# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1135 data_tiet _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H29 Cl5 N2 O2 Ti' _chemical_formula_weight 614.65 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.446(3) _cell_length_b 9.796(2) _cell_length_c 18.160(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.32(3) _cell_angle_gamma 90.00 _cell_volume 2725.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 25.12 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.831 _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 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Delft Instruments FAST TV area-detector diffractometer ; _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12060 _diffrn_reflns_av_R_equivalents 0.1880 _diffrn_reflns_av_sigmaI/netI 0.4004 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.12 _reflns_number_total 4283 _reflns_number_gt 1206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MADNES (Plugrath & Messerschmidt, 1992)' _computing_cell_refinement 'MADNES (Plugrath & Messerschmidt, 1992)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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 4283 _refine_ls_number_parameters 313 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.1820 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 0.597 _refine_ls_restrained_S_all 0.596 _refine_ls_shift/su_max 0.018 _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 Ti1 Ti 0.80459(10) 0.02738(13) 0.83364(9) 0.0251(4) Uani 1 1 d . . . Cl1 Cl 0.78527(15) -0.18641(18) 0.88016(13) 0.0383(6) Uani 1 1 d . . . Cl2 Cl 0.67224(14) 0.09302(19) 0.85014(13) 0.0320(6) Uani 1 1 d . . . N1 N 0.7966(4) 0.2357(5) 0.7884(3) 0.0172(15) Uani 1 1 d U . . N2 N 0.7157(4) 0.0082(6) 0.7094(3) 0.0207(16) Uani 1 1 d U . . O1 O 0.8806(3) 0.1040(5) 0.9216(3) 0.0251(13) Uani 1 1 d U . . O2 O 0.8813(3) -0.0430(4) 0.7918(3) 0.0271(14) Uani 1 1 d . . . C1 C 0.8960(5) 0.2279(7) 0.9581(4) 0.0219(19) Uani 1 1 d DU . . C2 C 0.9510(4) 0.2346(7) 1.0367(4) 0.028(2) Uani 1 1 d DU . . H2A H 0.9797 0.1540 1.0624 0.033 Uiso 1 1 calc R . . C3 C 0.9649(5) 0.3537(7) 1.0783(5) 0.033(2) Uani 1 1 d DU . . H3A H 1.0023 0.3572 1.1323 0.040 Uiso 1 1 calc R . . C4 C 0.9217(5) 0.4721(8) 1.0380(5) 0.035(2) Uani 1 1 d DU . . H4A H 0.9292 0.5558 1.0662 0.042 Uiso 1 1 calc R . . C5 C 0.8686(5) 0.4695(8) 0.9583(5) 0.029(2) Uani 1 1 d DU . . H5A H 0.8413 0.5508 0.9326 0.034 Uiso 1 1 calc R . . C6 C 0.8557(5) 0.3466(7) 0.9161(5) 0.0225(19) Uani 1 1 d DU . . C7 C 0.8013(5) 0.3442(6) 0.8311(4) 0.0158(18) Uiso 1 1 d U . . C8 C 0.7502(5) 0.4724(7) 0.7994(4) 0.030(2) Uani 1 1 d U . . H8A H 0.7251 0.4686 0.7410 0.036 Uiso 1 1 calc R . . H8B H 0.7894 0.5525 0.8151 0.036 Uiso 1 1 calc R . . C9 C 0.6761(5) 0.4876(7) 0.8321(5) 0.048(3) Uani 1 1 d U . . H9A H 0.6394 0.5658 0.8068 0.072 Uiso 1 1 calc R . . H9B H 0.7013 0.5022 0.8893 0.072 Uiso 1 1 calc R . . H9C H 0.6405 0.4044 0.8208 0.072 Uiso 1 1 calc R . . C10 C 0.7483(5) 0.2467(7) 0.7001(4) 0.0214(18) Uani 1 1 d U . . H10 H 0.6882 0.2820 0.6906 0.026 Uiso 1 1 calc R . . C11 C 0.7921(5) 0.3425(6) 0.6579(4) 0.028(2) Uani 1 1 d U . . H11A H 0.8038 0.4324 0.6845 0.034 Uiso 1 1 calc R . . H11B H 0.8485 0.3031 0.6602 0.034 Uiso 1 1 calc R . . C12 C 0.7318(5) 0.3596(7) 0.5721(4) 0.028(2) Uani 1 1 d U . . H12A H 0.7606 0.4178 0.5443 0.033 Uiso 1 1 calc R . . H12B H 0.6776 0.4063 0.5702 0.033 Uiso 1 1 calc R . . C13 C 0.7085(5) 0.2224(7) 