# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _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_requested_coeditor_name ; Matthew D Jones, Emma L. Whitelaw, Mary F. Mahon Gaynor Loraine ; _publ_contact_letter ; ; #================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Salalen Aluminium Complexes and Their Exploitation for the Ring Opening Polymerization of rac-lactide ; loop_ _publ_author_name _publ_author_address 'Emma L. Whitelaw' ; 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 ; 'Gaynor Loraine' ; University of Bath Department of Chemistry Bath, BA2 7AY United Kingdom ; _publ_contact_author_name 'Matthew D Jones' #========================================================= data_Al(Me)(2) _database_code_depnum_ccdc_archive 'CCDC 829021' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H55 Al N2 O2' _chemical_formula_weight 610.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 10.0400(5) _cell_length_b 22.8750(14) _cell_length_c 31.7450(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7290.7(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 95608 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _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 2656 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58588 _diffrn_reflns_av_R_equivalents 0.1130 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6295 _reflns_number_gt 4020 _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^)+(0.0548P)^2^+3.9470P] 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 6295 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.97851(7) 0.13637(3) 0.34104(2) 0.0270(2) Uani 1 1 d . . . O1 O 1.13226(15) 0.13457(7) 0.36830(5) 0.0273(4) Uani 1 1 d . . . N1 N 0.9043(2) 0.21363(9) 0.32860(6) 0.0286(5) Uani 1 1 d . . . C1 C 0.8554(3) 0.07113(12) 0.33261(9) 0.0412(7) Uani 1 1 d . . . H1A H 0.9061 0.0352 0.3275 0.062 Uiso 1 1 calc R . . H1B H 0.7981 0.0793 0.3083 0.062 Uiso 1 1 calc R . . H1C H 0.8002 0.0662 0.3578 0.062 Uiso 1 1 calc R . . O2 O 1.05651(16) 0.13458(7) 0.28932(5) 0.0302(4) Uani 1 1 d . . . N2 N 0.88729(19) 0.16406(9) 0.40496(6) 0.0277(5) Uani 1 1 d . . . C2 C 1.1772(2) 0.13911(10) 0.40835(8) 0.0259(6) Uani 1 1 d . . . C3 C 1.1096(2) 0.17491(10) 0.43698(8) 0.0266(6) Uani 1 1 d . . . C4 C 1.1541(3) 0.18000(11) 0.47839(8) 0.0304(6) Uani 1 1 d . . . H4 H 1.1050 0.2036 0.4975 0.036 Uiso 1 1 calc R . . C5 C 1.2680(3) 0.15169(11) 0.49267(8) 0.0329(7) Uani 1 1 d . . . C6 C 1.3351(3) 0.11717(11) 0.46291(8) 0.0331(7) Uani 1 1 d . . . H6 H 1.4144 0.0980 0.4716 0.040 Uiso 1 1 calc R . . C7 C 1.2932(2) 0.10898(11) 0.42128(8) 0.0281(6) Uani 1 1 d . . . C8 C 1.3728(3) 0.06947(11) 0.39106(8) 0.0311(6) Uani 1 1 d . . . C9 C 1.2835(3) 0.01998(11) 0.37411(9) 0.0419(7) Uani 1 1 d . . . H9A H 1.2069 0.0369 0.3594 0.063 Uiso 1 1 calc R . . H9B H 1.2521 -0.0041 0.3976 0.063 Uiso 1 1 calc R . . H9C H 1.3347 -0.0043 0.3545 0.063 Uiso 1 1 calc R . . C10 C 1.4249(3) 0.10596(12) 0.35414(8) 0.0347(7) Uani 1 1 d . . . H10A H 1.4809 0.1377 0.3649 0.052 Uiso 1 1 calc R . . H10B H 1.3495 0.1225 0.3385 0.052 Uiso 1 1 calc R . . H10C H 1.4776 0.0811 0.3354 0.052 Uiso 1 1 calc R . . C11 C 1.4934(3) 0.04087(13) 0.41247(9) 0.0440(8) Uani 1 1 d . . . H11A H 1.5393 0.0155 0.3923 0.066 Uiso 1 1 calc R . . H11B H 1.4632 0.0176 0.4365 0.066 Uiso 1 1 calc R . . H11C H 1.5548 0.0713 0.4223 0.066 Uiso 1 1 calc R . . C12 C 1.3229(3) 0.15948(12) 0.53756(8) 0.0386(7) Uani 1 1 d . . . C13 C 1.3733(3) 0.10126(13) 0.55524(9) 0.0485(8) Uani 1 1 d . . . H13A H 1.4094 0.1074 0.5836 0.073 Uiso 1 1 calc R . . H13B H 1.4434 0.0858 0.5369 0.073 Uiso 1 1 calc R . . H13C H 1.2995 0.0733 0.5566 0.073 Uiso 1 1 calc R . . C14 C 1.4398(3) 0.20309(14) 0.53632(10) 0.0544(9) Uani 1 1 d . . . H14A H 1.4072 0.2415 0.5273 0.082 Uiso 1 1 calc R . . H14B H 1.5073 0.1892 0.5164 0.082 Uiso 1 1 calc R . . H14C H 1.4793 0.2063 0.5645 0.082 Uiso 1 1 calc R . . C15 C 1.2175(3) 0.18350(15) 0.56737(9) 0.0575(9) Uani 1 1 d . . . H15A H 1.1402 0.1573 0.5675 0.086 Uiso 1 1 calc R . . H15B H 1.1899 0.2224 0.5579 0.086 Uiso 1 1 calc R . . H15C H 1.2544 0.1862 0.5959 0.086 Uiso 1 1 calc R . . C16 C 0.9870(2) 0.20667(11) 0.42242(8) 0.0282(6) Uani 1 1 d . . . H16A H 1.0115 0.2354 0.4004 0.034 Uiso 1 1 calc R . . H16B H 0.9471 0.2282 0.4464 0.034 Uiso 1 1 calc R . . C17 C 0.8558(3) 0.12042(12) 0.43732(8) 0.0336(7) Uani 1 1 d . . . C18 C 0.9080(3) 0.06446(12) 0.43429(9) 0.0393(7) Uani 1 1 d . . . H18 H 0.9630 0.0544 0.4110 0.047 Uiso 1 1 calc R . . C19 C 0.8803(3) 0.02311(14) 0.46494(10) 0.0515(8) Uani 1 1 d . . . H19 H 0.9160 -0.0152 0.4624 0.062 Uiso 1 1 calc R . . C20 C 0.8016(3) 0.03704(16) 0.49899(11) 0.0601(10) Uani 1 1 d . . . H20 H 0.7818 0.0084 0.5197 0.072 Uiso 1 1 calc R . . C21 C 0.7516(3) 0.09313(16) 0.50282(10) 0.0572(9) Uani 1 1 d . . . H21 H 0.6988 0.1032 0.5266 0.069 Uiso 1 1 calc R . . C22 C 0.7782(3) 0.13506(14) 0.47203(9) 0.0454(8) Uani 1 1 d . . . H22 H 0.7433 0.1735 0.4748 0.055 Uiso 1 1 calc R . . C23 C 0.7647(2) 0.19404(12) 0.39003(9) 0.0328(7) Uani 1 1 d . . . H23A H 0.7219 0.2146 0.4139 0.039 Uiso 1 1 calc R . . H23B H 0.7011 0.1647 0.3790 0.039 Uiso 1 1 calc R . . C24 C 0.7980(3) 0.23755(11) 0.35576(9) 0.0342(7) Uani 1 1 d . . . H24A H 0.7177 0.2456 0.3386 0.041 Uiso 1 1 calc R . . H24B H 0.8281 0.2748 0.3686 0.041 Uiso 1 1 calc R . . C25 C 0.9468(2) 0.24756(11) 0.29849(8) 0.0293(6) Uani 1 1 d . . . H25 H 0.9086 0.2855 0.2970 0.035 Uiso 1 1 calc R . . C26 C 1.0450(2) 0.23346(10) 0.26747(8) 0.0269(6) Uani 1 1 d . . . C27 C 1.0917(2) 0.17543(11) 0.26244(8) 0.0275(6) Uani 1 1 d . . . C28 C 1.1723(2) 0.16229(11) 0.22667(8) 0.0278(6) Uani 1 1 d . . . C29 C 1.2118(2) 0.20905(11) 0.20169(8) 0.0308(6) Uani 1 1 d . . . H29 H 1.2686 0.2006 0.1785 0.037 Uiso 1 1 calc R . . C30 C 1.1747(3) 0.26799(11) 0.20773(8) 0.0300(6) Uani 1 1 d . . . C31 C 1.0874(3) 0.27830(11) 0.24018(8) 0.0299(6) Uani 1 1 d . . . H31 H 1.0545 0.3168 0.2443 0.036 Uiso 1 1 calc R . . C32 C 1.2093(3) 0.09857(11) 0.21611(8) 0.0321(6) Uani 1 1 d . . . C33 C 1.0830(3) 0.06172(12) 0.21099(10) 0.0464(8) Uani 1 1 d . . . H33A H 1.0274 0.0785 0.1887 0.070 Uiso 1 1 calc R . . H33B H 1.0333 0.0615 0.2376 0.070 Uiso 1 1 calc R . . H33C H 1.1076 0.0216 0.2034 0.070 Uiso 1 1 calc R . . C34 C 1.2968(3) 0.07212(12) 0.25104(9) 0.0388(7) Uani 1 1 d . . . H34A H 1.3185 0.0315 0.2439 0.058 Uiso 1 1 calc R . . H34B H 1.2484 0.0731 0.2778 0.058 Uiso 1 1 calc R . . H34C H 1.3791 0.0948 0.2536 0.058 Uiso 1 1 calc R . . C35 C 1.2870(3) 0.09460(13) 0.17480(9) 0.0511(8) Uani 1 1 d . . . H35A H 1.3057 0.0535 0.1684 0.077 Uiso 1 1 calc R . . H35B H 1.3710 0.1161 0.1775 0.077 Uiso 1 1 calc R . . H35C H 1.2339 0.1117 0.1520 0.077 Uiso 1 1 calc R . . C36 C 1.2207(3) 0.31622(11) 0.17753(8) 0.0348(7) Uani 1 1 d . . . C37 C 1.2183(3) 0.37602(12) 0.19893(11) 0.0568(9) Uani 1 1 d . . . H37A H 1.2723 0.3747 0.2246 0.085 Uiso 1 1 calc R . . H37B H 1.1264 0.3863 0.2062 0.085 Uiso 1 1 calc R . . H37C H 1.2548 0.4055 0.1797 0.085 Uiso 1 1 calc R . . C38 C 1.1275(3) 0.31711(14) 0.13888(10) 0.0496(8) Uani 1 1 d . . . H38A H 1.0361 0.3251 0.1481 0.074 Uiso 1 1 calc R . . H38B H 1.1307 0.2791 0.1247 0.074 Uiso 1 1 calc R . . H38C H 1.1565 0.3477 0.1193 0.074 Uiso 1 1 calc R . . C39 C 1.3629(3) 0.30514(13) 0.16178(9) 0.0426(7) Uani 1 1 d . . . H39A H 1.3921 0.3382 0.1444 0.064 Uiso 1 1 calc R . . H39B H 1.3647 0.2693 0.1449 0.064 Uiso 1 1 calc R . . H39C H 1.4229 0.3009 0.1860 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0244(4) 0.0269(4) 0.0298(4) 0.0006(3) -0.0021(3) -0.0010(3) O1 0.0227(10) 0.0320(10) 0.0272(10) -0.0024(8) -0.0007(7) 0.0014(8) N1 0.0233(12) 0.0332(13) 0.0291(12) -0.0011(10) -0.0012(10) 0.0037(10) C1 0.0434(18) 0.0391(17) 0.0410(17) -0.0049(14) -0.0014(14) -0.0069(14) O2 0.0344(11) 0.0280(10) 0.0283(10) 0.0029(8) 0.0009(8) 0.0025(8) N2 0.0186(11) 0.0317(12) 0.0328(12) 0.0020(10) -0.0001(9) -0.0015(9) C2 0.0230(14) 0.0287(14) 0.0260(14) 0.0013(12) 0.0005(11) -0.0022(12) C3 0.0214(14) 0.0260(14) 