# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wei Gao' _publ_contact_author_email gw@jlu.edu.cn loop_ _publ_author_name 'Wei Gao' 'Nan Yang' 'Lan Xin' 'Jingshun Zhang' 'Xuyang Luo' ; Xiaoming Liu ; 'Yi Mu' data_complex_1a _database_code_depnum_ccdc_archive 'CCDC 871557' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H60 Al2 N6' _chemical_formula_weight 907.09 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.1381(16) _cell_length_b 8.4504(4) _cell_length_c 18.4874(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.3180(10) _cell_angle_gamma 90.00 _cell_volume 5012.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4565 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 25.98 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9747 _exptl_absorpt_correction_T_max 0.9787 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13200 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4943 _reflns_number_gt 4047 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+7.6605P] 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 4943 _refine_ls_number_parameters 303 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.258 _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 0.35467(2) 0.36344(9) -0.00876(4) 0.0266(2) Uani 1 1 d . . . C1 C 0.40387(7) 0.6508(3) -0.00949(13) 0.0265(5) Uani 1 1 d . . . C2 C 0.41526(8) 0.7786(3) -0.05361(14) 0.0312(6) Uani 1 1 d . . . H2 H 0.3952 0.8247 -0.0852 0.037 Uiso 1 1 calc R . . C3 C 0.45540(8) 0.8364(3) -0.05097(15) 0.0354(6) Uani 1 1 d . . . H3 H 0.4620 0.9194 -0.0813 0.042 Uiso 1 1 calc R . . C4 C 0.48627(8) 0.7727(3) -0.00359(15) 0.0364(6) Uani 1 1 d . . . H4 H 0.5132 0.8132 -0.0016 0.044 Uiso 1 1 calc R . . C5 C 0.47611(8) 0.6494(3) 0.03997(14) 0.0329(6) Uani 1 1 d . . . H5 H 0.4965 0.6071 0.0720 0.039 Uiso 1 1 calc R . . C6 C 0.43581(7) 0.5848(3) 0.03770(13) 0.0279(5) Uani 1 1 d . . . C7 C 0.42764(7) 0.4628(3) 0.08964(13) 0.0283(5) Uani 1 1 d . . . H7 H 0.4467 0.4503 0.1291 0.034 Uiso 1 1 calc R . . C8 C 0.33004(8) 0.6771(3) -0.04099(14) 0.0309(6) Uani 1 1 d . . . C9 C 0.32205(9) 0.8341(3) -0.02726(16) 0.0395(6) Uani 1 1 d . . . H9 H 0.3407 0.8924 0.0024 0.047 Uiso 1 1 calc R . . C10 C 0.28570(10) 0.9065(4) -0.05794(19) 0.0509(8) Uani 1 1 d . . . H10 H 0.2807 1.0121 -0.0472 0.061 Uiso 1 1 calc R . . C11 C 0.25773(9) 0.8278(4) -0.10266(19) 0.0523(8) Uani 1 1 d . . . H11 H 0.2344 0.8800 -0.1229 0.063 Uiso 1 1 calc R . . C12 C 0.26428(8) 0.6667(4) -0.11822(15) 0.0413(7) Uani 1 1 d . . . C13 C 0.30005(7) 0.5916(3) -0.08548(13) 0.0317(6) Uani 1 1 d . . . C14 C 0.23838(9) 0.5724(5) -0.16494(17) 0.0510(8) Uani 1 1 d . . . H14 H 0.2147 0.6162 -0.1882 0.061 Uiso 1 1 calc R . . C15 C 0.24788(9) 0.4185(5) -0.17611(16) 0.0516(9) Uani 1 1 d . . . H15 H 0.2311 0.3570 -0.2076 0.062 Uiso 1 1 calc R . . C16 C 0.28333(9) 0.3529(4) -0.13959(15) 0.0418(7) Uani 1 1 d . . . H16 H 0.2893 0.2466 -0.1470 0.050 Uiso 1 1 calc R . . C17 C 0.38715(7) 0.2813(3) 0.14966(13) 0.0295(6) Uani 1 1 d . . . C18 C 0.36649(8) 0.3603(4) 0.20342(14) 0.0392(7) Uani 1 1 d . . . C19 C 0.35459(9) 0.2723(5) 0.26245(16) 0.0539(9) Uani 1 1 d . . . H19 H 0.3407 0.3224 0.2988 0.065 Uiso 1 1 calc R . . C20 C 0.36280(10) 0.1137(5) 0.26815(16) 0.0558(9) Uani 1 1 d . . . H20 H 0.3540 0.0568 0.3075 0.067 Uiso 1 1 calc R . . C21 C 0.38427(10) 0.0381(4) 0.21529(16) 0.0463(7) Uani 1 1 d . . . H21 H 0.3903 -0.0691 0.2199 0.056 Uiso 1 1 calc R . . C22 C 0.39686(8) 0.1211(3) 0.15522(14) 0.0341(6) Uani 1 1 d . . . C23 C 0.35725(11) 0.5351(4) 0.19822(18) 0.0559(9) Uani 1 1 d . . . H23A H 0.3381 0.5636 0.2340 0.084 Uiso 1 1 calc R . . H23B H 0.3451 0.5591 0.1508 0.084 Uiso 1 1 calc R . . H23C H 0.3826 0.5938 0.2065 0.084 Uiso 1 1 calc R . . C24 C 0.42123(11) 0.0394(4) 0.09924(17) 0.0490(8) Uani 1 1 d . . . H24A H 0.4499 0.0714 0.1047 0.073 Uiso 1 1 calc R . . H24B H 0.4100 0.0676 0.0517 0.073 Uiso 1 1 calc R . . H24C H 0.4193 -0.0731 0.1055 0.073 Uiso 1 1 calc R . . C25 C 0.38889(9) 0.2405(4) -0.07450(15) 0.0388(6) Uani 1 1 d . . . H25A H 0.3824 0.2731 -0.1236 0.058 Uiso 1 1 calc R . . H25B H 0.3829 0.1298 -0.0697 0.058 Uiso 1 1 calc R . . H25C H 0.4179 0.2591 -0.0621 0.058 Uiso 1 1 calc R . . C26 C 0.30836(8) 0.2786(4) 0.04557(14) 0.0366(6) Uani 1 1 d . . . H26A H 0.3015 0.3529 0.0823 0.055 Uiso 1 1 calc R . . H26B H 0.3167 0.1801 0.0679 0.055 Uiso 1 1 calc R . . H26C H 0.2845 0.2616 0.0129 0.055 Uiso 1 1 calc R . . C27 C 0.0000 0.1324(8) 0.2500 0.095(2) Uani 1 2 d SU . . C28 C 0.02982(13) 0.0418(9) 0.2166(2) 0.0993(16) Uani 1 1 d U A . H28 H 0.0509 0.0909 0.1926 0.119 Uiso 1 1 calc R . . C29 C 0.0277(2) -0.1179(10) 0.2195(3) 0.124(2) Uani 1 1 d U . . H29 H 0.0477 -0.1786 0.1980 0.149 Uiso 1 1 calc R A . C30 C 0.0000 -0.1828(13) 0.2500 0.139(3) Uani 1 2 d SU . . H30 H 0.0000 -0.2929 0.2500 0.167 Uiso 1 2 calc SR . . C31 C -0.01653(4) 0.30090(14) 0.27609(6) 0.085(3) Uani 0.50 1 d PU A -1 H31A H -0.0423 0.2869 0.2991 0.127 Uiso 0.50 1 calc PR A -1 H31B H -0.0209 0.3694 0.2349 0.127 Uiso 0.50 1 calc PR A -1 H31C H 0.0038 0.3472 0.3099 0.127 Uiso 0.50 1 calc PR A -1 N1 N 0.36403(4) 0.58715(14) -0.01326(6) 0.0285(5) Uani 1 1 d R . . N2 N 0.30857(4) 0.43558(14) -0.09522(6) 0.0329(5) Uani 1 1 d R . . N3 N 0.39572(4) 0.36979(14) 0.08511(6) 0.0263(4) Uani 1 1 d 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 0.0239(4) 0.0294(4) 0.0263(4) 0.0009(3) 0.0000(3) -0.0027(3) C1 0.0264(12) 0.0267(12) 0.0263(12) -0.0058(10) 0.0012(9) 0.0006(9) C2 0.0314(13) 0.0322(13) 0.0298(13) 0.0007(10) 0.0001(10) -0.0001(11) C3 0.0375(14) 0.0333(14) 0.0358(14) 0.0012(11) 0.0065(11) -0.0053(11) C4 0.0263(13) 0.0404(15) 0.0429(15) -0.0038(12) 0.0055(11) -0.0076(11) C5 0.0257(12) 0.0377(15) 0.0349(14) -0.0046(11) -0.0017(10) 0.0000(11) C6 0.0253(12) 0.0299(13) 0.0284(12) -0.0040(10) 0.0006(9) 0.0006(10) C7 0.0235(12) 0.0333(13) 0.0276(12) -0.0020(10) -0.0028(9) 0.0046(10) C8 0.0245(12) 0.0378(14) 0.0304(13) 0.0077(11) 0.0025(10) 0.0027(10) C9 0.0343(14) 0.0393(16) 0.0448(16) 0.0020(13) 0.0017(12) 0.0052(12) C10 0.0432(17) 0.0478(18) 0.062(2) 0.0089(16) 0.0055(15) 0.0166(14) C11 0.0312(15) 0.064(2) 0.061(2) 0.0213(17) -0.0005(14) 0.0156(15) C12 0.0237(13) 0.0611(19) 0.0389(15) 0.0172(14) 0.0012(11) 0.0013(12) C13 0.0241(12) 0.0420(15) 0.0292(13) 0.0101(11) 0.0026(10) -0.0009(11) C14 0.0279(14) 0.079(2) 0.0446(17) 0.0224(17) -0.0074(12) -0.0058(15) C15 0.0380(16) 0.079(2) 0.0358(15) 0.0132(16) -0.0112(12) -0.0231(16) C16 0.0374(15) 0.0514(18) 0.0358(15) 0.0065(13) -0.0038(12) -0.0145(13) C17 0.0235(12) 0.0417(15) 0.0228(12) 0.0015(10) -0.0023(9) -0.0026(10) C18 0.0297(13) 0.0593(19) 0.0282(13) -0.0051(12) -0.0013(10) 0.0040(13) C19 0.0375(16) 0.098(3) 0.0264(14) -0.0033(16) 0.0053(12) -0.0020(17) C20 0.0494(18) 0.086(3) 0.0310(15) 0.0164(17) -0.0019(13) -0.0220(18) C21 0.0497(17) 0.0506(18) 0.0374(16) 0.0133(14) -0.0082(13) -0.0144(14) C22 0.0331(14) 0.0385(14) 0.0301(13) 0.0040(11) -0.0044(10) -0.0070(11) C23 0.0528(19) 0.071(2) 0.0441(18) -0.0165(16) 0.0011(14) 0.0226(17) C24 0.067(2) 0.0343(15) 0.0457(17) 0.0023(13) 0.0056(15) 0.0080(15) C25 0.0399(15) 0.0441(16) 0.0322(14) -0.0031(12) -0.0004(11) 0.0040(12) C26 0.0283(13) 0.0469(16) 0.0343(14) 0.0066(12) -0.0019(10) -0.0069(12) C27 0.112(4) 0.072(3) 0.092(4) 0.000 -0.073(3) 0.000 C28 0.052(2) 0.201(4) 0.043(2) 0.042(3) -0.0174(16) -0.037(3) C29 0.102(4) 0.193(5) 0.072(3) -0.057(3) -0.039(3) 0.081(4) C30 0.160(6) 0.114(5) 0.132(5) 0.000 -0.100(4) 0.000 C31 0.090(5) 0.084(5) 0.077(4) 0.001(4) -0.018(4) 0.019(4) N1 0.0232(10) 0.0295(11) 0.0323(11) 0.0018(9) -0.0032(8) 0.0007(8) N2 0.0277(11) 0.0422(13) 0.0284(11) 0.0062(9) -0.0011(8) -0.0081(10) N3 0.0238(10) 0.0301(11) 0.0250(10) -0.0005(8) 0.0012(8) 0.0013(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.9168(14) . ? Al1 C26 1.978(3) . ? Al1 C25 1.980(3) . ? Al1 N3 2.1189(14) . ? Al1 N2 2.2018(14) . ? C1 N1 1.387(3) . ? C1 C2 1.414(4) . ? C1 C6 1.422(3) . ? C2 C3 1.378(4) . ? C2 H2 0.9300 . ? C3 C4 1.393(4) . ? C3 H3 0.9300 . ? C4 C5 1.368(4) . ? C4 H4 0.9300 . ? C5 C6 1.404(3) . ? C5 H5 0.9300 . ? C6 C7 1.443(4) . ? C7 N3 1.291(3) . ? C7 H7 0.9300 . ? C8 C9 1.377(4) . ? C8 N1 1.403(3) . ? C8 C13 1.427(4) . ? C9 C10 1.409(4) . ? C9 H9 0.9300 . ? C10 C11 1.359(5) . ? C10 H10 0.9300 . ? C11 C12 1.410(5) . ? C11 H11 0.9300 . ? C12 C14 1.411(5) . ? C12 C13 1.418(4) . ? C13 N2 1.361(3) . ? C14 C15 1.354(5) . ? C14 H14 0.9300 . ? C15 C16 1.404(4) . ? C15 H15 0.9300 . ? C16 N2 1.320(3) . ? C16 H16 0.9300 . ? C17 C22 1.392(4) . ? C17 C18 1.397(4) . ? C17 N3 1.448(3) . ? C18 C19 1.393(4) . ? C18 C23 1.508(5) . ? C19 C20 1.368(5) . ? C19 H19 0.9300 . ? C20 C21 1.385(5) . ? C20 H20 0.9300 . ? C21 C22 1.393(4) . ? C21 H21 0.9300 . ? C22 C24 1.502(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.398(7) . ? C27 C28 1.398(7) 2 ? C27 C31 1.604(6) 2 ? C27 C31 1.604(6) . ? C28 C29 1.353(9) . ? C28 H28 0.9300 . ? C29 C30 1.212(10) . ? C29 H29 0.9300 . ? C30 C29 1.212(10) 2 ? C30 H30 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Al1 C26 120.28(10) . . ? N1 Al1 C25 113.37(10) . . ? C26 Al1 C25 125.63(13) . . ? N1 Al1 N3 85.34(5) . . ? C26 Al1 N3 92.54(9) . . ? C25 Al1 N3 100.05(9) . . ? N1 Al1 N2 78.2 . . ? C26 Al1 N2 88.54(9) . . ? C25 Al1 N2 94.25(9) . . ? N3 Al1 N2 161.53(8) . . ? N1 C1 C2 122.4(2) . . ? N1 C1 C6 120.7(2) . . ? C2 C1 C6 116.9(2) . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 121.1(2) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 118.6(2) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 122.0(2) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.8(2) . . ? C5 C6 C7 117.4(2) . . ? C1 C6 C7 122.4(2) . . ? N3 C7 C6 124.5(2) . . ? N3 C7 H7 117.8 . . ? C6 C7 H7 117.8 . . ? C9 C8 N1 127.1(2) . . ? C9 C8 C13 117.8(2) . . ? N1 C8 C13 115.0(2) . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 122.4(3) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 119.7(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C14 125.5(3) . . ? C11 C12 C13 118.2(3) . . ? C14 C12 C13 116.3(3) . . ? N2 C13 C12 122.8(2) . . ? N2 C13 C8 115.6(2) . . ? C12 C13 C8 121.6(3) . . ? C15 C14 C12 120.4(3) . . ? C15 C14 H14 119.8 . . ? C12 C14 H14 119.8 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? N2 C16 C15 122.8(3) . . ? N2 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C22 C17 C18 121.8(2) . . ? C22 C17 N3 120.7(2) . . ? C18 C17 N3 117.4(2) . . ? C19 C18 C17 117.7(3) . . ? C19 C18 C23 120.7(3) . . ? C17 C18 C23 121.5(3) . . ? C20 C19 C18 121.5(3) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 119.9(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 120.7(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C17 C22 C21 118.3(3) . . ? C17 C22 C24 121.3(2) . . ? C21 C22 C24 120.3(3) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al1 C25 H25A 109.5 . . ? Al1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Al1 C26 H26A 109.5 . . ? Al1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C28 113.6(7) . 2 ? C28 C27 C31 96.1(3) . 