#============================================================================= # 1. SUBMISSION DETAILS _publ_contact_author_name 'Yuan-Gen Yao' _publ_contact_author_address ; State Key Laboratory of Structural chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian, 350002, China ; _publ_contact_author_email yyg@fjirsm.ac.cn _publ_contact_author_fax 86-591-83714946 _publ_contact_author_phone 86-591-83711523 #============================================================================= data_Compound-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H20 N2 O4 Zn, C16 H8 O9, 3(H2 O)' _chemical_formula_sum 'C28 H34 N2 O16 Zn' _chemical_formula_weight 719.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 18.883(3) _cell_length_b 14.4900(8) _cell_length_c 14.237(4) _cell_angle_alpha 90.00 _cell_angle_beta 125.30(3) _cell_angle_gamma 90.00 _cell_volume 3179.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3833 _cell_measurement_theta_min 2.5794 _cell_measurement_theta_max 28.7270 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496.0 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_T_min 0.33376 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details crystalclear _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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6498 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2800 _reflns_number_gt 2130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.1895P] 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 2800 _refine_ls_number_parameters 215 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.924 _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 -0.7500 0.2500 -1.0000 0.03367(17) Uani 1 2 d S . . N1 N -0.68384(13) 0.33848(14) -0.84971(17) 0.0335(5) Uani 1 1 d . . . O1W O -0.69377(14) 0.13669(13) -0.88919(16) 0.0547(6) Uani 1 1 d . . . H1WA H -0.7081 0.0872 -0.9282 0.082 Uiso 1 1 d R . . H1WB H -0.6853 0.1409 -0.8238 0.082 Uiso 1 1 d R . . C1 C -0.72140(16) 0.40915(18) -0.8345(2) 0.0371(6) Uani 1 1 d . . . H1A H -0.7795 0.4211 -0.8916 0.045 Uiso 1 1 calc R . . O1 O -0.31751(17) 0.85091(16) -0.30632(18) 0.0704(7) Uani 1 1 d . . . O2W O -0.64094(13) 0.25619(12) -1.00940(16) 0.0478(5) Uani 1 1 d . . . H2WA H -0.6071 0.2111 -0.9726 0.072 Uiso 1 1 d R . . H2WB H -0.6561 0.2602 -1.0783 0.072 Uiso 1 1 d R . . C2 C -0.67870(16) 0.46586(18) -0.7384(2) 0.0372(6) Uani 1 1 d . . . H2A H -0.7081 0.5143 -0.7321 0.045 Uiso 1 1 calc R . . O2 O -0.20049(16) 0.76976(18) -0.24292(19) 0.0657(7) Uani 1 1 d . . . H2 H -0.1860 0.7167 -0.2519 0.099 Uiso 1 1 d R . . C3 C -0.59197(15) 0.44996(16) -0.6518(2) 0.0303(6) Uani 1 1 d . . . O3 O -0.15482(13) 0.63995(19) -0.29949(19) 0.0705(7) Uani 1 1 d . . . O3W O 0.0000 0.5154(3) -0.2500 0.1036(15) Uani 1 2 d S . . H3W H -0.0417 0.5536 -0.2790 0.155 Uiso 1 1 d R . . C4 C -0.55328(17) 0.37705(19) -0.6674(2) 0.0399(6) Uani 1 1 d . . . H4A H -0.4952 0.3634 -0.6117 0.048 Uiso 1 1 calc R . . O4 O -0.20575(15) 0.54433(16) -0.4428(2) 0.0704(7) Uani 1 1 d . . . O4W O -0.0174(2) 0.3757(3) -0.3995(3) 0.1397(15) Uani 1 1 d D . . H4WA H -0.0667 0.3996 -0.4484 0.210 Uiso 1 1 d RD . . H4WB H 0.0324 0.3909 -0.3817 0.210 Uiso 1 1 d RD . . C5 C -0.60045(17) 0.32401(19) -0.7659(2) 0.0412(6) Uani 1 1 d . . . H5A H -0.5724 0.2753 -0.7741 0.049 Uiso 1 1 calc R . . O5 O -0.5000 0.6106(2) -0.7500 0.0673(9) Uani 1 2 d S . . C6 C -0.54520(16) 0.51291(18) -0.5469(2) 0.0371(6) Uani 1 1 d . . . H6A H -0.5445 0.5748 -0.5724 0.045 Uiso 1 1 calc R . . H6B H -0.5788 0.5151 -0.5151 0.045 Uiso 1 1 calc R . . C7 C -0.32707(18) 0.74141(17) -0.4359(2) 0.0375(6) Uani 1 1 d . . . C8 C -0.30206(16) 0.66258(17) -0.4684(2) 0.0342(6) Uani 1 1 d . . . C9 C -0.36144(17) 0.62340(19) -0.5758(2) 0.0401(6) Uani 1 1 d . . . H9A H -0.3456 0.5715 -0.5980 0.048 Uiso 1 1 calc R . . C10 C -0.44285(17) 0.65991(19) -0.6495(2) 0.0454(7) Uani 1 1 d . . . C11 C -0.4675(2) 0.7385(2) -0.6220(3) 0.0550(8) Uani 1 1 d . . . H11A H -0.5219 0.7646 -0.6736 0.066 Uiso 1 1 calc R . . C12 C -0.40954(19) 0.7777(2) -0.5163(3) 0.0495(7) Uani 1 1 d . . . H12A H -0.4259 0.8311 -0.4972 0.059 Uiso 1 1 calc R . . C13 C -0.2787(2) 0.7911(2) -0.3216(2) 0.0478(7) Uani 1 1 d . . . C14 C -0.21577(17) 0.6119(2) -0.4002(2) 0.0439(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0384(3) 0.0332(3) 0.0217(2) -0.01010(16) 0.0128(2) -0.01031(17) N1 0.0340(11) 0.0355(12) 0.0252(11) -0.0102(9) 0.0138(10) -0.0075(9) O1W 0.0882(15) 0.0371(10) 0.0332(11) -0.0052(8) 0.0319(11) -0.0026(10) C1 0.0343(13) 0.0374(14) 0.0258(14) -0.0035(11) 0.0095(12) -0.0034(11) O1 0.113(2) 0.0568(14) 0.0468(14) -0.0078(11) 0.0495(15) 0.0015(14) O2W 0.0420(11) 0.0642(14) 0.0297(11) -0.0107(9) 0.0164(9) -0.0135(9) C2 0.0418(15) 0.0296(13) 0.0313(14) -0.0056(10) 0.0160(13) -0.0007(11) O2 0.0604(15) 0.0925(17) 0.0344(12) -0.0178(11) 0.0218(12) -0.0209(12) C3 0.0367(13) 0.0281(12) 0.0221(13) -0.0069(9) 0.0147(11) -0.0097(10) O3 0.0353(11) 0.1036(19) 0.0448(13) 0.0026(13) 0.0070(11) 0.0020(11) O3W 0.061(2) 0.073(3) 0.145(4) 0.000 0.041(3) 0.000 C4 0.0308(13) 0.0454(15) 0.0296(14) -0.0147(12) 0.0094(12) -0.0057(11) O4 0.0649(15) 0.0495(13) 0.0711(17) 0.0087(12) 0.0245(14) 0.0185(11) O4W 0.116(3) 0.163(3) 0.153(3) -0.072(3) 0.085(3) -0.057(3) C5 0.0361(14) 0.0445(15) 0.0357(15) -0.0153(12) 0.0166(13) -0.0027(12) O5 0.0625(19) 0.0482(17) 0.0363(17) 0.000 -0.0031(15) 0.000 C6 0.0445(14) 0.0380(14) 0.0224(13) -0.0118(10) 0.0156(12) -0.0109(12) C7 0.0426(15) 0.0444(16) 0.0295(14) 0.0014(11) 0.0230(13) -0.0096(12) C8 0.0367(14) 0.0363(14) 0.0281(14) 0.0071(11) 0.0179(12) -0.0036(11) C9 0.0462(15) 0.0372(14) 0.0293(14) 0.0019(11) 0.0174(13) 0.0006(12) C10 0.0433(16) 0.0431(16) 0.0308(15) 0.0001(12) 0.0104(14) -0.0043(13) C11 0.0388(16) 0.064(2) 0.0475(19) 0.0019(15) 0.0165(15) 0.0091(14) C12 0.0510(17) 0.0501(16) 0.0493(19) -0.0028(14) 0.0300(16) 0.0069(14) C13 0.068(2) 0.0490(17) 0.0347(17) -0.0045(14) 0.0341(17) -0.0161(16) C14 0.0402(15) 0.0453(17) 0.0380(16) 0.0131(13) 0.0179(14) 0.0008(13) _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 O1W 2.092(2) . ? Zn1 O1W 2.092(2) 7_353 ? Zn1 O2W 2.141(2) 7_353 ? Zn1 O2W 2.141(2) . ? Zn1 N1 2.166(2) 7_353 ? Zn1 N1 2.166(2) . ? N1 C1 1.332(3) . ? N1 C5 1.333(3) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? C1 C2 1.386(3) . ? C1 H1A 0.9300 . ? O1 C13 1.234(4) . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8500 . ? C2 C3 1.387(3) . ? C2 H2A 0.9300 . ? O2 C13 1.272(4) . ? O2 H2 0.8500 . ? C3 C4 1.374(4) . ? C3 C6 1.522(3) . ? O3 C14 1.280(3) . ? O3W H3W 0.8499 . ? C4 C5 1.380(3) . ? C4 H4A 0.9300 . ? O4 C14 1.222(4) . ? O4W H4WA 0.8499 . ? O4W H4WB 0.8500 . ? C5 H5A 0.9300 . ? O5 C10 1.392(3) . ? O5 C10 1.392(3) 2_453 ? C6 C6 1.484(5) 5_464 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.397(4) . ? C7 C8 1.412(4) . ? C7 C13 1.511(4) . ? C8 C9 1.392(3) . ? C8 C14 1.520(4) . ? C9 C10 1.371(4) . ? C9 H9A 0.9300 . ? C10 C11 1.370(4) . ? C11 C12 1.372(4) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? 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 O1W Zn1 O1W 180.0 . 7_353 ? O1W Zn1 O2W 90.42(8) . 7_353 ? O1W Zn1 O2W 89.58(8) 7_353 7_353 ? O1W Zn1 O2W 89.58(8) . . ? O1W Zn1 O2W 90.42(8) 7_353 . ? O2W Zn1 O2W 180.0 7_353 . ? O1W Zn1 N1 91.84(8) . 7_353 ? O1W Zn1 N1 88.16(8) 7_353 7_353 ? O2W Zn1 N1 90.60(8) 7_353 7_353 ? O2W Zn1 N1 89.40(8) . 7_353 ? O1W Zn1 N1 88.16(8) . . ? O1W Zn1 N1 91.84(8) 7_353 . ? O2W Zn1 N1 89.40(8) 7_353 . ? O2W Zn1 N1 90.60(8) . . ? N1 Zn1 N1 180.0 7_353 . ? C1 N1 C5 116.1(2) . . ? C1 N1 Zn1 123.91(16) . . ? C5 N1 Zn1 120.00(17) . . ? Zn1 O1W H1WA 109.7 . . ? Zn1 O1W H1WB 117.5 . . ? H1WA O1W H1WB 124.3 . . ? N1 C1 C2 123.7(2) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? Zn1 O2W H2WA 109.7 . . ? Zn1 O2W H2WB 112.4 . . ? H2WA O2W H2WB 113.3 . . ? C1 C2 C3 119.6(2) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? C13 O2 H2 113.5 . . ? C4 C3 C2 116.7(2) . . ? C4 C3 C6 124.0(2) . . ? C2 C3 C6 119.4(2) . . ? C3 C4 C5 120.1(2) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? H4WA O4W H4WB 129.6 . . ? N1 C5 C4 123.9(2) . . ? N1 C5 H5A 118.1 . . ? C4 C5 H5A 118.1 . . ? C10 O5 C10 118.3(3) . 