# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Samuel Dagorne' _publ_contact_author_email DAGORNE@UNISTRA.FR _publ_section_title ; Unusual reactivity in organoaluminum and NHC chemistry: deprotonation of AlMe3 by a NHC moiety involving the formation of a sterically bulky NHC/AlMe3 Lewis adduct ; loop_ _publ_author_name 'Samuel Dagorne' 'Anne-Laure Schmitt' 'Richard Welter' # Attachment 'complexes2-4.cif' data_welt33 _database_code_depnum_ccdc_archive 'CCDC 752342' #TrackingRef 'complexes2-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H29 Al N2' _chemical_formula_sum 'C14 H29 Al N2' _chemical_formula_weight 252.37 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4995(6) _cell_length_b 15.0660(10) _cell_length_c 11.2880(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.311(3) _cell_angle_gamma 90.00 _cell_volume 1608.60(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10803 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _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 12590 _diffrn_reflns_av_R_equivalents 0.1073 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3681 _reflns_number_gt 2542 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0604P)^2^+0.3096P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.012(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3681 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1242 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.26122(17) 0.29207(12) 0.72043(14) 0.0254(4) Uani 1 1 d . . . C2 C 0.35550(19) 0.15592(12) 0.76257(16) 0.0319(4) Uani 1 1 d . . . H2 H 0.4179 0.1109 0.7947 0.038 Uiso 1 1 calc R . . C3 C 0.23445(19) 0.14330(12) 0.69486(16) 0.0317(4) Uani 1 1 d . . . H3 H 0.1948 0.0877 0.6702 0.038 Uiso 1 1 calc R . . C4 C 0.50037(18) 0.28441(13) 0.84899(17) 0.0320(4) Uani 1 1 d . . . C5 C 0.5652(2) 0.35725(14) 0.77681(18) 0.0402(5) Uani 1 1 d . . . H5A H 0.5961 0.3317 0.7037 0.060 Uiso 1 1 calc R . . H5B H 0.6466 0.3833 0.8241 0.060 Uiso 1 1 calc R . . H5C H 0.4944 0.4034 0.7564 0.060 Uiso 1 1 calc R . . C6 C 0.6117(2) 0.21185(15) 0.8738(2) 0.0484(6) Uani 1 1 d . . . H6A H 0.5755 0.1664 0.9251 0.073 Uiso 1 1 calc R . . H6B H 0.6981 0.2379 0.9136 0.073 Uiso 1 1 calc R . . H6C H 0.6329 0.1848 0.7985 0.073 Uiso 1 1 calc R . . C7 C 0.4539(2) 0.31655(14) 0.96720(17) 0.0397(5) Uani 1 1 d . . . H7A H 0.3772 0.3597 0.9524 0.059 Uiso 1 1 calc R . . H7B H 0.5341 0.3447 1.0137 0.059 Uiso 1 1 calc R . . H7C H 0.4207 0.2660 1.0115 0.059 Uiso 1 1 calc R . . C8 C 0.04115(18) 0.23574(13) 0.58916(15) 0.0294(4) Uani 1 1 d . . . C9 C 0.0054(2) 0.14856(14) 0.52395(18) 0.0408(5) Uani 1 1 d . . . H9A H 0.0837 0.1316 0.4778 0.061 Uiso 1 1 calc R . . H9B H -0.0808 0.1562 0.4702 0.061 Uiso 1 1 calc R . . H9C H -0.0096 0.1019 0.5820 0.061 Uiso 1 1 calc R . . C10 C -0.07566(19) 0.25645(15) 0.66896(17) 0.0380(5) Uani 1 1 d . . . H10A H -0.0860 0.2066 0.7233 0.057 Uiso 1 1 calc R . . H10B H -0.1649 0.2658 0.6197 0.057 Uiso 1 1 calc R . . H10C H -0.0512 0.3103 0.7151 0.057 Uiso 1 1 calc R . . C11 C 0.0578(2) 0.30651(14) 0.49507(16) 0.0359(5) Uani 1 1 d . . . H11A H 0.0859 0.3627 0.5341 0.054 Uiso 1 1 calc R . . H11B H -0.0322 0.3144 0.4465 0.054 Uiso 1 1 calc R . . H11C H 0.1306 0.2879 0.4441 0.054 Uiso 1 1 calc R . . C12 C 0.3057(2) 0.50360(14) 0.85399(18) 0.0398(5) Uani 1 1 d . . . H12A H 0.4079 0.4935 0.8675 0.060 Uiso 1 1 calc R . . H12B H 0.2602 0.4844 0.9241 0.060 Uiso 1 1 calc R . . H12C H 0.2876 0.5669 0.8400 0.060 Uiso 1 1 calc R . . C13 C 0.3172(2) 0.46919(15) 0.56635(18) 0.0462(5) Uani 1 1 d . . . H13A H 0.3241 0.4173 0.5148 0.069 Uiso 1 1 calc R . . H13B H 0.4121 0.4925 0.5894 0.069 Uiso 1 1 calc R . . H13C H 0.2598 0.5151 0.5234 0.069 Uiso 1 1 calc R . . C14 C 0.0240(2) 0.47098(14) 0.70636(19) 0.0411(5) Uani 1 1 d . . . H14A