0.0325(15) -0.0002(12) 0.0006(11) -0.0002(11) C4 0.0305(16) 0.0319(15) 0.0288(15) -0.0048(12) 0.0017(12) 0.0032(12) C5 0.0346(16) 0.0355(16) 0.0286(15) -0.0003(12) -0.0018(12) 0.0044(13) C6 0.0318(16) 0.0350(16) 0.0324(15) 0.0016(13) -0.0043(12) 0.0081(12) C7 0.0242(15) 0.0289(15) 0.0313(15) 0.0010(12) 0.0002(11) 0.0015(12) C8 0.0307(15) 0.0314(15) 0.0313(15) -0.0001(12) -0.0003(12) 0.0051(12) C9 0.0457(19) 0.0330(16) 0.0470(18) -0.0034(14) 0.0036(14) 0.0016(14) C10 0.0287(15) 0.0404(17) 0.0351(15) -0.0050(13) 0.0016(12) 0.0028(13) C11 0.0429(18) 0.0483(18) 0.0409(17) -0.0042(14) -0.0022(14) 0.0200(15) C12 0.0407(17) 0.0460(17) 0.0291(15) 0.0015(13) -0.0013(13) 0.0082(14) C13 0.053(2) 0.058(2) 0.0342(17) 0.0063(15) -0.0059(14) 0.0088(16) C14 0.058(2) 0.064(2) 0.0418(18) 0.0003(16) -0.0078(16) -0.0122(17) C15 0.065(2) 0.079(2) 0.0295(17) -0.0016(16) -0.0004(16) 0.0178(19) C16 0.0248(15) 0.0307(15) 0.0292(14) -0.0041(12) 0.0014(11) 0.0012(12) C17 0.0235(15) 0.0426(17) 0.0348(16) 0.0049(13) -0.0011(12) -0.0059(13) C18 0.0316(17) 0.0406(18) 0.0457(17) 0.0094(15) 0.0008(13) -0.0028(14) C19 0.048(2) 0.0461(19) 0.060(2) 0.0173(17) -0.0003(17) -0.0035(16) C20 0.048(2) 0.073(3) 0.059(2) 0.0332(19) 0.0009(18) -0.0059(19) C21 0.0417(19) 0.084(3) 0.0463(19) 0.0231(19) 0.0128(15) 0.0016(19) C22 0.0315(17) 0.059(2) 0.0454(18) 0.0090(16) 0.0065(14) 0.0036(15) C23 0.0227(15) 0.0394(16) 0.0363(16) -0.0012(13) -0.0003(12) 0.0034(12) C24 0.0259(16) 0.0391(16) 0.0376(16) 0.0016(13) 0.0003(12) 0.0078(12) C25 0.0308(16) 0.0277(14) 0.0294(14) 0.0004(12) -0.0040(12) 0.0021(12) C26 0.0271(15) 0.0267(15) 0.0270(14) -0.0019(12) -0.0041(11) -0.0003(12) C27 0.0252(15) 0.0304(15) 0.0269(14) -0.0015(12) -0.0063(12) -0.0018(12) C28 0.0279(15) 0.0290(14) 0.0265(14) -0.0018(12) -0.0059(12) 0.0025(12) C29 0.0305(16) 0.0354(16) 0.0265(14) -0.0014(13) 0.0007(12) 0.0021(13) C30 0.0314(16) 0.0305(15) 0.0282(15) 0.0005(12) -0.0044(12) -0.0014(12) C31 0.0323(16) 0.0246(14) 0.0327(15) -0.0002(12) -0.0027(12) 0.0002(12) C32 0.0388(17) 0.0299(15) 0.0277(14) -0.0008(12) -0.0021(12) 0.0022(13) C33 0.055(2) 0.0336(17) 0.0502(19) -0.0098(14) -0.0120(16) 0.0031(14) C34 0.0429(18) 0.0365(16) 0.0371(16) 0.0011(13) -0.0039(13) 0.0088(13) C35 0.079(2) 0.0369(17) 0.0378(17) -0.0020(14) 0.0101(16) 0.0145(16) C36 0.0374(17) 0.0334(16) 0.0338(15) 0.0046(13) 0.0022(13) -0.0013(13) C37 0.076(2) 0.0363(18) 0.058(2) 0.0052(16) 0.0201(18) -0.0122(16) C38 0.0393(18) 0.060(2) 0.0500(19) 0.0223(16) -0.0042(15) -0.0003(15) C39 0.0371(18) 0.0468(18) 0.0439(17) 0.0086(15) 0.0002(14) -0.0069(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 O1 1.7701(17) . ? Al1 O2 1.8193(18) . ? Al1 C1 1.957(3) . ? Al1 N1 1.958(2) . ? Al1 N2 2.315(2) . ? O1 C2 1.353(3) . ? N1 C25 1.303(3) . ? N1 C24 1.477(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C27 1.314(3) . ? N2 C17 1.467(3) . ? N2 C23 1.486(3) . ? N2 C16 1.503(3) . ? C2 C3 1.399(3) . ? C2 C7 1.414(3) . ? C3 C4 1.393(3) . ? C3 C16 1.501(3) . ? C4 C5 1.390(4) . ? C4 H4 0.9500 . ? C5 C6 1.404(4) . ? C5 C12 1.539(4) . ? C6 C7 1.400(4) . ? C6 H6 0.9500 . ? C7 C8 1.541(3) . ? C8 C10 1.531(4) . ? C8 C11 1.535(4) . ? C8 C9 1.541(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.523(4) . ? C12 C13 1.531(4) . ? C12 C14 1.541(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.386(4) . ? C17 C22 1.391(4) . ? C18 C19 1.385(4) . ? C18 H18 0.9500 . ? C19 C20 1.376(4) . ? C19 H19 0.9500 . ? C20 C21 1.383(5) . ? C20 H20 0.9500 . ? C21 C22 1.395(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.512(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.430(3) . ? C25 H25 0.9500 . ? C26 C31 1.408(3) . ? C26 C27 1.417(3) . ? C27 C28 1.426(3) . ? C28 C29 1.389(3) . ? C28 C32 1.541(3) . ? C29 C30 1.412(3) . ? C29 H29 0.9500 . ? C30 C31 1.373(4) . ? C30 C36 1.533(4) . ? C31 H31 0.9500 . ? C32 C35 1.529(4) . ? C32 C33 1.531(4) . ? C32 C34 1.539(3) . ? 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 . ? C36 C37 1.528(4) . ? C36 C39 1.534(4) . ? C36 C38 1.543(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 93.74(8) . . ? O1 Al1 C1 126.88(11) . . ? O2 Al1 C1 97.56(10) . . ? O1 Al1 N1 116.83(9) . . ? O2 Al1 N1 90.12(8) . . ? C1 Al1 N1 114.87(11) . . ? O1 Al1 N2 85.58(8) . . ? O2 Al1 N2 165.36(8) . . ? C1 Al1 N2 94.50(10) . . ? N1 Al1 N2 77.25(8) . . ? C2 O1 Al1 138.46(15) . . ? C25 N1 C24 116.3(2) . . ? C25 N1 Al1 124.15(18) . . ? C24 N1 Al1 119.44(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 . . ? C27 O2 Al1 133.31(16) . . ? C17 N2 C23 111.05(19) . . ? C17 N2 C16 109.05(19) . . ? C23 N2 C16 111.71(19) . . ? C17 N2 Al1 120.86(16) . . ? C23 N2 Al1 100.04(15) . . ? C16 N2 Al1 103.71(14) . . ? O1 C2 C3 119.6(2) . . ? O1 C2 C7 120.7(2) . . ? C3 C2 C7 119.8(2) . . ? C4 C3 C2 120.4(2) . . ? C4 C3 C16 120.9(2) . . ? C2 C3 C16 118.7(2) . . ? C5 C4 C3 122.2(2) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 115.9(2) . . ? C4 C5 C12 122.9(2) . . ? C6 C5 C12 121.1(2) . . ? C7 C6 C5 124.5(2) . . ? C7 C6 H6 117.7 . . ? C5 C6 H6 117.7 . . ? C6 C7 C2 117.1(2) . . ? C6 C7 C8 120.7(2) . . ? C2 C7 C8 122.2(2) . . ? C10 C8 C11 107.6(2) . . ? C10 C8 C9 109.4(2) . . ? C11 C8 C9 107.5(2) . . ? C10 C8 C7 109.5(2) . . ? C11 C8 C7 112.5(2) . . ? C9 C8 C7 110.3(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 108.4(2) . . ? C15 C12 C5 111.6(2) . . ? C13 C12 C5 110.9(2) . . ? C15 C12 C14 108.2(3) . . ? C13 C12 C14 108.7(2) . . ? C5 C12 C14 108.9(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C3 C16 N2 110.2(2) . . ? C3 C16 H16A 109.6 . . ? N2 C16 H16A 109.6 . . ? C3 C16 H16B 109.6 . . ? N2 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C22 119.3(3) . . ? C18 C17 N2 119.9(2) . . ? C22 C17 N2 120.8(2) . . ? C19 C18 C17 120.4(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.5(3) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 119.8(3) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? N2 C23 C24 110.5(2) . . ? N2 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N2 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N1 C24 C23 109.6(2) . . ? N1 C24 H24A 109.7 . . ? C23 C24 H24A 109.7 . . ? N1 C24 H24B 109.7 . . ? C23 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? N1 C25 C26 126.6(2) . . ? N1 C25 H25 116.7 . . ? C26 C25 H25 116.7 . . ? C31 C26 C27 120.9(2) . . ? C31 C26 C25 117.9(2) . . ? C27 C26 C25 121.1(2) . . ? O2 C27 C26 120.2(2) . . ? O2 C27 C28 121.3(2) . . ? C26 C27 C28 118.4(2) . . ? C29 C28 C27 117.0(2) . . ? C29 C28 C32 122.4(2) . . ? C27 C28 C32 120.6(2) . . ? C28 C29 C30 125.6(2) . . ? C28 C29 H29 117.2 . . ? C30 C29 H29 117.2 . . ? C31 C30 C29 115.7(2) . . ? C31 C30 C36 122.5(2) . . ? C29 C30 C36 121.5(2) . . ? C30 C31 C26 122.0(2) . . ? C30 C31 H31 119.0 . . ? C26 C31 H31 119.0 . . ? C35 C32 C33 107.4(2) . . ? C35 C32 C34 107.7(2) . . ? C33 C32 C34 109.4(2) . . ? C35 C32 C28 111.5(2) . . ? C33 C32 C28 110.2(2) . . ? C34 C32 C28 110.6(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? 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 109.5 . . ? 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 . . ? C37 C36 C30 111.2(2) . . ? C37 C36 C39 107.9(2) . . ? C30 C36 C39 111.4(2) . . ? C37 C36 C38 109.4(2) . . ? C30 C36 C38 108.9(2) . . ? C39 C36 C38 107.9(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.576 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.077 #=== END data_Al(Me)(3) _database_code_depnum_ccdc_archive 'CCDC 829022' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 Al N2 O2' _chemical_formula_weight 450.