# 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 'Wen-Hua Sun' _publ_contact_author_email WHSUN@ICCAS.AC.CN _publ_section_title ; Synthesis, Characterization of Organoaluminum Compounds Containing Quinolin-8-amine Derivatives and Their Catalytic Behavior for Ring-Opening Polymerization of ?-Caprolactone ; loop_ _publ_author_name 'Wen-Hua Sun' 'Kotohiro Nomura' 'Miao Shen' 'Wenjuan Zhang' # Attachment 'CIF.CIF' data_C1 _database_code_depnum_ccdc_archive 'CCDC 733377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C20H23AlN2 _chemical_formula_sum 'C20 H23 Al N2' _chemical_formula_weight 318.38 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 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 7.8202(16) _cell_length_b 17.248(3) _cell_length_c 13.612(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.82(3) _cell_angle_gamma 90.00 _cell_volume 1809.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 466(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.32 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9403 _exptl_absorpt_correction_T_max 0.9561 _exptl_special_details ; ? ; _diffrn_ambient_temperature 466(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 14768 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0116 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.32 _reflns_number_total 3307 _reflns_number_gt 3085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.0772P)^2^+0.9439P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3307 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_ref 0.0443 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.08202(7) 0.68410(3) 0.70954(4) 0.02785(18) Uani 1 1 d . . . N1 N -0.07072(17) 0.60909(8) 0.62394(10) 0.0257(3) Uani 1 1 d . . . N2 N 0.12877(17) 0.72404(8) 0.58805(10) 0.0250(3) Uani 1 1 d . . . C11 C 0.2498(2) 0.78364(9) 0.57344(11) 0.0236(3) Uani 1 1 d . . . C9 C -0.0637(2) 0.62230(9) 0.52500(12) 0.0235(3) Uani 1 1 d . . . C16 C 0.4194(2) 0.76331(10) 0.56259(12) 0.0273(4) Uani 1 1 d . . . C4 C -0.1572(2) 0.57700(10) 0.44768(13) 0.0274(4) Uani 1 1 d . . . C8 C 0.0459(2) 0.68501(9) 0.50539(12) 0.0229(3) Uani 1 1 d . . . C7 C 0.0568(2) 0.69912(10) 0.40593(13) 0.0284(4) Uani 1 1 d . . . H7A H 0.1271 0.7390 0.3900 0.034 Uiso 1 1 calc R . . C15 C 0.5373(2) 0.82181(11) 0.55083(14) 0.0332(4) Uani 1 1 d . . . H15A H 0.6498 0.8088 0.5434 0.040 Uiso 1 1 calc R . . C2 C -0.2633(2) 0.50372(10) 0.57568(15) 0.0353(4) Uani 1 1 d . . . H2A H -0.3301 0.4634 0.5942 0.042 Uiso 1 1 calc R . . C6 C -0.0370(2) 0.65383(11) 0.32945(13) 0.0337(4) Uani 1 1 d . . . H6A H -0.0274 0.6649 0.2638 0.040 Uiso 1 1 calc R . . C5 C -0.1421(2) 0.59394(11) 0.34784(14) 0.0334(4) Uani 1 1 d . . . H5A H -0.2024 0.5649 0.2956 0.040 Uiso 1 1 calc R . . C13 C 0.3217(3) 0.91841(10) 0.56057(14) 0.0354(4) Uani 1 1 d . . . H13A H 0.2900 0.9704 0.5600 0.042 Uiso 1 1 calc R . . C3 C -0.2581(2) 0.51595(10) 0.47733(15) 0.0340(4) Uani 1 1 d . . . H3A H -0.3212 0.4840 0.4294 0.041 Uiso 1 1 calc R . . C12 C 0.1996(2) 0.86169(10) 0.57184(12) 0.0284(4) Uani 1 1 d . . . C20 C 0.4750(3) 0.67994(11) 0.56236(17) 0.0404(5) Uani 1 1 d . . . H20A H 0.5944 0.6773 0.5543 0.061 Uiso 1 1 calc R . . H20B H 0.4044 0.6532 0.5083 0.061 Uiso 1 1 calc R . . H20C H 0.4616 0.6561 0.6243 0.061 Uiso 1 1 calc R . . C1 C -0.1688(2) 0.55136(10) 0.64941(14) 0.0319(4) Uani 1 1 d . . . C17 C 0.0169(3) 0.88480(12) 0.58084(17) 0.0420(5) Uani 1 1 d . . . H17A H 0.0069 0.9403 0.5784 0.063 Uiso 1 1 calc R . . H17B H -0.0095 0.8663 0.6431 0.063 Uiso 1 1 calc R . . H17C H -0.0629 0.8625 0.5268 0.063 Uiso 1 1 calc R . . C23 C 0.2733(3) 0.62632(12) 0.79007(15) 0.0432(5) Uani 1 1 d . . . H23A H 0.3475 0.6617 0.8319 0.065 Uiso 1 1 calc R . . H23B H 0.3389 0.5999 0.7468 0.065 Uiso 1 1 calc R . . H23C H 0.2267 0.5891 0.8309 0.065 Uiso 1 1 calc R . . C14 C 0.4891(3) 0.89871(11) 0.55014(14) 0.0368(4) Uani 1 1 d . . . H14A H 0.5690 0.9373 0.5427 0.044 Uiso 1 1 calc R . . C10 C -0.1764(3) 0.53967(13) 0.75760(16) 0.0478(5) Uani 1 1 d . . . H10A H -0.1043 0.5775 0.7965 0.072 Uiso 1 1 calc R . . H10B H -0.1358 0.4886 0.7774 0.072 Uiso 1 1 calc R . . H10C H -0.2940 0.5455 0.7682 0.072 Uiso 1 1 calc R . . C24 C -0.0562(3) 0.75050(15) 0.78224(16) 0.0504(6) Uani 1 1 d . . . H24A H 0.0189 0.7861 0.8232 0.076 Uiso 1 1 calc R . . H24B H -0.1163 0.7190 0.8236 0.076 Uiso 1 1 calc R . . H24C H -0.1389 0.7789 0.7357 0.076 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 0.0305(3) 0.0315(3) 0.0221(3) 0.00139(19) 0.0060(2) -0.0045(2) N1 0.0217(7) 0.0266(7) 0.0294(7) 0.0048(6) 0.0058(6) -0.0007(5) N2 0.0258(7) 0.0256(7) 0.0242(7) -0.0005(5) 0.0057(6) -0.0063(5) C11 0.0262(8) 0.0262(8) 0.0186(7) 0.0000(6) 0.0041(6) -0.0062(6) C9 0.0191(7) 0.0227(8) 0.0286(8) 0.0013(6) 0.0040(6) 0.0028(6) C16 0.0280(8) 0.0288(9) 0.0257(8) -0.0012(7) 0.0062(7) -0.0034(7) C4 0.0207(8) 0.0250(8) 0.0356(9) -0.0020(7) 0.0022(7) 0.0016(6) C8 0.0199(8) 0.0235(8) 0.0252(8) 0.0005(6) 0.0041(6) 0.0012(6) C7 0.0290(9) 0.0299(9) 0.0269(8) 0.0033(7) 0.0061(7) -0.0023(7) C15 0.0272(9) 0.0411(10) 0.0331(9) -0.0019(7) 0.0097(7) -0.0082(7) C2 0.0257(9) 0.0271(9) 0.0537(12) 0.0064(8) 0.0082(8) -0.0047(7) C6 0.0368(10) 0.0393(10) 0.0244(8) 0.0003(7) 0.0035(7) 0.0006(8) C5 0.0322(9) 0.0339(9) 0.0312(9) -0.0069(7) -0.0029(7) -0.0009(7) C13 0.0461(11) 0.0240(8) 0.0369(10) 0.0015(7) 0.0096(8) -0.0051(7) C3 0.0247(9) 0.0261(9) 0.0495(11) -0.0041(8) 0.0016(8) -0.0024(7) C12 0.0314(9) 0.0278(9) 0.0256(8) 0.0021(7) 0.0040(7) -0.0009(7) C20 0.0344(10) 0.0328(10) 0.0570(13) 0.0001(8) 0.0162(9) 0.0020(7) C1 0.0249(8) 0.0300(9) 0.0419(10) 0.0093(7) 0.0086(7) -0.0006(7) C17 0.0372(10) 0.0356(10) 0.0544(12) 0.0073(9) 0.0109(9) 0.0068(8) C23 0.0440(11) 0.0459(11) 0.0358(10) 0.0076(9) -0.0041(8) -0.0072(9) C14 0.0415(10) 0.0334(10) 0.0367(10) 0.0002(8) 0.0099(8) -0.0172(8) C10 0.0467(12) 0.0531(13) 0.0453(12) 0.0167(10) 0.0126(9) -0.0123(10) C24 0.0648(14) 0.0561(14) 0.0353(11) 0.0002(9) 0.0230(10) 0.0049(11) _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 1.8840(15) . ? Al1 C24 1.955(2) . ? Al1 C23 1.968(2) . ? Al1 N1 1.9958(16) . ? N1 C1 1.338(2) . ? N1 C9 1.376(2) . ? N2 C8 1.375(2) . ? N2 C11 1.434(2) . ? C11 C12 1.401(2) . ? C11 C16 1.404(2) . ? C9 C4 1.411(2) . ? C9 C8 1.433(2) . ? C16 C15 1.394(2) . ? C16 C20 1.502(2) . ? C4 C5 1.415(3) . ? C4 C3 1.415(2) . ? C8 C7 1.392(2) . ? C7 C6 1.404(3) . ? C15 C14 1.378(3) . ? C2 C3 1.363(3) . ? C2 C1 1.406(3) . ? C6 C5 1.369(3) . ? C13 C14 1.383(3) . ? C13 C12 1.393(3) . ? C12 C17 1.509(3) . ? C1 C10 1.498(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 N2 Al1 C24 115.90(9) . . ? N2 Al1 C23 115.55(8) . . ? C24 Al1 C23 116.60(10) . . ? N2 Al1 N1 84.90(6) . . ? C24 Al1 N1 110.35(9) . . ? C23 Al1 N1 108.62(8) . . ? C1 N1 C9 119.81(15) . . ? C1 N1 Al1 130.05(13) . . ? C9 N1 Al1 110.13(11) . . ? C8 N2 C11 117.89(13) . . ? C8 N2 Al1 113.84(11) . . ? C11 N2 Al1 127.98(10) . . ? C12 C11 C16 120.33(15) . . ? C12 C11 N2 120.11(15) . . ? C16 C11 N2 119.55(15) . . ? N1 C9 C4 122.42(15) . . ? N1 C9 C8 115.61(14) . . ? C4 C9 C8 121.97(15) . . ? C15 C16 C11 119.11(16) . . ? C15 C16 C20 119.69(16) . . ? C11 C16 C20 121.20(15) . . ? C9 C4 C5 118.98(15) . . ? C9 C4 C3 116.27(16) . . ? C5 C4 C3 124.74(16) . . ? N2 C8 C7 127.69(15) . . ? N2 C8 C9 115.51(14) . . ? C7 C8 C9 116.80(15) . . ? C8 C7 C6 120.85(16) . . ? C14 C15 C16 120.79(17) . . ? C3 C2 C1 120.71(16) . . ? C5 C6 C7 122.54(17) . . ? C6 C5 C4 118.86(16) . . ? C14 C13 C12 121.14(17) . . ? C2 C3 C4 120.47(17) . . ? C13 C12 C11 118.76(16) . . ? C13 C12 C17 119.98(16) . . ? C11 C12 C17 121.25(16) . . ? N1 C1 C2 120.32(17) . . ? N1 C1 C10 118.40(17) . . ? C2 C1 C10 121.27(16) . . ? C15 C14 C13 119.86(17) . . ? 