# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), (I 1-), (C22 H12 N9 1-), 3.5(C1 H3 O1 H1)' _chemical_formula_sum 'C25.50 H26 I N9 O3.50 Zn' _chemical_formula_weight 706.82 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.006(1) _cell_length_b 15.3229(9) _cell_length_c 20.969(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5785.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24288 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.36 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow ' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2824 _exptl_absorpt_coefficient_mu 1.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7986 _exptl_absorpt_correction_T_max 0.8913 _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 'microfocus source 30W maximum continuous power' _diffrn_radiation_monochromator 'Wuazar(TM) Montel multilayer optic' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24288 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.36 _reflns_number_total 10433 _reflns_number_gt 6755 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 sofware Suite' _computing_cell_refinement 'APEX2 sofware Suite' _computing_data_reduction 'APEX2 sofware Suite' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Several restraints were applied to disordered methanols and TPHAP skeleton on a basis of chemical symmetry of the molecules. Several solvents were refined with isotropic thermal parameters. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1762P)^2^+26.9224P] 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 H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.39(4) _refine_ls_number_reflns 10433 _refine_ls_number_parameters 579 _refine_ls_number_restraints 147 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.2969 _refine_ls_wR_factor_gt 0.2607 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.004 _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 N1 N 0.0337(5) 0.3253(4) 0.4878(4) 0.040(3) Uani 1 1 d GU . . C1 C 0.0014(5) 0.2475(5) 0.4679(4) 0.044(4) Uani 1 1 d G . . H1 H -0.0342 0.2478 0.4345 0.052 Uiso 1 1 calc R . . C2 C 0.0214(5) 0.1693(4) 0.4967(4) 0.035(3) Uani 1 1 d G . . H2 H -0.0006 0.1161 0.4831 0.042 Uiso 1 1 calc R . . C3 C 0.0736(5) 0.1688(4) 0.5456(4) 0.015(2) Uani 1 1 d G . . C4 C 0.1058(5) 0.2466(5) 0.5656(4) 0.059(4) Uani 1 1 d GU . . H4 H 0.1415 0.2463 0.5989 0.071 Uiso 1 1 calc R . . C5 C 0.0858(6) 0.3248(4) 0.5367(5) 0.054(3) Uani 1 1 d GU . . H5 H 0.1079 0.3780 0.5503 0.065 Uiso 1 1 calc R . . N2 N 0.0411(5) -0.4542(4) 0.4840(5) 0.048(3) Uani 1 1 d GU . . C7 C 0.1089(5) -0.4477(5) 0.5153(5) 0.053(3) Uani 1 1 d GU . . H7 H 0.1419 -0.4961 0.5159 0.064 Uiso 1 1 calc R . . C8 C 0.1286(5) -0.3703(6) 0.5455(5) 0.062(5) Uani 1 1 d G . . H8 H 0.1750 -0.3658 0.5668 0.074 Uiso 1 1 calc R . . C9 C 0.0804(6) -0.2995(5) 0.5444(5) 0.038(4) Uani 1 1 d G . . C10 C 0.0125(5) -0.3060(5) 0.5132(5) 0.050(4) Uani 1 1 d G . . H10 H -0.0204 -0.2576 0.5125 0.060 Uiso 1 1 calc R . . C11 C -0.0071(5) -0.3834(6) 0.4830(5) 0.050(3) Uani 1 1 d GU . . H11 H -0.0535 -0.3878 0.4617 0.060 Uiso 1 1 calc R . . N3 N 0.3986(5) -0.0608(4) 0.8721(4) 0.040(3) Uani 1 1 d GU . . C13 C 0.3905(6) 0.0136(4) 0.8348(5) 0.046(3) Uani 1 1 d GU . . H13 H 0.4189 0.0643 0.8440 0.056 Uiso 1 1 calc R . . C14 C 0.3409(6) 0.0137(4) 0.7840(4) 0.056(5) Uani 1 1 d G . . H14 H 0.3354 0.0645 0.7585 0.067 Uiso 1 1 calc R . . C15 C 0.2993(5) -0.0605(5) 0.7706(4) 0.035(4) Uani 1 1 d G . . C16 C 0.3074(5) -0.1349(4) 0.8079(5) 0.036(4) Uani 1 1 d G . . H16 H 0.2790 -0.1856 0.7987 0.043 Uiso 1 1 calc R . . C17 C 0.3571(5) -0.1350(4) 0.8587(4) 0.040(3) Uani 1 1 d GU . . H17 H 0.3626 -0.1858 0.8842 0.048 Uiso 1 1 calc R . . C6 C 0.1027(12) 0.0855(9) 0.5752(7) 0.043(5) Uani 1 1 d . . . N4 N 0.0696(7) 0.0107(6) 0.5501(6) 0.029(3) Uani 1 1 d . . . C19 C 0.0979(9) -0.0651(7) 0.5729(7) 0.027(3) Uani 1 1 d . . . N5 N 0.0726(7) -0.1422(6) 0.5485(5) 0.027(3) Uani 1 1 d . . . C12 C 0.1038(10) -0.2135(9) 0.5707(7) 0.039(4) Uani 1 1 d . . . N6 N 0.1554(8) -0.2219(7) 0.6209(6) 0.034(3) Uani 1 1 d . . . C20 C 0.1762(9) -0.1406(8) 0.6444(7) 0.036(4) Uani 1 1 d . . . N7 N 0.2251(8) -0.1421(7) 0.6944(6) 0.038(3) Uani 1 1 d . . . C18 C 0.2476(9) -0.0610(8) 0.7136(8) 0.035(4) Uani 1 1 d . . . N8 N 0.2255(6) 0.0175(6) 0.6943(6) 0.028(3) Uani 1 1 d . . . C21 C 0.1750(8) 0.0157(8) 0.6464(7) 0.031(3) Uani 1 1 d . . . N9 N 0.1520(6) 0.0912(6) 0.6205(5) 0.022(3) Uani 1 1 d . . . C22 C 0.1478(9) -0.0641(7) 0.6212(7) 0.029(4) Uani 1 1 d . . . I1 I -0.09867(7) 0.43253(7) 0.37130(6) 0.0526(3) Uani 1 1 d . . . Zn1 Zn 0.01736(11) 0.43544(9) 0.43548(8) 0.0342(5) Uani 1 1 d . . . N11 N 0.4616(6) 0.4657(5) 0.7092(5) 0.047(3) Uani 1 1 d G . . C29 C 0.3959(7) 0.4602(5) 0.6747(7) 0.133(14) Uani 1 1 d G . . H29 H 0.3661 0.5107 0.6686 0.160 Uiso 1 1 calc R . . C30 C 0.3736(8) 0.3807(7) 0.6491(8) 0.128(13) Uani 1 1 d G . . H30 H 0.3287 0.3769 0.6255 0.154 Uiso 1 1 calc R . . C31 C 0.4171(8) 0.3068(5) 0.6579(7) 0.059(5) Uani 1 1 d GU . . C32 C 0.4829(7) 0.3123(6) 0.6925(7) 0.063(5) Uani 1 1 d GU . . H32 H 0.5126 0.2617 0.6985 0.075 Uiso 1 1 calc R . . C33 C 0.5051(5) 0.3918(7) 0.7181(6) 0.073(6) Uani 1 1 d GU . . H33 H 0.5500 0.3955 0.7417 0.088 Uiso 1 1 calc R . . N10 N 0.4674(5) -0.3131(4) 0.7072(5) 0.046(3) Uani 1 1 d GU . . C23 C 0.4960(5) -0.2353(6) 0.7307(4) 0.039(3) Uani 1 1 d GU . . H23 H 0.5296 -0.2361 0.7657 0.047 Uiso 1 1 calc R . . C24 C 0.4756(6) -0.1564(5) 0.7031(5) 0.044(4) Uani 1 1 d GU . . H24 H 0.4952 -0.1032 0.7192 0.053 Uiso 1 1 calc R . . C25 C 0.4265(8) -0.1553(5) 0.6520(6) 0.071(4) Uani 1 1 d GU . . C26 C 0.3978(8) -0.2331(6) 0.6284(6) 0.075(4) Uani 1 1 d GU . . H26 H 0.3643 -0.2324 0.5935 0.090 Uiso 1 1 calc R . . C27 C 0.4183(7) -0.3120(5) 0.6560(6) 0.078(4) Uani 1 1 d GU . . H27 H 0.3987 -0.3652 0.6399 0.094 Uiso 1 1 calc R . . N12 N 0.1014(5) 0.0723(5) 0.3270(4) 0.037(3) Uani 1 1 d G . . C35 C 0.1050(5) 0.0005(4) 0.3673(5) 0.047(4) Uani 1 1 d G . . H35 H 0.0738 -0.0485 0.3599 0.057 Uiso 1 1 calc R . . C36 C 0.1540(6) 0.0004(4) 0.4185(4) 0.039(4) Uani 1 1 d G . . H36 H 0.1564 -0.0487 0.4461 0.046 Uiso 1 1 calc R . . C37 C 0.1996(5) 0.0721(5) 0.4293(4) 0.032(3) Uani 1 1 d G . . C38 C 0.1960(5) 0.1440(4) 0.3890(5) 0.050(5) Uani 1 1 d G . . H38 H 0.2272 0.1930 0.3964 0.061 Uiso 1 1 calc R . . C39 C 0.1470(5) 0.1441(4) 0.3378(4) 0.052(4) Uani 1 1 d G . . H39 H 0.1446 0.1932 0.3102 0.062 Uiso 1 1 calc R . . C28 C 0.4014(9) -0.0733(8) 0.6255(9) 0.031(4) Uani 1 1 d . . . N13 N 0.4336(8) -0.0006(7) 0.6495(8) 0.047(4) Uani 1 1 d . . . C41 C 0.4076(10) 0.0745(10) 0.6273(12) 0.053(6) Uani 1 1 d . . . N14 N 0.4293(9) 0.1538(9) 0.6483(8) 0.061(5) Uani 1 1 d . . . C34 C 0.3963(10) 0.2231(8) 0.6233(8) 0.032(4) Uani 1 1 d . . . N15 N 0.3487(9) 0.2274(8) 0.5814(8) 0.054(5) Uani 1 1 d . . . C42 C 0.3234(10) 0.1526(8) 0.5516(7) 0.039(4) Uani 1 1 d . . . N16 N 0.2721(7) 0.1517(7) 0.5052(7) 0.037(3) Uani 1 1 d . . . C40 C 0.2550(10) 0.0742(8) 0.4839(8) 0.036(4) Uani 1 1 d . . . N17 N 0.2713(8) -0.0058(7) 0.5076(7) 0.047(4) Uani 1 1 d . . . C43 C 0.3266(9) -0.0053(9) 0.5531(7) 0.033(3) Uani 1 1 d . . . N18 N 0.3519(10) -0.0814(7) 0.5803(8) 0.058(6) Uani 1 1 d . . . C44 C 0.3504(9) 0.0763(8) 0.5750(9) 0.035(4) Uani 1 1 d . . . I2 I 0.59842(8) 0.57972(9) 0.82659(8) 0.0742(5) Uani 1 1 d . . . Zn2 Zn 0.48219(12) 0.57593(9) 0.76106(10) 0.0424(5) Uani 1 1 d . . . O1 O 0.2668(12) -0.3310(15) 0.7049(11) 0.149(8) Uiso 1 1 d DU . . C45 C 0.2047(13) -0.3680(16) 0.7296(13) 0.098(8) Uiso 1 1 d DU . . O2 O -0.201(2) 0.132(3) 0.4648(18) 0.261(17) Uiso 1 1 d DU . . C46 C -0.2434(18) 0.123(2) 0.5184(16) 0.129(10) Uiso 1 1 d DU . . O3 O -0.236(2) -0.297(2) 0.4650(19) 0.235(14) Uiso 1 1 d DU . . C47 C -0.221(5) -0.212(3) 0.477(5) 0.37(4) Uiso 1 1 d DU . . O4 O -0.098(2) -0.061(2) 0.493(2) 0.232(16) Uiso 1 1 d DU . . C48 C -0.058(3) -0.108(4) 0.449(2) 0.24(2) Uiso 1 1 d DU . . O5 O 0.055(3) -0.245(4) 0.353(4) 0.42(3) Uiso 1 1 d DU . . C49 C 0.129(3) -0.240(3) 0.336(3) 0.220(19) Uiso 1 1 d DU . . O6 O -0.299(3) 0.298(3) 0.785(3) 0.39(3) Uiso 1 1 d DU . . C50 C -0.305(3) 0.209(3) 0.780(3) 0.24(2) Uiso 1 1 d DU . . O7 O -0.301(2) 0.053(2) 0.616(2) 0.228(14) Uiso 1 1 d DU . . C51 C -0.357(4) 0.070(5) 0.660(3) 0.35(4) Uiso 1 1 d DU . . 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 N1 0.060(7) 0.031(5) 0.027(6) -0.005(4) -0.030(5) 0.006(5) C1 0.057(11) 0.018(6) 0.057(11) 0.011(7) 0.014(8) -0.003(6) C2 0.044(9) 0.032(7) 0.030(8) -0.001(6) 0.002(7) 0.012(6) C3 0.017(5) 0.018(5) 0.010(5) -0.005(4) 0.004(5) -0.004(4) C4 0.086(9) 0.028(5) 0.063(8) 0.008(5) -0.057(7) -0.001(6) C5 0.082(7) 0.037(5) 0.044(6) 0.015(5) -0.049(6) 0.000(5) N2 0.066(7) 0.029(4) 0.048(6) 0.024(4) -0.008(5) -0.010(5) C7 0.072(7) 0.034(5) 0.054(7) 0.018(5) -0.007(6) -0.006(5) C8 0.121(16) 0.030(7) 0.036(9) -0.007(6) -0.037(10) 0.004(9) C9 0.062(11) 0.033(7) 0.019(7) -0.013(6) 0.006(7) -0.017(7) C10 0.041(9) 0.046(8) 0.063(12) 0.009(8) -0.018(8) -0.004(7) C11 0.067(7) 0.036(5) 0.047(7) 0.017(5) -0.008(6) -0.008(5) N3 0.058(6) 0.015(4) 0.048(6) 0.004(4) 0.009(6) 0.004(4) C13 0.074(8) 0.028(5) 0.037(7) 0.008(6) -0.008(7) -0.009(6) C14 0.102(15) 0.016(6) 0.049(10) -0.001(6) -0.020(10) -0.009(7) C15 0.045(10) 0.031(7) 0.028(8) 0.012(5) -0.001(8) -0.001(6) C16 0.030(8) 0.035(7) 0.044(10) 0.019(6) -0.008(7) -0.008(6) C17 0.051(7) 0.014(5) 0.055(8) 0.003(5) -0.006(7) -0.007(5) C6 0.080(15) 0.042(8) 0.007(7) 0.007(5) -0.008(8) -0.004(8) N4 0.043(7) 0.017(5) 0.028(6) -0.004(4) -0.012(6) -0.006(5) C19 0.045(10) 0.017(6) 0.020(7) -0.006(5) 0.004(7) -0.007(5) N5 0.050(7) 0.020(5) 0.012(5) 0.009(4) -0.012(5) -0.015(5) C12 0.066(11) 0.026(7) 0.024(8) -0.019(6) -0.001(8) -0.010(7) N6 0.058(9) 0.022(5) 0.022(6) 0.007(4) -0.014(6) -0.004(5) C20 0.049(10) 0.029(7) 0.029(8) -0.006(6) 0.010(8) 0.005(6) N7 0.058(9) 0.032(6) 0.025(7) -0.008(5) -0.022(6) 0.011(6) C18 0.041(9) 0.020(6) 0.044(10) 0.005(6) 0.027(8) 0.000(5) N8 0.031(6) 0.026(5) 0.029(6) -0.016(5) -0.011(5) -0.003(4) C21 0.036(8) 0.021(6) 0.036(9) 0.005(6) 0.013(7) 0.009(5) N9 0.029(6) 0.019(4) 0.018(6) -0.003(4) -0.019(5) -0.005(4) C22 0.053(11) 0.023(6) 0.011(7) 0.007(5) 0.015(7) -0.005(6) I1 0.0448(7) 0.0689(7) 0.0441(7) -0.0006(6) -0.0047(7) 0.0028(5) Zn1 0.0519(12) 0.0236(7) 0.0271(9) -0.0009(6) -0.0057(9) -0.0029(7) N11 0.052(8) 0.059(8) 0.031(7) 0.015(6) 0.009(6) -0.013(7) C29 0.21(3) 0.028(9) 0.16(3) -0.029(13) -0.08(3) 0.018(14) C30 0.20(3) 0.026(9) 0.16(3) -0.028(12) -0.10(2) 0.021(13) C31 0.081(13) 0.030(8) 0.066(12) 0.015(8) 0.009(11) 0.004(8) C32 0.074(12) 0.030(7) 0.085(13) -0.014(8) 0.040(10) 0.001(8) C33 0.096(14) 0.054(10) 0.070(13) -0.018(9) 0.038(11) -0.016(10) N10 0.031(7) 0.053(7) 0.052(9) -0.025(6) 0.026(6) 0.001(5) C23 0.034(9) 0.049(8) 0.035(8) 0.005(7) 0.004(7) 0.005(6) C24 0.062(11) 0.035(7) 0.035(9) 0.003(6) 0.011(8) -0.006(7) C25 0.115(12) 0.026(6) 0.072(9) -0.003(6) -0.018(8) -0.002(6) C26 0.121(11) 0.028(5) 0.076(8) -0.006(5) -0.022(8) -0.004(6) C27 0.124(12) 0.032(6) 0.079(9) 0.001(6) -0.020(9) -0.005(6) N12 0.056(8) 0.024(5) 0.032(7) -0.013(5) 0.021(6) 0.006(5) C35 0.070(11) 0.022(6) 0.050(9) -0.012(7) -0.001(9) -0.003(7) C36 0.055(10) 0.022(6) 0.039(9) 0.006(5) 0.006(8) 0.001(6) C37 0.039(9) 0.031(6) 0.025(8) 0.002(5) 0.010(7) 0.005(5) C38 0.059(11) 0.040(8) 0.052(12) -0.016(7) 0.004(9) 0.016(7) C39 0.031(8) 0.078(11) 0.046(11) -0.012(8) 0.001(8) 0.015(8) C28 0.025(8) 0.025(7) 0.043(9) -0.022(6) 0.004(7) -0.009(5) N13 0.055(9) 0.024(6) 0.064(9) 0.001(5) 0.024(8) 0.006(6) C41 0.031(10) 0.043(9) 0.085(16) 0.019(8) 0.020(10) -0.001(7) N14 0.072(11) 0.041(8) 0.071(11) -0.020(7) 0.040(9) 0.005(7) C34 0.047(10) 0.016(6) 0.034(8) 0.017(5) 0.013(8) 0.003(6) N15 0.060(11) 0.032(7) 0.068(12) -0.018(6) 0.040(9) -0.006(6) C42 0.070(12) 0.023(6) 0.023(8) 0.007(5) 0.008(8) 0.000(7) N16 0.043(8) 0.026(6) 0.042(9) -0.004(5) 0.021(7) 0.003(5) C40 0.050(10) 0.037(8) 0.020(8) -0.008(5) -0.004(8) 0.008(6) N17 0.067(10) 0.012(5) 0.060(9) 0.003(5) 0.024(8) 0.002(5) C43 0.042(9) 0.035(7) 0.023(8) -0.007(6) -0.002(7) 0.001(6) N18 0.093(14) 0.013(5) 0.066(12) 0.008(5) 0.062(11) 0.009(6) C44 0.031(9) 0.031(7) 0.043(10) -0.003(6) 0.005(8) 0.003(5) I2 0.0499(9) 0.0911(10) 0.0817(12) 0.0106(8) 0.0103(9) 0.0096(6) Zn2 0.0560(13) 0.0269(8) 0.0443(12) -0.0012(7) 0.0045(11) 0.0043(7) _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 N1 C1 1.3900 . ? N1 C5 1.3900 . ? N1 Zn1 2.035(6) . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C6 1.515(16) . ? C4 C5 1.3900 . ? N2 C7 1.3900 . ? N2 C11 1.3900 . ? N2 Zn1 2.019(7) 1_545 ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C9 C12 1.489(14) . ? C10 C11 1.3900 . ? N3 C13 1.3900 . ? N3 C17 1.3900 . ? N3 Zn1 2.015(7) 3_545 ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 C18 1.515(19) . ? C16 C17 1.3900 . ? C6 N9 1.30(2) . ? C6 N4 1.395(18) . ? N4 C19 1.355(17) . ? C19 C22 1.35(2) . ? C19 N5 1.366(15) . ? N5 C12 1.314(19) . ? C12 N6 1.41(2) . ? N6 C20 1.391(17) . ? C20 C22 1.369(19) . ? C20 N7 1.37(2) . ? N7 C18 1.368(18) . ? C18 N8 1.329(17) . ? N8 C21 1.354(19) . ? C21 N9 1.343(16) . ? C21 C22 1.420(19) . ? I1 Zn1 2.486(2) . ? Zn1 N3 2.015(7) 3_554 ? Zn1 N2 2.019(7) 1_565 ? N11 C29 1.3900 . ? N11 C33 1.3900 . ? N11 Zn2 2.043(8) . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C31 C34 1.520(17) . ? C32 C33 1.3900 . ? N10 C23 1.3900 . ? N10 C27 1.3900 . ? N10 Zn2 2.058(7) 1_545 ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 C28 1.447(17) . ? C26 C27 1.3900 . ? N12 C35 1.3900 . ? N12 C39 1.3900 . ? N12 Zn2 2.045(8) 3_544 ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C37 C40 1.519(18) . ? C38 C39 1.3900 . ? C28 N18 1.31(2) . ? C28 N13 1.353(18) . ? N13 C41 1.33(2) . ? C41 N14 1.35(2) . ? C41 C44 1.50(3) . ? N14 C34 1.32(2) . ? C34 N15 1.23(2) . ? N15 C42 1.382(19) . ? C42 N16 1.34(2) . ? C42 C44 1.359(19) . ? N16 C40 1.306(17) . ? C40 N17 1.355(18) . ? N17 C43 1.38(2) . ? C43 N18 1.375(19) . ? C43 C44 1.399(19) . ? I2 Zn2 2.504(3) . ? Zn2 N12 2.045(8) 3 ? Zn2 N10 2.058(7) 1_565 ? O1 C45 1.356(14) . ? O2 C46 1.362(15) . ? O3 C47 1.365(15) . ? O4 C48 1.369(15) . ? O5 C49 1.382(15) . ? O6 C50 1.370(15) . ? O7 C51 1.391(15) . ? 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 C1 N1 C5 120.0 . . ? C1 N1 Zn1 119.2(4) . . ? C5 N1 Zn1 119.9(4) . . ? N1 C1 C2 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C6 122.8(8) . . ? C4 C3 C6 117.0(8) . . ? C3 C4 C5 120.0 . . ? C4 C5 N1 120.0 . . ? C7 N2 C11 120.0 . . ? C7 N2 Zn1 118.9(5) . 1_545 ? C11 N2 Zn1 120.9(5) . 1_545 ? N2 C7 C8 120.0 . . ? C9 C8 C7 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 C12 119.1(9) . . ? C8 C9 C12 120.6(9) . . ? C9 C10 C11 120.0 . . ? C10 C11 N2 120.0 . . ? C13 N3 C17 120.0 . . ? C13 N3 Zn1 118.3(4) . 3_545 ? C17 N3 Zn1 121.0(4) . 3_545 ? C14 C13 N3 120.0 . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 C18 119.6(7) . . ? C16 C15 C18 120.3(7) . . ? C17 C16 C15 120.0 . . ? C16 C17 N3 120.0 . . ? N9 C6 N4 128.4(13) . . ? N9 C6 C3 118.6(12) . . ? N4 C6 C3 112.9(13) . . ? C19 N4 C6 114.3(12) . . ? C22 C19 N4 120.2(11) . . ? C22 C19 N5 120.8(12) . . ? N4 C19 N5 119.0(13) . . ? C12 N5 C19 116.3(12) . . ? N5 C12 N6 128.5(11) . . ? N5 C12 C9 118.9(13) . . ? N6 C12 C9 112.5(12) . . ? C20 N6 C12 111.1(11) . . ? C22 C20 N7 121.8(13) . . ? C22 C20 N6 122.7(15) . . ? N7 C20 N6 115.4(12) . . ? C18 N7 C20 113.6(12) . . ? N8 C18 N7 130.1(16) . . ? N8 C18 C15 114.9(11) . . ? N7 C18 C15 114.7(11) . . ? C18 N8 C21 114.1(11) . . ? N9 C21 N8 119.3(12) . . ? N9 C21 C22 119.0(14) . . ? N8 C21 C22 121.7(11) . . ? C6 N9 C21 116.5(12) . . ? C19 C22 C20 120.2(13) . . ? C19 C22 C21 121.2(12) . . ? C20 C22 C21 118.4(15) . . ? N3 Zn1 N2 98.6(4) 3_554 1_565 ? N3 Zn1 N1 105.7(4) 3_554 . ? N2 Zn1 N1 113.1(4) 1_565 . ? N3 Zn1 I1 105.9(3) 3_554 . ? N2 Zn1 I1 117.8(3) 1_565 . ? N1 Zn1 I1 113.5(2) . . ? C29 N11 C33 120.0 . . ? C29 N11 Zn2 118.8(6) . . ? C33 N11 Zn2 120.0(6) . . ? N11 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 C34 120.7(10) . . ? C30 C31 C34 119.0(10) . . ? C31 C32 C33 120.0 . . ? C32 C33 N11 120.0 . . ? C23 N10 C27 120.0 . . ? C23 N10 Zn2 117.7(5) . 1_545 ? C27 N10 Zn2 121.1(5) . 1_545 ? C24 C23 N10 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 C28 119.5(9) . . ? C24 C25 C28 120.4(9) . . ? C25 C26 C27 120.0 . . ? C26 C27 N10 120.0 . . ? C35 N12 C39 120.0 . . ? C35 N12 Zn2 117.8(4) . 3_544 ? C39 N12 Zn2 121.6(4) . 3_544 ? C36 C35 N12 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 C40 118.2(8) . . ? C36 C37 C40 121.8(7) . . ? C39 C38 C37 120.0 . . ? C38 C39 N12 120.0 . . ? N18 C28 N13 129.8(15) . . ? N18 C28 C25 114.2(10) . . ? N13 C28 C25 116.0(15) . . ? C41 N13 C28 115.6(17) . . ? N13 C41 N14 124(2) . . ? N13 C41 C44 120.9(16) . . ? N14 C41 C44 114.7(15) . . ? C34 N14 C41 117.7(19) . . ? N15 C34 N14 129.6(16) . . ? N15 C34 C31 117.9(12) . . ? N14 C34 C31 112.2(15) . . ? C34 N15 C42 120.6(15) . . ? N16 C42 C44 120.0(14) . . ? N16 C42 N15 124.3(14) . . ? C44 C42 N15 115.6(16) . . ? C40 N16 C42 114.8(13) . . ? N16 C40 N17 130.3(16) . . ? N16 C40 C37 115.6(12) . . ? N17 C40 C37 113.6(12) . . ? C40 N17 C43 113.9(13) . . ? N18 C43 N17 121.4(14) . . ? N18 C43 C44 121.3(15) . . ? N17 C43 C44 117.0(13) . . ? C28 N18 C43 116.5(13) . . ? C42 C44 C43 122.7(16) . . ? C42 C44 C41 121.6(13) . . ? C43 C44 C41 115.6(13) . . ? N11 Zn2 N12 101.8(4) . 