# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 # 1. SUBMISSION DETAILS _publ_contact_author ; Matthew D Jones University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; _publ_contact_author_phone '# 44 1225 38 4908' _publ_contact_author_fax '# 44 1225 82 6231' _publ_contact_author_email mj205@bath.ac.uk _publ_contact_letter ; ; #================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Al(III) Homopiperazine Complexes for the Production of Polyesters ; loop_ _publ_author_name _publ_author_address 'Stuart L. Hancock' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Mary F. Mahon' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; 'Conrad J. Langridge' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; _publ_contact_author_name 'Matthew D Jones' #========================================================= data_Al(1)Me _database_code_depnum_ccdc_archive 'CCDC 877942' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.75 H58.75 Al N2 O2' _chemical_formula_weight 587.59 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 _platon_squeeze_void_content 1 0.500 0.000 0.393 888 54 ' ' 2 0.000 0.500 0.248 888 54 ' ' _platon_squeeze_details ; The electron density in the voids was consistent with an eighth of a hexane moiety per Al centre and has been treated as such. ; 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 35.6710(9) _cell_length_b 10.4360(3) _cell_length_c 24.9340(8) _cell_angle_alpha 90.00 _cell_angle_beta 116.4370(10) _cell_angle_gamma 90.00 _cell_volume 8311.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 102804 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2578 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Bond lengths in the disorded tBu and piperzaine ring moieties have been restrained, to the appropriate C-C distance, to assit convergence ; _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 70559 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9479 _reflns_number_gt 7945 _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^)+(0.1607P)^2^+24.1719P] 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 9479 _refine_ls_number_parameters 494 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1319 _refine_ls_R_factor_gt 0.1196 _refine_ls_wR_factor_ref 0.3350 _refine_ls_wR_factor_gt 0.3258 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.73298(3) 0.19844(10) 0.63741(4) 0.0440(3) Uani 1 1 d . . . O1 O 0.71712(9) 0.1051(3) 0.57023(11) 0.0661(9) Uani 1 1 d . A . N1 N 0.7330(2) 0.3515(5) 0.5843(2) 0.0320(10) Uani 0.50 1 d P A 1 C1 C 0.68589(15) 0.1851(6) 0.6575(3) 0.0909(19) Uani 1 1 d . A . H1C H 0.6644 0.2481 0.6341 0.136 Uiso 1 1 calc R . . H1A H 0.6957 0.2019 0.7003 0.136 Uiso 1 1 calc R . . H1B H 0.6740 0.0988 0.6480 0.136 Uiso 1 1 calc R . . O2 O 0.77550(7) 0.0931(2) 0.67490(9) 0.0418(5) Uani 1 1 d . A . N2 N 0.7646(2) 0.3376(5) 0.6971(2) 0.0297(14) Uiso 0.50 1 d P A 1 C2 C 0.65850(10) 0.0251(3) 0.48365(13) 0.0395(7) Uani 1 1 d . A . C3 C 0.62523(12) 0.0562(4) 0.42872(17) 0.0571(10) Uani 1 1 d . . . H3 H 0.6084 -0.0089 0.4023 0.069 Uiso 1 1 calc R B 1 C4 C 0.6174(8) 0.184(3) 0.4137(8) 0.049(5) Uani 0.50 1 d P A 1 C5 C 0.6492(3) 0.2691(9) 0.4382(4) 0.046(2) Uani 0.50 1 d P A 1 H5 H 0.6477 0.3505 0.4203 0.055 Uiso 0.50 1 calc PR A 1 C6 C 0.6844(2) 0.2341(6) 0.4906(3) 0.0337(11) Uani 0.50 1 d P A 1 C7 C 0.66736(13) -0.1143(3) 0.50552(15) 0.0503(9) Uani 1 1 d . . . C8 C 0.66789(13) -0.1283(3) 0.56743(15) 0.0498(8) Uani 1 1 d . A . H8A H 0.6894 -0.0719 0.5962 0.075 Uiso 1 1 calc R . . H8B H 0.6741 -0.2173 0.5809 0.075 Uiso 1 1 calc R . . H8C H 0.6404 -0.1044 0.5644 0.075 Uiso 1 1 calc R . . C9 C 0.70994(18) -0.1549(5) 0.5099(2) 0.0804(16) Uani 1 1 d . A . H9A H 0.7317 -0.0965 0.5368 0.121 Uiso 1 1 calc R . . H9B H 0.7090 -0.1517 0.4700 0.121 Uiso 1 1 calc R . . H9C H 0.7163 -0.2425 0.5255 0.121 Uiso 1 1 calc R . . C10 C 0.6330(2) -0.2080(4) 0.4634(2) 0.0838(17) Uani 1 1 d . A . H10A H 0.6058 -0.1825 0.4608 0.126 Uiso 1 1 calc R . . H10B H 0.6397 -0.2952 0.4794 0.126 Uiso 1 1 calc R . . H10C H 0.6318 -0.2052 0.4234 0.126 Uiso 1 1 calc R . . C11 C 0.5791(6) 0.1871(16) 0.3375(7) 0.055(3) Uani 0.50 1 d P A 1 C12 C 0.5394(4) 0.1300(15) 0.3388(7) 0.094(4) Uiso 0.50 1 d P A 1 H12D H 0.5468 0.0504 0.3621 0.141 Uiso 0.50 1 calc PR A 1 H12E H 0.5184 0.1119 0.2978 0.141 Uiso 0.50 1 calc PR A 1 H12F H 0.5280 0.1915 0.3574 0.141 Uiso 0.50 1 calc PR A 1 C13 C 0.5788(4) 0.0906(12) 0.2957(5) 0.088(3) Uiso 0.50 1 d P A 1 H13A H 0.5740 0.0062 0.3089 0.132 Uiso 0.50 1 calc PR A 1 H13B H 0.6057 0.0909 0.2942 0.132 Uiso 0.50 1 calc PR A 1 H13C H 0.5563 0.1092 0.2558 0.132 Uiso 0.50 1 calc PR A 1 C14 C 0.5628(6) 0.336(2) 0.3288(10) 0.144(6) Uiso 0.50 1 d PD A 1 H14A H 0.5808 0.3887 0.3175 0.216 Uiso 0.50 1 calc PR A 1 H14B H 0.5639 0.3675 0.3664 0.216 Uiso 0.50 1 calc PR A 1 H14C H 0.5339 0.3400 0.2972 0.216 Uiso 0.50 1 calc PR A 1 C15 C 0.7228(2) 0.3170(6) 0.5206(2) 0.0365(12) Uani 0.50 1 d P A 1 H15A H 0.7470 0.2714 0.5201 0.044 Uiso 0.50 1 calc PR A 1 H15B H 0.7185 0.3969 0.4971 0.044 Uiso 0.50 1 calc PR A 1 C16 C 0.7014(2) 0.4444(8) 0.5848(3) 0.0388(15) Uani 0.50 1 d P A 1 H16A H 0.6752 0.3984 0.5768 0.047 Uiso 0.50 1 calc PR A 1 H16B H 0.6950 0.5085 0.5526 0.047 Uiso 0.50 1 calc PR A 1 C17 C 0.7179(8) 0.514(2) 0.6461(7) 0.051(4) Uani 0.50 1 d P A 1 H17A H 0.7400 0.5743 0.6486 0.062 Uiso 0.50 1 calc PR A 1 H17B H 0.6946 0.5652 0.6461 0.062 Uiso 0.50 1 calc PR A 1 C18 C 0.7350(3) 0.4360(7) 0.7006(4) 0.0397(17) Uani 0.50 1 d P A 1 H18A H 0.7119 0.3929 0.7053 0.048 Uiso 0.50 1 calc PR A 1 H18B H 0.7500 0.4919 0.7359 0.048 Uiso 0.50 1 calc PR A 1 C19 C 0.7761(3) 0.4086(10) 0.6116(4) 0.0409(18) Uani 0.50 1 d P A 1 H19A H 0.7746 0.4999 0.6000 0.049 Uiso 0.50 1 calc PR A 1 H19B H 0.7940 0.3630 0.5967 0.049 Uiso 0.50 1 calc PR A 1 C20 C 0.7957(3) 0.3974(11) 0.6814(5) 0.040(2) Uani 0.50 1 d P A 1 H20A H 0.8214 0.3444 0.6965 0.048 Uiso 0.50 1 calc PR A 1 H20B H 0.8032 0.4834 0.6999 0.048 Uiso 0.50 1 calc PR A 1 C21 C 0.79102(13) 0.2906(3) 0.75961(14) 0.0507(9) Uani 1 1 d . . . H21A H 0.8068 0.3647 0.7840 0.061 Uiso 1 1 calc R A 1 H21B H 0.7720 0.2612 0.7763 0.061 Uiso 1 1 calc R A 1 C22 C 0.82171(10) 0.1852(3) 0.76846(13) 0.0380(7) Uani 1 1 d . A . C23 C 0.81163(10) 0.0886(3) 0.72527(12) 0.0355(6) Uani 1 1 d . . . C24 C 0.84007(11) -0.0131(3) 0.73458(13) 0.0410(7) Uani 1 1 d D A . C25 C 0.87644(11) -0.0161(4) 0.78878(15) 0.0483(8) Uani 1 1 d . . . H25 H 0.8951 -0.0861 0.7962 0.058 Uiso 1 1 calc R A . C26 C 0.88680(11) 0.0789(4) 0.83284(15) 0.0481(8) Uani 1 1 d . A . C27 C 0.85924(11) 0.1795(3) 0.82124(14) 0.0453(8) Uani 1 1 d . . . H27 H 0.8659 0.2466 0.8498 0.054 Uiso 1 1 calc R A . C28 C 0.83070(12) -0.1172(3) 0.68632(15) 0.0497(9) Uani 1 1 d . . . C29 C 0.78961(14) -0.1862(3) 0.67297(17) 0.0563(10) Uani 1 1 d . A . H29A H 0.7842 -0.2517 0.6422 0.084 Uiso 1 1 calc R . . H29B H 0.7666 -0.1242 0.6585 0.084 Uiso 1 1 calc R . . H29C H 0.7917 -0.2270 0.7096 0.084 Uiso 1 1 calc R . . C30 C 0.82769(13) -0.0544(4) 0.62889(16) 0.0541(9) Uani 1 1 d . A . H30A H 0.8540 -0.0099 0.6376 0.081 Uiso 1 1 calc R . . H30B H 0.8045 0.0072 0.6139 0.081 Uiso 1 1 calc R . . H30C H 0.8227 -0.1205 0.5985 0.081 Uiso 1 1 calc R . . C31 C 0.86490(17) -0.2209(5) 0.7062(2) 0.0766(15) Uani 1 1 d . A . H31A H 0.8920 -0.1808 0.7157 0.115 Uiso 1 1 calc R . . H31B H 0.8582 -0.2830 0.6737 0.115 Uiso 1 1 calc R . . H31C H 0.8663 -0.2648 0.7417 0.115 Uiso 1 1 calc R . . C32 C 0.92767(12) 0.0699(5) 0.89130(18) 0.0650(11) Uani 1 1 d . . . C33 C 0.9503(14) -0.055(3) 0.8950(19) 0.202(17) Uiso 0.33333 1 d PD A 1 H33A H 0.9761 -0.0583 0.9326 0.303 Uiso 0.33333 1 calc PR A 1 H33B H 0.9571 -0.0613 0.8611 0.303 Uiso 0.33333 1 calc PR A 1 H33C H 0.9322 -0.1272 0.8935 0.303 Uiso 0.33333 1 calc PR A 1 C34 C 0.9215(7) 0.094(2) 0.9458(9) 0.084(6) Uiso 0.33333 1 d PD A 1 H34A H 0.9174 0.1864 0.9491 0.126 Uiso 0.33333 1 calc PR A 1 H34B H 0.9463 0.0657 0.9814 0.126 Uiso 0.33333 1 calc PR A 1 H34C H 0.8969 0.0475 0.9427 0.126 Uiso 0.33333 1 calc PR A 1 C35 C 0.9562(9) 0.188(3) 0.8862(13) 0.119(9) Uiso 0.33333 1 d PD A 1 H35A H 0.9396 0.2669 0.8756 0.179 Uiso 0.33333 1 calc PR A 1 H35B H 0.9651 0.1681 0.8553 0.179 Uiso 0.33333 1 calc PR A 1 H35C H 0.9809 0.1993 0.9248 0.179 Uiso 0.33333 1 calc PR A 1 N1' N 0.7154(3) 0.3839(7) 0.5916(3) 0.0408(13) Uani 0.50 1 d P A 2 C1' C 0.68385(13) 0.1248(4) 0.51745(15) 0.0563(10) Uani 1 1 d . . . N2' N 0.7759(2) 0.3479(5) 0.6984(2) 0.0295(14) Uiso 0.50 1 d P A 2 C4' C 0.6142(8) 0.175(2) 0.3987(8) 0.047(4) Uani 0.50 1 d P A 2 C5' C 0.6313(3) 0.2777(11) 0.4418(4) 0.054(2) Uani 0.50 1 d P A 2 H5' H 0.6199 0.3611 0.4301 0.064 Uiso 0.50 1 calc PR A 2 C6' C 0.6635(2) 0.2615(7) 0.4990(3) 0.0453(15) Uani 0.50 1 d P A 2 C14' C 0.5870(3) 0.2827(10) 0.3052(5) 0.072(2) Uiso 0.50 1 d P A 2 H14D H 0.5613 0.3152 0.2723 0.108 Uiso 0.50 1 calc PR A 2 H14E H 0.5990 0.2154 0.2901 0.108 Uiso 0.50 1 calc PR A 2 H14F H 0.6072 0.3529 0.3218 0.108 Uiso 0.50 1 calc PR A 