 120.3(6) . . ? C24 C25 C30 120.0(6) . . ? C27 C26 C25 122.2(7) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 117.4(6) . . ? C26 C27 C31 121.0(8) . . ? C28 C27 C31 121.5(7) . . ? C29 C28 C27 123.2(7) . . ? C29 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? C28 C29 C30 118.1(7) . . ? C28 C29 C35 120.7(6) . . ? C30 C29 C35 121.2(6) . . ? O2 C30 C29 120.6(6) . . ? O2 C30 C25 120.6(5) . . ? C29 C30 C25 118.7(6) . . ? C27 C31 C32 110.0(6) . . ? C27 C31 C34 112.3(8) . . ? C32 C31 C34 107.8(7) . . ? C27 C31 C33 109.7(6) . . ? C32 C31 C33 109.2(8) . . ? C34 C31 C33 107.7(7) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C38 107.6(6) . . ? C37 C35 C29 109.0(6) . . ? C38 C35 C29 112.6(6) . . ? C37 C35 C36 110.2(6) . . ? C38 C35 C36 107.4(6) . . ? C29 C35 C36 110.0(6) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.307 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.063 data_Al(4)OCh2Ph _database_code_depnum_ccdc_archive 'CCDC 917783' #TrackingRef 'Dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39.50 H51 Al N2 O3' _chemical_formula_weight 628.80 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' O O 0.0106 0.0060 '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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.7960(3) _cell_length_b 12.55700(10) _cell_length_c 21.7940(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.5210(10) _cell_angle_gamma 90.00 _cell_volume 6940.84(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35162 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9806 _exptl_absorpt_correction_T_max 0.9854 _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 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55806 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7910 _reflns_number_gt 6084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0341P)^2^+6.7508P] 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 7910 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.662590(17) 0.20464(3) 0.647865(19) 0.01879(10) Uani 1 1 d . . . O1 O 0.70440(4) 0.09808(8) 0.63523(5) 0.0248(2) Uani 1 1 d . . . N1 N 0.71588(5) 0.31118(9) 0.61646(5) 0.0187(2) Uani 1 1 d . . . C1 C 0.75123(6) 0.08782(11) 0.61762(6) 0.0223(3) Uani 1 1 d . . . O2 O 0.62630(4) 0.11771(8) 0.69080(4) 0.0217(2) Uani 1 1 d . . . N2 N 0.67667(5) 0.30087(9) 0.72011(5) 0.0191(2) Uani 1 1 d . . . C2 C 0.76576(6) -0.01164(12) 0.59678(7) 0.0260(3) Uani 1 1 d . . . H2 H 0.7419 -0.0698 0.5941 0.031 Uiso 1 1 calc R . . O3 O 0.61237(4) 0.24904(8) 0.58950(5) 0.0252(2) Uani 1 1 d . . . C3 C 0.81469(7) -0.02577(12) 0.58013(7) 0.0282(3) Uani 1 1 d . . . H3 H 0.8240 -0.0935 0.5660 0.034 Uiso 1 1 calc R . . C4 C 0.85012(6) 0.05783(12) 0.58384(7) 0.0270(3) Uani 1 1 d . . . H4 H 0.8839 0.0477 0.5732 0.032 Uiso 1 1 calc R . . C5 C 0.83539(6) 0.15708(12) 0.60346(7) 