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 N2 Al1 N1 C1 179.78(15) . . . . ? C24 Al1 N1 C1 -64.45(17) . . . . ? C23 Al1 N1 C1 64.52(17) . . . . ? N2 Al1 N1 C9 1.01(11) . . . . ? C24 Al1 N1 C9 116.78(12) . . . . ? C23 Al1 N1 C9 -114.25(12) . . . . ? C24 Al1 N2 C8 -111.40(14) . . . . ? C23 Al1 N2 C8 106.99(13) . . . . ? N1 Al1 N2 C8 -1.23(11) . . . . ? C24 Al1 N2 C11 74.97(16) . . . . ? C23 Al1 N2 C11 -66.65(16) . . . . ? N1 Al1 N2 C11 -174.86(14) . . . . ? C8 N2 C11 C12 99.90(18) . . . . ? Al1 N2 C11 C12 -86.69(18) . . . . ? C8 N2 C11 C16 -81.25(19) . . . . ? Al1 N2 C11 C16 92.15(17) . . . . ? C1 N1 C9 C4 0.2(2) . . . . ? Al1 N1 C9 C4 179.09(12) . . . . ? C1 N1 C9 C8 -179.54(14) . . . . ? Al1 N1 C9 C8 -0.62(17) . . . . ? C12 C11 C16 C15 0.4(2) . . . . ? N2 C11 C16 C15 -178.46(15) . . . . ? C12 C11 C16 C20 -178.96(17) . . . . ? N2 C11 C16 C20 2.2(2) . . . . ? N1 C9 C4 C5 -179.56(15) . . . . ? C8 C9 C4 C5 0.1(2) . . . . ? N1 C9 C4 C3 -0.8(2) . . . . ? C8 C9 C4 C3 178.88(14) . . . . ? C11 N2 C8 C7 -4.1(2) . . . . ? Al1 N2 C8 C7 -178.44(14) . . . . ? C11 N2 C8 C9 175.54(13) . . . . ? Al1 N2 C8 C9 1.22(18) . . . . ? N1 C9 C8 N2 -0.4(2) . . . . ? C4 C9 C8 N2 179.93(14) . . . . ? N1 C9 C8 C7 179.35(14) . . . . ? C4 C9 C8 C7 -0.4(2) . . . . ? N2 C8 C7 C6 -179.87(16) . . . . ? C9 C8 C7 C6 0.5(2) . . . . ? C11 C16 C15 C14 0.2(3) . . . . ? C20 C16 C15 C14 179.58(18) . . . . ? C8 C7 C6 C5 -0.4(3) . . . . ? C7 C6 C5 C4 0.1(3) . . . . ? C9 C4 C5 C6 0.0(3) . . . . ? C3 C4 C5 C6 -178.64(17) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C9 C4 C3 C2 0.7(2) . . . . ? C5 C4 C3 C2 179.39(17) . . . . ? C14 C13 C12 C11 0.6(3) . . . . ? C14 C13 C12 C17 -178.69(18) . . . . ? C16 C11 C12 C13 -0.8(2) . . . . ? N2 C11 C12 C13 178.05(15) . . . . ? C16 C11 C12 C17 178.49(16) . . . . ? N2 C11 C12 C17 -2.7(2) . . . . ? C9 N1 C1 C2 0.6(2) . . . . ? Al1 N1 C1 C2 -178.11(13) . . . . ? C9 N1 C1 C10 -178.73(16) . . . . ? Al1 N1 C1 C10 2.6(3) . . . . ? C3 C2 C1 N1 -0.6(3) . . . . ? C3 C2 C1 C10 178.63(18) . . . . ? C16 C15 C14 C13 -0.4(3) . . . . ? C12 C13 C14 C15 0.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.258 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.052 #===END data__C3 _database_code_depnum_ccdc_archive 'CCDC 733378' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H31 Al N2 ' _chemical_formula_moiety 'C24 H31 Al N2 ' _chemical_formula_weight 374.50 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 10.5638(15) _cell_length_b 10.5967(13) _cell_length_c 10.7857(15) _cell_angle_alpha 82.936(4) _cell_angle_beta 71.200(4) _cell_angle_gamma 77.647(4) _cell_volume 1114.6(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4163 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 24.4 _cell_measurement_temperature 193.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404.00 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.396 _exptl_absorpt_correction_T_max 0.994 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 8377 _diffrn_reflns_av_R_equivalents 0.083 _diffrn_reflns_theta_max 24.41 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3666 _reflns_number_gt 1794 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.0818 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1823 _refine_ls_number_parameters 275 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0024Fo^2^ + 1.0000\s(Fo^2^)]' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.31 _refine_diff_density_min -0.26 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Al Al 0.064 0.051 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al(1) Al 0.15515(17) 0.26501(15) 0.17979(17) 0.0452(5) Uani 1.00 1 d . . . N(1) N 0.2496(4) 0.0962(3) 0.1036(4) 0.0410(13) Uani 1.00 1 d . . . N(2) N 0.2367(3) 0.2062(3) 0.3128(3) 0.0355(12) Uani 1.00 1 d . . . C(1) C 0.2459(5) 0.0454(5) -0.0012(5) 0.0530(19) Uani 1.00 1 d . . . C(2) C 0.3195(6) -0.0789(5) -0.0373(6) 0.061(2) Uani 1.00 1 d . . . C(3) C 0.3972(5) -0.1491(5) 0.0365(5) 0.0536(18) Uani 1.00 1 d . . . C(4) C 0.4029(5) -0.0979(4) 0.1483(5) 0.0435(16) Uani 1.00 1 d . . . C(5) C 0.4812(5) -0.1642(4) 0.2294(5) 0.0482(17) Uani 1.00 1 d . . . C(6) C 0.4753(5) -0.1046(4) 0.3382(5) 0.0510(18) Uani 1.00 1 d . . . C(7) C 0.3952(5) 0.0181(4) 0.3728(5) 0.0425(16) Uani 1.00 1 d . . . C(8) C 0.3197(4) 0.0854(4) 0.2935(4) 0.0343(15) Uani 1.00 1 d . . . C(9) C 0.3258(4) 0.0258(4) 0.1804(4) 0.0354(15) Uani 1.00 1 d . . . C(10) C 0.1621(6) 0.1255(6) -0.0814(6) 0.077(2) Uani 1.00 1 d . . . C(11) C 0.2326(5) 0.2735(4) 0.4227(5) 0.0351(15) Uani 1.00 1 d . . . C(12) C 0.1200(5) 0.2747(4) 0.5366(5) 0.0401(16) Uani 1.00 1 d . . . C(13) C 0.1172(5) 0.3399(4) 0.6431(5) 0.0465(17) Uani 1.00 1 d . . . C(14) C 0.2231(6) 0.3989(4) 0.6390(5) 0.0508(19) Uani 1.00 1 d . . . C(15) C 0.3321(6) 0.3974(4) 0.5271(6) 0.0495(18) Uani 1.00 1 d . . . C(16) C 0.3390(5) 0.3341(4) 0.4165(5) 0.0376(16) Uani 1.00 1 d . . . C(17) C 0.0043(5) 0.2064(5) 0.5485(5) 0.0488(17) Uani 1.00 1 d . . . C(18) C 0.0129(6) 0.0816(5) 0.6362(6) 0.067(2) Uani 1.00 1 d . . . C(19) C -0.1360(6) 0.2926(6) 0.5990(6) 0.078(2) Uani 1.00 1 d . . . C(20) C 0.4597(5) 0.3390(4) 0.2954(5) 0.0515(19) Uani 1.00 1 d . . . C(21) C 0.5963(5) 0.2802(5) 0.3220(6) 0.069(2) Uani 1.00 1 d . . . C(22) C 0.4622(6) 0.4780(5) 0.2365(6) 0.076(2) Uani 1.00 1 d . . . C(23) C -0.0403(5) 0.2720(5) 0.2212(6) 0.062(2) Uani 1.00 1 d . . . C(24) C 0.2253(6) 0.4096(5) 0.0639(6) 0.072(2) Uani 1.00 1 d . . . H(1) H 0.3146 -0.1191 -0.1237 0.077 Uiso 1.00 1 c R . . H(2) H 0.4548 -0.2451 0.0084 0.062 Uiso 1.00 1 c R . . H(3) H 0.5434 -0.2584 0.2067 0.056 Uiso 1.00 1 c R . . H(4) H 0.5285 -0.1488 0.3932 0.061 Uiso 1.00 1 c R . . H(5) H 0.3926 0.0596 0.4613 0.054 Uiso 1.00 1 c R . . H(6) H 0.1479 0.2179 -0.0643 0.097 Uiso 1.00 1 c R . . H(7) H 0.2100 0.1133 -0.1757 0.097 Uiso 1.00 1 c R . . H(8) H 0.0728 0.0981 -0.0573 0.097 Uiso 1.00 1 c R . . H(9) H 0.0415 0.3436 0.7190 0.054 Uiso 1.00 1 c R . . H(10) H 0.2202 0.4464 0.7242 0.060 Uiso 1.00 1 c R . . H(11) H 0.4146 0.4458 0.5235 0.062 Uiso 1.00 1 c R . . H(12) H 0.0151 0.1795 0.4508 0.058 Uiso 1.00 1 c R . . H(13) H -0.0719 0.0348 0.6441 0.083 Uiso 1.00 1 c R . . H(14) H 0.1086 0.0166 0.5934 0.083 Uiso 1.00 1 c R . . H(15) H 0.0083 0.1047 0.7335 0.083 Uiso 1.00 1 c R . . H(16) H -0.1519 0.3125 0.6897 0.093 Uiso 1.00 1 c R . . H(17) H -0.1395 0.3732 0.5438 0.093 Uiso 1.00 1 c R . . H(18) H -0.2064 0.2472 0.5956 0.093 Uiso 1.00 1 c R . . H(19) H 0.4497 0.2842 0.2255 0.064 Uiso 1.00 1 c R . . H(20) H 0.6770 0.3053 0.2425 0.084 Uiso 1.00 1 c R . . H(21) H 0.5979 0.3163 0.4078 0.084 Uiso 1.00 1 c R . . H(22) H 0.6068 0.1790 0.3339 0.084 Uiso 1.00 1 c R . . H(23) H 0.3699 0.5173 0.2194 0.087 Uiso 1.00 1 c R . . H(24) H 0.4776 0.5335 0.3016 0.087 Uiso 1.00 1 c R . . H(25) H 0.5407 0.4777 0.1485 0.087 Uiso 1.00 1 c R . . H(27) H -0.0937 0.3357 0.2973 0.074 Uiso 1.00 1 c R . . H(28) H -0.0707 0.3058 0.1366 0.074 Uiso 1.00 1 c R . . H(29) H -0.0626 0.1781 0.2521 0.074 Uiso 1.00 1 c R . . H(31) H 0.1727 0.4364 -0.0069 0.086 Uiso 1.00 1 c R . . H(32) H 0.2102 0.4896 0.1204 0.086 Uiso 1.00 1 c R . . H(33) H 0.3306 0.3805 0.0157 0.086 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al(1) 0.0444(11) 0.0500(9) 0.0408(11) -0.0073(7) -0.0161(8) 0.0045(7) N(1) 0.036(2) 0.058(2) 0.030(2) -0.017(2) -0.008(2) 0.003(2) N(2) 0.037(2) 0.037(2) 0.032(2) -0.007(2) -0.009(2) -0.0018(19) C(1) 0.055(4) 0.073(3) 0.038(3) -0.020(3) -0.019(3) -0.004(3) C(2) 0.072(4) 0.072(4) 0.048(4) -0.022(3) -0.019(3) -0.018(3) C(3) 0.057(4) 0.049(3) 0.048(4) -0.009(2) -0.004(3) -0.011(2) C(4) 0.046(3) 0.047(3) 0.037(3) -0.017(2) -0.004(2) -0.008(2) C(5) 0.048(3) 0.034(2) 0.057(4) -0.003(2) -0.012(3) -0.002(2) C(6) 0.056(4) 0.045(3) 0.053(4) -0.001(2) -0.024(3) 0.002(2) C(7) 0.048(3) 0.046(3) 0.040(3) -0.006(2) -0.026(2) -0.001(2) C(8) 0.031(3) 0.038(2) 0.032(3) -0.015(2) -0.002(2) -0.002(2) C(9) 0.033(3) 0.042(2) 0.034(3) -0.013(2) -0.010(2) -0.000(2) C(10) 0.084(5) 0.108(5) 0.050(4) -0.014(4) -0.039(4) -0.002(3) C(11) 0.037(3) 0.031(2) 0.036(3) -0.004(2) -0.013(2) 0.002(2) C(12) 0.040(3) 0.039(2) 0.042(3) -0.008(2) -0.016(2) 0.006(2) C(13) 0.051(3) 0.048(3) 0.037(3) -0.005(2) -0.011(3) -0.001(2) C(14) 0.061(4) 0.050(3) 0.039(3) -0.005(3) -0.015(3) -0.006(2) C(15) 0.057(4) 0.041(2) 0.056(4) -0.015(2) -0.021(3) -0.004(2) C(16) 0.034(3) 0.041(2) 0.041(3) -0.012(2) -0.013(2) -0.000(2) C(17) 0.043(3) 0.068(3) 0.034(3) -0.016(3) -0.009(2) 0.006(2) C(18) 0.078(5) 0.066(3) 0.063(4) -0.036(3) -0.022(3) 0.007(3) C(19) 0.054(4) 0.103(5) 0.074(5) -0.013(3) -0.017(3) -0.004(3) C(20) 0.047(3) 0.055(3) 