# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jui-Hsien Huang' _publ_contact_author_email JUIHUANG@CC.NCUE.EDU.TW _publ_section_title ; Deprotonation and Reductive Addition Reactions of Aluminum Dihydride Compounds Containing Substituted Pyrrolyl Ligands with Phenols, Ketones, and Aldehydes ; loop_ _publ_author_name Jui-Hsien Huang I-Chun Chen Ya-Chi Chen Amitabha Datta ; Shi-Mau ; Ho Ching-Han Hu Che-Yu Lin Cheng-Yi Tu data_ya87am _database_code_depnum_ccdc_archive 'CCDC 721352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H23 Al Cl2 N4' _chemical_formula_weight 369.26 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.3892(4) _cell_length_b 10.8311(4) _cell_length_c 13.4949(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.3530(10) _cell_angle_gamma 90.00 _cell_volume 1834.84(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9192 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.7643 _exptl_absorpt_correction_T_max 0.9053 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30689 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.98 _reflns_number_total 4872 _reflns_number_gt 4305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0387P)^2^+0.8896P] 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 4872 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.47968(3) 0.05062(3) 0.22996(3) 0.01912(9) Uani 1 1 d . . . N1 N 0.64294(8) 0.04124(10) 0.22116(8) 0.0238(2) Uani 1 1 d . . . N2 N 0.55179(8) -0.04311(9) 0.34814(8) 0.0208(2) Uani 1 1 d . . . N3 N 0.34542(8) -0.03324(9) 0.26804(8) 0.0210(2) Uani 1 1 d . . . N4 N 0.48240(9) 0.21235(10) 0.27804(8) 0.0230(2) Uani 1 1 d . . . Cl1 Cl 0.60076(3) 0.39720(3) 0.44516(3) 0.03569(9) Uani 1 1 d . . . Cl2 Cl 0.36124(4) 0.25927(3) 0.04699(3) 0.04753(12) Uani 1 1 d . . . C1 C 0.67546(12) 0.15631(15) 0.18201(14) 0.0413(4) Uani 1 1 d . . . H1A H 0.7459 0.1449 0.1763 0.062 Uiso 1 1 calc R . . H1B H 0.6785 0.2237 0.2314 0.062 Uiso 1 1 calc R . . H1C H 0.6236 0.1766 0.1123 0.062 Uiso 1 1 calc R . . C2 C 0.64328(11) -0.06108(15) 0.14878(11) 0.0332(3) Uani 1 1 d . . . H2A H 0.5931 -0.0425 0.0778 0.050 Uiso 1 1 calc R . . H2B H 0.6219 -0.1377 0.1744 0.050 Uiso 1 1 calc R . . H2C H 0.7151 -0.0708 0.1461 0.050 Uiso 1 1 calc R . . C3 C 0.71780(10) 0.00996(13) 0.32951(10) 0.0263(3) Uani 1 1 d . . . H3A H 0.7420 0.0861 0.3716 0.032 Uiso 1 1 calc R . . H3B H 0.7810 -0.0339 0.3252 0.032 Uiso 1 1 calc R . . C4 C 0.65816(9) -0.07109(12) 0.37986(9) 0.0225(2) Uani 1 1 d . . . C5 C 0.67982(10) -0.16592(12) 0.45213(9) 0.0256(2) Uani 1 1 d . . . H5 H 0.7472 -0.2031 0.4869 0.031 Uiso 1 1 calc R . . C6 C 0.58119(11) -0.19764(12) 0.46483(10) 0.0258(3) Uani 1 1 d . . . H6 H 0.5704 -0.2600 0.5096 0.031 Uiso 1 1 calc R . . C7 C 0.50455(10) -0.11980(11) 0.39913(9) 0.0221(2) Uani 1 1 d . . . C8 C 0.38877(10) -0.09098(12) 0.37609(10) 0.0254(2) Uani 1 1 d . . . H8A H 0.3809 -0.0333 0.4298 0.030 Uiso 1 1 calc R . . H8B H 0.3491 -0.1676 0.3780 0.030 Uiso 1 1 calc R . . C9 C 0.29935(11) -0.13128(13) 0.18859(11) 0.0314(3) Uani 1 1 d . . . H9A H 0.2390 -0.1698 0.2020 0.047 Uiso 1 1 calc R . . H9B H 0.3538 -0.1939 0.1936 0.047 Uiso 1 1 calc R . . H9C H 0.2748 -0.0950 0.1176 0.047 Uiso 1 1 calc R . . C10 C 0.26024(11) 0.05593(13) 0.26264(12) 0.0298(3) Uani 1 1 d . . . H10A H 0.2358 0.0961 0.1932 0.045 Uiso 1 1 calc R . . H10B H 0.2879 0.1184 0.3179 0.045 Uiso 1 1 calc R . . H10C H 0.2005 0.0124 0.2732 0.045 Uiso 1 1 calc R . . C11 C 0.48423(9) 0.33118(11) 0.24370(9) 0.0200(2) Uani 1 1 d . . . C12 C 0.53531(9) 0.42994(12) 0.31120(10) 0.0227(2) Uani 1 1 d . . . C13 C 0.53815(10) 0.55050(12) 0.27789(12) 0.0287(3) Uani 1 1 d . . . H13 H 0.5726 0.6128 0.3275 0.034 Uiso 1 1 calc R . . C14 C 0.49041(11) 0.57974(13) 0.17177(12) 0.0315(3) Uani 1 1 d . . . H14 H 0.4934 0.6616 0.1477 0.038 Uiso 1 1 calc R . . C15 C 0.43836(11) 0.48796(13) 0.10130(11) 0.0298(3) Uani 1 1 d . . . H15 H 0.4053 0.5067 0.0284 0.036 Uiso 1 1 calc R . . C16 C 0.43454(10) 0.36862(12) 0.13722(10) 0.0253(2) Uani 1 1 d . . . H1 H 0.4355(13) 0.0061(16) 0.1198(13) 0.035(4) Uiso 1 1 d . . . H2 H 0.5089(14) 0.2127(16) 0.3455(14) 0.034(4) Uiso 1 1 d . . . 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 0.02237(17) 0.01634(17) 0.01702(16) -0.00035(12) 0.00481(13) -0.00033(12) N1 0.0248(5) 0.0243(5) 0.0235(5) 0.0031(4) 0.0097(4) -0.0005(4) N2 0.0217(5) 0.0211(5) 0.0191(4) 0.0021(4) 0.0064(4) 0.0007(4) N3 0.0217(4) 0.0167(5) 0.0241(5) -0.0016(4) 0.0073(4) -0.0005(4) N4 0.0310(5) 0.0183(5) 0.0169(5) -0.0014(4) 0.0050(4) -0.0013(4) Cl1 0.04059(19) 0.03567(19) 0.02407(16) -0.00828(13) 0.00273(13) -0.00763(14) Cl2 0.0733(3) 0.02534(17) 0.02324(16) -0.00140(13) -0.00936(16) -0.00169(17) C1 0.0335(7) 0.0383(8) 0.0571(10) 0.0194(7) 0.0220(7) -0.0006(6) C2 0.0328(7) 0.0436(8) 0.0246(6) -0.0035(6) 0.0120(5) 0.0070(6) C3 0.0210(5) 0.0318(7) 0.0240(6) -0.0009(5) 0.0051(4) -0.0025(5) C4 0.0225(5) 0.0254(6) 0.0180(5) -0.0014(4) 0.0051(4) 0.0020(4) C5 0.0291(6) 0.0269(6) 0.0190(5) 0.0002(5) 0.0058(5) 0.0074(5) C6 0.0361(6) 0.0216(6) 0.0209(5) 0.0022(5) 0.0112(5) 0.0047(5) C7 0.0289(6) 0.0192(5) 0.0197(5) 0.0003(4) 0.0102(5) 0.0004(4) C8 0.0285(6) 0.0234(6) 0.0275(6) 0.0040(5) 0.0138(5) 0.0007(5) C9 0.0327(7) 0.0227(6) 0.0365(7) -0.0083(5) 0.0092(6) -0.0085(5) C10 0.0266(6) 0.0255(6) 0.0382(7) 0.0015(5) 0.0124(5) 0.0048(5) C11 0.0196(5) 0.0181(5) 0.0225(5) -0.0022(4) 0.0077(4) 0.0010(4) C12 0.0198(5) 0.0228(6) 0.0249(6) -0.0047(5) 0.0071(4) -0.0010(4) C13 0.0244(6) 0.0209(6) 0.0419(7) -0.0082(5) 0.0129(5) -0.0047(5) C14 0.0302(6) 0.0196(6) 0.0478(8) 0.0044(6) 0.0174(6) 0.0001(5) C15 0.0336(7) 0.0252(6) 0.0307(6) 0.0062(5) 0.0114(5) 0.0052(5) C16 0.0297(6) 0.0204(6) 0.0231(6) -0.0019(5) 0.0056(5) 0.0015(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 N2 1.8534(10) . ? Al1 N4 1.8640(11) . ? Al1 N3 2.2278(10) . ? Al1 N1 2.2323(11) . ? N1 C1 1.4773(17) . ? N1 C2 1.4783(17) . ? N1 C3 1.4960(16) . ? N2 C7 1.3661(15) . ? N2 C4 1.3709(15) . ? N3 C10 1.4767(16) . ? N3 C9 1.4824(16) . ? N3 C8 1.5052(16) . ? N4 C11 1.3711(15) . ? Cl1 C12 1.7492(13) . ? Cl2 C16 1.7371(13) . ? C3 C4 1.4992(17) . ? C4 C5 1.3759(17) . ? C5 C6 1.4314(18) . ? C6 C7 1.3846(17) . ? C7 C8 1.5040(17) . ? C11 C16 1.4166(17) . ? C11 C12 1.4172(16) . ? C12 C13 1.3859(18) . ? C13 C14 1.387(2) . ? C14 C15 1.385(2) . ? C15 C16 1.3877(18) . ? 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 N2 Al1 N4 105.90(5) . . ? N2 Al1 N3 78.40(4) . . ? N4 Al1 N3 102.86(5) . . ? N2 Al1 N1 78.12(4) . . ? N4 Al1 N1 99.22(5) . . ? N3 Al1 N1 151.32(4) . . ? C1 N1 C2 109.10(11) . . ? C1 N1 C3 111.10(11) . . ? C2 N1 C3 108.73(10) . . ? C1 N1 Al1 113.36(8) . . ? C2 N1 Al1 107.30(8) . . ? C3 N1 Al1 107.10(7) . . ? C7 N2 C4 108.72(10) . . ? C7 N2 Al1 124.93(8) . . ? C4 N2 Al1 124.30(8) . . ? C10 N3 C9 108.23(10) . . ? C10 N3 C8 110.52(10) . . ? C9 N3 C8 109.04(10) . . ? C10 N3 Al1 113.16(8) . . ? C9 N3 Al1 106.94(8) . . ? C8 N3 Al1 108.82(7) . . ? C11 N4 Al1 139.91(9) . . ? N1 C3 C4 107.11(10) . . ? N2 C4 C5 109.05(11) . . ? N2 C4 C3 112.85(10) . . ? C5 C4 C3 138.08(12) . . ? C4 C5 C6 106.75(11) . . ? C7 C6 C5 106.64(11) . . ? N2 C7 C6 108.84(11) . . ? N2 C7 C8 113.22(10) . . ? C6 C7 C8 137.71(11) . . ? C7 C8 N3 107.99(9) . . ? N4 C11 C16 123.66(11) . . ? N4 C11 C12 123.55(11) . . ? C16 C11 C12 112.79(11) . . ? C13 C12 C11 124.35(12) . . ? C13 C12 Cl1 117.76(10) . . ? C11 C12 Cl1 117.88(9) . . ? C12 C13 C14 119.69(12) . . ? C15 C14 C13 119.11(12) . . ? C14 C15 C16 119.98(13) . . ? C15 C16 C11 124.03(12) . . ? C15 C16 Cl2 118.08(10) . . ? C11 C16 Cl2 117.87(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.758 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.046 data_ic105m _database_code_depnum_ccdc_archive 'CCDC 721353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Al N5 S2' _chemical_formula_weight 479.63 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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)/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 10.2678(3) _cell_length_b 21.9497(6) _cell_length_c 11.3213(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.428(2) _cell_angle_gamma 90.00 _cell_volume 2530.13(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.8963 _exptl_absorpt_correction_T_max 0.9586 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27469 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 29.01 _reflns_number_total 6650 _reflns_number_gt 4556 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0459P)^2^+0.1087P] 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 6650 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 1.01624(4) 0.22358(2) 0.29886(4) 0.01901(12) Uani 1 1 d . . . S1 S 1.24916(4) 0.19824(2) 0.38403(4) 0.02766(11) Uani 1 1 d . . . S2 S 1.01081(4) 0.170038(19) 0.10444(4) 0.02589(11) Uani 1 1 d . . . N1 N 0.83442(12) 0.24437(6) 0.27931(11) 