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7286(7) _cell_length_b 12.5296(10) _cell_length_c 13.0282(10) _cell_angle_alpha 110.181(4) _cell_angle_beta 109.510(4) _cell_angle_gamma 103.090(5) _cell_volume 1295.98(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9203 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10691 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 24.84 _reflns_number_total 4417 _reflns_number_gt 2725 _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^)+(0.0883P)^2^+0.3405P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4417 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1144 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1797 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.30425(11) 0.01414(9) 0.63139(8) 0.0485(3) Uani 1 1 d . . . O1 O 0.2082(3) -0.00368(19) 0.72074(19) 0.0527(6) Uani 1 1 d . . . N1 N 0.1813(3) -0.0259(3) 0.4582(2) 0.0551(7) Uani 1 1 d . . . C1 C 0.5282(4) 0.0434(3) 0.6790(3) 0.0640(10) Uani 1 1 d . . . H1A H 0.5885 0.1312 0.7096 0.096 Uiso 1 1 calc R . . H1B H 0.5399 -0.0054 0.6077 0.096 Uiso 1 1 calc R . . H1C H 0.5681 0.0192 0.7434 0.096 Uiso 1 1 calc R . . O2 O 0.3160(3) 0.1725(2) 0.6778(2) 0.0610(6) Uani 1 1 d . . . N2 N 0.2270(3) -0.1936(2) 0.5391(2) 0.0514(7) Uani 1 1 d . . . C2 C 0.1762(3) -0.0859(3) 0.7623(3) 0.0463(7) Uani 1 1 d . . . C3 C 0.1150(3) -0.2114(3) 0.6815(3) 0.0489(8) Uani 1 1 d . . . C4 C 0.0816(4) -0.2997(3) 0.7205(3) 0.0535(8) Uani 1 1 d . . . H4 H 0.0417 -0.3845 0.6643 0.064 Uiso 1 1 calc R . . C5 C 0.1054(4) -0.2663(3) 0.8403(3) 0.0501(8) Uani 1 1 d . . . C6 C 0.1629(4) -0.1406(3) 0.9182(3) 0.0477(8) Uani 1 1 d . . . H6 H 0.1773 -0.1163 0.9999 0.057 Uiso 1 1 calc R . . C7 C 0.2007(3) -0.0480(3) 0.8843(3) 0.0450(7) Uani 1 1 d . . . C8 C 0.0650(4) -0.3667(3) 0.8797(3) 0.0540(8) Uani 1 1 d . . . C9 C -0.1154(4) -0.4383(3) 0.8116(4) 0.0674(10) Uani 1 1 d . . . H9A H -0.1673 -0.3831 0.8381 0.101 Uiso 1 1 calc R . . H9B H -0.1428 -0.5073 0.8302 0.101 Uiso 1 1 calc R . . H9C H -0.1511 -0.4700 0.7232 0.101 Uiso 1 1 calc R . . C10 C 0.1485(5) -0.4542(3) 0.8476(4) 0.0710(10) Uani 1 1 d . . . H10A H 0.1210 -0.4871 0.7602 0.106 Uiso 1 1 calc R . . H10B H 0.1148 -0.5224 0.8660 0.106 Uiso 1 1 calc R . . H10C H 0.2632 -0.4091 0.8961 0.106 Uiso 1 1 calc R . . C11 C 0.1181(5) -0.3137(4) 1.0172(3) 0.0746(11) Uani 1 1 d . . . H11A H 0.2328 -0.2677 1.0613 0.112 Uiso 1 1 calc R . . H11B H 0.0902 -0.3811 1.0379 0.112 Uiso 1 1 calc R . . H11C H 0.0652 -0.2584 1.0408 0.112 Uiso 1 1 calc R . . C12 C 0.2690(4) 0.0896(3) 0.9759(3) 0.0493(8) Uani 1 1 d . . . C13 C 0.1698(4) 0.1549(3) 0.9255(3) 0.0634(9) Uani 1 1 d . . . H13A H 0.2135 0.2419 0.9855 0.095 Uiso 1 1 calc R . . H13B H 0.0605 0.1159 0.9097 0.095 Uiso 1 1 calc R . . H13C H 0.1718 0.1488 0.8490 0.095 Uiso 1 1 calc R . . C14 C 0.4397(4) 0.1497(3) 1.0002(4) 0.0739(11) Uani 1 1 d . . . H14A H 0.4419 0.1410 0.9231 0.111 Uiso 1 1 calc R . . H14B H 0.5036 0.1092 1.0348 0.111 Uiso 1 1 calc R . . H14C H 0.4829 0.2374 1.0582 0.111 Uiso 1 1 calc R . . C15 C 0.2690(5) 0.1086(3) 1.0990(3) 0.0722(11) Uani 1 1 d . . . H15A H 0.3327 0.0686 1.1348 0.108 Uiso 1 1 calc R . . H15B H 0.1603 0.0722 1.0856 0.108 Uiso 1 1 calc R . . H15C H 0.3140 0.1970 1.1550 0.108 Uiso 1 1 calc R . . C16 C 0.0824(4) -0.2486(3) 0.5501(3) 0.0556(8) Uani 1 1 d . . . H16A H 0.0420 -0.3396 0.5046 0.067 Uiso 1 1 calc R . . H16B H -0.0006 -0.2218 0.5121 0.067 Uiso 1 1 calc R . . C17 C 0.3449(4) -0.2434(3) 0.5861(4) 0.0689(10) Uani 1 1 d . . . H17A H 0.2973 -0.3337 0.5424 0.103 Uiso 1 1 calc R . . H17B H 0.3783 -0.2159 0.6739 0.103 Uiso 1 1 calc R . . H17C H 0.4368 -0.2136 0.5732 0.103 Uiso 1 1 calc R . . C18 C 0.1877(4) -0.2266(3) 0.4091(3) 0.0603(9) Uani 1 1 d . . . H18A H 0.1242 -0.3162 0.3579 0.072 Uiso 1 1 calc R . . H18B H 0.2864 -0.2078 0.4003 0.072 Uiso 1 1 calc R . . C19 C 0.0963(4) -0.1563(3) 0.3657(3) 0.0628(10) Uani 1 1 d . . . H19A H 0.0893 -0.1655 0.2853 0.075 Uiso 1 1 calc R . . H19B H -0.0122 -0.1876 0.3566 0.075 Uiso 1 1 calc R . . C20 C 0.1877(4) 0.0557(4) 0.4183(3) 0.0566(9) Uani 1 1 d . . . H20 H 0.135(4) 0.030(3) 0.330(4) 0.077(11) Uiso 1 1 d . . . C21 C 0.2649(4) 0.1863(3) 0.4917(3) 0.0542(8) Uani 1 1 d . . . C22 C 0.3280(4) 0.2404(3) 0.6216(3) 0.0553(8) Uani 1 1 d . . . C23 C 0.3998(4) 0.3703(3) 0.6909(4) 0.0640(9) Uani 1 1 d . . . C24 C 0.4057(5) 0.4393(4) 0.6288(4) 0.0774(11) Uani 1 1 d . . . H24 H 0.4555 0.5265 0.6750 0.093 Uiso 1 1 calc R . . C25 C 0.3423(5) 0.3877(4) 0.5017(4) 0.0798(12) Uani 1 1 d . . . H25 H 0.3469 0.4390 0.4626 0.096 Uiso 1 1 calc R . . C26 C 0.2734(4) 0.2621(4) 0.4339(4) 0.0675(10) Uani 1 1 d . . . H26 H 0.2311 0.2260 0.3472 0.081 Uiso 1 1 calc R . . C27 C 0.4693(6) 0.4264(4) 0.8288(4) 0.0847(13) Uani 1 1 d . . . H27A H 0.5138 0.5165 0.8639 0.127 Uiso 1 1 calc R . . H27B H 0.5529 0.3981 0.8597 0.127 Uiso 1 1 calc R . . H27C H 0.3863 0.4011 0.8521 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0519(6) 0.0514(6) 0.0439(5) 0.0224(4) 0.0240(4) 0.0179(5) O1 0.0679(14) 0.0476(12) 0.0560(13) 0.0255(11) 0.0392(11) 0.0246(11) N1 0.0549(16) 0.0678(18) 0.0462(15) 0.0251(15) 0.0254(13) 0.0269(14) C1 0.055(2) 0.068(2) 0.063(2) 0.0290(19) 0.0263(17) 0.0157(18) O2 0.0845(17) 0.0547(14) 0.0560(13) 0.0299(12) 0.0388(12) 0.0292(12) N2 0.0525(16) 0.0563(16) 0.0514(15) 0.0243(13) 0.0288(13) 0.0232(13) C2 0.0442(17) 0.0476(18) 0.0532(18) 0.0243(16) 0.0260(14) 0.0198(14) C3 0.0442(17) 0.0514(19) 0.0482(18) 0.0200(15) 0.0228(14) 0.0151(15) C4 0.0529(19) 0.0400(17) 0.056(2) 0.0158(15) 0.0233(16) 0.0116(15) C5 0.0474(18) 0.0500(19) 0.0528(19) 0.0223(16) 0.0250(15) 0.0168(15) C6 0.0461(17) 0.0507(19) 0.0454(17) 0.0208(15) 0.0209(14) 0.0188(15) C7 0.0417(17) 0.0475(17) 0.0464(17) 0.0206(14) 0.0216(14) 0.0170(14) C8 0.059(2) 0.0481(19) 0.059(2) 0.0282(16) 0.0274(17) 0.0203(16) C9 0.064(2) 0.061(2) 0.083(3) 0.039(2) 0.036(2) 0.0193(18) C10 0.069(2) 0.057(2) 0.095(3) 0.040(2) 0.038(2) 0.0265(19) C11 0.098(3) 0.061(2) 0.066(2) 0.038(2) 0.031(2) 0.026(2) C12 0.0524(18) 0.0462(18) 0.0465(17) 0.0195(15) 0.0225(15) 0.0166(15) C13 0.077(2) 0.060(2) 0.059(2) 0.0253(18) 0.0321(18) 0.0367(19) C14 0.054(2) 0.052(2) 0.086(3) 0.013(2) 0.027(2) 0.0082(17) C15 0.097(3) 0.052(2) 0.049(2) 0.0153(17) 0.0260(19) 0.020(2) C16 0.0500(19) 0.0521(19) 0.057(2) 0.0191(16) 0.0258(16) 0.0124(16) C17 0.069(2) 0.065(2) 0.081(3) 0.034(2) 0.036(2) 0.036(2) C18 0.068(2) 0.055(2) 0.053(2) 0.0144(17) 0.0349(17) 0.0193(18) C19 0.065(2) 0.066(2) 0.0387(17) 0.0149(17) 0.0189(16) 0.0150(19) C20 0.052(2) 0.080(3) 0.050(2) 0.034(2) 0.0266(16) 0.0329(19) C21 0.0489(18) 0.071(2) 0.061(2) 0.0384(19) 0.0315(16) 0.0298(17) C22 0.0537(19) 0.065(2) 0.067(2) 0.0405(19) 0.0336(17) 0.0299(17) C23 0.062(2) 0.065(2) 0.078(2) 0.039(2) 0.0351(19) 0.0282(19) C24 0.074(3) 0.067(3) 0.098(3) 0.048(2) 0.037(2) 0.027(2) C25 0.079(3) 0.092(3) 0.097(3) 0.067(3) 0.043(3) 0.037(3) C26 0.064(2) 0.093(3) 0.075(2) 0.057(2) 0.039(2) 0.041(2) C27 0.109(3) 0.054(2) 0.080(3) 0.026(2) 0.039(3) 0.026(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 1.757(2) . ? Al1 O2 1.827(2) . ? Al1 C1 1.960(3) . ? Al1 N1 1.979(3) . ? Al1 N2 2.266(3) . ? O1 C2 1.343(4) . ? N1 C20 1.296(5) . ? N1 C19 1.473(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? O2 C22 1.309(4) . ? N2 C18 1.482(4) . ? N2 C17 1.484(4) . ? N2 C16 1.496(4) . ? C2 C3 1.396(4) . ? C2 C7 1.409(4) . ? C3 C4 1.386(4) . ? C3 C16 1.507(4) . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 C8 1.535(4) . ? C6 C7 1.394(4) . ? C6 H6 0.9500 . ? C7 C12 1.540(4) . ? C8 C11 1.523(5) . ? C8 C10 1.533(5) . ? C8 C9 1.540(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.531(5) . ? C12 C13 1.529(5) . ? C12 C15 1.538(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.500(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.429(5) . ? C20 H20 0.99(4) . ? C21 C26 1.406(5) . ? C21 C22 1.423(5) . ? C22 C23 1.416(5) . ? C23 C24 1.377(5) . ? C23 C27 1.510(5) . ? C24 C25 1.392(6) . ? C24 H24 0.9500 . ? C25 C26 1.369(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 90.48(11) . . ? O1 Al1 C1 124.68(14) . . ? O2 Al1 C1 99.65(14) . . ? O1 Al1 N1 120.70(12) . . ? O2 Al1 N1 89.51(12) . . ? C1 Al1 N1 113.68(13) . . ? O1 Al1 N2 87.64(10) . . ? O2 Al1 N2 165.45(12) . . ? C1 Al1 N2 93.26(13) . . ? N1 Al1 N2 79.10(11) . . ? C2 O1 Al1 134.78(19) . . ? C20 N1 C19 117.0(3) . . ? C20 N1 Al1 123.5(2) . . ? C19 N1 Al1 118.9(2) . . ? 