0.5301(4) 0.032(2) Uani 1 1 d U . . H13A H 0.6613 0.2360 0.4781 0.038 Uiso 1 1 calc R . . H13B H 0.7601 0.1864 0.5206 0.038 Uiso 1 1 calc R . . C14 C 0.6790(5) 0.1181(7) 0.5770(4) 0.028(2) Uani 1 1 d U . . H14A H 0.6202 0.1432 0.5756 0.034 Uiso 1 1 calc R . . H14B H 0.6748 0.0274 0.5518 0.034 Uiso 1 1 calc R . . C15 C 0.7399(5) 0.1090(7) 0.6610(4) 0.0216(18) Uani 1 1 d U . . H15 H 0.7987 0.0832 0.6609 0.026 Uiso 1 1 calc R . . C16 C 0.7181(5) -0.1333(7) 0.6806(5) 0.029(2) Uani 1 1 d U . . C17 C 0.6457(5) -0.2067(8) 0.6583(4) 0.033(2) Uani 1 1 d U . . H17A H 0.6593 -0.2857 0.6948 0.040 Uiso 1 1 calc R . . H17B H 0.6396 -0.2441 0.6059 0.040 Uiso 1 1 calc R . . C18 C 0.5560(5) -0.1633(7) 0.6503(5) 0.046(3) Uani 1 1 d U . . H18A H 0.5213 -0.2439 0.6520 0.069 Uiso 1 1 calc R . . H18B H 0.5283 -0.1158 0.5998 0.069 Uiso 1 1 calc R . . H18C H 0.5593 -0.1018 0.6939 0.069 Uiso 1 1 calc R . . C19 C 0.8015(5) -0.1848(8) 0.6797(4) 0.024(2) Uani 1 1 d D . . C20 C 0.8059(6) -0.2749(7) 0.6245(5) 0.034(2) Uani 1 1 d D . . H20A H 0.7537 -0.3089 0.5858 0.041 Uiso 1 1 calc R . . C21 C 0.8884(6) -0.3187(7) 0.6242(5) 0.035(2) Uani 1 1 d D . . H21A H 0.8906 -0.3822 0.5855 0.042 Uiso 1 1 calc R . . C22 C 0.9642(6) -0.2708(7) 0.6788(5) 0.040(3) Uani 1 1 d D . . H22A H 1.0189 -0.3032 0.6794 0.048 Uiso 1 1 calc R . . C23 C 0.9607(5) -0.1769(8) 0.7319(5) 0.031(2) Uani 1 1 d D . . H23A H 1.0136 -0.1406 0.7683 0.038 Uiso 1 1 calc R . . C24 C 0.8813(6) -0.1315(7) 0.7349(5) 0.029(2) Uani 1 1 d D . . Cl1S Cl 1.48431(15) -0.2286(2) 0.30268(14) 0.0528(7) Uani 1 1 d . . . Cl2S Cl 1.49427(19) -0.4618(3) 0.39964(19) 0.0925(12) Uani 1 1 d . . . Cl3S Cl 1.5901(2) -0.2180(3) 0.46531(17) 0.0973(11) Uani 1 1 d . . . C1S C 1.5509(5) -0.3228(8) 0.3848(5) 0.044(2) Uani 1 1 d . . . H1SA H 1.6018 -0.3577 0.3728 0.053 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 Ti1 0.0275(10) 0.0263(9) 0.0206(9) -0.0002(8) 0.0076(8) 0.0013(7) Cl1 0.0520(17) 0.0254(12) 0.0387(15) 0.0023(11) 0.0181(13) -0.0009(11) Cl2 0.0352(14) 0.0346(12) 0.0314(14) -0.0013(10) 0.0184(12) -0.0019(10) N1 0.014(4) 0.018(4) 0.019(3) -0.010(3) 0.007(3) 0.003(3) N2 0.031(4) 0.019(4) 0.013(4) 0.002(3) 0.008(3) -0.003(3) O1 0.028(3) 0.028(3) 0.017(3) 0.000(2) 0.005(3) -0.004(3) O2 0.027(4) 0.026(3) 0.030(4) -0.009(3) 0.011(3) 0.006(3) C1 0.017(5) 0.034(5) 0.020(5) -0.004(4) 0.012(4) -0.004(4) C2 0.022(5) 0.030(5) 0.026(5) -0.002(4) 0.002(4) -0.002(4) C3 0.030(6) 0.039(6) 0.026(5) -0.007(4) 0.005(5) -0.017(4) C4 0.044(6) 0.029(5) 0.032(5) -0.011(4) 0.016(5) -0.016(4) C5 0.032(6) 0.028(5) 0.024(5) -0.009(4) 0.008(4) -0.013(4) C6 0.014(5) 0.033(5) 0.022(5) -0.005(3) 0.009(4) -0.010(3) C8 0.045(6) 0.018(4) 0.026(5) -0.003(4) 0.012(4) 0.001(4) C9 0.037(6) 0.040(6) 0.065(8) -0.008(5) 0.017(5) 0.010(5) C10 0.024(5) 0.032(5) 0.013(4) 0.003(3) 0.013(4) 0.004(4) C11 0.042(6) 0.007(4) 0.033(5) 0.005(3) 0.010(4) 0.004(4) C12 0.033(6) 0.037(5) 0.020(5) 0.007(4) 0.017(4) 0.004(4) C13 0.034(6) 0.051(6) 0.011(5) 0.000(4) 0.010(4) 0.006(4) C14 0.044(6) 0.023(5) 0.023(4) -0.006(4) 0.018(4) -0.003(4) C15 0.015(5) 0.030(4) 0.019(4) 0.004(3) 0.006(4) 0.001(4) C16 0.029(5) 0.030(5) 0.029(6) -0.003(4) 0.010(5) -0.001(4) C17 0.037(5) 0.051(6) 0.011(5) 0.009(4) 0.009(5) -0.002(4) C18 0.034(5) 0.054(6) 0.055(7) -0.002(5) 0.023(6) -0.008(5) C19 0.021(5) 0.037(5) 0.019(5) 0.004(4) 0.013(5) 0.001(4) C20 0.038(6) 0.024(5) 0.039(6) 0.003(4) 0.012(5) 0.003(4) C21 0.055(7) 0.008(5) 