0.0183(3) Uani 1 1 d . . . N2 N 0.95187(13) 0.14379(6) 0.37745(12) 0.0228(3) Uani 1 1 d . . . N3 N 0.71929(13) 0.40472(6) 0.21131(13) 0.0266(3) Uani 1 1 d . . . N4 N 1.07702(12) 0.27380(6) 0.44116(12) 0.0198(3) Uani 1 1 d . . . N5 N 1.08229(13) 0.27740(6) 0.17464(12) 0.0225(3) Uani 1 1 d . . . C1 C 1.02700(17) 0.08709(7) 0.36353(18) 0.0317(4) Uani 1 1 d . . . H1A H 0.9819 0.0525 0.3951 0.048 Uiso 1 1 calc R . . H1B H 1.1154 0.0910 0.4074 0.048 Uiso 1 1 calc R . . H1C H 1.0334 0.0803 0.2789 0.048 Uiso 1 1 calc R . . C2 C 0.94820(18) 0.15269(8) 0.50777(15) 0.0286(4) Uani 1 1 d . . . H2A H 0.9091 0.1167 0.5406 0.043 Uiso 1 1 calc R . . H2B H 0.8953 0.1887 0.5203 0.043 Uiso 1 1 calc R . . H2C H 1.0378 0.1584 0.5480 0.043 Uiso 1 1 calc R . . C3 C 0.81425(15) 0.13558(7) 0.31710(15) 0.0229(4) Uani 1 1 d . . . H3A H 0.8153 0.1154 0.2391 0.027 Uiso 1 1 calc R . . H3B H 0.7638 0.1097 0.3666 0.027 Uiso 1 1 calc R . . C4 C 0.75189(15) 0.19664(7) 0.30005(14) 0.0202(3) Uani 1 1 d . . . C5 C 0.62471(15) 0.21629(7) 0.29198(14) 0.0222(3) Uani 1 1 d . . . H5 H 0.5499 0.1924 0.3026 0.027 Uiso 1 1 calc R . . C6 C 0.62648(15) 0.27944(7) 0.26453(14) 0.0216(3) Uani 1 1 d . . . H6 H 0.5527 0.3059 0.2530 0.026 Uiso 1 1 calc R . . C7 C 0.75535(15) 0.29514(7) 0.25768(14) 0.0192(3) Uani 1 1 d . . . C8 C 0.81300(15) 0.35411(7) 0.22363(15) 0.0220(3) Uani 1 1 d . . . H8A H 0.8873 0.3649 0.2848 0.026 Uiso 1 1 calc R . . H8B H 0.8485 0.3486 0.1471 0.026 Uiso 1 1 calc R . . C9 C 0.6878(2) 0.42573(9) 0.32685(19) 0.0415(5) Uani 1 1 d . . . H9A H 0.7680 0.4402 0.3750 0.062 Uiso 1 1 calc R . . H9B H 0.6503 0.3920 0.3681 0.062 Uiso 1 1 calc R . . H9C H 0.6240 0.4591 0.3149 0.062 Uiso 1 1 calc R . . C10 C 0.77443(19) 0.45453(8) 0.14972(18) 0.0376(5) Uani 1 1 d . . . H10A H 0.8555 0.4687 0.1970 0.056 Uiso 1 1 calc R . . H10B H 0.7111 0.4881 0.1388 0.056 Uiso 1 1 calc R . . H10C H 0.7940 0.4404 0.0718 0.056 Uiso 1 1 calc R . . C11 C 1.19633(15) 0.25361(7) 0.47179(15) 0.0241(4) Uani 1 1 d . . . H11 H 1.2507 0.2690 0.5395 0.029 Uiso 1 1 calc R . . C12 C 1.03146(15) 0.32490(7) 0.50331(14) 0.0211(3) Uani 1 1 d . . . C13 C 1.11217(16) 0.37532(8) 0.52923(15) 0.0276(4) Uani 1 1 d . . . H13 H 1.1973 0.3760 0.5049 0.033 Uiso 1 1 calc R . . C14 C 1.06933(18) 0.42450(8) 0.59021(17) 0.0342(4) Uani 1 1 d . . . H14 H 1.1247 0.4589 0.6070 0.041 Uiso 1 1 calc R . . C15 C 0.94571(19) 0.42349(9) 0.62684(17) 0.0374(5) Uani 1 1 d . . . H15 H 0.9168 0.4568 0.6703 0.045 Uiso 1 1 calc R . . C16 C 0.86484(17) 0.37384(8) 0.59977(16) 0.0329(4) Uani 1 1 d . . . H16 H 0.7798 0.3734 0.6243 0.039 Uiso 1 1 calc R . . C17 C 0.90620(16) 0.32454(8) 0.53712(15) 0.0264(4) Uani 1 1 d . . . H17 H 0.8493 0.2909 0.5176 0.032 Uiso 1 1 calc R . . C18 C 1.06752(16) 0.24126(8) 0.08263(16) 0.0261(4) Uani 1 1 d . . . H18 H 1.0875 0.2541 0.0069 0.031 Uiso 1 1 calc R . . C19 C 1.13102(16) 0.33806(8) 0.16285(16) 0.0267(4) Uani 1 1 d . . . C20 C 1.08012(17) 0.37510(8) 0.06767(17) 0.0317(4) Uani 1 1 d . . . H20 H 1.0152 0.3598 0.0076 0.038 Uiso 1 1 calc R . . C21 C 1.1252(2) 0.43413(9) 0.0619(2) 0.0413(5) Uani 1 1 d . . . H21 H 1.0910 0.4594 -0.0030 0.050 Uiso 1 1 calc R . . C22 C 1.2189(2) 0.45703(9) 0.1487(2) 0.0480(6) Uani 1 1 d . . . H22 H 1.2476 0.4980 0.1444 0.058 Uiso 1 1 calc R . . C23 C 1.2706(2) 0.42042(10) 0.2413(2) 0.0493(6) Uani 1 1 d . . . H23 H 1.3359 0.4361 0.3007 0.059 Uiso 1 1 calc R . . C24 C 1.22786(18) 0.36026(9) 0.24898(17) 0.0357(4) Uani 1 1 d . . . H24 H 1.2647 0.3348 0.3125 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 Al1 0.0181(2) 0.0213(2) 0.0170(2) 0.0003(2) -0.00016(18) 0.00014(18) S1 0.0217(2) 0.0313(2) 0.0288(2) -0.00084(19) -0.00110(17) 0.00380(17) S2 0.0277(2) 0.0268(2) 0.0230(2) -0.00369(18) 0.00281(17) 0.00233(17) N1 0.0190(6) 0.0187(7) 0.0166(7) 0.0003(5) -0.0001(5) -0.0016(5) N2 0.0232(7) 0.0219(7) 0.0216(7) 0.0012(6) -0.0033(6) 0.0011(5) N3 0.0281(7) 0.0213(7) 0.0300(8) 0.0032(6) 0.0019(6) 0.0036(6) N4 0.0206(6) 0.0217(7) 0.0170(7) 0.0010(6) 0.0017(5) -0.0023(5) N5 0.0220(7) 0.0254(7) 0.0200(7) 0.0001(6) 0.0027(5) 0.0000(6) C1 0.0299(9) 0.0211(9) 0.0423(11) 0.0022(8) -0.0023(8) 0.0040(7) C2 0.0359(9) 0.0303(9) 0.0182(9) 0.0048(7) -0.0011(7) -0.0056(7) C3 0.0226(8) 0.0223(8) 0.0225(9) 0.0009(7) -0.0018(7) -0.0038(6) C4 0.0238(8) 0.0213(8) 0.0150(8) -0.0007(7) 0.0002(6) -0.0033(6) C5 0.0219(8) 0.0279(9) 0.0165(8) -0.0008(7) 0.0013(6) -0.0042(6) C6 0.0206(8) 0.0275(9) 0.0164(8) -0.0006(7) 0.0009(6) 0.0022(6) C7 0.0229(8) 0.0199(8) 0.0140(8) -0.0014(6) -0.0001(6) 0.0013(6) C8 0.0214(8) 0.0228(8) 0.0209(9) -0.0002(7) -0.0003(6) 0.0006(6) C9 0.0498(12) 0.0295(10) 0.0473(13) -0.0072(9) 0.0146(10) 0.0036(9) C10 0.0417(11) 0.0247(9) 0.0448(12) 0.0074(9) -0.0002(9) 0.0019(8) C11 0.0235(8) 0.0280(9) 0.0197(8) 0.0033(7) -0.0011(7) -0.0043(7) C12 0.0247(8) 0.0241(8) 0.0134(8) 0.0008(7) -0.0020(6) -0.0007(6) C13 0.0256(8) 0.0313(9) 0.0252(9) -0.0012(8) 0.0002(7) -0.0050(7) C14 0.0384(10) 0.0288(10) 0.0339(11) -0.0068(8) -0.0014(8) -0.0053(8) C15 0.0414(11) 0.0354(11) 0.0343(11) -0.0101(9) 0.0009(9) 0.0061(8) C16 0.0301(9) 0.0408(11) 0.0278(10) -0.0020(9) 0.0037(8) 0.0048(8) C17 0.0251(8) 0.0314(9) 0.0217(9) -0.0010(7) -0.0006(7) -0.0020(7) C18 0.0252(8) 0.0314(9) 0.0216(9) 0.0021(7) 0.0031(7) 0.0048(7) C19 0.0268(8) 0.0284(9) 0.0274(9) 0.0003(8) 0.0129(7) -0.0031(7) C20 0.0307(9) 0.0337(10) 0.0333(10) 0.0042(9) 0.0134(8) 0.0033(8) C21 0.0461(12) 0.0318(11) 0.0513(13) 0.0116(10) 0.0259(10) 0.0052(9) C22 0.0634(14) 0.0300(11) 0.0575(15) -0.0043(11) 0.0345(12) -0.0128(10) C23 0.0611(14) 0.0522(14) 0.0383(12) -0.0110(11) 0.0210(11) -0.0285(11) C24 0.0404(11) 0.0420(11) 0.0265(10) -0.0020(9) 0.0114(8) -0.0148(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 N1 1.9068(13) . ? Al1 N4 1.9850(14) . ? Al1 N5 2.0198(14) . ? Al1 N2 2.1090(14) . ? Al1 S2 2.4894(6) . ? Al1 S1 2.5224(6) . ? S1 C11 1.7023(17) . ? S2 C18 1.6974(17) . ? N1 C7 1.3819(19) . ? N1 C4 1.3863(19) . ? N2 C1 1.483(2) . ? N2 C2 1.494(2) . ? N2 C3 1.499(2) . ? N3 C10 1.451(2) . ? N3 C9 1.462(2) . ? N3 C8 1.464(2) . ? N4 C11 1.307(2) . ? N4 C12 1.434(2) . ? N5 C18 1.302(2) . ? N5 C19 1.435(2) . ? C3 C4 1.487(2) . ? C4 C5 1.367(2) . ? C5 C6 1.421(2) . ? C6 C7 1.379(2) . ? C7 C8 1.494(2) . ? C12 C17 1.388(2) . ? C12 C13 1.391(2) . ? C13 C14 1.383(2) . ? C14 C15 1.386(3) . ? C15 C16 1.380(3) . ? C16 C17 1.390(2) . ? C19 C24 1.388(3) . ? C19 C20 1.396(2) . ? C20 C21 1.380(3) . ? C21 C22 1.378(3) . ? C22 C23 1.373(3) . ? C23 C24 1.398(3) . ? 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 N1 Al1 N4 99.31(6) . . ? N1 Al1 N5 101.02(6) . . ? N4 Al1 N5 98.14(6) . . ? N1 Al1 N2 83.81(5) . . ? N4 Al1 N2 101.63(6) . . ? N5 Al1 N2 158.62(6) . . ? N1 Al1 S2 95.78(4) . . ? N4 Al1 S2 161.54(4) . . ? N5 Al1 S2 68.39(4) . . ? N2 Al1 S2 90.49(4) . . ? N1 Al1 S1 164.33(5) . . ? N4 Al1 S1 68.23(4) . . ? N5 Al1 S1 90.46(4) . . ? N2 Al1 S1 89.37(4) . . ? S2 Al1 S1 98.38(2) . . ? C11 S1 Al1 73.01(6) . . ? C18 S2 Al1 74.03(6) . . ? C7 N1 C4 106.35(12) . . ? C7 N1 Al1 139.24(11) . . ? C4 N1 Al1 114.22(10) . . ? C1 N2 C2 107.13(13) . . ? C1 N2 C3 108.86(12) . . ? C2 N2 C3 108.87(13) . . ? C1 N2 Al1 117.14(11) . . ? C2 N2 Al1 110.95(10) . . ? C3 N2 Al1 103.65(9) . . ? C10 N3 C9 109.72(14) . . ? C10 N3 C8 108.97(13) . . ? C9 N3 C8 111.88(14) . . ? C11 N4 C12 119.28(13) . . ? C11 N4 Al1 102.28(11) . . ? C12 N4 Al1 138.09(10) . . ? C18 N5 C19 119.79(14) . . ? C18 N5 Al1 100.71(11) . . ? C19 N5 Al1 139.47(11) . . ? C4 C3 N2 108.39(12) . . ? C5 C4 N1 110.48(14) . . ? C5 C4 C3 133.20(14) . . ? N1 C4 C3 116.14(13) . . ? C4 C5 C6 106.45(14) . . ? C7 C6 C5 107.19(14) . . ? C6 C7 N1 109.53(13) . . ? C6 C7 C8 130.23(14) . . ? N1 C7 C8 120.07(13) . . ? N3 C8 C7 113.84(13) . . ? N4 C11 S1 116.47(12) . . ? C17 C12 C13 119.61(15) . . ? C17 C12 N4 120.22(14) . . ? C13 C12 N4 120.17(14) . . ? C14 C13 C12 120.46(16) . . ? C13 C14 C15 119.97(17) . . ? C16 C15 C14 119.62(17) . . ? C15 C16 C17 120.88(17) . . ? C12 C17 C16 119.42(16) . . ? N5 C18 S2 116.83(13) . . ? C24 C19 C20 120.03(17) . . ? C24 C19 N5 119.16(16) . . ? C20 C19 N5 120.79(16) . . ? C21 C20 C19 119.27(19) . . ? C22 C21 C20 121.1(2) . . ? C23 C22 C21 119.78(19) . . ? C22 C23 C24 120.5(2) . . ? C19 C24 C23 119.36(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.01 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.484 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.056 data_ic137dm _database_code_depnum_ccdc_archive 'CCDC 721354' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Al N3 O2' _chemical_formula_weight 573.69 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 9.7181(3) _cell_length_b 11.9863(4) _cell_length_c 14.7312(5) _cell_angle_alpha 90.608(2) _cell_angle_beta 107.021(2) _cell_angle_gamma 104.025(2) _cell_volume 1585.71(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.9546 _exptl_absorpt_correction_T_max 