# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christopher Ziegler' _publ_contact_author_email ZIEGLER@UAKRON.EDU _publ_section_title ; Zinc complexes of the carbahemiporphyrazines ; loop_ _publ_author_name 'Christopher Ziegler' 'Emily S. Bonner' 'James T. Engle' 'Saovalak Sripothongak' data_Zn1 _database_code_depnum_ccdc_archive 'CCDC 750084' #TrackingRef 'Zn1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H31 N9 Zn' _chemical_formula_weight 739.14 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.659(3) _cell_length_b 12.527(2) _cell_length_c 17.482(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.489(3) _cell_angle_gamma 90.00 _cell_volume 3394.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5057 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.61 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8364 _exptl_absorpt_correction_T_max 0.9698 _exptl_absorpt_process_details 'SADABS; Sheldrick, 2004 [Sheldrick, G. M. (2004)]' _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.263777 ; _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27460 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7363 _reflns_number_gt 4890 _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. Hydrogen atoms were assigned ideal positions and refined isotropically as riding atoms. ; _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^)+(0.1299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7363 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2159 _refine_ls_wR_factor_gt 0.1919 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.007 _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 0.9733(2) 0.3286(3) 0.7765(2) 0.0380(8) Uani 1 1 d . . . C2 C 1.0341(2) 0.4160(3) 0.7809(2) 0.0390(8) Uani 1 1 d . . . C3 C 1.0306(2) 0.5238(3) 0.7924(2) 0.0421(8) Uani 1 1 d . . . H3 H 0.9826 0.5553 0.8008 0.051 Uiso 1 1 calc R . . C4 C 1.0993(3) 0.5855(3) 0.7913(3) 0.0482(9) Uani 1 1 d . . . H4 H 1.0979 0.6606 0.7984 0.058 Uiso 1 1 calc R . . C5 C 1.1701(3) 0.5395(3) 0.7800(3) 0.0525(10) Uani 1 1 d . . . H5 H 1.2168 0.5836 0.7807 0.063 Uiso 1 1 calc R . . C6 C 1.1741(3) 0.4312(3) 0.7678(3) 0.0516(10) Uani 1 1 d . . . H6 H 1.2222 0.3999 0.7596 0.062 Uiso 1 1 calc R . . C7 C 1.1047(2) 0.3696(3) 0.7679(2) 0.0425(8) Uani 1 1 d . . . C8 C 1.0859(2) 0.2542(3) 0.7535(2) 0.0437(8) Uani 1 1 d . . . C9 C 1.1096(2) 0.0855(3) 0.7140(3) 0.0484(10) Uani 1 1 d . . . C10 C 1.0909(3) 0.0417(4) 0.6358(3) 0.0635(12) Uani 1 1 d . . . H10 H 1.0940 0.0849 0.5923 0.076 Uiso 1 1 calc R . . C11 C 1.0681(4) -0.0637(4) 0.6220(3) 0.0750(15) Uani 1 1 d . . . H11 H 1.0567 -0.0929 0.5689 0.090 Uiso 1 1 calc R . . C12 C 1.0612(3) -0.1287(4) 0.6832(3) 0.0712(14) Uani 1 1 d . . . H12 H 1.0459 -0.2018 0.6724 0.085 Uiso 1 1 calc R . . C13 C 1.0771(3) -0.0856(3) 0.7611(3) 0.0579(12) Uani 1 1 d . . . C14 C 1.1037(3) 0.0208(3) 0.7762(3) 0.0541(11) Uani 1 1 d . . . H14 H 1.1180 0.0493 0.8299 0.065 Uiso 1 1 calc R . . C15 C 1.0182(3) -0.1232(3) 0.8582(3) 0.0583(12) Uani 1 1 d . . . C16 C 1.0026(3) -0.1909(3) 0.9211(3) 0.0657(14) Uani 1 1 d . . . C17 C 1.0365(4) -0.2881(3) 0.9539(3) 0.0730(15) Uani 1 1 d . . . H17 H 1.0820 -0.3193 0.9410 0.088 Uiso 1 1 calc R . . C18 C 1.0041(4) -0.3388(4) 1.0053(3) 0.088(2) Uani 1 1 d . . . H18 H 1.0268 -0.4060 1.0284 0.106 Uiso 1 1 calc R . . C19 C 0.9372(4) -0.2919(4) 1.0241(3) 0.0796(18) Uani 1 1 d . . . H19 H 0.9149 -0.3282 1.0597 0.095 Uiso 1 1 calc R . . C20 C 0.9025(3) -0.1929(4) 0.9915(3) 0.0674(14) Uani 1 1 d . . . H20 H 0.8577 -0.1605 1.0048 0.081 Uiso 1 1 calc R . . C21 C 0.9366(3) -0.1445(3) 0.9391(2) 0.0587(12) Uani 1 1 d . . . C22 C 0.9094(3) -0.0470(3) 0.8874(2) 0.0555(11) Uani 1 1 d . . . C23 C 0.8143(3) 0.0894(3) 0.8251(2) 0.0469(9) Uani 1 1 d . . . C24 C 0.7325(3) 0.0878(3) 0.7632(3) 0.0555(11) Uani 1 1 d . . . H24 H 0.6946 0.0295 0.7590 0.067 Uiso 1 1 calc R . . C25 C 0.7070(2) 0.1714(3) 0.7082(3) 0.0529(10) Uani 1 1 d . . . H25 H 0.6514 0.1699 0.6660 0.063 Uiso 1 1 calc R . . C26 C 0.7612(2) 0.2584(3) 0.7131(2) 0.0453(9) Uani 1 1 d . . . H26 H 0.7425 0.3153 0.6747 0.054 Uiso 1 1 calc R . . C27 C 0.8428(2) 0.2610(3) 0.7747(2) 0.0380(8) Uani 1 1 d . . . C28 C 0.8684(2) 0.1768(3) 0.8320(2) 0.0415(8) Uani 1 1 d . . . H28 H 0.9229 0.1796 0.8758 0.050 Uiso 1 1 calc R . . C29 C 0.8571(3) 0.1086(4) 0.5898(3) 0.0658(12) Uani 1 1 d . . . H29 H 0.8926 0.1695 0.5950 0.079 Uiso 1 1 calc R . . C30 C 0.7923(4) 0.0889(5) 0.5138(3) 0.0784(16) Uani 1 1 d . . . H30 H 0.7835 0.1342 0.4678 0.094 Uiso 1 1 calc R . . C31 C 0.7419(4) 0.0009(6) 0.5090(4) 0.099(2) Uani 1 1 d . . . H31 H 0.6968 -0.0154 0.4583 0.118 Uiso 1 1 calc R . . C32 C 0.7548(4) -0.0633(6) 0.5745(4) 0.107(2) Uani 1 1 d . . . H32 H 0.7193 -0.1238 0.5708 0.129 Uiso 1 1 calc R . . C33 C 0.8208(3) -0.0382(4) 0.6465(3) 0.0845(17) Uani 1 1 d . . . H33 H 0.8310 -0.0836 0.6926 0.101 Uiso 1 1 calc R . . C34 C 0.6965(5) 0.9106(6) -0.0331(4) 0.116(3) Uani 1 1 d . . . H34 H 0.7316 0.9263 -0.0639 0.139 Uiso 1 1 calc R . . C35 C 0.6109(6) 0.9269(8) -0.0690(5) 0.146(4) Uani 1 1 d . . . H35 H 0.5862 0.9551 -0.1231 0.175 Uiso 1 1 calc R . . C36 C 0.5573(5) 0.8997(7) -0.0219(6) 0.142(3) Uani 1 1 d . . . H36 H 0.4963 0.9061 -0.0456 0.171 Uiso 1 1 calc R . . C37 C 0.5971(5) 0.8648(8) 0.0570(6) 0.149(4) Uani 1 1 d . . . H37 H 0.5643 0.8508 0.0904 0.178 Uiso 1 1 calc R . . C38 C 0.6840(4) 0.8501(6) 0.0875(4) 0.0948(18) Uani 1 1 d . . . H38 H 0.7102 0.8225 0.1416 0.114 Uiso 1 1 calc R . . N1 N 0.89862(18) 0.3478(2) 0.78037(17) 0.0381(7) Uani 1 1 d . . . N2 N 1.00819(18) 0.2316(2) 0.76390(18) 0.0399(7) Uani 1 1 d . . . N3 N 1.1336(2) 0.1925(3) 0.7300(2) 