H 0.0178 0.5359 0.7023 0.062 Uiso 1 1 calc R . . H14B H -0.0161 0.4500 0.7782 0.062 Uiso 1 1 calc R . . H14C H -0.0290 0.4452 0.6360 0.062 Uiso 1 1 calc R . . N1 N 0.37348(14) 0.24600(10) 0.77732(12) 0.0260(3) Uani 1 1 d . . . N2 N 0.17749(15) 0.22559(10) 0.66733(12) 0.0261(3) Uani 1 1 d . . . Al1 Al 0.22696(6) 0.43391(4) 0.71145(5) 0.03031(19) Uani 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 C1 0.0237(8) 0.0293(10) 0.0238(8) 0.0000(7) 0.0061(7) 0.0000(7) C2 0.0355(10) 0.0267(10) 0.0336(9) 0.0016(8) 0.0028(8) 0.0021(8) C3 0.0375(10) 0.0236(10) 0.0338(10) 0.0021(8) 0.0015(8) -0.0048(8) C4 0.0243(9) 0.0346(11) 0.0365(10) -0.0059(8) -0.0007(7) 0.0007(7) C5 0.0288(10) 0.0440(13) 0.0482(12) -0.0039(10) 0.0070(9) -0.0062(9) C6 0.0303(11) 0.0479(14) 0.0643(14) -0.0088(11) -0.0102(10) 0.0071(9) C7 0.0451(12) 0.0399(12) 0.0332(10) -0.0055(9) -0.0008(8) -0.0023(9) C8 0.0255(9) 0.0364(11) 0.0257(8) -0.0012(8) 0.0000(7) -0.0028(8) C9 0.0383(11) 0.0450(13) 0.0377(11) -0.0070(9) -0.0034(9) -0.0073(9) C10 0.0292(10) 0.0524(13) 0.0323(10) 0.0010(9) 0.0035(8) -0.0007(9) C11 0.0376(11) 0.0432(12) 0.0264(9) 0.0011(8) 0.0004(8) -0.0012(8) C12 0.0422(11) 0.0296(11) 0.0476(11) -0.0064(9) 0.0036(9) 0.0004(9) C13 0.0564(13) 0.0407(13) 0.0425(11) 0.0019(10) 0.0108(10) -0.0123(10) C14 0.0440(12) 0.0351(12) 0.0438(11) -0.0026(9) 0.0011(9) 0.0094(9) N1 0.0248(7) 0.0262(8) 0.0270(7) -0.0021(6) 0.0028(6) 0.0015(6) N2 0.0261(7) 0.0267(8) 0.0255(7) -0.0002(6) 0.0024(6) -0.0034(6) Al1 0.0336(3) 0.0260(3) 0.0317(3) -0.0006(2) 0.0047(2) 0.0005(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 C1 N1 1.380(2) . ? C1 N2 1.381(2) . ? C1 Al1 2.1625(18) . ? C2 C3 1.334(3) . ? C2 N1 1.376(2) . ? C2 H2 0.9500 . ? C3 N2 1.377(2) . ? C3 H3 0.9500 . ? C4 N1 1.504(2) . ? C4 C7 1.523(3) . ? C4 C6 1.529(3) . ? C4 C5 1.530(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N2 1.506(2) . ? C8 C11 1.524(3) . ? C8 C10 1.525(3) . ? C8 C9 1.528(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 Al1 2.007(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 Al1 1.990(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 Al1 2.003(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 103.08(15) . . ? N1 C1 Al1 128.70(12) . . ? N2 C1 Al1 128.19(12) . . ? C3 C2 N1 107.50(16) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 107.50(16) . . ? C2 C3 H3 126.2 . . ? N2 C3 H3 126.2 . . ? N1 C4 C7 108.12(14) . . ? N1 C4 C6 109.26(15) . . ? C7 C4 C6 108.59(17) . . ? N1 C4 C5 109.37(15) . . ? C7 C4 C5 113.71(16) . . ? C6 C4 C5 107.73(17) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C11 109.89(14) . . ? N2 C8 C10 107.94(13) . . ? C11 C8 C10 113.39(16) . . ? N2 C8 C9 109.62(15) . . ? C11 C8 C9 107.37(15) . . ? C10 C8 C9 108.59(16) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C12 H12A 109.5 . . ? Al1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Al1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Al1 C13 H13A 109.5 . . ? Al1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Al1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Al1 C14 H14A 109.5 . . ? Al1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Al1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 N1 C1 110.97(14) . . ? C2 N1 C4 121.93(14) . . ? C1 N1 C4 127.10(15) . . ? C3 N2 C1 110.90(14) . . ? C3 N2 C8 121.49(14) . . ? C1 N2 C8 127.61(14) . . ? C13 Al1 C14 112.87(10) . . ? C13 Al1 C12 111.29(9) . . ? C14 Al1 C12 99.42(9) . . ? C13 Al1 C1 103.19(8) . . ? C14 Al1 C1 114.66(8) . . ? C12 Al1 C1 115.85(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.2(2) . . . . ? C3 C2 N1 C1 1.2(2) . . . . ? C3 C2 N1 C4 -179.72(15) . . . . ? N2 C1 N1 C2 -2.04(18) . . . . ? Al1 C1 N1 C2 179.66(12) . . . . ? N2 C1 N1 C4 178.97(15) . . . . ? Al1 C1 N1 C4 0.7(2) . . . . ? C7 