0.058(4) -0.019(2) -0.014(3) -0.011(2) C(21) 0.044(3) 0.088(4) 0.078(5) -0.019(3) -0.009(3) -0.031(3) C(22) 0.077(5) 0.078(4) 0.063(4) -0.033(3) -0.001(3) 0.005(3) C(23) 0.052(4) 0.073(4) 0.059(4) -0.004(3) -0.024(3) 0.007(3) C(24) 0.082(5) 0.073(3) 0.060(4) -0.015(3) -0.029(4) 0.020(3) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Al(1) N(1) 1.985(4) yes . . Al(1) N(2) 1.880(4) yes . . Al(1) C(23) 1.954(6) yes . . Al(1) C(24) 1.968(6) yes . . N(1) C(1) 1.325(8) yes . . N(1) C(9) 1.382(6) yes . . N(2) C(8) 1.385(5) yes . . N(2) C(11) 1.441(7) yes . . C(1) C(2) 1.409(7) yes . . C(1) C(10) 1.498(9) yes . . C(2) C(3) 1.370(9) yes . . C(3) C(4) 1.404(9) yes . . C(4) C(5) 1.418(8) yes . . C(4) C(9) 1.405(6) yes . . C(5) C(6) 1.377(9) yes . . C(6) C(7) 1.411(6) yes . . C(7) C(8) 1.387(7) yes . . C(8) C(9) 1.418(7) yes . . C(11) C(12) 1.406(6) yes . . C(11) C(16) 1.390(8) yes . . C(12) C(13) 1.401(8) yes . . C(12) C(17) 1.513(8) yes . . C(13) C(14) 1.380(9) yes . . C(14) C(15) 1.372(7) yes . . C(15) C(16) 1.414(8) yes . . C(16) C(20) 1.507(6) yes . . C(17) C(18) 1.532(7) yes . . C(17) C(19) 1.533(7) yes . . C(20) C(21) 1.547(8) yes . . C(20) C(22) 1.533(7) yes . . C(2) H(1) 1.090 no . . C(3) H(2) 1.090 no . . C(5) H(3) 1.080 no . . C(6) H(4) 0.960 no . . C(7) H(5) 1.090 no . . C(10) H(6) 0.990 no . . C(10) H(7) 0.990 no . . C(10) H(8) 0.990 no . . C(13) H(9) 0.940 no . . C(14) H(10) 1.090 no . . C(15) H(11) 1.090 no . . C(17) H(12) 1.090 no . . C(18) H(13) 1.090 no . . C(18) H(14) 1.090 no . . C(18) H(15) 1.090 no . . C(19) H(16) 0.980 no . . C(19) H(17) 0.980 no . . C(19) H(18) 0.980 no . . C(20) H(19) 1.050 no . . C(21) H(20) 1.050 no . . C(21) H(21) 1.050 no . . C(21) H(22) 1.050 no . . C(22) H(23) 1.040 no . . C(22) H(24) 1.040 no . . C(22) H(25) 1.040 no . . C(23) H(27) 1.060 no . . C(23) H(28) 1.060 no . . C(23) H(29) 1.060 no . . C(24) H(31) 1.060 no . . C(24) H(32) 1.060 no . . C(24) H(33) 1.060 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 N(1) Al(1) N(2) 85.18(18) yes . . . N(1) Al(1) C(23) 107.5(2) yes . . . N(1) Al(1) C(24) 111.1(2) yes . . . N(2) Al(1) C(23) 118.4(2) yes . . . N(2) Al(1) C(24) 115.0(2) yes . . . C(23) Al(1) C(24) 115.0(2) yes . . . Al(1) N(1) C(1) 130.3(3) yes . . . Al(1) N(1) C(9) 109.9(3) yes . . . C(1) N(1) C(9) 119.7(4) yes . . . Al(1) N(2) C(8) 113.5(3) yes . . . Al(1) N(2) C(11) 128.8(2) yes . . . C(8) N(2) C(11) 117.4(4) yes . . . N(1) C(1) C(2) 121.3(5) yes . . . N(1) C(1) C(10) 117.8(4) yes . . . C(2) C(1) C(10) 120.9(6) yes . . . C(1) C(2) C(3) 119.7(6) yes . . . C(2) C(3) C(4) 120.2(4) yes . . . C(3) C(4) C(5) 123.7(4) yes . . . C(3) C(4) C(9) 117.5(5) yes . . . C(5) C(4) C(9) 118.9(5) yes . . . C(4) C(5) C(6) 118.0(4) yes . . . C(5) C(6) C(7) 123.4(5) yes . . . C(6) C(7) C(8) 119.6(5) yes . . . N(2) C(8) C(7) 126.9(4) yes . . . N(2) C(8) C(9) 115.4(4) yes . . . C(7) C(8) C(9) 117.7(4) yes . . . N(1) C(9) C(4) 121.5(5) yes . . . N(1) C(9) C(8) 115.9(3) yes . . . C(4) C(9) C(8) 122.5(4) yes . . . N(2) C(11) C(12) 118.7(5) yes . . . N(2) C(11) C(16) 120.4(4) yes . . . C(12) C(11) C(16) 120.9(5) yes . . . C(11) C(12) C(13) 118.3(5) yes . . . C(11) C(12) C(17) 122.4(5) yes . . . C(13) C(12) C(17) 119.3(4) yes . . . C(12) C(13) C(14) 121.4(4) yes . . . C(13) C(14) C(15) 119.7(6) yes . . . C(14) C(15) C(16) 121.0(6) yes . . . C(11) C(16) C(15) 118.7(4) yes . . . C(11) C(16) C(20) 122.9(5) yes . . . C(15) C(16) C(20) 118.4(5) yes . . . C(12) C(17) C(18) 110.8(5) yes . . . C(12) C(17) C(19) 112.9(4) yes . . . C(18) C(17) C(19) 110.2(4) yes . . . C(16) C(20) C(21) 112.5(5) yes . . . C(16) C(20) C(22) 111.0(4) yes . . . C(21) C(20) C(22) 109.8(5) yes . . . C(1) C(2) H(1) 120.2 no . . . C(3) C(2) H(1) 120.2 no . . . C(2) C(3) H(2) 119.9 no . . . C(4) C(3) H(2) 119.9 no . . . C(4) C(5) H(3) 121.0 no . . . C(6) C(5) H(3) 121.0 no . . . C(5) C(6) H(4) 118.3 no . . . C(7) C(6) H(4) 118.3 no . . . C(6) C(7) H(5) 120.2 no . . . C(8) C(7) H(5) 120.2 no . . . C(1) C(10) H(6) 109.5 no . . . C(1) C(10) H(7) 109.5 no . . . C(1) C(10) H(8) 109.5 no . . . H(6) C(10) H(7) 109.5 no . . . H(6) C(10) H(8) 109.5 no . . . H(7) C(10) H(8) 109.5 no . . . C(12) C(13) H(9) 119.3 no . . . C(14) C(13) H(9) 119.3 no . . . C(13) C(14) H(10) 120.2 no . . . C(15) C(14) H(10) 120.2 no . . . C(14) C(15) H(11) 119.5 no . . . C(16) C(15) H(11) 119.5 no . . . C(12) C(17) H(12) 107.6 no . . . C(18) C(17) H(12) 107.6 no . . . C(19) C(17) H(12) 107.6 no . . . C(17) C(18) H(13) 109.5 no . . . C(17) C(18) H(14) 109.5 no . . . C(17) C(18) H(15) 109.5 no . . . H(13) C(18) H(14) 109.5 no . . . H(13) C(18) H(15) 109.5 no . . . H(14) C(18) H(15) 109.5 no . . . C(17) C(19) H(16) 109.5 no . . . C(17) C(19) H(17) 109.5 no . . . C(17) C(19) H(18) 109.5 no . . . H(16) C(19) H(17) 109.5 no . . . H(16) C(19) H(18) 109.5 no . . . H(17) C(19) H(18) 109.5 no . . . C(16) C(20) H(19) 107.8 no . . . C(21) C(20) H(19) 107.8 no . . . C(22) C(20) H(19) 107.8 no . . . C(20) C(21) H(20) 109.5 no . . . C(20) C(21) H(21) 109.5 no . . . C(20) C(21) H(22) 109.5 no . . . H(20) C(21) H(21) 109.5 no . . . H(20) C(21) H(22) 109.5 no . . . H(21) C(21) H(22) 109.5 no . . . C(20) C(22) H(23) 109.5 no . . . C(20) C(22) H(24) 109.5 no . . . C(20) C(22) H(25) 109.5 no . . . H(23) C(22) H(24) 109.5 no . . . H(23) C(22) H(25) 109.5 no . . . H(24) C(22) H(25) 109.5 no . . . Al(1) C(23) H(27) 109.5 no . . . Al(1) C(23) H(28) 109.5 no . . . Al(1) C(23) H(29) 109.5 no . . . H(27) C(23) H(28) 109.5 no . . . H(27) C(23) H(29) 109.5 no . . . H(28) C(23) H(29) 109.5 no . . . Al(1) C(24) H(31) 109.5 no . . . Al(1) C(24) H(32) 109.5 no . . . Al(1) C(24) H(33) 109.5 no . . . H(31) C(24) H(32) 109.5 no . . . H(31) C(24) H(33) 109.5 no . . . H(32) C(24) H(33) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N(1) Al(1) N(2) C(8) 1.7(3) ? . . . . N(1) Al(1) N(2) C(11) 176.2(4) ? . . . . N(2) Al(1) N(1) C(1) 176.8(4) ? . . . . N(2) Al(1) N(1) C(9) -1.3(3) ? . . . . C(23) Al(1) N(1) C(1) 58.5(5) ? . . . . C(23) Al(1) N(1) C(9) -119.6(3) ? . . . . C(24) Al(1) N(1) C(1) -68.3(5) ? . . . . C(24) Al(1) N(1) C(9) 113.7(3) ? . . . . C(23) Al(1) N(2) C(8) 109.0(3) ? . . . . C(23) Al(1) N(2) C(11) -76.4(4) ? . . . . C(24) Al(1) N(2) C(8) -109.4(3) ? . . . . C(24) Al(1) N(2) C(11) 65.1(4) ? . . . . Al(1) N(1) C(1) C(2) -178.6(4) ? . . . . Al(1) N(1) C(1) C(10) 2.2(7) ? . . . . Al(1) N(1) C(9) C(4) 179.9(3) ? . . . . Al(1) N(1) C(9) C(8) 0.7(5) ? . . . . C(1) N(1) C(9) C(4) 1.6(7) ? . . . . C(1) N(1) C(9) C(8) -177.6(4) ? . . . . C(9) N(1) C(1) C(2) -0.7(7) ? . . . . C(9) N(1) C(1) C(10) -179.9(3) ? . . . . Al(1) N(2) C(8) C(7) 178.7(4) ? . . . . Al(1) N(2) C(8) C(9) -1.7(5) ? . . . . Al(1) N(2) C(11) C(12) 83.4(5) ? . . . . Al(1) N(2) C(11) C(16) -97.6(5) ? . . . . C(8) N(2) C(11) C(12) -102.2(5) ? . . . . C(8) N(2) C(11) C(16) 76.8(5) ? . . . . C(11) N(2) C(8) C(7) 3.5(6) ? . . . . C(11) N(2) C(8) C(9) -176.9(4) ? . . . . N(1) C(1) C(2) C(3) -0.3(7) ? . . . . C(10) C(1) C(2) C(3) 178.9(5) ? . . . . C(1) C(2) C(3) C(4) 0.5(8) ? . . . . C(2) C(3) C(4) C(5) -179.7(5) ? . . . . C(2) C(3) C(4) C(9) 0.4(7) ? . . . . C(3) C(4) C(5) C(6) -178.4(5) ? . . . . C(3) C(4) C(9) N(1) -1.5(7) ? . . . . C(3) C(4) C(9) C(8) 177.7(4) ? . . . . C(5) C(4) C(9) N(1) 178.7(4) ? . . . . C(5) C(4) C(9) C(8) -2.2(7) ? . . . . C(9) C(4) C(5) C(6) 1.4(7) ? . . . . C(4) C(5) C(6) C(7) 0.3(7) ? . . . . C(5) C(6) C(7) C(8) -1.4(8) ? . . . . C(6) C(7) C(8) N(2) -179.7(4) ? . . . . C(6) C(7) C(8) C(9) 0.7(7) ? . . . . N(2) C(8) C(9) N(1) 0.6(6) ? . . . . N(2) C(8) C(9) C(4) -178.6(4) ? . . . . C(7) C(8) C(9) N(1) -179.7(4) ? . . . . C(7) C(8) C(9) C(4) 1.1(7) ? . . . . N(2) C(11) C(12) C(13) 179.7(4) ? . . . . N(2) C(11) C(12) C(17) 0.9(6) ? . . . . N(2) C(11) C(16) C(15) -179.0(4) ? . . . . N(2) C(11) C(16) C(20) 2.9(7) ? . . . . C(12) C(11) C(16) C(15) -0.0(5) ? . . . . C(12) C(11) C(16) C(20) -178.1(4) ? . . . . C(16) C(11) C(12) C(13) 0.7(7) ? . . . . C(16) C(11) C(12) C(17) -178.1(4) ? . . . . C(11) C(12) C(13) C(14) -1.7(7) ? . . . . C(11) C(12) C(17) C(18) 104.9(5) ? . . . . C(11) C(12) C(17) C(19) -131.0(5) ? . . . . C(13) C(12) C(17) C(18) -73.9(5) ? . . . . C(13) C(12) C(17) C(19) 50.2(6) ? . . . . C(17) C(12) C(13) C(14) 177.2(4) ? . . . . C(12) C(13) C(14) C(15) 2.0(7) ? . . . . C(13) C(14) C(15) C(16) -1.3(7) ? . . . . C(14) C(15) C(16) C(11) 0.3(7) ? . . . . C(14) C(15) C(16) C(20) 178.5(4) ? . . . . C(11) C(16) C(20) C(21) -122.9(5) ? . . . . C(11) C(16) C(20) C(22) 113.6(6) ? . . . . C(15) C(16) C(20) C(21) 59.1(6) ? . . . . C(15) C(16) C(20) C(22) -64.5(7) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C(1) C(5) 3.489(7) ? . 