0.0242(3) Uani 1 1 d . . . H5 H 0.8594 0.2149 0.6056 0.029 Uiso 1 1 calc R . . C6 C 0.78643(6) 0.17381(11) 0.61997(6) 0.0212(3) Uani 1 1 d . . . C7 C 0.77153(6) 0.28140(11) 0.64247(7) 0.0212(3) Uani 1 1 d . . . H7A H 0.7765 0.2806 0.6886 0.025 Uiso 1 1 calc R . . H7B H 0.7954 0.3361 0.6303 0.025 Uiso 1 1 calc R . . C8 C 0.70737(6) 0.31344(12) 0.54730(6) 0.0225(3) Uani 1 1 d . . . H8A H 0.6723 0.3426 0.5309 0.034 Uiso 1 1 calc R . . H8B H 0.7098 0.2409 0.5315 0.034 Uiso 1 1 calc R . . H8C H 0.7343 0.3583 0.5339 0.034 Uiso 1 1 calc R . . C9 C 0.70048(6) 0.41576(11) 0.64051(6) 0.0196(3) Uani 1 1 d . . . H9 H 0.6631 0.4284 0.6199 0.023 Uiso 1 1 calc R . . C10 C 0.73121(6) 0.51485(11) 0.62759(7) 0.0240(3) Uani 1 1 d . . . H10A H 0.7321 0.5199 0.5825 0.029 Uiso 1 1 calc R . . H10B H 0.7680 0.5105 0.6507 0.029 Uiso 1 1 calc R . . C11 C 0.70394(7) 0.61310(12) 0.64869(7) 0.0269(3) Uani 1 1 d . . . H11A H 0.7247 0.6775 0.6430 0.032 Uiso 1 1 calc R . . H11B H 0.6686 0.6210 0.6223 0.032 Uiso 1 1 calc R . . C12 C 0.69826(7) 0.60439(12) 0.71716(7) 0.0274(3) Uani 1 1 d . . . H12A H 0.6780 0.6663 0.7281 0.033 Uiso 1 1 calc R . . H12B H 0.7337 0.6068 0.7438 0.033 Uiso 1 1 calc R . . C13 C 0.67039(6) 0.50162(11) 0.73069(7) 0.0236(3) Uani 1 1 d . . . H13A H 0.6696 0.4966 0.7759 0.028 Uiso 1 1 calc R . . H13B H 0.6336 0.5018 0.7076 0.028 Uiso 1 1 calc R . . C14 C 0.70013(6) 0.40623(11) 0.71040(6) 0.0199(3) Uani 1 1 d . . . H14 H 0.7373 0.4078 0.7336 0.024 Uiso 1 1 calc R . . C15 C 0.67060(6) 0.27674(11) 0.77629(6) 0.0208(3) Uani 1 1 d . . . H15 H 0.6814 0.3284 0.8079 0.025 Uiso 1 1 calc R . . C16 C 0.64910(6) 0.17928(11) 0.79488(6) 0.0195(3) Uani 1 1 d . . . C17 C 0.64659(6) 0.16534(11) 0.85872(7) 0.0216(3) Uani 1 1 d . . . H17 H 0.6596 0.2200 0.8876 0.026 Uiso 1 1 calc R . . C18 C 0.62581(6) 0.07451(11) 0.87991(6) 0.0209(3) Uani 1 1 d . . . C19 C 0.60900(6) -0.00594(11) 0.83499(7) 0.0212(3) Uani 1 1 d . . . H19 H 0.5957 -0.0702 0.8492 0.025 Uiso 1 1 calc R . . C20 C 0.61048(5) 0.00204(11) 0.77188(6) 0.0192(3) Uani 1 1 d . . . C21 C 0.62894(5) 0.10046(11) 0.75061(6) 0.0191(3) Uani 1 1 d . . . C22 C 0.62037(6) 0.05745(12) 0.94825(7) 0.0237(3) Uani 1 1 d . . . C23 C 0.56205(7) 0.04307(16) 0.95224(8) 0.0374(4) Uani 1 1 d . . . H23A H 0.5423 0.1066 0.9356 0.056 Uiso 1 1 calc R . . H23B H 0.5586 0.0328 0.9959 0.056 Uiso 1 1 calc R . . H23C H 0.5480 -0.0194 0.9278 0.056 Uiso 1 1 calc R . . C24 C 0.64209(8) 0.15221(13) 0.98947(7) 0.0344(4) Uani 1 1 d . . . H24A H 0.6794 0.1626 0.9874 0.052 Uiso 1 1 calc R . . H24B H 0.6385 0.1380 1.0327 0.052 Uiso 1 1 calc R . . H24C H 0.6222 0.2166 0.9746 0.052 Uiso 1 1 calc R . . C25 C 0.65115(7) -0.04220(13) 0.97430(7) 0.0304(4) Uani 1 1 d . . . H25A H 0.6379 -0.1041 0.9487 0.046 Uiso 1 1 calc R . . H25B H 0.6465 -0.0541 1.0174 0.046 Uiso 1 1 calc R . . H25C H 0.6887 -0.0321 