C4 N1 C2 -105.27(18) . . . . ? C6 C4 N1 C2 12.7(2) . . . . ? C5 C4 N1 C2 130.44(17) . . . . ? C7 C4 N1 C1 73.6(2) . . . . ? C6 C4 N1 C1 -168.37(17) . . . . ? C5 C4 N1 C1 -50.7(2) . . . . ? C2 C3 N2 C1 -1.5(2) . . . . ? C2 C3 N2 C8 178.64(15) . . . . ? N1 C1 N2 C3 2.14(18) . . . . ? Al1 C1 N2 C3 -179.56(12) . . . . ? N1 C1 N2 C8 -178.00(14) . . . . ? Al1 C1 N2 C8 0.3(2) . . . . ? C11 C8 N2 C3 -132.90(17) . . . . ? C10 C8 N2 C3 102.99(19) . . . . ? C9 C8 N2 C3 -15.1(2) . . . . ? C11 C8 N2 C1 47.3(2) . . . . ? C10 C8 N2 C1 -76.9(2) . . . . ? C9 C8 N2 C1 165.03(16) . . . . ? N1 C1 Al1 C13 90.12(15) . . . . ? N2 C1 Al1 C13 -87.77(16) . . . . ? N1 C1 Al1 C14 -146.73(14) . . . . ? N2 C1 Al1 C14 35.38(17) . . . . ? N1 C1 Al1 C12 -31.74(17) . . . . ? N2 C1 Al1 C12 150.37(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.307 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.054 data_welt30 _database_code_depnum_ccdc_archive 'CCDC 752343' #TrackingRef 'complexes2-4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H29 Al N2' _chemical_formula_sum 'C14 H29 Al N2' _chemical_formula_weight 252.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 15.7347(9) _cell_length_b 9.7457(3) _cell_length_c 10.8668(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1666.38(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4842 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.006 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _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 10157 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2018 _reflns_number_gt 1364 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0729P)^2^+0.5673P] 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 SHELXL _refine_ls_extinction_coef 0.033(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2018 _refine_ls_number_parameters 114 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1379 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C -0.08249(17) 0.2500 -0.4870(2) 0.0350(6) Uani 1 2 d S . . C2 C -0.11648(17) 0.2500 -0.3715(2) 0.0346(6) Uani 1 2 d S . . H2 H -0.1757 0.2500 -0.3544 0.042 Uiso 1 2 calc SR . . C3 C 0.01980(18) 0.2500 -0.3420(2) 0.0373(7) Uani 1 2 d S . . H3 H 0.0742 0.2500 -0.3041 0.045 Uiso 1 2 calc SR . . C4 C 0.07540(18) 0.2500 -0.5574(3) 0.0394(7) Uani 1 2 d S . . C5 C 0.0543(3) 0.1395(6) -0.6564(5) 0.0536(9) Uani 0.50 1 d P A 1 H5A H 0.1023 0.1306 -0.7134 0.080 Uiso 0.50 1 calc PR A 1 H5B H 0.0035 0.1673 -0.7022 0.080 Uiso 0.50 1 calc PR A 1 H5C H 0.0439 0.0512 -0.6161 0.080 Uiso 0.50 1 calc PR A 1 C6 C 0.1601(3) 0.2072(4) -0.4976(4) 0.0536(9) Uani 0.50 1 d P A 1 H6A H 0.1556 0.1128 -0.4672 0.080 Uiso 0.50 1 calc PR A 1 H6B H 0.1729 0.2688 -0.4288 0.080 Uiso 0.50 1 calc PR A 1 H6C H 0.2058 0.2127 -0.5587 0.080 Uiso 0.50 1 calc PR A 1 C5B C 0.0799(3) 0.1107(6) -0.6092(5) 0.0536(9) Uani 0.50 1 d P A 2 H5B1 H 0.0250 0.0866 -0.6457 0.080 Uiso 0.50 1 calc PR A 2 H5B2 H 0.0937 0.0452 -0.5437 0.080 Uiso 0.50 1 calc PR A 2 H5B3 H 0.1241 0.1074 -0.6726 0.080 Uiso 0.50 1 calc PR A 2 C7 C -0.06701(18) 0.2500 -0.1461(2) 0.0386(7) Uani 1 2 d S . . C8 C -0.11703(17) 0.3783(3) -0.1142(2) 0.0623(7) Uani 1 1 d . . . H8A H -0.0835 0.4597 -0.1355 0.093 Uiso 1 1 calc R . . H8B H -0.1295 0.3790 -0.0259 0.093 Uiso 1 1 calc R . . H8C H -0.1704 0.3791 -0.1607 0.093 Uiso 1 1 calc R . . C9 C 0.0181(3) 0.2500 -0.0814(3) 0.0624(10) Uani 1 2 d S . . C10 C -0.1503(2) 0.0826(3) -0.7402(3) 0.0879(10) Uani 1 1 d . . . H10A H -0.1455 0.0019 -0.6868 0.132 Uiso 1 1 calc R . . H10B H -0.0989 0.0907 -0.7907 0.132 Uiso 1 1 calc R . . H10C H -0.2000 0.0728 -0.7937 0.132 Uiso 1 1 calc R . . C11 C -0.2756(2) 0.2500 -0.5560(4) 0.0714(12) Uani 1 2 d S . . Al1 Al -0.16310(6) 0.2500 -0.63721(7) 0.0396(3) Uani 1 2 d S . . N1 N 0.00581(14) 