2_655 C(3) C(9) 3.495(7) ? . 2_655 C(5) C(1) 3.489(7) ? . 2_655 C(9) C(3) 3.495(7) ? . 2_655 N(1) H(2) 3.592 ? . 2_655 N(1) H(13) 3.122 ? . 2_556 N(2) H(13) 3.295 ? . 2_556 C(1) H(3) 3.563 ? . 2_655 C(2) H(19) 3.228 ? . 2_655 C(2) H(20) 3.444 ? . 2_655 C(2) H(22) 3.292 ? . 2_655 C(3) H(19) 3.116 ? . 2_655 C(3) H(33) 3.298 ? . 2_655 C(4) H(13) 3.465 ? . 2_556 C(4) H(18) 3.328 ? . 2_556 C(5) H(7) 3.275 ? . 2_655 C(5) H(18) 3.148 ? . 2_556 C(5) H(24) 3.208 ? . 1_545 C(5) H(33) 3.515 ? . 2_655 C(6) H(5) 3.054 ? . 2_656 C(6) H(7) 3.207 ? . 2_655 C(6) H(18) 3.335 ? . 2_556 C(6) H(21) 3.317 ? . 2_656 C(6) H(22) 3.393 ? . 2_656 C(7) H(4) 3.404 ? . 2_656 C(7) H(5) 3.214 ? . 2_656 C(7) H(22) 3.566 ? . 2_656 C(8) H(13) 3.001 ? . 2_556 C(9) H(13) 2.890 ? . 2_556 C(10) H(3) 3.491 ? . 2_655 C(10) H(9) 3.298 ? . 1_554 C(10) H(15) 3.003 ? . 1_554 C(13) H(6) 3.348 ? . 1_556 C(13) H(7) 3.102 ? . 1_556 C(13) H(17) 3.443 ? . 2_566 C(13) H(27) 3.516 ? . 2_566 C(14) H(3) 3.396 ? . 2_656 C(14) H(4) 3.270 ? . 2_656 C(14) H(6) 3.472 ? . 1_556 C(14) H(7) 3.418 ? . 1_556 C(14) H(17) 3.089 ? . 2_566 C(14) H(27) 2.911 ? . 2_566 C(15) H(3) 3.564 ? . 2_656 C(15) H(4) 2.906 ? . 2_656 C(15) H(11) 3.310 ? . 2_666 C(15) H(17) 3.010 ? . 2_566 C(15) H(21) 3.472 ? . 2_666 C(15) H(24) 3.368 ? . 2_666 C(16) H(4) 3.116 ? . 2_656 C(16) H(17) 3.345 ? . 2_566 C(17) H(13) 3.306 ? . 2_556 C(17) H(14) 3.553 ? . 2_556 C(18) H(7) 3.428 ? . 1_556 C(18) H(8) 3.591 ? . 1_556 C(18) H(12) 3.129 ? . 2_556 C(18) H(13) 3.229 ? . 2_556 C(18) H(14) 3.481 ? . 2_556 C(18) H(29) 2.877 ? . 2_556 C(19) H(23) 3.118 ? . 2_566 C(19) H(24) 3.566 ? . 2_566 C(20) H(1) 3.222 ? . 2_655 C(20) H(2) 3.325 ? . 2_655 C(21) H(1) 2.700 ? . 2_655 C(21) H(4) 3.199 ? . 2_656 C(21) H(11) 3.485 ? . 2_666 C(21) H(27) 3.371 ? . 1_655 C(21) H(28) 3.491 ? . 1_655 C(21) H(29) 3.391 ? . 1_655 C(22) H(2) 3.594 ? . 1_565 C(22) H(3) 3.044 ? . 1_565 C(22) H(11) 3.490 ? . 2_666 C(22) H(16) 3.456 ? . 2_566 C(22) H(33) 3.317 ? . 2_665 C(23) H(10) 3.186 ? . 2_566 C(23) H(13) 3.519 ? . 2_556 C(23) H(14) 3.519 ? . 2_556 C(23) H(20) 2.867 ? . 1_455 C(24) H(2) 3.344 ? . 2_655 C(24) H(3) 3.454 ? . 2_655 C(24) H(25) 3.118 ? . 2_665 H(1) C(20) 3.222 ? . 2_655 H(1) C(21) 2.700 ? . 2_655 H(1) H(19) 2.704 ? . 2_655 H(1) H(20) 2.453 ? . 2_655 H(1) H(22) 2.269 ? . 2_655 H(1) H(29) 3.564 ? . 2_555 H(2) N(1) 3.592 ? . 2_655 H(2) C(20) 3.325 ? . 2_655 H(2) C(22) 3.594 ? . 1_545 H(2) C(24) 3.344 ? . 2_655 H(2) H(19) 2.448 ? . 2_655 H(2) H(20) 3.592 ? . 2_655 H(2) H(23) 3.250 ? . 1_545 H(2) H(25) 3.222 ? . 1_545 H(2) H(25) 3.142 ? . 2_655 H(2) H(33) 2.363 ? . 2_655 H(3) C(1) 3.563 ? . 2_655 H(3) C(10) 3.491 ? . 2_655 H(3) C(14) 3.396 ? . 2_656 H(3) C(15) 3.564 ? . 2_656 H(3) C(22) 3.044 ? . 1_545 H(3) C(24) 3.454 ? . 2_655 H(3) H(6) 3.223 ? . 2_655 H(3) H(7) 3.207 ? . 2_655 H(3) H(10) 3.076 ? . 2_656 H(3) H(11) 3.412 ? . 2_656 H(3) H(18) 3.496 ? . 2_556 H(3) H(23) 3.264 ? . 1_545 H(3) H(24) 2.457 ? . 1_545 H(3) H(25) 2.948 ? . 1_545 H(3) H(31) 3.407 ? . 2_655 H(3) H(33) 2.677 ? . 2_655 H(4) C(7) 3.404 ? . 2_656 H(4) C(14) 3.270 ? . 2_656 H(4) C(15) 2.906 ? . 2_656 H(4) C(16) 3.116 ? . 2_656 H(4) C(21) 3.199 ? . 2_656 H(4) H(5) 2.364 ? . 2_656 H(4) H(7) 3.054 ? . 2_655 H(4) H(11) 3.149 ? . 2_656 H(4) H(21) 2.788 ? . 2_656 H(4) H(22) 2.839 ? . 2_656 H(5) C(6) 3.054 ? . 2_656 H(5) C(7) 3.214 ? . 2_656 H(5) H(4) 2.364 ? . 2_656 H(5) H(5) 2.678 ? . 2_656 H(5) H(22) 3.146 ? . 2_656 H(6) C(13) 3.348 ? . 1_554 H(6) C(14) 3.472 ? . 1_554 H(6) H(3) 3.223 ? . 2_655 H(6) H(9) 2.964 ? . 1_554 H(6) H(10) 3.156 ? . 1_554 H(6) H(15) 3.441 ? . 1_554 H(7) C(5) 3.275 ? . 2_655 H(7) C(6) 3.207 ? . 2_655 H(7) C(13) 3.102 ? . 1_554 H(7) C(14) 3.418 ? . 1_554 H(7) C(18) 3.428 ? . 1_554 H(7) H(3) 3.207 ? . 2_655 H(7) H(4) 3.054 ? . 2_655 H(7) H(9) 3.029 ? . 1_554 H(7) H(10) 3.576 ? . 1_554 H(7) H(14) 3.349 ? . 1_554 H(7) H(15) 2.637 ? . 1_554 H(7) H(22) 3.585 ? . 2_655 H(8) C(18) 3.591 ? . 1_554 H(8) H(8) 2.781 ? . 2_555 H(8) H(9) 3.361 ? . 1_554 H(8) H(15) 2.548 ? . 1_554 H(9) C(10) 3.298 ? . 1_556 H(9) H(6) 2.964 ? . 1_556 H(9) H(7) 3.029 ? . 1_556 H(9) H(8) 3.361 ? . 1_556 H(9) H(27) 3.532 ? . 2_566 H(9) H(32) 2.995 ? . 2_566 H(10) C(23) 3.186 ? . 2_566 H(10) H(3) 3.076 ? . 2_656 H(10) H(6) 3.156 ? . 1_556 H(10) H(7) 3.576 ? . 1_556 H(10) H(17) 3.503 ? . 2_566 H(10) H(20) 3.153 ? . 2_666 H(10) H(21) 3.386 ? . 2_666 H(10) H(24) 3.165 ? . 2_666 H(10) H(25) 3.505 ? . 2_666 H(10) H(27) 2.433 ? . 2_566 H(10) H(28) 3.052 ? . 2_566 H(10) H(31) 2.772 ? . 1_556 H(11) C(15) 3.310 ? . 2_666 H(11) C(21) 3.485 ? . 2_666 H(11) C(22) 3.490 ? . 2_666 H(11) H(3) 3.412 ? . 2_656 H(11) H(4) 3.149 ? . 2_656 H(11) H(11) 2.233 ? . 2_666 H(11) H(17) 3.359 ? . 2_566 H(11) H(21) 2.678 ? . 2_666 H(11) H(24) 2.548 ? . 2_666 H(12) C(18) 3.129 ? . 2_556 H(12) H(13) 2.481 ? . 2_556 H(12) H(14) 2.838 ? . 2_556 H(13) N(1) 3.122 ? . 2_556 H(13) N(2) 3.295 ? . 2_556 H(13) C(4) 3.465 ? . 2_556 H(13) C(8) 3.001 ? . 2_556 H(13) C(9) 2.890 ? . 2_556 H(13) C(17) 3.306 ? . 2_556 H(13) C(18) 3.229 ? . 2_556 H(13) C(23) 3.519 ? . 2_556 H(13) H(12) 2.481 ? . 2_556 H(13) H(13) 3.091 ? . 2_556 H(13) H(14) 2.843 ? . 2_556 H(13) H(29) 2.719 ? . 2_556 H(14) C(17) 3.553 ? . 2_556 H(14) C(18) 3.481 ? . 2_556 H(14) C(23) 3.519 ? . 2_556 H(14) H(7) 3.349 ? . 1_556 H(14) H(12) 2.838 ? . 2_556 H(14) H(13) 2.843 ? . 2_556 H(14) H(14) 3.597 ? . 2_556 H(14) H(18) 3.441 ? . 2_556 H(14) H(22) 3.522 ? . 2_656 H(14) H(29) 2.517 ? . 2_556 H(15) C(10) 3.003 ? . 1_556 H(15) H(6) 3.441 ? . 1_556 H(15) H(7) 2.637 ? . 1_556 H(15) H(8) 2.548 ? . 1_556 H(15) H(29) 2.923 ? . 2_556 H(16) C(22) 3.456 ? . 2_566 H(16) H(23) 2.592 ? . 2_566 H(16) H(24) 3.456 ? . 2_566 H(16) H(32) 2.943 ? . 2_566 H(17) C(13) 3.443 ? . 2_566 H(17) C(14) 3.089 ? . 2_566 H(17) C(15) 3.010 ? . 2_566 H(17) C(16) 3.345 ? . 2_566 H(17) H(10) 3.503 ? . 2_566 H(17) H(11) 3.359 ? . 2_566 H(17) H(23) 3.051 ? . 2_566 H(17) H(24) 3.402 ? . 2_566 H(18) C(4) 3.328 ? . 2_556 H(18) C(5) 3.148 ? . 2_556 H(18) C(6) 3.335 ? . 2_556 H(18) H(3) 3.496 ? . 2_556 H(18) H(14) 3.441 ? . 2_556 H(18) H(21) 3.256 ? . 1_455 H(18) H(23) 3.218 ? . 2_566 H(18) H(24) 3.253 ? . 2_566 H(19) C(2) 3.228 ? . 2_655 H(19) C(3) 3.116 ? . 2_655 H(19) H(1) 2.704 ? . 2_655 H(19) H(2) 2.448 ? . 2_655 H(20) C(2) 3.444 ? . 2_655 H(20) C(23) 2.867 ? . 1_655 H(20) H(1) 2.453 ? . 2_655 H(20) H(2) 3.592 ? . 2_655 H(20) H(10) 3.153 ? . 2_666 H(20) H(27) 2.762 ? . 1_655 H(20) H(28) 2.540 ? . 1_655 H(20) H(29) 2.821 ? . 1_655 H(21) C(6) 3.317 ? . 2_656 H(21) C(15) 3.472 ? . 2_666 H(21) H(4) 2.788 ? . 2_656 H(21) H(10) 3.386 ? . 2_666 H(21) H(11) 2.678 ? . 2_666 H(21) H(18) 3.256 ? . 1_655 H(21) H(24) 3.473 ? . 2_666 H(21) H(27) 3.130 ? . 1_655 H(21) H(29) 3.507 ? . 1_655 H(22) C(2) 3.292 ? . 2_655 H(22) C(6) 3.393 ? . 2_656 H(22) C(7) 3.566 ? . 2_656 H(22) H(1) 2.269 ? . 2_655 H(22) H(4) 2.839 ? . 2_656 H(22) H(5) 3.146 ? . 2_656 H(22) H(7) 3.585 ? . 2_655 H(22) H(14) 3.522 ? . 2_656 H(22) H(29) 3.313 ? . 1_655 H(23) C(19) 3.118 ? . 2_566 H(23) H(2) 3.250 ? . 1_565 H(23) H(3) 3.264 ? . 1_565 H(23) H(16) 2.592 ? . 2_566 H(23) H(17) 3.051 ? . 2_566 H(23) H(18) 3.218 ? . 2_566 H(24) C(5) 3.208 ? . 1_565 H(24) C(15) 3.368 ? . 2_666 H(24) C(19) 3.566 ? . 2_566 H(24) H(3) 2.457 ? . 1_565 H(24) H(10) 3.165 ? . 2_666 H(24) H(11) 2.548 ? . 2_666 H(24) H(16) 3.456 ? . 2_566 H(24) H(17) 3.402 ? . 2_566 H(24) H(18) 3.253 ? . 2_566 H(24) H(21) 3.473 ? . 2_666 H(24) H(33) 3.493 ? . 2_665 H(25) C(24) 3.118 ? . 2_665 H(25) H(2) 3.222 ? . 1_565 H(25) H(2) 3.142 ? . 2_655 H(25) H(3) 2.948 ? . 1_565 H(25) H(10) 3.505 ? . 2_666 H(25) H(25) 3.529 ? . 2_665 H(25) H(31) 3.191 ? . 2_665 H(25) H(32) 3.268 ? . 2_665 H(25) H(33) 2.431 ? . 