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 . . ? C22 O2 Al1 129.2(2) . . ? C18 N2 C17 109.0(3) . . ? C18 N2 C16 110.3(2) . . ? C17 N2 C16 108.5(3) . . ? C18 N2 Al1 104.4(2) . . ? C17 N2 Al1 116.5(2) . . ? C16 N2 Al1 107.99(19) . . ? O1 C2 C3 118.8(3) . . ? O1 C2 C7 121.4(3) . . ? C3 C2 C7 119.8(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 C16 120.8(3) . . ? C2 C3 C16 118.3(3) . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 116.7(3) . . ? C4 C5 C8 119.7(3) . . ? C6 C5 C8 123.6(3) . . ? C5 C6 C7 124.4(3) . . ? C5 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? C6 C7 C2 116.9(3) . . ? C6 C7 C12 121.9(3) . . ? C2 C7 C12 121.1(3) . . ? C11 C8 C10 107.3(3) . . ? C11 C8 C5 112.4(3) . . ? C10 C8 C5 109.8(3) . . ? C11 C8 C9 108.9(3) . . ? C10 C8 C9 110.1(3) . . ? C5 C8 C9 108.2(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C13 109.8(3) . . ? C14 C12 C15 108.2(3) . . ? C13 C12 C15 107.0(3) . . ? C14 C12 C7 109.5(3) . . ? C13 C12 C7 110.5(3) . . ? C15 C12 C7 111.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C3 112.2(3) . . ? N2 C16 H16A 109.2 . . ? C3 C16 H16A 109.2 . . ? N2 C16 H16B 109.2 . . ? C3 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 110.7(3) . . ? N2 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N1 C19 C18 107.2(3) . . ? N1 C19 H19A 110.3 . . ? C18 C19 H19A 110.3 . . ? N1 C19 H19B 110.3 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 108.5 . . ? N1 C20 C21 126.1(3) . . ? N1 C20 H20 121(2) . . ? C21 C20 H20 113(2) . . ? C26 C21 C22 119.9(3) . . ? C26 C21 C20 119.1(3) . . ? C22 C21 C20 121.0(3) . . ? O2 C22 C23 119.4(3) . . ? O2 C22 C21 121.3(3) . . ? C23 C22 C21 119.2(3) . . ? C24 C23 C22 118.0(4) . . ? C24 C23 C27 123.3(4) . . ? C22 C23 C27 118.7(3) . . ? C23 C24 C25 123.3(4) . . ? C23 C24 H24 118.3 . . ? C25 C24 H24 118.3 . . ? C26 C25 C24 119.1(4) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C21 120.4(4) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.84 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.197 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.043 #=== End data_Al2(Me)2(3) _database_code_depnum_ccdc_archive 'CCDC 829023' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H48 Al2 N2 O2' _chemical_formula_sum 'C30 H48 Al2 N2 O2' _chemical_formula_weight 522.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5560(9) _cell_length_b 10.7180(11) _cell_length_c 14.6300(13) _cell_angle_alpha 75.586(5) _cell_angle_beta 72.438(5) _cell_angle_gamma 78.516(6) _cell_volume 1514.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 46047 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description BLOCK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28305 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 27.58 _reflns_number_total 6868 _reflns_number_gt 5102 _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^)+(0.0497P)^2^+0.6615P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6868 _refine_ls_number_parameters 341 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.79894(5) 0.20699(5) 0.52072(4) 0.03033(14) Uani 1 1 d . . . O1 O 0.93460(12) 0.25464(12) 0.41908(8) 0.0331(3) Uani 1 1 d . . . N1 N 0.86093(15) 0.26504(14) 0.61489(10) 0.0296(3) Uani 1 1 d . . . C1 C 0.62824(19) 0.31190(19) 0.50699(14) 0.0376(4) Uani 1 1 d . . . H1A H 0.6374 0.4044 0.4937 0.056 Uiso 1 1 calc R . . H1B H 0.5579 0.2907 0.5677 0.056 Uiso 1 1 calc R . . H1C H 0.6042 0.2930 0.4526 0.056 Uiso 1 1 calc R . . Al2 Al 0.74535(6) 0.22566(5) 0.96422(4) 0.03213(14) Uani 1 1 d . . . O2 O 0.78612(12) 0.12134(11) 1.06832(8) 0.0324(3) Uani 1 1 d . . . N2 N 0.77491(14) 0.08814(14) 0.88098(9) 0.0273(3) Uani 1 1 d . . . C2 C 0.8027(2) 0.01907(19) 0.56461(15) 0.0420(5) Uani 1 1 d . . . H2A H 0.7903 -0.0178 0.5135 0.063 Uiso 1 1 calc R . . H2B H 0.7304 0.0001 0.6245 0.063 Uiso 1 1 calc R . . H2C H 0.8893 -0.0194 0.5779 0.063 Uiso 1 1 calc R . . C3 C 0.8824(2) 0.3401(2) 0.89803(15) 0.0498(5) Uani 1 1 d . . . H3A H 0.9021 0.3771 0.9463 0.075 Uiso 1 1 calc R . . H3B H 0.8497 0.4103 0.8499 0.075 Uiso 1 1 calc R . . H3C H 0.9641 0.2902 0.8646 0.075 Uiso 1 1 calc R . . C4 C 0.5558(3) 0.2991(3) 0.99392(18) 0.0656(7) Uani 1 1 d . . . H4A H 0.5002 0.2285 1.0179 0.098 Uiso 1 1 calc R . . H4B H 0.5355 0.3546 0.9345 0.098 Uiso 1 1 calc R . . H4C H 0.5368 0.3509 1.0442 0.098 Uiso 1 1 calc R . . C5 C 1.04329(17) 0.30343(16) 0.41332(12) 0.0287(4) Uani 1 1 d . . . C6 C 1.14209(18) 0.32268(16) 0.32273(12) 0.0319(4) Uani 1 1 d . . . C7 C 1.25588(19) 0.37238(18) 0.31697(14) 0.0376(4) Uani 1 1 d . . . H7 H 1.3223 0.3846 0.2562 0.045 Uiso 1 1 calc R . . C8 C 1.2768(2) 0.4053(2) 0.39728(15) 0.0408(4) Uani 1 1 d . . . H8 H 1.3562 0.4392 0.3912 0.049 Uiso 1 1 calc R . . C9 C 1.1810(2) 0.38777(19) 0.48495(14) 0.0387(4) Uani 1 1 d . . . H9 H 1.1941 0.4109 0.5398 0.046 Uiso 1 1 calc R . . C10 C 1.06379(18) 0.33635(17) 0.49537(12) 0.0301(4) Uani 1 1 d . . . C11 C 1.1233(2) 0.2826(2) 0.23664(13) 0.0423(5) Uani 1 1 d . . . H11A H 1.2061 0.2872 0.1834 0.063 Uiso 1 1 calc R . . H11B H 1.0498 0.3412 0.2142 0.063 Uiso 1 1 calc R . . H11C H 1.1016 0.1933 0.2562 0.063 Uiso 1 1 calc R . . C12 C 0.96926(19) 0.31794(17) 0.59075(12) 0.0310(4) Uani 1 1 d . . . H12 H 0.9928(18) 0.3473(18) 0.6418(14) 0.033(5) Uiso 1 1 d . . . C13 C 0.78205(19) 0.24750(18) 0.71860(12) 0.0347(4) Uani 1 1 d . . . H13A H 0.6894 0.2348 0.7244 0.042 Uiso 1 1 calc R . . H13B H 0.7779 0.3255 0.7447 0.042 Uiso 1 1 calc R . . C14 C 0.85048(18) 0.12831(17) 0.77644(12) 0.0301(4) Uani 1 1 d . . . H14A H 0.8650 0.0545 0.7434 0.036 Uiso 1 1 calc R . . H14B H 0.9397 0.1465 0.7746 0.036 Uiso 1 1 calc R . . C15 C 0.64853(18) 0.0417(2) 0.88552(14) 0.0372(4) Uani 1 1 d . . . H15A H 0.5870 0.1154 0.8619 0.056 Uiso 1 1 calc R . . H15B H 0.6064 0.0023 0.9533 0.056 Uiso 1 1 calc R . . H15C H 0.6692 -0.0230 0.8443 0.056 Uiso 1 1 calc R . . C16 C 0.86438(18) -0.02542(17) 0.92533(12) 0.0304(4) Uani 1 1 d . . . H16A H 0.8870 -0.0937 0.8860 0.036 Uiso 1 1 calc R . . H16B H 0.9491 0.0046 0.9213 0.036 Uiso 1 1 calc R . . C17 C 0.80124(17) -0.08378(17) 1.03044(12) 0.0301(4) Uani 1 1 d . . . C18 C 0.76626(17) -0.00518(16) 1.10013(12) 0.0290(4) Uani 1 1 d . . . C19 C 0.71460(17) -0.05840(17) 1.20043(12) 0.0294(4) Uani 1 1 d . . . C20 C 0.70124(18) -0.19042(17) 1.22467(12) 0.0317(4) Uani 1 1 d . . . H20 H 0.6668 -0.2278 1.2917 0.038 Uiso 1 1 calc R . . C21 C 0.73524(18) -0.27161(17) 1.15673(12) 0.0311(4) Uani 1 1 d . . . C22 C 0.78456(19) -0.21486(17) 1.05874(12) 0.0327(4) Uani 1 1 d . . . H22 H 0.8072 -0.2664 1.0104 0.039 Uiso 1 1 calc R . . C24 C 0.67578(18) 0.02622(17) 1.27832(12) 0.0316(4) Uani 1 1 d . . . C25 C 0.5638(2) 0.1359(2) 1.25896(15) 0.0421(5) Uani 1 1 d . . . H25A H 0.5969 0.1940 1.1962 0.063 Uiso 1 1 calc R . . H25B H 0.5355 0.1851 1.3116 0.063 Uiso 1 1 calc R . . H25C H 0.4874 0.0988 1.2567 0.063 Uiso 1 1 calc R . . C26 C 0.7980(2) 0.0852(2) 1.27661(14) 0.0401(4) Uani 1 1 d . . . H26A H 0.8661 0.0155 1.2961 0.060 Uiso 1 1 calc R . . H26B H 0.7704 0.1448 1.3223 0.060 Uiso 1 1 calc R . . H26C H 0.8355 0.1329 1.2103 0.060 Uiso 1 1 calc R . . C27 C 0.6249(2) -0.0522(2) 1.38189(13) 0.0424(5) Uani 1 1 d . . . H27A H 0.5448 -0.0887 1.3860 0.064 Uiso 1 1 calc R . . H27B H 0.6024 0.0048 1.4291 0.064 Uiso 1 1 calc R . . H27C H 0.6949 -0.1229 1.3969 0.064 Uiso 1 1 calc R . . C28 C 0.72227(19) -0.41767(17) 1.19162(13) 0.0335(4) Uani 1 1 d . . . C29 C 0.5751(2) -0.4378(2) 1.24008(15) 0.0447(5) Uani 1 1 d . . . H29A H 0.5401 -0.3944 1.2960 0.067 Uiso 1 1 calc R . . H29B H 0.5688 -0.5310 1.2627 0.067 Uiso 1 1 calc R . . H29C H 0.5224 -0.4008 1.1925 0.067 Uiso 1 1 calc R . . C30 C 0.7766(2) -0.49097(19) 1.10751(14) 0.0426(5) Uani 1 1 d . . . H30A H 0.7249 -0.4563 1.0591 0.064 Uiso 1 1 calc R . . H30B H 0.7687 -0.5835 1.1330 0.064 Uiso 1 1 calc R . . H30C H 0.8711 -0.4801 1.0766 0.064 Uiso 1 1 calc R . . C31 C 0.8015(2) -0.4774(2) 1.26816(15) 0.0454(5) Uani 1 1 d . . . H31A H 0.8955 -0.4634 1.2395 0.068 Uiso 1 1 calc R . . H31B H 0.7962 -0.5710 1.2887 0.068 Uiso 1 1 calc R . . H31C H 0.7634 -0.4362 1.3250 