3 ? N11 Zn2 N10 111.5(5) . 1_565 ? N12 Zn2 N10 107.3(4) 3 1_565 ? N11 Zn2 I2 117.6(3) . . ? N12 Zn2 I2 104.2(3) 3 . ? N10 Zn2 I2 113.0(3) 1_565 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.873 _refine_diff_density_min -1.502 _refine_diff_density_rms 0.200 _database_code_depnum_ccdc_archive 'CCDC 944048' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), (I 0.5-), (Cl 0.5-),(C22 H12 N9 1-), (H2 O1), 7(H2 O1)' _chemical_formula_sum 'C22 H28 Cl0.50 I0.50 N9 O8 Zn' _chemical_formula_weight 693.08 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' I I -0.4742 1.8119 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.47(2) _cell_length_b 15.79(1) _cell_length_c 13.591(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.64(2) _cell_angle_gamma 90.00 _cell_volume 5468(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36789 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 26.32 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 1.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8334 _exptl_absorpt_correction_T_max 0.9692 _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 'microfocus source 30W maximum continuous power' _diffrn_radiation_monochromator 'Wuazar(TM) Montel multilayer optic' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36789 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.32 _reflns_number_total 5553 _reflns_number_gt 3852 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 sofware Suite' _computing_cell_refinement 'APEX2 sofware Suite' _computing_data_reduction 'APEX2 sofware Suite' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; The occupancy factors of the disordered I and Cl are 0.5 and 0.5. Several solvents were refined with isotropic thermal parameters. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+50.7365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5553 _refine_ls_number_parameters 397 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.41059(16) 1.0218(2) 0.6313(3) 0.0246(10) Uani 1 1 d . A . C1 C 0.4571(2) 1.0162(3) 0.6096(5) 0.0382(15) Uani 1 1 d . . . H1 H 0.4731 1.0668 0.5945 0.046 Uiso 1 1 calc R . . C2 C 0.4824(2) 0.9411(3) 0.6083(5) 0.0331(14) Uani 1 1 d . . . H2 H 0.5157 0.9404 0.5945 0.040 Uiso 1 1 calc R . . C3 C 0.4597(2) 0.8657(3) 0.6271(4) 0.0216(10) Uani 1 1 d . . . C4 C 0.4115(2) 0.8714(3) 0.6504(4) 0.0269(12) Uani 1 1 d . . . H4 H 0.3944 0.8217 0.6642 0.032 Uiso 1 1 calc R . . C5 C 0.3890(2) 0.9501(3) 0.6533(5) 0.0303(13) Uani 1 1 d . . . H5 H 0.3569 0.9534 0.6716 0.036 Uiso 1 1 calc R . . N2 N 0.79858(17) 0.6388(2) 0.6351(3) 0.0244(9) Uani 1 1 d . . . C7 C 0.7657(2) 0.5839(3) 0.5774(4) 0.0275(12) Uani 1 1 d . . . H7 H 0.7789 0.5458 0.5361 0.033 Uiso 1 1 calc R . . C8 C 0.7134(2) 0.5793(3) 0.5746(4) 0.0267(11) Uani 1 1 d . . . H8 H 0.6917 0.5367 0.5354 0.032 Uiso 1 1 calc R . . C9 C 0.69257(19) 0.6383(3) 0.6301(4) 0.0216(10) Uani 1 1 d . . . C10 C 0.7268(2) 0.6982(3) 0.6874(4) 0.0284(12) Uani 1 1 d . . . H10 H 0.7140 0.7405 0.7242 0.034 Uiso 1 1 calc R . . C11 C 0.7792(2) 0.6958(3) 0.6905(4) 0.0294(12) Uani 1 1 d . . . H11 H 0.8025 0.7352 0.7325 0.035 Uiso 1 1 calc R . . N3 N 0.41150(16) 0.2537(2) 0.6346(3) 0.0205(9) Uani 1 1 d . . . C13 C 0.3867(2) 0.3265(3) 0.6409(4) 0.0279(12) Uani 1 1 d . . . H13 H 0.3518 0.3240 0.6471 0.033 Uiso 1 1 calc R . . C14 C 0.4094(2) 0.4054(3) 0.6390(4) 0.0256(11) Uani 1 1 d . . . H14 H 0.3905 0.4555 0.6445 0.031 Uiso 1 1 calc R . . C15 C 0.46043(18) 0.4104(3) 0.6290(3) 0.0167(10) Uani 1 1 d . . . C16 C 0.4861(2) 0.3339(3) 0.6221(4) 0.0205(10) Uani 1 1 d . . . H16 H 0.5208 0.3343 0.6149 0.025 Uiso 1 1 calc R . . C17 C 0.46085(19) 0.2583(3) 0.6256(4) 0.0208(10) Uani 1 1 d . . . H17 H 0.4790 0.2070 0.6216 0.025 Uiso 1 1 calc R . . C6 C 0.48644(19) 0.7826(3) 0.6250(4) 0.0187(10) Uani 1 1 d . . . N4 N 0.53744(16) 0.7896(2) 0.6236(3) 0.0199(9) Uani 1 1 d . . . C19 C 0.56296(19) 0.7150(3) 0.6265(4) 0.0172(10) Uani 1 1 d . . . N5 N 0.61423(16) 0.7144(2) 0.6263(3) 0.0214(9) Uani 1 1 d . . . C12 C 0.63587(19) 0.6373(3) 0.6276(4) 0.0199(10) Uani 1 1 d . . . N6 N 0.61483(16) 0.5604(2) 0.6279(3) 0.0207(9) Uani 1 1 d . . . C20 C 0.56333(19) 0.5601(3) 0.6281(4) 0.0176(10) Uani 1 1 d . . . N7 N 0.53792(16) 0.4867(2) 0.6266(3) 0.0183(8) Uani 1 1 d . . . C18 C 0.48701(18) 0.4936(3) 0.6272(3) 0.0155(10) Uani 1 1 d . . . N8 N 0.45820(15) 0.5628(2) 0.6279(3) 0.0168(8) Uani 1 1 d . . . C21 C 0.48397(18) 0.6383(3) 0.6279(3) 0.0173(9) Uani 1 1 d . . . C22 C 0.53660(19) 0.6379(3) 0.6288(3) 0.0174(9) Uani 1 1 d . . . N9 N 0.45794(16) 0.7131(2) 0.6263(3) 0.0195(9) Uani 1 1 d . . . Zn1 Zn 0.37712(2) 1.13829(3) 0.64126(5) 0.02701(19) Uani 1 1 d . . . O1W O 0.35722(17) 1.1419(2) 0.4750(3) 0.0340(9) Uani 1 1 d D A . I1 I 0.40814(19) 1.1465(2) 0.8520(3) 0.0373(7) Uani 0.50 1 d P A 1 Cl1 Cl 0.4106(6) 1.1291(9) 0.8379(13) 0.036(3) Uani 0.50 1 d P A 2 O2W O 0.1640(3) 0.8948(4) 0.6642(6) 0.093(2) Uani 1 1 d U . . O3W O 0.1574(13) 0.7582(15) 0.5451(17) 0.51(2) Uani 1 1 d U . . O4W O 0.3446(3) 0.6232(8) 0.6042(10) 0.182(5) Uani 1 1 d U . . O5W O 0.2710(3) 0.8881(5) 0.6863(8) 0.130(3) Uani 1 1 d U . . O8W O 0.2129(6) 1.0063(14) 0.3379(13) 0.323(12) Uani 1 1 d U . . O9W O 0.3185(3) 1.0046(4) 0.3553(5) 0.099(2) Uani 1 1 d U . . O6W O 0.2655(8) 0.8858(13) 0.4509(14) 0.144(8) Uani 0.50 1 d PU B 1 O7W O 0.2887(10) 0.7720(19) 0.559(2) 0.205(12) Uani 0.50 1 d PU C 2 H1W H 0.363(2) 1.181(3) 0.440(4) 0.033(17) Uiso 1 1 d D . . H2W H 0.349(2) 1.101(3) 0.435(4) 0.040(19) Uiso 1 1 d 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 N1 0.020(2) 0.0129(19) 0.043(3) 0.0027(18) 0.0121(19) 0.0021(17) C1 0.033(3) 0.012(2) 0.077(5) -0.000(3) 0.028(3) -0.003(2) C2 0.023(3) 0.017(3) 0.067(4) 0.001(3) 0.025(3) -0.000(2) C3 0.022(3) 0.012(2) 0.032(3) -0.000(2) 0.009(2) 0.002(2) C4 0.025(3) 0.010(2) 0.050(3) 0.005(2) 0.017(2) 0.001(2) C5 0.023(3) 0.019(2) 0.054(4) 0.009(2) 0.019(3) 0.002(2) N2 0.028(2) 0.0115(18) 0.040(3) 0.0013(18) 0.020(2) 0.0019(18) C7 0.026(3) 0.020(2) 0.041(3) 0.001(2) 0.016(2) 0.004(2) C8 0.025(3) 0.017(2) 0.039(3) -0.001(2) 0.010(2) -0.001(2) C9 0.022(3) 0.016(2) 0.031(3) 0.003(2) 0.014(2) 0.000(2) C10 0.028(3) 0.018(2) 0.043(3) -0.003(2) 0.017(2) 0.000(2) C11 0.028(3) 0.020(2) 0.043(3) -0.005(2) 0.015(2) -0.004(2) N3 0.021(2) 0.0097(18) 0.031(2) -0.0025(16) 0.0082(18) -0.0010(16) C13 0.021(3) 0.017(2) 0.048(3) -0.003(2) 0.014(2) -0.004(2) C14 0.020(3) 0.013(2) 0.044(3) -0.002(2) 0.010(2) 0.001(2) C15 0.018(2) 0.013(2) 0.019(2) 0.0017(18) 0.0056(18) -0.0030(19) C16 0.021(3) 0.017(2) 0.026(3) -0.0009(19) 0.010(2) 0.0001(19) C17 0.022(3) 0.011(2) 0.032(3) -0.002(2) 0.011(2) -0.0000(19) C6 0.019(2) 0.015(2) 0.023(3) 0.0043(19) 0.007(2) 0.0026(19) N4 0.018(2) 0.0141(19) 0.030(2) 0.0026(17) 0.0116(17) -0.0002(16) C19 0.022(3) 0.009(2) 0.022(2) -0.0008(18) 0.009(2) -0.0029(18) N5 0.023(2) 0.0125(19) 0.031(2) 0.0003(17) 0.0114(18) 0.0015(16) C12 0.019(2) 0.017(2) 0.025(2) 0.002(2) 0.0075(19) 0.000(2) N6 0.023(2) 0.0118(19) 0.029(2) -0.0004(16) 0.0116(18) 0.0025(16) C20 0.023(3) 0.014(2) 0.018(2) -0.0002(18) 0.0107(19) -0.0010(19) N7 0.023(2) 0.0098(18) 0.024(2) 0.0008(16) 0.0089(17) -0.0007(16) C18 0.018(2) 0.013(2) 0.015(2) 0.0004(17) 0.0041(19) -0.0017(18) N8 0.019(2) 0.0110(18) 0.021(2) 0.0005(15) 0.0071(16) -0.0029(16) C21 0.020(2) 0.014(2) 0.018(2) 0.0013(19) 0.0069(18) 0.001(2) C22 0.025(3) 0.012(2) 0.016(2) 0.0012(19) 0.0077(18) 0.000(2) N9 0.019(2) 0.0123(19) 0.029(2) 0.0015(17) 0.0089(17) 0.0012(16) Zn1 0.0210(3) 0.0092(3) 0.0558(4) -0.0016(3) 0.0190(3) -0.0013(2) O1W 0.046(2) 0.0189(19) 0.042(2) -0.0010(19) 0.020(2) -0.0085(19) I1 0.0327(9) 0.0427(18) 0.0348(8) 0.0043(11) 0.0060(5) -0.0033(11) Cl1 0.019(2) 0.025(4) 0.058(7) -0.000(3) -0.000(3) 0.001(2) O2W 0.091(5) 0.062(4) 0.150(6) 0.046(4) 0.074(5) 0.039(3) O3W 0.76(5) 0.35(3) 0.25(2) 0.09(2) -0.14(3) -0.19(3) O4W 0.070(6) 0.251(14) 0.221(12) -0.049(10) 0.029(7) -0.018(7) O5W 0.119(7) 0.088(5) 0.195(9) 0.037(6) 0.061(6) 0.013(5) O8W 0.216(15) 0.47(3) 0.279(18) -0.24(2) 0.052(13) 0.014(17) O9W 0.114(6) 0.080(4) 0.108(5) -0.056(4) 0.037(4) -0.031(4) O6W 0.163(17) 0.172(17) 0.123(14) -0.093(13) 0.081(13) -0.085(14) O7W 0.20(2) 0.26(3) 0.19(2) -0.10(2) 0.097(19) -0.07(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 N1 C5 1.337(6) . ? N1 C1 1.344(7) . ? N1 Zn1 2.061(4) . ? C1 C2 1.363(7) . ? C2 C3 1.387(7) . ? C3 C4 1.398(7) . ? C3 C6 1.495(6) . ? C4 C5 1.383(7) . ? N2 C7 1.325(7) . ? N2 C11 1.360(7) . ? N2 Zn1 2.058(5) 3_545 ? C7 C8 1.375(7) . ? C8 C9 1.402(7) . ? C9 C10 1.394(7) . ? C9 C12 1.492(7) . ? C10 C11 1.378(7) . ? N3 C13 1.337(6) . ? N3 C17 1.346(6) . ? N3 Zn1 2.050(4) 1_545 ? C13 C14 1.386(7) . ? C14 C15 1.395(7) . ? C15 C16 1.401(7) . ? C15 C18 1.493(6) . ? C16 C17 1.375(7) . ? C6 N9 1.334(6) . ? C6 N4 1.359(6) . ? N4 C19 1.354(6) . ? C19 N5 1.358(6) . ? C19 C22 1.408(6) . ? N5 C12 1.343(6) . ? C12 N6 1.336(6) . ? N6 C20 1.364(6) . ? C20 N7 1.337(6) . ? C20 C22 1.419(6) . ? N7 C18 1.354(6) . ? C18 N8 1.334(6) . ? N8 C21 1.373(6) . ? C21 N9 1.363(6) . ? C21 C22 1.390(7) . ? Zn1 N3 2.050(4) 1_565 ? Zn1 N2 2.058(5) 3_455 ? Zn1 O1W 2.179(5) . ? Zn1 Cl1 2.583(17) . ? Zn1 I1 2.762(5) . ? 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 C5 N1 C1 117.8(4) . . ? C5 N1 Zn1 121.5(3) . . ? C1 N1 Zn1 120.5(3) . . ? N1 C1 C2 122.7(5) . . ? C1 C2 C3 120.4(5) . . ? C2 C3 C4 116.9(4) . . ? C2 C3 C6 121.3(4) . . ? C4 C3 C6 121.8(4) . . ? C5 C4 C3 119.4(5) . . ? N1 C5 C4 122.7(5) . . ? C7 N2 C11 118.4(5) . . ? C7 N2 Zn1 121.1(3) . 3_545 ? C11 N2 Zn1 120.5(4) . 3_545 ? N2 C7 C8 123.1(5) . . ? C7 C8 C9 119.3(5) . . ? C10 C9 C8 117.4(5) . . ? C10 C9 C12 121.2(4) . . ? C8 C9 C12 121.4(4) . . ? C11 C10 C9 119.7(5) . . ? N2 C11 C10 121.9(5) . . ? C13 N3 C17 117.7(4) . . ? C13 N3 Zn1 122.0(3) . 1_545 ? C17 N3 Zn1 120.3(3) . 1_545 ? N3 C13 C14 123.2(5) . . ? C13 C14 C15 119.3(4) . . ? C14 C15 C16 117.1(4) . . ? C14 C15 C18 121.6(4) . . ? C16 C15 C18 121.2(4) . . ? C17 C16 C15 119.8(4) . . ? N3 C17 C16 122.8(4) . . ? N9 C6 N4 129.4(4) . . ? N9 C6 C3 116.7(4) . . ? N4 C6 C3 113.9(4) . . ? C19 N4 C6 114.7(4) . . ? N4 C19 N5 119.8(4) . . ? N4 C19 C22 120.5(4) . . ? N5 C19 C22 119.8(4) . . ? C12 N5 C19 115.4(4) . . ? N6 C12 N5 130.3(4) . . ? N6 C12 C9 115.3(4) . . ? N5 C12 C9 114.5(4) . . ? C12 N6 C20 114.9(4) . . ? N7 C20 N6 120.2(4) . . ? N7 C20 C22 120.0(4) . . ? N6 C20 C22 119.8(4) . . ? C20 N7 C18 115.3(4) . . ? N8 C18 N7 129.6(4) . . ? N8 C18 C15 116.6(4) . . ? N7 C18 C15 113.8(4) . . ? C18 N8 C21 115.2(4) . . ? N9 C21 N8 120.1(4) . . ? N9 C21 C22 120.4(4) . . ? N8 C21 C22 119.5(4) . . ? C21 C22 C19 119.8(4) . . ? C21 C22 C20 120.3(4) . . ? C19 C22 C20 119.8(4) . . ? C6 N9 C21 115.3(4) . . ? N3 Zn1 N2 116.78(16) 1_565 3_455 ? N3 Zn1 N1 125.88(17) 1_565 . ? N2 Zn1 N1 116.63(16) 3_455 . ? N3 Zn1 O1W 85.20(15) 1_565 . ? N2 Zn1 O1W 89.92(17) 3_455 . ? N1 Zn1 O1W 86.74(17) . . ? N3 Zn1 Cl1 93.6(4) 1_565 . ? N2 Zn1 Cl1 95.9(4) 3_455 . ? N1 Zn1 Cl1 89.1(3) . . ? O1W Zn1 Cl1 173.9(4) . . ? N3 Zn1 I1 89.59(15) 1_565 . ? N2 Zn1 I1 93.25(16) 3_455 . ? N1 Zn1 I1 95.59(15) . . ? O1W Zn1 I1 174.71(14) . . ? Cl1 Zn1 I1 6.5(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.987 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 944049' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), (I 1-), (C22 H12 N9 1-), 2(C1 H3 O1 H1), 3(C6 O1 H6)' _chemical_formula_sum 'C42 H38 I N9 O5 Zn' _chemical_formula_weight 941.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0029 0.0015 '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' I I -0.4926 1.7198 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0057 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0101 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.3005 1.3594 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 15.4187(2) _cell_length_b 12.4644(2) _cell_length_c 21.6037(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.2080(10) _cell_angle_gamma 90.00 _cell_volume 4151.88(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 66389 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 29.36 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8136 _exptl_absorpt_correction_T_max 0.8564 _exptl_absorpt_process_details 'PLATON MULABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68898 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PLSII 2D bending magnet' _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_measurement_device_type 'ADSC Q210 CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66389 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 29.36 _reflns_number_total 9607 _reflns_number_gt 6986 _reflns_threshold_expression >2\s(I) _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL3000 _computing_data_reduction HKL3000 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Because of severely disordered solvent molecules, diffractions are not observed at higher angle. Several restraints (DFIX and FLAT) were applied to methanols and phenols on a basis of chemical symmetry of the molecules. Several solvents were refined with isotropic thermal parameters. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1955P)^2^+22.1177P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9607 _refine_ls_number_parameters 477 _refine_ls_number_restraints 280 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.1162 _refine_ls_wR_factor_ref 0.3389 _refine_ls_wR_factor_gt 0.3266 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O5 O 0.822(2) 0.742(2) 1.0136(15) 0.308(14) Uiso 1 1 d DU . . C42 C 0.859(2) 0.659(3) 0.9768(15) 0.224(11) Uiso 1 1 d DU . . O4 O 0.4248(14) 0.6341(18) 0.7106(9) 0.124(6) Uiso 0.50 1 d PDU A 1 C41 C 0.350(3) 0.697(6) 0.700(3) 0.25(3) Uiso 0.50 1 d PDU A 1 O6 O 0.284(4) 0.845(4) 0.683(3) 0.32(2) Uiso 0.50 1 d PDU B 2 C43 C 0.322(3) 0.778(3) 0.636(2) 0.154(13) Uiso 0.50 1 d PDU B 2 N1 N 0.3881(4) 0.0365(6) 0.2847(3) 0.0653(16) Uani 1 1 d . . . C1 C 0.3156(5) 0.0850(9) 0.3039(5) 0.085(3) Uani 1 1 d . . . H1 H 0.2632 0.0702 0.2822 0.103 Uiso 1 1 calc R . . C2 C 0.3118(5) 0.1552(10) 0.3532(5) 0.090(3) Uani 1 1 d . . . H2 H 0.2584 0.1874 0.3646 0.108 Uiso 1 1 calc R . . C3 C 0.3876(5) 0.1782(7) 0.3862(4) 0.0623(18) Uani 1 1 d . . . C4 C 0.4636(5) 0.1240(9) 0.3670(4) 0.078(2) Uani 1 1 d . . . H4 H 0.5168 0.1349 0.3884 0.094 Uiso 1 1 calc R . . C5 C 0.4597(5) 0.0564(8) 0.3178(4) 0.074(2) Uani 1 1 d . . . H5 H 0.5116 0.0207 0.3061 0.088 Uiso 1 1 calc R . . N2 N 0.0066(3) 0.5278(6) 0.6735(3) 0.0636(16) Uani 1 1 d . . . C7 C 0.0751(5) 0.5911(8) 0.6776(4) 0.070(2) Uani 1 1 d . . . H7 H 0.0698 0.6579 0.6984 0.084 Uiso 1 1 calc R . . C8 C 0.1548(4) 0.5630(8) 0.6523(4) 0.071(2) Uani 1 1 d . . . H8 H 0.2033 0.6093 0.6571 0.085 Uiso 1 1 calc R . . C9 C 0.1632(4) 0.4695(8) 0.6207(4) 0.066(2) Uani 1 1 d . . . C10 C 0.0911(5) 0.4011(8) 0.6177(4) 0.069(2) Uani 1 1 d . . . H10 H 0.0944 0.3343 0.5966 0.083 Uiso 1 1 calc R . . C11 C 0.0144(5) 0.4333(8) 0.6461(4) 0.070(2) Uani 1 1 d . . . H11 H -0.0338 0.3858 0.6459 0.084 Uiso 1 1 calc R . . N3 N 0.7823(4) 0.5346(6) 0.6649(3) 0.0617(15) Uani 1 1 d . . . C13 C 0.7801(4) 0.4745(8) 0.6146(4) 0.071(2) Uani 1 1 d . . . H13 H 0.8335 0.4513 0.5974 0.085 Uiso 1 1 calc R . . C14 C 0.7032(4) 0.4434(8) 0.5857(4) 0.069(2) Uani 1 1 d . . . H14 H 0.7041 0.4014 0.5490 0.083 Uiso 1 1 calc R . . C15 C 0.6251(4) 0.4756(7) 0.6119(4) 0.0626(18) Uani 1 1 d . . . C16 C 0.6283(4) 0.5411(8) 0.6627(4) 0.072(2) Uani 1 1 d . . . H16 H 0.5762 0.5665 0.6808 0.086 Uiso 1 1 calc R . . C17 C 0.7076(4) 0.5702(8) 0.6875(4) 0.068(2) Uani 1 1 d . . . H17 H 0.7088 0.6173 0.7220 0.081 Uiso 1 1 calc R . . C6 C 0.3879(5) 0.2527(7) 0.4407(4) 0.0632(19) Uani 1 1 d . . . N4 N 0.3109(4) 0.2806(6) 0.4623(3) 0.0662(16) Uani 1 1 d . . . C19 C 0.3123(4) 0.3445(7) 0.5114(4) 0.0617(18) Uani 1 1 d . . . N5 N 0.2370(4) 0.3759(6) 0.5389(3) 0.0654(16) Uani 1 1 d . . . C12 C 0.2451(4) 0.4393(7) 0.5901(4) 0.0650(19) Uani 1 1 d . . . N6 N 0.3178(4) 0.4777(6) 0.6163(3) 0.0654(16) Uani 1 1 d . . . C20 C 0.3925(4) 0.4473(7) 0.5890(4) 0.0636(19) Uani 1 1 d . . . N7 N 0.4692(4) 0.4798(6) 0.6138(3) 0.0642(16) Uani 1 1 d . . . C18 C 0.5402(4) 0.4434(7) 0.5845(4) 0.0602(17) Uani 1 1 d . . . N8 N 0.5459(3) 0.3779(6) 0.5341(3) 0.0656(17) Uani 1 1 d . . . C21 C 0.4674(4) 0.3462(7) 0.5103(3) 0.0624(18) Uani 1 1 d . . . N9 N 0.4672(4) 0.2799(6) 0.4603(3) 0.0653(16) Uani 1 1 d . . . C22 C 0.3917(4) 0.3797(7) 0.5365(4) 0.0610(18) Uani 1 1 d . . . I1 I 0.39518(4) -0.26190(6) 0.25308(4) 0.0897(3) Uani 1 1 d . . . Zn1 Zn 0.39247(5) -0.07113(8) 0.21380(4) 0.0626(3) Uani 1 1 d . . . O1 O 0.4151(14) 0.0095(18) 0.5182(10) 0.305(13) Uani 1 1 d DU . . C23 C 0.3741(9) 0.0718(11) 0.5604(6) 0.174(8) Uani 1 1 d GDU . . C24 C 0.2843(9) 