2_665 H(27) C(13) 3.516 ? . 2_566 H(27) C(14) 2.911 ? . 2_566 H(27) C(21) 3.371 ? . 1_455 H(27) H(9) 3.532 ? . 2_566 H(27) H(10) 2.433 ? . 2_566 H(27) H(20) 2.762 ? . 1_455 H(27) H(21) 3.130 ? . 1_455 H(28) C(21) 3.491 ? . 1_455 H(28) H(10) 3.052 ? . 2_566 H(28) H(20) 2.540 ? . 1_455 H(28) H(31) 3.058 ? . 2_565 H(29) C(18) 2.877 ? . 2_556 H(29) C(21) 3.391 ? . 1_455 H(29) H(1) 3.564 ? . 2_555 H(29) H(13) 2.719 ? . 2_556 H(29) H(14) 2.517 ? . 2_556 H(29) H(15) 2.923 ? . 2_556 H(29) H(20) 2.821 ? . 1_455 H(29) H(21) 3.507 ? . 1_455 H(29) H(22) 3.313 ? . 1_455 H(31) H(3) 3.407 ? . 2_655 H(31) H(10) 2.772 ? . 1_554 H(31) H(25) 3.191 ? . 2_665 H(31) H(28) 3.058 ? . 2_565 H(31) H(31) 3.571 ? . 2_565 H(32) H(9) 2.995 ? . 2_566 H(32) H(16) 2.943 ? . 2_566 H(32) H(25) 3.268 ? . 2_665 H(33) C(3) 3.298 ? . 2_655 H(33) C(5) 3.515 ? . 2_655 H(33) C(22) 3.317 ? . 2_665 H(33) H(2) 2.363 ? . 2_655 H(33) H(3) 2.677 ? . 2_655 H(33) H(24) 3.493 ? . 2_665 H(33) H(25) 2.431 ? . 2_665 #===END data_C7 _database_code_depnum_ccdc_archive 'CCDC 733379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C32H34AlN4O _chemical_formula_sum 'C32 H34 Al N4 O' _chemical_formula_weight 517.61 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 8.1654(16) _cell_length_b 18.808(4) _cell_length_c 21.754(4) _cell_angle_alpha 76.24(3) _cell_angle_beta 82.70(3) _cell_angle_gamma 86.28(3) _cell_volume 3216.8(11) _cell_formula_units_Z 4 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.9690 _exptl_absorpt_correction_T_max 0.9946 _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 40032 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14700 _reflns_number_gt 10562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _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^)+(0.1016P)^2^+0.7790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14700 _refine_ls_number_parameters 705 _refine_ls_number_restraints 32 _refine_ls_R_factor_ref 0.1015 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2201 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.040 _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 0.79335(9) 0.15572(4) 0.43199(3) 0.03322(18) Uani 1 1 d . . . O1A O 0.0689(2) 0.81662(9) 0.14420(8) 0.0369(4) Uani 1 1 d . . . O1 O 0.9375(2) 0.20355(9) 0.37028(8) 0.0380(4) Uani 1 1 d . . . Al1A Al 0.19033(9) 0.89619(4) 0.11700(3) 0.03239(18) Uani 1 1 d . . . N1 N 0.7983(2) 0.05843(11) 0.49264(10) 0.0334(4) Uani 1 1 d . . . N1A N 0.1764(2) 0.98748(11) 0.04821(9) 0.0333(4) Uani 1 1 d . . . N2A N -0.0102(2) 0.95703(11) 0.15039(9) 0.0325(4) Uani 1 1 d . . . N2 N 0.9472(3) 0.16867(11) 0.49758(10) 0.0347(5) Uani 1 1 d . . . N3A N 0.3299(3) 0.86772(12) 0.04384(10) 0.0371(5) Uani 1 1 d . . . N3 N 0.7058(3) 0.09264(11) 0.38393(10) 0.0358(5) Uani 1 1 d . . . N4 N 0.6052(3) -0.01951(12) 0.38697(11) 0.0395(5) Uani 1 1 d . . . H4A H 0.5804 -0.0648 0.4003 0.047 Uiso 1 1 calc R . . C19A C -0.0519(3) 0.79773(13) 0.19215(11) 0.0339(5) Uani 1 1 d . . . C9 C 0.8533(3) 0.05239(13) 0.55016(11) 0.0332(5) Uani 1 1 d . . . C18A C -0.1469(3) 0.85199(13) 0.21800(12) 0.0341(5) Uani 1 1 d . . . C10A C 0.3586(3) 0.92361(14) -0.00927(11) 0.0359(5) Uani 1 1 d . . . N4A N 0.4626(3) 0.90819(13) -0.05650(10) 0.0399(5) Uani 1 1 d . . . H4AA H 0.4931 0.9364 -0.0930 0.048 Uiso 1 1 calc R . . C9A C 0.0867(3) 1.04643(13) 0.06111(11) 0.0327(5) Uani 1 1 d . . . C18 C 1.0998(3) 0.26571(13) 0.42455(12) 0.0360(5) Uani 1 1 d . . . C8A C -0.0162(3) 1.03269(13) 0.11932(12) 0.0339(5) Uani 1 1 d . . . C1 C 0.7279(3) 0.00200(13) 0.48032(12) 0.0360(5) Uani 1 1 d . . . C17A C -0.1299(3) 0.92904(13) 0.19239(11) 0.0352(5) Uani 1 1 d . . . H17A H -0.2095 0.9609 0.2068 0.042 Uiso 1 1 calc R . . C2A C 0.2872(3) 1.06031(15) -0.05200(12) 0.0397(6) Uani 1 1 d . . . H2AA H 0.3561 1.0640 -0.0900 0.048 Uiso 1 1 calc R . . C20 C 1.1169(3) 0.29629(13) 0.30845(12) 0.0364(5) Uani 1 1 d . . . C19 C 1.0462(3) 0.25413(13) 0.36845(12) 0.0361(5) Uani 1 1 d . . . C7 C 0.9908(3) 0.11349(15) 0.61300(12) 0.0414(6) Uani 1 1 d . . . H7A H 1.0435 0.1536 0.6184 0.050 Uiso 1 1 calc R . . C22A C -0.3151(3) 0.76025(14) 0.29296(12) 0.0383(6) Uani 1 1 d . A . C11A C 0.5101(3) 0.83686(15) -0.03350(12) 0.0385(6) Uani 1 1 d . . . C4 C 0.8360(3) -0.01111(13) 0.59880(12) 0.0373(6) Uani 1 1 d . . . C4A C 0.0915(3) 1.11519(13) 0.01815(12) 0.0356(5) Uani 1 1 d . . . C17 C 1.0561(3) 0.21858(13) 0.48581(12) 0.0376(5) Uani 1 1 d . . . H17B H 1.1097 0.2242 0.5195 0.045 Uiso 1 1 calc R . . C20A C -0.0934(3) 0.72370(13) 0.21627(12) 0.0374(6) Uani 1 1 d . . . C11 C 0.5784(3) 0.02783(15) 0.32979(13) 0.0391(6) Uani 1 1 d . . . C1A C 0.2735(3) 0.99289(14) -0.00687(11) 0.0355(5) Uani 1 1 d . . . C21 C 1.2282(3) 0.34883(14) 0.30956(13) 0.0403(6) Uani 1 1 d . . . H21A H 1.2742 0.3763 0.2705 0.048 Uiso 1 1 calc R . . C23A C -0.2749(3) 0.83157(14) 0.26818(12) 0.0373(5) Uani 1 1 d . . . H23A H -0.3340 0.8680 0.2849 0.045 Uiso 1 1 calc R . . C3A C 0.1977(3) 1.12035(15) -0.03925(12) 0.0407(6) Uani 1 1 d . . . H3AA H 0.2070 1.1651 -0.0687 0.049 Uiso 1 1 calc R . . C23 C 1.2134(3) 0.32062(13) 0.42180(13) 0.0380(6) Uani 1 1 d . . . H23B H 1.2456 0.3275 0.4594 0.046 Uiso 1 1 calc R . . C7A C -0.1101(3) 1.08938(14) 0.13712(13) 0.0405(6) Uani 1 1 d . . . H7AA H -0.1765 1.0817 0.1760 0.049 Uiso 1 1 calc R . . C8 C 0.9323(3) 0.11463(14) 0.55595(11) 0.0361(5) Uani 1 1 d . . . C16 C 0.6382(3) 0.09759(14) 0.32763(12) 0.0374(5) Uani 1 1 d . . . C3 C 0.7582(3) -0.07030(14) 0.58477(14) 0.0424(6) Uani 1 1 d . . . H3A H 0.7428 -0.1136 0.6158 0.051 Uiso 1 1 calc R . . C21A C -0.2217(3) 0.70850(14) 0.26490(12) 0.0403(6) Uani 1 1 d . . . H21B H -0.2484 0.6597 0.2804 0.048 Uiso 1 1 calc R . . C22 C 1.2770(3) 0.36391(13) 0.36451(13) 0.0382(6) Uani 1 1 d . . . C2 C 0.7064(3) -0.06424(14) 0.52675(13) 0.0395(6) Uani 1 1 d . . . H2A H 0.6574 -0.1033 0.5178 0.047 Uiso 1 1 calc R . . C32A C 0.3417(3) 0.90448(16) 0.17700(12) 0.0429(6) Uani 1 1 d . . . H32A H 0.4440 0.8786 0.1681 0.064 Uiso 1 1 calc R . . H32B H 0.2937 0.8837 0.2196 0.064 Uiso 1 1 calc R . . H32C H 0.3622 0.9552 0.1729 0.064 Uiso 1 1 calc R . . C5A C -0.0088(3) 1.17234(14) 0.03736(13) 0.0424(6) Uani 1 1 d . . . H5AA H -0.0101 1.2189 0.0105 0.051 Uiso 1 1 calc R . . C24 C 1.0653(3) 0.28733(15) 0.24536(12) 0.0417(6) Uani 1 1 d . . . C32 C 0.6029(3) 0.21685(14) 0.45518(14) 0.0442(6) Uani 1 1 d . . . H32D H 0.5184 0.2163 0.4284 0.066 Uiso 1 1 calc R . . H32E H 0.6364 0.2662 0.4497 0.066 Uiso 1 1 calc R . . H32F H 0.5605 0.1980 0.4989 0.066 Uiso 1 1 calc R . . C16A C 0.4310(3) 0.81097(14) 0.02903(12) 0.0379(6) Uani 1 1 d . . . C10 C 0.6784(3) 0.02154(13) 0.41621(12) 0.0359(5) Uani 1 1 d . . . C5 C 0.8973(3) -0.01055(15) 0.65680(13) 0.0435(6) Uani 1 1 d . . . H5A H 0.8884 -0.0516 0.6905 0.052 Uiso 1 1 calc R . . C25 C 1.3965(3) 0.42488(14) 0.35831(13) 0.0423(6) Uani 1 1 d . . . C6A C -0.1041(3) 1.15938(15) 0.09553(14) 0.0451(6) Uani 1 1 d . . . H6AA H -0.1663 1.1980 0.1077 0.054 Uiso 1 1 calc R . . C12 C 0.5004(3) 0.01740(16) 0.27907(13) 0.0432(6) Uani 1 1 d . . . H12A H 0.4602 -0.0280 0.2798 0.052 Uiso 1 1 calc R . . C12A C 0.6240(3) 0.79157(17) -0.06128(14) 0.0475(7) Uani 1 1 d . . . H12B H 0.6763 0.8078 -0.1024 0.057 Uiso 1 1 calc R . . C24A C 0.0051(4) 0.66153(14) 0.19124(13) 0.0445(6) Uani 1 1 d . . . C15 C 0.6187(3) 0.15684(15) 0.27672(13) 0.0424(6) Uani 1 1 d . . . H15A H 0.6554 0.2028 0.2761 0.051 Uiso 1 1 calc R . . C25A C -0.4540(4) 0.73692(15) 0.34638(13) 0.0469(7) Uani 1 1 d D . . C26 C 0.8874(4) 0.31773(16) 0.24097(14) 0.0492(7) Uani 1 1 d . . . H26A H 0.8165 0.2915 0.2766 0.074 Uiso 1 1 calc R . . H26B H 0.8516 0.3120 0.2021 0.074 Uiso 1 1 calc R . . H26C H 0.8826 0.3687 0.2414 0.074 Uiso 1 1 calc R . . C6 C 0.9690(4) 0.05024(16) 0.66290(13) 0.0457(7) Uani 1 1 d . . . H6A H 1.0053 0.0501 0.7017 0.055 Uiso 1 1 calc R . . C14 C 0.5421(3) 0.14502(17) 0.22663(14) 0.0472(7) Uani 1 1 d . . . H14A H 0.5286 0.1833 0.1915 0.057 Uiso 1 1 calc R . . C15A C 0.4661(3) 0.74123(16) 0.06485(15) 0.0475(7) Uani 1 1 d . . . H15B H 0.4152 0.7246 0.1061 0.057 Uiso 1 1 calc R . . C27 C 1.0782(4) 0.20706(16) 0.24014(14) 0.0485(7) Uani 1 1 d . . . H27A H 1.1900 0.1886 0.2433 0.073 Uiso 