0.048(7) 0.006(4) 0.027(6) 0.005(4) C22 0.042(7) 0.026(6) 0.057(8) 0.007(5) 0.025(6) 0.013(5) C23 0.023(6) 0.037(6) 0.037(6) 0.014(5) 0.013(5) 0.003(4) C24 0.042(7) 0.030(5) 0.024(6) 0.003(4) 0.021(5) 0.001(4) Cl1S 0.0371(16) 0.0741(18) 0.0455(17) 0.0005(14) 0.0127(14) -0.0022(13) Cl2S 0.081(2) 0.068(2) 0.157(3) 0.043(2) 0.078(2) 0.0189(17) Cl3S 0.067(2) 0.160(3) 0.055(2) -0.051(2) 0.0105(18) 0.011(2) C1S 0.028(6) 0.073(6) 0.042(6) 0.005(5) 0.026(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O1 1.796(5) . y Ti1 O2 1.827(5) . y Ti1 N1 2.186(5) . y Ti1 N2 2.205(6) . y Ti1 Cl1 2.323(2) . y Ti1 Cl2 2.391(3) . y N1 C7 1.301(7) . ? N1 C10 1.512(8) . ? N2 C15 1.470(8) . ? N2 C16 1.488(8) . ? O1 C1 1.361(8) . ? O2 C24 1.349(8) . ? C1 C2 1.387(9) . ? C1 C6 1.417(9) . ? C2 C3 1.363(9) . ? C3 C4 1.417(9) . ? C4 C5 1.393(10) . ? C5 C6 1.401(9) . ? C6 C7 1.476(9) . ? C7 C8 1.504(8) . ? C8 C9 1.544(10) . ? C10 C15 1.507(9) . ? C10 C11 1.547(9) . ? C11 C12 1.521(9) . ? C12 C13 1.524(8) . ? C13 C14 1.518(9) . ? C14 C15 1.491(9) . ? C16 C17 1.321(9) . ? C16 C19 1.467(10) . ? C17 C18 1.492(10) . ? C19 C20 1.358(9) . ? C19 C24 1.429(10) . ? C20 C21 1.424(10) . ? C21 C22 1.363(10) . ? C22 C23 1.349(10) . ? C23 C24 1.400(10) . ? Cl1S C1S 1.757(8) . ? Cl2S C1S 1.725(8) . ? Cl3S C1S 1.709(8) . ? 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 Ti1 O2 99.5(2) . . y O1 Ti1 N1 82.6(2) . . ? O2 Ti1 N1 98.8(2) . . ? O1 Ti1 N2 159.0(2) . . ? O2 Ti1 N2 81.0(2) . . ? N1 Ti1 N2 76.6(2) . . y O1 Ti1 Cl1 101.34(17) . . ? O2 Ti1 Cl1 90.99(16) . . ? N1 Ti1 Cl1 168.77(17) . . ? N2 Ti1 Cl1 99.67(16) . . y O1 Ti1 Cl2 98.44(18) . . ? O2 Ti1 Cl2 161.99(18) . . ? N1 Ti1 Cl2 82.11(16) . . ? N2 Ti1 Cl2 81.70(17) . . ? Cl1 Ti1 Cl2 86.89(9) . . y C7 N1 C10 117.9(6) . . ? C7 N1 Ti1 123.8(5) . . ? C10 N1 Ti1 113.6(4) . . ? C15 N2 C16 111.6(6) . . ? C15 N2 Ti1 109.4(4) . . ? C16 N2 Ti1 110.2(4) . . ? C1 O1 Ti1 138.8(5) . . ? C24 O2 Ti1 138.9(5) . . ? O1 C1 C2 118.7(7) . . ? O1 C1 C6 120.1(7) . . ? C2 C1 C6 121.2(7) . . ? C3 C2 C1 121.8(7) . . ? C2 C3 C4 117.6(8) . . ? C5 C4 C3 121.9(7) . . ? C4 C5 C6 119.9(8) . . ? C5 C6 C1 117.6(7) . . ? C5 C6 C7 120.0(7) . . ? C1 C6 C7 122.4(7) . . ? N1 C7 C6 121.2(6) . . ? N1 C7 C8 123.4(7) . . ? C6 C7 C8 115.4(6) . . ? C7 C8 C9 110.1(6) . . ? C15 C10 N1 111.1(5) . . ? C15 C10 C11 106.7(6) . . ? N1 C10 C11 114.1(6) . . ? C12 C11 C10 109.0(6) . . ? C11 C12 C13 111.5(6) . . ? C14 C13 C12 112.7(6) . . ? C15 C14 C13 112.4(6) . . ? N2 C15 C14 115.1(6) . . ? N2 C15 C10 108.5(6) . . ? C14 C15 C10 109.9(6) . . ? C17 C16 C19 123.4(8) . . ? C17 C16 N2 118.6(7) . . ? C19 C16 N2 118.0(7) . . ? C16 C17 C18 128.6(8) . . ? C20 C19 C24 118.2(8) . . ? C20 C19 C16 122.2(8) . . ? C24 C19 C16 119.4(7) . . ? C19 C20 C21 120.4(8) . . ? C22 C21 C20 121.0(8) . . ? C23 C22 C21 119.2(9) . . ? C22 C23 C24 121.9(8) . . ? O2 C24 C23 119.6(8) . . ? O2 C24 C19 121.1(8) . . ? C23 C24 C19 119.2(8) . . ? Cl3S C1S Cl2S 113.4(5) . . ? Cl3S C1S Cl1S 109.6(4) . . ? Cl2S C1S Cl1S 110.