# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email xiaodr98@swu.edu.cn loop_ _publ_author_name 'Jianghong He' 'Guangju Zhang' 'Dongrong Xiao' 'Haiyan Chen' 'Shiwei Yan' 'Xin Wang' 'Juan Yang' 'Enbo Wang' data_compound-L-1 _database_code_depnum_ccdc_archive 'CCDC 851266' #TrackingRef '- Compounds-L1 and D1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H38 N6 O27.50 Zn4' _chemical_formula_weight 1292.23 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.749(2) _cell_length_b 14.749(2) _cell_length_c 22.313(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4854.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24802 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 2.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4197 _exptl_absorpt_correction_T_max 0.5034 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24802 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0899 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.52 _reflns_number_total 6008 _reflns_number_gt 4406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. During the refinement, a restrained refinement comment "isor" is used to restraint the Non-H atoms with the NPD and ADP problems, these atoms are as follows: O3,O4,O9,N2,C8,C15,C16,OW2,OW3,OW3A,OW4. The carbon atom (C15) is disordered in two positions with the 50% occupancies respectively. ; _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^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 6008 _refine_ls_number_parameters 374 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.1572 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.218 _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 0.25677(6) 0.15077(6) 0.09577(4) 0.0397(2) Uani 1 1 d . . . Zn2 Zn 0.32077(7) 0.21161(7) 0.28201(7) 0.0661(4) Uani 1 1 d . . . O1 O 0.1229(3) 0.1650(4) 0.1218(3) 0.0470(13) Uani 1 1 d . . . OW1 O 0.2611(5) 0.1089(4) 0.0102(3) 0.0597(16) Uani 1 1 d . . . O2 O 0.1736(4) 0.0247(4) 0.1262(3) 0.0547(15) Uani 1 1 d . . . OW2 O 0.3605(5) 0.2427(6) 0.3733(3) 0.081(2) Uani 1 1 d U . . O3 O -0.0392(5) -0.2286(5) 0.1831(4) 0.097(3) Uani 1 1 d U . . O4 O -0.1848(4) -0.1940(4) 0.1959(4) 0.0681(19) Uani 1 1 d U . . O5 O -0.2936(4) 0.1247(4) 0.1813(3) 0.0504(14) Uani 1 1 d . . . O6 O -0.1920(5) 0.2323(4) 0.1704(3) 0.0664(19) Uani 1 1 d . . . O7 O 0.4497(4) 0.3060(4) 0.2409(3) 0.0469(14) Uani 1 1 d . . . O8 O 0.3122(4) 0.3480(4) 0.2642(3) 0.067(2) Uani 1 1 d . . . O10 O 0.3068(4) 0.1603(4) 0.1931(3) 0.0585(17) Uani 1 1 d . . . O11 O 0.3786(5) 0.0818(5) 0.1243(3) 0.069(2) Uani 1 1 d . . . C17 C 0.5317(6) -0.1035(7) 0.3055(4) 0.065(3) Uani 1 1 d D . . H17A H 0.4802 -0.1293 0.3224 0.078 Uiso 1 1 calc R . . C16 C 0.6787(8) -0.0583(8) 0.2950(6) 0.092(4) Uani 1 1 d DU . . H16A H 0.7402 -0.0519 0.3031 0.110 Uiso 1 1 calc R . . N3 N 0.4119(5) 0.1031(5) 0.2822(3) 0.0474(17) Uani 1 1 d . . . H3B H 0.4603 0.1174 0.3049 0.057 Uiso 1 1 calc R . . H3C H 0.3850 0.0542 0.2985 0.057 Uiso 1 1 calc R . . C1 C -0.0532(5) 0.1100(5) 0.1536(3) 0.0367(15) Uani 1 1 d . . . H1A H -0.0430 0.1707 0.1444 0.044 Uiso 1 1 calc R . . C2 C 0.0194(5) 0.0471(5) 0.1513(4) 0.0426(18) Uani 1 1 d . . . C3 C 0.0015(5) -0.0436(5) 0.1605(4) 0.0433(19) Uani 1 1 d . . . H3A H 0.0481 -0.0857 0.1568 0.052 Uiso 1 1 calc R . . C4 C -0.0836(5) -0.0721(5) 0.1747(4) 