0.0515(8) Uani 1 1 d . . . N4 N 1.0690(3) -0.1517(3) 0.8223(2) 0.0643(11) Uani 1 1 d . . . N5 N 0.9633(2) -0.0342(3) 0.8434(2) 0.0508(8) Uani 1 1 d . . . N6 N 0.8400(2) 0.0056(3) 0.8818(2) 0.0536(9) Uani 1 1 d . . . N7 N 0.8720(2) 0.0477(3) 0.6549(2) 0.0536(9) Uani 1 1 d . . . N8 N 0.7353(4) 0.8731(5) 0.0445(3) 0.1034(17) Uani 1 1 d . . . Zn1 Zn 0.96021(3) 0.08677(3) 0.76739(3) 0.04437(19) Uani 1 1 d . . . N9 N 0.3902(12) 0.7901(10) 0.0869(8) 0.250(7) Uani 1 1 d . . . C39 C 0.3098(10) 0.8192(14) 0.0753(9) 0.278(12) Uani 1 1 d . . . H39 H 0.2938 0.8255 0.1219 0.333 Uiso 1 1 calc R . . C40 C 0.2553(9) 0.8384(11) 0.0071(9) 0.190(5) Uani 1 1 d . . . H40 H 0.1992 0.8618 0.0016 0.228 Uiso 1 1 calc R . . C41 C 0.2757(6) 0.8259(7) -0.0583(6) 0.135(3) Uani 1 1 d . . . H41 H 0.2352 0.8443 -0.1110 0.162 Uiso 1 1 calc R . . C42 C 0.3520(10) 0.7881(10) -0.0514(8) 0.204(6) Uani 1 1 d . . . H42 H 0.3657 0.7744 -0.0987 0.245 Uiso 1 1 calc R . . C43 C 0.4128(8) 0.7687(12) 0.0290(10) 0.205(7) Uani 1 1 d . . . H43 H 0.4684 0.7406 0.0377 0.246 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 C1 0.0348(19) 0.0395(18) 0.0311(17) 0.0023(14) 0.0018(14) -0.0013(15) C2 0.0288(18) 0.049(2) 0.0320(17) 0.0007(14) 0.0028(14) 0.0005(15) C3 0.0334(19) 0.044(2) 0.0406(19) 0.0037(15) 0.0040(15) 0.0038(16) C4 0.043(2) 0.043(2) 0.052(2) 0.0052(17) 0.0099(18) 0.0032(17) C5 0.038(2) 0.056(2) 0.059(3) 0.006(2) 0.0126(19) -0.0078(19) C6 0.037(2) 0.063(3) 0.053(2) 0.0039(19) 0.0140(18) 0.0034(18) C7 0.035(2) 0.048(2) 0.0385(19) 0.0025(16) 0.0069(16) 0.0018(16) C8 0.0296(18) 0.049(2) 0.045(2) -0.0002(17) 0.0044(15) 0.0049(16) C9 0.031(2) 0.051(2) 0.052(2) -0.0076(18) 0.0022(17) 0.0116(16) C10 0.055(3) 0.074(3) 0.056(3) -0.010(2) 0.015(2) 0.017(2) C11 0.075(4) 0.076(3) 0.062(3) -0.025(3) 0.011(3) 0.017(3) C12 0.070(3) 0.053(3) 0.070(3) -0.017(2) 0.002(3) 0.017(2) C13 0.050(3) 0.047(2) 0.054(2) -0.0055(19) -0.007(2) 0.0165(19) C14 0.041(2) 0.051(2) 0.053(2) -0.0131(19) -0.0021(18) 0.0116(18) C15 0.060(3) 0.037(2) 0.047(2) -0.0038(18) -0.016(2) -0.0051(19) C16 0.069(3) 0.043(2) 0.047(2) -0.0012(18) -0.024(2) -0.011(2) C17 0.086(4) 0.043(2) 0.047(2) -0.0012(19) -0.025(2) 0.000(2) C18 0.111(5) 0.044(3) 0.051(3) 0.003(2) -0.039(3) -0.008(3) C19 0.101(4) 0.055(3) 0.040(2) 0.010(2) -0.025(2) -0.033(3) C20 0.072(3) 0.058(3) 0.040(2) 0.0032(19) -0.017(2) -0.023(2) C21 0.058(3) 0.045(2) 0.042(2) 0.0055(18) -0.0179(19) -0.018(2) C22 0.048(3) 0.046(2) 0.043(2) 0.0025(17) -0.0186(19) -0.0124(19) C23 0.041(2) 0.047(2) 0.0379(19) 0.0039(16) -0.0030(16) -0.0054(16) C24 0.036(2) 0.057(2) 0.053(2) 0.0098(19) -0.0081(18) -0.0117(18) C25 0.0304(19) 0.061(2) 0.051(2) 0.0062(19) -0.0053(17) -0.0024(18) C26 0.0332(19) 0.045(2) 0.044(2) 0.0005(16) -0.0013(16) 0.0021(16) C27 0.0285(17) 0.0412(18) 0.0379(18) -0.0015(15) 0.0045(14) 0.0017(14) C28 0.0300(18) 0.047(2) 0.0351(18) 0.0012(15) -0.0026(14) -0.0019(15) C29 0.056(3) 0.082(3) 0.048(3) -0.006(2) 0.007(2) 0.005(2) C30 0.067(3) 0.102(4) 0.048(3) 0.001(3) -0.001(2) 0.007(3) C31 0.083(4) 0.131(6) 0.060(3) -0.027(4) 0.000(3) -0.028(4) C32 0.090(5) 0.112(5) 0.077(4) -0.011(4) -0.021(3) -0.040(4) C33 0.075(4) 0.074(3) 0.068(3) -0.005(3) -0.018(3) -0.027(3) C34 0.128(7) 0.130(6) 0.062(4) 0.008(4) 0.002(4) 0.042(5) C35 0.121(7) 0.216(10) 0.061(4) -0.037(5) -0.015(4) 0.072(7) C36 0.075(5) 0.165(8) 0.143(8) 0.025(6) -0.012(5) 0.029(5) C37 0.076(5) 0.195(9) 0.148(8) 0.076(7) 0.008(5) 0.025(5) C38 0.078(4) 0.118(5) 0.078(4) 0.017(4) 0.016(3) 0.014(4) N1 0.0303(16) 0.0387(15) 0.0361(15) 0.0032(12) 0.0012(12) 0.0042(12) N2 0.0282(15) 0.0431(16) 0.0396(16) -0.0017(13) 0.0019(12) 0.0048(13) N3 0.0411(18) 0.056(2) 0.052(2) -0.0070(16) 0.0104(15) 0.0080(15) N4 0.067(2) 0.0436(19) 0.056(2) -0.0119(17) -0.0091(19) 0.0125(18) N5 0.0447(19) 0.0412(18) 0.0439(18) 0.0018(14) -0.0105(15) -0.0029(14) N6 0.047(2) 0.0490(19) 0.0456(19) 0.0072(15) -0.0059(15) -0.0116(16) N7 0.045(2) 0.061(2) 0.0385(18) -0.0057(16) -0.0035(15) 0.0070(17) N8 0.099(4) 0.123(4) 0.074(3) 0.003(3) 0.015(3) 0.029(3) Zn1 0.0386(3) 0.0396(3) 0.0384(3) -0.00140(17) -0.0054(2) 0.00132(18) N9 0.295(17) 0.244(13) 0.148(10) -0.026(8) 0.007(10) 0.109(12) C39 0.250(17) 0.38(2) 0.129(10) -0.030(11) -0.015(10) 0.216(18) C40 0.170(11) 0.245(15) 0.152(11) -0.020(10) 0.053(9) 0.059(10) C41 0.135(7) 0.119(6) 0.107(6) -0.021(5) -0.007(5) 0.039(5) C42 0.283(15) 0.204(11) 0.179(12) 0.035(9) 0.149(12) 0.138(11) C43 0.179(11) 0.269(15) 0.174(12) 0.073(11) 0.073(10) 0.169(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 C1 N1 1.293(4) . ? C1 N2 1.398(5) . ? C1 C2 1.474(5) . ? C2 C3 1.370(5) . ? C2 C7 1.402(5) . ? C3 C4 1.387(5) . ? C4 C5 1.391(6) . ? C5 C6 1.378(6) . ? C6 C7 1.390(6) . ? C7 C8 1.480(5) . ? C8 N3 1.280(5) . ? C8 N2 1.400(5) . ? C9 C14 1.388(6) . ? C9 N3 1.398(5) . ? C9 C10 1.399(6) . ? C10 C11 1.370(7) . ? C11 C12 1.383(8) . ? C12 C13 1.397(6) . ? C13 N4 1.399(6) . ? C13 C14 1.398(6) . ? C14 Zn1 2.480(4) . ? C15 N4 1.275(6) . ? C15 N5 1.405(6) . ? C15 C16 1.486(7) . ? C16 C17 1.375(6) . ? C16 C21 1.378(7) . ? C17 C18 1.363(9) . ? C18 C19 1.402(9) . ? C19 C20 1.398(7) . ? C20 C21 1.383(7) . ? C21 C22 1.489(6) . ? C22 N6 1.303(6) . ? C22 N5 1.388(6) . ? C23 C28 1.395(5) . ? C23 C24 1.395(5) . ? C23 N6 1.399(5) . ? C24 C25 1.380(6) . ? C25 C26 1.397(6) . ? C26 C27 1.392(5) . ? C27 C28 1.409(5) . ? C27 N1 1.410(5) . ? C28 Zn1 2.481(4) . ? C29 N7 1.316(6) . ? C29 C30 1.393(7) . ? C30 C31 1.369(8) . ? C31 C32 1.351(9) . ? C32 C33 1.370(7) . ? C33 N7 1.347(6) . ? C34 C35 1.347(10) . ? C34 N8 1.355(8) . ? C35 C36 1.458(13) . ? C36 C37 1.365(11) . ? C37 C38 1.359(9) . ? C38 N8 