0.0661(10) 0.5652(6) 0.144(6) Uani 1 1 d GDU . . H24 H 0.2520 0.0240 0.5366 0.173 Uiso 1 1 calc R . . C25 C 0.2419(8) 0.1222(11) 0.6117(7) 0.157(6) Uani 1 1 d GU . . H25 H 0.1805 0.1183 0.6150 0.188 Uiso 1 1 calc R . . C26 C 0.2892(12) 0.1839(10) 0.6535(6) 0.167(7) Uani 1 1 d GU . . H26 H 0.2601 0.2222 0.6853 0.200 Uiso 1 1 calc R . . C27 C 0.3789(12) 0.1896(10) 0.6487(6) 0.168(8) Uani 1 1 d GU . . H27 H 0.4112 0.2317 0.6772 0.201 Uiso 1 1 calc R . . C28 C 0.4214(8) 0.1335(12) 0.6021(8) 0.213(10) Uani 1 1 d GDU . . H28 H 0.4827 0.1374 0.5988 0.255 Uiso 1 1 calc R . . O2 O 0.0936(8) 0.4063(15) 0.4649(8) 0.217(8) Uani 1 1 d DU . . C29 C 0.0395(9) 0.3256(12) 0.4722(7) 0.177(8) Uani 1 1 d GDU . . C30 C -0.0484(9) 0.3473(13) 0.4785(6) 0.178(8) Uani 1 1 d GDU . . H30 H -0.0691 0.4187 0.4743 0.213 Uiso 1 1 calc R . . C31 C -0.1061(9) 0.2644(17) 0.4911(10) 0.253(12) Uani 1 1 d GU . . H31 H -0.1662 0.2792 0.4954 0.303 Uiso 1 1 calc R . . C32 C -0.0758(14) 0.1599(15) 0.4973(12) 0.306(13) Uani 1 1 d GU . . H32 H -0.1152 0.1033 0.5058 0.368 Uiso 1 1 calc R . . C33 C 0.0122(15) 0.1383(12) 0.4909(12) 0.290(12) Uani 1 1 d GU . . H33 H 0.0329 0.0669 0.4951 0.348 Uiso 1 1 calc R . . C34 C 0.0698(10) 0.2211(14) 0.4783(10) 0.219(10) Uani 1 1 d GDU . . H34 H 0.1300 0.2063 0.4740 0.262 Uiso 1 1 calc R . . O3 O 0.5447(13) 0.7255(15) 0.7729(8) 0.235(9) Uani 1 1 d DU . . C35 C 0.5925(11) 0.6675(11) 0.8115(6) 0.196(9) Uani 1 1 d GDU . . C36 C 0.5648(14) 0.5659(14) 0.8291(9) 0.224(10) Uani 1 1 d GDU . . H36 H 0.5103 0.5395 0.8150 0.269 Uiso 1 1 calc R . . C37 C 0.6167(19) 0.5028(14) 0.8672(10) 0.295(14) Uani 1 1 d GDU . . H37 H 0.5977 0.4333 0.8792 0.355 Uiso 1 1 calc R . . C38 C 0.6963(17) 0.541(2) 0.8877(9) 0.331(15) Uani 1 1 d GDU . . H38 H 0.7318 0.4982 0.9138 0.397 Uiso 1 1 calc R . . C39 C 0.7241(12) 0.643(2) 0.8702(11) 0.324(15) Uani 1 1 d GDU . . H39 H 0.7785 0.6692 0.8842 0.389 Uiso 1 1 calc R . . C40 C 0.6722(12) 0.7060(14) 0.8321(10) 0.226(11) Uani 1 1 d GDU . . H40 H 0.6911 0.7754 0.8201 0.272 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 N1 0.038(3) 0.088(4) 0.070(4) -0.000(3) -0.014(3) 0.003(3) C1 0.038(3) 0.122(8) 0.097(6) -0.027(6) -0.022(4) 0.012(4) C2 0.047(4) 0.126(8) 0.097(7) -0.032(6) -0.025(4) 0.017(4) C3 0.044(3) 0.082(5) 0.061(4) -0.000(3) -0.012(3) 0.000(3) C4 0.037(3) 0.122(7) 0.076(5) -0.008(5) -0.015(3) -0.001(4) C5 0.035(3) 0.103(6) 0.083(6) -0.017(5) -0.011(3) 0.008(3) N2 0.030(2) 0.087(4) 0.074(4) 0.003(3) -0.008(2) 0.001(2) C7 0.037(3) 0.091(6) 0.080(5) -0.004(4) -0.004(3) -0.002(3) C8 0.033(3) 0.091(6) 0.089(6) -0.007(4) -0.010(3) -0.004(3) C9 0.030(3) 0.100(6) 0.069(5) 0.000(4) -0.007(3) -0.004(3) C10 0.040(3) 0.088(5) 0.079(5) 0.001(4) -0.007(3) -0.003(3) C11 0.043(3) 0.086(6) 0.081(5) 0.004(4) -0.007(3) -0.005(3) N3 0.034(2) 0.085(4) 0.066(4) 0.001(3) -0.004(2) 0.001(2) C13 0.030(3) 0.108(6) 0.074(5) 0.005(4) -0.009(3) 0.002(3) C14 0.036(3) 0.102(6) 0.069(5) -0.001(4) -0.008(3) 0.001(3) C15 0.033(3) 0.090(5) 0.065(4) 0.008(4) -0.008(3) -0.001(3) C16 0.033(3) 0.109(6) 0.073(5) -0.005(4) -0.012(3) 0.001(3) C17 0.034(3) 0.098(6) 0.071(5) -0.008(4) -0.006(3) 0.002(3) C6 0.037(3) 0.088(5) 0.065(4) 0.003(4) -0.007(3) 0.000(3) N4 0.036(3) 0.087(4) 0.075(4) -0.003(3) -0.008(3) -0.000(3) C19 0.034(3) 0.087(5) 0.064(4) 0.003(4) -0.009(3) -0.001(3) N5 0.033(2) 0.091(5) 0.072(4) -0.001(3) -0.005(3) -0.000(3) C12 0.033(3) 0.094(6) 0.068(5) 0.001(4) -0.006(3) -0.001(3) N6 0.037(3) 0.089(5) 0.071(4) -0.004(3) -0.005(3) -0.001(3) C20 0.039(3) 0.088(5) 0.064(4) 0.009(4) -0.010(3) 0.000(3) N7 0.035(2) 0.091(5) 0.066(4) 0.003(3) -0.009(2) -0.003(3) C18 0.032(3) 0.090(5) 0.059(4) 0.004(3) -0.007(3) -0.002(3) N8 0.033(2) 0.099(5) 0.065(4) -0.000(3) -0.008(2) 0.000(3) C21 0.039(3) 0.090(5) 0.059(4) 0.003(4) -0.011(3) -0.005(3) N9 0.042(3) 0.085(4) 0.069(4) 0.001(3) -0.013(3) -0.002(3) C22 0.038(3) 0.080(5) 0.066(4) 0.005(3) -0.011(3) -0.002(3) I1 0.0520(3) 0.0902(5) 0.1267(7) 0.0176(4) -0.0190(3) -0.0048(2) Zn1 0.0311(3) 0.0873(6) 0.0692(6) 0.0018(4) -0.0090(3) 0.0010(3) O1 0.35(3) 0.27(3) 0.29(3) 0.08(2) 0.09(2) 0.06(2) C23 0.23(2) 0.145(15) 0.151(15) 0.063(12) 0.011(15) -0.004(14) C24 0.128(12) 0.151(13) 0.152(14) 0.030(11) 0.020(11) -0.005(11) C25 0.157(15) 0.143(14) 0.171(16) 0.012(12) -0.009(13) -0.027(12) C26 0.211(19) 0.143(14) 0.147(13) 0.046(11) 0.012(14) -0.006(14) C27 0.193(18) 0.140(13) 0.170(15) 0.070(12) -0.068(14) -0.023(14) C28 0.20(2) 0.20(2) 0.24(2) 0.138(17) -0.017(17) -0.008(16) O2 0.098(8) 0.36(2) 0.195(14) 0.036(15) -0.042(9) 0.001(12) C29 0.193(19) 0.195(18) 0.142(12) 0.028(13) -0.067(14) -0.045(16) C30 0.192(18) 0.198(18) 0.142(12) 0.022(13) -0.079(13) 0.005(15) C31 0.22(2) 0.25(3) 0.29(2) -0.01(2) 0.06(2) 0.050(19) C32 0.22(2) 0.29(3) 0.41(3) 0.00(3) 0.12(2) 0.05(2) C33 0.19(2) 0.28(3) 0.40(3) -0.05(3) 0.07(2) -0.03(2) C34 0.144(17) 0.21(2) 0.30(2) -0.06(2) 0.050(18) -0.043(15) O3 0.25(2) 0.234(17) 0.222(17) -0.070(15) 0.045(16) 0.080(15) C35 0.26(2) 0.154(16) 0.173(16) -0.012(14) -0.065(16) 0.052(16) C36 0.31(3) 0.149(16) 0.209(19) 0.043(15) -0.067(19) -0.067(17) C37 0.37(3) 0.24(2) 0.28(3) 0.06(2) -0.05(3) -0.08(2) C38 0.39(3) 0.28(3) 0.32(3) 0.02(3) 0.00(3) -0.05(3) C39 0.37(3) 0.30(3) 0.30(3) -0.00(3) 0.00(3) 0.02(3) C40 0.27(3) 0.21(2) 0.19(2) -0.058(18) -0.022(19) 0.03(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 O5 C42 1.431(17) . ? O4 C41 1.415(18) . ? O6 C43 1.437(18) . ? N1 C5 1.337(9) . ? N1 C1 1.339(11) . ? N1 Zn1 2.037(7) . ? C1 C2 1.379(14) . ? C2 C3 1.395(10) . ? C3 C4 1.415(11) . ? C3 C6 1.499(12) . ? C4 C5 1.358(13) . ? N2 C7 1.321(10) . ? N2 C11 1.324(12) . ? N2 Zn1 2.039(6) 4_566 ? C7 C8 1.391(11) . ? C8 C9 1.357(13) . ? C9 C10 1.403(10) . ? C9 C12 1.476(10) . ? C10 C11 1.393(12) . ? N3 C13 1.318(11) . ? N3 C17 1.330(9) . ? N3 Zn1 2.048(6) 4_666 ? C13 C14 1.394(9) . ? C14 C15 1.392(11) . ? C15 C16 1.368(12) . ? C15 C18 1.490(9) . ? C16 C17 1.382(9) . ? C6 N4 1.323(10) . ? C6 N9 1.337(9) . ? N4 C19 1.328(11) . ? C19 N5 1.363(9) . ? C19 C22 1.408(9) . ? N5 C12 1.365(11) . ? C12 N6 1.342(9) . ? N6 C20 1.350(10) . ? C20 N7 1.357(8) . ? C20 C22 1.413(12) . ? N7 C18 1.345(10) . ? C18 N8 1.365(11) . ? N8 C21 1.372(8) . ? C21 N9 1.359(11) . ? C21 C22 1.365(11) . ? I1 Zn1 2.5250(12) . ? Zn1 N2 2.039(6) 4_665 ? Zn1 N3 2.048(6) 4_565 ? O1 C23 1.355(11) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? O2 C29 1.316(10) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? O3 C35 1.326(10) . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? 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 C5 N1 C1 116.0(7) . . ? C5 N1 Zn1 119.7(5) . . ? C1 N1 Zn1 124.1(5) . . ? N1 C1 C2 124.3(7) . . ? C1 C2 C3 119.2(8) . . ? C2 C3 C4 116.4(8) . . ? C2 C3 C6 121.9(7) . . ? C4 C3 C6 121.7(6) . . ? C5 C4 C3 119.5(6) . . ? N1 C5 C4 124.6(7) . . ? C7 N2 C11 119.2(7) . . ? C7 N2 Zn1 120.3(6) . 4_566 ? C11 N2 Zn1 120.4(5) . 4_566 ? N2 C7 C8 122.0(9) . . ? C9 C8 C7 120.0(7) . . ? C8 C9 C10 117.9(7) . . ? C8 C9 C12 121.9(7) . . ? C10 C9 C12 120.3(8) . . ? C11 C10 C9 118.6(9) . . ? N2 C11 C10 122.1(8) . . ? C13 N3 C17 118.2(6) . . ? C13 N3 Zn1 124.7(5) . 4_666 ? C17 N3 Zn1 117.0(5) . 4_666 ? N3 C13 C14 123.1(7) . . ? C15 C14 C13 118.3(8) . . ? C16 C15 C14 118.0(6) . . ? C16 C15 C18 120.6(7) . . ? C14 C15 C18 121.4(7) . . ? C15 C16 C17 119.8(7) . . ? N3 C17 C16 122.5(8) . . ? N4 C6 N9 129.9(8) . . ? N4 C6 C3 116.0(6) . . ? N9 C6 C3 114.0(7) . . ? C6 N4 C19 115.3(6) . . ? N4 C19 N5 120.7(6) . . ? N4 C19 C22 120.4(7) . . ? N5 C19 C22 118.9(7) . . ? C19 N5 C12 116.3(6) . . ? N6 C12 N5 128.5(7) . . ? N6 C12 C9 115.8(7) . . ? N5 C12 C9 115.7(6) . . ? C12 N6 C20 115.4(7) . . ? N6 C20 N7 119.2(7) . . ? N6 C20 C22 120.8(6) . . ? N7 C20 C22 120.0(7) . . ? C18 N7 C20 115.0(7) . . ? N7 C18 N8 129.3(6) . . ? N7 C18 C15 115.9(7) . . ? N8 C18 C15 114.8(6) . . ? C18 N8 C21 114.3(6) . . ? N9 C21 C22 121.1(6) . . ? N9 C21 N8 118.2(7) . . ? C22 C21 N8 120.7(7) . . ? C6 N9 C21 113.9(7) . . ? C21 C22 C19 119.3(7) . . ? C21 C22 C20 120.7(6) . . ? C19 C22 C20 120.0(7) . . ? N1 Zn1 N2 100.2(3) . 4_665 ? N1 Zn1 N3 102.2(3) . 4_565 ? N2 Zn1 N3 115.8(3) 4_665 4_565 ? N1 Zn1 I1 111.6(2) . . ? N2 Zn1 I1 112.3(2) 4_665 . ? N3 Zn1 I1 113.3(2) 4_565 . ? O1 C23 C24 119.2(8) . . ? O1 C23 C28 120.5(8) . . ? C24 C23 C28 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? O2 C29 C30 118.8(8) . . ? O2 C29 C34 121.0(8) . . ? C30 C29 C34 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C29 120.0 . . ? O3 C35 C36 119.8(8) . . ? O3 C35 C40 120.1(8) . . ? C36 C35 C40 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? _diffrn_measured_fraction_theta_max 0.766 _diffrn_reflns_theta_full 24.42 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 2.098 _refine_diff_density_min -1.653 _refine_diff_density_rms 0.171 _database_code_depnum_ccdc_archive 'CCDC 944050' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), (I 1-), (C22 H12 N9 1-), 5(C6 O1 H6), 2.5(C1 H4 O1) ' _chemical_formula_sum 'C54.50 H52 I N9 O7.50 Zn' _chemical_formula_weight 1145.32 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' I I -0.4742 1.8119 '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 Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 21.500(11) _cell_length_b 21.500(11) _cell_length_c 22.454(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10379(9) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4680 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8398 _exptl_absorpt_correction_T_max 0.8763 _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 'microfocus source 30W maximum continuous power' _diffrn_radiation_monochromator 'Wuazar(TM) Montel multilayer optic' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38898 _diffrn_reflns_av_R_equivalents 0.1084 _diffrn_reflns_av_sigmaI/netI 0.1782 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 22.27 _reflns_number_total 11791 _reflns_number_gt 7019 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 sofware Suite' _computing_cell_refinement 'APEX2 sofware Suite' _computing_data_reduction 'APEX2 sofware Suite' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Because a large number of severely disordered solvent molecules, diffractions are not observed at higher angle. Anisotropic refinement were not applied for all non-H atoms of the solvent phenol and methanol molecules. Several restraints were applied to methanols and phenols on a basis of chemical symmetry of the molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1365P)^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 mixed _refine_ls_extinction_method constr _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.46(4) _refine_ls_number_reflns 11791 _refine_ls_number_parameters 868 _refine_ls_number_restraints 301 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.2519 _refine_ls_wR_factor_gt 0.2329 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.975 _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 Zn1 Zn 1.00494(8) 1.01459(10) 0.49376(9) 0.0313(5) Uani 1 1 d . . . I1 I 0.95241(6) 1.08771(8) 0.56474(6) 0.0615(5) Uani 1 1 d . . . N1 N 0.9563(6) 0.9362(8) 0.4628(6) 0.029(4) Uani 1 1 d . . . C1 C 0.9433(8) 0.9347(9) 0.4058(9) 0.035(5) Uani 1 1 d U . . H1 H 0.9514 0.9696 0.3811 0.042 Uiso 1 1 calc R . . C2 C 0.9179(7) 0.8818(11) 0.3830(8) 0.043(6) Uani 1 1 d . . . H2 H 0.9060 0.8811 0.3423 0.051 Uiso 1 1 calc R . . C3 C 0.9087(7) 0.8290(9) 0.4172(8) 0.030(5) Uani 1 1 d . . . C4 C 0.9206(8) 0.8349(11) 0.4767(7) 0.039(5) Uani 1 1 d . . . H4 H 0.9120 0.8017 0.5034 0.047 Uiso 1 1 calc R . . C5 C 0.9461(10) 0.8912(11) 0.4977(9) 0.051(6) Uani 1 1 d . . . H5 H 0.9557 0.8955 0.5388 0.062 Uiso 1 1 calc R . . N2 N 0.9577(6) 0.5530(9) 0.0814(6) 0.041(4) Uani 1 1 d . . . C7 C 0.9215(8) 0.5189(10) 0.1196(8) 0.042(5) Uani 1 1 d . . . H7 H 0.9127 0.4768 0.1100 0.050 Uiso 1 1 calc R . . C8 C 0.8984(7) 0.5425(10) 0.1695(8) 0.035(5) Uani 1 1 d . . . H8 H 0.8741 0.5166 0.1947 0.041 Uiso 1 1 calc R . . C9 C 0.9079(7) 0.6008(10) 0.1855(8) 0.034(5) Uani 1 1 d . . . C10 C 0.9441(7) 0.6394(10) 0.1460(7) 0.035(5) Uani 1 1 d . . . H10 H 0.9532 0.6815 0.1553 0.042 Uiso 1 1 calc R . . C11 C 0.9641(10) 0.6128(12) 0.0959(9) 0.053(6) Uani 1 1 d . . . H11 H 0.9848 0.6388 0.0680 0.064 Uiso 1 1 calc R . . N3 N 0.5794(4) 0.5302(5) 0.4678(4) 0.037(3) Uani 1 1 d GU . . C13 C 0.6055(4) 0.5827(5) 0.4939(4) 0.038(3) Uani 1 1 d GU . . H13 H 0.5871 0.6003 0.5284 0.045 Uiso 1 1 calc R . . C14 C 0.6586(4) 0.6093(5) 0.4695(5) 0.035(3) Uani 1 1 d GU . . H14 H 0.6765 0.6452 0.4873 0.042 Uiso 1 1 calc R . . C15 C 0.6856(4) 0.5835(5) 0.4189(5) 0.031(4) Uani 1 1 d GU . . C16 C 0.6594(5) 0.5310(6) 0.3928(4) 0.041(5) Uani 1 1 d G . . H16 H 0.6778 0.5134 0.3583 0.049 Uiso 1 1 calc R . . C17 C 0.6063(5) 0.5044(5) 0.4172(5) 0.045(4) Uani 1 1 d GU . . H17 H 0.5884 0.4686 0.3994 0.054 Uiso 1 1 calc R . . C6 C 0.8852(7) 0.7709(9) 0.3900(8) 0.033(5) Uani 1 1 d . . . N4 N 0.9096(6) 0.7531(8) 0.3371(6) 0.030(4) Uani 1 1 d . . . C19 C 0.8883(7) 0.7012(10) 0.3134(7) 0.025(4) Uani 1 1 d . . . N5 N 0.9086(5) 0.6815(7) 0.2636(6) 0.028(4) Uani 1 1 d U . . C12 C 0.8828(8) 0.6263(10) 0.2417(8) 0.037(5) Uani 1 1 d U . . N6 N 0.8363(6) 0.5952(7) 0.2654(6) 0.028(3) Uani 1 1 d U . . C20 C 0.8139(7) 0.6176(9) 0.3162(7) 0.025(4) Uani 1 1 d . . . N7 N 0.7619(6) 0.5888(8) 0.3423(6) 0.035(4) Uani 1 1 d . . . C18 C 0.7436(8) 0.6159(9) 0.3935(8) 0.028(5) Uani 1 1 d . . . N8 N 0.7644(6) 0.6641(7) 0.4233(6) 0.031(4) Uani 1 1 d . . . C21 C 0.8142(7) 0.6914(9) 0.3957(7) 0.027(5) Uani 1 1 d . . . N9 N 0.8380(6) 0.7439(7) 0.4230(6) 0.036(4) Uani 1 1 d . . . C22 C 0.8371(7) 0.6693(9) 0.3428(7) 0.021(4) Uani 1 1 d . . . Zn2 Zn 0.50672(8) 0.99309(10) 0.50131(8) 0.0306(5) Uani 1 1 d . . . I2 I 0.43107(5) 0.94238(7) 0.57167(6) 0.0500(4) Uani 1 1 d . . . N10 N 0.5381(4) 0.9465(5) 0.4292(3) 0.031(3) Uani 1 1 d GU . . C23 C 0.4962(3) 0.9302(6) 0.3847(4) 0.035(5) Uani 1 1 d G . . H23 H 0.4528 0.9349 0.3912 0.042 Uiso 1 1 calc R . . C24 C 0.5178(4) 0.9070(6) 0.3308(4) 0.047(5) Uani 1 1 d G . . H24 H 0.4892 0.8959 0.3004 0.056 Uiso 1 1 calc R . . C25 C 0.5813(4) 0.9001(6) 0.3213(4) 0.032(5) Uani 1 1 d G . . C26 C 0.6232(3) 0.9164(6) 0.3658(4) 0.031(4) Uani 1 1 d GU . . H26 H 0.6666 0.9117 0.3593 0.037 Uiso 1 1 calc R . . C27 C 0.6016(3) 0.9396(6) 0.4197(4) 0.031(3) Uani 1 1 d GU . . H27 H 0.6302 0.9507 0.4502 0.037 Uiso 1 1 calc R . . N11 N 0.5334(7) 0.5685(8) 0.0388(6) 0.041(4) Uani 1 1 d U . . C29 C 0.5837(8) 0.5949(11) 0.0171(8) 0.049(5) Uani 1 1 d U . . H29 H 0.6026 0.5763 -0.0168 0.059 Uiso 1 1 calc R . . C30 C 0.6110(8) 0.6479(10) 0.0399(8) 0.043(5) Uani 1 1 d U . . H30 H 0.6463 0.6656 0.0211 0.051 Uiso 1 1 calc R . . C31 C 0.5863(7) 0.6747(9) 0.0903(7) 0.027(4) Uani 1 1 d . . . C32 C 0.5356(8) 0.6443(11) 0.1186(8) 0.046(6) Uani 1 1 d . . . H32 H 0.5190 0.6589 0.1553 0.055 Uiso 1 1 calc R . . C33 C 0.5108(8) 0.5908(10) 0.0893(8) 0.040(5) Uani 1 1 d U . . H33 H 0.4763 0.5702 0.1070 0.048 Uiso 1 1 calc R . . N12 N 0.9125(6) 0.9713(8) 0.0375(6) 0.035(4) Uani 1 1 d . . . C35 C 0.8945(8) 0.9867(10) 0.0922(8) 0.037(5) Uani 1 1 d U . . H35 H 0.9201 1.0130 0.1159 0.045 Uiso 1 1 calc R . . C36 C 0.8387(8) 0.9648(10) 0.1150(8) 0.040(5) Uani 1 1 d U . . H36 H 0.8237 0.9809 0.1517 0.048 Uiso 1 1 calc R . . C37 C 0.8057(7) 0.9216(10) 0.0862(7) 0.033(4) Uani 1 1 d U . . C38 C 0.8241(8) 0.9062(10) 0.0282(8) 0.045(6) Uani 1 1 d . . . H38 H 0.8011 0.8773 0.0049 0.054 Uiso 1 1 calc R . . C39 C 0.8779(8) 0.9352(10) 0.0057(9) 0.049(6) Uani 1 1 d . . . H39 H 0.8892 0.9279 -0.0346 0.059 Uiso 1 1 calc R . . C28 C 0.6038(8) 0.8767(11) 0.2596(8) 0.040(6) Uani 1 1 d . . . N13 N 0.5766(6) 0.8267(7) 0.2386(6) 0.026(3) Uani 1 1 d . . . C41 C 0.6035(7) 0.8052(10) 0.1894(7) 0.028(5) Uani 1 1 d . . . N14 N 0.5814(6) 0.7510(7) 0.1652(6) 0.029(4) Uani 1 1 d . . . C34 C 0.6106(7) 0.7326(10) 0.1172(8) 0.033(5) Uani 1 1 d . . . N15 N 0.6589(6) 0.7558(7) 0.0883(5) 0.026(3) Uani 1 1 d . . . C42 C 0.6815(8) 0.8074(10) 0.1133(8) 0.034(5) Uani 1 1 d . . . N16 N 0.7331(6) 0.8379(8) 0.0880(6) 0.031(4) Uani 1 1 d . . . C40 C 0.7487(7) 0.8896(9) 0.1150(8) 0.029(4) Uani 1 1 d U . . N17 N 0.7276(5) 0.9181(8) 0.1632(6) 0.032(4) Uani 1 1 d U . . C43 C 0.6798(9) 0.8879(9) 0.1887(8) 0.034(5) Uani 1 1 d U . . N18 N 0.6546(6) 0.9118(8) 0.2395(5) 0.031(4) Uani 1 1 d . . . C44 C 0.6547(7) 0.8340(9) 0.1630(8) 0.033(5) Uani 1 1 d . . . O1 O 0.5304(9) 0.1547(10) 0.1505(9) 0.117(7) Uiso 1 1 d D . . C45 C 0.4953(9) 0.1117(9) 0.1819(9) 0.067(7) Uiso 1 1 d D . . C46 C 0.5168(9) 0.0524(10) 0.1754(9) 0.070(7) Uiso 1 1 d D . . H46 H 0.5535 0.0430 0.1536 0.084 Uiso 1 1 calc R . . C47 C 0.4817(10) 0.0073(11) 0.2025(9) 0.075(7) Uiso 1 1 d D . . H47 H 0.4915 -0.0354 0.1973 0.090 Uiso 1 1 calc R . . C48 C 0.4304(12) 0.0254(12) 0.2385(12) 0.106(10) Uiso 1 1 d D . . H48 H 0.4071 -0.0065 0.2575 0.127 Uiso 1 1 calc R . . C49 C 0.4132(9) 0.0824(10) 0.2470(9) 0.067(6) Uiso 1 1 d D . . H49 H 0.3788 0.0923 0.2718 0.081 Uiso 1 1 calc R . . C50 C 0.4469(10) 0.1282(10) 0.2184(9) 0.076(7) Uiso 