0.2500 -0.4631(2) 0.0351(6) Uani 1 2 d S A . N2 N -0.05372(14) 0.2500 -0.28258(19) 0.0334(5) Uani 1 2 d S . . H9A H 0.006(2) 0.2500 0.011(4) 0.069(11) Uiso 1 2 d S . . H9B H 0.0460(18) 0.159(3) -0.101(3) 0.090(9) Uiso 1 1 d . . . H11A H -0.317(3) 0.2500 -0.621(4) 0.095(14) Uiso 1 2 d S . . H11B H -0.2830(17) 0.171(3) -0.502(3) 0.099(11) 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 C1 0.0352(15) 0.0415(15) 0.0282(14) 0.000 0.0026(12) 0.000 C2 0.0303(14) 0.0467(16) 0.0269(13) 0.000 0.0005(11) 0.000 C3 0.0336(14) 0.0484(16) 0.0298(15) 0.000 -0.0025(12) 0.000 C4 0.0372(15) 0.0478(17) 0.0333(15) 0.000 0.0129(12) 0.000 C5 0.0468(19) 0.061(2) 0.053(2) -0.0055(14) 0.0182(14) 0.0066(13) C6 0.0468(19) 0.061(2) 0.053(2) -0.0055(14) 0.0182(14) 0.0066(13) C5B 0.0468(19) 0.061(2) 0.053(2) -0.0055(14) 0.0182(14) 0.0066(13) C7 0.0413(16) 0.0533(17) 0.0213(13) 0.000 0.0009(12) 0.000 C8 0.0819(19) 0.0732(17) 0.0318(12) -0.0061(11) 0.0062(11) 0.0176(14) C9 0.058(2) 0.096(3) 0.0330(18) 0.000 -0.0068(16) 0.000 C10 0.112(3) 0.092(2) 0.0599(17) -0.0332(16) -0.0350(17) 0.0329(19) C11 0.043(2) 0.127(4) 0.045(2) 0.000 -0.0099(17) 0.000 Al1 0.0443(6) 0.0486(5) 0.0259(5) 0.000 -0.0030(4) 0.000 N1 0.0327(12) 0.0472(14) 0.0255(11) 0.000 0.0062(9) 0.000 N2 0.0324(12) 0.0451(13) 0.0227(11) 0.000 0.0013(9) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.364(4) . ? C1 N1 1.413(3) . ? C1 Al1 2.067(3) . ? C2 N2 1.382(3) . ? C2 H2 0.9500 . ? C3 N2 1.325(3) . ? C3 N1 1.334(3) . ? C3 H3 0.9500 . ? C4 C5B 1.472(6) . ? C4 C5B 1.472(6) 8_565 ? C4 N1 1.499(3) . ? C4 C6 1.540(5) 8_565 ? C4 C6 1.540(5) . ? C4 C5 1.558(6) . ? C4 C5 1.558(6) 8_565 ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? C7 N2 1.497(3) . ? C7 C9 1.512(5) . ? C7 C8 1.518(3) 8_565 ? C7 C8 1.518(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 1.02(4) . ? C9 H9B 1.02(3) . ? C10 Al1 1.989(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 Al1 1.978(4) . ? C11 H11A 0.96(5) . ? C11 H11B 0.97(3) . ? Al1 C10 1.989(3) 8_565 ? 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 C2 C1 N1 102.5(2) . . ? C2 C1 Al1 119.1(2) . . ? N1 C1 Al1 138.42(19) . . ? C1 C2 N2 111.3(2) . . ? C1 C2 H2 124.4 . . ? N2 C2 H2 124.4 . . ? N2 C3 N1 109.7(2) . . ? N2 C3 H3 125.2 . . ? N1 C3 H3 125.2 . . ? C5B C4 C5B 134.6(5) . 8_565 ? C5B C4 N1 107.3(2) . . ? C5B C4 N1 107.3(2) 8_565 . ? C5B C4 C6 111.7(3) . 8_565 ? C5B C4 C6 82.5(3) 8_565 8_565 ? N1 C4 C6 110.1(2) . 8_565 ? C5B C4 C6 82.5(3) . . ? C5B C4 C6 111.7(3) 8_565 . ? N1 C4 C6 110.1(2) . . ? C5B C4 C5 112.6(4) 8_565 . ? N1 C4 C5 108.4(2) . . ? C6 C4 C5 131.5(3) 8_565 . ? C6 C4 C5 106.8(3) . . ? C5B C4 C5 112.6(4) . 8_565 ? N1 C4 C5 108.4(2) . 8_565 ? C6 C4 C5 106.8(3) 8_565 8_565 ? C6 C4 C5 131.5(3) . 8_565 ? C5 C4 C5 87.4(4) . 8_565 ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? C4 C5B H5B1 109.5 . . ? C4 C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C4 C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? N2 C7 C9 109.7(2) . . ? N2 C7 C8 107.38(15) . 8_565 ? C9 C7 C8 110.65(17) . 8_565 ? N2 C7 C8 107.38(15) . . ? C9 C7 C8 110.65(17) . . ? C8 C7 C8 111.0(3) 8_565 . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 107(2) . . ? C7 C9 H9B 106.5(17) . . ? H9A C9 H9B 107.0(19) . . ? Al1 C10 H10A 109.5 . . ? Al1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Al1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Al1 C11 H11A 106(3) . . ? Al1 C11 H11B 112.1(17) . . ? H11A C11 H11B 111(2) . . ? C11 Al1 C10 110.00(12) . . ? C11 Al1 C10 110.00(12) . 8_565 ? C10 Al1 C10 110.2(2) . 8_565 ? C11 Al1 C1 101.34(14) . . ? C10 Al1 C1 112.46(9) . . ? C10 Al1 C1 112.46(9) 8_565 . ? C3 N1 C1 110.1(2) . . ? C3 N1 C4 123.6(2) . . ? C1 N1 C4 126.3(2) . . ? C3 N2 C2 106.4(2) . . ? C3 N2 C7 127.2(2) . . ? C2 N2 C7 126.