1.361(8) . ? N2 Zn1 1.993(3) . ? N5 Zn1 2.003(3) . ? N7 Zn1 2.037(3) . ? N9 C43 1.233(15) . ? N9 C39 1.330(18) . ? C39 C40 1.229(15) . ? C40 C41 1.316(13) . ? C41 C42 1.319(13) . ? C42 C43 1.420(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 129.3(3) . . ? N1 C1 C2 121.0(3) . . ? N2 C1 C2 109.6(3) . . ? C3 C2 C7 121.1(3) . . ? C3 C2 C1 132.3(3) . . ? C7 C2 C1 106.6(3) . . ? C2 C3 C4 117.8(4) . . ? C3 C4 C5 121.2(4) . . ? C6 C5 C4 121.4(4) . . ? C5 C6 C7 117.3(4) . . ? C6 C7 C2 121.2(4) . . ? C6 C7 C8 131.7(4) . . ? C2 C7 C8 107.1(3) . . ? N3 C8 N2 129.2(4) . . ? N3 C8 C7 121.8(4) . . ? N2 C8 C7 108.9(3) . . ? C14 C9 N3 120.0(4) . . ? C14 C9 C10 118.9(4) . . ? N3 C9 C10 121.1(4) . . ? C11 C10 C9 119.9(5) . . ? C10 C11 C12 121.8(5) . . ? C11 C12 C13 119.1(5) . . ? N4 C13 C12 118.7(4) . . ? N4 C13 C14 122.2(4) . . ? C12 C13 C14 119.1(5) . . ? C9 C14 C13 121.1(4) . . ? C9 C14 Zn1 95.7(2) . . ? C13 C14 Zn1 94.3(3) . . ? N4 C15 N5 129.5(4) . . ? N4 C15 C16 122.2(4) . . ? N5 C15 C16 108.1(5) . . ? C17 C16 C21 121.3(5) . . ? C17 C16 C15 131.1(6) . . ? C21 C16 C15 107.4(4) . . ? C18 C17 C16 119.0(6) . . ? C17 C18 C19 120.0(5) . . ? C20 C19 C18 121.5(5) . . ? C21 C20 C19 116.7(6) . . ? C16 C21 C20 121.5(4) . . ? C16 C21 C22 107.3(4) . . ? C20 C21 C22 131.0(5) . . ? N6 C22 N5 129.5(4) . . ? N6 C22 C21 121.6(5) . . ? N5 C22 C21 108.5(4) . . ? C28 C23 C24 119.7(3) . . ? C28 C23 N6 120.4(3) . . ? C24 C23 N6 119.8(3) . . ? C25 C24 C23 119.5(4) . . ? C24 C25 C26 121.5(3) . . ? C27 C26 C25 119.4(3) . . ? C26 C27 C28 119.2(3) . . ? C26 C27 N1 120.3(3) . . ? C28 C27 N1 120.5(3) . . ? C23 C28 C27 120.5(3) . . ? C23 C28 Zn1 95.2(3) . . ? C27 C28 Zn1 95.3(2) . . ? N7 C29 C30 123.9(5) . . ? C31 C30 C29 116.4(5) . . ? C32 C31 C30 121.5(5) . . ? C31 C32 C33 117.9(6) . . ? N7 C33 C32 123.1(5) . . ? C35 C34 N8 123.7(9) . . ? C34 C35 C36 117.6(8) . . ? C37 C36 C35 118.3(7) . . ? C38 C37 C36 119.5(9) . . ? C37 C38 N8 123.3(7) . . ? C1 N1 C27 118.4(3) . . ? C8 N2 C1 107.6(3) . . ? C8 N2 Zn1 126.0(2) . . ? C1 N2 Zn1 126.3(2) . . ? C8 N3 C9 118.6(4) . . ? C15 N4 C13 118.6(4) . . ? C22 N5 C15 108.4(4) . . ? C22 N5 Zn1 126.2(3) . . ? C15 N5 Zn1 125.4(3) . . ? C22 N6 C23 117.8(4) . . ? C29 N7 C33 117.2(4) . . ? C29 N7 Zn1 122.4(3) . . ? C33 N7 Zn1 120.1(3) . . ? C34 N8 C38 117.4(6) . . ? N2 Zn1 N5 142.74(12) . . ? N2 Zn1 N7 110.18(14) . . ? N5 Zn1 N7 107.00(14) . . ? N2 Zn1 C14 85.25(13) . . ? N5 Zn1 C14 85.25(15) . . ? N7 Zn1 C14 108.53(14) . . ? N2 Zn1 C28 85.48(12) . . ? N5 Zn1 C28 84.94(14) . . ? N7 Zn1 C28 101.64(13) . . ? C14 Zn1 C28 149.81(12) . . ? C43 N9 C39 121.8(14) . . ? C40 C39 N9 123.2(16) . . ? C39 C40 C41 119.0(14) . . ? C42 C41 C40 120.7(10) . . ? C41 C42 C43 117.7(9) . . ? N9 C43 C42 117.0(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.827 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.110 data_Zn2py _database_code_depnum_ccdc_archive 'CCDC 750085' #TrackingRef 'Zn2py.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H38 N11 Zn' _chemical_formula_weight 846.27 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9957(13) _cell_length_b 14.2623(10) _cell_length_c 15.6668(12) _cell_angle_alpha 90.00 _cell_angle_beta 97.0500(10) _cell_angle_gamma 90.00 _cell_volume 3990.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9481 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.27 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1756 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9065 _exptl_absorpt_correction_T_max 0.9802 _exptl_absorpt_process_details 'SADABS; Sheldrick, 2004 [Sheldrick, G. M. (2004)]' _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.717640 ; _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32073 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8653 _reflns_number_gt 7190 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms were assigned ideal positions and refined isotropically as riding atoms. ; _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^)+(0.0731P)^2^+4.1520P] 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 8653 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.55727(14) 0.86652(19) 0.63432(17) 0.0221(5) Uani 1 1 d . . . C2 C 0.49394(15) 0.82493(19) 0.57687(17) 0.0223(5) Uani 1 1 d . . . C3 C 0.44457(15) 0.8639(2) 0.51162(18) 0.0270(6) Uani 1 1 d . . . H3 H 0.4470 0.9270 0.4973 0.032 Uiso 1 1 calc R . . C4 C 0.39118(16) 0.8044(2) 0.46840(19) 0.0289(6) Uani 1 1 d . . . H4 H 0.3575 0.8280 0.4239 0.035 Uiso 1 1 calc R . . C5 C 0.38742(16) 0.7098(2) 0.49086(19) 0.0294(6) Uani 1 1 d . . . H5 H 0.3509 0.6717 0.4614 0.035 Uiso 1 1 calc R . . C6 C 0.43745(15) 0.6718(2) 0.55658(18) 0.0258(6) Uani 1 1 d . . . H6 H 0.4351 0.6090 0.5719 0.031 Uiso 1 1 calc R . . C7 C 0.49104(15) 0.7314(2) 0.59832(17) 0.0228(5) Uani 1 1 d . . . C8 C 0.55348(15) 0.71219(18) 0.66779(17) 0.0213(5) Uani 1 1 d . . . C9 C 0.62090(15) 0.60551(19) 0.77005(17) 0.0234(5) Uani 1 1 d . . . C10 C 0.59087(15) 0.6216(2) 0.85694(17) 0.0250(6) Uani 1 1 d . . . H10A H 0.5748 0.6863 0.8599 0.030 Uiso 1 1 calc R . . H10B H 0.5473 0.5821 0.8595 0.030 Uiso 1 1 calc R . . C11 C 0.64781(17) 0.6009(3) 0.93485(19) 0.0358(7) Uani 1 1 d . . . H11A H 0.6627 0.5363 0.9337 0.054 Uiso 1 1 calc R . . H11B H 0.6257 0.6129 0.9865 0.054 Uiso 1 1 calc R . . H11C H 0.6909 0.6403 0.9334 0.054 Uiso 1 1 calc R . . C12 C 0.64465(15) 0.5046(2) 0.75762(16) 0.0237(5) Uani 1 1 d . . . C13 C 0.60345(17) 0.4226(2) 0.75505(18) 0.0293(6) Uani 1 1 d . . . H13 H 0.5532 0.4233 0.7636 0.035 Uiso 1 1 calc R . . C14 C 0.63898(19) 0.3393(2) 0.7394(2) 0.0343(7) Uani 1 1 d . . . H14 H 0.6125 0.2832 0.7387 0.041 Uiso 1 1 