0.9734 0.046 Uiso 1 1 calc R . . C26 C 0.59283(6) -0.08797(11) 0.72493(7) 0.0212(3) Uani 1 1 d . . . C27 C 0.54411(6) -0.05331(12) 0.67731(7) 0.0271(3) Uani 1 1 d . . . H27A H 0.5157 -0.0333 0.6994 0.041 Uiso 1 1 calc R . . H27B H 0.5324 -0.1124 0.6488 0.041 Uiso 1 1 calc R . . H27C H 0.5532 0.0079 0.6535 0.041 Uiso 1 1 calc R . . C28 C 0.63779(6) -0.11682(12) 0.68986(7) 0.0261(3) Uani 1 1 d . . . H28A H 0.6469 -0.0542 0.6671 0.039 Uiso 1 1 calc R . . H28B H 0.6262 -0.1746 0.6603 0.039 Uiso 1 1 calc R . . H28C H 0.6688 -0.1399 0.7199 0.039 Uiso 1 1 calc R . . C29 C 0.57873(6) -0.18995(12) 0.75726(7) 0.0265(3) Uani 1 1 d . . . H29A H 0.6095 -0.2140 0.7874 0.040 Uiso 1 1 calc R . . H29B H 0.5683 -0.2456 0.7259 0.040 Uiso 1 1 calc R . . H29C H 0.5495 -0.1753 0.7791 0.040 Uiso 1 1 calc R . . C30 C 0.55926(7) 0.26343(18) 0.59330(8) 0.0422(5) Uani 1 1 d . . . H30A H 0.5566 0.3157 0.6266 0.051 Uiso 1 1 calc R . . H30B H 0.5445 0.1950 0.6048 0.051 Uiso 1 1 calc R . . C31 C 0.52713(6) 0.30238(13) 0.53249(7) 0.0298(3) Uani 1 1 d . . . C32 C 0.48059(7) 0.35798(15) 0.53233(9) 0.0403(4) Uani 1 1 d . . . H32 H 0.4694 0.3718 0.5707 0.048 Uiso 1 1 calc R . . C33 C 0.45027(8) 0.39360(17) 0.47703(10) 0.0476(5) Uani 1 1 d . . . H33 H 0.4184 0.4311 0.4777 0.057 Uiso 1 1 calc R . . C34 C 0.46628(8) 0.37480(16) 0.42101(9) 0.0447(5) Uani 1 1 d . . . H34 H 0.4457 0.3997 0.3831 0.054 Uiso 1 1 calc R . . C35 C 0.51251(7) 0.31948(15) 0.42040(8) 0.0392(4) Uani 1 1 d . . . H35 H 0.5236 0.3058 0.3819 0.047 Uiso 1 1 calc R . . C36 C 0.54277(7) 0.28392(14) 0.47594(8) 0.0336(4) Uani 1 1 d . . . H36 H 0.5746 0.2464 0.4751 0.040 Uiso 1 1 calc R . . C37 C 0.5000 0.2085(2) 0.7500 0.0684(11) Uani 1 2 d S . . H37A H 0.5357 0.1825 0.7495 0.103 Uiso 0.50 1 calc PR . . H37B H 0.4760 0.1825 0.7129 0.103 Uiso 0.50 1 calc PR . . H37C H 0.4883 0.1825 0.7876 0.103 Uiso 0.50 1 calc PR . . C38 C 0.5000 0.3288(2) 0.7500 0.0374(6) Uani 1 2 d S . . C39 C 0.53991(7) 0.38574(15) 0.78691(9) 0.0410(4) Uani 1 1 d . . . H39 H 0.5676 0.3486 0.8130 0.049 Uiso 1 1 calc R . . C40 C 0.54004(7) 0.49574(16) 0.78642(9) 0.0421(4) Uani 1 1 d . . . H40 H 0.5681 0.5334 0.8115 0.051 Uiso 1 1 calc R . . C41 C 0.5000 0.5509(2) 0.7500 0.0402(6) Uani 1 2 d S . . H41 H 0.5000 0.6266 0.7500 0.048 Uiso 1 2 calc SR . . 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 0.0223(2) 0.0178(2) 0.0159(2) -0.00017(16) 0.00239(16) -0.00269(17) O1 0.0263(6) 0.0194(5) 0.0301(6) -0.0013(4) 0.0088(5) -0.0024(4) N1 0.0214(6) 0.0182(6) 0.0159(6) -0.0003(5) 0.0020(5) 0.0005(5) C1 0.0267(8) 0.0224(7) 0.0174(7) 0.0013(6) 0.0027(6) 0.0022(6) O2 0.0281(5) 0.0207(5) 0.0163(5) 0.0004(4) 0.0038(4) -0.0043(4) N2 0.0226(6) 0.0162(6) 0.0185(6) 0.0006(5) 0.0040(5) -0.0011(5) C2 0.0331(8) 0.0211(7) 0.0228(7) 0.0001(6) 0.0022(6) 0.0001(6) O3 0.0217(5) 0.0322(6) 0.0206(5) 0.0046(4) 