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 0.0 . . . . ? Al1 C1 C2 N2 180.0 . . . . ? C2 C1 Al1 C11 0.0 . . . . ? N1 C1 Al1 C11 180.0 . . . . ? C2 C1 Al1 C10 -117.41(13) . . . . ? N1 C1 Al1 C10 62.59(13) . . . . ? C2 C1 Al1 C10 117.41(13) . . . 8_565 ? N1 C1 Al1 C10 -62.59(13) . . . 8_565 ? N2 C3 N1 C1 0.0 . . . . ? N2 C3 N1 C4 180.0 . . . . ? C2 C1 N1 C3 0.0 . . . . ? Al1 C1 N1 C3 180.0 . . . . ? C2 C1 N1 C4 180.0 . . . . ? Al1 C1 N1 C4 0.0 . . . . ? C5B C4 N1 C3 104.9(3) . . . . ? C5B C4 N1 C3 -104.9(3) 8_565 . . . ? C6 C4 N1 C3 -16.76(18) 8_565 . . . ? C6 C4 N1 C3 16.76(18) . . . . ? C5 C4 N1 C3 133.2(2) . . . . ? C5 C4 N1 C3 -133.2(2) 8_565 . . . ? C5B C4 N1 C1 -75.1(3) . . . . ? C5B C4 N1 C1 75.1(3) 8_565 . . . ? C6 C4 N1 C1 163.24(18) 8_565 . . . ? C6 C4 N1 C1 -163.24(18) . . . . ? C5 C4 N1 C1 -46.8(2) . . . . ? C5 C4 N1 C1 46.8(2) 8_565 . . . ? N1 C3 N2 C2 0.0 . . . . ? N1 C3 N2 C7 180.0 . . . . ? C1 C2 N2 C3 0.0 . . . . ? C1 C2 N2 C7 180.0 . . . . ? C9 C7 N2 C3 0.0 . . . . ? C8 C7 N2 C3 -120.31(17) 8_565 . . . ? C8 C7 N2 C3 120.31(17) . . . . ? C9 C7 N2 C2 180.0 . . . . ? C8 C7 N2 C2 59.69(17) 8_565 . . . ? C8 C7 N2 C2 -59.69(17) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.366 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.085 # Attachment 'complex4.cif' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 752344' #TrackingRef 'complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H26 Al3, C11 H21 N2' _chemical_formula_sum 'C20 H47 Al3 N2' _chemical_formula_weight 396.54 _chemical_absolute_configuration . 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.036(1) _cell_length_b 12.480(1) _cell_length_c 19.024(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.60(5) _cell_angle_gamma 90.00 _cell_volume 2752.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9071 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6230 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1213 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6229 _reflns_number_gt 2975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. ; # start Validation Reply Form _vrf_PLAT390_complex4 ; PROBLEM: Deviating Methyl C12 X-C-H Bond Angle ...... 162.00 Deg. RESPONSE: the methyl group involving C12 is considered as the methyl group of Al2 but only of Al1. ; # end Validation Reply Form _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^)+(0.0997P)^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 6229 _refine_ls_number_parameters 229 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1517 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al -0.86691(9) 0.32019(8) 0.31416(5) 0.0452(3) Uani 1 1 d . . . Al2 Al -0.79810(9) 0.13853(8) 0.38419(6) 0.0435(3) Uani 1 1 d . . . Al3 Al -0.64465(9) 0.26086(8) 0.52021(5) 0.0393(3) Uani 1 1 d . . . N1 N -0.1999(2) 0.2589(2) 0.46599(13) 0.0372(6) Uani 1 1 d . A . N2 N -0.3177(2) 0.24765(19) 0.35788(13) 0.0348(6) Uani 1 1 d . . . C1 C -0.2650(3) 0.3146(3) 0.41058(17) 0.0366(7) Uani 1 1 d . . . H1 H -0.276(2) 0.389(2) 0.4078(15) 0.031(8) Uiso 1 1 d . . . C2 C -0.2127(3) 0.1527(3) 0.4483(2) 0.0505(10) Uani 1 1 d . . . H6 H -0.1770 0.0944 0.4780 0.061 Uiso 1 1 calc . . . C3 C -0.2855(3) 0.1457(3) 0.3806(2) 0.0518(10) Uani 1 1 d . . . H3 H -0.3097 0.0818 0.3538 0.062 Uiso 1 1 calc . . . C4 C -0.1252(2) 0.3026(2) 0.53679(16) 0.0461(9) Uani 1 1 d D . . C5A C 0.0014(3) 0.3002(7) 0.5342(5) 0.0607(9) Uiso 0.50 1 d PD A 1 H5A1 H 0.0066 0.3263 0.4866 0.091 Uiso 0.50 1 calc P B 1 H5A2 H 0.0306 0.2266 0.5415 0.091 Uiso 0.50 1 calc P C 1 H5A3 H 0.0477 0.3462 0.5728 0.091 Uiso 0.50 1 calc P D 1 C6A C -0.1133(7) 0.4243(3) 0.5277(4) 0.0607(9) Uiso 0.50 1 d PD A 1 H6A1 H -0.1861 0.4595 0.5277 0.091 Uiso 0.50 1 calc P E 1 H6A2 H -0.0949 0.4388 0.4815 0.091 Uiso 