2 C15' C 0.6738(2) 0.3772(7) 0.5405(3) 0.0535(18) Uani 0.50 1 d P A 2 H15C H 0.6700 0.4551 0.5160 0.064 Uiso 0.50 1 calc PR A 2 H15D H 0.6528 0.3809 0.5564 0.064 Uiso 0.50 1 calc PR A 2 C16' C 0.7484(3) 0.3993(7) 0.5689(3) 0.0461(16) Uani 0.50 1 d P A 2 H16C H 0.7378 0.4594 0.5346 0.055 Uiso 0.50 1 calc PR A 2 H16D H 0.7532 0.3154 0.5544 0.055 Uiso 0.50 1 calc PR A 2 C17' C 0.7901(4) 0.4496(9) 0.6175(5) 0.049(2) Uani 0.50 1 d P A 2 H17C H 0.8111 0.4481 0.6017 0.058 Uiso 0.50 1 calc PR A 2 H17D H 0.7863 0.5400 0.6260 0.058 Uiso 0.50 1 calc PR A 2 C18' C 0.8071(4) 0.3753(11) 0.6754(5) 0.036(2) Uani 0.50 1 d P A 2 H18C H 0.8185 0.2930 0.6694 0.044 Uiso 0.50 1 calc PR A 2 H18D H 0.8306 0.4242 0.7062 0.044 Uiso 0.50 1 calc PR A 2 C19' C 0.7508(3) 0.4670(8) 0.6944(4) 0.0458(18) Uani 0.50 1 d P A 2 H19C H 0.7700 0.5414 0.7078 0.055 Uiso 0.50 1 calc PR A 2 H19D H 0.7380 0.4582 0.7222 0.055 Uiso 0.50 1 calc PR A 2 C20' C 0.7154(7) 0.4944(16) 0.6299(6) 0.044(3) Uani 0.50 1 d P A 2 H20C H 0.6879 0.5015 0.6304 0.053 Uiso 0.50 1 calc PR A 2 H20D H 0.7211 0.5754 0.6142 0.053 Uiso 0.50 1 calc PR A 2 C11A C 0.5770(5) 0.2274(17) 0.3542(8) 0.077(5) Uani 0.50 1 d P A 2 C12A C 0.5646(8) 0.379(3) 0.3741(12) 0.185(9) Uiso 0.50 1 d P A 2 H12A H 0.5392 0.4123 0.3408 0.278 Uiso 0.50 1 calc PR A 2 H12B H 0.5879 0.4382 0.3828 0.278 Uiso 0.50 1 calc PR A 2 H12C H 0.5598 0.3698 0.4096 0.278 Uiso 0.50 1 calc PR A 2 C13A C 0.5405(4) 0.1893(12) 0.3487(6) 0.078(3) Uiso 0.50 1 d P A 2 H13D H 0.5182 0.2333 0.3147 0.118 Uiso 0.50 1 calc PR A 2 H13E H 0.5381 0.2095 0.3854 0.118 Uiso 0.50 1 calc PR A 2 H13F H 0.5378 0.0965 0.3418 0.118 Uiso 0.50 1 calc PR A 2 C33A C 0.9350(7) -0.0704(18) 0.9172(11) 0.061(4) Uiso 0.33333 1 d PD A 2 H33D H 0.9117 -0.0952 0.9257 0.091 Uiso 0.33333 1 calc PR A 2 H33E H 0.9612 -0.0738 0.9542 0.091 Uiso 0.33333 1 calc PR A 2 H33F H 0.9365 -0.1296 0.8878 0.091 Uiso 0.33333 1 calc PR A 2 C34A C 0.9262(4) 0.1593(17) 0.9423(5) 0.058(3) Uani 0.33333 1 d PD A 2 H34D H 0.9071 0.1221 0.9566 0.086 Uiso 0.33333 1 calc PR A 2 H34E H 0.9164 0.2449 0.9259 0.086 Uiso 0.33333 1 calc PR A 2 H34F H 0.9544 0.1656 0.9757 0.086 Uiso 0.33333 1 calc PR A 2 C35A C 0.9612(5) 0.116(2) 0.8790(8) 0.061(4) Uani 0.33333 1 d PD A 2 H35D H 0.9877 0.1111 0.9155 0.092 Uiso 0.33333 1 calc PR A 2 H35E H 0.9556 0.2048 0.8652 0.092 Uiso 0.33333 1 calc PR A 2 H35F H 0.9629 0.0626 0.8478 0.092 Uiso 0.33333 1 calc PR A 2 C33B C 0.9262(7) -0.047(2) 0.9251(9) 0.109(10) Uani 0.333333 1 d PD A 3 H33G H 0.9521 -0.0528 0.9625 0.164 Uiso 0.33333 1 calc PR A 3 H33H H 0.9234 -0.1232 0.9007 0.164 Uiso 0.33333 1 calc PR A 3 H33I H 0.9022 -0.0411 0.9342 0.164 Uiso 0.33333 1 calc PR A 3 C34B C 0.9387(8) 0.199(2) 0.9279(12) 0.116(9) Uiso 0.33333 1 d PD A 3 H34G H 0.9407 0.2682 0.9029 0.175 Uiso 0.33333 1 calc PR A 3 H34H H 0.9655 0.1894 0.9637 0.175 Uiso 0.33333 1 calc PR A 3 H34I H 0.9167 0.2188 0.9400 0.175 Uiso 0.33333 1 calc PR A 3 C35B C 0.9662(6) 0.044(3) 0.8770(10) 0.113(11) Uani 0.33333 1 d PD A 3 H35G H 0.9676 0.1117 0.8508 0.170 Uiso 0.33333 1 calc PR A 3 H35H H 0.9624 -0.0392 0.8568 0.170 Uiso 0.33333 1 calc PR A 3 H35I H 0.9921 0.0427 0.9144 0.170 Uiso 0.33333 1 calc PR A 3 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 0.0442(5) 0.0404(5) 0.0398(5) 0.0153(4) 0.0119(4) -0.0006(4) O1 0.0662(17) 0.0782(19) 0.0305(12) 0.0186(12) 0.0005(11) -0.0257(15) N1 0.042(3) 0.030(3) 0.023(2) -0.001(2) 0.014(2) -0.004(3) C1 0.063(3) 0.089(4) 0.127(5) 0.063(3) 0.048(3) 0.013(2) O2 0.0508(13) 0.0301(10) 0.0314(10) -0.0035(8) 0.0064(9) 0.0053(9) C2 0.0443(16) 0.0444(17) 0.0291(14) 0.0042(12) 0.0156(12) 0.0061(13) C3 0.051(2) 0.058(2) 0.0450(19) 0.0122(17) 0.0060(16) -0.0105(17) C4 0.035(6) 0.082(10) 0.018(9) 0.018(7) 0.002(6) 0.004(5) C5 0.051(5) 0.048(4) 0.047(4) 0.023(3) 0.028(4) 0.003(4) C6 0.043(3) 0.032(3) 0.030(3) 0.004(2) 0.021(3) 0.003(2) C7 0.079(2) 0.0419(17) 0.0329(15) 0.0026(13) 0.0270(16) 0.0112(17) C8 0.075(2) 0.0406(17) 0.0393(17) 0.0052(13) 0.0307(17) 0.0077(16) C9 0.119(4) 0.085(3) 0.058(2) 0.030(2) 0.058(3) 0.060(3) C10 0.147(5) 0.045(2) 0.050(2) -0.0059(18) 0.036(3) -0.013(3) C11 0.043(5) 0.058(7) 0.046(6) 0.004(4) 0.003(4) -0.003(5) C15 0.052(3) 0.039(3) 0.026(3) 0.001(2) 0.024(2) -0.003(3) C16 0.054(4) 0.029(3) 0.040(4) 0.011(3) 0.027(3) 0.016(3) C17 0.068(6) 0.059(8) 0.028(8) -0.001(6) 0.022(6) -0.002(5) C18 0.064(5) 0.025(3) 0.040(4) -0.004(3) 0.033(4) 0.004(3) C19 0.047(5) 0.044(5) 0.037(4) -0.003(4) 0.023(4) -0.007(3) C20 0.045(6) 0.040(5) 0.040(4) -0.008(3) 0.023(4) -0.011(4) C21 0.077(2) 0.0452(18) 0.0250(14) -0.0034(12) 0.0181(15) 0.0152(17) C22 0.0479(17) 0.0370(15) 0.0304(14) -0.0024(11) 0.0185(12) 0.0013(12) C23 0.0440(15) 0.0330(14) 0.0268(13) -0.0006(11) 0.0136(11) 0.0016(12) C24 0.0496(17) 0.0430(17) 0.0290(14) 0.0000(12) 0.0164(13) 0.0085(13) C25 0.0476(18) 0.056(2) 0.0377(16) -0.0006(14) 0.0155(14) 0.0128(15) C26 0.0417(17) 0.062(2) 0.0353(16) -0.0036(15) 0.0125(13) 0.0000(15) C27 0.0532(19) 0.0463(18) 0.0305(15) -0.0076(13) 0.0133(14) -0.0025(14) C28 0.069(2) 0.0406(17) 0.0345(15) -0.0022(13) 0.0187(15) 0.0211(16) C29 0.085(3) 0.0294(15) 0.0462(19) -0.0042(13) 0.0215(18) 0.0022(16) C30 0.068(2) 0.055(2) 0.0398(17) -0.0074(15) 0.0252(17) 0.0061(18) C31 0.097(3) 0.067(3) 0.052(2) -0.004(2) 0.021(2) 0.044(3) C32 0.0408(18) 0.093(3) 0.044(2) -0.011(2) 0.0039(15) 0.0047(19) N1' 0.059(4) 0.031(3) 0.041(3) 0.001(3) 0.030(3) 0.009(3) C1' 0.062(2) 0.061(2) 0.0301(15) 0.0147(15) 0.0066(15) -0.0219(18) C4' 0.047(6) 0.054(6) 0.019(9) 0.014(6) -0.002(6) -0.014(4) C5' 0.052(5) 0.059(5) 0.041(4) 0.020(4) 0.013(4) 0.000(5) C6' 0.050(4) 0.045(4) 0.034(3) 0.009(3) 0.012(3) 0.009(3) C15' 0.062(4) 0.037(3) 0.050(4) 0.009(3) 0.015(3) 0.019(3) C16' 0.076(5) 0.033(3) 0.041(4) 0.007(3) 0.037(4) 0.004(3) C17' 0.071(7) 0.035(5) 0.049(5) -0.006(4) 0.035(5) -0.001(4) C18' 0.044(5) 0.036(4) 0.036(4) -0.006(3) 0.024(4) -0.007(4) C19' 0.076(6) 0.028(4) 0.041(4) -0.001(3) 0.033(4) 0.016(4) C20' 0.064(6) 0.037(6) 0.029(9) 0.007(6) 0.019(7) 0.007(5) C11A 0.034(5) 0.090(12) 0.078(11) 0.051(8) -0.002(7) -0.002(7) C34A 0.046(6) 0.078(10) 0.024(5) -0.009(6) -0.007(4) 0.010(7) C35A 0.022(6) 0.093(13) 0.063(8) 0.015(9) 0.013(5) 0.005(7) C33B 0.065(12) 0.14(2) 0.051(10) 0.048(13) -0.034(9) -0.005(12) C35B 0.028(7) 0.21(3) 0.078(11) -0.015(18) 0.007(7) 0.037(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O2 1.767(2) . ? Al1 O1 1.797(3) . ? Al1 C1 1.959(5) . ? Al1 N2 2.025(6) . ? Al1 N1 2.075(6) . ? Al1 N1' 2.192(7) . ? Al1 N2' 2.240(6) . ? O1 C1' 1.338(4) . ? N1 C16 1.492(9) . ? N1 C19 1.500(10) . ? N1 C15 1.507(8) . ? C1 H1C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? O2 C23 1.341(4) . ? N2 C20 1.471(12) . ? N2 C21 1.500(6) . ? N2 C18 1.502(10) . ? C2 C1' 1.390(5) . ? C2 C3 1.394(5) . ? C2 C7 1.536(5) . ? C3 C4 1.38(3) . ? C3 C4' 1.41(2) . ? C3 H3 0.9500 . ? C4 C5 1.35(3) . ? C4 C11 1.78(3) . ? C5 C6 1.398(11) . ? C5 H5 0.9500 . ? C6 C1' 1.328(7) . ? C6 C15 1.508(9) . ? C7 C9 1.534(6) . ? C7 C8 1.542(4) . ? C7 C10 1.554(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? 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 C13 1.445(17) . ? C11 C12 1.55(2) . ? C11 C14 1.64(3) . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? 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 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.549(14) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.46(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.564(15) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.497(5) . ? C21 N2' 1.499(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.399(4) . ? C22 C23 1.400(4) . ? C23 C24 1.415(4) . ? C24 C25 1.396(4) . ? C24 C28 1.543(4) . ? C25 C26 1.402(5) . ? C25 H25 0.9500 . ? C26 C27 1.378(5) . ? C26 C32 1.538(5) . ? C27 H27 0.9500 . ? C28 C29 1.531(6) . ? C28 C30 1.534(5) . ? C28 C31 1.538(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C35A 1.441(15) . ? C32 C34 1.49(2) . ? C32 C33B 1.50(2) . ? C32 C33 1.52(3) . ? C32 C33A 1.57(2) . ? C32 C34B 1.57(2) . ? C32 C35B 1.589(18) . ? C32 C34A 1.596(12) . ? C32 C35 1.64(2) . ? 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 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? N1' C15' 1.466(10) . ? N1' C20' 1.496(15) . ? N1' C16' 1.524(10) . ? C1' C6' 1.574(8) . ? N2' C18' 1.489(10) . ? N2' C19' 1.509(9) . ? C4' C11A 1.41(3) . ? C4' C5' 1.45(2) . ? C5' C6' 1.387(11) . ? C5' H5' 0.9500 . ? C6' C15' 1.525(10) . ? C14' C11A 1.53(2) . ? C14' H14D 0.9800 . ? C14' H14E 0.9800 . ? C14' H14F 0.9800 . ? C15' H15C 0.9900 . ? C15' H15D 0.9900 . ? C16' C17' 1.533(13) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C17' C18' 1.508(16) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' C20' 1.568(18) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C11A C13A 1.31(2) . ? C11A C12A 1.77(3) . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34A H34D 0.9800 . ? C34A H34E 0.9800 . ? C34A H34F 0.9800 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? C33B H33G 0.9800 . ? C33B H33H 0.9800 . ? C33B H33I 0.9800 . ? C34B H34G 0.9800 . ? C34B H34H 0.9800 . ? C34B H34I 0.9800 . ? C35B H35G 0.9800 . ? C35B H35H 0.9800 . ? C35B H35I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Al1 O1 89.77(13) . . ? O2 Al1 C1 116.91(17) . . ? O1 Al1 C1 104.5(2) . . ? O2 Al1 N2 89.52(18) . . ? O1 Al1 N2 156.2(2) . . ? C1 Al1 N2 97.0(3) . . ? O2 Al1 N1 124.9(2) . . ? O1 Al1 N1 84.92(18) . . ? C1 Al1 N1 117.5(3) . . ? N2 Al1 N1 76.1(2) . . ? O2 Al1 N1' 143.5(2) . . ? O1 Al1 N1' 95.41(19) . . ? C1 Al1 N1' 96.7(3) . . ? N2 Al1 N1' 71.7(2) . . ? N1 Al1 N1' 21.45(19) . . ? O2 Al1 N2' 84.69(17) . . ? O1 Al1 N2' 147.8(2) . . ? C1 Al1 N2' 106.3(3) . . ? N2 Al1 N2' 9.3(2) . . ? N1 Al1 N2' 72.7(2) . . ? N1' Al1 N2' 71.9(2) . . ? C1' O1 Al1 127.4(3) . . ? C16 N1 C19 111.3(6) . . ? C16 N1 C15 109.5(5) . . ? C19 N1 C15 107.0(6) . . ? C16 N1 Al1 106.2(4) . . ? C19 N1 Al1 107.9(5) . . ? C15 N1 Al1 114.9(4) . . ? Al1 C1 H1C 109.5 . . ? Al1 C1 H1A 109.5 . . ? H1C C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1C C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C23 O2 Al1 139.28(19) . . ? C20 N2 C21 102.4(6) . . ? C20 N2 C18 111.0(7) . . ? C21 N2 C18 107.3(5) . . ? C20 N2 Al1 110.3(5) . . ? C21 N2 Al1 114.6(4) . . ? C18 N2 Al1 111.0(5) . . ? C1' C2 C3 117.5(3) . . ? C1' C2 C7 121.2(3) . . ? C3 C2 C7 121.3(3) . . ? C4 C3 C2 118.2(9) . . ? C4 C3 C4' 14.4(15) . . ? C2 C3 C4' 129.8(10) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C4' C3 H3 108.6 . . ? C5 C4 C3 118.9(18) . . ? C5 C4 C11 124.1(18) . . ? C3 C4 C11 105.9(16) . . ? C4 C5 C6 118.3(12) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C1' C6 C5 119.2(6) . . ? C1' C6 C15 117.2(5) . . ? C5 C6 C15 123.6(6) . . ? C9 C7 C2 109.1(3) . . ? C9 C7 C8 109.4(3) . . ? C2 C7 C8 110.7(3) . . ? C9 C7 C10 109.4(4) . . ? C2 C7 C10 112.3(3) . . ? C8 C7 C10 105.8(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 91.9(12) . . ? C13 C11 C14 132.6(15) . . ? C12 C11 C14 95.4(14) . . ? C13 C11 C4 120.9(15) . . ? C12 C11 C4 104.1(14) . . ? C14 C11 C4 102.5(14) . . ? C11 C12 H12D 109.5 . . ? C11 C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? C11 C12 H12F 109.5 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C6 113.6(5) . . ? N1 C15 H15A 108.9 . . ? C6 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? C6 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N1 C16 C17 110.7(11) . . ? N1 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C16 118.5(15) . . ? C18 C17 H17A 107.7 . . ? C16 C17 H17A 107.7 . . ? C18 C17 H17B 107.7 . . ? C16 C17 H17B 107.7 . . ? H17A C17 H17B 107.1 . . ? C17 C18 N2 109.8(10) . . ? C17 C18 H18A 109.7 . . ? N2 C18 H18A 109.7 . . ? C17 C18 H18B 109.7 . . ? N2 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N1 C19 C20 109.6(7) . . ? N1 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? N1 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? N2 C20 C19 108.2(8) . . ? N2 C20 H20A 110.1 . . ? C19 C20 H20A 110.1 . . ? N2 C20 H20B 110.1 . . ? C19 C20 H20B 110.1 . . ? H20A C20 H20B 108.4 . . ? C22 C21 N2' 110.6(3) . . ? C22 C21 N2 118.3(3) . . ? N2' C21 N2 15.6(3) . . ? C22 C21 H21A 107.7 . . ? N2' C21 H21A 99.3 . . ? N2 C21 H21A 107.7 . . ? C22 C21 H21B 107.7 . . ? N2' C21 H21B 123.2 . . ? N2 C21 H21B 107.7 . . ? H21A C21 H21B 107.1 . . ? C27 C22 C23 120.2(3) . . ? C27 C22 C21 120.0(3) . . ? C23 C22 C21 119.7(3) . . ? O2 C23 C22 120.4(3) . . ? O2 C23 C24 120.0(3) . . ? C22 C23 C24 119.6(3) . . ? C25 C24 C23 117.7(3) . . ? C25 C24 C28 121.6(3) . . ? C23 C24 C28 120.6(3) . . ? C24 C25 C26 123.4(3) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C27 C26 C25 117.4(3) . . ? C27 C26 C32 122.1(3) . . ? C25 C26 C32 120.5(3) . . ? C26 C27 C22 121.6(3) . . ? C26 C27 H27 119.2 . . ? C22 C27 H27 119.2 . . ? C29 C28 C30 109.6(3) . . ? C29 C28 C31 106.5(3) . . ? C30 C28 C31 108.4(3) . . ? C29 C28 C24 110.8(3) . . ? C30 C28 C24 109.2(3) . . ? C31 C28 C24 112.2(3) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C35A C32 C34 127.5(12) . . ? C35A C32 C33B 129.1(12) . . ? C34 C32 C33B 64.6(14) . . ? C35A C32 C33 80.2(16) . . ? C34 C32 C33 112.5(17) . . ? C33B C32 C33 54.2(17) . . ? C35A C32 C26 107.7(7) . . ? C34 C32 C26 113.0(9) . . ? C33B C32 C26 109.1(7) . . ? C33 C32 C26 111.3(16) . . ? C35A C32 C33A 113.3(11) . . ? C34 C32 C33A 81.4(11) . . ? C33B C32 C33A 18.5(15) . . ? C33 C32 C33A 35.7(17) . . ? C26 C32 C33A 111.0(10) . . ? C35A C32 C34B 79.8(13) . . ? C34 C32 C34B 54.9(11) . . ? C33B C32 C34B 115.6(14) . . ? C33 C32 C34B 135.4(19) . . ? C26 C32 C34B 112.6(10) . . ? C33A C32 C34B 127.1(14) . . ? C35A C32 C35B 29.3(12) . . ? C34 C32 C35B 136.6(12) . . ? C33B C32 C35B 103.7(14) . . ? C33 C32 C35B 51.4(16) . . ? C26 C32 C35B 110.3(8) . . ? C33A C32 C35B 86.0(15) . . ? C34B C32 C35B 105.1(14) . . ? C35A C32 C34A 107.4(11) . . ? C34 C32 C34A 26.4(8) . . ? C33B C32 C34A 90.4(13) . . ? C33 C32 C34A 131.3(17) . . ? C26 C32 C34A 111.5(5) . . ? C33A C32 C34A 105.9(10) . . ? C34B C32 C34A 29.2(10) . . ? C35B C32 C34A 128.1(12) . . ? C35A C32 C35 29.7(10) . . ? C34 C32 C35 106.8(13) . . ? C33B C32 C35 146.6(13) . . ? C33 C32 C35 108.7(17) . . ? C26 C32 C35 103.9(11) . . ? C33A C32 C35 137.4(13) . . ? C34B C32 C35 53.0(13) . . ? C35B C32 C35 58.9(13) . . ? C34A C32 C35 82.1(12) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.4 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C15' N1' C20' 107.6(10) . . ? C15' N1' C16' 109.5(6) . . ? C20' N1' C16' 112.0(10) . . ? C15' N1' Al1 110.7(4) . . ? C20' N1' Al1 115.4(7) . . ? C16' N1' Al1 101.4(5) . . ? C6 C1' O1 115.0(4) . . ? C6 C1' C2 119.3(4) . . ? O1 C1' C2 122.3(3) . . ? C6 C1' C6' 35.2(4) . . ? O1 C1' C6' 121.2(4) . . ? C2 C1' C6' 114.2(4) . . ? C18' N2' C21 118.5(7) . . ? C18' N2' C19' 109.9(7) . . ? C21 N2' C19' 109.2(5) . . ? C18' N2' Al1 105.9(5) . . ? C21 N2' Al1 103.9(4) . . ? C19' N2' Al1 108.8(5) . . ? C3 C4' C11A 134.7(19) . . ? C3 C4' C5' 109.4(13) . . ? C11A C4' C5' 104(2) . . ? C6' C5' C4' 123.8(13) . . ? C6' C5' H5' 118.1 . . ? C4' C5' H5' 118.1 . . ? C5' C6' C15' 116.2(7) . . ? C5' C6' C1' 118.3(7) . . ? C15' C6' C1' 125.4(5) . . ? C11A C14' H14D 109.5 . . ? C11A C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C11A C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? N1' C15' C6' 118.2(6) . . ? N1' C15' H15C 107.8 . . ? C6' C15' H15C 107.8 . . ? N1' C15' H15D 107.8 . . ? C6' C15' H15D 107.8 . . ? H15C C15' H15D 107.1 . . ? N1' C16' C17' 112.3(6) . . ? N1' C16' H16C 109.1 . . ? C17' C16' H16C 109.1 . . ? N1' C16' H16D 109.1 . . ? C17' C16' H16D 109.1 . . ? H16C C16' H16D 107.9 . . ? C18' C17' C16' 114.6(8) . . ? C18' C17' H17C 108.6 . . ? C16' C17' H17C 108.6 . . ? C18' C17' H17D 108.6 . . ? C16' C17' H17D 108.6 . . ? H17C C17' H17D 107.6 . . ? N2' C18' C17' 114.6(9) . . ? N2' C18' H18C 108.6 . . ? C17' C18' H18C 108.6 . . ? N2' C18' H18D 108.6 . . ? C17' C18' H18D 108.6 . . ? H18C C18' H18D 107.6 . . ? N2' C19' C20' 113.6(7) . . ? N2' C19' H19C 108.8 . . ? C20' C19' H19C 108.8 . . ? N2' C19' H19D 108.8 . . ? C20' C19' H19D 108.8 . . ? H19C C19' H19D 107.7 . . ? N1' C20' C19' 106.6(11) . . ? N1' C20' H20C 110.4 . . ? C19' C20' H20C 110.4 . . ? N1' C20' H20D 110.4 . . ? C19' C20' H20D 110.4 . . ? H20C C20' H20D 108.6 . . ? C13A C11A C4' 120.6(17) . . ? C13A C11A C14' 127.3(13) . . ? C4' C11A C14' 107.6(15) . . ? C13A C11A C12A 86.6(14) . . ? C4' C11A C12A 113.1(17) . . ? C14' C11A C12A 93.6(13) . . ? C11A C12A H12A 109.5 . . ? C11A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C11A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C32 C33A H33D 109.5 . . ? C32 C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C32 C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C32 C34A H34D 109.5 . . ? C32 C34A H34E 109.5 . . ? H34D C34A H34E 109.5 . . ? C32 C34A H34F 109.5 . . ? H34D C34A H34F 109.5 . . ? H34E C34A H34F 109.5 . . ? C32 C35A H35D 109.5 . . ? C32 C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C32 C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? C32 C33B H33G 109.5 . . ? C32 C33B H33H 109.5 . . ? H33G C33B H33H 109.5 . . ? C32 C33B H33I 109.5 . . ? H33G C33B H33I 109.5 . . ? H33H C33B H33I 109.5 . . ? C32 C34B H34G 109.5 . . ? C32 C34B H34H 109.5 . . ? H34G C34B H34H 109.5 . . ? C32 C34B H34I 109.5 . . ? H34G C34B H34I 109.5 . . ? H34H C34B H34I 109.5 . . ? C32 C35B H35G 109.4 . . ? C32 C35B H35H 109.5 . . ? H35G C35B H35H 109.5 . . ? C32 C35B H35I 109.5 . . ? H35G C35B H35I 109.5 . . ? H35H C35B H35I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.197 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.108 #====END data_Al(3)Me _database_code_depnum_ccdc_archive 'CCDC 877943' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33.50 H49 Al N2 O2' _chemical_formula_weight 538.73 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 Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.7810(2) _cell_length_b 15.1010(2) _cell_length_c 