2_453 ? C6 C6 C3 116.4(3) 5_464 . ? C6 C6 H6A 108.2 5_464 . ? C3 C6 H6A 108.2 . . ? C6 C6 H6B 108.2 5_464 . ? C3 C6 H6B 108.2 . . ? H6A C6 H6B 107.3 . . ? C12 C7 C8 117.5(2) . . ? C12 C7 C13 113.4(3) . . ? C8 C7 C13 129.0(3) . . ? C9 C8 C7 118.7(2) . . ? C9 C8 C14 113.0(2) . . ? C7 C8 C14 128.3(2) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C11 C10 C9 121.2(3) . . ? C11 C10 O5 122.0(3) . . ? C9 C10 O5 116.7(3) . . ? C10 C11 C12 118.0(3) . . ? C10 C11 H11A 121.0 . . ? C12 C11 H11A 121.0 . . ? C11 C12 C7 123.2(3) . . ? C11 C12 H12A 118.4 . . ? C7 C12 H12A 118.4 . . ? O1 C13 O2 121.4(3) . . ? O1 C13 C7 118.3(3) . . ? O2 C13 C7 120.4(3) . . ? O4 C14 O3 120.9(3) . . ? O4 C14 C8 119.1(3) . . ? O3 C14 C8 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.038 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.076 #=========================END data_Compound-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C68 H52 N6 O20 Zn4), C12 H12 N2, 7(O)' _chemical_formula_sum 'C148 H116 N14 O47 Zn8' _chemical_formula_weight 3365.67 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 'triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8606(4) _cell_length_b 16.9142(5) _cell_length_c 18.1588(5) _cell_angle_alpha 112.895(3) _cell_angle_beta 96.840(2) _cell_angle_gamma 101.840(2) _cell_volume 3743.76(19) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13324 _cell_measurement_theta_min 2.4574 _cell_measurement_theta_max 28.7447 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1718.0 _exptl_absorpt_coefficient_mu 1.348 _exptl_absorpt_correction_T_min 0.86457 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details crystalclear _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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 27355 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13158 _reflns_number_gt 9099 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13158 _refine_ls_number_parameters 991 _refine_ls_number_restraints 263 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1960 _refine_ls_wR_factor_gt 0.1857 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.262 _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 1.83887(5) 0.65338(4) 0.14821(4) 0.0269(2) Uani 1 1 d . . . Zn2 Zn 1.82146(5) 0.14901(4) 0.15318(4) 0.0266(2) Uani 1 1 d . . . Zn3 Zn 2.85881(5) 1.07231(5) 0.40150(4) 0.0344(2) Uani 1 1 d . . . Zn4 Zn 1.85004(5) 0.58633(5) 0.39635(4) 0.0324(2) Uani 1 1 d . . . C1 C 2.1182(4) 0.6429(4) 0.3297(3) 0.0284(12) Uani 1 1 d . . . C2 C 2.1057(4) 0.6268(4) 0.2472(3) 0.0256(12) Uani 1 1 d . . . C3 C 2.1892(4) 0.6261(4) 0.2103(4) 0.0322(13) Uani 1 1 d . . . H3A H 2.1809 0.6145 0.1551 0.039 Uiso 1 1 calc R . . C4 C 2.2828(4) 0.6426(4) 0.2563(4) 0.0398(15) Uani 1 1 d . . . C5 C 2.2979(5) 0.6598(5) 0.3375(4) 0.057(2) Uani 1 1 d . . . H5A H 2.3625 0.6721 0.3678 0.068 Uiso 1 1 calc R . . C6 C 2.2159(5) 0.6586(5) 0.3737(4) 0.0500(19) Uani 1 1 d . . . H6A H 2.2255 0.6685 0.4285 0.060 Uiso 1 1 calc R . . C7 C 2.0324(4) 0.6353(4) 0.3707(3) 0.0296(13) Uani 1 1 d . . . C8 C 2.0063(4) 0.6138(4) 0.1944(4) 0.0291(13) Uani 1 1 d . . . C9 C 2.6291(4) 0.8395(4) 0.2998(4) 0.0365(15) Uani 1 1 d . . . C10 C 2.6267(4) 0.7519(4) 0.2586(3) 0.0277(12) Uani 1 1 d . . . C11 C 2.5371(4) 0.6849(4) 0.2329(3) 0.0328(14) Uani 1 1 d . . . H11A H 2.5368 0.6257 0.2049 0.039 Uiso 1 1 calc R . . C12 C 2.4488(4) 0.7056(4) 0.2484(4) 0.0391(15) Uani 1 1 d . . . C13 C 2.4488(5) 0.7934(5) 0.2907(5) 0.0539(19) Uani 1 1 d . . . H13A H 2.3891 0.8076 0.3015 0.065 Uiso 1 1 calc R . . C14 C 2.5380(5) 0.8596(4) 0.3165(4) 0.0487(18) Uani 1 1 d . . . H14A H 2.5384 0.9187 0.3455 0.058 Uiso 1 1 calc R . . C15 C 2.7264(5) 0.9124(4) 0.3315(4) 0.0417(16) Uani 1 1 d . . . C16 C 2.7183(4) 0.7223(4) 0.2348(3) 0.0301(13) Uani 1 1 d . . . C17 C 1.6136(4) 0.3575(4) 0.2811(4) 0.0328(14) Uani 1 1 d . . . C18 C 1.6094(4) 0.2692(4) 0.2531(3) 0.0267(12) Uani 1 1 d . . . C19 C 1.5165(4) 0.2043(4) 0.2256(4) 0.0355(14) Uani 1 1 d . . . H19A H 1.5145 0.1443 0.2064 0.043 Uiso 1 1 calc R . . C20 C 1.4288(4) 0.2290(5) 0.2270(4) 0.0450(17) Uani 1 1 d . . . C21 C 1.4311(5) 0.3180(5) 0.2547(5) 0.055(2) Uani 1 1 d . . . H21A H 1.3712 0.3348 0.2553 0.067 Uiso 1 1 calc R . . C22 C 1.5227(5) 0.3817(4) 0.2814(4) 0.0479(17) Uani 1 1 d . . . H22A H 1.5243 0.4416 0.3000 0.058 Uiso 1 1 calc R . . C23 C 1.7113(5) 0.4283(4) 0.3191(4) 0.0451(10) Uani 1 1 d U . . C24 C 1.7013(4) 0.2340(4) 0.2431(4) 0.0311(13) Uani 1 1 d . . . C25 C 1.1175(4) 0.1417(4) 0.3275(3) 0.0301(13) Uani 1 1 d . . . C26 C 1.0929(4) 0.1262(4) 0.2452(3) 0.0263(12) Uani 1 1 d . . . C27 C 1.1691(4) 0.1343(4) 0.2024(4) 0.0305(13) Uani 1 1 d . . . H27A H 1.1521 0.1219 0.1472 0.037 Uiso 1 1 calc R . . C28 C 1.2693(4) 0.1605(4) 0.2419(4) 0.0394(16) Uani 1 1 d . . . C29 C 1.2959(4) 0.1786(5) 0.3233(4) 0.0504(18) Uani 1 1 d . . . H29A H 1.3637 0.1979 0.3500 0.060 Uiso 1 1 calc R . . C30 C 1.2205(4) 0.1676(5) 0.3652(4) 0.0442(16) Uani 1 1 d . . . H30A H 1.2386 0.1778 0.4198 0.053 Uiso 1 1 calc R . . C31 C 1.0396(4) 0.1247(4) 0.3734(4) 0.0315(13) Uani 1 1 d . . . C32 C 0.9882(4) 0.1074(4) 0.1982(4) 0.0305(13) Uani 1 1 d . . . C33 C 1.8253(6) 0.7211(5) 0.0182(4) 0.0491(18) Uani 1 1 d . . . H33A H 1.7915 0.7575 0.0517 0.059 Uiso 1 1 calc R . . C34 C 1.8320(7) 0.7232(5) -0.0556(4) 0.057(2) Uani 1 1 d . . . H34A H 1.8023 0.7603 -0.0715 0.069 Uiso 1 1 calc R . . C35 C 1.8826(5) 0.6709(4) -0.1066(4) 0.0421(16) Uani 1 1 d . . . C36 C 1.9245(5) 0.6183(5) -0.0794(4) 0.0455(17) Uani 1 1 d . . . H36A H 1.9597 0.5822 -0.1116 0.055 Uiso 1 1 calc R . . C37 C 1.9153(5) 0.6182(5) -0.0044(4) 0.0434(16) Uani 1 1 d . . . H37A H 1.9448 0.5817 0.0126 0.052 Uiso 1 1 calc R . . C38 C 1.7947(8) 0.5852(7) -0.4554(5) 0.0829(14) Uani 1 1 d U . . H38A H 1.7326 0.5822 -0.4838 0.099 Uiso 1 1 calc R . . C39 C 1.8006(8) 0.5861(7) -0.3774(5) 0.0858(13) Uani 1 1 d U . . H39A H 1.7430 0.5835 -0.3559 0.103 Uiso 1 1 calc R . . C40 C 1.8857(8) 0.5906(7) -0.3346(5) 0.0821(13) Uani 1 1 d U . . C41 C 1.9666(8) 0.5971(6) -0.3670(5) 0.0815(13) Uani 1 1 d U . . H41A H 2.0294 0.6024 -0.3379 0.098 Uiso 1 1 calc R . . C42 C 1.9568(7) 0.5958(6) -0.4445(5) 0.0778(13) Uani 1 1 d U . . H42A H 2.0147 0.6004 -0.4655 0.093 Uiso 1 1 calc R . . C43 C 1.8922(8) 0.6717(6) -0.1878(5) 0.0741(16) Uani 1 1 d U . . H43A H 1.8388 0.6938 -0.2053 0.089 Uiso 1 1 calc R . . H43B H 1.9560 0.7137 -0.1801 0.089 Uiso 1 1 calc R . . C44 C 1.8877(8) 0.5869(6) -0.2528(5) 0.0819(14) Uani 1 1 d U . . H44A H 1.8275 0.5428 -0.2572 0.098 Uiso 1 1 calc R . . H44B H 1.9459 0.5678 -0.2390 0.098 Uiso 1 1 calc R . . C45 C 1.7404(7) 0.4768(5) 0.1377(5) 0.0759(11) Uani 1 1 d U . . H45A H 1.7858 0.4986 0.1876 0.091 Uiso 1 1 calc R . . C46 C 1.6752(7) 0.3924(6) 0.1078(5) 0.0794(11) Uani 1 1 d U . . H46A H 1.6764 0.3599 0.1389 0.095 Uiso 1 1 calc R . . C47 C 1.6112(8) 0.3566(6) 0.0360(6) 0.0843(10) Uani 1 1 d DU . . C48 C 1.6154(7) 0.4105(6) -0.0083(6) 0.0844(11) Uani 1 1 d U . . H48A H 1.5749 0.3884 -0.0605 0.101 Uiso 1 1 calc R . . C49 C 1.6793(7) 0.4946(6) 0.0268(5) 0.0804(11) Uani 1 1 d U . . H49A H 1.6790 0.5299 -0.0018 0.096 Uiso 1 1 calc R . . C50 C 1.2728(7) 0.0254(5) -0.1481(5) 0.0748(11) Uani 1 1 d U . . H50A H 1.2243 0.0033 -0.1965 0.090 Uiso 1 1 calc R . . C51 C 1.3344(7) 0.1112(6) -0.1192(5) 0.0787(11) Uani 1 1 d U . . H51A H 1.3293 0.1442 -0.1495 0.094 Uiso 1 1 calc R . . C52 C 1.4012(7) 0.1469(6) -0.0480(6) 0.0834(10) Uani 1 1 d DU . . C53 C 1.4026(7) 0.0921(6) -0.0036(6) 0.0829(11) Uani 1 1 d U . . H53A H 1.4442 0.1148 0.0482 0.100 Uiso 1 1 calc R . . C54 C 1.3426(7) 0.0076(6) -0.0387(5) 0.0788(11) Uani 1 1 d U . . H54A H 1.3461 -0.0283 -0.0111 0.095 Uiso 1 1 calc R . . C55 C 1.5566(7) 0.2512(6) -0.0110(6) 0.0869(11) Uani 1 1 d DU . . H55A H 1.5603 0.2273 -0.0683 0.104 Uiso 1 1 calc R . . H55B H 1.5846 0.2180 0.0150 0.104 Uiso 1 1 calc R . . C56 C 1.4568(7) 0.2516(5) -0.0015(6) 0.0867(11) Uani 1 1 d DU . . H56A H 1.4290 0.2849 -0.0274 0.104 Uiso 1 1 calc R . . H56B H 1.4533 0.2756 0.0558 0.104 Uiso 1 1 calc R . . C57 C 1.8157(6) 0.2173(5) 0.0254(4) 0.0510(19) Uani 1 1 d . . . H57A H 1.7841 0.2553 0.0599 0.061 Uiso 1 1 calc R . . C58 C 1.8237(7) 0.2215(5) -0.0472(5) 0.059(2) Uani 1 1 d . . . H58A H 1.7969 0.2610 -0.0616 0.070 Uiso 1 1 calc R . . C59 C 1.8718(6) 0.1666(4) -0.0998(4) 0.0445(17) Uani 1 1 d . . . C60 C 1.9110(6) 0.1113(5) -0.0742(4) 0.055(2) Uani 1 1 d . . . H60A H 1.9463 0.0752 -0.1061 0.066 Uiso 1 1 calc R . . C61 C 1.8977(5) 0.1095(5) 0.0001(4) 0.0470(17) Uani 1 1 d . . . H61A H 1.9226 0.0701 0.0157 0.056 Uiso 1 1 calc R . . C62 C 1.7817(6) 0.0667(6) -0.4594(5) 0.063(2) Uani 1 1 d . . . H62A H 1.7215 0.0571 -0.4944 0.076 Uiso 1 1 calc R . . C63 C 1.7802(7) 0.0683(6) -0.3834(5) 