0.50 1 calc P F 1 H6A3 H -0.0514 0.4519 0.5683 0.091 Uiso 0.50 1 calc P G 1 C7A C -0.1713(7) 0.2697(6) 0.6017(3) 0.0607(9) Uiso 0.50 1 d PD A 1 H7A1 H -0.2552 0.2793 0.5886 0.091 Uiso 0.50 1 calc P H 1 H7A2 H -0.1356 0.3145 0.6440 0.091 Uiso 0.50 1 calc P I 1 H7A3 H -0.1525 0.1943 0.6137 0.091 Uiso 0.50 1 calc P J 1 C5B C -0.0043(4) 0.2538(6) 0.5474(5) 0.0607(9) Uiso 0.50 1 d PD A 2 H5B1 H -0.0116 0.1785 0.5323 0.091 Uiso 0.50 1 calc P K 2 H5B2 H 0.0388 0.2587 0.5989 0.091 Uiso 0.50 1 calc P L 2 H5B3 H 0.0370 0.2933 0.5177 0.091 Uiso 0.50 1 calc P M 2 C6B C -0.1716(6) 0.4136(4) 0.5501(4) 0.0607(9) Uiso 0.50 1 d PD A 2 H6B1 H -0.2561 0.4118 0.5365 0.091 Uiso 0.50 1 calc P N 2 H6B2 H -0.1455 0.4672 0.5205 0.091 Uiso 0.50 1 calc P O 2 H6B3 H -0.1427 0.4323 0.6019 0.091 Uiso 0.50 1 calc P P 2 C7B C -0.1483(7) 0.2280(6) 0.5958(4) 0.0607(9) Uiso 0.50 1 d PD A 2 H7B1 H -0.1200 0.1559 0.5898 0.091 Uiso 0.50 1 calc P Q 2 H7B2 H -0.2314 0.2252 0.5910 0.091 Uiso 0.50 1 calc P R 2 H7B3 H -0.1082 0.2556 0.6442 0.091 Uiso 0.50 1 calc P S 2 C8 C -0.3994(3) 0.2761(3) 0.28546(17) 0.0407(8) Uani 1 1 d . . . C9 C -0.4120(4) 0.3960(3) 0.2803(2) 0.0767(14) Uani 1 1 d . . . H9A H -0.4405 0.4224 0.3208 0.115 Uiso 1 1 calc . . . H9B H -0.4669 0.4152 0.2339 0.115 Uiso 1 1 calc . . . H9C H -0.3369 0.4286 0.2830 0.115 Uiso 1 1 calc . . . C10 C -0.3509(4) 0.2342(4) 0.2258(2) 0.0717(13) Uani 1 1 d . . . H10A H -0.2761 0.2681 0.2294 0.108 Uiso 1 1 calc . . . H10B H -0.4042 0.2507 0.1782 0.108 Uiso 1 1 calc . . . H10C H -0.3408 0.1564 0.2309 0.108 Uiso 1 1 calc . . . C11 C -0.5155(3) 0.2243(3) 0.2823(2) 0.0615(11) Uani 1 1 d . . . H11A H -0.5063 0.1463 0.2859 0.092 Uiso 1 1 calc . . . H11B H -0.5712 0.2428 0.2361 0.092 Uiso 1 1 calc . . . H11C H -0.5435 0.2505 0.3230 0.092 Uiso 1 1 calc . . . C12 C -0.8636(4) 0.1710(3) 0.26292(19) 0.0698(12) Uani 1 1 d . . . H12A H -0.9133 0.1740 0.2128 0.105 Uiso 1 1 calc . . . H12B H -0.8915 0.1151 0.2901 0.105 Uiso 1 1 calc . . . H12C H -0.7844 0.1545 0.2620 0.105 Uiso 1 1 calc . . . C13 C -0.6713(3) 0.0391(3) 0.3847(2) 0.0612(11) Uani 1 1 d . . . H13A H -0.6310 0.0206 0.4352 0.092 Uiso 1 1 calc . . . H13B H -0.6172 0.0732 0.3613 0.092 Uiso 1 1 calc . . . H13C H -0.7026 -0.0261 0.3580 0.092 Uiso 1 1 calc . . . C14 C -0.9362(3) 0.0778(3) 0.4057(2) 0.0606(10) Uani 1 1 d . . . H14A H -0.9495 0.0052 0.3855 0.091 Uiso 1 1 calc . . . H14B H -1.0032 0.1228 0.3836 0.091 Uiso 1 1 calc . . . H14C H -0.9247 0.0751 0.4586 0.091 Uiso 1 1 calc . . . C15 C -1.0285(3) 0.3540(3) 0.3103(2) 0.0603(11) Uani 1 1 d . . . H15A H -1.0304 0.4125 0.3443 0.090 Uiso 1 1 calc . . . H15B H -1.0657 0.2904 0.3240 0.090 Uiso 1 1 calc . . . H15C H -1.0696 0.3758 0.2606 0.090 Uiso 1 1 calc . . . C16 C -0.7919(4) 0.4220(4) 0.2631(2) 0.0734(13) Uani 1 1 d . . . H16A H -0.8237 0.4136 0.2103 0.110 Uiso 1 1 calc . . . H16B H -0.7087 0.4080 0.2762 0.110 Uiso 1 1 calc . . . H16C H -0.8057 0.4953 0.2772 0.110 Uiso 1 1 calc . . . C17 C -0.7688(3) 0.2891(3) 0.41900(18) 0.0393(8) Uani 1 1 d . . . H17A H -0.816(3) 0.328(3) 0.4383(18) 0.047(7) Uiso 1 1 d . . . H17B H -0.723(3) 0.342(3) 0.4078(17) 0.047(7) Uiso 1 1 d . . . C18 C -0.6568(3) 0.3904(3) 0.5786(2) 0.0623(11) Uani 1 1 d . . . H18A H -0.7358 0.3970 0.5829 0.093 Uiso 1 1 calc . . . H18B H -0.6372 0.4541 0.5543 0.093 Uiso 1 1 calc . . . H18C H -0.6033 0.3839 0.6274 0.093 Uiso 1 1 calc . . . C19 C -0.4904(3) 0.2587(4) 0.5002(2) 0.0702(12) Uani 1 1 d . . . H19A H -0.4465 0.1966 0.5244 0.105 Uiso 1 1 calc . . . H19B H -0.4485 0.3246 0.5190 0.105 Uiso 1 1 calc . . . H19C H -0.5002 0.2539 0.4475 0.105 Uiso 1 1 calc . . . C20 C -0.6782(3) 0.1296(3) 0.5696(2) 0.0570(10) Uani 1 1 d . . . H20A H -0.6145 0.1155 0.6129 0.085 Uiso 1 1 calc . . . H20B H -0.6871 0.0686 0.5360 0.085 Uiso 1 1 calc . . . H20C H -0.7497 0.1397 0.5841 0.085 Uiso 1 1 calc . . . 