2 ? C28 C27 C31 150.1(4) 2 2 ? C28 C27 C31 150.1(4) . . ? C28 C27 C31 96.1(3) 2 . ? C31 C27 C31 54.8(2) 2 . ? C29 C28 C27 119.4(5) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C30 C29 C28 120.6(8) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C29 126.2(12) 2 . ? C29 C30 H30 116.9 2 . ? C29 C30 H30 116.9 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 N1 C8 120.33(17) . . ? C1 N1 Al1 121.82(13) . . ? C8 N1 Al1 115.42(13) . . ? C16 N2 C13 118.3(2) . . ? C16 N2 Al1 131.94(16) . . ? C13 N2 Al1 107.72(12) . . ? C7 N3 C17 116.68(17) . . ? C7 N3 Al1 121.54(13) . . ? C17 N3 Al1 121.53(12) . . ? 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 C3 -177.6(2) . . . . ? C6 C1 C2 C3 0.0(4) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C1 -1.8(4) . . . . ? C4 C5 C6 C7 -175.6(2) . . . . ? N1 C1 C6 C5 179.0(2) . . . . ? C2 C1 C6 C5 1.5(3) . . . . ? N1 C1 C6 C7 -7.5(3) . . . . ? C2 C1 C6 C7 174.9(2) . . . . ? C5 C6 C7 N3 -164.8(2) . . . . ? C1 C6 C7 N3 21.6(4) . . . . ? N1 C8 C9 C10 -178.2(2) . . . . ? C13 C8 C9 C10 -1.3(4) . . . . ? C8 C9 C10 C11 -1.2(5) . . . . ? C9 C10 C11 C12 1.5(5) . . . . ? C10 C11 C12 C14 -178.3(3) . . . . ? C10 C11 C12 C13 0.7(4) . . . . ? C11 C12 C13 N2 178.0(2) . . . . ? C14 C12 C13 N2 -2.9(4) . . . . ? C11 C12 C13 C8 -3.3(4) . . . . ? C14 C12 C13 C8 175.8(2) . . . . ? C9 C8 C13 N2 -177.6(2) . . . . ? N1 C8 C13 N2 -0.3(3) . . . . ? C9 C8 C13 C12 3.6(4) . . . . ? N1 C8 C13 C12 -179.1(2) . . . . ? C11 C12 C14 C15 179.7(3) . . . . ? C13 C12 C14 C15 0.6(4) . . . . ? C12 C14 C15 C16 1.2(5) . . . . ? C14 C15 C16 N2 -1.1(4) . . . . ? C22 C17 C18 C19 -1.9(4) . . . . ? N3 C17 C18 C19 174.0(2) . . . . ? C22 C17 C18 C23 178.1(3) . . . . ? N3 C17 C18 C23 -6.0(4) . . . . ? C17 C18 C19 C20 0.2(4) . . . . ? C23 C18 C19 C20 -179.8(3) . . . . ? C18 C19 C20 C21 1.5(5) . . . . ? C19 C20 C21 C22 -1.5(5) . . . . ? C18 C17 C22 C21 2.0(4) . . . . ? N3 C17 C22 C21 -173.8(2) . . . . ? C18 C17 C22 C24 -176.4(3) . . . . ? N3 C17 C22 C24 7.8(4) . . . . ? C20 C21 C22 C17 -0.3(4) . . . . ? C20 C21 C22 C24 178.2(3) . . . . ? C28 C27 C28 C29 -0.4(3) 2 . . . ? C31 C27 C28 C29 -176.3(4) 2 . . . ? C31 C27 C28 C29 171.3(3) . . . . ? C27 C28 C29 C30 0.9(7) . . . . ? C28 C29 C30 C29 -0.5(3) . . . 2 ? C2 C1 N1 C8 -22.5(3) . . . . ? C6 C1 N1 C8 160.1(2) . . . . ? C2 C1 N1 Al1 139.06(19) . . . . ? C6 C1 N1 Al1 -38.4(3) . . . . ? C9 C8 N1 C1 -42.6(3) . . . . ? C13 C8 N1 C1 140.4(2) . . . . ? C9 C8 N1 Al1 154.8(2) . . . . ? C13 C8 N1 Al1 -22.2(2) . . . . ? C26 Al1 N1 C1 140.85(16) . . . . ? C25 Al1 N1 C1 -48.32(17) . . . . ? N3 Al1 N1 C1 50.63(16) . . . . ? N2 Al1 N1 C1 -137.89(13) . . . . ? C26 Al1 N1 C8 -56.77(17) . . . . ? C25 Al1 N1 C8 114.06(16) . . . . ? N3 Al1 N1 C8 -147.00(12) . . . . ? N2 Al1 N1 C8 24.49(15) . . . . ? C15 C16 N2 C13 -1.0(4) . . . . ? C15 C16 N2 Al1 160.5(2) . . . . ? C12 C13 N2 C16 3.0(3) . . . . ? C8 C13 N2 C16 -175.7(2) . . . . ? C12 C13 N2 Al1 -162.6(2) . . . . ? C8 C13 N2 Al1 18.7(2) . . . . ? N1 Al1 N2 C16 173.50(18) . . . . ? C26 Al1 N2 C16 -65.1(2) . . . . ? C25 Al1 N2 C16 60.5(2) . . . . ? N3 Al1 N2 C16 -158.8(2) . . . . ? N1 Al1 N2 C13 -23.60(14) . . . . ? C26 Al1 N2 C13 97.78(15) . . . . ? C25 Al1 N2 C13 -136.60(15) . . . . ? N3 Al1 N2 C13 4.1(3) . . . . ? C6 C7 N3 C17 -165.6(2) . . . . ? C6 C7 N3 Al1 8.8(3) . . . . ? C22 C17 N3 C7 -103.9(3) . . . . ? C18 C17 N3 C7 80.2(3) . . . . ? C22 C17 N3 Al1 81.8(2) . . . . ? C18 C17 N3 Al1 -94.2(2) . . . . ? N1 Al1 N3 C7 -36.70(17) . . . . ? C26 Al1 N3 C7 -156.89(17) . . . . ? C25 Al1 N3 C7 76.23(18) . . . . ? N2 Al1 N3 C7 -63.9(3) . . . . ? N1 Al1 N3 C17 137.38(14) . . . . ? C26 Al1 N3 C17 17.19(17) . . . . ? C25 Al1 N3 C17 -109.68(17) . . . . ? N2 Al1 N3 C17 110.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.787 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.055 #===END data_complex_2a _database_code_depnum_ccdc_archive 'CCDC 871558' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H35 Al2 N3' _chemical_formula_weight 479.56 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7793(8) _cell_length_b 11.1335(9) _cell_length_c 14.3337(11) _cell_angle_alpha 71.6540(10) _cell_angle_beta 72.7750(10) _cell_angle_gamma 79.3680(10) _cell_volume 1407.67(19) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 1081 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.08 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9829 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7341 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.04 _reflns_number_total 5427 _reflns_number_gt 3824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^2^+0.3185P] 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 5427 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.29799(8) 0.80406(7) 0.45130(6) 0.0386(2) Uani 1 1 d . . . Al2 Al 0.24956(8) 0.66423(8) 0.10818(6) 0.0391(2) Uani 1 1 d . . . C1 C 0.0002(2) 0.8133(2) 0.43443(17) 0.0334(5) Uani 1 1 d . . . C2 C -0.0383(2) 0.7423(2) 0.38110(17) 0.0334(5) Uani 1 1 d . . . C3 C -0.1720(3) 0.6921(2) 0.42057(18) 0.0389(6) Uani 1 1 d . . . H3 H -0.2002 0.6462 0.3847 0.047 Uiso 1 1 calc R . . C4 C -0.2629(3) 0.7087(2) 0.51099(19) 0.0428(6) Uani 1 1 d . . . H4 H -0.3526 0.6736 0.5374 0.051 Uiso 1 1 calc R . . C5 C -0.2232(3) 0.7762(2) 0.5626(2) 0.0447(6) Uani 1 1 d . . . H5 H -0.2856 0.7868 0.6250 0.054 Uiso 1 1 calc R . . C6 C -0.0938(3) 0.8287(2) 0.52473(19) 0.0406(6) Uani 1 1 d . . . H6 H -0.0688 0.8760 0.5610 0.049 Uiso 1 1 calc R . . C7 C 0.1564(3) 0.9685(2) 0.31362(17) 0.0337(5) Uani 1 1 d . . . C8 C 0.0582(3) 1.0382(2) 0.2598(2) 0.0420(6) Uani 1 1 d . . . H8 H -0.0373 1.0152 0.2802 0.050 Uiso 1 1 calc R . . C9 C 0.0976(3) 1.1429(3) 0.1752(2) 0.0522(7) Uani 1 1 d . . . H9 H 0.0279 1.1881 0.1392 0.063 Uiso 1 1 calc R . . C10 C 0.2323(3) 1.1818(3) 0.1431(2) 0.0517(7) Uani 1 1 d . . . H10 H 0.2559 1.2526 0.0854 0.062 Uiso 1 1 calc R . . C11 C 0.3359(3) 1.1158(2) 0.19637(18) 0.0423(6) Uani 1 1 d . . . C12 C 0.2970(3) 1.0089(2) 0.27985(17) 0.0350(5) Uani 1 1 d . . . C13 C 0.4766(3) 1.1496(3) 0.1742(2) 0.0517(7) Uani 1 1 d . . . H13 H 0.5074 1.2215 0.1192 0.062 Uiso 1 1 calc R . . C14 C 0.5690(3) 1.0796(3) 0.2315(2) 0.0539(7) Uani 1 1 d . . . H14 H 0.6634 1.1030 0.2168 0.065 Uiso 1 1 calc R . . C15 C 0.5240(3) 0.9742(3) 0.3111(2) 0.0497(7) Uani 1 1 d . . . H15 H 0.5897 0.9254 0.3494 0.060 Uiso 1 1 calc R . . C16 C 0.0706(2) 0.7182(2) 0.29233(17) 0.0336(5) Uani 1 1 d . . . H16 H 0.1649 0.7320 0.2894 0.040 Uiso 1 1 calc R . . C17 C -0.0730(2) 0.6637(2) 0.20496(17) 0.0341(5) Uani 1 1 d . . . C18 C -0.1513(3) 0.7674(2) 0.15474(18) 0.0401(6) Uani 1 1 d . . . C19 C -0.2793(3) 0.7482(3) 0.1405(2) 0.0539(7) Uani 1 1 d . . . H19 H -0.3361 0.8184 0.1078 0.065 Uiso 1 1 calc R . . C20 C -0.3243(3) 0.6286(3) 0.1735(2) 0.0629(9) Uani 1 1 d . . . H20 H -0.4118 0.6166 0.1631 0.076 Uiso 1 1 calc R . . C21 C -0.2434(3) 0.5256(3) 0.2217(2) 0.0588(8) Uani 1 1 d . . . H21 H -0.2756 0.4434 0.2437 0.071 Uiso 1 1 calc R . . C22 C -0.1156(3) 0.5408(2) 0.2383(2) 0.0423(6) Uani 1 1 d . . . C23 C 0.3751(3) 0.6349(3) 0.4369(3) 0.0639(8) Uani 1 1 d . . . H23A H 0.3090 0.5730 0.4838 0.096 Uiso 1 1 calc R . . H23B H 0.4691 0.6126 0.4526 0.096 Uiso 1 1 calc R . . H23C H 0.3861 0.6338 0.3669 0.096 Uiso 1 1 calc R . . C24 C 0.3021(3) 0.8467(3) 0.5728(2) 0.0521(7) Uani 1 1 d . . . H24A H 0.2862 0.9392 0.5610 0.078 Uiso 1 1 calc R . . H24B H 0.3960 0.8156 0.5877 0.078 Uiso 1 1 calc R . . H24C H 0.2263 0.8067 0.6306 0.078 Uiso 1 1 calc R . . C25 C 0.1845(3) 0.6742(4) -0.0119(2) 0.0654(9) Uani 1 1 d . . . H25A H 0.2653 0.6465 -0.0627 0.098 Uiso 1 1 calc R . . H25B H 0.1484 0.7622 -0.0410 0.098 Uiso 1 1 calc R . . H25C H 0.1074 0.6190 0.0083 0.098 Uiso 1 1 calc R . . C26 C 0.3420(3) 0.8137(3) 0.0975(2) 0.0476(7) Uani 1 1 d . . . H26A H 0.4307 0.8207 0.0426 0.071 Uiso 1 1 calc R . . H26B H 0.3649 0.8035 0.1619 0.071 Uiso 1 1 calc R . . H26C H 0.2761 0.8909 0.0828 0.071 Uiso 1 1 calc R . . C27 C 0.3499(3) 0.4984(3) 0.1655(3) 0.0639(9) Uani 1 1 d . . . H27A H 0.2952 0.4298 0.1712 0.096 Uiso 1 1 calc R . . H27B H 0.3579 0.4944 0.2329 0.096 Uiso 1 1 calc R . . H27C H 0.4463 0.4887 0.1207 0.096 Uiso 1 1 calc R . . C28 C -0.1012(3) 0.8980(3) 0.1157(2) 0.0545(7) Uani 1 1 d . . . H28A H -0.1136 0.9326 0.1729 0.082 Uiso 1 1 calc R . . H28B H -0.1580 0.9536 0.0696 0.082 Uiso 1 1 calc R . . H28C H 0.0007 0.8929 0.0789 0.082 Uiso 1 1 calc R . . C29 C -0.0295(3) 0.4296(3) 0.2944(3) 0.0606(8) Uani 1 1 d . . . H29A H -0.0785 0.3527 0.3146 0.091 Uiso 1 1 calc R . . H29B H -0.0204 0.4470 0.3551 0.091 Uiso 1 1 calc R . . H29C H 0.0665 0.4170 0.2498 0.091 Uiso 1 1 calc R . . N1 N 0.1343(2) 0.86587(18) 0.39906(14) 0.0338(4) Uani 1 1 d . . . N2 N 0.3922(2) 0.93901(19) 0.33573(15) 0.0376(5) Uani 1 1 d . . . N3 N 0.06341(19) 0.68169(17) 0.21716(14) 0.0322(4) 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 Al1 0.0379(4) 0.0374(4) 0.0437(4) -0.0078(3) -0.0174(3) -0.0056(3) Al2 0.0289(4) 0.0529(5) 0.0410(4) -0.0227(4) -0.0061(3) -0.0055(3) C1 0.0331(13) 0.0318(12) 0.0355(13) -0.0078(10) -0.0123(10) -0.0009(10) C2 0.0298(12) 0.0372(13) 0.0342(13) -0.0112(10) -0.0089(10) -0.0019(10) C3 0.0349(13) 0.0457(14) 0.0395(14) -0.0158(12) -0.0086(11) -0.0069(11) C4 0.0349(13) 0.0471(15) 0.0438(15) -0.0138(12) -0.0033(11) -0.0071(11) C5 0.0440(15) 0.0500(15) 0.0377(14) -0.0194(12) -0.0001(11) -0.0035(12) C6 0.0453(15) 0.0429(14) 0.0382(14) -0.0187(12) -0.0082(11) -0.0063(11) C7 0.0406(13) 0.0326(12) 0.0329(13) -0.0143(10) -0.0122(10) -0.0024(10) C8 0.0469(15) 0.0404(14) 0.0461(15) -0.0151(12) -0.0210(12) -0.0016(11) C9 0.072(2) 0.0437(16) 0.0500(17) -0.0092(13) -0.0356(15) -0.0009(14) C10 0.078(2) 0.0427(15) 0.0381(15) -0.0057(12) -0.0202(14) -0.0157(14) C11 0.0580(17) 0.0406(14) 0.0323(13) -0.0172(11) -0.0055(12) -0.0119(12) C12 0.0430(14) 0.0340(13) 0.0335(13) -0.0159(10) -0.0107(11) -0.0038(10) C13 0.0636(18) 0.0517(17) 0.0380(15) -0.0177(13) 0.0072(13) -0.0254(14) C14 0.0467(16) 0.0613(19) 0.0551(17) -0.0214(15) -0.0007(14) -0.0198(14) C15 0.0380(15) 0.0570(17) 0.0565(17) -0.0197(14) -0.0087(13) -0.0093(12) C16 0.0293(12) 0.0387(13) 0.0363(13) -0.0126(11) -0.0103(10) -0.0048(10) C17 0.0302(12) 0.0438(14) 0.0328(12) -0.0164(11) -0.0053(10) -0.0092(10) C18 0.0325(13) 0.0514(15) 0.0366(14) -0.0118(12) -0.0082(11) -0.0063(11) C19 0.0361(15) 0.075(2) 0.0536(17) -0.0169(15) -0.0188(13) -0.0032(14) C20 0.0442(17) 0.090(2) 0.069(2) -0.0251(19) -0.0229(15) -0.0213(16) C21 0.0556(18) 0.065(2) 0.068(2) -0.0243(16) -0.0142(16) -0.0274(15) C22 0.0397(14) 0.0470(15) 0.0443(15) -0.0187(12) -0.0059(11) -0.0113(11) C23 0.065(2) 0.0453(17) 0.084(2) -0.0131(16) -0.0344(18) 0.0043(14) C24 0.0533(17) 0.0601(18) 0.0471(16) -0.0101(14) -0.0204(13) -0.0116(14) C25 0.0495(18) 0.111(3) 0.0494(18) -0.0393(18) -0.0081(14) -0.0183(17) C26 0.0373(14) 0.0574(17) 0.0485(15) -0.0177(13) -0.0047(12) -0.0107(12) C27 0.0422(16) 0.0535(18) 0.100(3) -0.0342(18) -0.0125(17) -0.0023(13) C28 0.0461(16) 0.0498(17) 0.0610(18) -0.0027(14) -0.0186(14) -0.0030(13) C29 0.0594(19) 0.0397(16) 0.082(2) -0.0120(15) -0.0189(17) -0.0103(13) N1 0.0352(11) 0.0337(11) 0.0350(11) -0.0083(9) -0.0120(9) -0.0066(8) N2 0.0334(11) 0.0405(11) 0.0412(12) -0.0154(10) -0.0075(9) -0.0056(9) N3 0.0271(10) 0.0372(11) 0.0351(11) -0.0127(9) -0.0086(8) -0.0046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N1 1.891(2) . ? Al1 C23 1.946(3) . ? Al1 C24 1.958(3) . ? Al1 N2 1.973(2) . ? Al2 C25 1.970(3) . ? Al2 C27 1.975(3) . ? Al2 C26 1.981(3) . ? Al2 N3 2.0417(19) . ? C1 C6 1.388(3) . ? C1 C2 1.419(3) . ? C1 N1 1.422(3) . ? C2 C3 1.405(3) . ? C2 C16 1.460(3) . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.375(4) . ? C4 H4 0.9500 . ? C5 C6 1.380(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.380(3) . ? C7 C8 1.381(3) . ? C7 C12 1.423(3) . ? C8 C9 1.405(4) . ? C8 H8 0.9500 . ? C9 C10 1.365(4) . ? C9 H9 0.9500 . ? C10 C11 1.407(4) . ? C10 H10 0.9500 . ? C11 C13 1.412(4) . ? C11 C12 1.412(3) . ? C12 N2 1.377(3) . ? C13 C14 1.370(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 N2 1.330(3) . ? C15 H15 0.9500 . ? C16 N3 1.289(3) . ? C16 H16 0.9500 . ? C17 C18 1.384(3) . ? C17 C22 1.398(3) . ? C17 N3 1.453(3) . ? C18 C19 1.389(3) . ? C18 C28 1.501(4) . ? C19 C20 1.375(4) . ? C19 H19 0.9500 . ? C20 C21 1.381(4) . ? C20 H20 0.9500 . ? C21 C22 1.388(4) . ? C21 H21 0.9500 . ? C22 C29 1.509(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 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 Al1 C23 111.80(11) . . ? N1 Al1 C24 118.16(11) . . ? C23 Al1 C24 119.04(13) . . ? N1 Al1 N2 84.76(9) . . ? C23 Al1 N2 112.13(12) . . ? C24 Al1 N2 105.17(11) . . ? C25 Al2 C27 114.80(15) . . ? C25 Al2 C26 114.89(14) . . ? C27 Al2 C26 114.52(12) . . ? C25 Al2 N3 104.19(10) . . ? C27 Al2 N3 105.14(12) . . ? C26 Al2 N3 101.09(10) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 N1 119.4(2) . . ? C2 C1 N1 121.6(2) . . ? C3 C2 C1 118.7(2) . . ? C3 C2 C16 124.5(2) . . ? C1 C2 C16 116.6(2) . . ? C4 C3 C2 120.7(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.9(2) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.7(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.9(2) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? N1 C7 C8 128.1(2) . . ? N1 C7 C12 115.1(2) . . ? C8 C7 C12 116.8(2) . . ? C7 C8 C9 120.9(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 122.3(3) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 119.3(3) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C11 C13 125.0(3) . . ? C10 C11 C12 118.3(2) . . ? C13 C11 C12 116.7(2) . . ? N2 C12 C11 121.9(2) . . ? N2 C12 C7 115.6(2) . . ? C11 C12 C7 122.4(2) . . ? C14 C13 C11 120.4(3) . . ? C14 C13 H13 119.8 . . ? C11 C13 H13 119.8 . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N2 C15 C14 122.4(3) . . ? N2 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N3 C16 C2 132.4(2) . . ? N3 C16 H16 113.8 . . ? C2 C16 H16 113.8 . . ? C18 C17 C22 122.4(2) . . ? C18 C17 N3 118.7(2) . . ? C22 C17 N3 118.8(2) . . ? C17 C18 C19 118.2(2) . . ? C17 C18 C28 121.9(2) . . ? C19 C18 C28 120.0(2) . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 120.8(3) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 117.5(3) . . ? C21 C22 C29 121.1(2) . . ? C17 C22 C29 121.3(2) . . ? Al1 C23 H23A 109.5 . . ? Al1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Al1 C24 H24A 109.5 . . ? Al1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Al2 C26 H26A 109.5 . . ? Al2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Al2 C27 H27A 109.5 . . ? Al2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C22 C29 H29A 109.5 . . ? C22 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C22 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C7 N1 C1 119.14(19) . . ? C7 N1 Al1 113.64(15) . . ? C1 N1 Al1 127.09(15) . . ? C15 N2 C12 119.0(2) . . ? C15 N2 Al1 129.99(19) . . ? C12 N2 Al1 110.83(16) . . ? C16 N3 C17 121.77(19) . . ? C16 N3 Al2 117.56(15) . . ? C17 N3 Al2 120.47(14) . . ? 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 C6 C1 C2 C3 1.3(3) . . . . ? N1 C1 C2 C3 179.5(2) . . . . ? C6 C1 C2 C16 -173.9(2) . . . . ? N1 C1 C2 C16 4.3(3) . . . . ? C1 C2 C3 C4 -1.6(4) . . . . ? C16 C2 C3 C4 173.2(2) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C1 -0.8(4) . . . . ? C2 C1 C6 C5 -0.1(4) . . . . ? N1 C1 C6 C5 -178.3(2) . . . . ? N1 C7 C8 C9 178.4(2) . . . . ? C12 C7 C8 C9 0.7(3) . . . . ? C7 C8 C9 C10 -1.0(4) . . . . ? C8 C9 C10 C11 -0.3(4) . . . . ? C9 C10 C11 C13 -176.8(3) . . . . ? C9 C10 C11 C12 1.8(4) . . . . ? C10 C11 C12 N2 179.8(2) . . . . ? C13 C11 C12 N2 -1.4(3) . . . . ? C10 C11 C12 C7 -2.1(3) . . . . ? C13 C11 C12 C7 176.7(2) . . . . ? N1 C7 C12 N2 1.1(3) . . . . ? C8 C7 C12 N2 179.04(19) . . . . ? N1 C7 C12 C11 -177.15(19) . . . . ? C8 C7 C12 C11 0.8(3) . . . . ? C10 C11 C13 C14 179.3(3) . . . . ? C12 C11 C13 C14 0.7(4) . . . . ? C11 C13 C14 C15 0.6(4) . . . . ? C13 C14 C15 N2 -1.2(4) . . . . ? C3 C2 C16 N3 21.3(4) . . . . ? C1 C2 C16 N3 -163.7(2) . . . . ? C22 C17 C18 C19 2.3(4) . . . . ? N3 C17 C18 C19 177.9(2) . . . . ? C22 C17 C18 C28 -177.5(2) . . . . ? N3 C17 C18 C28 -1.9(4) . . . . ? C17 C18 C19 C20 -1.5(4) . . . . ? C28 C18 C19 C20 178.2(3) . . . . ? C18 C19 C20 C21 0.3(5) . . . . ? C19 C20 C21 C22 0.4(5) . . . . ? C20 C21 C22 C17 0.3(4) . . . . ? C20 C21 C22 C29 177.7(3) . . . . ? C18 C17 C22 C21 -1.7(4) . . . . ? N3 C17 C22 C21 -177.3(2) . . . . ? C18 C17 C22 C29 -179.0(2) . . . . ? N3 C17 C22 C29 5.4(4) . . . . ? C8 C7 N1 C1 6.5(3) . . . . ? C12 C7 N1 C1 -175.8(2) . . . . ? C8 C7 N1 Al1 -177.4(2) . . . . ? C12 C7 N1 Al1 0.4(2) . . . . ? C6 C1 N1 C7 -110.1(2) . . . . ? C2 C1 N1 C7 71.7(3) . . . . ? C6 C1 N1 Al1 74.3(3) . . . . ? C2 C1 N1 Al1 -103.9(2) . . . . ? C23 Al1 N1 C7 -112.86(18) . . . . ? C24 Al1 N1 C7 103.32(18) . . . . ? N2 Al1 N1 C7 -1.10(15) . . . . ? C23 Al1 N1 C1 62.9(2) . . . . ? C24 Al1 N1 C1 -80.9(2) . . . . ? N2 Al1 N1 C1 174.7(2) . . . . ? C14 C15 N2 C12 0.5(4) . . . . ? C14 C15 N2 Al1 -173.98(19) . . . . ? C11 C12 N2 C15 0.8(3) . . . . ? C7 C12 N2 C15 -177.4(2) . . . . ? C11 C12 N2 Al1 176.35(17) . . . . ? C7 C12 N2 Al1 -1.9(2) . . . . ? N1 Al1 N2 C15 176.5(2) . . . . ? C23 Al1 N2 C15 -72.1(3) . . . . ? C24 Al1 N2 C15 58.7(2) . . . . ? N1 Al1 N2 C12 1.64(15) . . . . ? C23 Al1 N2 C12 113.06(17) . . . . ? C24 Al1 N2 C12 -116.15(17) . . . . ? C2 C16 N3 C17 4.0(4) . . . . ? C2 C16 N3 Al2 179.0(2) . . . . ? C18 C17 N3 C16 86.2(3) . . . . ? C22 C17 N3 C16 -98.1(3) . . . . ? C18 C17 N3 Al2 -88.6(2) . . . . ? C22 C17 N3 Al2 87.2(2) . . . . ? C25 Al2 N3 C16 -158.68(19) . . . . ? C27 Al2 N3 C16 80.2(2) . . . . ? C26 Al2 N3 C16 -39.21(19) . . . . ? C25 Al2 N3 C17 16.3(2) . . . . ? C27 Al2 N3 C17 -104.80(19) . . . . ? C26 Al2 N3 C17 135.79(18) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.280 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.049 #===END data_complex_2c _database_code_depnum_ccdc_archive 'CCDC 871559' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H57 Al2 N3' _chemical_formula_weight 621.84 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1624(7) _cell_length_b 12.6833(7) _cell_length_c 13.7183(8) _cell_angle_alpha 80.7440(10) _cell_angle_beta 78.2440(10) _cell_angle_gamma 73.3270(10) _cell_volume 1972.82(19) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 3459 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.84 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.047 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9849 _exptl_absorpt_correction_T_max 0.9889 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10239 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.03 _reflns_number_total 7589 _reflns_number_gt 5741 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.7885P] 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 7589 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.003 _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 Al2 Al 0.28181(6) -0.01320(5) 0.27308(5) 0.03564(17) Uani 1 1 d . . . Al1 Al -0.12671(5) 0.29565(5) 0.11452(5) 0.03709(17) Uani 1 1 d . . . C1 C 0.12243(16) 0.33967(16) 0.23758(14) 0.0310(4) Uani 1 1 d . . . C7 C 0.10278(17) 0.27596(16) 0.02877(14) 0.0329(4) Uani 1 1 d . . . C16 C 0.16544(16) 0.21879(16) 0.24623(14) 0.0305(4) Uani 1 1 d . . . H16 H 0.1237 0.1834 0.2163 0.037 Uiso 1 1 calc R . . C12 C 0.06556(18) 0.20871(17) -0.02524(14) 0.0358(5) Uani 1 1 d . . . C17 C 0.32660(17) 0.18894(15) 0.33298(14) 0.0316(4) Uani 1 1 d . . . C8 C 0.21491(18) 0.28685(18) -0.00212(16) 0.0407(5) Uani 1 1 d . . . H8 H 0.2426 0.3319 0.0310 0.049 Uiso 1 1 calc R . . C2 C 0.04746(17) 0.38883(16) 0.16652(14) 0.0330(4) Uani 1 1 d . . . C22 C 0.41883(17) 0.22469(17) 0.27249(16) 0.0358(5) Uani 1 1 d . . . C18 C 0.30951(19) 0.18026(17) 0.43787(15) 0.0373(5) Uani 1 1 d . . . C6 C 0.14355(18) 0.40739(17) 0.29878(16) 0.0387(5) Uani 1 1 d . . . H6 H 0.1946 0.3755 0.3459 0.046 Uiso 1 1 calc R . . C11 C 0.1395(2) 0.15362(18) -0.10567(15) 0.0441(5) Uani 1 1 d . . . C19 C 0.3877(2) 0.21098(19) 0.48122(17) 0.0465(6) Uani 1 1 d . . . H19 H 0.3777 0.2071 0.5521 0.056 Uiso 1 1 calc R . . C15 C -0.0888(2) 0.1434(2) -0.04295(18) 0.0520(6) Uani 1 1 d . . . H15 H -0.1672 0.1397 -0.0221 0.062 Uiso 1 1 calc R . . C31 C 0.44046(19) 0.2320(2) 0.15890(16) 0.0434(5) Uani 1 1 d . . . H31 H 0.3781 0.2073 0.1386 0.052 Uiso 1 1 calc R . . C3 C -0.0037(2) 0.50234(18) 0.16128(17) 0.0446(5) Uani 1 1 d . . . H3 H -0.0542 0.5361 0.1140 0.054 Uiso 1 1 calc R . . C20 C 0.4792(2) 0.2469(2) 0.42344(19) 0.0508(6) Uani 1 1 d . . . H20 H 0.5321 0.2669 0.4547 0.061 Uiso 1 1 calc R . . C5 C 0.0916(2) 0.51961(18) 0.29197(18) 0.0471(6) Uani 1 1 d . . . H5 H 0.1066 0.5645 0.3343 0.057 Uiso 1 1 calc R . . C21 C 0.49471(19) 0.25412(19) 0.32046(18) 0.0456(5) Uani 1 1 d . . . H21 H 0.5581 0.2795 0.2815 0.055 Uiso 1 1 calc R . . C4 C 0.0176(2) 0.56647(18) 0.22340(18) 0.0516(6) Uani 1 1 d . . . H4 H -0.0189 0.6437 0.2191 0.062 Uiso 1 1 calc R . . C9 C 0.2884(2) 0.2317(2) -0.08215(18) 0.0512(6) Uani 1 1 d . . . H9 H 0.3652 0.2401 -0.1014 0.061 Uiso 1 1 calc R . . C28 C 0.2092(2) 0.1406(2) 0.50345(16) 0.0485(6) Uani 1 1 d . . . H28 H 0.1649 0.1208 0.4583 0.058 Uiso 1 1 calc R . . C10 C 0.2533(2) 0.1667(2) -0.13297(17) 0.0531(6) Uani 1 1 d . . . H10 H 0.3053 0.1304 -0.1865 0.064 Uiso 1 1 calc R . . C24 C -0.1630(2) 0.2039(2) 0.23914(18) 0.0529(6) Uani 1 1 d . . . H24A H -0.0916 0.1495 0.2548 0.079 Uiso 1 1 calc R . . H24B H -0.2193 0.1652 0.2314 0.079 Uiso 1 1 calc R . . H24C H -0.1962 0.2509 0.2937 0.079 Uiso 1 1 calc R . . C27 C 0.2967(2) -0.0126(2) 0.12692(17) 0.0514(6) Uani 1 1 d . . . H27A H 0.3641 0.0145 0.0928 0.077 Uiso 1 1 calc R . . H27B H 0.2260 0.0361 0.1042 0.077 Uiso 1 1 calc R . . H27C H 0.3075 -0.0879 0.1112 0.077 Uiso 1 1 calc R . . C14 C -0.0213(3) 0.0867(2) -0.12295(19) 0.0605(7) Uani 1 1 d . . . H14 H -0.0533 0.0451 -0.1560 0.073 Uiso 1 1 calc R . . C25 C 0.1422(2) -0.0547(2) 0.35174(19) 0.0547(6) Uani 1 1 d . . . H25A H 0.1408 -0.1266 0.3351 0.082 Uiso 1 1 calc R . . H25B H 0.0722 0.0015 0.3357 0.082 Uiso 1 1 calc R . . H25C H 0.1445 -0.0598 0.4234 0.082 Uiso 1 1 calc R . . C26 C 0.4299(2) -0.0819(2) 0.3230(2) 0.0559(6) Uani 1 1 d . . . H26A H 0.4923 -0.0549 0.2785 0.084 Uiso 1 1 calc R . . H26B H 0.4480 -0.1626 0.3246 0.084 Uiso 1 1 calc R . . H26C H 0.4229 -0.0625 0.3907 0.084 Uiso 1 1 calc R . . C33 C 0.4319(2) 0.3516(2) 0.11168(19) 0.0585(7) Uani 1 1 d . . . H33A H 0.3555 0.3991 0.1368 0.088 Uiso 1 1 calc R . . H33B H 0.4417 0.3545 0.0387 0.088 Uiso 1 1 calc R . . H33C H 0.4931 0.3776 0.1294 0.088 Uiso 1 1 calc R . . C23 C -0.2464(2) 0.4149(2) 0.0587(2) 0.0575(7) Uani 1 1 d . . . H23A H -0.2790 0.4713 0.1054 0.086 Uiso 1 1 calc R . . H23B H -0.3084 0.3849 0.0482 0.086 Uiso 1 1 calc R . . H23C H -0.2120 0.4483 -0.0054 0.086 Uiso 1 1 calc R . . C13 C 0.0913(3) 0.0916(2) -0.15330(17) 0.0574(7) Uani 1 1 d . . . H13 H 0.1378 0.0525 -0.2074 0.069 Uiso 1 1 calc R . . C32 C 0.5575(2) 0.1551(3) 0.1192(2) 0.0718(8) Uani 1 1 d . . . H32A H 0.6204 0.1782 0.1371 0.108 Uiso 1 1 calc R . . H32B H 0.5669 0.1588 0.0462 0.108 Uiso 1 1 calc R . . H32C H 0.5602 0.0790 0.1490 0.108 Uiso 1 1 calc R . . C29 C 0.2523(3) 0.0374(2) 0.5731(2) 0.0734(9) Uani 1 1 d . . . H29A H 0.3043 -0.0207 0.5335 0.110 Uiso 1 1 calc R . . H29B H 0.1857 0.0117 0.6113 0.110 Uiso 1 1 calc R . . H29C H 0.2946 0.0548 0.6194 0.110 Uiso 1 1 calc R . . C30 C 0.1249(3) 0.2310(3) 0.5642(2) 0.0757(9) Uani 1 1 d . . . H30A H 0.1666 0.2536 0.6078 0.114 Uiso 1 1 calc R . . H30B H 0.0615 0.2023 0.6051 0.114 Uiso 1 1 calc R . . H30C H 0.0926 0.2950 0.5184 0.114 Uiso 1 1 calc R . . N1 N 0.01933(14) 0.32519(14) 0.10369(12) 0.0332(4) Uani 1 1 d . . . N3 N 0.24917(13) 0.15160(13) 0.28676(11) 0.0294(4) Uani 1 1 d . . . N2 N -0.04701(15) 0.20216(14) 0.00502(13) 0.0389(4) Uani 1 1 d . . . C36 C 0.4633(7) 0.4150(4) 0.7104(7) 0.201(4) Uani 1 1 d . . . H36A H 0.4229 0.4442 0.7747 0.241 Uiso 1 1 calc R . . H36B H 0.4567 0.3382 0.7164 0.241 Uiso 1 1 calc R . . C34 C 0.6389(6) 0.3460(4) 0.7869(5) 0.181(3) Uani 1 1 d . . . H34A H 0.6182 0.3916 0.8425 0.271 Uiso 1 1 calc R . . H34B H 0.7236 0.3252 0.7664 0.271 Uiso 1 1 calc R . . H34C H 0.6115 0.2790 0.8083 0.271 Uiso 1 1 calc R . . C37 C 0.3906(9) 0.4806(7) 0.6319(5) 0.210(4) Uani 1 1 d . . . H37A H 0.3909 0.5587 0.6309 0.252 Uiso 1 1 calc R . . H37B H 0.4353 0.4568 0.5667 0.252 Uiso 1 1 calc R . . C35 C 0.5864(10) 0.4064(7) 0.7059(5) 0.210(4) Uani 1 1 d . . . H35A H 0.6298 0.3725 0.6445 0.252 Uiso 1 1 calc R . . H35B H 0.5959 0.4823 0.6985 0.252 Uiso 1 1 calc R . . C38 C 0.2720(7) 0.4823(6) 0.6308(8) 0.221(5) Uani 1 1 d . . . H38A H 0.2268 0.5030 0.6967 0.265 Uiso 1 1 calc R . . H38B H 0.2713 0.4052 0.6273 0.265 Uiso 1 1 calc R . . C39 C 0.2072(9) 0.5512(9) 0.5555(5) 0.232(5) Uani 1 1 d . . . H39A H 0.1735 0.6260 0.5757 0.349 Uiso 1 1 calc R . . H39B H 0.1448 0.5197 0.5488 0.349 Uiso 1 1 calc R . . H39C H 0.2596 0.5545 0.4912 0.349 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 Al2 0.0414(4) 0.0301(3) 0.0363(3) -0.0015(3) -0.0131(3) -0.0072(3) Al1 0.0293(3) 0.0415(4) 0.0404(4) -0.0020(3) -0.0087(3) -0.0086(3) C1 0.0282(10) 0.0315(10) 0.0325(10) -0.0028(8) -0.0047(8) -0.0071(8) C7 0.0320(11) 0.0326(10) 0.0296(10) 0.0041(8) -0.0088(8) -0.0032(8) C16 0.0307(10) 0.0339(10) 0.0285(9) -0.0018(8) -0.0070(8) -0.0106(8) C12 0.0394(12) 0.0353(11) 0.0290(10) 0.0046(8) -0.0114(9) -0.0045(9) C17 0.0321(11) 0.0271(9) 0.0360(10) -0.0021(8) -0.0129(8) -0.0044(8) C8 0.0365(12) 0.0461(12) 0.0373(11) 0.0036(9) -0.0081(9) -0.0107(10) C2 0.0287(10) 0.0365(11) 0.0328(10) -0.0020(8) -0.0040(8) -0.0089(8) C22 0.0285(11) 0.0344(11) 0.0442(12) -0.0045(9) -0.0109(9) -0.0041(9) C18 0.0440(12) 0.0347(11) 0.0348(11) -0.0012(9) -0.0143(9) -0.0089(9) C6 0.0389(12) 0.0370(11) 0.0416(12) -0.0048(9) -0.0124(9) -0.0080(9) C11 0.0550(14) 0.0404(12) 0.0295(11) 0.0022(9) -0.0093(10) -0.0028(10) C19 0.0557(15) 0.0488(13) 0.0402(12) -0.0028(10) -0.0232(11) -0.0123(11) C15 0.0597(16) 0.0558(15) 0.0492(14) -0.0042(11) -0.0220(12) -0.0204(12) C31 0.0356(12) 0.0563(14) 0.0411(12) -0.0059(10) -0.0039(9) -0.0178(10) C3 0.0488(13) 0.0374(12) 0.0439(12) 0.0015(10) -0.0176(10) -0.0018(10) C20 0.0462(14) 0.0571(15) 0.0594(15) -0.0078(12) -0.0281(12) -0.0158(12) C5 0.0567(15) 0.0365(12) 0.0510(13) -0.0094(10) -0.0154(11) -0.0100(11) C21 0.0334(12) 0.0500(13) 0.0579(14) -0.0050(11) -0.0140(10) -0.0139(10) C4 0.0646(16) 0.0291(11) 0.0573(15) -0.0034(10) -0.0181(12) -0.0019(11) C9 0.0362(13) 0.0622(15) 0.0449(13) 0.0065(12) 0.0011(10) -0.0089(11) C28 0.0611(15) 0.0581(14) 0.0328(11) -0.0018(10) -0.0097(10) -0.0265(12) C10 0.0549(15) 0.0551(15) 0.0346(12) -0.0019(11) 0.0019(11) 0.0001(12) C24 0.0473(14) 0.0600(15) 0.0498(14) 0.0011(12) -0.0036(11) -0.0186(12) C27 0.0710(17) 0.0422(13) 0.0446(13) -0.0075(10) -0.0159(12) -0.0146(12) C14 0.084(2) 0.0594(16) 0.0474(14) -0.0113(12) -0.0234(14) -0.0218(15) C25 0.0623(16) 0.0535(14) 0.0545(15) -0.0017(12) -0.0095(12) -0.0277(13) C26 0.0543(15) 0.0449(13) 0.0648(16) -0.0055(12) -0.0247(13) 0.0026(11) C33 0.0580(16) 0.0727(17) 0.0514(14) 0.0094(13) -0.0113(12) -0.0347(14) C23 0.0356(13) 0.0583(15) 0.0753(18) 0.0020(13) -0.0162(12) -0.0072(11) C13 0.086(2) 0.0498(14) 0.0336(12) -0.0083(11) -0.0124(13) -0.0094(14) C32 0.0549(17) 0.091(2) 0.0605(17) -0.0249(16) 0.0039(14) -0.0062(16) C29 0.102(2) 0.0595(17) 0.0494(15) 0.0075(13) 0.0004(15) -0.0234(17) C30 0.0597(18) 0.074(2) 0.080(2) -0.0016(16) 0.0104(15) -0.0160(15) N1 0.0288(9) 0.0364(9) 0.0345(9) -0.0028(7) -0.0096(7) -0.0064(7) N3 0.0287(8) 0.0325(8) 0.0270(8) -0.0007(7) -0.0075(7) -0.0076(7) N2 0.0414(10) 0.0402(10) 0.0375(9) 0.0001(8) -0.0151(8) -0.0107(8) C36 0.210(7) 0.071(3) 0.245(9) -0.034(4) 0.143(7) -0.035(4) C34 0.248(8) 0.071(3) 0.188(6) -0.007(3) 0.032(6) -0.037(4) C37 0.358(12) 0.207(8) 0.131(5) -0.048(5) 0.045(6) -0.224(9) C35 0.341(12) 0.187(7) 0.147(6) -0.002(5) 0.012(7) -0.185(8) C38 0.204(8) 0.129(5) 0.309(12) -0.085(6) 0.122(8) -0.092(6) C39 0.338(13) 0.307(13) 0.120(5) -0.028(6) -0.021(6) -0.201(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 Al2 C26 1.970(2) . ? Al2 C27 1.975(2) . ? Al2 C25 1.977(2) . ? Al2 N3 2.0449(17) . ? Al1 N1 1.8905(17) . ? Al1 C23 1.952(2) . ? Al1 C24 1.954(2) . ? Al1 N2 1.9804(19) . ? C1 C6 1.398(3) . ? C1 C2 1.418(3) . ? C1 C16 1.465(3) . ? C7 N1 1.376(3) . ? C7 C8 1.383(3) . ? C7 C12 1.429(3) . ? C16 N3 1.286(2) . ? C16 H16 0.9500 . ? C12 N2 1.370(3) . ? C12 C11 1.413(3) . ? C17 C22 1.394(3) . ? C17 C18 1.402(3) . ? C17 N3 1.452(2) . ? C8 C9 1.408(3) . ? C8 H8 0.9500 . ? C2 C3 1.391(3) . ? C2 N1 1.419(3) . ? C22 C21 1.396(3) . ? C22 C31 1.519(3) . ? C18 C19 1.388(3) . ? C18 C28 1.520(3) . ? C6 C5 1.378(3) . ? C6 H6 0.9500 . ? C11 C13 1.405(3) . ? C11 C10 1.409(3) . ? C19 C20 1.375(3) . ? C19 H19 0.9500 . ? C15 N2 1.327(3) . ? C15 C14 1.394(4) . ? C15 H15 0.9500 . ? C31 C32 1.527(4) . ? C31 C33 1.534(3) . ? C31 H31 1.0000 . ? C3 C4 1.374(3) . ? C3 H3 0.9500 . ? C20 C21 1.378(3) . ? C20 H20 0.9500 . ? C5 C4 1.380(3) . ? C5 H5 0.9500 . ? C21 H21 0.9500 . ? C4 H4 0.9500 . ? C9 C10 1.362(4) . ? C9 H9 0.9500 . ? C28 C29 1.519(3) . ? C28 C30 1.531(4) . ? C28 H28 1.0000 . ? C10 H10 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C14 C13 1.364(4) . ? C14 H14 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 H13 0.9500 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C36 C35 1.458(10) . ? C36 C37 1.521(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C34 C35 1.401(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C37 C38 1.439(10) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C38 C39 1.447(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 Al2 C27 113.04(12) . . ? C26 Al2 C25 116.82(11) . . ? C27 Al2 C25 114.23(11) . . ? C26 Al2 N3 104.55(9) . . ? C27 Al2 N3 101.83(8) . . ? C25 Al2 N3 104.15(9) . . ? N1 Al1 C23 115.81(9) . . ? N1 Al1 C24 111.45(9) . . ? C23 Al1 C24 121.81(11) . . ? N1 Al1 N2 84.40(7) . . ? C23 Al1 N2 105.98(10) . . ? C24 Al1 N2 110.58(10) . . ? C6 C1 C2 118.74(18) . . ? C6 C1 C16 124.57(17) . . ? C2 C1 C16 116.53(17) . . ? N1 C7 C8 128.16(19) . . ? N1 C7 C12 114.78(17) . . ? C8 C7 C12 117.02(19) . . ? N3 C16 C1 132.01(18) . . ? N3 C16 H16 114.0 . . ? C1 C16 H16 114.0 . . ? N2 C12 C11 122.0(2) . . ? N2 C12 C7 115.74(18) . . ? C11 C12 C7 122.26(19) . . ? C22 C17 C18 122.69(18) . . ? C22 C17 N3 119.23(17) . . ? C18 C17 N3 117.94(17) . . ? C7 C8 C9 120.6(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C3 C2 C1 118.82(19) . . ? C3 C2 N1 119.10(18) . . ? C1 C2 N1 122.02(17) . . ? C17 C22 C21 117.25(19) . . ? C17 C22 C31 123.46(18) . . ? C21 C22 C31 119.29(19) . . ? C19 C18 C17 117.4(2) . . ? C19 C18 C28 120.16(19) . . ? C17 C18 C28 122.45(18) . . ? C5 C6 C1 121.16(19) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C13 C11 C10 125.4(2) . . ? C13 C11 C12 116.4(2) . . ? C10 C11 C12 118.2(2) . . ? C20 C19 C18 121.2(2) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? N2 C15 C14 122.0(2) . . ? N2 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C22 C31 C32 111.5(2) . . ? C22 C31 C33 111.2(2) . . ? C32 C31 C33 110.9(2) . . ? C22 C31 H31 107.7 . . ? C32 C31 H31 107.7 . . ? C33 C31 H31 107.7 . . ? C4 C3 C2 121.0(2) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C19 C20 C21 120.4(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C6 C5 C4 119.7(2) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C20 C21 C22 121.1(2) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C10 C9 C8 122.4(2) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C29 C28 C18 111.7(2) . . ? C29 C28 C30 110.0(2) . . ? C18 C28 C30 112.0(2) . . ? C29 C28 H28 107.7 . . ? C18 C28 H28 107.7 . . ? C30 C28 H28 107.7 . . ? C9 C10 C11 119.6(2) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? Al1 C24 H24A 109.5 . . ? Al1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Al1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Al2 C27 H27A 109.5 . . ? Al2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Al2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C13 C14 C15 119.3(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? Al2 C25 H25A 109.5 . . ? Al2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Al2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Al2 C26 H26A 109.5 . . ? Al2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Al2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Al1 C23 H23A 109.5 . . ? Al1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Al1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C14 C13 C11 120.9(2) . . ? C14 C13 H13 119.6 . . ? C11 C13 H13 119.6 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C7 N1 C2 120.20(16) . . ? C7 N1 Al1 114.11(13) . . ? C2 N1 Al1 125.67(13) . . ? C16 N3 C17 122.74(16) . . ? C16 N3 Al2 117.61(13) . . ? C17 N3 Al2 119.41(12) . . ? C15 N2 C12 119.3(2) . . ? C15 N2 Al1 129.66(17) . . ? C12 N2 Al1 110.90(14) . . ? C35 C36 C37 124.9(6) . . ? C35 C36 H36A 106.1 . . ? C37 C36 H36A 106.1 . . ? C35 C36 H36B 106.1 . . ? C37 C36 H36B 106.1 . . ? H36A C36 H36B 106.3 . . ? C35 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 C37 C36 125.6(7) . . ? C38 C37 H37A 105.9 . . ? C36 C37 H37A 105.9 . . ? C38 C37 H37B 105.9 . . ? C36 C37 H37B 105.9 . . ? H37A C37 H37B 106.2 . . ? C34 C35 C36 117.4(7) . . ? C34 C35 H35A 107.9 . . ? C36 C35 H35A 107.9 . . ? C34 C35 H35B 107.9 . . ? C36 C35 H35B 107.9 . . ? H35A C35 H35B 107.2 . . ? C37 C38 C39 122.0(8) . . ? C37 C38 H38A 106.8 . . ? C39 C38 H38A 106.8 . . ? C37 C38 H38B 106.8 . . ? C39 C38 H38B 106.8 . . ? H38A C38 H38B 106.