0.073(3) Uani 1 1 d . . . H63A H 1.7189 0.0595 -0.3677 0.087 Uiso 1 1 calc R . . C64 C 1.8676(8) 0.0827(5) -0.3302(5) 0.065(2) Uani 1 1 d . . . C65 C 1.9569(7) 0.0989(5) -0.3550(4) 0.059(2) Uani 1 1 d . . . H65A H 2.0183 0.1110 -0.3202 0.070 Uiso 1 1 calc R . . C66 C 1.9546(6) 0.0970(5) -0.4311(4) 0.0469(17) Uani 1 1 d . . . H66A H 2.0155 0.1090 -0.4466 0.056 Uiso 1 1 calc R . . C67 C 1.8803(8) 0.1671(5) -0.1814(4) 0.072(3) Uani 1 1 d . . . H67A H 1.8296 0.1929 -0.1971 0.087 Uiso 1 1 calc R . . H67B H 1.9461 0.2055 -0.1753 0.087 Uiso 1 1 calc R . . C68 C 1.8682(9) 0.0803(6) -0.2470(5) 0.085(3) Uani 1 1 d . . . H68A H 1.8052 0.0401 -0.2502 0.103 Uiso 1 1 calc R . . H68B H 1.9228 0.0567 -0.2342 0.103 Uiso 1 1 calc R . . C69 C 1.5530(8) 1.2563(7) 0.4624(6) 0.0858(15) Uani 1 1 d U . . H69A H 1.5925 1.2234 0.4325 0.103 Uiso 1 1 calc R . . C70 C 1.5630(8) 1.3417(7) 0.4679(5) 0.0879(14) Uani 1 1 d U . . H70A H 1.6093 1.3654 0.4437 0.105 Uiso 1 1 calc R . . C71 C 1.5015(8) 1.3925(7) 0.5111(6) 0.0889(14) Uani 1 1 d U . . C72 C 1.4382(7) 1.3534(7) 0.5486(5) 0.0858(14) Uani 1 1 d U . . H72A H 1.3977 1.3843 0.5790 0.103 Uiso 1 1 calc R . . C73 C 1.4357(8) 1.2695(7) 0.5406(6) 0.0840(14) Uani 1 1 d U . . H73A H 1.3929 1.2459 0.5671 0.101 Uiso 1 1 calc R . . C74 C 1.4963(9) 1.4815(7) 0.5193(6) 0.0958(17) Uani 1 1 d DU . . H74A H 1.4310 1.4842 0.5327 0.115 Uiso 1 1 calc R . . H74B H 1.5455 1.5214 0.5698 0.115 Uiso 1 1 calc R . . N1 N 1.8663(4) 0.6678(3) 0.0440(3) 0.0331(11) Uani 1 1 d . . . N2 N 1.8714(6) 0.5885(5) -0.4904(4) 0.0713(13) Uani 1 1 d U . . N3 N 1.7411(6) 0.5282(4) 0.0984(4) 0.0751(11) Uani 1 1 d U . . N4 N 1.2789(5) -0.0265(4) -0.1109(4) 0.0736(11) Uani 1 1 d U . . N5 N 1.8508(4) 0.1617(3) 0.0494(3) 0.0338(11) Uani 1 1 d . . . N6 N 1.8695(4) 0.0788(4) -0.4839(3) 0.0427(13) Uani 1 1 d . . . N7 N 1.4901(6) 1.2176(6) 0.4975(4) 0.0838(14) Uani 1 1 d U . . O1 O 1.9484(3) 0.5801(3) 0.3266(2) 0.0345(10) Uani 1 1 d . . . O1W O 2.8213(4) 1.1874(3) 0.4235(3) 0.0479(12) Uani 1 1 d D . . H1WA H 2.8632 1.2299 0.4648 0.072 Uiso 1 1 d R . . H1WB H 2.8070 1.2121 0.3924 0.072 Uiso 1 1 d RD . . O2W O 1.8119(3) 0.7013(3) 0.4224(3) 0.0413(10) Uani 1 1 d D . . H2WA H 1.7921 0.7057 0.3783 0.062 Uiso 1 1 d R . . H2WB H 1.8520 0.7480 0.4612 0.062 Uiso 1 1 d RD . . O2 O 2.0447(3) 0.6787(3) 0.4449(3) 0.0525(13) Uani 1 1 d . . . O3 O 1.9653(3) 0.6765(3) 0.2205(2) 0.0324(9) Uani 1 1 d . . . O3W O 1.5692(8) 1.0538(6) 0.2928(6) 0.166(4) Uani 1 1 d . . . O4 O 1.9739(3) 0.5474(3) 0.1290(3) 0.0528(12) Uani 1 1 d . . . O4W O 1.4898(9) 1.0406(7) 0.4533(8) 0.213(6) Uani 1 1 d . . . O5 O 2.7213(3) 0.9916(3) 0.3438(3) 0.0455(11) Uani 1 1 d . . . O5W O 1.1047(16) 0.6083(11) -0.1987(11) 0.139(7) Uani 0.50 1 d P . . O6 O 2.8068(3) 0.8959(3) 0.3447(3) 0.0659(16) Uani 1 1 d . . . O6W O 1.899(2) 0.8866(15) 0.1873(13) 0.203(11) Uani 0.50 1 d P . . O7 O 2.7580(3) 0.6822(3) 0.2689(3) 0.0453(11) Uani 1 1 d . . . O7W O 1.4009(14) 0.9622(11) 0.1508(13) 0.196(10) Uani 0.50 1 d P . . O8 O 2.7447(3) 0.7309(3) 0.1734(3) 0.0382(10) Uani 1 1 d . . . O9 O 2.3618(3) 0.6360(3) 0.2158(3) 0.0593(15) Uani 1 1 d . . . O10 O 1.7108(3) 0.5090(3) 0.3410(3) 0.0449(9) Uani 1 1 d U . . O11 O 1.7909(3) 0.4082(3) 0.3302(3) 0.0584(12) Uani 1 1 d U . . O12 O 1.7364(3) 0.2313(3) 0.1819(3) 0.0386(10) Uani 1 1 d . . . O13 O 1.7280(4) 0.1986(4) 0.2871(3) 0.0613(14) Uani 1 1 d . . . O14 O 0.9540(3) 0.0712(3) 0.3306(2) 0.0401(11) Uani 1 1 d . . . O15 O 1.0586(4) 0.1600(3) 0.4482(3) 0.0559(14) Uani 1 1 d . . . O16 O 0.9449(3) 0.1692(3) 0.2265(3) 0.0354(10) Uani 1 1 d . . . O17 O 0.9537(3) 0.0396(3) 0.1344(3) 0.0476(12) Uani 1 1 d . . . O18 O 1.3381(3) 0.1628(3) 0.1933(3) 0.0634(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0236(3) 0.0304(4) 0.0283(4) 0.0137(3) 0.0084(3) 0.0068(3) Zn2 0.0215(3) 0.0305(4) 0.0286(4) 0.0128(3) 0.0079(3) 0.0073(3) Zn3 0.0324(4) 0.0407(4) 0.0254(4) 0.0142(3) 0.0086(3) -0.0012(3) Zn4 0.0278(4) 0.0408(4) 0.0270(4) 0.0146(3) 0.0109(3) 0.0026(3) C1 0.019(3) 0.033(3) 0.028(3) 0.010(3) 0.005(2) 0.001(2) C2 0.018(3) 0.028(3) 0.035(3) 0.018(3) 0.009(2) 0.003(2) C3 0.028(3) 0.031(3) 0.036(3) 0.013(3) 0.015(3) 0.003(3) C4 0.017(3) 0.044(4) 0.048(4) 0.010(3) 0.012(3) 0.002(3) C5 0.013(3) 0.087(6) 0.045(4) 0.011(4) -0.005(3) 0.003(3) C6 0.023(3) 0.083(5) 0.033(4) 0.019(4) -0.001(3) 0.006(3) C7 0.024(3) 0.033(3) 0.029(3) 0.013(3) 0.008(3) 0.002(3) C8 0.026(3) 0.039(3) 0.032(3) 0.023(3) 0.011(3) 0.007(3) C9 0.031(3) 0.036(3) 0.045(4) 0.019(3) 0.019(3) 0.006(3) C10 0.019(3) 0.037(3) 0.029(3) 0.016(3) 0.009(2) 0.006(2) C11 0.024(3) 0.031(3) 0.032(3) 0.005(3) 0.008(3) 0.000(2) C12 0.018(3) 0.044(4) 0.040(4) 0.007(3) 0.011(3) -0.003(3) C13 0.025(3) 0.057(5) 0.076(5) 0.020(4) 0.023(4) 0.014(3) C14 0.036(4) 0.036(4) 0.065(5) 0.008(3) 0.025(4) 0.009(3) C15 0.042(4) 0.040(4) 0.029(4) 0.004(3) 0.018(3) -0.002(3) C16 0.021(3) 0.032(3) 0.032(3) 0.011(3) 0.007(3) 0.001(2) C17 0.023(3) 0.039(3) 0.038(3) 0.016(3) 0.013(3) 0.008(3) C18 0.020(3) 0.031(3) 0.029(3) 0.012(3) 0.009(2) 0.003(2) C19 0.029(3) 0.034(3) 0.034(3) 0.007(3) 0.012(3) 0.000(3) C20 0.021(3) 0.054(4) 0.040(4) 0.005(3) 0.012(3) -0.004(3) C21 0.021(3) 0.063(5) 0.073(5) 0.015(4) 0.017(3) 0.018(3) C22 0.029(3) 0.040(4) 0.067(5) 0.013(4) 0.012(3) 0.011(3) C23 0.0316(18) 0.0337(18) 0.060(2) 0.0130(18) 0.0093(17) 0.0022(16) C24 0.024(3) 0.030(3) 0.039(4) 0.015(3) 0.004(3) 0.005(2) C25 0.023(3) 0.031(3) 0.032(3) 0.013(3) 0.004(2) 0.000(2) C26 0.019(3) 0.028(3) 0.035(3) 0.016(3) 0.009(2) 0.005(2) C27 0.024(3) 0.032(3) 0.033(3) 0.013(3) 0.011(3) 0.003(2) C28 0.018(3) 0.041(4) 0.046(4) 0.006(3) 0.014(3) 0.000(3) C29 0.015(3) 0.065(5) 0.048(4) 0.010(4) -0.003(3) -0.003(3) C30 0.023(3) 0.063(4) 0.033(4) 0.013(3) -0.001(3) 0.001(3) C31 0.030(3) 0.026(3) 0.031(3) 0.009(3) 0.007(3) -0.003(3) C32 0.020(3) 0.044(4) 0.035(4) 0.025(3) 0.010(3) 0.006(3) C33 0.072(5) 0.057(4) 0.048(4) 0.033(4) 0.036(4) 0.043(4) C34 0.093(6) 0.062(5) 0.054(5) 0.042(4) 0.036(4) 0.052(5) C35 0.065(5) 0.032(3) 0.034(4) 0.017(3) 0.017(3) 0.013(3) C36 0.062(5) 0.053(4) 0.031(4) 0.018(3) 0.022(3) 0.027(4) C37 0.055(4) 0.055(4) 0.040(4) 0.030(3) 0.020(3) 0.030(4) C38 0.089(3) 0.123(3) 0.054(2) 0.048(2) 0.031(2) 0.035(3) C39 0.097(3) 0.123(3) 0.053(2) 0.047(2) 0.032(2) 0.035(3) C40 0.104(3) 0.110(3) 0.052(2) 0.046(2) 0.029(2) 0.037(3) C41 0.097(3) 0.113(3) 0.053(2) 0.049(2) 0.022(2) 0.036(3) C42 0.088(3) 0.112(3) 0.054(2) 0.051(2) 0.024(2) 0.035(3) C43 0.110(4) 0.090(3) 0.051(3) 0.048(3) 0.033(3) 0.041(3) C44 0.112(3) 0.100(3) 0.053(2) 0.043(2) 0.031(2) 0.040(3) C45 0.088(2) 0.0599(19) 0.065(2) 0.0376(16) -0.0079(17) -0.0191(17) C46 0.090(2) 0.0611(18) 0.0686(19) 0.0362(16) -0.0077(17) -0.0207(17) C47 0.092(2) 0.0650(17) 0.0721(19) 0.0345(15) -0.0113(16) -0.0208(16) C48 0.092(2) 0.0673(18) 0.0699(19) 0.0346(16) -0.0145(17) -0.0197(17) C49 0.090(2) 0.0653(19) 0.066(2) 0.0361(17) -0.0139(17) -0.0182(17) C50 0.082(2) 0.0600(19) 0.067(2) 0.0373(16) -0.0118(17) -0.0173(17) C51 0.086(2) 0.0611(18) 0.070(2) 0.0362(16) -0.0119(17) -0.0192(17) C52 0.089(2) 0.0645(17) 0.0728(19) 0.0340(16) -0.0147(16) -0.0194(16) C53 0.088(2) 0.0664(18) 0.071(2) 0.0336(16) -0.0172(17) -0.0179(17) C54 0.084(2) 0.0649(19) 0.067(2) 0.0355(17) -0.0167(17) -0.0164(17) C55 0.092(2) 0.0662(17) 0.0757(19) 0.0325(16) -0.0115(17) -0.0208(16) C56 0.091(2) 0.0660(17) 0.0758(19) 0.0321(16) -0.0132(17) -0.0201(16) C57 0.070(5) 0.058(5) 0.045(4) 0.026(4) 0.030(4) 0.039(4) C58 0.092(6) 0.056(5) 0.050(5) 0.034(4) 0.030(4) 0.036(4) C59 0.066(5) 0.031(3) 0.031(4) 0.015(3) 0.011(3) 0.000(3) C60 0.077(5) 0.060(5) 0.034(4) 0.015(4) 0.027(4) 0.030(4) C61 0.067(5) 0.058(4) 0.032(4) 0.024(3) 0.022(3) 0.033(4) C62 0.059(5) 0.089(6) 0.042(4) 0.030(4) 0.025(4) 0.011(4) C63 0.087(7) 0.088(6) 0.049(5) 0.032(5) 0.039(5) 0.018(5) C64 0.112(8) 0.048(4) 0.032(4) 0.017(4) 0.022(5) 0.013(5) C65 0.085(6) 0.061(5) 0.033(4) 0.023(4) 0.010(4) 0.022(4) C66 0.051(4) 0.054(4) 0.035(4) 0.022(3) 0.005(3) 0.008(3) C67 0.128(8) 0.053(5) 0.040(4) 0.025(4) 0.030(5) 0.016(5) C68 0.168(10) 0.061(5) 0.038(5) 0.025(4) 0.043(6) 0.032(6) C69 0.082(3) 0.098(3) 0.062(3) 0.027(3) -0.001(2) 0.018(3) C70 0.087(3) 0.099(3) 0.063(3) 0.029(3) 0.001(2) 0.015(3) C71 0.091(3) 0.097(3) 0.066(3) 0.029(2) -0.002(2) 0.019(3) C72 0.084(3) 0.096(3) 0.064(3) 0.027(3) -0.001(2) 0.021(3) C73 0.080(3) 0.096(3) 0.062(3) 0.028(3) -0.001(2) 0.018(3) C74 0.102(4) 0.098(3) 0.071(3) 0.031(3) -0.004(3) 0.017(3) N1 0.038(3) 