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0355(3) 0.0295(3) 0.0245(3) -0.0017(2) -0.0073(2) -0.0067(2) O1 0.0378(7) 0.0384(7) 0.0233(6) -0.0048(5) -0.0071(5) -0.0089(6) N1 0.0371(8) 0.0271(7) 0.0201(7) -0.0006(6) -0.0059(6) -0.0018(6) C1 0.0378(10) 0.0373(10) 0.0364(10) -0.0057(8) -0.0096(8) -0.0050(8) Al2 0.0402(3) 0.0287(3) 0.0254(3) -0.0046(2) -0.0071(2) -0.0035(2) O2 0.0438(7) 0.0292(6) 0.0243(6) -0.0040(5) -0.0075(5) -0.0094(5) N2 0.0292(7) 0.0305(7) 0.0195(6) -0.0014(6) -0.0041(5) -0.0061(6) C2 0.0528(12) 0.0335(10) 0.0400(11) -0.0021(8) -0.0142(9) -0.0105(9) C3 0.0751(15) 0.0422(12) 0.0358(11) -0.0007(9) -0.0148(10) -0.0253(11) C4 0.0607(15) 0.0831(19) 0.0507(14) -0.0293(13) -0.0213(12) 0.0255(13) C5 0.0351(9) 0.0219(8) 0.0263(8) -0.0029(6) -0.0071(7) -0.0019(7) C6 0.0407(10) 0.0241(8) 0.0257(8) -0.0025(7) -0.0048(7) -0.0018(7) C7 0.0374(10) 0.0318(10) 0.0342(10) -0.0025(8) 0.0006(8) -0.0044(8) C8 0.0366(10) 0.0391(11) 0.0449(11) -0.0042(9) -0.0073(8) -0.0120(8) C9 0.0463(11) 0.0370(10) 0.0351(10) -0.0059(8) -0.0125(8) -0.0102(9) C10 0.0372(9) 0.0269(9) 0.0244(8) -0.0020(7) -0.0074(7) -0.0054(7) C11 0.0552(12) 0.0411(11) 0.0260(9) -0.0084(8) -0.0027(8) -0.0068(9) C12 0.0412(10) 0.0280(9) 0.0244(8) -0.0054(7) -0.0104(7) -0.0029(8) C13 0.0399(10) 0.0368(10) 0.0216(8) -0.0033(7) -0.0039(7) -0.0021(8) C14 0.0336(9) 0.0322(9) 0.0209(8) -0.0037(7) -0.0033(7) -0.0043(7) C15 0.0353(10) 0.0433(11) 0.0319(9) -0.0036(8) -0.0065(8) -0.0118(8) C16 0.0355(9) 0.0300(9) 0.0217(8) -0.0032(7) -0.0050(7) -0.0021(7) C17 0.0346(9) 0.0307(9) 0.0232(8) -0.0044(7) -0.0066(7) -0.0032(7) C18 0.0343(9) 0.0273(9) 0.0242(8) -0.0030(7) -0.0073(7) -0.0049(7) C19 0.0322(9) 0.0324(9) 0.0224(8) -0.0061(7) -0.0055(7) -0.0037(7) C20 0.0371(9) 0.0333(9) 0.0209(8) -0.0026(7) -0.0041(7) -0.0056(8) C21 0.0382(10) 0.0289(9) 0.0248(8) -0.0039(7) -0.0073(7) -0.0045(7) C22 0.0437(10) 0.0293(9) 0.0240(8) -0.0060(7) -0.0081(7) -0.0031(8) C24 0.0360(9) 0.0341(9) 0.0235(8) -0.0079(7) -0.0041(7) -0.0052(8) C25 0.0419(11) 0.0453(11) 0.0367(10) -0.0147(9) -0.0069(8) 0.0018(9) C26 0.0432(11) 0.0489(12) 0.0325(10) -0.0156(9) -0.0077(8) -0.0100(9) C27 0.0548(12) 0.0449(11) 0.0246(9) -0.0102(8) -0.0018(8) -0.0097(9) C28 0.0421(10) 0.0281(9) 0.0275(9) -0.0025(7) -0.0074(7) -0.0054(8) C29 0.0467(12) 0.0403(11) 0.0437(11) -0.0067(9) -0.0042(9) -0.0123(9) C30 0.0589(13) 0.0296(10) 0.0349(10) -0.0067(8) -0.0053(9) -0.0071(9) C31 0.0583(13) 0.0348(10) 0.0425(11) 0.0042(9) -0.0204(10) -0.0091(9) _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 1.7750(13) . ? Al1 C2 1.952(2) . ? Al1 N1 1.9613(15) . ? Al1 C1 1.9624(19) . ? O1 C5 1.325(2) . ? N1 C12 1.292(2) . ? N1 C13 1.479(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Al2 O2 1.7638(13) . ? Al2 C3 1.950(2) . ? Al2 C4 1.957(2) . ? Al2 N2 2.0577(15) . ? O2 C18 1.356(2) . ? N2 C15 1.492(2) . ? N2 C14 1.495(2) . ? N2 C16 1.521(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.415(2) . ? C5 C10 1.418(2) . ? C6 C7 1.380(3) . ? C6 C11 1.505(3) . ? C7 C8 1.395(3) . ? C7 H7 0.9500 . ? C8 C9 1.370(3) . ? C8 H8 0.9500 . ? C9 C10 1.405(3) . ? C9 H9 0.9500 . ? C10 C12 1.443(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12 0.990(19) . ? C13 C14 1.527(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.506(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.393(2) . ? C17 C18 1.401(2) . ? C18 C19 1.414(2) . ? C19 C20 1.396(2) . ? C19 C24 1.541(2) . ? C20 C21 1.402(2) . ? C20 H20 0.9500 . ? C21 C22 1.392(2) . ? C21 C28 1.541(2) . ? C22 H22 0.9500 . ? C24 C25 1.530(3) . ? C24 C27 1.532(2) . ? C24 C26 1.537(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 C30 1.528(3) . ? C28 C29 1.535(3) . ? C28 C31 1.536(3) . ? 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 . ? 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 C2 114.01(8) . . ? O1 Al1 N1 95.00(6) . . ? C2 Al1 N1 105.89(8) . . ? O1 Al1 C1 111.74(7) . . ? C2 Al1 C1 118.11(9) . . ? N1 Al1 C1 109.22(8) . . ? C5 O1 Al1 131.10(11) . . ? C12 N1 C13 117.71(15) . . ? C12 N1 Al1 122.88(12) . . ? C13 N1 Al1 119.41(12) . . ? 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 . . ? O2 Al2 C3 109.84(8) . . ? O2 Al2 C4 111.27(9) . . ? C3 Al2 C4 119.75(12) . . ? O2 Al2 N2 97.96(6) . . ? C3 Al2 N2 106.86(8) . . ? C4 Al2 N2 108.83(9) . . ? C18 O2 Al2 125.40(11) . . ? C15 N2 C14 109.52(13) . . ? C15 N2 C16 108.62(13) . . ? C14 N2 C16 105.88(12) . . ? C15 N2 Al2 113.41(11) . . ? C14 N2 Al2 114.25(11) . . ? C16 N2 Al2 104.64(10) . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Al2 C3 H3A 109.5 . . ? Al2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Al2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Al2 C4 H4A 109.5 . . ? Al2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Al2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 C6 119.03(15) . . ? O1 C5 C10 121.93(15) . . ? C6 C5 C10 119.04(16) . . ? C7 C6 C5 119.02(17) . . ? C7 C6 C11 121.80(16) . . ? C5 C6 C11 119.12(17) . . ? C6 C7 C8 122.34(17) . . ? C6 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C9 C8 C7 118.88(18) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 121.27(18) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C5 119.45(16) . . ? C9 C10 C12 117.90(16) . . ? C5 C10 C12 122.65(16) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 C10 126.21(16) . . ? N1 C12 H12 118.4(11) . . ? C10 C12 H12 115.4(11) . . ? N1 C13 C14 108.14(14) . . ? N1 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? N1 C13 H13B 110.1 . . ? C14 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N2 C14 C13 114.91(14) . . ? N2 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? N2 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 113.52(14) . . ? C17 C16 H16A 108.9 . . ? N2 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? N2 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C22 C17 C18 120.57(15) . . ? C22 C17 C16 120.78(15) . . ? C18 C17 C16 118.55(15) . . ? O2 C18 C17 117.90(14) . . ? O2 C18 C19 121.80(15) . . ? C17 C18 C19 120.29(16) . . ? C20 C19 C18 116.68(15) . . ? C20 C19 C24 122.18(15) . . ? C18 C19 C24 121.14(15) . . ? C19 C20 C21 124.41(15) . . ? C19 C20 H20 117.8 . . ? C21 C20 H20 117.8 . . ? C22 C21 C20 116.95(16) . . ? C22 C21 C28 122.70(16) . . ? C20 C21 C28 120.32(15) . . ? C21 C22 C17 121.10(16) . . ? C21 C22 H22 119.5 . . ? C17 C22 H22 119.5 . . ? C25 C24 C27 107.43(15) . . ? C25 C24 C26 109.24(16) . . ? C27 C24 C26 107.51(15) . . ? C25 C24 C19 110.26(15) . . ? C27 C24 C19 112.09(15) . . ? C26 C24 C19 110.20(14) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 108.63(16) . . ? C30 C28 C31 108.32(16) . . ? C29 C28 C31 107.91(16) . . ? C30 C28 C21 112.06(14) . . ? C29 C28 C21 110.54(15) . . ? C31 C28 C21 109.28(15) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.320 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.047 #====End data_Al(Me)(7) _database_code_depnum_ccdc_archive 'CCDC 829024' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 Al Cl2 N2 O2' _chemical_formula_weight 505.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.708(4) _cell_length_b 9.824(4) _cell_length_c 15.270(4) _cell_angle_alpha 82.591(15) _cell_angle_beta 75.027(16) _cell_angle_gamma 72.308(17) _cell_volume 1338.