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ti1 N1 C7 -35.5(6) . . . . ? O2 Ti1 N1 C7 -134.0(6) . . . . ? N2 Ti1 N1 C7 147.5(6) . . . . ? Cl1 Ti1 N1 C7 75.8(11) . . . . ? Cl2 Ti1 N1 C7 64.2(6) . . . . ? O1 Ti1 N1 C10 169.3(5) . . . . ? O2 Ti1 N1 C10 70.7(5) . . . . ? N2 Ti1 N1 C10 -7.8(4) . . . . ? Cl1 Ti1 N1 C10 -79.5(10) . . . . ? Cl2 Ti1 N1 C10 -91.1(4) . . . . ? O1 Ti1 N2 C15 23.4(9) . . . . ? O2 Ti1 N2 C15 -69.8(5) . . . . ? N1 Ti1 N2 C15 31.5(4) . . . . ? Cl1 Ti1 N2 C15 -159.3(4) . . . . ? Cl2 Ti1 N2 C15 115.4(4) . . . . ? O1 Ti1 N2 C16 146.4(6) . . . . ? O2 Ti1 N2 C16 53.2(5) . . . . ? N1 Ti1 N2 C16 154.6(5) . . . . ? Cl1 Ti1 N2 C16 -36.2(5) . . . . ? Cl2 Ti1 N2 C16 -121.6(5) . . . . ? O2 Ti1 O1 C1 125.7(7) . . . . ? N1 Ti1 O1 C1 28.0(7) . . . . ? N2 Ti1 O1 C1 36.0(11) . . . . ? Cl1 Ti1 O1 C1 -141.3(6) . . . . ? Cl2 Ti1 O1 C1 -52.8(7) . . . . ? O1 Ti1 O2 C24 166.9(7) . . . . ? N1 Ti1 O2 C24 -109.2(7) . . . . ? N2 Ti1 O2 C24 -34.4(7) . . . . ? Cl1 Ti1 O2 C24 65.2(7) . . . . ? Cl2 Ti1 O2 C24 -17.7(11) . . . . ? Ti1 O1 C1 C2 164.4(5) . . . . ? Ti1 O1 C1 C6 -14.9(11) . . . . ? O1 C1 C2 C3 -175.8(6) . . . . ? C6 C1 C2 C3 3.6(10) . . . . ? C1 C2 C3 C4 -0.6(10) . . . . ? C2 C3 C4 C5 -1.8(11) . . . . ? C3 C4 C5 C6 1.1(12) . . . . ? C4 C5 C6 C1 1.9(11) . . . . ? C4 C5 C6 C7 -178.4(7) . . . . ? O1 C1 C6 C5 175.2(6) . . . . ? C2 C1 C6 C5 -4.2(10) . . . . ? O1 C1 C6 C7 -4.5(10) . . . . ? C2 C1 C6 C7 176.1(6) . . . . ? C10 N1 C7 C6 -172.8(6) . . . . ? Ti1 N1 C7 C6 32.9(9) . . . . ? C10 N1 C7 C8 9.6(10) . . . . ? Ti1 N1 C7 C8 -144.7(6) . . . . ? C5 C6 C7 N1 171.7(7) . . . . ? C1 C6 C7 N1 -8.7(11) . . . . ? C5 C6 C7 C8 -10.6(10) . . . . ? C1 C6 C7 C8 169.1(6) . . . . ? N1 C7 C8 C9 107.4(8) . . . . ? C6 C7 C8 C9 -70.3(8) . . . . ? C7 N1 C10 C15 -173.3(6) . . . . ? Ti1 N1 C10 C15 -16.5(7) . . . . ? C7 N1 C10 C11 66.0(8) . . . . ? Ti1 N1 C10 C11 -137.2(5) . . . . ? C15 C10 C11 C12 64.4(7) . . . . ? N1 C10 C11 C12 -172.5(5) . . . . ? C10 C11 C12 C13 -56.7(8) . . . . ? C11 C12 C13 C14 48.6(9) . . . . ? C12 C13 C14 C15 -49.0(9) . . . . ? C16 N2 C15 C14 64.3(8) . . . . ? Ti1 N2 C15 C14 -173.5(5) . . . . ? C16 N2 C15 C10 -172.2(6) . . . . ? Ti1 N2 C15 C10 -49.9(6) . . . . ? C13 C14 C15 N2 -179.2(6) . . . . ? C13 C14 C15 C10 58.0(8) . . . . ? N1 C10 C15 N2 43.4(8) . . . . ? C11 C10 C15 N2 168.4(6) . . . . ? N1 C10 C15 C14 170.1(6) . . . . ? C11 C10 C15 C14 -65.0(8) . . . . ? C15 N2 C16 C17 -120.6(8) . . . . ? Ti1 N2 C16 C17 117.7(7) . . . . ? C15 N2 C16 C19 60.3(8) . . . . ? Ti1 N2 C16 C19 -61.4(8) . . . . ? C19 C16 C17 C18 -174.6(8) . . . . ? N2 C16 C17 C18 6.4(13) . . . . ? C17 C16 C19 C20 33.3(12) . . . . ? N2 C16 C19 C20 -147.6(7) . . . . ? C17 C16 C19 C24 -151.4(8) . . . . ? N2 C16 C19 C24 27.7(10) . . . . ? C24 C19 C20 C21 2.5(9) . . . . ? C16 C19 C20 C21 177.9(7) . . . . ? C19 C20 C21 C22 -0.4(10) . . . . ? C20 C21 C22 C23 -2.3(11) . . . . ? C21 C22 C23 C24 2.9(12) . . . . ? Ti1 O2 C24 C23 -167.8(5) . . . . ? Ti1 O2 C24 C19 9.3(11) . . . . ? C22 C23 C24 O2 176.4(7) . . . . ? C22 C23 C24 C19 -0.7(12) . . . . ? C20 C19 C24 O2 -179.1(6) . . . . ? C16 C19 C24 O2 5.3(11) . . . . ? C20 C19 C24 C23 -2.0(10) . . . . ? C16 C19 C24 C23 -177.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.481 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.090 #=END data_tiets _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H34 Al3 Cl3 N2 O2' _chemical_formula_weight 569.82 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.7057(15) _cell_length_b 9.7173(9) _cell_length_c 19.5089(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2977.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 4023 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 23.