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 0.0436(6) 0.0495(6) 0.0374(6) 0.0035(5) 0.0022(4) 0.0036(5) Al2 0.0468(6) 0.0374(6) 0.0446(6) -0.0052(5) 0.0092(5) -0.0004(5) Al3 0.0398(6) 0.0390(6) 0.0350(5) 0.0007(4) 0.0031(4) -0.0002(4) N1 0.0409(15) 0.0339(14) 0.0337(14) -0.0003(12) 0.0049(12) 0.0008(12) N2 0.0374(14) 0.0346(14) 0.0310(14) -0.0016(11) 0.0066(11) -0.0039(11) C1 0.0444(19) 0.0284(17) 0.0341(17) -0.0019(14) 0.0054(14) -0.0007(15) C2 0.055(2) 0.0315(18) 0.056(2) 0.0017(16) -0.0010(18) 0.0022(16) C3 0.060(2) 0.0290(17) 0.059(2) -0.0064(16) 0.0018(19) 0.0004(16) C4 0.0448(19) 0.049(2) 0.0375(18) -0.0016(16) -0.0017(15) 0.0008(17) C8 0.0472(19) 0.0449(19) 0.0282(16) 0.0002(14) 0.0069(14) -0.0056(16) C9 0.111(4) 0.050(2) 0.046(2) 0.0062(19) -0.018(2) -0.004(2) C10 0.061(3) 0.111(4) 0.045(2) -0.014(2) 0.0159(19) -0.005(2) C11 0.044(2) 0.086(3) 0.048(2) 0.002(2) 0.0024(17) -0.010(2) C12 0.089(3) 0.078(3) 0.033(2) -0.007(2) 0.000(2) 0.011(2) C13 0.067(3) 0.049(2) 0.072(3) -0.005(2) 0.027(2) 0.0082(19) C14 0.053(2) 0.051(2) 0.077(3) -0.004(2) 0.016(2) -0.0068(19) C15 0.045(2) 0.067(3) 0.059(2) -0.002(2) -0.0018(18) 0.0008(19) C16 0.076(3) 0.080(3) 0.065(3) 0.028(2) 0.020(2) 0.008(2) C17 0.041(2) 0.0391(19) 0.0343(18) -0.0007(14) 0.0042(15) -0.0027(15) C18 0.081(3) 0.044(2) 0.048(2) -0.0042(18) -0.0071(19) 0.003(2) C19 0.040(2) 0.104(3) 0.062(2) 0.000(2) 0.0064(18) -0.002(2) C20 0.070(3) 0.049(2) 0.048(2) 0.0095(18) 0.0095(19) -0.0030(19) _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 C16 1.961(4) . ? Al1 C15 1.972(4) . ? Al1 C17 2.063(3) . ? Al1 C12 2.107(4) . ? Al1 Al2 2.6471(15) . ? Al2 C13 1.964(4) . ? Al2 C14 1.967(4) . ? Al3 C20 1.983(4) . ? Al3 C18 1.989(4) . ? Al3 C19 1.993(4) . ? Al3 C17 2.126(3) . ? N1 C1 1.328(4) . ? N1 C2 1.367(4) . ? N1 C4 1.506(4) . ? N2 C1 1.328(4) . ? N2 C3 1.366(4) . ? N2 C8 1.504(4) . ? C1 H1 0.93(3) . ? C2 C3 1.350(5) . ? C2 H6 0.9500 . ? C3 H3 0.9500 . ? C4 C5A 1.5386(10) . ? C4 C7A 1.5389(11) . ? C4 C6A 1.5395(10) . ? C4 C6B 1.5399(10) . ? C4 C7B 1.5402(10) . ? C4 C5B 1.5402(10) . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8 C10 1.503(5) . ? C8 C9 1.505(5) . ? C8 C11 1.526(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.90(3) . ? C17 H17B 0.92(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Al1 C15 115.08(18) . . ? C16 Al1 C17 112.39(16) . . ? C15 Al1 C17 112.25(17) . . ? C16 Al1 C12 105.94(19) . . ? C15 Al1 C12 108.24(18) . . ? C17 Al1 C12 101.76(15) . . ? C16 Al1 Al2 132.90(13) . . ? C15 Al1 Al2 111.96(13) . . ? C17 Al1 Al2 48.08(10) . . ? C12 Al1 Al2 55.51(11) . . ? C13 Al2 C14 116.99(17) . . ? C13 Al2 Al1 132.93(13) . . ? C14 Al2 Al1 105.49(12) . . ? C20 Al3 C18 110.63(17) . . ? C20 Al3 C19 113.46(18) . . ? C18 Al3 C19 109.24(19) . . ? C20 Al3 C17 112.48(15) . . ? C18 Al3 C17 103.42(15) . . ? C19 Al3 C17 107.07(17) . . ? C1 N1 C2 108.0(3) . . ? C1 N1 C4 127.1(3) . . ? C2 N1 C4 124.9(3) . . ? C1 N2 C3 108.0(3) . . ? C1 N2 C8 127.2(3) . . ? C3 N2 C8 124.8(3) . . ? N1 C1 N2 109.3(3) . . ? N1 C1 H1 127.6(17) . . ? N2 C1 H1 123.1(17) . . ? C3 C2 N1 107.4(3) . . ? C3 C2 H6 126.3 . . ? N1 C2 H6 126.3 . . ? C2 C3 N2 107.4(3) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? N1 C4 C5A 108.8(4) . . ? N1 C4 C7A 111.3(4) . . ? C5A C4 C7A 126.5(5) . . ? N1 C4 C6A 107.9(4) . . ? C5A C4 C6A 83.8(5) . . ? C7A C4 C6A 114.6(5) . . ? N1 C4 C6B 108.5(4) . . ? C5A C4 C6B 115.4(5) . . ? C7A C4 C6B 83.3(5) . . ? C6A C4 C6B 34.9(4) . . ? N1 C4 C7B 104.6(4) . . ? C5A C4 C7B 112.7(5) . . ? C7A C4 C7B 23.0(4) . . ? C6A C4 C7B 135.9(5) . . ? C6B C4 C7B 106.2(5) . . ? N1 C4 C5B 106.9(4) . . ? C5A C4 C5B 24.1(4) . . ? C7A C4 C5B 108.8(5) . . ? C6A C4 C5B 106.9(5) . . ? C6B C4 C5B 134.9(5) . . ? C7B