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11719 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.300 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15193 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 25.15 _reflns_number_total 4732 _reflns_number_gt 3014 _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^)+(0.0578P)^2^+0.4945P] 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 4732 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Cl1 Cl 0.30218(11) -0.00450(8) 0.53357(6) 0.0505(3) Uani 1 1 d . . . Al1 Al 0.28043(10) 0.45526(9) 0.40934(6) 0.0312(2) Uani 1 1 d . . . O1 O 0.1941(2) 0.4211(2) 0.32950(13) 0.0323(5) Uani 1 1 d . . . N1 N 0.1697(3) 0.5770(2) 0.51478(16) 0.0315(6) Uani 1 1 d . . . C1 C 0.4995(3) 0.3996(3) 0.3930(2) 0.0367(7) Uani 1 1 d . . . H1A H 0.5321 0.3061 0.4243 0.055 Uiso 1 1 calc R . . H1B H 0.5273 0.4713 0.4185 0.055 Uiso 1 1 calc R . . H1C H 0.5472 0.3939 0.3281 0.055 Uiso 1 1 calc R . . Cl2 Cl 0.24515(12) 0.16500(9) 0.86653(6) 0.0547(3) Uani 1 1 d . . . O2 O 0.2374(2) 0.3010(2) 0.48199(13) 0.0348(5) Uani 1 1 d . . . N2 N 0.2649(3) 0.6747(2) 0.34299(16) 0.0316(6) Uani 1 1 d . . . C2 C 0.2003(3) 0.4692(3) 0.24179(19) 0.0293(7) Uani 1 1 d . . . C3 C 0.1715(3) 0.6168(3) 0.2209(2) 0.0310(7) Uani 1 1 d . . . C4 C 0.1780(3) 0.6711(3) 0.1316(2) 0.0340(7) Uani 1 1 d . . . H4 H 0.1591 0.7714 0.1187 0.041 Uiso 1 1 calc R . . C5 C 0.2115(3) 0.5821(3) 0.0611(2) 0.0331(7) Uani 1 1 d . . . C6 C 0.2370(3) 0.4357(3) 0.0842(2) 0.0339(7) Uani 1 1 d . . . H6 H 0.2578 0.3734 0.0368 0.041 Uiso 1 1 calc R . . C7 C 0.2339(3) 0.3746(3) 0.1725(2) 0.0310(7) Uani 1 1 d . . . C8 C 0.2250(4) 0.6386(3) -0.0383(2) 0.0404(8) Uani 1 1 d . . . C9 C 0.1955(5) 0.8000(4) -0.0494(3) 0.0673(12) Uani 1 1 d . . . H9A H 0.2680 0.8278 -0.0265 0.101 Uiso 1 1 calc R . . H9B H 0.0949 0.8459 -0.0151 0.101 Uiso 1 1 calc R . . H9C H 0.2047 0.8306 -0.1138 0.101 Uiso 1 1 calc R . . C10 C 0.3775(5) 0.5663(5) -0.0940(3) 0.0800(14) Uani 1 1 d . . . H10A H 0.3830 0.5965 -0.1582 0.120 Uiso 1 1 calc R . . H10B H 0.3955 0.4622 -0.0862 0.120 Uiso 1 1 calc R . . H10C H 0.4530 0.5932 -0.0736 0.120 Uiso 1 1 calc R . . C11 C 0.1110(5) 0.6020(4) -0.0769(3) 0.0674(12) Uani 1 1 d . . . H11A H 0.0107 0.6463 -0.0415 0.101 Uiso 1 1 calc R . . H11B H 0.1292 0.4980 -0.0735 0.101 Uiso 1 1 calc R . . H11C H 0.1199 0.6383 -0.1403 0.101 Uiso 1 1 calc R . . C12 C 0.2682(4) 0.2112(3) 0.1924(2) 0.0348(7) Uani 1 1 d . . . C13 C 0.3010(4) 0.1301(3) 0.1063(2) 0.0475(9) Uani 1 1 d . . . H13A H 0.2145 0.1619 0.0792 0.071 Uiso 1 1 calc R . . H13B H 0.3220 0.0271 0.1221 0.071 Uiso 1 1 calc R . . H13C H 0.3874 0.1497 0.0626 0.071 Uiso 1 1 calc R . . C14 C 0.4052(4) 0.1551(3) 0.2333(2) 0.0446(8) Uani 1 1 d . . . H14A H 0.4907 0.1781 0.1907 0.067 Uiso 1 1 calc R . . H14B H 0.4268 0.0511 0.2447 0.067 Uiso 1 1 calc R . . H14C H 0.3855 0.2003 0.2905 0.067 Uiso 1 1 calc R . . C15 C 0.1351(4) 0.1746(3) 0.2599(2) 0.0410(8) Uani 1 1 d . . . H15A H 0.1180 0.2173 0.3177 0.062 Uiso 1 1 calc R . . H15B H 0.1560 0.0704 0.2698 0.062 Uiso 1 1 calc R . . H15C H 0.0463 0.2126 0.2352 0.062 Uiso 1 1 calc R . . C16 C 0.1394(3) 0.7125(3) 0.2968(2) 0.0346(7) Uani 1 1 d . . . H16A H 0.1221 0.8131 0.2724 0.041 Uiso 1 1 calc R . . H16B H 0.0478 0.7040 0.3414 0.041 Uiso 1 1 calc R . . C17 C 0.4000(4) 0.6928(3) 0.2763(2) 0.0410(8) Uani 1 1 d . . . H17A H 0.3798 0.7908 0.2492 0.061 Uiso 1 1 calc R . . H17B H 0.4282 0.6251 0.2286 0.061 Uiso 1 1 calc R . . H17C H 0.4814 0.6746 0.3070 0.061 Uiso 1 1 calc R . . C18 C 0.2306(4) 0.7717(3) 0.4171(2) 0.0358(7) Uani 1 1 d . . . H18A H 0.1910 0.8718 0.3951 0.043 Uiso 1 1 calc R . . H18B H 0.3227 0.7642 0.4362 0.043 Uiso 1 1 calc R . . C19 C 0.1178(4) 0.7330(3) 0.4970(2) 0.0347(7) Uani 1 1 d . . . H19A H 0.1104 0.7835 0.5509 0.042 Uiso 1 1 calc R . . H19B H 0.0188 0.7603 0.4828 0.042 Uiso 1 1 calc R . . C20 C 0.1616(3) 0.5297(3) 0.5980(2) 0.0342(7) Uani 1 1 d . . . H20 H 0.1236 0.5984 0.6431 0.041 Uiso 1 1 calc R . . C21 C 0.2053(3) 0.3817(3) 0.6286(2) 0.0310(7) Uani 1 1 d . . . C22 C 0.2398(3) 0.2732(3) 0.5676(2) 0.0331(7) Uani 1 1 d . . . C23 C 0.2698(3) 0.1308(3) 0.6051(2) 0.0351(7) Uani 1 1 d . . . C24 C 0.2723(4) 0.0972(3) 0.6950(2) 0.0384(8) Uani 1 1 d . . . H24 H 0.2956 0.0002 0.7175 0.046 Uiso 1 1 calc R . . C25 C 0.2402(4) 0.2077(3) 0.7526(2) 0.0392(8) Uani 1 1 d . . . C26 C 0.2051(3) 0.3475(3) 0.7210(2) 0.0358(7) Uani 1 1 d . . . H26 H 0.1804 0.4217 0.7614 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0786(7) 0.0348(4) 0.0454(5) -0.0032(4) -0.0244(5) -0.0179(4) Al1 0.0387(6) 0.0320(5) 0.0278(5) -0.0003(4) -0.0120(4) -0.0142(4) O1 0.0444(13) 0.0336(11) 0.0255(11) 0.0020(9) -0.0132(10) -0.0178(10) N1 0.0383(16) 0.0329(13) 0.0283(14) -0.0008(11) -0.0094(12) -0.0163(12) C1 0.0412(19) 0.0375(17) 0.0338(18) 0.0017(14) -0.0126(15) -0.0127(15) Cl2 0.0770(7) 0.0523(5) 0.0297(5) 0.0038(4) -0.0149(4) -0.0112(5) O2 0.0506(14) 0.0334(11) 0.0286(12) 0.0016(9) -0.0161(10) -0.0195(10) N2 0.0358(15) 0.0345(14) 0.0297(14) -0.0002(11) -0.0095(12) -0.0164(12) C2 0.0291(17) 0.0362(16) 0.0262(16) 0.0006(13) -0.0092(13) -0.0133(14) C3 0.0321(17) 0.0353(16) 0.0305(17) -0.0019(13) -0.0112(14) -0.0134(14) C4 0.0384(19) 0.0313(16) 0.0353(18) 0.0033(14) -0.0125(15) -0.0128(14) C5 0.0323(18) 0.0416(18) 0.0289(17) 0.0023(14) -0.0106(14) -0.0142(14) C6 0.0335(18) 0.0399(17) 0.0271(17) -0.0049(14) -0.0067(14) -0.0078(14) C7 0.0345(18) 0.0346(16) 0.0272(16) -0.0001(13) -0.0118(14) -0.0113(14) C8 0.046(2) 0.0466(19) 0.0284(17) 0.0039(14) -0.0089(15) -0.0159(16) C9 0.112(4) 0.051(2) 0.040(2) 0.0117(18) -0.020(2) -0.029(2) C10 0.067(3) 0.101(3) 0.041(2) 0.025(2) 0.002(2) -0.002(3) C11 0.100(3) 0.076(3) 0.044(2) 0.016(2) -0.038(2) -0.039(3) C12 0.044(2) 0.0333(16) 0.0282(17) -0.0035(13) -0.0119(15) -0.0094(15) C13 0.067(3) 0.0387(18) 0.0364(19) -0.0024(15) -0.0177(18) -0.0085(17) C14 0.048(2) 0.0395(18) 0.043(2) -0.0019(15) -0.0147(17) -0.0048(16) C15 0.054(2) 0.0372(17) 0.0369(19) 0.0018(14) -0.0138(16) -0.0190(16) C16 0.0370(19) 0.0346(16) 0.0355(18) -0.0004(14) -0.0119(15) -0.0129(14) C17 0.040(2) 0.0465(19) 0.0403(19) 0.0015(15) -0.0071(16) -0.0217(16) C18 0.047(2) 0.0329(16) 0.0353(18) -0.0027(13) -0.0150(16) -0.0178(15) C19 0.0430(19) 0.0322(16) 0.0324(17) -0.0043(13) -0.0115(15) -0.0122(14) C20 0.0367(19) 0.0381(17) 0.0327(18) -0.0062(14) -0.0077(15) -0.0163(15) C21 0.0345(18) 0.0358(16) 0.0268(16) -0.0029(13) -0.0060(14) -0.0161(14) C22 0.0331(18) 0.0403(17) 0.0313(17) 0.0028(14) -0.0112(14) -0.0171(14) C23 0.0396(19) 0.0327(16) 0.0362(18) -0.0043(14) -0.0128(15) -0.0109(14) C24 0.041(2) 0.0380(18) 0.0385(19) 0.0065(15) -0.0145(16) -0.0137(15) C25 0.041(2) 0.048(2) 0.0280(17) 0.0035(15) -0.0087(15) -0.0145(16) C26 0.0376(19) 0.0429(18) 0.0293(17) -0.0039(14) -0.0076(14) -0.0142(15) _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 Cl1 C23 1.732(3) . ? Al1 O1 1.762(2) . ? Al1 O2 1.847(2) . ? Al1 C1 1.984(3) . ? Al1 N1 2.000(3) . ? Al1 N2 2.239(3) . ? O1 C2 1.354(3) . ? N1 C20 1.287(4) . ? N1 C19 1.474(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Cl2 C25 1.745(3) . ? O2 C22 1.305(3) . ? N2 C18 1.480(4) . ? N2 C17 1.481(4) . ? N2 C16 1.491(4) . ? C2 C3 1.401(4) . ? C2 C7 1.407(4) . ? C3 C4 1.391(4) . ? C3 C16 1.497(4) . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.397(4) . ? C5 C8 1.534(4) . ? C6 C7 1.400(4) . ? C6 H6 0.9500 . ? C7 C12 1.544(4) . ? C8 C10 1.512(5) . ? C8 C9 1.518(5) . ? C8 C11 1.528(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.535(4) . ? C12 C15 1.536(4) . ? C12 C13 1.538(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.508(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.437(4) . ? C20 H20 0.9500 . ? C21 C26 1.407(4) . ? C21 C22 1.412(4) . ? C22 C23 1.415(4) . ? C23 C24 1.374(4) . ? C24 C25 1.396(4) . ? C24 H24 0.9500 . ? C25 C26 1.366(4) . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Al1 O2 89.71(9) . . ? O1 Al1 C1 122.72(13) . . ? O2 Al1 C1 100.04(12) . . ? O1 Al1 N1 123.13(11) . . ? O2 Al1 N1 87.81(10) . . ? C1 Al1 N1 113.62(12) . . ? O1 Al1 N2 88.90(9) . . ? O2 Al1 N2 163.15(11) . . ? C1 Al1 N2 94.82(11) . . ? N1 Al1 N2 78.94(10) . . ? C2 O1 Al1 130.56(17) . . ? C20 N1 C19 117.5(2) . . ? C20 N1 Al1 123.3(2) . . ? C19 N1 Al1 118.28(18) . . ? 