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.419 _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 230(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART area-detector diffractometer ; _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5592 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0977 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 23.00 _reflns_number_total 3804 _reflns_number_gt 2555 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0827P)^2^+2.0618P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.10(18) _refine_ls_number_reflns 3804 _refine_ls_number_parameters 314 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1607 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.89967(17) 1.1660(3) 0.83013(13) 0.0468(7) Uani 1 1 d . . . Al2 Al 0.77237(16) 1.1313(3) 0.93627(14) 0.0428(6) Uani 1 1 d . . . Al3 Al 0.97165(19) 0.3981(3) 1.13744(15) 0.0553(8) Uani 1 1 d U . . Cl11 Cl 1.0312(3) 0.2281(4) 1.1865(2) 0.1209(14) Uani 1 1 d U . . Cl12 Cl 0.9511(2) 0.3254(4) 1.03437(17) 0.0983(11) Uani 1 1 d U . . Cl13 Cl 1.0628(2) 0.5594(3) 1.13375(19) 0.1001(11) Uani 1 1 d U . . O1 O 0.8723(3) 1.0514(6) 0.9022(3) 0.0418(15) Uani 1 1 d . . . O2 O 0.8147(3) 1.2647(5) 0.8756(3) 0.0434(15) Uani 1 1 d . . . N1 N 0.8034(5) 1.0612(7) 1.0271(4) 0.0507(19) Uani 1 1 d . . . N2 N 0.7164(4) 1.2786(7) 0.9864(3) 0.0454(19) Uani 1 1 d . . . C1 C 0.9027(5) 0.9240(9) 0.9207(5) 0.046(2) Uani 1 1 d D . . C2 C 0.9442(5) 0.8458(9) 0.8726(5) 0.053(2) Uani 1 1 d D . . H2 H 0.9500 0.8783 0.8274 0.063 Uiso 1 1 calc R . . C3 C 0.9764(6) 0.7232(11) 0.8900(6) 0.075(3) Uani 1 1 d DU . . H3 H 1.0074 0.6732 0.8572 0.090 Uiso 1 1 calc R . . C4 C 0.9662(9) 0.6706(12) 0.9512(8) 0.108(5) Uani 1 1 d DU . . H4 H 0.9859 0.5812 0.9606 0.129 Uiso 1 1 calc R . . C5 C 0.9261(8) 0.7464(12) 1.0026(6) 0.098(4) Uani 1 1 d DU . . H5 H 0.9202 0.7101 1.0470 0.117 Uiso 1 1 calc R . . C6 C 0.8941(7) 0.8799(10) 0.9867(5) 0.063(3) Uani 1 1 d D . . C7 C 0.8559(6) 0.9630(11) 1.0427(5) 0.063(3) Uani 1 1 d . . . C8 C 0.8835(9) 0.9348(12) 1.1184(6) 0.090(4) Uani 1 1 d . . . H8A H 0.9403 0.8931 1.1192 0.108 Uiso 1 1 calc R . . H8B H 0.8858 1.0216 1.1439 0.108 Uiso 1 1 calc R . . C9 C 0.8217(10) 0.8414(13) 1.1505(8) 0.125(5) Uani 1 1 d . . . H9A H 0.8317 0.8384 1.1996 0.188 Uiso 1 1 calc R . . H9B H 0.8282 0.7499 1.1315 0.188 Uiso 1 1 calc R . . H9C H 0.7644 0.8744 1.1418 0.188 Uiso 1 1 calc R . . C10 C 0.7654(7) 1.1436(10) 1.0835(5) 0.060(3) Uani 1 1 d . . . H10A H 0.8080 1.2065 1.1026 0.072 Uiso 1 1 calc R . . H10B H 0.7455 1.0827 1.1202 0.072 Uiso 1 1 calc R . . C11 C 0.6907(7) 1.2252(10) 1.0540(5) 0.064(3) Uani 1 1 d . . . H11A H 0.6407 1.1655 1.0492 0.077 Uiso 1 1 calc R . . H11B H 0.6760 1.3015 1.0846 0.077 Uiso 1 1 calc R . . C12 C 0.6889(6) 1.3955(12) 0.9644(5) 0.064(3) Uani 1 1 d . . . C13 C 0.6248(7) 1.4826(11) 1.0044(6) 0.075(3) Uani 1 1 d . . . H13A H 0.5858 1.5270 0.9720 0.091 Uiso 1 1 calc R . . H13B H 0.5910 1.4222 1.0340 0.091 Uiso 1 1 calc R . . C14 C 0.6653(9) 1.5877(14) 1.0462(6) 0.100(4) Uani 1 1 d . . . H14A H 0.6226 1.6522 1.0623 0.150 Uiso 1 1 calc R . . H14B H 0.7074 1.6363 1.0191 0.150 Uiso 1 1 calc R . . H14C H 0.6929 1.5447 1.0852 0.150 Uiso 1 1 calc R . . C15 C 0.7206(6) 1.4558(9) 0.8989(4) 0.049(2) Uani 1 1 d D . . C16 C 0.6939(7) 1.5811(10) 0.8762(5) 0.075(3) Uani 1 1 d D . . H16 H 0.6513 1.6260 0.9016 0.090 Uiso 1 1 calc R . . C17 C 0.7241(8) 1.6451(11) 0.8204(6) 0.081(4) Uani 1 1 d D . . H17 H 0.7026 1.7315 0.8073 0.097 Uiso 1 1 calc R . . C18 C 0.7860(8) 1.5831(11) 0.7832(5) 0.071(3) Uani 1 1 d D . . H18 