# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Donal O'Shea" _publ_contact_author_email DONAL.F.OSHEA@UCD.IE _publ_section_title ; Co(II), Ni(II), Cu(II) and Zn(II) Complexes of Tetraphenylazadipyrromethene ; loop_ _publ_author_name "Donal O'Shea" 'John Gallagher' 'Eric McInnes' 'Helge Muller-Bunz' 'Aniello Palma' ; J.Wolowska ; # Attachment 'AZA-4M.CIF' # Four Datasets for archiving at the RSC & CSD # data_Cobalt _database_code_depnum_ccdc_archive 'CCDC 668337' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 589 _chemical_formula_moiety 'C64 H44 Co N6' _chemical_formula_sum 'C64 H44 Co N6' _chemical_formula_weight 955.98 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 19.860(3) _cell_length_b 44.375(5) _cell_length_c 10.7534(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9477(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3053 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.9 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 0.413 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9834 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.16 _diffrn_measured_fraction_theta_max 1.00 _diffrn_reflns_theta_full 24.2 _diffrn_measured_fraction_theta_full 1.00 _reflns_number_total 3161 _reflns_number_gt 2943 _reflns_threshold_expression I>2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+6.4463P] 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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack -0.006(17) _refine_ls_number_reflns 3161 _refine_ls_number_parameters 321 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.40 _refine_diff_density_min -0.32 _refine_diff_density_rms 0.05 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 Co1 Co 0.2500 0.2500 0.99765(5) 0.01782(18) Uani 1 2 d S . . C1 C 0.19716(18) 0.15698(7) 1.1831(3) 0.0251(8) Uani 1 1 d . . . H1 H 0.1553 0.1487 1.1578 0.030 Uiso 1 1 calc R . . C2 C 0.24702(18) 0.13819(8) 1.2278(4) 0.0340(9) Uani 1 1 d . . . H2 H 0.2389 0.1172 1.2353 0.041 Uiso 1 1 calc R . . C3 C 0.30898(18) 0.14999(8) 1.2618(4) 0.0340(9) Uani 1 1 d . . . H3 H 0.3439 0.1370 1.2898 0.041 Uiso 1 1 calc R . . C4 C 0.31975(17) 0.18062(8) 1.2550(4) 0.0312(8) Uani 1 1 d . . . H4 H 0.3620 0.1888 1.2793 0.037 Uiso 1 1 calc R . . C5 C 0.26915(17) 0.19954(8) 1.2127(3) 0.0231(8) Uani 1 1 d . . . H5 H 0.2767 0.2207 1.2097 0.028 Uiso 1 1 calc R . . C6 C 0.20746(16) 0.18797(7) 1.1746(3) 0.0197(7) Uani 1 1 d . . . C7 C 0.15436(16) 0.20730(7) 1.1246(3) 0.0181(7) Uani 1 1 d . . . N1 N 0.16603(13) 0.23431(6) 1.0738(3) 0.0180(6) Uani 1 1 d . . . C8 C 0.08410(17) 0.20034(7) 1.1214(3) 0.0220(8) Uani 1 1 d . . . H8 H 0.0634 0.1825 1.1516 0.026 Uiso 1 1 calc R . . C9 C 0.05226(16) 0.22421(7) 1.0665(3) 0.0193(7) Uani 1 1 d . . . C10 C -0.02039(16) 0.22689(7) 1.0413(3) 0.0214(8) Uani 1 1 d . . . C11 C -0.06631(17) 0.21171(7) 1.1167(4) 0.0260(8) Uani 1 1 d . . . H11 H -0.0503 0.1998 1.1841 0.031 Uiso 1 1 calc R . . C12 C -0.13456(18) 0.21365(8) 1.0951(4) 0.0290(9) Uani 1 1 d . . . H12 H -0.1652 0.2032 1.1477 0.035 Uiso 1 1 calc R . . C13 C -0.15858(17) 0.23066(8) 0.9974(4) 0.0328(9) Uani 1 1 d . . . H13 H -0.2056 0.2319 0.9823 0.039 Uiso 1 1 calc R . . C14 C -0.11414(18) 0.24596(8) 0.9215(4) 0.0306(9) Uani 1 1 d . . . H14 H -0.1306 0.2580 0.8550 0.037 Uiso 1 1 calc R . . C15 C -0.04512(17) 0.24375(7) 0.9426(4) 0.0255(8) Uani 1 1 d . . . H15 H -0.0146 0.2539 0.8889 0.031 Uiso 1 1 calc R . . C16 C 0.10380(16) 0.24585(7) 1.0368(3) 0.0179(7) Uani 1 1 d . . . N2 N 0.09198(13) 0.27246(6) 0.9863(3) 0.0199(6) Uani 1 1 d . . . C17 C 0.13751(16) 0.29155(7) 0.9414(3) 0.0187(7) Uani 1 1 d . . . N3 N 0.20557(13) 0.28524(6) 0.9214(3) 0.0187(6) Uani 1 1 d . . . C18 C 0.12341(17) 0.32215(7) 0.9044(3) 0.0198(7) Uani 1 1 d . . . C19 C 0.05792(16) 0.33755(7) 0.8955(3) 0.0190(7) Uani 1 1 d . . . C20 C -0.00233(17) 0.32475(7) 0.9368(4) 0.0245(8) Uani 1 1 d . . . H20 H -0.0017 0.3057 0.9773 0.029 Uiso 1 1 calc R . . C21 C -0.06317(18) 0.33956(8) 0.9191(4) 0.0300(9) Uani 1 1 d . . . H21 H -0.1038 0.3305 0.9468 0.036 Uiso 1 1 calc R . . C22 C -0.06492(17) 0.36744(8) 0.8615(3) 0.0277(9) Uani 1 1 d . . . H22 H -0.1066 0.3775 0.8495 0.033 Uiso 1 1 calc R . . C23 C -0.00552(18) 0.38061(8) 0.8215(4) 0.0286(9) Uani 1 1 d . . . H23 H -0.0063 0.3997 0.7819 0.034 Uiso 1 1 calc R . . C24 C 0.05462(18) 0.36581(7) 0.8393(4) 0.0266(8) Uani 1 1 d . . . H24 H 0.0951 0.3751 0.8124 0.032 Uiso 1 1 calc R . . C25 C 0.18474(16) 0.33371(7) 0.8678(3) 0.0196(7) Uani 1 1 d . . . H25 H 0.1931 0.3538 0.8418 0.024 Uiso 1 1 calc R . . C26 C 0.23258(17) 0.31063(7) 0.8758(3) 0.0203(7) Uani 1 1 d . . . C27 C 0.30281(17) 0.31235(7) 0.8324(3) 0.0202(7) Uani 1 1 d . . . C28 C 0.33684(17) 0.33961(8) 0.8349(4) 0.0257(8) Uani 1 1 d . . . H28 H 0.3149 0.3571 0.8660 0.031 Uiso 1 1 calc R . . C29 C 0.40263(19) 0.34159(8) 0.7925(3) 0.0305(9) Uani 1 1 d . . . H29 H 0.4254 0.3604 0.7942 0.037 Uiso 1 1 calc R . . C30 C 0.43493(17) 0.31648(8) 0.7483(4) 0.0321(8) Uani 1 1 d . . . H30 H 0.4804 0.3178 0.7215 0.039 Uiso 1 1 calc R . . C31 C 0.40146(17) 0.28919(8) 0.7427(4) 0.0307(8) Uani 1 1 d . . . H31 H 0.4235 0.2719 0.7100 0.037 Uiso 1 1 calc R . . C32 C 0.33587(17) 0.28719(7) 0.7847(3) 0.0239(8) Uani 1 1 d . . . H32 H 0.3130 0.2684 0.7810 0.029 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 Co1 0.0145(3) 0.0182(3) 0.0208(4) 0.000 0.000 0.0002(3) C1 0.027(2) 0.0243(18) 0.024(2) 0.0018(16) 0.0046(16) 0.0000(15) C2 0.041(2) 0.0245(19) 0.037(3) 0.0063(18) 0.0071(18) 0.0081(16) C3 0.032(2) 0.035(2) 0.034(2) 0.0051(19) 0.0041(18) 0.0141(16) C4 0.0245(18) 0.039(2) 0.030(2) 0.0000(19) -0.0014(18) 0.0034(15) C5 0.0240(18) 0.0250(18) 0.020(2) 0.0020(14) 0.0024(15) 0.0016(14) C6 0.0220(18) 0.0223(18) 0.0149(18) -0.0015(14) 0.0030(14) 0.0031(14) C7 0.0175(17) 0.0191(17) 0.0178(18) -0.0030(15) 0.0005(13) -0.0027(14) N1 0.0163(14) 0.0183(14) 0.0195(16) 0.0004(12) 0.0014(11) -0.0017(11) C8 0.0216(18) 0.0208(17) 0.023(2) 0.0015(15) 0.0032(14) -0.0048(14) C9 0.0185(17) 0.0222(18) 0.0172(18) -0.0018(15) 0.0002(14) 0.0003(14) C10 0.0158(16) 0.0254(18) 0.0230(19) -0.0032(15) 0.0001(14) -0.0016(14) C11 0.026(2) 0.0280(19) 0.024(2) 0.0019(16) -0.0005(15) -0.0010(15) C12 0.0192(18) 0.036(2) 0.032(2) -0.0008(18) 0.0032(16) -0.0033(15) C13 0.0195(18) 0.043(2) 0.036(2) -0.005(2) -0.0058(18) 0.0003(16) C14 0.024(2) 0.037(2) 0.031(2) 0.0042(18) -0.0098(16) -0.0034(16) C15 0.0198(18) 0.032(2) 0.0253(19) 0.0020(16) -0.0013(15) -0.0018(14) C16 0.0187(17) 0.0199(18) 0.0152(18) 0.0009(14) -0.0002(12) 0.0023(13) N2 0.0173(14) 0.0225(14) 0.0198(16) -0.0024(13) 0.0006(12) 0.0000(11) C17 0.0175(18) 0.0216(18) 0.0170(18) -0.0022(15) 0.0001(14) -0.0021(14) N3 0.0175(14) 0.0215(15) 0.0170(15) 0.0001(12) 0.0007(11) 0.0022(11) C18 0.0223(18) 0.0206(17) 0.0165(18) -0.0007(14) -0.0020(14) -0.0010(14) C19 0.0216(18) 0.0201(17) 0.0152(18) -0.0020(14) -0.0021(14) 0.0014(13) C20 0.0261(19) 0.0191(17) 0.028(2) 0.0005(16) 0.0022(15) 0.0031(14) C21 0.026(2) 0.031(2) 0.033(2) -0.0067(18) 0.0013(16) 0.0006(15) C22 0.023(2) 0.033(2) 0.028(2) -0.0040(17) -0.0059(16) 0.0104(15) C23 0.032(2) 0.0255(19) 0.028(2) 0.0007(17) -0.0033(16) 0.0111(15) C24 0.0256(19) 0.0277(19) 0.027(2) 0.0035(16) 0.0019(15) 0.0019(15) C25 0.0241(18) 0.0152(16) 0.0194(19) 0.0020(15) -0.0008(14) -0.0021(14) C26 0.0236(18) 0.0223(18) 0.0150(18) 0.0001(15) -0.0033(14) -0.0036(14) C27 0.0177(17) 0.0256(19) 0.0173(18) 0.0033(15) -0.0011(14) -0.0006(14) C28 0.0268(19) 0.0266(19) 0.024(2) 0.0014(15) -0.0005(16) -0.0004(16) C29 0.029(2) 0.035(2) 0.027(2) 0.0051(17) 0.0020(16) -0.0144(16) C30 0.0223(18) 0.047(2) 0.027(2) 0.0045(19) 0.0020(17) -0.0042(16) C31 0.0290(19) 0.035(2) 0.028(2) 0.0026(18) 0.0097(17) 0.0017(16) C32 0.0247(18) 0.0256(18) 0.021(2) -0.0015(14) 0.0011(14) -0.0038(15) _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 Co1 N3 1.974(3) 14 ? Co1 N3 1.974(3) . ? Co1 N1 1.984(3) 14 ? Co1 N1 1.984(3) . ? C1 C2 1.381(5) . ? C1 C6 1.394(4) . ? C1 H1 0.9500 . ? C2 C3 1.386(5) . ? C2 H2 0.9500 . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 C7 1.462(5) . ? C7 N1 1.337(4) . ? C7 C8 1.430(5) . ? N1 C16 1.396(4) . ? C8 C9 1.367(5) . ? C8 H8 0.9500 . ? C9 C16 1.439(5) . ? C9 C10 1.473(5) . ? C10 C15 1.388(5) . ? C10 C11 1.394(5) . ? C11 C12 1.378(5) . ? C11 H11 0.9500 . ? C12 C13 1.379(6) . ? C12 H12 0.9500 . ? C13 C14 1.380(6) . ? C13 H13 0.9500 . ? C14 C15 1.393(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.321(4) . ? N2 C17 1.329(4) . ? C17 N3 1.397(4) . ? C17 C18 1.442(4) . ? N3 C26 1.341(4) . ? C18 C25 1.379(5) . ? C18 C19 1.472(4) . ? C19 C24 1.394(5) . ? C19 C20 1.397(5) . ? C20 C21 1.389(5) . ? C20 H20 0.9500 . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.385(5) . ? C22 H22 0.9500 . ? C23 C24 1.377(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.400(5) . ? C25 H25 0.9500 . ? C26 C27 1.473(5) . ? C27 C28 1.386(5) . ? C27 C32 1.393(5) . ? C28 C29 1.387(5) . ? C28 H28 0.9500 . ? C29 C30 1.371(5) . ? C29 H29 0.9500 . ? C30 C31 1.383(5) . ? C30 H30 0.9500 . ? C31 C32 1.382(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 N3 Co1 N3 130.92(16) 14 . ? N3 Co1 N1 94.22(11) 14 14 ? N3 Co1 N1 105.62(10) . 14 ? N3 Co1 N1 105.62(10) 14 . ? N3 Co1 N1 94.22(11) . . ? N1 Co1 N1 131.25(16) 14 . ? C2 C1 C6 120.9(3) . . ? C2 C1 H1 119.6 . . ? C6 C1 H1 119.6 . . ? C1 C2 C3 120.0(3) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.2(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 118.3(3) . . ? C5 C6 C7 121.8(3) . . ? C1 C6 C7 119.8(3) . . ? N1 C7 C8 110.7(3) . . ? N1 C7 C6 123.4(3) . . ? C8 C7 C6 125.9(3) . . ? C7 N1 C16 107.0(3) . . ? C7 N1 Co1 129.0(2) . . ? C16 N1 Co1 119.9(2) . . ? C9 C8 C7 107.1(3) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? C8 C9 C16 106.5(3) . . ? C8 C9 C10 126.5(3) . . ? C16 C9 C10 127.0(3) . . ? C15 C10 C11 118.3(3) . . ? C15 C10 C9 122.1(3) . . ? C11 C10 C9 119.6(3) . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 120.7(3) . . ? C10 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? N2 C16 N1 127.0(3) . . ? N2 C16 C9 124.2(3) . . ? N1 C16 C9 108.8(3) . . ? C16 N2 C17 126.7(3) . . ? N2 C17 N3 125.9(3) . . ? N2 C17 C18 124.6(3) . . ? N3 C17 C18 109.5(3) . . ? C26 N3 C17 106.0(3) . . ? C26 N3 Co1 129.7(2) . . ? C17 N3 Co1 121.8(2) . . ? C25 C18 C17 104.9(3) . . ? C25 C18 C19 126.1(3) . . ? C17 C18 C19 128.8(3) . . ? C24 C19 C20 117.6(3) . . ? C24 C19 C18 119.1(3) . . ? C20 C19 C18 123.2(3) . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.7(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C19 122.0(3) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? C18 C25 C26 108.0(3) . . ? C18 C25 H25 126.0 . . ? C26 C25 H25 126.0 . . ? N3 C26 C25 111.5(3) . . ? N3 C26 C27 122.6(3) . . ? C25 C26 C27 125.9(3) . . ? C28 C27 C32 118.5(3) . . ? C28 C27 C26 120.0(3) . . ? C32 C27 C26 121.4(3) . . ? C27 C28 C29 120.5(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.1(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 119.7(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C27 120.9(3) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? 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 C6 C1 C2 C3 -1.8(6) . . . . ? C1 C2 C3 C4 2.3(6) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 C6 -1.2(6) . . . . ? C4 C5 C6 C1 1.7(5) . . . . ? C4 C5 C6 C7 -177.3(3) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? C2 C1 C6 C7 178.8(3) . . . . ? C5 C6 C7 N1 22.7(5) . . . . ? C1 C6 C7 N1 -156.3(3) . . . . ? C5 C6 C7 C8 -157.9(3) . . . . ? C1 C6 C7 C8 23.1(5) . . . . ? C8 C7 N1 C16 0.4(4) . . . . ? C6 C7 N1 C16 179.8(3) . . . . ? C8 C7 N1 Co1 -155.9(2) . . . . ? C6 C7 N1 Co1 23.5(5) . . . . ? N3 Co1 N1 C7 32.4(3) 14 . . . ? N3 Co1 N1 C7 167.1(3) . . . . ? N1 Co1 N1 C7 -77.9(3) 14 . . . ? N3 Co1 N1 C16 -121.3(2) 14 . . . ? N3 Co1 N1 C16 13.3(2) . . . . ? N1 Co1 N1 C16 128.4(2) 14 . . . ? N1 C7 C8 C9 -0.1(4) . . . . ? C6 C7 C8 C9 -179.5(3) . . . . ? C7 C8 C9 C16 -0.2(4) . . . . ? C7 C8 C9 C10 178.9(3) . . . . ? C8 C9 C10 C15 -150.9(4) . . . . ? C16 C9 C10 C15 28.0(5) . . . . ? C8 C9 C10 C11 28.0(5) . . . . ? C16 C9 C10 C11 -153.1(3) . . . . ? C15 C10 C11 C12 -0.8(5) . . . . ? C9 C10 C11 C12 -179.7(3) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? C11 C12 C13 C14 -0.4(6) . . . . ? C12 C13 C14 C15 1.1(6) . . . . ? C11 C10 C15 C14 1.5(5) . . . . ? C9 C10 C15 C14 -179.7(3) . . . . ? C13 C14 C15 C10 -1.6(6) . . . . ? C7 N1 C16 N2 177.5(3) . . . . ? Co1 N1 C16 N2 -23.6(4) . . . . ? C7 N1 C16 C9 -0.5(4) . . . . ? Co1 N1 C16 C9 158.4(2) . . . . ? C8 C9 C16 N2 -177.6(3) . . . . ? C10 C9 C16 N2 3.3(6) . . . . ? C8 C9 C16 N1 0.5(4) . . . . ? C10 C9 C16 N1 -178.6(3) . . . . ? N1 C16 N2 C17 12.1(6) . . . . ? C9 C16 N2 C17 -170.2(3) . . . . ? C16 N2 C17 N3 10.7(5) . . . . ? C16 N2 C17 C18 -170.2(3) . . . . ? N2 C17 N3 C26 180.0(3) . . . . ? C18 C17 N3 C26 0.7(4) . . . . ? N2 C17 N3 Co1 -16.4(4) . . . . ? C18 C17 N3 Co1 164.3(2) . . . . ? N3 Co1 N3 C26 -81.7(3) 14 . . . ? N1 Co1 N3 C26 28.3(3) 14 . . . ? N1 Co1 N3 C26 163.3(3) . . . . ? N3 Co1 N3 C17 118.9(3) 14 . . . ? N1 Co1 N3 C17 -131.0(2) 14 . . . ? N1 Co1 N3 C17 4.0(3) . . . . ? N2 C17 C18 C25 178.2(3) . . . . ? N3 C17 C18 C25 -2.5(4) . . . . ? N2 C17 C18 C19 -6.7(6) . . . . ? N3 C17 C18 C19 172.6(3) . . . . ? C25 C18 C19 C24 3.9(5) . . . . ? C17 C18 C19 C24 -170.2(3) . . . . ? C25 C18 C19 C20 -178.6(3) . . . . ? C17 C18 C19 C20 7.3(6) . . . . ? C24 C19 C20 C21 1.5(5) . . . . ? C18 C19 C20 C21 -176.0(3) . . . . ? C19 C20 C21 C22 -0.7(6) . . . . ? C20 C21 C22 C23 -0.1(6) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C22 C23 C24 C19 0.8(6) . . . . ? C20 C19 C24 C23 -1.5(5) . . . . ? C18 C19 C24 C23 176.1(3) . . . . ? C17 C18 C25 C26 3.2(4) . . . . ? C19 C18 C25 C26 -172.0(3) . . . . ? C17 N3 C26 C25 1.4(4) . . . . ? Co1 N3 C26 C25 -160.5(2) . . . . ? C17 N3 C26 C27 -174.7(3) . . . . ? Co1 N3 C26 C27 23.5(5) . . . . ? C18 C25 C26 N3 -3.0(4) . . . . ? C18 C25 C26 C27 172.8(3) . . . . ? N3 C26 C27 C28 -153.3(3) . . . . ? C25 C26 C27 C28 31.2(5) . . . . ? N3 C26 C27 C32 28.7(5) . . . . ? C25 C26 C27 C32 -146.7(4) . . . . ? C32 C27 C28 C29 -0.9(5) . . . . ? C26 C27 C28 C29 -179.0(3) . . . . ? C27 C28 C29 C30 -0.4(6) . . . . ? C28 C29 C30 C31 1.7(6) . . . . ? C29 C30 C31 C32 -1.6(6) . . . . ? C30 C31 C32 C27 0.2(6) . . . . ? C28 C27 C32 C31 1.0(5) . . . . ? C26 C27 C32 C31 179.1(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C15 H15 N2 0.95 2.50 3.043(4) 116 . yes C20 H20 N2 0.95 2.38 3.029(4) 126 . yes C12 H12 Cg1 0.95 2.80 3.548(3) 137 6 yes C31 