1 1 d D . . H50 H 0.4367 0.1708 0.2241 0.091 Uiso 1 1 calc R . . O2 O 0.7019(15) 0.2910(18) 0.6616(14) 0.197(13) Uiso 1 1 d . . . C51 C 0.7233(6) 0.2588(7) 0.7089(5) 0.062(6) Uiso 1 1 d G . . C52 C 0.7012(5) 0.2046(6) 0.7351(6) 0.050(6) Uiso 1 1 d G . . H52 H 0.6673 0.1829 0.7177 0.060 Uiso 1 1 calc R . . C53 C 0.7286(6) 0.1822(5) 0.7869(6) 0.058(6) Uiso 1 1 d G . . H53 H 0.7134 0.1452 0.8049 0.070 Uiso 1 1 calc R . . C54 C 0.7781(6) 0.2140(7) 0.8125(5) 0.052(6) Uiso 1 1 d G . . H54 H 0.7969 0.1987 0.8479 0.063 Uiso 1 1 calc R . . C55 C 0.8003(5) 0.2682(7) 0.7863(6) 0.067(7) Uiso 1 1 d G . . H55 H 0.8341 0.2900 0.8037 0.081 Uiso 1 1 calc R . . C56 C 0.7728(6) 0.2907(6) 0.7345(6) 0.061(6) Uiso 1 1 d G . . H56 H 0.7880 0.3277 0.7165 0.073 Uiso 1 1 calc R . . O3 O 0.7245(6) -0.0037(7) 0.2973(6) 0.057(4) Uiso 1 1 d . . . C57 C 0.6923(8) 0.0479(10) 0.3124(8) 0.039(5) Uiso 1 1 d . . . C58 C 0.6367(8) 0.0622(11) 0.2877(8) 0.044(5) Uiso 1 1 d . . . H58 H 0.6169 0.0345 0.2609 0.053 Uiso 1 1 calc R . . C59 C 0.6095(12) 0.1184(13) 0.3027(11) 0.074(7) Uiso 1 1 d . . . H59 H 0.5724 0.1309 0.2831 0.089 Uiso 1 1 calc R . . C60 C 0.6350(9) 0.1569(11) 0.3454(9) 0.050(6) Uiso 1 1 d . . . H60 H 0.6133 0.1931 0.3578 0.060 Uiso 1 1 calc R . . C61 C 0.6893(10) 0.1433(13) 0.3690(10) 0.063(6) Uiso 1 1 d . . . H61 H 0.7079 0.1706 0.3971 0.075 Uiso 1 1 calc R . . C62 C 0.7194(11) 0.0885(13) 0.3525(9) 0.064(6) Uiso 1 1 d . . . H62 H 0.7589 0.0789 0.3690 0.077 Uiso 1 1 calc R . . O4 O 0.6529(6) 1.0256(8) 0.7832(6) 0.061(4) Uiso 1 1 d . . . C63 C 0.6209(9) 0.9828(11) 0.7565(8) 0.047(5) Uiso 1 1 d . . . C64 C 0.5556(10) 0.9932(12) 0.7499(9) 0.062(6) Uiso 1 1 d . . . H64 H 0.5356 1.0298 0.7639 0.074 Uiso 1 1 calc R . . C65 C 0.5228(10) 0.9441(14) 0.7205(10) 0.068(7) Uiso 1 1 d . . . H65 H 0.4790 0.9472 0.7154 0.081 Uiso 1 1 calc R . . C66 C 0.5547(11) 0.8905(13) 0.6988(10) 0.070(7) Uiso 1 1 d . . . H66 H 0.5311 0.8598 0.6784 0.085 Uiso 1 1 calc R . . C67 C 0.6174(10) 0.8805(12) 0.7056(9) 0.060(6) Uiso 1 1 d . . . H67 H 0.6373 0.8435 0.6924 0.072 Uiso 1 1 calc R . . C68 C 0.6506(10) 0.9300(11) 0.7342(8) 0.054(6) Uiso 1 1 d . . . H68 H 0.6945 0.9267 0.7381 0.065 Uiso 1 1 calc R . . O5 O 0.3842(8) 1.4277(8) 0.5824(8) 0.102(6) Uiso 1 1 d D . . C69 C 0.3756(11) 1.3647(10) 0.5953(9) 0.080(8) Uiso 1 1 d D . . C70 C 0.3430(10) 1.3316(10) 0.5535(9) 0.073(7) Uiso 1 1 d D . . H70 H 0.3315 1.3494 0.5164 0.087 Uiso 1 1 calc R . . C71 C 0.3278(9) 1.2714(10) 0.5679(9) 0.069(6) Uiso 1 1 d D . . H71 H 0.3015 1.2471 0.5431 0.082 Uiso 1 1 calc R . . C72 C 0.3527(12) 1.2475(12) 0.6211(11) 0.105(10) Uiso 1 1 d D . . H72 H 0.3448 1.2050 0.6299 0.126 Uiso 1 1 calc R . . C73 C 0.3858(11) 1.2789(11) 0.6591(10) 0.083(8) Uiso 1 1 d D . . H73 H 0.4007 1.2600 0.6945 0.099 Uiso 1 1 calc R . . C74 C 0.3986(10) 1.3403(10) 0.6468(9) 0.068(7) Uiso 1 1 d D . . H74 H 0.4227 1.3649 0.6733 0.082 Uiso 1 1 calc R . . O6 O 0.6790(11) -0.1608(13) 0.5467(10) 0.134(8) Uiso 1 1 d . . . C75 C 0.6292(11) -0.1844(12) 0.5130(10) 0.064(7) Uiso 1 1 d . . . C76 C 0.5721(10) -0.1741(11) 0.5298(9) 0.054(6) Uiso 1 1 d . . . H76 H 0.5654 -0.1501 0.5648 0.065 Uiso 1 1 calc R . . C77 C 0.5204(11) -0.1962(13) 0.4992(11) 0.076(7) Uiso 1 1 d . . . H77 H 0.4793 -0.1895 0.5134 0.091 Uiso 1 1 calc R . . C78 C 0.5318(13) -0.2280(16) 0.4477(12) 0.097(9) Uiso 1 1 d . . . H78 H 0.4985 -0.2396 0.4221 0.117 Uiso 1 1 calc R . . C79 C 0.5920(10) -0.2431(13) 0.4336(11) 0.075(7) Uiso 1 1 d . . . H79 H 0.5998 -0.2699 0.4008 0.091 Uiso 1 1 calc R . . C80 C 0.6401(11) -0.2208(13) 0.4651(10) 0.070(7) Uiso 1 1 d . . . H80 H 0.6815 -0.2305 0.4537 0.083 Uiso 1 1 calc R . . O7 O -0.0040(6) 0.8192(8) 0.2685(6) 0.071(4) Uiso 1 1 d D . . C81 C 0.0525(9) 0.8289(12) 0.2969(9) 0.079(7) Uiso 1 1 d D . . C82 C 0.0901(10) 0.8695(12) 0.2667(9) 0.076(8) Uiso 1 1 d D . . H82 H 0.0809 0.8852 0.2281 0.091 Uiso 1 1 calc R . . C83 C 0.1431(12) 0.8853(15) 0.2986(12) 0.112(11) Uiso 1 1 d D . . H83 H 0.1702 0.9167 0.2837 0.135 Uiso 1 1 calc R . . C84 C 0.1573(12) 0.8555(15) 0.3529(12) 0.107(10) Uiso 1 1 d D . . H84 H 0.1945 0.8669 0.3728 0.129 Uiso 1 1 calc R . . C85 C 0.1223(10) 0.8131(13) 0.3773(10) 0.086(8) Uiso 1 1 d D . . H85 H 0.1348 0.7910 0.4119 0.103 Uiso 1 1 calc R . . C86 C 0.0662(9) 0.8022(11) 0.3499(8) 0.064(6) Uiso 1 1 d D . . H86 H 0.0366 0.7757 0.3685 0.077 Uiso 1 1 calc R . . O8 O 0.0230(7) 1.2341(9) 0.7890(7) 0.078(5) Uiso 1 1 d U . . C87 C 0.0741(8) 1.2183(10) 0.7545(8) 0.079(7) Uiso 1 1 d GU . . C88 C 0.0748(9) 1.1780(10) 0.7061(9) 0.097(9) Uiso 1 1 d GU . . H88 H 0.0368 1.1638 0.6893 0.117 Uiso 1 1 calc R . . C89 C 0.1312(12) 1.1584(11) 0.6822(9) 0.145(14) Uiso 1 1 d GU . . H89 H 0.1317 1.1309 0.6491 0.174 Uiso 1 1 calc R . . C90 C 0.1868(9) 1.1791(14) 0.7067(13) 0.191(18) Uiso 1 1 d GU . . H90 H 0.2253 1.1658 0.6904 0.229 Uiso 1 1 calc R . . C91 C 0.1861(8) 1.2194(14) 0.7551(12) 0.178(16) Uiso 1 1 d GU . . H91 H 0.2241 1.2336 0.7719 0.214 Uiso 1 1 calc R . . C92 C 0.1297(11) 1.2390(10) 0.7790(8) 0.107(10) Uiso 1 1 d GU . . H92 H 0.1292 1.2665 0.8121 0.128 Uiso 1 1 calc R . . O9 O 0.1929(10) 1.2561(15) 0.4826(10) 0.149(9) Uiso 1 1 d D . . C93 C 0.1288(11) 1.2595(17) 0.4738(12) 0.109(10) Uiso 1 1 d D . . C94 C 0.1129(12) 1.2850(18) 0.4198(12) 0.128(12) Uiso 1 1 d D . . H94 H 0.1422 1.2997 0.3915 0.153 Uiso 1 1 calc R . . C95 C 0.0489(16) 1.287(6) 0.412(3) 0.59(10) Uiso 1 1 d D . . H95 H 0.0302 1.3050 0.3777 0.705 Uiso 1 1 calc R . . C96 C 0.0140(14) 1.259(2) 0.4575(17) 0.179(18) Uiso 1 1 d D . . H96 H -0.0275 1.2493 0.4467 0.215 Uiso 1 1 calc R . . C97 C 0.0286(14) 1.246(2) 0.5119(16) 0.171(17) Uiso 1 1 d D . . H97 H -0.0012 1.2354 0.5416 0.205 Uiso 1 1 calc R . . C98 C 0.0921(15) 1.247(3) 0.5225(15) 0.25(3) Uiso 1 1 d D . . H98 H 0.1092 1.2398 0.5609 0.303 Uiso 1 1 calc R . . O10 O 0.2492(12) 1.0861(12) 0.3857(11) 0.161(10) Uiso 1 1 d D . . C99 C 0.2717(15) 1.0263(13) 0.3805(11) 0.119(11) Uiso 1 1 d D . . C100 C 0.2791(15) 1.0074(15) 0.3234(11) 0.127(12) Uiso 1 1 d D . . H100 H 0.2639 1.0295 0.2898 0.152 Uiso 1 1 calc R . . C101 C 0.3115(19) 0.9522(17) 0.3202(14) 0.161(16) Uiso 1 1 d D . . H101 H 0.3215 0.9354 0.2822 0.194 Uiso 1 1 calc R . . C102 C 0.3298(18) 0.9204(17) 0.3713(16) 0.167(17) Uiso 1 1 d D . . H102 H 0.3503 0.8816 0.3664 0.200 Uiso 1 1 calc R . . C103 C 0.3208(15) 0.9403(15) 0.4249(14) 0.137(12) Uiso 1 1 d D . . H103 H 0.3339 0.9169 0.4585 0.165 Uiso 1 1 calc R . . C104 C 0.291(2) 0.9965(16) 0.4312(13) 0.186(18) Uiso 1 1 d D . . H104 H 0.2847 1.0143 0.4694 0.223 Uiso 1 1 calc R . . O11 O 0.8129(8) 0.0053(9) 0.4932(8) 0.092(5) Uiso 1 1 d D . . C105 C 0.7768(12) -0.0391(13) 0.4597(11) 0.091(9) Uiso 1 1 d D . . O12 O 0.7903(8) 0.7898(10) 0.5287(8) 0.095(6) Uiso 1 1 d D . . C106 C 0.7938(14) 0.7381(14) 0.5666(14) 0.116(10) Uiso 1 1 d D . . O13 O 0.8188(19) -0.0371(19) 0.6058(17) 0.247(18) Uiso 1 1 d D . . C107 C 0.8021(14) -0.0918(17) 0.6372(14) 0.109(10) Uiso 1 1 d D . . O14 O 0.2650(14) 1.0457(17) 0.6819(14) 0.176(11) Uiso 1 1 d D . . C108 C 0.307(2) 1.067(3) 0.637(2) 0.19(2) Uiso 1 1 d D . . O15 O 0.2359(17) 1.140(2) 0.4918(18) 0.223(16) Uiso 1 1 d D . . C109 C 0.218(4) 1.107(4) 0.544(3) 0.31(4) Uiso 1 1 d 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 Zn1 0.0241(10) 0.0321(12) 0.0376(11) -0.0028(11) 0.0013(9) 0.0027(9) I1 0.0643(9) 0.0652(11) 0.0550(8) -0.0067(9) 0.0077(7) 0.0308(7) N1 0.035(8) 0.028(11) 0.024(9) -0.006(8) -0.001(6) -0.005(7) C1 0.039(11) 0.010(11) 0.055(13) -0.011(9) -0.004(9) -0.005(9) C2 0.015(10) 0.08(2) 0.033(10) -0.001(12) 0.003(8) 0.016(10) C3 0.023(10) 0.021(12) 0.046(13) 0.004(10) 0.004(8) -0.004(8) C4 0.038(11) 0.055(16) 0.024(10) 0.009(10) -0.004(8) -0.019(10) C5 0.072(15) 0.053(16) 0.029(11) 0.004(13) -0.002(11) 0.016(12) N2 0.040(8) 0.046(13) 0.037(9) 0.011(9) 0.007(7) -0.020(8) C7 0.041(11) 0.032(13) 0.053(12) -0.002(11) 0.002(10) -0.008(10) C8 0.011(9) 0.059(17) 0.034(10) 0.002(11) 0.008(8) -0.008(9) C9 0.023(10) 0.029(14) 0.049(12) -0.024(10) -0.005(8) -0.006(9) C10 0.027(11) 0.043(14) 0.036(11) -0.007(10) 0.017(8) -0.013(9) C11 0.056(14) 0.059(19) 0.045(13) -0.008(12) -0.001(10) -0.032(12) N3 0.013(6) 0.054(8) 0.046(6) -0.000(6) -0.004(5) 0.008(5) C13 0.022(6) 0.052(8) 0.039(7) -0.002(6) -0.000(5) 0.001(6) C14 0.018(6) 0.048(8) 0.040(7) -0.007(6) -0.002(5) 0.007(6) C15 0.020(7) 0.041(9) 0.032(8) 0.000(8) 0.001(6) 0.009(7) C16 0.037(11) 0.057(16) 0.029(10) -0.011(10) 0.015(8) -0.012(10) C17 0.029(8) 0.052(10) 0.054(8) -0.011(7) -0.001(7) 0.002(7) C6 0.015(9) 0.030(13) 0.055(13) 0.011(11) -0.015(9) -0.005(9) N4 0.030(8) 0.044(12) 0.017(8) -0.004(8) 0.008(6) 0.003(8) C19 0.018(10) 0.039(14) 0.017(10) 0.000(10) -0.004(8) -0.002(9) N5 0.009(7) 0.036(11) 0.038(9) -0.002(8) -0.011(6) -0.002(6) C12 0.015(9) 0.056(14) 0.040(11) 0.002(10) -0.017(8) 0.007(9) N6 0.031(8) 0.023(9) 0.029(8) -0.006(7) 0.011(6) 0.006(7) C20 0.016(9) 0.023(12) 0.037(11) -0.003(9) -0.002(8) 0.014(8) N7 0.030(8) 0.044(11) 0.030(8) 0.006(9) 0.004(6) -0.003(8) C18 0.038(11) 0.022(13) 0.024(10) 0.014(10) 0.007(8) 0.008(9) N8 0.029(8) 0.026(10) 0.039(9) -0.004(9) -0.005(7) -0.001(7) C21 0.023(10) 0.035(13) 0.024(10) 0.013(10) -0.013(8) -0.003(9) N9 0.044(9) 0.032(10) 0.032(8) -0.007(8) -0.010(7) -0.000(8) C22 0.014(9) 0.032(13) 0.017(9) 0.007(9) -0.005(7) 0.014(8) Zn2 0.0230(10) 0.0338(13) 0.0349(11) -0.0010(11) 0.0027(9) -0.0022(9) I2 0.0307(6) 0.0587(10) 0.0606(8) 0.0197(8) 0.0092(6) -0.0041(6) N10 0.022(5) 0.041(8) 0.032(6) 0.003(7) -0.009(6) 0.008(6) C23 0.038(10) 0.023(12) 0.043(10) -0.017(9) 0.013(9) -0.015(9) C24 0.062(14) 0.055(15) 0.024(10) -0.007(11) 0.002(9) -0.009(11) C25 0.041(12) 0.013(12) 0.041(11) -0.003(9) -0.003(9) 0.006(8) C26 0.018(7) 0.042(9) 0.031(7) -0.005(7) -0.006(6) 0.004(7) C27 0.021(5) 0.042(8) 0.030(6) -0.008(7) -0.016(5) 0.003(6) N11 0.040(9) 0.063(13) 0.019(7) -0.018(8) -0.014(6) -0.005(8) C29 0.025(10) 0.079(16) 0.043(11) -0.012(11) 0.020(8) -0.022(10) C30 0.028(10) 0.049(15) 0.051(12) 0.002(11) 0.016(9) -0.024(10) C31 0.019(10) 0.023(12) 0.037(11) 0.007(9) 0.004(8) -0.005(8) C32 0.034(11) 0.063(18) 0.042(11) 0.010(12) -0.006(9) 0.013(11) C33 0.038(10) 0.039(13) 0.044(11) -0.010(10) -0.004(9) 0.002(10) N12 0.032(9) 0.042(12) 0.032(9) -0.001(8) 0.001(7) 0.003(8) C35 0.031(9) 0.046(13) 0.035(10) -0.007(10) 0.004(7) -0.001(8) C36 0.027(9) 0.052(13) 0.043(10) -0.020(9) 0.010(7) -0.013(8) C37 0.025(9) 0.054(14) 0.020(9) -0.005(8) 0.005(7) -0.004(7) C38 0.047(12) 0.028(13) 0.060(13) -0.027(11) 0.016(9) -0.025(10) C39 0.040(11) 0.056(16) 0.050(12) -0.027(12) 0.010(10) -0.028(11) C28 0.024(11) 0.054(16) 0.041(12) 0.022(12) 0.007(9) 0.023(11) N13 0.022(7) 0.013(9) 0.042(9) -0.016(7) -0.010(7) -0.001(7) C41 0.007(9) 0.052(15) 0.023(10) 0.021(10) 0.002(7) 0.005(9) N14 0.029(8) 0.019(10) 0.039(9) -0.015(8) -0.002(7) -0.003(7) C34 0.004(8) 0.046(14) 0.049(12) 0.009(11) -0.003(8) -0.007(9) N15 0.032(8) 0.015(10) 0.031(8) -0.009(7) 0.003(6) -0.007(7) C42 0.033(11) 0.029(14) 0.039(11) 0.014(11) 0.013(9) 0.016(10) N16 0.015(7) 0.028(11) 0.049(10) 0.006(8) 0.011(7) 0.011(7) C40 0.023(9) 0.023(13) 0.041(11) -0.004(10) -0.023(8) 0.003(8) N17 0.005(7) 0.060(11) 0.031(8) -0.004(8) -0.001(6) 0.001(7) C43 0.050(12) 0.021(12) 0.030(11) 0.011(9) -0.006(9) 0.015(9) N18 0.015(7) 0.051(11) 0.027(8) 0.003(8) 0.006(6) 0.006(7) C44 0.019(10) 0.031(13) 0.049(12) -0.002(11) -0.009(9) 0.008(9) _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 N2 2.044(16) 4_755 ? Zn1 N3 2.058(7) 3_566 ? Zn1 N1 2.103(15) . ? Zn1 I1 2.507(2) . ? N1 C5 1.26(2) . ? N1 C1 1.31(2) . ? C1 C2 1.36(3) . ? C2 C3 1.38(3) . ? C3 C4 1.37(2) . ? C3 C6 1.48(3) . ? C4 C5 1.41(3) . ? N2 C11 1.33(3) . ? N2 C7 1.37(2) . ? N2 Zn1 2.044(16) 4_745 ? C7 C8 1.33(2) . ? C8 C9 1.32(3) . ? C9 C10 1.44(3) . ? C9 C12 1.48(3) . ? C10 C11 1.33(3) . ? N3 C13 1.3900 . ? N3 C17 1.3900 . ? N3 Zn1 2.058(7) 3_466 ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 C18 1.538(19) . ? C16 C17 1.3900 . ? C6 N4 1.35(2) . ? C6 N9 1.38(2) . ? N4 C19 1.32(2) . ? C19 N5 1.27(2) . ? C19 C22 1.46(2) . ? N5 C12 1.40(2) . ? C12 N6 1.32(2) . ? N6 C20 1.33(2) . ? C20 C22 1.36(2) . ? C20 N7 1.41(2) . ? N7 C18 1.35(2) . ? C18 N8 1.31(2) . ? N8 C21 1.37(2) . ? C21 C22 1.37(2) . ? C21 N9 1.38(2) . ? Zn2 N10 2.019(7) . ? Zn2 N11 2.045(16) 4_655 ? Zn2 N12 2.065(14) 2_675 ? Zn2 I2 2.516(2) . ? N10 C23 1.3900 . ? N10 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 C28 1.55(2) . ? C26 C27 1.3900 . ? N11 C29 1.32(2) . ? N11 C33 1.32(2) . ? N11 Zn2 2.045(16) 4_645 ? C29 C30 1.38(3) . ? C30 C31 1.38(2) . ? C31 C32 1.42(3) . ? C31 C34 1.48(3) . ? C32 C33 1.43(3) . ? N12 C39 1.29(2) . ? N12 C35 1.33(2) . ? N12 Zn2 2.065(14) 2_674 ? C35 C36 1.39(2) . ? C36 C37 1.34(3) . ? C37 C38 1.40(2) . ? C37 C40 1.55(2) . ? C38 C39 1.41(2) . ? C28 N13 1.31(3) . ? C28 N18 1.40(2) . ? N13 C41 1.33(2) . ? C41 N14 1.37(2) . ? C41 C44 1.40(2) . ? N14 C34 1.31(2) . ? C34 N15 1.32(2) . ? N15 C42 1.33(2) . ? C42 C44 1.38(3) . ? C42 N16 1.41(2) . ? N16 C40 1.31(2) . ? C40 N17 1.32(2) . ? N17 C43 1.34(2) . ? C43 N18 1.36(2) . ? C43 C44 1.40(3) . ? O1 C45 1.387(18) . ? C45 C46 1.36(2) . ? C45 C50 1.37(2) . ? C46 C47 1.37(2) . ? C47 C48 1.42(2) . ? C48 C49 1.30(2) . ? C49 C50 1.38(2) . ? O2 C51 1.35(4) . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? O3 C57 1.35(2) . ? C57 C58 1.35(2) . ? C57 C62 1.38(3) . ? C58 C59 1.38(3) . ? C59 C60 1.38(3) . ? C60 C61 1.31(3) . ? C61 C62 1.39(3) . ? O4 C63 1.30(2) . ? C63 C68 1.40(3) . ? C63 C64 1.43(3) . ? C64 C65 1.43(3) . ? C65 C66 1.43(3) . ? C66 C67 1.37(3) . ? C67 C68 1.43(3) . ? O5 C69 1.396(18) . ? C69 C74 1.36(2) . ? C69 C70 1.37(2) . ? C70 C71 1.37(2) . ? C71 C72 1.41(2) . ? C72 C73 1.30(2) . ? C73 C74 1.38(2) . ? O6 C75 1.41(3) . ? C75 C76 1.30(3) . ? C75 C80 1.35(3) . ? C76 C77 1.39(3) . ? C77 C78 1.37(3) . ? C78 C79 1.37(3) . ? C79 C80 1.34(3) . ? O7 C81 1.388(17) . ? C81 C86 1.354(19) . ? C81 C82 1.37(2) . ? C82 C83 1.39(2) . ? C83 C84 1.41(2) . ? C84 C85 1.30(2) . ? C85 C86 1.37(2) . ? O8 C87 1.39(2) . ? C87 C88 1.3900 . ? C87 C92 1.3900 . ? C88 C89 1.3900 . ? C89 C90 1.3900 . ? C90 C91 1.3900 . ? C91 C92 1.3900 . ? O9 C93 1.395(19) . ? C93 C98 1.37(2) . ? C93 C94 1.37(2) . ? C94 C95 1.39(2) . ? C95 C96 1.40(2) . ? C96 C97 1.30(2) . ? C97 C98 1.39(2) . ? O10 C99 1.38(2) . ? C99 C100 1.35(2) . ? C99 C104 1.37(2) . ? C100 C101 1.38(2) . ? C101 C102 1.39(2) . ? C102 C103 1.29(2) . ? C103 C104 1.37(2) . ? O11 C105 1.443(16) . ? O12 C106 1.402(17) . ? O13 C107 1.416(18) . ? O14 C108 1.433(18) . ? O15 C109 1.427(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 N2 Zn1 N3 103.3(5) 4_755 3_566 ? N2 Zn1 N1 104.3(6) 4_755 . ? N3 Zn1 N1 98.6(5) 3_566 . ? N2 Zn1 I1 116.6(5) 4_755 . ? N3 Zn1 I1 112.2(3) 3_566 . ? N1 Zn1 I1 119.3(4) . . ? C5 N1 C1 123.5(18) . . ? C5 N1 Zn1 119.6(13) . . ? C1 N1 Zn1 116.6(13) . . ? N1 C1 C2 118.2(19) . . ? C1 C2 C3 122.2(17) . . ? C4 C3 C2 116.1(18) . . ? C4 C3 C6 123.0(18) . . ? C2 C3 C6 120.8(17) . . ? C3 C4 C5 118.6(18) . . ? N1 C5 C4 121.1(17) . . ? C11 N2 C7 115.0(17) . . ? C11 N2 Zn1 123.4(13) . 4_745 ? C7 N2 Zn1 121.5(15) . 4_745 ? C8 C7 N2 122(2) . . ? C9 C8 C7 122.2(19) . . ? C8 C9 C10 117.7(17) . . ? C8 C9 C12 121.8(18) . . ? C10 C9 C12 120.5(18) . . ? C11 C10 C9 116.5(19) . . ? N2 C11 C10 126(2) . . ? C13 N3 C17 120.0 . . ? C13 N3 Zn1 121.2(5) . 3_466 ? C17 N3 Zn1 118.7(5) . 3_466 ? C14 C13 N3 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 C18 122.6(10) . . ? C14 C15 C18 117.4(10) . . ? C15 C16 C17 120.0 . . ? C16 C17 N3 120.0 . . ? N4 C6 N9 129.5(17) . . ? N4 C6 C3 117.9(16) . . ? N9 C6 C3 112.6(16) . . ? C19 N4 C6 117.3(15) . . ? N5 C19 N4 121.2(16) . . ? N5 C19 C22 120.1(17) . . ? N4 C19 C22 118.6(15) . . ? C19 N5 C12 117.1(15) . . ? N6 C12 N5 126.1(16) . . ? N6 C12 C9 115.8(17) . . ? N5 C12 C9 118.0(17) . . ? C12 N6 C20 116.0(17) . . ? N6 C20 C22 122.8(16) . . ? N6 C20 N7 119.1(17) . . ? C22 C20 N7 118.0(15) . . ? C18 N7 C20 113.4(16) . . ? N8 C18 N7 132.5(16) . . ? N8 C18 C15 116.4(14) . . ? N7 C18 C15 111.0(16) . . ? C18 N8 C21 112.0(15) . . ? N8 C21 C22 121.6(17) . . ? N8 C21 N9 116.0(16) . . ? C22 C21 N9 122.4(16) . . ? C21 N9 C6 112.1(14) . . ? C20 C22 C21 122.3(16) . . ? C20 C22 C19 117.7(15) . . ? C21 C22 C19 120.0(17) . . ? N10 Zn2 N11 100.4(5) . 4_655 ? N10 Zn2 N12 102.6(5) . 2_675 ? N11 Zn2 N12 103.5(6) 4_655 2_675 ? N10 Zn2 I2 120.3(3) . . ? N11 Zn2 I2 110.3(4) 4_655 . ? N12 Zn2 I2 117.2(4) 2_675 . ? C23 N10 C27 120.0 . . ? C23 N10 Zn2 119.0(5) . . ? C27 N10 Zn2 120.2(5) . . ? C24 C23 N10 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 C28 118.5(9) . . ? C26 C25 C28 121.4(9) . . ? C27 C26 C25 120.0 . . ? C26 C27 N10 120.0 . . ? C29 N11 C33 117.5(17) . . ? C29 N11 Zn2 121.8(13) . 4_645 ? C33 N11 Zn2 120.6(14) . 4_645 ? N11 C29 C30 124.6(18) . . ? C31 C30 C29 119.3(16) . . ? C30 C31 C32 118.0(18) . . ? C30 C31 C34 123.6(15) . . ? C32 C31 C34 118.4(16) . . ? C31 C32 C33 116.8(17) . . ? N11 C33 C32 123.3(18) . . ? C39 N12 C35 119.6(16) . . ? C39 N12 Zn2 119.4(12) . 2_674 ? C35 N12 Zn2 121.0(13) . 