calc R . . C15 C 0.71419(19) 0.3383(2) 0.7246(2) 0.0371(7) Uani 1 1 d . . . H15 H 0.7367 0.2817 0.7131 0.045 Uiso 1 1 calc R . . C16 C 0.75562(18) 0.4207(2) 0.7268(2) 0.0334(7) Uani 1 1 d . . . H16 H 0.8055 0.4205 0.7167 0.040 Uiso 1 1 calc R . . C17 C 0.71944(16) 0.5038(2) 0.74469(18) 0.0262(6) Uani 1 1 d . . . C18 C 0.74559(16) 0.6020(2) 0.74974(17) 0.0251(6) Uani 1 1 d . . . C19 C 0.83993(16) 0.7110(2) 0.73216(18) 0.0259(6) Uani 1 1 d . . . C20 C 0.91810(16) 0.7316(2) 0.71890(19) 0.0300(6) Uani 1 1 d . . . C21 C 0.97736(17) 0.6718(3) 0.7093(2) 0.0371(7) Uani 1 1 d . . . H21 H 0.9725 0.6070 0.7130 0.044 Uiso 1 1 calc R . . C22 C 1.04449(18) 0.7133(3) 0.6937(2) 0.0422(8) Uani 1 1 d . . . H22 H 1.0852 0.6754 0.6860 0.051 Uiso 1 1 calc R . . C23 C 1.05195(18) 0.8103(3) 0.6894(2) 0.0425(8) Uani 1 1 d . . . H23 H 1.0976 0.8357 0.6790 0.051 Uiso 1 1 calc R . . C24 C 0.99283(17) 0.8699(3) 0.7003(2) 0.0375(7) Uani 1 1 d . . . H24 H 0.9977 0.9348 0.6979 0.045 Uiso 1 1 calc R . . C25 C 0.92544(15) 0.8270(2) 0.71493(18) 0.0284(6) Uani 1 1 d . . . C26 C 0.85172(15) 0.8685(2) 0.72563(17) 0.0255(6) Uani 1 1 d . . . C27 C 0.76740(15) 0.99089(19) 0.73349(17) 0.0237(5) Uani 1 1 d . . . C28 C 0.75767(16) 1.0588(2) 0.79534(18) 0.0276(6) Uani 1 1 d . . . H28 H 0.7988 1.0818 0.8310 0.033 Uiso 1 1 calc R . . C29 C 0.68605(16) 1.09185(19) 0.80328(19) 0.0275(6) Uani 1 1 d . . . H29 H 0.6797 1.1372 0.8444 0.033 Uiso 1 1 calc R . . C30 C 0.62388(16) 1.05840(19) 0.75091(18) 0.0254(6) Uani 1 1 d . . . H30 H 0.5764 1.0811 0.7572 0.030 Uiso 1 1 calc R . . C31 C 0.63302(15) 0.99027(19) 0.68849(17) 0.0233(5) Uani 1 1 d . . . C32 C 0.70545(15) 0.95922(19) 0.67862(17) 0.0242(5) Uani 1 1 d . . . H32 H 0.7123 0.9170 0.6350 0.029 Uiso 1 1 calc R . . C33 C 0.73798(18) 0.8830(2) 0.9303(2) 0.0356(7) Uani 1 1 d . . . H33 H 0.7862 0.8714 0.9174 0.043 Uiso 1 1 calc R . . C34 C 0.7292(2) 0.9237(3) 1.0091(2) 0.0466(9) Uani 1 1 d . . . H34 H 0.7706 0.9396 1.0478 0.056 Uiso 1 1 calc R . . C35 C 0.6576(2) 0.9397(3) 1.0284(2) 0.0456(9) Uani 1 1 d . . . H35 H 0.6500 0.9659 1.0810 0.055 Uiso 1 1 calc R . . C36 C 0.59775(19) 0.9167(2) 0.9693(2) 0.0361(7) Uani 1 1 d . . . H36 H 0.5491 0.9274 0.9812 0.043 Uiso 1 1 calc R . . C37 C 0.61089(17) 0.8773(2) 0.89161(19) 0.0288(6) Uani 1 1 d . . . H37 H 0.5702 0.8625 0.8514 0.035 Uiso 1 1 calc R . . C38 C 0.8548(3) 0.6911(3) 0.9970(3) 0.0641(12) Uani 1 1 d . . . H38 H 0.8132 0.7158 1.0189 0.077 Uiso 1 1 calc R . . C39 C 0.8527(2) 0.6029(3) 0.9744(3) 0.0562(10) Uani 1 1 d . . . H39 H 0.8114 0.5651 0.9799 0.067 Uiso 1 1 calc R . . C40 C 0.9128(3) 0.5707(3) 0.9431(3) 0.0670(12) Uani 1 1 d . . . H40 H 0.9121 0.5082 0.9260 0.080 Uiso 1 1 calc R . . C41 C 0.9740(3) 0.6199(3) 0.9341(3) 0.0665(12) Uani 1 1 d . . . H41 H 1.0145 0.5926 0.9120 0.080 Uiso 1 1 calc R . . C42 C 0.9755(3) 0.7120(4) 0.9584(4) 0.0740(14) Uani 1 1 d . . . H42 H 1.0174 0.7488 0.9533 0.089 Uiso 1 1 calc R . . C43 C 0.2137(2) 0.8662(3) 0.5426(2) 0.0481(9) Uani 1 1 d . . . H43 H 0.2307 0.9096 0.5848 0.058 Uiso 1 1 calc R . . C44 C 0.2095(2) 0.7733(3) 0.5625(3) 0.0453(8) Uani 1 1 d . . . H44 H 0.2225 0.7541 0.6191 0.054 Uiso 1 1 calc R . . C45 C 0.1873(2) 0.7097(3) 0.5026(3) 0.0552(10) Uani 1 1 d . . . H45 H 0.1856 0.6468 0.5176 0.066 Uiso 1 1 calc R . . C46 C 0.1674(3) 0.7355(3) 0.4210(3) 0.0625(12) Uani 1 1 d . . . H46 H 0.1528 0.6906 0.3793 0.075 Uiso 1 1 calc R . . C47 C 0.1685(2) 0.8276(3) 0.3994(3) 0.0582(11) Uani 1 1 d . . . H47 H 0.1528 0.8454 0.3429 0.070 Uiso 1 1 calc R . . C48 C 0.0356(2) 0.4849(3) 0.5795(2) 0.0491(9) Uani 1 1 d . . . H48 H 0.0591 0.4739 0.6348 0.059 Uiso 1 1 calc R . . C49 C 0.0383(2) 0.5352(3) 0.4390(3) 0.0580(10) Uani 1 1 d . . . H49 H 0.0639 0.5596 0.3959 0.070 Uiso 1 1 calc R . . N1 N 0.59328(12) 0.79664(15) 0.68558(14) 0.0218(5) Uani 1 1 d . . . N2 N 0.56240(12) 0.62936(16) 0.70032(14) 0.0232(5) Uani 1 1 d . . . N3 N 0.69167(12) 0.65822(17) 0.76604(14) 0.0232(5) Uani 1 1 d . . . N4 N 0.81724(13) 0.62387(18) 0.73721(15) 0.0272(5) Uani 1 1 d . . . N5 N 0.80159(12) 0.79394(16) 0.73592(14) 0.0231(5) Uani 1 1 d . . . N6 N 0.84017(13) 0.95704(17) 0.72694(15) 0.0275(5) Uani 1 1 d . . . N7 N 0.57041(13) 0.95583(16) 0.63459(14) 0.0234(5) Uani 1 1 d . . . N8 N 0.68030(13) 0.85996(16) 0.87250(14) 0.0233(5) Uani 1 1 d . . . N9 N 0.9142(3) 0.7495(4) 0.9907(3) 0.0961(15) Uani 1 1 d . . . N10 N 0.1923(2) 0.8949(3) 0.4588(3) 0.0671(10) Uani 1 1 d . . . N11 N 0.0766(2) 0.5208(3) 0.5194(3) 0.0642(10) Uani 1 1 d . . . Zn1 Zn 0.693073(16) 0.79796(2) 0.757112(19) 0.02081(11) 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 0.0213(12) 0.0265(13) 0.0190(12) 0.0005(10) 0.0050(10) 0.0024(10) C2 0.0197(12) 0.0274(13) 0.0204(12) 0.0004(10) 0.0047(10) 0.0008(10) C3 0.0256(14) 0.0297(14) 0.0257(14) 0.0023(11) 0.0028(11) 0.0013(11) C4 0.0240(14) 0.0373(16) 0.0243(14) 0.0023(12) -0.0009(11) 0.0011(12) C5 0.0256(14) 0.0377(16) 0.0241(14) -0.0026(12) 0.0002(11) -0.0049(12) C6 0.0248(14) 0.0290(14) 0.0241(13) 0.0006(11) 0.0047(11) -0.0023(11) C7 0.0196(12) 0.0291(14) 0.0202(13) -0.0009(11) 0.0046(10) 0.0011(10) C8 0.0193(12) 0.0253(13) 0.0199(12) -0.0006(10) 0.0043(10) 0.0003(10) C9 0.0222(13) 0.0253(13) 0.0226(13) 0.0029(10) 0.0021(10) 0.0018(10) C10 0.0253(14) 0.0284(14) 0.0217(13) 0.0007(11) 0.0044(11) 0.0009(11) C11 0.0326(16) 0.053(2) 0.0219(14) 0.0012(13) 0.0039(12) 0.0002(14) C12 0.0288(14) 0.0271(14) 0.0150(12) 0.0040(10) 0.0020(10) 0.0031(11) C13 0.0324(15) 0.0297(15) 0.0256(14) 0.0039(11) 0.0029(12) -0.0001(12) C14 0.0449(18) 0.0274(15) 0.0299(15) 0.0018(12) 0.0011(13) -0.0022(13) C15 0.0469(19) 0.0284(16) 0.0360(17) 0.0008(13) 0.0050(14) 