0.0401(17) Uani 1 1 d . . . C5 C -0.1552(5) -0.0093(4) 0.1761(3) 0.0348(15) Uani 1 1 d . . . H5A H -0.2142 -0.0299 0.1816 0.042 Uiso 1 1 calc R . . C6 C -0.1396(5) 0.0811(5) 0.1695(3) 0.0327(15) Uani 1 1 d . . . C7 C 0.1090(6) 0.0817(7) 0.1304(4) 0.050(2) Uani 1 1 d . . . C8 C -0.1039(6) -0.1718(6) 0.1848(5) 0.057(2) Uani 1 1 d U . . C9 C -0.2097(5) 0.1506(5) 0.1760(3) 0.0380(16) Uani 1 1 d . . . C10 C 0.5111(5) 0.4889(5) 0.2500 0.032(2) Uani 1 2 d S . . H10 H 0.5557 0.4443 0.2500 0.032 Uiso 1 2 calc SR . . C11 C 0.4191(5) 0.4647(6) 0.2529(4) 0.0441(18) Uani 1 1 d . . . C12 C 0.3517(6) 0.5326(6) 0.2514(5) 0.064(3) Uani 1 1 d . . . H12 H 0.2906 0.5169 0.2514 0.064 Uiso 1 1 calc R . . C13 C 0.3774(7) 0.6226(7) 0.2500 0.089(6) Uani 1 2 d S . . C14 C 0.3924(6) 0.3665(6) 0.2504(4) 0.049(2) Uani 1 1 d . . . N2 N 0.6176(6) -0.1099(6) 0.3208(4) 0.070(2) Uani 1 1 d DU . . H2A H 0.6338 -0.1480 0.3479 0.084 Uiso 1 1 calc R . . N1 N 0.6261(5) -0.0168(6) 0.2526(4) 0.061(2) Uani 1 1 d . . . H1B H 0.6459 0.0229 0.2275 0.073 Uiso 1 1 calc R . . C18 C 0.5413(6) -0.0451(6) 0.2550(4) 0.051(2) Uani 1 1 d . . . C19 C 0.4660(6) -0.0167(6) 0.2142(4) 0.058(2) Uani 1 1 d . . . H19A H 0.4132 -0.0542 0.2217 0.069 Uiso 1 1 calc R . . H19B H 0.4843 -0.0259 0.1729 0.069 Uiso 1 1 calc R . . C20 C 0.4411(6) 0.0818(5) 0.2232(3) 0.0428(18) Uani 1 1 d . . . H20A H 0.4958 0.1176 0.2155 0.051 Uiso 1 1 calc R . . C21 C 0.3703(7) 0.1117(6) 0.1785(5) 0.061(3) Uani 1 1 d . . . OW3 O 0.1061(14) -0.2839(17) 0.1254(10) 0.038(5) Uani 0.25 1 d PU A 1 OW3A O 0.1061(15) -0.3328(17) 0.1167(9) 0.042(5) Uani 0.25 1 d PU B 2 OW4 O 0.1014(15) 0.7857(16) 0.2610(9) 0.049(5) Uani 0.25 1 d PU . . O9 O 0.2321(9) 0.6699(9) 0.2629(6) 0.157(5) Uani 1 1 d DU . . C15 C 0.3109(14) 0.6980(16) 0.2651(14) 0.122(12) Uani 0.50 1 d PDU . . 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 0.0360(5) 0.0272(4) 0.0560(5) 0.0052(4) -0.0111(4) -0.0027(3) Zn2 0.0317(5) 0.0488(6) 0.1177(9) -0.0227(6) -0.0021(6) 0.0019(4) O1 0.036(3) 0.046(4) 0.059(3) 0.000(3) 0.010(2) 0.001(2) OW1 0.074(4) 0.056(3) 0.049(3) 0.009(3) -0.005(3) -0.012(3) O2 0.039(3) 0.049(3) 0.076(4) 0.003(3) -0.007(3) 0.003(3) OW2 0.072(4) 0.090(5) 0.080(4) -0.038(4) 0.025(3) -0.025(4) O3 0.089(5) 0.065(5) 0.137(6) -0.003(4) 0.029(5) 0.028(4) O4 0.042(3) 0.043(3) 0.119(5) -0.018(3) 0.008(3) -0.012(3) O5 0.043(3) 0.039(3) 0.069(4) -0.008(3) -0.002(3) 0.005(2) O6 0.068(4) 0.036(3) 0.095(5) 0.021(3) 0.006(3) 0.018(3) O7 0.048(3) 0.039(3) 0.053(3) 0.008(2) -0.008(2) 0.005(2) O8 0.044(3) 0.044(3) 0.114(6) -0.010(4) 0.020(3) -0.017(3) O10 0.057(4) 0.043(3) 0.075(4) -0.011(3) -0.032(3) 0.006(3) O11 0.083(5) 0.046(4) 0.078(5) 0.012(3) -0.046(4) -0.004(3) C17 0.064(6) 0.062(6) 0.068(6) 0.017(5) -0.024(5) 0.001(5) C16 0.085(7) 0.096(7) 0.094(7) 0.018(6) -0.006(6) 0.017(6) N3 0.064(4) 0.052(4) 0.026(3) -0.008(3) -0.018(3) 0.013(3) C1 0.046(4) 0.031(3) 0.033(4) 0.000(3) 0.014(3) 0.001(3) C2 0.039(4) 0.031(4) 0.058(5) 0.005(4) -0.004(4) 0.002(3) C3 0.041(4) 0.036(4) 0.052(5) -0.018(4) -0.012(4) 0.015(3) C4 0.042(4) 0.028(4) 0.050(4) 0.004(3) 0.015(3) -0.004(3) C5 0.035(3) 0.031(4) 0.039(4) 0.005(3) 0.001(3) -0.009(3) C6 0.045(4) 0.029(3) 0.025(3) -0.008(2) -0.003(3) 0.013(3) C7 0.032(4) 0.063(6) 0.057(5) -0.029(4) 0.008(4) -0.010(4) C8 0.045(4) 0.037(4) 0.089(6) 0.007(4) 