2_674 ? N12 C35 C36 120.4(17) . . ? C37 C36 C35 121.2(17) . . ? C36 C37 C38 117.7(16) . . ? C36 C37 C40 121.9(15) . . ? C38 C37 C40 120.4(16) . . ? C37 C38 C39 117.4(17) . . ? N12 C39 C38 122.8(17) . . ? N13 C28 N18 132.2(17) . . ? N13 C28 C25 116.7(15) . . ? N18 C28 C25 110.8(17) . . ? C28 N13 C41 112.9(16) . . ? N13 C41 N14 118.3(15) . . ? N13 C41 C44 122.8(18) . . ? N14 C41 C44 118.8(16) . . ? C34 N14 C41 114.7(15) . . ? N14 C34 N15 131.8(18) . . ? N14 C34 C31 114.9(15) . . ? N15 C34 C31 113.3(16) . . ? C34 N15 C42 113.2(14) . . ? N15 C42 C44 122.2(17) . . ? N15 C42 N16 120.2(16) . . ? C44 C42 N16 117.5(19) . . ? C40 N16 C42 114.2(15) . . ? N16 C40 N17 133.1(17) . . ? N16 C40 C37 112.8(16) . . ? N17 C40 C37 114.0(16) . . ? C40 N17 C43 112.8(17) . . ? N17 C43 N18 118.6(18) . . ? N17 C43 C44 121.2(17) . . ? N18 C43 C44 120.1(18) . . ? C43 N18 C28 112.2(17) . . ? C42 C44 C41 119.2(19) . . ? C42 C44 C43 121.0(18) . . ? C41 C44 C43 119.7(17) . . ? C46 C45 C50 124.3(17) . . ? C46 C45 O1 112.6(17) . . ? C50 C45 O1 123.0(18) . . ? C45 C46 C47 115.2(17) . . ? C46 C47 C48 119(2) . . ? C49 C48 C47 124(2) . . ? C48 C49 C50 117.2(19) . . ? C45 C50 C49 119.4(18) . . ? O2 C51 C52 130.3(18) . . ? O2 C51 C56 109.5(18) . . ? C52 C51 C56 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C58 C57 O3 122.5(18) . . ? C58 C57 C62 120(2) . . ? O3 C57 C62 117.7(18) . . ? C57 C58 C59 118(2) . . ? C60 C59 C58 122(2) . . ? C61 C60 C59 120(2) . . ? C60 C61 C62 120(2) . . ? C57 C62 C61 121(2) . . ? O4 C63 C68 120.1(18) . . ? O4 C63 C64 117(2) . . ? C68 C63 C64 123(2) . . ? C63 C64 C65 115(2) . . ? C66 C65 C64 121(2) . . ? C67 C66 C65 124(2) . . ? C66 C67 C68 115(2) . . ? C63 C68 C67 122(2) . . ? C74 C69 C70 124.4(18) . . ? C74 C69 O5 120.1(18) . . ? C70 C69 O5 115.4(17) . . ? C69 C70 C71 116.8(18) . . ? C70 C71 C72 117.0(19) . . ? C73 C72 C71 125(2) . . ? C72 C73 C74 118(2) . . ? C69 C74 C73 117.9(18) . . ? C76 C75 C80 119(2) . . ? C76 C75 O6 120(2) . . ? C80 C75 O6 120(2) . . ? C75 C76 C77 124(2) . . ? C78 C77 C76 117(2) . . ? C77 C78 C79 119(3) . . ? C80 C79 C78 121(3) . . ? C79 C80 C75 120(2) . . ? C86 C81 C82 125.3(17) . . ? C86 C81 O7 122.0(17) . . ? C82 C81 O7 112.7(16) . . ? C81 C82 C83 112.6(17) . . ? C82 C83 C84 121(2) . . ? C85 C84 C83 124(2) . . ? C84 C85 C86 116(2) . . ? C81 C86 C85 120.8(18) . . ? O8 C87 C88 126.8(16) . . ? O8 C87 C92 112.4(16) . . ? C88 C87 C92 120.0 . . ? C87 C88 C89 120.0 . . ? C90 C89 C88 120.0 . . ? C91 C90 C89 120.0 . . ? C90 C91 C92 120.0 . . ? C91 C92 C87 120.0 . . ? C98 C93 C94 130(2) . . ? C98 C93 O9 116(2) . . ? C94 C93 O9 113.1(19) . . ? C93 C94 C95 112(2) . . ? C94 C95 C96 115(2) . . ? C97 C96 C95 131(3) . . ? C96 C97 C98 113(2) . . ? C93 C98 C97 116(2) . . ? C100 C99 C104 128(2) . . ? C100 C99 O10 114(2) . . ? C104 C99 O10 118(2) . . ? C99 C100 C101 112(2) . . ? C100 C101 C102 121(2) . . ? C103 C102 C101 124(2) . . ? C102 C103 C104 117(2) . . ? C103 C104 C99 118(2) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 22.27 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 1.504 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.146 _database_code_depnum_ccdc_archive 'CCDC 944051' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), (I 1-), (C22 H12 N9 1-), 6(C1 H4 O1), 2(C6 H5 N1 O2)' _chemical_formula_sum 'C40 H46 I N11 O10 Zn' _chemical_formula_weight 1033.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0029 0.0015 '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' I I -0.4925 1.7199 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0057 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.3005 1.3595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0101 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' 'y, x, -z+1/2' '-x+y, -x, z' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+y+2/3, -x+1/3, z+1/3' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+y+1/3, -x+2/3, z+2/3' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' '-y, -x, z-1/2' 'x-y, x, -z' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x-y+2/3, x+1/3, -z+1/3' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x-y+1/3, x+2/3, -z+2/3' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 44.006(1) _cell_length_b 44.006(1) _cell_length_c 28.267(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 47406(2) _cell_formula_units_Z 36 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 140618 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.31 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 18936 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8029 _exptl_absorpt_correction_T_max 1.0643 _exptl_absorpt_process_details 'PLATON MULABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(2) _diffrn_radiation_wavelength 0.68900 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'KEK PF-AR NW2 beamline' _diffrn_radiation_monochromator 'Si 111' _diffrn_measurement_device_type 'RIGAKU Mercury CCD system' _diffrn_measurement_method 'oscillation method, \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 140618 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -57 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.31 _reflns_number_total 12797 _reflns_number_gt 7155 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Crystal Clear (Molecular Structure Corporation, 2001)' _computing_cell_refinement 'HKL2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Several restraints were applied to disordered methanol and nitrobeneze on a basis of chemical symmetry of the molecules. A nitrobeneze is disordered at two positions with occupancy of 0.5, respectively. Large residual electron density peaks sit around zinc atoms. Several solvents were refined with isotropic thermal parameters. 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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_number_reflns 12797 _refine_ls_number_parameters 482 _refine_ls_number_restraints 210 _refine_ls_R_factor_all 0.1610 _refine_ls_R_factor_gt 0.1240 _refine_ls_wR_factor_ref 0.3849 _refine_ls_wR_factor_gt 0.3556 _refine_ls_goodness_of_fit_ref 1.365 _refine_ls_restrained_S_all 1.360 _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 Zn1 Zn 0.492837(19) 0.645565(17) -0.193100(19) 0.0673(3) Uani 1 1 d . . . I1 I 0.454047(19) 0.671974(19) -0.19214(2) 0.1174(3) Uani 1 1 d . . . N1 N 0.54373(13) 0.68255(11) -0.17890(13) 0.0644(12) Uani 1 1 d . . . C1 C 0.55882(18) 0.71303(15) -0.20397(18) 0.0698(15) Uani 1 1 d . . . H1 H 0.5453 0.7158 -0.2280 0.084 Uiso 1 1 calc R . . C2 C 0.59192(17) 0.73954(16) -0.19655(18) 0.0677(14) Uani 1 1 d . . . H2 H 0.6017 0.7602 -0.2154 0.081 Uiso 1 1 calc R . . C3 C 0.61129(17) 0.73572(14) -0.16044(16) 0.0651(14) Uani 1 1 d . . . C4 C 0.59688(16) 0.70488(14) -0.13556(16) 0.0622(13) Uani 1 1 d . . . H4 H 0.6098 0.7016 -0.1112 0.075 Uiso 1 1 calc R . . C5 C 0.56288(18) 0.67842(15) -0.14658(17) 0.0690(15) Uani 1 1 d . . . H5 H 0.5533 0.6567 -0.1302 0.083 Uiso 1 1 calc R . . N2 N 0.79538(13) 0.94234(12) -0.30932(13) 0.0643(11) Uani 1 1 d . . . C7 C 0.81080(18) 0.94512(15) -0.26707(17) 0.0707(15) Uani 1 1 d . . . H7 H 0.8336 0.9646 -0.2618 0.085 Uiso 1 1 calc R . . C8 C 0.79530(16) 0.92122(15) -0.23146(17) 0.0689(14) Uani 1 1 d . . . H8 H 0.8069 0.9243 -0.2020 0.083 Uiso 1 1 calc R . . C9 C 0.76224(16) 0.89233(14) -0.23896(16) 0.0654(14) Uani 1 1 d . . . C10 C 0.74532(17) 0.89022(17) -0.28168(18) 0.0815(19) Uani 1 1 d . . . H10 H 0.7221 0.8716 -0.2872 0.098 Uiso 1 1 calc R . . C11 C 0.76252(18) 0.91507(16) -0.31525(18) 0.0802(18) Uani 1 1 d . . . H11 H 0.7509 0.9132 -0.3443 0.096 Uiso 1 1 calc R . . N3 N 0.79362(15) 0.83520(13) 0.07889(13) 0.0674(12) Uani 1 1 d . . . C13 C 0.7641(2) 0.8069(2) 0.0683(2) 0.087(2) Uani 1 1 d . . . H13 H 0.7541 0.7885 0.0909 0.104 Uiso 1 1 calc R . . C14 C 0.74650(18) 0.80237(17) 0.02634(19) 0.0789(18) Uani 1 1 d . . . H14 H 0.7249 0.7813 0.0210 0.095 Uiso 1 1 calc R . . C15 C 0.75936(17) 0.82709(15) -0.00684(16) 0.0670(14) Uani 1 1 d . . . C16 C 0.7898(3) 0.8578(2) 0.0037(2) 0.123(3) Uani 1 1 d . . . H16 H 0.7995 0.8767 -0.0181 0.148 Uiso 1 1 calc R . . C17 C 0.8063(3) 0.8605(2) 0.0475(2) 0.125(4) Uani 1 1 d . . . H17 H 0.8274 0.8815 0.0546 0.150 Uiso 1 1 calc R . . C6 C 0.64740(15) 0.76556(13) -0.15055(16) 0.0591(13) Uani 1 1 d . . . N4 N 0.66181(13) 0.78894(12) -0.18643(13) 0.0643(11) Uani 1 1 d . . . C19 C 0.69456(15) 0.81558(13) -0.17851(15) 0.0582(12) Uani 1 1 d . . . N5 N 0.71119(13) 0.83996(11) -0.21264(13) 0.0632(11) Uani 1 1 d . . . C12 C 0.74365(17) 0.86480(14) -0.20147(16) 0.0650(14) Uani 1 1 d . . . N6 N 0.76233(13) 0.86996(12) -0.16166(14) 0.0694(12) Uani 1 1 d . . . C20 C 0.74517(17) 0.84583(14) -0.12752(15) 0.0664(14) Uani 1 1 d . . . N7 N 0.76101(14) 0.84842(12) -0.08504(13) 0.0679(12) Uani 1 1 d . . . C18 C 0.74208(17) 0.82359(15) -0.05365(15) 0.0641(14) Uani 1 1 d . . . N8 N 0.70915(14) 0.79542(12) -0.05741(13) 0.0626(11) Uani 1 1 d . . . C21 C 0.69314(17) 0.79261(15) -0.10021(16) 0.0628(13) Uani 1 1 d . . . N9 N 0.66088(13) 0.76572(12) -0.10788(14) 0.0614(11) Uani 1 1 d . . . C22 C 0.71104(16) 0.81812(13) -0.13491(15) 0.0605(13) Uani 1 1 d . . . C23 C 0.8504(3) 0.6937(3) -0.0473(3) 0.095(4) Uiso 0.50 1 d PGDU A -1 C24 C 0.8477(3) 0.7219(3) -0.0641(3) 0.111(5) Uiso 0.50 1 d PGDU A -1 H24 H 0.8555 0.7306 -0.0951 0.134 Uiso 0.50 1 calc PR A -1 C25 C 0.8336(3) 0.7375(3) -0.0355(5) 0.112(5) Uiso 0.50 1 d PGDU A -1 H25 H 0.8317 0.7568 -0.0469 0.134 Uiso 0.50 1 calc PR A -1 C26 C 0.8221(3) 0.7247(3) 0.0099(4) 0.137(7) Uiso 0.50 1 d PGDU A -1 H26 H 0.8125 0.7353 0.0295 0.164 Uiso 0.50 1 calc PR A -1 C27 C 0.8248(3) 0.6965(4) 0.0267(3) 0.117(6) Uiso 0.50 1 d PGDU A -1 H27 H 0.8170 0.6878 0.0577 0.141 Uiso 0.50 1 calc PR A -1 C28 C 0.8389(3) 0.6809(3) -0.0019(4) 0.110(5) Uiso 0.50 1 d PGDU A -1 H28 H 0.8407 0.6616 0.0096 0.132 Uiso 0.50 1 calc PR A -1 N10 N 0.8650(4) 0.6775(4) -0.0784(5) 0.134(6) Uiso 0.50 1 d PDU A -1 O1 O 0.8771(4) 0.6929(3) -0.1153(4) 0.118(4) Uiso 0.50 1 d PDU A -1 O2 O 0.8657(5) 0.6503(4) -0.0678(6) 0.175(7) Uiso 0.50 1 d PDU A -1 C29 C 0.7199(4) 0.5103(4) 0.0253(5) 0.141(7) Uiso 0.50 1 d PGDU B -2 C30 C 0.7124(4) 0.5173(4) 0.0704(6) 0.132(6) Uiso 0.50 1 d PGDU B -2 H30 H 0.7113 0.5380 0.0762 0.159 Uiso 0.50 1 calc PR B -2 C31 C 0.7066(5) 0.4940(5) 0.1072(5) 0.171(9) Uiso 0.50 1 d PGDU B -2 H31 H 0.7015 0.4988 0.1380 0.205 Uiso 0.50 1 calc PR B -2 C32 C 0.7082(5) 0.4637(5) 0.0988(6) 0.185(10) Uiso 0.50 1 d PGDU B -2 H32 H 0.7042 0.4478 0.1239 0.221 Uiso 0.50 1 calc PR B -2 C33 C 0.7157(6) 0.4567(4) 0.0537(8) 0.178(10) Uiso 0.50 1 d PGDU B -2 H33 H 0.7168 0.4360 0.0479 0.214 Uiso 0.50 1 calc PR B -2 C34 C 0.7215(5) 0.4800(5) 0.0169(5) 0.210(13) Uiso 0.50 1 d PGDU B -2 H34 H 0.7266 0.4753 -0.0139 0.251 Uiso 0.50 1 calc PR B -2 N11 N 0.7261(8) 0.5331(6) -0.0158(7) 0.222(11) Uiso 0.50 1 d PDU B -2 O3 O 0.7389(6) 0.5254(6) -0.0488(8) 0.217(9) Uiso 0.50 1 d PDU B -2 O4 O 0.7225(10) 0.5588(8) -0.0157(12) 0.34(2) Uiso 0.50 1 d PDU B -2 O10 O 0.6892(3) 0.6256(3) -0.2227(5) 0.111(3) Uiso 0.50 1 d PDU C -2 C48 C 0.7022(14) 0.6513(11) -0.2562(14) 0.239(17) Uiso 0.50 1 d PDU C -2 O13 O 0.8140(10) 0.7935(9) -0.3335(13) 0.276(14) Uiso 0.50 1 d PDU D -2 C51 C 0.7868(14) 0.7600(12) -0.316(2) 0.29(2) Uiso 0.50 1 d PDU D -2 O18 O 0.6331(14) 0.6422(16) -0.425(2) 0.40(3) Uiso 0.50 1 d PDU E -2 C56 C 0.632(3) 0.647(3) -0.475(2) 0.47(5) Uiso 0.50 1 d PDU E -2 C35 C 0.7788(5) 0.6296(4) -0.1111(5) 0.154(8) Uiso 0.50 1 d PGDU F -3 C36 C 0.7694(5) 0.6553(5) -0.1068(6) 0.178(10) Uiso 0.50 1 d PGDU F -3 H36 H 0.7578 0.6564 -0.0791 0.214 Uiso 0.50 1 calc PR F -3 C37 C 0.7771(5) 0.6794(4) -0.1431(7) 0.187(11) Uiso 0.50 1 d PGDU F -3 H37 H 0.7707 0.6969 -0.1402 0.225 Uiso 0.50 1 calc PR F -3 C38 C 0.7940(5) 0.6777(5) -0.1837(6) 0.187(11) Uiso 0.50 1 d PGDU F -3 H38 H 0.7993 0.6942 -0.2085 0.225 Uiso 0.50 1 calc PR F -3 C39 C 0.8034(4) 0.6520(5) -0.1879(5) 0.125(6) Uiso 0.50 1 d PGDU F -3 H39 H 0.8150 0.6509 -0.2156 0.150 Uiso 0.50 1 calc PR F -3 C40 C 0.7958(4) 0.6279(4) -0.1516(5) 0.133(6) Uiso 0.50 1 d PGDU F -3 H40 H 0.8022 0.6103 -0.1545 0.160 Uiso 0.50 1 calc PR F -3 N12 N 0.7732(7) 0.6040(6) -0.0732(7) 0.197(10) Uiso 0.50 1 d PDU F -3 O5 O 0.7647(7) 0.6108(6) -0.0355(7) 0.218(9) Uiso 0.50 1 d PDU F -3 O6 O 0.7782(8) 0.5793(7) -0.0800(9) 0.246(11) Uiso 0.50 1 d PDU F -3 C41 C 0.7033(5) 0.6230(6) 0.1339(7) 0.194(11) Uiso 0.50 1 d PGDU G -3 C42 C 0.7126(7) 0.6035(7) 0.1049(10) 0.292(19) Uiso 0.50 1 d PGDU G -3 H42 H 0.7076 0.5807 0.1144 0.350 Uiso 0.50 1 calc PR G -3 C43 C 0.7294(8) 0.6173(10) 0.0620(10) 0.31(2) Uiso 0.50 1 d PGDU G -3 H43 H 0.7358 0.6039 0.0422 0.371 Uiso 0.50 1 calc PR G -3 C44 C 0.7368(7) 0.6506(11) 0.0482(8) 0.279(18) Uiso 0.50 1 d PGDU G -3 H44 H 0.7483 0.6601 0.0189 0.335 Uiso 0.50 1 calc PR G -3 C45 C 0.7275(8) 0.6702(7) 0.0772(11) 0.27(2) Uiso 0.50 1 d PGDU G -3 H45 H 0.7326 0.6929 0.0677 0.325 Uiso 0.50 1 calc PR G -3 C46 C 0.7108(7) 0.6564(6) 0.1200(10) 0.231(14) Uiso 0.50 1 d PGDU G -3 H47 H 0.7044 0.6697 0.1399 0.277 Uiso 0.50 1 calc PR G -3 N13 N 0.6860(9) 0.6093(7) 0.1797(8) 0.275(15) Uiso 0.50 1 d PDU G -3 O7 O 0.6808(9) 0.6303(7) 0.2014(10) 0.261(14) Uiso 0.50 1 d PDU G -3 O8 O 0.6776(6) 0.5799(6) 0.1941(8) 0.198(8) Uiso 0.50 1 d PDU G -3 O11 O 0.6990(7) 0.5116(8) -0.1571(10) 0.227(10) Uiso 0.50 1 d PDU H -3 C49 C 0.7206(7) 0.5079(7) -0.1888(10) 0.153(8) Uiso 0.50 1 d PDU H -3 O15 O 0.7104(15) 0.4810(14) 0.2251(17) 0.36(2) Uiso 0.50 1 d PDU I -3 C53 C 0.6940(14) 0.4932(14) 0.1927(19) 0.259(19) Uiso 0.50 1 d PDU I -3 O12 O 0.6907(17) 0.3499(18) 0.072(2) 0.23(3) Uiso 0.17 1 d PDU J -4 C50 C 0.6908(13) 0.3648(12) 0.0276(18) 0.097(12) Uiso 0.17 1 d PDU J -4 O14 O 0.7540(15) 0.7451(15) -0.457(2) 0.64(3) Uiso 1 1 d DU K -4 C52 C 0.7263(14) 0.7292(14) -0.4235(19) 0.42(2) Uiso 1 1 d DU K -4 O16 O 0.6446(14) 0.2919(13) -0.1073(19) 0.278(19) Uiso 0.33 1 d PDU L -4 C54 C 0.6681(16) 0.3030(16) -0.069(2) 0.23(2) Uiso 0.33 1 d PDU L -4 O17 O 0.5475(15) 0.2287(16) -0.094(2) 0.63(3) Uiso 1 1 d DU M -4 C55 C 0.529(2) 0.224(2) -0.138(3) 0.61(4) Uiso 1 1 d DU M -4 O9 O 0.62642(19) 0.72594(19) -0.0231(3) 0.131(2) Uiso 1 1 d DU . . C47 C 0.6455(3) 0.7186(3) 0.0079(4) 0.127(3) Uiso 1 1 d DU . . 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 0.0978(5) 0.0689(4) 0.0316(3) 0.0062(2) 0.0067(3) 0.0390(4) I1 0.1311(6) 0.1302(6) 0.1076(5) 0.0152(3) 0.0077(3) 0.0777(4) N1 0.102(3) 0.059(2) 0.0305(17) 0.0059(16) 0.0043(19) 0.039(2) C1 0.094(4) 0.068(3) 0.042(2) 0.013(2) 0.007(3) 0.037(3) C2 0.097(4) 0.070(3) 0.046(3) 0.011(2) 0.004(3) 0.048(3) C3 0.097(4) 0.066(3) 0.032(2) 0.001(2) 0.007(2) 0.041(3) C4 0.089(4) 0.062(3) 0.038(2) 0.005(2) -0.004(2) 0.040(3) C5 0.107(4) 0.063(3) 0.034(2) 0.004(2) 0.001(2) 0.040(3) N2 0.086(3) 0.066(3) 0.0322(18) 0.0057(17) -0.0030(18) 0.031(2) C7 0.097(4) 0.070(3) 0.035(2) -0.001(2) -0.014(2) 0.034(3) C8 0.092(4) 0.074(3) 0.032(2) 0.000(2) -0.009(2) 0.034(3) C9 0.101(4) 0.063(3) 0.028(2) 0.0047(19) -0.003(2) 0.038(3) C10 0.085(4) 0.087(4) 0.037(2) 0.014(2) -0.012(2) 0.016(3) C11 0.099(4) 0.078(4) 0.038(2) 0.011(2) -0.012(3) 0.025(3) N3 0.102(4) 0.080(3) 0.0268(17) 0.0025(18) 0.002(2) 0.051(3) C13 0.106(5) 0.101(5) 0.042(3) 0.022(3) -0.006(3) 0.043(4) C14 0.091(4) 0.080(4) 0.043(3) 0.012(2) -0.012(3) 0.026(3) C15 0.108(4) 0.070(3) 0.030(2) 0.000(2) -0.006(2) 0.049(3) C16 0.148(7) 0.109(6) 0.052(3) 0.023(4) -0.031(4) 0.018(5) C17 0.154(8) 0.112(6) 0.048(3) 0.019(4) -0.023(4) 0.021(5) C6 0.093(4) 0.055(3) 0.035(2) 0.0058(19) 0.005(2) 0.042(3) N4 0.096(3) 0.064(3) 0.0341(18) 0.0081(17) 0.0015(19) 0.041(3) C19 0.089(4) 0.057(3) 0.0301(19) 0.0059(18) 0.004(2) 0.037(3) N5 0.097(3) 0.062(2) 0.0292(17) 0.0044(16) -0.0005(19) 0.039(3) C12 0.101(4) 0.063(3) 0.031(2) 0.006(2) 0.002(2) 0.041(3) N6 0.097(3) 0.063(3) 0.0335(19) 0.0061(17) -0.005(2) 0.029(2) C20 0.108(4) 0.066(3) 0.0249(19) 0.0034(19) -0.003(2) 0.043(3) N7 0.101(3) 0.070(3) 0.0290(17) 0.0022(17) -0.0053(19) 0.040(3) C18 0.100(4) 0.066(3) 0.030(2) 0.001(2) -0.004(2) 0.044(3) N8 0.097(3) 0.067(3) 0.0281(17) 0.0057(17) 0.0001(19) 0.045(3) C21 0.099(4) 0.066(3) 0.033(2) 0.004(2) 0.000(2) 0.048(3) N9 0.089(3) 0.062(3) 0.0362(18) 0.0053(17) 0.0014(19) 0.039(3) C22 0.095(4) 0.056(3) 0.031(2) -0.0011(18) -0.002(2) 0.039(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 2.010(4) 36_545 ? Zn1 N3 2.021(4) 14_654 ? Zn1 N1 2.045(5) . ? Zn1 I1 2.4998(10) . ? N1 C5 1.316(7) . ? N1 C1 1.361(7) . ? C1 C2 1.352(9) . ? C2 C3 1.393(8) . ? C3 C4 1.370(7) . ? C3 C6 1.497(9) . ? C4 C5 1.396(9) . ? N2 C7 1.349(6) . ? N2 C11 1.350(8) . ? N2 Zn1 2.010(4) 30 ? C7 C8 1.366(8) . ? C8 C9 1.389(8) . ? C9 C10 1.397(7) . ? C9 C12 1.507(7) . ? C10 C11 1.357(8) . ? N3 C13 1.308(9) . ? N3 C17 1.309(9) . ? N3 Zn1 2.021(4) 10_565 ? C13 C14 1.373(8) . ? C14 C15 1.330(8) . ? C15 C16 1.378(10) . ? C15 C18 1.495(7) . ? C16 C17 1.409(10) . ? C6 N9 1.343(6) . ? C6 N4 1.355(6) . ? N4 C19 1.346(7) . ? C19 N5 1.353(6) . ? C19 C22 1.406(7) . ? N5 C12 1.332(8) . ? C12 N6 1.344(7) . ? N6 C20 1.352(7) . ? C20 N7 1.364(6) . ? C20 C22 1.398(8) . ? N7 C18 1.328(7) . ? C18 N8 1.361(8) . ? N8 C21 1.374(6) . ? C21 N9 1.335(8) . ? C21 C22 1.399(7) . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C23 N10 1.467(9) . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? N10 O1 1.214(9) . ? N10 O2 1.248(9) . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C29 N11 1.468(10) . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? N11 O4 1.220(10) . ? N11 O3 1.221(10) . ? O10 C48 1.36(2) . ? O13 C51 1.44(2) . ? O18 C56 1.43(3) . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C35 N12 1.481(10) . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? N12 O5 1.215(10) . ? N12 O6 1.228(9) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 N13 1.470(10) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? N13 O7 1.222(10) . ? N13 O8 1.224(10) . ? O11 C49 1.38(2) . ? O15 C53 1.43(2) . ? O12 C50 1.42(3) . ? O14 C52 1.43(2) . ? O16 C54 1.41(2) . ? O17 C55 1.43(3) . ? O9 C47 1.359(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N3 107.36(19) 36_545 14_654 ? N2 Zn1 N1 104.54(18) 36_545 . ? N3 Zn1 N1 101.47(18) 14_654 . ? N2 Zn1 I1 112.74(14) 36_545 . ? N3 Zn1 I1 118.33(15) 14_654 . ? N1 Zn1 I1 111.01(13) . . ? C5 N1 C1 117.9(5) . . ? C5 N1 Zn1 123.3(4) . . ? C1 N1 Zn1 118.9(4) . . ? C2 C1 N1 123.6(6) . . ? C1 C2 C3 118.0(5) . . ? C4 C3 C2 119.2(6) . . ? C4 C3 C6 122.4(5) . . ? C2 C3 C6 118.4(5) . . ? C3 C4 C5 118.9(5) . . ? N1 C5 C4 122.2(5) . . ? C7 N2 C11 117.2(5) . . ? C7 N2 Zn1 121.1(4) . 30 ? C11 N2 Zn1 121.6(3) . 30 ? N2 C7 C8 123.2(6) . . ? C7 C8 C9 118.9(5) . . ? C8 C9 C10 118.2(5) . . ? C8 C9 C12 121.9(4) . . ? C10 C9 C12 119.8(5) . . ? C11 C10 C9 119.1(6) . . ? N2 C11 C10 123.2(5) . . ? C13 N3 C17 116.8(5) . . ? C13 N3 Zn1 122.7(4) . 10_565 ? C17 N3 Zn1 120.5(5) . 10_565 ? N3 C13 C14 123.8(6) . . ? C15 C14 C13 120.7(6) . . ? C14 C15 C16 117.1(5) . . ? C14 C15 C18 123.6(6) . . ? C16 C15 C18 119.2(5) . . ? C15 C16 C17 118.7(6) . . ? N3 C17 C16 122.7(8) . . ? N9 C6 N4 129.1(5) . . ? N9 C6 C3 116.4(4) . . ? N4 C6 C3 114.5(4) . . ? C19 N4 C6 115.3(4) . . ? N4 C19 N5 119.4(4) . . ? N4 C19 C22 120.0(4) . . ? N5 C19 C22 120.6(5) . . ? C12 N5 C19 114.5(4) . . ? N5 C12 N6 130.7(5) . . ? N5 C12 C9 114.9(4) . . ? N6 C12 C9 114.4(5) . . ? C12 N6 C20 114.2(5) . . ? N6 C20 N7 120.1(5) . . ? N6 C20 C22 120.9(4) . . ? N7 C20 C22 119.0(5) . . ? C18 N7 C20 115.8(5) . . ? N7 C18 N8 129.9(5) . . ? N7 C18 C15 115.4(5) . . ? N8 C18 C15 114.7(4) . . ? C18 N8 C21 114.5(4) . . ? N9 C21 N8 119.5(5) . . ? N9 C21 C22 121.3(5) . . ? N8 C21 C22 119.2(5) . . ? C21 N9 C6 114.9(4) . . ? C20 C22 C21 121.6(5) . . ? C20 C22 C19 119.1(4) . . ? C21 C22 C19 119.3(5) . . ? C24 C23 C28 120.0 . . ? C24 C23 N10 119.0(8) . . ? C28 C23 N10 121.0(8) . . ? C23 C24 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? O1 N10 O2 121.8(12) . . ? O1 N10 C23 114.9(11) . . ? O2 N10 C23 123.3(13) . . ? C30 C29 C34 120.0 . . ? C30 C29 N11 124.0(12) . . ? C34 C29 N11 116.0(12) . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C29 120.0 . . ? O4 N11 O3 123.5(15) . . ? O4 N11 C29 124.4(19) . . ? O3 N11 C29 111.7(16) . . ? C36 C35 C40 120.0 . . ? C36 C35 N12 123.4(11) . . ? C40 C35 N12 116.6(11) . . ? C35 C36 C37 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? O5 N12 O6 124.6(14) . . ? O5 N12 C35 113.8(16) . . ? O6 N12 C35 121.5(16) . . ? C42 C41 C46 120.0 . . ? C42 C41 N13 121.3(15) . . ? C46 C41 N13 118.7(15) . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? O7 N13 O8 124.0(15) . . ? O7 N13 C41 112.9(17) . . ? O8 N13 C41 123.2(17) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 24.42 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.123 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.215 _database_code_depnum_ccdc_archive 'CCDC 944052' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), (I 1-), (C22 H12 N9 1-), 1(C1 H3 O1 H1), 3(C6 N1 H7)' _chemical_formula_sum 'C41 H37 I N12 O Zn' _chemical_formula_weight 906.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0029 0.0015 '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' I I -0.4926 1.7198 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0057 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.3005 1.3594 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0101 0.0057 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 15.1138(1) _cell_length_b 18.5709(1) _cell_length_c 15.6792(1) _cell_angle_alpha 90.00 _cell_angle_beta 117.212(2) _cell_angle_gamma 90.00 _cell_volume 3913.71(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 83132 _cell_measurement_theta_min 1.84 _cell_measurement_theta_max 29.47 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 1.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7833 _exptl_absorpt_correction_T_max 0.8142 _exptl_absorpt_process_details 'PLATON MULABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68899 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PLSII 2D bending magnet' _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_measurement_device_type 'ADSC Q210 CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83132 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.47 _reflns_number_total 11902 _reflns_number_gt 9890 _reflns_threshold_expression >2\s(I) _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL3000 _computing_data_reduction HKL3000 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Several restraints (DFIX, SADI and FLAT) were applied to disordered aniline on a basis of chemical symmetry of the molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+5.8306P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method constr _refine_ls_extinction_coef ? _refine_ls_number_reflns 11902 _refine_ls_number_parameters 603 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _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 H1O H 0.697(3) 0.412(3) 0.774(3) 0.041(11) Uiso 1 1 d . . . N1 N 0.57537(18) 0.33485(15) 0.54145(15) 0.0273(5) Uani 1 1 d . . . C1 C 0.6103(3) 0.3091(2) 0.4839(2) 0.0424(8) Uani 1 1 d . . . H1 H 0.6570 0.2707 0.5064 0.051 Uiso 1 1 calc R . . C2 C 0.5819(3) 0.3356(2) 0.3926(2) 0.0464(10) Uani 1 1 d . . . H2 H 0.6094 0.3161 0.3539 0.056 Uiso 1 1 calc R . . C3 C 0.5131(2) 0.39073(17) 0.35835(18) 0.0272(5) Uani 1 1 d . . . C4 C 0.4780(3) 0.4187(2) 0.4188(2) 0.0386(7) Uani 1 1 d . . . H4 H 0.4314 0.4572 0.3985 0.046 Uiso 1 1 calc R . . C5 C 0.5122(3) 0.3894(2) 0.5100(2) 0.0425(8) Uani 1 1 d . . . H5 H 0.4890 0.4095 0.5518 0.051 Uiso 1 1 calc R . . N2 N 0.5569(2) 0.31545(15) -0.23380(16) 0.0288(5) Uani 1 1 d . . . C7 C 0.4816(3) 0.3624(2) -0.2620(2) 0.0441(9) Uani 1 1 d . . . H7 H 0.4505 0.3773 -0.3272 0.053 Uiso 1 1 calc R . . C8 C 0.4467(3) 0.3904(2) -0.2014(2) 0.0430(8) Uani 1 1 d . . . H8 H 0.3930 0.4237 -0.2247 0.052 Uiso 1 1 calc R . . C9 C 0.4915(2) 0.36917(17) -0.10586(19) 0.0296(6) Uani 1 1 d . . . C10 C 0.5680(3) 0.31881(18) -0.07658(19) 0.0318(6) Uani 1 1 d . . . H10 H 0.5988 0.3018 -0.0123 0.038 Uiso 1 1 calc R . . C11 C 0.5988(3) 0.29376(17) -0.1418(2) 0.0312(6) Uani 1 1 d . . . H11 H 0.6517 0.2599 -0.1208 0.037 Uiso 1 1 calc R . . N3 N 0.0187(2) 0.71319(15) -0.10100(17) 0.0294(5) Uani 1 1 d . . . C13 C 0.0730(3) 0.70351(18) -0.0057(2) 0.0323(6) Uani 1 1 d . . . H13 H 0.0579 0.7322 0.0361 0.039 Uiso 1 1 calc R . . C14 C 0.1495(2) 0.65415(19) 0.03442(19) 0.0327(6) Uani 1 1 d . . . H14 H 0.1849 0.6490 0.1021 0.039 Uiso 1 1 calc R . . C15 C 0.1744(2) 0.61226(17) -0.02442(19) 0.0278(5) Uani 1 1 d . . . C16 C 0.1187(3) 0.6218(2) -0.1230(2) 0.0398(8) Uani 1 1 d . . . H16 H 0.1329 0.5942 -0.1663 0.048 Uiso 1 1 calc R . . C17 C 0.0427(3) 0.6718(2) -0.1572(2) 0.0409(8) Uani 1 1 d . . . H17 H 0.0051 0.6771 -0.2247 0.049 Uiso 1 1 calc R . . C6 C 0.4738(2) 0.41785(17) 0.25752(18) 0.0275(5) Uani 1 1 d . . . N4 N 0.5114(2) 0.38477(15) 0.20485(16) 0.0303(5) Uani 1 1 d . . . C19 C 0.4712(2) 0.40611(17) 0.11193(19) 0.0286(5) Uani 1 1 d . . . N5 N 0.5028(2) 0.37615(15) 0.05205(17) 0.0308(5) Uani 1 1 d . . . C12 C 0.4574(2) 0.40091(17) -0.03873(19) 0.0296(6) Uani 1 1 d . . . N6 N 0.3860(2) 0.45090(15) -0.07804(16) 0.0306(5) Uani 1 1 d . . . C20 C 0.3535(2) 0.48032(16) -0.01838(19) 0.0283(5) Uani 1 1 d . . . N7 N 0.2813(2) 0.53056(15) -0.05128(16) 0.0303(5) Uani 1 1 d . . . C18 C 0.2560(2) 0.55797(16) 0.01391(19) 0.0283(5) Uani 1 1 d . . . N8 N 0.29494(19) 0.54266(14) 0.10837(16) 0.0270(5) Uani 1 1 d . . . C21 C 0.3652(2) 0.49051(16) 0.14083(18) 0.0262(5) Uani 1 1 d . . . N9 N 0.40569(19) 0.46955(14) 0.23332(15) 0.0270(5) Uani 1 1 d . . . C22 C 0.3965(2) 0.45871(16) 0.07821(18) 0.0270(5) Uani 1 1 d . . . I1 I 0.75839(2) 0.201033(16) 0.73571(2) 0.05619(12) Uani 1 1 d . . . Zn1 Zn 0.60924(3) 0.285265(19) 0.67084(2) 0.02639(10) Uani 1 1 d . . . C29 C 0.2907(15) -0.0430(12) 0.8581(8) 0.124(7) Uani 0.50 1 d PDU A 1 C30 C 0.3189(5) -0.1180(5) 0.9001(6) 0.187(10) Uani 0.50 1 d PDU A 1 H30 H 0.3500 -0.1521 0.8772 0.224 Uiso 0.50 1 calc PR A 1 C31 C 0.2959(5) -0.1333(5) 0.9746(6) 0.183(10) Uani 0.50 1 d PRU A 1 H31 H 0.3148 -0.1773 1.0066 0.219 Uiso 0.50 1 d PR A 1 C32 C 0.2447(5) -0.0829(5) 1.0013(6) 0.122(7) Uani 0.50 1 d PRU A 1 H32 H 0.2293 -0.0931 1.0511 0.147 Uiso 0.50 1 d PR A 1 C33 C 0.2165(5) -0.0171(5) 0.9534(6) 0.105(6) Uani 0.50 1 d PRU A 1 H33 H 0.1823 0.0167 0.9712 0.126 Uiso 0.50 1 d PR A 1 C34 C 0.2395(5) -0.0018(5) 0.8789(6) 0.115(6) Uani 0.50 1 d PRDU A 1 H34 H 0.2196 0.0418 0.8461 0.139 Uiso 0.50 1 d PR A 1 N11 N 0.3208(10) -0.0307(8) 0.7853(8) 0.112(5) Uani 0.50 1 d PDU A 1 H11A H 0.3026 0.0090 0.7510 0.135 Uiso 0.50 1 calc PR A 1 H11B H 0.3574 -0.0629 0.7748 0.135 Uiso 0.50 1 calc PR A 1 C24 C 0.2643(11) 0.2624(5) 0.8418(8) 0.245(13) Uani 0.50 1 d PDU B 1 H24 H 0.3293 0.2429 0.8649 0.293 Uiso 0.50 1 calc PR B 1 C25 C 0.2432(11) 0.3107(5) 0.8981(8) 0.232(13) Uani 0.50 1 d PRU B 1 H25 H 0.2928 0.3237 0.9583 0.279 Uiso 0.50 1 d PR B 1 C26 C 0.1479(11) 0.3395(5) 0.8645(8) 0.240(15) Uani 0.50 1 d PRU B 1 H26 H 0.1338 0.3718 0.9022 0.288 Uiso 0.50 1 d PR B 1 C27 C 0.0738(11) 0.3201(5) 0.7746(8) 0.35(4) Uani 0.50 1 d PR B 1 H27 H 0.0101 0.3394 0.7521 0.420 Uiso 0.50 1 d PR B 1 C28 C 0.0950(11) 0.2718(5) 0.7183(8) 0.243(18) Uani 0.50 1 d PRDU B 1 H28 H 0.0454 0.2588 0.6582 0.292 Uiso 0.50 1 d PR B 1 C23 C 0.1902(11) 0.2430(5) 0.7519(8) 0.191(13) Uani 0.50 1 d PRDU B 1 N10 N 0.2133(8) 0.2000(6) 0.6953(6) 0.078(3) Uani 0.50 1 d PDU B 1 H10A H 0.2748 0.1848 0.7155 0.094 Uiso 0.50 1 calc PR B 1 H10B H 0.1669 0.1874 0.6382 0.094 Uiso 0.50 1 calc PR B 1 C39 C 0.2734(6) -0.1569(5) 0.9535(7) 0.100(5) Uani 0.50 1 d PU . 2 H39 H 0.2351 -0.1854 0.8985 0.120 Uiso 0.50 1 calc PR . 2 C38 C 0.2307(6) -0.1314(5) 1.0098(7) 0.097(5) Uani 0.50 1 d PRU . 2 H38 H 0.1646 -0.1422 0.9936 0.117 Uiso 0.50 1 d PR . 2 C37 C 0.2867(6) -0.0897(5) 1.0903(7) 0.139(7) Uani 0.50 1 d PRU . 2 H37 H 0.2581 -0.0727 1.1280 0.167 Uiso 0.50 1 d PR . 2 C36 C 0.3855(6) -0.0736(5) 1.1145(7) 0.153(8) Uani 0.50 1 d PRDU . 2 H36 H 0.4230 -0.0457 1.1684 0.184 Uiso 0.50 1 d PR . 2 C35 C 0.4282(6) -0.0991(5) 1.0582(7) 0.153(7) Uani 0.50 1 d PRDU . 2 C40 C 0.3722(6) -0.1408(5) 0.9777(7) 0.149(8) Uani 0.50 1 d PRDU . 2 H40 H 0.4008 -0.1578 0.9400 0.178 Uiso 0.50 1 d PR . 2 N12 N 0.5271(11) -0.0890(14) 1.0876(15) 0.176(9) Uani 0.50 1 d PDU . 2 C44 C 0.2747(16) 0.0938(10) 0.8340(10) 0.273(14) Uani 0.50 1 d PGDU . 2 C45 C 0.331(2) 0.0890(12) 0.9330(11) 0.336(19) Uani 0.50 1 d PGDU . 2 H45 H 0.3410 0.0435 0.9638 0.403 Uiso 0.50 1 calc PR . 2 C46 C 0.371(2) 0.1508(15) 0.9869(10) 0.35(2) Uani 0.50 1 d PGDU . 2 H46 H 0.4094 0.1475 1.0545 0.418 Uiso 0.50 1 calc PR . 2 C47 C 0.3560(19) 0.2173(13) 0.9417(14) 0.285(17) Uani 0.50 1 d PGDU . 2 H47 H 0.3837 0.2595 0.9785 0.342 Uiso 0.50 1 calc PR . 2 C48 C 0.300(2) 0.2221(10) 0.8427(14) 0.265(16) Uani 0.50 1 d PGDU . 2 H48 H 0.2897 0.2676 0.8119 0.318 Uiso 0.50 1 calc PR . 2 C49 C 0.2594(17) 0.1603(10) 0.7888(9) 0.216(12) Uani 0.50 1 d PGDU . 2 H49 H 0.2212 0.1636 0.7212 0.259 Uiso 0.50 1 calc PR . 2 N14 N 0.2405(17) 0.0314(9) 0.7838(10) 0.158(9) Uani 0.50 1 d PDU . 2 H14A H 0.2540 -0.0101 0.8141 0.190 Uiso 0.50 1 calc PR . 2 H14B H 0.2049 0.0327 0.7210 0.190 Uiso 0.50 1 calc PR . 2 C53 C 0.0324(13) 0.3157(11) 0.7045(12) 0.31(2) Uani 0.50 1 d PU . 2 H53 H 0.0388 0.2654 0.7171 0.377 Uiso 0.50 1 calc PR . 2 C52 C -0.0546(13) 0.3432(11) 0.6310(12) 0.284(17) Uani 0.50 1 d PRU . 2 H52 H -0.1066 0.3121 0.5941 0.341 Uiso 0.50 1 d PR . 2 C51 C -0.0639(13) 0.4171(11) 0.6125(12) 0.249(15) Uani 0.50 1 d PRDU . 2 H51 H -0.1221 0.4355 0.5633 0.299 Uiso 0.50 1 d PR . 2 C50 C 0.0138(13) 0.4634(11) 0.6676(12) 0.189(10) Uani 0.50 1 d PRDU . 2 C55 C 0.1008(13) 0.4359(11) 0.7412(12) 0.236(13) Uani 0.50 1 d PRDU . 2 H55 H 0.1528 0.4669 0.7780 0.284 Uiso 0.50 1 d PR . 2 C54 C 0.1101(13) 0.3620(11) 0.7596(12) 0.244(16) Uani 0.50 1 d PRU . 2 H54 H 0.1684 0.3436 0.8088 0.292 Uiso 0.50 1 d PR . 2 N15 N 0.0083(18) 0.5342(12) 0.6419(16) 0.244(14) Uani 0.50 1 d PDU . 2 C42 C 0.5660(4) 0.0303(3) 0.5841(5) 0.0773(18) Uani 1 1 d U C 2 H42 H 0.6118 0.0507 0.6437 0.093 Uiso 1 1 calc R C 2 C41 C 0.5686(5) 0.0538(3) 0.5012(5) 0.0795(19) Uani 1 1 d DU . 2 C43 C 0.4993(5) -0.0219(3) 0.5842(5) 0.087(2) Uani 1 1 d U . 2 H43 H 0.5003 -0.0357 0.6430 0.104 Uiso 1 1 calc R . 2 N13 N 0.6347(8) 0.1062(5) 0.4954(6) 0.071(2) Uani 0.50 1 d PDU D 2 H13A H 0.6795 0.1270 0.5479 0.085 Uiso 0.50 1 calc PR D 2 H13B H 0.6308 0.1177 0.4394 0.085 Uiso 0.50 1 calc PR D 2 O1 O 0.69482(19) 0.38941(14) 0.72715(16) 0.0357(5) Uani 1 1 d . . . C56 C 0.7648(4) 0.4205(3) 0.7021(4) 0.0684(16) Uani 1 1 d . . . H56B H 0.7894 0.4657 0.7375 0.103 Uiso 1 1 calc R . . H56C H 0.7330 0.4303 0.6331 0.103 Uiso 1 1 calc R . . H56A H 0.8205 0.3872 0.7184 0.103 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 N1 0.0311(12) 0.0381(13) 0.0124(9) -0.0010(8) 0.0096(8) 0.0010(10) C1 0.051(2) 0.058(2) 0.0202(13) 0.0077(13) 0.0182(14) 0.0234(17) C2 0.061(2) 0.064(2) 0.0199(13) 0.0091(14) 0.0233(14) 0.0283(19) C3 0.0331(13) 0.0348(14) 0.0138(10) 0.0006(9) 0.0109(10) -0.0007(11) C4 0.0535(19) 0.0466(18) 0.0215(13) 0.0102(12) 0.0221(13) 0.0176(16) C5 0.064(2) 0.0518(19) 0.0230(13) 0.0099(13) 0.0296(15) 0.0204(17) N2 0.0392(13) 0.0358(12) 0.0133(9) -0.0017(8) 0.0137(9) -0.0001(10) C7 0.057(2) 0.062(2) 0.0168(12) 0.0077(13) 0.0206(13) 0.0206(18) C8 0.059(2) 0.055(2) 0.0220(13) 0.0091(13) 0.0242(14) 0.0211(17) C9 0.0422(16) 0.0334(14) 0.0164(11) -0.0008(9) 0.0161(11) 0.0006(12) C10 0.0450(17) 0.0363(14) 0.0156(11) 0.0010(10) 0.0152(11) 0.0032(13) C11 0.0404(16) 0.0364(15) 0.0169(11) 0.0002(10) 0.0132(11) 0.0041(12) N3 0.0357(13) 0.0370(13) 0.0147(9) 0.0011(8) 0.0107(9) -0.0009(10) C13 0.0406(16) 0.0404(16) 0.0146(11) -0.0002(10) 0.0116(11) 0.0041(12) C14 0.0379(15) 0.0434(16) 0.0128(10) 0.0004(10) 0.0080(10) 0.0068(13) C15 0.0323(13) 0.0332(13) 0.0167(10) 0.0000(9) 0.0101(10) -0.0005(11) C16 0.053(2) 0.0474(18) 0.0153(11) -0.0000(11) 0.0127(12) 0.0132(16) C17 0.0490(19) 0.051(2) 0.0164(12) 0.0007(12) 0.0095(12) 0.0126(16) C6 0.0330(13) 0.0364(14) 0.0141(10) 0.0002(9) 0.0115(10) -0.0011(11) N4 0.0378(13) 0.0407(14) 0.0144(9) 0.0023(9) 0.0136(9) 0.0036(11) C19 0.0377(14) 0.0347(14) 0.0160(10) 0.0007(10) 0.0145(10) -0.0006(12) N5 0.0430(14) 0.0365(13) 0.0173(10) 0.0020(9) 0.0177(10) 0.0042(11) C12 0.0421(15) 0.0336(14) 0.0167(11) -0.0004(10) 0.0165(11) 0.0002(12) N6 0.0423(14) 0.0367(13) 0.0147(9) 0.0003(9) 0.0146(10) 0.0034(11) C20 0.0376(14) 0.0330(14) 0.0150(10) -0.0008(9) 0.0126(10) -0.0009(11) N7 0.0399(13) 0.0372(13) 0.0143(9) 0.0004(9) 0.0127(9) 0.0029(11) C18 0.0351(14) 0.0337(14) 0.0155(10) -0.0009(9) 0.0109(10) 0.0004(11) N8 0.0334(12) 0.0329(12) 0.0143(9) -0.0022(8) 0.0104(9) -0.0010(10) C21 0.0327(13) 0.0336(13) 0.0133(10) -0.0009(9) 0.0115(10) -0.0021(11) N9 0.0341(12) 0.0338(12) 0.0134(9) -0.0006(8) 0.0112(9) -0.0013(10) C22 0.0357(14) 0.0331(13) 0.0137(10) -0.0008(9) 0.0125(10) -0.0009(11) I1 0.04368(16) 0.05316(18) 0.04743(17) -0.01006(11) -0.00019(12) 0.02161(11) Zn1 0.03198(18) 0.03496(18) 0.01159(14) 0.00090(10) 0.00941(12) 0.00585(13) C29 0.154(15) 0.136(14) 0.037(5) 0.005(7) 0.005(7) -0.004(12) C30 0.28(2) 0.19(2) 0.121(15) 0.022(15) 0.117(16) 0.078(19) C31 0.27(2) 0.190(19) 0.103(12) 0.099(13) 0.096(14) 0.097(18) C32 0.099(11) 0.21(2) 0.073(9) -0.010(11) 0.056(8) -0.049(13) C33 0.052(6) 0.118(12) 0.124(12) -0.040(10) 0.022(7) 0.024(7) C34 0.043(6) 0.099(11) 0.142(14) 0.030(10) -0.011(7) -0.000(6) N11 0.118(11) 0.147(12) 0.058(6) 0.007(7) 0.027(7) 0.037(10) C24 0.32(3) 0.31(3) 0.20(2) -0.107(19) 0.20(2) -0.23(2) C25 0.33(3) 0.22(2) 0.28(2) -0.177(18) 0.26(2) -0.22(2) C26 0.35(4) 0.16(2) 0.33(3) -0.06(2) 0.26(3) -0.12(3) C27 0.91(12) 0.082(12) 0.14(2) 0.039(14) 0.32(5) 0.06(3) C28 0.35(4) 0.27(3) 0.106(15) 0.007(17) 0.10(2) -0.21(3) C23 0.24(2) 0.26(2) 0.087(12) -0.026(14) 0.090(15) -0.18(2) N10 0.083(6) 0.125(9) 0.046(4) -0.013(5) 0.046(5) -0.034(6) C39 0.068(8) 0.125(13) 0.105(11) -0.038(10) 0.040(8) -0.024(8) C38 0.058(7) 0.091(9) 0.131(13) -0.039(9) 0.033(7) -0.023(7) C37 0.119(13) 0.139(15) 0.186(18) -0.062(14) 0.093(13) -0.019(12) C36 