H31 Cg2 0.95 2.82 3.606(3) 141 9_554 yes # C12 H12 C25 0.95 2.91 3.743(5) 148 6 yes # C12 H12 C26 0.95 2.86 3.750(5) 156 6 yes # C31 H31 C10 0.95 2.92 3.839(5) 163 9_554 yes # C31 H31 C11 0.95 2.86 3.750(5) 156 9_554 yes #========================================================== data_Nickel _database_code_depnum_ccdc_archive 'CCDC 668338' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 599 _chemical_formula_moiety 'C64 H44 N6 Ni' _chemical_formula_sum 'C64 H44 N6 Ni' _chemical_formula_weight 955.76 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F d d 2 ' _symmetry_space_group_name_Hall 'F 2 -2d ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 19.842(3) _cell_length_b 44.333(5) _cell_length_c 10.7588(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9464(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2371 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.75 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3984 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9708 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.16 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.16 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 3176 _reflns_number_gt 2642 _reflns_threshold_expression I>2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+13.731P] 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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 3176 _refine_ls_number_parameters 322 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.401 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.064 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 Ni1 Ni 0.2500 0.2500 0.99889(9) 0.0315(3) Uani 1 2 d S . . C1 C 0.1974(2) 0.15709(10) 1.1816(4) 0.0259(11) Uani 1 1 d . . . H1 H 0.1556 0.1487 1.1559 0.031 Uiso 1 1 calc R . . C2 C 0.2472(2) 0.13829(10) 1.2274(4) 0.0344(12) Uani 1 1 d . . . H2 H 0.2390 0.1173 1.2357 0.041 Uiso 1 1 calc R . . C3 C 0.3089(2) 0.15024(10) 1.2613(5) 0.0345(12) Uani 1 1 d . . . H3 H 0.3438 0.1373 1.2898 0.041 Uiso 1 1 calc R . . C4 C 0.3199(2) 0.18075(10) 1.2540(5) 0.0297(11) Uani 1 1 d . . . H4 H 0.3623 0.1889 1.2781 0.036 Uiso 1 1 calc R . . C5 C 0.2698(2) 0.19970(10) 1.2118(4) 0.0255(11) Uani 1 1 d . . . H5 H 0.2775 0.2208 1.2097 0.031 Uiso 1 1 calc R . . C6 C 0.2079(2) 0.18828(10) 1.1723(4) 0.0206(10) Uani 1 1 d . . . C7 C 0.1544(2) 0.20717(9) 1.1217(4) 0.0209(10) Uani 1 1 d . . . N1 N 0.16534(16) 0.23441(7) 1.0701(3) 0.0201(8) Uani 1 1 d . . . C8 C 0.0842(2) 0.20038(9) 1.1191(4) 0.0213(10) Uani 1 1 d . . . H8 H 0.0638 0.1825 1.1499 0.026 Uiso 1 1 calc R . . C9 C 0.0513(2) 0.22400(9) 1.0649(4) 0.0215(10) Uani 1 1 d . . . C10 C -0.0213(2) 0.22653(9) 1.0399(4) 0.0223(10) Uani 1 1 d . . . C11 C -0.0675(2) 0.21125(10) 1.1157(4) 0.0266(11) Uani 1 1 d . . . H11 H -0.0513 0.1994 1.1831 0.032 Uiso 1 1 calc R . . C12 C -0.1357(2) 0.21301(10) 1.0946(4) 0.0306(12) Uani 1 1 d . . . H12 H -0.1660 0.2022 1.1466 0.037 Uiso 1 1 calc R . . C13 C -0.1602(2) 0.23035(10) 0.9984(5) 0.0325(11) Uani 1 1 d . . . H13 H -0.2074 0.2318 0.9845 0.039 Uiso 1 1 calc R . . C14 C -0.1158(2) 0.24552(10) 0.9227(4) 0.0296(11) Uani 1 1 d . . . H14 H -0.1326 0.2575 0.8564 0.036 Uiso 1 1 calc R . . C15 C -0.0469(2) 0.24356(9) 0.9418(4) 0.0241(11) Uani 1 1 d . . . H15 H -0.0170 0.2539 0.8877 0.029 Uiso 1 1 calc R . . C16 C 0.1033(2) 0.24563(9) 1.0351(4) 0.0192(10) Uani 1 1 d . . . N2 N 0.09058(16) 0.27260(7) 0.9848(3) 0.0187(8) Uani 1 1 d . . . C17 C 0.13694(19) 0.29138(9) 0.9424(4) 0.0169(10) Uani 1 1 d . . . N3 N 0.20501(17) 0.28510(7) 0.9244(3) 0.0205(8) Uani 1 1 d . . . C18 C 0.1236(2) 0.32224(9) 0.9049(4) 0.0211(10) Uani 1 1 d . . . C19 C 0.0583(2) 0.33778(9) 0.8947(4) 0.0202(10) Uani 1 1 d . . . C20 C -0.0027(2) 0.32520(10) 0.9341(4) 0.0266(11) Uani 1 1 d . . . H20 H -0.0026 0.3061 0.9743 0.032 Uiso 1 1 calc R . . C21 C -0.0635(2) 0.34008(10) 0.9156(4) 0.0278(11) Uani 1 1 d . . . H21 H -0.1045 0.3310 0.9416 0.033 Uiso 1 1 calc R . . C22 C -0.0644(2) 0.36826(10) 0.8592(4) 0.0257(11) Uani 1 1 d . . . H22 H -0.1059 0.3785 0.8465 0.031 Uiso 1 1 calc R . . C23 C -0.0051(2) 0.38113(10) 0.8219(4) 0.0286(11) Uani 1 1 d . . . H23 H -0.0055 0.4004 0.7835 0.034 Uiso 1 1 calc R . . C24 C 0.0557(2) 0.36624(10) 0.8397(4) 0.0275(11) Uani 1 1 d . . . H24 H 0.0964 0.3756 0.8140 0.033 Uiso 1 1 calc R . . C25 C 0.1854(2) 0.33353(10) 0.8676(4) 0.0201(10) Uani 1 1 d . . . H25 H 0.1940 0.3535 0.8400 0.024 Uiso 1 1 calc R . . C26 C 0.2333(2) 0.31021(10) 0.8777(4) 0.0231(10) Uani 1 1 d . . . C27 C 0.3033(2) 0.31179(10) 0.8341(4) 0.0214(10) Uani 1 1 d . . . C28 C 0.3381(2) 0.33911(10) 0.8363(4) 0.0255(10) Uani 1 1 d . . . H28 H 0.3167 0.3566 0.8681 0.031 Uiso 1 1 calc R . . C29 C 0.4031(2) 0.34093(10) 0.7930(4) 0.0285(11) Uani 1 1 d . . . H29 H 0.4263 0.3597 0.7958 0.034 Uiso 1 1 calc R . . C30 C 0.4349(2) 0.31577(10) 0.7454(4) 0.0321(11) Uani 1 1 d . . . H30 H 0.4802 0.3171 0.7170 0.038 Uiso 1 1 calc R . . C31 C 0.4010(2) 0.28866(10) 0.7390(4) 0.0300(11) Uani 1 1 d . . . H31 H 0.4222 0.2714 0.7039 0.036 Uiso 1 1 calc R . . C32 C 0.3358(2) 0.28679(10) 0.7840(4) 0.0269(11) Uani 1 1 d . . . H32 H 0.3127 0.2680 0.7807 0.032 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 Ni1 0.0177(4) 0.0169(5) 0.0600(6) 0.000 0.000 0.0003(4) C1 0.028(3) 0.022(3) 0.027(3) -0.001(2) 0.004(2) 0.002(2) C2 0.042(3) 0.028(3) 0.033(3) 0.004(2) 0.011(3) 0.009(2) C3 0.034(3) 0.039(3) 0.031(3) 0.011(2) 0.007(2) 0.018(2) C4 0.028(2) 0.035(3) 0.027(3) 0.002(2) -0.002(2) 0.004(2) C5 0.030(3) 0.023(3) 0.023(3) -0.002(2) -0.001(2) 0.006(2) C6 0.025(3) 0.020(3) 0.016(2) -0.0035(19) 0.003(2) 0.0034(19) C7 0.026(2) 0.024(3) 0.013(2) 0.001(2) -0.0013(19) 0.001(2) N1 0.0211(19) 0.018(2) 0.0206(19) -0.0001(16) 0.0023(16) 0.0000(16) C8 0.023(2) 0.024(3) 0.017(2) 0.003(2) 0.002(2) -0.0028(19) C9 0.024(2) 0.025(3) 0.015(2) 0.000(2) 0.0025(19) 0.003(2) C10 0.020(2) 0.027(3) 0.020(2) -0.005(2) 0.0000(19) 0.0038(19) C11 0.028(3) 0.031(3) 0.020(2) 0.000(2) 0.002(2) 0.002(2) C12 0.028(3) 0.036(3) 0.028(3) 0.003(2) 0.005(2) 0.002(2) C13 0.023(2) 0.039(3) 0.036(3) -0.006(3) -0.004(3) 0.003(2) C14 0.029(3) 0.030(3) 0.030(3) 0.005(2) -0.004(2) -0.004(2) C15 0.024(2) 0.026(3) 0.022(2) 0.003(2) 0.002(2) -0.0023(19) C16 0.019(2) 0.024(3) 0.014(2) -0.002(2) -0.0019(17) 0.0036(19) N2 0.0228(19) 0.020(2) 0.0136(18) 0.0006(17) 0.0024(16) -0.0004(16) C17 0.018(2) 0.020(3) 0.012(2) 0.0007(18) -0.0012(18) 0.0005(19) N3 0.022(2) 0.020(2) 0.0202(19) -0.0032(16) 0.0013(16) 0.0006(16) C18 0.026(2) 0.022(3) 0.015(2) 0.0019(19) 0.000(2) -0.0006(19) C19 0.031(3) 0.016(2) 0.014(2) 0.0009(18) -0.002(2) 0.0022(19) C20 0.034(3) 0.022(3) 0.024(3) -0.003(2) 0.003(2) 0.003(2) C21 0.022(3) 0.029(3) 0.033(3) -0.005(2) 0.000(2) 0.004(2) C22 0.025(3) 0.030(3) 0.022(3) -0.007(2) -0.005(2) 0.013(2) C23 0.039(3) 0.025(3) 0.023(2) 0.004(2) -0.007(2) 0.008(2) C24 0.031(3) 0.029(3) 0.023(3) 0.001(2) -0.001(2) 0.000(2) C25 0.028(3) 0.020(3) 0.013(2) 0.003(2) 0.0011(19) -0.001(2) C26 0.023(3) 0.029(3) 0.017(2) -0.005(2) -0.0024(19) -0.006(2) C27 0.020(2) 0.029(3) 0.015(2) -0.002(2) -0.0031(19) -0.004(2) C28 0.031(3) 0.026(3) 0.019(2) -0.0009(19) 0.000(2) -0.002(2) C29 0.032(3) 0.029(3) 0.025(3) 0.002(2) 0.001(2) -0.011(2) C30 0.023(2) 0.050(3) 0.023(2) 0.004(2) 0.004(2) -0.004(2) C31 0.032(3) 0.034(3) 0.024(3) -0.004(2) 0.008(2) -0.001(2) C32 0.032(3) 0.026(3) 0.022(3) -0.005(2) 0.002(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 1.965(3) 14 ? Ni1 N3 1.965(3) . ? Ni1 N1 1.971(3) 14 ? Ni1 N1 1.971(3) . ? C1 C2 1.383(6) . ? C1 C6 1.402(5) . ? C1 H1 0.9500 . ? C2 C3 1.384(6) . ? C2 H2 0.9500 . ? C3 C4 1.372(6) . ? C3 H3 0.9500 . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(6) . ? C5 H5 0.9500 . ? C6 C7 1.459(6) . ? C7 N1 1.347(5) . ? C7 C8 1.424(6) . ? N1 C16 1.379(5) . ? C8 C9 1.365(6) . ? C8 H8 0.9500 . ? C9 C16 1.445(6) . ? C9 C10 1.469(6) . ? C10 C15 1.394(6) . ? C10 C11 1.401(6) . ? C11 C12 1.374(6) . ? C11 H11 0.9500 . ? C12 C13 1.379(7) . ? C12 H12 0.9500 . ? C13 C14 1.375(6) . ? C13 H13 0.9500 . ? C14 C15 1.385(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.337(5) . ? N2 C17 1.322(5) . ? C17 N3 1.393(5) . ? C17 C18 1.451(6) . ? N3 C26 1.344(5) . ? C18 C25 1.385(6) . ? C18 C19 1.470(6) . ? C19 C24 1.394(6) . ? C19 C20 1.399(6) . ? C20 C21 1.389(6) . ? C20 H20 0.9500 . ? C21 C22 1.389(6) . ? C21 H21 0.9500 . ? C22 C23 1.368(6) . ? C22 H22 0.9500 . ? C23 C24 1.389(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.409(6) . ? C25 H25 0.9500 . ? C26 C27 1.466(6) . ? C27 C32 1.391(6) . ? C27 C28 1.395(6) . ? C28 C29 1.373(6) . ? C28 H28 0.9500 . ? C29 C30 1.380(6) . ? C29 H29 0.9500 . ? C30 C31 1.379(6) . ? C30 H30 0.9500 . ? C31 C32 1.384(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 N3 Ni1 N3 131.8(2) 14 . ? N3 Ni1 N1 92.81(14) 14 14 ? N3 Ni1 N1 105.55(14) . 14 ? N3 Ni1 N1 105.55(14) 14 . ? N3 Ni1 N1 92.81(14) . . ? N1 Ni1 N1 134.3(2) 14 . ? C2 C1 C6 120.9(4) . . ? C2 C1 H1 119.5 . . ? C6 C1 H1 119.5 . . ? C1 C2 C3 119.7(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 117.8(4) . . ? C5 C6 C7 123.2(4) . . ? C1 C6 C7 119.0(4) . . ? N1 C7 C8 109.9(3) . . ? N1 C7 C6 123.4(4) . . ? C8 C7 C6 126.7(4) . . ? C7 N1 C16 106.9(3) . . ? C7 N1 Ni1 127.8(3) . . ? C16 N1 Ni1 121.9(3) . . ? C9 C8 C7 108.3(4) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? C8 C9 C16 105.2(4) . . ? C8 C9 C10 127.3(4) . . ? C16 C9 C10 127.5(4) . . ? C15 C10 C11 117.6(4) . . ? C15 C10 C9 122.5(4) . . ? C11 C10 C9 119.9(4) . . ? C12 C11 C10 121.4(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 120.2(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 120.9(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 120.5(4) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? N2 C16 N1 127.0(4) . . ? N2 C16 C9 123.2(4) . . ? N1 C16 C9 109.7(3) . . ? C17 N2 C16 124.9(3) . . ? N2 C17 N3 126.6(4) . . ? N2 C17 C18 124.2(4) . . ? N3 C17 C18 109.1(3) . . ? C26 N3 C17 107.0(3) . . ? C26 N3 Ni1 128.2(3) . . ? C17 N3 Ni1 122.8(3) . . ? C25 C18 C17 105.0(4) . . ? C25 C18 C19 126.1(4) . . ? C17 C18 C19 128.6(4) . . ? C24 C19 C20 117.2(4) . . ? C24 C19 C18 119.2(4) . . ? C20 C19 C18 123.5(4) . . ? C21 C20 C19 121.2(4) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 120.1(4) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.4(4) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 121.4(4) . . ? C23 C24 H24 119.3 . . ? C19 C24 H24 119.3 . . ? C18 C25 C26 108.1(4) . . ? C18 C25 H25 126.0 . . ? C26 C25 H25 126.0 . . ? N3 C26 C25 110.8(4) . . ? N3 C26 C27 123.7(4) . . ? C25 C26 C27 125.4(4) . . ? C32 C27 C28 117.9(4) . . ? C32 C27 C26 121.7(4) . . ? C28 C27 C26 120.3(4) . . ? C29 C28 C27 120.7(4) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 120.0(4) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 119.4(4) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C31 C32 C27 121.4(4) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.9(7) . . . . ? C1 C2 C3 C4 2.5(7) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 C6 -2.0(7) . . . . ? C4 C5 C6 C1 2.5(6) . . . . ? C4 C5 C6 C7 -177.1(4) . . . . ? C2 C1 C6 C5 -0.5(6) . . . . ? C2 C1 C6 C7 179.1(4) . . . . ? C5 C6 C7 N1 22.9(6) . . . . ? C1 C6 C7 N1 -156.7(4) . . . . ? C5 C6 C7 C8 -156.6(4) . . . . ? C1 C6 C7 C8 23.7(6) . . . . ? C8 C7 N1 C16 0.6(5) . . . . ? C6 C7 N1 C16 -179.0(4) . . . . ? C8 C7 N1 Ni1 -158.4(3) . . . . ? C6 C7 N1 Ni1 22.0(6) . . . . ? N3 Ni1 N1 C7 33.9(4) 14 . . . ? N3 Ni1 N1 C7 168.8(3) . . . . ? N1 Ni1 N1 C7 -76.2(3) 14 . . . ? N3 Ni1 N1 C16 -122.4(3) 14 . . . ? N3 Ni1 N1 C16 12.6(3) . . . . ? N1 Ni1 N1 C16 127.6(3) 14 . . . ? N1 C7 C8 C9 -0.1(5) . . . . ? C6 C7 C8 C9 179.5(4) . . . . ? C7 C8 C9 C16 -0.5(5) . . . . ? C7 C8 C9 C10 178.4(4) . . . . ? C8 C9 C10 C15 -151.3(4) . . . . ? C16 C9 C10 C15 27.4(7) . . . . ? C8 C9 C10 C11 28.2(7) . . . . ? C16 C9 C10 C11 -153.2(4) . . . . ? C15 C10 C11 C12 -0.2(6) . . . . ? C9 C10 C11 C12 -179.7(4) . . . . ? C10 C11 C12 C13 -0.8(7) . . . . ? C11 C12 C13 C14 0.9(7) . . . . ? C12 C13 C14 C15 0.1(7) . . . . ? C13 C14 C15 C10 -1.1(7) . . . . ? C11 C10 C15 C14 1.2(6) . . . . ? C9 C10 C15 C14 -179.4(4) . . . . ? C7 N1 C16 N2 177.1(4) . . . . ? Ni1 N1 C16 N2 -22.4(6) . . . . ? C7 N1 C16 C9 -0.9(5) . . . . ? Ni1 N1 C16 C9 159.6(3) . . . . ? C8 C9 C16 N2 -177.2(4) . . . . ? C10 C9 C16 N2 3.9(7) . . . . ? C8 C9 C16 N1 0.9(5) . . . . ? C10 C9 C16 N1 -178.0(4) . . . . ? N1 C16 N2 C17 11.0(7) . . . . ? C9 C16 N2 C17 -171.2(4) . . . . ? C16 N2 C17 N3 10.5(7) . . . . ? C16 N2 C17 C18 -170.6(4) . . . . ? N2 C17 N3 C26 178.7(4) . . . . ? C18 C17 N3 C26 -0.3(4) . . . . ? N2 C17 N3 Ni1 -16.2(6) . . . . ? C18 C17 N3 Ni1 164.7(3) . . . . ? N3 Ni1 N3 C26 -80.3(3) 14 . . . ? N1 Ni1 N3 C26 28.2(4) 14 . . . ? N1 Ni1 N3 C26 165.8(4) . . . . ? N3 Ni1 N3 C17 118.0(3) 14 . . . ? N1 Ni1 N3 C17 -133.5(3) 14 . . . ? N1 Ni1 N3 C17 4.2(3) . . . . ? N2 C17 C18 C25 179.8(4) . . . . ? N3 C17 C18 C25 -1.1(4) . . . . ? N2 C17 C18 C19 -6.2(7) . . . . ? N3 C17 C18 C19 172.9(4) . . . . ? C25 C18 C19 C24 2.0(7) . . . . ? C17 C18 C19 C24 -170.8(4) . . . . ? C25 C18 C19 C20 -180.0(4) . . . . ? C17 C18 C19 C20 7.2(7) . . . . ? C24 C19 C20 C21 2.0(6) . . . . ? C18 C19 C20 C21 -176.1(4) . . . . ? C19 C20 C21 C22 -1.2(7) . . . . ? C20 C21 C22 C23 0.1(6) . . . . ? C21 C22 C23 C24 0.2(7) . . . . ? C22 C23 C24 C19 0.6(7) . . . . ? C20 C19 C24 C23 -1.6(6) . . . . ? C18 C19 C24 C23 176.5(4) . . . . ? C17 C18 C25 C26 2.1(5) . . . . ? C19 C18 C25 C26 -172.2(4) . . . . ? C17 N3 C26 C25 1.6(5) . . . . ? Ni1 N3 C26 C25 -162.3(3) . . . . ? C17 N3 C26 C27 -173.5(4) . . . . ? Ni1 N3 C26 C27 22.5(6) . . . . ? C18 C25 C26 N3 -2.4(5) . . . . ? C18 C25 C26 C27 172.6(4) . . . . ? N3 C26 C27 C32 30.1(6) . . . . ? C25 C26 C27 C32 -144.3(4) . . . . ? N3 C26 C27 C28 -153.0(4) . . . . ? C25 C26 C27 C28 32.5(6) . . . . ? C32 C27 C28 C29 -1.5(6) . . . . ? C26 C27 C28 C29 -178.5(4) . . . . ? C27 C28 C29 C30 0.6(7) . . . . ? C28 C29 C30 C31 1.2(7) . . . . ? C29 C30 C31 C32 -1.9(7) . . . . ? C30 C31 C32 C27 0.9(7) . . . . ? C28 C27 C32 C31 0.8(6) . . . . ? C26 C27 C32 C31 177.