0.0014(4) -0.0029(4) C3 0.0384(9) 0.0236(8) 0.0221(7) 0.0004(6) 0.0043(7) 0.0094(7) C4 0.0285(8) 0.0312(8) 0.0214(7) 0.0022(6) 0.0046(6) 0.0082(7) C5 0.0247(8) 0.0271(8) 0.0198(7) 0.0021(6) 0.0019(6) 0.0007(6) C6 0.0248(7) 0.0221(7) 0.0157(7) 0.0017(5) 0.0012(6) 0.0012(6) C7 0.0201(7) 0.0207(7) 0.0220(7) -0.0003(6) 0.0021(6) -0.0013(6) C8 0.0283(8) 0.0236(7) 0.0159(7) 0.0016(6) 0.0044(6) -0.0012(6) C9 0.0225(7) 0.0164(7) 0.0197(7) 0.0002(5) 0.0034(6) 0.0002(5) C10 0.0285(8) 0.0191(7) 0.0250(7) 0.0012(6) 0.0066(6) -0.0023(6) C11 0.0333(9) 0.0172(7) 0.0301(8) 0.0022(6) 0.0056(7) -0.0001(6) C12 0.0356(9) 0.0173(7) 0.0296(8) -0.0021(6) 0.0065(7) 0.0002(6) C13 0.0301(8) 0.0196(7) 0.0217(7) -0.0006(6) 0.0064(6) 0.0003(6) C14 0.0229(7) 0.0172(7) 0.0189(7) -0.0003(5) 0.0021(6) -0.0026(5) C15 0.0242(7) 0.0204(7) 0.0175(7) -0.0017(5) 0.0028(6) 0.0011(6) C16 0.0214(7) 0.0182(7) 0.0188(7) 0.0005(5) 0.0028(6) 0.0014(5) C17 0.0260(7) 0.0200(7) 0.0185(7) -0.0018(6) 0.0034(6) 0.0019(6) C18 0.0223(7) 0.0214(7) 0.0188(7) 0.0024(6) 0.0038(6) 0.0041(6) C19 0.0219(7) 0.0191(7) 0.0228(7) 0.0038(6) 0.0045(6) 0.0010(6) C20 0.0188(7) 0.0188(7) 0.0198(7) 0.0007(5) 0.0027(6) 0.0004(5) C21 0.0196(7) 0.0207(7) 0.0169(7) 0.0016(5) 0.0036(5) 0.0025(5) C22 0.0276(8) 0.0266(8) 0.0175(7) 0.0030(6) 0.0055(6) 0.0029(6) C23 0.0318(9) 0.0541(11) 0.0287(9) 0.0037(8) 0.0119(7) 0.0042(8) C24 0.0511(11) 0.0325(9) 0.0205(8) -0.0002(7) 0.0087(7) 0.0000(8) C25 0.0387(9) 0.0299(8) 0.0224(8) 0.0072(6) 0.0054(7) 0.0043(7) C26 0.0233(7) 0.0190(7) 0.0209(7) 0.0004(6) 0.0028(6) -0.0028(6) C27 0.0273(8) 0.0242(8) 0.0274(8) 0.0002(6) -0.0013(6) -0.0041(6) C28 0.0316(8) 0.0207(7) 0.0268(8) -0.0015(6) 0.0073(7) 0.0004(6) C29 0.0309(8) 0.0209(7) 0.0276(8) 0.0012(6) 0.0053(6) -0.0041(6) C30 0.0236(8) 0.0697(13) 0.0332(9) 0.0182(9) 0.0047(7) 0.0014(8) C31 0.0243(8) 0.0346(9) 0.0290(8) 0.0070(7) 0.0012(6) -0.0067(7) C32 0.0336(9) 0.0504(11) 0.0369(10) 0.0044(8) 0.0066(8) 0.0019(8) C33 0.0359(10) 0.0504(12) 0.0539(12) 0.0101(10) 0.0016(9) 0.0113(9) C34 0.0403(11) 0.0490(11) 0.0384(10) 0.0113(9) -0.0100(8) 0.0030(9) C35 0.0435(10) 0.0444(10) 0.0266(9) 0.0007(7) -0.0013(8) -0.0014(8) C36 0.0309(9) 0.0362(9) 0.0323(9) 0.0035(7) 0.0019(7) 0.0020(7) C37 0.060(2) 0.0315(15) 0.126(3) 0.000 0.050(2) 0.000 C38 0.0365(14) 0.0320(13) 0.0497(15) 0.000 0.0239(12) 0.000 C39 0.0339(10) 0.0471(11) 0.0418(10) 0.0041(9) 0.0063(8) 0.0133(8) C40 0.0335(10) 0.0468(11) 0.0434(10) -0.0153(9) 0.0001(8) 0.0003(8) C41 0.0376(14) 0.0304(13) 0.0535(16) 0.000 0.0106(12) 0.000 _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 1.7335(11) . ? Al1 O1 1.7714(11) . ? Al1 O2 1.8065(10) . ? Al1 N2 1.9652(12) . ? Al1 N1 2.1192(12) . ? O1 C1 1.3389(18) . ? N1 C8 1.4832(17) . ? N1 C7 1.4915(18) . ? N1 C9 1.4943(17) . ? C1 C2 1.403(2) . ? C1 C6 1.406(2) . ? O2 C21 1.3108(16) . ? N2 C15 1.2984(18) . ? N2 C14 1.4860(17) . ? C2 C3 1.387(2) . ? C2 H2 0.9500 . ? O3 C30 1.3993(19) . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.393(2) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 C7 1.5107(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.5289(19) . ? C9 C14 1.5296(19) . ? C9 H9 1.0000 . ? C10 C11 1.532(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.530(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.532(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.5305(19) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14 1.0000 . ? C15 C16 1.4322(19) . ? C15 H15 0.9500 . ? C16 C21 1.413(2) . ? C16 C17 1.4154(19) . ? C17 C18 1.376(2) . ? C17 H17 0.9500 . ? C18 C19 1.418(2) . ? C18 C22 1.5363(19) . ? C19 C20 1.387(2) . ? C19 H19 0.9500 . ? C20 C21 1.4317(19) . ? C20 C26 1.5368(19) . ? C22 C23 1.533(2) . ? C22 C24 1.534(2) . ? C22 C25 1.534(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C29 1.5370(19) . ? C26 C27 1.539(2) . ? C26 C28 1.544(2) . ? 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 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.510(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.385(2) . ? C31 C32 1.388(2) . ? C32 C33 1.386(3) . ? C32 H32 0.9500 . ? C33 C34 1.379(3) . ? C33 H33 0.9500 . ? C34 C35 1.382(3) . ? C34 H34 0.9500 . ? C35 C36 1.389(2) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.510(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.384(2) . ? C38 C39 1.384(2) 2_656 ? C39 C40 1.381(3) . ? C39 H39 0.9500 . ? C40 C41 1.370(2) . ? C40 H40 0.9500 . ? C41 C40 1.370(2) 2_656 ? C41 H41 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 O3 Al1 O1 121.57(5) . . ? O3 Al1 O2 100.71(5) . . ? O1 Al1 O2 90.68(5) . . ? O3 Al1 N2 113.22(5) . . ? O1 Al1 N2 124.07(5) . . ? O2 Al1 N2 89.65(5) . . ? O3 Al1 N1 90.11(5) . . ? O1 Al1 N1 88.71(5) . . ? O2 Al1 N1 167.62(5) . . ? N2 Al1 N1 80.49(5) . . ? C1 O1 Al1 136.39(9) . . ? C8 N1 C7 110.15(11) . . ? C8 N1 C9 109.88(11) . . ? C7 N1 C9 112.71(11) . . ? C8 N1 Al1 110.85(9) . . ? C7 N1 Al1 110.80(8) . . ? C9 N1 Al1 102.23(8) . . ? O1 C1 C2 119.13(13) . . ? O1 C1 C6 121.75(13) . . ? C2 C1 C6 119.12(13) . . ? C21 O2 Al1 132.62(9) . . ? C15 N2 C14 117.68(12) . . ? C15 N2 Al1 125.14(10) . . ? C14 N2 Al1 116.99(8) . . ? C3 C2 C1 120.55(14) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C30 O3 Al1 127.36(10) . . ? C4 C3 C2 120.68(14) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 118.83(14) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 121.74(14) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 119.04(13) . . ? C5 C6 C7 121.06(13) . . ? C1 C6 C7 119.86(12) . . ? N1 C7 C6 112.65(12) . . ? N1 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N1 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 118.08(11) . . ? N1 C9 C14 109.32(11) . . ? C10 C9 C14 110.15(11) . . ? N1 C9 H9 106.2 . . ? C10 C9 H9 106.2 . . ? C14 C9 H9 106.2 . . ? C9 C10 C11 108.55(12) . . ? C9 C10 H10A 110.0 . . ? C11 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? C11 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C12 C11 C10 111.48(12) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 112.34(12) . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 109.03(12) . . ? C14 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? C14 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N2 C14 C9 106.74(11) . . ? N2 C14 C13 114.65(11) . . ? C9 C14 C13 108.72(11) . . ? N2 C14 H14 108.9 . . ? C9 C14 H14 108.9 . . ? C13 C14 H14 108.9 . . ? N2 C15 C16 125.86(13) . . ? N2 C15 H15 117.1 . . ? C16 C15 H15 117.1 . . ? C21 C16 C17 120.48(13) . . ? C21 C16 C15 121.23(12) . . ? C17 C16 C15 118.24(13) . . ? C18 C17 C16 121.54(13) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 116.60(13) . . ? C17 C18 C22 123.45(13) . . ? C19 C18 C22 119.95(13) . . ? C20 C19 C18 124.95(13) . . ? C20 C19 H19 117.5 . . ? C18 C19 H19 117.5 . . ? C19 C20 C21 117.04(13) . . ? C19 C20 C26 123.29(12) . . ? C21 C20 C26 119.66(12) . . ? O2 C21 C16 120.60(12) . . ? O2 C21 C20 120.31(12) . . ? C16 C21 C20 119.09(12) . . ? C23 C22 C24 108.38(13) . . ? C23 C22 C25 109.25(13) . . ? C24 C22 C25 107.88(13) . . ? C23 C22 C18 109.61(13) . . ? C24 C22 C18 111.80(12) . . ? C25 C22 C18 109.86(12) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 C29 111.94(12) . . ? C20 C26 C27 110.30(12) . . ? C29 C26 C27 108.19(12) . . ? C20 C26 C28 110.13(12) . . ? C29 C26 C28 107.07(12) . . ? C27 C26 C28 109.10(12) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O3 C30 C31 112.10(13) . . ? O3 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? O3 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C36 C31 C32 118.32(16) . . ? C36 C31 C30 121.63(15) . . ? C32 C31 C30 120.05(15) . . ? C33 C32 C31 121.00(17) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 120.15(18) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.53(17) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.13(17) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 120.88(16) . . ? C31 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C38 C37 H37A 109.5 . . ? C38 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C38 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C39 117.8(2) . 2_656 ? C39 C38 C37 121.10(12) . . ? C39 C38 C37 121.10(12) 2_656 . ? C40 C39 C38 120.98(18) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C41 C40 C39 120.49(19) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C40 119.3(2) 2_656 . ? C40 C41 H41 120.4 2_656 . ? C40 C41 H41 120.4 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.330 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.047