0.0077(14) C16 0.0354(16) 0.0320(16) 0.0325(16) 0.0021(12) 0.0033(13) 0.0048(13) C17 0.0302(14) 0.0259(14) 0.0220(13) 0.0019(11) 0.0017(11) 0.0023(11) C18 0.0275(14) 0.0284(14) 0.0189(12) 0.0023(11) 0.0010(11) 0.0038(11) C19 0.0235(14) 0.0328(15) 0.0212(13) -0.0022(11) 0.0020(11) 0.0031(11) C20 0.0202(13) 0.0437(17) 0.0264(14) -0.0030(13) 0.0042(11) 0.0016(12) C21 0.0290(16) 0.0444(18) 0.0382(17) -0.0042(14) 0.0059(13) 0.0050(14) C22 0.0210(15) 0.059(2) 0.047(2) -0.0117(16) 0.0067(14) 0.0077(14) C23 0.0234(15) 0.057(2) 0.049(2) -0.0148(17) 0.0097(14) -0.0066(14) C24 0.0284(16) 0.0464(19) 0.0389(18) -0.0116(14) 0.0088(13) -0.0061(14) C25 0.0192(13) 0.0424(16) 0.0240(14) -0.0086(12) 0.0042(11) 0.0010(12) C26 0.0201(13) 0.0352(15) 0.0214(13) -0.0023(11) 0.0037(10) -0.0040(11) C27 0.0248(13) 0.0248(13) 0.0224(13) 0.0019(11) 0.0062(11) -0.0012(11) C28 0.0282(14) 0.0278(14) 0.0264(14) 0.0002(11) 0.0019(11) -0.0053(11) C29 0.0312(15) 0.0238(14) 0.0284(14) -0.0025(11) 0.0075(12) -0.0023(11) C30 0.0257(14) 0.0234(13) 0.0275(14) 0.0020(11) 0.0052(11) 0.0028(11) C31 0.0261(14) 0.0234(13) 0.0202(12) 0.0043(10) 0.0022(11) -0.0015(10) C32 0.0273(14) 0.0247(13) 0.0213(13) 0.0001(10) 0.0054(11) -0.0009(11) C33 0.0342(16) 0.0442(18) 0.0277(15) -0.0023(13) 0.0010(13) 0.0014(14) C34 0.054(2) 0.058(2) 0.0247(16) -0.0075(15) -0.0069(15) -0.0007(18) C35 0.070(3) 0.046(2) 0.0239(15) -0.0038(14) 0.0142(16) 0.0016(18) C36 0.0449(19) 0.0311(16) 0.0364(17) -0.0002(13) 0.0211(14) 0.0003(13) C37 0.0321(15) 0.0273(14) 0.0284(15) 0.0014(11) 0.0090(12) 0.0025(12) C38 0.061(3) 0.059(3) 0.070(3) 0.017(2) 0.002(2) -0.003(2) C39 0.042(2) 0.050(2) 0.078(3) 0.007(2) 0.010(2) -0.0054(17) C40 0.062(3) 0.056(3) 0.082(3) 0.002(2) 0.004(2) -0.001(2) C41 0.064(3) 0.062(3) 0.072(3) 0.001(2) 0.008(2) -0.003(2) C42 0.060(3) 0.077(4) 0.085(4) 0.006(3) 0.008(3) -0.011(2) C43 0.044(2) 0.058(2) 0.044(2) -0.0057(17) 0.0126(16) -0.0114(17) C44 0.0412(19) 0.051(2) 0.044(2) 0.0022(16) 0.0073(16) 0.0079(16) C45 0.060(3) 0.037(2) 0.071(3) 0.0018(18) 0.019(2) -0.0044(17) C46 0.075(3) 0.057(3) 0.058(3) -0.007(2) 0.019(2) -0.020(2) C47 0.064(3) 0.070(3) 0.041(2) 0.003(2) 0.0101(19) -0.014(2) C48 0.057(2) 0.049(2) 0.0404(19) 0.0032(16) 0.0024(17) 0.0008(18) C49 0.060(3) 0.064(3) 0.052(2) -0.001(2) 0.012(2) -0.013(2) N1 0.0216(11) 0.0239(11) 0.0198(11) 0.0021(9) 0.0027(9) 0.0018(9) N2 0.0228(11) 0.0251(12) 0.0215(11) 0.0019(9) 0.0021(9) -0.0007(9) N3 0.0233(11) 0.0281(12) 0.0183(11) 0.0027(9) 0.0024(9) 0.0003(9) N4 0.0243(12) 0.0301(13) 0.0276(12) -0.0001(10) 0.0044(10) 0.0061(10) N5 0.0204(11) 0.0271(12) 0.0223(12) -0.0005(9) 0.0051(9) 0.0005(9) N6 0.0245(12) 0.0323(13) 0.0266(12) -0.0024(10) 0.0068(10) -0.0046(10) N7 0.0236(11) 0.0260(11) 0.0209(11) -0.0004(9) 0.0033(9) 0.0015(9) N8 0.0271(12) 0.0251(11) 0.0179(11) 0.0006(9) 0.0036(9) -0.0006(9) N9 0.082(3) 0.119(4) 0.085(3) 0.023(3) 0.001(3) -0.002(3) N10 0.069(2) 0.072(3) 0.065(2) 0.007(2) 0.026(2) 0.005(2) N11 0.060(2) 0.066(2) 0.066(2) -0.0043(19) 0.0065(19) -0.0028(18) Zn1 0.01868(17) 0.02507(18) 0.01901(17) -0.00052(11) 0.00361(12) 0.00095(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 C1 N7 1.295(3) . ? C1 N1 1.389(3) . ? C1 C2 1.486(4) . ? C2 C7 1.378(4) . ? C2 C3 1.386(4) . ? C3 C4 1.394(4) . ? C4 C5 1.398(4) . ? C5 C6 1.391(4) . ? C6 C7 1.387(4) . ? C7 C8 1.491(4) . ? C8 N2 1.289(3) . ? C8 N1 1.412(3) . ? C9 N2 1.461(3) . ? C9 N3 1.487(3) . ? C9 C12 1.520(4) . ? C9 C10 1.542(4) . ? C10 C11 1.523(4) . ? C12 C13 1.383(4) . ? C12 C17 1.385(4) . ? C13 C14 1.386(4) . ? C14 C15 1.401(5) . ? C15 C16 1.390(4) . ? C16 C17 1.397(4) . ? C17 C18 1.477(4) . ? C18 N3 1.308(4) . ? C18 N4 1.364(4) . ? C19 N4 1.314(4) . ? C19 N5 1.374(3) . ? C19 C20 1.476(4) . ? C20 C25 1.370(4) . ? C20 C21 1.388(4) . ? C21 C22 1.393(5) . ? C22 C23 1.392(5) . ? C23 C24 1.389(5) . ? C24 C25 1.402(4) . ? C25 C26 1.480(4) . ? C26 N6 1.281(4) . ? C26 N5 1.416(3) . ? C27 C28 1.396(4) . ? C27 C32 1.397(4) . ? C27 N6 1.411(4) . ? C28 C29 1.392(4) . ? C29 C30 1.388(4) . ? C30 C31 1.402(4) . ? C31 C32 1.403(4) . ? C31 N7 1.411(3) . ? C33 N8 1.332(4) . ? C33 C34 1.391(4) . ? C34 C35 1.377(5) . ? C35 C36 1.371(5) . ? C36 C37 1.387(4) . ? C37 N8 1.343(4) . ? C38 C39 1.306(6) . ? C38 N9 1.368(7) . ? C39 C40 1.324(6) . ? C40 C41 1.328(6) . ? C41 C42 1.367(7) . ? C42 N9 1.378(7) . ? C43 C44 1.365(5) . ? C43 N10 1.383(5) . ? C44 C45 1.331(6) . ? C45 C46 1.335(6) . ? C46 C47 1.357(6) . ? C47 N10 1.369(6) . ? C48 C49 1.357(5) 3_566 ? C48 N11 1.365(5) . ? C49 C48 1.357(5) 3_566 ? C49 N11 1.374(5) . ? N1 Zn1 1.997(2) . ? N3 Zn1 1.998(2) . ? N5 Zn1 2.021(2) . ? N8 Zn1 2.051(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 C1 N1 129.2(2) . . ? N7 C1 C2 121.4(2) . . ? N1 C1 C2 109.4(2) . . ? C7 C2 C3 121.9(3) . . ? C7 C2 C1 106.7(2) . . ? C3 C2 C1 131.4(3) . . ? C2 C3 C4 117.1(3) . . ? C3 C4 C5 121.1(3) . . ? C6 C5 C4 121.0(3) . . ? C7 C6 C5 117.4(3) . . ? C2 C7 C6 121.5(3) . . ? C2 C7 C8 108.0(2) . . ? C6 C7 C8 130.5(3) . . ? N2 C8 N1 131.9(3) . . ? N2 C8 C7 120.2(2) . . ? N1 C8 C7 107.8(2) . . ? N2 C9 N3 113.1(2) . . ? N2 C9 C12 108.2(2) . . ? N3 C9 C12 102.6(2) . . ? N2 C9 C10 109.1(2) . . ? N3 C9 C10 110.9(2) . . ? C12 C9 C10 112.9(2) . . ? C11 C10 C9 113.9(2) . . ? C13 C12 C17 121.0(3) . . ? C13 C12 C9 130.2(3) . . ? C17 C12 C9 108.7(2) . . ? C12 C13 C14 118.2(3) . . ? C13 C14 C15 121.0(3) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 117.4(3) . . ? C12 C17 C16 121.5(3) . . ? C12 C17 C18 107.0(2) . . ? C16 C17 C18 131.5(3) . . ? N3 C18 N4 128.7(3) . . ? N3 C18 C17 110.6(2) . . ? N4 C18 C17 120.6(2) . . ? N4 C19 N5 130.6(3) . . ? N4 C19 C20 