H 0.8086 1.6273 0.7444 0.085 Uiso 1 1 calc R . . C19 C 0.8153(6) 1.4570(9) 0.8020(5) 0.053(2) Uani 1 1 d D . . H19 H 0.8577 1.4138 0.7757 0.063 Uiso 1 1 calc R . . C20 C 0.7830(6) 1.3914(8) 0.8596(4) 0.044(2) Uani 1 1 d D . . C21 C 1.0121(6) 1.2387(13) 0.8383(6) 0.080(3) Uani 1 1 d . . . H21A H 1.0196 1.3129 0.8056 0.120 Uiso 1 1 calc R . . H21B H 1.0532 1.1666 0.8290 0.120 Uiso 1 1 calc R . . H21C H 1.0206 1.2735 0.8844 0.120 Uiso 1 1 calc R . . C22 C 0.8565(7) 1.1007(9) 0.7424(5) 0.064(3) Uani 1 1 d . . . H22A H 0.8827 1.1527 0.7056 0.096 Uiso 1 1 calc R . . H22B H 0.7952 1.1129 0.7408 0.096 Uiso 1 1 calc R . . H22C H 0.8701 1.0039 0.7371 0.096 Uiso 1 1 calc R . . C23 C 0.8639(6) 0.4507(11) 1.1804(6) 0.083(3) Uani 1 1 d . . . H23A H 0.8435 0.3757 1.2088 0.124 Uiso 1 1 calc R . . H23B H 0.8222 0.4708 1.1451 0.124 Uiso 1 1 calc R . . H23C H 0.8726 0.5318 1.2085 0.124 Uiso 1 1 calc R . . C24 C 0.6826(6) 1.0167(10) 0.9013(6) 0.069(3) Uani 1 1 d . . . H24A H 0.6907 0.9230 0.9172 0.104 Uiso 1 1 calc R . . H24B H 0.6836 1.0183 0.8515 0.104 Uiso 1 1 calc R . . H24C H 0.6281 1.0508 0.9174 0.104 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 0.0498(16) 0.0488(16) 0.0417(14) -0.0001(13) 0.0025(14) 0.0058(14) Al2 0.0407(14) 0.0378(14) 0.0501(15) 0.0055(13) 0.0019(13) 0.0037(13) Al3 0.0580(19) 0.0553(17) 0.0526(16) -0.0038(15) 0.0007(15) 0.0100(14) Cl11 0.142(4) 0.107(3) 0.113(3) 0.040(2) -0.005(2) 0.018(2) Cl12 0.109(2) 0.116(3) 0.0702(18) -0.0076(18) -0.0012(19) -0.030(2) Cl13 0.118(3) 0.083(2) 0.100(2) 0.002(2) -0.017(2) -0.0140(19) O1 0.043(4) 0.038(3) 0.044(3) 0.002(3) 0.003(3) 0.005(3) O2 0.051(4) 0.030(3) 0.050(3) 0.003(3) 0.014(3) 0.009(3) N1 0.058(5) 0.043(4) 0.051(5) 0.002(4) 0.013(4) 0.005(4) N2 0.052(5) 0.036(4) 0.048(5) 0.008(4) 0.009(4) 0.010(4) C1 0.038(5) 0.045(6) 0.054(6) 0.012(5) -0.014(5) -0.006(5) C2 0.060(7) 0.051(6) 0.047(6) 0.004(5) -0.001(5) 0.015(5) C3 0.066(8) 0.072(8) 0.087(7) 0.007(6) 0.003(6) 0.030(6) C4 0.132(12) 0.058(8) 0.134(10) 0.034(7) 0.025(9) 0.061(8) C5 0.124(10) 0.079(8) 0.090(8) 0.050(7) 0.027(8) 0.059(8) C6 0.062(7) 0.056(6) 0.071(7) 0.018(6) 0.010(5) 0.022(6) C7 0.062(7) 0.066(7) 0.062(7) 0.017(6) -0.005(6) 0.015(6) C8 0.103(10) 0.087(8) 0.080(8) 0.018(7) 0.022(7) 0.006(8) C9 0.156(14) 0.097(10) 0.122(13) 0.028(10) 0.015(11) 0.032(10) C10 0.082(8) 0.046(6) 0.051(6) 0.005(5) 0.015(6) -0.003(6) C11 0.074(7) 0.052(6) 0.065(7) 0.000(5) 0.027(6) 0.006(6) C12 0.048(6) 0.078(8) 0.067(7) -0.012(6) 0.014(5) 0.021(6) C13 0.081(8) 0.073(7) 0.073(7) 0.018(7) 0.002(6) 0.011(7) C14 0.117(11) 0.117(11) 0.066(8) -0.006(8) -0.005(8) 0.014(9) C15 0.062(6) 0.035(5) 0.049(6) -0.005(5) 0.002(5) 0.005(5) C16 0.103(10) 0.061(7) 0.061(7) 0.007(6) 0.017(7) 0.027(7) C17 0.123(10) 0.048(7) 0.073(8) 0.008(6) 0.022(8) 0.033(7) C18 0.113(10) 0.054(7) 0.047(6) 0.006(5) 0.005(6) -0.011(7) C19 0.073(7) 0.031(6) 0.054(6) -0.003(5) -0.004(5) 0.001(5) C20 0.056(6) 0.031(5) 0.044(5) 0.004(4) 0.001(5) 0.001(5) C21 0.062(7) 0.109(9) 0.068(7) -0.017(7) -0.001(6) -0.013(7) C22 0.088(8) 0.054(7) 0.050(6) -0.012(5) -0.006(6) 0.012(6) C23 0.062(7) 0.083(7) 0.103(9) -0.033(7) 0.028(6) 0.008(6) C24 0.045(6) 0.059(6) 0.104(9) -0.010(6) -0.016(6) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 O1 1.845(6) . y Al1 O2 1.868(6) . y Al1 C21 1.908(10) . ? Al1 C22 1.947(9) . ? Al1 Al2 2.898(4) . ? Al2 O1 1.873(6) . y Al2 O2 1.877(6) . y Al2 C24 1.922(9) . ? Al2 N2 1.945(7) . y Al2 