0.009(4) -0.014(3) C9 0.048(4) 0.031(3) 0.036(4) -0.008(3) -0.005(3) -0.010(3) C10 0.031(3) 0.031(3) 0.033(5) -0.002(3) -0.002(3) -0.009(4) C11 0.037(4) 0.055(5) 0.040(4) 0.017(4) 0.007(3) -0.002(3) C12 0.031(4) 0.041(5) 0.122(8) 0.020(5) 0.009(5) 0.004(3) C13 0.065(6) 0.065(6) 0.139(15) 0.053(8) 0.053(8) 0.018(7) C14 0.047(5) 0.051(5) 0.050(4) 0.010(4) -0.004(4) -0.017(4) N2 0.086(6) 0.072(5) 0.053(4) 0.011(4) -0.013(4) 0.035(4) N1 0.048(4) 0.074(5) 0.061(5) -0.005(4) 0.000(4) 0.005(4) C18 0.054(5) 0.053(5) 0.045(4) -0.014(4) -0.015(4) 0.001(4) C19 0.069(6) 0.057(5) 0.047(5) 0.016(4) 0.019(4) 0.011(4) C20 0.051(5) 0.048(4) 0.029(4) 0.000(3) -0.011(3) 0.006(3) C21 0.071(6) 0.026(4) 0.086(7) 0.006(4) -0.038(5) 0.004(4) OW3 0.034(6) 0.037(6) 0.044(6) -0.002(5) -0.002(5) 0.009(5) OW3A 0.046(8) 0.041(9) 0.039(8) -0.002(7) -0.015(7) -0.010(7) OW4 0.043(8) 0.060(9) 0.044(8) 0.002(7) -0.003(7) 0.013(7) O9 0.146(8) 0.141(8) 0.183(9) 0.004(7) 0.022(7) -0.016(7) C15 0.118(14) 0.124(14) 0.124(16) 0.004(9) -0.012(9) -0.010(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 O6 1.917(5) 6 ? Zn1 OW1 2.008(6) . ? Zn1 O1 2.070(5) . ? Zn1 O11 2.162(7) . ? Zn1 O10 2.297(6) . ? Zn1 O2 2.329(6) . ? Zn1 C7 2.526(8) . ? Zn1 C21 2.557(9) . ? Zn2 O4 1.974(6) 8 ? Zn2 O8 2.054(6) . ? Zn2 N3 2.090(7) . ? Zn2 O10 2.134(6) . ? Zn2 OW2 2.168(7) . ? O1 C7 1.260(11) . ? O2 C7 1.274(10) . ? O3 C8 1.269(11) . ? O4 C8 1.262(10) . ? O4 Zn2 1.974(6) 8 ? O5 C9 1.300(9) . ? O6 C9 1.240(9) . ? O6 Zn1 1.917(5) 6_455 ? O7 C14 1.248(10) . ? O8 C14 1.253(10) . ? O10 C21 1.225(11) . ? O11 C21 1.292(12) . ? C17 N2 1.315(8) . ? C17 C18 1.425(12) . ? C17 H17A 0.9300 . ? C16 N2 1.312(9) . ? C16 N1 1.367(14) . ? C16 H16A 0.9300 . ? N3 C20 1.419(9) . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? C1 C6 1.390(10) . ? C1 C2 1.417(10) . ? C1 H1A 0.9300 . ? C2 C3 1.378(10) . ? C2 C7 1.492(11) . ? C3 C4 1.362(11) . ? C3 H3A 0.9300 . ? C4 C5 1.405(10) . ? C4 C8 1.517(11) . ? C5 C6 1.362(9) . ? C5 H5A 0.9300 . ? C6 C9 1.462(10) . ? C10 C11 1.404(9) 8_665 ? C10 C11 1.404(9) . ? C10 H10 0.9300 . ? C11 C12 1.411(10) . ? C11 C14 1.502(12) . ? C12 C13 1.380(11) . ? C12 H12 0.9300 . ? C13 C12 1.380(11) 8_665 ? C13 C15 1.52(3) 8_665 ? C13 C15 1.52(3) . ? N2 H2A 0.8600 . ? N1 C18 1.320(11) . ? N1 H1B 0.8600 . ? C18 C19 1.497(12) . ? C19 C20 1.511(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.511(10) . ? C20 H20A 0.9800 . ? O9 C15 1.235(10) . ? O9 C15 1.240(10) 8_665 ? C15 C15 0.70(7) 8_665 ? C15 O9 1.240(10) 8_665 ? 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 O6 Zn1 OW1 94.9(3) 6 . ? O6 Zn1 O1 109.7(3) 6 . ? OW1 Zn1 O1 109.2(3) . . ? O6 Zn1 O11 98.7(3) 6 . ? OW1 Zn1 O11 96.3(3) . . ? O1 Zn1 O11 139.3(3) . . ? O6 Zn1 O10 89.7(3) 6 . ? OW1 Zn1 O10 155.2(2) . . ? O1 Zn1 O10 92.0(2) . . ? O11 Zn1 O10 58.9(2) . . ? O6 Zn1 O2 168.7(3) 6 . ? OW1 Zn1 O2 92.8(2) . . ? O1 Zn1 O2 59.8(2) . . ? O11 Zn1 O2 88.6(2) . . ? O10 Zn1 O2 86.7(2) . . ? O6 Zn1 C7 139.5(3) 6 . ? OW1 Zn1 C7 101.2(3) . . ? O1 Zn1 C7 29.8(3) . . ? O11 Zn1 C7 115.9(3) . . ? O10 Zn1 C7 90.7(3) . . ? O2 Zn1 C7 30.1(2) . . ? O6 Zn1 C21 94.6(3) 6 . ? OW1 Zn1 C21 126.6(3) . . ? O1 Zn1 C21 116.4(3) . . ? O11 Zn1 C21 30.3(3) . . ? O10 Zn1 C21 28.6(3) . . ? O2 Zn1 C21 87.4(3) . . ? C7 Zn1 C21 104.7(3) . . ? O4 Zn2 O8 100.7(3) 8 . ? O4 Zn2 N3 117.1(3) 8 . ? O8 Zn2 N3 142.2(3) . . ? O4 Zn2 O10 94.0(3) 8 . ? O8 Zn2 O10 99.3(3) . . ? N3 Zn2 O10 78.0(2) . . ? O4 Zn2 OW2 93.7(3) 8 . ? O8 Zn2 OW2 89.5(3) . . ? N3 Zn2 OW2 89.2(3) . . ? O10 Zn2 OW2 167.1(3) . . ? C7 O1 Zn1 95.6(5) . . ? C7 O2 Zn1 83.6(5) . . ? C8 O4 Zn2 118.9(6) . 