1 1 calc R . . H27B H 1.0466 0.2040 0.1998 0.073 Uiso 1 1 calc R . . H27C H 1.0062 0.1784 0.2740 0.073 Uiso 1 1 calc R . . C13 C 0.4847(3) 0.07499(17) 0.22887(14) 0.0470(7) Uani 1 1 d . . . H13A H 0.4345 0.0682 0.1947 0.056 Uiso 1 1 calc R . . C29 C 1.4257(4) 0.43638(16) 0.42306(15) 0.0540(8) Uani 1 1 d . . . H29A H 1.4705 0.3919 0.4479 0.081 Uiso 1 1 calc R . . H29B H 1.3228 0.4497 0.4449 0.081 Uiso 1 1 calc R . . H29C H 1.5021 0.4748 0.4172 0.081 Uiso 1 1 calc R . . C14A C 0.5798(4) 0.69774(17) 0.03642(16) 0.0538(7) Uani 1 1 d . . . H14B H 0.6064 0.6509 0.0593 0.065 Uiso 1 1 calc R . . C26A C 0.0113(4) 0.67459(16) 0.11804(14) 0.0519(7) Uani 1 1 d . . . H26D H 0.0570 0.7214 0.0982 0.078 Uiso 1 1 calc R . . H26E H -0.0984 0.6737 0.1069 0.078 Uiso 1 1 calc R . . H26F H 0.0792 0.6368 0.1037 0.078 Uiso 1 1 calc R . . C30 C 1.3253(4) 0.49677(15) 0.31956(17) 0.0610(9) Uani 1 1 d . . . H30A H 1.3060 0.4904 0.2786 0.091 Uiso 1 1 calc R . . H30B H 1.4024 0.5348 0.3140 0.091 Uiso 1 1 calc R . . H30C H 1.2230 0.5100 0.3418 0.091 Uiso 1 1 calc R . . C27A C 0.1807(4) 0.65777(17) 0.21035(15) 0.0539(7) Uani 1 1 d . . . H27D H 0.1753 0.6496 0.2558 0.081 Uiso 1 1 calc R . . H27E H 0.2333 0.7031 0.1907 0.081 Uiso 1 1 calc R . . H27F H 0.2432 0.6182 0.1965 0.081 Uiso 1 1 calc R . . C13A C 0.6560(4) 0.72220(18) -0.02573(16) 0.0556(8) Uani 1 1 d . . . H13B H 0.7301 0.6909 -0.0435 0.067 Uiso 1 1 calc R . . C31 C 1.5631(4) 0.40563(18) 0.32369(16) 0.0575(8) Uani 1 1 d . . . H31A H 1.5468 0.3984 0.2827 0.086 Uiso 1 1 calc R . . H31B H 1.6098 0.3615 0.3484 0.086 Uiso 1 1 calc R . . H31C H 1.6368 0.4449 0.3183 0.086 Uiso 1 1 calc R . . C28 C 1.1745(4) 0.33078(18) 0.18685(14) 0.0574(8) Uani 1 1 d . . . H28A H 1.2870 0.3127 0.1882 0.086 Uiso 1 1 calc R . . H28B H 1.1682 0.3818 0.1875 0.086 Uiso 1 1 calc R . . H28C H 1.1361 0.3248 0.1485 0.086 Uiso 1 1 calc R . . C28A C -0.0687(5) 0.58615(16) 0.22074(16) 0.0627(9) Uani 1 1 d . . . H28D H -0.0733 0.5762 0.2663 0.094 Uiso 1 1 calc R . . H28E H -0.0008 0.5491 0.2052 0.094 Uiso 1 1 calc R . . H28F H -0.1783 0.5861 0.2091 0.094 Uiso 1 1 calc R . . C29A C -0.5504(5) 0.8023(2) 0.36592(18) 0.0769(11) Uani 1 1 d . A . H29D H -0.4810 0.8438 0.3556 0.115 Uiso 1 1 calc R . . H29E H -0.5843 0.7900 0.4110 0.115 Uiso 1 1 calc R . . H29F H -0.6461 0.8140 0.3435 0.115 Uiso 1 1 calc R . . C30A C -0.3951(9) 0.6836(5) 0.4028(3) 0.074(3) Uani 0.72(2) 1 d PDU A 1 H30D H -0.3357 0.6433 0.3891 0.111 Uiso 0.72(2) 1 calc PR A 1 H30E H -0.4883 0.6657 0.4329 0.111 Uiso 0.72(2) 1 calc PR A 1 H30F H -0.3236 0.7076 0.4226 0.111 Uiso 0.72(2) 1 calc PR A 1 C30' C -0.358(2) 0.7260(19) 0.4043(6) 0.086(6) Uani 0.28(2) 1 d PDU A 2 H30G H -0.2803 0.6855 0.4046 0.129 Uiso 0.28(2) 1 calc PR A 2 H30H H -0.4339 0.7162 0.4426 0.129 Uiso 0.28(2) 1 calc PR A 2 H30I H -0.3003 0.7696 0.4019 0.129 Uiso 0.28(2) 1 calc PR A 2 C31A C -0.5908(6) 0.7038(3) 0.3178(2) 0.0700(17) Uani 0.750(8) 1 d PDU A 1 H31D H -0.5454 0.6616 0.3031 0.105 Uiso 0.750(8) 1 calc PR A 1 H31E H -0.6285 0.7398 0.2828 0.105 Uiso 0.750(8) 1 calc PR A 1 H31F H -0.6819 0.6897 0.3501 0.105 Uiso 0.750(8) 1 calc PR A 1 C31' C -0.500(2) 0.6556(6) 0.3543(8) 0.077(5) Uani 0.250(8) 1 d PDU A 2 H31G H -0.4081 0.6292 0.3368 0.116 Uiso 0.250(8) 1 calc PR A 2 H31H H -0.5940 0.6543 0.3321 0.116 Uiso 0.250(8) 1 calc PR A 2 H31I H -0.5264 0.6333 0.3987 0.116 Uiso 0.250(8) 1 calc PR A 2 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.500 247 48 ' ' 2 -0.075 0.500 0.000 403 78 ' ' 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 0.0335(4) 0.0334(4) 0.0318(4) -0.0070(3) 0.0001(3) -0.0038(3) O1A 0.0368(9) 0.0386(9) 0.0343(9) -0.0091(7) 0.0033(7) -0.0054(7) O1 0.0406(10) 0.0407(9) 0.0325(9) -0.0069(7) -0.0009(7) -0.0116(8) Al1A 0.0331(4) 0.0354(4) 0.0285(4) -0.0067(3) -0.0018(3) -0.0058(3) N1 0.0327(10) 0.0305(10) 0.0355(11) -0.0074(8) 0.0016(8) -0.0020(8) N1A 0.0319(10) 0.0381(11) 0.0292(10) -0.0064(8) -0.0007(8) -0.0062(8) N2A 0.0352(11) 0.0331(10) 0.0287(10) -0.0052(8) -0.0034(8) -0.0065(8) N2 0.0370(11) 0.0327(10) 0.0338(11) -0.0076(9) -0.0007(9) -0.0032(8) N3A 0.0341(11) 0.0433(12) 0.0337(11) -0.0100(9) 0.0011(9) -0.0063(9) N3 0.0358(11) 0.0381(11) 0.0331(11) -0.0088(9) 0.0009(9) -0.0049(9) N4 0.0351(11) 0.0348(11) 0.0482(13) -0.0104(10) -0.0008(10) -0.0041(9) C19A 0.0363(12) 0.0383(13) 0.0270(12) -0.0069(10) -0.0019(10) -0.0073(10) C9 0.0300(12) 0.0352(12) 0.0326(13) -0.0061(10) -0.0013(10) 0.0010(10) C18A 0.0339(12) 0.0368(12) 0.0314(12) -0.0077(10) -0.0011(10) -0.0065(10) C10A 0.0357(13) 0.0453(14) 0.0272(12) -0.0074(10) -0.0034(10) -0.0099(11) N4A 0.0354(11) 0.0573(14) 0.0271(11) -0.0099(10) 0.0002(9) -0.0086(10) C9A 0.0325(12) 0.0345(12) 0.0321(12) -0.0069(10) -0.0066(10) -0.0066(10) C18 0.0368(13) 0.0348(12) 0.0334(13) -0.0044(10) 0.0021(10) -0.0048(10) C8A 0.0362(12) 0.0320(12) 0.0328(13) -0.0045(10) -0.0052(10) -0.0061(10) C1 0.0292(12) 0.0344(12) 0.0427(14) -0.0088(11) 0.0019(10) -0.0014(10) C17A 0.0382(13) 0.0356(12) 0.0310(12) -0.0067(10) -0.0017(10) -0.0047(10) C2A 0.0389(13) 0.0512(15) 0.0278(12) -0.0041(11) -0.0038(10) -0.0126(12) C20 0.0371(13) 0.0354(12) 0.0330(13) -0.0037(10) 0.0015(10) -0.0010(10) C19 0.0399(13) 0.0308(12) 0.0360(13) -0.0074(10) 0.0026(11) -0.0039(10) C7 0.0424(14) 0.0450(14) 0.0344(14) -0.0059(11) 0.0000(11) -0.0062(11) C22A 0.0416(14) 0.0427(14) 0.0293(12) -0.0037(10) -0.0020(10) -0.0130(11) C11A 0.0363(13) 0.0482(15) 0.0348(13) -0.0163(11) -0.0035(10) -0.0061(11) C4 0.0313(12) 0.0358(13) 0.0383(14) -0.0012(11) 0.0053(10) 0.0011(10) C4A 0.0341(12) 0.0369(13) 0.0367(13) -0.0062(10) -0.0087(10) -0.0079(10) C17 0.0431(14) 0.0351(12) 0.0352(13) -0.0095(10) -0.0034(11) -0.0034(11) C20A 0.0435(14) 0.0349(13) 0.0323(13) -0.0047(10) -0.0035(11) -0.0024(11) C11 0.0309(12) 0.0443(14) 0.0447(15) -0.0194(12) 0.0017(11) 0.0011(10) C1A 0.0320(12) 0.0483(14) 0.0275(12) -0.0085(10) -0.0049(9) -0.0095(11) C21 0.0437(14) 0.0344(13) 0.0372(14) -0.0014(11) 0.0051(11) -0.0044(11) C23A 0.0374(13) 0.0393(13) 0.0339(13) -0.0066(11) -0.0011(10) -0.0051(10) C3A 0.0430(14) 0.0444(14) 0.0316(13) 0.0043(11) -0.0105(11) -0.0151(11) C23 0.0388(13) 0.0343(12) 0.0399(14) -0.0077(11) -0.0003(11) -0.0047(10) C7A 0.0422(14) 0.0367(13) 0.0421(15) -0.0101(11) -0.0001(11) -0.0041(11) C8 0.0337(12) 0.0405(13) 0.0293(12) -0.0009(10) 0.0018(10) -0.0046(10) C16 0.0321(12) 0.0441(14) 0.0367(13) -0.0125(11) -0.0001(10) -0.0029(10) C3 0.0354(13) 0.0356(13) 0.0489(16) -0.0006(11) 0.0042(11) 0.0005(11) C21A 0.0502(15) 0.0361(13) 0.0322(13) -0.0019(10) -0.0018(11) -0.0126(11) C22 0.0396(13) 0.0283(12) 0.0441(15) -0.0057(10) 0.0003(11) -0.0023(10) C2 0.0339(13) 0.0332(12) 0.0487(16) -0.0080(11) 0.0037(11) -0.0032(10) C32A 0.0412(14) 0.0523(16) 0.0356(14) -0.0092(12) -0.0037(11) -0.0085(12) C5A 0.0433(14) 0.0343(13) 0.0467(16) 0.0009(11) -0.0104(12) -0.0076(11) C24 0.0439(15) 0.0436(14) 0.0332(13) -0.0033(11) 0.0033(11) -0.0055(12) C32 0.0459(15) 0.0393(14) 0.0465(16) -0.0109(12) -0.0001(12) -0.0018(12) C16A 0.0347(13) 0.0425(14) 0.0389(14) -0.0136(11) -0.0025(11) -0.0056(11) C10 0.0341(12) 0.0341(12) 0.0385(13) -0.0108(10) 0.0036(10) -0.0015(10) C5 0.0371(14) 0.0471(15) 0.0373(14) 0.0057(12) 0.0009(11) -0.0028(11) C25 0.0466(15) 0.0319(13) 0.0457(15) -0.0055(11) 0.0026(12) -0.0096(11) C6A 0.0453(15) 0.0387(14) 0.0517(17) -0.0103(12) -0.0068(13) -0.0044(12) C12 0.0364(14) 0.0499(15) 0.0470(16) -0.0208(13) -0.0006(12) -0.0010(12) C12A 0.0346(14) 0.0666(19) 0.0462(16) -0.0257(14) 0.0031(12) -0.0061(13) C24A 0.0579(17) 0.0317(13) 0.0400(15) -0.0031(11) 0.0003(13) -0.0049(12) C15 0.0422(14) 0.0436(14) 0.0429(15) -0.0139(12) -0.0031(12) -0.0027(11) C25A 0.0529(17) 0.0473(15) 0.0367(14) -0.0047(12) 0.0079(12) -0.0194(13) C26 0.0515(17) 0.0509(16) 0.0406(15) -0.0014(13) -0.0057(13) -0.0012(13) C6 0.0489(16) 0.0561(17) 0.0279(13) -0.0014(12) -0.0035(11) -0.0042(13) C14 0.0417(15) 0.0583(17) 0.0404(15) -0.0104(13) -0.0025(12) -0.0017(13) C15A 0.0433(15) 0.0482(16) 0.0507(17) -0.0135(13) 0.0016(13) -0.0057(12) C27 0.0464(16) 0.0577(17) 0.0417(15) -0.0165(13) 0.0030(12) -0.0009(13) C13 0.0402(14) 0.0637(18) 0.0439(16) -0.0256(14) -0.0056(12) -0.0017(13) C29 0.0624(19) 