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 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 C6 C1 C16 N3 -20.2(3) . . . . ? C2 C1 C16 N3 164.5(2) . . . . ? N1 C7 C12 N2 -0.3(2) . . . . ? C8 C7 C12 N2 -178.08(17) . . . . ? N1 C7 C12 C11 178.89(17) . . . . ? C8 C7 C12 C11 1.1(3) . . . . ? N1 C7 C8 C9 -178.64(19) . . . . ? C12 C7 C8 C9 -1.2(3) . . . . ? C6 C1 C2 C3 -0.9(3) . . . . ? C16 C1 C2 C3 174.60(18) . . . . ? C6 C1 C2 N1 -178.26(18) . . . . ? C16 C1 C2 N1 -2.7(3) . . . . ? C18 C17 C22 C21 -1.0(3) . . . . ? N3 C17 C22 C21 -176.61(18) . . . . ? C18 C17 C22 C31 178.5(2) . . . . ? N3 C17 C22 C31 2.9(3) . . . . ? C22 C17 C18 C19 1.2(3) . . . . ? N3 C17 C18 C19 176.83(18) . . . . ? C22 C17 C18 C28 -179.6(2) . . . . ? N3 C17 C18 C28 -4.0(3) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? C16 C1 C6 C5 -174.1(2) . . . . ? N2 C12 C11 C13 0.1(3) . . . . ? C7 C12 C11 C13 -179.04(18) . . . . ? N2 C12 C11 C10 178.78(18) . . . . ? C7 C12 C11 C10 -0.3(3) . . . . ? C17 C18 C19 C20 -0.9(3) . . . . ? C28 C18 C19 C20 179.9(2) . . . . ? C17 C22 C31 C32 -117.8(2) . . . . ? C21 C22 C31 C32 61.7(3) . . . . ? C17 C22 C31 C33 117.8(2) . . . . ? C21 C22 C31 C33 -62.7(3) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? N1 C2 C3 C4 177.5(2) . . . . ? C18 C19 C20 C21 0.6(4) . . . . ? C1 C6 C5 C4 -0.2(4) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C17 C22 C21 C20 0.6(3) . . . . ? C31 C22 C21 C20 -178.9(2) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C6 C5 C4 C3 -0.6(4) . . . . ? C7 C8 C9 C10 0.5(3) . . . . ? C19 C18 C28 C29 -60.6(3) . . . . ? C17 C18 C28 C29 120.3(2) . . . . ? C19 C18 C28 C30 63.3(3) . . . . ? C17 C18 C28 C30 -115.8(2) . . . . ? C8 C9 C10 C11 0.3(3) . . . . ? C13 C11 C10 C9 178.2(2) . . . . ? C12 C11 C10 C9 -0.4(3) . . . . ? N2 C15 C14 C13 -0.1(4) . . . . ? C15 C14 C13 C11 -0.6(4) . . . . ? C10 C11 C13 C14 -178.0(2) . . . . ? C12 C11 C13 C14 0.6(3) . . . . ? C8 C7 N1 C2 -6.1(3) . . . . ? C12 C7 N1 C2 176.36(16) . . . . ? C8 C7 N1 Al1 175.64(16) . . . . ? C12 C7 N1 Al1 -1.9(2) . . . . ? C3 C2 N1 C7 113.3(2) . . . . ? C1 C2 N1 C7 -69.3(2) . . . . ? C3 C2 N1 Al1 -68.6(2) . . . . ? C1 C2 N1 Al1 108.68(19) . . . . ? C23 Al1 N1 C7 -102.64(16) . . . . ? C24 Al1 N1 C7 112.36(15) . . . . ? N2 Al1 N1 C7 2.42(13) . . . . ? C23 Al1 N1 C2 79.23(18) . . . . ? C24 Al1 N1 C2 -65.78(18) . . . . ? N2 Al1 N1 C2 -175.72(16) . . . . ? C1 C16 N3 C17 -2.5(3) . . . . ? C1 C16 N3 Al2 -176.79(16) . . . . ? C22 C17 N3 C16 -80.8(2) . . . . ? C18 C17 N3 C16 103.5(2) . . . . ? C22 C17 N3 Al2 93.41(18) . . . . ? C18 C17 N3 Al2 -82.4(2) . . . . ? C26 Al2 N3 C16 170.38(15) . . . . ? C27 Al2 N3 C16 52.51(16) . . . . ? C25 Al2 N3 C16 -66.52(16) . . . . ? C26 Al2 N3 C17 -4.08(16) . . . . ? C27 Al2 N3 C17 -121.95(15) . . . . ? C25 Al2 N3 C17 119.02(15) . . . . ? C14 C15 N2 C12 0.7(3) . . . . ? C14 C15 N2 Al1 176.23(17) . . . . ? C11 C12 N2 C15 -0.7(3) . . . . ? C7 C12 N2 C15 178.47(18) . . . . ? C11 C12 N2 Al1 -177.01(15) . . . . ? C7 C12 N2 Al1 2.1(2) . . . . ? N1 Al1 N2 C15 -178.3(2) . . . . ? C23 Al1 N2 C15 -63.1(2) . . . . ? C24 Al1 N2 C15 70.8(2) . . . . ? N1 Al1 N2 C12 -2.50(13) . . . . ? C23 Al1 N2 C12 112.78(14) . . . . ? C24 Al1 N2 C12 -113.33(14) . . . . ? C35 C36 C37 C38 174.4(7) . . . . ? C37 C36 C35 C34 177.5(6) . . . . ? C36 C37 C38 C39 177.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.356 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.044 #===END data_complex_3b _database_code_depnum_ccdc_archive 'CCDC 871560' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H29 N3 Zn' _chemical_formula_weight 472.91 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7628(7) _cell_length_b 10.9313(7) _cell_length_c 11.4905(8) _cell_angle_alpha 69.8200(10) _cell_angle_beta 88.4390(10) _cell_angle_gamma 66.2230(10) _cell_volume 1151.30(13) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3431 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 25.98 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8119 _exptl_absorpt_correction_T_max 0.8806 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5975 _diffrn_reflns_av_R_equivalents 0.0116 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4398 _reflns_number_gt 3990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.4879P] 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 4398 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 C1 C 0.60377(19) 0.6610(2) 0.88995(18) 0.0258(4) Uani 1 1 d . . . C2 C 0.67208(19) 0.5169(2) 0.97506(18) 0.0266(4) Uani 1 1 d . . . C3 C 0.6492(2) 0.4814(2) 1.10052(19) 0.0331(5) Uani 1 1 d . . . H3 H 0.6925 0.3863 1.1548 0.040 Uiso 1 1 calc R . . C4 C 0.5647(2) 0.5829(3) 1.1457(2) 0.0388(5) Uani 1 1 d . . . H4 H 0.5533 0.5579 1.2299 0.047 Uiso 1 1 calc R . . C5 C 0.4966(2) 0.7236(2) 1.0631(2) 0.0367(5) Uani 1 1 d . . . H5 H 0.4378 0.7930 1.0922 0.044 Uiso 1 1 calc R . . C6 C 0.5147(2) 0.7622(2) 0.9382(2) 0.0315(4) Uani 1 1 d . . . H6 H 0.4670 0.8571 0.8847 0.038 Uiso 1 1 calc R . . C7 C 0.5346(2) 0.7769(2) 0.66521(18) 0.0265(4) Uani 1 1 d . . . C8 C 0.3942(2) 0.8505(2) 0.6608(2) 0.0311(4) Uani 1 1 d . . . H8 H 0.3567 0.8461 0.7353 0.037 Uiso 1 1 calc R . . C9 C 0.3073(2) 0.9313(2) 0.5469(2) 0.0366(5) Uani 1 1 d . . . H9 H 0.2141 0.9808 0.5481 0.044 Uiso 1 1 calc R . . C10 C 0.3550(2) 0.9399(2) 0.4343(2) 0.0378(5) Uani 1 1 d . . . H10 H 0.2956 0.9965 0.3601 0.045 Uiso 1 1 calc R . . C11 C 0.4954(2) 0.8618(2) 0.43204(19) 0.0320(4) Uani 1 1 d . . . C12 C 0.5845(2) 0.7814(2) 0.54599(18) 0.0272(4) Uani 1 1 d . . . C13 C 0.5542(3) 0.8579(2) 0.3210(2) 0.0399(5) Uani 1 1 d . . . H13 H 0.4990 0.9091 0.2442 0.048 Uiso 1 1 calc R . . C14 C 0.6906(3) 0.7801(3) 0.3257(2) 0.0422(5) Uani 1 1 d . . . H14 H 0.7291 0.7776 0.2526 0.051 Uiso 1 1 calc R . . C15 C 0.7723(2) 0.7040(2) 0.4420(2) 0.0371(5) Uani 1 1 d . . . H15 H 0.8658 0.6523 0.4446 0.045 Uiso 1 1 calc R . . C16 C 0.7594(2) 0.3972(2) 0.93873(18) 0.0280(4) Uani 1 1 d . . . H16 H 0.7726 0.3059 0.9926 0.034 Uiso 1 1 calc R . . C27 C 1.0061(2) 0.6055(2) 0.7491(2) 0.0342(5) Uani 1 1 d . . . H27A H 1.0337 0.5815 0.8367 0.041 Uiso 1 1 calc R . . H27B H 1.0717 0.5309 0.7235 0.041 Uiso 1 1 calc R . . C28 C 1.0121(2) 0.7474(3) 0.6734(2) 0.0421(5) Uani 1 1 d . . . H28A H 0.9823 0.7738 0.5867 0.063 Uiso 1 1 calc R . . H28B H 1.1044 0.7375 0.6828 0.063 Uiso 1 1 calc R . . H28C H 0.9532 0.8206 0.7028 0.063 Uiso 1 1 calc R . . C17 C 0.89964(19) 0.2734(2) 0.82083(18) 0.0261(4) Uani 1 1 d . . . C18 C 1.0282(2) 0.1800(2) 0.89298(19) 0.0294(4) Uani 1 1 d . . . C19 C 1.1033(2) 0.0559(2) 0.8689(2) 0.0355(5) Uani 1 1 d . . . H19 H 1.1878 -0.0087 0.9161 0.043 Uiso 1 1 calc R . . C20 C 1.0545(2) 0.0268(2) 0.7760(2) 0.0371(5) Uani 1 1 d . . . H20 H 1.1062 -0.0570 0.7616 0.044 Uiso 1 1 calc R . . C21 C 0.9296(2) 0.1215(2) 0.7046(2) 0.0357(5) Uani 1 1 d . . . H21 H 0.8986 0.1014 0.6416 0.043 Uiso 1 1 calc R . . C22 C 0.8491(2) 0.2470(2) 0.72555(19) 0.0295(4) Uani 1 1 d . . . C25 C 1.0812(2) 0.2176(2) 0.9905(2) 0.0378(5) Uani 1 1 d . . . H25A H 1.0170 0.2263 1.0512 0.045 Uiso 1 1 calc R . . H25B H 1.0821 0.3111 0.9497 0.045 Uiso 1 1 calc R . . C26 C 1.2226(2) 0.1130(3) 1.0602(2) 0.0428(5) Uani 1 1 d . . . H26A H 1.2220 0.0214 1.1062 0.064 Uiso 1 1 calc R . . H26B H 1.2477 0.1487 1.1170 0.064 Uiso 1 1 calc R . . H26C H 1.2877 0.1025 1.0015 0.064 Uiso 1 1 calc R . . C23 C 0.7101(2) 0.3480(2) 0.6493(2) 0.0354(5) Uani 1 1 d . . . H23A H 0.6758 0.4348 0.6685 0.043 Uiso 1 1 calc R . . H23B H 0.6474 0.3031 0.6753 0.043 Uiso 1 1 calc R . . C24 C 0.7089(3) 0.3900(3) 0.5081(2) 0.0465(6) Uani 1 1 d . . . H24A H 0.7780 0.4247 0.4823 0.070 Uiso 1 1 calc R . . H24B H 0.6207 0.4640 0.4667 0.070 Uiso 1 1 calc R . . H24C H 0.7274 0.3076 0.4863 0.070 Uiso 1 1 calc R . . N1 N 0.63259(17) 0.69407(17) 0.76738(15) 0.0275(4) Uani 1 1 d . . . N2 N 0.72118(18) 0.70263(18) 0.54874(16) 0.0304(4) Uani 1 1 d . . . N3 N 0.81998(16) 0.40475(17) 0.84025(15) 0.0259(3) Uani 1 1 d . . . Zn1 Zn 0.82409(2) 0.60533(2) 0.73184(2) 0.02894(9) 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 0.0224(9) 0.0295(10) 0.0258(10) -0.0124(8) 0.0024(7) -0.0092(8) C2 0.0222(9) 0.0308(10) 0.0249(9) -0.0113(8) 0.0018(7) -0.0082(8) C3 0.0277(10) 0.0368(11) 0.0251(10) -0.0076(9) 0.0013(8) -0.0072(9) C4 0.0347(12) 0.0527(14) 0.0228(10) -0.0158(10) 0.0054(8) -0.0110(10) C5 0.0307(11) 0.0441(13) 0.0376(12) -0.0267(10) 0.0090(9) -0.0085(9) C6 0.0280(10) 0.0295(11) 0.0338(11) -0.0140(9) 0.0024(8) -0.0068(8) C7 0.0315(10) 0.0207(9) 0.0257(10) -0.0063(8) 0.0025(8) -0.0113(8) C8 0.0301(11) 0.0289(10) 0.0304(10) -0.0079(8) 0.0036(8) -0.0111(8) C9 0.0286(11) 0.0324(11) 0.0420(12) -0.0080(9) -0.0026(9) -0.0102(9) C10 0.0388(12) 0.0335(12) 0.0327(11) -0.0018(9) -0.0075(9) -0.0150(10) C11 0.0416(12) 0.0270(10) 0.0288(10) -0.0066(8) 0.0009(9) -0.0184(9) C12 0.0325(10) 0.0219(9) 0.0266(10) -0.0061(8) 0.0025(8) -0.0131(8) C13 0.0561(15) 0.0390(12) 0.0256(11) -0.0059(9) 0.0006(10) -0.0254(11) C14 0.0614(16) 0.0438(13) 0.0270(11) -0.0134(10) 0.0139(10) -0.0275(12) C15 0.0421(13) 0.0365(12) 0.0336(11) -0.0147(9) 0.0125(9) -0.0163(10) C16 0.0255(10) 0.0253(10) 0.0270(10) -0.0070(8) -0.0014(8) -0.0068(8) C27 0.0256(10) 0.0325(11) 0.0387(12) -0.0106(9) 0.0020(9) -0.0085(9) C28 0.0347(12) 0.0409(13) 0.0487(14) -0.0131(11) 0.0060(10) -0.0167(10) C17 0.0250(10) 0.0235(10) 0.0287(10) -0.0106(8) 0.0072(8) -0.0083(8) C18 0.0292(10) 0.0253(10) 0.0305(10) -0.0085(8) 0.0050(8) -0.0098(8) C19 0.0272(11) 0.0272(11) 0.0446(13) -0.0109(9) 0.0051(9) -0.0061(8) C20 0.0340(11) 0.0289(11) 0.0503(13) -0.0212(10) 0.0135(10) -0.0101(9) C21 0.0365(12) 0.0386(12) 0.0404(12) -0.0235(10) 0.0108(9) -0.0166(10) C22 0.0276(10) 0.0307(11) 0.0312(10) -0.0130(9) 0.0075(8) -0.0120(8) C25 0.0362(12) 0.0317(11) 0.0389(12) -0.0127(10) -0.0042(9) -0.0076(9) C26 0.0355(12) 0.0437(13) 0.0412(13) -0.0108(11) -0.0020(10) -0.0124(10) C23 0.0313(11) 0.0399(12) 0.0342(11) -0.0179(10) 0.0019(9) -0.0101(9) C24 0.0505(15) 0.0450(14) 0.0368(13) -0.0157(11) 0.0017(11) -0.0124(11) N1 0.0258(8) 0.0258(8) 0.0239(8) -0.0073(7) 0.0029(6) -0.0055(7) N2 0.0336(9) 0.0299(9) 0.0284(9) -0.0122(7) 0.0069(7) -0.0128(7) N3 0.0237(8) 0.0247(8) 0.0261(8) -0.0105(7) 0.0019(6) -0.0061(7) Zn1 0.02567(14) 0.02914(14) 0.02863(14) -0.01043(10) 0.00522(9) -0.00845(10) _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 1.388(2) . ? C1 C6 1.411(3) . ? C1 C2 1.422(3) . ? C2 C3 1.400(3) . ? C2 C16 1.460(3) . ? C3 C4 1.374(3) . ? C3 H3 0.9300 . ? C4 C5 1.388(3) . ? C4 H4 0.9300 . ? C5 C6 1.381(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N1 1.369(2) . ? C7 C8 1.389(3) . ? C7 C12 1.450(3) . ? C8 C9 1.404(3) . ? C8 H8 0.9300 . ? C9 C10 1.366(3) . ? C9 H9 0.9300 . ? C10 C11 1.410(3) . ? C10 H10 0.9300 . ? C11 C13 1.415(3) . ? C11 C12 1.415(3) . ? C12 N2 1.367(3) . ? C13 C14 1.359(4) . ? C13 H13 0.9300 . ? C14 C15 1.399(3) . ? C14 H14 0.9300 . ? C15 N2 1.329(3) . ? C15 H15 0.9300 . ? C16 N3 1.285(3) . ? C16 H16 0.9300 . ? C27 C28 1.522(3) . ? C27 Zn1 1.975(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C17 C22 1.398(3) . ? C17 C18 1.408(3) . ? C17 N3 1.437(2) . ? C18 C19 1.390(3) . ? C18 C25 1.513(3) . ? C19 C20 1.384(3) . ? C19 H19 0.9300 . ? C20 C21 1.380(3) . ? C20 H20 0.9300 . ? C21 C22 1.397(3) . ? C21 H21 0.9300 . ? C22 C23 1.515(3) . ? C25 C26 1.515(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C23 C24 1.526(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? N1 Zn1 1.9927(16) . ? N2 Zn1 2.1018(17) . ? N3 Zn1 2.1335(16) . ? 