8 ? C9 O6 Zn1 144.2(6) . 6_455 ? C14 O8 Zn2 101.7(6) . . ? C21 O10 Zn2 112.4(6) . . ? C21 O10 Zn1 87.6(6) . . ? Zn2 O10 Zn1 158.7(3) . . ? C21 O11 Zn1 92.1(6) . . ? N2 C17 C18 98.8(9) . . ? N2 C17 H17A 130.6 . . ? C18 C17 H17A 130.6 . . ? N2 C16 N1 100.1(9) . . ? N2 C16 H16A 130.0 . . ? N1 C16 H16A 130.0 . . ? C20 N3 Zn2 111.3(4) . . ? C20 N3 H3B 109.4 . . ? Zn2 N3 H3B 109.4 . . ? C20 N3 H3C 109.4 . . ? Zn2 N3 H3C 109.4 . . ? H3B N3 H3C 108.0 . . ? C6 C1 C2 120.1(6) . . ? C6 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C3 C2 C1 119.0(7) . . ? C3 C2 C7 123.2(7) . . ? C1 C2 C7 117.1(7) . . ? C4 C3 C2 120.7(7) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 119.6(7) . . ? C3 C4 C8 121.1(7) . . ? C5 C4 C8 119.2(7) . . ? C6 C5 C4 121.1(7) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C1 C6 C5 118.8(6) . . ? C1 C6 C9 117.3(6) . . ? C5 C6 C9 123.8(7) . . ? O2 C7 O1 120.8(8) . . ? O2 C7 C2 117.3(8) . . ? O1 C7 C2 121.6(7) . . ? O2 C7 Zn1 66.3(5) . . ? O1 C7 Zn1 54.6(4) . . ? C2 C7 Zn1 176.2(6) . . ? O3 C8 O4 123.1(8) . . ? O3 C8 C4 119.1(7) . . ? O4 C8 C4 117.8(8) . . ? O6 C9 O5 119.7(7) . . ? O6 C9 C6 121.5(7) . . ? O5 C9 C6 118.4(6) . . ? C11 C10 C11 119.6(10) 8_665 . ? C11 C10 H10 120.2 8_665 . ? C11 C10 H10 120.2 . . ? C10 C11 C12 119.9(8) . . ? C10 C11 C14 119.8(7) . . ? C12 C11 C14 119.9(8) . . ? C13 C12 C11 119.3(9) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C12 121.9(13) . 8_665 ? C12 C13 C15 115.1(8) . 8_665 ? C12 C13 C15 121.3(8) 8_665 8_665 ? C12 C13 C15 121.3(8) . . ? C12 C13 C15 115.1(8) 8_665 . ? C15 C13 C15 27(2) 8_665 . ? O8 C14 O7 121.7(8) . . ? O8 C14 C11 116.7(8) . . ? O7 C14 C11 121.3(7) . . ? C16 N2 C17 120.3(9) . . ? C16 N2 H2A 119.8 . . ? C17 N2 H2A 119.8 . . ? C18 N1 C16 111.5(9) . . ? C18 N1 H1B 124.2 . . ? C16 N1 H1B 124.2 . . ? N1 C18 C17 108.5(8) . . ? N1 C18 C19 126.2(9) . . ? C17 C18 C19 125.2(8) . . ? C18 C19 C20 111.6(8) . . ? C18 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? C18 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? N3 C20 C21 109.8(7) . . ? N3 C20 C19 114.2(7) . . ? C21 C20 C19 111.1(7) . . ? N3 C20 H20A 107.1 . . ? C21 C20 H20A 107.1 . . ? C19 C20 H20A 107.1 . . ? O10 C21 O11 121.5(8) . . ? O10 C21 C20 121.6(9) . . ? O11 C21 C20 116.9(8) . . ? O10 C21 Zn1 63.8(4) . . ? O11 C21 Zn1 57.6(4) . . ? C20 C21 Zn1 174.4(7) . . ? C15 O9 C15 33(3) . 8_665 ? C15 C15 O9 74(2) 8_665 . ? C15 C15 O9 73.2(19) 8_665 8_665 ? O9 C15 O9 118(2) . 8_665 ? C15 C15 C13 76.7(12) 8_665 . ? O9 C15 C13 110.7(19) . . ? O9 C15 C13 110.4(19) 8_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O11 0.90 2.37 3.253(10) 166.7 4 N3 H3C O3 0.90 2.35 2.966(11) 125.2 8 N2 H2A O5 0.86 2.05 2.849(10) 153.3 4_545 N1 H1B O5 0.86 2.03 2.879(10) 169.4 1_655 _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.580 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.097 #===END data_compound-D-1 _database_code_depnum_ccdc_archive 'CCDC 851267' #TrackingRef '- Compounds-L1 and D1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H38 N6 O27.50 Zn4' _chemical_formula_weight 1292.23 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.672(2) _cell_length_b 14.672(2) _cell_length_c 22.225(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4784.