0.147(16) 0.131(14) 0.171(17) -0.070(13) 0.064(15) -0.001(13) C35 0.119(13) 0.170(16) 0.190(17) -0.090(14) 0.087(13) -0.040(12) C40 0.081(10) 0.21(2) 0.144(15) -0.096(14) 0.040(10) -0.037(12) N12 0.142(14) 0.21(2) 0.21(2) -0.090(16) 0.113(14) -0.101(14) C44 0.28(3) 0.33(3) 0.22(2) -0.04(3) 0.12(2) -0.18(2) C45 0.32(3) 0.39(4) 0.22(3) 0.02(3) 0.06(3) -0.13(3) C46 0.33(3) 0.39(4) 0.21(3) -0.01(3) 0.02(3) -0.15(3) C47 0.29(3) 0.37(3) 0.128(19) -0.02(2) 0.04(2) -0.25(3) C48 0.29(3) 0.34(3) 0.129(19) -0.04(2) 0.07(2) -0.22(2) C49 0.32(3) 0.28(3) 0.067(9) -0.058(13) 0.102(14) -0.18(2) N14 0.29(3) 0.113(12) 0.066(7) -0.021(8) 0.081(12) -0.026(15) C53 0.27(3) 0.27(3) 0.31(3) 0.08(3) 0.05(3) 0.07(3) C52 0.21(3) 0.32(3) 0.28(3) 0.08(3) 0.08(2) 0.11(3) C51 0.20(2) 0.34(3) 0.21(3) 0.03(3) 0.09(2) 0.11(3) C50 0.21(2) 0.26(3) 0.154(19) 0.018(19) 0.124(17) 0.08(2) C55 0.26(3) 0.28(3) 0.20(2) -0.05(2) 0.13(2) 0.08(2) C54 0.25(3) 0.20(3) 0.25(3) -0.07(2) 0.09(2) 0.12(2) N15 0.29(3) 0.24(3) 0.152(19) -0.04(2) 0.06(2) 0.12(3) C42 0.054(3) 0.057(3) 0.086(4) -0.022(3) 0.002(3) 0.012(2) C41 0.060(3) 0.061(3) 0.083(4) -0.016(3) 0.003(3) 0.022(3) C43 0.067(3) 0.065(3) 0.095(4) -0.018(3) 0.009(3) 0.021(3) N13 0.083(6) 0.066(5) 0.049(4) -0.007(4) 0.017(4) 0.009(5) O1 0.0439(13) 0.0448(13) 0.0213(9) -0.0076(9) 0.0174(9) -0.0035(10) C56 0.075(3) 0.097(4) 0.052(2) -0.031(3) 0.044(2) -0.041(3) _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 N1 C5 1.323(4) . ? N1 C1 1.326(4) . ? N1 Zn1 2.068(2) . ? C1 C2 1.384(4) . ? C2 C3 1.381(5) . ? C3 C4 1.382(4) . ? C3 C6 1.499(4) . ? C4 C5 1.389(4) . ? N2 C7 1.338(5) . ? N2 C11 1.345(4) . ? N2 Zn1 2.063(2) 1_554 ? C7 C8 1.382(4) . ? C8 C9 1.389(4) . ? C9 C10 1.392(5) . ? C9 C12 1.489(4) . ? C10 C11 1.384(4) . ? N3 C17 1.339(4) . ? N3 C13 1.348(4) . ? N3 Zn1 2.189(3) 2 ? C13 C14 1.381(5) . ? C14 C15 1.384(4) . ? C15 C16 1.393(4) . ? C15 C18 1.490(4) . ? C16 C17 1.380(5) . ? C6 N9 1.330(4) . ? C6 N4 1.345(4) . ? N4 C19 1.356(3) . ? C19 N5 1.352(4) . ? C19 C22 1.401(4) . ? N5 C12 1.347(3) . ? C12 N6 1.341(4) . ? N6 C20 1.355(4) . ? C20 N7 1.347(4) . ? C20 C22 1.406(3) . ? N7 C18 1.343(3) . ? C18 N8 1.351(3) . ? N8 C21 1.353(4) . ? C21 N9 1.348(3) . ? C21 C22 1.401(4) . ? I1 Zn1 2.5428(4) . ? Zn1 N2 2.063(2) 1_556 ? Zn1 N3 2.189(3) 2_545 ? Zn1 O1 2.269(3) . ? C29 C34 1.23(2) . ? C29 N11 1.426(15) . ? C29 C30 1.52(2) . ? C30 C31 1.3920 . ? C31 C32 1.3957 . ? C32 C33 1.3942 . ? C33 C34 1.3921 . ? C24 C23 1.3884 . ? C24 C25 1.3938 . ? C25 C26 1.3941 . ? C26 C27 1.3884 . ? C27 C28 1.3939 . ? C28 C23 1.3941 . ? C23 N10 1.353(11) . ? C39 C38 1.3939 . ? C39 C40 1.3946 . ? C38 C37 1.3902 . ? C37 C36 1.3946 . ? C36 C35 1.3939 . ? C36 N15 1.85(3) 4_666 ? C35 N12 1.360(11) . ? C35 C40 1.3901 . ? C35 N15 1.78(2) 4_666 ? N12 N15 1.44(3) 4_666 ? C44 N14 1.363(12) . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C46 C52 2.01(2) 4_666 ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C53 C52 1.3903 . ? C53 C54 1.3927 . ? C52 C51 1.3960 . ? C52 C46 2.01(8) 4_565 ? C51 C50 1.3927 . ? C50 N15 1.367(14) . ? C50 C55 1.3903 . ? C55 C54 1.3960 . ? N15 N12 1.44(3) 4_565 ? N15 C35 1.78(2) 4_565 ? N15 C36 1.85(3) 4_565 ? C42 C41 1.389(11) . ? C42 C43 1.400(10) . ? C41 C43 1.393(8) 3_656 ? C41 N13 1.427(11) . ? C43 C41 1.393(8) 3_656 ? O1 C56 1.409(5) . ? 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 C5 N1 C1 117.8(3) . . ? C5 N1 Zn1 121.31(19) . . ? C1 N1 Zn1 120.7(2) . . ? N1 C1 C2 122.9(3) . . ? C3 C2 C1 119.3(3) . . ? C2 C3 C4 117.9(3) . . ? C2 C3 C6 121.6(3) . . ? C4 C3 C6 120.4(3) . . ? C3 C4 C5 118.7(3) . . ? N1 C5 C4 123.3(3) . . ? C7 N2 C11 117.5(3) . . ? C7 N2 Zn1 119.17(18) . 1_554 ? C11 N2 Zn1 123.2(2) . 1_554 ? N2 C7 C8 123.5(3) . . ? C7 C8 C9 118.9(3) . . ? C8 C9 C10 117.9(3) . . ? C8 C9 C12 119.6(3) . . ? C10 C9 C12 122.5(2) . . ? C11 C10 C9 119.5(3) . . ? N2 C11 C10 122.6(3) . . ? C17 N3 C13 116.2(3) . . ? C17 N3 Zn1 117.7(2) . 2 ? C13 N3 Zn1 125.9(2) . 2 ? N3 C13 C14 123.5(3) . . ? C13 C14 C15 119.7(3) . . ? C14 C15 C16 117.2(3) . . ? C14 C15 C18 122.6(2) . . ? C16 C15 C18 120.2(3) . . ? C17 C16 C15 119.4(3) . . ? N3 C17 C16 123.9(3) . . ? N9 C6 N4 130.0(2) . . ? N9 C6 C3 115.1(2) . . ? N4 C6 C3 114.8(3) . . ? C6 N4 C19 114.8(3) . . ? N5 C19 N4 119.9(3) . . ? N5 C19 C22 120.3(2) . . ? N4 C19 C22 119.8(3) . . ? C12 N5 C19 114.9(3) . . ? N6 C12 N5 129.5(3) . . ? N6 C12 C9 114.5(2) . . ? N5 C12 C9 116.0(3) . . ? C12 N6 C20 115.6(2) . . ? N7 C20 N6 120.1(2) . . ? N7 C20 C22 120.3(3) . . ? N6 C20 C22 119.6(3) . . ? C18 N7 C20 115.7(2) . . ? N7 C18 N8 128.5(3) . . ? N7 C18 C15 114.8(2) . . ? N8 C18 C15 116.7(2) . . ? C18 N8 C21 115.9(2) . . ? N9 C21 N8 120.2(2) . . ? N9 C21 C22 120.0(3) . . ? N8 C21 C22 119.8(2) . . ? C6 N9 C21 115.3(2) . . ? C21 C22 C19 120.1(2) . . ? C21 C22 C20 119.8(3) . . ? C19 C22 C20 120.1(2) . . ? N2 Zn1 N1 125.80(10) 1_556 . ? N2 Zn1 N3 89.13(10) 1_556 2_545 ? N1 Zn1 N3 90.90(10) . 2_545 ? N2 Zn1 O1 79.97(10) 1_556 . ? N1 Zn1 O1 81.00(9) . . ? N3 Zn1 O1 158.69(10) 2_545 . ? N2 Zn1 I1 116.16(7) 1_556 . ? N1 Zn1 I1 116.28(7) . . ? N3 Zn1 I1 104.04(7) 2_545 . ? O1 Zn1 I1 97.20(7) . . ? C34 C29 N11 125.4(17) . . ? C34 C29 C30 122.8(13) . . ? N11 C29 C30 111.4(15) . . ? C31 C30 C29 115.1(7) . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.1 . . ? C34 C33 C32 119.9 . . ? C29 C34 C33 121.5(8) . . ? C23 C24 C25 119.9 . . ? C24 C25 C26 120.3 . . ? C27 C26 C25 119.9 . . ? C26 C27 C28 119.9 . . ? C27 C28 C23 120.3 . . ? N10 C23 C24 119.3(6) . . ? N10 C23 C28 120.7(6) . . ? C24 C23 C28 119.9 . . ? C38 C39 C40 120.2 . . ? C37 C38 C39 119.9 . . ? C38 C37 C36 119.9 . . ? C35 C36 C37 120.2 . . ? C35 C36 N15 64.9(9) . 4_666 ? C37 C36 N15 169.1(8) . 4_666 ? N12 C35 C40 120.2(7) . . ? N12 C35 C36 119.6(7) . . ? C40 C35 C36 119.9 . . ? N12 C35 N15 52.3(12) . 4_666 ? C40 C35 N15 166.0(9) . 4_666 ? C36 C35 N15 70.1(10) . 4_666 ? C35 C40 C39 119.9 . . ? C35 N12 N15 79.3(13) . 4_666 ? N14 C44 C45 117.8(8) . . ? N14 C44 C49 122.1(8) . . ? C45 C44 C49 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 C52 126.3(13) . 4_666 ? C47 C46 C52 113.5(14) . 4_666 ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? C52 C53 C54 119.8 . . ? C53 C52 C51 120.0 . . ? C53 C52 C46 141(4) . 4_565 ? C51 C52 C46 76(2) . 4_565 ? C50 C51 C52 120.2 . . ? N15 C50 C55 120.3(8) . . ? N15 C50 C51 119.4(8) . . ? C55 C50 C51 119.8 . . ? C50 C55 C54 120.0 . . ? C53 C54 C55 120.2 . . ? C50 N15 N12 149(3) . 4_565 ? C50 N15 C35 142.7(13) . 4_565 ? N12 N15 C35 48.5(8) 4_565 4_565 ? C50 N15 C36 111.5(17) . 4_565 ? N12 N15 C36 91.8(12) 4_565 4_565 ? C35 N15 C36 45.0(5) 4_565 4_565 ? C41 C42 C43 123.2(6) . . ? C42 C41 C43 116.3(7) . 3_656 ? C42 C41 N13 126.4(6) . . ? C43 C41 N13 117.3(8) 3_656 . ? C41 C43 C42 120.5(8) 3_656 . ? C56 O1 Zn1 127.4(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.246 _refine_diff_density_min -2.852 _refine_diff_density_rms 0.151 _database_code_depnum_ccdc_archive 'CCDC 944053' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(Zn 2+), 2(C22 H12 N9 1-), 3(Zn1 I2), 6(C1 H3 O1 H), 5(C3 H7 N1 O1) ' _chemical_formula_sum 'C65 H83 I6 N23 O11 Zn4' _chemical_formula_weight 2385.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0036 0.0018 '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' I I -0.3619 1.9974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0071 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0123 0.0068 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2522 1.5759 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 23.1344(2) _cell_length_b 14.7104(1) _cell_length_c 26.8906(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.4115(3) _cell_angle_gamma 90.00 _cell_volume 8576.74(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 139862 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 29.63 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4640 _exptl_absorpt_coefficient_mu 3.663 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4062 _exptl_absorpt_correction_T_max 0.7836 _exptl_absorpt_process_details 'PLATON MULABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.75002 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'PLSII 2D bending magnet' _diffrn_radiation_monochromator 'Si(111) double crystal monochromator' _diffrn_measurement_device_type 'ADSC Q210 CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 139862 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 29.63 _reflns_number_total 19128 _reflns_number_gt 14665 _reflns_threshold_expression >2\s(I) _computing_data_collection 'PAL ADSC Quantum-210 ADX Program' _computing_cell_refinement HKL3000 _computing_data_reduction HKL3000 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 3' _computing_publication_material WinGX _refine_special_details ; Several restraints (SADI and FLAT) were applied to disordered aniline on a basis of chemical symmetry of the molecules. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1233P)^2^+18.7365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19128 _refine_ls_number_parameters 988 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1878 _refine_ls_wR_factor_gt 0.1760 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.055 _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 Zn1 Zn 0.10390(3) 0.05486(5) 0.36139(3) 0.03394(17) Uani 1 1 d . . . I1 I 0.033522(19) 0.13060(3) 0.405769(16) 0.04106(12) Uani 1 1 d . . . I2 I 0.10000(3) -0.11875(4) 0.35558(2) 0.05242(14) Uani 1 1 d . . . N1 N 0.1937(2) 0.0907(4) 0.40082(19) 0.0339(11) Uani 1 1 d . . . C1 C 0.2101(3) 0.1438(5) 0.4442(2) 0.0359(13) Uani 1 1 d . . . H1 H 0.1787 0.1682 0.4555 0.043 Uiso 1 1 calc R . . C2 C 0.2710(3) 0.1642(5) 0.4728(2) 0.0352(13) Uani 1 1 d . . . H2 H 0.2810 0.2010 0.5037 0.042 Uiso 1 1 calc R . . C3 C 0.3173(3) 0.1305(4) 0.4562(2) 0.0330(13) Uani 1 1 d . . . C4 C 0.3005(3) 0.0757(5) 0.4107(2) 0.0377(14) Uani 1 1 d . . . H4 H 0.3309 0.0519 0.3978 0.045 Uiso 1 1 calc R . . C5 C 0.2381(3) 0.0570(5) 0.3847(2) 0.0394(15) Uani 1 1 d . . . H5 H 0.2265 0.0187 0.3544 0.047 Uiso 1 1 calc R . . N2 N 0.5819(2) 0.3885(4) 0.7869(2) 0.0378(12) Uani 1 1 d . . . C7 C 0.6206(4) 0.3813(9) 0.7611(4) 0.081(4) Uani 1 1 d . . . H7 H 0.6601 0.4087 0.7761 0.097 Uiso 1 1 calc R . . C8 C 0.6067(4) 0.3358(8) 0.7134(4) 0.079(3) Uani 1 1 d . . . H8 H 0.6371 0.3291 0.6973 0.095 Uiso 1 1 calc R . . C9 C 0.5489(3) 0.3005(5) 0.6895(2) 0.0364(14) Uani 1 1 d . . . C10 C 0.5059(3) 0.3158(5) 0.7139(2) 0.0425(16) Uani 1 1 d . . . H10 H 0.4642 0.2972 0.6974 0.051 Uiso 1 1 calc R . . C11 C 0.5249(3) 0.3583(5) 0.7622(2) 0.0433(16) Uani 1 1 d . . . H11 H 0.4954 0.3667 0.7792 0.052 Uiso 1 1 calc R . . N3 N 0.7255(2) 0.0444(4) 0.44460(19) 0.0344(11) Uani 1 1 d . . . C13 C 0.6649(3) 0.0283(5) 0.4181(3) 0.0389(14) Uani 1 1 d . . . H13 H 0.6533 0.0027 0.3835 0.047 Uiso 1 1 calc R . . C14 C 0.6199(3) 0.0470(5) 0.4382(2) 0.0364(13) Uani 1 1 d . . . H14 H 0.5780 0.0343 0.4181 0.044 Uiso 1 1 calc R . . C15 C 0.6357(3) 0.0848(4) 0.4884(2) 0.0327(12) Uani 1 1 d . . . C16 C 0.6979(3) 0.1014(5) 0.5162(2) 0.0350(13) Uani 1 1 d . . . H16 H 0.7106 0.1277 0.5506 0.042 Uiso 1 1 calc R . . C17 C 0.7411(3) 0.0792(5) 0.4934(2) 0.0355(13) Uani 1 1 d . . . H17 H 0.7835 0.0891 0.5132 0.043 Uiso 1 1 calc R . . C6 C 0.3837(3) 0.1475(4) 0.4873(2) 0.0310(12) Uani 1 1 d . . . N4 N 0.3945(2) 0.1893(4) 0.53397(18) 0.0322(11) Uani 1 1 d . . . C19 C 0.4549(3) 0.2006(4) 0.5636(2) 0.0293(12) Uani 1 1 d . . . N5 N 0.4704(2) 0.2432(4) 0.61144(19) 0.0333(11) Uani 1 1 d . . . C12 C 0.5315(3) 0.2499(5) 0.6381(2) 0.0343(13) Uani 1 1 d . . . N6 N 0.5789(2) 0.2202(4) 0.62552(19) 0.0347(11) Uani 1 1 d . . . C20 C 0.5631(3) 0.1788(4) 0.5769(2) 0.0318(12) Uani 1 1 d . . . N7 N 0.6080(2) 0.1489(4) 0.55901(19) 0.0325(11) Uani 1 1 d . . . C18 C 0.5873(3) 0.1120(4) 0.5102(2) 0.0335(13) Uani 1 1 d . . . N8 N 0.5290(2) 0.0985(4) 0.47740(19) 0.0323(11) Uani 1 1 d . . . C21 C 0.4841(3) 0.1269(4) 0.4953(2) 0.0305(12) Uani 1 1 d . . . N9 N 0.4242(2) 0.1158(4) 0.46549(19) 0.0341(11) Uani 1 1 d . . . C22 C 0.5009(3) 0.1679(4) 0.5461(2) 0.0313(12) Uani 1 1 d . . . O6 O 0.8542(2) 0.1028(4) 0.45092(18) 0.0466(12) Uani 1 1 d D . . C56 C 0.9043(3) 0.0829(6) 0.4864(3) 0.0456(17) Uani 1 1 d D . . N22 N 0.9448(3) 0.1455(4) 0.5106(2) 0.0436(14) Uani 1 1 d D . . C58 C 0.9355(4) 0.2411(6) 0.4964(4) 0.066(2) Uani 1 1 d D . . H58A H 0.9709 0.2763 0.5191 0.099 Uiso 1 1 calc R . . H58B H 0.8978 0.2627 0.5014 0.099 Uiso 1 1 calc R . . H58C H 0.9316 0.2489 0.4592 0.099 Uiso 1 1 calc R . . C57 C 1.0035(4) 0.1229(7) 0.5513(3) 0.064(2) Uani 1 1 d . . . H57A H 1.0269 0.1787 0.5645 0.097 Uiso 1 1 calc R . . H57B H 1.0271 0.0831 0.5362 0.097 Uiso 1 1 calc R . . H57C H 0.9961 0.0916 0.5807 0.097 Uiso 1 1 calc R . . Zn2 Zn 0.78806(3) 0.01874(6) 0.40814(3) 0.0419(2) Uani 1 1 d . . . I3 I 0.82380(2) -0.14615(4) 0.42258(2) 0.05324(15) Uani 1 1 d . . . I4 I 0.74291(2) 0.08183(5) 0.313434(18) 0.06024(17) Uani 1 1 d . . . N10 N 0.3444(2) 0.4843(4) 0.58324(19) 0.0319(11) Uani 1 1 d . . . C23 C 0.3321(3) 0.4485(4) 0.5352(2) 0.0326(12) Uani 1 1 d . . . H23 H 0.2901 0.4418 0.5133 0.039 Uiso 1 1 calc R . . C24 C 0.3765(3) 0.4206(4) 0.5154(2) 0.0327(12) Uani 1 1 d . . . H24 H 0.3651 0.3950 0.4809 0.039 Uiso 1 1 calc R . . C25 C 0.4382(3) 0.4301(4) 0.5465(2) 0.0301(12) Uani 1 1 d . . . C26 C 0.4528(3) 0.4681(5) 0.5968(2) 0.0332(13) Uani 1 1 d . . . H26 H 0.4946 0.4757 0.6193 0.040 Uiso 1 1 calc R . . C27 C 0.4050(3) 0.4946(5) 0.6134(2) 0.0330(12) Uani 1 1 d . . . H27 H 0.4150 0.5212 0.6476 0.040 Uiso 1 1 calc R . . N11 N 0.5007(2) 0.1481(4) 0.24650(18) 0.0332(11) Uani 1 1 d . . . C29 C 0.5592(3) 0.1479(5) 0.2808(2) 0.0367(14) Uani 1 1 d . . . H29 H 0.5894 0.1148 0.2717 0.044 Uiso 1 1 calc R . . C30 C 0.5770(3) 0.1933(5) 0.3282(2) 0.0354(13) Uani 1 1 d . . . H30 H 0.6189 0.1919 0.3511 0.042 Uiso 1 1 calc R . . C31 C 0.5336(3) 0.2416(4) 0.3430(2) 0.0325(12) Uani 1 1 d . . . C32 C 0.4740(3) 0.2449(5) 0.3070(2) 0.0406(15) Uani 1 1 d . . . H32 H 0.4432 0.2787 0.3148 0.049 Uiso 1 1 calc R . . C33 C 0.4595(3) 0.1983(5) 0.2594(2) 0.0391(15) Uani 1 1 d . . . H33 H 0.4186 0.2021 0.2348 0.047 Uiso 1 1 calc R . . N12 N 0.8838(2) 0.4094(4) 0.64564(19) 0.0322(11) Uani 1 1 d . . . C35 C 0.8392(3) 0.4424(5) 0.6624(2) 0.0397(15) Uani 1 1 d . . . H35 H 0.8510 0.4762 0.6945 0.048 Uiso 1 1 calc R . . C36 C 0.7774(3) 0.4291(5) 0.6348(3) 0.0401(15) Uani 1 1 d . . . H36 H 0.7472 0.4532 0.6478 0.048 Uiso 1 1 calc R . . C37 C 0.7595(3) 0.3792(4) 0.5873(2) 0.0323(13) Uani 1 1 d . . . C38 C 0.8053(3) 0.3434(5) 0.5716(2) 0.0379(14) Uani 1 1 d . . . H38 H 0.7949 0.3075 0.5403 0.045 Uiso 1 1 calc R . . C39 C 0.8666(3) 0.3595(5) 0.6013(3) 0.0382(14) Uani 1 1 d . . . H39 H 0.8975 0.3342 0.5898 0.046 Uiso 1 1 calc R . . C28 C 0.4889(3) 0.4005(4) 0.5277(2) 0.0294(12) Uani 1 1 d . . . N13 N 0.4693(2) 0.3673(4) 0.47743(19) 0.0309(10) Uani 1 1 d . . . C41 C 0.5152(2) 0.3407(4) 0.4604(2) 0.0294(12) Uani 1 1 d . . . N14 N 0.5010(2) 0.3067(4) 0.41050(19) 0.0322(11) Uani 1 1 d . . . C34 C 0.5490(2) 0.2831(4) 0.3967(2) 0.0315(12) Uani 1 1 d . . . N15 N 0.6105(2) 0.2898(4) 0.42494(18) 0.0316(10) Uani 1 1 d . . . C42 C 0.6246(3) 0.3235(4) 0.4752(2) 0.0297(12) Uani 1 1 d . . . N16 N 0.6837(2) 0.3324(4) 0.50598(19) 0.0305(10) Uani 1 1 d . . . C40 C 0.6928(3) 0.3669(4) 0.5544(2) 0.0299(12) Uani 1 1 d . . . N17 N 0.6521(2) 0.3943(4) 0.57649(19) 0.0308(10) Uani 1 1 d . . . C43 C 0.5921(2) 0.3854(4) 0.5448(2) 0.0274(11) Uani 1 1 d . . . N18 N 0.5463(2) 0.4113(4) 0.56241(19) 0.0321(11) Uani 1 1 d . . . C44 C 0.5772(2) 0.3491(4) 0.4936(2) 0.0293(12) Uani 1 1 d . . . I5 I 0.53942(2) 0.09102(4) 0.124988(17) 0.04311(12) Uani 1 1 d . . . I6 I 0.48006(2) -0.10001(4) 0.22070(2) 0.05604(15) Uani 1 1 d . . . Zn3 Zn 0.27368(3) 0.52271(5) 0.61177(3) 0.03420(17) Uani 1 1 d . . . Zn4 Zn 0.47510(3) 0.06010(5) 0.18375(3) 0.03284(16) Uani 1 1 d . . . O1 O 0.20731(19) 0.5032(4) 0.53632(17) 0.0420(11) Uani 1 1 d D . . C45 C 0.1563(3) 0.4675(5) 0.5297(3) 0.0399(14) Uani 1 1 d D . . N19 N 0.1239(3) 0.4214(4) 0.4867(2) 0.0400(13) Uani 1 1 d D . . C46 C 0.1479(4) 0.4025(6) 0.4447(3) 0.0515(18) Uani 1 1 d D . . H46A H 0.1174 0.3678 0.4165 0.077 Uiso 1 1 calc R . . H46B H 0.1861 0.3671 0.4589 0.077 Uiso 1 1 calc R . . H46C H 0.1566 0.4599 0.4301 0.077 Uiso 1 1 calc R . . C47 C 0.0658(4) 0.3789(6) 0.4822(3) 0.058(2) Uani 1 1 d . . . H47A H 0.0488 0.3481 0.4478 0.087 Uiso 1 1 calc R . . H47B H 0.0367 0.4255 0.4849 0.087 Uiso 1 1 calc R . . H47C H 0.0725 0.3344 0.5108 0.087 Uiso 1 1 calc R . . O2 O 0.19904(19) 0.5622(3) 0.63457(17) 0.0378(10) Uani 1 1 d . . . C48 C 0.1970(3) 0.5836(5) 0.6786(3) 0.0439(16) Uani 1 1 d . . . N20 N 0.1562(3) 0.6399(5) 0.6852(3) 0.0508(16) Uani 1 1 d . . . C50 C 0.1081(4) 0.6796(7) 0.6416(4) 0.065(2) Uani 1 1 d . . . H50A H 0.0829 0.7195 0.6550 0.098 Uiso 1 1 calc R . . H50B H 0.0821 0.6313 0.6199 0.098 Uiso 1 1 calc R . . H50C H 0.1263 0.7151 0.6199 0.098 Uiso 1 1 calc R . . C49 C 0.1589(4) 0.6629(9) 0.7388(4) 0.079(3) Uani 1 1 d . . . H49A H 0.1257 0.7056 0.7369 0.119 Uiso 1 1 