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 C6 124.42(18) . . ? N1 C1 C2 118.50(17) . . ? C6 C1 C2 117.02(18) . . ? C3 C2 C1 119.82(18) . . ? C3 C2 C16 116.03(18) . . ? C1 C2 C16 123.99(17) . . ? C4 C3 C2 121.9(2) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 118.68(19) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 121.04(19) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 121.50(19) . . ? C5 C6 H6 119.3 . . ? C1 C6 H6 119.3 . . ? N1 C7 C8 128.95(18) . . ? N1 C7 C12 114.90(17) . . ? C8 C7 C12 116.06(18) . . ? C7 C8 C9 121.7(2) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C10 C9 C8 122.2(2) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 119.10(19) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C13 123.6(2) . . ? C10 C11 C12 119.30(19) . . ? C13 C11 C12 117.1(2) . . ? N2 C12 C11 121.47(18) . . ? N2 C12 C7 117.01(17) . . ? C11 C12 C7 121.51(19) . . ? C14 C13 C11 120.6(2) . . ? C14 C13 H13 119.7 . . ? C11 C13 H13 119.7 . . ? C13 C14 C15 119.0(2) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N2 C15 C14 122.5(2) . . ? N2 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N3 C16 C2 126.93(18) . . ? N3 C16 H16 116.5 . . ? C2 C16 H16 116.5 . . ? C28 C27 Zn1 114.38(14) . . ? C28 C27 H27A 108.7 . . ? Zn1 C27 H27A 108.7 . . ? C28 C27 H27B 108.7 . . ? Zn1 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C22 C17 C18 122.38(18) . . ? C22 C17 N3 118.19(17) . . ? C18 C17 N3 119.33(17) . . ? C19 C18 C17 117.40(19) . . ? C19 C18 C25 122.39(19) . . ? C17 C18 C25 120.20(18) . . ? C20 C19 C18 121.2(2) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.9(2) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 117.71(19) . . ? C21 C22 C23 120.53(19) . . ? C17 C22 C23 121.73(18) . . ? C18 C25 C26 116.27(19) . . ? C18 C25 H25A 108.2 . . ? C26 C25 H25A 108.2 . . ? C18 C25 H25B 108.2 . . ? C26 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C23 C24 114.91(19) . . ? C22 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C22 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 N1 C1 123.82(16) . . ? C7 N1 Zn1 116.01(13) . . ? C1 N1 Zn1 119.95(12) . . ? C15 N2 C12 119.38(18) . . ? C15 N2 Zn1 129.12(15) . . ? C12 N2 Zn1 111.33(13) . . ? C16 N3 C17 118.05(17) . . ? C16 N3 Zn1 117.87(13) . . ? C17 N3 Zn1 123.26(12) . . ? C27 Zn1 N1 142.27(8) . . ? C27 Zn1 N2 115.60(8) . . ? N1 Zn1 N2 80.52(7) . . ? C27 Zn1 N3 113.16(7) . . ? N1 Zn1 N3 85.75(6) . . ? N2 Zn1 N3 115.50(6) . . ? 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 C3 177.49(18) . . . . ? C6 C1 C2 C3 0.0(3) . . . . ? N1 C1 C2 C16 -7.3(3) . . . . ? C6 C1 C2 C16 175.19(18) . . . . ? C1 C2 C3 C4 -1.8(3) . . . . ? C16 C2 C3 C4 -177.3(2) . . . . ? C2 C3 C4 C5 2.3(3) . . . . ? C3 C4 C5 C6 -1.1(3) . . . . ? C4 C5 C6 C1 -0.6(3) . . . . ? N1 C1 C6 C5 -176.15(19) . . . . ? C2 C1 C6 C5 1.2(3) . . . . ? N1 C7 C8 C9 179.97(19) . . . . ? C12 C7 C8 C9 -3.6(3) . . . . ? C7 C8 C9 C10 1.4(3) . . . . ? C8 C9 C10 C11 1.9(3) . . . . ? C9 C10 C11 C13 177.0(2) . . . . ? C9 C10 C11 C12 -2.7(3) . . . . ? C10 C11 C12 N2 179.23(18) . . . . ? C13 C11 C12 N2 -0.5(3) . . . . ? C10 C11 C12 C7 0.3(3) . . . . ? C13 C11 C12 C7 -179.39(18) . . . . ? N1 C7 C12 N2 0.7(3) . . . . ? C8 C7 C12 N2 -176.18(17) . . . . ? N1 C7 C12 C11 179.68(17) . . . . ? C8 C7 C12 C11 2.8(3) . . . . ? C10 C11 C13 C14 -179.9(2) . . . . ? C12 C11 C13 C14 -0.2(3) . . . . ? C11 C13 C14 C15 -0.1(3) . . . . ? C13 C14 C15 N2 1.2(3) . . . . ? C3 C2 C16 N3 -162.7(2) . . . . ? C1 C2 C16 N3 22.0(3) . . . . ? C22 C17 C18 C19 -2.0(3) . . . . ? N3 C17 C18 C19 -178.42(18) . . . . ? C22 C17 C18 C25 176.79(19) . . . . ? N3 C17 C18 C25 0.4(3) . . . . ? C17 C18 C19 C20 1.2(3) . . . . ? C25 C18 C19 C20 -177.5(2) . . . . ? C18 C19 C20 C21 0.2(3) . . . . ? C19 C20 C21 C22 -0.9(3) . . . . ? C20 C21 C22 C17 0.2(3) . . . . ? C20 C21 C22 C23 -178.1(2) . . . . ? C18 C17 C22 C21 1.3(3) . . . . ? N3 C17 C22 C21 177.77(18) . . . . ? C18 C17 C22 C23 179.58(19) . . . . ? N3 C17 C22 C23 -4.0(3) . . . . ? C19 C18 C25 C26 0.8(3) . . . . ? C17 C18 C25 C26 -178.0(2) . . . . ? C21 C22 C23 C24 -50.1(3) . . . . ? C17 C22 C23 C24 131.6(2) . . . . ? C8 C7 N1 C1 4.9(3) . . . . ? C12 C7 N1 C1 -171.54(17) . . . . ? C8 C7 N1 Zn1 179.47(17) . . . . ? C12 C7 N1 Zn1 3.1(2) . . . . ? C6 C1 N1 C7 -47.8(3) . . . . ? C2 C1 N1 C7 134.88(19) . . . . ? C6 C1 N1 Zn1 137.77(17) . . . . ? C2 C1 N1 Zn1 -39.5(2) . . . . ? C14 C15 N2 C12 -1.9(3) . . . . ? C14 C15 N2 Zn1 -176.71(16) . . . . ? C11 C12 N2 C15 1.5(3) . . . . ? C7 C12 N2 C15 -179.51(18) . . . . ? C11 C12 N2 Zn1 177.22(14) . . . . ? C7 C12 N2 Zn1 -3.8(2) . . . . ? C2 C16 N3 C17 -178.83(18) . . . . ? C2 C16 N3 Zn1 11.2(3) . . . . ? C22 C17 N3 C16 108.6(2) . . . . ? C18 C17 N3 C16 -74.8(2) . . . . ? C22 C17 N3 Zn1 -81.9(2) . . . . ? C18 C17 N3 Zn1 94.63(19) . . . . ? C28 C27 Zn1 N1 -64.8(2) . . . . ? C28 C27 Zn1 N2 43.91(19) . . . . ? C28 C27 Zn1 N3 -179.69(15) . . . . ? C7 N1 Zn1 C27 116.04(16) . . . . ? C1 N1 Zn1 C27 -69.1(2) . . . . ? C7 N1 Zn1 N2 -3.95(13) . . . . ? C1 N1 Zn1 N2 170.87(15) . . . . ? C7 N1 Zn1 N3 -120.70(14) . . . . ? C1 N1 Zn1 N3 54.12(15) . . . . ? C15 N2 Zn1 C27 35.3(2) . . . . ? C12 N2 Zn1 C27 -139.85(13) . . . . ? C15 N2 Zn1 N1 179.32(19) . . . . ? C12 N2 Zn1 N1 4.15(13) . . . . ? C15 N2 Zn1 N3 -100.06(18) . . . . ? C12 N2 Zn1 N3 84.77(14) . . . . ? C16 N3 Zn1 C27 106.89(15) . . . . ? C17 N3 Zn1 C27 -62.56(16) . . . . ? C16 N3 Zn1 N1 -39.29(15) . . . . ? C17 N3 Zn1 N1 151.27(15) . . . . ? C16 N3 Zn1 N2 -116.67(14) . . . . ? C17 N3 Zn1 N2 73.89(15) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.439 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.055 #===END data_complex_4c _database_code_depnum_ccdc_archive 'CCDC 871561' #TrackingRef '- combined cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H119 N12 Zn2' _chemical_formula_weight 1799.96 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' Zn Zn 0.2839 1.4301 '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 11.438(2) _cell_length_b 13.475(3) _cell_length_c 17.838(4) _cell_angle_alpha 101.71(3) _cell_angle_beta 94.18(3) _cell_angle_gamma 108.97(3) _cell_volume 2517.2(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13228 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.39 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 953 _exptl_absorpt_coefficient_mu 0.530 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8833 _exptl_absorpt_correction_T_max 0.8968 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24531 _diffrn_reflns_av_R_equivalents 0.1271 _diffrn_reflns_av_sigmaI/netI 0.1919 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.43 _reflns_number_total 11255 _reflns_number_gt 4250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^2^+2.0052P] 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 11255 _refine_ls_number_parameters 598 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2669 _refine_ls_R_factor_gt 0.1131 _refine_ls_wR_factor_ref 0.2985 _refine_ls_wR_factor_gt 0.2288 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.020 _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 Zn1 Zn 0.57052(7) 0.57644(7) 0.70617(5) 0.0605(3) Uani 1 1 d . . . N2 N 0.6984(6) 0.6988(5) 0.6670(4) 0.0721(17) Uani 1 1 d . . . N1 N 0.4989(5) 0.6939(5) 0.7302(3) 0.0654(16) Uani 1 1 d . . . N3 N 0.5575(5) 0.5743(4) 0.8245(3) 0.0620(15) Uani 1 1 d . . . N5 N 0.6836(5) 0.4747(5) 0.6923(3) 0.0597(15) Uani 1 1 d . . . N4 N 0.4534(5) 0.4494(4) 0.6300(3) 0.0546(14) Uani 1 1 d . . . N6 N 0.1376(6) 0.1990(5) 0.6501(4) 0.0677(16) Uani 1 1 d . . . C15 C 0.7985(8) 0.6955(8) 0.6343(5) 0.089(3) Uani 1 1 d . . . H15 H 0.8146 0.6311 0.6240 0.106 Uiso 1 1 calc R . . C14 C 0.8795(9) 0.7854(11) 0.6149(6) 0.109(3) Uani 1 1 d . . . H14 H 0.9496 0.7814 0.5928 0.131 Uiso 1 1 calc R . . C13 C 0.8553(10) 0.8782(9) 0.6285(6) 0.102(3) Uani 1 1 d . . . H13 H 0.9092 0.9384 0.6155 0.123 Uiso 1 1 calc R . . C11 C 0.7507(9) 0.8859(7) 0.6618(5) 0.083(2) Uani 1 1 d . . . C12 C 0.6740(7) 0.7917(6) 0.6789(4) 0.0646(19) Uani 1 1 d . . . C10 C 0.7184(11) 0.9785(8) 0.6771(6) 0.106(3) Uani 1 1 d . . . H10 H 0.7659 1.0398 0.6623 0.127 Uiso 1 1 calc R . . C9 C 0.6212(12) 0.9802(8) 0.7124(6) 0.106(3) Uani 1 1 d . . . H9 H 0.6060 1.0448 0.7263 0.128 Uiso 1 1 calc R . . C8 C 0.5402(9) 0.8863(7) 0.7294(5) 0.087(2) Uani 1 1 d . . . H8 H 0.4699 0.8889 0.7516 0.105 Uiso 1 1 calc R . . C7 C 0.5641(7) 0.7891(6) 0.7133(4) 0.071(2) Uani 1 1 d . . . C1 C 0.3878(7) 0.6758(6) 0.7597(5) 0.071(2) Uani 1 1 d . . . C2 C 0.2896(8) 0.7085(7) 0.7339(5) 0.092(3) Uani 1 1 d . . . H2 H 0.3005 0.7478 0.6961 0.110 Uiso 1 1 calc R . . C3 C 0.1806(8) 0.6841(8) 0.7624(7) 0.101(3) Uani 1 1 d . . . H3 H 0.1162 0.7028 0.7414 0.121 Uiso 1 1 calc R . . C4 C 0.1627(8) 0.6324(9) 0.8217(7) 0.105(3) Uani 1 1 d . . . H4 H 0.0884 0.6189 0.8425 0.126 Uiso 1 1 calc R . . C5 C 0.2566(8) 0.6010(7) 0.8497(5) 0.089(3) Uani 1 1 d . . . H5 H 0.2456 0.5666 0.8903 0.107 Uiso 1 1 calc R . . C6 C 0.3684(7) 0.6195(6) 0.8187(5) 0.068(2) Uani 1 1 d . . . C16 C 0.4641(7) 0.5863(6) 0.8540(4) 0.0670(19) Uani 1 1 d . . . H16 H 0.4558 0.5725 0.9027 0.080 Uiso 1 1 calc R . . C17 C 0.6491(6) 0.5527(6) 0.8721(4) 0.0619(18) Uani 1 1 d . . . C18 C 0.7596(7) 0.6383(7) 0.9031(4) 0.071(2) Uani 1 1 d . . . C19 C 0.8504(8) 0.6213(8) 0.9466(5) 0.090(3) Uani 1 1 d . . . H19 H 0.9236 0.6784 0.9696 0.108 Uiso 1 1 calc R . . C20 C 0.8340(9) 0.5196(10) 0.9567(5) 0.106(3) Uani 1 1 d . . . H20 H 0.8973 0.5082 0.9858 0.127 Uiso 1 1 calc R . . C21 C 0.7246(8) 0.4335(8) 0.9243(5) 0.092(3) Uani 1 1 d . . . H21 H 0.7149 0.3651 0.9316 0.110 Uiso 1 1 calc R . . C22 C 0.6306(7) 0.4494(7) 0.8814(4) 0.069(2) Uani 1 1 d . . . C23 C 0.7812(8) 0.7486(7) 0.8895(6) 0.091(3) Uani 1 1 d . . . H23 H 0.7150 0.7409 0.8483 0.109 Uiso 1 1 calc R . . C24 C 0.9016(14) 0.7966(10) 0.8629(8) 0.174(4) Uani 1 1 d . . . H24A H 0.9670 0.8279 0.9066 0.261 Uiso 1 1 calc R . . H24B H 0.8967 0.8517 0.8374 0.261 Uiso 1 1 calc R . . H24C H 0.9194 0.7414 0.8274 0.261 Uiso 1 1 calc R . . C25 C 0.7681(14) 0.8233(10) 0.9588(8) 0.174(4) Uani 1 1 d . . . H25A H 0.7839 0.8935 0.9489 0.261 Uiso 1 1 calc R . . H25B H 0.8271 0.8284 1.0018 0.261 Uiso 1 1 calc R . . H25C H 0.6848 0.7965 0.9708 0.261 Uiso 1 1 calc R . . C26 C 0.5122(8) 0.3557(7) 0.8458(5) 0.083(2) Uani 1 1 d . . . H26 H 0.4642 0.3794 0.8098 0.099 Uiso 1 1 calc R . . C28 C 0.4315(9) 0.3217(9) 0.9068(6) 0.121(4) Uani 1 1 d . . . H28A H 0.4783 0.3026 