0.9745 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30540 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 29.02 _reflns_number_total 8386 _reflns_number_gt 5408 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0465P)^2^+0.1172P] 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 8386 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1042 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.02559(5) 0.30421(4) 0.30183(3) 0.02075(11) Uani 1 1 d . . . N1 N 0.18262(14) 0.48299(11) 0.34456(8) 0.0252(3) Uani 1 1 d . . . N2 N -0.09806(14) 0.39455(11) 0.31408(9) 0.0259(3) Uani 1 1 d . . . N3 N -0.19388(13) 0.17550(10) 0.28885(8) 0.0230(3) Uani 1 1 d . . . O1 O 0.05148(11) 0.27659(8) 0.19375(6) 0.0239(2) Uani 1 1 d . . . O2 O 0.12937(11) 0.23910(8) 0.39083(7) 0.0228(2) Uani 1 1 d . . . C1 C 0.33403(19) 0.48710(15) 0.40586(13) 0.0395(4) Uani 1 1 d . . . H1A H 0.3818 0.4449 0.3722 0.059 Uiso 1 1 calc R . . H1B H 0.3286 0.4515 0.4647 0.059 Uiso 1 1 calc R . . H1C H 0.3924 0.5676 0.4215 0.059 Uiso 1 1 calc R . . C2 C 0.1930(2) 0.53772(14) 0.25593(11) 0.0354(4) Uani 1 1 d . . . H2A H 0.2553 0.6171 0.2724 0.053 Uiso 1 1 calc R . . H2B H 0.0931 0.5385 0.2158 0.053 Uiso 1 1 calc R . . H2C H 0.2374 0.4937 0.2212 0.053 Uiso 1 1 calc R . . C3 C 0.11085(19) 0.55080(14) 0.39391(11) 0.0324(4) Uani 1 1 d . . . H3A H 0.1436 0.6340 0.3859 0.039 Uiso 1 1 calc R . . H3B H 0.1390 0.5402 0.4629 0.039 Uiso 1 1 calc R . . C4 C -0.05414(19) 0.50752(13) 0.34994(11) 0.0297(4) Uani 1 1 d . . . C5 C -0.1792(2) 0.54519(15) 0.34231(13) 0.0403(4) Uani 1 1 d . . . H5 H -0.1814 0.6207 0.3609 0.048 Uiso 1 1 calc R . . C6 C -0.3042(2) 0.45105(15) 0.30179(13) 0.0384(4) Uani 1 1 d . . . H6 H -0.4059 0.4512 0.2884 0.046 Uiso 1 1 calc R . . C7 C -0.25042(17) 0.35980(14) 0.28557(11) 0.0280(3) Uani 1 1 d . . . C8 C -0.31109(17) 0.23663(13) 0.24571(11) 0.0279(3) Uani 1 1 d . . . H8A H -0.4032 0.2017 0.2620 0.034 Uiso 1 1 calc R . . H8B H -0.3347 0.2312 0.1755 0.034 Uiso 1 1 calc R . . C9 C -0.19317(18) 0.15334(14) 0.38792(11) 0.0311(4) Uani 1 1 d . . . H9A H -0.2885 0.1012 0.3869 0.047 Uiso 1 1 calc R . . H9B H -0.1784 0.2264 0.4243 0.047 Uiso 1 1 calc R . . H9C H -0.1121 0.1178 0.4179 0.047 Uiso 1 1 calc R . . C10 C -0.22754(18) 0.06247(13) 0.23465(11) 0.0293(4) Uani 1 1 d . . . H10A H -0.1468 0.0252 0.2609 0.044 Uiso 1 1 calc R . . H10B H -0.2369 0.0740 0.1676 0.044 Uiso 1 1 calc R . . H10C H -0.3212 0.0133 0.2396 0.044 Uiso 1 1 calc R . . C11 C -0.00263(17) 0.30605(13) 0.10043(10) 0.0243(3) Uani 1 1 d . . . H11 H -0.0418 0.3754 0.1032 0.029 Uiso 1 1 calc R . . C12 C -0.12928(17) 0.20825(14) 0.04049(10) 0.0264(3) Uani 1 1 d . . . C13 C -0.26622(19) 0.22636(17) -0.00869(11) 0.0379(4) Uani 1 1 d . . . H13 H -0.2809 0.3018 -0.0071 0.045 Uiso 1 1 calc R . . C14 C -0.11053(19) 0.09702(14) 0.03631(11) 0.0316(4) Uani 1 1 d . . . H14 H -0.0170 0.0834 0.0690 0.038 Uiso 1 1 calc R . . C15 C -0.3826(2) 0.1347(2) -0.06054(13) 0.0502(5) Uani 1 1 d . . . H15 H -0.4759 0.1478 -0.0943 0.060 Uiso 1 1 calc R . . C16 C -0.2265(2) 0.00594(16) -0.01485(12) 0.0423(5) Uani 1 1 d . . . H16 H -0.2125 -0.0697 -0.0169 0.051 Uiso 1 1 calc R . . C17 C -0.3623(2) 0.0253(2) -0.06282(13) 0.0515(6) Uani 1 1 d . . . H17 H -0.4422 -0.0372 -0.0976 0.062 Uiso 1 1 calc R . . C18 C 0.12123(17) 0.33626(12) 0.05365(10) 0.0247(3) Uani 1 1 d . . . C19 C 0.09482(19) 0.38543(14) -0.03299(11) 0.0332(4) Uani 1 1 d . . . H19 H 0.0011 0.4015 -0.0610 0.040 Uiso 1 1 calc R . . C20 C 0.25848(19) 0.31381(15) 0.09346(12) 0.0341(4) Uani 1 1 d . . . H20 H 0.2792 0.2812 0.1529 0.041 Uiso 1 1 calc R . . C21 C 0.2028(2) 0.41140(15) -0.07909(12) 0.0395(4) Uani 1 1 d . . . H21 H 0.1835 0.4458 -0.1378 0.047 Uiso 1 1 calc R . . C22 C 0.3660(2) 0.33874(16) 0.04673(13) 0.0431(4) Uani 1 1 d . . . H22 H 0.4596 0.3224 0.0743 0.052 Uiso 1 1 calc R . . C23 C 0.3385(2) 0.38705(16) -0.03932(13) 0.0428(5) Uani 1 1 d . . . H23 H 0.4125 0.4034 -0.0710 0.051 Uiso 1 1 calc R . . C24 C 0.24095(16) 0.18398(12) 0.38658(10) 0.0209(3) Uani 1 1 d . . . H24 H 0.2968 0.2257 0.3445 0.025 Uiso 1 1 calc R . . C25 C 0.17069(15) 0.05948(12) 0.34479(10) 0.0202(3) Uani 1 1 d . . . C26 C 0.09896(16) -0.01918(13) 0.39635(10) 0.0242(3) Uani 1 1 d . . . H26 H 0.0980 0.0053 0.4576 0.029 Uiso 1 1 calc R . . C27 C 0.17114(17) 0.02104(13) 0.25582(10) 0.0264(3) Uani 1 1 d . . . H27 H 0.2200 0.0729 0.2199 0.032 Uiso 1 1 calc R . . C28 C 0.02998(17) -0.13135(14) 0.35938(11) 0.0299(4) Uani 1 1 d . . . H28 H -0.0180 -0.1837 0.3954 0.036 Uiso 1 1 calc R . . C29 C 0.10100(19) -0.09235(14) 0.21848(11) 0.0335(4) Uani 1 1 d . . . H29 H 0.1020 -0.1174 0.1573 0.040 Uiso 1 1 calc R . . C30 C 0.02987(19) -0.16876(14) 0.26996(11) 0.0327(4) Uani 1 1 d . . . H30 H -0.0187 -0.2462 0.2444 0.039 Uiso 1 1 calc R . . C31 C 0.34966(16) 0.18750(12) 0.48561(10) 0.0211(3) Uani 1 1 d . . . C32 C 0.31853(17) 0.21921(14) 0.56633(11) 0.0283(4) Uani 1 1 d . . . H32 H 0.2322 0.2461 0.5599 0.034 Uiso 1 1 calc R . . C33 C 0.47809(18) 0.15094(14) 0.49713(11) 0.0323(4) Uani 1 1 d . . . H33 H 0.5027 0.1303 0.4425 0.039 Uiso 1 1 calc R . . C34 C 0.41111(19) 0.21241(15) 0.65658(11) 0.0353(4) Uani 1 1 d . . . H34 H 0.3878 0.2345 0.7113 0.042 Uiso 1 1 calc R . . C35 C 0.57117(19) 0.14407(15) 0.58730(13) 0.0388(4) Uani 1 1 d . . . H35 H 0.6588 0.1188 0.5940 0.047 Uiso 1 1 calc R . . C36 C 0.53693(19) 0.17372(14) 0.66710(12) 0.0355(4) Uani 1 1 d . . . H36 H 0.5995 0.1676 0.7289 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 Al1 0.0232(2) 0.0199(2) 0.0192(2) 0.00159(17) 0.00412(18) 0.00854(19) N1 0.0261(7) 0.0218(7) 0.0244(6) 0.0015(5) 0.0030(5) 0.0059(6) N2 0.0255(7) 0.0204(7) 0.0313(7) -0.0001(5) 0.0056(6) 0.0085(6) N3 0.0229(7) 0.0226(7) 0.0236(6) 0.0031(5) 0.0057(5) 0.0075(5) O1 0.0278(6) 0.0241(6) 0.0189(5) 0.0016(4) 0.0050(4) 0.0074(5) O2 0.0255(6) 0.0231(6) 0.0230(5) 0.0038(4) 0.0069(4) 0.0128(5) C1 0.0294(10) 0.0302(10) 0.0474(10) 0.0010(8) -0.0016(8) 0.0029(8) C2 0.0432(10) 0.0256(9) 0.0315(9) 0.0027(7) 0.0109(8) -0.0013(8) C3 0.0426(10) 0.0205(9) 0.0306(8) -0.0037(6) 0.0077(8) 0.0063(8) C4 0.0374(10) 0.0206(8) 0.0336(8) 0.0012(6) 0.0123(7) 0.0101(7) C5 0.0485(11) 0.0281(10) 0.0542(11) 0.0002(8) 0.0230(9) 0.0192(9) C6 0.0327(10) 0.0375(11) 0.0535(11) 0.0064(8) 0.0187(9) 0.0180(9) C7 0.0246(9) 0.0306(9) 0.0307(8) 0.0049(7) 0.0083(7) 0.0106(7) C8 0.0213(8) 0.0313(9) 0.0310(8) 0.0047(7) 0.0063(7) 0.0080(7) C9 0.0323(9) 0.0354(10) 0.0275(8) 0.0078(7) 0.0129(7) 0.0074(8) C10 0.0280(9) 0.0229(9) 0.0340(8) 0.0000(6) 0.0089(7) 0.0020(7) C11 0.0274(8) 0.0235(8) 0.0217(7) 0.0028(6) 0.0059(6) 0.0082(7) C12 0.0277(9) 0.0308(9) 0.0192(7) 0.0015(6) 0.0092(6) 0.0025(7) C13 0.0309(10) 0.0496(12) 0.0304(9) 0.0043(8) 0.0059(7) 0.0093(9) C14 0.0338(10) 0.0316(9) 0.0278(8) -0.0026(7) 0.0123(7) 0.0020(8) C15 0.0271(10) 0.0760(16) 0.0365(10) -0.0022(10) 0.0025(8) 0.0018(10) C16 0.0480(12) 0.0356(11) 0.0388(10) -0.0106(8) 0.0214(9) -0.0067(9) C17 0.0373(12) 0.0643(15) 0.0373(10) -0.0167(9) 0.0125(9) -0.0163(10) C18 0.0289(9) 0.0186(8) 0.0224(7) -0.0014(6) 0.0053(6) 0.0016(7) C19 0.0342(10) 0.0353(10) 0.0256(8) 0.0050(7) 0.0061(7) 0.0040(8) C20 0.0319(10) 0.0354(10) 0.0352(9) 0.0080(7) 0.0108(8) 0.0083(8) C21 0.0448(11) 0.0393(11) 0.0257(8) 0.0032(7) 0.0106(8) -0.0051(9) C22 0.0325(10) 0.0493(12) 0.0497(11) 0.0073(9) 0.0172(9) 0.0090(9) C23 0.0412(11) 0.0425(11) 0.0419(10) -0.0033(8) 0.0222(9) -0.0058(9) C24 0.0231(8) 0.0208(8) 0.0224(7) 0.0043(6) 0.0091(6) 0.0095(6) C25 0.0186(7) 0.0197(8) 0.0230(7) 0.0028(6) 0.0042(6) 0.0085(6) C26 0.0274(8) 0.0240(8) 0.0239(7) 0.0022(6) 0.0098(6) 0.0092(7) C27 0.0328(9) 0.0260(9) 0.0231(7) 0.0050(6) 0.0095(7) 0.0110(7) C28 0.0270(9) 0.0259(9) 0.0361(9) 0.0064(7) 0.0095(7) 0.0055(7) C29 0.0450(11) 0.0304(10) 0.0251(8) -0.0019(7) 0.0085(7) 0.0127(8) C30 0.0349(10) 0.0215(9) 0.0354(9) -0.0028(7) 0.0025(7) 0.0059(7) C31 0.0204(8) 0.0168(8) 0.0251(7) 0.0012(6) 0.0052(6) 0.0048(6) C32 0.0246(8) 0.0343(9) 0.0276(8) 0.0027(7) 0.0064(7) 0.0124(7) C33 0.0259(9) 0.0357(10) 0.0350(9) -0.0066(7) 0.0054(7) 0.0125(8) C34 0.0389(10) 0.0394(10) 0.0240(8) 0.0008(7) 0.0055(7) 0.0086(8) C35 0.0263(9) 0.0345(10) 0.0492(11) -0.0032(8) -0.0022(8) 0.0133(8) C36 0.0312(10) 0.0268(9) 0.0351(9) 0.0046(7) -0.0070(7) 0.0034(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 Al1 O1 1.7239(10) . ? Al1 O2 1.7246(10) . ? Al1 N2 1.8446(12) . ? Al1 N3 2.2640(13) . ? Al1 N1 2.2674(13) . ? N1 C1 1.473(2) . ? N1 C2 1.4862(19) . ? N1 C3 1.4948(19) . ? N2 C4 1.3665(19) . ? N2 C7 1.370(2) . ? N3 C10 1.4796(19) . ? N3 C9 1.4844(18) . ? N3 C8 1.4929(18) . ? O1 C11 1.4028(16) . ? O2 C24 1.4150(16) . ? C3 C4 1.497(2) . ? C4 C5 1.371(2) . ? C5 C6 1.415(3) . ? C6 C7 1.368(2) . ? C7 C8 1.493(2) . ? C11 C12 1.520(2) . ? C11 C18 1.528(2) . ? C12 C13 1.386(2) . ? C12 C14 1.392(2) . ? C13 C15 1.394(3) . ? C14 C16 1.385(2) . ? C15 C17 1.373(3) . ? C16 C17 1.379(3) . ? C18 C20 1.384(2) . ? C18 C19 1.393(2) . ? C19 C21 1.386(2) . ? C20 C22 1.389(2) . ? C21 C23 1.381(3) . ? C22 C23 1.380(2) . ? C24 C25 1.521(2) . ? C24 C31 1.5235(19) . ? C25 C27 1.3863(19) . ? C25 C26 1.399(2) . ? C26 C28 1.374(2) . ? C27 C29 1.389(2) . ? C28 C30 1.387(2) . ? C29 C30 1.381(2) . ? C31 C32 1.381(2) . ? C31 C33 1.386(2) . ? C32 C34 1.386(2) . ? C33 C35 1.387(2) . ? C34 C36 1.378(2) . ? C35 C36 1.377(2) . ? 