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30639 _cell_measurement_theta_min 1.66 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 2.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4345 _exptl_absorpt_correction_T_max 0.5209 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30639 _diffrn_reflns_av_R_equivalents 0.0816 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5824 _reflns_number_gt 4043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0128(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_number_reflns 5824 _refine_ls_number_parameters 369 _refine_ls_number_restraints 76 _refine_ls_R_factor_all 0.1264 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1876 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.275 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.15081(6) 0.25674(6) 0.09584(4) 0.0412(3) Uani 1 1 d . . . Zn2 Zn 0.21139(8) 0.32072(7) 0.28173(7) 0.0666(4) Uani 1 1 d . . . O1 O 0.1640(4) 0.1221(4) 0.1203(3) 0.0569(16) Uani 1 1 d . . . O2 O 0.0251(4) 0.1724(4) 0.1259(3) 0.0526(15) Uani 1 1 d . . . O3 O -0.2285(5) -0.0381(5) 0.1828(4) 0.083(2) Uani 1 1 d U . . O4 O -0.1935(5) -0.1848(5) 0.1982(4) 0.077(2) Uani 1 1 d U . . O5 O 0.1245(4) -0.2931(4) 0.1818(3) 0.0520(15) Uani 1 1 d . . . O6 O 0.2307(4) -0.1915(5) 0.1722(4) 0.0661(19) Uani 1 1 d . . . O7 O 0.3047(4) 0.4509(4) 0.2397(3) 0.0537(16) Uani 1 1 d . . . O8 O 0.3464(5) 0.3125(5) 0.2634(4) 0.075(2) Uani 1 1 d . . . O10 O 0.1603(4) 0.3069(5) 0.1928(3) 0.0649(19) Uani 1 1 d . . . O11 O 0.0823(5) 0.3797(6) 0.1231(3) 0.071(2) Uani 1 1 d . . . N3 N 0.1037(5) 0.4111(6) 0.2822(3) 0.0546(19) Uani 1 1 d . . . H3B H 0.0545 0.3838 0.2983 0.066 Uiso 1 1 calc R . . H3C H 0.1180 0.4593 0.3054 0.066 Uiso 1 1 calc R . . C1 C 0.1092(5) -0.0513(5) 0.1540(4) 0.0421(18) Uani 1 1 d . . . H1A H 0.1704 -0.0405 0.1457 0.051 Uiso 1 1 calc R . . C2 C 0.0469(6) 0.0199(5) 0.1494(4) 0.0432(19) Uani 1 1 d . . . C3 C -0.0429(6) 0.0025(6) 0.1595(4) 0.044(2) Uani 1 1 d . . . H3A H -0.0848 0.0498 0.1560 0.053 Uiso 1 1 calc R . . C4 C -0.0733(5) -0.0826(6) 0.1748(4) 0.0428(18) Uani 1 1 d . . . C5 C -0.0094(5) -0.1565(6) 0.1770(4) 0.047(2) Uani 1 1 d . . . H5A H -0.0300 -0.2158 0.1825 0.056 Uiso 1 1 calc R . . C6 C 0.0813(4) -0.1398(5) 0.1710(3) 0.0321(15) Uani 1 1 d . . . C7 C 0.0801(7) 0.1102(6) 0.1312(4) 0.049(2) Uani 1 1 d . . . C8 C -0.1729(6) -0.1034(6) 0.1847(5) 0.059(3) Uani 1 1 d . . . C9 C 0.1506(6) -0.2104(6) 0.1767(4) 0.0424(18) Uani 1 1 d . . . C10 C 0.4877(6) 0.5123(6) 0.2500 0.039(2) Uani 1 2 d S . . H10A H 0.4429 0.5571 0.2500 0.047 Uiso 1 2 calc SR . . C11 C 0.4636(6) 0.4205(5) 0.2518(4) 0.0446(19) Uani 1 1 d . . . C12 C 0.5325(7) 0.3543(7) 0.2507(5) 0.060(2) Uani 1 1 d U . . H12A H 0.5168 0.2928 0.2503 0.072 Uiso 1 1 calc R . . C13 C 0.6214(7) 0.3786(7) 0.2500 0.063(4) Uani 1 2 d S . . C14 C 0.3667(6) 0.3912(7) 0.2509(5) 0.053(2) Uani 1 1 d . . . C18 C -0.0478(6) 0.5410(6) 0.2558(3) 0.049(2) Uani 1 1 d D . . C19 C -0.0172(6) 0.4681(7) 0.2148(4) 0.053(2) Uani 1 1 d . . . H19A H -0.0260 0.4881 0.1736 0.064 Uiso 1 1 calc R . . H19B H -0.0550 0.4147 0.2211 0.064 