120.3(3) . . ? N5 C19 C20 109.1(2) . . ? C25 C20 C21 121.7(3) . . ? C25 C20 C19 107.6(2) . . ? C21 C20 C19 130.6(3) . . ? C20 C21 C22 116.9(3) . . ? C23 C22 C21 121.4(3) . . ? C24 C23 C22 121.5(3) . . ? C23 C24 C25 116.3(3) . . ? C20 C25 C24 122.1(3) . . ? C20 C25 C26 107.4(2) . . ? C24 C25 C26 130.5(3) . . ? N6 C26 N5 129.2(3) . . ? N6 C26 C25 123.0(3) . . ? N5 C26 C25 107.8(2) . . ? C28 C27 C32 119.5(3) . . ? C28 C27 N6 119.0(2) . . ? C32 C27 N6 121.5(2) . . ? C29 C28 C27 119.6(3) . . ? C30 C29 C28 121.2(3) . . ? C29 C30 C31 119.7(3) . . ? C30 C31 C32 119.1(2) . . ? C30 C31 N7 120.3(2) . . ? C32 C31 N7 120.6(2) . . ? C27 C32 C31 120.8(3) . . ? N8 C33 C34 122.8(3) . . ? C35 C34 C33 118.4(3) . . ? C36 C35 C34 119.4(3) . . ? C35 C36 C37 119.0(3) . . ? N8 C37 C36 122.3(3) . . ? C39 C38 N9 124.4(5) . . ? C38 C39 C40 115.9(4) . . ? C39 C40 C41 125.6(5) . . ? C40 C41 C42 117.8(5) . . ? C41 C42 N9 119.1(5) . . ? C44 C43 N10 119.2(4) . . ? C45 C44 C43 121.3(4) . . ? C44 C45 C46 120.6(4) . . ? C45 C46 C47 119.7(4) . . ? C46 C47 N10 121.4(4) . . ? C49 C48 N11 122.0(4) 3_566 . ? C48 C49 N11 122.1(4) 3_566 . ? C1 N1 C8 108.0(2) . . ? C1 N1 Zn1 129.87(18) . . ? C8 N1 Zn1 121.23(17) . . ? C8 N2 C9 123.5(2) . . ? C18 N3 C9 111.0(2) . . ? C18 N3 Zn1 125.55(19) . . ? C9 N3 Zn1 121.71(17) . . ? C19 N4 C18 122.1(2) . . ? C19 N5 C26 108.1(2) . . ? C19 N5 Zn1 122.12(19) . . ? C26 N5 Zn1 129.74(18) . . ? C26 N6 C27 119.5(2) . . ? C1 N7 C31 118.4(2) . . ? C33 N8 C37 118.1(3) . . ? C33 N8 Zn1 122.9(2) . . ? C37 N8 Zn1 118.95(19) . . ? C38 N9 C42 117.2(6) . . ? C47 N10 C43 117.8(4) . . ? C48 N11 C49 115.8(4) . . ? N1 Zn1 N3 90.67(9) . . ? N1 Zn1 N5 136.72(9) . . ? N3 Zn1 N5 90.23(9) . . ? N1 Zn1 N8 107.97(9) . . ? N3 Zn1 N8 111.38(9) . . ? N5 Zn1 N8 111.84(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.789 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.100 data_Zn2THF _database_code_depnum_ccdc_archive 'CCDC 750086' #TrackingRef 'Zn2THF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H50 N7 O Zn' _chemical_formula_weight 770.29 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.968(6) _cell_length_b 13.937(4) _cell_length_c 15.456(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.326(6) _cell_angle_gamma 90.00 _cell_volume 3860(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3065 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.16 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details 'SADABS; Sheldrick, 2004 [Sheldrick, G. M. (2004)]' _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.364845 ; _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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31392 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.0874 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8401 _reflns_number_gt 5127 _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. Hydrogen atoms were assigned ideal positions and refined isotropically as riding atoms. Some of the solvent (two hexanes per unit cell) were modeled as a diffuse contribution to the reflection array without specific atom positions by using the SQUEEZE program. However, all parameters, including density, F(000) and extinction coefficient, reflect the full formula. ; _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^)+(0.0618P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8401 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _refine_ls_shift/su_max 0.012 _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 0.56325(15) 0.86004(19) 0.63669(16) 0.0215(6) Uani 1 1 d . . . C2 C 0.50261(15) 0.81980(19) 0.57751(17) 0.0220(6) Uani 1 1 d . . . C3 C 0.45600(15) 0.8617(2) 0.51331(18) 0.0267(7) Uani 1 1 d . . . H3 H 0.4581 0.9284 0.5014 0.032 Uiso 1 1 calc R . . C4 C 0.40565(16) 0.8016(2) 0.46661(19) 0.0309(7) Uani 1 1 d . . . H4 H 0.3726 0.8280 0.4219 0.037 Uiso 1 1 calc R . . C5 C 0.40271(16) 0.7035(2) 0.48409(18) 0.0306(7) Uani 1 1 d . . . H5 H 0.3680 0.6641 0.4510 0.037 Uiso 1 1 calc R . . C6 C 0.44968(15) 0.6629(2) 0.54905(17) 0.0258(6) Uani 1 1 d . . . H6 H 0.4480 0.5961 0.5612 0.031 Uiso 1 1 calc R . . C7 C 0.49900(14) 0.72279(19) 0.59547(16) 0.0216(6) Uani 1 1 d . . . C8 C 0.55774(14) 0.70125(18) 0.66586(17) 0.0208(6) Uani 1 1 d . . . C9 C 0.62071(15) 0.58783(18) 0.76447(17) 0.0221(6) Uani 1 1 d . . . C10 C 0.58922(15) 0.6029(2) 0.85352(16) 0.0236(6) Uani 1 1 d . . . H16A H 0.5738 0.6707 0.8587 0.028 Uiso 1 1 calc R . . H16B H 0.5443 0.5623 0.8570 0.028 Uiso 1 1 calc R . . C11 C 0.64532(16) 0.5784(2) 0.92913(18) 0.0345(7) Uani 1 1 d . . . H17A H 0.6630 0.5125 0.9227 0.052 Uiso 1 1 calc R . . H17B H 0.6213 0.5842 0.9837 0.052 Uiso 1 1 calc R . . H17C H 0.6877 0.6227 0.9296 0.052 Uiso 1 1 calc R . . C12 C 0.64320(16) 0.48474(19) 0.74984(16) 0.0237(6) Uani 1 1 d . . . C13 C 0.60201(17) 0.4017(2) 0.74944(17) 0.0284(7) Uani 1 1 d . . . H13 H 0.5501 0.4031 0.7574 0.034 Uiso 1 1 calc R . . C14 C 0.63860(18) 0.3157(2) 0.73709(19) 0.0335(7) Uani 1 1 d . . . H14 H 0.6117 0.2571 0.7388 0.040 Uiso 1 1 calc R . . C15 C 0.71445(18) 0.3137(2) 0.7222(2) 0.0370(8) Uani 1 1 d . . . H15 H 0.7382 0.2540 0.7130 0.044 Uiso 1 1 calc R . . C16 C 0.75528(17) 0.3978(2) 0.72076(19) 0.0336(7) Uani 1 1 d . . . H16 H 0.8065 0.3973 0.7094 0.040 Uiso 1 1 calc R . . C17 C 0.71869(16) 0.4829(2) 0.73648(17) 0.0259(6) Uani 1 1 d . . . C18 C 0.74541(16) 0.5826(2) 0.74322(17) 0.0243(6) Uani 1 1 d . . . C19 C 0.84147(16) 0.6935(2) 0.73193(18) 0.0275(7) Uani 1 1 d . . . C20 C 0.92160(15) 0.7129(2) 0.72389(18) 0.0291(7) Uani 1 1 d . . . C21 C 0.98162(17) 0.6513(2) 0.7197(2) 0.0412(8) Uani 1 1 d . . . H21 H 0.9754 0.5836 