0.037(3) 0.030(3) 0.018(2) 0.013(2) 0.011(2) N2 0.082(3) 0.108(3) 0.051(2) 0.053(2) 0.029(2) 0.037(3) N3 0.086(2) 0.0609(19) 0.063(2) 0.0375(16) -0.0100(17) -0.0178(17) N4 0.080(2) 0.0607(19) 0.065(2) 0.0369(16) -0.0131(17) -0.0158(17) N5 0.040(3) 0.036(3) 0.028(3) 0.015(2) 0.012(2) 0.012(2) N6 0.052(3) 0.045(3) 0.029(3) 0.017(3) 0.011(3) 0.007(3) N7 0.081(3) 0.095(3) 0.062(3) 0.028(2) -0.003(2) 0.019(3) O1 0.025(2) 0.045(2) 0.029(2) 0.014(2) 0.0109(18) -0.0008(19) O1W 0.056(3) 0.042(3) 0.037(3) 0.016(2) -0.004(2) 0.003(2) O2W 0.042(3) 0.044(3) 0.031(2) 0.013(2) 0.003(2) 0.006(2) O2 0.045(3) 0.066(3) 0.024(3) 0.005(2) 0.010(2) -0.002(2) O3 0.024(2) 0.032(2) 0.043(2) 0.0150(19) 0.0073(18) 0.0114(18) O3W 0.178(9) 0.123(7) 0.201(10) 0.085(7) 0.005(8) 0.039(7) O4 0.046(3) 0.056(3) 0.039(3) 0.004(2) -0.010(2) 0.022(2) O4W 0.209(12) 0.131(9) 0.263(14) 0.012(8) 0.116(11) 0.077(8) O5 0.047(3) 0.032(2) 0.047(3) 0.015(2) 0.005(2) -0.003(2) O5W 0.178(19) 0.107(13) 0.128(15) 0.042(11) 0.061(14) 0.033(13) O6 0.021(2) 0.056(3) 0.091(4) 0.007(3) 0.010(3) 0.000(2) O6W 0.28(3) 0.18(2) 0.138(19) 0.055(16) 0.056(19) 0.05(2) O7 0.039(3) 0.064(3) 0.044(3) 0.029(2) 0.010(2) 0.025(2) O7W 0.132(16) 0.105(14) 0.24(2) 0.007(14) -0.051(15) -0.004(12) O8 0.039(2) 0.047(3) 0.045(3) 0.027(2) 0.025(2) 0.019(2) O9 0.023(2) 0.061(3) 0.059(3) -0.005(3) 0.020(2) -0.008(2) O10 0.0337(18) 0.0324(17) 0.059(2) 0.0141(17) 0.0084(17) 0.0015(16) O11 0.0297(19) 0.043(2) 0.076(3) 0.003(2) 0.0049(19) 0.0040(18) O12 0.036(2) 0.044(3) 0.050(3) 0.025(2) 0.025(2) 0.019(2) O13 0.052(3) 0.085(4) 0.068(4) 0.050(3) 0.009(3) 0.029(3) O14 0.034(2) 0.047(3) 0.033(2) 0.016(2) 0.014(2) -0.004(2) O15 0.060(3) 0.060(3) 0.025(3) 0.008(2) 0.009(2) -0.011(3) O16 0.024(2) 0.040(2) 0.045(3) 0.018(2) 0.0056(19) 0.0127(19) O17 0.031(2) 0.055(3) 0.039(3) 0.004(2) -0.004(2) 0.013(2) O18 0.023(2) 0.071(3) 0.049(3) -0.010(3) 0.016(2) -0.018(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 Zn1 O3 1.928(4) . ? Zn1 O8 2.002(4) 1_455 ? Zn1 N3 2.045(6) . ? Zn1 N1 2.069(4) . ? Zn1 C16 2.574(6) 1_455 ? Zn2 O16 1.919(4) 1_655 ? Zn2 O12 1.964(4) . ? Zn2 N4 2.035(6) 2_855 ? Zn2 N5 2.056(5) . ? Zn3 O14 1.948(4) 1_765 ? Zn3 O5 1.985(4) . ? Zn3 O1W 2.020(5) . ? Zn3 N6 2.027(5) 1_666 ? Zn4 O1 1.959(4) . ? Zn4 O10 1.982(4) . ? Zn4 O2W 2.012(4) . ? Zn4 N2 2.027(6) 1_556 ? C1 C2 1.396(7) . ? C1 C6 1.404(8) . ? C1 C7 1.486(7) . ? C2 C3 1.405(7) . ? C2 C8 1.505(8) . ? C3 C4 1.369(8) . ? C3 H3A 0.9300 . ? C4 C5 1.367(9) . ? C4 O9 1.389(7) . ? C5 C6 1.380(9) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 O2 1.228(7) . ? C7 O1 1.272(7) . ? C8 O4 1.225(7) . ? C8 O3 1.263(7) . ? C9 C10 1.367(8) . ? C9 C14 1.409(8) . ? C9 C15 1.500(8) . ? C10 C11 1.384(7) . ? C10 C16 1.508(7) . ? C11 C12 1.371(8) . ? C11 H11A 0.9300 . ? C12 O9 1.377(7) . ? C12 C13 1.382(9) . ? C13 C14 1.374(9) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O6 1.221(8) . ? C15 O5 1.289(8) . ? C16 O7 1.243(7) . ? C16 O8 1.265(6) . ? C16 Zn1 2.574(6) 1_655 ? C17 C18 1.363(8) . ? C17 C22 1.403(8) . ? C17 C23 1.489(8) . ? C18 C19 1.397(7) . ? C18 C24 1.514(7) . ? C19 C20 1.363(9) . ? C19 H19A 0.9300 . ? C20 C21 1.381(9) . ? C20 O18 1.385(7) . ? C21 C22 1.375(9) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 O11 1.237(8) . ? C23 O10 1.265(7) . ? C24 O13 1.236(7) . ? C24 O12 1.253(7) . ? C25 C26 1.399(8) . ? C25 C30 1.406(8) . ? C25 C31 1.488(8) . ? C26 C27 1.398(7) . ? C26 C32 1.497(8) . ? C27 C28 1.379(8) . ? C27 H27A 0.9300 . ? C28 C29 1.374(9) . ? C28 O18 1.379(7) . ? C29 C30 1.388(9) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 O15 1.222(7) . ? C31 O14 1.274(7) . ? C32 O17 1.223(7) . ? C32 O16 1.275(7) . ? C33 N1 1.353(8) . ? C33 C34 1.367(9) . ? C33 H33A 0.9300 . ? C34 C35 1.379(9) . ? C34 H34A 0.9300 . ? C35 C36 1.364(9) . ? C35 C43 1.502(9) . ? C36 C37 1.384(8) . ? C36 H36A 0.9300 . ? C37 N1 1.319(8) . ? C37 H37A 0.9300 . ? C38 N2 1.305(10) . ? C38 C39 1.404(11) . ? C38 H38A 0.9300 . ? C39 C40 1.304(13) . ? C39 H39A 0.9300 . ? C40 C41 1.332(12) . ? C40 C44 1.507(11) . ? C41 C42 1.388(10) . ? C41 H41A 0.9300 . ? C42 N2 1.319(11) . ? C42 H42A 0.9300 . ? C43 C44 1.444(12) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 N3 1.320(9) . ? C45 C46 1.379(10) . ? C45 H45A 0.9300 . ? C46 C47 1.320(11) . ? C46 H46A 0.9300 . ? C47 C48 1.427(11) . ? C47 C55 1.609(10) . ? C48 C49 1.364(11) . ? C48 H48A 0.9300 . ? C49 N3 1.306(10) . ? C49 H49A 0.9300 . ? C50 N4 1.310(9) . ? C50 C51 1.380(10) . ? C50 H50A 0.9300 . ? C51 C52 1.331(11) . ? C51 H51A 0.9300 . ? C52 C53 1.447(11) . ? C52 C56 1.600(10) . ? C53 C54 1.349(11) . ? C53 H53A 0.9300 . ? C54 N4 1.326(10) . ? C54 H54A 0.9300 . ? C55 C56 1.416(14) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 N5 1.330(8) . ? C57 C58 1.364(9) . ? C57 H57A 0.9300 . ? C58 C59 1.391(10) . ? C58 H58A 0.9300 . ? C59 C60 1.369(10) . ? C59 C67 1.504(9) . ? C60 C61 1.394(9) . ? C60 H60A 0.9300 . ? C61 N5 1.327(8) . ? C61 H61A 0.9300 . ? C62 N6 1.348(9) . ? C62 C63 1.373(10) . ? C62 H62A 0.9300 . ? C63 C64 1.369(12) . ? C63 H63A 0.9300 . ? C64 C65 1.378(11) . ? C64 C68 1.528(10) . ? C65 C66 1.365(9) . ? C65 H65A 0.9300 . ? C66 N6 1.325(9) . ? C66 H66A 0.9300 . ? C67 C68 1.446(11) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C69 N7 1.349(12) . ? C69 C70 1.385(13) . ? C69 H69A 0.9300 . ? C70 C71 1.419(13) . ? C70 H70A 0.9300 . ? C71 C72 1.387(13) . ? C71 C74 1.471(14) . ? C72 C73 1.362(12) . ? C72 H72A 0.9300 . ? C73 N7 1.352(11) . ? C73 H73A 0.9300 . ? C74 C74 1.109(17) 2_886 ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? N2 Zn4 2.027(6) 1_554 ? N4 Zn2 2.035(6) 2_855 ? N6 Zn3 2.027(5) 1_444 ? O1W H1WA 0.8498 . ? O1W H1WB 0.8498 . ? O2W H2WA 0.8503 . ? O2W H2WB 0.8499 . ? O8 Zn1 2.002(4) 1_655 ? O14 Zn3 1.948(4) 1_345 ? O16 Zn2 1.919(4) 1_455 ? 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 O3 Zn1 O8 124.19(17) . 1_455 ? O3 Zn1 N3 118.9(2) . . ? O8 Zn1 N3 102.0(3) 1_455 . ? O3 Zn1 N1 109.67(18) . . ? O8 Zn1 N1 96.54(18) 1_455 . ? N3 Zn1 N1 101.3(2) . . ? O3 Zn1 C16 108.72(18) . 1_455 ? O8 Zn1 C16 28.78(17) 1_455 1_455 ? N3 Zn1 C16 92.7(3) . 1_455 ? N1 Zn1 C16 125.26(19) . 1_455 ? O16 Zn2 O12 121.42(18) 1_655 . ? O16 Zn2 N4 116.3(2) 1_655 2_855 ? O12 Zn2 N4 103.5(3) . 2_855 ? O16 Zn2 N5 110.58(19) 1_655 . ? O12 Zn2 N5 97.69(18) . . ? N4 Zn2 N5 104.7(2) 2_855 . ? O14 Zn3 O5 114.42(18) 1_765 . ? O14 Zn3 O1W 103.68(18) 1_765 . ? O5 Zn3 O1W 96.25(19) . . ? O14 Zn3 N6 134.1(2) 1_765 1_666 ? O5 Zn3 N6 102.7(2) . 1_666 ? O1W Zn3 N6 97.8(2) . 1_666 ? O1 Zn4 O10 116.14(18) . . ? O1 Zn4 O2W 108.60(17) . . ? O10 Zn4 O2W 94.66(18) . . ? O1 Zn4 N2 127.1(2) . 1_556 ? O10 Zn4 N2 104.7(3) . 1_556 ? O2W Zn4 N2 99.6(2) . 1_556 ? C2 C1 C6 118.0(5) . . ? C2 C1 C7 123.3(5) . . ? C6 C1 C7 118.4(5) . . ? C1 C2 C3 120.2(5) . . ? C1 C2 C8 123.4(5) . . ? C3 C2 C8 116.4(5) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C5 C4 C3 122.0(5) . . ? C5 C4 O9 120.9(6) . . ? C3 C4 O9 117.0(6) . . ? C4 C5 C6 119.0(6) . . ? C4 C5 H5A 120.5 . . ? C6 C5 H5A 120.5 . . ? C5 C6 C1 121.5(6) . . ? C5 C6 H6A 119.3 . . ? C1 C6 H6A 119.3 . . ? O2 C7 O1 122.2(5) . . ? O2 C7 C1 120.3(5) . . ? O1 C7 C1 117.4(5) . . ? O4 C8 O3 125.1(5) . . ? O4 C8 C2 119.2(5) . . ? O3 C8 C2 115.5(5) . . ? C10 C9 C14 118.1(5) . . ? C10 C9 C15 121.4(5) . . ? C14 C9 C15 120.4(6) . . ? C9 C10 C11 121.0(5) . . ? C9 C10 C16 123.0(5) . . ? C11 C10 C16 116.0(5) . . ? C12 C11 C10 120.3(5) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 O9 116.9(5) . . ? C11 C12 C13 120.2(5) . . ? O9 C12 C13 122.8(5) . . ? C14 C13 C12 119.2(6) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C9 121.3(6) . . ? C13 C14 H14A 119.4 . . ? C9 C14 H14A 119.4 . . ? O6 C15 O5 122.2(6) . . ? O6 C15 C9 120.4(6) . . ? O5 C15 C9 117.5(6) . . ? O7 C16 O8 122.1(5) . . ? O7 C16 C10 120.4(5) . . ? O8 C16 C10 117.0(5) . . ? O7 C16 Zn1 72.8(3) . 1_655 ? O8 C16 Zn1 49.7(3) . 1_655 ? C10 C16 Zn1 161.6(4) . 