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 . . ? C22 O2 Al1 126.98(18) . . ? C18 N2 C17 108.2(2) . . ? C18 N2 C16 110.1(2) . . ? C17 N2 C16 108.9(2) . . ? C18 N2 Al1 106.27(17) . . ? C17 N2 Al1 116.09(19) . . ? C16 N2 Al1 107.20(16) . . ? O1 C2 C3 118.5(3) . . ? O1 C2 C7 121.4(3) . . ? C3 C2 C7 120.1(3) . . ? C4 C3 C2 120.5(3) . . ? C4 C3 C16 121.5(3) . . ? C2 C3 C16 118.0(3) . . ? C5 C4 C3 121.4(3) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 116.8(3) . . ? C4 C5 C8 122.5(3) . . ? C6 C5 C8 120.7(3) . . ? C5 C6 C7 124.4(3) . . ? C5 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? C6 C7 C2 116.8(3) . . ? C6 C7 C12 121.4(3) . . ? C2 C7 C12 121.8(3) . . ? C10 C8 C9 110.2(3) . . ? C10 C8 C11 107.5(3) . . ? C9 C8 C11 106.9(3) . . ? C10 C8 C5 109.7(3) . . ? C9 C8 C5 112.7(3) . . ? C11 C8 C5 109.7(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C15 108.9(3) . . ? C14 C12 C13 107.4(3) . . ? C15 C12 C13 107.8(3) . . ? C14 C12 C7 110.2(2) . . ? C15 C12 C7 110.1(3) . . ? C13 C12 C7 112.3(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 C3 111.3(2) . . ? N2 C16 H16A 109.4 . . ? C3 C16 H16A 109.4 . . ? N2 C16 H16B 109.4 . . ? C3 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 110.3(2) . . ? N2 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N2 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N1 C19 C18 106.8(2) . . ? N1 C19 H19A 110.4 . . ? C18 C19 H19A 110.4 . . ? N1 C19 H19B 110.4 . . ? C18 C19 H19B 110.4 . . ? H19A C19 H19B 108.6 . . ? N1 C20 C21 125.5(3) . . ? N1 C20 H20 117.2 . . ? C21 C20 H20 117.2 . . ? C26 C21 C22 121.0(3) . . ? C26 C21 C20 118.8(3) . . ? C22 C21 C20 120.2(3) . . ? O2 C22 C21 122.6(3) . . ? O2 C22 C23 121.0(3) . . ? C21 C22 C23 116.3(3) . . ? C24 C23 C22 122.7(3) . . ? C24 C23 Cl1 119.7(2) . . ? C22 C23 Cl1 117.6(2) . . ? C23 C24 C25 119.0(3) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 120.9(3) . . ? C26 C25 Cl2 120.1(3) . . ? C24 C25 Cl2 119.0(2) . . ? C25 C26 C21 120.0(3) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.237 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.061 #=== END data_Al(Me)(8) _database_code_depnum_ccdc_archive 'CCDC 829025' #TrackingRef '- Xray.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H37 Al Cl2 N2 O2' _chemical_formula_weight 567.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0450(3) _cell_length_b 11.7530(3) _cell_length_c 17.2050(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.5930(10) _cell_angle_gamma 90.00 _cell_volume 2990.41(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16513 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 25.68 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.277 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; 'tbu group C29-C31 is disordered over two positions in a 60:40 ratio. The 40% occupied part was left isotropic. The c-C distances in this tBu were constrained to fit in the normal range' ; _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 35301 _diffrn_reflns_av_R_equivalents 0.1508 _diffrn_reflns_av_sigmaI/netI 0.1124 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 25.70 _reflns_number_total 5671 _reflns_number_gt 3462 _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^)+(0.0465P)^2^+4.2808P] 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 5671 _refine_ls_number_parameters 359 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.006 _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 Cl1 Cl 0.01437(7) -0.06993(10) 0.28311(6) 0.0575(3) Uani 1 1 d . . . Al1 Al 0.04748(7) 0.17777(9) 0.08052(6) 0.0315(3) Uani 1 1 d . . . O1 O 0.14905(15) 0.1087(2) 0.07433(13) 0.0325(6) Uani 1 1 d . . . N1 N -0.0689(2) 0.1654(2) 0.00504(17) 0.0361(7) Uani 1 1 d . . . C1 C 0.0330(3) 0.3030(3) 0.1524(2) 0.0389(9) Uani 1 1 d . . . H1A H 0.0827 0.3013 0.1981 0.058 Uiso 1 1 calc R . . H1B H -0.0247 0.2946 0.1706 0.058 Uiso 1 1 calc R . . H1C H 0.0337 0.3756 0.1246 0.058 Uiso 1 1 calc R . . Cl2 Cl -0.34173(9) 0.0295(2) 0.22799(9) 0.1401(10) Uani 1 1 d . . . O2 O 0.01265(15) 0.0560(2) 0.13555(14) 0.0351(6) Uani 1 1 d . . . N2 N 0.0750(2) 0.2900(2) -0.02404(17) 0.0346(7) Uani 1 1 d . . . C2 C -0.0671(2) 0.0480(3) 0.1546(2) 0.0355(9) Uani 1 1 d . . . C3 C -0.0795(3) -0.0081(4) 0.2246(2) 0.0439(10) Uani 1 1 d . . . C4 C -0.1623(3) -0.0142(5) 0.2472(3) 0.0614(13) Uani 1 1 d . . . H4 H -0.1681 -0.0502 0.2954 0.074 Uiso 1 1 calc R . . C5 C -0.2380(3) 0.0330(5) 0.1985(3) 0.0727(16) Uani 1 1 d . . . C6 C -0.2309(3) 0.0809(4) 0.1277(3) 0.0586(12) Uani 1 1 d . . . H6 H -0.2834 0.1085 0.0936 0.070 Uiso 1 1 calc R . . C7 C -0.1462(2) 0.0893(3) 0.1051(2) 0.0409(9) Uani 1 1 d . . . C8 C -0.1417(3) 0.1357(3) 0.0285(2) 0.0415(10) Uani 1 1 d . . . H8 H -0.1971 0.1451 -0.0077 0.050 Uiso 1 1 calc R . . C9 C -0.0772(3) 0.2133(3) -0.0751(2) 0.0425(10) Uani 1 1 d . . . H9A H -0.1408 0.2348 -0.0959 0.051 Uiso 1 1 calc R . . H9B H -0.0583 0.1564 -0.1112 0.051 Uiso 1 1 calc R . . C10 C -0.0168(3) 0.3173(3) -0.0698(2) 0.0407(9) Uani 1 1 d . . . H10A H -0.0118 0.3428 -0.1236 0.049 Uiso 1 1 calc R . . H10B H -0.0438 0.3799 -0.0434 0.049 Uiso 1 1 calc R . . C11 C 0.1312(2) 0.3930(3) -0.0076(2) 0.0346(8) Uani 1 1 d . . . C12 C 0.1308(3) 0.4758(3) -0.0644(2) 0.0428(9) Uani 1 1 d . . . H12 H 0.0908 0.4692 -0.1138 0.051 Uiso 1 1 calc R . . C13 C 0.1884(3) 0.5686(4) -0.0502(3) 0.0530(11) Uani 1 1 d . . . H13 H 0.1870 0.6260 -0.0893 0.064 Uiso 1 1 calc R . . C14 C 0.2479(3) 0.5775(4) 0.0210(3) 0.0522(11) Uani 1 1 d . . . H14 H 0.2883 0.6401 0.0307 0.063 Uiso 1 1 calc R . . C15 C 0.2482(3) 0.4951(3) 0.0776(3) 0.0458(10) Uani 1 1 d . . . H15 H 0.2885 0.5017 0.1268 0.055 Uiso 1 1 calc R . . C16 C 0.1906(2) 0.4027(3) 0.0639(2) 0.0379(9) Uani 1 1 d . . . H16 H 0.1917 0.3460 0.1035 0.045 Uiso 1 1 calc R . . C17 C 0.1222(3) 0.2094(3) -0.0720(2) 0.0403(9) Uani 1 1 d . . . H17A H 0.0876 0.1375 -0.0813 0.048 Uiso 1 1 calc R . . H17B H 0.1248 0.2439 -0.1240 0.048 Uiso 1 1 calc R . . C18 C 0.2159(3) 0.1849(3) -0.0290(2) 0.0361(9) Uani 1 1 d . . . C19 C 0.2912(3) 0.2157(3) -0.0590(2) 0.0434(10) Uani 1 1 d . . . H19 H 0.2835 0.2489 -0.1102 0.052 Uiso 1 1 calc R . . C20 C 0.3782(3) 0.1994(3) -0.0165(2) 0.0408(9) Uani 1 1 d . A . C21 C 0.3851(3) 0.1514(3) 0.0587(2) 0.0359(9) Uani 1 1 d . . . H21 H 0.4439 0.1401 0.0889 0.043 Uiso 1 1 calc R . . C22 C 0.3115(2) 0.1188(3) 0.0925(2) 0.0311(8) Uani 1 1 d . . . C23 C 0.2246(2) 0.1364(3) 0.0465(2) 0.0311(8) Uani 1 1 d . . . C24 C 0.3233(2) 0.0747(3) 0.1779(2) 0.0305(8) Uani 1 1 d . . . C25 C 0.4237(2) 0.0597(3) 0.2150(2) 0.0370(9) Uani 1 1 d . . . H25A H 0.4524 0.0083 0.1821 0.055 Uiso 1 1 calc R . . H25B H 0.4288 0.0274 0.2682 0.055 Uiso 1 1 calc R . . H25C H 0.4540 0.1338 0.2185 0.055 Uiso 1 1 calc R . . C26 C 0.2773(2) -0.0420(3) 0.1804(2) 0.0374(9) Uani 1 1 d . . . H26A H 0.2123 -0.0344 0.1601 0.056 Uiso 1 1 calc R . . H26B H 0.2870 -0.0697 0.2350 0.056 Uiso 1 1 calc R . . H26C H 0.3034 -0.0962 0.1475 0.056 Uiso 1 1 calc R . . C27 C 0.2834(3) 0.1605(3) 0.2293(2) 0.0378(9) Uani 1 1 d . . . H27A H 0.3128 0.2345 0.2271 0.057 Uiso 1 1 calc R . . H27B H 0.2936 0.1335 0.2841 0.057 Uiso 1 1 calc R . . H27C H 0.2183 0.1682 0.2096 0.057 Uiso 1 1 calc R . . C28 C 0.4612(3) 0.2416(3) -0.0469(2) 0.0547(12) Uani 1 1 d D . . C29 C 0.4436(6) 0.2370(9) -0.1381(2) 0.074(3) Uani 0.60 1 d PD A 1 H29A H 0.4345 0.1578 -0.1556 0.111 Uiso 0.60 1 calc PR A 1 H29B H 0.4957 0.2688 -0.1575 0.111 Uiso 0.60 1 calc PR A 1 H29C H 0.3894 0.2814 -0.1593 0.111 Uiso 0.60 1 calc PR A 1 C30 C 0.4752(7) 0.3678(4) -0.0248(7) 0.085(3) Uani 0.60 1 d PD A 1 H30A H 0.4191 0.4098 -0.0437 0.127 Uiso 0.60 1 calc PR A 1 H30B H 0.5238 0.3989 -0.0493 0.127 Uiso 0.60 1 calc PR A 1 H30C H 0.4916 0.3751 0.0328 0.127 Uiso 0.60 1 calc PR A 1 C31 C 0.5414(8) 0.1608(14) -0.0204(9) 0.097(7) Uani 0.60 1 d PD A 1 H31A H 0.5237 0.0830 -0.0370 0.145 Uiso 0.60 1 calc PR A 1 H31B H 0.5590 0.1634 0.0374 0.145 Uiso 0.60 1 calc PR A 1 H31C H 0.5925 0.1846 -0.0445 0.145 Uiso 0.60 1 calc PR A 1 C29' C 0.4504(12) 0.3130(14) -0.1229(6) 0.094(6) Uiso 0.40 1 d PD A 2 H29D H 0.5102 0.3342 -0.1331 0.142 Uiso 0.40 1 calc PR A 2 H29E H 0.4158 0.3820 -0.1167 0.142 Uiso 0.40 1 calc PR A 2 H29F H 0.4183 0.2684 -0.1675 0.142 Uiso 0.40 1 calc PR A 2 C30' C 0.5116(10) 0.3212(12) 0.0179(7) 0.084(5) Uiso 0.40 1 d PD A 2 H30D H 0.5217 0.2816 0.0689 0.126 Uiso 0.40 1 calc PR A 2 H30E H 0.4751 0.3895 0.0212 0.126 Uiso 0.40 1 calc PR A 2 H30F H 0.5699 0.3430 0.0047 0.126 Uiso 0.40 1 calc PR A 2 C31' C 0.5375(11) 0.1530(15) -0.0397(13) 0.050(5) Uiso 0.40 1 d PD A 