29.1190(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6499.59(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 99764 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9729 _exptl_absorpt_correction_T_max 0.9818 _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 81419 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.44 _reflns_number_total 14759 _reflns_number_gt 13533 _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^)+(0.0882P)^2^+2.3759P] 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 0.06(14) _refine_ls_number_reflns 14759 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _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 0.43355(5) 0.16890(4) 1.23975(2) 0.03023(15) Uani 1 1 d . . . O1 O 0.32398(13) 0.14950(13) 1.21583(7) 0.0436(4) Uani 1 1 d . . . N1 N 0.45723(14) 0.03040(14) 1.23214(7) 0.0349(4) Uani 1 1 d . . . C1 C 0.5232(2) 0.2161(2) 1.19550(11) 0.0530(7) Uani 1 1 d . . . H1A H 0.5122 0.1901 1.1651 0.080 Uiso 1 1 calc R . . H1B H 0.5843 0.2007 1.2058 0.080 Uiso 1 1 calc R . . H1C H 0.5172 0.2806 1.1937 0.080 Uiso 1 1 calc R . . Al2 Al 0.41690(5) -0.18160(5) 1.49387(2) 0.03204(15) Uani 1 1 d . . . O2 O 0.39281(13) 0.26153(11) 1.27255(6) 0.0377(4) Uani 1 1 d . . . N2 N 0.51306(13) 0.13048(12) 1.29644(6) 0.0285(4) Uani 1 1 d . . . C2 C 0.28642(19) 0.0834(2) 1.19016(9) 0.0430(6) Uani 1 1 d . . . O3 O 0.40941(14) -0.07138(12) 1.47206(7) 0.0445(4) Uani 1 1 d . . . N3 N 0.27433(15) -0.19224(14) 1.48461(7) 0.0373(5) Uani 1 1 d . . . C3 C 0.1930(2) 0.0867(2) 1.18083(10) 0.0481(7) Uani 1 1 d . . . O4 O 0.50825(12) -0.15038(12) 1.53135(7) 0.0407(4) Uani 1 1 d . . . N4 N 0.37028(13) -0.26682(13) 1.54639(7) 0.0321(4) Uani 1 1 d . . . C4 C 0.1542(2) 0.0190(2) 1.15391(11) 0.0527(7) Uani 1 1 d . . . H4 H 0.0912 0.0216 1.1478 0.063 Uiso 1 1 calc R . . C5 C 0.2034(2) -0.0516(2) 1.13575(11) 0.0519(7) Uani 1 1 d . . . C6 C 0.2956(2) -0.0541(2) 1.14669(11) 0.0504(7) Uani 1 1 d . . . H6 H 0.3318 -0.1014 1.1356 0.061 Uiso 1 1 calc R . . C7 C 0.3356(2) 0.01234(19) 1.17384(10) 0.0460(6) Uani 1 1 d . . . C8 C 0.1366(2) 0.1607(3) 1.19992(11) 0.0573(8) Uani 1 1 d . . . H8A H 0.0794 0.1641 1.1830 0.086 Uiso 1 1 calc R . . H8B H 0.1694 0.2167 1.1967 0.086 Uiso 1 1 calc R . . H8C H 0.1242 0.1494 1.2325 0.086 Uiso 1 1 calc R . . C9 C 0.1619(3) -0.1245(2) 1.10509(13) 0.0619(9) Uani 1 1 d . . . C10 C 0.2115(3) -0.1290(4) 1.05932(16) 0.0896(15) Uani 1 1 d . . . H10A H 0.1827 -0.1734 1.0396 0.134 Uiso 1 1 calc R . . H10B H 0.2748 -0.1454 1.0646 0.134 Uiso 1 1 calc R . . H10C H 0.2090 -0.0710 1.0443 0.134 Uiso 1 1 calc R . . C11 C 0.0650(3) -0.1041(4) 1.09331(19) 0.0945(16) Uani 1 1 d . . . H11A H 0.0616 -0.0458 1.0786 0.142 Uiso 1 1 calc R . . H11B H 0.0286 -0.1039 1.1214 0.142 Uiso 1 1 calc R . . H11C H 0.0419 -0.1493 1.0722 0.142 Uiso 1 1 calc R . . C12 C 0.1703(6) -0.2123(3) 1.1290(2) 0.125(3) Uani 1 1 d . . . H12A H 0.1352 -0.2111 1.1575 0.187 Uiso 1 1 calc R . . H12B H 0.2341 -0.2237 1.1361 0.187 Uiso 1 1 calc R . . H12C H 0.1472 -0.2592 1.1089 0.187 Uiso 1 1 calc R . . C13 C 0.4354(2) 0.00531(19) 1.18353(10) 0.0453(6) Uani 1 1 d . . . H13A H 0.4556 -0.0562 1.1778 0.054 Uiso 1 1 calc R . . H13B H 0.4689 0.0447 1.1623 0.054 Uiso 1 1 calc R . . C14 C 0.55436(17) 0.01363(17) 1.24054(9) 0.0385(5) Uani 1 1 d . . . H14A H 0.5894 0.0257 1.2122 0.046 Uiso 1 1 calc R . . H14B H 0.5635 -0.0492 1.2490 0.046 Uiso 1 1 calc R . . C15 C 0.58807(16) 0.07419(16) 1.27982(9) 0.0351(5) Uani 1 1 d . . . H15A H 0.6114 0.0375 1.3054 0.042 Uiso 1 1 calc R . . H15B H 0.6381 0.1120 1.2686 0.042 Uiso 1 1 calc R . . C16 C 0.40140(19) -0.02185(17) 1.26508(10) 0.0410(6) Uani 1 1 d . . . H16A H 0.4020 -0.0849 1.2558 0.049 Uiso 1 1 calc R . . H16B H 0.3380 -0.0008 1.2637 0.049 Uiso 1 1 calc R . . C17 C 0.43571(19) -0.01424(16) 1.31464(9) 0.0394(5) Uani 1 1 d . . . H17A H 0.3899 -0.0401 1.3355 0.047 Uiso 1 1 calc R . . H17B H 0.4917 -0.0498 1.3177 0.047 Uiso 1 1 calc R . . C18 C 0.45563(18) 0.08063(16) 1.33017(8) 0.0341(5) Uani 1 1 d . . . H18A H 0.3977 0.1126 1.3344 0.041 Uiso 1 1 calc R . . H18B H 0.4870 0.0789 1.3602 0.041 Uiso 1 1 calc R . . C19 C 0.55249(17) 0.20991(15) 1.31980(9) 0.0347(5) Uani 1 1 d . . . H19A H 0.5878 0.2444 1.2971 0.042 Uiso 1 1 calc R . . H19B H 0.5947 0.1898 1.3440 0.042 Uiso 1 1 calc R . . C20 C 0.48221(19) 0.26928(15) 1.34107(9) 0.0358(5) Uani 1 1 d . . . C21 C 0.4931(2) 0.30218(16) 1.38534(9) 0.0413(6) Uani 1 1 d . . . H21 H 0.5435 0.2832 1.4030 0.050 Uiso 1 1 calc R . . C22 C 0.4322(2) 0.36204(17) 1.40439(10) 0.0486(7) Uani 1 1 d . . . C23 C 0.3589(2) 0.38628(18) 1.37807(10) 0.0503(7) Uani 1 1 d . . . H23 H 0.3166 0.4268 1.3907 0.060 Uiso 1 1 calc R . . C24 C 0.34363(19) 0.35427(16) 1.33362(10) 0.0409(6) Uani 1 1 d . . . C25 C 0.40646(18) 0.29342(15) 1.31500(9) 0.0348(5) Uani 1 1 d . . . C26 C 0.2626(2) 0.38245(19) 1.30570(11) 0.0491(7) Uani 1 1 d . . . H26A H 0.2249 0.3306 1.2990 0.074 Uiso 1 1 calc R . . H26B H 0.2830 0.4092 1.2768 0.074 Uiso 1 1 calc R . . H26C H 0.2272 0.4258 1.3231 0.074 Uiso 1 1 calc R . . C27 C 0.4456(3) 0.4017(2) 1.45340(11) 0.0633(9) Uani 1 1 d . . . C28 C 0.4622(6) 0.5007(3) 1.44793(16) 0.125(3) Uani 1 1 d . . . H28A H 0.4502 0.5307 1.4772 0.187 Uiso 1 1 calc R . . H28B H 0.4218 0.5244 1.4242 0.187 Uiso 1 1 calc R . . H28C H 0.5252 0.5108 1.4389 0.187 Uiso 1 1 calc R . . C29 C 0.5258(5) 0.3613(3) 1.47823(16) 0.106(2) Uani 1 1 d . . . H29A H 0.5813 0.3733 1.4609 0.160 Uiso 1 1 calc R . . H29B H 0.5172 0.2972 1.4809 0.160 Uiso 1 1 calc R . . H29C H 0.5309 0.3873 1.5090 0.160 Uiso 1 1 calc R . . C30 C 0.3592(5) 0.3853(4) 1.48219(15) 0.112(2) Uani 1 1 d . . . H30A H 0.3469 0.3216 1.4836 0.168 Uiso 1 1 calc R . . H30B H 0.3078 0.4156 1.4678 0.168 Uiso 1 1 calc R . . H30C H 0.3681 0.4083 1.5133 0.168 Uiso 1 1 calc R . . C31 C 0.4634(2) -0.2644(2) 1.44688(10) 0.0519(7) Uani 1 1 d . . . H31A H 0.4918 -0.2307 1.4220 0.078 Uiso 1 1 calc R . . H31B H 0.4133 -0.2995 1.4345 0.078 Uiso 1 1 calc R . . H31C H 0.5082 -0.3039 1.4608 0.078 Uiso 1 1 calc R . . C32 C 0.3477(2) -0.02443(17) 1.44897(9) 0.0406(5) Uani 1 1 d . . . C33 C 0.3632(2) 0.06671(17) 1.44172(9) 0.0417(6) Uani 1 1 d . . . C34 C 0.2978(2) 0.11626(19) 1.41861(10) 0.0478(7) Uani 1 1 d . . . H34 H 0.3091 0.1774 1.4135 0.057 Uiso 1 1 calc R . . C35 C 0.2171(2) 0.0807(2) 1.40277(10) 0.0482(7) Uani 1 1 d . . . C36 C 0.2032(2) -0.0102(2) 1.40975(10) 0.0482(7) Uani 1 1 d . . . H36 H 0.1489 -0.0369 1.3990 0.058 Uiso 1 1 calc R . . C37 C 0.2676(2) -0.06248(19) 1.43226(10) 0.0461(6) Uani 1 1 d . . . C38 C 0.4498(2) 0.10758(18) 1.45918(10) 0.0489(7) Uani 1 1 d . . . H38A H 0.4447 0.1723 1.4584 0.073 Uiso 1 1 calc R . . H38B H 0.5004 0.0889 1.4397 0.073 Uiso 1 1 calc R . . H38C H 0.4607 0.0881 1.4908 0.073 Uiso 1 1 calc R . . C39 C 0.1479(2) 0.1371(2) 1.37615(13) 0.0598(8) Uani 1 1 d . . . C40 C 0.0539(3) 0.0950(3) 1.37526(17) 0.0784(12) Uani 1 1 d . . . H40A H 0.0108 0.1363 1.3612 0.118 Uiso 1 1 calc R . . H40B H 0.0347 0.0815 1.4067 0.118 Uiso 1 1 calc R . . H40C H 0.0559 0.0402 1.3573 0.118 Uiso 1 1 calc R . . C41 C 0.1835(3) 0.1510(3) 1.32715(13) 0.0729(11) Uani 1 1 d . . . H41A H 0.2427 0.1800 1.3284 0.109 Uiso 1 1 calc R . . H41B H 0.1411 0.1883 1.3100 0.109 Uiso 1 1 calc R . . H41C H 0.1894 0.0935 1.3118 0.109 Uiso 1 1 calc R . . C42 C 0.1391(3) 0.2300(3) 1.39859(16) 0.0769(11) Uani 1 1 d . . . H42A H 0.1991 0.2572 1.4009 0.115 Uiso 1 1 calc R . . H42B H 0.1129 0.2239 1.4293 0.115 Uiso 1 1 calc R . . H42C H 0.0998 0.2673 1.3797 0.115 Uiso 1 1 calc R . . C43 C 0.2509(2) -0.1606(2) 1.43728(10) 0.0491(7) Uani 1 1 d . . . H43A H 0.1864 -0.1735 1.4309 0.059 Uiso 1 1 calc R . . H43B H 0.2878 -0.1931 1.4145 0.059 Uiso 1 1 calc R . . C44 C 0.25013(19) -0.28766(17) 1.48815(10) 0.0432(6) Uani 1 1 d . . . H44A H 0.2605 -0.3170 1.4582 0.052 Uiso 1 1 calc R . . H44B H 0.1852 -0.2936 1.4960 0.052 Uiso 1 1 calc R . . C45 C 0.30769(18) -0.33274(17) 1.52526(9) 0.0394(5) Uani 1 1 d . . . H45A H 0.2678 -0.3581 1.5492 0.047 Uiso 1 1 calc R . . H45B H 0.3431 -0.3816 1.5114 0.047 Uiso 1 1 calc R . . C46 C 0.22536(18) -0.13963(18) 1.52073(10) 0.0418(6) Uani 1 1 d . . . H46A H 0.1615 -0.1318 1.5113 0.050 Uiso 1 1 calc R . . H46B H 0.2531 -0.0801 1.5231 0.050 Uiso 1 1 calc R . . C47 C 0.22823(17) -0.18395(19) 1.56741(10) 0.0415(6) Uani 1 1 d . . . H47A H 0.1882 -0.2365 1.5668 0.050 Uiso 1 1 calc R . . H47B H 0.2038 -0.1423 1.5906 0.050 Uiso 1 1 calc R . . C48 C 0.32265(16) -0.21314(18) 1.58248(9) 0.0367(5) Uani 1 1 d . . . H48A H 0.3593 -0.1601 1.5896 0.044 Uiso 1 1 calc R . . H48B H 0.3175 -0.2488 1.6109 0.044 Uiso 1 1 calc R . . C49 C 0.44730(17) -0.31640(17) 1.56763(8) 0.0368(5) Uani 1 1 d . . . H49A H 0.4805 -0.3486 1.5433 0.044 Uiso 1 1 calc R . . H49B H 0.4230 -0.3607 1.5894 0.044 Uiso 1 1 calc R . . C50 C 0.51187(16) -0.25627(18) 1.59261(9) 0.0376(5) Uani 1 1 d . . . C51 C 0.54530(18) -0.2820(2) 1.63583(9) 0.0435(6) Uani 1 1 d . . . H51 H 0.5247 -0.3357 1.6493 0.052 Uiso 1 1 calc R . . C52 C 0.60829(19) -0.2298(2) 