0.0418(15) 0.0578(19) -0.0107(13) -0.0012(15) -0.0156(14) C14A 0.0526(18) 0.0491(16) 0.0604(19) -0.0179(15) 0.0017(15) -0.0030(14) C26A 0.069(2) 0.0469(16) 0.0440(16) -0.0180(13) -0.0069(14) -0.0046(14) C30 0.077(2) 0.0327(14) 0.069(2) -0.0038(14) -0.0061(18) -0.0051(14) C27A 0.0552(18) 0.0513(17) 0.0482(17) -0.0015(14) -0.0034(14) 0.0063(14) C13A 0.0459(17) 0.063(2) 0.064(2) -0.0321(17) 0.0001(15) 0.0025(14) C31 0.0481(17) 0.0600(19) 0.0600(19) -0.0103(15) 0.0117(14) -0.0166(14) C28 0.0616(19) 0.070(2) 0.0379(16) -0.0094(14) 0.0066(14) -0.0191(16) C28A 0.087(3) 0.0425(16) 0.0550(19) -0.0095(14) 0.0057(17) -0.0116(16) C29A 0.067(2) 0.077(2) 0.065(2) 0.0073(18) 0.0292(18) -0.0003(19) C30A 0.078(4) 0.070(5) 0.050(3) 0.018(3) 0.014(3) 0.010(3) C30' 0.077(8) 0.095(11) 0.067(8) 0.005(7) 0.017(6) 0.004(7) C31A 0.060(3) 0.079(3) 0.073(3) -0.026(3) 0.014(2) -0.032(2) C31' 0.077(8) 0.076(7) 0.076(8) -0.019(6) 0.026(6) -0.037(6) _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 1.777(2) . ? Al1 C32 1.960(3) . ? Al1 N3 1.975(2) . ? Al1 N1 1.987(2) . ? Al1 N2 2.082(2) . ? O1A C19A 1.340(3) . ? O1A Al1A 1.7878(19) . ? O1 C19 1.333(3) . ? Al1A C32A 1.946(3) . ? Al1A N3A 1.996(2) . ? Al1A N1A 1.999(2) . ? Al1A N2A 2.090(2) . ? N1 C1 1.335(3) . ? N1 C9 1.360(3) . ? N1A C1A 1.336(3) . ? N1A C9A 1.355(3) . ? N2A C17A 1.296(3) . ? N2A C8A 1.424(3) . ? N2 C17 1.294(3) . ? N2 C8 1.422(3) . ? N3A C10A 1.371(3) . ? N3A C16A 1.381(3) . ? N3 C10 1.373(3) . ? N3 C16 1.387(3) . ? N4 C10 1.322(3) . ? N4 C11 1.380(3) . ? C19A C20A 1.413(3) . ? C19A C18A 1.421(3) . ? C9 C4 1.396(3) . ? C9 C8 1.411(3) . ? C18A C23A 1.413(3) . ? C18A C17A 1.433(3) . ? C10A N4A 1.322(3) . ? C10A C1A 1.446(4) . ? N4A C11A 1.365(3) . ? C9A C4A 1.404(3) . ? C9A C8A 1.407(3) . ? C18 C19 1.415(4) . ? C18 C23 1.419(3) . ? C18 C17 1.431(3) . ? C8A C7A 1.374(3) . ? C1 C2 1.410(3) . ? C1 C10 1.457(4) . ? C2A C3A 1.370(4) . ? C2A C1A 1.408(3) . ? C20 C21 1.392(4) . ? C20 C19 1.429(3) . ? C20 C24 1.535(4) . ? C7 C8 1.380(4) . ? C7 C6 1.411(4) . ? C22A C23A 1.366(3) . ? C22A C21A 1.403(4) . ? C22A C25A 1.522(3) . ? C11A C12A 1.398(4) . ? C11A C16A 1.417(4) . ? C4 C5 1.417(4) . ? C4 C3 1.428(4) . ? C4A C3A 1.414(4) . ? C4A C5A 1.419(4) . ? C20A C21A 1.383(4) . ? C20A C24A 1.543(4) . ? C11 C12 1.400(4) . ? C11 C16 1.418(4) . ? C21 C22 1.402(4) . ? C23 C22 1.376(4) . ? C7A C6A 1.409(4) . ? C16 C15 1.389(4) . ? C3 C2 1.359(4) . ? C22 C25 1.524(3) . ? C5A C6A 1.376(4) . ? C24 C26 1.532(4) . ? C24 C27 1.537(4) . ? C24 C28 1.548(4) . ? C16A C15A 1.390(4) . ? C5 C6 1.359(4) . ? C25 C29 1.525(4) . ? C25 C31 1.534(4) . ? C25 C30 1.535(4) . ? C12 C13 1.355(4) . ? C12A C13A 1.377(4) . ? C24A C27A 1.535(4) . ? C24A C28A 1.538(4) . ? C24A C26A 1.547(4) . ? C15 C14 1.391(4) . ? C25A C30A 1.499(5) . ? C25A C30' 1.532(9) . ? C25A C29A 1.533(5) . ? C25A C31' 1.564(9) . ? C25A C31A 1.573(5) . ? C14 C13 1.415(4) . ? C15A C14A 1.382(4) . ? C14A C13A 1.398(4) . ? 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 C32 113.61(11) . . ? O1 Al1 N3 98.47(9) . . ? C32 Al1 N3 104.68(11) . . ? O1 Al1 N1 133.95(9) . . ? C32 Al1 N1 111.55(11) . . ? N3 Al1 N1 78.21(9) . . ? O1 Al1 N2 88.44(9) . . ? C32 Al1 N2 99.40(11) . . ? N3 Al1 N2 149.59(9) . . ? N1 Al1 N2 75.82(9) . . ? C19A O1A Al1A 132.54(16) . . ? C19 O1 Al1 132.77(16) . . ? O1A Al1A C32A 112.50(11) . . ? O1A Al1A N3A 99.20(9) . . ? C32A Al1A N3A 105.98(11) . . ? O1A Al1A N1A 134.12(9) . . ? C32A Al1A N1A 112.12(11) . . ? N3A Al1A N1A 78.27(9) . . ? O1A Al1A N2A 88.24(8) . . ? C32A Al1A N2A 98.44(11) . . ? N3A Al1A N2A 149.19(9) . . ? N1A Al1A N2A 75.27(9) . . ? C1 N1 C9 120.3(2) . . ? C1 N1 Al1 119.76(17) . . ? C9 N1 Al1 119.38(16) . . ? C1A N1A C9A 120.6(2) . . ? C1A N1A Al1A 119.29(18) . . ? C9A N1A Al1A 119.47(16) . . ? C17A N2A C8A 120.5(2) . . ? C17A N2A Al1A 124.22(17) . . ? C8A N2A Al1A 115.09(16) . . ? C17 N2 C8 121.5(2) . . ? C17 N2 Al1 123.70(18) . . ? C8 N2 Al1 114.67(16) . . ? C10A N3A C16A 103.2(2) . . ? C10A N3A Al1A 114.79(17) . . ? C16A N3A Al1A 141.25(18) . . ? C10 N3 C16 102.9(2) . . ? C10 N3 Al1 116.09(17) . . ? C16 N3 Al1 140.35(17) . . ? C10 N4 C11 103.2(2) . . ? O1A C19A C20A 120.9(2) . . ? O1A C19A C18A 120.8(2) . . ? C20A C19A C18A 118.2(2) . . ? N1 C9 C4 122.4(2) . . ? N1 C9 C8 114.6(2) . . ? C4 C9 C8 123.0(2) . . ? C23A C18A C19A 120.3(2) . . ? C23A C18A C17A 116.1(2) . . ? C19A C18A C17A 123.3(2) . . ? N4A C10A N3A 116.3(2) . . ? N4A C10A C1A 127.5(2) . . ? N3A C10A C1A 116.3(2) . . ? C10A N4A C11A 103.4(2) . . ? N1A C9A C4A 122.2(2) . . ? N1A C9A C8A 115.0(2) . . ? C4A C9A C8A 122.8(2) . . ? C19 C18 C23 121.1(2) . . ? C19 C18 C17 122.1(2) . . ? C23 C18 C17 116.5(2) . . ? C7A C8A C9A 119.3(2) . . ? C7A C8A N2A 129.4(2) . . ? C9A C8A N2A 111.2(2) . . ? N1 C1 C2 120.9(2) . . ? N1 C1 C10 110.3(2) . . ? C2 C1 C10 128.8(2) . . ? N2A C17A C18A 123.9(2) . . ? C3A C2A C1A 119.2(2) . . ? C21 C20 C19 117.2(2) . . ? C21 C20 C24 121.1(2) . . ? C19 C20 C24 121.6(2) . . ? O1 C19 C18 121.9(2) . . ? O1 C19 C20 119.8(2) . . ? C18 C19 C20 118.3(2) . . ? C8 C7 C6 118.6(3) . . ? C23A C22A C21A 115.6(2) . . ? C23A C22A C25A 123.3(3) . . ? C21A C22A C25A 121.1(2) . . ? N4A C11A C12A 129.7(3) . . ? N4A C11A C16A 110.0(2) . . ? C12A C11A C16A 120.2(3) . . ? C9 C4 C5 117.1(2) . . ? C9 C4 C3 116.3(2) . . ? C5 C4 C3 126.6(2) . . ? C9A C4A C3A 116.5(2) . . ? C9A C4A C5A 116.6(2) . . ? C3A C4A C5A 127.0(2) . . ? N2 C17 C18 124.6(2) . . ? C21A C20A C19A 117.7(2) . . ? C21A C20A C24A 120.9(2) . . ? C19A C20A C24A 121.3(2) . . ? N4 C11 C12 130.7(3) . . ? N4 C11 C16 109.6(2) . . ? C12 C11 C16 119.7(3) . . ? N1A C1A C2A 120.6(2) . . ? N1A C1A C10A 110.5(2) . . ? C2A C1A C10A 128.8(2) . . ? C20 C21 C22 125.6(2) . . ? C22A C23A C18A 122.3(2) . . ? C2A C3A C4A 120.9(2) . . ? C22 C23 C18 121.3(3) . . ? C8A C7A C6A 118.9(2) . . ? C7 C8 C9 118.5(2) . . ? C7 C8 N2 129.9(2) . . ? C9 C8 N2 111.5(2) . . ? N3 C16 C15 130.9(2) . . ? N3 C16 C11 107.4(2) . . ? C15 C16 C11 121.6(2) . . ? C2 C3 C4 120.9(2) . . ? C20A C21A C22A 125.8(2) . . ? C23 C22 C21 116.4(2) . . ? C23 C22 C25 123.9(2) . . ? C21 C22 C25 119.7(2) . . ? C3 C2 C1 119.2(2) . . ? C6A C5A C4A 120.4(2) . . ? C26 C24 C20 107.9(2) . . ? C26 C24 C27 110.4(2) . . ? C20 C24 C27 112.2(2) . . ? C26 C24 C28 107.6(2) . . ? C20 C24 C28 112.2(2) . . ? C27 C24 C28 106.4(2) . . ? N3A C16A C15A 131.3(2) . . ? N3A C16A C11A 107.0(2) . . ? C15A C16A C11A 121.6(2) . . ? N4 C10 N3 116.9(2) . . ? N4 C10 C1 128.1(2) . . ? N3 C10 C1 114.9(2) . . ? C6 C5 C4 119.7(2) . . ? C22 C25 C29 112.0(2) . . ? C22 C25 C31 109.5(2) . . ? C29 C25 C31 108.5(2) . . ? C22 C25 C30 109.3(2) . . ? C29 C25 C30 108.4(2) . . ? C31 C25 C30 109.1(2) . . ? C5A C6A C7A 121.9(3) . . ? C13 C12 C11 118.4(3) . . ? C13A C12A C11A 117.7(3) . . ? C27A C24A C28A 107.1(2) . . ? C27A C24A C20A 108.0(2) . . ? C28A C24A C20A 112.5(2) . . ? C27A C24A C26A 110.2(2) . . ? C28A C24A C26A 107.5(2) . . ? C20A C24A C26A 111.5(2) . . ? C16 C15 C14 117.6(3) . . ? C30A C25A C22A 112.4(3) . . ? C30A C25A C30' 33.7(9) . . ? C22A C25A C30' 100.0(8) . . ? C30A C25A C29A 111.4(4) . . ? C22A C25A C29A 112.6(2) . . ? C30' C25A C29A 89.9(10) . . ? C30A C25A C31' 64.6(9) . . ? C22A C25A C31' 112.2(6) . . ? C30' C25A C31' 98.3(15) . . ? C29A C25A C31' 132.1(6) . . ? C30A C25A C31A 111.6(6) . . ? C22A C25A C31A 107.3(3) . . ? C30' C25A C31A 143.7(12) . . ? C29A C25A C31A 100.8(3) . . ? C31' C25A C31A 49.4(7) . . ? C5 C6 C7 123.0(3) . . ? C15 C14 C13 120.3(3) . . ? C14A C15A C16A 117.0(3) . . ? C12 C13 C14 122.3(3) . . ? C15A C14A C13A 121.9(3) . . ? C12A C13A C14A 121.6(3) . . ? 