0.9449 0.182 Uiso 1 1 calc R . . H28B H 0.3582 0.2605 0.8826 0.182 Uiso 1 1 calc R . . H28C H 0.4070 0.3805 0.9315 0.182 Uiso 1 1 calc R . . C27 C 0.5412(10) 0.2604(7) 0.7996(6) 0.112(3) Uani 1 1 d . . . H27A H 0.5941 0.2840 0.7626 0.168 Uiso 1 1 calc R . . H27B H 0.4647 0.2048 0.7729 0.168 Uiso 1 1 calc R . . H27C H 0.5830 0.2323 0.8342 0.168 Uiso 1 1 calc R . . C43 C 0.7947(7) 0.4852(7) 0.7260(4) 0.074(2) Uani 1 1 d . . . H43 H 0.8336 0.5439 0.7679 0.089 Uiso 1 1 calc R . . C42 C 0.8573(7) 0.4142(8) 0.7028(5) 0.086(3) Uani 1 1 d . . . H42 H 0.9362 0.4255 0.7282 0.104 Uiso 1 1 calc R . . C41 C 0.8016(7) 0.3291(8) 0.6430(6) 0.088(3) Uani 1 1 d . . . H41 H 0.8419 0.2803 0.6274 0.106 Uiso 1 1 calc R . . C39 C 0.6823(7) 0.3116(7) 0.6029(5) 0.071(2) Uani 1 1 d . . . C40 C 0.6256(6) 0.3880(6) 0.6321(4) 0.0571(17) Uani 1 1 d . . . C38 C 0.6221(8) 0.2286(7) 0.5373(5) 0.084(2) Uani 1 1 d . . . H38 H 0.6596 0.1793 0.5172 0.101 Uiso 1 1 calc R . . C37 C 0.5090(7) 0.2204(7) 0.5031(5) 0.077(2) Uani 1 1 d . . . H37 H 0.4706 0.1662 0.4585 0.093 Uiso 1 1 calc R . . C36 C 0.4492(7) 0.2894(6) 0.5321(4) 0.069(2) Uani 1 1 d . . . H36 H 0.3699 0.2785 0.5077 0.083 Uiso 1 1 calc R . . C35 C 0.5024(6) 0.3757(6) 0.5971(4) 0.0518(16) Uani 1 1 d . . . C29 C 0.3326(6) 0.4393(6) 0.5988(4) 0.0550(17) Uani 1 1 d . . . C34 C 0.2260(6) 0.3594(6) 0.6067(4) 0.0584(18) Uani 1 1 d . . . C33 C 0.1100(7) 0.3581(7) 0.5772(5) 0.086(3) Uani 1 1 d . . . H33 H 0.0382 0.3037 0.5822 0.103 Uiso 1 1 calc R . . C32 C 0.0996(8) 0.4353(8) 0.5409(6) 0.103(3) Uani 1 1 d . . . H32 H 0.0210 0.4327 0.5208 0.124 Uiso 1 1 calc R . . C31 C 0.2045(8) 0.5171(8) 0.5339(5) 0.094(3) Uani 1 1 d . . . H31 H 0.1971 0.5710 0.5105 0.113 Uiso 1 1 calc R . . C30 C 0.3198(7) 0.5184(6) 0.5615(4) 0.071(2) Uani 1 1 d . . . H30 H 0.3909 0.5726 0.5555 0.085 Uiso 1 1 calc R . . C44 C 0.2324(7) 0.2789(6) 0.6483(4) 0.0632(19) Uani 1 1 d . . . H44 H 0.3091 0.2864 0.6746 0.076 Uiso 1 1 calc R . . C45 C 0.1498(7) 0.1280(6) 0.6969(5) 0.070(2) Uani 1 1 d . . . C50 C 0.0941(8) 0.1323(7) 0.7637(5) 0.082(2) Uani 1 1 d . . . C49 C 0.1019(10) 0.0621(9) 0.8091(6) 0.108(3) Uani 1 1 d . . . H49 H 0.0652 0.0628 0.8539 0.130 Uiso 1 1 calc R . . C48 C 0.1632(12) -0.0077(10) 0.7882(8) 0.128(4) Uani 1 1 d . . . H48 H 0.1726 -0.0504 0.8215 0.153 Uiso 1 1 calc R . . C47 C 0.2132(10) -0.0184(8) 0.7185(8) 0.116(4) Uani 1 1 d . . . H47 H 0.2482 -0.0714 0.7034 0.139 Uiso 1 1 calc R . . C46 C 0.2082(8) 0.0535(7) 0.6729(6) 0.085(2) Uani 1 1 d . . . C54 C 0.0278(8) 0.2119(8) 0.7856(5) 0.093(3) Uani 1 1 d . . . H54 H -0.0143 0.2176 0.7376 0.111 Uiso 1 1 calc R . . C56 C 0.1192(9) 0.3222(8) 0.8246(6) 0.116(3) Uani 1 1 d . . . H56A H 0.1619 0.3192 0.8721 0.175 Uiso 1 1 calc R . . H56B H 0.0753 0.3720 0.8357 0.175 Uiso 1 1 calc R . . H56C H 0.1790 0.3459 0.7911 0.175 Uiso 1 1 calc R . . C55 C -0.0712(10) 0.1773(10) 0.8367(6) 0.144(5) Uani 1 1 d . . . H55A H -0.1246 0.1039 0.8144 0.217 Uiso 1 1 calc R . . H55B H -0.1202 0.2235 0.8406 0.217 Uiso 1 1 calc R . . H55C H -0.0314 0.1827 0.8874 0.217 Uiso 1 1 calc R . . C51 C 0.2564(9) 0.0406(7) 0.5952(7) 0.098(3) Uani 1 1 d . . . H51 H 0.2732 0.1091 0.5798 0.117 Uiso 1 1 calc R . . C52 C 0.1592(10) -0.0465(11) 0.5330(6) 0.134(4) Uani 1 1 d . . . H52A H 0.1904 -0.0503 0.4844 0.202 Uiso 1 1 calc R . . H52B H 0.0841 -0.0295 0.5288 0.202 Uiso 1 1 calc R . . H52C H 0.1414 -0.1149 0.5464 0.202 Uiso 1 1 calc R . . C53 C 0.3768(9) 0.0161(9) 0.5985(7) 0.135(4) Uani 1 1 d . . . H53A H 0.3639 -0.0494 0.6154 0.203 Uiso 1 1 calc R . . H53B H 0.4414 0.0747 0.6341 0.203 Uiso 1 1 calc R . . H53C H 0.4013 0.0074 0.5479 0.203 Uiso 1 1 calc R . . C58 C 0.629(2) 0.106(3) -0.027(2) 0.30(2) Uani 0.50 1 d PDU . . H58A H 0.6155 0.0616 -0.0795 0.357 Uiso 0.50 1 calc PR . . H58B H 0.6075 0.1690 -0.0287 0.357 Uiso 0.50 1 calc PR . . C59 C 0.763(3) 0.138(2) 0.0089(15) 0.27(2) Uani 0.50 1 d PDU . . H59A H 0.7661 0.1352 0.0624 0.403 Uiso 0.50 1 calc PR . . H59B H 0.8085 0.2097 0.0052 0.403 Uiso 0.50 1 calc PR . . H59C H 0.7996 0.0886 -0.0177 0.403 Uiso 0.50 1 calc PR . . C57 C 0.553(3) 0.042(3) 0.0239(12) 0.31(2) Uani 0.50 1 d PDU . . H57A H 0.6035 0.0101 0.0508 0.370 Uiso 0.50 1 calc PR . . H57B H 0.5269 0.0888 0.0622 0.370 Uiso 0.50 1 calc PR . . 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 Zn1 0.0515(5) 0.0644(6) 0.0690(6) 0.0163(4) 0.0150(4) 0.0232(4) N2 0.059(4) 0.082(5) 0.081(4) 0.027(4) 0.021(3) 0.025(4) N1 0.057(4) 0.073(4) 0.072(4) 0.026(3) 0.016(3) 0.025(3) N3 0.053(3) 0.063(4) 0.068(4) 0.010(3) 0.013(3) 0.021(3) N5 0.048(3) 0.071(4) 0.055(3) 0.009(3) 0.004(3) 0.018(3) N4 0.041(3) 0.053(3) 0.071(4) 0.014(3) 0.014(3) 0.017(3) N6 0.059(4) 0.065(4) 0.083(4) 0.026(4) 0.020(3) 0.020(3) C15 0.070(6) 0.098(7) 0.095(6) 0.029(5) 0.025(5) 0.019(5) C14 0.082(7) 0.142(10) 0.100(7) 0.047(8) 0.027(5) 0.022(7) C13 0.088(7) 0.098(8) 0.095(7) 0.034(6) 0.011(6) -0.006(6) C11 0.078(6) 0.068(6) 0.080(6) 0.016(5) 0.000(5) -0.002(5) C12 0.058(5) 0.064(5) 0.060(5) 0.015(4) 0.003(4) 0.007(4) C10 0.117(9) 0.071(7) 0.105(8) 0.025(6) -0.009(7) 0.002(6) C9 0.129(9) 0.070(7) 0.111(8) 0.020(6) -0.005(7) 0.026(7) C8 0.096(6) 0.064(6) 0.097(6) 0.016(5) 0.004(5) 0.026(5) C7 0.074(5) 0.069(6) 0.071(5) 0.015(4) -0.005(4) 0.029(5) C1 0.062(5) 0.064(5) 0.085(6) 0.007(4) 0.015(4) 0.026(4) C2 0.069(6) 0.097(7) 0.122(7) 0.024(6) 0.013(5) 0.049(5) C3 0.063(6) 0.106(8) 0.137(9) 0.017(7) 0.008(6) 0.043(6) C4 0.061(6) 0.127(9) 0.131(9) 0.005(7) 0.032(6) 0.048(6) C5 0.068(5) 0.092(6) 0.102(7) 0.013(5) 0.033(5) 0.025(5) C6 0.056(5) 0.069(5) 0.078(5) 0.007(4) 0.017(4) 0.025(4) C16 0.063(5) 0.069(5) 0.066(5) 0.013(4) 0.020(4) 0.020(4) C17 0.048(4) 0.072(5) 0.059(4) 0.012(4) 0.009(3) 0.014(4) C18 0.060(5) 0.077(6) 0.072(5) 0.013(4) 0.007(4) 0.023(4) C19 0.065(5) 0.081(7) 0.101(7) 0.014(5) -0.005(5) 0.006(5) C20 0.075(6) 0.155(11) 0.090(7) 0.028(7) -0.004(5) 0.047(7) C21 0.088(6) 0.092(7) 0.094(6) 0.032(5) -0.014(5) 0.029(6) C22 0.066(5) 0.074(6) 0.065(5) 0.018(4) 0.002(4) 0.020(4) C23 0.068(6) 0.087(7) 0.098(7) 0.013(6) 0.015(5) 0.006(5) C24 0.221(11) 0.109(7) 0.207(10) 0.052(7) 0.120(9) 0.052(7) C25 0.221(11) 0.109(7) 0.207(10) 0.052(7) 0.120(9) 0.052(7) C26 0.081(6) 0.073(6) 0.092(6) 0.022(5) -0.003(5) 0.025(5) C28 0.090(7) 0.132(9) 0.128(9) 0.044(7) 0.011(6) 0.013(7) C27 0.139(9) 0.070(6) 0.106(7) 0.006(6) 0.011(6) 0.019(6) C43 0.052(4) 0.093(6) 0.075(5) 0.007(4) 0.007(4) 0.030(4) C42 0.051(5) 0.112(7) 0.092(6) 0.004(6) -0.006(4) 0.039(5) C41 0.060(5) 0.109(7) 0.113(7) 0.029(6) 0.024(5) 0.049(5) C39 0.053(4) 0.089(6) 0.083(5) 0.021(5) 0.027(4) 0.038(4) C40 0.048(4) 0.064(5) 0.067(5) 0.020(4) 0.026(3) 0.023(4) C38 0.079(6) 0.080(6) 0.094(6) -0.004(5) 0.015(5) 0.043(5) C37 0.066(5) 0.080(6) 0.079(5) 0.000(4) 0.011(4) 0.028(5) C36 0.059(5) 0.076(5) 0.078(5) 0.023(5) 0.018(4) 0.028(4) C35 0.040(4) 0.061(4) 0.056(4) 0.016(4) 0.013(3) 0.017(3) C29 0.053(4) 0.067(5) 0.059(4) 0.023(4) 0.022(3) 0.032(4) C34 0.044(4) 0.063(5) 0.076(5) 0.024(4) 0.016(3) 0.023(4) C33 0.047(4) 0.105(7) 0.126(7) 0.056(6) 0.017(4) 0.036(5) C32 0.064(6) 0.131(8) 0.144(9) 0.069(7) 0.014(5) 0.051(6) C31 0.075(6) 0.108(7) 0.129(8) 0.074(6) 0.017(5) 0.045(6) C30 0.057(5) 0.079(5) 0.091(6) 0.038(5) 0.022(4) 0.027(4) C44 0.058(5) 0.073(5) 0.070(5) 0.031(4) 0.016(4) 0.029(4) C45 0.057(5) 0.064(5) 0.087(6) 0.029(5) 0.016(4) 0.011(4) C50 0.072(5) 0.071(6) 0.078(6) 0.018(5) 0.007(5) -0.005(5) C49 0.114(8) 0.089(8) 0.104(8) 0.036(7) 0.027(6) 0.002(6) C48 0.149(11) 0.103(9) 0.122(10) 0.068(8) 0.012(8) 0.011(8) C47 0.122(9) 0.085(7) 0.159(10) 0.066(7) 0.026(8) 0.036(6) C46 0.078(6) 0.065(6) 0.116(7) 0.038(5) 0.023(5) 0.019(5) C54 0.084(6) 0.097(7) 0.079(6) 0.008(5) 0.020(5) 0.014(6) C56 0.096(7) 0.106(8) 0.123(8) -0.003(7) 0.020(6) 0.019(6) C55 0.103(8) 0.179(12) 0.106(8) 0.011(8) 0.034(7) -0.001(8) C51 0.089(7) 0.065(6) 0.154(9) 0.044(6) 0.053(7) 0.028(5) C52 0.096(8) 0.209(14) 0.109(8) 0.044(9) 0.027(7) 0.061(9) C53 0.087(7) 0.121(9) 0.173(11) -0.021(8) 0.007(7) 0.040(7) C58 0.57(7) 0.30(4) 0.14(3) 0.10(3) 0.01(3) 0.29(4) C59 0.56(6) 0.13(2) 0.11(2) -0.009(17) -0.04(3) 0.15(4) C57 0.55(7) 0.30(5) 0.17(3) 0.07(3) 0.06(4) 0.28(4) _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 Zn1 N4 1.968(5) . ? Zn1 N1 1.995(6) . ? Zn1 N2 2.096(6) . ? Zn1 N3 2.132(6) . ? Zn1 N5 2.163(5) . ? N2 C15 1.331(9) . ? N2 C12 1.349(9) . ? N1 C7 1.364(9) . ? N1 C1 1.379(9) . ? N3 C16 1.266(8) . ? N3 C17 1.441(8) . ? N5 C43 1.316(8) . ? N5 C40 1.357(8) . ? N4 C35 1.348(8) . ? N4 C29 1.405(8) . ? N6 C44 1.263(8) . ? N6 C45 1.423(9) . ? C15 C14 1.390(13) . ? C15 H15 0.9300 . ? C14 C13 1.346(13) . ? C14 H14 0.9300 . ? C13 C11 1.399(13) . ? C13 H13 0.9300 . ? C11 C10 1.394(13) . ? C11 C12 1.395(11) . ? C12 C7 1.432(10) . ? C10 C9 1.321(13) . ? C10 H10 0.9300 . ? C9 C8 1.410(13) . ? C9 H9 0.9300 . ? C8 C7 1.401(10) . ? C8 H8 0.9300 . ? C1 C6 1.408(10) . ? C1 C2 1.412(10) . ? C2 C3 1.347(12) . ? C2 H2 0.9300 . ? C3 C4 1.373(13) . ? C3 H3 0.9300 . ? C4 C5 1.374(11) . ? C4 H4 0.9300 . ? C5 C6 1.398(10) . ? C5 H5 0.9300 . ? C6 C16 1.459(10) . ? C16 H16 0.9300 . ? C17 C22 1.383(10) . ? C17 C18 1.388(10) . ? C18 C19 1.357(10) . ? C18 C23 1.498(11) . ? C19 C20 1.373(12) . ? C19 H19 0.9300 . ? C20 C21 1.388(12) . ? C20 H20 0.9300 . ? C21 C22 1.373(10) . ? C21 H21 0.9300 . ? C22 C26 1.506(11) . ? C23 C25 1.477(14) . ? C23 C24 1.477(14) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C28 1.524(12) . ? C26 C27 1.525(11) . ? C26 H26 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C43 C42 1.390(10) . ? C43 H43 0.9300 . ? C42 C41 1.336(11) . ? C42 H42 0.9300 . ? C41 C39 1.417(10) . ? C41 H41 0.9300 . ? C39 C38 1.396(11) . ? C39 C40 1.421(9) . ? C40 C35 1.442(8) . ? C38 C37 1.349(10) . ? C38 H38 0.9300 . ? C37 C36 1.367(9) . ? C37 H37 0.9300 . ? C36 C35 1.399(10) . ? C36 H36 0.9300 . ? C29 C34 1.379(9) . ? C29 C30 1.406(9) . ? C34 C33 1.384(9) . ? C34 C44 1.450(9) . ? C33 C32 1.364(11) . ? C33 H33 0.9300 . ? C32 C31 1.375(12) . ? C32 H32 0.9300 . ? C31 C30 1.366(10) . ? C31 H31 0.9300 . ? C30 H30 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.391(11) . ? C45 C46 1.393(11) . ? C50 C49 1.383(12) . ? C50 C54 1.510(12) . ? C49 C48 1.356(14) . ? C49 H49 0.9300 . ? C48 C47 1.406(15) . ? C48 H48 0.9300 . ? C47 C46 1.398(12) . ? C47 H47 0.9300 . ? C46 C51 1.526(12) . ? C54 C56 1.500(12) . ? C54 C55 1.521(12) . ? C54 H54 0.9800 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C51 C52 1.513(14) . ? C51 C53 1.517(11) . ? C51 H51 0.9800 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C58 C59 1.499(18) . ? C58 C57 1.508(19) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C57 C57 1.43(2) 2_655 ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn1 N1 111.1(2) . . ? N4 Zn1 N2 119.2(2) . . ? N1 Zn1 N2 79.1(3) . . ? N4 Zn1 N3 115.4(2) . . ? N1 Zn1 N3 83.2(2) . . ? N2 Zn1 N3 125.4(2) . . ? N4 Zn1 N5 80.3(2) . . ? N1 Zn1 N5 168.2(2) . . ? N2 Zn1 N5 93.3(2) . . ? N3 Zn1 N5 94.3(2) . . ? C15 N2 C12 118.2(7) . . ? C15 N2 Zn1 128.2(6) . . ? C12 N2 Zn1 113.6(5) . . ? C7 N1 C1 123.5(6) . . ? C7 N1 Zn1 116.0(5) . . ? C1 N1 