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 111.34(5) . . ? O1 Al1 N2 121.58(5) . . ? O2 Al1 N2 127.08(5) . . ? O1 Al1 N3 101.90(5) . . ? O2 Al1 N3 94.84(5) . . ? N2 Al1 N3 75.88(5) . . ? O1 Al1 N1 99.31(5) . . ? O2 Al1 N1 94.98(5) . . ? N2 Al1 N1 76.82(5) . . ? N3 Al1 N1 151.47(5) . . ? C1 N1 C2 108.74(13) . . ? C1 N1 C3 109.87(12) . . ? C2 N1 C3 107.75(12) . . ? C1 N1 Al1 115.58(10) . . ? C2 N1 Al1 107.85(9) . . ? C3 N1 Al1 106.78(9) . . ? C4 N2 C7 108.67(13) . . ? C4 N2 Al1 126.11(11) . . ? C7 N2 Al1 125.18(10) . . ? C10 N3 C9 107.66(12) . . ? C10 N3 C8 110.08(12) . . ? C9 N3 C8 109.22(11) . . ? C10 N3 Al1 118.25(9) . . ? C9 N3 Al1 105.82(9) . . ? C8 N3 Al1 105.51(9) . . ? C11 O1 Al1 135.78(9) . . ? C24 O2 Al1 128.07(8) . . ? N1 C3 C4 107.49(12) . . ? N2 C4 C5 108.24(15) . . ? N2 C4 C3 113.27(13) . . ? C5 C4 C3 138.14(15) . . ? C4 C5 C6 107.53(15) . . ? C7 C6 C5 106.77(15) . . ? C6 C7 N2 108.78(15) . . ? C6 C7 C8 137.91(15) . . ? N2 C7 C8 113.31(13) . . ? N3 C8 C7 106.98(12) . . ? O1 C11 C12 110.82(12) . . ? O1 C11 C18 111.10(12) . . ? C12 C11 C18 109.88(11) . . ? C13 C12 C14 118.55(16) . . ? C13 C12 C11 121.40(15) . . ? C14 C12 C11 120.02(14) . . ? C12 C13 C15 120.48(18) . . ? C16 C14 C12 120.86(17) . . ? C17 C15 C13 120.07(18) . . ? C17 C16 C14 119.84(18) . . ? C15 C17 C16 120.19(18) . . ? C20 C18 C19 118.56(15) . . ? C20 C18 C11 122.10(13) . . ? C19 C18 C11 119.31(14) . . ? C21 C19 C18 121.19(16) . . ? C18 C20 C22 120.20(16) . . ? C23 C21 C19 119.70(16) . . ? C23 C22 C20 120.78(17) . . ? C22 C23 C21 119.56(16) . . ? O2 C24 C25 110.24(11) . . ? O2 C24 C31 110.38(11) . . ? C25 C24 C31 109.88(11) . . ? C27 C25 C26 118.27(13) . . ? C27 C25 C24 122.47(13) . . ? C26 C25 C24 119.24(12) . . ? C28 C26 C25 120.79(13) . . ? C25 C27 C29 120.84(14) . . ? C26 C28 C30 120.53(15) . . ? C30 C29 C27 120.22(14) . . ? C29 C30 C28 119.35(15) . . ? C32 C31 C33 118.19(13) . . ? C32 C31 C24 121.28(13) . . ? C33 C31 C24 120.39(13) . . ? C31 C32 C34 121.11(14) . . ? C31 C33 C35 120.90(15) . . ? C36 C34 C32 120.15(15) . . ? C36 C35 C33 120.20(15) . . ? C35 C36 C34 119.43(15) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.268 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.048 data_sn236m _database_code_depnum_ccdc_archive 'CCDC 721355' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H48 Al N3 O2' _chemical_formula_weight 545.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.7168(3) _cell_length_b 17.7020(6) _cell_length_c 20.9094(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.726(2) _cell_angle_gamma 90.00 _cell_volume 3204.22(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.9675 _exptl_absorpt_correction_T_max 0.9877 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36733 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 29.05 _reflns_number_total 8521 _reflns_number_gt 5310 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0512P)^2^+0.5244P] 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 8521 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.004 _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 0.13307(5) 0.72636(3) 0.04270(2) 0.02184(12) Uani 1 1 d . . . O1 O 0.00637(12) 0.79884(6) 0.04412(5) 0.0292(3) Uani 1 1 d . . . O2 O 0.18048(13) 0.69501(7) -0.03038(5) 0.0322(3) Uani 1 1 d . . . N1 N 0.21698(15) 0.67124(8) 0.11222(6) 0.0280(3) Uani 1 1 d . . . N2 N -0.03835(15) 0.63651(7) 0.04845(6) 0.0283(3) Uani 1 1 d . . . N3 N 0.34023(15) 0.79189(8) 0.07562(6) 0.0277(3) Uani 1 1 d . . . C1 C 0.33886(19) 0.69299(10) 0.15504(7) 0.0320(4) Uani 1 1 d . . . C2 C 0.3798(2) 0.63302(12) 0.19534(8) 0.0441(5) Uani 1 1 d . . . H2 H 0.4612 0.6321 0.2298 0.053 Uiso 1 1 calc R . . C3 C 0.2770(2) 0.57235(11) 0.17561(9) 0.0446(5) Uani 1 1 d . . . H3 H 0.2765 0.5235 0.1944 0.054 Uiso 1 1 calc R . . C4 C 0.17888(19) 0.59850(10) 0.12410(8) 0.0318(4) Uani 1 1 d . . . C5 C 0.0535(2) 0.56915(9) 0.07503(8) 0.0339(4) Uani 1 1 d . . . H5A H -0.0137 0.5335 0.0953 0.041 Uiso 1 1 calc R . . H5B H 0.0989 0.5424 0.0401 0.041 Uiso 1 1 calc R . . C6 C 0.38088(19) 0.77372(10) 0.14582(7) 0.0337(4) Uani 1 1 d . . . H6A H 0.4927 0.7815 0.1586 0.040 Uiso 1 1 calc R . . H6B H 0.3228 0.8069 0.1725 0.040 Uiso 1 1 calc R . . C7 C -0.14466(19) 0.65932(10) 0.09508(8) 0.0364(4) Uani 1 1 d . . . H7A H -0.1994 0.7055 0.0799 0.055 Uiso 1 1 calc R . . H7B H -0.0855 0.6688 0.1371 0.055 Uiso 1 1 calc R . . H7C H -0.2196 0.6189 0.0991 0.055 Uiso 1 1 calc R . . C8 C -0.1295(2) 0.61767(11) -0.01330(8) 0.0402(4) Uani 1 1 d . . . H8A H -0.2020 0.5769 -0.0067 0.060 Uiso 1 1 calc R . . H8B H -0.0600 0.6012 -0.0442 0.060 Uiso 1 1 calc R . . H8C H -0.1871 0.6624 -0.0301 0.060 Uiso 1 1 calc R . . C9 C 0.47022(19) 0.76592(11) 0.04115(8) 0.0367(4) Uani 1 1 d . . . H9A H 0.5639 0.7941 0.0568 0.055 Uiso 1 1 calc R . . H9B H 0.4448 0.7747 -0.0052 0.055 Uiso 1 1 calc R . . H9C H 0.4877 0.7119 0.0490 0.055 Uiso 1 1 calc R . . C10 C 0.3203(2) 0.87437(10) 0.06675(9) 0.0394(4) Uani 1 1 d . . . H10A H 0.4137 0.9004 0.0860 0.059 Uiso 1 1 calc R . . H10B H 0.2315 0.8913 0.0877 0.059 Uiso 1 1 calc R . . H10C H 0.3026 0.8860 0.0206 0.059 Uiso 1 1 calc R . . C11 C 0.20147(18) 0.70892(10) -0.09190(7) 0.0289(4) Uani 1 1 d . . . C12 C 0.2335(2) 0.77596(11) -0.11470(8) 0.0421(5) Uani 1 1 d . . . H12A H 0.2432 0.8186 -0.0869 0.050 Uiso 1 1 calc R . . H12B H 0.2469 0.7816 -0.1589 0.050 Uiso 1 1 calc R . . C13 C 0.18442(19) 0.63970(10) -0.13361(7) 0.0303(4) Uani 1 1 d . . . C14 C 0.0493(2) 0.62965(11) -0.17633(7) 0.0371(4) Uani 1 1 d . . . C15 C 0.0344(2) 0.56531(12) -0.21471(8) 0.0437(5) Uani 1 1 d . . . H15 H -0.0571 0.5587 -0.2436 0.052 Uiso 1 1 calc R . . C16 C 0.1483(3) 0.51067(11) -0.21217(8) 0.0454(5) Uani 1 1 d . . . C17 C 0.2812(2) 0.52157(11) -0.16968(8) 0.0415(5) Uani 1 1 d . . . H17 H 0.3607 0.4847 -0.1675 0.050 Uiso 1 1 calc R . . C18 C 0.3013(2) 0.58508(10) -0.13010(8) 0.0353(4) Uani 1 1 d . . . C19 C 0.4477(2) 0.59501(12) -0.08516(10) 0.0503(5) Uani 1 1 d . . . H19A H 0.5195 0.5539 -0.0918 0.075 Uiso 1 1 calc R . . H19B H 0.4238 0.5940 -0.0405 0.075 Uiso 1 1 calc R . . H19C H 0.4953 0.6435 -0.0938 0.075 Uiso 1 1 calc R . . C20 C -0.0796(2) 0.68701(13) -0.18050(9) 0.0541(6) Uani 1 1 d . . . H20A H -0.0518 0.7307 -0.2055 0.081 Uiso 1 1 calc R . . H20B H -0.0959 0.7034 -0.1370 0.081 Uiso 1 1 calc R . . H20C H -0.1747 0.6642 -0.2017 0.081 Uiso 1 1 calc R . . C21 C 0.1269(3) 0.44038(12) -0.25393(9) 0.0658(7) Uani 1 1 d . . . H21A H 0.2229 0.4110 -0.2494 0.099 Uiso 1 1 calc R . . H21B H 0.1011 0.4552 -0.2991 0.099 Uiso 1 1 calc R . . H21C H 0.0431 0.4096 -0.2403 0.099 Uiso 1 1 calc R . . C22 C -0.09824(16) 0.85275(8) 0.05265(7) 0.0234(3) Uani 1 1 d . . . C23 C -0.12393(17) 0.87508(9) 0.11517(7) 0.0252(3) Uani 1 1 d . . . C24 C -0.23026(18) 0.93268(10) 0.12159(8) 0.0315(4) Uani 1 1 d . . . H24 H -0.2490 0.9481 0.1635 0.038 Uiso 1 1 calc R . . C25 C -0.30892(19) 0.96779(10) 0.06870(8) 0.0351(4) Uani 1 1 d . . . H25 H -0.3789 1.0078 0.0741 0.042 Uiso 1 1 calc R . . C26 C -0.28439(18) 0.94395(10) 0.00781(8) 0.0323(4) Uani 1 1 d . . . H26 H -0.3399 0.9676 -0.0286 0.039 Uiso 1 1 calc R . . C27 C -0.18111(17) 0.88654(9) -0.00183(7) 0.0258(3) Uani 1 1 d . . . C28 C -0.03824(19) 0.84049(10) 0.17563(7) 0.0308(4) Uani 1 1 d . . . H28 H 0.0345 0.8014 0.1622 0.037 Uiso 1 1 calc R . . C29 C 0.0570(2) 0.90037(12) 0.21580(8) 0.0434(5) Uani 1 1 d . . . H29A H 0.1342 0.9218 0.1905 0.065 Uiso 1 1 calc R . . H29B H 0.1092 0.8770 0.2549 0.065 Uiso 1 1 calc R . . H29C H -0.0116 0.9406 0.2277 0.065 Uiso 1 1 calc R . . C30 C -0.1490(2) 0.80177(11) 0.21734(8) 0.0414(5) Uani 1 1 d . . . H30A H -0.2173 0.8397 0.2332 0.062 Uiso 1 1 calc R . . H30B H -0.0892 0.7768 0.2540 0.062 Uiso 1 1 calc R . . H30C H -0.2111 0.7641 0.1915 0.062 Uiso 1 1 calc R . . C31 C -0.15604(19) 0.86255(10) -0.06947(7) 0.0322(4) Uani 1 1 d . . . H31 H -0.0844 0.8182 -0.0655 0.039 Uiso 1 1 calc R . . C32 C -0.0778(4) 0.92504(14) -0.10332(12) 0.0808(9) Uani 1 1 d . . . H32A H -0.1466 0.9689 -0.1091 0.121 Uiso 1 1 calc R . . H32B H -0.0547 0.9071 -0.1455 0.121 Uiso 1 1 calc R . . H32C H 0.0185 0.9395 -0.0772 0.121 Uiso 1 1 calc R . . C33 C -0.3058(3) 0.83719(16) -0.10861(10) 0.0713(8) Uani 1 1 d . . . H33A H -0.3501 0.7949 -0.0867 0.107 Uiso 1 1 calc R . . H33B H -0.2843 0.8211 -0.1515 0.107 Uiso 1 1 calc R . . H33C H -0.3793 0.8793 -0.1127 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0216(2) 