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 C32 Al1 O1 C19 72.0(2) . . . . ? N3 Al1 O1 C19 -177.8(2) . . . . ? N1 Al1 O1 C19 -96.1(2) . . . . ? N2 Al1 O1 C19 -27.6(2) . . . . ? C19A O1A Al1A C32A 68.5(2) . . . . ? C19A O1A Al1A N3A -179.9(2) . . . . ? C19A O1A Al1A N1A -97.4(2) . . . . ? C19A O1A Al1A N2A -30.0(2) . . . . ? O1 Al1 N1 C1 -98.9(2) . . . . ? C32 Al1 N1 C1 92.8(2) . . . . ? N3 Al1 N1 C1 -8.48(18) . . . . ? N2 Al1 N1 C1 -172.51(19) . . . . ? O1 Al1 N1 C9 90.0(2) . . . . ? C32 Al1 N1 C9 -78.3(2) . . . . ? N3 Al1 N1 C9 -179.60(19) . . . . ? N2 Al1 N1 C9 16.37(17) . . . . ? O1A Al1A N1A C1A -100.3(2) . . . . ? C32A Al1A N1A C1A 93.9(2) . . . . ? N3A Al1A N1A C1A -8.76(18) . . . . ? N2A Al1A N1A C1A -172.83(19) . . . . ? O1A Al1A N1A C9A 88.9(2) . . . . ? C32A Al1A N1A C9A -76.9(2) . . . . ? N3A Al1A N1A C9A -179.60(19) . . . . ? N2A Al1A N1A C9A 16.32(17) . . . . ? O1A Al1A N2A C17A 20.0(2) . . . . ? C32A Al1A N2A C17A -92.5(2) . . . . ? N3A Al1A N2A C17A 125.1(2) . . . . ? N1A Al1A N2A C17A 156.7(2) . . . . ? O1A Al1A N2A C8A -154.44(16) . . . . ? C32A Al1A N2A C8A 93.07(18) . . . . ? N3A Al1A N2A C8A -49.3(3) . . . . ? N1A Al1A N2A C8A -17.70(16) . . . . ? O1 Al1 N2 C17 21.5(2) . . . . ? C32 Al1 N2 C17 -92.2(2) . . . . ? N3 Al1 N2 C17 125.6(2) . . . . ? N1 Al1 N2 C17 157.8(2) . . . . ? O1 Al1 N2 C8 -154.29(17) . . . . ? C32 Al1 N2 C8 92.03(18) . . . . ? N3 Al1 N2 C8 -50.1(3) . . . . ? N1 Al1 N2 C8 -17.98(16) . . . . ? O1A Al1A N3A C10A 140.43(17) . . . . ? C32A Al1A N3A C10A -102.86(19) . . . . ? N1A Al1A N3A C10A 7.06(17) . . . . ? N2A Al1A N3A C10A 38.3(3) . . . . ? O1A Al1A N3A C16A -51.4(3) . . . . ? C32A Al1A N3A C16A 65.3(3) . . . . ? N1A Al1A N3A C16A 175.2(3) . . . . ? N2A Al1A N3A C16A -153.6(2) . . . . ? O1 Al1 N3 C10 139.46(18) . . . . ? C32 Al1 N3 C10 -103.31(19) . . . . ? N1 Al1 N3 C10 6.16(17) . . . . ? N2 Al1 N3 C10 38.0(3) . . . . ? O1 Al1 N3 C16 -52.3(3) . . . . ? C32 Al1 N3 C16 65.0(3) . . . . ? N1 Al1 N3 C16 174.4(3) . . . . ? N2 Al1 N3 C16 -153.8(2) . . . . ? Al1A O1A C19A C20A -159.99(19) . . . . ? Al1A O1A C19A C18A 23.1(3) . . . . ? C1 N1 C9 C4 -1.5(4) . . . . ? Al1 N1 C9 C4 169.60(18) . . . . ? C1 N1 C9 C8 177.1(2) . . . . ? Al1 N1 C9 C8 -11.8(3) . . . . ? O1A C19A C18A C23A 179.4(2) . . . . ? C20A C19A C18A C23A 2.4(4) . . . . ? O1A C19A C18A C17A 4.8(4) . . . . ? C20A C19A C18A C17A -172.2(2) . . . . ? C16A N3A C10A N4A 1.7(3) . . . . ? Al1A N3A C10A N4A 174.15(17) . . . . ? C16A N3A C10A C1A -177.5(2) . . . . ? Al1A N3A C10A C1A -5.1(3) . . . . ? N3A C10A N4A C11A -0.9(3) . . . . ? C1A C10A N4A C11A 178.2(2) . . . . ? C1A N1A C9A C4A -0.3(3) . . . . ? Al1A N1A C9A C4A 170.42(17) . . . . ? C1A N1A C9A C8A 177.1(2) . . . . ? Al1A N1A C9A C8A -12.1(3) . . . . ? N1A C9A C8A C7A 178.9(2) . . . . ? C4A C9A C8A C7A -3.7(4) . . . . ? N1A C9A C8A N2A -3.7(3) . . . . ? C4A C9A C8A N2A 173.7(2) . . . . ? C17A N2A C8A C7A 19.2(4) . . . . ? Al1A N2A C8A C7A -166.1(2) . . . . ? C17A N2A C8A C9A -157.8(2) . . . . ? Al1A N2A C8A C9A 16.9(2) . . . . ? C9 N1 C1 C2 1.1(4) . . . . ? Al1 N1 C1 C2 -169.93(18) . . . . ? C9 N1 C1 C10 179.6(2) . . . . ? Al1 N1 C1 C10 8.6(3) . . . . ? C8A N2A C17A C18A 169.3(2) . . . . ? Al1A N2A C17A C18A -4.9(3) . . . . ? C23A C18A C17A N2A 173.5(2) . . . . ? C19A C18A C17A N2A -11.6(4) . . . . ? Al1 O1 C19 C18 18.4(4) . . . . ? Al1 O1 C19 C20 -164.20(18) . . . . ? C23 C18 C19 O1 -178.9(2) . . . . ? C17 C18 C19 O1 7.4(4) . . . . ? C23 C18 C19 C20 3.6(4) . . . . ? C17 C18 C19 C20 -170.0(2) . . . . ? C21 C20 C19 O1 179.3(2) . . . . ? C24 C20 C19 O1 2.7(4) . . . . ? C21 C20 C19 C18 -3.2(3) . . . . ? C24 C20 C19 C18 -179.8(2) . . . . ? C10A N4A C11A C12A -177.2(3) . . . . ? C10A N4A C11A C16A -0.3(3) . . . . ? N1 C9 C4 C5 -179.6(2) . . . . ? C8 C9 C4 C5 2.0(4) . . . . ? N1 C9 C4 C3 0.6(4) . . . . ? C8 C9 C4 C3 -177.9(2) . . . . ? N1A C9A C4A C3A -1.1(3) . . . . ? C8A C9A C4A C3A -178.4(2) . . . . ? N1A C9A C4A C5A 179.8(2) . . . . ? C8A C9A C4A C5A 2.6(3) . . . . ? C8 N2 C17 C18 167.6(2) . . . . ? Al1 N2 C17 C18 -7.8(4) . . . . ? C19 C18 C17 N2 -10.4(4) . . . . ? C23 C18 C17 N2 175.7(2) . . . . ? O1A C19A C20A C21A -178.7(2) . . . . ? C18A C19A C20A C21A -1.7(4) . . . . ? O1A C19A C20A C24A 3.7(4) . . . . ? C18A C19A C20A C24A -179.3(2) . . . . ? C10 N4 C11 C12 -177.6(3) . . . . ? C10 N4 C11 C16 -0.3(3) . . . . ? C9A N1A C1A C2A 1.4(3) . . . . ? Al1A N1A C1A C2A -169.35(18) . . . . ? C9A N1A C1A C10A 179.0(2) . . . . ? Al1A N1A C1A C10A 8.2(3) . . . . ? C3A C2A C1A N1A -1.0(4) . . . . ? C3A C2A C1A C10A -178.1(2) . . . . ? N4A C10A C1A N1A 179.0(2) . . . . ? N3A C10A C1A N1A -1.9(3) . . . . ? N4A C10A C1A C2A -3.6(4) . . . . ? N3A C10A C1A C2A 175.5(2) . . . . ? C19 C20 C21 C22 0.0(4) . . . . ? C24 C20 C21 C22 176.6(2) . . . . ? C21A C22A C23A C18A -0.6(4) . . . . ? C25A C22A C23A C18A -179.1(2) . . . . ? C19A C18A C23A C22A -1.3(4) . . . . ? C17A C18A C23A C22A 173.7(2) . . . . ? C1A C2A C3A C4A -0.5(4) . . . . ? C9A C4A C3A C2A 1.5(4) . . . . ? C5A C4A C3A C2A -179.5(2) . . . . ? C19 C18 C23 C22 -0.8(4) . . . . ? C17 C18 C23 C22 173.2(2) . . . . ? C9A C8A C7A C6A 1.9(4) . . . . ? N2A C8A C7A C6A -175.0(2) . . . . ? C6 C7 C8 C9 0.0(4) . . . . ? C6 C7 C8 N2 -175.5(3) . . . . ? N1 C9 C8 C7 179.5(2) . . . . ? C4 C9 C8 C7 -2.0(4) . . . . ? N1 C9 C8 N2 -4.2(3) . . . . ? C4 C9 C8 N2 174.3(2) . . . . ? C17 N2 C8 C7 17.2(4) . . . . ? Al1 N2 C8 C7 -166.9(2) . . . . ? C17 N2 C8 C9 -158.5(2) . . . . ? Al1 N2 C8 C9 17.3(3) . . . . ? C10 N3 C16 C15 175.8(3) . . . . ? Al1 N3 C16 C15 6.6(5) . . . . ? C10 N3 C16 C11 -1.4(3) . . . . ? Al1 N3 C16 C11 -170.6(2) . . . . ? N4 C11 C16 N3 1.1(3) . . . . ? C12 C11 C16 N3 178.8(2) . . . . ? N4 C11 C16 C15 -176.4(2) . . . . ? C12 C11 C16 C15 1.3(4) . . . . ? C9 C4 C3 C2 0.7(4) . . . . ? C5 C4 C3 C2 -179.2(2) . . . . ? C19A C20A C21A C22A -0.2(4) . . . . ? C24A C20A C21A C22A 177.4(2) . . . . ? C23A C22A C21A C20A 1.4(4) . . . . ? C25A C22A C21A C20A 180.0(3) . . . . ? C18 C23 C22 C21 -2.3(4) . . . . ? C18 C23 C22 C25 178.6(2) . . . . ? C20 C21 C22 C23 2.8(4) . . . . ? C20 C21 C22 C25 -178.1(2) . . . . ? C4 C3 C2 C1 -1.0(4) . . . . ? N1 C1 C2 C3 0.1(4) . . . . ? C10 C1 C2 C3 -178.1(2) . . . . ? C9A C4A C5A C6A 0.2(4) . . . . ? C3A C4A C5A C6A -178.7(3) . . . . ? C21 C20 C24 C26 -107.2(3) . . . . ? C19 C20 C24 C26 69.3(3) . . . . ? C21 C20 C24 C27 131.0(3) . . . . ? C19 C20 C24 C27 -52.6(3) . . . . ? C21 C20 C24 C28 11.2(4) . . . . ? C19 C20 C24 C28 -172.3(2) . . . . ? C10A N3A C16A C15A 175.1(3) . . . . ? Al1A N3A C16A C15A 6.2(5) . . . . ? C10A N3A C16A C11A -1.7(3) . . . . ? Al1A N3A C16A C11A -170.7(2) . . . . ? N4A C11A C16A N3A 1.3(3) . . . . ? C12A C11A C16A N3A 178.6(2) . . . . ? N4A C11A C16A C15A -175.9(2) . . . . ? C12A C11A C16A C15A 1.3(4) . . . . ? C11 N4 C10 N3 -0.7(3) . . . . ? C11 N4 C10 C1 176.2(2) . . . . ? C16 N3 C10 N4 1.4(3) . . . . ? Al1 N3 C10 N4 173.74(17) . . . . ? C16 N3 C10 C1 -176.0(2) . . . . ? Al1 N3 C10 C1 -3.6(3) . . . . ? N1 C1 C10 N4 180.0(2) . . . . ? C2 C1 C10 N4 -1.6(4) . . . . ? N1 C1 C10 N3 -3.0(3) . . . . ? C2 C1 C10 N3 175.4(2) . . . . ? C9 C4 C5 C6 0.0(4) . . . . ? C3 C4 C5 C6 179.8(3) . . . . ? C23 C22 C25 C29 -4.8(4) . . . . ? C21 C22 C25 C29 176.2(2) . . . . ? C23 C22 C25 C31 115.6(3) . . . . ? C21 C22 C25 C31 -63.5(3) . . . . ? C23 C22 C25 C30 -125.0(3) . . . . ? C21 C22 C25 C30 56.0(3) . . . . ? C4A C5A C6A C7A -1.9(4) . . . . ? C8A C7A C6A C5A 0.9(4) . . . . ? N4 C11 C12 C13 177.2(3) . . . . ? C16 C11 C12 C13 0.1(4) . . . . ? N4A C11A C12A C13A 176.3(3) . . . . ? C16A C11A C12A C13A -0.4(4) . . . . ? C21A C20A C24A C27A -111.5(3) . . . . ? C19A C20A C24A C27A 66.1(3) . . . . ? C21A C20A C24A C28A 6.5(4) . . . . ? C19A C20A C24A C28A -176.0(3) . . . . ? C21A C20A C24A C26A 127.3(3) . . . . ? C19A C20A C24A C26A -55.2(3) . . . . ? N3 C16 C15 C14 -178.7(3) . . . . ? C11 C16 C15 C14 -1.8(4) . . . . ? C23A C22A C25A C30A -123.0(6) . . . . ? C21A C22A C25A C30A 58.5(6) . . . . ? C23A C22A C25A C30' -90.2(13) . . . . ? C21A C22A C25A C30' 91.3(13) . . . . ? C23A C22A C25A C29A 3.8(4) . . . . ? C21A C22A C25A C29A -174.7(3) . . . . ? C23A C22A C25A C31' 166.4(9) . . . . ? C21A C22A C25A C31' -12.1(9) . . . . ? C23A C22A C25A C31A 113.9(3) . . . . ? C21A C22A C25A C31A -64.6(4) . . . . ? C4 C5 C6 C7 -2.0(4) . . . . ? C8 C7 C6 C5 2.0(4) . . . . ? C16 C15 C14 C13 1.0(4) . . . . ? N3A C16A C15A C14A -177.4(3) . . . . ? C11A C16A C15A C14A -0.9(4) . . . . ? C11 C12 C13 C14 -1.0(4) . . . . ? C15 C14 C13 C12 0.4(4) . . . . ? C16A C15A C14A C13A -0.4(4) . . . . ? C11A C12A C13A C14A -0.9(4) . . . . ? C15A C14A C13A C12A 1.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.324 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.059 #===END