Uiso 1 1 calc R . . C20 C 0.0825(6) 0.4416(6) 0.2235(4) 0.050(2) Uani 1 1 d . . . H20A H 0.1192 0.4962 0.2160 0.060 Uiso 1 1 calc R . . C21 C 0.1085(6) 0.3720(7) 0.1766(5) 0.058(2) Uani 1 1 d . . . N2 N -0.1140(7) 0.6197(7) 0.3245(5) 0.087(3) Uani 1 1 d DU . . H2A H -0.1520 0.6363 0.3518 0.105 Uiso 1 1 calc R . . N1 N -0.0164(7) 0.6256(5) 0.2530(4) 0.073(3) Uani 1 1 d D . . H1B H 0.0241 0.6453 0.2282 0.087 Uiso 1 1 calc R . . C17 C -0.1029(8) 0.5338(7) 0.3055(4) 0.071(3) Uani 1 1 d DU . . H17A H -0.1272 0.4811 0.3222 0.086 Uiso 1 1 calc R . . C16 C -0.0585(8) 0.6757(7) 0.2955(5) 0.077(3) Uani 1 1 d DU . . H16A H -0.0502 0.7375 0.3030 0.092 Uiso 1 1 calc R . . O9 O 0.6707(10) 0.2303(9) 0.2647(7) 0.165(5) Uani 1 1 d DU . . C15 C 0.6966(16) 0.3097(13) 0.259(2) 0.107(11) Uani 0.50 1 d PDU . . OW1 O 0.1093(5) 0.2634(5) 0.0120(3) 0.0628(18) Uani 1 1 d . . . HW1A H 0.0625 0.2289 0.0111 0.075 Uiso 1 1 d R . . HW1B H 0.1438 0.2511 -0.0177 0.075 Uiso 1 1 d R . . OW2 O 0.2396(7) 0.3603(6) 0.3721(4) 0.087(2) Uani 1 1 d U . . HW2A H 0.2849 0.3248 0.3757 0.105 Uiso 1 1 d R . . HW2B H 0.2252 0.3806 0.4068 0.105 Uiso 1 1 d R . . OW3 O -0.3120(17) 0.1093(16) 0.1218(10) 0.109(6) Uani 0.50 1 d PDU . . HW3A H -0.280(14) 0.10(2) 0.153(6) 0.115 Uiso 0.50 1 d PD . . HW3B H -0.281(14) 0.094(19) 0.091(6) 0.112 Uiso 0.50 1 d PD . . OW4 O 0.7814(19) 0.1057(19) 0.2627(11) 0.060(6) Uani 0.25 1 d PU . . HW4A H 0.7314 0.1266 0.2491 0.072 Uiso 0.25 1 d PR . . HW4B H 0.8202 0.1486 0.2638 0.072 Uiso 0.25 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0309(5) 0.0382(5) 0.0544(5) -0.0116(4) 0.0060(4) -0.0031(4) Zn2 0.0503(6) 0.0360(6) 0.1136(10) 0.0016(6) -0.0210(7) 0.0006(4) O1 0.042(4) 0.048(3) 0.081(4) 0.010(3) 0.000(3) 0.005(3) O2 0.050(3) 0.039(3) 0.069(4) 0.006(3) -0.003(3) 0.003(3) O3 0.062(4) 0.081(5) 0.107(5) 0.029(4) 0.000(4) 0.025(4) O4 0.045(4) 0.064(4) 0.122(6) 0.013(4) -0.012(4) -0.007(3) O5 0.040(3) 0.043(3) 0.073(4) 0.002(3) -0.005(3) 0.005(2) O6 0.027(3) 0.061(4) 0.110(6) 0.011(4) 0.013(3) 0.011(3) O7 0.051(4) 0.058(4) 0.052(4) -0.011(3) 0.005(3) 0.010(3) O8 0.057(4) 0.050(4) 0.118(6) 0.028(4) -0.018(4) -0.017(3) O10 0.043(3) 0.064(4) 0.088(5) -0.034(4) -0.001(3) 0.001(3) O11 0.062(5) 0.088(6) 0.062(4) -0.027(4) 0.009(4) -0.006(4) N3 0.061(5) 0.056(5) 0.047(4) -0.002(4) 0.007(4) 0.017(4) C1 0.024(3) 0.047(4) 0.055(5) 0.010(4) 0.002(3) 0.001(3) C2 0.039(4) 0.040(4) 0.050(5) -0.015(4) -0.006(4) 0.003(3) C3 0.045(4) 0.049(5) 0.039(4) -0.011(4) -0.020(4) 0.013(4) C4 0.035(4) 0.042(4) 0.052(5) 0.002(4) 0.002(3) 0.004(3) C5 0.034(4) 0.035(4) 0.071(6) 0.008(4) -0.013(4) -0.006(3) C6 0.023(3) 0.048(4) 0.025(3) 0.008(3) 0.001(2) 0.010(3) C7 0.055(6) 0.037(5) 0.054(5) -0.003(4) -0.011(4) -0.008(4) C8 0.036(4) 0.033(4) 0.107(8) 0.000(5) 0.008(5) -0.005(4) C9 0.045(4) 0.045(5) 0.037(4) 0.000(3) -0.003(3) 0.000(4) C10 0.040(4) 0.040(4) 0.037(6) -0.002(3) -0.002(3) -0.003(5) C11 0.058(5) 0.034(4) 0.041(4) 0.020(3) 0.014(4) 0.006(4) C12 0.053(5) 0.040(4) 0.088(6) 0.007(4) 0.010(4) -0.001(4) C13 0.053(5) 0.053(5) 0.083(10) 0.018(5) 0.018(5) -0.001(6) C14 0.042(5) 0.052(5) 0.067(6) 0.017(5) 0.006(4) -0.007(4) C18 0.039(4) 0.069(6) 0.041(4) -0.002(4) -0.008(4) 0.006(4) C19 0.041(5) 0.070(6) 0.048(5) 0.004(5) -0.001(4) 0.014(4) C20 0.052(5) 0.046(5) 0.052(5) -0.019(4) -0.006(4) 0.013(4) C21 