0.0251(3) 0.0186(2) 0.00076(18) 0.00121(17) 0.00275(19) O1 0.0284(6) 0.0311(7) 0.0284(6) 0.0028(5) 0.0042(5) 0.0092(5) O2 0.0346(7) 0.0396(7) 0.0235(5) -0.0049(5) 0.0075(5) -0.0013(5) N1 0.0290(7) 0.0278(8) 0.0261(6) 0.0027(6) -0.0012(6) 0.0030(6) N2 0.0279(7) 0.0286(8) 0.0280(6) 0.0008(6) 0.0015(6) -0.0002(6) N3 0.0248(7) 0.0288(8) 0.0291(7) -0.0007(6) 0.0014(5) 0.0004(6) C1 0.0288(9) 0.0414(11) 0.0247(8) 0.0020(7) -0.0017(7) 0.0072(8) C2 0.0376(10) 0.0585(14) 0.0334(9) 0.0137(9) -0.0077(8) 0.0096(9) C3 0.0473(11) 0.0427(12) 0.0431(10) 0.0199(9) 0.0027(9) 0.0088(9) C4 0.0338(9) 0.0297(10) 0.0328(8) 0.0072(7) 0.0070(7) 0.0056(7) C5 0.0398(10) 0.0233(9) 0.0392(9) 0.0049(7) 0.0076(8) 0.0009(7) C6 0.0268(9) 0.0442(11) 0.0283(8) -0.0049(8) -0.0051(7) 0.0019(8) C7 0.0307(9) 0.0386(11) 0.0419(9) 0.0060(8) 0.0125(8) -0.0009(8) C8 0.0387(10) 0.0385(11) 0.0411(10) -0.0004(8) -0.0048(8) -0.0086(8) C9 0.0228(9) 0.0493(12) 0.0383(9) -0.0009(8) 0.0052(7) -0.0019(8) C10 0.0382(10) 0.0301(10) 0.0486(10) -0.0012(8) 0.0003(8) -0.0049(8) C11 0.0268(8) 0.0383(10) 0.0214(7) -0.0036(7) 0.0025(6) 0.0026(7) C12 0.0580(13) 0.0389(11) 0.0298(9) -0.0013(8) 0.0070(8) 0.0000(9) C13 0.0338(9) 0.0388(10) 0.0194(7) -0.0008(7) 0.0074(6) -0.0072(8) C14 0.0432(10) 0.0469(12) 0.0216(8) -0.0002(8) 0.0049(7) -0.0104(9) C15 0.0513(12) 0.0555(14) 0.0242(8) -0.0028(8) 0.0037(8) -0.0213(10) C16 0.0716(14) 0.0413(12) 0.0262(8) -0.0055(8) 0.0185(9) -0.0251(10) C17 0.0573(12) 0.0331(11) 0.0378(9) -0.0021(8) 0.0207(9) -0.0048(9) C18 0.0403(10) 0.0371(11) 0.0303(8) -0.0040(8) 0.0112(7) -0.0050(8) C19 0.0410(11) 0.0498(13) 0.0592(12) -0.0122(10) 0.0022(9) 0.0082(10) C20 0.0455(12) 0.0754(16) 0.0376(10) -0.0037(10) -0.0107(9) 0.0018(11) C21 0.114(2) 0.0471(14) 0.0390(11) -0.0131(10) 0.0207(12) -0.0339(13) C22 0.0181(7) 0.0207(8) 0.0313(8) 0.0020(6) 0.0029(6) -0.0002(6) C23 0.0205(8) 0.0267(9) 0.0282(8) 0.0009(6) 0.0015(6) -0.0002(6) C24 0.0262(8) 0.0324(10) 0.0362(9) -0.0041(7) 0.0046(7) 0.0026(7) C25 0.0268(9) 0.0301(10) 0.0479(10) -0.0004(8) 0.0025(8) 0.0073(7) C26 0.0241(8) 0.0319(10) 0.0393(9) 0.0083(7) -0.0035(7) 0.0039(7) C27 0.0212(8) 0.0253(9) 0.0302(8) 0.0038(7) 0.0002(6) -0.0028(6) C28 0.0300(9) 0.0372(10) 0.0254(8) 0.0003(7) 0.0033(7) 0.0074(7) C29 0.0386(10) 0.0552(13) 0.0337(9) -0.0091(9) -0.0067(8) 0.0057(9) C30 0.0464(11) 0.0473(12) 0.0325(9) 0.0066(8) 0.0124(8) 0.0098(9) C31 0.0312(9) 0.0371(10) 0.0276(8) 0.0056(7) 0.0001(7) 0.0019(7) C32 0.130(2) 0.0574(16) 0.0662(15) 0.0051(12) 0.0598(16) -0.0136(15) C33 0.0446(13) 0.118(2) 0.0471(12) -0.0260(13) -0.0113(10) 0.0095(13) _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 1.6954(11) . ? Al1 O2 1.7209(11) . ? Al1 N1 1.8306(13) . ? Al1 N3 2.1884(14) . ? Al1 N2 2.1952(14) . ? O1 C22 1.3461(17) . ? O2 C11 1.3432(18) . ? N1 C4 1.360(2) . ? N1 C1 1.362(2) . ? N2 C8 1.473(2) . ? N2 C7 1.478(2) . ? N2 C5 1.506(2) . ? N3 C10 1.479(2) . ? N3 C9 1.485(2) . ? N3 C6 1.504(2) . ? C1 C2 1.376(2) . ? C1 C6 1.493(2) . ? C2 C3 1.429(3) . ? C3 C4 1.375(2) . ? C4 C5 1.501(2) . ? C11 C12 1.321(2) . ? C11 C13 1.501(2) . ? C13 C18 1.400(2) . ? C13 C14 1.404(2) . ? C14 C15 1.390(3) . ? C14 C20 1.509(3) . ? C15 C16 1.383(3) . ? C16 C17 1.388(3) . ? C16 C21 1.519(3) . ? C17 C18 1.395(2) . ? C18 C19 1.504(3) . ? C22 C23 1.408(2) . ? C22 C27 1.409(2) . ? C23 C24 1.395(2) . ? C23 C28 1.520(2) . ? C24 C25 1.379(2) . ? C25 C26 1.381(2) . ? C26 C27 1.388(2) . ? C27 C31 1.517(2) . ? C28 C29 1.534(2) . ? C28 C30 1.536(2) . ? C31 C32 1.518(3) . ? C31 C33 1.525(3) . ? 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 118.97(6) . . ? O1 Al1 N1 126.15(6) . . ? O2 Al1 N1 114.71(6) . . ? O1 Al1 N3 96.23(6) . . ? O2 Al1 N3 100.08(5) . . ? N1 Al1 N3 78.14(6) . . ? O1 Al1 N2 95.65(6) . . ? O2 Al1 N2 92.91(5) . . ? N1 Al1 N2 77.38(6) . . ? N3 Al1 N2 155.32(5) . . ? C22 O1 Al1 172.56(10) . . ? C11 O2 Al1 149.90(11) . . ? C4 N1 C1 109.63(13) . . ? C4 N1 Al1 124.49(11) . . ? C1 N1 Al1 125.42(12) . . ? C8 N2 C7 108.95(13) . . ? C8 N2 C5 110.68(13) . . ? C7 N2 C5 108.69(12) . . ? C8 N2 Al1 114.63(10) . . ? C7 N2 Al1 108.76(10) . . ? C5 N2 Al1 104.95(10) . . ? C10 N3 C9 109.24(13) . . ? C10 N3 C6 110.13(13) . . ? C9 N3 C6 107.55(13) . . ? C10 N3 Al1 113.78(10) . . ? C9 N3 Al1 109.37(10) . . ? C6 N3 Al1 106.56(10) . . ? N1 C1 C2 108.11(16) . . ? N1 C1 C6 111.71(13) . . ? C2 C1 C6 140.10(16) . . ? C1 C2 C3 107.09(16) . . ? C4 C3 C2 106.56(16) . . ? N1 C4 C3 108.60(16) . . ? N1 C4 C5 112.12(13) . . ? C3 C4 C5 139.04(17) . . ? C4 C5 N2 106.94(13) . . ? C1 C6 N3 107.30(13) . . ? C12 C11 O2 124.65(15) . . ? C12 C11 C13 122.30(14) . . ? O2 C11 C13 113.05(14) . . ? C18 C13 C14 119.80(16) . . ? C18 C13 C11 120.75(15) . . ? C14 C13 C11 119.45(16) . . ? C15 C14 C13 119.06(18) . . ? C15 C14 C20 119.95(17) . . ? C13 C14 C20 120.99(16) . . ? C16 C15 C14 122.18(18) . . ? C15 C16 C17 117.97(17) . . ? C15 C16 C21 120.8(2) . . ? C17 C16 C21 121.2(2) . . ? C16 C17 C18 121.95(19) . . ? C17 C18 C13 119.03(17) . . ? C17 C18 C19 120.23(17) . . ? C13 C18 C19 120.73(16) . . ? O1 C22 C23 120.37(13) . . ? O1 C22 C27 119.02(13) . . ? C23 C22 C27 120.60(14) . . ? C24 C23 C22 118.30(14) . . ? C24 C23 C28 118.80(14) . . ? C22 C23 C28 122.88(14) . . ? C25 C24 C23 121.71(15) . . ? C24 C25 C26 119.04(15) . . ? C25 C26 C27 122.05(15) . . ? C26 C27 C22 118.25(14) . . ? C26 C27 C31 120.48(14) . . ? C22 C27 C31 121.25(14) . . ? C23 C28 C29 111.02(14) . . ? C23 C28 C30 111.83(14) . . ? C29 C28 C30 109.44(14) . . ? C27 C31 C32 110.64(15) . . ? C27 C31 C33 112.02(14) . . ? C32 C31 C33 111.57(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.239 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.045 data_ya165m _database_code_depnum_ccdc_archive 'CCDC 721356' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H36 Al Cl2 N5' _chemical_formula_weight 624.57 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' 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 Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 20.656(3) _cell_length_b 36.021(7) _cell_length_c 8.4360(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6276.9(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.9262 _exptl_absorpt_correction_T_max 0.9788 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37239 _diffrn_reflns_av_R_equivalents 0.1282 _diffrn_reflns_av_sigmaI/netI 0.2064 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 29.03 _reflns_number_total 8295 _reflns_number_gt 3119 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0829P)^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 8295 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1996 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1874 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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 0.45496(5) 0.11541(3) 0.61985(11) 0.0218(3) Uani 1 1 d . . . N1 N 0.38467(12) 0.09737(7) 0.7276(3) 0.0226(7) Uani 1 1 d . . . N2 N 0.41695(12) 0.06826(7) 0.4575(3) 0.0210(6) Uani 1 1 d . . . N3 N 0.45261(12) 0.15232(7) 0.8345(3) 0.0237(7) Uani 1 1 d . . . N4 N 0.45109(12) 0.15522(7) 0.4783(3) 0.0228(7) Uani 1 1 d . . . N5 N 0.53623(12) 0.09328(7) 0.6344(3) 0.0212(6) Uani 1 1 d . . . Cl1 Cl 0.68238(5) 0.13775(4) 0.80399(15) 0.0678(4) Uani 1 1 d . . . Cl2 Cl 0.70323(7) 0.19499(4) 1.03742(17) 0.0970(5) Uani 1 1 d . . . C1 C 0.36922(16) 0.10602(9) 0.8829(4) 0.0236(8) Uani 1 1 d . . . C2 C 0.31683(16) 0.08499(10) 0.9286(4) 0.0290(9) Uani 1 1 d . . . H2 H 0.2961 0.0853 1.0291 0.035 Uiso 1 1 calc R . . C3 C 0.29966(16) 0.06256(10) 0.7958(4) 0.0286(9) Uani 1 1 d . . . H3 H 0.2654 0.0450 0.7916 0.034 Uiso 1 1 calc R . . C4 C 0.34150(15) 0.07091(9) 0.6760(4) 0.0225(8) Uani 1 1 d . . . C5 C 0.41519(16) 0.13215(9) 0.9601(4) 0.0285(8) Uani 1 1 d . . . H5A H 0.4453 0.1183 1.0296 0.034 Uiso 1 1 calc R . . H5B H 0.3911 0.1502 1.0262 0.034 Uiso 1 1 calc R . . C6 C 0.34824(15) 0.06073(9) 0.5051(4) 0.0258(8) Uani 1 1 d . . . H6A H 0.3182 0.0757 0.4398 0.031 Uiso 1 1 calc R . . H6B H 0.3378 0.0342 0.4896 0.031 Uiso 1 1 calc R . . C7 C 0.41423(17) 0.18599(9) 0.7915(4) 0.0319(9) Uani 1 1 d . . . H7A H 0.4106 0.2023 0.8841 0.048 Uiso 1 1 calc R . . H7B H 0.3709 0.1785 0.7568 0.048 Uiso 1 1 calc R . . H7C H 0.4360 0.1993 0.7054 0.048 Uiso 1 1 calc R . . C8 C 0.51489(16) 0.16428(10) 0.9033(4) 0.0309(9) Uani 1 1 d . . . H8A H 0.5374 0.1805 0.8280 0.046 Uiso 1 1 calc R . . H8B H 0.5417 0.1424 0.9255 0.046 Uiso 1 1 calc R . . H8C H 0.5069 0.1779 1.0020 0.046 Uiso 1 1 calc R . . C9 C 0.41896(16) 0.07423(10) 0.2830(4) 0.0328(9) Uani 1 1 d . . . H9A H 0.4640 0.0774 0.2490 0.049 Uiso 1 1 calc R . . H9B H 0.3941 0.0965 0.2561 0.049 Uiso 1 1 calc R . . H9C H 0.4001 0.0527 0.2291 0.049 Uiso 1 1 calc R . . C10 C 0.45470(16) 0.03435(9) 0.4935(4) 0.0282(8) Uani 1 1 d . . . H10A H 0.4372 0.0134 0.4328 0.042 Uiso 1 1 calc R . . H10B H 0.4518 0.0289 0.6070 0.042 Uiso 1 1 calc R . . H10C H 0.5001 0.0383 0.4643 0.042 Uiso 1 1 calc R . . C11 C 0.55757(15) 0.06944(9) 0.7559(4) 0.0221(8) Uani 1 1 d . . . C12 C 0.52578(17) 0.05968(9) 0.8983(4) 0.0267(8) Uani 1 1 d . . . H12 H 0.4846 0.0698 0.9238 0.032 Uiso 1 1 calc R . . C13 C 0.55618(18) 0.03503(10) 0.9997(4) 0.0330(9) Uani 1 1 d . . . H13 H 0.5356 0.0288 1.0969 0.040 Uiso 1 1 calc R . . C14 C 0.61618(18) 0.01895(10) 0.9640(4) 0.0358(10) Uani 1 1 d . . . H14 H 0.6356 0.0021 1.0362 0.043 Uiso 1 1 calc R . . C15 C 0.64707(17) 0.02771(10) 0.8234(4) 0.0318(9) Uani 1 1 d . . . H15 H 0.6879 0.0170 0.7985 0.038 Uiso 1 1 calc R . . C16 C 0.61750(16) 0.05252(9) 0.7183(4) 0.0231(8) Uani 1 1 d . . . C17 C 0.63411(15) 0.06525(9) 0.5613(4) 0.0245(8) Uani 1 1 d . . . C18 C 0.68506(16) 0.05745(10) 0.4583(4) 0.0323(9) Uani 1 1 d . . . H18 H 0.7193 0.0416 0.4906 0.039 Uiso 1 1 calc R . . C19 C 0.68517(17) 0.07295(10) 0.3094(4) 0.0351(10) Uani 1 1 d . . . H19 H 0.7200 0.0680 0.2391 0.042 Uiso 1 1 calc R . . C20 C 0.63463(16) 0.09596(10) 0.2603(4) 0.0293(9) Uani 1 1 d . . . H20 H 0.6354 0.1061 0.1563 0.035 Uiso 1 1 calc R . . C21 C 0.58323(16) 0.10436(9) 0.3601(4) 0.0265(8) Uani 1 1 d . . . H21 H 0.5488 0.1199 0.3257 0.032 Uiso 1 1 calc R . . C22 C 0.58371(15) 0.08924(9) 0.5135(4) 0.0213(8) Uani 1 1 d . . . C23 C 0.50052(16) 0.18082(9) 0.4410(4) 0.0208(8) Uani 1 1 d . . . C24 C 0.56341(16) 0.18244(9) 0.5020(4) 0.0262(8) Uani 1 1 d . . . H24 H 0.5780 0.1652 0.5793 0.031 Uiso 1 1 calc R . . C25 C 0.60399(17) 0.21039(9) 0.4451(4) 0.0298(9) Uani 1 1 d . . . H25 H 0.6465 0.2126 0.4872 0.036 Uiso 1 1 calc R . . C26 C 0.58398(18) 0.23510(10) 0.3285(4) 0.0339(9) Uani 1 1 d . . . H26 H 0.6134 0.2532 0.2898 0.041 Uiso 1 1 calc R . . C27 C 0.52203(17) 0.23364(9) 0.2681(4) 0.0291(9) Uani 1 1 d . . . H27 H 0.5088 0.2503 0.1869 0.035 Uiso 1 1 calc R . . C28 C 0.47895(16) 0.20725(9) 0.3286(4) 0.0227(8) Uani 1 1 d . . . C29 C 0.41169(17) 0.19900(9) 0.3000(4) 0.0256(8) Uani 1 1 d . . . C30 C 0.36347(18) 0.21604(10) 0.2082(4) 0.0323(9) Uani 1 1 d . . . H30 H 0.3733 0.2372 0.1453 0.039 Uiso 1 1 calc R . . C31 C 0.30170(19) 0.20173(11) 0.2104(4) 0.0394(10) Uani 1 1 d . . . H31 H 0.2692 0.2123 0.1449 0.047 Uiso 1 1 calc R . . C32 C 0.28661(18) 0.17175(11) 0.3081(4) 0.0402(10) Uani 1 1 d . . . H32 H 0.2434 0.1627 0.3105 0.048 Uiso 1 1 calc R . . C33 C 0.33303(17) 0.15483(10) 0.4016(4) 0.0333(9) Uani 1 1 d . . . H33 H 0.3220 0.1347 0.4691 0.040 Uiso 1 1 calc R . . C34 C 0.39628(17) 0.16798(9) 0.3947(4) 0.0246(8) Uani 1 1 d . . . C35 C 0.7377(2) 0.15901(13) 0.9297(5) 0.0646(14) Uani 1 1 d . . . H35A H 0.7553 0.1403 1.0040 0.078 Uiso 1 1 calc R . . H35B H 0.7741 0.1688 0.8662 0.078 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 0.0194(6) 0.0225(5) 0.0236(5) 0.0038(5) 0.0020(4) 0.0009(5) N1 0.0171(16) 0.0252(16) 0.0255(16) 0.0026(13) 0.0015(12) -0.0008(14) N2 0.0185(16) 0.0214(15) 0.0231(15) 0.0027(12) 0.0014(12) 0.0037(13) N3 0.0205(16) 0.0238(16) 0.0267(15) -0.0012(12) 0.0030(13) -0.0022(14) N4 0.0172(16) 0.0246(16) 0.0265(15) 0.0051(13) 0.0026(12) -0.0002(14) N5 0.0163(16) 0.0238(15) 0.0235(15) 0.0015(12) 0.0016(12) 0.0010(13) Cl1 0.0430(7) 0.0778(10) 0.0825(9) -0.0204(7) -0.0115(6) -0.0052(7) Cl2 0.1195(13) 0.0831(11) 0.0884(10) -0.0337(9) -0.0175(9) 0.0362(9) C1 0.021(2) 0.027(2) 0.0232(18) 0.0003(15) 0.0009(15) 0.0047(16) C2 0.019(2) 0.038(2) 0.029(2) 0.0082(17) 0.0067(15) -0.0003(18) C3 0.017(2) 0.032(2) 0.037(2) 0.0073(18) -0.0002(16) -0.0056(17) C4 0.0146(19) 0.0212(18) 0.0318(19) 0.0017(15) -0.0010(15) -0.0004(16) C5 0.030(2) 0.033(2) 0.0224(18) 0.0037(16) 0.0029(16) -0.0024(18) C6 0.019(2) 0.0256(19) 0.033(2) 0.0031(16) -0.0033(15) -0.0002(17) C7 0.036(2) 0.025(2) 0.035(2) 0.0033(16) 0.0100(17) 0.0034(18) C8 0.030(2) 0.034(2) 0.029(2) -0.0078(17) 0.0036(16) -0.0019(18) C9 0.033(2) 0.037(2) 0.0275(19) -0.0020(17) 0.0004(16) 0.0019(19) C10 0.024(2) 0.0227(18) 0.038(2) -0.0033(16) -0.0049(17) 0.0042(17) C11 0.019(2) 0.0234(18) 0.0244(18) 0.0002(15) -0.0042(14) -0.0025(16) C12 0.028(2) 0.0253(19) 0.0272(19) 0.0002(16) -0.0046(16) 0.0013(17) C13 0.039(2) 0.031(2) 0.0285(19) 0.0008(17) -0.0056(17) -0.0036(19) C14 0.043(3) 0.027(2) 0.038(2) 0.0035(18) -0.0157(19) -0.002(2) C15 0.024(2) 0.029(2) 0.042(2) -0.0056(17) -0.0134(18) 0.0042(18) C16 0.021(2) 0.0205(19) 0.0281(19) -0.0043(15) -0.0075(15) -0.0011(16) C17 0.016(2) 0.025(2) 0.033(2) -0.0055(16) -0.0039(16) -0.0013(16) C18 0.017(2) 0.033(2) 0.048(2) -0.0111(19) -0.0024(17) 0.0046(18) C19 0.022(2) 0.042(2) 0.041(2) -0.010(2) 0.0114(17) 0.002(2) C20 0.029(2) 0.031(2) 0.028(2) -0.0061(17) 0.0038(16) -0.0030(19) C21 0.024(2) 0.027(2) 0.029(2) -0.0032(16) 0.0014(16) -0.0047(17) C22 0.0147(19) 0.0194(18) 0.0299(19) -0.0051(15) 0.0015(15) -0.0046(16) C23 0.023(2) 0.0188(18) 0.0209(17) -0.0032(14) 0.0059(15) 0.0034(16) C24 0.030(2) 0.0235(19) 0.0253(18) 0.0011(16) 0.0048(15) 0.0023(17) C25 0.023(2) 0.031(2) 0.035(2) -0.0060(17) 0.0053(16) -0.0031(18) C26 0.040(3) 0.021(2) 0.041(2) 0.0032(17) 0.0135(19) -0.0043(19) C27 0.034(2) 0.025(2) 0.029(2) 0.0033(16) 0.0021(17) 0.0020(19) C28 0.029(2) 0.0167(17) 0.0223(18) 0.0014(14) 0.0036(15) 0.0034(17) C29 0.031(2) 0.0238(19) 0.0220(18) -0.0008(15) 0.0008(16) 0.0059(18) C30 0.038(2) 0.025(2) 0.034(2) 0.0013(17) -0.0068(18) 0.0062(19) C31 0.033(3) 0.036(2) 0.050(3) 0.001(2) -0.0168(19) 0.015(2) C32 0.026(2) 0.039(2) 0.056(3) 0.006(2) -0.0056(19) 0.005(2) C33 0.025(2) 0.031(2) 0.045(2) 0.0076(18) -0.0023(17) 0.0032(19) C34 0.027(2) 0.024(2) 0.0231(18) 0.0007(15) -0.0013(15) 0.0076(17) C35 0.050(3) 0.083(4) 0.061(3) -0.025(3) -0.005(2) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.832(3) . ? Al1 N5 1.862(3) . ? Al1 N4 1.868(3) . ? Al1 N3 2.247(3) . ? Al1 N2 2.319(3) . ? N1 C4 1.376(4) . ? N1 C1 1.384(4) . ? N2 C10 1.481(4) . ? N2 C9 1.488(4) . ? N2 C6 1.500(4) . ? N3 C8 1.476(4) . ? N3 C7 1.494(4) . ? N3 C5 1.500(4) . ? N4 C34 1.411(4) . ? N4 C23 1.411(4) . ? N5 C11 1.408(4) . ? N5 C22 1.422(4) . ? Cl1 C35 1.736(4) . ? Cl2 C35 1.735(4) . ? C1 C2 1.376(4) . ? C1 C5 1.487(4) . ? C2 C3 1.426(5) . ? C3 C4 1.363(4) . ? C4 C6 1.494(4) . ? C11 C12 1.414(4) . ? C11 C16 1.416(4) . ? C12 C13 1.384(4) . ? C13 C14 1.401(5) . ? C14 C15 1.384(5) . ? C15 C16 1.399(4) . ? C16 C17 1.443(4) . ? C17 C18 1.393(4) . ? C17 C22 1.412(4) . ? C18 C19 1.374(5) . ? C19 C20 1.396(5) . ? C20 C21 1.389(4) . ? C21 C22 1.404(4) . ? C23 C24 1.399(4) . ? C23 C28 1.416(4) . ? C24 C25 1.395(4) . ? C25 C26 1.390(5) . ? C26 C27 1.378(4) . ? C27 C28 1.398(4) . ? C28 C29 1.441(5) . ? C29 C30 1.403(4) . ? C29 C34 1.410(4) . ? C30 C31 1.376(5) . ? C31 C32 1.394(5) . ? C32 C33 1.383(4) . ? C33 C34 1.391(5) . ? 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 N1 Al1 N5 121.99(12) . . ? N1 Al1 N4 123.76(12) . . ? N5 Al1 N4 114.16(12) . . ? N1 Al1 N3 78.05(11) . . ? N5 Al1 N3 102.68(11) . . ? N4 Al1 N3 93.45(11) . . ? N1 Al1 N2 76.40(11) . . ? N5 Al1 N2 91.76(11) . . ? N4 Al1 N2 99.79(11) . . ? N3 Al1 N2 154.43(10) . . ? C4 N1 C1 107.8(3) . . ? C4 N1 Al1 127.0(2) . . ? C1 N1 Al1 124.9(2) . . ? C10 N2 C9 107.9(2) . . ? C10 N2 C6 107.1(2) . . ? C9 N2 C6 108.5(2) . . ? C10 N2 Al1 107.75(18) . . ? C9 N2 Al1 118.0(2) . . ? C6 N2 Al1 107.13(18) . . ? C8 N3 C7 108.7(3) . . ? C8 N3 C5 108.2(2) . . ? C7 N3 C5 106.9(2) . . ? C8 N3 Al1 118.09(19) . . ? C7 N3 Al1 107.23(19) . . ? C5 N3 Al1 107.11(19) . . ? C34 N4 C23 104.8(3) . . ? C34 N4 Al1 127.2(2) . . ? C23 N4 Al1 127.8(2) . . ? C11 N5 C22 104.1(2) . . ? C11 N5 Al1 126.3(2) . . ? C22 N5 Al1 128.2(2) . . ? C2 C1 N1 108.8(3) . . ? C2 C1 C5 136.7(3) . . ? N1 C1 C5 114.2(3) . . ? C1 C2 C3 106.7(3) . . ? C4 C3 C2 107.5(3) . . ? C3 C4 N1 109.2(3) . . ? C3 C4 C6 136.1(3) . . ? N1 C4 C6 114.5(3) . . ? C1 C5 N3 109.0(3) . . ? C4 C6 N2 107.6(2) . . ? N5 C11 C12 128.7(3) . . ? N5 C11 C16 111.9(3) . . ? C12 C11 C16 119.3(3) . . ? C13 C12 C11 118.3(3) . . ? C12 C13 C14 122.3(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 119.2(3) . . ? C15 C16 C11 121.0(3) . . ? C15 C16 C17 132.9(3) . . ? C11 C16 C17 106.1(3) . . ? C18 C17 C22 120.2(3) . . ? C18 C17 C16 133.5(3) . . ? C22 C17 C16 106.3(3) . . ? C19 C18 C17 119.3(3) . . ? C18 C19 C20 120.7(3) . . ? C21 C20 C19 121.4(3) . . ? C20 C21 C22 118.0(3) . . ? C21 C22 C17 120.4(3) . . ? C21 C22 N5 128.0(3) . . ? C17 C22 N5 111.5(3) . . ? C24 C23 N4 128.1(3) . . ? C24 C23 C28 120.7(3) . . ? N4 C23 C28 111.2(3) . . ? C25 C24 C23 117.5(3) . . ? C26 C25 C24 121.8(3) . . ? C27 C26 C25 120.9(3) . . ? C26 C27 C28 118.8(3) . . ? C27 C28 C23 120.1(3) . . ? C27 C28 C29 133.8(3) . . ? C23 C28 C29 106.1(3) . . ? C30 C29 C34 119.9(3) . . ? C30 C29 C28 133.3(3) . . ? C34 C29 C28 106.7(3) . . ? C31 C30 C29 119.1(3) . . ? C30 C31 C32 120.4(3) . . ? C33 C32 C31 121.6(4) . . ? C32 C33 C34 118.5(3) . . ? C33 C34 C29 120.4(3) . . ? C33 C34 N4 128.4(3) . . ? C29 C34 N4 111.1(3) . . ? Cl2 C35 Cl1 112.3(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.358 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.077 data_ic166c _database_code_depnum_ccdc_archive 'CCDC 721534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 Al Cl4 N5' _chemical_formula_weight 529.26 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' 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 Monoclinic _symmetry_space_group_name_H-M Cc 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 21.4849(5) _cell_length_b 9.0569(2) _cell_length_c 25.5170(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.4260(10) _cell_angle_gamma 90.00 _cell_volume 4965.