1.65929(11) 0.0517(7) Uani 1 1 d . A . C53 C 0.6354(2) -0.1527(2) 1.63834(12) 0.0545(8) Uani 1 1 d . . . H53 H 0.6784 -0.1167 1.6538 0.065 Uiso 1 1 calc R . . C54 C 0.60341(17) -0.1236(2) 1.59526(11) 0.0462(7) Uani 1 1 d . . . C55 C 0.53954(15) -0.17738(18) 1.57196(9) 0.0375(5) Uani 1 1 d . . . C56 C 0.6350(2) -0.0385(2) 1.57314(14) 0.0592(9) Uani 1 1 d . . . H56A H 0.6808 -0.0519 1.5498 0.089 Uiso 1 1 calc R . . H56B H 0.6612 0.0003 1.5966 0.089 Uiso 1 1 calc R . . H56C H 0.5834 -0.0088 1.5586 0.089 Uiso 1 1 calc R . . C57 C 0.6443(3) -0.2615(3) 1.70682(13) 0.0707(11) Uani 1 1 d . . . C58 C 0.5886(8) -0.3238(8) 1.7284(3) 0.146(5) Uani 0.80 1 d P A 1 H58A H 0.5292 -0.2974 1.7343 0.219 Uiso 0.80 1 calc PR A 1 H58B H 0.6161 -0.3420 1.7575 0.219 Uiso 0.80 1 calc PR A 1 H58C H 0.5815 -0.3756 1.7084 0.219 Uiso 0.80 1 calc PR A 1 C59 C 0.7388(7) -0.3009(13) 1.6973(4) 0.186(8) Uani 0.80 1 d P A 1 H59A H 0.7766 -0.2564 1.6821 0.278 Uiso 0.80 1 calc PR A 1 H59B H 0.7328 -0.3529 1.6773 0.278 Uiso 0.80 1 calc PR A 1 H59C H 0.7670 -0.3185 1.7263 0.278 Uiso 0.80 1 calc PR A 1 C60 C 0.6545(8) -0.1791(7) 1.7374(2) 0.132(4) Uani 0.80 1 d P A 1 H60A H 0.6944 -0.1363 1.7222 0.198 Uiso 0.80 1 calc PR A 1 H60B H 0.6805 -0.1963 1.7670 0.198 Uiso 0.80 1 calc PR A 1 H60C H 0.5949 -0.1522 1.7423 0.198 Uiso 0.80 1 calc PR A 1 C61 C 0.1512(4) 0.4549(4) 1.1890(2) 0.0954(15) Uani 1 1 d . . . H61A H 0.1667 0.4232 1.2173 0.143 Uiso 1 1 calc R . . H61B H 0.0983 0.4271 1.1747 0.143 Uiso 1 1 calc R . . H61C H 0.1375 0.5168 1.1962 0.143 Uiso 1 1 calc R . . C62 C 0.2282(2) 0.4511(2) 1.15698(15) 0.0639(9) Uani 1 1 d . . . C63 C 0.2934(3) 0.3845(2) 1.15963(14) 0.0613(9) Uani 1 1 d . . . H63 H 0.2889 0.3402 1.1827 0.074 Uiso 1 1 calc R . . C64 C 0.3640(2) 0.3829(2) 1.12901(15) 0.0633(10) Uani 1 1 d . . . H64 H 0.4080 0.3371 1.1310 0.076 Uiso 1 1 calc R . . C65 C 0.3720(3) 0.4471(3) 1.09519(16) 0.0698(11) Uani 1 1 d . . . H65 H 0.4207 0.4453 1.0739 0.084 Uiso 1 1 calc R . . C66 C 0.3079(3) 0.5139(3) 1.09286(17) 0.0745(11) Uani 1 1 d . . . H66 H 0.3130 0.5587 1.0701 0.089 Uiso 1 1 calc R . . C67 C 0.2361(3) 0.5156(2) 1.12367(15) 0.0687(11) Uani 1 1 d . . . H67 H 0.1923 0.5615 1.1218 0.082 Uiso 1 1 calc R . . C58' C 0.5586(3) -0.2790(2) 1.74133(15) 0.090(13) Uani 0.20 1 d P A 2 H58D H 0.5150 -0.3184 1.7264 0.134 Uiso 0.20 1 calc PR B 2 H58E H 0.5293 -0.2224 1.7486 0.134 Uiso 0.20 1 calc PR C 2 H58F H 0.5803 -0.3065 1.7697 0.134 Uiso 0.20 1 calc PR D 2 C60' C 0.7053(3) -0.2014(2) 1.73255(15) 0.073(7) Uani 0.20 1 d P A 2 H60D H 0.6774 -0.1427 1.7349 0.109 Uiso 0.20 1 calc PR E 2 H60E H 0.7632 -0.1965 1.7163 0.109 Uiso 0.20 1 calc PR F 2 H60F H 0.7157 -0.2252 1.7634 0.109 Uiso 0.20 1 calc PR G 2 C59' C 0.689(2) -0.355(3) 1.7040(10) 0.107(13) Uani 0.20 1 d P A 2 H59D H 0.6973 -0.3787 1.7351 0.161 Uiso 0.20 1 calc PR A 2 H59E H 0.7475 -0.3506 1.6886 0.161 Uiso 0.20 1 calc PR A 2 H59F H 0.6493 -0.3951 1.6866 0.161 Uiso 0.20 1 calc PR A 2 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 0.0334(3) 0.0314(3) 0.0259(3) 0.0020(2) -0.0031(3) 0.0050(3) O1 0.0383(9) 0.0491(10) 0.0436(10) -0.0061(8) -0.0146(8) 0.0102(8) N1 0.0350(10) 0.0361(10) 0.0337(10) -0.0057(8) -0.0104(8) 0.0048(8) C1 0.0582(18) 0.0529(16) 0.0479(16) 0.0139(13) 0.0120(13) 0.0077(14) Al2 0.0346(3) 0.0325(3) 0.0290(3) 0.0011(3) 0.0005(3) -0.0076(3) O2 0.0438(9) 0.0349(8) 0.0344(9) -0.0027(7) -0.0036(7) 0.0129(7) N2 0.0312(9) 0.0286(9) 0.0257(9) -0.0010(7) -0.0030(7) 0.0026(7) C2 0.0426(14) 0.0513(15) 0.0351(13) 0.0057(11) -0.0143(10) 0.0000(11) O3 0.0500(11) 0.0356(9) 0.0480(10) 0.0110(8) -0.0088(9) -0.0124(8) N3 0.0392(10) 0.0361(10) 0.0365(11) 0.0064(8) -0.0086(8) -0.0101(8) C3 0.0450(15) 0.0566(16) 0.0427(14) 0.0118(12) -0.0131(12) 0.0041(13) O4 0.0339(8) 0.0420(9) 0.0462(10) 0.0003(8) -0.0036(8) -0.0101(7) N4 0.0297(9) 0.0369(10) 0.0296(9) 0.0002(8) -0.0033(7) -0.0062(8) C4 0.0439(15) 0.0663(19) 0.0480(16) 0.0117(14) -0.0173(13) -0.0066(14) C5 0.0565(18) 0.0516(16) 0.0476(16) 0.0085(13) -0.0211(14) -0.0076(13) C6 0.0597(18) 0.0428(14) 0.0488(16) -0.0019(12) -0.0201(14) 0.0004(13) C7 0.0499(15) 0.0451(14) 0.0430(14) -0.0022(11) -0.0199(12) 0.0019(12) C8 0.0409(14) 0.083(2) 0.0479(16) 0.0069(16) -0.0064(12) 0.0079(15) C9 0.071(2) 0.0565(17) 0.0586(19) 0.0066(15) -0.0242(17) -0.0172(17) C10 0.086(3) 0.116(4) 0.066(2) -0.035(2) -0.007(2) -0.032(3) C11 0.064(2) 0.126(4) 0.093(3) -0.041(3) -0.025(2) -0.010(3) C12 0.205(7) 0.064(2) 0.105(4) 0.015(3) -0.090(5) -0.044(3) C13 0.0493(15) 0.0480(14) 0.0386(13) -0.0151(11) -0.0151(12) 0.0082(12) C14 0.0374(12) 0.0399(12) 0.0381(12) -0.0106(10) -0.0051(10) 0.0102(10) C15 0.0308(11) 0.0341(11) 0.0404(12) -0.0045(9) -0.0049(9) 0.0078(9) C16 0.0426(13) 0.0331(11) 0.0473(15) 0.0030(10) -0.0110(11) -0.0010(10) C17 0.0435(13) 0.0306(11) 0.0440(13) 0.0068(10) -0.0065(11) 0.0023(10) C18 0.0404(12) 0.0350(11) 0.0270(11) 0.0029(9) 0.0014(9) 0.0029(10) C19 0.0374(12) 0.0306(10) 0.0360(12) -0.0030(9) -0.0048(10) 0.0022(9) C20 0.0466(14) 0.0266(10) 0.0342(12) -0.0015(9) 0.0007(10) 0.0023(9) C21 0.0597(16) 0.0275(11) 0.0365(13) 0.0008(9) -0.0054(11) 0.0014(11) C22 0.073(2) 0.0326(12) 0.0401(14) -0.0045(10) 0.0046(13) 0.0042(13) C23 0.071(2) 0.0326(12) 0.0471(15) -0.0008(11) 0.0158(14) 0.0142(13) C24 0.0465(14) 0.0314(11) 0.0447(14) 0.0044(10) 0.0093(11) 0.0061(10) C25 0.0422(13) 0.0244(9) 0.0380(12) 0.0024(9) 0.0027(10) 0.0037(9) C26 0.0488(15) 0.0395(13) 0.0589(18) 0.0083(12) 0.0099(13) 0.0150(12) C27 0.105(3) 0.0447(15) 0.0400(15) -0.0127(12) -0.0012(17) 0.0094(17) C28 0.260(9) 0.056(2) 0.058(2) -0.0228(19) -0.007(4) -0.004(4) C29 0.166(6) 0.087(3) 0.065(3) -0.040(2) -0.046(3) 0.030(3) C30 0.167(6) 0.127(4) 0.042(2) -0.008(2) 0.030(3) 0.013(4) C31 0.0666(19) 0.0465(15) 0.0426(15) -0.0064(12) 0.0115(14) -0.0098(14) C32 0.0492(14) 0.0392(12) 0.0333(12) 0.0050(10) 0.0038(11) -0.0041(11) C33 0.0543(16) 0.0384(12) 0.0325(12) 0.0015(10) 0.0116(11) -0.0042(11) C34 0.0611(17) 0.0379(13) 0.0444(15) 0.0110(11) 0.0153(13) 0.0028(12) C35 0.0521(16) 0.0531(16) 0.0393(14) 0.0148(12) 0.0119(12) 0.0106(13) C36 0.0487(15) 0.0564(16) 0.0394(14) 0.0137(12) 0.0008(12) -0.0046(13) C37 0.0491(15) 0.0445(14) 0.0446(15) 0.0130(11) -0.0036(12) -0.0055(12) C38 0.0667(19) 0.0403(13) 0.0398(14) 0.0052(11) 0.0033(13) -0.0114(13) C39 0.0533(17) 0.067(2) 0.0594(19) 0.0238(16) 0.0095(15) 0.0134(16) C40 0.054(2) 0.084(3) 0.097(3) 0.032(2) -0.011(2) 0.0042(19) C41 0.075(2) 0.087(3) 0.056(2) 0.0308(19) 0.0034(18) 0.021(2) C42 0.076(3) 0.072(2) 0.083(3) 0.012(2) 0.012(2) 0.026(2) C43 0.0543(16) 0.0506(15) 0.0424(15) 0.0101(12) -0.0185(12) -0.0150(13) C44 0.0471(14) 0.0393(12) 0.0433(14) 0.0043(10) -0.0124(11) -0.0171(11) C45 0.0427(13) 0.0354(12) 0.0402(13) 0.0074(10) -0.0081(10) -0.0145(10) C46 0.0344(12) 0.0437(13) 0.0473(15) 0.0078(11) -0.0001(10) -0.0042(10) C47 0.0304(11) 0.0492(14) 0.0448(14) 0.0050(11) 0.0032(10) -0.0025(11) C48 0.0323(11) 0.0480(13) 0.0299(11) -0.0017(10) 0.0026(9) -0.0040(10) C49 0.0362(11) 0.0404(12) 0.0339(11) 0.0056(10) -0.0016(9) -0.0009(10) C50 0.0255(10) 0.0525(14) 0.0348(12) -0.0035(10) -0.0019(9) 0.0043(10) C51 0.0313(12) 0.0634(17) 0.0357(13) -0.0009(12) -0.0001(10) 0.0062(11) C52 0.0345(13) 0.078(2) 0.0422(15) -0.0130(14) -0.0079(11) 0.0070(14) C53 0.0344(13) 0.073(2) 0.0566(18) -0.0198(15) -0.0099(12) -0.0012(13) C54 0.0268(11) 0.0517(15) 0.0600(18) -0.0202(13) -0.0020(11) 0.0000(11) C55 0.0250(10) 0.0457(13) 0.0417(13) -0.0094(11) 0.0004(9) 0.0004(10) C56 0.0379(14) 0.0525(16) 0.087(2) -0.0211(16) -0.0052(15) -0.0097(13) C57 0.0533(19) 0.108(3) 0.0512(19) -0.007(2) -0.0221(16) 0.012(2) C58 0.185(10) 0.171(9) 0.082(5) 0.062(6) -0.083(6) -0.070(9) C59 0.106(7) 0.36(2) 0.095(6) 0.018(10) -0.030(6) 0.125(11) C60 0.204(11) 0.141(7) 0.050(3) -0.001(4) -0.049(5) -0.011(8) C61 0.075(3) 0.113(4) 0.098(4) -0.017(3) -0.014(3) 0.003(3) C62 0.0500(18) 0.062(2) 0.080(2) -0.0225(18) -0.0161(17) -0.0079(15) C63 0.061(2) 0.0475(16) 0.075(2) -0.0149(15) -0.0261(18) -0.0049(14) C64 0.0491(18) 0.0517(17) 0.089(3) -0.0225(17) -0.0274(18) 0.0005(14) C65 0.056(2) 0.066(2) 0.087(3) -0.024(2) -0.0217(19) -0.0111(17) C66 0.075(3) 0.059(2) 0.089(3) -0.0043(19) -0.033(2) -0.0111(19) C67 0.061(2) 0.0478(17) 0.097(3) -0.0132(18) -0.040(2) 0.0051(15) C58' 0.038(8) 0.20(4) 0.026(8) 0.021(13) -0.005(7) -0.003(13) C60' 0.082(14) 0.109(18) 0.028(8) -0.018(9) -0.035(9) 0.000(12) C59' 0.088(19) 0.18(3) 0.050(12) -0.007(16) -0.025(14) 0.10(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 1.7873(19) . ? Al1 O2 1.7975(18) . ? Al1 C1 1.980(3) . ? Al1 N2 2.108(2) . ? Al1 N1 2.132(2) . ? O1 C2 1.365(3) . ? N1 C14 1.478(3) . ? N1 C16 1.491(4) . ? N1 C13 1.500(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Al2 O3 1.7850(19) . ? Al2 O4 1.7991(19) . ? Al2 C31 1.977(3) . ? Al2 N4 2.114(2) . ? Al2 N3 2.131(2) . ? O2 C25 1.342(3) . ? N2 C15 1.479(3) . ? N2 C19 1.497(3) . ? N2 C18 1.501(3) . ? C2 C7 1.381(4) . ? C2 C3 1.408(4) . ? O3 C32 1.337(3) . ? N3 C44 1.488(3) . ? N3 C43 1.499(3) . ? N3 C46 1.504(4) . ? C3 C4 1.410(5) . ? C3 C8 1.500(5) . ? O4 C55 1.334(3) . ? N4 C45 1.492(3) . ? N4 C49 1.496(3) . ? N4 C48 1.502(3) . ? C4 C5 1.395(5) . ? C4 H4 0.9500 . ? C5 C6 1.399(5) . ? C5 C9 1.544(4) . ? C6 C7 1.408(4) . ? C6 H6 0.9500 . ? C7 C13 1.506(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.502(6) . ? C9 C11 1.503(6) . ? C9 C10 1.523(6) . ? 