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C15 H15 N2 0.95 2.52 3.053(5) 116 . yes C20 H20 N2 0.95 2.37 3.026(5) 126 . yes C12 H12 Cg1 0.95 2.81 3.548(6) 136 6 yes C31 H31 Cg2 0.95 2.78 3.577(6) 142 9_554 yes # C12 H12 C25 0.95 2.88 3.722(6) 148 6 yes # C12 H12 C26 0.95 2.88 3.754(6) 154 6 yes # C31 H31 C10 0.95 2.89 3.815(6) 166 9_554 yes # C31 H31 C11 0.95 2.84 3.732(6) 157 9_554 yes #============================================================ data_Copper _database_code_depnum_ccdc_archive 'CCDC 668339' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 585 _chemical_formula_moiety 'C64 H44 Cu N6' _chemical_formula_sum 'C64 H44 Cu N6' _chemical_formula_weight 960.59 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 19.8465(18) _cell_length_b 44.707(4) _cell_length_c 10.6333(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9434.6(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4554 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 24.9 _exptl_crystal_description plate _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3992 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14342 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.42 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 4755 _reflns_number_gt 4342 _reflns_threshold_expression I>2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^] 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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack -0.003(11) _refine_ls_number_reflns 4755 _refine_ls_number_parameters 321 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.757 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.062 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 Cu1 Cu 0.2500 0.2500 0.99621(4) 0.01690(12) Uani 1 2 d S . . C1 C 0.19596(14) 0.15744(6) 1.1819(3) 0.0229(6) Uani 1 1 d . . . H1 H 0.1543 0.1492 1.1548 0.027 Uiso 1 1 calc R . . C2 C 0.24535(13) 0.13890(6) 1.2310(3) 0.0307(7) Uani 1 1 d . . . H2 H 0.2370 0.1181 1.2393 0.037 Uiso 1 1 calc R . . C3 C 0.30669(15) 0.15061(6) 1.2681(3) 0.0335(7) Uani 1 1 d . . . H3 H 0.3409 0.1377 1.2993 0.040 Uiso 1 1 calc R . . C4 C 0.31826(13) 0.18105(6) 1.2598(3) 0.0269(6) Uani 1 1 d . . . H4 H 0.3604 0.1891 1.2854 0.032 Uiso 1 1 calc R . . C5 C 0.26816(13) 0.19981(6) 1.2138(2) 0.0225(6) Uani 1 1 d . . . H5 H 0.2756 0.2208 1.2109 0.027 Uiso 1 1 calc R . . C6 C 0.20741(13) 0.18821(5) 1.1723(2) 0.0191(5) Uani 1 1 d . . . C7 C 0.15405(13) 0.20726(5) 1.1191(2) 0.0179(5) Uani 1 1 d . . . N1 N 0.16616(10) 0.23397(4) 1.0661(2) 0.0170(4) Uani 1 1 d . . . C8 C 0.08416(13) 0.20066(5) 1.1190(2) 0.0205(5) Uani 1 1 d . . . H8 H 0.0636 0.1831 1.1513 0.025 Uiso 1 1 calc R . . C9 C 0.05178(13) 0.22440(5) 1.0638(2) 0.0188(5) Uani 1 1 d . . . C10 C -0.02090(13) 0.22741(6) 1.0405(2) 0.0196(5) Uani 1 1 d . . . C11 C -0.06639(13) 0.21266(6) 1.1195(3) 0.0246(6) Uani 1 1 d . . . H11 H -0.0500 0.2012 1.1882 0.029 Uiso 1 1 calc R . . C12 C -0.13493(14) 0.21456(6) 1.0987(3) 0.0290(6) Uani 1 1 d . . . H12 H -0.1652 0.2043 1.1526 0.035 Uiso 1 1 calc R . . C13 C -0.15958(13) 0.23128(6) 1.0002(3) 0.0311(6) Uani 1 1 d . . . H13 H -0.2068 0.2325 0.9862 0.037 Uiso 1 1 calc R . . C14 C -0.11537(15) 0.24627(6) 0.9214(3) 0.0288(6) Uani 1 1 d . . . H14 H -0.1323 0.2581 0.8542 0.035 Uiso 1 1 calc R . . C15 C -0.04640(13) 0.24404(6) 0.9406(3) 0.0238(6) Uani 1 1 d . . . H15 H -0.0163 0.2540 0.8850 0.029 Uiso 1 1 calc R . . C16 C 0.10389(12) 0.24568(5) 1.0318(2) 0.0154(5) Uani 1 1 d . . . N2 N 0.09147(10) 0.27260(4) 0.9859(2) 0.0188(4) Uani 1 1 d . . . C17 C 0.13818(12) 0.29184(5) 0.9467(2) 0.0171(5) Uani 1 1 d . . . N3 N 0.20623(10) 0.28575(4) 0.9303(2) 0.0176(4) Uani 1 1 d . . . C18 C 0.12404(13) 0.32240(5) 0.9086(2) 0.0176(5) Uani 1 1 d . . . C19 C 0.05881(13) 0.33752(5) 0.8983(2) 0.0194(5) Uani 1 1 d . . . C20 C -0.00223(12) 0.32476(6) 0.9361(3) 0.0236(6) Uani 1 1 d . . . H20 H -0.0021 0.3057 0.9752 0.028 Uiso 1 1 calc R . . C21 C -0.06256(14) 0.33938(6) 0.9178(3) 0.0280(6) Uani 1 1 d . . . H21 H -0.1035 0.3302 0.9433 0.034 Uiso 1 1 calc R . . C22 C -0.06375(13) 0.36755(6) 0.8622(3) 0.0260(6) Uani 1 1 d . . . H22 H -0.1054 0.3776 0.8495 0.031 Uiso 1 1 calc R . . C23 C -0.00366(13) 0.38091(6) 0.8253(3) 0.0262(6) Uani 1 1 d . . . H23 H -0.0039 0.4002 0.7879 0.031 Uiso 1 1 calc R . . C24 C 0.05623(13) 0.36591(6) 0.8434(3) 0.0234(6) Uani 1 1 d . . . H24 H 0.0971 0.3752 0.8178 0.028 Uiso 1 1 calc R . . C25 C 0.18579(12) 0.33379(5) 0.8733(2) 0.0196(5) Uani 1 1 d . . . H25 H 0.1943 0.3537 0.8466 0.023 Uiso 1 1 calc R . . C26 C 0.23418(13) 0.31085(5) 0.8835(2) 0.0185(5) Uani 1 1 d . . . C27 C 0.30380(13) 0.31268(5) 0.8384(2) 0.0185(5) Uani 1 1 d . . . C28 C 0.33826(13) 0.33993(6) 0.8433(3) 0.0246(6) Uani 1 1 d . . . H28 H 0.3169 0.3571 0.8778 0.030 Uiso 1 1 calc R . . C29 C 0.40361(14) 0.34199(6) 0.7978(3) 0.0277(6) Uani 1 1 d . . . H29 H 0.4264 0.3607 0.8005 0.033 Uiso 1 1 calc R . . C30 C 0.43563(13) 0.31743(6) 0.7490(3) 0.0305(6) Uani 1 1 d . . . H30 H 0.4809 0.3189 0.7204 0.037 Uiso 1 1 calc R . . C31 C 0.40149(13) 0.29028(6) 0.7414(3) 0.0290(6) Uani 1 1 d . . . H31 H 0.4230 0.2733 0.7059 0.035 Uiso 1 1 calc R . . C32 C 0.33666(13) 0.28815(6) 0.7855(3) 0.0231(6) Uani 1 1 d . . . H32 H 0.3137 0.2696 0.7799 0.028 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 Cu1 0.0154(2) 0.01191(18) 0.0234(2) 0.000 0.000 0.00028(17) C1 0.0258(15) 0.0187(12) 0.0242(14) 0.0010(11) 0.0060(11) 0.0017(10) C2 0.0377(17) 0.0189(13) 0.0356(17) 0.0054(12) 0.0101(13) 0.0082(11) C3 0.0379(17) 0.0307(15) 0.0320(17) 0.0071(13) 0.0018(13) 0.0168(13) C4 0.0240(14) 0.0301(14) 0.0265(15) 0.0040(12) -0.0014(12) 0.0065(10) C5 0.0286(14) 0.0193(12) 0.0197(14) -0.0016(10) -0.0002(11) 0.0024(10) C6 0.0224(14) 0.0158(12) 0.0190(13) 0.0013(10) 0.0042(10) 0.0040(10) C7 0.0211(13) 0.0163(12) 0.0162(13) -0.0029(10) 0.0026(10) -0.0002(10) N1 0.0170(10) 0.0140(10) 0.0201(11) 0.0012(8) 0.0018(8) 0.0001(8) C8 0.0253(14) 0.0171(12) 0.0192(13) 0.0008(10) 0.0010(10) -0.0047(10) C9 0.0193(13) 0.0199(13) 0.0173(13) -0.0001(10) -0.0004(10) -0.0012(10) C10 0.0197(12) 0.0186(12) 0.0205(13) -0.0036(10) -0.0011(10) -0.0010(10) C11 0.0239(14) 0.0261(14) 0.0238(14) 0.0028(11) 0.0006(11) -0.0009(11) C12 0.0223(14) 0.0319(15) 0.0327(17) -0.0006(13) 0.0028(12) -0.0042(11) C13 0.0185(13) 0.0359(15) 0.0390(16) -0.0033(15) -0.0041(13) 0.0008(11) C14 0.0272(16) 0.0296(15) 0.0295(16) 0.0034(12) -0.0092(12) -0.0018(11) C15 0.0230(14) 0.0227(13) 0.0256(14) 0.0013(11) 0.0013(11) -0.0018(10) C16 0.0128(12) 0.0167(12) 0.0168(13) 0.0000(9) 0.0015(9) 0.0004(9) N2 0.0198(11) 0.0166(10) 0.0199(11) 0.0005(9) 0.0001(9) 0.0001(8) C17 0.0188(13) 0.0147(12) 0.0178(12) -0.0025(10) -0.0010(10) 0.0011(9) N3 0.0192(11) 0.0149(10) 0.0187(11) -0.0001(8) -0.0015(9) -0.0004(8) C18 0.0226(13) 0.0159(12) 0.0145(12) 0.0001(9) -0.0020(10) 0.0004(10) C19 0.0242(14) 0.0171(12) 0.0169(13) -0.0029(10) -0.0025(10) 0.0032(10) C20 0.0239(14) 0.0172(12) 0.0296(15) 0.0009(11) 0.0008(11) -0.0007(10) C21 0.0233(15) 0.0268(14) 0.0340(17) -0.0051(12) 0.0003(12) 0.0010(11) C22 0.0243(15) 0.0270(14) 0.0268(15) -0.0069(11) -0.0085(12) 0.0090(11) C23 0.0339(17) 0.0203(14) 0.0243(15) 0.0014(11) -0.0035(12) 0.0069(11) C24 0.0236(14) 0.0220(13) 0.0246(14) 0.0016(11) 0.0017(11) 0.0026(10) C25 0.0234(14) 0.0139(11) 0.0213(13) 0.0007(10) -0.0014(10) -0.0005(10) C26 0.0245(14) 0.0155(12) 0.0155(13) -0.0001(9) -0.0039(10) -0.0031(10) C27 0.0166(13) 0.0202(13) 0.0187(12) 0.0033(10) -0.0011(10) -0.0017(10) C28 0.0301(15) 0.0192(13) 0.0245(14) 0.0011(10) -0.0044(12) -0.0044(11) C29 0.0291(15) 0.0286(15) 0.0253(14) 0.0055(11) -0.0015(11) -0.0103(12) C30 0.0211(13) 0.0411(15) 0.0293(15) 0.0044(14) 0.0015(13) -0.0075(11) C31 0.0265(14) 0.0321(14) 0.0284(15) -0.0003(13) 0.0060(13) 0.0014(11) C32 0.0263(14) 0.0200(12) 0.0231(14) 0.0020(10) 0.0006(11) -0.0037(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 Cu1 N3 1.949(2) . ? Cu1 N3 1.949(2) 14 ? Cu1 N1 1.958(2) 14 ? Cu1 N1 1.958(2) . ? C1 C2 1.386(4) . ? C1 C6 1.398(3) . ? C1 H1 0.9500 . ? C2 C3 1.383(4) . ? C2 H2 0.9500 . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 C7 1.472(3) . ? C7 N1 1.343(3) . ? C7 C8 1.418(4) . ? N1 C16 1.391(3) . ? C8 C9 1.373(4) . ? C8 H8 0.9500 . ? C9 C16 1.446(3) . ? C9 C10 1.470(4) . ? C10 C15 1.392(4) . ? C10 C11 1.398(4) . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 C13 1.377(4) . ? C12 H12 0.9500 . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.322(3) . ? N2 C17 1.332(3) . ? C17 N3 1.389(3) . ? C17 C18 1.452(3) . ? N3 C26 1.347(3) . ? C18 C25 1.379(4) . ? C18 C19 1.464(3) . ? C19 C24 1.398(4) . ? C19 C20 1.398(4) . ? C20 C21 1.378(4) . ? C20 H20 0.9500 . ? C21 C22 1.392(4) . ? C21 H21 0.9500 . ? C22 C23 1.390(4) . ? C22 H22 0.9500 . ? C23 C24 1.378(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.409(3) . ? C25 H25 0.9500 . ? C26 C27 1.465(3) . ? C27 C32 1.394(4) . ? C27 C28 1.398(3) . ? C28 C29 1.387(4) . ? C28 H28 0.9500 . ? C29 C30 1.371(4) . ? C29 H29 0.9500 . ? C30 C31 1.392(4) . ? C30 H30 0.9500 . ? C31 C32 1.373(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 N3 Cu1 N3 137.86(13) . 14 ? N3 Cu1 N1 102.42(8) . 14 ? N3 Cu1 N1 93.31(8) 14 14 ? N3 Cu1 N1 93.31(8) . . ? N3 Cu1 N1 102.42(8) 14 . ? N1 Cu1 N1 135.41(13) 14 . ? C2 C1 C6 120.1(3) . . ? C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.6(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C1 119.1(2) . . ? C5 C6 C7 122.2(2) . . ? C1 C6 C7 118.7(2) . . ? N1 C7 C8 111.1(2) . . ? N1 C7 C6 123.2(2) . . ? C8 C7 C6 125.7(2) . . ? C7 N1 C16 106.61(19) . . ? C7 N1 Cu1 129.58(16) . . ? C16 N1 Cu1 121.20(16) . . ? C9 C8 C7 107.3(2) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? C8 C9 C16 105.9(2) . . ? C8 C9 C10 127.0(2) . . ? C16 C9 C10 127.0(2) . . ? C15 C10 C11 118.4(2) . . ? C15 C10 C9 122.3(2) . . ? C11 C10 C9 119.3(2) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.6(3) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? N2 C16 N1 127.2(2) . . ? N2 C16 C9 123.5(2) . . ? N1 C16 C9 109.0(2) . . ? C16 N2 C17 125.0(2) . . ? N2 C17 N3 126.1(2) . . ? N2 C17 C18 124.1(2) . . ? N3 C17 C18 109.7(2) . . ? C26 N3 C17 106.5(2) . . ? C26 N3 Cu1 129.22(17) . . ? C17 N3 Cu1 123.31(16) . . ? C25 C18 C17 104.6(2) . . ? C25 C18 C19 126.5(2) . . ? C17 C18 C19 128.7(2) . . ? C24 C19 C20 117.3(2) . . ? C24 C19 C18 118.9(2) . . ? C20 C19 C18 123.8(2) . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.3(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.6(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 119.4(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C19 122.1(2) . . ? C23 C24 H24 118.9 . . ? C19 C24 H24 118.9 . . ? C18 C25 C26 108.4(2) . . ? C18 C25 H25 125.8 . . ? C26 C25 H25 125.8 . . ? N3 C26 C25 110.7(2) . . ? N3 C26 C27 123.8(2) . . ? C25 C26 C27 125.2(2) . . ? C32 C27 C28 118.1(2) . . ? C32 C27 C26 121.9(2) . . ? C28 C27 C26 119.9(2) . . ? C29 C28 C27 120.1(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.8(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 121.4(2) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.4(4) . . . . ? C1 C2 C3 C4 1.9(5) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 -2.2(4) . . . . ? C4 C5 C6 C1 2.7(4) . . . . ? C4 C5 C6 C7 -177.9(2) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? C2 C1 C6 C7 179.7(3) . . . . ? C5 C6 C7 N1 24.2(4) . . . . ? C1 C6 C7 N1 -156.4(2) . . . . ? C5 C6 C7 C8 -154.2(3) . . . . ? C1 C6 C7 C8 25.2(4) . . . . ? C8 C7 N1 C16 0.9(3) . . . . ? C6 C7 N1 C16 -177.7(2) . . . . ? C8 C7 N1 Cu1 -160.48(18) . . . . ? C6 C7 N1 Cu1 20.9(4) . . . . ? N3 Cu1 N1 C7 173.0(2) . . . . ? N3 Cu1 N1 C7 32.4(2) 14 . . . ? N1 Cu1 N1 C7 -75.5(2) 14 . . . ? N3 Cu1 N1 C16 14.0(2) . . . . ? N3 Cu1 N1 C16 -126.68(18) 14 . . . ? N1 Cu1 N1 C16 125.41(19) 14 . . . ? N1 C7 C8 C9 -0.2(3) . . . . ? C6 C7 C8 C9 178.4(2) . . . . ? C7 C8 C9 C16 -0.7(3) . . . . ? C7 C8 C9 C10 178.7(2) . . . . ? C8 C9 C10 C15 -150.6(3) . . . . ? C16 C9 C10 C15 28.6(4) . . . . ? C8 C9 C10 C11 28.1(4) . . . . ? C16 C9 C10 C11 -152.7(3) . . . . ? C15 C10 C11 C12 0.0(4) . . . . ? C9 C10 C11 C12 -178.7(2) . . . . ? C10 C11 C12 C13 -0.6(4) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C12 C13 C14 C15 1.0(5) . . . . ? C13 C14 C15 C10 -1.6(4) . . . . ? C11 C10 C15 C14 1.0(4) . . . . ? C9 C10 C15 C14 179.8(2) . . . . ? C7 N1 C16 N2 174.0(2) . . . . ? Cu1 N1 C16 N2 -22.7(3) . . . . ? C7 N1 C16 C9 -1.3(3) . . . . ? Cu1 N1 C16 C9 161.96(17) . . . . ? C8 C9 C16 N2 -174.3(2) . . . . ? C10 C9 C16 N2 6.3(4) . . . . ? C8 C9 C16 N1 1.3(3) . . . . ? C10 C9 C16 N1 -178.1(2) . . . . ? N1 C16 N2 C17 10.6(4) . . . . ? C9 C16 N2 C17 -174.7(2) . . . . ? C16 N2 C17 N3 9.8(4) . . . . ? C16 N2 C17 C18 -173.4(2) . . . . ? N2 C17 N3 C26 176.8(2) . . . . ? C18 C17 N3 C26 -0.4(3) . . . . ? N2 C17 N3 Cu1 -13.8(3) . . . . ? C18 C17 N3 Cu1 169.00(17) . . . . ? N3 Cu1 N3 C26 -78.7(2) 14 . . . ? N1 Cu1 N3 C26 30.7(2) 14 . . . ? N1 Cu1 N3 C26 168.7(2) . . . . ? N3 Cu1 N3 C17 114.47(19) 14 . . . ? N1 Cu1 N3 C17 -136.17(18) 14 . . . ? N1 Cu1 N3 C17 1.83(19) . . . . ? N2 C17 C18 C25 -178.8(2) . . . . ? N3 C17 C18 C25 -1.5(3) . . . . ? N2 C17 C18 C19 -3.7(4) . . . . ? N3 C17 C18 C19 173.5(2) . . . . ? C25 C18 C19 C24 2.5(4) . . . . ? C17 C18 C19 C24 -171.5(2) . . . . ? C25 C18 C19 C20 -179.9(3) . . . . ? C17 C18 C19 C20 6.1(4) . . . . ? C24 C19 C20 C21 1.2(4) . . . . ? C18 C19 C20 C21 -176.4(3) . . . . ? C19 C20 C21 C22 -0.8(4) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? C21 C22 C23 C24 0.6(4) . . . . ? C22 C23 C24 C19 -0.1(4) . . . . ? C20 C19 C24 C23 -0.8(4) . . . . ? C18 C19 C24 C23 177.0(2) . . . . ? C17 C18 C25 C26 2.8(3) . . . . ? C19 C18 C25 C26 -172.4(2) . . . . ? C17 N3 C26 C25 2.2(3) . . . . ? Cu1 N3 C26 C25 -166.38(18) . . . . ? C17 N3 C26 C27 -172.3(2) . . . . ? Cu1 N3 C26 C27 19.1(4) . . . . ? C18 C25 C26 N3 -3.2(3) . . . . ? C18 C25 C26 C27 171.1(2) . . . . ? N3 C26 C27 C32 30.5(4) . . . . ? C25 C26 C27 C32 -143.2(3) . . . . ? N3 C26 C27 C28 -152.1(3) . . . . ? C25 C26 C27 C28 34.2(4) . . . . ? C32 C27 C28 C29 -0.8(4) . . . . ? C26 C27 C28 C29 -178.3(2) . . . . ? C27 C28 C29 C30 -0.8(4) . . . . ? C28 C29 C30 C31 2.0(4) . . . . ? C29 C30 C31 C32 -1.5(5) . . . . ? C30 C31 C32 C27 -0.1(4) . . . . ? C28 C27 C32 C31 1.3(4) . . . . ? C26 C27 C32 C31 178.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C15 H15 N2 0.95 2.53 3.058(3) 115 . yes C20 H20 N2 0.95 2.38 3.029(3) 126 . yes C12 H12 Cg1 0.95 2.80 3.560(3) 138 6 yes C31 H31 Cg2 0.95 2.80 3.602(3) 143 9_554 yes # C12 H12 C25 0.95 2.93 3.771(4) 148.6 6 # C12 H12 C26 0.95 2.89 3.787(4) 157.8 6 # C31 H31 C10 0.95 2.92 3.852(4) 166.4 9_554 # C31 H31 C11 0.95 2.87 3.759(4) 156.3 9_554 #============================================================ data_Zinc _database_code_depnum_ccdc_archive 'CCDC 668340' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 585 _chemical_formula_moiety 'C64 H44 N6 Zn' _chemical_formula_sum 'C64 H44 N6 Zn' _chemical_formula_weight 962.42 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 Orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 19.884(2) _cell_length_b 44.428(4) _cell_length_c 10.7669(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9511.