N1 1.960(8) . y Al3 C23 1.956(10) . ? Al3 Cl13 2.124(4) . ? Al3 Cl11 2.126(4) . ? Al3 Cl12 2.155(4) . ? O1 C1 1.375(10) . ? O2 C20 1.364(9) . ? N1 C7 1.298(11) . ? N1 C10 1.485(11) . ? N2 C12 1.289(11) . ? N2 C11 1.473(11) . ? C1 C6 1.363(13) . ? C1 C2 1.374(12) . ? C2 C3 1.338(13) . ? C3 C4 1.308(17) . ? C4 C5 1.395(16) . ? C5 C6 1.425(13) . ? C6 C7 1.484(14) . ? C7 C8 1.564(15) . ? C8 C9 1.469(16) . ? C10 C11 1.528(14) . ? C12 C15 1.491(13) . ? C12 C13 1.529(14) . ? C13 C14 1.454(15) . ? C15 C16 1.361(13) . ? C15 C20 1.393(12) . ? C16 C17 1.341(15) . ? C17 C18 1.354(14) . ? C18 C19 1.360(14) . ? C19 C20 1.389(12) . ? 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 77.4(2) . . y O1 Al1 C21 112.0(4) . . ? O2 Al1 C21 115.5(4) . . ? O1 Al1 C22 113.1(4) . . ? O2 Al1 C22 109.6(4) . . ? C21 Al1 C22 121.1(5) . . ? O1 Al1 Al2 39.13(18) . . ? O2 Al1 Al2 39.41(18) . . ? C21 Al1 Al2 128.4(4) . . ? C22 Al1 Al2 110.5(4) . . ? O1 Al2 O2 76.5(2) . . y O1 Al2 C24 104.4(4) . . ? O2 Al2 C24 115.8(4) . . ? O1 Al2 N2 149.6(3) . . y O2 Al2 N2 88.2(3) . . y C24 Al2 N2 105.9(4) . . ? O1 Al2 N1 88.2(3) . . y O2 Al2 N1 136.2(3) . . y C24 Al2 N1 107.6(4) . . ? N2 Al2 N1 85.0(3) . . y O1 Al2 Al1 38.43(18) . . ? O2 Al2 Al1 39.19(17) . . ? C24 Al2 Al1 108.6(3) . . ? N2 Al2 Al1 125.9(2) . . ? N1 Al2 Al1 121.0(2) . . ? C23 Al3 Cl13 113.9(4) . . ? C23 Al3 Cl11 113.0(4) . . ? Cl13 Al3 Cl11 106.99(19) . . ? C23 Al3 Cl12 110.8(4) . . ? Cl13 Al3 Cl12 108.13(19) . . ? Cl11 Al3 Cl12 103.39(19) . . ? C1 O1 Al1 131.5(5) . . ? C1 O1 Al2 124.8(5) . . ? Al1 O1 Al2 102.4(3) . . ? C20 O2 Al1 128.0(5) . . ? C20 O2 Al2 129.7(5) . . ? Al1 O2 Al2 101.4(3) . . ? C7 N1 C10 118.6(8) . . ? C7 N1 Al2 128.6(7) . . ? C10 N1 Al2 112.5(6) . . ? C12 N2 C11 121.2(8) . . ? C12 N2 Al2 129.2(6) . . ? C11 N2 Al2 108.3(6) . . ? C6 C1 O1 119.8(8) . . ? C6 C1 C2 121.3(9) . . ? O1 C1 C2 118.9(8) . . ? C3 C2 C1 119.8(10) . . ? C4 C3 C2 122.3(12) . . ? C3 C4 C5 120.3(10) . . ? C4 C5 C6 118.9(10) . . ? C1 C6 C5 117.2(10) . . ? C1 C6 C7 124.3(8) . . ? C5 C6 C7 118.5(10) . . ? N1 C7 C6 119.0(9) . . ? N1 C7 C8 121.7(10) . . ? C6 C7 C8 119.2(9) . . ? C9 C8 C7 109.2(11) . . ? N1 C10 C11 108.0(8) . . ? N2 C11 C10 108.0(8) . . ? N2 C12 C15 121.4(8) . . ? N2 C12 C13 122.5(9) . . ? C15 C12 C13 116.1(9) . . ? C14 C13 C12 112.8(10) . . ? C16 C15 C20 116.1(9) . . ? C16 C15 C12 121.8(9) . . ? C20 C15 C12 122.0(8) . . ? C17 C16 C15 124.8(10) . . ? C16 C17 C18 118.9(10) . . ? C17 C18 C19 120.0(10) . . ? C18 C19 C20 120.6(9) . . ? O2 C20 C19 117.8(8) . . ? O2 C20 C15 122.4(8) . . ? C19 C20 C15 119.8(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Al1 Al2 O1 -161.8(4) . . . . ? C21 Al1 Al2 O1 -77.5(6) . . . . ? C22 Al1 Al2 O1 101.8(4) . . . . ? O1 Al1 Al2 O2 161.8(4) . . . . ? C21 Al1 Al2 O2 84.3(6) . . . . ? C22 Al1 Al2 O2 -96.4(4) . . . . ? O1 Al1 Al2 C24 -89.8(4) . . . . ? O2 Al1 Al2 C24 108.3(5) . . . . ? C21 Al1 Al2 C24 -167.3(6) . . . . ? C22 Al1 Al2 C24 12.0(5) . . . . ? O1 Al1 Al2 N2 143.2(4) . . . . ? O2 Al1 Al2 N2 -18.6(4) . . . . ? C21 Al1 Al2 N2 65.8(6) . . . . ? C22 Al1 Al2 N2 -114.9(4) . . . . ? O1 Al1 Al2 N1 35.3(4) . . . . ? O2 Al1 Al2 N1 -126.6(4) . . . . ? C21 Al1 Al2 N1 -42.2(6) . . . . ? C22 Al1 Al2 N1 137.1(4) . . . . ? O2 Al1 O1 C1 179.1(7) . . . . ? C21 Al1 O1 C1 -68.2(8) . . . . ? C22 Al1 O1 C1 72.9(7) . . . . ? Al2 Al1 O1 C1 167.4(8) . . . . ? O2 Al1 O1 Al2 11.7(3) . . . . ? C21 Al1 O1 Al2 124.4(4) . . . . ? C22 Al1 