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 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.547(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.534(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.531(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.506(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.391(4) . ? C20 C25 1.401(4) . ? C21 C22 1.391(4) . ? C21 H21 0.9500 . ? C22 C23 1.376(5) . ? C22 C27 1.560(4) . ? C23 C24 1.400(4) . ? C23 H23 0.9500 . ? C24 C25 1.415(3) . ? C24 C26 1.509(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.517(7) . ? C27 C28 1.524(6) . ? C27 C30 1.548(8) . ? 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 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.403(4) . ? C32 C33 1.411(4) . ? C33 C34 1.395(4) . ? C33 C38 1.510(4) . ? C34 C35 1.387(5) . ? C34 H34 0.9500 . ? C35 C36 1.403(4) . ? C35 C39 1.540(4) . ? C36 C37 1.400(4) . ? C36 H36 0.9500 . ? C37 C43 1.510(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.528(6) . ? C39 C41 1.535(5) . ? C39 C42 1.552(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.534(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.516(4) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.528(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.505(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C55 1.396(4) . ? C50 C51 1.407(4) . ? C51 C52 1.398(4) . ? C51 H51 0.9500 . ? C52 C53 1.375(5) . ? C52 C57 1.558(5) . ? C53 C54 1.411(5) . ? C53 H53 0.9500 . ? C54 C55 1.418(4) . ? C54 C56 1.511(5) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.398(10) . ? C57 C60' 1.484(5) . ? C57 C60 1.537(10) . ? C57 C59 1.544(10) . ? C57 C59' 1.56(3) . ? C57 C58' 1.637(7) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.472(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C67 1.379(6) . ? C62 C63 1.395(5) . ? C63 C64 1.373(6) . ? C63 H63 0.9500 . ? C64 C65 1.387(6) . ? C64 H64 0.9500 . ? C65 C66 1.386(6) . ? C65 H65 0.9500 . ? C66 C67 1.389(7) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C58' H58D 0.9800 . ? C58' H58E 0.9800 . ? C58' H58F 0.9800 . ? C60' H60D 0.9800 . ? C60' H60E 0.9800 . ? C60' H60F 0.9800 . ? C59' H59D 0.9800 . ? C59' H59E 0.9800 . ? C59' H59F 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 91.79(9) . . ? O1 Al1 C1 114.29(13) . . ? O2 Al1 C1 106.86(12) . . ? O1 Al1 N2 139.94(10) . . ? O2 Al1 N2 89.13(8) . . ? C1 Al1 N2 103.63(12) . . ? O1 Al1 N1 86.98(9) . . ? O2 Al1 N1 150.87(9) . . ? C1 Al1 N1 100.09(12) . . ? N2 Al1 N1 73.74(8) . . ? C2 O1 Al1 134.59(17) . . ? C14 N1 C16 109.9(2) . . ? C14 N1 C13 108.8(2) . . ? C16 N1 C13 110.8(2) . . ? C14 N1 Al1 108.07(15) . . ? C16 N1 Al1 111.17(16) . . ? C13 N1 Al1 108.10(16) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 Al2 O4 91.03(9) . . ? O3 Al2 C31 111.41(12) . . ? O4 Al2 C31 108.94(13) . . ? O3 Al2 N4 143.58(10) . . ? O4 Al2 N4 88.01(9) . . ? C31 Al2 N4 103.25(11) . . ? O3 Al2 N3 87.94(9) . . ? O4 Al2 N3 147.02(10) . . ? C31 Al2 N3 102.05(13) . . ? N4 Al2 N3 73.93(8) . . ? C25 O2 Al1 135.92(16) . . ? C15 N2 C19 108.51(18) . . ? C15 N2 C18 110.49(18) . . ? C19 N2 C18 108.96(18) . . ? C15 N2 Al1 108.66(14) . . ? C19 N2 Al1 110.63(14) . . ? C18 N2 Al1 109.58(14) . . ? O1 C2 C7 122.9(2) . . ? O1 C2 C3 118.6(3) . . ? C7 C2 C3 118.5(3) . . ? C32 O3 Al2 135.70(17) . . ? C44 N3 C43 108.5(2) . . ? C44 N3 C46 110.3(2) . . ? C43 N3 C46 111.3(2) . . ? C44 N3 Al2 107.57(16) . . ? C43 N3 Al2 108.71(17) . . ? C46 N3 Al2 110.35(15) . . ? C2 C3 C4 118.7(3) . . ? C2 C3 C8 120.0(3) . . ? C4 C3 C8 121.3(3) . . ? C55 O4 Al2 135.90(17) . . ? C45 N4 C49 107.96(19) . . ? C45 N4 C48 111.0(2) . . ? C49 N4 C48 109.72(18) . . ? C45 N4 Al2 108.05(14) . . ? C49 N4 Al2 110.82(15) . . ? C48 N4 Al2 109.29(15) . . ? C5 C4 C3 123.6(3) . . ? C5 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? C4 C5 C6 116.2(3) . . ? C4 C5 C9 123.8(3) . . ? C6 C5 C9 120.0(3) . . ? C5 C6 C7 121.2(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C2 C7 C6 121.7(3) . . ? C2 C7 C13 120.4(2) . . ? C6 C7 C13 117.9(3) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 C11 111.4(5) . . ? C12 C9 C10 109.0(5) . . ? C11 C9 C10 105.6(4) . . ? C12 C9 C5 109.1(3) . . ? C11 C9 C5 111.4(4) . . ? C10 C9 C5 110.2(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C7 111.7(2) . . ? N1 C13 H13A 109.3 . . ? C7 C13 H13A 109.3 . . ? N1 C13 H13B 109.3 . . ? C7 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N1 C14 C15 109.52(19) . . ? N1 C14 H14A 109.8 . . ? C15 C14 H14A 109.8 . . ? N1 C14 H14B 109.8 . . ? C15 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? N2 C15 C14 109.90(19) . . ? N2 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N2 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N1 C16 C17 112.5(2) . . ? N1 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N1 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C16 114.3(2) . . ? C18 C17 H17A 108.7 . . ? C16 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? C16 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N2 C18 C17 112.65(19) . . ? N2 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? N2 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? N2 C19 C20 113.3(2) . . ? N2 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? N2 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C25 120.1(2) . . ? C21 C20 C19 120.9(2) . . ? C25 C20 C19 118.9(2) . . ? C20 C21 C22 121.8(3) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 117.4(3) . . ? C23 C22 C27 120.5(3) . . ? C21 C22 C27 122.2(3) . . ? C22 C23 C24 123.4(3) . . ? C22 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C25 118.2(3) . . ? C23 C24 C26 121.9(2) . . ? C25 C24 C26 119.9(3) . . ? O2 C25 C20 121.7(2) . . ? O2 C25 C24 119.2(2) . . ? C20 C25 C24 119.1(2) . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 108.6(5) . . ? C29 C27 C30 108.8(4) . . ? C28 C27 C30 110.3(5) . . ? C29 C27 C22 112.4(3) . . ? C28 C27 C22 107.5(3) . . ? C30 C27 C22 109.2(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Al2 C31 H31A 109.5 . . ? Al2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Al2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O3 C32 C37 122.2(2) . . ? O3 C32 C33 118.8(3) . . ? C37 C32 C33 119.0(3) . . ? C34 C33 C32 118.9(3) . . ? C34 C33 C38 122.1(2) . . ? C32 C33 C38 119.1(3) . . ? C35 C34 C33 123.2(3) . . ? C35 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? C34 C35 C36 117.2(3) . . ? C34 C35 C39 121.6(3) . . ? C36 C35 C39 121.1(3) . . ? C37 C36 C35 121.3(3) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C32 120.4(3) . . ? C36 C37 C43 119.2(3) . . ? C32 C37 C43 120.4(3) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C41 110.6(4) . . ? C40 C39 C35 112.4(3) . . ? C41 C39 C35 108.4(3) . . ? C40 C39 C42 107.9(3) . . ? C41 C39 C42 107.3(3) . . ? C35 C39 C42 110.1(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N3 C43 C37 111.3(2) . . ? N3 C43 H43A 109.4 . . ? C37 C43 H43A 109.4 . . ? N3 C43 H43B 109.4 . . ? C37 C43 H43B 109.4 . . ? H43A C43 H43B 108.0 . . ? N3 C44 C45 110.2(2) . . ? N3 C44 H44A 109.6 . . ? C45 C44 H44A 109.6 . . ? N3 C44 H44B 109.6 . . ? C45 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? N4 C45 C44 109.8(2) . . ? N4 C45 H45A 109.7 . . ? C44 C45 H45A 109.7 . . ? N4 C45 H45B 109.7 . . ? C44 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? N3 C46 C47 112.4(2) . . ? N3 C46 H46A 109.1 . . ? C47 C46 H46A 109.1 . . ? N3 C46 H46B 109.1 . . ? C47 C46 H46B 109.1 . . ? H46A C46 H46B 107.9 . . ? C46 C47 C48 114.2(2) . . ? C46 C47 H47A 108.7 . . ? C48 C47 H47A 108.7 . . ? C46 C47 H47B 108.7 . . ? C48 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N4 C48 C47 112.5(2) . . ? N4 C48 H48A 109.1 . . ? C47 C48 H48A 109.1 . . ? N4 C48 H48B 109.1 . . ? C47 C48 H48B 109.1 . . ? H48A C48 H48B 107.8 . . ? N4 C49 C50 112.4(2) . . ? N4 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? N4 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C55 C50 C51 121.2(3) . . ? C55 C50 C49 119.5(2) . . ? C51 C50 C49 119.3(3) . . ? C52 C51 C50 121.0(3) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C53 C52 C51 117.1(3) . . ? C53 C52 C57 123.7(3) . . ? C51 C52 C57 119.2(3) . . ? C52 C53 C54 124.1(3) . . ? C52 C53 H53 118.0 . . ? C54 C53 H53 118.0 . . ? C53 C54 C55 118.1(3) . . ? C53 C54 C56 122.7(3) . . ? C55 C54 C56 119.3(3) . . ? O4 C55 C50 122.8(2) . . ? O4 C55 C54 118.7(3) . . ? C50 C55 C54 118.6(3) . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C60' 122.9(5) . . ? C58 C57 C60 110.0(7) . . ? C60' C57 C60 32.1(5) . . ? C58 C57 C59 110.8(9) . . ? C60' C57 C59 77.1(7) . . ? C60 C57 C59 109.1(9) . . ? C58 C57 C52 113.9(4) . . ? C60' C57 C52 117.9(4) . . ? C60 C57 C52 107.4(4) . . ? C59 C57 C52 105.5(5) . . ? C58 C57 C59' 70.3(17) . . ? C60' C57 C59' 109.0(13) . . ? C60 C57 C59' 136.3(12) . . ? C59 C57 C59' 42.3(15) . . ? C52 C57 C59' 112.0(10) . . ? C58 C57 C58' 33.0(6) . . ? C60' C57 C58' 105.0(3) . . ? C60 C57 C58' 81.4(5) . . ? C59 C57 C58' 138.4(7) . . ? C52 C57 C58' 109.3(3) . . ? C59' C57 C58' 102.2(16) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C67 C62 C63 119.3(4) . . ? C67 C62 C61 118.9(4) . . ? C63 C62 C61 121.8(4) . . ? C64 C63 C62 120.1(4) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C63 C64 C65 120.9(4) . . ? C63 C64 H64 119.6 . . ? C65 C64 H64 119.6 . . ? C66 C65 C64 119.0(4) . . ? C66 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? C65 C66 C67 120.3(4) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C62 C67 C66 120.4(4) . . ? C62 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C57 C58' H58D 109.5 . . ? C57 C58' H58E 109.5 . . ? H58D C58' H58E 109.5 . . ? C57 C58' H58F 109.5 . . ? H58D C58' H58F 109.5 . . ? H58E C58' H58F 109.5 . . ? C57 C60' H60D 109.5 . . ? C57 C60' H60E 109.5 . . ? H60D C60' H60E 109.5 . . ? C57 C60' H60F 109.5 . . ? H60D C60' H60F 109.5 . . ? H60E C60' H60F 109.5 . . ? C57 C59' H59D 109.5 . . ? C57 C59' H59E 109.5 . . ? H59D C59' H59E 109.5 . . ? C57 C59' H59F 109.5 . . ? H59D C59' H59F 109.5 . . ? H59E C59' H59F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.450 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.058 #====END data_Al(5)Me _database_code_depnum_ccdc_archive 'CCDC 877944' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H49 Al N2 O2' _chemical_formula_weight 556.74 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 32.935(3) _cell_length_b 7.0560(10) _cell_length_c 31.375(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.289(5) _cell_angle_gamma 90.00 _cell_volume 6645.8(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 118414 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'NB the half occupied H atom on C30 was not refined in the model' Bond lengths in the disorded tBu and toluene solvent moieties have been restrained, to the appropriate C-C distance, to assit convergence ; _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 24788 _diffrn_reflns_av_R_equivalents 0.1342 _diffrn_reflns_av_sigmaI/netI 0.1149 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5755 _reflns_number_gt 3246 _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^)+(0.1082P)^2^+33.2978P] 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 SHELXL _refine_ls_extinction_coef 0.0046(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5755 _refine_ls_number_parameters 395 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1818 _refine_ls_R_factor_gt 0.1154 _refine_ls_wR_factor_ref 0.3088 _refine_ls_wR_factor_gt 0.2713 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.085 _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 Al Al 0.17905(6) 0.0263(2) 0.62662(6) 0.0478(6) Uani 1 1 d . . . O1 O 0.16154(13) -0.1107(5) 0.57423(12) 0.0520(11) Uani 1 1 d . . . N1 N 0.14823(14) 0.2636(6) 0.58503(14) 0.0424(11) Uiso 1 1 d . . . C1 C 0.1410(2) -0.0182(10) 0.6602(2) 0.0649(18) Uani 1 1 d . . . H1A H 0.1332 -0.1529 0.6584 0.097 Uiso 1 1 calc R . . H1B H 0.1137 0.0572 0.6458 0.097 Uiso 1 1 calc R . . H1C H 0.1570 0.0190 0.6930 0.097 Uiso 1 1 calc R . . O2 O 0.22747(13) -0.1210(5) 0.65320(15) 0.0645(13) Uani 1 1 d . . . N2 N 0.21779(15) 0.2607(6) 0.66158(15) 0.0451(11) Uani 1 1 d . . . C2 C 0.13571(19) -0.0797(8) 0.5284(2) 0.0487(15) Uani 1 1 d . A . C3 C 0.1377(2) -0.1990(8) 0.4943(2) 0.0568(16) Uani 1 1 d . . . H3 H 0.1580 -0.3023 0.5032 0.068 Uiso 1 1 calc R . . C4 C 0.1106(2) -0.1703(9) 0.4473(2) 0.0612(17) Uani 1 1 d . A . H4 H 0.1120 -0.2573 0.4249 0.073 Uiso 1 1 calc R . . C5 C 0.0815(2) -0.0181(9) 0.4322(2) 0.0627(18) Uani 1 1 d . . . C6 C 0.0802(2) 0.1010(9) 0.4664(2) 0.0575(17) Uani 1 1 d . A . H6 H 0.0608 0.2073 0.4570 0.069 Uiso 1 1 calc R . . C7 C 0.10568(19) 0.0741(8) 0.51393(19) 0.0473(14) Uani 1 1 d . . . C8 C 0.0478(7) 0.008(3) 0.3832(9) 0.090(9) Uani 0.60 1 d PD A 1 C9 C 0.0508(6) 0.215(3) 0.3681(4) 0.064(7) Uani 0.60 1 d PD A 1 H9A H 0.0420 0.3021 0.3871 0.096 Uiso 0.60 1 calc PR A 1 H9B H 0.0308 0.2310 0.3350 0.096 Uiso 0.60 1 calc PR A 1 H9C H 0.0814 0.2425 0.3726 0.096 Uiso 0.60 1 calc PR A 1 C10 C -0.0020(5) -0.005(2) 0.3737(5) 0.081(5) Uani 0.60 1 d PD A 1 H10A H -0.0087 -0.1333 0.3810 0.122 Uiso 0.60 1 calc PR A 1 H10B H -0.0203 0.0228 0.3407 0.122 Uiso 0.60 1 calc PR A 1 H10C H -0.0086 0.0868 0.3934 0.122 Uiso 0.60 1 calc PR A 1 C11 C 0.0539(7) -0.121(3) 0.3470(6) 0.108(7) Uani 0.60 1 d PD A 1 H11A H 0.0843 -0.1070 0.3491 0.162 Uiso 0.60 1 calc PR A 1 H11B H 0.0325 -0.0853 0.3156 0.162 Uiso 0.60 1 calc PR A 1 H11C H 0.0489 -0.2531 0.3532 0.162 Uiso 0.60 1 calc PR A 1 C8A C 0.0560(9) 0.026(4) 0.3770(11) 0.059(9) Uani 0.40 1 d PD A 2 C9A C 0.0512(17) 0.241(4) 0.3652(16) 0.14(2) Uani 0.40 1 d PD A 2 H9A1 H 0.0412 0.2580 0.3314 0.210 Uiso 0.40 1 calc PR A 2 H9A2 H 0.0800 0.3037 0.3816 0.210 Uiso 0.40 1 calc PR A 2 H9A3 H 0.0292 0.2965 0.3751 0.210 Uiso 0.40 1 calc PR A 2 C10A C 0.0188(12) -0.124(5) 0.3659(10) 0.150(17) Uani 0.40 1 d PD A 2 H10D H -0.0007 -0.0887 0.3813 0.225 Uiso 0.40 1 calc PR A 2 H10E H 0.0322 -0.2482 0.3773 0.225 Uiso 0.40 1 calc PR A 2 H10F H 0.0012 -0.1303 0.3320 0.225 Uiso 0.40 1 calc PR A 2 C11A C 0.0845(10) -0.050(4) 0.3516(8) 0.110(11) Uani 0.40 1 d PD A 2 H11D H 0.0828 -0.1883 0.3500 0.165 Uiso 0.40 1 calc PR A 2 H11E H 0.1156 -0.0107 0.3689 0.165 Uiso 0.40 1 calc PR A 2 H11F H 0.0731 0.0024 0.3198 0.165 Uiso 0.40 1 calc PR A 2 C12 C 0.1032(2) 0.2090(8) 0.5496(2) 0.0553(16) Uani 1 1 d . A . H12A H 0.0871 0.3245 0.5335 0.066 Uiso 1 1 calc R . . H12B H 0.0861 0.1496 0.5656 0.066 Uiso 1 1 calc R . . C13 C 0.1437(2) 0.4091(9) 0.6169(2) 0.0558(16) Uani 1 1 d . . . H13A H 0.1172 0.3811 0.6232 0.067 Uiso 1 1 calc R . . H13B H 0.1396 0.5355 0.6020 0.067 Uiso 1 1 calc R . . C14 C 0.1864(2) 0.4088(8) 0.6636(2) 0.0552(16) Uani 1 1 d . . . H14A H 0.2009 0.5347 0.6685 0.066 Uiso 1 1 calc R . . H14B H 0.1783 0.3829 0.6901 0.066 Uiso 1 1 calc R . . C15 C 0.1749(2) 0.3384(8) 0.56021(19) 0.0511(15) Uani 1 1 d . . . H15A H 0.1560 0.4238 0.5348 0.061 Uiso 1 1 calc R . . H15B H 0.1841 0.2313 0.5458 0.061 Uiso 1 1 calc R . . C16 C 0.2162(2) 0.4460(8) 0.5924(2) 0.0544(16) Uani 1 1 d . . . H16A H 0.2071 0.5664 0.6020 0.065 Uiso 1 1 calc R . . H16B H 0.2346 0.4775 0.5750 0.065 Uiso 1 1 calc R . . C17 C 0.24426(19) 0.3317(8) 0.6358(2) 0.0500(15) Uani 1 1 d . . . H17A H 0.2576 0.2223 0.6264 0.060 Uiso 1 1 calc R . . H17B H 0.2689 0.4120 0.6571 0.060 Uiso 1 1 calc R . . C18 C 0.24859(19) 0.2069(8) 0.71037(18) 0.0503(15) Uani 1 1 d . . . H18A H 0.2315 0.1451 0.7261 0.060 Uiso 1 1 calc R . . H18B H 0.2628 0.3222 0.7283 0.060 Uiso 1 1 calc R . . C19 C 0.2843(2) 0.0721(8) 0.70948(19) 0.0523(15) Uani 1 1 d . . . C20 C 0.3299(2) 0.1059(9) 0.73514(19) 0.0527(16) Uani 1 1 d . . . H20 H 0.3385 0.2150 0.7546 0.063 Uiso 1 1 calc R . . C21 C 0.3624(2) -0.0091(9) 0.7337(2) 0.0535(15) Uani 1 1 d . . . C22 C 0.3489(2) -0.1656(10) 0.7042(2) 0.0639(18) Uani 1 1 d . . . H22 H 0.3706 -0.2486 0.7020 0.077 Uiso 1 1 calc R . . C23 C 0.3039(2) -0.2021(9) 0.6780(2) 0.0657(19) Uani 1 1 d . . . H23 H 0.2956 -0.3105 0.6583 0.079 Uiso 1 1 calc R . . C24 C 0.2712(2) -0.0847(8) 0.6798(2) 0.0570(17) Uani 1 1 d . . . C25 C 0.4119(2) 0.0370(10) 0.7619(2) 0.0599(17) Uani 1 1 d . . . C26 C 0.4207(3) 0.2434(13) 0.7522(3) 0.102(3) Uani 1 1 d . . . H26A H 0.4032 0.3292 0.7627 0.152 Uiso 1 1 calc R . . H26B H 0.4120 0.2605 0.7185 0.152 Uiso 1 1 calc R . . H26C H 0.4525 0.2720 0.7691 0.152 Uiso 1 1 calc R . . C27 C 0.4234(2) 0.0160(11) 0.8132(2) 0.071(2) Uani 1 1 d . . . H27A H 0.4042 0.0990 0.8220 0.107 Uiso 1 1 calc R . . H27B H 0.4546 0.0512 0.8312 0.107 Uiso 1 1 calc R . . H27C H 0.4189 -0.1159 0.8200 0.107 Uiso 1 1 calc R . . C28 C 0.4423(2) -0.0883(15) 0.7493(3) 0.108(3) Uani 1 1 d . . . H28A H 0.4733 -0.0486 0.7670 0.163 Uiso 1 1 calc R . . H28B H 0.4348 -0.0775 0.7157 0.163 Uiso 1 1 calc R . . H28C H 0.4388 -0.2202 0.7569 0.163 Uiso 1 1 calc R . . C29 C 0.0451(5) -0.215(2) 0.5636(5) 0.082(4) Uani 0.50 1 d PD B 1 H29A H 0.0764 -0.2048 0.5688 0.122 Uiso 0.50 1 calc PR . . H29B H 0.0431 -0.2410 0.5934 0.122 Uiso 0.50 1 calc PR . . H29C H 0.0298 -0.0954 0.5506 0.122 Uiso 0.50 1 calc PR . . C30 C 0.0239(3) -0.3693(13) 0.5307(3) 0.102(3) Uani 1 1 d D . . C31 C 0.0194(4) -0.3514(15) 0.4854(4) 0.111(3) Uani 1 1 d . B . H31 H 0.0322 -0.2475 0.4760 0.133 Uiso 1 1 calc R . . C32 C -0.0038(4) -0.4854(16) 0.4548(4) 0.110(4) Uani 1 1 d . . . H32 H -0.0066 -0.4816 0.4234 0.132 Uiso 1 1 calc R B . C41 C 0.2719(5) 0.185(2) 0.5262(5) 0.130(7) Uiso 0.50 1 d PGD C -1 C42 C 0.2320(6) 0.0951(19) 0.4990(6) 0.117(7) Uiso 0.50 1 d PGD C -1 H42 H 0.2267 -0.0304 0.5064 0.140 Uiso 