1_655 ? C18 C17 C22 118.6(5) . . ? C18 C17 C23 121.6(5) . . ? C22 C17 C23 119.5(6) . . ? C17 C18 C19 120.6(5) . . ? C17 C18 C24 123.7(5) . . ? C19 C18 C24 115.5(5) . . ? C20 C19 C18 120.1(6) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C21 120.4(6) . . ? C19 C20 O18 118.4(6) . . ? C21 C20 O18 120.9(6) . . ? C22 C21 C20 119.4(6) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C17 121.0(6) . . ? C21 C22 H22A 119.5 . . ? C17 C22 H22A 119.5 . . ? O11 C23 O10 121.2(6) . . ? O11 C23 C17 120.1(6) . . ? O10 C23 C17 118.7(6) . . ? O13 C24 O12 123.8(6) . . ? O13 C24 C18 119.2(5) . . ? O12 C24 C18 116.2(5) . . ? C26 C25 C30 117.6(5) . . ? C26 C25 C31 122.6(5) . . ? C30 C25 C31 119.7(5) . . ? C27 C26 C25 120.3(5) . . ? C27 C26 C32 114.9(5) . . ? C25 C26 C32 124.6(5) . . ? C28 C27 C26 120.2(6) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C29 C28 C27 120.8(5) . . ? C29 C28 O18 123.6(6) . . ? C27 C28 O18 115.5(6) . . ? C28 C29 C30 119.1(6) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? C29 C30 C25 121.8(6) . . ? C29 C30 H30A 119.1 . . ? C25 C30 H30A 119.1 . . ? O15 C31 O14 122.6(5) . . ? O15 C31 C25 120.8(5) . . ? O14 C31 C25 116.6(5) . . ? O17 C32 O16 125.2(5) . . ? O17 C32 C26 119.4(5) . . ? O16 C32 C26 115.1(5) . . ? N1 C33 C34 122.1(6) . . ? N1 C33 H33A 118.9 . . ? C34 C33 H33A 118.9 . . ? C33 C34 C35 120.6(6) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 116.6(6) . . ? C36 C35 C43 121.1(6) . . ? C34 C35 C43 122.2(6) . . ? C35 C36 C37 120.6(6) . . ? C35 C36 H36A 119.7 . . ? C37 C36 H36A 119.7 . . ? N1 C37 C36 122.5(6) . . ? N1 C37 H37A 118.8 . . ? C36 C37 H37A 118.8 . . ? N2 C38 C39 123.7(9) . . ? N2 C38 H38A 118.1 . . ? C39 C38 H38A 118.1 . . ? C40 C39 C38 121.0(9) . . ? C40 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C39 C40 C41 117.1(8) . . ? C39 C40 C44 119.3(9) . . ? C41 C40 C44 123.6(9) . . ? C40 C41 C42 119.7(9) . . ? C40 C41 H41A 120.1 . . ? C42 C41 H41A 120.1 . . ? N2 C42 C41 124.7(9) . . ? N2 C42 H42A 117.7 . . ? C41 C42 H42A 117.7 . . ? C44 C43 C35 115.8(7) . . ? C44 C43 H43A 108.3 . . ? C35 C43 H43A 108.3 . . ? C44 C43 H43B 108.3 . . ? C35 C43 H43B 108.3 . . ? H43A C43 H43B 107.4 . . ? C43 C44 C40 112.8(8) . . ? C43 C44 H44A 109.0 . . ? C40 C44 H44A 109.0 . . ? C43 C44 H44B 109.0 . . ? C40 C44 H44B 109.0 . . ? H44A C44 H44B 107.8 . . ? N3 C45 C46 122.9(8) . . ? N3 C45 H45A 118.6 . . ? C46 C45 H45A 118.6 . . ? C47 C46 C45 121.5(8) . . ? C47 C46 H46A 119.3 . . ? C45 C46 H46A 119.3 . . ? C46 C47 C48 115.6(7) . . ? C46 C47 C55 122.2(8) . . ? C48 C47 C55 119.7(8) . . ? C49 C48 C47 119.4(8) . . ? C49 C48 H48A 120.3 . . ? C47 C48 H48A 120.3 . . ? N3 C49 C48 123.3(8) . . ? N3 C49 H49A 118.4 . . ? C48 C49 H49A 118.4 . . ? N4 C50 C51 123.4(8) . . ? N4 C50 H50A 118.3 . . ? C51 C50 H50A 118.3 . . ? C52 C51 C50 120.1(8) . . ? C52 C51 H51A 120.0 . . ? C50 C51 H51A 120.0 . . ? C51 C52 C53 116.5(7) . . ? C51 C52 C56 122.4(8) . . ? C53 C52 C56 119.2(8) . . ? C54 C53 C52 118.9(8) . . ? C54 C53 H53A 120.5 . . ? C52 C53 H53A 120.5 . . ? N4 C54 C53 122.7(8) . . ? N4 C54 H54A 118.6 . . ? C53 C54 H54A 118.6 . . ? C56 C55 C47 99.6(8) . . ? C56 C55 H55A 111.9 . . ? C47 C55 H55A 111.9 . . ? C56 C55 H55B 111.9 . . ? C47 C55 H55B 111.9 . . ? H55A C55 H55B 109.6 . . ? C55 C56 C52 100.3(8) . . ? C55 C56 H56A 111.7 . . ? C52 C56 H56A 111.7 . . ? C55 C56 H56B 111.7 . . ? C52 C56 H56B 111.7 . . ? H56A C56 H56B 109.5 . . ? N5 C57 C58 123.3(6) . . ? N5 C57 H57A 118.3 . . ? C58 C57 H57A 118.3 . . ? C57 C58 C59 119.9(7) . . ? C57 C58 H58A 120.0 . . ? C59 C58 H58A 120.0 . . ? C60 C59 C58 116.9(6) . . ? C60 C59 C67 121.1(7) . . ? C58 C59 C67 122.0(7) . . ? C59 C60 C61 119.7(6) . . ? C59 C60 H60A 120.2 . . ? C61 C60 H60A 120.2 . . ? N5 C61 C60 122.7(6) . . ? N5 C61 H61A 118.6 . . ? C60 C61 H61A 118.6 . . ? N6 C62 C63 120.7(8) . . ? N6 C62 H62A 119.7 . . ? C63 C62 H62A 119.7 . . ? C64 C63 C62 121.1(8) . . ? C64 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? C63 C64 C65 117.3(7) . . ? C63 C64 C68 122.4(9) . . ? C65 C64 C68 120.3(9) . . ? C66 C65 C64 119.5(8) . . ? C66 C65 H65A 120.2 . . ? C64 C65 H65A 120.2 . . ? N6 C66 C65 123.0(7) . . ? N6 C66 H66A 118.5 . . ? C65 C66 H66A 118.5 . . ? C68 C67 C59 114.8(6) . . ? C68 C67 H67A 108.6 . . ? C59 C67 H67A 108.6 . . ? C68 C67 H67B 108.6 . . ? C59 C67 H67B 108.6 . . ? H67A C67 H67B 107.5 . . ? C67 C68 C64 113.0(7) . . ? C67 C68 H68A 109.0 . . ? C64 C68 H68A 109.0 . . ? C67 C68 H68B 109.0 . . ? C64 C68 H68B 109.0 . . ? H68A C68 H68B 107.8 . . ? N7 C69 C70 124.5(10) . . ? N7 C69 H69A 117.7 . . ? C70 C69 H69A 117.7 . . ? C69 C70 C71 119.0(10) . . ? C69 C70 H70A 120.5 . . ? C71 C70 H70A 120.5 . . ? C72 C71 C70 116.4(10) . . ? C72 C71 C74 116.4(10) . . ? C70 C71 C74 127.2(10) . . ? C73 C72 C71 119.7(11) . . ? C73 C72 H72A 120.1 . . ? C71 C72 H72A 120.1 . . ? N7 C73 C72 125.7(10) . . ? N7 C73 H73A 117.1 . . ? C72 C73 H73A 117.1 . . ? C74 C74 C71 136.1(16) 2_886 . ? C74 C74 H74A 103.1 2_886 . ? C71 C74 H74A 103.1 . . ? C74 C74 H74B 103.1 2_886 . ? C71 C74 H74B 103.1 . . ? H74A C74 H74B 105.1 . . ? C37 N1 C33 117.5(5) . . ? C37 N1 Zn1 120.9(4) . . ? C33 N1 Zn1 121.2(4) . . ? C38 N2 C42 113.7(7) . . ? C38 N2 Zn4 118.8(6) . 1_554 ? C42 N2 Zn4 127.4(6) . 1_554 ? C49 N3 C45 117.3(7) . . ? C49 N3 Zn1 122.5(5) . . ? C45 N3 Zn1 120.2(6) . . ? C50 N4 C54 118.0(7) . . ? C50 N4 Zn2 120.9(6) . 2_855 ? C54 N4 Zn2 120.4(5) . 2_855 ? C61 N5 C57 117.4(5) . . ? C61 N5 Zn2 121.4(4) . . ? C57 N5 Zn2 120.9(4) . . ? C66 N6 C62 118.3(6) . . ? C66 N6 Zn3 125.7(5) . 1_444 ? C62 N6 Zn3 115.9(5) . 1_444 ? C69 N7 C73 114.5(10) . . ? C7 O1 Zn4 108.2(3) . . ? Zn3 O1W H1WA 109.8 . . ? Zn3 O1W H1WB 132.0 . . ? H1WA O1W H1WB 103.3 . . ? Zn4 O2W H2WA 110.0 . . ? Zn4 O2W H2WB 116.9 . . ? H2WA O2W H2WB 116.3 . . ? C8 O3 Zn1 112.2(4) . . ? C15 O5 Zn3 106.3(4) . . ? C16 O8 Zn1 101.6(4) . 1_655 ? C12 O9 C4 118.4(5) . . ? C23 O10 Zn4 108.7(4) . . ? C24 O12 Zn2 112.4(4) . . ? C31 O14 Zn3 109.5(4) . 1_345 ? C32 O16 Zn2 112.3(4) . 1_455 ? C28 O18 C20 118.5(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.390 _refine_diff_density_min -1.567 _refine_diff_density_rms 0.107 #=========================END data_Compound-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C40 H30 N4 O9 Zn2), 8(O0.50), 2(O0.50), 4(O0.50)' _chemical_formula_sum 'C80 H60 N8 O27 Zn4 ' _chemical_formula_weight 1826.92 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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' 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 21.0705(5) _cell_length_b 18.4633(5) _cell_length_c 12.0995(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.461(3) _cell_angle_gamma 90.00 _cell_volume 4577.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4553 _cell_measurement_theta_min 2.4149 _cell_measurement_theta_max 28.7678 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.111 _exptl_absorpt_correction_T_min 0.97257 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details crystalclear _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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 8531 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4014 _reflns_number_gt 2939 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0991P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4014 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.207027(19) 0.02312(2) 0.89935(4) 0.0348(2) Uani 1 1 d . . . O1 O 0.14517(13) 0.05017(16) 1.3218(3) 0.0460(7) Uani 1 1 d . . . N1 N 0.29632(15) -0.0034(2) 0.9952(3) 0.0393(8) Uani 1 1 d . . . C1 C 0.12084(17) 0.1479(2) 1.1922(3) 0.0359(9) Uani 1 1 d . . . O1W O 0.1867(3) 0.2854(3) 0.8062(5) 0.136(2) Uani 1 1 d . . . O2 O 0.22443(13) 0.09441(18) 1.2518(2) 0.0526(8) Uani 1 1 d . . . N2 N 0.22698(16) 0.08432(18) 0.7736(3) 0.0424(8) Uani 1 1 d . . . C2 C 0.1256(2) 0.1706(2) 1.0854(4) 0.0463(10) Uani 1 1 d . . . O2W O 0.0583(8) 0.3135(12) 0.6720(9) 0.293(14) Uani 0.50 1 d P . . O3 O 0.15903(13) 0.06572(16) 1.0041(3) 0.0490(8) Uani 1 1 d . . . C3 C 0.0885(3) 0.2292(3) 1.0349(4) 0.0627(13) Uani 1 1 d . . . H3A H 0.0924 0.2457 0.9642 0.075 Uiso 1 1 calc R . . C4 C 0.0458(2) 0.2632(3) 1.0898(5) 0.0613(13) Uani 1 1 d . . . H4A H 0.0210 0.3023 1.0557 0.074 Uiso 1 1 calc R . . O4 O 0.2090(2) 0.1669(2) 0.9835(4) 0.0917(14) Uani 1 1 d . . . O5 O 0.0000 0.2781(2) 1.2500 0.0536(12) Uani 1 2 d S . . C5 C 0.04007(18) 0.2391(2) 1.1940(4) 0.0430(10) Uani 1 1 d . . . C6 C 0.07768(18) 0.1823(2) 1.2465(4) 0.0378(9) Uani 1 1 d . . . H6A H 0.0742 0.1668 1.3181 0.045 Uiso 1 1 calc R . . C7 C 0.16763(18) 0.0941(2) 1.2582(3) 0.0366(9) Uani 1 1 d . . . C8 C 0.1678(2) 0.1331(3) 1.0184(4) 0.0530(12) Uani 1 1 d . . . O3W O 0.0000 -0.0055(14) 1.2500 0.220(13) Uani 0.50 2 d SP . . C9 C 0.3168(2) 0.0287(3) 1.0946(4) 0.0619(14) Uani 1 1 d . . . H9A H 0.2875 0.0570 1.1225 0.074 Uiso 1 1 calc R . . O4W O -0.0367(8) 0.0241(16) 1.0341(16) 0.298(15) Uani 0.50 1 d P . . C10 C 0.3793(2) 0.0221(3) 1.1581(5) 0.080(2) Uani 1 1 d . . . H10A H 0.3918 