0.7219 0.049 Uiso 1 1 calc R . . C22 C 1.05136(18) 0.6921(3) 0.7122(2) 0.0502(10) Uani 1 1 d . . . H22 H 1.0937 0.6517 0.7098 0.060 Uiso 1 1 calc R . . C23 C 1.06022(18) 0.7903(3) 0.7081(2) 0.0518(10) Uani 1 1 d . . . H23 H 1.1083 0.8162 0.7014 0.062 Uiso 1 1 calc R . . C24 C 0.99981(17) 0.8520(2) 0.7138(2) 0.0413(8) Uani 1 1 d . . . H24 H 1.0060 0.9196 0.7118 0.050 Uiso 1 1 calc R . . C25 C 0.93032(16) 0.8112(2) 0.72222(19) 0.0315(7) Uani 1 1 d . . . C26 C 0.85570(16) 0.8540(2) 0.73014(18) 0.0286(7) Uani 1 1 d . . . C27 C 0.77179(16) 0.97989(19) 0.74108(18) 0.0253(6) Uani 1 1 d . . . C28 C 0.75960(16) 1.04784(19) 0.80443(18) 0.0258(6) Uani 1 1 d . . . H28 H 0.8000 1.0703 0.8423 0.031 Uiso 1 1 calc R . . C29 C 0.68808(15) 1.08264(18) 0.81200(17) 0.0251(6) Uani 1 1 d . . . H29 H 0.6803 1.1296 0.8549 0.030 Uiso 1 1 calc R . . C30 C 0.62789(16) 1.05099(19) 0.75891(17) 0.0247(6) Uani 1 1 d . . . H30 H 0.5793 1.0751 0.7660 0.030 Uiso 1 1 calc R . . C31 C 0.63913(15) 0.98289(19) 0.69449(17) 0.0239(6) Uani 1 1 d . . . C32 C 0.71157(15) 0.95034(19) 0.68418(17) 0.0242(6) Uani 1 1 d . . . H32 H 0.7201 0.9077 0.6380 0.029 Uiso 1 1 calc R . . C33 C 0.75115(17) 0.8321(2) 0.93954(18) 0.0345(7) Uani 1 1 d . . . H33A H 0.7889 0.8783 0.9216 0.041 Uiso 1 1 calc R . . H33B H 0.7740 0.7676 0.9445 0.041 Uiso 1 1 calc R . . C34 C 0.72160(18) 0.8624(2) 1.02474(19) 0.0394(8) Uani 1 1 d . . . H34A H 0.7594 0.8997 1.0604 0.047 Uiso 1 1 calc R . . H34B H 0.7067 0.8059 1.0583 0.047 Uiso 1 1 calc R . . C35 C 0.65428(17) 0.9241(2) 0.99637(18) 0.0349(8) Uani 1 1 d . . . H35A H 0.6189 0.9283 1.0423 0.042 Uiso 1 1 calc R . . H35B H 0.6694 0.9895 0.9802 0.042 Uiso 1 1 calc R . . C36 C 0.62134(16) 0.8693(2) 0.91893(19) 0.0316(7) Uani 1 1 d . . . H36A H 0.5892 0.8165 0.9371 0.038 Uiso 1 1 calc R . . H36B H 0.5913 0.9122 0.8790 0.038 Uiso 1 1 calc R . . C37 C 0.9293(4) 0.6908(6) 0.9776(4) 0.144(3) Uani 1 1 d . . . H37A H 0.8931 0.7208 1.0135 0.216 Uiso 1 1 calc R . . H37B H 0.9330 0.7287 0.9246 0.216 Uiso 1 1 calc R . . H37C H 0.9782 0.6881 1.0101 0.216 Uiso 1 1 calc R . . C38 C 0.9062(7) 0.5994(7) 0.9558(6) 0.247(6) Uani 1 1 d . . . H38A H 0.8742 0.6068 0.9012 0.297 Uiso 1 1 calc R . . H38B H 0.9517 0.5659 0.9398 0.297 Uiso 1 1 calc R . . C39 C 0.8702(4) 0.5348(7) 1.0030(4) 0.127(2) Uani 1 1 d . . . H39A H 0.8233 0.5666 1.0168 0.152 Uiso 1 1 calc R . . H39B H 0.9009 0.5288 1.0586 0.152 Uiso 1 1 calc R . . C40 C 0.8491(4) 0.4367(7) 0.9779(5) 0.151(3) Uani 1 1 d . . . H40A H 0.8105 0.4445 0.9292 0.181 Uiso 1 1 calc R . . H40B H 0.8935 0.4104 0.9520 0.181 Uiso 1 1 calc R . . C41 C 0.8222(6) 0.3582(9) 1.0286(7) 0.249(6) Uani 1 1 d . . . H41A H 0.7779 0.3826 1.0561 0.299 Uiso 1 1 calc R . . H41B H 0.8611 0.3463 1.0763 0.299 Uiso 1 1 calc R . . C42 C 0.8014(4) 0.2639(6) 0.9915(5) 0.174(4) Uani 1 1 d . . . H42A H 0.7736 0.2728 0.9350 0.262 Uiso 1 1 calc R . . H42B H 0.7700 0.2298 1.0306 0.262 Uiso 1 1 calc R . . H42C H 0.8466 0.2265 0.9840 0.262 Uiso 1 1 calc R . . N1 N 0.59664(12) 0.78638(15) 0.68686(13) 0.0209(5) Uani 1 1 d . . . N2 N 0.56388(12) 0.61537(16) 0.69553(14) 0.0218(5) Uani 1 1 d . . . N3 N 0.69193(12) 0.64124(15) 0.76010(13) 0.0210(5) Uani 1 1 d . . . N4 N 0.81832(12) 0.60427(17) 0.73358(14) 0.0270(5) Uani 1 1 d . . . N5 N 0.80325(12) 0.77846(16) 0.73582(13) 0.0238(5) Uani 1 1 d . . . N6 N 0.84480(13) 0.94436(17) 0.73447(15) 0.0291(6) Uani 1 1 d . . . N7 N 0.57797(12) 0.95096(15) 0.63899(14) 0.0228(5) Uani 1 1 d . . . O1 O 0.68541(10) 0.83157(13) 0.87732(11) 0.0264(4) Uani 1 1 d . . . Zn1 Zn 0.694297(17) 0.78320(2) 0.754284(19) 0.02132(10) 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 0.0227(15) 0.0283(16) 0.0138(13) 0.0022(11) 0.0038(11) 0.0046(12) C2 0.0244(15) 0.0235(14) 0.0185(14) -0.0013(11) 0.0033(12) 0.0006(12) C3 0.0263(16) 0.0268(16) 0.0269(16) 0.0040(12) 0.0027(13) 0.0012(12) C4 0.0307(17) 0.0361(19) 0.0247(16) 0.0059(13) -0.0045(13) 0.0008(13) C5 0.0323(17) 0.0339(19) 0.0247(15) 0.0013(13) -0.0041(13) -0.0078(14) C6 0.0276(16) 0.0272(16) 0.0229(15) 0.0035(12) 0.0021(12) -0.0002(13) C7 0.0205(14) 0.0261(15) 0.0187(13) 0.0021(12) 0.0038(11) 0.0027(12) C8 0.0197(14) 0.0244(16) 0.0190(14) -0.0002(11) 0.0062(11) 0.0016(11) C9 0.0254(15) 0.0214(15) 0.0191(14) 0.0018(11) -0.0012(12) 0.0002(12) C10 0.0270(15) 0.0234(15) 0.0209(14) 0.0005(12) 0.0052(12) -0.0038(12) C11 0.0386(19) 0.0437(19) 0.0213(16) 0.0031(14) 0.0037(14) -0.0044(15) C12 0.0321(17) 0.0258(15) 0.0129(13) 0.0024(11) -0.0011(12) 0.0023(13) C13 0.0362(18) 0.0281(16) 0.0208(15) 0.0021(12) 0.0013(13) 0.0001(14) C14 0.048(2) 0.0251(16) 0.0272(17) 0.0008(13) 0.0003(15) -0.0006(14) C15 0.051(2) 0.0249(17) 0.0347(18) -0.0024(13) 0.0005(16) 0.0119(15) C16 0.0344(18) 0.0361(18) 0.0297(17) -0.0013(14) -0.0017(14) 0.0074(15) C17 0.0309(17) 0.0295(17) 0.0168(14) 0.0010(12) -0.0025(12) 0.0040(13) C18 0.0284(16) 0.0292(16) 0.0148(14) 0.0022(12) -0.0026(12) 0.0032(13) C19 0.0239(16) 0.0388(19) 0.0195(15) 0.0011(12) 0.0006(12) 0.0043(13) C20 0.0228(15) 0.0370(17) 0.0278(15) -0.0067(14) 0.0027(12) 0.0019(14) C21 0.0295(19) 0.047(2) 0.047(2) -0.0060(17) 0.0007(15) 0.0062(16) C22 0.0208(18) 0.062(3) 0.068(3) -0.0170(19) 0.0027(17) 0.0068(16) C23 0.0218(18) 0.073(3) 0.061(2) -0.022(2) 0.0049(16) -0.0054(18) C24 0.0296(18) 0.048(2) 0.047(2) -0.0153(17) 0.0037(15) -0.0071(16) C25 0.0192(16) 0.048(2) 0.0277(16) -0.0073(14) 0.0007(12) -0.0010(13) C26 0.0279(17) 0.0367(18) 0.0214(15) -0.0046(13) 0.0038(13) -0.0058(14) C27 0.0264(16) 0.0222(15) 0.0281(16) 0.0018(12) 0.0077(12) -0.0039(13) C28 0.0290(16) 0.0235(15) 0.0251(16) 0.0013(12) 0.0026(12) -0.0067(13) C29 0.0350(17) 0.0184(14) 