O1 Al2 -94.5(4) . . . . ? O2 Al2 O1 C1 179.8(6) . . . . ? C24 Al2 O1 C1 -66.6(7) . . . . ? N2 Al2 O1 C1 118.1(7) . . . . ? N1 Al2 O1 C1 41.1(6) . . . . ? Al1 Al2 O1 C1 -168.5(7) . . . . ? O2 Al2 O1 Al1 -11.7(3) . . . . ? C24 Al2 O1 Al1 101.9(4) . . . . ? N2 Al2 O1 Al1 -73.4(6) . . . . ? N1 Al2 O1 Al1 -150.3(3) . . . . ? O1 Al1 O2 C20 178.6(7) . . . . ? C21 Al1 O2 C20 70.0(8) . . . . ? C22 Al1 O2 C20 -71.1(7) . . . . ? Al2 Al1 O2 C20 -169.7(8) . . . . ? O1 Al1 O2 Al2 -11.6(3) . . . . ? C21 Al1 O2 Al2 -120.3(5) . . . . ? C22 Al1 O2 Al2 98.7(4) . . . . ? O1 Al2 O2 C20 -179.0(7) . . . . ? C24 Al2 O2 C20 81.3(7) . . . . ? N2 Al2 O2 C20 -25.5(7) . . . . ? N1 Al2 O2 C20 -106.3(7) . . . . ? Al1 Al2 O2 C20 169.5(8) . . . . ? O1 Al2 O2 Al1 11.5(3) . . . . ? C24 Al2 O2 Al1 -88.1(4) . . . . ? N2 Al2 O2 Al1 165.0(3) . . . . ? N1 Al2 O2 Al1 84.2(5) . . . . ? O1 Al2 N1 C7 -19.6(8) . . . . ? O2 Al2 N1 C7 -87.8(9) . . . . ? C24 Al2 N1 C7 84.9(9) . . . . ? N2 Al2 N1 C7 -169.9(8) . . . . ? Al1 Al2 N1 C7 -40.6(9) . . . . ? O1 Al2 N1 C10 154.7(6) . . . . ? O2 Al2 N1 C10 86.4(7) . . . . ? C24 Al2 N1 C10 -100.8(7) . . . . ? N2 Al2 N1 C10 4.3(6) . . . . ? Al1 Al2 N1 C10 133.6(6) . . . . ? O1 Al2 N2 C12 87.3(10) . . . . ? O2 Al2 N2 C12 28.4(9) . . . . ? C24 Al2 N2 C12 -88.0(9) . . . . ? N1 Al2 N2 C12 165.1(9) . . . . ? Al1 Al2 N2 C12 40.0(9) . . . . ? O1 Al2 N2 C11 -105.6(7) . . . . ? O2 Al2 N2 C11 -164.5(6) . . . . ? C24 Al2 N2 C11 79.1(7) . . . . ? N1 Al2 N2 C11 -27.8(6) . . . . ? Al1 Al2 N2 C11 -152.9(5) . . . . ? Al1 O1 C1 C6 158.3(7) . . . . ? Al2 O1 C1 C6 -36.8(11) . . . . ? Al1 O1 C1 C2 -19.2(11) . . . . ? Al2 O1 C1 C2 145.8(6) . . . . ? C6 C1 C2 C3 0.6(12) . . . . ? O1 C1 C2 C3 178.1(8) . . . . ? C1 C2 C3 C4 3.6(14) . . . . ? C2 C3 C4 C5 -5(2) . . . . ? C3 C4 C5 C6 2(2) . . . . ? O1 C1 C6 C5 179.4(9) . . . . ? C2 C1 C6 C5 -3.2(15) . . . . ? O1 C1 C6 C7 -2.3(14) . . . . ? C2 C1 C6 C7 175.2(9) . . . . ? C4 C5 C6 C1 1.8(18) . . . . ? C4 C5 C6 C7 -176.6(12) . . . . ? C10 N1 C7 C6 179.9(8) . . . . ? Al2 N1 C7 C6 -6.2(13) . . . . ? C10 N1 C7 C8 -3.2(13) . . . . ? Al2 N1 C7 C8 170.7(8) . . . . ? C1 C6 C7 N1 23.6(15) . . . . ? C5 C6 C7 N1 -158.1(10) . . . . ? C1 C6 C7 C8 -153.4(10) . . . . ? C5 C6 C7 C8 24.9(15) . . . . ? N1 C7 C8 C9 87.3(13) . . . . ? C6 C7 C8 C9 -95.9(12) . . . . ? C7 N1 C10 C11 -165.9(8) . . . . ? Al2 N1 C10 C11 19.3(9) . . . . ? C12 N2 C11 C10 -146.6(9) . . . . ? Al2 N2 C11 C10 45.1(9) . . . . ? N1 C10 C11 N2 -41.4(10) . . . . ? C11 N2 C12 C15 174.6(9) . . . . ? Al2 N2 C12 C15 -19.9(14) . . . . ? C11 N2 C12 C13 -3.4(15) . . . . ? Al2 N2 C12 C13 162.2(8) . . . . ? N2 C12 C13 C14 95.7(13) . . . . ? C15 C12 C13 C14 -82.3(12) . . . . ? N2 C12 C15 C16 -178.0(9) . . . . ? C13 C12 C15 C16 0.0(14) . . . . ? N2 C12 C15 C20 -2.1(14) . . . . ? C13 C12 C15 C20 176.0(9) . . . . ? C20 C15 C16 C17 -0.9(12) . . . . ? C12 C15 C16 C17 175.3(10) . . . . ? C15 C16 C17 C18 -0.4(14) . . . . ? C16 C17 C18 C19 1.3(16) . . . . ? C17 C18 C19 C20 -0.8(15) . . . . ? Al1 O2 C20 C19 1.4(11) . . . . ? Al2 O2 C20 C19 -165.5(6) . . . . ? Al1 O2 C20 C15 -178.4(6) . . . . ? Al2 O2 C20 C15 14.7(12) . . . . ? C18 C19 C20 O2 179.7(8) . . . . ? C18 C19 C20 C15 -0.5(13) . . . . ? C16 C15 C20 O2 -178.9(8) . . . . ? C12 C15 C20 O2 4.9(13) . . . . ? C16 C15 C20 C19 1.3(12) . . . . ? C12 C15 C20 C19 -174.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.338 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.068