0.50 1 calc PR C -1 C43 C 0.2000(4) 0.189(3) 0.4611(5) 0.118(7) Uiso 0.50 1 d PG C -1 H43 H 0.1728 0.1271 0.4425 0.142 Uiso 0.50 1 calc PR C -1 C44 C 0.2078(5) 0.372(3) 0.4503(4) 0.138(8) Uiso 0.50 1 d PG C -1 H44 H 0.1859 0.4364 0.4244 0.166 Uiso 0.50 1 calc PR C -1 C45 C 0.2476(6) 0.4625(18) 0.4775(6) 0.117(7) Uiso 0.50 1 d PG C -1 H45 H 0.2530 0.5881 0.4701 0.140 Uiso 0.50 1 calc PR C -1 C46 C 0.2797(4) 0.369(2) 0.5154(5) 0.106(6) Uiso 0.50 1 d PGD C -1 H46 H 0.3069 0.4306 0.5340 0.127 Uiso 0.50 1 calc PR C -1 C47 C 0.3095(9) 0.095(5) 0.5677(9) 0.217(15) Uiso 0.50 1 d PD C -1 H47A H 0.3186 0.1798 0.5947 0.325 Uiso 0.50 1 calc PR C -1 H47B H 0.3349 0.0713 0.5597 0.325 Uiso 0.50 1 calc PR C -1 H47C H 0.2993 -0.0259 0.5753 0.325 Uiso 0.50 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.0506(11) 0.0363(10) 0.0463(10) 0.0028(8) 0.0095(8) 0.0002(8) O1 0.066(3) 0.034(2) 0.043(2) 0.0035(17) 0.0094(19) 0.0040(19) N1 0.049(3) 0.030(2) 0.045(2) -0.003(2) 0.015(2) 0.003(2) C1 0.066(4) 0.059(4) 0.058(4) 0.010(3) 0.014(3) -0.007(3) O2 0.051(3) 0.036(2) 0.075(3) -0.002(2) -0.006(2) 0.0009(19) N2 0.053(3) 0.030(2) 0.051(3) -0.001(2) 0.020(2) 0.004(2) C2 0.053(3) 0.036(3) 0.050(3) -0.004(3) 0.014(3) -0.007(3) C3 0.074(4) 0.038(3) 0.054(4) 0.002(3) 0.023(3) 0.005(3) C4 0.087(5) 0.041(3) 0.052(4) -0.005(3) 0.024(3) 0.002(3) C5 0.081(5) 0.046(4) 0.049(4) -0.006(3) 0.015(3) -0.002(3) C6 0.064(4) 0.053(4) 0.045(3) 0.001(3) 0.011(3) 0.004(3) C7 0.053(3) 0.036(3) 0.047(3) -0.002(3) 0.015(3) 0.006(3) C8 0.14(2) 0.086(17) 0.047(10) 0.029(10) 0.047(12) 0.030(15) C9 0.065(10) 0.091(17) 0.019(5) 0.026(7) -0.001(6) -0.001(9) C10 0.071(10) 0.072(10) 0.060(8) 0.026(8) -0.014(7) -0.014(8) C11 0.104(15) 0.134(17) 0.071(10) -0.021(11) 0.021(11) 0.015(13) C8A 0.113(19) 0.034(14) 0.025(12) -0.009(11) 0.023(12) -0.028(12) C9A 0.16(4) 0.026(14) 0.22(4) 0.012(18) 0.06(3) 0.043(17) C10A 0.13(3) 0.15(3) 0.09(2) 0.00(2) -0.04(2) -0.09(3) C11A 0.17(3) 0.11(2) 0.042(11) 0.028(13) 0.033(16) 0.10(2) C12 0.059(4) 0.046(4) 0.049(3) 0.005(3) 0.011(3) 0.009(3) C13 0.065(4) 0.046(3) 0.051(3) -0.003(3) 0.018(3) 0.016(3) C14 0.065(4) 0.045(3) 0.052(3) -0.012(3) 0.020(3) 0.000(3) C15 0.063(4) 0.039(3) 0.045(3) 0.000(3) 0.015(3) 0.004(3) C16 0.067(4) 0.035(3) 0.061(4) -0.005(3) 0.026(3) -0.004(3) C17 0.049(3) 0.044(3) 0.053(3) -0.002(3) 0.017(3) -0.005(3) C18 0.053(3) 0.045(3) 0.039(3) -0.005(3) 0.006(3) -0.003(3) C19 0.061(4) 0.040(3) 0.044(3) 0.003(3) 0.010(3) 0.004(3) C20 0.059(4) 0.052(4) 0.040(3) -0.007(3) 0.013(3) -0.009(3) C21 0.055(4) 0.054(4) 0.048(3) -0.007(3) 0.018(3) -0.005(3) C22 0.052(4) 0.059(4) 0.067(4) -0.006(4) 0.011(3) 0.010(3) C23 0.059(4) 0.043(4) 0.077(4) -0.011(3) 0.009(3) 0.003(3) C24 0.057(4) 0.037(3) 0.059(4) 0.002(3) 0.005(3) -0.002(3) C25 0.048(4) 0.075(5) 0.051(4) -0.010(3) 0.015(3) -0.008(3) C26 0.080(5) 0.110(7) 0.094(6) 0.009(5) 0.015(4) -0.041(5) C27 0.057(4) 0.087(5) 0.055(4) -0.002(4) 0.008(3) 0.003(4) C28 0.059(5) 0.162(9) 0.106(6) -0.063(6) 0.035(5) -0.021(5) C29 0.073(10) 0.088(12) 0.076(10) 0.018(9) 0.023(8) -0.008(9) C30 0.135(8) 0.087(7) 0.107(7) 0.035(6) 0.073(7) 0.057(6) C31 0.150(9) 0.078(6) 0.138(9) 0.043(7) 0.094(8) 0.055(7) C32 0.166(10) 0.087(7) 0.114(8) 0.046(7) 0.094(8) 0.059(7) _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 Al O1 1.786(4) . ? Al O2 1.796(4) . ? Al C1 1.966(7) . ? Al N2 2.101(5) . ? Al N1 2.109(5) . ? O1 C2 1.354(6) . ? N1 C13 1.482(7) . ? N1 C15 1.490(7) . ? N1 C12 1.492(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C24 1.358(7) . ? N2 C14 1.489(7) . ? N2 C18 1.496(7) . ? N2 C17 1.499(7) . ? C2 C3 1.384(8) . ? C2 C7 1.412(8) . ? C3 C4 1.389(8) . ? C3 H3 0.9500 . ? C4 C5 1.386(9) . ? C4 H4 0.9500 . ? C5 C6 1.377(9) . ? C5 C8 1.49(3) . ? C5 C8A 1.62(3) . ? C6 C7 1.391(8) . ? C6 H6 0.9500 . ? C7 C12 1.495(8) . ? C8 C11 1.531(17) . ? C8 C10 1.545(18) . ? C8 C9 1.552(16) . ? 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 . ? C8A C10A 1.549(18) . ? C8A C9A 1.553(19) . ? C8A C11A 1.553(19) . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C11A H11D 0.9800 . ? C11A H11E 0.9800 . ? C11A H11F 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.559(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.523(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.525(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.521(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C24 1.395(8) . ? C19 C20 1.403(8) . ? C20 C21 1.359(8) . ? C20 H20 0.9500 . ? C21 C22 1.391(9) . ? C21 C25 1.535(8) . ? C22 C23 1.389(9) . ? C22 H22 0.9500 . ? C23 C24 1.381(9) . ? C23 H23 0.9500 . ? C25 C27 1.503(9) . ? C25 C28 1.507(10) . ? C25 C26 1.540(11) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 C30 1.466(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.371(12) . ? C30 C32 1.396(13) 5_546 ? C31 C32 1.341(14) . ? C31 H31 0.9500 . ? C32 C30 1.396(13) 5_546 ? C32 H32 0.9500 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C47 1.522(10) . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 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 Al O2 90.2(2) . . ? O1 Al C1 111.8(3) . . ? O2 Al C1 107.4(3) . . ? O1 Al N2 143.4(2) . . ? O2 Al N2 88.88(18) . . ? C1 Al N2 103.3(2) . . ? O1 Al N1 88.23(17) . . ? O2 Al N1 148.9(2) . . ? C1 Al N1 102.0(2) . . ? N2 Al N1 74.48(17) . . ? C2 O1 Al 135.6(4) . . ? C13 N1 C15 110.6(5) . . ? C13 N1 C12 109.7(4) . . ? C15 N1 C12 108.6(4) . . ? C13 N1 Al 106.8(3) . . ? C15 N1 Al 111.6(3) . . ? C12 N1 Al 109.5(3) . . ? Al C1 H1A 109.5 . . ? Al C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C24 O2 Al 133.7(4) . . ? C14 N2 C18 109.0(4) . . ? C14 N2 C17 110.8(4) . . ? C18 N2 C17 109.7(4) . . ? C14 N2 Al 106.9(3) . . ? C18 N2 Al 110.2(3) . . ? C17 N2 Al 110.2(3) . . ? O1 C2 C3 120.9(5) . . ? O1 C2 C7 121.1(5) . . ? C3 C2 C7 118.0(5) . . ? C2 C3 C4 121.2(6) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 121.9(6) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C6 C5 C4 116.4(6) . . ? C6 C5 C8 118.7(9) . . ? C4 C5 C8 124.3(9) . . ? C6 C5 C8A 123.3(10) . . ? C4 C5 C8A 119.8(10) . . ? C8 C5 C8A 14.7(14) . . ? C5 C6 C7 123.6(6) . . ? C5 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C6 C7 C2 118.9(5) . . ? C6 C7 C12 121.4(5) . . ? C2 C7 C12 119.7(5) . . ? C5 C8 C11 115.0(16) . . ? C5 C8 C10 118.2(16) . . ? C11 C8 C10 106.0(17) . . ? C5 C8 C9 108.5(14) . . ? C11 C8 C9 107(2) . . ? C10 C8 C9 101.0(16) . . ? C10A C8A C9A 128(3) . . ? C10A C8A C11A 104(2) . . ? C9A C8A C11A 104(3) . . ? C10A C8A C5 97.0(19) . . ? C9A C8A C5 114(2) . . ? C11A C8A C5 109(2) . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C8A C10A H10D 109.5 . . ? C8A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C8A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C8A C11A H11D 109.5 . . ? C8A C11A H11E 109.5 . . ? H11D C11A H11E 109.5 . . ? C8A C11A H11F 109.5 . . ? H11D C11A H11F 109.5 . . ? H11E C11A H11F 109.5 . . ? N1 C12 C7 112.3(5) . . ? N1 C12 H12A 109.1 . . ? C7 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? C7 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N1 C13 C14 109.3(4) . . ? N1 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? N1 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N2 C14 C13 109.6(4) . . ? N2 C14 H14A 109.7 . . ? C13 C14 H14A 109.7 . . ? N2 C14 H14B 109.7 . . ? C13 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? N1 C15 C16 112.9(4) . . ? N1 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 C17 112.1(5) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N2 C17 C16 112.8(5) . . ? N2 C17 H17A 109.0 . . ? C16 C17 H17A 109.0 . . ? N2 C17 H17B 109.0 . . ? C16 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? N2 C18 C19 110.1(4) . . ? N2 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N2 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.2 . . ? C24 C19 C20 118.8(6) . . ? C24 C19 C18 118.6(5) . . ? C20 C19 C18 122.4(5) . . ? C21 C20 C19 123.5(6) . . ? C21 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? C20 C21 C22 117.1(6) . . ? C20 C21 C25 121.2(6) . . ? C22 C21 C25 121.7(6) . . ? C23 C22 C21 120.9(6) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 121.7(6) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? O2 C24 C23 120.7(6) . . ? O2 C24 C19 121.2(6) . . ? C23 C24 C19 118.1(6) . . ? C27 C25 C28 108.7(6) . . ? C27 C25 C21 109.7(5) . . ? C28 C25 C21 112.8(5) . . ? C27 C25 C26 108.7(6) . . ? C28 C25 C26 107.6(7) . . ? C21 C25 C26 109.2(6) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C32 122.9(10) . 5_546 ? C31 C30 C29 118.7(12) . . ? C32 C30 C29 117.8(11) 5_546 . ? C32 C31 C30 117.7(10) . . ? C32 C31 H31 121.2 . . ? C30 C31 H31 121.2 . . ? C31 C32 C30 119.4(9) . 5_546 ? C31 C32 H32 120.3 . . ? C30 C32 H32 120.3 5_546 . ? C42 C41 C46 120.0 . . ? C42 C41 C47 124.3(18) . . ? C46 C41 C47 115.6(18) . . ? C43 C42 C41 120.0 . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.643 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.073 #====END