0.0472 1.2263 0.096 Uiso 1 1 calc R . . C11 C 0.4240(2) -0.0212(3) 1.1228(4) 0.0557(13) Uani 1 1 d . . . C12 C 0.4031(2) -0.0562(3) 1.0230(4) 0.0516(11) Uani 1 1 d . . . H12A H 0.4312 -0.0868 0.9960 0.062 Uiso 1 1 calc R . . C13 C 0.33904(19) -0.0462(2) 0.9604(4) 0.0469(11) Uani 1 1 d . . . H13A H 0.3255 -0.0705 0.8916 0.056 Uiso 1 1 calc R . . C14 C 0.4940(2) -0.0272(3) 1.1882(5) 0.084(2) Uani 1 1 d . . . H14A H 0.5119 -0.0716 1.1650 0.101 Uiso 1 1 calc R . . H14B H 0.5182 0.0127 1.1658 0.101 Uiso 1 1 calc R . . C15 C 0.1864(2) 0.0865(2) 0.6709(4) 0.0496(11) Uani 1 1 d . . . H15A H 0.1486 0.0587 0.6580 0.059 Uiso 1 1 calc R . . C16 C 0.1980(3) 0.1279(3) 0.5834(4) 0.0591(13) Uani 1 1 d . . . H16A H 0.1677 0.1288 0.5139 0.071 Uiso 1 1 calc R . . C17 C 0.2550(3) 0.1683(2) 0.5989(4) 0.0556(12) Uani 1 1 d . . . C18 C 0.2957(3) 0.1662(3) 0.7038(5) 0.0701(15) Uani 1 1 d . . . H18A H 0.3340 0.1932 0.7184 0.084 Uiso 1 1 calc R . . C19 C 0.2810(2) 0.1246(3) 0.7885(4) 0.0598(13) Uani 1 1 d . . . H19A H 0.3100 0.1245 0.8594 0.072 Uiso 1 1 calc R . . C20 C 0.2685(3) 0.2158(3) 0.5047(5) 0.0712(15) Uani 1 1 d . . . H20A H 0.3148 0.2263 0.5198 0.085 Uiso 1 1 calc R . . H20B H 0.2565 0.1898 0.4331 0.085 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 0.0339(3) 0.0381(3) 0.0288(3) 0.0029(2) 0.00003(18) -0.00552(19) O1 0.0470(16) 0.0440(16) 0.0447(18) 0.0069(15) 0.0060(14) 0.0133(13) N1 0.0352(17) 0.0484(19) 0.0315(19) -0.0016(16) 0.0020(14) -0.0033(15) C1 0.0336(19) 0.030(2) 0.040(2) -0.0017(18) 0.0000(16) -0.0006(16) O1W 0.134(4) 0.108(4) 0.159(6) -0.001(4) 0.019(4) -0.035(3) O2 0.0371(15) 0.072(2) 0.0438(18) 0.0053(16) 0.0001(13) 0.0088(15) N2 0.0513(19) 0.0409(19) 0.0329(19) 0.0018(16) 0.0056(15) -0.0108(17) C2 0.056(3) 0.041(2) 0.038(3) -0.001(2) 0.004(2) 0.005(2) O2W 0.32(2) 0.47(3) 0.057(7) 0.004(12) -0.001(10) -0.32(2) O3 0.0519(17) 0.0477(19) 0.0469(19) -0.0021(15) 0.0107(14) 0.0061(14) C3 0.084(3) 0.055(3) 0.048(3) 0.014(2) 0.013(3) 0.023(3) C4 0.071(3) 0.044(3) 0.062(3) 0.012(2) 0.001(3) 0.019(2) O4 0.121(3) 0.071(3) 0.101(4) -0.009(2) 0.062(3) -0.017(2) O5 0.042(2) 0.031(2) 0.092(4) 0.000 0.024(2) 0.000 C5 0.034(2) 0.029(2) 0.063(3) -0.003(2) 0.0047(19) -0.0007(17) C6 0.036(2) 0.033(2) 0.041(2) 0.0020(19) 0.0035(17) -0.0018(17) C7 0.039(2) 0.037(2) 0.030(2) -0.0046(18) 0.0004(17) 0.0045(18) C8 0.064(3) 0.048(3) 0.047(3) 0.001(2) 0.013(2) 0.006(2) O3W 0.080(12) 0.195(19) 0.40(4) 0.000 0.092(18) 0.000 C9 0.045(2) 0.086(4) 0.048(3) -0.018(3) -0.005(2) 0.023(3) O4W 0.115(12) 0.62(5) 0.157(16) -0.05(2) 0.037(11) -0.095(17) C10 0.047(3) 0.124(5) 0.055(3) -0.046(3) -0.017(2) 0.019(3) C11 0.038(2) 0.074(3) 0.048(3) -0.019(3) -0.006(2) 0.008(2) C12 0.044(2) 0.061(3) 0.046(3) -0.009(2) 0.003(2) 0.007(2) C13 0.041(2) 0.056(3) 0.037(2) -0.009(2) -0.0048(19) 0.002(2) C14 0.039(3) 0.121(5) 0.078(4) -0.048(3) -0.016(3) 0.023(3) C15 0.060(3) 0.043(3) 0.039(2) 0.006(2) -0.001(2) -0.011(2) C16 0.089(4) 0.050(3) 0.031(2) 0.004(2) 0.002(2) -0.010(3) C17 0.081(3) 0.039(2) 0.052(3) 0.010(2) 0.026(3) -0.003(2) C18 0.079(3) 0.063(3) 0.069(4) 0.011(3) 0.019(3) -0.028(3) C19 0.066(3) 0.060(3) 0.047(3) 0.012(2) 0.000(2) -0.025(2) C20 0.112(4) 0.052(3) 0.062(3) 0.005(3) 0.046(3) 0.002(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 Zn1 O1 1.960(3) 6 ? Zn1 O3 1.961(3) . ? Zn1 N2 2.016(3) . ? Zn1 N1 2.027(3) . ? O1 C7 1.282(5) . ? O1 Zn1 1.960(3) 6_556 ? N1 C9 1.320(6) . ? N1 C13 1.338(5) . ? C1 C2 1.384(6) . ? C1 C6 1.393(5) . ? C1 C7 1.493(5) . ? O2 C7 1.217(5) . ? N2 C15 1.335(5) . ? N2 C19 1.337(5) . ? C2 C3 1.390(6) . ? C2 C8 1.505(6) . ? O3 C8 1.263(6) . ? C3 C4 1.386(7) . ? C3 H3A 0.9300 . ? C4 C5 1.369(6) . ? C4 H4A 0.9300 . ? O4 C8 1.223(6) . ? O5 C5 1.399(4) . ? O5 C5 1.399(4) 2_557 ? C5 C6 1.378(6) . ? C6 H6A 0.9300 . ? C9 C10 1.368(7) . ? C9 H9A 0.9300 . ? C10 C11 1.376(7) . ? C10 H10A 0.9300 . ? C11 C12 1.351(6) . ? C11 C14 1.507(6) . ? C12 C13 1.398(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C14 1.458(11) 2_657 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.372(6) . ? C15 H15A 0.9300 . ? C16 C17 1.390(7) . ? C16 H16A 0.9300 . ? C17 C18 1.357(7) . ? C17 C20 1.515(7) . ? C18 C19 1.373(7) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C20 1.475(10) 7_556 ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 101.60(13) 6 . ? O1 Zn1 N2 104.93(13) 6 . ? O3 Zn1 N2 119.51(14) . . ? O1 Zn1 N1 122.18(13) 6 . ? O3 Zn1 N1 106.06(13) . . ? N2 Zn1 N1 103.77(14) . . ? C7 O1 Zn1 115.3(2) . 6_556 ? C9 N1 C13 116.8(4) . . ? C9 N1 Zn1 118.4(3) . . ? C13 N1 Zn1 124.5(3) . . ? C2 C1 C6 120.0(4) . . ? C2 C1 C7 121.3(3) . . ? C6 C1 C7 118.2(4) . . ? C15 N2 C19 116.7(4) . . ? C15 N2 Zn1 121.3(3) . . ? C19 N2 Zn1 122.1(3) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 C8 122.9(4) . . ? C3 C2 C8 117.6(4) . . ? C8 O3 Zn1 113.7(3) . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C5 O5 C5 118.0(4) . 2_557 ? C4 C5 C6 120.5(4) . . ? C4 C5 O5 118.1(4) . . ? C6 C5 O5 121.1(4) . . ? C5 C6 C1 119.9(4) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? O2 C7 O1 123.1(4) . . ? O2 C7 C1 120.0(4) . . ? O1 C7 C1 116.9(3) . . ? O4 C8 O3 123.3(5) . . ? O4 C8 C2 120.5(4) . . ? O3 C8 C2 116.2(4) . . ? N1 C9 C10 122.6(4) . . ? N1 C9 H9A 118.7 . . ? C10 C9 H9A 118.7 . . ? C9 C10 C11 121.2(5) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C12 C11 C10 116.8(4) . . ? C12 C11 C14 120.6(4) . . ? C10 C11 C14 122.5(4) . . ? C11 C12 C13 119.5(4) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? N1 C13 C12 123.0(4) . . ? N1 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C14 C14 C11 117.0(6) 2_657 . ? C14 C14 H14A 108.1 2_657 . ? C11 C14 H14A 108.1 . . ? C14 C14 H14B 108.1 2_657 . ? C11 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? N2 C15 C16 123.0(4) . . ? N2 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C15 C16 C17 119.9(4) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 116.7(4) . . ? C18 C17 C20 122.1(5) . . ? C16 C17 C20 121.1(5) . . ? C17 C18 C19 120.7(5) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? N2 C19 C18 123.0(5) . . ? N2 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? C20 C20 C17 111.4(5) 7_556 . ? C20 C20 H20A 109.3 7_556 . ? C17 C20 H20A 109.3 . . ? C20 C20 H20B 109.3 7_556 . ? C17 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.091 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.105 #=========================END data_Compound-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H12 N O9 Zn2 ' _chemical_formula_sum 'C22 H12 N O9 Zn2 ' _chemical_formula_weight 565.11 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 monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc ' 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 27.8969(13) _cell_length_b 7.5757(2) _cell_length_c 21.3408(9) _cell_angle_alpha 90.00 _cell_angle_beta 118.087(6) _cell_angle_gamma 90.00 _cell_volume 3979.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4163 _cell_measurement_theta_min 2.4777 _cell_measurement_theta_max 28.8905 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 2.471 _exptl_absorpt_correction_T_min 0.68472 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details crystalclear _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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 7511 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3479 _reflns_number_gt 2487 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3479 _refine_ls_number_parameters 307 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.976 _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 0.262447(18) 0.25697(5) 0.41155(2) 0.02112(16) Uani 1 1 d . . . N1 N 0.31058(15) 0.2513(4) 0.15949(19) 0.0285(6) Uani 1 1 d U . . O1 O 0.22544(12) 0.3902(3) 0.31590(12) 0.0296(7) Uani 1 1 d . . . C1 C 0.15286(16) 0.3830(4) 0.20094(17) 0.0187(8) Uani 1 1 d . . . Zn2 Zn 0.23306(2) 0.25437(6) 0.13909(2) 0.02937(17) Uani 1 1 d . . . C2 C 0.13630(16) 0.4926(5) 0.14234(18) 0.0220(8) Uani 1 1 d . . . O2 O 0.23970(13) 0.2494(3) 0.23503(14) 0.0334(7) Uani 1 1 d . . . O3 O 0.21763(11) 0.5178(4) 0.12958(13) 0.0286(7) Uani 1 1 d . . . C3 C 0.08053(17) 0.5208(5) 0.0984(2) 0.0296(10) Uani 1 1 d . . . H3A H 0.0693 0.5967 0.0598 0.036 Uiso 1 1 calc R . . C4 C 0.04198(18) 0.4382(6) 0.1113(2) 0.0351(10) Uani 1 1 d . . . H4A H 0.0051 0.4553 0.0813 0.042 Uiso 1 1 calc R . . O4 O 0.16187(13) 0.7404(4) 0.09910(16) 0.0356(8) Uani 1 1 d . . . O5 O -0.18894(11) 0.1687(4) 