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.8032 _exptl_absorpt_correction_T_max 0.9102 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24423 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 29.02 _reflns_number_total 11866 _reflns_number_gt 10255 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0362P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 11866 _refine_ls_number_parameters 601 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.02775(2) 0.43591(6) 0.37525(2) 0.02701(12) Uani 1 1 d . . . Al2 Al 0.78211(2) 0.76600(7) 0.63012(2) 0.02720(12) Uani 1 1 d . . . N1 N 0.01876(7) 0.22966(19) 0.31556(7) 0.0354(4) Uani 1 1 d . . . N2 N -0.00870(6) 0.28644(17) 0.41323(6) 0.0303(3) Uani 1 1 d . . . N3 N 0.01196(7) 0.54871(18) 0.44973(6) 0.0325(3) Uani 1 1 d . . . N4 N 0.00263(7) 0.56776(18) 0.32528(7) 0.0304(4) Uani 1 1 d . . . N5 N 0.11322(7) 0.4111(2) 0.37529(7) 0.0330(4) Uani 1 1 d . . . N6 N 0.78408(8) 0.9203(2) 0.55625(7) 0.0377(4) Uani 1 1 d . . . N7 N 0.75099(7) 0.9439(2) 0.65296(7) 0.0375(4) Uani 1 1 d . . . N8 N 0.75438(7) 0.7092(2) 0.71046(6) 0.0393(4) Uani 1 1 d . . . N9 N 0.86778(6) 0.7805(2) 0.63716(6) 0.0317(3) Uani 1 1 d . . . N10 N 0.75575(7) 0.60468(19) 0.59293(6) 0.0310(3) Uani 1 1 d . . . C1 C -0.04080(9) 0.2431(3) 0.28705(9) 0.0443(5) Uani 1 1 d . . . H1A H -0.0414 0.3357 0.2672 0.066 Uiso 1 1 calc R . . H1B H -0.0752 0.2426 0.3121 0.066 Uiso 1 1 calc R . . H1C H -0.0455 0.1598 0.2628 0.066 Uiso 1 1 calc R . . C2 C 0.06887(10) 0.2158(3) 0.27619(9) 0.0500(6) Uani 1 1 d . . . H2A H 0.0616 0.1276 0.2548 0.075 Uiso 1 1 calc R . . H2B H 0.1092 0.2075 0.2942 0.075 Uiso 1 1 calc R . . H2C H 0.0689 0.3034 0.2536 0.075 Uiso 1 1 calc R . . C3 C 0.01660(9) 0.0985(2) 0.35019(9) 0.0394(5) Uani 1 1 d . . . H3A H 0.0593 0.0642 0.3584 0.047 Uiso 1 1 calc R . . H3B H -0.0062 0.0171 0.3326 0.047 Uiso 1 1 calc R . . C4 C -0.01591(8) 0.1421(2) 0.39930(8) 0.0327(4) Uani 1 1 d . . . C5 C -0.04868(8) 0.0709(2) 0.43800(10) 0.0397(5) Uani 1 1 d . . . H5 H -0.0605 -0.0302 0.4383 0.048 Uiso 1 1 calc R . . C6 C -0.06160(8) 0.1775(2) 0.47759(9) 0.0381(5) Uani 1 1 d . . . H6 H -0.0832 0.1613 0.5094 0.046 Uiso 1 1 calc R . . C7 C -0.03652(8) 0.3080(2) 0.46053(8) 0.0316(4) Uani 1 1 d . . . C8 C -0.03764(9) 0.4641(2) 0.47873(8) 0.0360(4) Uani 1 1 d . . . H8A H -0.0295 0.4685 0.5169 0.043 Uiso 1 1 calc R . . H8B H -0.0790 0.5081 0.4717 0.043 Uiso 1 1 calc R . . C9 C 0.07050(9) 0.5403(3) 0.48106(8) 0.0424(5) Uani 1 1 d . . . H9A H 0.1032 0.5963 0.4634 0.064 Uiso 1 1 calc R . . H9B H 0.0833 0.4369 0.4845 0.064 Uiso 1 1 calc R . . H9C H 0.0635 0.5821 0.5159 0.064 Uiso 1 1 calc R . . C10 C -0.00798(9) 0.7038(2) 0.44573(9) 0.0397(5) Uani 1 1 d . . . H10A H -0.0135 0.7446 0.4810 0.060 Uiso 1 1 calc R . . H10B H -0.0475 0.7092 0.4264 0.060 Uiso 1 1 calc R . . H10C H 0.0238 0.7608 0.4272 0.060 Uiso 1 1 calc R . . C11 C -0.04695(7) 0.6418(2) 0.30388(7) 0.0254(3) Uani 1 1 d . . . C12 C -0.10929(8) 0.6193(2) 0.31865(7) 0.0296(4) Uani 1 1 d . . . C13 C -0.04002(8) 0.7483(2) 0.26377(7) 0.0292(4) Uani 1 1 d . . . C14 C -0.15894(8) 0.6934(2) 0.29621(8) 0.0347(4) Uani 1 1 d . . . H14 H -0.2001 0.6726 0.3075 0.042 Uiso 1 1 calc R . . C15 C -0.08890(9) 0.8242(2) 0.24144(8) 0.0362(4) Uani 1 1 d . . . H15 H -0.0813 0.8954 0.2149 0.043 Uiso 1 1 calc R . . C16 C -0.14934(9) 0.7969(2) 0.25774(8) 0.0392(5) Uani 1 1 d . . . H16 H -0.1834 0.8488 0.2426 0.047 Uiso 1 1 calc R . . C17 C 0.17156(8) 0.4723(2) 0.37756(7) 0.0284(4) Uani 1 1 d . . . C18 C 0.18532(7) 0.6224(2) 0.37327(7) 0.0282(4) Uani 1 1 d . . . C19 C 0.22496(8) 0.3820(2) 0.38477(7) 0.0321(4) Uani 1 1 d . . . C20 C 0.24516(8) 0.6810(2) 0.37700(7) 0.0335(4) Uani 1 1 d . . . H20 H 0.2515 0.7846 0.3747 0.040 Uiso 1 1 calc R . . C21 C 0.28515(8) 0.4378(3) 0.38738(7) 0.0373(5) Uani 1 1 d . . . H21 H 0.3194 0.3724 0.3915 0.045 Uiso 1 1 calc R . . C22 C 0.29511(8) 0.5869(3) 0.38404(8) 0.0400(5) Uani 1 1 d . . . H22 H 0.3362 0.6254 0.3866 0.048 Uiso 1 1 calc R . . C23 C 0.83488(10) 0.8839(3) 0.51963(8) 0.0487(6) Uani 1 1 d . . . H23A H 0.8365 0.9586 0.4919 0.073 Uiso 1 1 calc R . . H23B H 0.8272 0.7867 0.5040 0.073 Uiso 1 1 calc R . . H23C H 0.8746 0.8825 0.5387 0.073 Uiso 1 1 calc R . . C24 C 0.72483(10) 0.9189(3) 0.52702(9) 0.0472(5) Uani 1 1 d . . . H24A H 0.6906 0.9415 0.5509 0.071 Uiso 1 1 calc R . . H24B H 0.7183 0.8211 0.5115 0.071 Uiso 1 1 calc R . . H24C H 0.7261 0.9933 0.4991 0.071 Uiso 1 1 calc R . . C25 C 0.79333(11) 1.0700(2) 0.57856(10) 0.0488(6) Uani 1 1 d . . . H25A H 0.7796 1.1464 0.5533 0.059 Uiso 1 1 calc R . . H25B H 0.8378 1.0866 0.5871 0.059 Uiso 1 1 calc R . . C26 C 0.75474(10) 1.0759(3) 0.62721(10) 0.0466(5) Uani 1 1 d . . . C27 C 0.72437(11) 1.1815(3) 0.65491(12) 0.0598(7) Uani 1 1 d . . . H27 H 0.7197 1.2826 0.6458 0.072 Uiso 1 1 calc R . . C28 C 0.70123(9) 1.1106(3) 0.69980(12) 0.0640(8) Uani 1 1 d . . . H28 H 0.6779 1.1561 0.7268 0.077 Uiso 1 1 calc R . . C29 C 0.71833(8) 0.9629(3) 0.69787(8) 0.0446(6) Uani 1 1 d . . . C30 C 0.70722(8) 0.8245(3) 0.72735(8) 0.0509(7) Uani 1 1 d . . . H30A H 0.6645 0.7883 0.7202 0.061 Uiso 1 1 calc R . . H30B H 0.7114 0.8432 0.7654 0.061 Uiso 1 1 calc R . . C31 C 0.81057(9) 0.7256(3) 0.74482(8) 0.0502(6) Uani 1 1 d . . . H31A H 0.7991 0.7075 0.7814 0.075 Uiso 1 1 calc R . . H31B H 0.8272 0.8259 0.7414 0.075 Uiso 1 1 calc R . . H31C H 0.8423 0.6542 0.7342 0.075 Uiso 1 1 calc R . . C32 C 0.72896(11) 0.5591(3) 0.71859(10) 0.0565(7) Uani 1 1 d . . . H32A H 0.7602 0.4856 0.7087 0.085 Uiso 1 1 calc R . . H32B H 0.6915 0.5460 0.6969 0.085 Uiso 1 1 calc R . . H32C H 0.7183 0.5462 0.7556 0.085 Uiso 1 1 calc R . . C33 C 0.92510(8) 0.7147(2) 0.63411(7) 0.0315(4) Uani 1 1 d . . . C34 C 0.93580(8) 0.5630(3) 0.63799(8) 0.0378(5) Uani 1 1 d . . . C35 C 0.98004(8) 0.7987(3) 0.62745(8) 0.0393(5) Uani 1 1 d . . . C36 C 0.99485(10) 0.5002(3) 0.63694(9) 0.0503(6) Uani 1 1 d . . . H36 H 0.9994 0.3962 0.6402 0.060 Uiso 1 1 calc R . . C37 C 1.03924(9) 0.7372(3) 0.62630(9) 0.0535(7) Uani 1 1 d . . . H37 H 1.0746 0.7990 0.6221 0.064 Uiso 1 1 calc R . . C38 C 1.04682(9) 0.5882(3) 0.63120(10) 0.0572(7) Uani 1 1 d . . . H38 H 1.0872 0.5457 0.6307 0.069 Uiso 1 1 calc R . . C39 C 0.70869(7) 0.5652(2) 0.55961(7) 0.0268(4) Uani 1 1 d . . . C40 C 0.71792(8) 0.4734(2) 0.51563(7) 0.0316(4) Uani 1 1 d . . . C41 C 0.64641(8) 0.6119(2) 0.56501(7) 0.0316(4) Uani 1 1 d . . . C42 C 0.67165(10) 0.4329(3) 0.48111(8) 0.0429(5) Uani 1 1 d . . . H42 H 0.6806 0.3695 0.4525 0.051 Uiso 1 1 calc R . . C43 C 0.59930(9) 0.5766(3) 0.53038(8) 0.0407(5) Uani 1 1 d . . . H43 H 0.5586 0.6147 0.5353 0.049 Uiso 1 1 calc R . . C44 C 0.61190(10) 0.4853(3) 0.48840(9) 0.0483(6) Uani 1 1 d . . . H44 H 0.5796 0.4585 0.4646 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.03485(2) 0.78440(6) 0.241057(19) 0.03761(11) Uani 1 1 d . . . Cl2 Cl -0.124564(19) 0.49191(6) 0.36811(2) 0.04032(12) Uani 1 1 d . . . Cl3 Cl 0.125355(19) 0.74731(6) 0.36071(2) 0.03512(10) Uani 1 1 d . . . Cl4 Cl 0.21420(2) 0.19307(7) 0.39262(3) 0.04994(14) Uani 1 1 d . . . Cl5 Cl 0.87315(2) 0.44397(7) 0.64668(3) 0.05415(16) Uani 1 1 d . . . Cl6 Cl 0.97317(2) 0.99003(7) 0.62134(2) 0.05377(16) Uani 1 1 d . . . Cl7 Cl 0.79380(2) 0.41520(6) 0.50210(2) 0.04082(12) Uani 1 1 d . . . Cl8 Cl 0.62900(2) 0.72590(7) 0.61781(2) 0.04755(14) Uani 1 1 d . . . H9 H 0.8731(11) 0.874(3) 0.6376(10) 0.052(7) Uiso 1 1 d . . . H10 H 0.7846(12) 0.557(3) 0.5901(10) 0.052(7) Uiso 1 1 d . . . H4A H 0.0287(11) 0.594(3) 0.3111(10) 0.047(7) Uiso 1 1 d . . . H5A H 0.1183(11) 0.319(3) 0.3832(10) 0.048(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0216(2) 0.0271(3) 0.0324(3) 0.0044(2) 0.00339(18) 0.0001(2) Al2 0.0213(2) 0.0341(3) 0.0262(3) -0.0034(2) 0.00075(18) 0.0007(2) N1 0.0298(7) 0.0363(10) 0.0402(9) -0.0032(7) 0.0038(6) -0.0023(7) N2 0.0270(7) 0.0280(9) 0.0359(8) 0.0037(7) 0.0035(6) -0.0010(6) N3 0.0311(7) 0.0313(9) 0.0353(9) 0.0015(7) 0.0046(6) -0.0017(7) N4 0.0216(6) 0.0332(10) 0.0366(9) 0.0078(7) 0.0054(6) -0.0023(6) N5 0.0239(7) 0.0265(10) 0.0486(10) 0.0020(8) 0.0009(6) -0.0013(6) N6 0.0387(8) 0.0404(10) 0.0339(9) 0.0089(7) 0.0008(7) -0.0026(7) N7 0.0317(7) 0.0404(10) 