0.0222(15) -0.0005(11) 0.0042(13) -0.0027(12) C30 0.0282(16) 0.0217(15) 0.0245(15) 0.0019(12) 0.0037(12) 0.0034(12) C31 0.0298(16) 0.0208(15) 0.0213(15) 0.0058(12) 0.0025(12) -0.0012(12) C32 0.0290(16) 0.0219(15) 0.0223(15) 0.0000(12) 0.0060(12) -0.0024(12) C33 0.0340(18) 0.0450(19) 0.0231(16) -0.0035(14) -0.0069(13) 0.0031(15) C34 0.050(2) 0.047(2) 0.0206(16) 0.0000(14) 0.0000(15) -0.0035(16) C35 0.050(2) 0.0352(18) 0.0207(16) -0.0036(13) 0.0126(14) -0.0031(15) C36 0.0357(18) 0.0323(17) 0.0278(16) -0.0020(13) 0.0102(14) 0.0032(14) C37 0.101(5) 0.235(9) 0.096(5) 0.054(6) -0.002(4) 0.032(5) C38 0.394(17) 0.191(10) 0.138(8) 0.030(7) -0.104(9) -0.125(11) C39 0.120(5) 0.187(8) 0.072(4) 0.014(5) 0.002(4) -0.026(5) C40 0.130(6) 0.192(8) 0.123(6) -0.086(6) -0.040(5) 0.052(6) C41 0.287(13) 0.285(14) 0.190(10) -0.019(10) 0.121(9) -0.152(11) C42 0.125(6) 0.226(8) 0.182(8) -0.095(7) 0.079(6) -0.090(6) N1 0.0216(12) 0.0215(12) 0.0198(11) 0.0027(10) 0.0032(9) 0.0003(10) N2 0.0212(12) 0.0250(13) 0.0193(12) 0.0019(10) 0.0032(9) -0.0009(10) N3 0.0188(12) 0.0268(13) 0.0171(12) 0.0012(10) -0.0004(9) 0.0012(10) N4 0.0238(14) 0.0299(14) 0.0273(14) 0.0023(11) 0.0015(10) 0.0063(11) N5 0.0211(12) 0.0275(13) 0.0228(12) -0.0045(11) 0.0020(10) -0.0012(11) N6 0.0238(14) 0.0331(15) 0.0306(14) -0.0059(11) 0.0041(11) -0.0058(11) N7 0.0270(13) 0.0217(12) 0.0194(12) 0.0007(10) -0.0001(10) 0.0005(10) O1 0.0261(11) 0.0364(11) 0.0167(10) -0.0019(8) 0.0016(8) 0.0042(9) Zn1 0.02098(17) 0.02428(18) 0.01879(17) -0.00040(14) 0.00210(12) 0.00049(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 C1 N7 1.294(3) . ? C1 N1 1.395(3) . ? C1 C2 1.479(4) . ? C2 C3 1.379(4) . ? C2 C7 1.383(4) . ? C3 C4 1.394(4) . ? C4 C5 1.396(4) . ? C5 C6 1.383(4) . ? C6 C7 1.379(4) . ? C7 C8 1.488(4) . ? C8 N2 1.284(3) . ? C8 N1 1.403(3) . ? C9 N2 1.470(3) . ? C9 N3 1.486(3) . ? C9 C12 1.514(4) . ? C9 C10 1.541(4) . ? C10 C11 1.523(4) . ? C12 C13 1.374(4) . ? C12 C17 1.388(4) . ? C13 C14 1.387(4) . ? C14 C15 1.400(4) . ? C15 C16 1.384(4) . ? C16 C17 1.386(4) . ? C17 C18 1.471(4) . ? C18 N3 1.303(3) . ? C18 N4 1.364(3) . ? C19 N4 1.312(4) . ? C19 N5 1.373(3) . ? C19 C20 1.479(4) . ? C20 C25 1.380(4) . ? C20 C21 1.384(4) . ? C21 C22 1.389(4) . ? C22 C23 1.379(5) . ? C23 C24 1.393(4) . ? C24 C25 1.387(4) . ? C25 C26 1.480(4) . ? C26 N6 1.278(3) . ? C26 N5 1.420(3) . ? C27 C28 1.391(4) . ? C27 C32 1.404(4) . ? C27 N6 1.413(4) . ? C28 C29 1.387(4) . ? C29 C30 1.380(4) . ? C30 C31 1.401(4) . ? C31 C32 1.399(4) . ? C31 N7 1.414(3) . ? C33 O1 1.466(3) . ? C33 C34 1.516(4) . ? C34 C35 1.521(4) . ? C35 C36 1.503(4) . ? C36 O1 1.458(3) . ? C37 C38 1.373(9) . ? C38 C39 1.354(10) . ? C39 C40 1.463(8) . ? C40 C41 1.449(10) . ? C41 C42 1.472(10) . ? N1 Zn1 1.973(2) . ? N3 Zn1 1.981(2) . ? N5 Zn1 2.001(2) . ? O1 Zn1 2.0353(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 C1 N1 128.8(3) . . ? N7 C1 C2 121.8(2) . . ? N1 C1 C2 109.3(2) . . ? C3 C2 C7 121.5(3) . . ? C3 C2 C1 131.6(3) . . ? C7 C2 C1 106.9(2) . . ? C2 C3 C4 117.0(3) . . ? C3 C4 C5 121.4(3) . . ? C6 C5 C4 120.8(3) . . ? C7 C6 C5 117.6(3) . . ? C6 C7 C2 121.7(2) . . ? C6 C7 C8 130.6(3) . . ? C2 C7 C8 107.6(2) . . ? N2 C8 N1 132.7(3) . . ? N2 C8 C7 119.1(2) . . ? N1 C8 C7 108.2(2) . . ? N2 C9 N3 112.9(2) . . ? N2 C9 C12 108.6(2) . . ? N3 C9 C12 103.2(2) . . ? N2 C9 C10 109.3(2) . . ? N3 C9 C10 110.3(2) . . ? C12 C9 C10 112.5(2) . . ? C11 C10 C9 112.8(2) . . ? C13 C12 C17 121.0(3) . . ? C13 C12 C9 130.6(3) . . ? C17 C12 C9 108.4(2) . . ? C12 C13 C14 117.9(3) . . ? C13 C14 C15 121.1(3) . . ? C16 C15 C14 120.6(3) . . ? C15 C16 C17 117.6(3) . . ? C16 C17 C12 121.6(3) . . ? C16 C17 C18 131.6(3) . . ? C12 C17 C18 106.8(2) . . ? N3 C18 N4 127.7(3) . . ? N3 C18 C17 111.4(2) . . ? N4 C18 C17 120.8(3) . . ? N4 C19 N5 131.0(3) . . ? N4 C19 C20 119.1(3) . . ? N5 C19 C20 109.8(3) . . ? C25 C20 C21 121.7(3) . . ? C25 C20 C19 107.2(2) . . ? C21 C20 C19 131.1(3) . . ? C20 C21 C22 117.4(3) . . ? C23 C22 C21 121.2(3) . . ? C22 C23 C24 121.1(3) . . ? C25 C24 C23 117.7(3) . . ? C20 C25 C24 120.8(3) . . ? C20 C25 C26 107.0(2) . . ? C24 C25 C26 132.1(3) . . ? N6 C26 N5 128.5(3) . . ? N6 C26 C25 123.0(3) . . ? N5 C26 C25 108.5(2) . . ? C28 C27 C32 119.1(3) . . ? C28 C27 N6 119.1(3) . . ? C32 C27 N6 121.9(2) . . ? C29 C28 C27 119.6(3) . . ? C30 C29 C28 121.9(3) . . ? C29 C30 C31 119.4(3) . . ? C32 C31 C30 119.1(3) . . ? C32 C31 N7 121.1(2) . . ? C30 C31 N7 119.8(2) . . ? C31 C32 C27 120.9(3) . . ? O1 C33 C34 104.7(2) . . ? C33 C34 C35 103.3(2) . . ? C36 C35 C34 101.5(2) . . ? O1 C36 C35 104.9(2) . . ? C39 C38 C37 129.3(11) . . ? C38 C39 C40 127.2(8) . . ? C41 C40 C39 130.7(8) . . ? C40 C41 C42 123.2(8) . . ? C1 N1 C8 107.9(2) . . ? C1 N1 Zn1 129.68(18) . . ? C8 N1 Zn1 120.74(17) . . ? C8 N2 C9 122.6(2) . . ? C18 N3 C9 110.2(2) . . ? C18 N3 Zn1 126.79(19) . . ? C9 N3 Zn1 121.57(16) . . ? C19 N4 C18 121.4(2) . . ? C19 N5 C26 107.5(2) . . ? C19 N5 Zn1 122.21(19) . . ? C26 N5 Zn1 130.21(19) . . ? C26 N6 C27 119.7(2) . . ? C1 N7 C31 118.2(2) . . ? C36 O1 C33 109.4(2) . . ? C36 O1 Zn1 130.67(16) . . ? C33 O1 Zn1 119.91(16) . . ? N1 Zn1 N3 91.44(9) . . ? N1 Zn1 N5 140.03(9) . . ? N3 Zn1 N5 89.89(9) . . ? N1 Zn1 O1 110.90(8) . . ? N3 Zn1 O1 106.56(8) . . ? N5 Zn1 O1 106.91(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.570 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.080 loop_ _platon_squeeze_void_nr 2 _platon_squeeze_void_average_x 1.000 _platon_squeeze_void_average_y 0.500 _platon_squeeze_void_average_z 0.500 _platon_squeeze_void_volume ? _platon_squeeze_void_count_electrons 117 _platon_squeeze_void_content 58 _platon_squeeze_details ; ;