0.10682(13) 0.0285(6) Uani 1 1 d . . . C5 C 0.05945(16) 0.3303(6) 0.16952(19) 0.0272(9) Uani 1 1 d . . . O6 O -0.19737(11) 0.3318(3) 0.01587(13) 0.0259(6) Uani 1 1 d . . . C6 C 0.11366(17) 0.3051(5) 0.21547(19) 0.0238(9) Uani 1 1 d . . . H6A H 0.1242 0.2366 0.2560 0.029 Uiso 1 1 calc R . . O7 O -0.21232(11) -0.0105(3) -0.04415(12) 0.0263(6) Uani 1 1 d . . . C7 C -0.12055(16) 0.1456(5) 0.07185(17) 0.0199(8) Uani 1 1 d . . . O8 O -0.15980(13) -0.1857(4) -0.06517(16) 0.0447(8) Uani 1 1 d . . . C8 C -0.07312(18) 0.2175(5) 0.1260(2) 0.0272(9) Uani 1 1 d . . . H8A H -0.0750 0.2950 0.1585 0.033 Uiso 1 1 calc R . . C9 C -0.02346(17) 0.1739(5) 0.13123(19) 0.0278(9) Uani 1 1 d . . . O9 O 0.02231(13) 0.2481(4) 0.18704(15) 0.0385(8) Uani 1 1 d . . . C10 C -0.01876(17) 0.0549(6) 0.0854(2) 0.0335(10) Uani 1 1 d . . . H10A H 0.0150 0.0270 0.0892 0.040 Uiso 1 1 calc R . . C11 C -0.06599(17) -0.0217(5) 0.0334(2) 0.0293(10) Uani 1 1 d . . . H11A H -0.0635 -0.1048 0.0030 0.035 Uiso 1 1 calc R . . C12 C -0.11646(16) 0.0223(5) 0.02568(17) 0.0218(8) Uani 1 1 d . . . C13 C 0.21056(16) 0.3408(5) 0.25342(18) 0.0213(8) Uani 1 1 d . . . C14 C 0.17396(16) 0.5894(5) 0.12282(17) 0.0224(9) Uani 1 1 d . . . C15 C -0.17358(16) 0.2173(5) 0.06327(18) 0.0209(9) Uani 1 1 d . . . C16 C -0.16594(17) -0.0617(5) -0.03098(18) 0.0229(9) Uani 1 1 d . . . C17 C 0.34769(18) 0.3113(6) 0.2212(2) 0.0361(7) Uani 1 1 d U . . H17A H 0.3363 0.3567 0.2525 0.043 Uiso 1 1 calc R . . C18 C 0.4023(2) 0.3104(7) 0.2420(3) 0.0435(8) Uani 1 1 d U . . H18A H 0.4268 0.3572 0.2858 0.052 Uiso 1 1 calc R . . C19 C 0.4211(2) 0.2394(6) 0.1976(3) 0.0440(8) Uani 1 1 d U . . C20 C 0.38201(18) 0.1782(6) 0.1332(2) 0.0375(7) Uani 1 1 d U . . H20A H 0.3923 0.1317 0.1010 0.045 Uiso 1 1 calc R . . C21 C 0.32811(18) 0.1846(6) 0.1156(2) 0.0319(7) Uani 1 1 d U . . H21A H 0.3027 0.1410 0.0717 0.038 Uiso 1 1 calc R . . C22 C 0.4795(2) 0.2343(8) 0.2170(3) 0.0646(11) Uani 1 1 d U . . H22A H 0.4843 0.1297 0.1944 0.078 Uiso 1 1 calc R . . H22B H 0.4856 0.3344 0.1934 0.078 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 0.0157(3) 0.0274(3) 0.0203(2) -0.00086(17) 0.0085(2) 0.00187(19) N1 0.0190(13) 0.0312(14) 0.0350(13) -0.0019(11) 0.0126(10) -0.0024(12) O1 0.0251(18) 0.0394(16) 0.0176(13) 0.0009(11) 0.0046(12) 0.0059(13) C1 0.016(2) 0.0214(19) 0.0209(18) -0.0044(14) 0.0109(16) -0.0046(15) Zn2 0.0170(3) 0.0457(3) 0.0257(3) -0.0103(2) 0.0103(2) -0.0052(2) C2 0.019(2) 0.025(2) 0.0209(18) -0.0016(15) 0.0085(16) -0.0032(16) O2 0.0270(19) 0.0467(18) 0.0269(15) 0.0036(12) 0.0131(14) 0.0118(14) O3 0.0205(17) 0.0366(16) 0.0311(14) -0.0020(12) 0.0141(13) -0.0063(13) C3 0.021(2) 0.038(2) 0.026(2) 0.0071(17) 0.0082(17) 0.0014(19) C4 0.016(2) 0.048(3) 0.034(2) 0.0014(19) 0.0047(19) -0.004(2) O4 0.0293(19) 0.0360(17) 0.0371(16) 0.0114(13) 0.0120(14) -0.0050(13) O5 0.0185(16) 0.0461(16) 0.0250(13) 0.0010(12) 0.0136(12) -0.0002(13) C5 0.017(2) 0.040(2) 0.029(2) -0.0094(18) 0.0138(18) -0.0127(19) O6 0.0213(17) 0.0294(14) 0.0233(14) -0.0025(12) 0.0076(12) -0.0031(12) C6 0.021(2) 0.028(2) 0.0221(19) 0.0002(15) 0.0101(17) -0.0033(17) O7 0.0152(17) 0.0279(14) 0.0278(14) 0.0024(11) 0.0035(12) -0.0053(12) C7 0.017(2) 0.023(2) 0.0210(18) 0.0017(15) 0.0101(16) -0.0022(16) O8 0.030(2) 0.0453(18) 0.0461(18) -0.0248(15) 0.0070(15) -0.0017(15) C8 0.023(2) 0.034(2) 0.024(2) -0.0035(16) 0.0110(18) -0.0061(18) C9 0.017(2) 0.039(2) 0.0219(19) 0.0060(17) 0.0045(17) -0.0081(18) O9 0.0195(17) 0.067(2) 0.0263(15) -0.0018(13) 0.0087(13) -0.0184(15) C10 0.017(2) 0.051(3) 0.035(2) -0.0014(19) 0.0136(19) 0.002(2) C11 0.024(3) 0.032(2) 0.031(2) -0.0066(17) 0.0123(19) -0.0002(18) C12 0.018(2) 0.023(2) 0.0226(18) 0.0016(15) 0.0081(16) -0.0011(16) C13 0.020(2) 0.023(2) 0.0234(19) 0.0012(15) 0.0130(17) -0.0040(17) C14 0.016(2) 0.032(2) 0.0147(17) -0.0007(15) 0.0027(16) -0.0079(17) C15 0.014(2) 0.027(2) 0.0167(18) -0.0084(15) 0.0031(16) -0.0078(16) C16 0.023(3) 0.020(2) 0.0191(18) 0.0017(15) 0.0048(17) -0.0028(17) C17 0.0220(14) 0.0437(16) 0.0379(14) -0.0057(13) 0.0103(12) -0.0007(14) C18 0.0223(14) 0.0571(17) 0.0420(15) -0.0033(14) 0.0075(12) -0.0018(15) C19 0.0219(14) 0.0634(17) 0.0447(14) 0.0035(13) 0.0141(11) -0.0006(14) C20 0.0227(14) 0.0499(17) 0.0422(14) 0.0015(13) 0.0171(12) 0.0008(14) C21 0.0216(14) 0.0376(15) 0.0372(14) -0.0009(12) 0.0144(12) -0.0011(14) C22 0.0242(16) 0.111(3) 0.053(2) 0.0029(19) 0.0134(15) 0.000(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 Zn1 O5 2.012(3) 2 ? Zn1 O1 2.066(2) . ? Zn1 O6 2.077(2) 8_556 ? Zn1 O7 2.110(3) 8_556 ? Zn1 O3 2.196(3) 4_545 ? Zn1 O4 2.231(3) 4_545 ? Zn1 C14 2.554(4) 4_545 ? N1 C17 1.315(5) . ? N1 C21 1.342(5) . ? N1 Zn2 1.995(4) . ? O1 C13 1.252(4) . ? C1 C2 1.387(5) . ? C1 C6 1.400(5) . ? C1 C13 1.500(5) . ? Zn2 O2 1.967(3) . ? Zn2 O8 1.975(3) 5 ? Zn2 O3 2.031(3) . ? C2 C3 1.404(5) . ? C2 C14 1.492(5) . ? O2 C13 1.263(5) . ? O3 C14 1.278(5) . ? O3 Zn1 2.196(3) 4 ? C3 C4 1.380(6) . ? C3 H3A 0.9300 . ? C4 C5 1.370(6) . ? C4 H4A 0.9300 . ? O4 C14 1.232(4) . ? O4 Zn1 2.231(3) 4 ? O5 C15 1.248(4) . ? O5 Zn1 2.012(3) 2 ? C5 C6 1.374(6) . ? C5 O9 1.402(5) . ? O6 C15 1.258(4) . ? O6 Zn1 2.077(2) 8_455 ? C6 H6A 0.9300 . ? O7 C16 1.249(5) . ? O7 Zn1 2.110(3) 8_455 ? C7 C8 1.394(5) . ? C7 C12 1.401(5) . ? C7 C15 1.504(5) . ? O8 C16 1.250(4) . ? O8 Zn2 1.975(3) 5 ? C8 C9 1.376(6) . ? C8 H8A 0.9300 . ? C9 C10 1.382(6) . ? C9 O9 1.390(5) . ? C10 C11 1.388(5) . ? C10 H10A 0.9300 . ? C11 C12 1.379(6) . ? C11 H11A 0.9300 . ? C12 C16 1.483(5) . ? C14 Zn1 2.554(4) 4 ? C17 C18 1.372(6) . ? C17 H17A 0.9300 . ? C18 C19 1.389(7) . ? C18 H18A 0.9300 . ? C19 C20 1.371(6) . ? C19 C22 1.480(7) . ? C20 C21 1.369(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C22 1.333(11) 2_655 ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O1 88.88(11) 2 . ? O5 Zn1 O6 95.02(11) 2 8_556 ? O1 Zn1 O6 169.63(10) . 8_556 ? O5 Zn1 O7 118.95(11) 2 8_556 ? O1 Zn1 O7 84.50(10) . 8_556 ? O6 Zn1 O7 85.21(10) 8_556 8_556 ? O5 Zn1 O3 94.27(11) 2 4_545 ? O1 Zn1 O3 96.37(9) . 4_545 ? O6 Zn1 O3 92.92(10) 8_556 4_545 ? O7 Zn1 O3 146.77(11) 8_556 4_545 ? O5 Zn1 O4 152.64(11) 2 4_545 ? O1 Zn1 O4 89.05(11) . 4_545 ? O6 Zn1 O4 91.83(11) 8_556 4_545 ? O7 Zn1 O4 87.98(10) 8_556 4_545 ? O3 Zn1 O4 58.88(10) 4_545 4_545 ? O5 Zn1 C14 124.12(12) 2 4_545 ? O1 Zn1 C14 92.90(11) . 4_545 ? O6 Zn1 C14 92.84(10) 8_556 4_545 ? O7 Zn1 C14 116.81(12) 8_556 4_545 ? O3 Zn1 C14 30.03(11) 4_545 4_545 ? O4 Zn1 C14 28.85(11) 4_545 4_545 ? C17 N1 C21 117.1(4) . . ? C17 N1 Zn2 118.4(3) . . ? C21 N1 Zn2 124.4(3) . . ? C13 O1 Zn1 131.8(2) . . ? C2 C1 C6 119.3(4) . . ? C2 C1 C13 125.9(3) . . ? C6 C1 C13 114.9(3) . . ? O2 Zn2 O8 112.40(14) . 5 ? O2 Zn2 N1 102.21(14) . . ? O8 Zn2 N1 141.18(14) 5 . ? O2 Zn2 O3 91.97(10) . . ? O8 Zn2 O3 95.05(12) 5 . ? N1 Zn2 O3 100.97(11) . . ? C1 C2 C3 119.1(4) . . ? C1 C2 C14 124.5(4) . . ? C3 C2 C14 116.3(3) . . ? C13 O2 Zn2 123.7(2) . . ? C14 O3 Zn2 125.0(3) . . ? C14 O3 Zn1 90.7(2) . 4 ? Zn2 O3 Zn1 140.26(14) . 4 ? C4 C3 C2 121.4(4) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C5 C4 C3 118.3(4) . . ? C5 C4 H4A 120.9 . . ? C3 C4 H4A 120.9 . . ? C14 O4 Zn1 90.3(3) . 4 ? C15 O5 Zn1 115.6(3) . 2 ? C4 C5 C6 122.1(4) . . ? C4 C5 O9 120.9(4) . . ? C6 C5 O9 116.8(4) . . ? C15 O6 Zn1 116.9(2) . 8_455 ? C5 C6 C1 119.7(4) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? C16 O7 Zn1 118.3(2) . 8_455 ? C8 C7 C12 118.9(4) . . ? C8 C7 C15 117.1(3) . . ? C12 C7 C15 123.8(3) . . ? C16 O8 Zn2 106.8(3) . 5 ? C9 C8 C7 120.0(4) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 121.8(4) . . ? C8 C9 O9 117.1(4) . . ? C10 C9 O9 121.0(4) . . ? C9 O9 C5 116.6(3) . . ? C9 C10 C11 117.9(4) . . ? C9 C10 H10A 121.1 . . ? C11 C10 H10A 121.1 . . ? C12 C11 C10 121.8(4) . . ? C12 C11 H11A 119.1 . . ? C10 C11 H11A 119.1 . . ? C11 C12 C7 119.6(3) . . ? C11 C12 C16 120.0(3) . . ? C7 C12 C16 120.4(4) . . ? O1 C13 O2 123.7(4) . . ? O1 C13 C1 115.6(3) . . ? O2 C13 C1 120.4(3) . . ? O4 C14 O3 120.2(4) . . ? O4 C14 C2 118.6(4) . . ? O3 C14 C2 121.3(3) . . ? O4 C14 Zn1 60.9(2) . 4 ? O3 C14 Zn1 59.29(19) . 4 ? C2 C14 Zn1 179.4(3) . 