C4 C5B 90.9(5) . . ? C4 C5A H5A1 109.5 . . ? C4 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C4 C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C4 C6A H6A1 109.5 . . ? C4 C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C4 C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C4 C7A H7A1 109.5 . . ? C4 C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C4 C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C4 C5B H5B1 109.5 . . ? C4 C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C4 C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? C4 C6B H6B1 109.5 . . ? C4 C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C4 C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C4 C7B H7B1 109.5 . . ? C4 C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C4 C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? C10 C8 N2 108.6(3) . . ? C10 C8 C9 110.5(3) . . ? N2 C8 C9 108.9(3) . . ? C10 C8 C11 111.1(3) . . ? N2 C8 C11 107.6(3) . . ? C9 C8 C11 110.1(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Al1 C12 H12A 109.5 . . ? Al1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Al1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Al2 C13 H13A 109.5 . . ? Al2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Al2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Al2 C14 H14A 109.5 . . ? Al2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Al2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Al1 C15 H15A 109.5 . . ? Al1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Al1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Al1 C16 H16A 109.5 . . ? Al1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Al1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Al1 C17 Al3 170.8(2) . . ? Al1 C17 H17A 92(2) . . ? Al3 C17 H17A 95(2) . . ? Al1 C17 H17B 82(2) . . ? Al3 C17 H17B 90(2) . . ? H17A C17 H17B 102(3) . . ? Al3 C18 H18A 109.5 . . ? Al3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Al3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Al3 C19 H19A 109.5 . . ? Al3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Al3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Al3 C20 H20A 109.5 . . ? Al3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Al3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 Al1 Al2 C13 -17.2(3) . . . . ? C15 Al1 Al2 C13 159.8(2) . . . . ? C17 Al1 Al2 C13 -99.4(2) . . . . ? C12 Al1 Al2 C13 62.2(2) . . . . ? C16 Al1 Al2 C14 -171.5(2) . . . . ? C15 Al1 Al2 C14 5.50(18) . . . . ? C17 Al1 Al2 C14 106.26(19) . . . . ? C12 Al1 Al2 C14 -92.1(2) . . . . ? C2 N1 C1 N2 -0.7(4) . . . . ? C4 N1 C1 N2 179.8(3) . . . . ? C3 N2 C1 N1 0.2(4) . . . . ? C8 N2 C1 N1 180.0(3) . . . . ? C1 N1 C2 C3 0.9(4) . . . . ? C4 N1 C2 C3 -179.6(3) . . . . ? N1 C2 C3 N2 -0.7(5) . . . . ? C1 N2 C3 C2 0.3(4) . . . . ? C8 N2 C3 C2 -179.4(3) . . . . ? C1 N1 C4 C5A -102.8(5) . . . . ? C2 N1 C4 C5A 77.8(5) . . . . ? C1 N1 C4 C7A 113.3(5) . . . . ? C2 N1 C4 C7A -66.1(5) . . . . ? C1 N1 C4 C6A -13.3(5) . . . . ? C2 N1 C4 C6A 167.3(4) . . . . ? C1 N1 C4 C6B 23.4(5) . . . . ? C2 N1 C4 C6B -156.0(4) . . . . ? C1 N1 C4 C7B 136.4(4) . . . . ? C2 N1 C4 C7B -43.0(5) . . . . ? C1 N1 C4 C5B -128.0(4) . . . . ? C2 N1 C4 C5B 52.6(5) . . . . ? C1 N2 C8 C10 121.3(4) . . . . ? C3 N2 C8 C10 -58.9(4) . . . . ? C1 N2 C8 C9 0.9(5) . . . . ? C3 N2 C8 C9 -179.3(4) . . . . ? C1 N2 C8 C11 -118.3(4) . . . . ? C3 N2 C8 C11 61.4(4) . . . . ? C16 Al1 C17 Al3 -31.9(13) . . . . ? C15 Al1 C17 Al3 -163.5(12) . . . . ? C12 Al1 C17 Al3 81.0(12) . . . . ? Al2 Al1 C17 Al3 96.3(13) . . . . ? C20 Al3 C17 Al1 -132.2(12) . . . . ? C18 Al3 C17 Al1 108.4(12) . . . . ? C19 Al3 C17 Al1 -6.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.529 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.063