calc R . . H49B H 0.1988 0.6910 0.7583 0.119 Uiso 1 1 calc R . . H49C H 0.1540 0.6075 0.7572 0.119 Uiso 1 1 calc R . . O3 O 0.3352(2) 0.5349(4) 0.69196(19) 0.0515(13) Uani 1 1 d . . . C51 C 0.3455(3) 0.6053(6) 0.7185(3) 0.0458(17) Uani 1 1 d . . . N21 N 0.3790(3) 0.6078(5) 0.7694(2) 0.0436(14) Uani 1 1 d . . . C52 C 0.4057(4) 0.5294(6) 0.8014(3) 0.061(2) Uani 1 1 d . . . H52A H 0.4286 0.5488 0.8378 0.092 Uiso 1 1 calc R . . H52B H 0.4338 0.4986 0.7867 0.092 Uiso 1 1 calc R . . H52C H 0.3728 0.4874 0.8014 0.092 Uiso 1 1 calc R . . C53 C 0.3901(4) 0.6950(6) 0.7980(3) 0.060(2) Uani 1 1 d . . . H53A H 0.4158 0.6848 0.8352 0.090 Uiso 1 1 calc R . . H53B H 0.3506 0.7216 0.7963 0.090 Uiso 1 1 calc R . . H53C H 0.4113 0.7366 0.7817 0.090 Uiso 1 1 calc R . . O4 O 0.2638(2) 0.3854(4) 0.62902(19) 0.0444(11) Uani 1 1 d . . . C54 C 0.2442(4) 0.3572(5) 0.6713(3) 0.0466(16) Uani 1 1 d . . . H54A H 0.2427 0.2906 0.6722 0.070 Uiso 1 1 calc R . . H54B H 0.2030 0.3818 0.6658 0.070 Uiso 1 1 calc R . . H54C H 0.2733 0.3797 0.7051 0.070 Uiso 1 1 calc R . . O5 O 0.2888(2) 0.6608(4) 0.6028(2) 0.0473(12) Uani 1 1 d . . . C55 C 0.2393(4) 0.7185(6) 0.5778(3) 0.0538(19) Uani 1 1 d . . . H55A H 0.2546 0.7805 0.5770 0.081 Uiso 1 1 calc R . . H55B H 0.2106 0.7181 0.5973 0.081 Uiso 1 1 calc R . . H55C H 0.2179 0.6975 0.5414 0.081 Uiso 1 1 calc R . . O7 O 0.3583(3) 0.2758(4) 0.6328(2) 0.0579(14) Uani 1 1 d . . . C59 C 0.3521(4) 0.1852(7) 0.6389(4) 0.065(2) Uani 1 1 d . . . H59A H 0.3907 0.1609 0.6641 0.097 Uiso 1 1 calc R . . H59B H 0.3428 0.1548 0.6046 0.097 Uiso 1 1 calc R . . H59C H 0.3185 0.1745 0.6524 0.097 Uiso 1 1 calc R . . O8 O 0.3635(3) 0.3381(8) 0.3614(4) 0.124(4) Uani 1 1 d . . . C60 C 0.3672(5) 0.4285(9) 0.3354(5) 0.092(4) Uani 1 1 d . . . H60A H 0.3685 0.4781 0.3601 0.138 Uiso 1 1 calc R . . H60B H 0.3309 0.4357 0.3032 0.138 Uiso 1 1 calc R . . H60C H 0.4046 0.4300 0.3261 0.138 Uiso 1 1 calc R . . O9 O 0.2617(5) 0.3501(7) 0.3927(4) 0.117(3) Uani 1 1 d . . . C61 C 0.2142(6) 0.3163(8) 0.3448(5) 0.087(3) Uani 1 1 d . . . H61A H 0.1789 0.2945 0.3536 0.131 Uiso 1 1 calc R . . H61B H 0.2310 0.2661 0.3300 0.131 Uiso 1 1 calc R . . H61C H 0.2009 0.3654 0.3187 0.131 Uiso 1 1 calc R . . O10 O 0.7053(8) 0.145(2) 0.6878(8) 0.305(14) Uani 1 1 d . . . C62 C 0.7436(8) 0.1939(17) 0.6767(13) 0.242(18) Uani 1 1 d . . . H62A H 0.7328 0.2580 0.6778 0.362 Uiso 1 1 calc R . . H62B H 0.7429 0.1787 0.6410 0.362 Uiso 1 1 calc R . . H62C H 0.7849 0.1829 0.7025 0.362 Uiso 1 1 calc R . . O11 O 0.5738(8) -0.0345(15) 0.6514(6) 0.270(11) Uani 1 1 d DU . . C63 C 0.6250(11) -0.005(3) 0.6804(12) 0.52(2) Uani 1 1 d DU . . N23 N 0.6751(9) -0.048(4) 0.7080(10) 0.48(2) Uani 1 1 d DU . . C64 C 0.7412(6) -0.039(2) 0.7368(5) 0.202(12) Uani 1 1 d DU . . H64A H 0.7581 -0.0986 0.7512 0.303 Uiso 1 1 calc R . . H64B H 0.7483 0.0043 0.7660 0.303 Uiso 1 1 calc R . . H64C H 0.7616 -0.0176 0.7126 0.303 Uiso 1 1 calc R . . C65 C 0.6748(16) -0.152(3) 0.7065(15) 0.37(2) Uani 1 1 d DU . . H65A H 0.6692 -0.1756 0.7386 0.553 Uiso 1 1 calc R . . H65B H 0.7142 -0.1738 0.7050 0.553 Uiso 1 1 calc R . . H65C H 0.6410 -0.1731 0.6752 0.553 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 0.0319(3) 0.0375(4) 0.0256(3) 0.0030(3) 0.0013(3) 0.0005(3) I1 0.0361(2) 0.0488(3) 0.0331(2) -0.00210(17) 0.00566(16) 0.00415(17) I2 0.0638(3) 0.0379(3) 0.0559(3) -0.0027(2) 0.0213(2) -0.0018(2) N1 0.029(2) 0.039(3) 0.026(2) -0.000(2) 0.0004(18) 0.001(2) C1 0.033(3) 0.039(4) 0.034(3) -0.003(2) 0.009(2) -0.000(2) C2 0.032(3) 0.037(4) 0.034(3) -0.005(2) 0.008(2) -0.001(2) C3 0.034(3) 0.036(4) 0.023(2) 0.003(2) 0.003(2) 0.001(2) C4 0.032(3) 0.047(4) 0.029(3) -0.005(3) 0.005(2) 0.002(3) C5 0.035(3) 0.046(4) 0.029(3) -0.003(3) -0.001(2) 0.007(3) N2 0.032(3) 0.046(3) 0.029(2) -0.009(2) 0.002(2) -0.001(2) C7 0.041(4) 0.140(10) 0.059(5) -0.059(6) 0.016(4) -0.021(5) C8 0.047(5) 0.130(9) 0.061(5) -0.055(6) 0.020(4) -0.013(5) C9 0.035(3) 0.044(4) 0.026(3) -0.003(2) 0.006(2) 0.002(3) C10 0.035(3) 0.056(5) 0.031(3) -0.009(3) 0.004(2) 0.001(3) C11 0.035(3) 0.064(5) 0.029(3) -0.012(3) 0.008(2) -0.004(3) N3 0.033(3) 0.040(3) 0.029(2) -0.002(2) 0.0090(19) -0.001(2) C13 0.034(3) 0.041(4) 0.037(3) -0.007(3) 0.007(2) 0.003(3) C14 0.035(3) 0.034(4) 0.035(3) -0.003(2) 0.006(2) 0.001(2) C15 0.038(3) 0.025(3) 0.032(3) 0.002(2) 0.008(2) 0.001(2) C16 0.036(3) 0.039(4) 0.028(3) 0.002(2) 0.009(2) 0.002(2) C17 0.030(3) 0.043(4) 0.031(3) -0.002(2) 0.007(2) -0.000(2) C6 0.029(3) 0.034(3) 0.026(3) 0.002(2) 0.005(2) 0.000(2) N4 0.033(2) 0.033(3) 0.027(2) 0.0010(19) 0.0056(19) 0.004(2) C19 0.031(3) 0.026(3) 0.026(2) 0.001(2) 0.005(2) -0.001(2) N5 0.033(2) 0.035(3) 0.028(2) -0.001(2) 0.0050(19) 0.003(2) C12 0.031(3) 0.040(4) 0.026(3) 0.001(2) 0.001(2) 0.002(2) N6 0.033(3) 0.037(3) 0.028(2) -0.004(2) 0.0042(19) 0.001(2) C20 0.032(3) 0.031(3) 0.028(3) -0.001(2) 0.005(2) 0.003(2) N7 0.035(3) 0.031(3) 0.030(2) -0.0024(19) 0.010(2) 0.001(2) C18 0.036(3) 0.033(4) 0.029(3) 0.002(2) 0.008(2) 0.004(2) N8 0.032(2) 0.035(3) 0.028(2) -0.0023(19) 0.0073(19) 0.002(2) C21 0.031(3) 0.031(3) 0.027(3) 0.001(2) 0.007(2) 0.002(2) N9 0.032(2) 0.038(3) 0.028(2) 0.000(2) 0.0046(19) 0.002(2) C22 0.037(3) 0.030(3) 0.026(3) 0.001(2) 0.010(2) -0.001(2) O6 0.032(2) 0.065(3) 0.034(2) -0.003(2) -0.0004(18) -0.003(2) C56 0.029(3) 0.067(5) 0.036(3) -0.007(3) 0.006(2) -0.005(3) N22 0.031(3) 0.062(4) 0.034(3) 0.001(3) 0.006(2) -0.007(2) C58 0.046(4) 0.075(7) 0.064(5) -0.011(4) 0.005(4) -0.006(4) C57 0.035(4) 0.086(7) 0.055(5) 0.002(4) -0.006(3) -0.012(4) Zn2 0.0293(3) 0.0629(6) 0.0306(3) -0.0088(3) 0.0069(3) -0.0043(3) I3 0.0386(2) 0.0657(4) 0.0541(3) -0.0174(2) 0.0146(2) 0.0014(2) I4 0.0462(3) 0.1012(5) 0.0297(2) -0.0005(2) 0.00860(18) -0.0033(3) N10 0.025(2) 0.035(3) 0.035(2) -0.003(2) 0.0095(19) -0.0011(19) C23 0.025(3) 0.036(4) 0.034(3) -0.004(2) 0.006(2) 0.000(2) C24 0.030(3) 0.031(3) 0.032(3) 0.000(2) 0.006(2) 0.002(2) C25 0.027(3) 0.030(3) 0.031(3) 0.003(2) 0.007(2) 0.006(2) C26 0.026(3) 0.041(4) 0.031(3) 0.001(2) 0.007(2) 0.002(2) C27 0.024(3) 0.039(4) 0.033(3) -0.002(2) 0.006(2) 0.001(2) N11 0.029(2) 0.041(3) 0.024(2) -0.0003(19) 0.0028(18) 0.004(2) C29 0.027(3) 0.048(4) 0.032(3) -0.000(3) 0.006(2) 0.002(2) C30 0.026(3) 0.044(4) 0.029(3) -0.000(2) 0.001(2) 0.004(2) C31 0.029(3) 0.035(4) 0.030(3) 0.003(2) 0.005(2) 0.002(2) C32 0.032(3) 0.054(4) 0.030(3) -0.004(3) 0.004(2) 0.013(3) C33 0.027(3) 0.051(4) 0.031(3) -0.003(3) 0.002(2) 0.007(3) N12 0.020(2) 0.039(3) 0.032(2) -0.003(2) 0.0026(18) -0.0005(19) C35 0.024(3) 0.057(4) 0.035(3) -0.012(3) 0.006(2) -0.001(3) C36 0.025(3) 0.055(4) 0.036(3) -0.007(3) 0.005(2) -0.001(3) C37 0.025(3) 0.037(4) 0.030(3) 0.006(2) 0.004(2) 0.002(2) C38 0.029(3) 0.042(4) 0.037(3) -0.010(3) 0.004(2) 0.000(2) C39 0.028(3) 0.043(4) 0.038(3) -0.007(3) 0.004(2) -0.001(2) C28 0.027(3) 0.031(3) 0.028(3) 0.002(2) 0.007(2) 0.004(2) N13 0.024(2) 0.035(3) 0.029(2) -0.0018(19) 0.0041(18) 0.0010(19) C41 0.021(2) 0.033(3) 0.030(3) 0.001(2) 0.005(2) 0.003(2) N14 0.026(2) 0.038(3) 0.029(2) 0.003(2) 0.0052(18) 0.002(2) C34 0.023(2) 0.037(4) 0.029(3) 0.004(2) 0.002(2) 0.003(2) N15 0.027(2) 0.038(3) 0.025(2) 0.0006(19) 0.0027(18) 0.002(2) C42 0.028(3) 0.032(3) 0.026(2) 0.003(2) 0.005(2) 0.002(2) N16 0.024(2) 0.035(3) 0.030(2) 0.0029(19) 0.0057(18) -0.0007(19) C40 0.023(3) 0.036(3) 0.027(3) 0.001(2) 0.005(2) 0.003(2) N17 0.023(2) 0.036(3) 0.029(2) 0.0026(19) 0.0032(18) 0.0011(19) C43 0.021(2) 0.031(3) 0.029(3) 0.002(2) 0.007(2) 0.003(2) N18 0.025(2) 0.034(3) 0.032(2) 0.001(2) 0.0032(18) -0.0010(19) C44 0.022(2) 0.030(3) 0.031(3) 0.004(2) 0.003(2) -0.002(2) I5 0.0351(2) 0.0575(3) 0.0372(2) -0.00087(18) 0.01315(16) 0.00271(18) I6 0.0424(3) 0.0492(3) 0.0699(3) 0.0191(2) 0.0112(2) 0.0061(2) Zn3 0.0258(3) 0.0424(5) 0.0319(3) -0.0045(3) 0.0070(3) -0.0003(3) Zn4 0.0243(3) 0.0398(4) 0.0288(3) -0.0007(3) 0.0022(2) 0.0014(3) O1 0.0234(19) 0.066(3) 0.032(2) -0.005(2) 0.0028(16) -0.001(2) C45 0.037(3) 0.043(4) 0.035(3) -0.002(3) 0.007(2) 0.000(3) N19 0.036(3) 0.047(4) 0.031(2) -0.000(2) 0.004(2) -0.003(2) C46 0.052(4) 0.067(5) 0.033(3) -0.002(3) 0.013(3) 0.001(4) C47 0.056(5) 0.060(5) 0.055(4) -0.012(4) 0.015(4) -0.023(4) O2 0.031(2) 0.048(3) 0.038(2) 0.0018(19) 0.0164(17) 0.0065(19) C48 0.038(3) 0.050(5) 0.046(4) -0.005(3) 0.017(3) -0.003(3) N20 0.031(3) 0.065(5) 0.055(4) -0.021(3) 0.012(3) 0.000(3) C50 0.056(5) 0.071(6) 0.066(5) 0.006(4) 0.019(4) 0.012(4) C49 0.056(5) 0.116(9) 0.066(6) -0.030(6) 0.022(4) 0.003(5) O3 0.036(2) 0.071(4) 0.042(3) -0.015(2) 0.006(2) -0.001(2) C51 0.034(3) 0.068(5) 0.035(3) -0.006(3) 0.011(3) -0.003(3) N21 0.034(3) 0.062(4) 0.029(3) -0.001(2) 0.004(2) -0.003(3) C52 0.053(5) 0.055(5) 0.058(5) 0.005(4) -0.003(4) 0.001(4) C53 0.069(5) 0.058(6) 0.051(4) -0.004(4) 0.019(4) -0.010(4) O4 0.040(2) 0.053(3) 0.044(3) 0.006(2) 0.019(2) 0.004(2) C54 0.052(4) 0.046(5) 0.049(4) 0.003(3) 0.027(3) -0.001(3) O5 0.040(3) 0.051(3) 0.051(3) -0.005(2) 0.016(2) 0.002(2) C55 0.048(4) 0.057(5) 0.055(4) 0.014(4) 0.015(3) 0.011(3) O7 0.063(3) 0.056(4) 0.061(3) 0.002(3) 0.028(3) 0.013(3) C59 0.053(5) 0.077(7) 0.064(5) 0.006(4) 0.021(4) -0.008(4) O8 0.046(4) 0.167(10) 0.122(7) 0.001(7) -0.015(4) -0.003(5) C60 0.061(6) 0.105(10) 0.086(8) -0.031(7) -0.006(5) 0.018(6) O9 0.154(9) 0.107(7) 0.078(5) 0.016(5) 0.025(6) -0.008(6) C61 0.104(9) 0.077(8) 0.094(8) 0.014(6) 0.050(7) 0.007(6) O10 0.131(14) 0.50(4) 0.215(19) 0.12(2) -0.031(13) 0.007(19) C62 0.094(12) 0.20(2) 0.48(5) 0.17(3) 0.16(2) 0.078(14) O11 0.25(2) 0.35(2) 0.161(13) 0.074(15) 0.015(13) -0.168(18) C63 0.58(4) 0.61(4) 0.43(4) 0.06(4) 0.23(4) 0.02(4) N23 0.55(4) 0.64(4) 0.34(3) 0.06(4) 0.27(3) 0.00(4) C64 0.056(7) 0.49(4) 0.051(6) -0.039(13) 0.010(5) 0.044(14) C65 0.45(5) 0.37(5) 0.40(4) -0.05(4) 0.31(4) -0.09(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.046(5) . ? Zn1 N2 2.062(5) 4_565 ? Zn1 I2 2.5583(9) . ? Zn1 I1 2.5828(9) . ? N1 C5 1.340(9) . ? N1 C1 1.344(8) . ? C1 C2 1.382(8) . ? C2 C3 1.388(9) . ? C3 C4 1.404(8) . ? C3 C6 1.490(8) . ? C4 C5 1.395(9) . ? N2 C7 1.315(11) . ? N2 C11 1.329(8) . ? N2 Zn1 2.062(5) 4_666 ? C7 C8 1.382(11) . ? C8 C9 1.368(10) . ? C9 C10 1.388(9) . ? C9 C12 1.496(8) . ? C10 C11 1.369(9) . ? N3 C17 1.337(8) . ? N3 C13 1.354(8) . ? N3 Zn2 2.046(5) . ? C13 C14 1.359(9) . ? C14 C15 1.386(8) . ? C15 C16 1.392(9) . ? C15 C18 1.489(9) . ? C16 C17 1.381(9) . ? C6 N4 1.341(8) . ? C6 N9 1.350(8) . ? N4 C19 1.356(7) . ? C19 N5 1.361(7) . ? C19 C22 1.391(9) . ? N5 C12 1.347(7) . ? C12 N6 1.329(8) . ? N6 C20 1.372(7) . ? C20 N7 1.361(8) . ? C20 C22 1.397(8) . ? N7 C18 1.343(8) . ? C18 N8 1.345(8) . ? N8 C21 1.355(8) . ? C21 N9 1.347(7) . ? C21 C22 1.416(8) . ? O6 C56 1.253(7) . ? O6 Zn2 1.991(5) . ? C56 N22 1.313(9) . ? N22 C58 1.454(11) . ? N22 C57 1.455(9) . ? Zn2 I3 2.5484(11) . ? Zn2 I4 2.5657(9) . ? N10 C23 1.331(8) . ? N10 C27 1.361(7) . ? N10 Zn3 2.112(5) . ? C23 C24 1.374(9) . ? C24 C25 1.387(8) . ? C25 C26 1.392(8) . ? C25 C28 1.495(8) . ? C26 C27 1.385(8) . ? N11 C33 1.344(8) . ? N11 C29 1.345(7) . ? N11 Zn4 2.044(5) . ? C29 C30 1.370(9) . ? C30 C31 1.396(9) . ? C31 C32 1.382(8) . ? C31 C34 1.491(8) . ? C32 C33 1.385(9) . ? N12 C39 1.337(8) . ? N12 C35 1.352(8) . ? N12 Zn4 2.051(5) 4_666 ? C35 C36 1.375(8) . ? C36 C37 1.404(9) . ? C37 C38 1.377(9) . ? C37 C40 1.497(7) . ? C38 C39 1.383(8) . ? C28 N18 1.340(7) . ? C28 N13 1.358(7) . ? N13 C41 1.352(8) . ? C41 N14 1.361(7) . ? C41 C44 1.408(7) . ? N14 C34 1.335(8) . ? C34 N15 1.363(7) . ? N15 C42 1.367(7) . ? C42 N16 1.334(7) . ? C42 C44 1.403(8) . ? N16 C40 1.343(7) . ? C40 N17 1.339(8) . ? N17 C43 1.360(7) . ? C43 N18 1.357(8) . ? C43 C44 1.402(8) . ? I5 Zn4 2.5607(9) . ? I6 Zn4 2.5433(9) . ? Zn3 O5 2.090(6) . ? Zn3 O1 2.094(4) . ? Zn3 O4 2.102(5) . ? Zn3 O2 2.105(4) . ? Zn3 O3 2.137(5) . ? Zn4 N12 2.051(5) 4_565 ? O1 C45 1.246(8) . ? C45 N19 1.323(8) . ? N19 C47 1.450(10) . ? N19 C46 1.451(9) . ? O2 C48 1.242(8) . ? C48 N20 1.314(9) . ? N20 C50 1.429(10) . ? N20 C49 1.461(11) . ? O3 C51 1.231(9) . ? C51 N21 1.317(8) . ? N21 C52 1.444(10) . ? N21 C53 1.472(11) . ? O4 C54 1.426(8) . ? O5 C55 1.397(9) . ? O7 C59 1.356(11) . ? O8 C60 1.518(16) . ? O9 C61 1.458(14) . ? O10 C62 1.25(3) . ? O11 C63 1.248(18) . ? C63 N23 1.30(2) . ? N23 C64 1.460(18) . ? N23 C65 1.53(6) . ? 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 Zn1 N2 105.2(2) . 4_565 ? N1 Zn1 I2 107.25(16) . . ? N2 Zn1 I2 110.65(17) 4_565 . ? N1 Zn1 I1 109.86(16) . . ? N2 Zn1 I1 106.99(17) 4_565 . ? I2 Zn1 I1 116.38(3) . . ? C5 N1 C1 118.7(5) . . ? C5 N1 Zn1 119.4(4) . . ? C1 N1 Zn1 121.8(4) . . ? N1 C1 C2 122.2(6) . . ? C1 C2 C3 119.7(6) . . ? C2 C3 C4 118.4(6) . . ? C2 C3 C6 121.4(5) . . ? C4 C3 C6 120.1(6) . . ? C5 C4 C3 118.2(6) . . ? N1 C5 C4 122.8(6) . . ? C7 N2 C11 116.7(6) . . ? C7 N2 Zn1 124.2(5) . 4_666 ? C11 N2 Zn1 119.1(5) . 4_666 ? N2 C7 C8 123.2(8) . . ? C9 C8 C7 119.6(8) . . ? C8 C9 C10 117.4(6) . . ? C8 C9 C12 121.8(6) . . ? C10 C9 C12 120.8(6) . . ? C11 C10 C9 118.5(6) . . ? N2 C11 C10 124.1(7) . . ? C17 N3 C13 117.3(6) . . ? C17 N3 Zn2 123.3(4) . . ? C13 N3 Zn2 119.4(4) . . ? N3 C13 C14 123.4(6) . . ? C13 C14 C15 119.4(6) . . ? C14 C15 C16 117.8(6) . . ? C14 C15 C18 120.8(6) . . ? C16 C15 C18 121.3(5) . . ? C17 C16 C15 119.5(6) . . ? N3 C17 C16 122.5(6) . . ? N4 C6 N9 129.3(5) . . ? N4 C6 C3 114.9(5) . . ? N9 C6 C3 115.8(5) . . ? C6 N4 C19 115.1(5) . . ? N4 C19 N5 119.3(5) . . ? N4 C19 C22 120.7(5) . . ? N5 C19 C22 120.0(5) . . ? C12 N5 C19 114.7(5) . . ? N6 C12 N5 130.3(6) . . ? N6 C12 C9 114.8(5) . . ? N5 C12 C9 115.0(6) . . ? C12 N6 C20 114.8(5) . . ? N7 C20 N6 119.8(5) . . ? N7 C20 C22 120.6(5) . . ? N6 C20 C22 119.6(6) . . ? C18 N7 C20 114.8(5) . . ? N7 C18 N8 129.4(6) . . ? N7 C18 C15 115.7(5) . . ? N8 C18 C15 114.9(5) . . ? C18 N8 C21 116.1(5) . . ? N9 C21 N8 120.5(5) . . ? N9 C21 C22 120.3(6) . . ? N8 C21 C22 119.1(5) . . ? C21 N9 C6 115.2(5) . . ? C19 C22 C20 120.7(5) . . ? C19 C22 C21 119.3(5) . . ? C20 C22 C21 120.0(6) . . ? C56 O6 Zn2 128.0(5) . . ? O6 C56 N22 121.7(7) . . ? C56 N22 C58 122.3(6) . . ? C56 N22 C57 122.0(7) . . ? C58 N22 C57 115.6(6) . . ? O6 Zn2 N3 97.9(2) . . ? O6 Zn2 I3 111.11(15) . . ? N3 Zn2 I3 110.39(16) . . ? O6 Zn2 I4 108.27(15) . . ? N3 Zn2 I4 107.33(14) . . ? I3 Zn2 I4 119.59(3) . . ? C23 N10 C27 116.7(5) . . ? C23 N10 Zn3 121.9(4) . . ? C27 N10 Zn3 121.4(4) . . ? N10 C23 C24 124.0(5) . . ? C23 C24 C25 119.2(6) . . ? C24 C25 C26 118.5(6) . . ? C24 C25 C28 122.0(5) . . ? C26 C25 C28 119.6(5) . . ? C27 C26 C25 118.4(5) . . ? N10 C27 C26 123.3(5) . . ? C33 N11 C29 117.3(5) . . ? C33 N11 Zn4 122.3(4) . . ? C29 N11 Zn4 119.8(4) . . ? N11 C29 C30 122.8(6) . . ? C29 C30 C31 120.0(5) . . ? C32 C31 C30 117.4(5) . . ? C32 C31 C34 120.4(6) . . ? C30 C31 C34 122.1(5) . . ? C31 C32 C33 119.3(6) . . ? N11 C33 C32 123.1(5) . . ? C39 N12 C35 118.0(5) . . ? C39 N12 Zn4 120.0(4) . 4_666 ? C35 N12 Zn4 121.9(4) . 4_666 ? N12 C35 C36 122.7(6) . . ? C35 C36 C37 119.1(6) . . ? C38 C37 C36 117.7(5) . . ? C38 C37 C40 121.1(5) . . ? C36 C37 C40 121.2(6) . . ? C37 C38 C39 120.1(6) . . ? N12 C39 C38 122.3(6) . . ? N18 C28 N13 129.9(6) . . ? N18 C28 C25 115.7(5) . . ? N13 C28 C25 114.4(5) . . ? C41 N13 C28 114.4(5) . . ? N13 C41 N14 119.5(5) . . ? N13 C41 C44 120.5(5) . . ? N14 C41 C44 120.0(5) . . ? C34 N14 C41 115.6(5) . . ? N14 C34 N15 129.3(5) . . ? N14 C34 C31 115.8(5) . . ? N15 C34 C31 114.8(5) . . ? C34 N15 C42 114.9(5) . . ? N16 C42 N15 119.3(5) . . ? N16 C42 C44 120.8(5) . . ? N15 C42 C44 119.9(5) . . ? C42 N16 C40 114.8(5) . . ? N17 C40 N16 130.3(5) . . ? N17 C40 C37 116.0(5) . . ? N16 C40 C37 113.7(5) . . ? C40 N17 C43 114.5(5) . . ? N18 C43 N17 120.3(5) . . ? N18 C43 C44 119.8(5) . . ? N17 C43 C44 119.9(5) . . ? C28 N18 C43 115.3(5) . . ? C43 C44 C42 119.7(5) . . ? C43 C44 C41 120.1(5) . . ? C42 C44 C41 120.1(5) . . ? O5 Zn3 O1 96.8(2) . . ? O5 Zn3 O4 174.2(2) . . ? O1 Zn3 O4 89.0(2) . . ? O5 Zn3 O2 87.31(19) . . ? O1 Zn3 O2 85.48(18) . . ? O4 Zn3 O2 92.16(19) . . ? O5 Zn3 N10 92.0(2) . . ? O1 Zn3 N10 90.61(18) . . ? O4 Zn3 N10 88.9(2) . . ? O2 Zn3 N10 175.93(18) . . ? O5 Zn3 O3 87.4(2) . . ? O1 Zn3 O3 174.0(2) . . ? O4 Zn3 O3 86.8(2) . . ? O2 Zn3 O3 90.47(19) . . ? N10 Zn3 O3 93.52(19) . . ? N11 Zn4 N12 103.0(2) . 4_565 ? N11 Zn4 I6 107.68(15) . . ? N12 Zn4 I6 107.23(15) 4_565 . ? N11 Zn4 I5 109.46(16) . . ? N12 Zn4 I5 111.83(15) 4_565 . ? I6 Zn4 I5 116.67(3) . . ? C45 O1 Zn3 122.3(4) . . ? O1 C45 N19 124.1(6) . . ? C45 N19 C47 121.3(6) . . ? C45 N19 C46 121.7(6) . . ? C47 N19 C46 116.7(6) . . ? C48 O2 Zn3 131.0(4) . . ? O2 C48 N20 123.8(7) . . ? C48 N20 C50 122.4(7) . . ? C48 N20 C49 119.6(7) . . ? C50 N20 C49 118.0(7) . . ? C51 O3 Zn3 125.5(5) . . ? O3 C51 N21 123.4(8) . . ? C51 N21 C52 124.9(7) . . ? C51 N21 C53 120.0(7) . . ? C52 N21 C53 115.1(6) . . ? C54 O4 Zn3 123.0(5) . . ? C55 O5 Zn3 120.3(5) . . ? O11 C63 N23 130(3) . . ? C63 N23 C64 145(4) . . ? C63 N23 C65 118(3) . . ? C64 N23 C65 95(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 1.363 _refine_diff_density_min -2.622 _refine_diff_density_rms 0.222 _database_code_depnum_ccdc_archive 'CCDC 944054'