Zn1 120.5(5) . . ? C16 N3 C17 117.6(6) . . ? C16 N3 Zn1 120.4(5) . . ? C17 N3 Zn1 121.8(4) . . ? C43 N5 C40 118.1(6) . . ? C43 N5 Zn1 133.2(5) . . ? C40 N5 Zn1 108.6(4) . . ? C35 N4 C29 118.3(5) . . ? C35 N4 Zn1 115.6(4) . . ? C29 N4 Zn1 125.1(4) . . ? C44 N6 C45 119.0(6) . . ? N2 C15 C14 122.0(9) . . ? N2 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C13 C14 C15 119.1(10) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C13 C11 121.3(10) . . ? C14 C13 H13 119.3 . . ? C11 C13 H13 119.3 . . ? C10 C11 C12 119.4(10) . . ? C10 C11 C13 124.9(10) . . ? C12 C11 C13 115.7(9) . . ? N2 C12 C11 123.6(8) . . ? N2 C12 C7 115.2(7) . . ? C11 C12 C7 121.1(8) . . ? C9 C10 C11 120.8(10) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C9 C8 121.3(10) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C7 C8 C9 121.0(9) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? N1 C7 C8 127.8(8) . . ? N1 C7 C12 116.1(7) . . ? C8 C7 C12 116.1(8) . . ? N1 C1 C6 118.6(6) . . ? N1 C1 C2 124.4(8) . . ? C6 C1 C2 117.0(8) . . ? C3 C2 C1 121.8(9) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 121.4(8) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C3 C4 C5 118.7(9) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 121.5(9) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 119.4(7) . . ? C5 C6 C16 117.5(8) . . ? C1 C6 C16 122.9(7) . . ? N3 C16 C6 126.1(7) . . ? N3 C16 H16 116.9 . . ? C6 C16 H16 116.9 . . ? C22 C17 C18 122.1(7) . . ? C22 C17 N3 121.0(6) . . ? C18 C17 N3 116.6(7) . . ? C19 C18 C17 118.9(8) . . ? C19 C18 C23 119.4(8) . . ? C17 C18 C23 121.7(7) . . ? C18 C19 C20 120.0(8) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 121.0(8) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 120.0(8) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 117.9(7) . . ? C21 C22 C26 119.9(7) . . ? C17 C22 C26 122.2(6) . . ? C25 C23 C24 110.3(10) . . ? C25 C23 C18 111.2(8) . . ? C24 C23 C18 114.2(8) . . ? C25 C23 H23 106.9 . . ? C24 C23 H23 106.9 . . ? C18 C23 H23 106.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 C28 111.5(7) . . ? C22 C26 C27 111.0(7) . . ? C28 C26 C27 110.8(8) . . ? C22 C26 H26 107.8 . . ? C28 C26 H26 107.8 . . ? C27 C26 H26 107.8 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C43 C42 124.0(7) . . ? N5 C43 H43 118.0 . . ? C42 C43 H43 118.0 . . ? C41 C42 C43 118.4(7) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C42 C41 C39 121.5(7) . . ? C42 C41 H41 119.3 . . ? C39 C41 H41 119.3 . . ? C38 C39 C41 124.6(7) . . ? C38 C39 C40 119.8(7) . . ? C41 C39 C40 115.6(8) . . ? N5 C40 C39 122.4(6) . . ? N5 C40 C35 117.5(6) . . ? C39 C40 C35 120.1(7) . . ? C37 C38 C39 119.5(7) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C37 C36 122.0(8) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C36 C35 122.7(7) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? N4 C35 C36 127.9(6) . . ? N4 C35 C40 116.4(6) . . ? C36 C35 C40 115.8(6) . . ? C34 C29 N4 123.2(6) . . ? C34 C29 C30 118.5(6) . . ? N4 C29 C30 118.1(6) . . ? C29 C34 C33 119.6(6) . . ? C29 C34 C44 121.3(6) . . ? C33 C34 C44 119.0(7) . . ? C32 C33 C34 120.9(8) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C32 C31 120.4(7) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C30 C31 C32 119.3(7) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C31 C30 C29 121.1(7) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? N6 C44 C34 122.5(6) . . ? N6 C44 H44 118.8 . . ? C34 C44 H44 118.8 . . ? C50 C45 C46 122.6(8) . . ? C50 C45 N6 117.0(7) . . ? C46 C45 N6 120.3(8) . . ? C49 C50 C45 118.1(9) . . ? C49 C50 C54 121.4(9) . . ? C45 C50 C54 120.5(8) . . ? C48 C49 C50 120.0(11) . . ? C48 C49 H49 120.0 . . ? C50 C49 H49 120.0 . . ? C49 C48 C47 123.0(10) . . ? C49 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C46 C47 C48 117.4(10) . . ? C46 C47 H47 121.3 . . ? C48 C47 H47 121.3 . . ? C45 C46 C47 118.8(9) . . ? C45 C46 C51 122.4(7) . . ? C47 C46 C51 118.6(9) . . ? C56 C54 C50 111.1(7) . . ? C56 C54 C55 109.4(8) . . ? C50 C54 C55 113.5(9) . . ? C56 C54 H54 107.5 . . ? C50 C54 H54 107.5 . . ? C55 C54 H54 107.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C52 C51 C53 109.0(8) . . ? C52 C51 C46 111.3(7) . . ? C53 C51 C46 113.4(9) . . ? C52 C51 H51 107.6 . . ? C53 C51 H51 107.6 . . ? C46 C51 H51 107.6 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C59 C58 C57 105.2(18) . . ? C59 C58 H58A 110.7 . . ? C57 C58 H58A 110.7 . . ? C59 C58 H58B 110.7 . . ? C57 C58 H58B 110.7 . . ? H58A C58 H58B 108.8 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C57 C58 108(2) 2_655 . ? C57 C57 H57A 110.0 2_655 . ? C58 C57 H57A 110.0 . . ? C57 C57 H57B 110.0 2_655 . ? C58 C57 H57B 110.0 . . ? H57A C57 H57B 108.4 . . ? 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 N4 Zn1 N2 C15 -71.0(7) . . . . ? N1 Zn1 N2 C15 -179.2(7) . . . . ? N3 Zn1 N2 C15 107.4(7) . . . . ? N5 Zn1 N2 C15 9.8(7) . . . . ? N4 Zn1 N2 C12 110.4(5) . . . . ? N1 Zn1 N2 C12 2.2(5) . . . . ? N3 Zn1 N2 C12 -71.2(5) . . . . ? N5 Zn1 N2 C12 -168.9(5) . . . . ? N4 Zn1 N1 C7 -119.1(5) . . . . ? N2 Zn1 N1 C7 -1.9(5) . . . . ? N3 Zn1 N1 C7 126.2(5) . . . . ? N5 Zn1 N1 C7 48.1(14) . . . . ? N4 Zn1 N1 C1 58.9(6) . . . . ? N2 Zn1 N1 C1 176.1(6) . . . . ? N3 Zn1 N1 C1 -55.7(6) . . . . ? N5 Zn1 N1 C1 -133.9(11) . . . . ? N4 Zn1 N3 C16 -71.1(6) . . . . ? N1 Zn1 N3 C16 39.1(6) . . . . ? N2 Zn1 N3 C16 110.5(6) . . . . ? N5 Zn1 N3 C16 -152.4(6) . . . . ? N4 Zn1 N3 C17 104.9(5) . . . . ? N1 Zn1 N3 C17 -144.9(5) . . . . ? N2 Zn1 N3 C17 -73.5(6) . . . . ? N5 Zn1 N3 C17 23.6(5) . . . . ? N4 Zn1 N5 C43 -176.0(7) . . . . ? N1 Zn1 N5 C43 16.1(15) . . . . ? N2 Zn1 N5 C43 64.9(7) . . . . ? N3 Zn1 N5 C43 -61.0(7) . . . . ? N4 Zn1 N5 C40 9.3(4) . . . . ? N1 Zn1 N5 C40 -158.6(10) . . . . ? N2 Zn1 N5 C40 -109.7(5) . . . . ? N3 Zn1 N5 C40 124.4(4) . . . . ? N1 Zn1 N4 C35 165.9(4) . . . . ? N2 Zn1 N4 C35 76.8(5) . . . . ? N3 Zn1 N4 C35 -101.7(5) . . . . ? N5 Zn1 N4 C35 -11.5(5) . . . . ? N1 Zn1 N4 C29 -2.8(6) . . . . ? N2 Zn1 N4 C29 -91.9(5) . . . . ? N3 Zn1 N4 C29 89.6(5) . . . . ? N5 Zn1 N4 C29 179.8(5) . . . . ? C12 N2 C15 C14 2.3(12) . . . . ? Zn1 N2 C15 C14 -176.3(7) . . . . ? N2 C15 C14 C13 -1.0(15) . . . . ? C15 C14 C13 C11 0.2(16) . . . . ? C14 C13 C11 C10 -179.4(10) . . . . ? C14 C13 C11 C12 -0.6(14) . . . . ? C15 N2 C12 C11 -2.7(11) . . . . ? Zn1 N2 C12 C11 176.1(6) . . . . ? C15 N2 C12 C7 179.1(7) . . . . ? Zn1 N2 C12 C7 -2.1(8) . . . . ? C10 C11 C12 N2 -179.2(7) . . . . ? C13 C11 C12 N2 1.9(12) . . . . ? C10 C11 C12 C7 -1.2(12) . . . . ? C13 C11 C12 C7 179.9(7) . . . . ? C12 C11 C10 C9 4.7(14) . . . . ? C13 C11 C10 C9 -176.5(9) . . . . ? C11 C10 C9 C8 -5.9(16) . . . . ? C10 C9 C8 C7 3.6(15) . . . . ? C1 N1 C7 C8 7.2(12) . . . . ? Zn1 N1 C7 C8 -174.9(6) . . . . ? C1 N1 C7 C12 -176.6(6) . . . . ? Zn1 N1 C7 C12 1.4(8) . . . . ? C9 C8 C7 N1 176.1(8) . . . . ? C9 C8 C7 C12 -0.2(12) . . . . ? N2 C12 C7 N1 0.6(10) . . . . ? C11 C12 C7 N1 -177.6(7) . . . . ? N2 C12 C7 C8 177.2(7) . . . . ? C11 C12 C7 C8 -0.9(11) . . . . ? C7 N1 C1 C6 -138.6(7) . . . . ? Zn1 N1 C1 C6 43.6(9) . . . . ? C7 N1 C1 C2 42.6(11) . . . . ? Zn1 N1 C1 C2 -135.3(7) . . . . ? N1 C1 C2 C3 176.8(8) . . . . ? C6 C1 C2 C3 -2.1(13) . . . . ? C1 C2 C3 C4 4.3(15) . . . . ? C2 C3 C4 C5 -2.9(16) . . . . ? C3 C4 C5 C6 -0.7(14) . . . . ? C4 C5 C6 C1 2.8(13) . . . . ? C4 C5 C6 C16 178.1(8) . . . . ? N1 C1 C6 C5 179.6(7) . . . . ? C2 C1 C6 C5 -1.5(11) . . . . ? N1 C1 C6 C16 4.6(11) . . . . ? C2 C1 C6 C16 -176.5(7) . . . . ? C17 N3 C16 C6 173.2(7) . . . . ? Zn1 N3 C16 C6 -10.6(10) . . . . ? C5 C6 C16 N3 163.5(8) . . . . ? C1 C6 C16 N3 -21.4(12) . . . . ? C16 N3 C17 C22 81.3(9) . . . . ? Zn1 N3 C17 C22 -94.8(7) . . . . ? C16 N3 C17 C18 -103.3(8) . . . . ? Zn1 N3 C17 C18 80.6(7) . . . . ? C22 C17 C18 C19 -2.9(12) . . . . ? N3 C17 C18 C19 -178.2(7) . . . . ? C22 C17 C18 C23 177.0(8) . . . . ? N3 C17 C18 C23 1.7(11) . . . . ? C17 C18 C19 C20 2.6(13) . . . . ? C23 C18 C19 C20 -177.2(9) . . . . ? C18 C19 C20 C21 -1.2(15) . . . . ? C19 C20 C21 C22 -0.1(14) . . . . ? C20 C21 C22 C17 -0.1(13) . . . . ? C20 C21 C22 C26 179.6(8) . . . . ? C18 C17 C22 C21 1.6(11) . . . . ? N3 C17 C22 C21 176.7(7) . . . . ? C18 C17 C22 C26 -178.2(7) . . . . ? N3 C17 C22 C26 -3.1(11) . . . . ? C19 C18 C23 C25 -76.0(12) . . . . ? C17 C18 C23 C25 104.2(10) . . . . ? C19 C18 C23 C24 49.5(13) . . . . ? C17 C18 C23 C24 -130.3(10) . . . . ? C21 C22 C26 C28 72.7(10) . . . . ? C17 C22 C26 C28 -107.6(9) . . . . ? C21 C22 C26 C27 -51.4(11) . . . . ? C17 C22 C26 C27 128.3(8) . . . . ? C40 N5 C43 C42 1.3(12) . . . . ? Zn1 N5 C43 C42 -173.0(6) . . . . ? N5 C43 C42 C41 -0.6(14) . . . . ? C43 C42 C41 C39 1.0(14) . . . . ? C42 C41 C39 C38 175.8(9) . . . . ? C42 C41 C39 C40 -2.0(12) . . . . ? C43 N5 C40 C39 -2.4(10) . . . . ? Zn1 N5 C40 C39 173.2(5) . . . . ? C43 N5 C40 C35 178.3(6) . . . . ? Zn1 N5 C40 C35 -6.1(7) . . . . ? C38 C39 C40 N5 -175.2(7) . . . . ? C41 C39 C40 N5 2.7(11) . . . . ? C38 C39 C40 C35 4.1(11) . . . . ? C41 C39 C40 C35 -178.0(6) . . . . ? C41 C39 C38 C37 -179.2(8) . . . . ? C40 C39 C38 C37 -1.4(13) . . . . ? C39 C38 C37 C36 -1.9(13) . . . . ? C38 C37 C36 C35 2.6(13) . . . . ? C29 N4 C35 C36 2.4(10) . . . . ? Zn1 N4 C35 C36 -167.1(6) . . . . ? C29 N4 C35 C40 -178.7(5) . . . . ? Zn1 N4 C35 C40 11.8(7) . . . . ? C37 C36 C35 N4 178.9(7) . . . . ? C37 C36 C35 C40 0.1(10) . . . . ? N5 C40 C35 N4 -3.0(9) . . . . ? C39 C40 C35 N4 177.7(6) . . . . ? N5 C40 C35 C36 176.0(6) . . . . ? C39 C40 C35 C36 -3.3(10) . . . . ? C35 N4 C29 C34 71.6(9) . . . . ? Zn1 N4 C29 C34 -120.0(7) . . . . ? C35 N4 C29 C30 -112.1(7) . . . . ? Zn1 N4 C29 C30 56.3(8) . . . . ? N4 C29 C34 C33 177.1(7) . . . . ? C30 C29 C34 C33 0.9(11) . . . . ? N4 C29 C34 C44 -0.4(11) . . . . ? C30 C29 C34 C44 -176.6(6) . . . . ? C29 C34 C33 C32 -0.6(13) . . . . ? C44 C34 C33 C32 176.9(8) . . . . ? C34 C33 C32 C31 -0.8(15) . . . . ? C33 C32 C31 C30 2.0(15) . . . . ? C32 C31 C30 C29 -1.7(14) . . . . ? C34 C29 C30 C31 0.3(11) . . . . ? N4 C29 C30 C31 -176.1(7) . . . . ? C45 N6 C44 C34 -175.4(7) . . . . ? C29 C34 C44 N6 -173.0(7) . . . . ? C33 C34 C44 N6 9.5(11) . . . . ? C44 N6 C45 C50 108.4(8) . . . . ? C44 N6 C45 C46 -75.7(10) . . . . ? C46 C45 C50 C49 2.5(12) . . . . ? N6 C45 C50 C49 178.3(7) . . . . ? C46 C45 C50 C54 -177.7(8) . . . . ? N6 C45 C50 C54 -1.9(11) . . . . ? C45 C50 C49 C48 0.4(14) . . . . ? C54 C50 C49 C48 -179.3(9) . . . . ? C50 C49 C48 C47 -4.7(18) . . . . ? C49 C48 C47 C46 5.8(17) . . . . ? C50 C45 C46 C47 -1.3(13) . . . . ? N6 C45 C46 C47 -176.9(8) . . . . ? C50 C45 C46 C51 173.0(8) . . . . ? N6 C45 C46 C51 -2.6(12) . . . . ? C48 C47 C46 C45 -2.7(14) . . . . ? C48 C47 C46 C51 -177.3(9) . . . . ? C49 C50 C54 C56 99.0(10) . . . . ? C45 C50 C54 C56 -80.8(10) . . . . ? C49 C50 C54 C55 -24.8(12) . . . . ? C45 C50 C54 C55 155.5(8) . . . . ? C45 C46 C51 C52 -92.8(10) . . . . ? C47 C46 C51 C52 81.5(11) . . . . ? C45 C46 C51 C53 143.8(8) . . . . ? C47 C46 C51 C53 -41.9(12) . . . . ? C59 C58 C57 C57 -146(5) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.549 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.067