4 ? O5 C15 O6 124.5(4) . . ? O5 C15 C7 117.8(3) . . ? O6 C15 C7 117.6(3) . . ? O7 C16 O8 120.9(4) . . ? O7 C16 C12 121.2(3) . . ? O8 C16 C12 117.9(4) . . ? N1 C17 C18 123.5(4) . . ? N1 C17 H17A 118.2 . . ? C18 C17 H17A 118.2 . . ? C17 C18 C19 120.0(4) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C20 C19 C18 116.0(5) . . ? C20 C19 C22 121.5(5) . . ? C18 C19 C22 122.5(5) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? N1 C21 C20 122.4(4) . . ? N1 C21 H21A 118.8 . . ? C20 C21 H21A 118.8 . . ? C22 C22 C19 125.6(7) 2_655 . ? C22 C22 H22A 105.9 2_655 . ? C19 C22 H22A 105.9 . . ? C22 C22 H22B 105.9 2_655 . ? C19 C22 H22B 105.9 . . ? H22A C22 H22B 106.2 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.155 _refine_diff_density_min -1.254 _refine_diff_density_rms 0.080 #=========================END data_Compound-5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 N2 O11 Zn2 ' _chemical_formula_sum 'C28 H22 N2 O11 Zn2 ' _chemical_formula_weight 693.26 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 orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' _symmetry_space_group_name_Hall 'C 2c 2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.5741(8) _cell_length_b 11.4403(14) _cell_length_c 25.674(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2812.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2488 _cell_measurement_theta_min 2.3751 _cell_measurement_theta_max 28.3310 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 1.771 _exptl_absorpt_correction_T_min 0.92532 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details crystalclear _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 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count 0 _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 2996 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2180 _reflns_number_gt 1963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+28.2811P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(4) _refine_ls_number_reflns 2180 _refine_ls_number_parameters 200 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1366 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.193 _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 Zn1 Zn -0.84017(11) 1.0000 0.0000 0.0273(3) Uani 1 2 d S . . O1 O -1.2026(6) 0.9129(6) 0.0560(2) 0.0328(14) Uani 1 1 d . . . C1 C -1.0596(8) 0.8000(6) 0.1088(3) 0.0204(15) Uani 1 1 d . . . O1W O -0.6783(6) 0.8810(5) 0.0137(2) 0.0409(17) Uani 1 1 d D . . H1WA H -0.7081 0.8257 0.0307 0.061 Uiso 1 1 calc RD . . N1 N -0.8531(7) 0.9476(7) -0.0786(3) 0.0375(14) Uani 1 1 d U . . Zn2 Zn -1.28686(10) 1.0000 0.0000 0.0223(3) Uani 1 2 d S . . C2 C -1.1326(9) 0.8331(8) 0.1526(3) 0.032(2) Uani 1 1 d . . . H2A H -1.1991 0.8920 0.1496 0.038 Uiso 1 1 calc R . . O2 O -0.9931(5) 0.8630(5) 0.0243(2) 0.0260(12) Uani 1 1 d . . . C3 C -1.1115(11) 0.7831(9) 0.2002(3) 0.043(2) Uani 1 1 d . . . H3A H -1.1603 0.8091 0.2293 0.051 Uiso 1 1 calc R . . O3 O -0.9310(6) 0.5942(4) 0.03781(19) 0.0255(11) Uani 1 1 d . . . O4 O -0.7468(5) 0.6905(5) 0.0683(2) 0.0347(14) Uani 1 1 d . . . C4 C -1.0158(10) 0.6930(9) 0.2042(3) 0.038(2) Uani 1 1 d . . . C5 C -0.9411(11) 0.6548(8) 0.1614(3) 0.039(2) Uani 1 1 d . . . H5A H -0.8790 0.5927 0.1643 0.047 Uiso 1 1 calc R . . O5 O -1.0000 0.6268(8) 0.2500 0.051(3) Uani 1 2 d S . . C6 C -0.9610(8) 0.7122(7) 0.1131(3) 0.0252(18) Uani 1 1 d . . . C7 C -1.0853(8) 0.8635(6) 0.0586(3) 0.0184(15) Uani 1 1 d . . . C8 C -0.8718(8) 0.6656(6) 0.0693(3) 0.0209(16) Uani 1 1 d . . . C9 C -0.7791(8) 0.9996(12) -0.1157(3) 0.0451(15) Uani 1 1 d U . . H9A H -0.7091 1.0512 -0.1057 0.054 Uiso 1 1 calc R . . C13 C -0.9459(10) 0.8694(10) -0.0950(3) 0.0460(16) Uani 1 1 d U . . H13A H -0.9945 0.8257 -0.0705 0.055 Uiso 1 1 calc R . . C12 C -0.9730(10) 0.8507(11) -0.1466(4) 0.0513(17) Uani 1 1 d U . . H12A H -1.0422 0.7979 -0.1562 0.062 Uiso 1 1 calc R . . C11 C -0.9005(10) 0.9080(10) -0.1839(4) 0.0492(16) Uani 1 1 d U . . C10 C -0.8000(9) 0.9815(10) -0.1676(3) 0.0461(16) Uani 1 1 d U . . H10A H -0.7446 1.0202 -0.1918 0.055 Uiso 1 1 calc R . . C14 C -0.9288(11) 0.8898(11) -0.2418(4) 0.057(2) Uani 1 1 d U . . H14A H -0.8803 0.9507 -0.2609 0.069 Uiso 1 1 calc R . . H14B H -0.8876 0.8158 -0.2520 0.069 Uiso 1 1 calc R . . H1WB H -0.613(9) 0.863(5) -0.004(4) 0.10(5) 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 0.0196(6) 0.0399(7) 0.0225(6) -0.0033(8) 0.000 0.000 O1 0.025(3) 0.049(4) 0.025(3) 0.005(3) 0.002(2) 0.013(3) C1 0.021(3) 0.022(4) 0.017(3) 0.000(3) -0.004(3) -0.003(4) O1W 0.023(3) 0.044(3) 0.056(5) 0.008(3) 0.014(3) 0.003(3) N1 0.029(3) 0.058(3) 0.026(3) -0.001(3) 0.004(2) 0.002(3) Zn2 0.0158(5) 0.0297(6) 0.0215(6) -0.0017(7) 0.000 0.000 C2 0.034(4) 0.034(5) 0.028(4) -0.006(4) -0.002(4) 0.006(4) O2 0.027(3) 0.027(3) 0.024(3) -0.001(2) 0.003(2) 0.006(2) C3 0.054(6) 0.047(6) 0.027(5) -0.005(4) 0.009(4) 0.006(5) O3 0.027(3) 0.020(2) 0.029(3) -0.008(2) -0.006(3) 0.009(3) O4 0.015(3) 0.040(3) 0.048(4) 0.006(3) 0.000(3) -0.003(3) C4 0.061(6) 0.043(6) 0.010(4) 0.000(4) -0.003(4) -0.012(5) C5 0.043(5) 0.047(5) 0.029(4) -0.003(4) -0.008(4) 0.012(5) O5 0.096(8) 0.033(5) 0.024(4) 0.000 -0.010(5) 0.000 C6 0.017(4) 0.040(5) 0.019(4) -0.003(3) -0.005(3) -0.005(4) C7 0.027(4) 0.006(3) 0.022(3) 0.004(3) -0.002(3) 0.006(3) C8 0.025(4) 0.017(4) 0.021(4) 0.002(3) -0.006(3) 0.004(3) C9 0.042(3) 0.061(4) 0.032(3) 0.000(3) 0.007(2) -0.001(3) C13 0.034(3) 0.073(4) 0.031(3) -0.007(3) 0.004(3) -0.009(3) C12 0.040(3) 0.081(4) 0.033(3) -0.011(3) 0.004(3) -0.010(3) C11 0.040(3) 0.078(4) 0.029(3) -0.007(3) 0.006(2) 0.004(3) C10 0.044(3) 0.065(4) 0.030(3) 0.000(3) 0.010(3) 0.001(3) C14 0.047(4) 0.092(5) 0.033(3) -0.006(4) 0.002(3) 0.005(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 O1W 2.093(6) 4_575 ? Zn1 O1W 2.093(6) . ? Zn1 N1 2.108(7) 4_575 ? Zn1 N1 2.108(7) . ? Zn1 O2 2.234(6) . ? Zn1 O2 2.234(6) 4_575 ? O1 C7 1.259(9) . ? O1 Zn2 1.927(5) . ? C1 C2 1.377(11) . ? C1 C6 1.382(11) . ? C1 C7 1.500(10) . ? O1W H1WA 0.8200 . ? O1W H1WB 0.80(9) . ? N1 C9 1.328(11) . ? N1 C13 1.330(12) . ? Zn2 O1 1.927(5) 4_575 ? Zn2 O3 2.002(5) 8_465 ? Zn2 O3 2.002(5) 5_455 ? C2 C3 1.365(12) . ? C2 H2A 0.9300 . ? O2 C7 1.247(9) . ? C3 C4 1.383(14) . ? C3 H3A 0.9300 . ? O3 C8 1.281(9) . ? O3 Zn2 2.002(5) 5_545 ? O4 C8 1.230(9) . ? C4 C5 1.382(12) . ? C4 O5 1.406(10) . ? C5 C6 1.416(11) . ? C5 H5A 0.9300 . ? O5 C4 1.406(10) 3_355 ? C6 C8 1.510(10) . ? C9 C10 1.364(11) . ? C9 H9A 0.9300 . ? C13 C12 1.366(13) . ? C13 H13A 0.9300 . ? C12 C11 1.351(14) . ? C12 H12A 0.9300 . ? C11 C10 1.345(14) . ? C11 C14 1.526(12) . ? C10 H10A 0.9300 . ? C14 C14 1.43(2) 3_354 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Zn1 O1W 84.4(3) 4_575 . ? O1W Zn1 N1 91.1(3) 4_575 4_575 ? O1W Zn1 N1 93.9(3) . 4_575 ? O1W Zn1 N1 93.9(3) 4_575 . ? O1W Zn1 N1 91.1(3) . . ? N1 Zn1 N1 173.3(4) 4_575 . ? O1W Zn1 O2 171.4(2) 4_575 . ? O1W Zn1 O2 89.0(2) . . ? N1 Zn1 O2 83.9(2) 4_575 . ? N1 Zn1 O2 91.7(2) . . ? O1W Zn1 O2 89.0(2) 4_575 4_575 ? O1W Zn1 O2 171.4(2) . 4_575 ? N1 Zn1 O2 91.7(2) 4_575 4_575 ? N1 Zn1 O2 83.9(2) . 4_575 ? O2 Zn1 O2 98.1(3) . 4_575 ? C7 O1 Zn2 130.2(5) . . ? C2 C1 C6 118.8(7) . . ? C2 C1 C7 119.0(7) . . ? C6 C1 C7 122.1(7) . . ? Zn1 O1W H1WA 109.5 . . ? Zn1 O1W H1WB 131(6) . . ? H1WA O1W H1WB 111.8 . . ? C9 N1 C13 115.4(8) . . ? C9 N1 Zn1 121.8(7) . . ? C13 N1 Zn1 122.4(6) . . ? O1 Zn2 O1 130.5(3) . 4_575 ? O1 Zn2 O3 111.8(2) . 8_465 ? O1 Zn2 O3 101.8(2) 4_575 8_465 ? O1 Zn2 O3 101.8(2) . 5_455 ? O1 Zn2 O3 111.8(2) 4_575 5_455 ? O3 Zn2 O3 92.8(3) 8_465 5_455 ? C3 C2 C1 122.7(8) . . ? C3 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? C7 O2 Zn1 131.1(5) . . ? C2 C3 C4 118.5(8) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C8 O3 Zn2 110.1(5) . 5_545 ? C5 C4 C3 121.2(8) . . ? C5 C4 O5 116.0(9) . . ? C3 C4 O5 122.3(8) . . ? C4 C5 C6 118.7(8) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C4 O5 C4 114.8(10) 3_355 . ? C1 C6 C5 119.9(7) . . ? C1 C6 C8 125.7(7) . . ? C5 C6 C8 114.4(7) . . ? O2 C7 O1 126.6(6) . . ? O2 C7 C1 119.2(6) . . ? O1 C7 C1 114.1(6) . . ? O4 C8 O3 124.4(7) . . ? O4 C8 C6 118.9(7) . . ? O3 C8 C6 116.4(7) . . ? N1 C9 C10 123.7(10) . . ? N1 C9 H9A 118.1 . . ? C10 C9 H9A 118.1 . . ? N1 C13 C12 122.7(10) . . ? N1 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? C11 C12 C13 120.9(10) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C10 C11 C12 116.8(9) . . ? C10 C11 C14 121.0(9) . . ? C12 C11 C14 122.2(10) . . ? C11 C10 C9 120.2(9) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C14 C14 C11 117.2(11) 3_354 . ? C14 C14 H14A 108.0 3_354 . ? C11 C14 H14A 108.0 . . ? C14 C14 H14B 108.0 3_354 . ? C11 C14 H14B 108.0 . . ? H14A C14 H14B 107.2 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.683 _refine_diff_density_min -1.258 _refine_diff_density_rms 0.114 #================END