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4791 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.9 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4000 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18019 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.82 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.82 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 4094 _reflns_number_gt 3844 _reflns_threshold_expression I>2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+4.4312P] 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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 4094 _refine_ls_number_parameters 322 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.493 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.054 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 0.2500 0.2500 0.99756(4) 0.01667(11) Uani 1 2 d S . . C1 C 0.19717(14) 0.15699(6) 1.1832(3) 0.0243(6) Uani 1 1 d . . . H1 H 0.1551 0.1488 1.1582 0.029 Uiso 1 1 calc R . . C2 C 0.24696(14) 0.13811(6) 1.2269(3) 0.0326(7) Uani 1 1 d . . . H2 H 0.2390 0.1171 1.2328 0.039 Uiso 1 1 calc R . . C3 C 0.30865(15) 0.14996(6) 1.2620(3) 0.0323(7) Uani 1 1 d . . . H3 H 0.3433 0.1369 1.2902 0.039 Uiso 1 1 calc R . . C4 C 0.31976(14) 0.18045(6) 1.2563(3) 0.0288(6) Uani 1 1 d . . . H4 H 0.3619 0.1885 1.2812 0.035 Uiso 1 1 calc R . . C5 C 0.26934(14) 0.19942(6) 1.2142(3) 0.0239(6) Uani 1 1 d . . . H5 H 0.2769 0.2205 1.2120 0.029 Uiso 1 1 calc R . . C6 C 0.20800(13) 0.18795(6) 1.1752(2) 0.0190(6) Uani 1 1 d . . . C7 C 0.15416(13) 0.20739(5) 1.1257(2) 0.0182(6) Uani 1 1 d . . . N1 N 0.16628(10) 0.23439(5) 1.0761(2) 0.0170(5) Uani 1 1 d . . . C8 C 0.08455(13) 0.20049(6) 1.1218(2) 0.0215(6) Uani 1 1 d . . . H8 H 0.0640 0.1826 1.1517 0.026 Uiso 1 1 calc R . . C9 C 0.05247(13) 0.22432(6) 1.0672(2) 0.0197(6) Uani 1 1 d . . . C10 C -0.02013(13) 0.22709(6) 1.0418(2) 0.0201(6) Uani 1 1 d . . . C11 C -0.06603(14) 0.21195(6) 1.1171(3) 0.0257(6) Uani 1 1 d . . . H11 H -0.0502 0.2002 1.1847 0.031 Uiso 1 1 calc R . . C12 C -0.13419(14) 0.21385(7) 1.0948(3) 0.0285(7) Uani 1 1 d . . . H12 H -0.1648 0.2033 1.1467 0.034 Uiso 1 1 calc R . . C13 C -0.15815(13) 0.23095(6) 0.9974(3) 0.0309(7) Uani 1 1 d . . . H13 H -0.2052 0.2324 0.9828 0.037 Uiso 1 1 calc R . . C14 C -0.11349(15) 0.24598(7) 0.9211(3) 0.0298(7) Uani 1 1 d . . . H14 H -0.1299 0.2578 0.8540 0.036 Uiso 1 1 calc R . . C15 C -0.04470(13) 0.24393(6) 0.9421(3) 0.0238(6) Uani 1 1 d . . . H15 H -0.0142 0.2540 0.8884 0.029 Uiso 1 1 calc R . . C16 C 0.10443(13) 0.24577(6) 1.0378(2) 0.0169(6) Uani 1 1 d . . . N2 N 0.09243(10) 0.27243(4) 0.9859(2) 0.0191(5) Uani 1 1 d . . . C17 C 0.13782(12) 0.29143(6) 0.9410(2) 0.0168(6) Uani 1 1 d . . . N3 N 0.20554(10) 0.28522(5) 0.9198(2) 0.0175(5) Uani 1 1 d . . . C18 C 0.12338(13) 0.32203(6) 0.9033(2) 0.0189(6) Uani 1 1 d . . . C19 C 0.05806(13) 0.33738(6) 0.8951(2) 0.0201(6) Uani 1 1 d . . . C20 C -0.00204(13) 0.32480(6) 0.9367(3) 0.0252(6) Uani 1 1 d . . . H20 H -0.0013 0.3059 0.9779 0.030 Uiso 1 1 calc R . . C21 C -0.06280(14) 0.33933(6) 0.9192(3) 0.0289(7) Uani 1 1 d . . . H21 H -0.1033 0.3302 0.9469 0.035 Uiso 1 1 calc R . . C22 C -0.06499(14) 0.36717(6) 0.8617(3) 0.0278(7) Uani 1 1 d . . . H22 H -0.1068 0.3771 0.8498 0.033 Uiso 1 1 calc R . . C23 C -0.00589(14) 0.38031(6) 0.8217(3) 0.0284(7) Uani 1 1 d . . . H23 H -0.0068 0.3995 0.7826 0.034 Uiso 1 1 calc R . . C24 C 0.05446(14) 0.36557(6) 0.8385(3) 0.0262(6) Uani 1 1 d . . . H24 H 0.0948 0.3749 0.8108 0.031 Uiso 1 1 calc R . . C25 C 0.18471(13) 0.33363(6) 0.8665(3) 0.0198(6) Uani 1 1 d . . . H25 H 0.1929 0.3537 0.8405 0.024 Uiso 1 1 calc R . . C26 C 0.23298(13) 0.31045(6) 0.8744(2) 0.0179(6) Uani 1 1 d . . . C27 C 0.30304(13) 0.31227(6) 0.8313(2) 0.0189(6) Uani 1 1 d . . . C28 C 0.33695(13) 0.33971(6) 0.8339(3) 0.0251(6) Uani 1 1 d . . . H28 H 0.3148 0.3571 0.8647 0.030 Uiso 1 1 calc R . . C29 C 0.40244(14) 0.34177(7) 0.7922(3) 0.0286(7) Uani 1 1 d . . . H29 H 0.4250 0.3606 0.7939 0.034 Uiso 1 1 calc R . . C30 C 0.43534(13) 0.31661(7) 0.7480(3) 0.0303(6) Uani 1 1 d . . . H30 H 0.4808 0.3180 0.7217 0.036 Uiso 1 1 calc R . . C31 C 0.40172(13) 0.28930(6) 0.7422(3) 0.0290(6) Uani 1 1 d . . . H31 H 0.4237 0.2720 0.7097 0.035 Uiso 1 1 calc R . . C32 C 0.33612(13) 0.28727(6) 0.7839(2) 0.0236(6) Uani 1 1 d . . . H32 H 0.3134 0.2685 0.7800 0.028 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 Zn1 0.0147(2) 0.0167(2) 0.0187(2) 0.000 0.000 0.00038(19) C1 0.0257(16) 0.0223(15) 0.0248(15) 0.0028(13) 0.0069(12) -0.0009(12) C2 0.0391(18) 0.0204(15) 0.0383(19) 0.0039(13) 0.0106(14) 0.0088(12) C3 0.0336(17) 0.0323(17) 0.0311(17) 0.0070(14) 0.0041(14) 0.0157(13) C4 0.0254(15) 0.0355(16) 0.0256(15) 0.0018(14) -0.0021(14) 0.0034(12) C5 0.0251(15) 0.0225(14) 0.0242(16) 0.0030(11) 0.0003(12) 0.0011(12) C6 0.0207(14) 0.0214(14) 0.0151(14) -0.0005(12) 0.0020(11) 0.0006(11) C7 0.0216(14) 0.0183(13) 0.0147(13) -0.0049(11) 0.0021(11) -0.0007(11) N1 0.0167(11) 0.0169(11) 0.0174(12) 0.0014(9) 0.0014(9) -0.0014(9) C8 0.0243(15) 0.0209(14) 0.0193(14) 0.0015(12) 0.0022(11) -0.0050(11) C9 0.0199(14) 0.0217(15) 0.0177(14) 0.0009(12) 0.0003(11) 0.0023(11) C10 0.0167(13) 0.0216(14) 0.0221(14) -0.0028(11) 0.0007(11) -0.0012(11) C11 0.0258(15) 0.0281(16) 0.0233(15) 0.0010(13) 0.0015(12) -0.0003(12) C12 0.0226(15) 0.0349(17) 0.0279(16) -0.0012(14) 0.0039(12) -0.0048(13) C13 0.0191(14) 0.0389(16) 0.0346(16) -0.0034(16) -0.0028(14) -0.0003(12) C14 0.0268(16) 0.0325(17) 0.0302(17) 0.0043(14) -0.0071(13) -0.0019(13) C15 0.0207(15) 0.0269(15) 0.0238(14) 0.0037(12) 0.0009(12) -0.0011(11) C16 0.0147(13) 0.0201(15) 0.0159(13) -0.0018(11) 0.0016(9) 0.0003(10) N2 0.0186(11) 0.0214(11) 0.0172(12) -0.0026(10) -0.0002(10) 0.0001(9) C17 0.0165(14) 0.0184(14) 0.0156(13) -0.0047(11) -0.0001(11) 0.0000(11) N3 0.0162(11) 0.0187(12) 0.0176(11) -0.0007(9) -0.0021(9) 0.0012(9) C18 0.0226(14) 0.0186(14) 0.0154(13) -0.0012(11) -0.0023(11) -0.0003(11) C19 0.0234(15) 0.0207(14) 0.0164(14) -0.0034(11) -0.0031(11) 0.0014(11) C20 0.0270(16) 0.0188(14) 0.0298(16) -0.0007(12) 0.0049(13) 0.0040(12) C21 0.0230(16) 0.0289(16) 0.0348(17) -0.0073(14) 0.0018(13) 0.0001(12) C22 0.0262(16) 0.0306(16) 0.0267(16) -0.0083(13) -0.0061(13) 0.0106(13) C23 0.0359(18) 0.0240(16) 0.0253(16) 0.0009(13) -0.0034(13) 0.0085(12) C24 0.0251(15) 0.0264(16) 0.0271(16) 0.0024(13) -0.0010(12) 0.0028(12) C25 0.0254(15) 0.0147(13) 0.0192(14) 0.0015(11) -0.0013(12) -0.0003(11) C26 0.0223(14) 0.0180(13) 0.0135(13) 0.0002(11) -0.0025(11) -0.0040(11) C27 0.0165(13) 0.0238(15) 0.0165(13) 0.0027(11) -0.0016(11) -0.0016(11) C28 0.0287(15) 0.0239(15) 0.0229(15) -0.0001(12) 0.0009(13) -0.0036(12) C29 0.0256(15) 0.0346(17) 0.0255(15) 0.0047(13) -0.0021(12) -0.0125(13) C30 0.0183(14) 0.0449(17) 0.0277(15) 0.0030(15) 0.0025(13) -0.0034(12) C31 0.0260(14) 0.0326(15) 0.0284(15) -0.0013(14) 0.0087(14) 0.0024(12) C32 0.0253(15) 0.0222(14) 0.0234(16) 0.0010(11) 0.0003(11) -0.0042(12) _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 N3 1.982(2) 14 ? Zn1 N3 1.982(2) . ? Zn1 N1 1.992(2) 14 ? Zn1 N1 1.992(2) . ? C1 C2 1.380(4) . ? C1 C6 1.395(4) . ? C1 H1 0.9500 . ? C2 C3 1.388(4) . ? C2 H2 0.9500 . ? C3 C4 1.374(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 H5 0.9500 . ? C6 C7 1.476(4) . ? C7 N1 1.335(3) . ? C7 C8 1.418(4) . ? N1 C16 1.392(3) . ? C8 C9 1.369(4) . ? C8 H8 0.9500 . ? C9 C16 1.441(4) . ? C9 C10 1.475(4) . ? C10 C11 1.394(4) . ? C10 C15 1.397(4) . ? C11 C12 1.379(4) . ? C11 H11 0.9500 . ? C12 C13 1.379(4) . ? C12 H12 0.9500 . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 N2 1.332(3) . ? N2 C17 1.327(3) . ? C17 N3 1.393(3) . ? C17 C18 1.447(4) . ? N3 C26 1.339(3) . ? C18 C25 1.382(4) . ? C18 C19 1.470(4) . ? C19 C20 1.393(4) . ? C19 C24 1.395(4) . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.384(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.379(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.410(4) . ? C25 H25 0.9500 . ? C26 C27 1.471(4) . ? C27 C32 1.388(4) . ? C27 C28 1.394(4) . ? C28 C29 1.381(4) . ? C28 H28 0.9500 . ? C29 C30 1.380(4) . ? C29 H29 0.9500 . ? C30 C31 1.387(4) . ? C30 H30 0.9500 . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 N3 Zn1 N3 130.07(12) 14 . ? N3 Zn1 N1 94.66(8) 14 14 ? N3 Zn1 N1 106.08(8) . 14 ? N3 Zn1 N1 106.08(8) 14 . ? N3 Zn1 N1 94.66(8) . . ? N1 Zn1 N1 129.76(12) 14 . ? C2 C1 C6 120.6(3) . . ? C2 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? C1 C2 C3 119.8(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 120.8(3) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 118.7(2) . . ? C5 C6 C7 122.1(2) . . ? C1 C6 C7 119.2(2) . . ? N1 C7 C8 111.0(2) . . ? N1 C7 C6 122.7(2) . . ? C8 C7 C6 126.3(2) . . ? C7 N1 C16 106.6(2) . . ? C7 N1 Zn1 129.32(17) . . ? C16 N1 Zn1 119.09(16) . . ? C9 C8 C7 107.5(2) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? C8 C9 C16 105.8(2) . . ? C8 C9 C10 126.9(2) . . ? C16 C9 C10 127.3(2) . . ? C11 C10 C15 118.5(2) . . ? C11 C10 C9 119.5(2) . . ? C15 C10 C9 122.0(2) . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 120.3(3) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? N2 C16 N1 127.3(2) . . ? N2 C16 C9 123.5(2) . . ? N1 C16 C9 109.2(2) . . ? C17 N2 C16 126.7(2) . . ? N2 C17 N3 126.2(2) . . ? N2 C17 C18 124.4(2) . . ? N3 C17 C18 109.4(2) . . ? C26 N3 C17 106.7(2) . . ? C26 N3 Zn1 129.29(18) . . ? C17 N3 Zn1 121.22(16) . . ? C25 C18 C17 104.8(2) . . ? C25 C18 C19 126.1(2) . . ? C17 C18 C19 128.9(2) . . ? C20 C19 C24 117.2(2) . . ? C20 C19 C18 123.5(2) . . ? C24 C19 C18 119.2(2) . . ? C21 C20 C19 121.2(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C23 C22 C21 119.4(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C19 121.9(3) . . ? C23 C24 H24 119.0 . . ? C19 C24 H24 119.0 . . ? C18 C25 C26 108.1(2) . . ? C18 C25 H25 125.9 . . ? C26 C25 H25 125.9 . . ? N3 C26 C25 110.9(2) . . ? N3 C26 C27 123.2(2) . . ? C25 C26 C27 125.8(2) . . ? C32 C27 C28 118.6(2) . . ? C32 C27 C26 121.4(2) . . ? C28 C27 C26 120.0(2) . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 120.4(3) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 119.7(2) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 121.0(3) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? 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 C2 C3 -0.7(4) . . . . ? C1 C2 C3 C4 1.6(5) . . . . ? C2 C3 C4 C5 -0.6(5) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C4 C5 C6 C1 2.1(4) . . . . ? C4 C5 C6 C7 -177.8(3) . . . . ? C2 C1 C6 C5 -1.1(4) . . . . ? C2 C1 C6 C7 178.8(3) . . . . ? C5 C6 C7 N1 23.2(4) . . . . ? C1 C6 C7 N1 -156.7(3) . . . . ? C5 C6 C7 C8 -157.7(3) . . . . ? C1 C6 C7 C8 22.4(4) . . . . ? C8 C7 N1 C16 -0.3(3) . . . . ? C6 C7 N1 C16 178.9(2) . . . . ? C8 C7 N1 Zn1 -154.39(18) . . . . ? C6 C7 N1 Zn1 24.8(4) . . . . ? N3 Zn1 N1 C7 31.3(2) 14 . . . ? N3 Zn1 N1 C7 165.4(2) . . . . ? N1 Zn1 N1 C7 -79.2(2) 14 . . . ? N3 Zn1 N1 C16 -120.08(18) 14 . . . ? N3 Zn1 N1 C16 13.99(19) . . . . ? N1 Zn1 N1 C16 129.43(19) 14 . . . ? N1 C7 C8 C9 0.1(3) . . . . ? C6 C7 C8 C9 -179.1(2) . . . . ? C7 C8 C9 C16 0.2(3) . . . . ? C7 C8 C9 C10 179.1(2) . . . . ? C8 C9 C10 C11 28.1(4) . . . . ? C16 C9 C10 C11 -153.2(3) . . . . ? C8 C9 C10 C15 -150.4(3) . . . . ? C16 C9 C10 C15 28.4(4) . . . . ? C15 C10 C11 C12 -0.8(4) . . . . ? C9 C10 C11 C12 -179.3(3) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C12 C13 C14 C15 0.0(5) . . . . ? C13 C14 C15 C10 -1.1(4) . . . . ? C11 C10 C15 C14 1.5(4) . . . . ? C9 C10 C15 C14 179.9(3) . . . . ? C7 N1 C16 N2 178.3(2) . . . . ? Zn1 N1 C16 N2 -24.5(3) . . . . ? C7 N1 C16 C9 0.4(3) . . . . ? Zn1 N1 C16 C9 157.63(17) . . . . ? C8 C9 C16 N2 -178.3(2) . . . . ? C10 C9 C16 N2 2.7(4) . . . . ? C8 C9 C16 N1 -0.3(3) . . . . ? C10 C9 C16 N1 -179.3(2) . . . . ? N1 C16 N2 C17 12.3(4) . . . . ? C9 C16 N2 C17 -170.1(2) . . . . ? C16 N2 C17 N3 11.8(4) . . . . ? C16 N2 C17 C18 -169.9(3) . . . . ? N2 C17 N3 C26 180.0(3) . . . . ? C18 C17 N3 C26 1.4(3) . . . . ? N2 C17 N3 Zn1 -17.3(3) . . . . ? C18 C17 N3 Zn1 164.17(17) . . . . ? N3 Zn1 N3 C26 -82.0(2) 14 . . . ? N1 Zn1 N3 C26 28.7(2) 14 . . . ? N1 Zn1 N3 C26 162.4(2) . . . . ? N3 Zn1 N3 C17 119.56(19) 14 . . . ? N1 Zn1 N3 C17 -129.76(19) 14 . . . ? N1 Zn1 N3 C17 3.98(19) . . . . ? N2 C17 C18 C25 178.3(2) . . . . ? N3 C17 C18 C25 -3.1(3) . . . . ? N2 C17 C18 C19 -6.1(4) . . . . ? N3 C17 C18 C19 172.5(2) . . . . ? C25 C18 C19 C20 -178.3(3) . . . . ? C17 C18 C19 C20 7.0(4) . . . . ? C25 C18 C19 C24 4.4(4) . . . . ? C17 C18 C19 C24 -170.3(3) . . . . ? C24 C19 C20 C21 1.8(4) . . . . ? C18 C19 C20 C21 -175.6(3) . . . . ? C19 C20 C21 C22 -1.3(4) . . . . ? C20 C21 C22 C23 0.1(4) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C22 C23 C24 C19 0.2(5) . . . . ? C20 C19 C24 C23 -1.3(4) . . . . ? C18 C19 C24 C23 176.2(3) . . . . ? C17 C18 C25 C26 3.5(3) . . . . ? C19 C18 C25 C26 -172.2(2) . . . . ? C17 N3 C26 C25 0.8(3) . . . . ? Zn1 N3 C26 C25 -160.04(18) . . . . ? C17 N3 C26 C27 -175.2(2) . . . . ? Zn1 N3 C26 C27 23.9(4) . . . . ? C18 C25 C26 N3 -2.9(3) . . . . ? C18 C25 C26 C27 173.1(2) . . . . ? N3 C26 C27 C32 28.6(4) . . . . ? C25 C26 C27 C32 -146.9(3) . . . . ? N3 C26 C27 C28 -153.5(3) . . . . ? C25 C26 C27 C28 31.1(4) . . . . ? C32 C27 C28 C29 -1.1(4) . . . . ? C26 C27 C28 C29 -179.1(2) . . . . ? C27 C28 C29 C30 -0.4(4) . . . . ? C28 C29 C30 C31 1.9(5) . . . . ? C29 C30 C31 C32 -1.8(5) . . . . ? C30 C31 C32 C27 0.2(4) . . . . ? C28 C27 C32 C31 1.2(4) . . . . ? C26 C27 C32 C31 179.2(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # # Hydrogen bonding scheme # ======== ======= ====== # # D H A D-H H...A D...A D-H...A symm publ # - - - --- ----- ----- ------- ---- ---- C15 H15 N2 0.95 2.50 3.043(3) 116 . yes C20 H20 N2 0.95 2.38 3.037(3) 126 . yes C12 H12 Cg1 0.95 2.80 3.547(3) 136 6 yes C31 H31 Cg2 0.95 2.82 3.604(3) 141 9_554 yes # C12 H12 C25 0.95 2.91 3.745(4) 147.6 6 # C12 H12 C26 0.95 2.87 3.754(4) 155.7 6 # C31 H31 C10 0.95 2.92 3.836(4) 163.3 9_554 # C31 H31 C11 0.95 2.86 3.746(4) 156.4 9_554 #====================================================================== # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];,./ #====================================================================== # END of CIF #======================================================================