0.039(5) 0.058(6) 0.076(7) -0.020(5) 0.005(4) 0.001(4) N2 0.083(6) 0.101(7) 0.078(5) -0.005(5) 0.009(5) 0.014(5) N1 0.091(7) 0.044(5) 0.083(6) -0.003(4) -0.003(5) 0.007(5) C17 0.067(6) 0.079(6) 0.067(6) -0.010(5) 0.009(5) 0.002(5) C16 0.083(6) 0.077(6) 0.071(6) 0.002(5) 0.023(5) 0.008(5) O9 0.156(9) 0.153(9) 0.185(9) 0.001(8) 0.000(8) -0.017(8) C15 0.105(13) 0.102(13) 0.114(15) -0.008(9) 0.004(9) 0.005(9) OW1 0.052(4) 0.081(5) 0.055(4) 0.000(3) 0.010(3) -0.020(4) OW2 0.095(5) 0.082(5) 0.085(4) 0.018(4) -0.024(4) -0.019(4) OW3 0.134(10) 0.090(9) 0.103(9) -0.011(8) 0.005(8) 0.000(8) OW4 0.065(10) 0.062(10) 0.053(9) 0.004(8) -0.002(8) 0.008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O6 1.939(6) 5 ? Zn1 OW1 1.962(7) . ? Zn1 O1 2.058(6) . ? Zn1 O11 2.152(8) . ? Zn1 O10 2.281(7) . ? Zn1 O2 2.319(6) . ? Zn1 C7 2.514(9) . ? Zn1 C21 2.543(10) . ? Zn2 O4 1.958(7) 8 ? Zn2 O8 2.026(8) . ? Zn2 N3 2.062(8) . ? Zn2 OW2 2.132(8) . ? Zn2 O10 2.124(7) . ? Zn2 C14 2.595(9) . ? O1 C7 1.267(12) . ? O2 C7 1.223(11) . ? O3 C8 1.259(11) . ? O4 C8 1.268(11) . ? O4 Zn2 1.958(7) 8 ? O5 C9 1.278(10) . ? O6 C9 1.211(11) . ? O6 Zn1 1.939(6) 5_545 ? O7 C14 1.287(11) . ? O8 C14 1.226(11) . ? O10 C21 1.273(12) . ? O11 C21 1.254(12) . ? N3 C20 1.414(12) . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? C1 C2 1.392(11) . ? C1 C6 1.412(11) . ? C1 H1A 0.9300 . ? C2 C3 1.360(12) . ? C2 C7 1.469(12) . ? C3 C4 1.370(12) . ? C3 H3A 0.9300 . ? C4 C5 1.434(11) . ? C4 C8 1.508(12) . ? C5 C6 1.360(10) . ? C5 H5A 0.9300 . ? C6 C9 1.458(11) . ? C10 C11 1.393(10) 8_665 ? C10 C11 1.393(10) . ? C10 H10A 0.9300 . ? C11 C12 1.402(12) . ? C11 C14 1.485(12) . ? C12 C13 1.353(12) . ? C12 H12A 0.9300 . ? C13 C12 1.353(12) 8_665 ? C13 C15 1.51(3) 8_665 ? C13 C15 1.51(3) . ? C18 N1 1.326(8) . ? C18 C17 1.373(8) . ? C18 C19 1.474(12) . ? C19 C20 1.527(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.508(12) . ? C20 H20A 0.9800 . ? N2 C16 1.323(9) . ? N2 C17 1.339(9) . ? N2 H2A 0.8600 . ? N1 C16 1.347(8) . ? N1 H1B 0.8600 . ? C17 H17A 0.9300 . ? C16 H16A 0.9300 . ? O9 C15 1.230(10) . ? O9 C15 1.233(10) 8_665 ? C15 C15 0.44(10) 8_665 ? C15 O9 1.233(10) 8_665 ? OW1 HW1A 0.8537 . ? OW1 HW1B 0.8511 . ? OW2 HW2A 0.8485 . ? OW2 HW2B 0.8522 . ? OW3 HW3A 0.850(10) . ? OW3 HW3B 0.851(10) . ? OW4 HW4A 0.8497 . ? OW4 HW4B 0.8501 . ? 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 O6 Zn1 OW1 93.6(3) 5 . ? O6 Zn1 O1 110.2(3) 5 . ? OW1 Zn1 O1 109.2(3) . . ? O6 Zn1 O11 98.6(3) 5 . ? OW1 Zn1 O11 94.6(3) . . ? O1 Zn1 O11 140.7(3) . . ? O6 Zn1 O10 90.8(3) 5 . ? OW1 Zn1 O10 154.1(3) . . ? O1 Zn1 O10 93.1(3) . . ? O11 Zn1 O10 59.5(3) . . ? O6 Zn1 O2 168.9(3) 5 . ? OW1 Zn1 O2 93.1(3) . . ? O1 Zn1 O2 59.1(2) . . ? O11 Zn1 O2 89.7(3) . . ? O10 Zn1 O2 87.1(3) . . ? O6 Zn1 C7 140.3(3) 5 . ? OW1 Zn1 C7 102.2(3) . . ? O1 Zn1 C7 30.1(3) . . ? O11 Zn1 C7 115.9(3) . . ? O10 Zn1 C7 90.3(3) . . ? O2 Zn1 C7 29.0(3) . . ? O6 Zn1 C21 96.0(3) 5 . ? OW1 Zn1 C21 124.1(3) . . ? O1 Zn1 C21 118.3(3) . . ? O11 Zn1 C21 29.5(3) . . ? O10 Zn1 C21 30.0(3) . . ? O2 Zn1 C21 87.6(3) . . ? C7 Zn1 C21 104.3(3) . . ? O4 Zn2 O8 100.6(3) 8 . ? O4 Zn2 N3 117.3(3) 8 . ? O8 Zn2 N3 142.0(3) . . ? O4 Zn2 OW2 94.8(4) 8 . ? O8 Zn2 OW2 90.9(4) . . ? N3 Zn2 OW2 88.2(3) . . ? O4 Zn2 O10 92.9(3) 8 . ? O8 Zn2 O10 98.8(3) . . ? N3 Zn2 O10 78.2(3) . . ? OW2 Zn2 O10 166.3(3) . . ? O4 Zn2 C14 128.0(3) 8 . ? O8 Zn2 C14 27.4(3) . . ? N3 Zn2 C14 114.7(3) . . ? OW2 Zn2 C14 88.3(3) . . ? O10 Zn2 C14 95.9(3) . . ? C7 O1 Zn1 95.2(5) . . ? C7 O2 Zn1 84.4(5) . . ? C8 O4 Zn2 118.0(6) . 