0.0403(9) -0.0106(8) 0.0009(7) 0.0041(7) N8 0.0293(7) 0.0635(13) 0.0250(8) 0.0003(8) 0.0012(6) -0.0095(7) N9 0.0235(7) 0.0361(10) 0.0355(9) 0.0006(8) 0.0008(6) -0.0023(7) N10 0.0247(7) 0.0327(9) 0.0354(9) -0.0032(7) -0.0022(6) 0.0056(7) C1 0.0417(10) 0.0466(14) 0.0444(12) -0.0093(10) -0.0053(9) -0.0069(9) C2 0.0456(11) 0.0616(16) 0.0429(12) -0.0096(11) 0.0129(9) -0.0038(10) C3 0.0338(9) 0.0295(11) 0.0551(13) -0.0045(9) 0.0077(9) -0.0008(8) C4 0.0236(7) 0.0259(10) 0.0487(11) 0.0045(9) 0.0014(7) 0.0006(7) C5 0.0295(8) 0.0263(11) 0.0634(14) 0.0102(10) 0.0069(8) 0.0000(8) C6 0.0280(8) 0.0376(12) 0.0489(12) 0.0152(10) 0.0083(8) 0.0009(8) C7 0.0253(7) 0.0337(11) 0.0358(10) 0.0070(8) 0.0020(7) 0.0009(7) C8 0.0359(9) 0.0393(12) 0.0327(10) 0.0028(9) 0.0089(8) -0.0007(8) C9 0.0405(10) 0.0519(14) 0.0348(11) -0.0044(10) -0.0021(8) -0.0063(9) C10 0.0409(10) 0.0312(11) 0.0472(12) -0.0047(9) 0.0105(9) -0.0003(8) C11 0.0251(7) 0.0257(9) 0.0254(8) -0.0047(7) -0.0013(6) -0.0003(6) C12 0.0279(8) 0.0310(11) 0.0298(9) -0.0035(8) 0.0013(7) -0.0001(7) C13 0.0288(8) 0.0295(11) 0.0293(9) -0.0051(8) 0.0002(7) -0.0001(7) C14 0.0258(8) 0.0404(12) 0.0380(10) -0.0106(9) -0.0008(7) 0.0032(8) C15 0.0417(9) 0.0369(12) 0.0299(10) 0.0021(9) -0.0059(8) 0.0041(9) C16 0.0357(9) 0.0444(13) 0.0374(11) -0.0066(9) -0.0080(8) 0.0107(9) C17 0.0239(7) 0.0377(11) 0.0238(8) 0.0013(8) 0.0032(6) 0.0005(7) C18 0.0240(7) 0.0388(12) 0.0218(8) -0.0008(8) 0.0010(6) -0.0007(7) C19 0.0268(8) 0.0395(12) 0.0301(9) 0.0016(8) 0.0041(7) 0.0033(8) C20 0.0280(8) 0.0477(13) 0.0248(9) -0.0020(8) 0.0038(7) -0.0103(8) C21 0.0237(8) 0.0587(15) 0.0295(10) 0.0002(9) 0.0033(7) 0.0044(8) C22 0.0244(8) 0.0647(16) 0.0309(10) -0.0025(9) 0.0022(7) -0.0067(8) C23 0.0493(11) 0.0639(16) 0.0329(11) 0.0120(11) 0.0072(9) -0.0090(11) C24 0.0497(11) 0.0520(15) 0.0399(12) 0.0132(10) -0.0082(9) -0.0005(10) C25 0.0552(12) 0.0307(13) 0.0602(15) 0.0111(10) -0.0077(11) -0.0023(10) C26 0.0410(10) 0.0343(13) 0.0645(15) -0.0076(11) -0.0129(10) 0.0060(9) C27 0.0430(12) 0.0485(16) 0.088(2) -0.0231(14) -0.0133(12) 0.0130(11) C28 0.0301(9) 0.078(2) 0.0835(19) -0.0537(17) -0.0118(11) 0.0174(11) C29 0.0236(8) 0.0675(16) 0.0427(12) -0.0255(11) -0.0016(8) -0.0006(9) C30 0.0267(8) 0.098(2) 0.0286(10) -0.0183(12) 0.0062(7) -0.0051(10) C31 0.0387(10) 0.087(2) 0.0246(10) 0.0037(11) -0.0056(8) -0.0060(11) C32 0.0494(12) 0.0790(19) 0.0414(13) 0.0160(12) 0.0054(10) -0.0183(12) C33 0.0255(7) 0.0492(13) 0.0198(8) -0.0016(8) 0.0005(6) 0.0004(8) C34 0.0283(8) 0.0548(15) 0.0301(10) 0.0058(9) -0.0020(7) 0.0038(8) C35 0.0286(8) 0.0613(15) 0.0279(10) -0.0101(9) 0.0031(7) -0.0063(9) C36 0.0392(11) 0.0641(17) 0.0476(13) 0.0008(12) -0.0054(9) 0.0174(11) C37 0.0233(8) 0.094(2) 0.0431(12) -0.0146(13) 0.0029(8) -0.0073(11) C38 0.0271(9) 0.093(2) 0.0518(14) -0.0059(14) -0.0017(9) 0.0153(11) C39 0.0279(8) 0.0257(10) 0.0268(9) 0.0025(7) 0.0009(6) -0.0043(7) C40 0.0368(9) 0.0280(10) 0.0303(9) 0.0003(8) 0.0069(7) -0.0050(8) C41 0.0287(8) 0.0346(11) 0.0315(9) -0.0017(8) 0.0027(7) -0.0014(8) C42 0.0525(11) 0.0416(13) 0.0346(11) -0.0104(9) -0.0010(9) -0.0163(10) C43 0.0299(8) 0.0509(14) 0.0413(11) 0.0040(10) -0.0036(8) -0.0098(9) C44 0.0442(11) 0.0590(16) 0.0416(12) -0.0069(11) -0.0082(9) -0.0195(11) Cl1 0.0333(2) 0.0449(3) 0.0347(2) 0.0087(2) 0.00382(17) -0.0031(2) Cl2 0.02764(19) 0.0463(3) 0.0471(3) 0.0095(2) 0.00528(18) -0.00395(19) Cl3 0.02976(19) 0.0328(3) 0.0427(3) -0.0002(2) -0.00381(17) -0.00184(17) Cl4 0.0355(2) 0.0423(3) 0.0721(4) 0.0140(3) 0.0119(2) 0.0116(2) Cl5 0.0384(2) 0.0459(3) 0.0782(4) 0.0224(3) -0.0031(2) 0.0048(2) Cl6 0.0420(2) 0.0590(4) 0.0605(4) -0.0167(3) 0.0147(2) -0.0216(3) Cl7 0.0459(2) 0.0357(3) 0.0410(3) -0.0045(2) 0.0131(2) 0.0036(2) Cl8 0.0300(2) 0.0667(4) 0.0460(3) -0.0191(3) 0.00073(19) 0.0089(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 N4 1.8256(17) . ? Al1 N2 1.8429(15) . ? Al1 N5 1.8499(15) . ? Al1 N3 2.1865(17) . ? Al1 N1 2.4171(18) . ? Al2 N10 1.8298(18) . ? Al2 N7 1.8411(18) . ? Al2 N9 1.8527(15) . ? Al2 N8 2.2001(16) . ? Al2 N6 2.3470(17) . ? N1 C1 1.472(3) . ? N1 C3 1.482(3) . ? N1 C2 1.483(2) . ? N2 C4 1.364(2) . ? N2 C7 1.365(2) . ? N3 C10 1.471(3) . ? N3 C9 1.487(3) . ? N3 C8 1.511(2) . ? N4 C11 1.369(2) . ? N5 C17 1.371(2) . ? N6 C24 1.471(3) . ? N6 C23 1.479(3) . ? N6 C25 1.483(3) . ? N7 C29 1.359(3) . ? N7 C26 1.367(3) . ? N8 C32 1.481(3) . ? N8 C31 1.494(3) . ? N8 C30 1.519(3) . ? N9 C33 1.371(2) . ? N10 C39 1.364(2) . ? C3 C4 1.492(3) . ? C4 C5 1.377(3) . ? C5 C6 1.426(3) . ? C6 C7 1.371(3) . ? C7 C8 1.489(3) . ? C11 C12 1.409(2) . ? C11 C13 1.415(3) . ? C12 C14 1.381(3) . ? C12 Cl2 1.7431(19) . ? C13 C15 1.376(3) . ? C13 Cl1 1.7449(17) . ? C14 C16 1.374(3) . ? C15 C16 1.389(3) . ? C17 C18 1.396(3) . ? C17 C19 1.420(3) . ? C18 C20 1.393(2) . ? C18 Cl3 1.7424(19) . ? C19 C21 1.390(3) . ? C19 Cl4 1.738(2) . ? C20 C22 1.381(3) . ? C21 C22 1.370(3) . ? C25 C26 1.499(3) . ? C26 C27 1.359(3) . ? C27 C28 1.407(4) . ? C28 C29 1.389(3) . ? C29 C30 1.482(4) . ? C33 C34 1.396(3) . ? C33 C35 1.416(3) . ? C34 C36 1.391(3) . ? C34 Cl5 1.740(2) . ? C35 C37 1.389(3) . ? C35 Cl6 1.746(3) . ? C36 C38 1.380(4) . ? C37 C38 1.365(4) . ? C39 C41 1.411(2) . ? C39 C40 1.412(3) . ? C40 C42 1.373(3) . ? C40 Cl7 1.7501(19) . ? C41 C43 1.376(3) . ? C41 Cl8 1.7405(19) . ? C42 C44 1.383(3) . ? C43 C44 1.382(3) . ? 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 N4 Al1 N2 136.32(7) . . ? N4 Al1 N5 111.60(8) . . ? N2 Al1 N5 109.64(8) . . ? N4 Al1 N3 104.74(7) . . ? N2 Al1 N3 79.44(7) . . ? N5 Al1 N3 102.51(7) . . ? N4 Al1 N1 92.50(7) . . ? N2 Al1 N1 74.42(7) . . ? N5 Al1 N1 88.93(7) . . ? N3 Al1 N1 153.73(6) . . ? N10 Al2 N7 138.72(8) . . ? N10 Al2 N9 114.23(8) . . ? N7 Al2 N9 105.67(8) . . ? N10 Al2 N8 102.23(7) . . ? N7 Al2 N8 78.94(8) . . ? N9 Al2 N8 101.65(7) . . ? N10 Al2 N6 93.80(7) . . ? N7 Al2 N6 75.04(7) . . ? N9 Al2 N6 90.67(7) . . ? N8 Al2 N6 153.39(7) . . ? C1 N1 C3 109.26(16) . . ? C1 N1 C2 107.75(17) . . ? C3 N1 C2 111.25(16) . . ? C1 N1 Al1 108.23(12) . . ? C3 N1 Al1 104.27(12) . . ? C2 N1 Al1 115.91(13) . . ? C4 N2 C7 108.54(15) . . ? C4 N2 Al1 127.96(13) . . ? C7 N2 Al1 123.42(13) . . ? C10 N3 C9 109.33(16) . . ? C10 N3 C8 108.18(14) . . ? C9 N3 C8 107.91(15) . . ? C10 N3 Al1 115.63(13) . . ? C9 N3 Al1 107.89(11) . . ? C8 N3 Al1 107.66(12) . . ? C11 N4 Al1 145.51(13) . . ? C17 N5 Al1 149.09(15) . . ? C24 N6 C23 108.52(17) . . ? C24 N6 C25 108.38(17) . . ? C23 N6 C25 110.40(17) . . ? C24 N6 Al2 112.43(12) . . ? C23 N6 Al2 113.12(13) . . ? C25 N6 Al2 103.84(13) . . ? C29 N7 C26 109.13(19) . . ? C29 N7 Al2 124.64(17) . . ? C26 N7 Al2 126.20(14) . . ? C32 N8 C31 107.82(18) . . ? C32 N8 C30 110.12(17) . . ? C31 N8 C30 107.65(17) . . ? C32 N8 Al2 116.61(14) . . ? C31 N8 Al2 107.48(11) . . ? C30 N8 Al2 106.82(13) . . ? C33 N9 Al2 148.85(16) . . ? C39 N10 Al2 139.28(14) . . ? N1 C3 C4 107.80(16) . . ? N2 C4 C5 108.62(17) . . ? N2 C4 C3 114.80(15) . . ? C5 C4 C3 136.35(19) . . ? C4 C5 C6 107.13(17) . . ? C7 C6 C5 106.24(17) . . ? N2 C7 C6 109.47(18) . . ? N2 C7 C8 114.82(16) . . ? C6 C7 C8 135.44(17) . . ? C7 C8 N3 108.42(14) . . ? N4 C11 C12 124.12(17) . . ? N4 C11 C13 122.45(15) . . ? C12 C11 C13 113.42(16) . . ? C14 C12 C11 123.49(17) . . ? C14 C12 Cl2 118.22(13) . . ? C11 C12 Cl2 118.29(14) . . ? C15 C13 C11 123.81(17) . . ? C15 C13 Cl1 118.13(15) . . ? C11 C13 Cl1 118.07(13) . . ? C16 C14 C12 120.54(17) . . ? C13 C15 C16 119.96(19) . . ? C14 C16 C15 118.78(18) . . ? N5 C17 C18 125.76(17) . . ? N5 C17 C19 120.67(19) . . ? C18 C17 C19 113.57(16) . . ? C20 C18 C17 124.15(17) . . ? C20 C18 Cl3 116.50(16) . . ? C17 C18 Cl3 119.34(13) . . ? C21 C19 C17 123.19(19) . . ? C21 C19 Cl4 118.49(15) . . ? C17 C19 Cl4 118.29(14) . . ? C22 C20 C18 119.3(2) . . ? C22 C21 C19 120.07(18) . . ? C21 C22 C20 119.66(17) . . ? N6 C25 C26 106.10(17) . . ? C27 C26 N7 109.6(2) . . ? C27 C26 C25 136.6(3) . . ? N7 C26 C25 113.69(18) . . ? C26 C27 C28 106.1(2) . . ? C29 C28 C27 108.4(2) . . ? N7 C29 C28 106.9(2) . . ? N7 C29 C30 114.04(19) . . ? C28 C29 C30 138.9(2) . . ? C29 C30 N8 109.09(15) . . ? N9 C33 C34 124.85(17) . . ? N9 C33 C35 121.6(2) . . ? C34 C33 C35 113.58(17) . . ? C36 C34 C33 123.4(2) . . ? C36 C34 Cl5 117.10(19) . . ? C33 C34 Cl5 119.43(14) . . ? C37 C35 C33 123.5(2) . . ? C37 C35 Cl6 118.22(18) . . ? C33 C35 Cl6 118.29(16) . . ? C38 C36 C34 120.3(2) . . ? C38 C37 C35 120.2(2) . . ? C37 C38 C36 119.0(2) . . ? N10 C39 C41 124.03(17) . . ? N10 C39 C40 122.82(16) . . ? C41 C39 C40 113.15(16) . . ? C42 C40 C39 124.18(18) . . ? C42 C40 Cl7 117.65(15) . . ? C39 C40 Cl7 118.08(14) . . ? C43 C41 C39 124.13(18) . . ? C43 C41 Cl8 118.27(14) . . ? C39 C41 Cl8 117.57(14) . . ? C40 C42 C44 119.4(2) . . ? C41 C43 C44 119.30(19) . . ? C43 C44 C42 119.80(19) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.250 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.040