2 H31D H 0.5450 0.1160 0.0121 0.075 Uiso 0.40 1 calc PR A 2 H31E H 0.5940 0.1909 -0.0453 0.075 Uiso 0.40 1 calc PR A 2 H31F H 0.5221 0.0957 -0.0814 0.075 Uiso 0.40 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 Cl1 0.0506(6) 0.0716(8) 0.0503(6) 0.0163(6) 0.0093(5) 0.0014(5) Al1 0.0311(6) 0.0305(6) 0.0304(6) -0.0027(5) -0.0008(4) 0.0015(5) O1 0.0304(13) 0.0331(13) 0.0331(13) 0.0034(10) 0.0035(10) 0.0034(10) N1 0.0351(18) 0.0331(17) 0.0361(17) -0.0048(14) -0.0041(14) 0.0039(14) C1 0.040(2) 0.037(2) 0.038(2) -0.0054(17) -0.0003(17) 0.0008(17) Cl2 0.0421(8) 0.307(3) 0.0770(10) 0.0101(14) 0.0262(7) -0.0019(12) O2 0.0291(13) 0.0368(14) 0.0390(14) 0.0013(11) 0.0048(11) 0.0018(11) N2 0.0398(18) 0.0316(17) 0.0295(16) -0.0012(13) -0.0015(13) 0.0075(13) C2 0.033(2) 0.033(2) 0.040(2) -0.0130(17) 0.0042(16) -0.0045(16) C3 0.039(2) 0.053(3) 0.039(2) -0.0104(19) 0.0040(17) -0.0040(19) C4 0.046(3) 0.095(4) 0.044(3) -0.011(3) 0.014(2) -0.018(3) C5 0.035(3) 0.130(5) 0.054(3) -0.014(3) 0.012(2) -0.009(3) C6 0.030(2) 0.091(4) 0.053(3) -0.021(3) 0.0023(19) -0.001(2) C7 0.031(2) 0.046(2) 0.044(2) -0.0115(19) 0.0017(17) -0.0009(17) C8 0.032(2) 0.041(2) 0.046(2) -0.0126(18) -0.0078(17) 0.0059(17) C9 0.046(2) 0.040(2) 0.036(2) -0.0022(17) -0.0077(17) 0.0072(18) C10 0.043(2) 0.039(2) 0.034(2) 0.0043(17) -0.0077(16) 0.0098(18) C11 0.035(2) 0.030(2) 0.039(2) -0.0002(16) 0.0078(16) 0.0086(16) C12 0.043(2) 0.042(2) 0.044(2) 0.0053(18) 0.0088(18) 0.0078(18) C13 0.055(3) 0.043(2) 0.064(3) 0.011(2) 0.017(2) 0.004(2) C14 0.040(2) 0.040(2) 0.079(3) 0.002(2) 0.017(2) 0.0005(19) C15 0.038(2) 0.044(2) 0.054(3) -0.006(2) 0.0039(19) 0.0027(19) C16 0.038(2) 0.034(2) 0.041(2) -0.0009(17) 0.0046(17) 0.0044(17) C17 0.052(2) 0.037(2) 0.030(2) -0.0032(16) 0.0020(17) 0.0118(18) C18 0.049(2) 0.031(2) 0.0288(19) 0.0005(16) 0.0080(16) 0.0112(17) C19 0.064(3) 0.035(2) 0.035(2) 0.0067(17) 0.020(2) 0.0154(19) C20 0.046(2) 0.032(2) 0.050(2) 0.0074(18) 0.0239(19) 0.0080(17) C21 0.036(2) 0.0283(19) 0.045(2) 0.0019(16) 0.0111(17) 0.0036(16) C22 0.034(2) 0.0251(18) 0.034(2) -0.0009(15) 0.0053(15) 0.0032(15) C23 0.036(2) 0.0264(18) 0.0313(19) -0.0022(15) 0.0069(15) 0.0050(15) C24 0.0302(18) 0.0280(19) 0.0315(19) 0.0032(15) 0.0010(15) -0.0004(15) C25 0.034(2) 0.036(2) 0.039(2) 0.0017(17) 0.0016(16) 0.0018(16) C26 0.035(2) 0.037(2) 0.038(2) 0.0064(17) -0.0011(16) -0.0018(16) C27 0.039(2) 0.042(2) 0.0316(19) -0.0020(17) 0.0041(16) 0.0024(17) C28 0.064(3) 0.042(2) 0.067(3) 0.008(2) 0.037(2) 0.005(2) C29 0.067(6) 0.097(8) 0.070(6) 0.018(5) 0.045(5) -0.004(5) C30 0.091(7) 0.038(5) 0.149(10) -0.017(6) 0.086(7) -0.019(5) C31 0.061(7) 0.129(12) 0.120(13) 0.071(10) 0.072(8) 0.038(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 Cl1 C3 1.736(4) . ? Al1 O1 1.751(2) . ? Al1 O2 1.845(3) . ? Al1 C1 1.960(4) . ? Al1 N1 1.985(3) . ? Al1 N2 2.329(3) . ? O1 C23 1.352(4) . ? N1 C8 1.283(5) . ? N1 C9 1.474(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Cl2 C5 1.728(5) . ? O2 C2 1.304(4) . ? N2 C11 1.474(5) . ? N2 C10 1.494(4) . ? N2 C17 1.516(5) . ? C2 C3 1.414(5) . ? C2 C7 1.416(5) . ? C3 C4 1.372(6) . ? C4 C5 1.399(7) . ? C4 H4 0.9500 . ? C5 C6 1.363(7) . ? C6 C7 1.403(6) . ? C6 H6 0.9500 . ? C7 C8 1.440(6) . ? C8 H8 0.9500 . ? C9 C10 1.515(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.379(5) . ? C11 C16 1.386(5) . ? C12 C13 1.387(6) . ? C12 H12 0.9500 . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.373(6) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.495(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.378(5) . ? C18 C23 1.402(5) . ? C19 C20 1.391(6) . ? C19 H19 0.9500 . ? C20 C21 1.398(5) . ? C20 C28 1.522(5) . ? C21 C22 1.395(5) . ? C21 H21 0.9500 . ? C22 C23 1.414(5) . ? C22 C24 1.538(5) . ? C24 C27 1.535(5) . ? C24 C25 1.538(5) . ? C24 C26 1.540(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 C30 1.536(2) . ? C28 C31 1.537(2) . ? C28 C29' 1.538(2) . ? C28 C31' 1.538(2) . ? C28 C30' 1.543(2) . ? C28 C29 1.544(2) . ? 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 . ? C29' H29D 0.9800 . ? C29' H29E 0.9800 . ? C29' H29F 0.9800 . ? C30' H30D 0.9800 . ? C30' H30E 0.9800 . ? C30' H30F 0.9800 . ? C31' H31D 0.9800 . ? C31' H31E 0.9800 . ? C31' H31F 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 90.30(11) . . ? O1 Al1 C1 125.87(14) . . ? O2 Al1 C1 100.58(14) . . ? O1 Al1 N1 126.98(13) . . ? O2 Al1 N1 88.81(12) . . ? C1 Al1 N1 106.29(14) . . ? O1 Al1 N2 86.21(11) . . ? O2 Al1 N2 160.71(12) . . ? C1 Al1 N2 96.81(14) . . ? N1 Al1 N2 78.29(12) . . ? C23 O1 Al1 135.3(2) . . ? C8 N1 C9 117.9(3) . . ? C8 N1 Al1 121.1(3) . . ? C9 N1 Al1 119.8(2) . . ? 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 . . ? C2 O2 Al1 123.1(2) . . ? C11 N2 C10 111.5(3) . . ? C11 N2 C17 108.0(3) . . ? C10 N2 C17 109.1(3) . . ? C11 N2 Al1 119.6(2) . . ? C10 N2 Al1 104.5(2) . . ? C17 N2 Al1 103.5(2) . . ? O2 C2 C3 121.3(3) . . ? O2 C2 C7 122.3(3) . . ? C3 C2 C7 116.4(3) . . ? C4 C3 C2 122.3(4) . . ? C4 C3 Cl1 119.8(3) . . ? C2 C3 Cl1 117.9(3) . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.7(4) . . ? C6 C5 Cl2 119.7(4) . . ? C4 C5 Cl2 119.6(4) . . ? C5 C6 C7 120.1(4) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 121.0(4) . . ? C6 C7 C8 118.6(4) . . ? C2 C7 C8 120.4(3) . . ? N1 C8 C7 125.2(3) . . ? N1 C8 H8 117.4 . . ? C7 C8 H8 117.4 . . ? N1 C9 C10 107.7(3) . . ? N1 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? N1 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N2 C10 C9 110.2(3) . . ? N2 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? N2 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C16 119.3(4) . . ? C12 C11 N2 121.1(3) . . ? C16 C11 N2 119.4(3) . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 119.5(4) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 119.8(4) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? C18 C17 N2 110.1(3) . . ? C18 C17 H17A 109.6 . . ? N2 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? N2 C17 H17B 109.6 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C23 120.8(3) . . ? C19 C18 C17 121.9(3) . . ? C23 C18 C17 117.1(3) . . ? C18 C19 C20 121.7(3) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C19 C20 C21 116.4(3) . . ? C19 C20 C28 121.7(3) . . ? C21 C20 C28 121.6(4) . . ? C22 C21 C20 124.5(3) . . ? C22 C21 H21 117.7 . . ? C20 C21 H21 117.7 . . ? C21 C22 C23 116.8(3) . . ? C21 C22 C24 122.0(3) . . ? C23 C22 C24 121.1(3) . . ? O1 C23 C18 119.0(3) . . ? O1 C23 C22 121.2(3) . . ? C18 C23 C22 119.8(3) . . ? C27 C24 C25 107.1(3) . . ? C27 C24 C22 109.9(3) . . ? C25 C24 C22 111.6(3) . . ? C27 C24 C26 110.1(3) . . ? C25 C24 C26 107.4(3) . . ? C22 C24 C26 110.7(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? 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 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 C30 108.3(4) . . ? C20 C28 C31 110.2(6) . . ? C30 C28 C31 117.2(10) . . ? C20 C28 C29' 120.3(7) . . ? C30 C28 C29' 70.9(8) . . ? C31 C28 C29' 123.0(9) . . ? C20 C28 C31' 113.5(10) . . ? C30 C28 C31' 124.5(10) . . ? C31 C28 C31' 12.7(13) . . ? C29' C28 C31' 113.5(11) . . ? C20 C28 C30' 105.9(7) . . ? C30 C28 C30' 37.7(6) . . ? C31 C28 C30' 84.5(10) . . ? C29' C28 C30' 104.2(9) . . ? C31' C28 C30' 95.3(11) . . ? C20 C28 C29 109.9(4) . . ? C30 C28 C29 106.0(7) . . ? C31 C28 C29 105.0(8) . . ? C29' C28 C29 35.2(6) . . ? C31' C28 C29 92.5(9) . . ? C30' C28 C29 136.5(8) . . ? 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 . . ? C28 C29' H29D 109.5 . . ? C28 C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C28 C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C28 C30' H30D 109.5 . . ? C28 C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C28 C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C28 C31' H31D 109.5 . . ? C28 C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C28 C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.70 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.824 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.064 #===END