8 ? C9 O6 Zn1 142.9(7) . 5_545 ? C14 O8 Zn2 103.1(6) . . ? C21 O10 Zn2 113.7(6) . . ? C21 O10 Zn1 86.5(6) . . ? Zn2 O10 Zn1 158.7(3) . . ? C21 O11 Zn1 92.8(6) . . ? C20 N3 Zn2 111.6(5) . . ? C20 N3 H3B 109.3 . . ? Zn2 N3 H3B 109.3 . . ? C20 N3 H3C 109.3 . . ? Zn2 N3 H3C 109.3 . . ? H3B N3 H3C 108.0 . . ? C2 C1 C6 121.2(7) . . ? C2 C1 H1A 119.4 . . ? C6 C1 H1A 119.4 . . ? C3 C2 C1 118.9(8) . . ? C3 C2 C7 122.4(8) . . ? C1 C2 C7 118.6(8) . . ? C2 C3 C4 121.8(8) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? C3 C4 C5 119.0(8) . . ? C3 C4 C8 122.4(7) . . ? C5 C4 C8 118.4(7) . . ? C6 C5 C4 120.0(8) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 118.4(7) . . ? C5 C6 C9 123.1(7) . . ? C1 C6 C9 118.3(6) . . ? O2 C7 O1 121.3(8) . . ? O2 C7 C2 118.8(9) . . ? O1 C7 C2 119.9(8) . . ? O2 C7 Zn1 66.7(5) . . ? O1 C7 Zn1 54.6(4) . . ? C2 C7 Zn1 174.2(7) . . ? O3 C8 O4 124.7(9) . . ? O3 C8 C4 118.0(8) . . ? O4 C8 C4 117.2(8) . . ? O6 C9 O5 121.0(8) . . ? O6 C9 C6 120.5(8) . . ? O5 C9 C6 118.3(7) . . ? C11 C10 C11 119.5(11) 8_665 . ? C11 C10 H10A 120.3 8_665 . ? C11 C10 H10A 120.3 . . ? C10 C11 C12 119.1(9) . . ? C10 C11 C14 121.5(8) . . ? C12 C11 C14 119.3(8) . . ? C13 C12 C11 120.9(10) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C12 120.6(14) 8_665 . ? C12 C13 C15 121.8(9) 8_665 8_665 ? C12 C13 C15 117.0(10) . 8_665 ? C12 C13 C15 117.0(10) 8_665 . ? C12 C13 C15 121.8(9) . . ? C15 C13 C15 17(4) 8_665 . ? O8 C14 O7 120.9(8) . . ? O8 C14 C11 120.1(8) . . ? O7 C14 C11 118.9(8) . . ? O8 C14 Zn2 49.5(5) . . ? O7 C14 Zn2 72.6(5) . . ? C11 C14 Zn2 162.3(6) . . ? N1 C18 C17 108.3(9) . . ? N1 C18 C19 123.0(8) . . ? C17 C18 C19 128.3(8) . . ? C18 C19 C20 113.5(8) . . ? C18 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? N3 C20 C21 111.6(8) . . ? N3 C20 C19 114.1(8) . . ? C21 C20 C19 109.1(8) . . ? N3 C20 H20A 107.2 . . ? C21 C20 H20A 107.2 . . ? C19 C20 H20A 107.2 . . ? O11 C21 O10 121.2(9) . . ? O11 C21 C20 121.2(9) . . ? O10 C21 C20 117.6(9) . . ? O11 C21 Zn1 57.7(5) . . ? O10 C21 Zn1 63.5(5) . . ? C20 C21 Zn1 178.9(8) . . ? C16 N2 C17 110.9(10) . . ? C16 N2 H2A 124.6 . . ? C17 N2 H2A 124.6 . . ? C18 N1 C16 108.6(9) . . ? C18 N1 H1B 125.7 . . ? C16 N1 H1B 125.7 . . ? N2 C17 C18 104.6(9) . . ? N2 C17 H17A 127.7 . . ? C18 C17 H17A 127.7 . . ? N2 C16 N1 106.5(10) . . ? N2 C16 H16A 126.7 . . ? N1 C16 H16A 126.7 . . ? C15 O9 C15 20(5) . 8_665 ? C15 C15 O9 80(3) 8_665 . ? C15 C15 O9 79(3) 8_665 8_665 ? O9 C15 O9 122(3) . 8_665 ? C15 C15 C13 81.7(19) 8_665 . ? O9 C15 C13 115(2) . . ? O9 C15 C13 114.8(19) 8_665 . ? Zn1 OW1 HW1A 104.1 . . ? Zn1 OW1 HW1B 122.8 . . ? HW1A OW1 HW1B 109.6 . . ? Zn2 OW2 HW2A 94.2 . . ? Zn2 OW2 HW2B 154.0 . . ? HW2A OW2 HW2B 108.9 . . ? HW3A OW3 HW3B 108.3(18) . . ? HW4A OW4 HW4B 108.6 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O3 0.90 2.33 2.951(12) 126.1 8 N3 H3C O11 0.90 2.35 3.233(11) 166.9 3 N2 H2A O5 0.86 1.96 2.749(12) 152.0 3_455 N1 H1B O5 0.86 2.01 2.864(12) 169.9 1_565 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.815 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.104 #===END